# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_p_1
_database_code_depnum_ccdc_archive 'CCDC 1971987'
loop_
_audit_author_name
_audit_author_address
'Alasdair McKay'
;Monash University
Australia
;
_audit_update_record             
;
2019-12-14 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT232_p_1                 
;
PROBLEM: Hirshfeld Test Diff (M-X)  Rh1      --C2_a     .       11.5 s.u.
RESPONSE: Several Carbon atoms associated with bridging CO moieties display  prolate ellipsoids. Attempts to model these as disorder were unsuccessful.
;
# Added during the CSD deposition process: Saturday 14 December 2019 01:17 PM
# end Validation Reply Form

_audit_creation_date             2019-12-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
''
alasdair.mckay@monash.edu
_chemical_name_common            ?
_chemical_name_systematic        '[{Rh(CO)2(N3Dipp2)}2]'
_chemical_formula_moiety         '2(C26 H34 N3 O2 Rh)'
_chemical_formula_sum            'C52 H68 N6 O4 Rh2'
_chemical_formula_weight         1046.94
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.2722(5)
_cell_length_b                   13.4363(5)
_cell_length_c                   15.3662(7)
_cell_angle_alpha                81.307(2)
_cell_angle_beta                 74.676(2)
_cell_angle_gamma                77.317(2)
_cell_volume                     2565.68(18)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2611
_cell_measurement_temperature    150
_cell_measurement_theta_max      23.36
_cell_measurement_theta_min      2.45
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.691
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.1342 before and 0.0579 after correction. The Ratio of minimum to maximum transmission is 0.8940. The λ/2 correction factor is 0.00150.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_av_unetI/netI     0.0771
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            39793
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.177
_diffrn_reflns_theta_min         1.620
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7895
_reflns_number_total             11201
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.830
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     593
_refine_ls_number_reflns         11201
_refine_ls_number_restraints     467
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0409
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0323P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0780
_refine_ls_wR_factor_ref         0.0891
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Rh2-C28 \\sim Rh2_$1-C28
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Rh2 \\sim C28 \\sim O4: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Ternary CH refined with riding coordinates:
 C35(H35), C47(H47), C9(H9), C38(H38), C24(H24), C50(H50), C12(H12), C21(H21)
5.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C19(H19), C17(H17), C32(H32), C33(H33), C18(H18), C43(H43),
 C45(H45), C44(H44), C7(H7), C6(H6), C5(H5)
5.c Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C48(H48A,H48B,H48C), C25(H25A,H25B,H25C), C49(H49A,H49B,
 H49C), C37(H37A,H37B,H37C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C51(H51A,
 H51B,H51C), C11(H11A,H11B,H11C), C52(H52A,H52B,H52C), C26(H26A,H26B,H26C),
 C10(H10A,H10B,H10C), C40(H40A,H40B,H40C), C39(H39A,H39B,H39C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.57880(2) 0.46754(2) 0.53400(2) 0.01653(8) Uani 1 1 d . U . . .
Rh2 Rh -0.05095(2) 1.05818(2) 0.06004(2) 0.01823(8) Uani 1 1 d D U . . .
N4 N 0.07533(19) 1.00506(18) 0.11976(17) 0.0173(6) Uani 1 1 d . U . . .
N6 N 0.16756(18) 0.90601(19) 0.01133(18) 0.0181(6) Uani 1 1 d . U . . .
C1 C 0.7008(3) 0.4179(3) 0.5840(3) 0.0294(9) Uani 1 1 d . U . . .
N1 N 0.64101(18) 0.58754(18) 0.45570(17) 0.0169(6) Uani 1 1 d . U . . .
N3 N 0.50043(19) 0.64716(18) 0.39729(18) 0.0187(6) Uani 1 1 d . U . . .
N5 N 0.16078(19) 0.94134(19) 0.08688(18) 0.0182(6) Uani 1 1 d . U . . .
N2 N 0.59446(19) 0.65595(18) 0.40156(18) 0.0178(6) Uani 1 1 d . U . . .
C15 C 0.4577(2) 0.7235(2) 0.3322(2) 0.0191(7) Uani 1 1 d . U . . .
C29 C 0.0742(2) 1.0389(2) 0.2047(2) 0.0187(7) Uani 1 1 d . U . . .
O1 O 0.77226(19) 0.3906(2) 0.6135(2) 0.0502(8) Uani 1 1 d . U . . .
C3 C 0.7451(2) 0.6051(2) 0.4570(2) 0.0198(7) Uani 1 1 d . U . . .
C31 C 0.1072(3) 1.1596(3) 0.2884(2) 0.0275(8) Uani 1 1 d . U . . .
H31 H 0.136174 1.217651 0.290448 0.033 Uiso 1 1 calc R . . . .
C16 C 0.4887(2) 0.7079(2) 0.2409(2) 0.0234(7) Uani 1 1 d . U . . .
C8 C 0.7530(3) 0.6605(2) 0.5237(2) 0.0255(8) Uani 1 1 d . U . . .
C19 C 0.3323(3) 0.8736(2) 0.3032(3) 0.0318(9) Uani 1 1 d . U . . .
H19 H 0.280219 0.931448 0.323468 0.038 Uiso 1 1 calc R . . . .
C46 C 0.3492(2) 0.8715(2) -0.0831(2) 0.0249(8) Uani 1 1 d . U . . .
C30 C 0.1176(2) 1.1252(2) 0.2047(2) 0.0220(7) Uani 1 1 d . U . . .
C17 C 0.4365(3) 0.7765(3) 0.1821(3) 0.0304(8) Uani 1 1 d . U . . .
H17 H 0.454906 0.766633 0.119451 0.036 Uiso 1 1 calc R . . . .
C35 C 0.1750(3) 1.1802(3) 0.1193(2) 0.0287(8) Uani 1 1 d . U . . .
H35 H 0.180176 1.141116 0.067323 0.034 Uiso 1 1 calc R . . . .
C32 C 0.0561(3) 1.1114(3) 0.3679(2) 0.0306(8) Uani 1 1 d . U . . .
H32 H 0.049227 1.136754 0.424017 0.037 Uiso 1 1 calc R . . . .
C20 C 0.3801(2) 0.8064(2) 0.3653(2) 0.0267(8) Uani 1 1 d . U . . .
C33 C 0.0151(3) 1.0271(2) 0.3662(2) 0.0264(8) Uani 1 1 d . U . . .
H33 H -0.019381 0.994015 0.421719 0.032 Uiso 1 1 calc R . . . .
C18 C 0.3593(3) 0.8575(3) 0.2128(3) 0.0339(9) Uani 1 1 d . U . . .
H18 H 0.324135 0.902891 0.171656 0.041 Uiso 1 1 calc R . . . .
C34 C 0.0225(2) 0.9885(2) 0.2852(2) 0.0219(7) Uani 1 1 d . U . . .
C47 C 0.1841(3) 0.6872(3) 0.0801(3) 0.0320(9) Uani 1 1 d . U . . .
H47 H 0.129187 0.745802 0.105945 0.038 Uiso 1 1 calc R . . . .
C4 C 0.8351(2) 0.5593(2) 0.3953(2) 0.0247(8) Uani 1 1 d . U . . .
C36 C 0.2885(3) 1.1823(3) 0.1246(3) 0.0422(10) Uani 1 1 d . U . . .
H36A H 0.285365 1.223406 0.173081 0.063 Uiso 1 1 calc GR . . . .
H36B H 0.326850 1.212646 0.066612 0.063 Uiso 1 1 calc GR . . . .
H36C H 0.325648 1.112203 0.137390 0.063 Uiso 1 1 calc GR . . . .
C43 C 0.3703(3) 0.6652(3) -0.0167(2) 0.0314(9) Uani 1 1 d . U . . .
H43 H 0.378399 0.594532 0.004884 0.038 Uiso 1 1 calc R . . . .
C41 C 0.2665(2) 0.8351(2) -0.0181(2) 0.0195(7) Uani 1 1 d . U . . .
C9 C 0.8300(3) 0.4974(3) 0.3227(3) 0.0362(9) Uani 1 1 d . U . . .
H9 H 0.753615 0.507375 0.320797 0.043 Uiso 1 1 calc R . . . .
C45 C 0.4424(3) 0.8021(3) -0.1121(3) 0.0318(9) Uani 1 1 d . U . . .
H45 H 0.499932 0.825334 -0.155825 0.038 Uiso 1 1 calc R . . . .
C44 C 0.4531(3) 0.7003(3) -0.0788(3) 0.0329(9) Uani 1 1 d . U . . .
H44 H 0.517957 0.654236 -0.098968 0.040 Uiso 1 1 calc R . . . .
C7 C 0.8542(3) 0.6675(3) 0.5292(3) 0.0331(9) Uani 1 1 d . U . . .
H7 H 0.861488 0.704204 0.574742 0.040 Uiso 1 1 calc R . . . .
C6 C 0.9428(3) 0.6228(3) 0.4706(3) 0.0356(9) Uani 1 1 d . U . . .
H6 H 1.011142 0.628520 0.475510 0.043 Uiso 1 1 calc R . . . .
C42 C 0.2748(2) 0.7305(2) 0.0155(2) 0.0236(7) Uani 1 1 d . U . . .
C38 C -0.0178(3) 0.8921(3) 0.2844(2) 0.0307(8) Uani 1 1 d . U . . .
H38 H -0.021231 0.887971 0.220796 0.037 Uiso 1 1 calc R . . . .
C5 C 0.9340(3) 0.5693(3) 0.4044(3) 0.0339(9) Uani 1 1 d . U . . .
H5 H 0.996616 0.538525 0.363985 0.041 Uiso 1 1 calc R . . . .
C48 C 0.2200(3) 0.6167(3) 0.1592(3) 0.0472(11) Uani 1 1 d . U . . .
H48A H 0.269353 0.555436 0.136072 0.071 Uiso 1 1 calc GR . . . .
H48B H 0.157836 0.596286 0.203097 0.071 Uiso 1 1 calc GR . . . .
H48C H 0.255781 0.653305 0.188868 0.071 Uiso 1 1 calc GR . . . .
C24 C 0.3519(3) 0.8240(3) 0.4644(3) 0.0340(9) Uani 1 1 d . U . . .
H24 H 0.363942 0.755118 0.499355 0.041 Uiso 1 1 calc R . . . .
C25 C 0.2363(3) 0.8731(3) 0.5002(3) 0.0614(13) Uani 1 1 d . U . . .
H25A H 0.189884 0.834262 0.485003 0.092 Uiso 1 1 calc GR . . . .
H25B H 0.223334 0.943908 0.472516 0.092 Uiso 1 1 calc GR . . . .
H25C H 0.221145 0.872800 0.566218 0.092 Uiso 1 1 calc GR . . . .
C50 C 0.3402(3) 0.9838(3) -0.1192(3) 0.0414(10) Uani 1 1 d . U . . .
H50 H 0.262982 1.015782 -0.106679 0.050 Uiso 1 1 calc R . . . .
C49 C 0.1331(3) 0.6306(3) 0.0301(3) 0.0534(12) Uani 1 1 d . U . . .
H49A H 0.112648 0.675924 -0.021205 0.080 Uiso 1 1 calc GR . . . .
H49B H 0.069678 0.609465 0.071485 0.080 Uiso 1 1 calc GR . . . .
H49C H 0.183882 0.569830 0.007638 0.080 Uiso 1 1 calc GR . . . .
C37 C 0.1146(3) 1.2891(3) 0.1009(3) 0.0501(11) Uani 1 1 d . U . . .
H37A H 0.041565 1.286710 0.100303 0.075 Uiso 1 1 calc GR . . . .
H37B H 0.150261 1.319934 0.042059 0.075 Uiso 1 1 calc GR . . . .
H37C H 0.113417 1.330434 0.148716 0.075 Uiso 1 1 calc GR . . . .
C13 C 0.6544(3) 0.8270(3) 0.5857(3) 0.0524(12) Uani 1 1 d . U . . .
H13A H 0.657687 0.858068 0.523283 0.079 Uiso 1 1 calc GR . . . .
H13B H 0.715438 0.837650 0.605214 0.079 Uiso 1 1 calc GR . . . .
H13C H 0.588340 0.858901 0.625746 0.079 Uiso 1 1 calc GR . . . .
C12 C 0.6569(3) 0.7121(3) 0.5900(3) 0.0370(9) Uani 1 1 d . U . . .
H12 H 0.592133 0.703809 0.572337 0.044 Uiso 1 1 calc R . . . .
C14 C 0.6514(4) 0.6612(3) 0.6862(3) 0.0572(12) Uani 1 1 d . U . . .
H14A H 0.714716 0.666901 0.705068 0.086 Uiso 1 1 calc GR . . . .
H14B H 0.648393 0.588634 0.688017 0.086 Uiso 1 1 calc GR . . . .
H14C H 0.587583 0.695143 0.727346 0.086 Uiso 1 1 calc GR . . . .
C51 C 0.3928(4) 1.0357(3) -0.0679(3) 0.0724(15) Uani 1 1 d . U . . .
H51A H 0.360651 1.025412 -0.002845 0.109 Uiso 1 1 calc GR . . . .
H51B H 0.382978 1.109278 -0.087855 0.109 Uiso 1 1 calc GR . . . .
H51C H 0.468955 1.006319 -0.079776 0.109 Uiso 1 1 calc GR . . . .
C11 C 0.8682(3) 0.3831(3) 0.3457(3) 0.0623(14) Uani 1 1 d . U . . .
H11A H 0.942547 0.370942 0.349362 0.093 Uiso 1 1 calc GR . . . .
H11B H 0.862334 0.344858 0.298278 0.093 Uiso 1 1 calc GR . . . .
H11C H 0.824182 0.360121 0.404068 0.093 Uiso 1 1 calc GR . . . .
C52 C 0.3871(4) 1.0013(3) -0.2214(3) 0.0646(13) Uani 1 1 d . U . . .
H52A H 0.369351 1.074311 -0.241819 0.097 Uiso 1 1 calc GR . . . .
H52B H 0.357230 0.961463 -0.253449 0.097 Uiso 1 1 calc GR . . . .
H52C H 0.464531 0.979326 -0.234494 0.097 Uiso 1 1 calc GR . . . .
C26 C 0.4261(4) 0.8857(4) 0.4833(3) 0.0689(15) Uani 1 1 d . U . . .
H26A H 0.412044 0.889078 0.548755 0.103 Uiso 1 1 calc GR . . . .
H26B H 0.413790 0.955204 0.452749 0.103 Uiso 1 1 calc GR . . . .
H26C H 0.500096 0.852415 0.460440 0.103 Uiso 1 1 calc GR . . . .
C10 C 0.8909(4) 0.5337(4) 0.2299(3) 0.0718(15) Uani 1 1 d . U . . .
H10A H 0.966767 0.521738 0.228560 0.108 Uiso 1 1 calc GR . . . .
H10B H 0.865035 0.607075 0.216435 0.108 Uiso 1 1 calc GR . . . .
H10C H 0.880339 0.495707 0.184301 0.108 Uiso 1 1 calc GR . . . .
O2 O 0.40526(19) 0.62300(18) 0.64678(17) 0.0382(7) Uani 1 1 d . U . . .
O4 O 0.09257(19) 1.1736(2) -0.09092(19) 0.0461(7) Uani 1 1 d . U . . .
C21 C 0.5731(3) 0.6175(3) 0.2049(2) 0.0317(9) Uani 1 1 d . U . . .
H21 H 0.605023 0.581756 0.255989 0.038 Uiso 1 1 calc R . . . .
C2 C 0.4452(3) 0.5727(3) 0.5893(3) 0.0321(9) Uani 1 1 d . U . . .
O3 O -0.1804(2) 1.1887(3) 0.2127(2) 0.0852(13) Uani 1 1 d . U . . .
C27 C -0.1330(3) 1.1400(3) 0.1561(3) 0.0433(11) Uani 1 1 d . U . . .
C28 C 0.0526(3) 1.1049(4) -0.0526(3) 0.0596(14) Uani 1 1 d D U . . .
C40 C -0.1292(3) 0.8911(3) 0.3451(3) 0.0474(11) Uani 1 1 d . U . . .
H40A H -0.127347 0.890561 0.408552 0.071 Uiso 1 1 calc GR . . . .
H40B H -0.153475 0.829737 0.337834 0.071 Uiso 1 1 calc GR . . . .
H40C H -0.178197 0.952418 0.328039 0.071 Uiso 1 1 calc GR . . . .
C39 C 0.0605(3) 0.7995(3) 0.3101(3) 0.0563(13) Uani 1 1 d . U . . .
H39A H 0.131159 0.801559 0.270095 0.084 Uiso 1 1 calc GR . . . .
H39B H 0.037658 0.736888 0.303814 0.084 Uiso 1 1 calc GR . . . .
H39C H 0.063368 0.799990 0.373108 0.084 Uiso 1 1 calc GR . . . .
C22 C 0.5252(4) 0.5406(3) 0.1732(4) 0.0694(15) Uani 1 1 d . U . . .
H22A H 0.498580 0.571666 0.119680 0.104 Uiso 1 1 calc GR . . . .
H22B H 0.466299 0.521020 0.221852 0.104 Uiso 1 1 calc GR . . . .
H22C H 0.579735 0.479608 0.157722 0.104 Uiso 1 1 calc GR . . . .
C23 C 0.6619(4) 0.6513(4) 0.1295(3) 0.0840(18) Uani 1 1 d . U . . .
H23A H 0.696356 0.695910 0.152322 0.126 Uiso 1 1 calc GR . . . .
H23B H 0.632573 0.688819 0.079144 0.126 Uiso 1 1 calc GR . . . .
H23C H 0.714329 0.590894 0.108295 0.126 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 Rh1 2.5113(5) 2_666 ?
Rh1 C1 1.920(3) . ?
Rh1 N1 2.050(2) . ?
Rh1 N3 2.056(3) 2_666 ?
Rh1 C2 2.165(4) 2_666 ?
Rh1 C2 2.081(4) . ?
Rh2 Rh2 2.5106(5) 2_575 ?
Rh2 N4 2.062(2) . ?
Rh2 N6 2.059(2) 2_575 ?
Rh2 C27 1.921(4) . ?
Rh2 C28 2.217(5) 2_575 ?
Rh2 C28 2.018(4) . ?
N4 N5 1.295(3) . ?
N4 C29 1.441(4) . ?
N6 N5 1.294(3) . ?
N6 C41 1.451(4) . ?
C1 O1 1.124(4) . ?
N1 N2 1.308(3) . ?
N1 C3 1.457(4) . ?
N3 N2 1.299(3) . ?
N3 C15 1.452(4) . ?
C15 C16 1.388(5) . ?
C15 C20 1.396(4) . ?
C29 C30 1.404(4) . ?
C29 C34 1.400(4) . ?
C3 C8 1.393(4) . ?
C3 C4 1.399(4) . ?
C31 C30 1.393(4) . ?
C31 C32 1.374(5) . ?
C16 C17 1.395(4) . ?
C16 C21 1.521(4) . ?
C8 C7 1.393(4) . ?
C8 C12 1.511(5) . ?
C19 C20 1.391(4) . ?
C19 C18 1.378(5) . ?
C46 C41 1.396(4) . ?
C46 C45 1.387(4) . ?
C46 C50 1.517(5) . ?
C30 C35 1.508(5) . ?
C17 C18 1.367(5) . ?
C35 C36 1.536(4) . ?
C35 C37 1.531(5) . ?
C32 C33 1.367(4) . ?
C20 C24 1.512(5) . ?
C33 C34 1.391(4) . ?
C34 C38 1.509(4) . ?
C47 C42 1.507(5) . ?
C47 C48 1.537(5) . ?
C47 C49 1.518(5) . ?
C4 C9 1.513(5) . ?
C4 C5 1.393(4) . ?
C43 C44 1.370(5) . ?
C43 C42 1.391(4) . ?
C41 C42 1.413(4) . ?
C9 C11 1.526(5) . ?
C9 C10 1.509(5) . ?
C45 C44 1.377(5) . ?
C7 C6 1.360(5) . ?
C6 C5 1.373(5) . ?
C38 C40 1.527(5) . ?
C38 C39 1.512(5) . ?
C24 C25 1.520(5) . ?
C24 C26 1.524(5) . ?
C50 C51 1.505(6) . ?
C50 C52 1.532(6) . ?
C13 C12 1.528(5) . ?
C12 C14 1.522(5) . ?
O2 C2 1.138(4) . ?
O4 C28 1.169(5) . ?
C21 C22 1.521(5) . ?
C21 C23 1.514(5) . ?
O3 C27 1.132(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Rh1 Rh1 179.03(11) . 2_666 ?
C1 Rh1 N1 93.62(12) . . ?
C1 Rh1 N3 94.44(12) . 2_666 ?
C1 Rh1 C2 127.03(15) . 2_666 ?
C1 Rh1 C2 125.47(15) . . ?
N1 Rh1 Rh1 85.78(7) . 2_666 ?
N1 Rh1 N3 171.85(9) . 2_666 ?
N1 Rh1 C2 86.64(11) . 2_666 ?
N1 Rh1 C2 88.41(11) . . ?
N3 Rh1 Rh1 86.14(7) 2_666 2_666 ?
N3 Rh1 C2 87.92(11) 2_666 . ?
N3 Rh1 C2 87.52(12) 2_666 2_666 ?
C2 Rh1 Rh1 55.30(11) . 2_666 ?
C2 Rh1 Rh1 52.20(9) 2_666 2_666 ?
C2 Rh1 C2 107.50(13) . 2_666 ?
N4 Rh2 Rh2 85.62(7) . 2_575 ?
N4 Rh2 C28 86.59(11) . 2_575 ?
N6 Rh2 Rh2 86.23(7) 2_575 2_575 ?
N6 Rh2 N4 171.65(9) 2_575 . ?
N6 Rh2 C28 86.79(11) 2_575 2_575 ?
C27 Rh2 Rh2 176.33(13) . 2_575 ?
C27 Rh2 N4 94.29(12) . . ?
C27 Rh2 N6 93.72(12) . 2_575 ?
C27 Rh2 C28 126.28(17) . 2_575 ?
C27 Rh2 C28 126.3(2) . . ?
C28 Rh2 Rh2 57.39(15) . 2_575 ?
C28 Rh2 Rh2 50.06(11) 2_575 2_575 ?
C28 Rh2 N4 88.30(12) . . ?
C28 Rh2 N6 88.84(12) . 2_575 ?
C28 Rh2 C28 107.45(16) . 2_575 ?
N5 N4 Rh2 125.30(19) . . ?
N5 N4 C29 114.1(2) . . ?
C29 N4 Rh2 120.63(18) . . ?
N5 N6 Rh2 124.77(19) . 2_575 ?
N5 N6 C41 112.7(2) . . ?
C41 N6 Rh2 122.47(19) . 2_575 ?
O1 C1 Rh1 178.7(3) . . ?
N2 N1 Rh1 125.75(19) . . ?
N2 N1 C3 112.9(2) . . ?
C3 N1 Rh1 121.38(18) . . ?
N2 N3 Rh1 125.25(19) . 2_666 ?
N2 N3 C15 112.9(2) . . ?
C15 N3 Rh1 121.71(18) . 2_666 ?
N6 N5 N4 118.0(2) . . ?
N3 N2 N1 117.0(2) . . ?
C16 C15 N3 119.4(3) . . ?
C16 C15 C20 122.3(3) . . ?
C20 C15 N3 118.1(3) . . ?
C30 C29 N4 119.6(3) . . ?
C34 C29 N4 118.4(3) . . ?
C34 C29 C30 121.8(3) . . ?
C8 C3 N1 119.0(3) . . ?
C8 C3 C4 121.9(3) . . ?
C4 C3 N1 119.0(3) . . ?
C32 C31 C30 121.5(3) . . ?
C15 C16 C17 117.6(3) . . ?
C15 C16 C21 122.4(3) . . ?
C17 C16 C21 120.0(3) . . ?
C3 C8 C7 117.9(3) . . ?
C3 C8 C12 122.8(3) . . ?
C7 C8 C12 119.2(3) . . ?
C18 C19 C20 121.0(3) . . ?
C41 C46 C50 121.7(3) . . ?
C45 C46 C41 117.9(3) . . ?
C45 C46 C50 120.4(3) . . ?
C29 C30 C35 123.0(3) . . ?
C31 C30 C29 117.4(3) . . ?
C31 C30 C35 119.6(3) . . ?
C18 C17 C16 121.3(3) . . ?
C30 C35 C36 110.4(3) . . ?
C30 C35 C37 111.7(3) . . ?
C37 C35 C36 110.4(3) . . ?
C33 C32 C31 120.1(3) . . ?
C15 C20 C24 121.0(3) . . ?
C19 C20 C15 117.6(3) . . ?
C19 C20 C24 121.4(3) . . ?
C32 C33 C34 121.6(3) . . ?
C17 C18 C19 120.2(3) . . ?
C29 C34 C38 121.1(3) . . ?
C33 C34 C29 117.6(3) . . ?
C33 C34 C38 121.2(3) . . ?
C42 C47 C48 111.9(3) . . ?
C42 C47 C49 110.6(3) . . ?
C49 C47 C48 110.6(3) . . ?
C3 C4 C9 123.4(3) . . ?
C5 C4 C3 117.3(3) . . ?
C5 C4 C9 119.2(3) . . ?
C44 C43 C42 121.7(3) . . ?
C46 C41 N6 118.6(3) . . ?
C46 C41 C42 121.8(3) . . ?
C42 C41 N6 119.5(3) . . ?
C4 C9 C11 111.3(3) . . ?
C10 C9 C4 112.2(3) . . ?
C10 C9 C11 110.8(3) . . ?
C44 C45 C46 121.3(3) . . ?
C43 C44 C45 120.1(3) . . ?
C6 C7 C8 121.2(3) . . ?
C7 C6 C5 120.3(3) . . ?
C43 C42 C47 119.6(3) . . ?
C43 C42 C41 117.2(3) . . ?
C41 C42 C47 123.2(3) . . ?
C34 C38 C40 113.2(3) . . ?
C34 C38 C39 109.6(3) . . ?
C39 C38 C40 110.9(3) . . ?
C6 C5 C4 121.4(3) . . ?
C20 C24 C25 114.0(3) . . ?
C20 C24 C26 110.8(3) . . ?
C25 C24 C26 110.6(3) . . ?
C46 C50 C52 113.6(3) . . ?
C51 C50 C46 109.0(3) . . ?
C51 C50 C52 110.5(3) . . ?
C8 C12 C13 111.7(3) . . ?
C8 C12 C14 111.3(3) . . ?
C14 C12 C13 111.0(3) . . ?
C22 C21 C16 111.6(3) . . ?
C23 C21 C16 112.1(3) . . ?
C23 C21 C22 110.2(4) . . ?
Rh1 C2 Rh1 72.50(13) . 2_666 ?
O2 C2 Rh1 145.9(3) . . ?
O2 C2 Rh1 141.6(3) . 2_666 ?
O3 C27 Rh2 179.2(4) . . ?
Rh2 C28 Rh2 72.55(16) . 2_575 ?
O4 C28 Rh2 142.7(4) . 2_575 ?
O4 C28 Rh2 144.8(4) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4
_database_code_depnum_ccdc_archive 'CCDC 1971990'
loop_
_audit_author_name
_audit_author_address
'Alasdair McKay'
;Monash University
Australia
;
_audit_update_record             
;
2019-12-14 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_audit_creation_date             2019-12-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
''
alasdair.mckay@monash.edu
_chemical_name_common            ?
_chemical_name_systematic        '[Rh(cod)(DippForm)]'
_chemical_formula_moiety         'C33 H47 N2 Rh'
_chemical_formula_sum            'C33 H47 N2 Rh'
_chemical_formula_weight         574.63
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.5092(6)
_cell_length_b                   11.2966(6)
_cell_length_c                   14.1488(7)
_cell_angle_alpha                93.648(2)
_cell_angle_beta                 102.187(2)
_cell_angle_gamma                113.466(2)
_cell_volume                     1485.51(14)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6469
_cell_measurement_temperature    150
_cell_measurement_theta_max      26.92
_cell_measurement_theta_min      2.31
_shelx_estimated_absorpt_T_max   0.959
_shelx_estimated_absorpt_T_min   0.959
_exptl_absorpt_coefficient_mu    0.598
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.1812 before and 0.0676 after correction. The Ratio of minimum to maximum transmission is 0.9192. The λ/2 correction factor is 0.00150.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0676
_diffrn_reflns_av_unetI/netI     0.0757
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22600
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.152
_diffrn_reflns_theta_min         2.831
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4912
_reflns_number_total             6536
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.622
_refine_diff_density_min         -1.507
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       0.0034(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         6536
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0460
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0464P)²+0.3260P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1134
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C21A-C20 \\sim C21-C20
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C20 \\sim C21: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C20 \\sim C21A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
4. Rigid body (RIGU) restrains
 C20, C21
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C20, C21A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(1)
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C10(H10), C7(H7), C23(H23), C20(H20)
6.b Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C29(H29A,H29B), C32(H32A,H32B), C28(H28A,H28B)
6.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C16(H16), C17(H17), C5(H5), C18(H18), C3(H3), C4(H4)
6.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C8(H8A,H8B,H8C),
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C22(H22A,H22B,H22C), C21(H21A,H21B,
 H21C), C21A(H21D,H21E,H21F)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.82606(3) 0.69052(2) 0.70305(2) 0.03563(12) Uani 1 1 d . . . . .
N1 N 0.8139(3) 0.5036(2) 0.7186(2) 0.0345(6) Uani 1 1 d . . . . .
N2 N 0.9574(3) 0.6756(3) 0.8321(2) 0.0375(7) Uani 1 1 d . . . . .
C14 C 1.0607(4) 0.7443(3) 0.9224(3) 0.0358(8) Uani 1 1 d . . . . .
C13 C 0.8966(3) 0.5483(3) 0.8093(2) 0.0333(7) Uani 1 1 d . . . . .
H13 H 0.910444 0.492415 0.853907 0.040 Uiso 1 1 calc R . . . .
C1 C 0.7166(4) 0.3709(3) 0.6856(2) 0.0356(8) Uani 1 1 d . . . . .
C15 C 1.0165(4) 0.7706(3) 1.0048(3) 0.0393(8) Uani 1 1 d . . . . .
C6 C 0.7502(4) 0.2948(3) 0.6206(2) 0.0412(9) Uani 1 1 d . . . . .
C16 C 1.1217(4) 0.8375(4) 1.0918(3) 0.0479(9) Uani 1 1 d . . . . .
H16 H 1.093607 0.854324 1.148884 0.057 Uiso 1 1 calc R . . . .
C10 C 0.8829(4) 0.3566(4) 0.5838(3) 0.0549(11) Uani 1 1 d . . . . .
H10 H 0.902365 0.450663 0.583350 0.066 Uiso 1 1 calc R . . . .
C7 C 0.5430(4) 0.3998(3) 0.7772(3) 0.0540(11) Uani 1 1 d . . . . .
H7 H 0.612203 0.493450 0.784386 0.065 Uiso 1 1 calc R . . . .
C30 C 0.9142(5) 0.8938(4) 0.7022(3) 0.0481(10) Uani 1 1 d . . . . .
C17 C 1.2645(4) 0.8792(3) 1.0962(3) 0.0556(11) Uani 1 1 d . . . . .
H17 H 1.334650 0.923452 1.156242 0.067 Uiso 1 1 calc R . . . .
C26 C 0.6375(4) 0.6358(4) 0.5914(3) 0.0430(9) Uani 1 1 d . . . . .
C5 C 0.6583(5) 0.1638(4) 0.5916(3) 0.0501(10) Uani 1 1 d . . . . .
H5 H 0.680517 0.110590 0.549167 0.060 Uiso 1 1 calc R . . . .
C2 C 0.5881(4) 0.3179(3) 0.7133(3) 0.0438(9) Uani 1 1 d . . . . .
C31 C 0.7878(5) 0.8571(3) 0.7329(3) 0.0470(9) Uani 1 1 d . . . . .
C23 C 0.8598(4) 0.7282(4) 1.0025(3) 0.0505(10) Uani 1 1 d . . . . .
H23 H 0.802646 0.689777 0.933191 0.061 Uiso 1 1 calc R . . . .
C33 C 0.5514(4) 0.7091(4) 0.6127(3) 0.0533(10) Uani 1 1 d . . . . .
H33A H 0.486498 0.660705 0.652249 0.064 Uiso 1 1 calc R . . . .
H33B H 0.491403 0.713810 0.550212 0.064 Uiso 1 1 calc R . . . .
C27 C 0.7549(4) 0.6847(4) 0.5515(3) 0.0466(9) Uani 1 1 d . . . . .
C18 C 1.3061(4) 0.8567(4) 1.0134(4) 0.0661(13) Uani 1 1 d . . . . .
H18 H 1.405466 0.888066 1.016436 0.079 Uiso 1 1 calc R . . . .
C9 C 0.3927(5) 0.3888(4) 0.7299(3) 0.0621(12) Uani 1 1 d . . . . .
H9A H 0.321568 0.299339 0.726702 0.093 Uiso 1 1 calc GR . . . .
H9B H 0.388480 0.409815 0.663473 0.093 Uiso 1 1 calc GR . . . .
H9C H 0.371885 0.450147 0.769168 0.093 Uiso 1 1 calc GR . . . .
C19 C 1.2058(4) 0.7893(3) 0.9257(3) 0.0549(11) Uani 1 1 d . . . . .
C24 C 0.8140(5) 0.6216(4) 1.0642(3) 0.0652(12) Uani 1 1 d . . . . .
H24A H 0.835208 0.549287 1.041634 0.098 Uiso 1 1 calc GR . . . .
H24B H 0.710662 0.589558 1.057893 0.098 Uiso 1 1 calc GR . . . .
H24C H 0.866503 0.656929 1.133037 0.098 Uiso 1 1 calc GR . . . .
C29 C 0.9285(5) 0.9220(4) 0.6019(3) 0.0604(11) Uani 1 1 d . . . . .
H29A H 1.023315 0.929255 0.595642 0.072 Uiso 1 1 calc R . . . .
H29B H 0.925258 1.007339 0.594364 0.072 Uiso 1 1 calc R . . . .
C25 C 0.8256(5) 0.8413(5) 1.0341(4) 0.0757(14) Uani 1 1 d . . . . .
H25A H 0.870316 0.873826 1.104248 0.114 Uiso 1 1 calc GR . . . .
H25B H 0.721289 0.810796 1.021549 0.114 Uiso 1 1 calc GR . . . .
H25C H 0.863024 0.911852 0.996815 0.114 Uiso 1 1 calc GR . . . .
C3 C 0.4991(5) 0.1854(3) 0.6820(3) 0.0518(10) Uani 1 1 d . . . . .
H3 H 0.412309 0.147126 0.701478 0.062 Uiso 1 1 calc R . . . .
C32 C 0.6476(5) 0.8469(4) 0.6678(3) 0.0582(11) Uani 1 1 d . . . . .
H32A H 0.669238 0.907528 0.619923 0.070 Uiso 1 1 calc R . . . .
H32B H 0.595502 0.874533 0.708759 0.070 Uiso 1 1 calc R . . . .
C4 C 0.5363(5) 0.1093(3) 0.6228(3) 0.0564(11) Uani 1 1 d . . . . .
H4 H 0.476502 0.018392 0.603640 0.068 Uiso 1 1 calc R . . . .
C28 C 0.8116(5) 0.8175(4) 0.5202(3) 0.0565(11) Uani 1 1 d . . . . .
H28A H 0.731516 0.843193 0.499483 0.068 Uiso 1 1 calc R . . . .
H28B H 0.850613 0.811763 0.463019 0.068 Uiso 1 1 calc R . . . .
C20 C 1.2548(5) 0.7683(4) 0.8342(4) 0.0765(15) Uani 1 1 d D U . . .
H20 H 1.176095 0.693778 0.785368 0.092 Uiso 1 1 calc R . . A 2
C8 C 0.5523(5) 0.3634(4) 0.8785(3) 0.0681(13) Uani 1 1 d . . . . .
H8A H 0.483622 0.272502 0.873975 0.102 Uiso 1 1 calc GR . . . .
H8B H 0.529538 0.421307 0.919712 0.102 Uiso 1 1 calc GR . . . .
H8C H 0.649734 0.372577 0.907610 0.102 Uiso 1 1 calc GR . . . .
C11 C 1.0136(5) 0.3534(6) 0.6524(3) 0.0806(15) Uani 1 1 d . . . . .
H11A H 1.031493 0.401969 0.717326 0.121 Uiso 1 1 calc GR . . . .
H11B H 1.097447 0.393811 0.626281 0.121 Uiso 1 1 calc GR . . . .
H11C H 0.996077 0.262505 0.657836 0.121 Uiso 1 1 calc GR . . . .
C12 C 0.8628(5) 0.2958(5) 0.4784(3) 0.0772(15) Uani 1 1 d . . . . .
H12A H 0.851025 0.205154 0.476877 0.116 Uiso 1 1 calc GR . . . .
H12B H 0.947291 0.346172 0.455420 0.116 Uiso 1 1 calc GR . . . .
H12C H 0.777223 0.297458 0.435540 0.116 Uiso 1 1 calc GR . . . .
C22 C 1.3025(5) 0.8875(5) 0.7898(3) 0.0746(13) Uani 1 1 d . . . . .
H22A H 1.222569 0.912203 0.769839 0.112 Uiso 1 1 calc GR . . . .
H22B H 1.334733 0.870958 0.732197 0.112 Uiso 1 1 calc GR . . . .
H22C H 1.382030 0.958639 0.837651 0.112 Uiso 1 1 calc GR . . . .
C21 C 1.308(3) 0.6733(18) 0.8167(13) 0.068(5) Uani 0.304(16) 1 d D U P B 1
H21A H 1.398311 0.695169 0.865664 0.102 Uiso 0.304(16) 1 calc GR . P B 1
H21B H 1.323854 0.672415 0.751003 0.102 Uiso 0.304(16) 1 calc GR . P B 1
H21C H 1.237267 0.586717 0.821399 0.102 Uiso 0.304(16) 1 calc GR . P B 1
H31 H 0.797(3) 0.868(3) 0.803(2) 0.032(8) Uiso 1 1 d . . . . .
H26 H 0.593(3) 0.548(3) 0.585(2) 0.034(9) Uiso 1 1 d . . . . .
H27 H 0.782(4) 0.627(3) 0.524(2) 0.046(10) Uiso 1 1 d . . . . .
H30 H 0.997(4) 0.928(3) 0.745(3) 0.044(11) Uiso 1 1 d . . . . .
C21A C 1.3953(11) 0.7373(9) 0.8682(8) 0.077(3) Uani 0.696(16) 1 d D U P B 2
H21D H 1.478376 0.817886 0.902738 0.115 Uiso 0.696(16) 1 calc GR . P B 2
H21E H 1.415370 0.703401 0.810223 0.115 Uiso 0.696(16) 1 calc GR . P B 2
H21F H 1.376515 0.671953 0.911923 0.115 Uiso 0.696(16) 1 calc GR . P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 N1 2.092(2) . ?
Rh1 N2 2.104(3) . ?
Rh1 C30 2.109(4) . ?
Rh1 C26 2.094(4) . ?
Rh1 C31 2.110(3) . ?
Rh1 C27 2.105(4) . ?
N1 C13 1.324(4) . ?
N1 C1 1.414(4) . ?
N2 C14 1.425(4) . ?
N2 C13 1.305(4) . ?
C14 C15 1.400(5) . ?
C14 C19 1.391(5) . ?
C1 C6 1.410(4) . ?
C1 C2 1.395(5) . ?
C15 C16 1.396(5) . ?
C15 C23 1.512(5) . ?
C6 C10 1.510(5) . ?
C6 C5 1.380(5) . ?
C16 C17 1.368(5) . ?
C10 C11 1.520(5) . ?
C10 C12 1.537(5) . ?
C7 C2 1.524(4) . ?
C7 C9 1.532(6) . ?
C7 C8 1.510(6) . ?
C30 C31 1.397(5) . ?
C30 C29 1.499(5) . ?
C17 C18 1.377(6) . ?
C26 C33 1.507(5) . ?
C26 C27 1.393(5) . ?
C5 C4 1.365(6) . ?
C2 C3 1.392(5) . ?
C31 C32 1.520(6) . ?
C23 C24 1.515(6) . ?
C23 C25 1.524(6) . ?
C33 C32 1.521(5) . ?
C27 C28 1.512(5) . ?
C18 C19 1.385(6) . ?
C19 C20 1.529(6) . ?
C29 C28 1.521(6) . ?
C3 C4 1.381(5) . ?
C20 C22 1.471(7) . ?
C20 C21 1.422(12) . ?
C20 C21A 1.634(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Rh1 N2 63.49(11) . . ?
N1 Rh1 C30 160.22(15) . . ?
N1 Rh1 C26 98.41(13) . . ?
N1 Rh1 C31 155.23(13) . . ?
N1 Rh1 C27 105.55(12) . . ?
N2 Rh1 C30 102.38(15) . . ?
N2 Rh1 C31 107.61(14) . . ?
N2 Rh1 C27 156.27(13) . . ?
C30 Rh1 C31 38.69(15) . . ?
C26 Rh1 N2 156.15(13) . . ?
C26 Rh1 C30 98.61(16) . . ?
C26 Rh1 C31 82.17(16) . . ?
C26 Rh1 C27 38.75(14) . . ?
C27 Rh1 C30 81.95(16) . . ?
C27 Rh1 C31 90.46(15) . . ?
C13 N1 Rh1 90.47(18) . . ?
C13 N1 C1 123.0(3) . . ?
C1 N1 Rh1 139.5(2) . . ?
C14 N2 Rh1 145.8(2) . . ?
C13 N2 Rh1 90.5(2) . . ?
C13 N2 C14 123.4(3) . . ?
C15 C14 N2 120.3(3) . . ?
C19 C14 N2 118.7(3) . . ?
C19 C14 C15 120.9(3) . . ?
N2 C13 N1 114.2(3) . . ?
C6 C1 N1 118.2(3) . . ?
C2 C1 N1 121.0(3) . . ?
C2 C1 C6 120.8(3) . . ?
C14 C15 C23 122.2(3) . . ?
C16 C15 C14 118.2(3) . . ?
C16 C15 C23 119.6(3) . . ?
C1 C6 C10 120.2(3) . . ?
C5 C6 C1 118.2(3) . . ?
C5 C6 C10 121.6(3) . . ?
C17 C16 C15 121.2(4) . . ?
C6 C10 C11 111.6(3) . . ?
C6 C10 C12 112.9(4) . . ?
C11 C10 C12 110.7(3) . . ?
C2 C7 C9 111.8(3) . . ?
C8 C7 C2 110.9(3) . . ?
C8 C7 C9 111.1(3) . . ?
C31 C30 Rh1 70.7(2) . . ?
C31 C30 C29 125.4(4) . . ?
C29 C30 Rh1 110.7(3) . . ?
C16 C17 C18 119.7(4) . . ?
C33 C26 Rh1 111.5(3) . . ?
C27 C26 Rh1 71.1(2) . . ?
C27 C26 C33 125.0(3) . . ?
C4 C5 C6 121.4(3) . . ?
C1 C2 C7 122.3(3) . . ?
C3 C2 C1 118.6(3) . . ?
C3 C2 C7 119.2(3) . . ?
C30 C31 Rh1 70.6(2) . . ?
C30 C31 C32 122.9(4) . . ?
C32 C31 Rh1 112.7(3) . . ?
C15 C23 C24 110.0(3) . . ?
C15 C23 C25 113.1(3) . . ?
C24 C23 C25 111.0(3) . . ?
C26 C33 C32 111.8(3) . . ?
C26 C27 Rh1 70.2(2) . . ?
C26 C27 C28 124.8(3) . . ?
C28 C27 Rh1 113.5(3) . . ?
C17 C18 C19 121.2(4) . . ?
C14 C19 C20 121.1(4) . . ?
C18 C19 C14 118.7(4) . . ?
C18 C19 C20 120.2(4) . . ?
C30 C29 C28 113.1(3) . . ?
C4 C3 C2 120.4(4) . . ?
C31 C32 C33 112.7(3) . . ?
C5 C4 C3 120.5(4) . . ?
C27 C28 C29 112.2(3) . . ?
C19 C20 C21A 107.8(5) . . ?
C22 C20 C19 111.7(3) . . ?
C22 C20 C21A 106.0(4) . . ?
C21 C20 C19 124.2(8) . . ?
C21 C20 C22 119.1(9) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 1971989'
loop_
_audit_author_name
_audit_author_address
'Alasdair McKay'
;Monash University
Australia
;
_audit_update_record             
;
2019-12-14 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_audit_creation_date             2019-12-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
''
alasdair.mckay@monash.edu
_chemical_name_common            ?
_chemical_name_systematic        '[Rh(N3Dipp2)(COD)]'
_chemical_formula_moiety         'C32 H46 N3 Rh'
_chemical_formula_sum            'C32 H46 N3 Rh'
_chemical_formula_weight         575.63
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   17.0526(8)
_cell_length_b                   8.8969(3)
_cell_length_c                   18.8292(8)
_cell_angle_alpha                90
_cell_angle_beta                 93.738(2)
_cell_angle_gamma                90
_cell_volume                     2850.6(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9825
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      27.10
_cell_measurement_theta_min      2.58
_shelx_estimated_absorpt_T_max   0.907
_shelx_estimated_absorpt_T_min   0.835
_exptl_absorpt_coefficient_mu    0.624
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0902 before and 0.0371 after correction. The Ratio of minimum to maximum transmission is 0.9132. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20172
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.109
_diffrn_reflns_theta_min         3.124
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3107
_reflns_number_total             3153
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.32B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.32B (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         3153
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0189
_refine_ls_R_factor_gt           0.0186
_refine_ls_restrained_S_all      1.117
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0162P)²+3.6497P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0477
_refine_ls_wR_factor_ref         0.0479
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2), C11(H11), C14(H14), C1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B)
2.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C8(H8)
2.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.500000 0.55720(2) 0.750000 0.01210(5) Uani 1 2 d S T P . .
N1 N 0.49132(6) 0.35404(12) 0.69426(6) 0.0139(2) Uani 1 1 d . . . . .
N2 N 0.500000 0.26541(17) 0.750000 0.0130(3) Uani 1 2 d S T P . .
C5 C 0.46815(7) 0.28388(14) 0.62807(7) 0.0132(2) Uani 1 1 d . . . . .
C2 C 0.53599(8) 0.72587(16) 0.67907(7) 0.0193(3) Uani 1 1 d . . . . .
H2 H 0.562848 0.686059 0.637326 0.023 Uiso 1 1 calc R . . . .
C10 C 0.39070(8) 0.22872(15) 0.61584(7) 0.0155(3) Uani 1 1 d . . . . .
C11 C 0.60549(8) 0.33838(16) 0.58820(7) 0.0175(3) Uani 1 1 d . . . . .
H11 H 0.605109 0.413815 0.627547 0.021 Uiso 1 1 calc R . . . .
C14 C 0.33107(8) 0.24365(17) 0.67232(8) 0.0200(3) Uani 1 1 d . . . . .
H14 H 0.357465 0.210996 0.718754 0.024 Uiso 1 1 calc R . . . .
C7 C 0.49860(9) 0.21242(16) 0.51005(7) 0.0200(3) Uani 1 1 d . . . . .
H7 H 0.534689 0.205981 0.473806 0.024 Uiso 1 1 calc R . . . .
C6 C 0.52223(8) 0.27880(15) 0.57495(7) 0.0149(3) Uani 1 1 d . . . . .
C9 C 0.37007(8) 0.16486(16) 0.54964(7) 0.0202(3) Uani 1 1 d . . . . .
H9 H 0.318387 0.126887 0.540132 0.024 Uiso 1 1 calc R . . . .
C12 C 0.66125(9) 0.21197(19) 0.61277(10) 0.0313(4) Uani 1 1 d . . . . .
H12A H 0.641832 0.163503 0.654940 0.047 Uiso 1 1 calc GR . . . .
H12B H 0.713727 0.253444 0.624600 0.047 Uiso 1 1 calc GR . . . .
H12C H 0.664038 0.137747 0.574563 0.047 Uiso 1 1 calc GR . . . .
C3 C 0.57813(9) 0.85664(17) 0.71651(9) 0.0248(3) Uani 1 1 d . . . . .
H3A H 0.543444 0.945967 0.713921 0.030 Uiso 1 1 calc R . . . .
H3B H 0.625936 0.881159 0.691693 0.030 Uiso 1 1 calc R . . . .
C8 C 0.42346(9) 0.15573(17) 0.49750(7) 0.0228(3) Uani 1 1 d . . . . .
H8 H 0.408444 0.110415 0.452990 0.027 Uiso 1 1 calc R . . . .
C13 C 0.63535(10) 0.4173(2) 0.52313(9) 0.0299(4) Uani 1 1 d . . . . .
H13A H 0.640464 0.343909 0.484895 0.045 Uiso 1 1 calc GR . . . .
H13B H 0.686700 0.462772 0.535827 0.045 Uiso 1 1 calc GR . . . .
H13C H 0.598031 0.495789 0.506946 0.045 Uiso 1 1 calc GR . . . .
C15 C 0.25786(8) 0.14641(17) 0.65838(9) 0.0245(3) Uani 1 1 d . . . . .
H15A H 0.226932 0.184510 0.616510 0.037 Uiso 1 1 calc GR . . . .
H15B H 0.226057 0.149958 0.699864 0.037 Uiso 1 1 calc GR . . . .
H15C H 0.273619 0.042388 0.649826 0.037 Uiso 1 1 calc GR . . . .
C4 C 0.60147(9) 0.82098(18) 0.79495(9) 0.0266(3) Uani 1 1 d . . . . .
H4A H 0.655128 0.777984 0.798570 0.032 Uiso 1 1 calc R . . . .
H4B H 0.602617 0.915589 0.822675 0.032 Uiso 1 1 calc R . . . .
C1 C 0.45416(8) 0.71198(16) 0.67294(7) 0.0200(3) Uani 1 1 d . . . . .
H1 H 0.432955 0.664754 0.627468 0.024 Uiso 1 1 calc R . . . .
C16 C 0.30603(10) 0.40715(19) 0.68047(11) 0.0360(4) Uani 1 1 d . . . . .
H16A H 0.352097 0.468380 0.694980 0.054 Uiso 1 1 calc GR . . . .
H16B H 0.267490 0.413936 0.716734 0.054 Uiso 1 1 calc GR . . . .
H16C H 0.282441 0.444110 0.634925 0.054 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 N1 2.0905(11) 2_656 ?
Rh1 N1 2.0905(11) . ?
Rh1 C2 2.1258(13) . ?
Rh1 C2 2.1258(13) 2_656 ?
Rh1 C1 2.1130(13) 2_656 ?
Rh1 C1 2.1130(13) . ?
N1 N2 1.3134(14) . ?
N1 C5 1.4264(16) . ?
C5 C10 1.4137(18) . ?
C5 C6 1.4048(18) . ?
C2 C3 1.517(2) . ?
C2 C1 1.398(2) . ?
C10 C14 1.5245(18) . ?
C10 C9 1.3938(19) . ?
C11 C6 1.5209(18) . ?
C11 C12 1.525(2) . ?
C11 C13 1.528(2) . ?
C14 C15 1.5275(19) . ?
C14 C16 1.527(2) . ?
C7 C6 1.3930(18) . ?
C7 C8 1.383(2) . ?
C9 C8 1.384(2) . ?
C3 C4 1.537(2) . ?
C4 C1 1.510(2) 2_656 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Rh1 N1 60.32(6) 2_656 . ?
N1 Rh1 C2 107.99(5) . . ?
N1 Rh1 C2 107.99(5) 2_656 2_656 ?
N1 Rh1 C2 155.76(5) 2_656 . ?
N1 Rh1 C2 155.76(5) . 2_656 ?
N1 Rh1 C1 101.99(5) 2_656 2_656 ?
N1 Rh1 C1 156.80(5) 2_656 . ?
N1 Rh1 C1 101.99(5) . . ?
N1 Rh1 C1 156.80(5) . 2_656 ?
C2 Rh1 C2 90.19(8) 2_656 . ?
C1 Rh1 C2 38.52(5) 2_656 2_656 ?
C1 Rh1 C2 82.09(6) 2_656 . ?
C1 Rh1 C2 38.52(5) . . ?
C1 Rh1 C2 82.09(6) . 2_656 ?
C1 Rh1 C1 98.66(8) 2_656 . ?
N2 N1 Rh1 96.74(8) . . ?
N2 N1 C5 116.48(11) . . ?
C5 N1 Rh1 145.44(9) . . ?
N1 N2 N1 106.20(15) . 2_656 ?
C10 C5 N1 119.80(11) . . ?
C6 C5 N1 118.61(11) . . ?
C6 C5 C10 121.50(12) . . ?
C3 C2 Rh1 113.39(10) . . ?
C1 C2 Rh1 70.25(8) . . ?
C1 C2 C3 123.11(13) . . ?
C5 C10 C14 120.97(12) . . ?
C9 C10 C5 117.76(12) . . ?
C9 C10 C14 121.24(12) . . ?
C6 C11 C12 110.47(12) . . ?
C6 C11 C13 112.64(11) . . ?
C12 C11 C13 110.39(13) . . ?
C10 C14 C15 113.93(12) . . ?
C10 C14 C16 110.90(13) . . ?
C16 C14 C15 109.04(12) . . ?
C8 C7 C6 121.09(13) . . ?
C5 C6 C11 121.41(11) . . ?
C7 C6 C5 118.20(12) . . ?
C7 C6 C11 120.35(12) . . ?
C8 C9 C10 121.26(13) . . ?
C2 C3 C4 111.92(12) . . ?
C7 C8 C9 120.15(13) . . ?
C1 C4 C3 112.77(12) 2_656 . ?
C2 C1 Rh1 71.24(8) . . ?
C2 C1 C4 124.04(13) . 2_656 ?
C4 C1 Rh1 110.95(9) 2_656 . ?

_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_24
_database_code_depnum_ccdc_archive 'CCDC 1971991'
loop_
_audit_author_name
_audit_author_address
'Alasdair McKay'
;Monash University
Australia
;
_audit_update_record             
;
2019-12-14 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_audit_creation_date             2019-12-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C62 H87 N7 O2 Rh2, 1.5(C6 H14)'
_chemical_formula_sum            'C71 H108 N7 O2 Rh2'
_chemical_formula_weight         1297.46
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.5047(12)
_cell_length_b                   14.7204(12)
_cell_length_c                   18.3174(17)
_cell_angle_alpha                85.510(4)
_cell_angle_beta                 76.563(4)
_cell_angle_gamma                84.116(4)
_cell_volume                     3517.5(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9911
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.912
_cell_measurement_theta_min      2.177
_shelx_estimated_absorpt_T_max   0.990
_shelx_estimated_absorpt_T_min   0.927
_exptl_absorpt_coefficient_mu    0.515
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.1321 before and 0.0558 after correction. The Ratio of minimum to maximum transmission is 0.9226. The λ/2 correction factor is 0.00150.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1378
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0863
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            48305
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.212
_diffrn_reflns_theta_min         2.507
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10217
_reflns_number_total             15295
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.897
_refine_diff_density_min         -0.789
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     786
_refine_ls_number_reflns         15295
_refine_ls_number_restraints     146
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0438
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0422P)²+0.3934P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.1039
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C69-C70 \\sim C70-C71 \\sim C71-C72 \\sim C72-C73 \\sim C73-C74
 with sigma of 0.02
 C69-C71 \\sim C71-C73 \\sim C70-C72 \\sim C72-C74
 with sigma of 0.04
 C63-C64 \\sim C64-C65 \\sim C65-C66 \\sim C66-C67 \\sim C67-C68
 with sigma of 0.02
 C63-C65 \\sim C65-C67 \\sim C64-C66 \\sim C66-C68
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73 \\sim C74: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
C63 \\sim C64 \\sim C65 \\sim C66 \\sim C67 \\sim C68: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 C69, C70, C71, C72, C73, C74
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C63, C64, C65, C66, C67, C68
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C69(0.5) H69A(0.5) H69B(0.5) H69C(0.5) C70(0.5) H70A(0.5)
 H70B(0.5) C71(0.5) H71A(0.5) H71B(0.5) C72(0.5) H72A(0.5) H72B(0.5) C73(0.5)
 H73A(0.5) H73B(0.5) C74(0.5) H74A(0.5) H74B(0.5) H74C(0.5)
6.a Ternary CH refined with riding coordinates:
 C32(H32), C45(H45), C24(H24), C57(H57), C21(H21), C48(H48), C12(H12),
 C36(H36), C60(H60), C9(H9)
6.b Secondary CH2 refined with riding coordinates:
 N7(H7A,H7B), C70(H70A,H70B), C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B),
 C64(H64A,H64B), C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B)
6.c Me refined with riding coordinates:
 C69(H69A,H69B,H69C), C74(H74A,H74B,H74C), C63(H63A,H63B,H63C), C68(H68A,H68B,
 H68C)
6.d Aromatic/amide H refined with riding coordinates:
 C33(H33), C30(H30), C29(H29), C41(H41), C17(H17), C18(H18), C42(H42),
 C19(H19), C54(H54), C7(H7), C53(H53), C43(H43), C55(H55), C5(H5), C6(H6)
6.e Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C35(H35A,H35B,H35C), C58(H58A,H58B,H58C), C22(H22A,H22B,
 H22C), C46(H46A,H46B,H46C), C34(H34A,H34B,H34C), C23(H23A,H23B,H23C), C26(H26A,
 H26B,H26C), C25(H25A,H25B,H25C), C50(H50A,H50B,H50C), C49(H49A,H49B,H49C),
 C59(H59A,H59B,H59C), C37(H37A,H37B,H37C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C61(H61A,H61B,H61C), C11(H11A,H11B,H11C), C10(H10A,H10B,H10C), C38(H38A,
 H38B,H38C), C62(H62A,H62B,H62C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh2 Rh 0.31866(2) 0.21875(2) 0.34457(2) 0.01780(7) Uani 1 1 d . . . . .
Rh1 Rh 0.36207(2) 0.11492(2) 0.23836(2) 0.01971(8) Uani 1 1 d . . . . .
O2 O 0.48757(16) 0.07383(14) 0.35169(12) 0.0287(5) Uani 1 1 d . . . . .
N4 N 0.25276(18) 0.03695(15) 0.30189(14) 0.0194(6) Uani 1 1 d . . . . .
N1 N 0.46032(18) 0.20863(16) 0.18418(14) 0.0223(6) Uani 1 1 d . . . . .
N5 N 0.20074(18) 0.05192(15) 0.36965(14) 0.0197(6) Uani 1 1 d . . . . .
N2 N 0.47606(19) 0.28305(15) 0.21215(14) 0.0204(6) Uani 1 1 d . . . . .
N3 N 0.42047(18) 0.30411(15) 0.27751(14) 0.0187(6) Uani 1 1 d . . . . .
N6 N 0.21934(18) 0.12462(15) 0.39947(14) 0.0187(6) Uani 1 1 d . . . . .
N7 N 0.18704(19) 0.31800(16) 0.38187(16) 0.0301(7) Uani 1 1 d . . . . .
H7A H 0.132678 0.288991 0.377172 0.036 Uiso 1 1 calc R . . . .
H7B H 0.181893 0.318998 0.432229 0.036 Uiso 1 1 calc R . . . .
C2 C 0.4234(2) 0.12014(19) 0.33058(17) 0.0214(7) Uani 1 1 d . . . . .
C33 C 0.1347(2) -0.1147(2) 0.19968(18) 0.0290(8) Uani 1 1 d . . . . .
H33 H 0.084284 -0.110915 0.170736 0.035 Uiso 1 1 calc R . . . .
O1 O 0.4557(2) -0.02793(17) 0.12786(15) 0.0597(8) Uani 1 1 d . . . . .
C27 C 0.2270(2) -0.04484(19) 0.27393(17) 0.0207(7) Uani 1 1 d . . . . .
C15 C 0.4454(2) 0.39080(19) 0.29730(17) 0.0202(7) Uani 1 1 d . . . . .
C28 C 0.2839(2) -0.12839(19) 0.28411(18) 0.0232(7) Uani 1 1 d . . . . .
C30 C 0.1894(3) -0.1975(2) 0.20976(19) 0.0332(8) Uani 1 1 d . . . . .
H30 H 0.176917 -0.250013 0.187385 0.040 Uiso 1 1 calc R . . . .
C40 C 0.2034(2) 0.1303(2) 0.53565(18) 0.0259(8) Uani 1 1 d . . . . .
C31 C 0.1525(2) -0.0367(2) 0.23148(18) 0.0255(7) Uani 1 1 d . . . . .
C29 C 0.2616(3) -0.2041(2) 0.25188(19) 0.0303(8) Uani 1 1 d . . . . .
H29 H 0.297381 -0.261808 0.259293 0.036 Uiso 1 1 calc R . . . .
C41 C 0.1424(3) 0.1482(2) 0.60610(19) 0.0346(9) Uani 1 1 d . . . . .
H41 H 0.172607 0.144594 0.648292 0.041 Uiso 1 1 calc R . . . .
C32 C 0.3637(2) -0.1386(2) 0.32996(19) 0.0279(8) Uani 1 1 d . . . . .
H32 H 0.373281 -0.076101 0.343418 0.034 Uiso 1 1 calc R . . . .
C45 C 0.3158(2) 0.0992(2) 0.52633(18) 0.0280(8) Uani 1 1 d . . . . .
H45 H 0.354051 0.130658 0.479404 0.034 Uiso 1 1 calc R . . . .
C3 C 0.5360(3) 0.1896(2) 0.11561(18) 0.0284(8) Uani 1 1 d . . . . .
C39 C 0.1562(2) 0.13720(19) 0.47419(18) 0.0235(7) Uani 1 1 d . . . . .
C16 C 0.4725(2) 0.3952(2) 0.36631(18) 0.0252(7) Uani 1 1 d . . . . .
C47 C 0.3332(3) -0.0042(2) 0.5166(2) 0.0385(9) Uani 1 1 d . . . . .
H47A H 0.297733 -0.036647 0.562513 0.058 Uiso 1 1 calc GR . . . .
H47B H 0.406518 -0.023190 0.507178 0.058 Uiso 1 1 calc GR . . . .
H47C H 0.306328 -0.018815 0.474037 0.058 Uiso 1 1 calc GR . . . .
C17 C 0.4975(3) 0.4783(2) 0.3849(2) 0.0371(9) Uani 1 1 d . . . . .
H17 H 0.515629 0.482104 0.431561 0.045 Uiso 1 1 calc R . . . .
C20 C 0.4457(2) 0.4688(2) 0.24704(18) 0.0278(8) Uani 1 1 d . . . . .
C24 C 0.4262(3) 0.4694(2) 0.16864(19) 0.0341(9) Uani 1 1 d . . . . .
H24 H 0.392431 0.412957 0.165528 0.041 Uiso 1 1 calc R . . . .
C18 C 0.4966(3) 0.5555(2) 0.3369(2) 0.0453(10) Uani 1 1 d . . . . .
H18 H 0.513163 0.611907 0.350754 0.054 Uiso 1 1 calc R . . . .
C57 C 0.2116(3) 0.4581(3) 0.4757(2) 0.0486(11) Uani 1 1 d . . . . .
H57 H 0.265243 0.405604 0.466257 0.058 Uiso 1 1 calc R . . . .
C44 C 0.0503(2) 0.16061(19) 0.48374(19) 0.0261(8) Uani 1 1 d . . . . .
C21 C 0.4845(3) 0.3111(2) 0.41762(19) 0.0296(8) Uani 1 1 d . . . . .
H21 H 0.431618 0.269803 0.414256 0.036 Uiso 1 1 calc R . . . .
C42 C 0.0384(3) 0.1713(2) 0.6160(2) 0.0391(10) Uani 1 1 d . . . . .
H42 H -0.002257 0.182868 0.664694 0.047 Uiso 1 1 calc R . . . .
C48 C -0.0046(2) 0.1653(2) 0.4196(2) 0.0310(8) Uani 1 1 d . . . . .
H48 H 0.048216 0.166172 0.371204 0.037 Uiso 1 1 calc R . . . .
C8 C 0.5052(3) 0.1960(2) 0.04774(19) 0.0346(9) Uani 1 1 d . . . . .
C12 C 0.3971(3) 0.2223(2) 0.0415(2) 0.0397(9) Uani 1 1 d . . . . .
H12 H 0.353136 0.220836 0.093653 0.048 Uiso 1 1 calc R . . . .
C52 C 0.1760(3) 0.4816(2) 0.4039(2) 0.0387(10) Uani 1 1 d . . . . .
C1 C 0.4164(3) 0.0268(2) 0.1683(2) 0.0339(9) Uani 1 1 d . . . . .
C35 C 0.4672(3) -0.1798(2) 0.2866(2) 0.0423(10) Uani 1 1 d . . . . .
H35A H 0.460147 -0.241185 0.272352 0.063 Uiso 1 1 calc GR . . . .
H35B H 0.516756 -0.183674 0.318508 0.063 Uiso 1 1 calc GR . . . .
H35C H 0.491059 -0.140914 0.241292 0.063 Uiso 1 1 calc GR . . . .
C51 C 0.1616(2) 0.4127(2) 0.3592(2) 0.0324(9) Uani 1 1 d . . . . .
C58 C 0.1240(3) 0.4266(3) 0.5388(2) 0.0543(11) Uani 1 1 d . . . . .
H58A H 0.072752 0.478211 0.552504 0.081 Uiso 1 1 calc GR . . . .
H58B H 0.150709 0.403617 0.582796 0.081 Uiso 1 1 calc GR . . . .
H58C H 0.092337 0.377672 0.521644 0.081 Uiso 1 1 calc GR . . . .
C22 C 0.4709(3) 0.3305(2) 0.4996(2) 0.0404(9) Uani 1 1 d . . . . .
H22A H 0.528009 0.363215 0.505506 0.061 Uiso 1 1 calc GR . . . .
H22B H 0.469438 0.272676 0.530043 0.061 Uiso 1 1 calc GR . . . .
H22C H 0.406577 0.368196 0.516237 0.061 Uiso 1 1 calc GR . . . .
C46 C 0.3607(3) 0.1211(2) 0.59103(19) 0.0389(9) Uani 1 1 d . . . . .
H46A H 0.345086 0.186239 0.600409 0.058 Uiso 1 1 calc GR . . . .
H46B H 0.434997 0.106828 0.578088 0.058 Uiso 1 1 calc GR . . . .
H46C H 0.331055 0.084420 0.636324 0.058 Uiso 1 1 calc GR . . . .
C34 C 0.3277(3) -0.1948(2) 0.4030(2) 0.0402(9) Uani 1 1 d . . . . .
H34A H 0.261573 -0.167351 0.430172 0.060 Uiso 1 1 calc GR . . . .
H34B H 0.377888 -0.195782 0.434120 0.060 Uiso 1 1 calc GR . . . .
H34C H 0.320611 -0.257483 0.391696 0.060 Uiso 1 1 calc GR . . . .
C36 C 0.0940(3) 0.0534(2) 0.2171(2) 0.0405(9) Uani 1 1 d . . . . .
H36 H 0.097327 0.094497 0.257277 0.049 Uiso 1 1 calc R . . . .
C23 C 0.5888(3) 0.2605(2) 0.3903(2) 0.0480(10) Uani 1 1 d . . . . .
H23A H 0.596414 0.244601 0.338203 0.072 Uiso 1 1 calc GR . . . .
H23B H 0.595156 0.204572 0.422169 0.072 Uiso 1 1 calc GR . . . .
H23C H 0.642182 0.299756 0.392854 0.072 Uiso 1 1 calc GR . . . .
C19 C 0.4718(3) 0.5499(2) 0.2693(2) 0.0395(9) Uani 1 1 d . . . . .
H19 H 0.472351 0.603061 0.236387 0.047 Uiso 1 1 calc R . . . .
C26 C 0.5296(3) 0.4650(2) 0.1106(2) 0.0471(10) Uani 1 1 d . . . . .
H26A H 0.567249 0.516651 0.115869 0.071 Uiso 1 1 calc GR . . . .
H26B H 0.517322 0.468037 0.059718 0.071 Uiso 1 1 calc GR . . . .
H26C H 0.569685 0.407499 0.119267 0.071 Uiso 1 1 calc GR . . . .
C25 C 0.3561(3) 0.5518(2) 0.1503(2) 0.0510(11) Uani 1 1 d . . . . .
H25A H 0.293811 0.556659 0.190387 0.077 Uiso 1 1 calc GR . . . .
H25B H 0.338143 0.544051 0.102491 0.077 Uiso 1 1 calc GR . . . .
H25C H 0.391390 0.607532 0.146391 0.077 Uiso 1 1 calc GR . . . .
C60 C 0.1020(3) 0.3570(3) 0.2488(2) 0.0503(11) Uani 1 1 d . . . . .
H60 H 0.101240 0.297935 0.279828 0.060 Uiso 1 1 calc R . . . .
C56 C 0.1197(3) 0.4310(2) 0.2969(2) 0.0425(10) Uani 1 1 d . . . . .
C54 C 0.1097(4) 0.5919(3) 0.3200(3) 0.0659(15) Uani 1 1 d . . . . .
H54 H 0.091992 0.653905 0.306056 0.079 Uiso 1 1 calc R . . . .
C50 C -0.0781(3) 0.2514(2) 0.4186(2) 0.0446(10) Uani 1 1 d . . . . .
H50A H -0.133496 0.249897 0.463839 0.067 Uiso 1 1 calc GR . . . .
H50B H -0.106726 0.253783 0.373894 0.067 Uiso 1 1 calc GR . . . .
H50C H -0.041114 0.305601 0.417327 0.067 Uiso 1 1 calc GR . . . .
C9 C 0.6713(3) 0.1504(3) 0.1938(2) 0.0431(10) Uani 1 1 d . . . . .
H9 H 0.610083 0.164922 0.235114 0.052 Uiso 1 1 calc R . . . .
C7 C 0.5801(4) 0.1756(3) -0.0171(2) 0.0517(11) Uani 1 1 d . . . . .
H7 H 0.562129 0.180726 -0.064451 0.062 Uiso 1 1 calc R . . . .
C49 C -0.0614(3) 0.0799(2) 0.4242(2) 0.0447(10) Uani 1 1 d . . . . .
H49A H -0.011909 0.026010 0.415990 0.067 Uiso 1 1 calc GR . . . .
H49B H -0.101417 0.085572 0.385519 0.067 Uiso 1 1 calc GR . . . .
H49C H -0.107178 0.073136 0.473945 0.067 Uiso 1 1 calc GR . . . .
C53 C 0.1505(3) 0.5713(2) 0.3815(3) 0.0552(12) Uani 1 1 d . . . . .
H53 H 0.161550 0.619464 0.409520 0.066 Uiso 1 1 calc R . . . .
C43 C -0.0058(3) 0.1773(2) 0.5556(2) 0.0368(9) Uani 1 1 d . . . . .
H43 H -0.077263 0.193506 0.563220 0.044 Uiso 1 1 calc R . . . .
C4 C 0.6361(3) 0.1615(2) 0.1204(2) 0.0390(9) Uani 1 1 d . . . . .
C59 C 0.2587(3) 0.5356(3) 0.5021(3) 0.0744(16) Uani 1 1 d . . . . .
H59A H 0.311718 0.558767 0.460754 0.112 Uiso 1 1 calc GR . . . .
H59B H 0.289192 0.512766 0.544385 0.112 Uiso 1 1 calc GR . . . .
H59C H 0.205602 0.585053 0.518243 0.112 Uiso 1 1 calc GR . . . .
C55 C 0.0939(3) 0.5227(3) 0.2777(3) 0.0593(13) Uani 1 1 d . . . . .
H55 H 0.065156 0.537901 0.235174 0.071 Uiso 1 1 calc R . . . .
C37 C -0.0187(3) 0.0444(3) 0.2206(3) 0.0626(13) Uani 1 1 d . . . . .
H37A H -0.024911 0.013523 0.176571 0.094 Uiso 1 1 calc GR . . . .
H37B H -0.055513 0.105327 0.221011 0.094 Uiso 1 1 calc GR . . . .
H37C H -0.047900 0.008453 0.266462 0.094 Uiso 1 1 calc GR . . . .
C5 C 0.7070(3) 0.1409(3) 0.0543(3) 0.0576(12) Uani 1 1 d . . . . .
H5 H 0.775791 0.121506 0.056010 0.069 Uiso 1 1 calc R . . . .
C13 C 0.3571(3) 0.1566(3) -0.0033(2) 0.0564(12) Uani 1 1 d . . . . .
H13A H 0.395933 0.159351 -0.055655 0.085 Uiso 1 1 calc GR . . . .
H13B H 0.284618 0.174139 -0.001660 0.085 Uiso 1 1 calc GR . . . .
H13C H 0.365004 0.094099 0.018606 0.085 Uiso 1 1 calc GR . . . .
C14 C 0.3839(4) 0.3203(3) 0.0069(2) 0.0612(12) Uani 1 1 d . . . . .
H14A H 0.403504 0.363352 0.038091 0.092 Uiso 1 1 calc GR . . . .
H14B H 0.312319 0.335382 0.004477 0.092 Uiso 1 1 calc GR . . . .
H14C H 0.427489 0.324373 -0.043911 0.092 Uiso 1 1 calc GR . . . .
C61 C -0.0003(4) 0.3732(4) 0.2252(3) 0.0887(17) Uani 1 1 d . . . . .
H61A H -0.055472 0.385071 0.269554 0.133 Uiso 1 1 calc GR . . . .
H61B H -0.012351 0.318830 0.201946 0.133 Uiso 1 1 calc GR . . . .
H61C H 0.001545 0.425986 0.188994 0.133 Uiso 1 1 calc GR . . . .
C11 C 0.7127(3) 0.0527(3) 0.2098(3) 0.0624(13) Uani 1 1 d . . . . .
H11A H 0.660040 0.011132 0.210876 0.094 Uiso 1 1 calc GR . . . .
H11B H 0.731579 0.047842 0.258551 0.094 Uiso 1 1 calc GR . . . .
H11C H 0.772997 0.036163 0.170266 0.094 Uiso 1 1 calc GR . . . .
C10 C 0.7488(3) 0.2183(3) 0.1953(2) 0.0560(12) Uani 1 1 d . . . . .
H10A H 0.809180 0.207057 0.154486 0.084 Uiso 1 1 calc GR . . . .
H10B H 0.768913 0.210605 0.243656 0.084 Uiso 1 1 calc GR . . . .
H10C H 0.718017 0.280754 0.188809 0.084 Uiso 1 1 calc GR . . . .
C38 C 0.1440(4) 0.0979(3) 0.1431(3) 0.0746(15) Uani 1 1 d . . . . .
H38A H 0.213610 0.110108 0.144262 0.112 Uiso 1 1 calc GR . . . .
H38B H 0.104534 0.155580 0.133942 0.112 Uiso 1 1 calc GR . . . .
H38C H 0.146600 0.057039 0.102858 0.112 Uiso 1 1 calc GR . . . .
C6 C 0.6788(4) 0.1484(3) -0.0133(3) 0.0658(14) Uani 1 1 d . . . . .
H6 H 0.728285 0.134602 -0.057983 0.079 Uiso 1 1 calc R . . . .
C62 C 0.1892(3) 0.3461(3) 0.1810(3) 0.0673(13) Uani 1 1 d . . . . .
H62A H 0.196413 0.404761 0.151826 0.101 Uiso 1 1 calc GR . . . .
H62B H 0.175292 0.300107 0.149668 0.101 Uiso 1 1 calc GR . . . .
H62C H 0.252559 0.326492 0.197321 0.101 Uiso 1 1 calc GR . . . .
C69 C -0.1803(15) 0.3867(11) -0.0103(14) 0.139(7) Uani 0.5 1 d D U P A -1
H69A H -0.232826 0.352584 0.023657 0.208 Uiso 0.5 1 calc R . P A -1
H69B H -0.212919 0.441247 -0.032311 0.208 Uiso 0.5 1 calc R . P A -1
H69C H -0.142585 0.347818 -0.050444 0.208 Uiso 0.5 1 calc R . P A -1
C70 C -0.111(2) 0.414(2) 0.0310(14) 0.233(11) Uani 0.5 1 d D U P A -1
H70A H -0.154726 0.448439 0.072623 0.279 Uiso 0.5 1 calc R . P A -1
H70B H -0.085261 0.356163 0.054713 0.279 Uiso 0.5 1 calc R . P A -1
C71 C -0.024(3) 0.464(3) 0.004(2) 0.247(11) Uani 0.5 1 d D U P A -1
H71A H 0.019097 0.420679 -0.031084 0.297 Uiso 0.5 1 calc R . P A -1
H71B H -0.052185 0.511486 -0.028717 0.297 Uiso 0.5 1 calc R . P A -1
C72 C 0.052(3) 0.511(3) 0.023(2) 0.280(11) Uani 0.5 1 d D U P A -1
H72A H 0.074805 0.463731 0.058089 0.336 Uiso 0.5 1 calc R . P A -1
H72B H 0.006016 0.555140 0.056411 0.336 Uiso 0.5 1 calc R . P A -1
C73 C 0.140(3) 0.5607(19) 0.0055(19) 0.295(14) Uani 0.5 1 d D U P A -1
H73A H 0.180046 0.543870 -0.044850 0.354 Uiso 0.5 1 calc R . P A -1
H73B H 0.182566 0.538342 0.041808 0.354 Uiso 0.5 1 calc R . P A -1
C74 C 0.129(4) 0.660(2) 0.005(2) 0.40(2) Uani 0.5 1 d D U P A -1
H74A H 0.196454 0.682968 -0.007621 0.601 Uiso 0.5 1 calc R . P A -1
H74B H 0.089864 0.684086 -0.031879 0.601 Uiso 0.5 1 calc R . P A -1
H74C H 0.092398 0.678526 0.055279 0.601 Uiso 0.5 1 calc R . P A -1
C63 C 0.2345(15) 0.4578(17) -0.2200(18) 0.552(18) Uani 1 1 d D U . . .
H63A H 0.286025 0.489726 -0.256829 0.829 Uiso 1 1 calc R . . . .
H63B H 0.166142 0.485643 -0.222495 0.829 Uiso 1 1 calc R . . . .
H63C H 0.245334 0.462535 -0.169430 0.829 Uiso 1 1 calc R . . . .
C64 C 0.2426(15) 0.3679(17) -0.2357(14) 0.488(15) Uani 1 1 d D U . . .
H64A H 0.315608 0.349618 -0.237062 0.586 Uiso 1 1 calc R . . . .
H64B H 0.238033 0.372255 -0.289044 0.586 Uiso 1 1 calc R . . . .
C65 C 0.1978(12) 0.2862(14) -0.2093(12) 0.468(13) Uani 1 1 d D U . . .
H65A H 0.155419 0.280914 -0.245964 0.562 Uiso 1 1 calc R . . . .
H65B H 0.256593 0.240009 -0.223342 0.562 Uiso 1 1 calc R . . . .
C66 C 0.1411(15) 0.2446(16) -0.1447(12) 0.472(13) Uani 1 1 d D U . . .
H66A H 0.085001 0.293932 -0.133949 0.566 Uiso 1 1 calc R . . . .
H66B H 0.185409 0.255082 -0.110623 0.566 Uiso 1 1 calc R . . . .
C67 C 0.0890(10) 0.1742(14) -0.1003(12) 0.393(12) Uani 1 1 d D U . . .
H67A H 0.055567 0.150740 -0.136832 0.472 Uiso 1 1 calc R . . . .
H67B H 0.146763 0.127921 -0.097261 0.472 Uiso 1 1 calc R . . . .
C68 C 0.0206(16) 0.153(2) -0.0330(12) 0.517(16) Uani 1 1 d D U . . .
H68A H 0.009542 0.088021 -0.029773 0.776 Uiso 1 1 calc R . . . .
H68B H 0.048784 0.166559 0.009297 0.776 Uiso 1 1 calc R . . . .
H68C H -0.044515 0.189903 -0.031186 0.776 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh2 Rh1 2.4932(4) . ?
Rh2 N3 2.075(2) . ?
Rh2 N6 2.065(2) . ?
Rh2 N7 2.196(2) . ?
Rh2 C2 1.908(3) . ?
Rh1 N4 2.047(2) . ?
Rh1 N1 2.049(2) . ?
Rh1 C2 2.056(3) . ?
Rh1 C1 1.870(4) . ?
O2 C2 1.166(3) . ?
N4 N5 1.299(3) . ?
N4 C27 1.449(4) . ?
N1 N2 1.301(3) . ?
N1 C3 1.450(4) . ?
N5 N6 1.310(3) . ?
N2 N3 1.298(3) . ?
N3 C15 1.446(3) . ?
N6 C39 1.449(4) . ?
N7 C51 1.453(4) . ?
C33 C30 1.382(5) . ?
C33 C31 1.393(4) . ?
O1 C1 1.141(4) . ?
C27 C28 1.405(4) . ?
C27 C31 1.398(4) . ?
C15 C16 1.403(4) . ?
C15 C20 1.415(4) . ?
C28 C29 1.391(4) . ?
C28 C32 1.502(4) . ?
C30 C29 1.369(5) . ?
C40 C41 1.389(4) . ?
C40 C45 1.514(4) . ?
C40 C39 1.410(5) . ?
C31 C36 1.511(4) . ?
C41 C42 1.384(5) . ?
C32 C35 1.529(4) . ?
C32 C34 1.522(5) . ?
C45 C47 1.534(4) . ?
C45 C46 1.520(4) . ?
C3 C8 1.393(5) . ?
C3 C4 1.393(5) . ?
C39 C44 1.409(4) . ?
C16 C17 1.388(4) . ?
C16 C21 1.513(4) . ?
C17 C18 1.382(5) . ?
C20 C24 1.518(5) . ?
C20 C19 1.394(4) . ?
C24 C26 1.545(5) . ?
C24 C25 1.525(5) . ?
C18 C19 1.365(5) . ?
C57 C52 1.505(6) . ?
C57 C58 1.532(5) . ?
C57 C59 1.523(5) . ?
C44 C48 1.523(5) . ?
C44 C43 1.385(5) . ?
C21 C22 1.516(5) . ?
C21 C23 1.518(5) . ?
C42 C43 1.366(5) . ?
C48 C50 1.528(4) . ?
C48 C49 1.526(4) . ?
C8 C12 1.500(5) . ?
C8 C7 1.399(5) . ?
C12 C13 1.531(5) . ?
C12 C14 1.539(5) . ?
C52 C51 1.407(5) . ?
C52 C53 1.385(5) . ?
C51 C56 1.384(5) . ?
C36 C37 1.527(5) . ?
C36 C38 1.498(6) . ?
C60 C56 1.524(5) . ?
C60 C61 1.532(6) . ?
C60 C62 1.506(6) . ?
C56 C55 1.398(5) . ?
C54 C53 1.367(6) . ?
C54 C55 1.388(6) . ?
C9 C4 1.519(5) . ?
C9 C11 1.520(5) . ?
C9 C10 1.525(5) . ?
C7 C6 1.367(6) . ?
C4 C5 1.391(5) . ?
C5 C6 1.372(6) . ?
C69 C70 1.433(15) . ?
C70 C71 1.420(15) . ?
C71 C72 1.418(13) . ?
C72 C73 1.422(15) . ?
C73 C74 1.447(18) . ?
C63 C64 1.364(14) . ?
C64 C65 1.402(13) . ?
C65 C66 1.387(13) . ?
C66 C67 1.408(13) . ?
C67 C68 1.392(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Rh2 Rh1 86.65(7) . . ?
N3 Rh2 N7 100.34(9) . . ?
N6 Rh2 Rh1 86.26(7) . . ?
N6 Rh2 N3 172.81(9) . . ?
N6 Rh2 N7 83.53(9) . . ?
N7 Rh2 Rh1 131.76(8) . . ?
C2 Rh2 Rh1 53.73(10) . . ?
C2 Rh2 N3 89.40(11) . . ?
C2 Rh2 N6 87.39(10) . . ?
C2 Rh2 N7 168.80(11) . . ?
N4 Rh1 Rh2 86.05(7) . . ?
N4 Rh1 N1 171.48(9) . . ?
N4 Rh1 C2 89.37(10) . . ?
N1 Rh1 Rh2 86.06(7) . . ?
N1 Rh1 C2 87.80(10) . . ?
C2 Rh1 Rh2 48.43(8) . . ?
C1 Rh1 Rh2 168.08(11) . . ?
C1 Rh1 N4 95.11(12) . . ?
C1 Rh1 N1 93.28(12) . . ?
C1 Rh1 C2 119.67(14) . . ?
N5 N4 Rh1 126.19(18) . . ?
N5 N4 C27 112.5(2) . . ?
C27 N4 Rh1 121.29(19) . . ?
N2 N1 Rh1 125.36(19) . . ?
N2 N1 C3 111.2(2) . . ?
C3 N1 Rh1 122.29(18) . . ?
N4 N5 N6 116.6(2) . . ?
N3 N2 N1 118.3(2) . . ?
N2 N3 Rh2 123.36(18) . . ?
N2 N3 C15 110.2(2) . . ?
C15 N3 Rh2 126.33(19) . . ?
N5 N6 Rh2 124.67(19) . . ?
N5 N6 C39 112.8(2) . . ?
C39 N6 Rh2 122.31(17) . . ?
C51 N7 Rh2 133.7(2) . . ?
Rh2 C2 Rh1 77.84(12) . . ?
O2 C2 Rh2 150.4(3) . . ?
O2 C2 Rh1 131.7(2) . . ?
C30 C33 C31 120.8(3) . . ?
C28 C27 N4 119.2(3) . . ?
C31 C27 N4 118.8(3) . . ?
C31 C27 C28 121.8(3) . . ?
C16 C15 N3 118.7(3) . . ?
C16 C15 C20 120.7(3) . . ?
C20 C15 N3 120.6(3) . . ?
C27 C28 C32 122.6(3) . . ?
C29 C28 C27 117.4(3) . . ?
C29 C28 C32 120.0(3) . . ?
C29 C30 C33 120.2(3) . . ?
C41 C40 C45 120.7(3) . . ?
C41 C40 C39 117.9(3) . . ?
C39 C40 C45 121.3(3) . . ?
C33 C31 C27 118.1(3) . . ?
C33 C31 C36 119.4(3) . . ?
C27 C31 C36 122.4(3) . . ?
C30 C29 C28 121.7(3) . . ?
C42 C41 C40 121.3(3) . . ?
C28 C32 C35 112.7(3) . . ?
C28 C32 C34 110.8(3) . . ?
C34 C32 C35 110.5(3) . . ?
C40 C45 C47 109.9(3) . . ?
C40 C45 C46 114.1(3) . . ?
C46 C45 C47 108.8(3) . . ?
C8 C3 N1 118.9(3) . . ?
C8 C3 C4 122.3(3) . . ?
C4 C3 N1 118.7(3) . . ?
C40 C39 N6 118.8(3) . . ?
C40 C39 C44 121.3(3) . . ?
C44 C39 N6 119.8(3) . . ?
C15 C16 C21 122.2(3) . . ?
C17 C16 C15 118.6(3) . . ?
C17 C16 C21 119.0(3) . . ?
C18 C17 C16 121.4(3) . . ?
C15 C20 C24 124.8(3) . . ?
C19 C20 C15 117.6(3) . . ?
C19 C20 C24 117.5(3) . . ?
C20 C24 C26 109.1(3) . . ?
C20 C24 C25 113.1(3) . . ?
C25 C24 C26 110.8(3) . . ?
C19 C18 C17 119.4(3) . . ?
C52 C57 C58 110.8(3) . . ?
C52 C57 C59 114.1(4) . . ?
C59 C57 C58 109.2(4) . . ?
C39 C44 C48 123.1(3) . . ?
C43 C44 C39 117.7(3) . . ?
C43 C44 C48 119.2(3) . . ?
C16 C21 C22 114.4(3) . . ?
C16 C21 C23 109.6(3) . . ?
C22 C21 C23 109.1(3) . . ?
C43 C42 C41 119.9(3) . . ?
C44 C48 C50 112.8(3) . . ?
C44 C48 C49 109.7(3) . . ?
C49 C48 C50 110.4(3) . . ?
C3 C8 C12 123.3(3) . . ?
C3 C8 C7 117.2(4) . . ?
C7 C8 C12 119.4(3) . . ?
C8 C12 C13 113.3(3) . . ?
C8 C12 C14 111.8(3) . . ?
C13 C12 C14 109.1(3) . . ?
C51 C52 C57 121.1(3) . . ?
C53 C52 C57 121.5(4) . . ?
C53 C52 C51 117.3(4) . . ?
O1 C1 Rh1 174.9(3) . . ?
C52 C51 N7 118.4(3) . . ?
C56 C51 N7 118.7(3) . . ?
C56 C51 C52 122.8(3) . . ?
C31 C36 C37 113.0(3) . . ?
C38 C36 C31 110.3(3) . . ?
C38 C36 C37 110.7(3) . . ?
C18 C19 C20 122.3(3) . . ?
C56 C60 C61 113.4(4) . . ?
C62 C60 C56 110.5(3) . . ?
C62 C60 C61 110.6(4) . . ?
C51 C56 C60 123.4(3) . . ?
C51 C56 C55 117.3(4) . . ?
C55 C56 C60 119.3(4) . . ?
C53 C54 C55 120.4(4) . . ?
C4 C9 C11 112.0(3) . . ?
C4 C9 C10 111.2(3) . . ?
C11 C9 C10 111.4(3) . . ?
C6 C7 C8 121.1(4) . . ?
C54 C53 C52 121.3(4) . . ?
C42 C43 C44 122.0(3) . . ?
C3 C4 C9 123.7(3) . . ?
C5 C4 C3 117.9(4) . . ?
C5 C4 C9 118.4(4) . . ?
C54 C55 C56 120.8(4) . . ?
C6 C5 C4 120.7(4) . . ?
C7 C6 C5 120.7(4) . . ?
C71 C70 C69 128(2) . . ?
C72 C71 C70 147(2) . . ?
C71 C72 C73 154(3) . . ?
C72 C73 C74 120(2) . . ?
C63 C64 C65 141(2) . . ?
C66 C65 C64 141(2) . . ?
C65 C66 C67 156(3) . . ?
C68 C67 C66 145(2) . . ?

_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_PLAT410_24                  
;
PROBLEM: Short Intra H...H Contact  H64A     ..H65B     .       1.79 Ang.  
RESPONSE: This is associated with a hexane molecule lying in a void. Attempts 
to introduce a disorder model were unsuccessful.
;
_vrf_PLAT250_24                  
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        4.5 Note  
RESPONSE: These are associated with hexane molecules lying in a large void. 
Attempts to introduce a disorder model were unsuccessful.
;
_vrf_PLAT260_24                  
;
PROBLEM: Large Average Ueq of Residue Including       C63      0.471 Check 
RESPONSE: hese are associated with hexane molecules lying in a large void. 
Attempts to introduce a disorder model were unsuccessful.
;
_vrf_PLAT910_24                  
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         13 Note  
RESPONSE: Several outlier reflections were omitted from the final refinement.
;
_vrf_PLAT934_24                  
;
PROBLEM: Number of (Iobs-Icalc)/Sigma(W) > 10 Outliers ..          2 Check 
RESPONSE: ...
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2LiCl
_database_code_depnum_ccdc_archive 'CCDC 1971988'
loop_
_audit_author_name
_audit_author_address
'Alasdair McKay'
;Monash University
Australia
;
_audit_update_record             
;
2019-12-14 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_audit_creation_date             2019-12-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
''
alasdair.mckay@monash.edu
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C81 H105 Cl Li N6 O6 Rh3'
_chemical_formula_sum            'C81 H105 Cl Li N6 O6 Rh3'
_chemical_formula_weight         1609.82
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   34.876(3)
_cell_length_b                   26.438(3)
_cell_length_c                   22.979(2)
_cell_angle_alpha                90
_cell_angle_beta                 115.098(5)
_cell_angle_gamma                90
_cell_volume                     19187(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    7401
_cell_measurement_temperature    150
_cell_measurement_theta_max      20.662
_cell_measurement_theta_min      2.393
_shelx_estimated_absorpt_T_max   0.988
_shelx_estimated_absorpt_T_min   0.944
_exptl_absorpt_coefficient_mu    0.582
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.1354 before and 0.0808 after correction. The Ratio of minimum to maximum transmission is 0.9027. The λ/2 correction factor is 0.00150.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.115
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             6688
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1459
_diffrn_reflns_av_unetI/netI     0.0737
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            96613
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        20.813
_diffrn_reflns_theta_max         20.813
_diffrn_reflns_theta_min         2.393
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6601
_reflns_number_total             10018
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.839
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       0.00032(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     908
_refine_ls_number_reflns         10018
_refine_ls_number_restraints     935
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0589
_refine_ls_restrained_S_all      0.993
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1152P)²+25.2332P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1656
_refine_ls_wR_factor_ref         0.1918
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Ternary CH refined with riding coordinates:
 C61(H61), C64(H64), C34(H34), C47(H47), C77(H77), C23(H23), C7(H7), C74(H74),
 C50(H50), C10(H10), C20(H20), C37(H37)
3.b Aromatic/amide H refined with riding coordinates:
 C59(H59), C40(H40), C57(H57), C58(H58), C18(H18), C67(H67), C45(H45),
 C44(H44), C5(H5), C71(H71), C43(H43), C70(H70), C72(H72), C4(H4), C13(H13),
 C17(H17), C30(H30), C3(H3), C16(H16), C32(H32), C31(H31)
3.c Idealised Me refined as rotating group:
 C63(H63A,H63B,H63C), C62(H62A,H62B,H62C), C36(H36A,H36B,H36C), C9(H9A,H9B,
 H9C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C8(H8A,H8B,H8C), C79(H79A,H79B,
 H79C), C78(H78A,H78B,H78C), C49(H49A,H49B,H49C), C11(H11A,H11B,H11C), C35(H35A,
 H35B,H35C), C51(H51A,H51B,H51C), C75(H75A,H75B,H75C), C52(H52A,H52B,H52C),
 C48(H48A,H48B,H48C), C76(H76A,H76B,H76C), C12(H12A,H12B,H12C), C25(H25A,H25B,
 H25C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C21(H21A,H21B,H21C), C39(H39A,
 H39B,H39C), C38(H38A,H38B,H38C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.76544(3) 0.43961(3) 0.79871(4) 0.0455(3) Uani 1 1 d . U . . .
Rh2 Rh 0.78754(3) 0.34253(3) 0.80751(3) 0.0451(3) Uani 1 1 d . U . . .
Rh3 Rh 0.84410(2) 0.41227(3) 0.87406(3) 0.0435(3) Uani 1 1 d . U . . .
Cl1 Cl 0.81597(8) 0.40675(8) 0.74986(11) 0.0506(7) Uani 1 1 d . U . . .
O3 O 0.7542(2) 0.3197(2) 0.8994(3) 0.0493(16) Uani 1 1 d . U . . .
O5 O 0.8314(2) 0.3955(2) 0.9873(3) 0.0473(16) Uani 1 1 d . U . . .
O1 O 0.7388(2) 0.4445(2) 0.9013(3) 0.0531(17) Uani 1 1 d . U . . .
O4 O 0.8701(2) 0.3010(2) 0.9101(3) 0.0595(19) Uani 1 1 d . U . . .
O6 O 0.8224(2) 0.5209(2) 0.8892(3) 0.0590(18) Uani 1 1 d . U . . .
N6 N 0.8977(2) 0.4216(2) 1.0052(3) 0.0448(18) Uani 1 1 d . U . . .
N4 N 0.7516(2) 0.2550(3) 0.8331(3) 0.0461(19) Uani 1 1 d . U . . .
N5 N 0.9078(2) 0.4372(2) 0.9156(4) 0.0433(18) Uani 1 1 d . U . . .
O2 O 0.6927(2) 0.3666(2) 0.7381(3) 0.064(2) Uani 1 1 d . U . . .
N1 N 0.7248(2) 0.4936(2) 0.7355(3) 0.0447(18) Uani 1 1 d . U . . .
N2 N 0.7075(3) 0.5015(3) 0.8202(4) 0.053(2) Uani 1 1 d . U . . .
N3 N 0.7804(2) 0.2725(3) 0.7629(3) 0.0476(19) Uani 1 1 d . U . . .
C60 C 0.9441(3) 0.4313(4) 0.8460(4) 0.050(2) Uani 1 1 d . U . . .
C55 C 0.9311(3) 0.4615(3) 0.8851(4) 0.044(2) Uani 1 1 d . U . . .
C61 C 0.9240(3) 0.5475(3) 0.9322(4) 0.049(2) Uani 1 1 d . U . . .
H61 H 0.903819 0.527212 0.943372 0.059 Uiso 1 1 calc R . . . .
C64 C 0.9346(3) 0.3756(4) 0.8354(5) 0.057(3) Uani 1 1 d . U . . .
H64 H 0.908857 0.369042 0.843044 0.068 Uiso 1 1 calc R . . . .
C54 C 0.8481(3) 0.3330(3) 0.8773(4) 0.046(2) Uani 1 1 d . U . . .
C63 C 0.9581(3) 0.5667(4) 0.9934(5) 0.068(3) Uani 1 1 d . U . . .
H63A H 0.973439 0.537985 1.020188 0.101 Uiso 1 1 calc GR . . . .
H63B H 0.945414 0.586841 1.016532 0.101 Uiso 1 1 calc GR . . . .
H63C H 0.977742 0.587734 0.983727 0.101 Uiso 1 1 calc GR . . . .
C59 C 0.9685(3) 0.4556(4) 0.8194(5) 0.064(3) Uani 1 1 d . U . . .
H59 H 0.977493 0.437055 0.791945 0.077 Uiso 1 1 calc R . . . .
C40 C 0.7627(3) 0.2402(3) 0.7860(4) 0.045(2) Uani 1 1 d . U . . .
H40 H 0.757618 0.206489 0.770188 0.054 Uiso 1 1 calc R . . . .
C34 C 0.8552(4) 0.2060(4) 0.8037(5) 0.067(3) Uani 1 1 d . U . . .
H34 H 0.841336 0.220397 0.830282 0.081 Uiso 1 1 calc R . . . .
C57 C 0.9656(3) 0.5347(4) 0.8679(4) 0.052(2) Uani 1 1 d . U . . .
H57 H 0.973273 0.569379 0.874460 0.063 Uiso 1 1 calc R . . . .
C19 C 0.6993(4) 0.5701(4) 0.8841(5) 0.063(3) Uani 1 1 d . U . . .
C81 C 0.8156(3) 0.4815(4) 0.8640(4) 0.049(2) Uani 1 1 d . U . . .
C27 C 0.7277(4) 0.3770(3) 0.7611(5) 0.048(3) Uani 1 1 d . U . . .
C56 C 0.9402(3) 0.5139(3) 0.8949(4) 0.052(2) Uani 1 1 d . U . . .
C46 C 0.6847(4) 0.2194(3) 0.8218(5) 0.055(2) Uani 1 1 d . U . . .
C53 C 0.7627(3) 0.3053(3) 0.8556(4) 0.043(2) Uani 1 1 d . U . . .
C1 C 0.7193(4) 0.5013(3) 0.6707(5) 0.054(2) Uani 1 1 d . U . . .
C41 C 0.7281(3) 0.2225(3) 0.8558(5) 0.048(2) Uani 1 1 d . U . . .
C42 C 0.7501(3) 0.1951(3) 0.9130(5) 0.052(2) Uani 1 1 d . U . . .
C80 C 0.8546(3) 0.4085(3) 0.9628(4) 0.045(2) Uani 1 1 d . U . . .
C62 C 0.9002(3) 0.5931(4) 0.8936(5) 0.068(3) Uani 1 1 d . U . . .
H62A H 0.891058 0.614445 0.920239 0.102 Uiso 1 1 calc GR . . . .
H62B H 0.875318 0.581700 0.855673 0.102 Uiso 1 1 calc GR . . . .
H62C H 0.918799 0.612603 0.879858 0.102 Uiso 1 1 calc GR . . . .
C58 C 0.9798(3) 0.5049(4) 0.8317(5) 0.062(3) Uani 1 1 d . U . . .
H58 H 0.997919 0.519390 0.814952 0.074 Uiso 1 1 calc R . . . .
C14 C 0.6831(4) 0.5268(4) 0.8490(5) 0.061(3) Uani 1 1 d . U . . .
C68 C 0.9134(3) 0.4165(3) 1.0750(4) 0.046(2) Uani 1 1 d . U . . .
C18 C 0.6749(4) 0.5962(4) 0.9087(5) 0.075(3) Uani 1 1 d . U . . .
H18 H 0.685410 0.626232 0.932930 0.090 Uiso 1 1 calc R . . . .
C67 C 0.9226(3) 0.4376(3) 0.9769(5) 0.046(2) Uani 1 1 d . U . . .
H67 H 0.950635 0.448921 1.002274 0.055 Uiso 1 1 calc R . . . .
C36 C 0.8504(4) 0.1479(4) 0.8045(6) 0.080(4) Uani 1 1 d . U . . .
H36A H 0.820374 0.139152 0.788850 0.121 Uiso 1 1 calc GR . . . .
H36B H 0.865848 0.135391 0.848539 0.121 Uiso 1 1 calc GR . . . .
H36C H 0.861995 0.132336 0.776706 0.121 Uiso 1 1 calc GR . . . .
C45 C 0.6623(4) 0.1864(4) 0.8447(5) 0.062(3) Uani 1 1 d . U . . .
H45 H 0.632398 0.183491 0.822504 0.075 Uiso 1 1 calc R . . . .
C6 C 0.6828(4) 0.4849(4) 0.6206(5) 0.065(3) Uani 1 1 d . U . . .
C29 C 0.8323(4) 0.2274(4) 0.7377(6) 0.069(3) Uani 1 1 d . U . . .
C44 C 0.6843(4) 0.1585(4) 0.8999(5) 0.063(3) Uani 1 1 d . U . . .
H44 H 0.669168 0.135829 0.914578 0.075 Uiso 1 1 calc R . . . .
C47 C 0.7979(3) 0.1986(4) 0.9508(5) 0.060(2) Uani 1 1 d . U . . .
H47 H 0.807979 0.227577 0.933023 0.072 Uiso 1 1 calc R . . . .
C77 C 0.9388(4) 0.3276(3) 1.0650(5) 0.061(3) Uani 1 1 d . U . . .
H77 H 0.928399 0.339201 1.019408 0.074 Uiso 1 1 calc R . . . .
C5 C 0.6791(4) 0.4908(4) 0.5574(5) 0.080(3) Uani 1 1 d . U . . .
H5 H 0.654149 0.479913 0.521930 0.096 Uiso 1 1 calc R . . . .
C71 C 0.9391(3) 0.4053(4) 1.2040(5) 0.059(3) Uani 1 1 d . U . . .
H71 H 0.948147 0.401464 1.249002 0.071 Uiso 1 1 calc R . . . .
C73 C 0.9329(3) 0.3720(3) 1.1035(4) 0.049(2) Uani 1 1 d . U . . .
C26 C 0.7359(3) 0.4603(3) 0.8489(5) 0.049(2) Uani 1 1 d . U . . .
C23 C 0.7443(4) 0.5897(4) 0.8990(6) 0.077(3) Uani 1 1 d . U . . .
H23 H 0.760803 0.559955 0.895246 0.093 Uiso 1 1 calc R . . . .
C43 C 0.7278(4) 0.1625(3) 0.9341(5) 0.058(3) Uani 1 1 d . U . . .
H43 H 0.742153 0.143023 0.971952 0.069 Uiso 1 1 calc R . . . .
C70 C 0.9194(3) 0.4497(4) 1.1739(5) 0.056(3) Uani 1 1 d . U . . .
H70 H 0.914530 0.475589 1.198660 0.067 Uiso 1 1 calc R . . . .
C72 C 0.9453(3) 0.3675(4) 1.1692(5) 0.057(3) Uani 1 1 d . U . . .
H72 H 0.958447 0.337114 1.190285 0.069 Uiso 1 1 calc R . . . .
C9 C 0.7817(4) 0.6006(4) 0.7270(5) 0.070(3) Uani 1 1 d . U . . .
H9A H 0.778241 0.620613 0.689143 0.105 Uiso 1 1 calc GR . . . .
H9B H 0.805590 0.613917 0.764869 0.105 Uiso 1 1 calc GR . . . .
H9C H 0.755828 0.602533 0.733608 0.105 Uiso 1 1 calc GR . . . .
C69 C 0.9069(3) 0.4573(3) 1.1092(5) 0.050(2) Uani 1 1 d . U . . .
C7 C 0.7905(3) 0.5452(4) 0.7164(5) 0.063(3) Uani 1 1 d . U . . .
H7 H 0.793916 0.525962 0.755746 0.075 Uiso 1 1 calc R . . . .
C2 C 0.7523(4) 0.5234(4) 0.6606(5) 0.063(3) Uani 1 1 d . U . . .
C28 C 0.7975(4) 0.2573(4) 0.7187(5) 0.063(3) Uani 1 1 d . U . . .
C4 C 0.7119(4) 0.5125(4) 0.5469(6) 0.076(3) Uani 1 1 d . U . . .
H4 H 0.709616 0.515944 0.504343 0.091 Uiso 1 1 calc R . . . .
C74 C 0.8868(4) 0.5071(4) 1.0765(5) 0.064(3) Uani 1 1 d . U . . .
H74 H 0.888986 0.508188 1.034512 0.076 Uiso 1 1 calc R . . . .
C50 C 0.6593(4) 0.2508(4) 0.7621(5) 0.069(3) Uani 1 1 d . U . . .
H50 H 0.680294 0.270303 0.751944 0.082 Uiso 1 1 calc R . . . .
C13 C 0.7020(3) 0.5156(4) 0.7600(5) 0.058(3) Uani 1 1 d . U . . .
H13 H 0.682048 0.540921 0.736865 0.070 Uiso 1 1 calc R . . . .
C65 C 0.9710(4) 0.3436(4) 0.8849(6) 0.098(4) Uani 1 1 d . U . . .
H65A H 0.996996 0.349436 0.879205 0.147 Uiso 1 1 calc GR . . . .
H65B H 0.963522 0.307703 0.878343 0.147 Uiso 1 1 calc GR . . . .
H65C H 0.975686 0.353528 0.928494 0.147 Uiso 1 1 calc GR . . . .
C66 C 0.9245(4) 0.3580(4) 0.7674(5) 0.085(4) Uani 1 1 d . U . . .
H66A H 0.900837 0.377898 0.736724 0.128 Uiso 1 1 calc GR . . . .
H66B H 0.916715 0.322164 0.763139 0.128 Uiso 1 1 calc GR . . . .
H66C H 0.949421 0.362734 0.758684 0.128 Uiso 1 1 calc GR . . . .
C17 C 0.6364(4) 0.5789(5) 0.8984(6) 0.083(4) Uani 1 1 d . U . . .
H17 H 0.619258 0.598000 0.913197 0.099 Uiso 1 1 calc R . . . .
C8 C 0.8308(4) 0.5395(4) 0.7088(6) 0.081(3) Uani 1 1 d . U . . .
H8A H 0.828648 0.558291 0.670754 0.121 Uiso 1 1 calc GR . . . .
H8B H 0.835764 0.503668 0.703709 0.121 Uiso 1 1 calc GR . . . .
H8C H 0.854385 0.552954 0.746999 0.121 Uiso 1 1 calc GR . . . .
C10 C 0.6444(4) 0.4632(4) 0.6291(6) 0.079(3) Uani 1 1 d . U . . .
H10 H 0.653664 0.455863 0.675818 0.095 Uiso 1 1 calc R . . . .
C33 C 0.7759(4) 0.2757(4) 0.6553(6) 0.083(3) Uani 1 1 d . U . . .
C20 C 0.6270(5) 0.4572(6) 0.8070(8) 0.116(4) Uani 1 1 d . U . . .
H20 H 0.646853 0.444569 0.789063 0.139 Uiso 1 1 calc R . . . .
C30 C 0.8487(5) 0.2164(4) 0.6930(7) 0.093(4) Uani 1 1 d . U . . .
H30 H 0.873689 0.196556 0.705484 0.112 Uiso 1 1 calc R . . . .
C79 C 0.9116(3) 0.2820(4) 1.0652(5) 0.069(3) Uani 1 1 d . U . . .
H79A H 0.919549 0.270967 1.109517 0.104 Uiso 1 1 calc GR . . . .
H79B H 0.916282 0.254218 1.040640 0.104 Uiso 1 1 calc GR . . . .
H79C H 0.881642 0.291585 1.045453 0.104 Uiso 1 1 calc GR . . . .
C78 C 0.9856(4) 0.3126(4) 1.0875(6) 0.091(4) Uani 1 1 d . U . . .
H78A H 1.001410 0.341271 1.081584 0.136 Uiso 1 1 calc GR . . . .
H78B H 0.987574 0.283757 1.062185 0.136 Uiso 1 1 calc GR . . . .
H78C H 0.997521 0.303312 1.133065 0.136 Uiso 1 1 calc GR . . . .
C3 C 0.7470(4) 0.5287(4) 0.5969(5) 0.072(3) Uani 1 1 d . U . . .
H3 H 0.768813 0.544193 0.588868 0.086 Uiso 1 1 calc R . . . .
C37 C 0.7339(5) 0.3045(5) 0.6307(6) 0.105(4) Uani 1 1 d . U . . .
H37 H 0.731555 0.318268 0.669601 0.126 Uiso 1 1 calc R . . . .
C49 C 0.8199(4) 0.1505(5) 0.9424(7) 0.111(5) Uani 1 1 d . U . . .
H49A H 0.812745 0.121880 0.962989 0.167 Uiso 1 1 calc GR . . . .
H49B H 0.850676 0.155582 0.962332 0.167 Uiso 1 1 calc GR . . . .
H49C H 0.810414 0.143453 0.896497 0.167 Uiso 1 1 calc GR . . . .
C15 C 0.6451(4) 0.5067(4) 0.8425(6) 0.080(3) Uani 1 1 d . U . . .
C11 C 0.6279(4) 0.4130(5) 0.5914(6) 0.101(4) Uani 1 1 d . U . . .
H11A H 0.614399 0.420104 0.545197 0.152 Uiso 1 1 calc GR . . . .
H11B H 0.607171 0.397508 0.604384 0.152 Uiso 1 1 calc GR . . . .
H11C H 0.651655 0.389721 0.600902 0.152 Uiso 1 1 calc GR . . . .
C35 C 0.9032(4) 0.2204(5) 0.8381(7) 0.103(4) Uani 1 1 d . U . . .
H35A H 0.915074 0.207930 0.882442 0.154 Uiso 1 1 calc GR . . . .
H35B H 0.906198 0.257260 0.838254 0.154 Uiso 1 1 calc GR . . . .
H35C H 0.918352 0.205010 0.815137 0.154 Uiso 1 1 calc GR . . . .
C51 C 0.6342(4) 0.2180(5) 0.7032(6) 0.117(5) Uani 1 1 d . U . . .
H51A H 0.653818 0.197074 0.693182 0.175 Uiso 1 1 calc GR . . . .
H51B H 0.618039 0.239817 0.666475 0.175 Uiso 1 1 calc GR . . . .
H51C H 0.614756 0.196151 0.712382 0.175 Uiso 1 1 calc GR . . . .
C16 C 0.6213(4) 0.5342(5) 0.8668(7) 0.095(4) Uani 1 1 d . U . . .
H16 H 0.594383 0.521977 0.861636 0.114 Uiso 1 1 calc R . . . .
C75 C 0.9082(4) 0.5535(4) 1.1127(6) 0.099(4) Uani 1 1 d . U . . .
H75A H 0.908156 0.553005 1.155317 0.149 Uiso 1 1 calc GR . . . .
H75B H 0.893041 0.583583 1.089187 0.149 Uiso 1 1 calc GR . . . .
H75C H 0.937448 0.554434 1.117371 0.149 Uiso 1 1 calc GR . . . .
C52 C 0.6314(5) 0.2904(5) 0.7767(7) 0.118(5) Uani 1 1 d . U . . .
H52A H 0.608255 0.272987 0.781980 0.177 Uiso 1 1 calc GR . . . .
H52B H 0.619573 0.314416 0.740932 0.177 Uiso 1 1 calc GR . . . .
H52C H 0.648759 0.308650 0.816263 0.177 Uiso 1 1 calc GR . . . .
C48 C 0.8112(4) 0.2090(4) 1.0220(5) 0.084(4) Uani 1 1 d . U . . .
H48A H 0.802074 0.243126 1.027337 0.126 Uiso 1 1 calc GR . . . .
H48B H 0.842023 0.206520 1.045202 0.126 Uiso 1 1 calc GR . . . .
H48C H 0.797882 0.184167 1.039324 0.126 Uiso 1 1 calc GR . . . .
C76 C 0.8401(4) 0.5093(5) 1.0611(7) 0.108(5) Uani 1 1 d . U . . .
H76A H 0.826171 0.478577 1.037800 0.163 Uiso 1 1 calc GR . . . .
H76B H 0.827387 0.538983 1.034412 0.163 Uiso 1 1 calc GR . . . .
H76C H 0.836627 0.511558 1.101133 0.163 Uiso 1 1 calc GR . . . .
C32 C 0.7943(5) 0.2642(5) 0.6119(7) 0.109(5) Uani 1 1 d . U . . .
H32 H 0.782225 0.277792 0.569640 0.131 Uiso 1 1 calc R . . . .
C31 C 0.8283(6) 0.2345(5) 0.6302(7) 0.115(5) Uani 1 1 d . U . . .
H31 H 0.838918 0.225430 0.599766 0.138 Uiso 1 1 calc R . . . .
C12 C 0.6078(4) 0.5009(5) 0.6086(7) 0.110(5) Uani 1 1 d . U . . .
H12A H 0.618421 0.533769 0.628774 0.165 Uiso 1 1 calc GR . . . .
H12B H 0.586381 0.488492 0.622199 0.165 Uiso 1 1 calc GR . . . .
H12C H 0.595109 0.504661 0.561785 0.165 Uiso 1 1 calc GR . . . .
C25 C 0.7700(5) 0.6123(6) 0.9677(7) 0.144(6) Uani 1 1 d . U . . .
H25A H 0.757929 0.645054 0.970984 0.216 Uiso 1 1 calc GR . . . .
H25B H 0.799622 0.616813 0.975231 0.216 Uiso 1 1 calc GR . . . .
H25C H 0.768511 0.589079 0.999962 0.216 Uiso 1 1 calc GR . . . .
C22 C 0.6265(5) 0.4184(6) 0.8560(9) 0.147(6) Uani 1 1 d . U . . .
H22A H 0.655467 0.412876 0.888633 0.221 Uiso 1 1 calc GR . . . .
H22B H 0.614783 0.386454 0.834171 0.221 Uiso 1 1 calc GR . . . .
H22C H 0.608972 0.431130 0.876739 0.221 Uiso 1 1 calc GR . . . .
C24 C 0.7465(5) 0.6273(7) 0.8556(8) 0.159(7) Uani 1 1 d . U . . .
H24A H 0.752091 0.610942 0.821692 0.239 Uiso 1 1 calc GR . . . .
H24B H 0.769378 0.651208 0.879075 0.239 Uiso 1 1 calc GR . . . .
H24C H 0.719539 0.645599 0.836211 0.239 Uiso 1 1 calc GR . . . .
C21 C 0.5829(5) 0.4602(7) 0.7519(9) 0.159(7) Uani 1 1 d . U . . .
H21A H 0.562787 0.472250 0.768274 0.238 Uiso 1 1 calc GR . . . .
H21B H 0.574333 0.426546 0.732888 0.238 Uiso 1 1 calc GR . . . .
H21C H 0.583273 0.483664 0.719133 0.238 Uiso 1 1 calc GR . . . .
C39 C 0.7348(6) 0.3519(6) 0.5891(6) 0.146(6) Uani 1 1 d . U . . .
H39A H 0.764227 0.360266 0.598378 0.219 Uiso 1 1 calc GR . . . .
H39B H 0.721449 0.380837 0.599700 0.219 Uiso 1 1 calc GR . . . .
H39C H 0.719333 0.343825 0.543307 0.219 Uiso 1 1 calc GR . . . .
C38 C 0.6975(5) 0.2703(6) 0.5992(9) 0.163(7) Uani 1 1 d . U . . .
H38A H 0.701879 0.249738 0.567028 0.244 Uiso 1 1 calc GR . . . .
H38B H 0.671595 0.290332 0.578132 0.244 Uiso 1 1 calc GR . . . .
H38C H 0.694835 0.248109 0.631435 0.244 Uiso 1 1 calc GR . . . .
Li1 Li 0.7747(5) 0.3881(5) 0.9218(8) 0.052(3) Uani 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 Rh2 2.6627(10) . ?
Rh1 Rh3 2.6489(11) . ?
Rh1 Cl1 2.607(2) . ?
Rh1 N1 2.100(7) . ?
Rh1 C81 2.077(10) . ?
Rh1 C27 2.062(10) . ?
Rh1 C26 1.924(9) . ?
Rh1 Li1 3.030(15) . ?
Rh2 Rh3 2.6591(11) . ?
Rh2 Cl1 2.595(2) . ?
Rh2 N3 2.078(7) . ?
Rh2 C54 2.054(11) . ?
Rh2 C27 2.106(11) . ?
Rh2 C53 1.936(8) . ?
Rh2 Li1 3.090(16) . ?
Rh3 Cl1 2.599(2) . ?
Rh3 N5 2.116(8) . ?
Rh3 C54 2.100(9) . ?
Rh3 C81 2.049(9) . ?
Rh3 C80 1.915(9) . ?
Rh3 Li1 3.118(16) . ?
O3 C53 1.225(9) . ?
O3 Li1 1.932(15) . ?
O5 C80 1.216(10) . ?
O5 Li1 1.922(18) . ?
O1 C26 1.237(10) . ?
O1 Li1 1.873(17) . ?
O4 C54 1.176(10) . ?
O6 C81 1.165(10) . ?
N6 C80 1.444(12) . ?
N6 C68 1.466(11) . ?
N6 C67 1.352(11) . ?
N4 C40 1.353(10) . ?
N4 C53 1.419(11) . ?
N4 C41 1.430(11) . ?
N5 C55 1.432(10) . ?
N5 C67 1.279(11) . ?
O2 C27 1.139(11) . ?
N1 C1 1.433(11) . ?
N1 C13 1.291(11) . ?
N2 C14 1.445(12) . ?
N2 C26 1.433(11) . ?
N2 C13 1.366(11) . ?
N3 C40 1.294(11) . ?
N3 C28 1.437(12) . ?
C60 C55 1.412(12) . ?
C60 C64 1.505(13) . ?
C60 C59 1.398(13) . ?
C55 C56 1.418(12) . ?
C61 C63 1.493(13) . ?
C61 C56 1.502(13) . ?
C61 C62 1.519(13) . ?
C64 C65 1.549(14) . ?
C64 C66 1.520(13) . ?
C59 C58 1.357(14) . ?
C34 C36 1.546(14) . ?
C34 C29 1.494(15) . ?
C34 C35 1.566(15) . ?
C57 C56 1.392(12) . ?
C57 C58 1.378(13) . ?
C19 C14 1.377(14) . ?
C19 C18 1.388(14) . ?
C19 C23 1.549(16) . ?
C46 C41 1.380(13) . ?
C46 C45 1.413(13) . ?
C46 C50 1.525(14) . ?
C53 Li1 2.598(18) . ?
C1 C6 1.375(14) . ?
C1 C2 1.396(14) . ?
C41 C42 1.408(13) . ?
C42 C47 1.521(14) . ?
C42 C43 1.382(13) . ?
C80 Li1 2.593(19) . ?
C14 C15 1.374(15) . ?
C68 C73 1.376(12) . ?
C68 C69 1.407(12) . ?
C18 C17 1.339(16) . ?
C45 C44 1.384(14) . ?
C6 C5 1.411(14) . ?
C6 C10 1.545(15) . ?
C29 C28 1.354(15) . ?
C29 C30 1.402(15) . ?
C44 C43 1.385(14) . ?
C47 C49 1.539(14) . ?
C47 C48 1.525(13) . ?
C77 C73 1.537(13) . ?
C77 C79 1.537(13) . ?
C77 C78 1.540(14) . ?
C5 C4 1.390(15) . ?
C71 C70 1.386(13) . ?
C71 C72 1.354(13) . ?
C73 C72 1.387(12) . ?
C26 Li1 2.519(18) . ?
C23 C25 1.565(17) . ?
C23 C24 1.434(17) . ?
C70 C69 1.375(12) . ?
C9 C7 1.536(13) . ?
C69 C74 1.533(13) . ?
C7 C2 1.517(15) . ?
C7 C8 1.495(13) . ?
C2 C3 1.401(13) . ?
C28 C33 1.414(15) . ?
C4 C3 1.343(15) . ?
C74 C75 1.492(14) . ?
C74 C76 1.511(15) . ?
C50 C51 1.529(15) . ?
C50 C52 1.562(15) . ?
C17 C16 1.369(17) . ?
C10 C11 1.557(16) . ?
C10 C12 1.527(15) . ?
C33 C37 1.529(17) . ?
C33 C32 1.429(16) . ?
C20 C15 1.530(18) . ?
C20 C22 1.53(2) . ?
C20 C21 1.52(2) . ?
C30 C31 1.396(18) . ?
C37 C39 1.586(18) . ?
C37 C38 1.48(2) . ?
C15 C16 1.388(15) . ?
C32 C31 1.333(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Rh2 Rh1 Li1 65.4(3) . . ?
Rh3 Rh1 Rh2 60.08(3) . . ?
Rh3 Rh1 Li1 66.2(3) . . ?
Cl1 Rh1 Rh2 58.99(5) . . ?
Cl1 Rh1 Rh3 59.26(6) . . ?
Cl1 Rh1 Li1 115.4(3) . . ?
N1 Rh1 Rh2 142.76(19) . . ?
N1 Rh1 Rh3 147.8(2) . . ?
N1 Rh1 Cl1 108.1(2) . . ?
N1 Rh1 Li1 136.4(4) . . ?
C81 Rh1 Rh2 109.4(3) . . ?
C81 Rh1 Rh3 49.6(3) . . ?
C81 Rh1 Cl1 88.4(3) . . ?
C81 Rh1 N1 104.6(3) . . ?
C81 Rh1 Li1 80.9(4) . . ?
C27 Rh1 Rh2 51.0(3) . . ?
C27 Rh1 Rh3 110.8(3) . . ?
C27 Rh1 Cl1 88.8(3) . . ?
C27 Rh1 N1 97.6(3) . . ?
C27 Rh1 C81 157.4(4) . . ?
C27 Rh1 Li1 80.0(4) . . ?
C26 Rh1 Rh2 116.1(3) . . ?
C26 Rh1 Rh3 110.8(3) . . ?
C26 Rh1 Cl1 170.0(3) . . ?
C26 Rh1 N1 81.1(4) . . ?
C26 Rh1 C81 85.2(4) . . ?
C26 Rh1 C27 94.0(4) . . ?
C26 Rh1 Li1 55.9(4) . . ?
Rh1 Rh2 Li1 63.0(3) . . ?
Rh3 Rh2 Rh1 59.70(3) . . ?
Rh3 Rh2 Li1 65.2(3) . . ?
Cl1 Rh2 Rh1 59.44(5) . . ?
Cl1 Rh2 Rh3 59.28(6) . . ?
Cl1 Rh2 Li1 113.8(3) . . ?
N3 Rh2 Rh1 148.3(2) . . ?
N3 Rh2 Rh3 143.6(2) . . ?
N3 Rh2 Cl1 108.8(2) . . ?
N3 Rh2 C27 104.5(3) . . ?
N3 Rh2 Li1 137.4(3) . . ?
C54 Rh2 Rh1 110.3(2) . . ?
C54 Rh2 Rh3 51.0(2) . . ?
C54 Rh2 Cl1 89.4(3) . . ?
C54 Rh2 N3 98.3(3) . . ?
C54 Rh2 C27 156.6(4) . . ?
C54 Rh2 Li1 81.7(4) . . ?
C27 Rh2 Rh1 49.6(3) . . ?
C27 Rh2 Rh3 109.0(3) . . ?
C27 Rh2 Cl1 88.2(3) . . ?
C27 Rh2 Li1 78.0(4) . . ?
C53 Rh2 Rh1 110.4(3) . . ?
C53 Rh2 Rh3 115.3(3) . . ?
C53 Rh2 Cl1 169.7(3) . . ?
C53 Rh2 N3 80.8(3) . . ?
C53 Rh2 C54 93.0(4) . . ?
C53 Rh2 C27 85.5(4) . . ?
C53 Rh2 Li1 56.8(4) . . ?
Rh1 Rh3 Rh2 60.22(3) . . ?
Rh1 Rh3 Li1 62.8(3) . . ?
Rh2 Rh3 Li1 64.1(3) . . ?
Cl1 Rh3 Rh1 59.57(6) . . ?
Cl1 Rh3 Rh2 59.14(6) . . ?
Cl1 Rh3 Li1 112.8(3) . . ?
N5 Rh3 Rh1 143.87(18) . . ?
N5 Rh3 Rh2 148.83(18) . . ?
N5 Rh3 Cl1 110.4(2) . . ?
N5 Rh3 Li1 136.7(4) . . ?
C54 Rh3 Rh1 109.3(3) . . ?
C54 Rh3 Rh2 49.4(3) . . ?
C54 Rh3 Cl1 88.3(2) . . ?
C54 Rh3 N5 104.7(3) . . ?
C54 Rh3 Li1 80.4(4) . . ?
C81 Rh3 Rh1 50.5(3) . . ?
C81 Rh3 Rh2 110.4(3) . . ?
C81 Rh3 Cl1 89.3(3) . . ?
C81 Rh3 N5 98.0(3) . . ?
C81 Rh3 C54 156.6(4) . . ?
C81 Rh3 Li1 79.1(4) . . ?
C80 Rh3 Rh1 112.8(3) . . ?
C80 Rh3 Rh2 109.7(3) . . ?
C80 Rh3 Cl1 168.2(3) . . ?
C80 Rh3 N5 81.1(4) . . ?
C80 Rh3 C54 86.0(3) . . ?
C80 Rh3 C81 91.8(4) . . ?
C80 Rh3 Li1 56.1(4) . . ?
Rh2 Cl1 Rh1 61.57(6) . . ?
Rh2 Cl1 Rh3 61.59(5) . . ?
Rh3 Cl1 Rh1 61.17(5) . . ?
C53 O3 Li1 108.7(7) . . ?
C80 O5 Li1 109.3(8) . . ?
C26 O1 Li1 106.4(7) . . ?
C80 N6 C68 121.0(7) . . ?
C67 N6 C80 116.5(8) . . ?
C67 N6 C68 122.5(8) . . ?
C40 N4 C53 115.8(7) . . ?
C40 N4 C41 121.3(7) . . ?
C53 N4 C41 122.8(7) . . ?
C55 N5 Rh3 128.6(6) . . ?
C67 N5 Rh3 110.8(6) . . ?
C67 N5 C55 119.2(8) . . ?
C1 N1 Rh1 124.7(6) . . ?
C13 N1 Rh1 111.3(6) . . ?
C13 N1 C1 123.6(8) . . ?
C26 N2 C14 124.6(7) . . ?
C13 N2 C14 118.8(8) . . ?
C13 N2 C26 116.5(8) . . ?
C40 N3 Rh2 111.4(6) . . ?
C40 N3 C28 121.2(8) . . ?
C28 N3 Rh2 126.9(6) . . ?
C55 C60 C64 123.2(8) . . ?
C59 C60 C55 115.9(9) . . ?
C59 C60 C64 120.7(9) . . ?
C60 C55 N5 117.3(8) . . ?
C60 C55 C56 122.9(8) . . ?
C56 C55 N5 119.8(8) . . ?
C63 C61 C56 113.4(8) . . ?
C63 C61 C62 107.5(8) . . ?
C56 C61 C62 112.3(8) . . ?
C60 C64 C65 111.1(9) . . ?
C60 C64 C66 113.8(8) . . ?
C66 C64 C65 110.3(9) . . ?
Rh2 C54 Rh3 79.6(4) . . ?
O4 C54 Rh2 139.8(7) . . ?
O4 C54 Rh3 139.2(8) . . ?
C58 C59 C60 121.7(10) . . ?
N3 C40 N4 119.0(8) . . ?
C36 C34 C35 109.4(10) . . ?
C29 C34 C36 112.1(9) . . ?
C29 C34 C35 114.6(10) . . ?
C58 C57 C56 120.2(9) . . ?
C14 C19 C18 118.8(11) . . ?
C14 C19 C23 122.2(9) . . ?
C18 C19 C23 119.0(10) . . ?
Rh3 C81 Rh1 79.9(4) . . ?
O6 C81 Rh1 140.2(8) . . ?
O6 C81 Rh3 139.0(8) . . ?
Rh1 C27 Rh2 79.4(4) . . ?
O2 C27 Rh1 139.1(8) . . ?
O2 C27 Rh2 140.1(8) . . ?
C55 C56 C61 123.7(8) . . ?
C57 C56 C55 117.1(9) . . ?
C57 C56 C61 119.2(8) . . ?
C41 C46 C45 118.2(10) . . ?
C41 C46 C50 123.8(9) . . ?
C45 C46 C50 118.0(10) . . ?
Rh2 C53 Li1 84.6(4) . . ?
O3 C53 Rh2 129.2(6) . . ?
O3 C53 N4 117.8(7) . . ?
O3 C53 Li1 44.8(5) . . ?
N4 C53 Rh2 112.9(6) . . ?
N4 C53 Li1 162.5(7) . . ?
C6 C1 N1 119.6(9) . . ?
C6 C1 C2 121.8(10) . . ?
C2 C1 N1 118.5(10) . . ?
C46 C41 N4 119.3(9) . . ?
C46 C41 C42 122.1(9) . . ?
C42 C41 N4 118.6(9) . . ?
C41 C42 C47 122.4(8) . . ?
C43 C42 C41 118.8(10) . . ?
C43 C42 C47 118.8(9) . . ?
Rh3 C80 Li1 86.2(5) . . ?
O5 C80 Rh3 130.1(8) . . ?
O5 C80 N6 117.5(8) . . ?
O5 C80 Li1 44.4(6) . . ?
N6 C80 Rh3 112.4(6) . . ?
N6 C80 Li1 161.1(7) . . ?
C59 C58 C57 121.9(9) . . ?
C19 C14 N2 118.5(10) . . ?
C15 C14 N2 120.0(10) . . ?
C15 C14 C19 121.5(10) . . ?
C73 C68 N6 118.7(8) . . ?
C73 C68 C69 123.5(9) . . ?
C69 C68 N6 117.8(8) . . ?
C17 C18 C19 119.9(12) . . ?
N5 C67 N6 119.0(9) . . ?
C44 C45 C46 119.4(10) . . ?
C1 C6 C5 118.4(11) . . ?
C1 C6 C10 123.7(10) . . ?
C5 C6 C10 117.8(11) . . ?
C28 C29 C34 124.5(10) . . ?
C28 C29 C30 118.3(12) . . ?
C30 C29 C34 117.2(11) . . ?
C45 C44 C43 121.8(10) . . ?
C42 C47 C49 111.3(9) . . ?
C42 C47 C48 112.6(9) . . ?
C48 C47 C49 110.2(9) . . ?
C73 C77 C78 112.7(9) . . ?
C79 C77 C73 111.4(8) . . ?
C79 C77 C78 111.3(8) . . ?
C4 C5 C6 120.1(12) . . ?
C72 C71 C70 120.0(9) . . ?
C68 C73 C77 122.5(8) . . ?
C68 C73 C72 117.1(9) . . ?
C72 C73 C77 120.3(8) . . ?
Rh1 C26 Li1 84.9(5) . . ?
O1 C26 Rh1 130.2(7) . . ?
O1 C26 N2 117.3(8) . . ?
O1 C26 Li1 45.5(6) . . ?
N2 C26 Rh1 112.5(6) . . ?
N2 C26 Li1 162.5(8) . . ?
C19 C23 C25 116.3(11) . . ?
C24 C23 C19 115.2(12) . . ?
C24 C23 C25 105.2(12) . . ?
C42 C43 C44 119.6(10) . . ?
C69 C70 C71 121.7(9) . . ?
C71 C72 C73 121.6(9) . . ?
C68 C69 C74 122.2(8) . . ?
C70 C69 C68 116.1(9) . . ?
C70 C69 C74 121.7(9) . . ?
C2 C7 C9 109.5(9) . . ?
C8 C7 C9 111.9(9) . . ?
C8 C7 C2 113.3(9) . . ?
C1 C2 C7 120.5(9) . . ?
C1 C2 C3 117.5(11) . . ?
C3 C2 C7 121.7(10) . . ?
C29 C28 N3 121.3(10) . . ?
C29 C28 C33 123.1(10) . . ?
C33 C28 N3 115.6(10) . . ?
C3 C4 C5 120.0(11) . . ?
C75 C74 C69 114.6(9) . . ?
C75 C74 C76 109.6(10) . . ?
C76 C74 C69 111.7(9) . . ?
C46 C50 C51 112.6(9) . . ?
C46 C50 C52 110.3(9) . . ?
C51 C50 C52 113.2(11) . . ?
N1 C13 N2 118.2(9) . . ?
C18 C17 C16 121.4(12) . . ?
C6 C10 C11 112.4(10) . . ?
C12 C10 C6 112.0(10) . . ?
C12 C10 C11 108.8(11) . . ?
C28 C33 C37 124.1(10) . . ?
C28 C33 C32 116.3(12) . . ?
C32 C33 C37 119.5(12) . . ?
C22 C20 C15 108.1(13) . . ?
C21 C20 C15 116.1(14) . . ?
C21 C20 C22 108.8(13) . . ?
C31 C30 C29 119.8(13) . . ?
C4 C3 C2 122.1(12) . . ?
C33 C37 C39 110.8(13) . . ?
C38 C37 C33 111.5(12) . . ?
C38 C37 C39 114.9(13) . . ?
C14 C15 C20 123.2(11) . . ?
C14 C15 C16 117.9(12) . . ?
C16 C15 C20 118.8(12) . . ?
C17 C16 C15 120.2(13) . . ?
C31 C32 C33 120.6(13) . . ?
C32 C31 C30 121.6(13) . . ?
Rh1 Li1 Rh2 51.6(3) . . ?
Rh1 Li1 Rh3 51.0(2) . . ?
Rh2 Li1 Rh3 50.7(3) . . ?
O3 Li1 Rh1 106.9(7) . . ?
O3 Li1 Rh2 65.1(5) . . ?
O3 Li1 Rh3 110.6(7) . . ?
O3 Li1 C53 26.5(3) . . ?
O3 Li1 C80 120.6(8) . . ?
O3 Li1 C26 119.9(8) . . ?
O5 Li1 Rh1 110.6(6) . . ?
O5 Li1 Rh2 103.5(7) . . ?
O5 Li1 Rh3 63.9(5) . . ?
O5 Li1 O3 116.4(8) . . ?
O5 Li1 C53 113.6(8) . . ?
O5 Li1 C80 26.3(3) . . ?
O5 Li1 C26 121.9(7) . . ?
O1 Li1 Rh1 67.3(5) . . ?
O1 Li1 Rh2 114.8(7) . . ?
O1 Li1 Rh3 106.6(6) . . ?
O1 Li1 O3 123.1(9) . . ?
O1 Li1 O5 118.2(8) . . ?
O1 Li1 C53 126.8(8) . . ?
O1 Li1 C80 115.3(7) . . ?
O1 Li1 C26 28.1(3) . . ?
C53 Li1 Rh1 84.5(5) . . ?
C53 Li1 Rh2 38.6(3) . . ?
C53 Li1 Rh3 85.5(5) . . ?
C80 Li1 Rh1 85.3(5) . . ?
C80 Li1 Rh2 82.4(5) . . ?
C80 Li1 Rh3 37.8(3) . . ?
C80 Li1 C53 105.6(6) . . ?
C26 Li1 Rh1 39.2(3) . . ?
C26 Li1 Rh2 87.8(5) . . ?
C26 Li1 Rh3 83.7(5) . . ?
C26 Li1 C53 110.0(7) . . ?
C26 Li1 C80 106.0(6) . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 -0.067 2544.8 1147.6 ?
2 0.500 0.500 -0.015 2544.8 1147.6 ?

_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_THETM01_2LiCl               
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Diffraction data for these crystals was weak at high Bragg angles.
These reflections were not used in the final refinement.
;
_vrf_PLAT910_2LiCl               
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         14 Note  
RESPONSE: Diffraction data for these crystals was weak at high Bragg angles.
These reflections were not used in the final refinement.
;
# end Validation Reply Form
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_25
_database_code_depnum_ccdc_archive 'CCDC 1971992'
loop_
_audit_author_name
_audit_author_address
'Alasdair McKay'
;Monash University
Australia
;
_audit_update_record             
;
2019-12-14 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT094_25                  
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       4.03 Report
RESPONSE: The final Fourier  difference  map  revealed  two notable  peaks  of electron density (ca. 1.00 angstrom) proximal to the formamidinate donor set. Twinning was investigated, but twin scale factors refine to zero for all sensible twin laws. The locations of the electron densities are such that a chemically  sensible  disorder  model  could  not  be  generated.
;
_vrf_PLAT420_25                  
;
PROBLEM: D-H Without Acceptor       O1       --H1       .     Please Check
RESPONSE: This belongs to a bridged hydroxide.
;
_vrf_PLAT910_25                  
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         13 Note
RESPONSE: Several outlying reflections were omitted from the final refinement.
;
# Added during the CSD deposition process: Saturday 14 December 2019 01:17 PM
# end Validation Reply Form

_audit_creation_date             2019-12-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
''
alasdair.mckay@monash.edu
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C41 H60 N2 O Rh2'
_chemical_formula_sum            'C41 H60 N2 O Rh2'
_chemical_formula_weight         802.73
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   15.7881(19)
_cell_length_b                   13.8759(18)
_cell_length_c                   17.064(2)
_cell_angle_alpha                90
_cell_angle_beta                 90.921(5)
_cell_angle_gamma                90
_cell_volume                     3737.9(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9602
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.11
_cell_measurement_theta_min      2.28
_shelx_estimated_absorpt_T_max   0.898
_shelx_estimated_absorpt_T_min   0.890
_exptl_absorpt_coefficient_mu    0.916
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.7011
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/3 (Bruker,2014/3) was used for absorption correction. wR2(int) was 0.0658 before and 0.0405 after correction. The Ratio of minimum to maximum transmission is 0.9404. The λ/2 correction factor is 0.00150.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       cube
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            54865
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.114
_diffrn_reflns_theta_min         3.170
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7416
_reflns_number_total             8211
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.460
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         8211
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0237
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0231P)²+4.0927P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0556
_refine_ls_wR_factor_ref         0.0581
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10), C23(H23), C7(H7), C20(H20), C26(H26), C27(H27), C39(H39), C30(H30),
 C35(H35), C34(H34), C31(H31), C38(H38)
2.b Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C36(H36A,H36B), C33(H33A,H33B), C28(H28A,H28B), C40(H40A,
 H40B), C41(H41A,H41B), C37(H37A,H37B), C29(H29A,H29B)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C18(H18), C16(H16), C17(H17), C3(H3), C13(H13), C4(H4)
2.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C24(H24A,H24B,H24C),
 C22(H22A,H22B,H22C), C12(H12A,H12B,H12C), C11(H11A,H11B,H11C), C21(H21A,H21B,
 H21C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.34199(2) 0.11386(2) 0.20542(2) 0.01568(5) Uani 1 1 d . . . A 1
Rh2 Rh 0.46409(2) 0.28548(2) 0.18994(2) 0.01652(5) Uani 1 1 d . . . A 1
N2 N 0.52301(10) 0.19446(11) 0.27625(9) 0.0154(3) Uani 1 1 d . . . A 1
N1 N 0.41062(10) 0.09044(11) 0.30911(9) 0.0172(3) Uani 1 1 d . . . A 1
C5 C 0.37210(15) -0.11712(17) 0.44405(14) 0.0337(5) Uani 1 1 d . . . A 1
H5 H 0.393366 -0.179912 0.454612 0.040 Uiso 1 1 calc R . . A 1
C10 C 0.48619(14) -0.10307(16) 0.34459(14) 0.0306(5) Uani 1 1 d . . . A 1
H10 H 0.503872 -0.056081 0.303545 0.037 Uiso 1 1 calc R . . A 1
C14 C 0.60544(11) 0.22174(14) 0.30652(11) 0.0175(4) Uani 1 1 d . . . A 1
C1 C 0.37747(12) 0.03133(14) 0.37101(11) 0.0205(4) Uani 1 1 d . . . A 1
C18 C 0.69210(13) 0.32321(15) 0.38951(13) 0.0256(4) Uani 1 1 d . . . A 1
H18 H 0.697642 0.374875 0.425756 0.031 Uiso 1 1 calc R . . A 1
C16 C 0.75607(13) 0.19711(16) 0.31593(13) 0.0258(4) Uani 1 1 d . . . A 1
H16 H 0.805462 0.163109 0.300940 0.031 Uiso 1 1 calc R . . A 1
C19 C 0.61242(12) 0.30115(14) 0.35776(11) 0.0187(4) Uani 1 1 d . . . A 1
C17 C 0.76317(13) 0.27116(16) 0.36912(13) 0.0269(5) Uani 1 1 d . . . A 1
H17 H 0.816799 0.286581 0.391846 0.032 Uiso 1 1 calc R . . A 1
C3 C 0.27388(15) 0.00788(18) 0.47180(13) 0.0333(5) Uani 1 1 d . . . A 1
H3 H 0.227233 0.030829 0.500917 0.040 Uiso 1 1 calc R . . A 1
C23 C 0.53618(12) 0.36352(15) 0.37690(12) 0.0226(4) Uani 1 1 d . . . A 1
H23 H 0.495056 0.357613 0.331969 0.027 Uiso 1 1 calc R . . A 1
C6 C 0.41021(13) -0.06140(15) 0.38593(13) 0.0260(5) Uani 1 1 d . . . A 1
C25 C 0.55919(15) 0.47027(16) 0.38451(15) 0.0337(5) Uani 1 1 d . . . A 1
H25A H 0.594381 0.479966 0.431688 0.051 Uiso 1 1 calc GR . . A 1
H25B H 0.507287 0.508591 0.388418 0.051 Uiso 1 1 calc GR . . A 1
H25C H 0.590640 0.490630 0.338316 0.051 Uiso 1 1 calc GR . . A 1
C7 C 0.27441(14) 0.16826(16) 0.40309(12) 0.0271(5) Uani 1 1 d . . . A 1
H7 H 0.316409 0.205566 0.372030 0.032 Uiso 1 1 calc R . . A 1
C2 C 0.30965(13) 0.06744(16) 0.41529(12) 0.0245(4) Uani 1 1 d . . . A 1
C8 C 0.26096(16) 0.22203(18) 0.47996(14) 0.0355(5) Uani 1 1 d . . . A 1
H8A H 0.219150 0.187550 0.511226 0.053 Uiso 1 1 calc GR . . A 1
H8B H 0.240353 0.287273 0.468705 0.053 Uiso 1 1 calc GR . . A 1
H8C H 0.314731 0.225764 0.509297 0.053 Uiso 1 1 calc GR . . A 1
C15 C 0.67766(13) 0.17088(15) 0.28349(12) 0.0215(4) Uani 1 1 d . . . A 1
C9 C 0.19164(15) 0.1650(2) 0.35583(15) 0.0398(6) Uani 1 1 d . . . A 1
H9A H 0.201172 0.132685 0.305661 0.060 Uiso 1 1 calc GR . . A 1
H9B H 0.171529 0.230789 0.346200 0.060 Uiso 1 1 calc GR . . A 1
H9C H 0.149039 0.129307 0.385270 0.060 Uiso 1 1 calc GR . . A 1
C13 C 0.48408(12) 0.13227(13) 0.32247(11) 0.0168(4) Uani 1 1 d . . . A 1
H13 H 0.512322 0.116306 0.370308 0.020 Uiso 1 1 calc R . . A 1
C20 C 0.67342(15) 0.08981(17) 0.22401(14) 0.0326(5) Uani 1 1 d . . . A 1
H20 H 0.613719 0.085315 0.203860 0.039 Uiso 1 1 calc R . . A 1
C24 C 0.49099(15) 0.32913(18) 0.44995(14) 0.0354(5) Uani 1 1 d . . . A 1
H24A H 0.472854 0.262132 0.442675 0.053 Uiso 1 1 calc GR . . A 1
H24B H 0.441330 0.369809 0.458886 0.053 Uiso 1 1 calc GR . . A 1
H24C H 0.529695 0.333305 0.495295 0.053 Uiso 1 1 calc GR . . A 1
C4 C 0.30467(16) -0.08343(19) 0.48631(14) 0.0376(6) Uani 1 1 d . . . A 1
H4 H 0.279590 -0.122806 0.525127 0.045 Uiso 1 1 calc R . . A 1
C22 C 0.73072(18) 0.1098(2) 0.15398(16) 0.0506(8) Uani 1 1 d . . . A 1
H22A H 0.789902 0.112763 0.172055 0.076 Uiso 1 1 calc GR . . A 1
H22B H 0.714751 0.171452 0.129897 0.076 Uiso 1 1 calc GR . . A 1
H22C H 0.724093 0.058046 0.115317 0.076 Uiso 1 1 calc GR . . A 1
C12 C 0.46703(19) -0.19932(18) 0.30422(19) 0.0476(7) Uani 1 1 d . . . A 1
H12A H 0.453258 -0.247806 0.343781 0.071 Uiso 1 1 calc GR . . A 1
H12B H 0.516757 -0.220323 0.275119 0.071 Uiso 1 1 calc GR . . A 1
H12C H 0.418806 -0.191453 0.267906 0.071 Uiso 1 1 calc GR . . A 1
C11 C 0.56040(18) -0.1155(2) 0.40299(19) 0.0550(8) Uani 1 1 d . . . A 1
H11A H 0.576407 -0.052489 0.424566 0.082 Uiso 1 1 calc GR . . A 1
H11B H 0.608848 -0.143631 0.376041 0.082 Uiso 1 1 calc GR . . A 1
H11C H 0.543310 -0.158230 0.445624 0.082 Uiso 1 1 calc GR . . A 1
C21 C 0.6964(2) -0.00634(19) 0.26179(19) 0.0517(7) Uani 1 1 d . . . A 1
H21A H 0.684927 -0.058620 0.224488 0.078 Uiso 1 1 calc GR . . A 1
H21B H 0.662362 -0.015810 0.308695 0.078 Uiso 1 1 calc GR . . A 1
H21C H 0.756645 -0.006453 0.276485 0.078 Uiso 1 1 calc GR . . A 1
C26 C 0.23772(13) 0.13940(16) 0.12823(12) 0.0243(4) Uani 1 1 d . . . A 1
H26 H 0.212342 0.205162 0.132725 0.029 Uiso 1 1 calc R . . A 1
C27 C 0.31111(13) 0.13567(15) 0.08382(12) 0.0233(4) Uani 1 1 d . . . A 1
H27 H 0.329304 0.199741 0.063185 0.028 Uiso 1 1 calc R . . A 1
C39 C 0.40023(13) 0.36496(15) 0.10015(12) 0.0236(4) Uani 1 1 d . . . A 1
H39 H 0.337457 0.355329 0.098777 0.028 Uiso 1 1 calc R . . A 1
C30 C 0.37946(14) -0.02088(15) 0.16236(13) 0.0269(5) Uani 1 1 d . . . A 1
H30 H 0.425930 -0.051802 0.193939 0.032 Uiso 1 1 calc R . . A 1
C35 C 0.58297(13) 0.33362(17) 0.14673(13) 0.0280(5) Uani 1 1 d . . . A 1
H35 H 0.633110 0.314333 0.179668 0.034 Uiso 1 1 calc R . . A 1
C32 C 0.21697(14) -0.03965(17) 0.14863(13) 0.0308(5) Uani 1 1 d . . . A 1
H32A H 0.177590 -0.082201 0.177052 0.037 Uiso 1 1 calc R . . A 1
H32B H 0.229054 -0.070120 0.097552 0.037 Uiso 1 1 calc R . . A 1
C34 C 0.54957(13) 0.26008(17) 0.10000(13) 0.0275(5) Uani 1 1 d . . . A 1
H34 H 0.580715 0.197627 0.105407 0.033 Uiso 1 1 calc R . . A 1
C31 C 0.29906(14) -0.02984(15) 0.19587(13) 0.0261(5) Uani 1 1 d . . . A 1
H31 H 0.299282 -0.065695 0.246706 0.031 Uiso 1 1 calc R . . A 1
C36 C 0.58192(14) 0.43954(17) 0.12255(15) 0.0342(5) Uani 1 1 d . . . A 1
H36A H 0.579628 0.444262 0.064664 0.041 Uiso 1 1 calc R . . A 1
H36B H 0.634704 0.471118 0.141283 0.041 Uiso 1 1 calc R . . A 1
C38 C 0.42877(14) 0.42659(15) 0.16007(13) 0.0258(4) Uani 1 1 d . . . A 1
H38 H 0.382226 0.452953 0.192848 0.031 Uiso 1 1 calc R . . A 1
C33 C 0.17478(13) 0.05795(17) 0.13456(14) 0.0309(5) Uani 1 1 d . . . A 1
H33A H 0.140361 0.054800 0.085621 0.037 Uiso 1 1 calc R . . A 1
H33B H 0.136011 0.071657 0.178207 0.037 Uiso 1 1 calc R . . A 1
C28 C 0.33581(15) 0.05146(17) 0.03245(13) 0.0304(5) Uani 1 1 d . . . A 1
H28A H 0.363164 0.075986 -0.015384 0.036 Uiso 1 1 calc R . . A 1
H28B H 0.284234 0.015632 0.016166 0.036 Uiso 1 1 calc R . . A 1
C40 C 0.44128(14) 0.35525(17) 0.02099(13) 0.0294(5) Uani 1 1 d . . . A 1
H40A H 0.469443 0.416669 0.007531 0.035 Uiso 1 1 calc R . . A 1
H40B H 0.397060 0.342332 -0.019436 0.035 Uiso 1 1 calc R . . A 1
C41 C 0.50671(15) 0.27349(18) 0.02066(13) 0.0313(5) Uani 1 1 d . . . A 1
H41A H 0.478220 0.212682 0.005180 0.038 Uiso 1 1 calc R . . A 1
H41B H 0.550199 0.287838 -0.018832 0.038 Uiso 1 1 calc R . . A 1
C37 C 0.50558(16) 0.49138(16) 0.15673(14) 0.0342(5) Uani 1 1 d . . . A 1
H37A H 0.520151 0.514125 0.210265 0.041 Uiso 1 1 calc R . . A 1
H37B H 0.491894 0.548531 0.124188 0.041 Uiso 1 1 calc R . . A 1
C29 C 0.39666(15) -0.01682(18) 0.07570(14) 0.0340(5) Uani 1 1 d . . . A 1
H29A H 0.390989 -0.082306 0.053203 0.041 Uiso 1 1 calc R . . A 1
H29B H 0.455603 0.005021 0.067808 0.041 Uiso 1 1 calc R . . A 1
O1 O 0.34866(9) 0.25734(10) 0.24107(8) 0.0188(3) Uani 1 1 d . . . A 1
H1 H 0.3154(17) 0.2880(19) 0.2207(16) 0.032(8) Uiso 1 1 d . . . B 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 Rh2 3.0780(3) . ?
Rh1 N1 2.0853(16) . ?
Rh1 C26 2.1216(19) . ?
Rh1 C27 2.1454(19) . ?
Rh1 C30 2.098(2) . ?
Rh1 C31 2.111(2) . ?
Rh1 O1 2.0840(14) . ?
Rh2 N2 2.1415(15) . ?
Rh2 C39 2.1284(19) . ?
Rh2 C35 2.135(2) . ?
Rh2 C34 2.090(2) . ?
Rh2 C38 2.096(2) . ?
Rh2 O1 2.0704(14) . ?
N2 C14 1.443(2) . ?
N2 C13 1.327(2) . ?
N1 C1 1.442(2) . ?
N1 C13 1.314(2) . ?
C5 C6 1.401(3) . ?
C5 C4 1.377(4) . ?
C10 C6 1.516(3) . ?
C10 C12 1.531(3) . ?
C10 C11 1.535(3) . ?
C14 C19 1.410(3) . ?
C14 C15 1.402(3) . ?
C1 C6 1.408(3) . ?
C1 C2 1.412(3) . ?
C18 C19 1.396(3) . ?
C18 C17 1.384(3) . ?
C16 C17 1.374(3) . ?
C16 C15 1.396(3) . ?
C19 C23 1.522(3) . ?
C3 C2 1.396(3) . ?
C3 C4 1.378(4) . ?
C23 C25 1.530(3) . ?
C23 C24 1.523(3) . ?
C7 C2 1.519(3) . ?
C7 C8 1.527(3) . ?
C7 C9 1.525(3) . ?
C15 C20 1.516(3) . ?
C20 C22 1.536(4) . ?
C20 C21 1.523(4) . ?
C26 C27 1.396(3) . ?
C26 C33 1.510(3) . ?
C27 C28 1.515(3) . ?
C39 C38 1.402(3) . ?
C39 C40 1.514(3) . ?
C30 C31 1.406(3) . ?
C30 C29 1.509(3) . ?
C35 C34 1.393(3) . ?
C35 C36 1.527(3) . ?
C32 C31 1.521(3) . ?
C32 C33 1.527(3) . ?
C34 C41 1.515(3) . ?
C36 C37 1.527(4) . ?
C38 C37 1.511(3) . ?
C28 C29 1.530(3) . ?
C40 C41 1.534(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Rh1 Rh2 82.87(4) . . ?
N1 Rh1 C26 160.09(8) . . ?
N1 Rh1 C27 161.72(7) . . ?
N1 Rh1 C30 90.73(7) . . ?
N1 Rh1 C31 94.59(7) . . ?
C26 Rh1 Rh2 107.35(6) . . ?
C26 Rh1 C27 38.18(8) . . ?
C27 Rh1 Rh2 86.60(6) . . ?
C30 Rh1 Rh2 118.62(6) . . ?
C30 Rh1 C26 98.73(8) . . ?
C30 Rh1 C27 81.25(8) . . ?
C30 Rh1 C31 39.03(9) . . ?
C31 Rh1 Rh2 157.63(6) . . ?
C31 Rh1 C26 82.24(8) . . ?
C31 Rh1 C27 89.48(8) . . ?
O1 Rh1 Rh2 42.02(4) . . ?
O1 Rh1 N1 83.00(6) . . ?
O1 Rh1 C26 93.25(7) . . ?
O1 Rh1 C27 99.04(7) . . ?
O1 Rh1 C30 160.16(7) . . ?
O1 Rh1 C31 159.95(7) . . ?
N2 Rh2 Rh1 75.54(4) . . ?
C39 Rh2 Rh1 99.94(6) . . ?
C39 Rh2 N2 174.98(7) . . ?
C39 Rh2 C35 89.90(8) . . ?
C35 Rh2 Rh1 145.80(7) . . ?
C35 Rh2 N2 92.72(7) . . ?
C34 Rh2 Rh1 110.20(7) . . ?
C34 Rh2 N2 97.31(7) . . ?
C34 Rh2 C39 82.11(8) . . ?
C34 Rh2 C35 38.50(9) . . ?
C34 Rh2 C38 98.71(9) . . ?
C38 Rh2 Rh1 125.38(6) . . ?
C38 Rh2 N2 145.99(7) . . ?
C38 Rh2 C39 38.74(8) . . ?
C38 Rh2 C35 81.70(9) . . ?
O1 Rh2 Rh1 42.36(4) . . ?
O1 Rh2 N2 88.54(6) . . ?
O1 Rh2 C39 89.49(7) . . ?
O1 Rh2 C35 171.64(8) . . ?
O1 Rh2 C34 149.42(8) . . ?
O1 Rh2 C38 92.64(7) . . ?
C14 N2 Rh2 118.08(11) . . ?
C13 N2 Rh2 126.31(12) . . ?
C13 N2 C14 112.44(15) . . ?
C1 N1 Rh1 121.35(12) . . ?
C13 N1 Rh1 121.58(13) . . ?
C13 N1 C1 116.99(16) . . ?
C4 C5 C6 121.9(2) . . ?
C6 C10 C12 113.0(2) . . ?
C6 C10 C11 110.0(2) . . ?
C12 C10 C11 109.7(2) . . ?
C19 C14 N2 119.22(17) . . ?
C15 C14 N2 120.02(17) . . ?
C15 C14 C19 120.75(17) . . ?
C6 C1 N1 121.03(19) . . ?
C6 C1 C2 120.44(19) . . ?
C2 C1 N1 118.51(18) . . ?
C17 C18 C19 121.2(2) . . ?
C17 C16 C15 121.27(19) . . ?
C14 C19 C23 121.55(17) . . ?
C18 C19 C14 118.24(18) . . ?
C18 C19 C23 120.20(18) . . ?
C16 C17 C18 119.90(19) . . ?
C4 C3 C2 121.5(2) . . ?
C19 C23 C25 112.40(17) . . ?
C19 C23 C24 112.33(18) . . ?
C24 C23 C25 110.34(19) . . ?
C5 C6 C10 118.1(2) . . ?
C5 C6 C1 118.1(2) . . ?
C1 C6 C10 123.73(19) . . ?
C2 C7 C8 112.84(18) . . ?
C2 C7 C9 110.72(19) . . ?
C9 C7 C8 109.82(19) . . ?
C1 C2 C7 122.19(18) . . ?
C3 C2 C1 118.6(2) . . ?
C3 C2 C7 119.3(2) . . ?
C14 C15 C20 122.26(18) . . ?
C16 C15 C14 118.52(19) . . ?
C16 C15 C20 119.22(19) . . ?
N1 C13 N2 126.90(17) . . ?
C15 C20 C22 111.5(2) . . ?
C15 C20 C21 111.0(2) . . ?
C21 C20 C22 110.4(2) . . ?
C5 C4 C3 119.4(2) . . ?
C27 C26 Rh1 71.83(11) . . ?
C27 C26 C33 124.3(2) . . ?
C33 C26 Rh1 109.60(14) . . ?
C26 C27 Rh1 69.99(11) . . ?
C26 C27 C28 124.48(19) . . ?
C28 C27 Rh1 113.21(14) . . ?
C38 C39 Rh2 69.40(11) . . ?
C38 C39 C40 124.61(19) . . ?
C40 C39 Rh2 113.05(14) . . ?
C31 C30 Rh1 71.02(12) . . ?
C31 C30 C29 125.43(19) . . ?
C29 C30 Rh1 111.48(15) . . ?
C34 C35 Rh2 69.01(12) . . ?
C34 C35 C36 123.2(2) . . ?
C36 C35 Rh2 112.88(15) . . ?
C31 C32 C33 111.70(18) . . ?
C35 C34 Rh2 72.49(13) . . ?
C35 C34 C41 125.5(2) . . ?
C41 C34 Rh2 110.56(14) . . ?
C30 C31 Rh1 69.95(12) . . ?
C30 C31 C32 124.01(19) . . ?
C32 C31 Rh1 113.27(14) . . ?
C35 C36 C37 110.82(18) . . ?
C39 C38 Rh2 71.86(12) . . ?
C39 C38 C37 125.7(2) . . ?
C37 C38 Rh2 110.75(15) . . ?
C26 C33 C32 112.91(17) . . ?
C27 C28 C29 111.33(18) . . ?
C39 C40 C41 111.54(17) . . ?
C34 C41 C40 112.23(19) . . ?
C38 C37 C36 111.88(19) . . ?
C30 C29 C28 111.98(19) . . ?
Rh2 O1 Rh1 95.61(6) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_6(dme)2
_database_code_depnum_ccdc_archive 'CCDC 1971996'
loop_
_audit_author_name
_audit_author_address
'Alasdair McKay'
;Monash University
Australia
;
_audit_update_record             
;
2019-12-14 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_audit_creation_date             2019-12-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
''
alasdair.mckay@monash.edu
_chemical_name_common            ?
_chemical_name_systematic        '[Na(DME)2(N3Dipp2)]'
_chemical_formula_moiety         '0.5(C64 H108 N6 Na2 O8)'
_chemical_formula_sum            'C32 H54 N3 Na O4'
_chemical_formula_weight         567.77
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   20.0231(15)
_cell_length_b                   10.9042(8)
_cell_length_c                   33.135(3)
_cell_angle_alpha                90
_cell_angle_beta                 105.340(4)
_cell_angle_gamma                90
_cell_volume                     6976.8(9)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    1886
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      18.005
_cell_measurement_theta_min      2.550
_shelx_estimated_absorpt_T_max   0.998
_shelx_estimated_absorpt_T_min   0.986
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1563 before and 0.0671 after correction. The Ratio of minimum to maximum transmission is 0.9018. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1518
_diffrn_reflns_av_unetI/netI     0.1665
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            51336
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.123
_diffrn_reflns_theta_max         25.123
_diffrn_reflns_theta_min         1.078
_diffrn_ambient_temperature      149.99
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4571
_reflns_number_total             12438
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.32B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.32B (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.0017(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     860
_refine_ls_number_reflns         12438
_refine_ls_number_restraints     268
_refine_ls_R_factor_all          0.2242
_refine_ls_R_factor_gt           0.0780
_refine_ls_restrained_S_all      0.974
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0970P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1772
_refine_ls_wR_factor_ref         0.2454
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C64A-C63A = C62A-C61A
 2.394 with sigma of 0.04
 C63A-O7A = O8A-C62A
 2.412 with sigma of 0.04
 C61-C62 = C63-C64
 2.394 with sigma of 0.04
 C62-O8 = O7-C63
 2.412 with sigma of 0.04
 C57-C58 = C59-C60
 2.394 with sigma of 0.04
 C58-O6 = O5-C59
 2.412 with sigma of 0.04
 C57A-C58A = C59A-C60A
 2.394 with sigma of 0.04
 C58A-O6A = O5A-C59A
 2.412 with sigma of 0.04
 O8A-C64A \\sim O7A-C61A \\sim O8A-C63A \\sim O7A-C62A
 with sigma of 0.02
 O7-C61 \\sim O8-C64 \\sim O7-C62 \\sim O8-C63
 with sigma of 0.02
 O5-C57 \\sim O6-C60 \\sim O5-C58 \\sim O6-C59
 with sigma of 0.02
 O5A-C57A \\sim O6A-C60A \\sim O5A-C58A \\sim O6A-C59A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C64A \\sim C63A \\sim C62A \\sim C61A \\sim O7A \\sim O8A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
C61 \\sim C62 \\sim C63 \\sim C64 \\sim O8 \\sim O7: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C57 \\sim C58 \\sim C59 \\sim C60 \\sim O6 \\sim O5: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
C57A \\sim C58A \\sim C59A \\sim C60A \\sim O6A \\sim O5A: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 C64A, C63A, C62A, C61A, O7A, O8A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C61, C62, C63, C64, O8, O7
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C57, C58, C59, C60, O6, O5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C57A, C58A, C59A, C60A, O6A, O5A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O8A)=Sof(O7A)=Sof(C64A)=Sof(H0AA)=Sof(H0AB)=Sof(H0AC)=Sof(C63A)=Sof(H1AA)=
 Sof(H1AB)=Sof(C62A)=Sof(H1BA)=Sof(H1BB)=Sof(C61A)=Sof(H1CA)=Sof(H1CB)=
 Sof(H1CC)=1-FVAR(1)
 Sof(O7)=Sof(O8)=Sof(C61)=Sof(H1DA)=Sof(H1DB)=Sof(H1DC)=Sof(C62)=Sof(H1EA)=
 Sof(H1EB)=Sof(C63)=Sof(H1FA)=Sof(H1FB)=Sof(C64)=Sof(H1GA)=Sof(H1GB)=Sof(H1GC)=
 FVAR(1)
 Sof(O5A)=Sof(O6A)=Sof(C57A)=Sof(H1LA)=Sof(H1LB)=Sof(H1LC)=Sof(C58A)=Sof(H1MA)=
 Sof(H1MB)=Sof(C59A)=Sof(H1NA)=Sof(H1NB)=Sof(C60A)=Sof(H1OA)=Sof(H1OB)=
 Sof(H1OC)=1-FVAR(2)
 Sof(O5)=Sof(O6)=Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H57C)=Sof(C58)=Sof(H58A)=
 Sof(H58B)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(H60C)=
 FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C22(H22), C19(H19), C10(H10), C7(H7), C39(H39), C51(H51), C42(H42), C54(H54)
6.b Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C27(H27A,H27B), C31(H31A,H31B), C30(H30A,H30B), C63A(H1AA,
 H1AB), C62A(H1BA,H1BB), C62(H1EA,H1EB), C63(H1FA,H1FB), C58(H58A,H58B),
 C59(H59A,H59B), C58A(H1MA,H1MB), C59A(H1NA,H1NB)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C15(H15), C5(H5), C17(H17), C16(H16), C35(H35), C47(H47),
 C37(H37), C36(H36), C49(H49), C48(H48)
6.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C11(H11A,H11B,H11C), C24(H24A,H24B,H24C), C20(H20A,H20B,
 H20C), C23(H23A,H23B,H23C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C12(H12A,H12B,
 H12C), C28(H28A,H28B,H28C), C25(H25A,H25B,H25C), C32(H32A,H32B,H32C), C29(H29A,
 H29B,H29C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C40(H40A,H40B,H40C),
 C44(H44A,H44B,H44C), C56(H56A,H56B,H56C), C55(H55A,H55B,H55C), C52(H52A,H52B,
 H52C), C53(H53A,H53B,H53C), C64A(H0AA,H0AB,H0AC), C61A(H1CA,H1CB,H1CC),
 C61(H1DA,H1DB,H1DC), C64(H1GA,H1GB,H1GC), C57(H57A,H57B,H57C), C60(H60A,H60B,
 H60C), C57A(H1LA,H1LB,H1LC), C60A(H1OA,H1OB,H1OC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Na2 Na 0.52047(8) 0.51514(15) 0.11221(6) 0.0478(5) Uani 1 1 d . . . . .
Na1 Na 0.47283(8) 0.44700(15) 0.38047(5) 0.0429(5) Uani 1 1 d . . . . .
N1 N 0.37243(17) 0.5626(3) 0.39423(12) 0.0397(9) Uani 1 1 d . . . . .
C14 C 0.3558(2) 0.7206(4) 0.28037(14) 0.0386(12) Uani 1 1 d . . . . .
C13 C 0.4157(2) 0.7108(4) 0.31358(14) 0.0353(11) Uani 1 1 d . . . . .
C1 C 0.3227(2) 0.5879(4) 0.41670(14) 0.0374(11) Uani 1 1 d . . . . .
C18 C 0.4755(2) 0.7782(4) 0.31321(15) 0.0418(12) Uani 1 1 d . . . . .
C2 C 0.2830(2) 0.4870(4) 0.42328(14) 0.0431(12) Uani 1 1 d . . . . .
C6 C 0.3142(2) 0.7029(4) 0.43396(15) 0.0431(12) Uani 1 1 d . . . . .
C3 C 0.2351(2) 0.5041(5) 0.44642(15) 0.0528(14) Uani 1 1 d . . . . .
H3 H 0.208459 0.436412 0.451403 0.063 Uiso 1 1 calc R . . . .
C22 C 0.5414(2) 0.7656(5) 0.34833(17) 0.0553(14) Uani 1 1 d . . . . .
H22 H 0.539731 0.684041 0.361830 0.066 Uiso 1 1 calc R . . . .
C4 C 0.2256(2) 0.6163(6) 0.46205(16) 0.0604(15) Uani 1 1 d . . . . .
H4 H 0.191580 0.626453 0.477016 0.072 Uiso 1 1 calc R . . . .
C19 C 0.2932(2) 0.6360(4) 0.27587(15) 0.0466(13) Uani 1 1 d . . . . .
H19 H 0.308106 0.566611 0.295991 0.056 Uiso 1 1 calc R . . . .
C15 C 0.3551(2) 0.8057(4) 0.24953(16) 0.0518(14) Uani 1 1 d . . . . .
H15 H 0.313967 0.815630 0.227549 0.062 Uiso 1 1 calc R . . . .
C10 C 0.3591(3) 0.8137(4) 0.43087(16) 0.0533(13) Uani 1 1 d . . . . .
H10 H 0.399768 0.783601 0.421541 0.064 Uiso 1 1 calc R . . . .
C7 C 0.2901(3) 0.3640(4) 0.40394(16) 0.0562(14) Uani 1 1 d . . . . .
H7 H 0.337576 0.360022 0.399602 0.067 Uiso 1 1 calc R . . . .
C21 C 0.2682(2) 0.5809(5) 0.23231(16) 0.0616(15) Uani 1 1 d . . . . .
H21A H 0.250427 0.646272 0.212009 0.092 Uiso 1 1 calc GR . . . .
H21B H 0.231202 0.521653 0.231855 0.092 Uiso 1 1 calc GR . . . .
H21C H 0.306788 0.539356 0.225006 0.092 Uiso 1 1 calc GR . . . .
C5 C 0.2650(3) 0.7154(5) 0.45639(16) 0.0542(14) Uani 1 1 d . . . . .
H5 H 0.258398 0.792777 0.467933 0.065 Uiso 1 1 calc R . . . .
C17 C 0.4718(3) 0.8605(4) 0.28081(17) 0.0589(15) Uani 1 1 d . . . . .
H17 H 0.511677 0.906944 0.280225 0.071 Uiso 1 1 calc R . . . .
C16 C 0.4116(3) 0.8765(5) 0.24942(17) 0.0649(16) Uani 1 1 d . . . . .
H16 H 0.409390 0.935609 0.228048 0.078 Uiso 1 1 calc R . . . .
C11 C 0.3868(3) 0.8775(5) 0.47316(19) 0.084(2) Uani 1 1 d . . . . .
H11A H 0.348793 0.919875 0.480844 0.127 Uiso 1 1 calc GR . . . .
H11B H 0.422365 0.937246 0.471116 0.127 Uiso 1 1 calc GR . . . .
H11C H 0.407063 0.816377 0.494573 0.127 Uiso 1 1 calc GR . . . .
C24 C 0.5442(3) 0.8642(6) 0.3818(2) 0.101(2) Uani 1 1 d . . . . .
H24A H 0.550184 0.945028 0.370333 0.152 Uiso 1 1 calc GR . . . .
H24B H 0.583171 0.847538 0.406165 0.152 Uiso 1 1 calc GR . . . .
H24C H 0.500881 0.863013 0.390357 0.152 Uiso 1 1 calc GR . . . .
C20 C 0.2339(2) 0.7013(5) 0.28753(19) 0.0744(18) Uani 1 1 d . . . . .
H20A H 0.249163 0.728892 0.316678 0.112 Uiso 1 1 calc GR . . . .
H20B H 0.194749 0.644885 0.284255 0.112 Uiso 1 1 calc GR . . . .
H20C H 0.219554 0.772389 0.269166 0.112 Uiso 1 1 calc GR . . . .
C23 C 0.6073(3) 0.7699(7) 0.3345(2) 0.106(3) Uani 1 1 d . . . . .
H23A H 0.606366 0.705263 0.313861 0.159 Uiso 1 1 calc GR . . . .
H23B H 0.647049 0.757307 0.358800 0.159 Uiso 1 1 calc GR . . . .
H23C H 0.611306 0.850059 0.321988 0.159 Uiso 1 1 calc GR . . . .
C8 C 0.2825(4) 0.2552(5) 0.4314(2) 0.096(2) Uani 1 1 d . . . . .
H8A H 0.318330 0.259681 0.458053 0.144 Uiso 1 1 calc GR . . . .
H8B H 0.287689 0.178558 0.417083 0.144 Uiso 1 1 calc GR . . . .
H8C H 0.236674 0.257419 0.436772 0.144 Uiso 1 1 calc GR . . . .
C9 C 0.2394(4) 0.3549(6) 0.36184(19) 0.119(3) Uani 1 1 d . . . . .
H9A H 0.192189 0.353107 0.365159 0.179 Uiso 1 1 calc GR . . . .
H9B H 0.248121 0.279661 0.347908 0.179 Uiso 1 1 calc GR . . . .
H9C H 0.244631 0.426102 0.344878 0.179 Uiso 1 1 calc GR . . . .
C12 C 0.3204(3) 0.9052(5) 0.39864(19) 0.0853(19) Uani 1 1 d . . . . .
H12A H 0.306072 0.865570 0.371157 0.128 Uiso 1 1 calc GR . . . .
H12B H 0.350762 0.974783 0.397345 0.128 Uiso 1 1 calc GR . . . .
H12C H 0.279384 0.934504 0.406591 0.128 Uiso 1 1 calc GR . . . .
N2 N 0.37109(17) 0.6447(3) 0.36560(12) 0.0387(9) Uani 1 1 d . . . . .
N3 N 0.42182(17) 0.6275(3) 0.34691(12) 0.0407(10) Uani 1 1 d . . . . .
O2 O 0.54058(15) 0.5057(3) 0.44967(10) 0.0599(10) Uani 1 1 d . . . . .
O1 O 0.59660(16) 0.4303(4) 0.38683(12) 0.0686(11) Uani 1 1 d . . . . .
C28 C 0.5220(3) 0.6105(5) 0.46987(19) 0.0842(19) Uani 1 1 d . . . . .
H28A H 0.538397 0.684762 0.458824 0.126 Uiso 1 1 calc GR . . . .
H28B H 0.543354 0.604993 0.500054 0.126 Uiso 1 1 calc GR . . . .
H28C H 0.471546 0.613986 0.464642 0.126 Uiso 1 1 calc GR . . . .
C26 C 0.6324(3) 0.4250(7) 0.4280(2) 0.088(2) Uani 1 1 d . . . . .
H26A H 0.682015 0.439061 0.429876 0.106 Uiso 1 1 calc R . . . .
H26B H 0.628268 0.340608 0.438124 0.106 Uiso 1 1 calc R . . . .
C27 C 0.6131(3) 0.5059(7) 0.4552(2) 0.094(2) Uani 1 1 d . . . . .
H27A H 0.628330 0.589742 0.450352 0.113 Uiso 1 1 calc R . . . .
H27B H 0.636497 0.482732 0.484416 0.113 Uiso 1 1 calc R . . . .
C25 C 0.6203(3) 0.3724(7) 0.3571(2) 0.125(3) Uani 1 1 d . . . . .
H25A H 0.609926 0.284640 0.357365 0.187 Uiso 1 1 calc GR . . . .
H25B H 0.670530 0.384000 0.363029 0.187 Uiso 1 1 calc GR . . . .
H25C H 0.597698 0.406764 0.329589 0.187 Uiso 1 1 calc GR . . . .
O3 O 0.46659(19) 0.2264(3) 0.38610(13) 0.0681(11) Uani 1 1 d . . . . .
O4 O 0.4460(2) 0.3436(4) 0.31303(12) 0.0942(14) Uani 1 1 d . . . . .
C31 C 0.4385(3) 0.2186(6) 0.31268(19) 0.0738(17) Uani 1 1 d . . . . .
H31A H 0.478785 0.180900 0.305395 0.089 Uiso 1 1 calc R . . . .
H31B H 0.396517 0.196157 0.290520 0.089 Uiso 1 1 calc R . . . .
C32 C 0.4485(3) 0.3984(5) 0.27479(17) 0.0853(19) Uani 1 1 d . . . . .
H32A H 0.451814 0.487641 0.278234 0.128 Uiso 1 1 calc GR . . . .
H32B H 0.406303 0.377700 0.253062 0.128 Uiso 1 1 calc GR . . . .
H32C H 0.488992 0.367870 0.266580 0.128 Uiso 1 1 calc GR . . . .
C29 C 0.4744(3) 0.1729(5) 0.42518(19) 0.094(2) Uani 1 1 d . . . . .
H29A H 0.505974 0.222627 0.446592 0.141 Uiso 1 1 calc GR . . . .
H29B H 0.493444 0.090121 0.425150 0.141 Uiso 1 1 calc GR . . . .
H29C H 0.429185 0.168167 0.431328 0.141 Uiso 1 1 calc GR . . . .
C30 C 0.4331(4) 0.1687(6) 0.3514(2) 0.118(3) Uani 1 1 d . . . . .
H30A H 0.383453 0.165653 0.350735 0.142 Uiso 1 1 calc R . . . .
H30B H 0.450101 0.083070 0.353190 0.142 Uiso 1 1 calc R . . . .
N4 N 0.57831(18) 0.3549(3) 0.15568(12) 0.0423(10) Uani 1 1 d . . . . .
N5 N 0.62879(18) 0.3307(3) 0.13746(12) 0.0403(9) Uani 1 1 d . . . . .
N6 N 0.62445(17) 0.4003(3) 0.10516(12) 0.0437(10) Uani 1 1 d . . . . .
C33 C 0.5861(2) 0.2825(4) 0.19207(14) 0.0362(11) Uani 1 1 d . . . . .
C34 C 0.6420(2) 0.3011(4) 0.22725(15) 0.0396(12) Uani 1 1 d . . . . .
C45 C 0.6755(2) 0.3679(5) 0.08397(14) 0.0469(13) Uani 1 1 d . . . . .
C39 C 0.6962(2) 0.4008(4) 0.22866(15) 0.0457(12) Uani 1 1 d . . . . .
H39 H 0.676817 0.458637 0.205063 0.055 Uiso 1 1 calc R . . . .
C38 C 0.5348(2) 0.1950(4) 0.19221(15) 0.0447(12) Uani 1 1 d . . . . .
C46 C 0.7126(2) 0.4665(5) 0.07303(16) 0.0536(14) Uani 1 1 d . . . . .
C35 C 0.6469(3) 0.2276(4) 0.26218(16) 0.0502(13) Uani 1 1 d . . . . .
H35 H 0.684687 0.238434 0.286240 0.060 Uiso 1 1 calc R . . . .
C47 C 0.7596(3) 0.4441(7) 0.05031(18) 0.0778(19) Uani 1 1 d . . . . .
H47 H 0.784332 0.510882 0.042823 0.093 Uiso 1 1 calc R . . . .
C37 C 0.5422(3) 0.1253(4) 0.22819(17) 0.0569(14) Uani 1 1 d . . . . .
H37 H 0.507785 0.066197 0.229097 0.068 Uiso 1 1 calc R . . . .
C36 C 0.5977(3) 0.1391(5) 0.26243(17) 0.0599(15) Uani 1 1 d . . . . .
H36 H 0.602229 0.088088 0.286243 0.072 Uiso 1 1 calc R . . . .
C51 C 0.7018(3) 0.5948(5) 0.08758(17) 0.0682(16) Uani 1 1 d . . . . .
H51 H 0.652516 0.602744 0.088539 0.082 Uiso 1 1 calc R . . . .
C42 C 0.4747(2) 0.1746(4) 0.15406(16) 0.0521(13) Uani 1 1 d . . . . .
H42 H 0.473962 0.244609 0.134454 0.062 Uiso 1 1 calc R . . . .
C54 C 0.6474(3) 0.1382(5) 0.08137(16) 0.0651(16) Uani 1 1 d . . . . .
H54 H 0.606726 0.170391 0.090260 0.078 Uiso 1 1 calc R . . . .
C41 C 0.7627(2) 0.3456(4) 0.22144(17) 0.0599(15) Uani 1 1 d . . . . .
H41A H 0.782409 0.286512 0.243684 0.090 Uiso 1 1 calc GR . . . .
H41B H 0.796310 0.411230 0.221771 0.090 Uiso 1 1 calc GR . . . .
H41C H 0.751842 0.303990 0.194275 0.090 Uiso 1 1 calc GR . . . .
C50 C 0.6868(2) 0.2487(5) 0.07173(15) 0.0557(14) Uani 1 1 d . . . . .
C49 C 0.7357(3) 0.2325(6) 0.04835(18) 0.0753(19) Uani 1 1 d . . . . .
H49 H 0.744017 0.152513 0.039378 0.090 Uiso 1 1 calc R . . . .
C43 C 0.4047(3) 0.1720(5) 0.16446(17) 0.0735(17) Uani 1 1 d . . . . .
H43A H 0.401164 0.096929 0.180033 0.110 Uiso 1 1 calc GR . . . .
H43B H 0.367403 0.173642 0.138465 0.110 Uiso 1 1 calc GR . . . .
H43C H 0.400819 0.243615 0.181533 0.110 Uiso 1 1 calc GR . . . .
C40 C 0.7126(3) 0.4757(5) 0.26930(17) 0.0693(16) Uani 1 1 d . . . . .
H40A H 0.669691 0.510283 0.273339 0.104 Uiso 1 1 calc GR . . . .
H40B H 0.744602 0.542235 0.267530 0.104 Uiso 1 1 calc GR . . . .
H40C H 0.734044 0.422280 0.292981 0.104 Uiso 1 1 calc GR . . . .
C48 C 0.7713(3) 0.3301(8) 0.0384(2) 0.090(2) Uani 1 1 d . . . . .
H48 H 0.804552 0.317137 0.022984 0.108 Uiso 1 1 calc R . . . .
C44 C 0.4839(3) 0.0583(5) 0.13149(19) 0.0791(18) Uani 1 1 d . . . . .
H44A H 0.526572 0.063591 0.122391 0.119 Uiso 1 1 calc GR . . . .
H44B H 0.444283 0.047485 0.107020 0.119 Uiso 1 1 calc GR . . . .
H44C H 0.486819 -0.011800 0.150393 0.119 Uiso 1 1 calc GR . . . .
C56 C 0.6190(4) 0.0538(5) 0.04423(18) 0.099(2) Uani 1 1 d . . . . .
H56A H 0.590849 0.101499 0.020793 0.148 Uiso 1 1 calc GR . . . .
H56B H 0.590422 -0.010023 0.052120 0.148 Uiso 1 1 calc GR . . . .
H56C H 0.657599 0.015540 0.035854 0.148 Uiso 1 1 calc GR . . . .
C55 C 0.6915(3) 0.0642(5) 0.11822(19) 0.087(2) Uani 1 1 d . . . . .
H55A H 0.733382 0.034950 0.111302 0.131 Uiso 1 1 calc GR . . . .
H55B H 0.664735 -0.006065 0.123781 0.131 Uiso 1 1 calc GR . . . .
H55C H 0.704477 0.116523 0.143126 0.131 Uiso 1 1 calc GR . . . .
C52 C 0.7482(3) 0.6094(6) 0.13187(19) 0.097(2) Uani 1 1 d . . . . .
H52A H 0.734661 0.549781 0.150369 0.145 Uiso 1 1 calc GR . . . .
H52B H 0.743347 0.692627 0.141897 0.145 Uiso 1 1 calc GR . . . .
H52C H 0.796559 0.595258 0.131848 0.145 Uiso 1 1 calc GR . . . .
C53 C 0.7172(3) 0.6960(6) 0.0595(2) 0.103(2) Uani 1 1 d . . . . .
H53A H 0.766309 0.693596 0.060010 0.155 Uiso 1 1 calc GR . . . .
H53B H 0.706158 0.775862 0.069654 0.155 Uiso 1 1 calc GR . . . .
H53C H 0.688864 0.683392 0.030763 0.155 Uiso 1 1 calc GR . . . .
O8A O 0.4443(15) 0.4124(14) 0.0474(6) 0.055(4) Uani 0.399(13) 1 d D U P A 2
O7A O 0.4761(10) 0.6584(16) 0.0600(5) 0.052(4) Uani 0.399(13) 1 d D U P A 2
C64A C 0.4715(14) 0.2923(17) 0.0401(9) 0.061(5) Uani 0.399(13) 1 d D U P A 2
H0AA H 0.521438 0.298502 0.043383 0.091 Uiso 0.399(13) 1 calc GR . P A 2
H0AB H 0.448463 0.264632 0.011720 0.091 Uiso 0.399(13) 1 calc GR . P A 2
H0AC H 0.462697 0.233234 0.060441 0.091 Uiso 0.399(13) 1 calc GR . P A 2
C63A C 0.4462(10) 0.4946(10) 0.0139(4) 0.060(4) Uani 0.399(13) 1 d D U P A 2
H1AA H 0.414317 0.464810 -0.012489 0.072 Uiso 0.399(13) 1 calc R . P A 2
H1AB H 0.493565 0.496721 0.010053 0.072 Uiso 0.399(13) 1 calc R . P A 2
C62A C 0.4253(9) 0.6209(12) 0.0232(5) 0.063(4) Uani 0.399(13) 1 d D U P A 2
H1BA H 0.424700 0.677177 -0.000316 0.076 Uiso 0.399(13) 1 calc R . P A 2
H1BB H 0.378666 0.619994 0.028189 0.076 Uiso 0.399(13) 1 calc R . P A 2
C61A C 0.4776(14) 0.7855(18) 0.0721(9) 0.082(7) Uani 0.399(13) 1 d D U P A 2
H1CA H 0.487420 0.791376 0.102583 0.123 Uiso 0.399(13) 1 calc GR . P A 2
H1CB H 0.432587 0.823240 0.059153 0.123 Uiso 0.399(13) 1 calc GR . P A 2
H1CC H 0.513802 0.828400 0.062666 0.123 Uiso 0.399(13) 1 calc GR . P A 2
O7 O 0.4602(8) 0.6706(14) 0.0578(5) 0.094(4) Uani 0.601(13) 1 d D U P A 1
O8 O 0.4457(11) 0.4273(12) 0.0565(5) 0.087(4) Uani 0.601(13) 1 d D U P A 1
C61 C 0.4497(9) 0.7868(16) 0.0725(8) 0.099(6) Uani 0.601(13) 1 d D U P A 1
H1DA H 0.429449 0.778924 0.096217 0.148 Uiso 0.601(13) 1 calc GR . P A 1
H1DB H 0.418248 0.833525 0.050073 0.148 Uiso 0.601(13) 1 calc GR . P A 1
H1DC H 0.494200 0.829822 0.081504 0.148 Uiso 0.601(13) 1 calc GR . P A 1
C62 C 0.3970(6) 0.6196(10) 0.0431(5) 0.097(4) Uani 0.601(13) 1 d D U P A 1
H1EA H 0.369612 0.671299 0.020076 0.117 Uiso 0.601(13) 1 calc R . P A 1
H1EB H 0.373186 0.620467 0.065793 0.117 Uiso 0.601(13) 1 calc R . P A 1
C63 C 0.3970(7) 0.4971(9) 0.0282(4) 0.096(4) Uani 0.601(13) 1 d D U P A 1
H1FA H 0.350458 0.460559 0.024349 0.115 Uiso 0.601(13) 1 calc R . P A 1
H1FB H 0.407854 0.497492 0.000739 0.115 Uiso 0.601(13) 1 calc R . P A 1
C64 C 0.4489(10) 0.3063(16) 0.0427(8) 0.098(6) Uani 0.601(13) 1 d D U P A 1
H1GA H 0.470399 0.305413 0.019338 0.147 Uiso 0.601(13) 1 calc GR . P A 1
H1GB H 0.402028 0.272457 0.033458 0.147 Uiso 0.601(13) 1 calc GR . P A 1
H1GC H 0.476655 0.256522 0.065731 0.147 Uiso 0.601(13) 1 calc GR . P A 1
O5 O 0.4265(4) 0.5178(10) 0.1470(3) 0.096(3) Uani 0.714(16) 1 d D U P A 1
O6 O 0.5360(5) 0.6824(7) 0.1643(3) 0.076(2) Uani 0.714(16) 1 d D U P A 1
C57 C 0.3557(5) 0.4884(13) 0.1277(6) 0.128(6) Uani 0.714(16) 1 d D U P A 1
H57A H 0.330620 0.562970 0.116061 0.192 Uiso 0.714(16) 1 calc GR . P A 1
H57B H 0.334578 0.453188 0.148664 0.192 Uiso 0.714(16) 1 calc GR . P A 1
H57C H 0.353202 0.428708 0.105274 0.192 Uiso 0.714(16) 1 calc GR . P A 1
C58 C 0.4342(7) 0.6137(10) 0.1776(4) 0.099(4) Uani 0.714(16) 1 d D U P A 1
H58A H 0.411944 0.589412 0.199697 0.119 Uiso 0.714(16) 1 calc R . P A 1
H58B H 0.411635 0.689580 0.164148 0.119 Uiso 0.714(16) 1 calc R . P A 1
C59 C 0.5093(7) 0.636(3) 0.1962(4) 0.099(5) Uani 0.714(16) 1 d D U P A 1
H59A H 0.516081 0.695934 0.219390 0.118 Uiso 0.714(16) 1 calc R . P A 1
H59B H 0.532969 0.558747 0.207304 0.118 Uiso 0.714(16) 1 calc R . P A 1
C60 C 0.6039(5) 0.7338(12) 0.1810(5) 0.103(5) Uani 0.714(16) 1 d D U P A 1
H60A H 0.634255 0.672086 0.198114 0.154 Uiso 0.714(16) 1 calc GR . P A 1
H60B H 0.600724 0.805216 0.198357 0.154 Uiso 0.714(16) 1 calc GR . P A 1
H60C H 0.623051 0.759041 0.157967 0.154 Uiso 0.714(16) 1 calc GR . P A 1
O5A O 0.4473(12) 0.582(2) 0.1539(6) 0.082(7) Uani 0.286(16) 1 d D U P A 2
O6A O 0.5736(13) 0.6903(18) 0.1593(6) 0.072(6) Uani 0.286(16) 1 d D U P A 2
C57A C 0.3911(17) 0.508(3) 0.1547(15) 0.117(13) Uani 0.286(16) 1 d D U P A 2
H1LA H 0.347893 0.550773 0.141630 0.175 Uiso 0.286(16) 1 calc GR . P A 2
H1LB H 0.392505 0.487840 0.183803 0.175 Uiso 0.286(16) 1 calc GR . P A 2
H1LC H 0.393398 0.431608 0.139337 0.175 Uiso 0.286(16) 1 calc GR . P A 2
C58A C 0.492(3) 0.608(6) 0.1934(10) 0.096(10) Uani 0.286(16) 1 d D U P A 2
H1MA H 0.519621 0.534484 0.204390 0.116 Uiso 0.286(16) 1 calc R . P A 2
H1MB H 0.464001 0.629571 0.213130 0.116 Uiso 0.286(16) 1 calc R . P A 2
C59A C 0.5396(16) 0.714(3) 0.1905(9) 0.096(8) Uani 0.286(16) 1 d D U P A 2
H1NA H 0.512363 0.790614 0.183788 0.115 Uiso 0.286(16) 1 calc R . P A 2
H1NB H 0.574195 0.725268 0.217773 0.115 Uiso 0.286(16) 1 calc R . P A 2
C60A C 0.6176(11) 0.788(3) 0.1547(11) 0.111(11) Uani 0.286(16) 1 d D U P A 2
H1OA H 0.636649 0.770871 0.130884 0.166 Uiso 0.286(16) 1 calc GR . P A 2
H1OB H 0.655565 0.795356 0.180236 0.166 Uiso 0.286(16) 1 calc GR . P A 2
H1OC H 0.591126 0.864312 0.149747 0.166 Uiso 0.286(16) 1 calc GR . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Na2 N4 2.364(4) . ?
Na2 N5 2.913(4) . ?
Na2 N6 2.493(4) . ?
Na2 O8A 2.54(2) . ?
Na2 O7A 2.326(19) . ?
Na2 O7 2.536(16) . ?
Na2 O8 2.260(16) . ?
Na2 O5 2.455(10) . ?
Na2 O6 2.473(9) . ?
Na2 O5A 2.38(2) . ?
Na2 O6A 2.52(2) . ?
Na1 N1 2.514(4) . ?
Na1 N2 2.917(4) . ?
Na1 N3 2.357(4) . ?
Na1 O2 2.421(4) . ?
Na1 O1 2.438(3) . ?
Na1 O3 2.418(4) . ?
Na1 O4 2.433(4) . ?
N1 C1 1.419(5) . ?
N1 N2 1.300(4) . ?
C14 C13 1.402(6) . ?
C14 C19 1.531(6) . ?
C14 C15 1.377(6) . ?
C13 C18 1.406(6) . ?
C13 N3 1.410(5) . ?
C1 C2 1.408(6) . ?
C1 C6 1.407(6) . ?
C18 C22 1.517(6) . ?
C18 C17 1.386(6) . ?
C2 C3 1.390(6) . ?
C2 C7 1.509(6) . ?
C6 C10 1.525(6) . ?
C6 C5 1.389(6) . ?
C3 C4 1.361(6) . ?
C22 C24 1.536(7) . ?
C22 C23 1.507(6) . ?
C4 C5 1.379(7) . ?
C19 C21 1.520(6) . ?
C19 C20 1.521(6) . ?
C15 C16 1.371(6) . ?
C10 C11 1.531(7) . ?
C10 C12 1.517(7) . ?
C7 C8 1.528(7) . ?
C7 C9 1.495(8) . ?
C17 C16 1.379(6) . ?
N2 N3 1.336(4) . ?
O2 C28 1.423(6) . ?
O2 C27 1.415(5) . ?
O1 C26 1.365(6) . ?
O1 C25 1.356(6) . ?
C26 C27 1.388(7) . ?
O3 C29 1.391(6) . ?
O3 C30 1.327(7) . ?
O4 C31 1.370(6) . ?
O4 C32 1.414(6) . ?
C31 C30 1.423(8) . ?
N4 N5 1.334(4) . ?
N4 C33 1.415(5) . ?
N5 N6 1.296(5) . ?
N6 C45 1.429(5) . ?
C33 C34 1.401(6) . ?
C33 C38 1.404(6) . ?
C34 C39 1.528(6) . ?
C34 C35 1.389(6) . ?
C45 C46 1.408(6) . ?
C45 C50 1.398(7) . ?
C39 C41 1.536(6) . ?
C39 C40 1.534(6) . ?
C38 C37 1.388(6) . ?
C38 C42 1.513(6) . ?
C46 C47 1.372(7) . ?
C46 C51 1.514(7) . ?
C35 C36 1.382(6) . ?
C47 C48 1.344(8) . ?
C37 C36 1.370(7) . ?
C51 C52 1.524(7) . ?
C51 C53 1.526(7) . ?
C42 C43 1.529(6) . ?
C42 C44 1.508(6) . ?
C54 C50 1.519(7) . ?
C54 C56 1.521(7) . ?
C54 C55 1.533(7) . ?
C50 C49 1.411(7) . ?
C49 C48 1.370(8) . ?
O8A C64A 1.463(15) . ?
O8A C63A 1.437(16) . ?
O7A C62A 1.424(15) . ?
O7A C61A 1.441(14) . ?
C63A C62A 1.496(16) . ?
O7 C61 1.394(12) . ?
O7 C62 1.350(12) . ?
O8 C63 1.388(13) . ?
O8 C64 1.403(13) . ?
C62 C63 1.424(13) . ?
O5 C57 1.429(10) . ?
O5 C58 1.435(12) . ?
O6 C59 1.399(13) . ?
O6 C60 1.439(11) . ?
C58 C59 1.486(18) . ?
O5A C57A 1.39(2) . ?
O5A C58A 1.40(2) . ?
O6A C59A 1.40(2) . ?
O6A C60A 1.41(2) . ?
C58A C59A 1.52(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Na2 N5 26.77(10) . . ?
N4 Na2 N6 53.05(12) . . ?
N4 Na2 O8A 106.1(3) . . ?
N4 Na2 O7 172.7(4) . . ?
N4 Na2 O5 92.0(2) . . ?
N4 Na2 O6 99.7(2) . . ?
N4 Na2 O5A 98.7(5) . . ?
N4 Na2 O6A 97.1(5) . . ?
N6 Na2 N5 26.28(10) . . ?
N6 Na2 O8A 91.6(6) . . ?
N6 Na2 O7 121.4(5) . . ?
N6 Na2 O6A 102.3(6) . . ?
O8A Na2 N5 100.0(4) . . ?
O7A Na2 N4 168.2(5) . . ?
O7A Na2 N5 141.8(5) . . ?
O7A Na2 N6 115.6(5) . . ?
O7A Na2 O8A 69.0(5) . . ?
O7A Na2 O5A 93.1(7) . . ?
O7A Na2 O6A 88.2(6) . . ?
O7 Na2 N5 147.5(5) . . ?
O8 Na2 N4 107.3(3) . . ?
O8 Na2 N5 102.9(4) . . ?
O8 Na2 N6 95.7(5) . . ?
O8 Na2 O7 67.3(4) . . ?
O8 Na2 O5 88.0(6) . . ?
O8 Na2 O6 144.8(5) . . ?
O5 Na2 N5 118.6(3) . . ?
O5 Na2 N6 144.4(3) . . ?
O5 Na2 O7 92.7(5) . . ?
O5 Na2 O6 68.5(3) . . ?
O6 Na2 N5 111.2(2) . . ?
O6 Na2 N6 118.8(2) . . ?
O6 Na2 O7 87.2(4) . . ?
O5A Na2 N5 124.8(5) . . ?
O5A Na2 N6 150.0(5) . . ?
O5A Na2 O8A 107.6(9) . . ?
O5A Na2 O6A 68.3(6) . . ?
O6A Na2 N5 100.7(6) . . ?
O6A Na2 O8A 156.8(6) . . ?
N1 Na1 N2 26.38(10) . . ?
N3 Na1 N1 53.09(12) . . ?
N3 Na1 N2 26.73(10) . . ?
N3 Na1 O2 106.89(14) . . ?
N3 Na1 O1 114.01(14) . . ?
N3 Na1 O3 147.39(15) . . ?
N3 Na1 O4 89.48(14) . . ?
O2 Na1 N1 88.30(12) . . ?
O2 Na1 N2 98.97(12) . . ?
O2 Na1 O1 68.64(12) . . ?
O2 Na1 O4 157.63(14) . . ?
O1 Na1 N1 149.88(14) . . ?
O1 Na1 N2 135.91(13) . . ?
O3 Na1 N1 115.11(13) . . ?
O3 Na1 N2 134.44(13) . . ?
O3 Na1 O2 102.55(14) . . ?
O3 Na1 O1 89.50(14) . . ?
O3 Na1 O4 66.82(14) . . ?
O4 Na1 N1 113.94(15) . . ?
O4 Na1 N2 102.28(13) . . ?
O4 Na1 O1 91.00(15) . . ?
C1 N1 Na1 153.9(3) . . ?
N2 N1 Na1 94.4(2) . . ?
N2 N1 C1 111.5(3) . . ?
C13 C14 C19 122.6(4) . . ?
C15 C14 C13 118.2(4) . . ?
C15 C14 C19 119.1(4) . . ?
C14 C13 C18 120.5(4) . . ?
C14 C13 N3 122.9(4) . . ?
C18 C13 N3 116.5(4) . . ?
C2 C1 N1 115.6(4) . . ?
C6 C1 N1 124.3(4) . . ?
C6 C1 C2 120.0(4) . . ?
C13 C18 C22 121.0(4) . . ?
C17 C18 C13 118.3(4) . . ?
C17 C18 C22 120.6(4) . . ?
C1 C2 C7 120.6(4) . . ?
C3 C2 C1 118.7(4) . . ?
C3 C2 C7 120.7(4) . . ?
C1 C6 C10 122.8(4) . . ?
C5 C6 C1 118.9(4) . . ?
C5 C6 C10 118.2(4) . . ?
C4 C3 C2 121.1(5) . . ?
C18 C22 C24 110.4(4) . . ?
C23 C22 C18 114.7(4) . . ?
C23 C22 C24 109.3(5) . . ?
C3 C4 C5 120.7(5) . . ?
C21 C19 C14 112.7(4) . . ?
C21 C19 C20 110.0(4) . . ?
C20 C19 C14 111.5(4) . . ?
C16 C15 C14 122.3(5) . . ?
C6 C10 C11 112.1(4) . . ?
C12 C10 C6 111.6(4) . . ?
C12 C10 C11 109.8(4) . . ?
C2 C7 C8 113.7(4) . . ?
C9 C7 C2 109.8(5) . . ?
C9 C7 C8 110.8(5) . . ?
C4 C5 C6 120.5(5) . . ?
C16 C17 C18 121.5(4) . . ?
C15 C16 C17 119.0(4) . . ?
N1 N2 Na1 59.2(2) . . ?
N1 N2 N3 111.7(3) . . ?
N3 N2 Na1 52.53(19) . . ?
C13 N3 Na1 147.6(3) . . ?
N2 N3 Na1 100.7(2) . . ?
N2 N3 C13 110.7(3) . . ?
C28 O2 Na1 120.5(3) . . ?
C27 O2 Na1 115.0(3) . . ?
C27 O2 C28 108.9(4) . . ?
C26 O1 Na1 110.1(3) . . ?
C25 O1 Na1 121.0(4) . . ?
C25 O1 C26 120.9(5) . . ?
O1 C26 C27 117.3(5) . . ?
C26 C27 O2 111.6(5) . . ?
C29 O3 Na1 119.6(3) . . ?
C30 O3 Na1 115.4(4) . . ?
C30 O3 C29 120.9(5) . . ?
C31 O4 Na1 117.8(3) . . ?
C31 O4 C32 116.3(4) . . ?
C32 O4 Na1 125.1(4) . . ?
O4 C31 C30 114.0(5) . . ?
O3 C30 C31 117.3(6) . . ?
N5 N4 Na2 100.3(3) . . ?
N5 N4 C33 110.5(3) . . ?
C33 N4 Na2 149.0(3) . . ?
N4 N5 Na2 53.0(2) . . ?
N6 N5 Na2 58.4(2) . . ?
N6 N5 N4 111.4(3) . . ?
N5 N6 Na2 95.3(2) . . ?
N5 N6 C45 111.1(4) . . ?
C45 N6 Na2 153.4(3) . . ?
C34 C33 N4 120.8(4) . . ?
C34 C33 C38 121.4(4) . . ?
C38 C33 N4 117.8(4) . . ?
C33 C34 C39 122.2(4) . . ?
C35 C34 C33 118.3(4) . . ?
C35 C34 C39 119.5(5) . . ?
C46 C45 N6 115.6(4) . . ?
C50 C45 N6 124.3(4) . . ?
C50 C45 C46 119.9(4) . . ?
C34 C39 C41 110.8(4) . . ?
C34 C39 C40 113.0(4) . . ?
C40 C39 C41 110.6(4) . . ?
C33 C38 C42 121.2(4) . . ?
C37 C38 C33 117.6(5) . . ?
C37 C38 C42 121.2(4) . . ?
C45 C46 C51 119.6(4) . . ?
C47 C46 C45 119.4(5) . . ?
C47 C46 C51 121.0(5) . . ?
C36 C35 C34 121.0(5) . . ?
C48 C47 C46 121.6(6) . . ?
C36 C37 C38 122.0(5) . . ?
C37 C36 C35 119.7(5) . . ?
C46 C51 C52 107.6(5) . . ?
C46 C51 C53 113.9(5) . . ?
C52 C51 C53 110.0(5) . . ?
C38 C42 C43 112.8(4) . . ?
C44 C42 C38 111.4(4) . . ?
C44 C42 C43 109.6(4) . . ?
C50 C54 C56 114.4(5) . . ?
C50 C54 C55 111.3(5) . . ?
C56 C54 C55 109.8(4) . . ?
C45 C50 C54 123.0(4) . . ?
C45 C50 C49 117.7(5) . . ?
C49 C50 C54 119.4(5) . . ?
C48 C49 C50 121.1(6) . . ?
C47 C48 C49 120.3(6) . . ?
C64A O8A Na2 111.6(17) . . ?
C63A O8A Na2 104.3(13) . . ?
C63A O8A C64A 110.1(17) . . ?
C62A O7A Na2 119.3(11) . . ?
C62A O7A C61A 118.1(16) . . ?
C61A O7A Na2 117.6(14) . . ?
O8A C63A C62A 110.4(12) . . ?
O7A C62A C63A 105.4(12) . . ?
C61 O7 Na2 116.5(13) . . ?
C62 O7 Na2 101.8(11) . . ?
C62 O7 C61 106.7(13) . . ?
C63 O8 Na2 121.0(9) . . ?
C63 O8 C64 112.4(14) . . ?
C64 O8 Na2 125.9(13) . . ?
O7 C62 C63 115.1(11) . . ?
O8 C63 C62 110.2(11) . . ?
C57 O5 Na2 125.5(8) . . ?
C57 O5 C58 112.9(10) . . ?
C58 O5 Na2 112.7(8) . . ?
C59 O6 Na2 105.0(11) . . ?
C59 O6 C60 111.2(12) . . ?
C60 O6 Na2 119.2(7) . . ?
O5 C58 C59 108.8(13) . . ?
O6 C59 C58 107.0(12) . . ?
C57A O5A Na2 117(2) . . ?
C57A O5A C58A 115(3) . . ?
C58A O5A Na2 106(3) . . ?
C59A O6A Na2 112.9(17) . . ?
C59A O6A C60A 112(2) . . ?
C60A O6A Na2 132.5(16) . . ?
O5A C58A C59A 110(3) . . ?
O6A C59A C58A 110(3) . . ?

_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_PLAT026_6dme2               
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..        37% Check 
RESPONSE: Data was weak and the quality of this structure is poor.
;
# end Validation Reply Form
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_5(OEt2)2
_database_code_depnum_ccdc_archive 'CCDC 1971993'
loop_
_audit_author_name
_audit_author_address
'Alasdair McKay'
;Monash University
Australia
;
_audit_update_record             
;
2019-12-14 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_audit_creation_date             2019-12-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
''
alasdair.mckay@monash.edu
_chemical_name_common            ?
_chemical_name_systematic        '[Li(OEt2)2(N3Dipp2)]'
_chemical_formula_moiety         'C32 H54 Li N3 O2'
_chemical_formula_sum            'C32 H54 Li N3 O2'
_chemical_formula_weight         519.72
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.5557(5)
_cell_length_b                   11.0635(3)
_cell_length_c                   18.9451(6)
_cell_angle_alpha                90
_cell_angle_beta                 104.9150(10)
_cell_angle_gamma                90
_cell_volume                     3353.15(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7817
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.14
_cell_measurement_theta_min      2.35
_shelx_estimated_absorpt_T_max   0.994
_shelx_estimated_absorpt_T_min   0.988
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6772
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1145 before and 0.0624 after correction. The Ratio of minimum to maximum transmission is 0.9084. The λ/2 correction factor is 0.00150.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.029
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0601
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39776
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.131
_diffrn_reflns_theta_min         2.238
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4870
_reflns_number_total             7364
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         7364
_refine_ls_number_restraints     44
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0613
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0900P)²+1.4861P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1647
_refine_ls_wR_factor_ref         0.1900
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C28-C27 \\sim C28A-C27A
 with sigma of 0.02
 O1-C27 \\sim O1-C27A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1 \\sim C27A \\sim C28A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
O1 \\sim C27 \\sim C28: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
4. Rigid body (RIGU) restrains
 O1, C27A, C28A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, C27, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C27A)=Sof(H27A)=Sof(H27B)=Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(H28C)=1-FVAR(1)
 Sof(C28)=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C27)=Sof(H27C)=Sof(H27D)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C22(H22), C19(H19), C7(H7), C10(H10)
6.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C29(H29A,H29B), C25(H25A,H25B), C27A(H27A,H27B), C27(H27C,H27D)
6.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C17(H17), C16(H16), C5(H5), C3(H3), C4(H4)
6.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C9(H9A,H9B,H9C), C30(H30A,H30B,H30C), C8(H8A,H8B,H8C),
 C32(H32A,H32B,H32C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C26(H26A,H26B,
 H26C), C23(H23A,H23B,H23C), C12(H12A,H12B,H12C), C11(H11A,H11B,H11C),
 C28A(H28A,H28B,H28C), C28(H28D,H28E,H28F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N3 N 0.20512(8) 0.43569(13) 0.11689(8) 0.0244(3) Uani 1 1 d . . . . .
N2 N 0.25966(8) 0.34889(13) 0.11910(8) 0.0253(3) Uani 1 1 d . . . . .
N1 N 0.30158(9) 0.36428(14) 0.07001(8) 0.0285(4) Uani 1 1 d . . . . .
O2 O 0.15897(8) 0.50985(13) -0.06379(7) 0.0361(3) Uani 1 1 d . . . . .
C13 C 0.15534(10) 0.41677(16) 0.16659(9) 0.0229(4) Uani 1 1 d . . . . .
C18 C 0.14526(10) 0.51601(16) 0.21031(9) 0.0259(4) Uani 1 1 d . . . . .
C14 C 0.11334(10) 0.30692(17) 0.17147(9) 0.0263(4) Uani 1 1 d . . . . .
C15 C 0.06393(11) 0.30028(18) 0.22075(10) 0.0325(4) Uani 1 1 d . . . . .
H15 H 0.036221 0.226538 0.225127 0.039 Uiso 1 1 calc R . . . .
C17 C 0.09431(11) 0.50462(18) 0.25754(10) 0.0314(4) Uani 1 1 d . . . . .
H17 H 0.086934 0.571791 0.286497 0.038 Uiso 1 1 calc R . . . .
O1 O 0.30869(9) 0.66882(15) 0.04444(9) 0.0507(4) Uani 1 1 d D U . . .
C22 C 0.19503(12) 0.63048(18) 0.20864(11) 0.0343(4) Uani 1 1 d . . . . .
H22 H 0.202554 0.638459 0.158138 0.041 Uiso 1 1 calc R . . . .
C16 C 0.05397(12) 0.39695(19) 0.26323(11) 0.0351(5) Uani 1 1 d . . . . .
H16 H 0.019662 0.389923 0.296232 0.042 Uiso 1 1 calc R . . . .
C1 C 0.36110(12) 0.2694(2) 0.07407(10) 0.0355(5) Uani 1 1 d . . . . .
C19 C 0.11878(12) 0.19766(17) 0.12474(11) 0.0339(4) Uani 1 1 d . . . . .
H19 H 0.143562 0.225332 0.084628 0.041 Uiso 1 1 calc R . . . .
C6 C 0.43263(12) 0.2628(2) 0.13300(11) 0.0434(5) Uani 1 1 d . . . . .
C2 C 0.34702(13) 0.1837(2) 0.01732(11) 0.0424(5) Uani 1 1 d . . . . .
C24 C 0.15270(15) 0.7452(2) 0.22473(14) 0.0501(6) Uani 1 1 d . . . . .
H24A H 0.096248 0.749975 0.192150 0.075 Uiso 1 1 calc GR . . . .
H24B H 0.185231 0.815577 0.216829 0.075 Uiso 1 1 calc GR . . . .
H24C H 0.149300 0.744069 0.275614 0.075 Uiso 1 1 calc GR . . . .
C31 C 0.17592(13) 0.4943(2) -0.13353(11) 0.0424(5) Uani 1 1 d . . . . .
H31A H 0.137435 0.544995 -0.170455 0.051 Uiso 1 1 calc R . . . .
H31B H 0.167345 0.408803 -0.149014 0.051 Uiso 1 1 calc R . . . .
C7 C 0.27063(14) 0.1909(2) -0.04703(11) 0.0430(5) Uani 1 1 d . . . . .
H7 H 0.241740 0.269112 -0.043275 0.052 Uiso 1 1 calc R . . . .
C5 C 0.48643(15) 0.1645(3) 0.13558(13) 0.0583(7) Uani 1 1 d . . . . .
H5 H 0.534725 0.157587 0.175344 0.070 Uiso 1 1 calc R . . . .
C9 C 0.29299(17) 0.1899(3) -0.12058(12) 0.0561(6) Uani 1 1 d . . . . .
H9A H 0.330772 0.257282 -0.122450 0.084 Uiso 1 1 calc GR . . . .
H9B H 0.241918 0.198206 -0.160203 0.084 Uiso 1 1 calc GR . . . .
H9C H 0.320608 0.113401 -0.126146 0.084 Uiso 1 1 calc GR . . . .
C29 C 0.07281(12) 0.4890(2) -0.06476(13) 0.0430(5) Uani 1 1 d . . . . .
H29A H 0.036635 0.534558 -0.105915 0.052 Uiso 1 1 calc R . . . .
H29B H 0.062558 0.520602 -0.018952 0.052 Uiso 1 1 calc R . . . .
C10 C 0.45032(12) 0.3572(2) 0.19343(11) 0.0459(6) Uani 1 1 d . . . . .
H10 H 0.411585 0.426625 0.176190 0.055 Uiso 1 1 calc R . . . .
C30 C 0.04903(14) 0.3586(2) -0.07234(13) 0.0494(6) Uani 1 1 d . . . . .
H30A H 0.055249 0.328135 -0.119223 0.074 Uiso 1 1 calc GR . . . .
H30B H -0.009232 0.349556 -0.070368 0.074 Uiso 1 1 calc GR . . . .
H30C H 0.085449 0.312603 -0.032412 0.074 Uiso 1 1 calc GR . . . .
C8 C 0.20975(17) 0.0888(2) -0.04335(14) 0.0552(6) Uani 1 1 d . . . . .
H8A H 0.235198 0.011045 -0.049888 0.083 Uiso 1 1 calc GR . . . .
H8B H 0.158150 0.099708 -0.082103 0.083 Uiso 1 1 calc GR . . . .
H8C H 0.196828 0.090247 0.004302 0.083 Uiso 1 1 calc GR . . . .
C32 C 0.26453(14) 0.5306(3) -0.12761(13) 0.0535(6) Uani 1 1 d . . . . .
H32A H 0.272116 0.615929 -0.113630 0.080 Uiso 1 1 calc GR . . . .
H32B H 0.277305 0.518695 -0.174849 0.080 Uiso 1 1 calc GR . . . .
H32C H 0.302180 0.480852 -0.090477 0.080 Uiso 1 1 calc GR . . . .
C20 C 0.17766(17) 0.1019(2) 0.16880(13) 0.0529(6) Uani 1 1 d . . . . .
H20A H 0.232790 0.137878 0.189437 0.079 Uiso 1 1 calc GR . . . .
H20B H 0.182945 0.034566 0.136705 0.079 Uiso 1 1 calc GR . . . .
H20C H 0.154877 0.072165 0.208442 0.079 Uiso 1 1 calc GR . . . .
C21 C 0.03314(16) 0.1434(2) 0.08888(13) 0.0559(7) Uani 1 1 d . . . . .
H21A H 0.009889 0.106585 0.126410 0.084 Uiso 1 1 calc GR . . . .
H21B H 0.039070 0.081559 0.053508 0.084 Uiso 1 1 calc GR . . . .
H21C H -0.004451 0.207216 0.063725 0.084 Uiso 1 1 calc GR . . . .
C3 C 0.40236(15) 0.0871(2) 0.02270(13) 0.0555(7) Uani 1 1 d . . . . .
H3 H 0.392587 0.027571 -0.014690 0.067 Uiso 1 1 calc R . . . .
C26 C 0.18350(16) 0.7848(2) 0.02210(18) 0.0674(8) Uani 1 1 d . . . . .
H26A H 0.175321 0.774775 -0.030669 0.101 Uiso 1 1 calc GR . . . .
H26B H 0.159970 0.862502 0.031779 0.101 Uiso 1 1 calc GR . . . .
H26C H 0.155309 0.719070 0.040933 0.101 Uiso 1 1 calc GR . . . .
C23 C 0.28124(14) 0.6182(2) 0.26017(19) 0.0719(9) Uani 1 1 d . . . . .
H23A H 0.276410 0.613457 0.310573 0.108 Uiso 1 1 calc GR . . . .
H23B H 0.315156 0.688623 0.254958 0.108 Uiso 1 1 calc GR . . . .
H23C H 0.307973 0.544602 0.248330 0.108 Uiso 1 1 calc GR . . . .
C25 C 0.27553(17) 0.7820(2) 0.05935(18) 0.0677(8) Uani 1 1 d . . . . .
H25A H 0.304362 0.848830 0.041008 0.081 Uiso 1 1 calc R . . . .
H25B H 0.284313 0.792393 0.112703 0.081 Uiso 1 1 calc R . . . .
Li1 Li 0.2419(2) 0.5182(3) 0.03007(17) 0.0339(7) Uani 1 1 d . . . . .
C4 C 0.47095(16) 0.0769(3) 0.08154(14) 0.0618(7) Uani 1 1 d . . . . .
H4 H 0.507642 0.009889 0.085090 0.074 Uiso 1 1 calc R . . . .
C12 C 0.43062(17) 0.3071(3) 0.26164(13) 0.0648(8) Uani 1 1 d . . . . .
H12A H 0.372180 0.280714 0.249985 0.097 Uiso 1 1 calc GR . . . .
H12B H 0.439664 0.370146 0.299231 0.097 Uiso 1 1 calc GR . . . .
H12C H 0.467285 0.238244 0.279789 0.097 Uiso 1 1 calc GR . . . .
C11 C 0.53924(15) 0.4063(3) 0.21020(18) 0.0764(9) Uani 1 1 d . . . . .
H11A H 0.578692 0.342175 0.231899 0.115 Uiso 1 1 calc GR . . . .
H11B H 0.544967 0.473861 0.244576 0.115 Uiso 1 1 calc GR . . . .
H11C H 0.551253 0.434370 0.164900 0.115 Uiso 1 1 calc GR . . . .
C27A C 0.3975(6) 0.678(2) 0.0787(9) 0.078(5) Uani 0.499(11) 1 d D U P A 2
H27A H 0.409237 0.649013 0.129838 0.094 Uiso 0.499(11) 1 calc R . P A 2
H27B H 0.415584 0.762963 0.079173 0.094 Uiso 0.499(11) 1 calc R . P A 2
C28A C 0.4450(4) 0.6016(11) 0.0368(4) 0.094(4) Uani 0.499(11) 1 d D U P A 2
H28A H 0.440825 0.638390 -0.011046 0.141 Uiso 0.499(11) 1 calc GR . P A 2
H28B H 0.421173 0.520066 0.030201 0.141 Uiso 0.499(11) 1 calc GR . P A 2
H28C H 0.503858 0.597125 0.064137 0.141 Uiso 0.499(11) 1 calc GR . P A 2
C28 C 0.4454(4) 0.7079(9) 0.0279(4) 0.076(3) Uani 0.501(11) 1 d D U P A 1
H28D H 0.427855 0.679538 -0.022751 0.114 Uiso 0.501(11) 1 calc GR . P A 1
H28E H 0.505085 0.691066 0.047885 0.114 Uiso 0.501(11) 1 calc GR . P A 1
H28F H 0.435667 0.795100 0.029382 0.114 Uiso 0.501(11) 1 calc GR . P A 1
C27 C 0.3962(6) 0.6437(19) 0.0725(7) 0.062(3) Uani 0.501(11) 1 d D U P A 1
H27C H 0.405885 0.555519 0.071063 0.075 Uiso 0.501(11) 1 calc R . P A 1
H27D H 0.414853 0.670574 0.123985 0.075 Uiso 0.501(11) 1 calc R . P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N3 N2 1.3115(19) . ?
N3 C13 1.417(2) . ?
N3 Li1 2.104(3) . ?
N2 N1 1.307(2) . ?
N1 C1 1.428(2) . ?
N1 Li1 2.016(4) . ?
O2 C31 1.430(2) . ?
O2 C29 1.440(2) . ?
O2 Li1 1.949(3) . ?
C13 C18 1.411(2) . ?
C13 C14 1.415(2) . ?
C18 C17 1.385(2) . ?
C18 C22 1.516(3) . ?
C14 C15 1.393(3) . ?
C14 C19 1.515(3) . ?
C15 C16 1.374(3) . ?
C17 C16 1.383(3) . ?
O1 C25 1.425(3) . ?
O1 Li1 1.979(4) . ?
O1 C27A 1.449(11) . ?
O1 C27 1.436(10) . ?
C22 C24 1.518(3) . ?
C22 C23 1.514(3) . ?
C1 C6 1.405(3) . ?
C1 C2 1.407(3) . ?
C19 C20 1.533(3) . ?
C19 C21 1.529(3) . ?
C6 C5 1.399(3) . ?
C6 C10 1.522(3) . ?
C2 C7 1.516(3) . ?
C2 C3 1.395(3) . ?
C31 C32 1.497(3) . ?
C7 C9 1.531(3) . ?
C7 C8 1.527(3) . ?
C5 C4 1.384(4) . ?
C29 C30 1.492(3) . ?
C10 C12 1.517(3) . ?
C10 C11 1.524(3) . ?
C3 C4 1.376(4) . ?
C26 C25 1.506(4) . ?
C27A C28A 1.509(15) . ?
C28 C27 1.496(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 N3 C13 112.58(14) . . ?
N2 N3 Li1 90.42(13) . . ?
C13 N3 Li1 156.68(14) . . ?
N1 N2 N3 111.68(14) . . ?
N2 N1 C1 110.58(14) . . ?
N2 N1 Li1 94.49(13) . . ?
C1 N1 Li1 154.93(15) . . ?
C31 O2 C29 113.47(15) . . ?
C31 O2 Li1 126.08(15) . . ?
C29 O2 Li1 118.82(15) . . ?
C18 C13 N3 116.86(15) . . ?
C18 C13 C14 119.71(15) . . ?
C14 C13 N3 123.35(15) . . ?
C13 C18 C22 119.40(15) . . ?
C17 C18 C13 119.50(17) . . ?
C17 C18 C22 120.96(17) . . ?
C13 C14 C19 122.89(15) . . ?
C15 C14 C13 118.19(16) . . ?
C15 C14 C19 118.91(17) . . ?
C16 C15 C14 122.10(18) . . ?
C16 C17 C18 121.02(18) . . ?
C25 O1 Li1 122.49(17) . . ?
C25 O1 C27A 104.5(8) . . ?
C25 O1 C27 120.0(8) . . ?
C27A O1 Li1 125.8(9) . . ?
C27 O1 Li1 111.3(8) . . ?
C18 C22 C24 114.38(16) . . ?
C23 C22 C18 109.82(17) . . ?
C23 C22 C24 110.66(19) . . ?
C15 C16 C17 119.45(17) . . ?
C6 C1 N1 120.68(18) . . ?
C6 C1 C2 120.78(18) . . ?
C2 C1 N1 118.53(17) . . ?
C14 C19 C20 110.98(16) . . ?
C14 C19 C21 112.67(17) . . ?
C21 C19 C20 110.96(19) . . ?
C1 C6 C10 121.44(18) . . ?
C5 C6 C1 117.9(2) . . ?
C5 C6 C10 120.66(19) . . ?
C1 C2 C7 121.27(18) . . ?
C3 C2 C1 119.0(2) . . ?
C3 C2 C7 119.7(2) . . ?
O2 C31 C32 108.68(17) . . ?
C2 C7 C9 112.60(18) . . ?
C2 C7 C8 110.40(19) . . ?
C8 C7 C9 110.67(19) . . ?
C4 C5 C6 121.5(2) . . ?
O2 C29 C30 113.07(18) . . ?
C6 C10 C11 112.95(19) . . ?
C12 C10 C6 110.4(2) . . ?
C12 C10 C11 111.1(2) . . ?
C4 C3 C2 120.8(2) . . ?
O1 C25 C26 108.7(2) . . ?
N1 Li1 N3 63.41(11) . . ?
O2 Li1 N3 114.51(16) . . ?
O2 Li1 N1 117.66(18) . . ?
O2 Li1 O1 113.76(17) . . ?
O1 Li1 N3 121.45(17) . . ?
O1 Li1 N1 117.20(16) . . ?
C3 C4 C5 119.9(2) . . ?
O1 C27A C28A 109.5(11) . . ?
O1 C27 C28 110.1(10) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_5(THF)2
_database_code_depnum_ccdc_archive 'CCDC 1971994'
loop_
_audit_author_name
_audit_author_address
'Alasdair McKay'
;Monash University
Australia
;
_audit_update_record             
;
2019-12-14 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_audit_creation_date             2019-12-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
''
alasdair.mckay@monash.edu
_chemical_name_common            ?
_chemical_name_systematic        '[Li(THF)2(N3Dipp2)]'
_chemical_formula_moiety         'C32 H50 Li N3 O2'
_chemical_formula_sum            'C32 H50 Li N3 O2'
_chemical_formula_weight         515.69
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   18.8789(9)
_cell_length_b                   18.6075(9)
_cell_length_c                   19.5150(8)
_cell_angle_alpha                90
_cell_angle_beta                 111.063(2)
_cell_angle_gamma                90
_cell_volume                     6397.4(5)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    8242
_cell_measurement_temperature    150
_cell_measurement_theta_max      22.96
_cell_measurement_theta_min      2.31
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6528
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1022 before and 0.0798 after correction. The Ratio of minimum to maximum transmission is 0.8757. The λ/2 correction factor is 0.00150.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.071
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0923
_diffrn_reflns_av_unetI/netI     0.0792
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            78234
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.139
_diffrn_reflns_theta_min         1.565
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7373
_reflns_number_total             14123
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       0.0019(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     758
_refine_ls_number_reflns         14123
_refine_ls_number_restraints     178
_refine_ls_R_factor_all          0.1352
_refine_ls_R_factor_gt           0.0621
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0750P)²+2.0450P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1548
_refine_ls_wR_factor_ref         0.1917
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C64-C63 \\sim C63-C62 \\sim C62-C61
 with sigma of 0.02
 O4-C64 \\sim O4-C61
 with sigma of 0.02
 O4-C63 \\sim O4-C62
 with sigma of 0.04
 C63-C61 \\sim C64-C62
 with sigma of 0.04
 C64A-C63A \\sim C63A-C62A \\sim C62A-C61A
 with sigma of 0.02
 O4A-C64A \\sim O4A-C61A
 with sigma of 0.02
 O4A-C63A \\sim O4A-C62A
 with sigma of 0.04
 C63A-C61A \\sim C64A-C62A
 with sigma of 0.04
 O4-Li3 \\sim O4A-Li3
 with sigma of 0.02
 C30-C31 \\sim C30-C31A \\sim C32-C31A \\sim C32-C31
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O4 \\sim C64 \\sim C63 \\sim C62 \\sim C61: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O4A \\sim C64A \\sim C63A \\sim C62A \\sim C61A: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
C32 \\sim C31 \\sim C30: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C32 \\sim C31A \\sim C30: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
4. Rigid body (RIGU) restrains
 O4, C64, C63, C62, C61
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4A, C64A, C63A, C62A, C61A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32, C31, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32, C31A, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O4A)=Sof(C64A)=Sof(H64C)=Sof(H64D)=Sof(C63A)=Sof(H63C)=Sof(H63D)=
 Sof(C62A)=Sof(H62C)=Sof(H62D)=Sof(C61A)=Sof(H61C)=Sof(H61D)=1-FVAR(1)
 Sof(O4)=Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(C62)=
 Sof(H62A)=Sof(H62B)=Sof(C61)=Sof(H61A)=Sof(H61B)=FVAR(1)
 Sof(H32C)=Sof(H32D)=Sof(H30C)=Sof(H30D)=Sof(C31A)=Sof(H31C)=Sof(H31D)=1-FVAR(2)
 Sof(H32A)=Sof(H32B)=Sof(H30A)=Sof(H30B)=Sof(C31)=Sof(H31A)=Sof(H31B)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C19(H19), C39(H39), C22(H22), C51(H51), C54(H54), C42(H42), C10(H10)
6.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C57(H57A,H57B), C26(H26A,H26B), C25(H25A,H25B), C29(H29A,
 H29B), C60(H60A,H60B), C27(H27A,H27B), C32(H32A,H32B), C32(H32C,H32D),
 C30(H30A,H30B), C30(H30C,H30D), C58(H58A,H58B), C59(H59A,H59B), C31(H31A,H31B),
  C64(H64A,H64B), C63(H63A,H63B), C62(H62A,H62B), C61(H61A,H61B), C64A(H64C,
 H64D), C63A(H63C,H63D), C62A(H62C,H62D), C61A(H61C,H61D), C31A(H31C,H31D)
6.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C47(H47), C17(H17), C3(H3), C35(H35), C4(H4), C49(H49),
 C48(H48), C5(H5), C37(H37), C36(H36)
6.d Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C12(H12A,H12B,H12C), C11(H11A,H11B,H11C), C20(H20A,H20B,
 H20C), C24(H24A,H24B,H24C), C21(H21A,H21B,H21C), C43(H43A,H43B,H43C), C44(H44A,
 H44B,H44C), C55(H55A,H55B,H55C), C41(H41A,H41B,H41C), C53(H53A,H53B,H53C),
 C23(H23A,H23B,H23C), C8(H8A,H8B,H8C), C56(H56A,H56B,H56C), C52(H52A,H52B,H52C),
  C9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.24681(10) 0.20966(9) 0.19096(9) 0.0292(4) Uani 1 1 d . . . . .
N3 N 0.16534(10) 0.23868(9) 0.08559(9) 0.0298(4) Uani 1 1 d . . . . .
N2 N 0.17842(10) 0.19779(9) 0.14361(9) 0.0290(4) Uani 1 1 d . . . . .
N5 N 0.30317(10) 0.70593(9) 0.33651(9) 0.0314(4) Uani 1 1 d . . . . .
N4 N 0.30523(10) 0.74259(9) 0.39482(9) 0.0322(4) Uani 1 1 d . . . . .
N6 N 0.23824(10) 0.71513(9) 0.28281(9) 0.0331(4) Uani 1 1 d . . . . .
O3 O 0.12740(9) 0.75248(9) 0.38505(9) 0.0501(4) Uani 1 1 d . . . . .
O1 O 0.31493(9) 0.37211(9) 0.17147(9) 0.0504(4) Uani 1 1 d . . . . .
C13 C 0.09407(12) 0.22542(11) 0.02904(10) 0.0294(5) Uani 1 1 d . . . . .
C1 C 0.26390(12) 0.17362(11) 0.25927(11) 0.0300(5) Uani 1 1 d . . . . .
C33 C 0.37189(12) 0.73165(12) 0.45630(11) 0.0336(5) Uani 1 1 d . . . . .
C14 C 0.07480(12) 0.15835(11) -0.00534(11) 0.0336(5) Uani 1 1 d . . . . .
C45 C 0.23524(12) 0.67974(11) 0.21726(11) 0.0316(5) Uani 1 1 d . . . . .
C46 C 0.19126(12) 0.61759(12) 0.19544(11) 0.0347(5) Uani 1 1 d . . . . .
C50 C 0.27243(13) 0.70926(12) 0.17295(12) 0.0380(5) Uani 1 1 d . . . . .
C34 C 0.39952(13) 0.66328(12) 0.48443(12) 0.0396(6) Uani 1 1 d . . . . .
C2 C 0.32715(12) 0.12810(11) 0.28177(11) 0.0349(5) Uani 1 1 d . . . . .
O2 O 0.32781(10) 0.26079(10) 0.06509(10) 0.0594(5) Uani 1 1 d . . . . .
C7 C 0.36600(12) 0.10813(12) 0.22868(12) 0.0389(5) Uani 1 1 d . . . . .
H7 H 0.357313 0.148437 0.192686 0.047 Uiso 1 1 calc R . . . .
C15 C 0.00465(13) 0.15090(13) -0.06155(12) 0.0420(6) Uani 1 1 d . . . . .
H15 H -0.009433 0.105457 -0.084634 0.050 Uiso 1 1 calc R . . . .
C6 C 0.22363(13) 0.18847(11) 0.30655(12) 0.0352(5) Uani 1 1 d . . . . .
C16 C -0.04504(14) 0.20792(14) -0.08464(13) 0.0465(6) Uani 1 1 d . . . . .
H16 H -0.092981 0.201573 -0.122750 0.056 Uiso 1 1 calc R . . . .
C18 C 0.04432(12) 0.28433(12) 0.00498(11) 0.0336(5) Uani 1 1 d . . . . .
C38 C 0.40908(13) 0.79390(12) 0.49280(12) 0.0393(6) Uani 1 1 d . . . . .
C19 C 0.12906(14) 0.09490(12) 0.01529(12) 0.0397(6) Uani 1 1 d . . . . .
H19 H 0.180254 0.114088 0.045548 0.048 Uiso 1 1 calc R . . . .
C47 C 0.18522(13) 0.58557(12) 0.12940(12) 0.0411(6) Uani 1 1 d . . . . .
H47 H 0.154851 0.543715 0.113772 0.049 Uiso 1 1 calc R . . . .
C39 C 0.36077(15) 0.59398(12) 0.44867(13) 0.0443(6) Uani 1 1 d . . . . .
H39 H 0.309436 0.606822 0.412699 0.053 Uiso 1 1 calc R . . . .
C17 C -0.02443(13) 0.27424(13) -0.05184(12) 0.0418(6) Uani 1 1 d . . . . .
H17 H -0.058121 0.313748 -0.068601 0.050 Uiso 1 1 calc R . . . .
C22 C 0.06769(13) 0.35736(12) 0.04037(12) 0.0403(6) Uani 1 1 d . . . . .
H22 H 0.102999 0.349268 0.092024 0.048 Uiso 1 1 calc R . . . .
C3 C 0.35012(14) 0.09787(13) 0.35133(12) 0.0461(6) Uani 1 1 d . . . . .
H3 H 0.392941 0.066855 0.367011 0.055 Uiso 1 1 calc R . . . .
C51 C 0.15235(14) 0.58496(13) 0.24380(13) 0.0447(6) Uani 1 1 d . . . . .
H51 H 0.159800 0.618885 0.285561 0.054 Uiso 1 1 calc R . . . .
C54 C 0.31925(15) 0.77700(14) 0.19583(13) 0.0494(7) Uani 1 1 d . . . . .
H54 H 0.305335 0.799973 0.235580 0.059 Uiso 1 1 calc R . . . .
C35 C 0.46493(15) 0.65964(15) 0.54670(13) 0.0548(7) Uani 1 1 d . . . . .
H35 H 0.484550 0.613838 0.565721 0.066 Uiso 1 1 calc R . . . .
C4 C 0.31189(16) 0.11207(14) 0.39795(13) 0.0530(7) Uani 1 1 d . . . . .
H4 H 0.328643 0.091305 0.445591 0.064 Uiso 1 1 calc R . . . .
C49 C 0.26562(15) 0.67456(13) 0.10798(13) 0.0462(6) Uani 1 1 d . . . . .
H49 H 0.291230 0.693375 0.077979 0.055 Uiso 1 1 calc R . . . .
C48 C 0.22219(14) 0.61304(13) 0.08609(12) 0.0456(6) Uani 1 1 d . . . . .
H48 H 0.217962 0.589929 0.041378 0.055 Uiso 1 1 calc R . . . .
C42 C 0.38046(15) 0.86744(12) 0.46151(13) 0.0464(6) Uani 1 1 d . . . . .
H42 H 0.323854 0.864537 0.439181 0.056 Uiso 1 1 calc R . . . .
C10 C 0.15705(14) 0.24013(12) 0.28429(13) 0.0422(6) Uani 1 1 d . . . . .
H10 H 0.123809 0.227614 0.232948 0.051 Uiso 1 1 calc R . . . .
C5 C 0.24913(15) 0.15654(13) 0.37549(12) 0.0471(6) Uani 1 1 d . . . . .
H5 H 0.222796 0.165499 0.407950 0.057 Uiso 1 1 calc R . . . .
C37 C 0.47390(15) 0.78651(15) 0.55520(13) 0.0539(7) Uani 1 1 d . . . . .
H37 H 0.499245 0.828291 0.580131 0.065 Uiso 1 1 calc R . . . .
C40 C 0.40505(16) 0.55820(14) 0.40610(14) 0.0566(7) Uani 1 1 d . . . . .
H40A H 0.405297 0.589798 0.366012 0.085 Uiso 1 1 calc GR . . . .
H40B H 0.380923 0.512425 0.385784 0.085 Uiso 1 1 calc GR . . . .
H40C H 0.457355 0.549414 0.439189 0.085 Uiso 1 1 calc GR . . . .
C12 C 0.18391(16) 0.31749(13) 0.28313(15) 0.0572(7) Uani 1 1 d . . . . .
H12A H 0.217819 0.331196 0.332526 0.086 Uiso 1 1 calc GR . . . .
H12B H 0.139926 0.349724 0.267131 0.086 Uiso 1 1 calc GR . . . .
H12C H 0.211203 0.321133 0.249003 0.086 Uiso 1 1 calc GR . . . .
C11 C 0.10811(15) 0.23522(15) 0.33196(14) 0.0552(7) Uani 1 1 d . . . . .
H11A H 0.090060 0.185774 0.331454 0.083 Uiso 1 1 calc GR . . . .
H11B H 0.064521 0.267627 0.312473 0.083 Uiso 1 1 calc GR . . . .
H11C H 0.138429 0.249127 0.382464 0.083 Uiso 1 1 calc GR . . . .
C36 C 0.50199(17) 0.72003(16) 0.58149(14) 0.0633(8) Uani 1 1 d . . . . .
H36 H 0.546984 0.715911 0.623674 0.076 Uiso 1 1 calc R . . . .
C20 C 0.10698(15) 0.04079(13) 0.06259(14) 0.0551(7) Uani 1 1 d . . . . .
H20A H 0.106163 0.064607 0.107088 0.083 Uiso 1 1 calc GR . . . .
H20B H 0.144056 0.001537 0.076237 0.083 Uiso 1 1 calc GR . . . .
H20C H 0.056500 0.021391 0.034896 0.083 Uiso 1 1 calc GR . . . .
C28 C 0.32011(17) 0.43841(14) 0.13808(15) 0.0627(8) Uani 1 1 d . . . . .
H28A H 0.269638 0.461640 0.117911 0.075 Uiso 1 1 calc R . . . .
H28B H 0.339132 0.430762 0.097522 0.075 Uiso 1 1 calc R . . . .
C24 C 0.11089(16) 0.39870(14) 0.00082(14) 0.0563(7) Uani 1 1 d . . . . .
H24A H 0.155441 0.370930 0.002061 0.084 Uiso 1 1 calc GR . . . .
H24B H 0.127300 0.445067 0.025178 0.084 Uiso 1 1 calc GR . . . .
H24C H 0.077811 0.406791 -0.050312 0.084 Uiso 1 1 calc GR . . . .
C21 C 0.13672(18) 0.05862(14) -0.05175(15) 0.0620(8) Uani 1 1 d . . . . .
H21A H 0.088284 0.036299 -0.081122 0.093 Uiso 1 1 calc GR . . . .
H21B H 0.176288 0.021682 -0.035734 0.093 Uiso 1 1 calc GR . . . .
H21C H 0.150498 0.094563 -0.081493 0.093 Uiso 1 1 calc GR . . . .
C57 C 0.15319(18) 0.71033(17) 0.45070(16) 0.0687(9) Uani 1 1 d . . . . .
H57A H 0.140701 0.733813 0.490462 0.082 Uiso 1 1 calc R . . . .
H57B H 0.208678 0.702332 0.467612 0.082 Uiso 1 1 calc R . . . .
C43 C 0.40903(19) 0.88627(15) 0.40061(15) 0.0686(8) Uani 1 1 d . . . . .
H43A H 0.464427 0.890883 0.420881 0.103 Uiso 1 1 calc GR . . . .
H43B H 0.386498 0.931893 0.378085 0.103 Uiso 1 1 calc GR . . . .
H43C H 0.394665 0.848234 0.363388 0.103 Uiso 1 1 calc GR . . . .
C44 C 0.39996(18) 0.92722(14) 0.51899(16) 0.0675(8) Uani 1 1 d . . . . .
H44A H 0.385537 0.912310 0.560337 0.101 Uiso 1 1 calc GR . . . .
H44B H 0.372215 0.970986 0.496968 0.101 Uiso 1 1 calc GR . . . .
H44C H 0.454654 0.936720 0.536517 0.101 Uiso 1 1 calc GR . . . .
C55 C 0.3030(2) 0.83129(15) 0.13409(16) 0.0751(9) Uani 1 1 d . . . . .
H55A H 0.317544 0.811053 0.094702 0.113 Uiso 1 1 calc GR . . . .
H55B H 0.332177 0.875204 0.152789 0.113 Uiso 1 1 calc GR . . . .
H55C H 0.248659 0.842682 0.114890 0.113 Uiso 1 1 calc GR . . . .
C41 C 0.34957(19) 0.54075(14) 0.50392(16) 0.0688(8) Uani 1 1 d . . . . .
H41A H 0.399194 0.524818 0.538038 0.103 Uiso 1 1 calc GR . . . .
H41B H 0.320668 0.499115 0.477589 0.103 Uiso 1 1 calc GR . . . .
H41C H 0.321701 0.564292 0.531444 0.103 Uiso 1 1 calc GR . . . .
C53 C 0.06768(17) 0.5763(2) 0.20417(17) 0.0805(10) Uani 1 1 d . . . . .
H53A H 0.045385 0.622755 0.184011 0.121 Uiso 1 1 calc GR . . . .
H53B H 0.044559 0.558960 0.238717 0.121 Uiso 1 1 calc GR . . . .
H53C H 0.058261 0.541540 0.164134 0.121 Uiso 1 1 calc GR . . . .
C23 C 0.00070(17) 0.40164(15) 0.04338(17) 0.0676(8) Uani 1 1 d . . . . .
H23A H -0.031276 0.416123 -0.006443 0.101 Uiso 1 1 calc GR . . . .
H23B H 0.019667 0.444555 0.073518 0.101 Uiso 1 1 calc GR . . . .
H23C H -0.029266 0.372643 0.064987 0.101 Uiso 1 1 calc GR . . . .
C8 C 0.32844(19) 0.04158(16) 0.18589(17) 0.0758(9) Uani 1 1 d . . . . .
H8A H 0.337326 0.000571 0.219458 0.114 Uiso 1 1 calc GR . . . .
H8B H 0.350050 0.031337 0.148170 0.114 Uiso 1 1 calc GR . . . .
H8C H 0.273734 0.049886 0.162448 0.114 Uiso 1 1 calc GR . . . .
C56 C 0.40375(17) 0.75903(18) 0.22842(18) 0.0762(9) Uani 1 1 d . . . . .
H56A H 0.413371 0.727075 0.270730 0.114 Uiso 1 1 calc GR . . . .
H56B H 0.433040 0.803412 0.244227 0.114 Uiso 1 1 calc GR . . . .
H56C H 0.419068 0.735060 0.191221 0.114 Uiso 1 1 calc GR . . . .
C26 C 0.42222(17) 0.43203(17) 0.25003(16) 0.0686(8) Uani 1 1 d . . . . .
H26A H 0.465094 0.415832 0.236009 0.082 Uiso 1 1 calc R . . . .
H26B H 0.442429 0.452555 0.300158 0.082 Uiso 1 1 calc R . . . .
C25 C 0.36918(19) 0.37277(18) 0.24545(15) 0.0790(10) Uani 1 1 d . . . . .
H25A H 0.396774 0.326475 0.257005 0.095 Uiso 1 1 calc R . . . .
H25B H 0.343159 0.380411 0.280778 0.095 Uiso 1 1 calc R . . . .
Li2 Li 0.2700(2) 0.2842(2) 0.1242(2) 0.0418(9) Uani 1 1 d . . . . .
C29 C 0.40728(16) 0.27354(19) 0.0848(2) 0.0854(11) Uani 1 1 d . . . . .
H29A H 0.429403 0.291087 0.136039 0.102 Uiso 1 1 calc R . . . .
H29B H 0.416304 0.310070 0.051982 0.102 Uiso 1 1 calc R . . . .
C52 C 0.1897(2) 0.51451(16) 0.27629(19) 0.0826(10) Uani 1 1 d . . . . .
H52A H 0.181177 0.479094 0.236969 0.124 Uiso 1 1 calc GR . . . .
H52B H 0.167696 0.496852 0.311592 0.124 Uiso 1 1 calc GR . . . .
H52C H 0.244339 0.522018 0.301337 0.124 Uiso 1 1 calc GR . . . .
C60 C 0.05214(17) 0.73061(19) 0.3421(2) 0.0808(10) Uani 1 1 d . . . . .
H60A H 0.047768 0.722362 0.290656 0.097 Uiso 1 1 calc R . . . .
H60B H 0.015556 0.768554 0.342586 0.097 Uiso 1 1 calc R . . . .
C27 C 0.37431(19) 0.48465(18) 0.19670(18) 0.0866(11) Uani 1 1 d . . . . .
H27A H 0.405201 0.514913 0.176399 0.104 Uiso 1 1 calc R . . . .
H27B H 0.346835 0.516053 0.219730 0.104 Uiso 1 1 calc R . . . .
C32 C 0.30954(17) 0.19919(18) 0.01793(17) 0.0733(9) Uani 1 1 d D U . . .
H32A H 0.295137 0.158460 0.042853 0.088 Uiso 0.565(12) 1 calc R . P A 1
H32B H 0.266160 0.210201 -0.027646 0.088 Uiso 0.565(12) 1 calc R . P A 1
H32C H 0.295384 0.213343 -0.034198 0.088 Uiso 0.435(12) 1 calc R . P A 2
H32D H 0.267396 0.171390 0.023847 0.088 Uiso 0.435(12) 1 calc R . P A 2
C9 C 0.45032(15) 0.09750(19) 0.26386(16) 0.0749(9) Uani 1 1 d . . . . .
H9A H 0.473650 0.141206 0.290455 0.112 Uiso 1 1 calc GR . . . .
H9B H 0.471519 0.087327 0.225824 0.112 Uiso 1 1 calc GR . . . .
H9C H 0.460771 0.057045 0.298225 0.112 Uiso 1 1 calc GR . . . .
Li3 Li 0.1987(2) 0.7833(2) 0.3422(2) 0.0444(10) Uani 1 1 d D . . . .
C30 C 0.44110(18) 0.20605(19) 0.0774(2) 0.0822(10) Uani 1 1 d D U . . .
H30A H 0.446226 0.172844 0.118533 0.099 Uiso 0.565(12) 1 calc R . P A 1
H30B H 0.490889 0.212330 0.071951 0.099 Uiso 0.565(12) 1 calc R . P A 1
H30C H 0.472771 0.212393 0.046929 0.099 Uiso 0.435(12) 1 calc R . P A 2
H30D H 0.473920 0.188211 0.126296 0.099 Uiso 0.435(12) 1 calc R . P A 2
C58 C 0.1105(3) 0.64097(18) 0.4277(3) 0.1100(16) Uani 1 1 d . . . . .
H58A H 0.136873 0.608399 0.404587 0.132 Uiso 1 1 calc R . . . .
H58B H 0.104560 0.616287 0.470267 0.132 Uiso 1 1 calc R . . . .
C59 C 0.0354(3) 0.6639(2) 0.3737(3) 0.1104(16) Uani 1 1 d . . . . .
H59A H 0.014317 0.626894 0.335270 0.132 Uiso 1 1 calc R . . . .
H59B H -0.001320 0.672738 0.398454 0.132 Uiso 1 1 calc R . . . .
C31 C 0.3747(3) 0.1806(4) 0.0007(5) 0.072(2) Uani 0.565(12) 1 d D U P A 1
H31A H 0.376749 0.207787 -0.042198 0.087 Uiso 0.565(12) 1 calc R . P A 1
H31B H 0.377019 0.128423 -0.008159 0.087 Uiso 0.565(12) 1 calc R . P A 1
O4 O 0.1658(7) 0.8789(4) 0.3088(5) 0.070(3) Uani 0.610(10) 1 d D U P B 1
C64 C 0.1931(6) 0.9222(4) 0.2644(6) 0.081(3) Uani 0.610(10) 1 d D U P B 1
H64A H 0.176793 0.902705 0.213836 0.097 Uiso 0.610(10) 1 calc R . P B 1
H64B H 0.249200 0.924541 0.284806 0.097 Uiso 0.610(10) 1 calc R . P B 1
C63 C 0.1612(6) 0.9910(3) 0.2645(5) 0.092(3) Uani 0.610(10) 1 d D U P B 1
H63A H 0.201019 1.028443 0.275568 0.111 Uiso 0.610(10) 1 calc R . P B 1
H63B H 0.122038 1.001445 0.215891 0.111 Uiso 0.610(10) 1 calc R . P B 1
C62 C 0.1298(8) 0.9903(5) 0.3168(8) 0.161(5) Uani 0.610(10) 1 d D U P B 1
H62A H 0.080884 1.016394 0.298737 0.193 Uiso 0.610(10) 1 calc R . P B 1
H62B H 0.163871 1.015423 0.361132 0.193 Uiso 0.610(10) 1 calc R . P B 1
C61 C 0.1175(7) 0.9193(4) 0.3355(7) 0.133(4) Uani 0.610(10) 1 d D U P B 1
H61A H 0.063798 0.904945 0.311024 0.160 Uiso 0.610(10) 1 calc R . P B 1
H61B H 0.132105 0.913681 0.389234 0.160 Uiso 0.610(10) 1 calc R . P B 1
O4A O 0.1848(10) 0.8845(6) 0.3204(7) 0.059(4) Uani 0.390(10) 1 d D U P B 2
C64A C 0.1665(11) 0.9234(9) 0.2531(8) 0.099(6) Uani 0.390(10) 1 d D U P B 2
H64C H 0.137289 0.892332 0.211363 0.119 Uiso 0.390(10) 1 calc R . P B 2
H64D H 0.213708 0.938474 0.246065 0.119 Uiso 0.390(10) 1 calc R . P B 2
C63A C 0.1212(12) 0.9872(9) 0.2557(7) 0.133(7) Uani 0.390(10) 1 d D U P B 2
H63C H 0.069792 0.983620 0.217551 0.159 Uiso 0.390(10) 1 calc R . P B 2
H63D H 0.145786 1.031249 0.246549 0.159 Uiso 0.390(10) 1 calc R . P B 2
C62A C 0.1159(8) 0.9903(8) 0.3295(5) 0.077(4) Uani 0.390(10) 1 d D U P B 2
H62C H 0.128664 1.038630 0.351684 0.092 Uiso 0.390(10) 1 calc R . P B 2
H62D H 0.064714 0.976386 0.328100 0.092 Uiso 0.390(10) 1 calc R . P B 2
C61A C 0.1734(5) 0.9368(4) 0.3689(3) 0.045(2) Uani 0.390(10) 1 d D U P B 2
H61C H 0.221995 0.961609 0.395256 0.054 Uiso 0.390(10) 1 calc R . P B 2
H61D H 0.157204 0.912346 0.405929 0.054 Uiso 0.390(10) 1 calc R . P B 2
C31A C 0.3828(4) 0.1565(4) 0.0440(5) 0.062(2) Uani 0.435(12) 1 d D U P A 2
H31C H 0.381246 0.119213 0.079647 0.075 Uiso 0.435(12) 1 calc R . P A 2
H31D H 0.390821 0.132665 0.002013 0.075 Uiso 0.435(12) 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 N2 1.309(2) . ?
N1 C1 1.422(2) . ?
N1 Li2 2.055(4) . ?
N3 N2 1.312(2) . ?
N3 C13 1.422(3) . ?
N3 Li2 2.029(4) . ?
N5 N4 1.315(2) . ?
N5 N6 1.306(2) . ?
N4 C33 1.407(3) . ?
N4 Li3 2.047(4) . ?
N6 C45 1.422(2) . ?
N6 Li3 2.033(4) . ?
O3 C57 1.430(3) . ?
O3 C60 1.425(3) . ?
O3 Li3 1.910(4) . ?
O1 C28 1.415(3) . ?
O1 C25 1.439(3) . ?
O1 Li2 1.920(4) . ?
C13 C14 1.402(3) . ?
C13 C18 1.410(3) . ?
C1 C2 1.400(3) . ?
C1 C6 1.418(3) . ?
C33 C34 1.409(3) . ?
C33 C38 1.408(3) . ?
C14 C15 1.390(3) . ?
C14 C19 1.520(3) . ?
C45 C46 1.398(3) . ?
C45 C50 1.407(3) . ?
C46 C47 1.387(3) . ?
C46 C51 1.516(3) . ?
C50 C54 1.512(3) . ?
C50 C49 1.387(3) . ?
C34 C39 1.522(3) . ?
C34 C35 1.388(3) . ?
C2 C7 1.515(3) . ?
C2 C3 1.387(3) . ?
O2 Li2 1.902(4) . ?
O2 C29 1.428(3) . ?
O2 C32 1.432(3) . ?
C7 C8 1.519(3) . ?
C7 C9 1.503(3) . ?
C15 C16 1.380(3) . ?
C6 C10 1.517(3) . ?
C6 C5 1.389(3) . ?
C16 C17 1.380(3) . ?
C18 C17 1.384(3) . ?
C18 C22 1.516(3) . ?
C38 C42 1.516(3) . ?
C38 C37 1.389(3) . ?
C19 C20 1.522(3) . ?
C19 C21 1.524(3) . ?
C47 C48 1.374(3) . ?
C39 C40 1.527(3) . ?
C39 C41 1.534(3) . ?
C22 C24 1.518(3) . ?
C22 C23 1.528(3) . ?
C3 C4 1.375(3) . ?
C51 C53 1.514(4) . ?
C51 C52 1.515(4) . ?
C54 C55 1.517(4) . ?
C54 C56 1.527(4) . ?
C35 C36 1.368(4) . ?
C4 C5 1.381(3) . ?
C49 C48 1.383(3) . ?
C42 C43 1.512(4) . ?
C42 C44 1.528(3) . ?
C10 C12 1.529(3) . ?
C10 C11 1.531(3) . ?
C37 C36 1.371(4) . ?
C28 C27 1.501(4) . ?
C57 C58 1.502(5) . ?
C26 C25 1.470(4) . ?
C26 C27 1.478(4) . ?
C29 C30 1.440(4) . ?
C60 C59 1.471(5) . ?
C32 C31 1.429(6) . ?
C32 C31A 1.515(7) . ?
Li3 O4 1.919(8) . ?
Li3 O4A 1.927(12) . ?
C30 C31 1.640(7) . ?
C30 C31A 1.404(7) . ?
C58 C59 1.493(6) . ?
O4 C64 1.410(9) . ?
O4 C61 1.416(10) . ?
C64 C63 1.416(10) . ?
C63 C62 1.352(9) . ?
C62 C61 1.412(11) . ?
O4A C64A 1.429(15) . ?
O4A C61A 1.428(13) . ?
C64A C63A 1.475(14) . ?
C63A C62A 1.481(12) . ?
C62A C61A 1.469(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 N1 C1 114.61(16) . . ?
N2 N1 Li2 92.68(15) . . ?
C1 N1 Li2 152.20(18) . . ?
N2 N3 C13 113.67(16) . . ?
N2 N3 Li2 93.75(16) . . ?
C13 N3 Li2 152.12(17) . . ?
N1 N2 N3 110.10(16) . . ?
N6 N5 N4 110.69(16) . . ?
N5 N4 C33 113.70(17) . . ?
N5 N4 Li3 92.29(16) . . ?
C33 N4 Li3 153.87(17) . . ?
N5 N6 C45 112.54(16) . . ?
N5 N6 Li3 93.18(17) . . ?
C45 N6 Li3 153.92(18) . . ?
C57 O3 Li3 119.4(2) . . ?
C60 O3 C57 108.4(2) . . ?
C60 O3 Li3 122.6(2) . . ?
C28 O1 C25 108.20(19) . . ?
C28 O1 Li2 127.85(19) . . ?
C25 O1 Li2 121.5(2) . . ?
C14 C13 N3 122.44(19) . . ?
C14 C13 C18 120.37(19) . . ?
C18 C13 N3 117.06(18) . . ?
C2 C1 N1 117.40(18) . . ?
C2 C1 C6 120.68(19) . . ?
C6 C1 N1 121.61(18) . . ?
N4 C33 C34 123.7(2) . . ?
N4 C33 C38 116.28(19) . . ?
C38 C33 C34 119.9(2) . . ?
C13 C14 C19 122.05(19) . . ?
C15 C14 C13 118.5(2) . . ?
C15 C14 C19 119.5(2) . . ?
C46 C45 N6 118.98(18) . . ?
C46 C45 C50 120.59(19) . . ?
C50 C45 N6 120.33(19) . . ?
C45 C46 C51 120.63(19) . . ?
C47 C46 C45 118.7(2) . . ?
C47 C46 C51 120.7(2) . . ?
C45 C50 C54 120.80(19) . . ?
C49 C50 C45 118.5(2) . . ?
C49 C50 C54 120.7(2) . . ?
C33 C34 C39 122.4(2) . . ?
C35 C34 C33 118.2(2) . . ?
C35 C34 C39 119.3(2) . . ?
C1 C2 C7 120.12(19) . . ?
C3 C2 C1 118.9(2) . . ?
C3 C2 C7 120.8(2) . . ?
C29 O2 Li2 125.1(2) . . ?
C29 O2 C32 107.0(2) . . ?
C32 O2 Li2 121.0(2) . . ?
C2 C7 C8 109.3(2) . . ?
C9 C7 C2 114.42(19) . . ?
C9 C7 C8 110.6(2) . . ?
C16 C15 C14 121.6(2) . . ?
C1 C6 C10 121.35(19) . . ?
C5 C6 C1 117.8(2) . . ?
C5 C6 C10 120.8(2) . . ?
C15 C16 C17 119.4(2) . . ?
C13 C18 C22 119.68(19) . . ?
C17 C18 C13 118.8(2) . . ?
C17 C18 C22 121.5(2) . . ?
C33 C38 C42 119.9(2) . . ?
C37 C38 C33 119.0(2) . . ?
C37 C38 C42 121.1(2) . . ?
C14 C19 C20 111.66(19) . . ?
C14 C19 C21 112.3(2) . . ?
C20 C19 C21 111.0(2) . . ?
C48 C47 C46 121.4(2) . . ?
C34 C39 C40 110.6(2) . . ?
C34 C39 C41 112.9(2) . . ?
C40 C39 C41 110.0(2) . . ?
C16 C17 C18 121.3(2) . . ?
C18 C22 C24 110.12(18) . . ?
C18 C22 C23 113.0(2) . . ?
C24 C22 C23 110.5(2) . . ?
C4 C3 C2 121.1(2) . . ?
C53 C51 C46 112.6(2) . . ?
C53 C51 C52 111.6(2) . . ?
C52 C51 C46 110.5(2) . . ?
C50 C54 C55 113.0(2) . . ?
C50 C54 C56 110.7(2) . . ?
C55 C54 C56 111.1(2) . . ?
C36 C35 C34 122.0(2) . . ?
C3 C4 C5 120.0(2) . . ?
C48 C49 C50 121.2(2) . . ?
C47 C48 C49 119.6(2) . . ?
C38 C42 C44 113.9(2) . . ?
C43 C42 C38 110.4(2) . . ?
C43 C42 C44 110.4(2) . . ?
C6 C10 C12 110.8(2) . . ?
C6 C10 C11 114.0(2) . . ?
C12 C10 C11 109.9(2) . . ?
C4 C5 C6 121.5(2) . . ?
C36 C37 C38 121.2(2) . . ?
C35 C36 C37 119.7(2) . . ?
O1 C28 C27 106.8(2) . . ?
O3 C57 C58 103.3(3) . . ?
C25 C26 C27 102.9(2) . . ?
O1 C25 C26 106.9(2) . . ?
N3 Li2 N1 63.46(13) . . ?
O1 Li2 N1 115.4(2) . . ?
O1 Li2 N3 137.5(2) . . ?
O2 Li2 N1 122.0(2) . . ?
O2 Li2 N3 111.9(2) . . ?
O2 Li2 O1 103.62(19) . . ?
O2 C29 C30 106.8(3) . . ?
O3 C60 C59 108.3(3) . . ?
C26 C27 C28 103.5(3) . . ?
O2 C32 C31A 102.9(3) . . ?
C31 C32 O2 108.4(3) . . ?
N6 Li3 N4 63.82(13) . . ?
O3 Li3 N4 112.9(2) . . ?
O3 Li3 N6 121.6(2) . . ?
O3 Li3 O4 103.5(3) . . ?
O3 Li3 O4A 109.2(5) . . ?
O4 Li3 N4 130.8(4) . . ?
O4 Li3 N6 121.7(3) . . ?
O4A Li3 N4 120.2(6) . . ?
O4A Li3 N6 122.2(4) . . ?
C29 C30 C31 97.0(3) . . ?
C31A C30 C29 108.5(4) . . ?
C59 C58 C57 103.7(3) . . ?
C60 C59 C58 104.1(3) . . ?
C32 C31 C30 98.9(4) . . ?
C64 O4 Li3 126.4(7) . . ?
C64 O4 C61 110.3(7) . . ?
C61 O4 Li3 122.7(5) . . ?
O4 C64 C63 105.4(7) . . ?
C62 C63 C64 107.1(6) . . ?
C63 C62 C61 111.2(7) . . ?
C62 C61 O4 102.4(6) . . ?
C64A O4A Li3 131.8(10) . . ?
C64A O4A C61A 102.7(10) . . ?
C61A O4A Li3 124.1(8) . . ?
O4A C64A C63A 109.2(9) . . ?
C64A C63A C62A 107.9(9) . . ?
C61A C62A C63A 100.8(7) . . ?
O4A C61A C62A 112.0(8) . . ?
C30 C31A C32 106.3(4) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_6(THF)3
_database_code_depnum_ccdc_archive 'CCDC 1971995'
loop_
_audit_author_name
_audit_author_address
'Alasdair McKay'
;Monash University
Australia
;
_audit_update_record             
;
2019-12-14 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_audit_creation_date             2019-12-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
''
alasdair.mckay@monash.edu
_chemical_name_common            ?
_chemical_name_systematic        '[Na(THF)3(N3Dipp2)]'
_chemical_formula_moiety         'C36 H58 N3 Na O3'
_chemical_formula_sum            'C36 H58 N3 Na O3'
_chemical_formula_weight         603.84
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.105(3)
_cell_length_b                   14.969(5)
_cell_length_c                   24.904(7)
_cell_angle_alpha                90
_cell_angle_beta                 99.173(16)
_cell_angle_gamma                90
_cell_volume                     3719.0(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1668
_cell_measurement_temperature    150
_cell_measurement_theta_max      19.83
_cell_measurement_theta_min      2.45
_shelx_estimated_absorpt_T_max   0.998
_shelx_estimated_absorpt_T_min   0.988
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5418
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1275 before and 0.0692 after correction. The Ratio of minimum to maximum transmission is 0.7262. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.078
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1513
_diffrn_reflns_av_unetI/netI     0.3154
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            21509
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.121
_diffrn_reflns_theta_max         25.121
_diffrn_reflns_theta_min         2.483
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2453
_reflns_number_total             6601
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.892
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         6601
_refine_ls_number_restraints     300
_refine_ls_R_factor_all          0.2305
_refine_ls_R_factor_gt           0.0817
_refine_ls_restrained_S_all      0.875
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[σ²(Fo²)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1968
_refine_ls_wR_factor_ref         0.2909
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
3. Others
 Sof(H29C)=Sof(H29D)=Sof(H32C)=Sof(H32D)=Sof(C30A)=Sof(H30A)=Sof(H30B)=
 Sof(C31A)=Sof(H31C)=Sof(H31D)=1-FVAR(1)
 Sof(H29A)=Sof(H29B)=Sof(H32A)=Sof(H32B)=Sof(C31B)=Sof(H31A)=Sof(H31B)=
 Sof(C30B)=Sof(H30C)=Sof(H30D)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C19(H19), C22(H22)
4.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29C,
 H29D), C29(H29A,H29B), C32(H32A,H32B), C32(H32C,H32D), C33(H33A,H33B),
 C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C30A(H30A,H30B), C31B(H31A,
 H31B), C30B(H30C,H30D), C31A(H31C,H31D)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C15(H15), C16(H16), C17(H17)
4.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Na1 Na 0.92640(17) 0.28760(13) 0.12066(7) 0.0461(6) Uani 1 1 d . U . . .
O1 O 0.8644(4) 0.4356(3) 0.11838(16) 0.0620(11) Uani 1 1 d . U . . .
O2 O 0.7604(3) 0.2111(3) 0.06240(14) 0.0566(11) Uani 1 1 d . U . . .
O3 O 0.8157(3) 0.2400(3) 0.19129(14) 0.0649(12) Uani 1 1 d . U . . .
N1 N 1.1541(4) 0.2657(3) 0.16613(15) 0.0402(11) Uani 1 1 d . U . . .
N2 N 1.2132(4) 0.2781(3) 0.12372(14) 0.0349(10) Uani 1 1 d . U . . .
N3 N 1.1265(3) 0.2991(3) 0.07981(14) 0.0362(10) Uani 1 1 d . U . . .
C1 C 1.2465(4) 0.2312(3) 0.21091(18) 0.0366(12) Uani 1 1 d . U . . .
C2 C 1.2665(4) 0.2812(4) 0.25921(18) 0.0388(13) Uani 1 1 d . U . . .
C3 C 1.3499(4) 0.2449(4) 0.30407(18) 0.0435(14) Uani 1 1 d . U . . .
H3 H 1.364231 0.277072 0.337377 0.052 Uiso 1 1 calc R . . . .
C4 C 1.4116(5) 0.1640(4) 0.30108(19) 0.0477(15) Uani 1 1 d . U . . .
H4 H 1.470831 0.141780 0.331622 0.057 Uiso 1 1 calc R . . . .
C5 C 1.3876(5) 0.1147(4) 0.25377(19) 0.0445(14) Uani 1 1 d . U . . .
H5 H 1.428800 0.057865 0.252570 0.053 Uiso 1 1 calc R . . . .
C6 C 1.3042(4) 0.1464(4) 0.20753(18) 0.0404(13) Uani 1 1 d . U . . .
C7 C 1.2080(5) 0.3730(4) 0.26112(19) 0.0454(14) Uani 1 1 d . U . . .
H7 H 1.124740 0.374925 0.233419 0.054 Uiso 1 1 calc R . . . .
C8 C 1.1685(6) 0.3986(4) 0.3157(2) 0.0670(18) Uani 1 1 d . U . . .
H8A H 1.101965 0.355987 0.324946 0.101 Uiso 1 1 calc GR . . . .
H8B H 1.130132 0.458823 0.313300 0.101 Uiso 1 1 calc GR . . . .
H8C H 1.248015 0.397254 0.343945 0.101 Uiso 1 1 calc GR . . . .
C9 C 1.3037(5) 0.4421(4) 0.2446(2) 0.0632(17) Uani 1 1 d . U . . .
H9A H 1.386213 0.442788 0.271313 0.095 Uiso 1 1 calc GR . . . .
H9B H 1.261590 0.501191 0.243130 0.095 Uiso 1 1 calc GR . . . .
H9C H 1.325254 0.426917 0.208701 0.095 Uiso 1 1 calc GR . . . .
C10 C 1.2701(5) 0.0871(4) 0.15703(19) 0.0474(14) Uani 1 1 d . U . . .
H10 H 1.264782 0.127660 0.124850 0.057 Uiso 1 1 calc R . . . .
C11 C 1.1332(6) 0.0475(5) 0.1551(3) 0.094(2) Uani 1 1 d . U . . .
H11A H 1.108729 0.014228 0.121045 0.142 Uiso 1 1 calc GR . . . .
H11B H 1.067934 0.095411 0.156893 0.142 Uiso 1 1 calc GR . . . .
H11C H 1.133324 0.006983 0.185987 0.142 Uiso 1 1 calc GR . . . .
C12 C 1.3694(6) 0.0177(5) 0.1500(3) 0.087(2) Uani 1 1 d . U . . .
H12A H 1.373210 -0.026442 0.179249 0.130 Uiso 1 1 calc GR . . . .
H12B H 1.457757 0.045296 0.151205 0.130 Uiso 1 1 calc GR . . . .
H12C H 1.343201 -0.011908 0.114789 0.130 Uiso 1 1 calc GR . . . .
C13 C 1.1950(4) 0.3154(3) 0.03496(17) 0.0331(12) Uani 1 1 d . U . . .
C14 C 1.1624(4) 0.2620(3) -0.01105(18) 0.0368(12) Uani 1 1 d . U . . .
C15 C 1.2288(4) 0.2763(3) -0.05483(18) 0.0402(13) Uani 1 1 d . U . . .
H15 H 1.207685 0.239760 -0.086216 0.048 Uiso 1 1 calc R . . . .
C16 C 1.3242(5) 0.3418(4) -0.05420(19) 0.0448(14) Uani 1 1 d . U . . .
H16 H 1.370210 0.349376 -0.084309 0.054 Uiso 1 1 calc R . . . .
C17 C 1.3524(4) 0.3966(4) -0.00905(19) 0.0402(13) Uani 1 1 d . U . . .
H17 H 1.417515 0.442479 -0.008598 0.048 Uiso 1 1 calc R . . . .
C18 C 1.2874(4) 0.3858(3) 0.03550(17) 0.0309(11) Uani 1 1 d . U . . .
C19 C 1.0616(5) 0.1867(4) -0.01346(19) 0.0465(14) Uani 1 1 d . U . . .
H19 H 1.024739 0.186991 0.021488 0.056 Uiso 1 1 calc R . . . .
C20 C 0.9436(5) 0.1999(5) -0.0600(2) 0.080(2) Uani 1 1 d . U . . .
H20A H 0.898241 0.256350 -0.054795 0.120 Uiso 1 1 calc GR . . . .
H20B H 0.880240 0.150347 -0.060185 0.120 Uiso 1 1 calc GR . . . .
H20C H 0.977289 0.201456 -0.094825 0.120 Uiso 1 1 calc GR . . . .
C21 C 1.1293(7) 0.0975(4) -0.0180(3) 0.082(2) Uani 1 1 d . U . . .
H21A H 1.165864 0.095135 -0.052136 0.124 Uiso 1 1 calc GR . . . .
H21B H 1.063753 0.049343 -0.017527 0.124 Uiso 1 1 calc GR . . . .
H21C H 1.202199 0.090090 0.012731 0.124 Uiso 1 1 calc GR . . . .
C22 C 1.3153(4) 0.4519(3) 0.08241(18) 0.0381(13) Uani 1 1 d . U . . .
H22 H 1.249730 0.439777 0.107629 0.046 Uiso 1 1 calc R . . . .
C23 C 1.2960(5) 0.5488(3) 0.0633(2) 0.0504(14) Uani 1 1 d . U . . .
H23A H 1.360700 0.563121 0.039143 0.076 Uiso 1 1 calc GR . . . .
H23B H 1.310017 0.588748 0.094855 0.076 Uiso 1 1 calc GR . . . .
H23C H 1.204726 0.556671 0.043562 0.076 Uiso 1 1 calc GR . . . .
C24 C 1.4569(4) 0.4365(4) 0.11429(19) 0.0528(15) Uani 1 1 d . U . . .
H24A H 1.463872 0.375293 0.128397 0.079 Uiso 1 1 calc GR . . . .
H24B H 1.473597 0.478786 0.144666 0.079 Uiso 1 1 calc GR . . . .
H24C H 1.523281 0.445653 0.090116 0.079 Uiso 1 1 calc GR . . . .
C25 C 0.8199(6) 0.4836(5) 0.1614(3) 0.0757(19) Uani 1 1 d . U . . .
H25A H 0.810403 0.442497 0.191719 0.091 Uiso 1 1 calc R . . . .
H25B H 0.731545 0.511154 0.148473 0.091 Uiso 1 1 calc R . . . .
C26 C 0.9192(5) 0.5534(4) 0.1803(2) 0.0655(18) Uani 1 1 d . U . . .
H26A H 0.968291 0.538658 0.216866 0.079 Uiso 1 1 calc R . . . .
H26B H 0.874682 0.611994 0.182055 0.079 Uiso 1 1 calc R . . . .
C27 C 1.0138(5) 0.5555(4) 0.1390(2) 0.0595(16) Uani 1 1 d . U . . .
H27A H 1.024626 0.617156 0.125912 0.071 Uiso 1 1 calc R . . . .
H27B H 1.102959 0.531622 0.154649 0.071 Uiso 1 1 calc R . . . .
C28 C 0.9472(5) 0.4972(4) 0.0939(2) 0.0542(15) Uani 1 1 d . U . . .
H28A H 0.891765 0.533464 0.065543 0.065 Uiso 1 1 calc R . . . .
H28B H 1.014996 0.464370 0.076931 0.065 Uiso 1 1 calc R . . . .
C29 C 0.7506(6) 0.1171(4) 0.0670(3) 0.0746(19) Uani 1 1 d . U . . .
H29C H 0.808253 0.089219 0.043003 0.089 Uiso 0.29(2) 1 calc R . P A 2
H29D H 0.787051 0.099865 0.104832 0.089 Uiso 0.29(2) 1 calc R . P A 2
H29A H 0.754333 0.099558 0.105518 0.089 Uiso 0.71(2) 1 calc R . P A 1
H29B H 0.825316 0.087493 0.052595 0.089 Uiso 0.71(2) 1 calc R . P A 1
C32 C 0.6419(6) 0.2437(5) 0.0300(3) 0.0735(19) Uani 1 1 d . U . . .
H32A H 0.653991 0.249316 -0.008542 0.088 Uiso 0.71(2) 1 calc R . P A 1
H32B H 0.616616 0.302745 0.043182 0.088 Uiso 0.71(2) 1 calc R . P A 1
H32C H 0.664328 0.287064 0.002778 0.088 Uiso 0.29(2) 1 calc R . P A 2
H32D H 0.583898 0.273717 0.052988 0.088 Uiso 0.29(2) 1 calc R . P A 2
C33 C 0.6741(5) 0.2465(5) 0.1895(2) 0.076(2) Uani 1 1 d . U . . .
H33A H 0.633225 0.186229 0.187652 0.092 Uiso 1 1 calc R . . . .
H33B H 0.633059 0.280880 0.157093 0.092 Uiso 1 1 calc R . . . .
C34 C 0.6530(6) 0.2923(5) 0.2394(2) 0.080(2) Uani 1 1 d . U . . .
H34A H 0.568285 0.273260 0.251157 0.096 Uiso 1 1 calc R . . . .
H34B H 0.652337 0.358010 0.234787 0.096 Uiso 1 1 calc R . . . .
C35 C 0.7713(7) 0.2625(7) 0.2783(3) 0.111(3) Uani 1 1 d . U . . .
H35A H 0.809075 0.312871 0.301599 0.133 Uiso 1 1 calc R . . . .
H35B H 0.745815 0.214327 0.301937 0.133 Uiso 1 1 calc R . . . .
C36 C 0.8697(7) 0.2296(7) 0.2455(3) 0.120(3) Uani 1 1 d . U . . .
H36A H 0.954190 0.263827 0.254084 0.144 Uiso 1 1 calc R . . . .
H36B H 0.889504 0.165758 0.253610 0.144 Uiso 1 1 calc R . . . .
C30A C 0.630(5) 0.084(4) 0.0547(18) 0.075(8) Uani 0.29(2) 1 d . U P A 2
H30A H 0.579129 0.086923 0.085455 0.089 Uiso 0.29(2) 1 calc R . P A 2
H30B H 0.630621 0.021796 0.040976 0.089 Uiso 0.29(2) 1 calc R . P A 2
C31B C 0.5352(12) 0.1729(9) 0.0365(9) 0.088(4) Uani 0.71(2) 1 d . U P A 1
H31A H 0.503436 0.178270 0.072000 0.106 Uiso 0.71(2) 1 calc R . P A 1
H31B H 0.457636 0.176233 0.006777 0.106 Uiso 0.71(2) 1 calc R . P A 1
C30B C 0.614(2) 0.0897(14) 0.0333(8) 0.091(5) Uani 0.71(2) 1 d . U P A 1
H30C H 0.623417 0.075103 -0.004753 0.109 Uiso 0.71(2) 1 calc R . P A 1
H30D H 0.574349 0.038233 0.049801 0.109 Uiso 0.71(2) 1 calc R . P A 1
C31A C 0.571(3) 0.163(2) 0.0020(18) 0.077(8) Uani 0.29(2) 1 d . U P A 2
H31C H 0.602844 0.148369 -0.032716 0.092 Uiso 0.29(2) 1 calc R . P A 2
H31D H 0.472697 0.168942 -0.004116 0.092 Uiso 0.29(2) 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Na1 O1 2.301(4) . ?
Na1 O2 2.336(4) . ?
Na1 O3 2.341(4) . ?
Na1 N1 2.419(4) . ?
Na1 N2 2.891(4) . ?
Na1 N3 2.410(4) . ?
O1 C25 1.421(7) . ?
O1 C28 1.444(6) . ?
O2 C29 1.417(7) . ?
O2 C32 1.419(6) . ?
O3 C33 1.428(6) . ?
O3 C36 1.382(6) . ?
N1 N2 1.307(5) . ?
N1 C1 1.431(5) . ?
N2 N3 1.326(4) . ?
N3 C13 1.426(6) . ?
C1 C2 1.404(6) . ?
C1 C6 1.405(7) . ?
C2 C3 1.398(6) . ?
C2 C7 1.499(7) . ?
C3 C4 1.369(7) . ?
C4 C5 1.378(7) . ?
C5 C6 1.397(6) . ?
C6 C10 1.533(7) . ?
C7 C8 1.525(7) . ?
C7 C9 1.517(7) . ?
C10 C11 1.499(7) . ?
C10 C12 1.474(7) . ?
C13 C14 1.393(6) . ?
C13 C18 1.407(6) . ?
C14 C15 1.385(6) . ?
C14 C19 1.513(7) . ?
C15 C16 1.374(7) . ?
C16 C17 1.384(6) . ?
C17 C18 1.386(6) . ?
C18 C22 1.523(6) . ?
C19 C20 1.538(7) . ?
C19 C21 1.514(8) . ?
C22 C23 1.529(7) . ?
C22 C24 1.539(6) . ?
C25 C26 1.472(8) . ?
C26 C27 1.513(7) . ?
C27 C28 1.495(7) . ?
C29 C30A 1.31(5) . ?
C29 C30B 1.548(17) . ?
C32 C31B 1.540(15) . ?
C32 C31A 1.52(3) . ?
C33 C34 1.466(8) . ?
C34 C35 1.482(8) . ?
C35 C36 1.469(10) . ?
C30A C31A 1.79(5) . ?
C31B C30B 1.49(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Na1 O2 106.90(14) . . ?
O1 Na1 O3 98.66(16) . . ?
O1 Na1 N1 112.16(15) . . ?
O1 Na1 N2 108.44(14) . . ?
O1 Na1 N3 99.47(15) . . ?
O2 Na1 O3 86.32(14) . . ?
O2 Na1 N1 139.44(16) . . ?
O2 Na1 N2 127.60(14) . . ?
O2 Na1 N3 109.91(14) . . ?
O3 Na1 N1 98.03(14) . . ?
O3 Na1 N2 124.22(13) . . ?
O3 Na1 N3 150.74(14) . . ?
N1 Na1 N2 26.65(11) . . ?
N3 Na1 N1 53.70(13) . . ?
N3 Na1 N2 27.07(10) . . ?
C25 O1 Na1 125.8(4) . . ?
C25 O1 C28 105.7(4) . . ?
C28 O1 Na1 116.8(3) . . ?
C29 O2 Na1 119.3(3) . . ?
C29 O2 C32 108.9(4) . . ?
C32 O2 Na1 129.9(4) . . ?
C33 O3 Na1 123.5(3) . . ?
C36 O3 Na1 127.4(4) . . ?
C36 O3 C33 106.0(4) . . ?
N2 N1 Na1 97.2(2) . . ?
N2 N1 C1 110.8(4) . . ?
C1 N1 Na1 150.1(3) . . ?
N1 N2 Na1 56.1(2) . . ?
N1 N2 N3 111.9(4) . . ?
N3 N2 Na1 55.8(2) . . ?
N2 N3 Na1 97.1(3) . . ?
N2 N3 C13 110.3(3) . . ?
C13 N3 Na1 152.6(3) . . ?
C2 C1 N1 117.5(4) . . ?
C2 C1 C6 121.9(4) . . ?
C6 C1 N1 120.3(4) . . ?
C1 C2 C7 120.8(4) . . ?
C3 C2 C1 117.6(5) . . ?
C3 C2 C7 121.4(5) . . ?
C4 C3 C2 121.5(5) . . ?
C3 C4 C5 120.0(4) . . ?
C4 C5 C6 121.6(5) . . ?
C1 C6 C10 122.1(4) . . ?
C5 C6 C1 117.3(4) . . ?
C5 C6 C10 120.5(5) . . ?
C2 C7 C8 114.7(4) . . ?
C2 C7 C9 110.1(4) . . ?
C9 C7 C8 109.9(5) . . ?
C11 C10 C6 110.0(5) . . ?
C12 C10 C6 115.9(4) . . ?
C12 C10 C11 111.1(6) . . ?
C14 C13 N3 117.7(4) . . ?
C14 C13 C18 120.5(4) . . ?
C18 C13 N3 121.7(4) . . ?
C13 C14 C19 122.0(4) . . ?
C15 C14 C13 118.5(5) . . ?
C15 C14 C19 119.4(4) . . ?
C16 C15 C14 121.9(5) . . ?
C15 C16 C17 119.0(5) . . ?
C16 C17 C18 121.3(5) . . ?
C13 C18 C22 122.4(4) . . ?
C17 C18 C13 118.5(4) . . ?
C17 C18 C22 119.0(4) . . ?
C14 C19 C20 111.7(5) . . ?
C14 C19 C21 110.5(4) . . ?
C21 C19 C20 111.2(5) . . ?
C18 C22 C23 112.2(4) . . ?
C18 C22 C24 110.0(4) . . ?
C23 C22 C24 111.4(4) . . ?
O1 C25 C26 108.5(5) . . ?
C25 C26 C27 105.7(5) . . ?
C28 C27 C26 104.0(4) . . ?
O1 C28 C27 106.1(4) . . ?
O2 C29 C30B 106.7(9) . . ?
C30A C29 O2 116(2) . . ?
O2 C32 C31B 104.1(6) . . ?
O2 C32 C31A 106.1(11) . . ?
O3 C33 C34 106.6(5) . . ?
C33 C34 C35 101.7(6) . . ?
C36 C35 C34 106.5(5) . . ?
O3 C36 C35 108.0(5) . . ?
C29 C30A C31A 96(3) . . ?
C30B C31B C32 100.3(13) . . ?
C31B C30B C29 100.9(13) . . ?
C32 C31A C30A 96(3) . . ?

_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_PLAT026_6THF3               
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low .. 37% Check
RESPONSE: Data was weak and the quality of this structure is poor. X-ray 
diffraction data for this compound has been included as confirmation of 
connectivity and for provision of unit cell parameters only.
;
# end Validation Reply Form
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_7(THF)
_database_code_depnum_ccdc_archive 'CCDC 1971998'
loop_
_audit_author_name
_audit_author_address
'Alasdair McKay'
;Monash University
Australia
;
_audit_update_record             
;
2019-12-14 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT220_7(THF)              
;
PROBLEM: NonSolvent Resd 1  C   Ueq(max) / Ueq(min) Range        7.5 Ratio
RESPONSE: There are a large number of disordered atoms in this structure.
;
_vrf_PLAT250_7(THF)              
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        4.4 Note
RESPONSE: There are a large number of disordered atoms in this structure.
;
# Added during the CSD deposition process: Saturday 14 December 2019 01:17 PM
# end Validation Reply Form

_audit_creation_date             2019-04-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
''
alasdair.mckay@monash.edu
_chemical_name_common            '[K(THF)1.5(N3Dipp2)]'
_chemical_name_systematic        ?
_chemical_formula_moiety         'C54 H80 K2 N6 O1.5, 0.5(C7 H8)'
_chemical_formula_sum            'C57.50 H84 K2 N6 O1.50'
_chemical_formula_weight         961.50
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.1068(9)
_cell_length_b                   14.9847(10)
_cell_length_c                   15.9757(11)
_cell_angle_alpha                96.923(4)
_cell_angle_beta                 110.851(3)
_cell_angle_gamma                98.577(3)
_cell_volume                     2847.7(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8313
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.21
_cell_measurement_theta_min      2.29
_shelx_estimated_absorpt_T_max   0.994
_shelx_estimated_absorpt_T_min   0.971
_exptl_absorpt_coefficient_mu    0.209
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1829 before and 0.0494 after correction. The Ratio of minimum to maximum transmission is 0.8873. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1042
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_unetI/netI     0.0617
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            42503
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.101
_diffrn_reflns_theta_min         2.149
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7559
_reflns_number_total             12220
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     797
_refine_ls_number_reflns         12220
_refine_ls_number_restraints     266
_refine_ls_R_factor_all          0.1096
_refine_ls_R_factor_gt           0.0612
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0694P)²+1.4929P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1501
_refine_ls_wR_factor_ref         0.1725
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 O1-C25 = O1-C28
 1.408 with sigma of 0.02
 C26-C25 = C28-C27
 1.472 with sigma of 0.02
 C26-C27
 1.459 with sigma of 0.02
 N4-N5A = N5A-N6A
 1.318 with sigma of 0.02
 N3A-N2A = N1-N2A
 1.318 with sigma of 0.02
 O1-C26 = O1-C27
 2.315 with sigma of 0.02
 C25-C27 = C28-C26
 2.332 with sigma of 0.02
 N1-N3A = N4-N6A
 2.183 with sigma of 0.02
 C29-C30 \\sim C30-C31 \\sim C31-C32
 with sigma of 0.02
 O2-C29 \\sim O2-C32
 with sigma of 0.02
 O2-C30 \\sim O2-C31
 with sigma of 0.04
 C30-C32 \\sim C29-C31
 with sigma of 0.04
 C58-C63 \\sim C63-C62 \\sim C62-C61 \\sim C61-C60 \\sim C60-C59 \\sim C59-C58
 with sigma of 0.02
 C58-C60 \\sim C58-C62 \\sim C59-C61 \\sim C63-C59 \\sim C62-C60 \\sim C63-C61
 with sigma of 0.04
 C57-C59 \\sim C57-C63
 with sigma of 0.04
3. Restrained planarity
 C57, C58, C63, C62, C61, C60, C59
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O2 \\sim C29 \\sim C30 \\sim C31 \\sim C32: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04
C57 \\sim C58 \\sim C63 \\sim C62 \\sim C61 \\sim C60 \\sim C59: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C24A \\sim C22A \\sim C23 \\sim C18A \\sim C17 \\sim C13A: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 O2, C29, C30, C31, C32
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C57, C58, C63, C62, C61, C60, C59
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C24A, C22A, C23, C18A, C17, C13A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: N5(0.7) N6(0.7) C45(0.7) C50(0.7) H49(0.7) H49A(0.3) C54(0.7)
 H54(0.7) C55(0.7) H55A(0.7) H55B(0.7) H55C(0.7) C56(0.7) H56A(0.7) H56B(0.7)
 H56C(0.7) N2(0.8) N3(0.8) C13(0.8) H17(0.8) H17A(0.2) C18(0.8) C22(0.8)
 H22(0.8) H23A(0.8) H23B(0.8) H23C(0.8) H23D(0.2) H23E(0.2) H23F(0.2) C24(0.8)
 H24A(0.8) H24B(0.8) H24C(0.8) N5A(0.3) N6A(0.3) C45A(0.3) C50A(0.3) C54A(0.3)
 H54A(0.3) C55A(0.3) H55D(0.3) H55E(0.3) H55F(0.3) C56A(0.3) H56D(0.3)
 H56E(0.3) H56F(0.3) N2A(0.2) N3A(0.2) C13A(0.2) C18A(0.2) C22A(0.2) H22A(0.2)
 C24A(0.2) H24D(0.2) H24E(0.2) H24F(0.2) O2(0.5) C29(0.5) H29A(0.5) H29B(0.5)
 C30(0.5) H30A(0.5) H30B(0.5) C31(0.5) H31A(0.5) H31B(0.5) C32(0.5) H32A(0.5)
 H32B(0.5) C57(0.5) H57A(0.5) H57B(0.5) H57C(0.5) C58(0.5) C63(0.5) H63(0.5)
 C62(0.5) H62(0.5) C61(0.5) H61(0.5) C60(0.5) H60(0.5) C59(0.5) H59(0.5)
7.a Ternary CH refined with riding coordinates:
 C42(H42), C39(H39), C54(H54), C51(H51), C7(H7), C10(H10), C19(H19), C22(H22),
 C54A(H54A), C22A(H22A)
7.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C28(H28A,H28B), C27(H27A,H27B), C29(H29A,
 H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B)
7.c Me refined with riding coordinates:
 C23(H23A,H23B,H23C), C23(H23D,H23E,H23F)
7.d Aromatic/amide H refined with riding coordinates:
 C37(H37), C36(H36), C35(H35), C49(H49), C49(H49A), C48(H48), C47(H47), C3(H3),
  C4(H4), C5(H5), C15(H15), C16(H16), C17(H17), C17(H17A), C63(H63), C62(H62),
 C61(H61), C60(H60), C59(H59)
7.e Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C40(H40A,H40B,H40C), C41(H41A,H41B,
 H41C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C52(H52A,H52B,H52C), C53(H53A,
 H53B,H53C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C11(H11A,
 H11B,H11C), C21(H21A,H21B,H21C), C20(H20A,H20B,H20C), C24(H24A,H24B,H24C),
 C55A(H55D,H55E,H55F), C56A(H56D,H56E,H56F), C24A(H24D,H24E,H24F), C57(H57A,
 H57B,H57C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K3 K 0.000000 1.500000 0.000000 0.0389(2) Uani 1 2 d S T P . .
N4 N 0.12236(18) 1.41258(14) 0.23139(15) 0.0402(5) Uani 1 1 d D . . . .
N5 N 0.1623(5) 1.3725(4) 0.1819(4) 0.0320(12) Uani 0.7 1 d . . . A 1
N6 N 0.1403(5) 1.3934(4) 0.1004(3) 0.0322(12) Uani 0.7 1 d . . . A 1
C33 C 0.0533(2) 1.47694(16) 0.20358(16) 0.0332(6) Uani 1 1 d . . . . .
C38 C -0.0633(2) 1.44793(18) 0.16792(18) 0.0389(6) Uani 1 1 d . . . . .
C37 C -0.1294(3) 1.5124(2) 0.1451(2) 0.0492(7) Uani 1 1 d . . . . .
H37 H -0.208356 1.493220 0.120430 0.059 Uiso 1 1 calc R . . . .
C36 C -0.0820(3) 1.6040(2) 0.1578(2) 0.0564(8) Uani 1 1 d . . . . .
H36 H -0.128087 1.647314 0.140993 0.068 Uiso 1 1 calc R . . . .
C35 C 0.0319(3) 1.63252(19) 0.1946(2) 0.0501(8) Uani 1 1 d . . . . .
H35 H 0.063804 1.695952 0.204208 0.060 Uiso 1 1 calc R . . . .
C34 C 0.1016(2) 1.57065(17) 0.21817(17) 0.0389(6) Uani 1 1 d . . . . .
C42 C -0.1172(2) 1.34821(19) 0.1549(2) 0.0475(7) Uani 1 1 d . . . . .
H42 H -0.056146 1.313977 0.178459 0.057 Uiso 1 1 calc R . . . .
C43 C -0.1820(5) 1.3070(3) 0.0548(3) 0.1133(18) Uani 1 1 d . . . . .
H43A H -0.246853 1.335246 0.031135 0.170 Uiso 1 1 calc GR . . . .
H43B H -0.207265 1.240643 0.047715 0.170 Uiso 1 1 calc GR . . . .
H43C H -0.133799 1.318641 0.020705 0.170 Uiso 1 1 calc GR . . . .
C44 C -0.1895(5) 1.3369(3) 0.2100(4) 0.125(2) Uani 1 1 d . . . . .
H44A H -0.144723 1.363100 0.274366 0.188 Uiso 1 1 calc GR . . . .
H44B H -0.219605 1.271409 0.203677 0.188 Uiso 1 1 calc GR . . . .
H44C H -0.251227 1.368788 0.187695 0.188 Uiso 1 1 calc GR . . . .
C39 C 0.2267(2) 1.60339(19) 0.26225(18) 0.0465(7) Uani 1 1 d . . . . .
H39 H 0.261161 1.549790 0.252812 0.056 Uiso 1 1 calc R . . . .
C40 C 0.2717(3) 1.6791(2) 0.2216(2) 0.0734(11) Uani 1 1 d . . . . .
H40A H 0.246479 1.658912 0.155552 0.110 Uiso 1 1 calc GR . . . .
H40B H 0.353403 1.692754 0.248834 0.110 Uiso 1 1 calc GR . . . .
H40C H 0.244127 1.734450 0.234340 0.110 Uiso 1 1 calc GR . . . .
C41 C 0.2624(3) 1.6349(3) 0.3654(2) 0.0732(11) Uani 1 1 d . . . . .
H41A H 0.226734 1.685547 0.376759 0.110 Uiso 1 1 calc GR . . . .
H41B H 0.343650 1.655720 0.393474 0.110 Uiso 1 1 calc GR . . . .
H41C H 0.239538 1.583496 0.391825 0.110 Uiso 1 1 calc GR . . . .
C45 C 0.1954(4) 1.3429(3) 0.0548(3) 0.0341(9) Uani 0.7 1 d . . . A 1
C50 C 0.2935(4) 1.3873(4) 0.0494(4) 0.0465(13) Uani 0.7 1 d . . . A 1
C49 C 0.3445(3) 1.3328(3) -0.0041(2) 0.0750(11) Uani 1 1 d . . . . .
H49 H 0.415727 1.358522 -0.003106 0.090 Uiso 0.7 1 calc R . . A 1
H49A H 0.392206 1.375047 -0.020613 0.090 Uiso 0.3 1 calc R . . A 2
C48 C 0.2915(3) 1.2476(3) -0.0539(3) 0.0702(10) Uani 1 1 d . . . . .
H48 H 0.320420 1.218433 -0.094125 0.084 Uiso 1 1 calc R . . . .
C47 C 0.1963(3) 1.2031(2) -0.0465(2) 0.0627(9) Uani 1 1 d . . . . .
H47 H 0.161241 1.142902 -0.080620 0.075 Uiso 1 1 calc R . . . .
C46 C 0.1509(3) 1.2447(2) 0.0100(2) 0.0540(8) Uani 1 1 d . . . . .
C54 C 0.3487(6) 1.4839(6) 0.1039(5) 0.0596(19) Uani 0.7 1 d . . . A 1
H54 H 0.288334 1.515646 0.108110 0.071 Uiso 0.7 1 calc R . . A 1
C55 C 0.4160(4) 1.5425(4) 0.0629(4) 0.0664(16) Uani 0.7 1 d . . . A 1
H55A H 0.437177 1.606201 0.095850 0.100 Uiso 0.7 1 calc GR . . A 1
H55B H 0.370961 1.540191 -0.001457 0.100 Uiso 0.7 1 calc GR . . A 1
H55C H 0.483460 1.519086 0.067833 0.100 Uiso 0.7 1 calc GR . . A 1
C56 C 0.4245(5) 1.4812(4) 0.2000(3) 0.0815(17) Uani 0.7 1 d . . . A 1
H56A H 0.485251 1.451043 0.198081 0.122 Uiso 0.7 1 calc GR . . A 1
H56B H 0.381649 1.446833 0.229311 0.122 Uiso 0.7 1 calc GR . . A 1
H56C H 0.455769 1.544068 0.234779 0.122 Uiso 0.7 1 calc GR . . A 1
C51 C 0.0515(3) 1.1921(2) 0.0212(2) 0.0742(11) Uani 1 1 d . . . . .
H51 H 0.022330 1.236505 0.054139 0.089 Uiso 1 1 calc R . . . .
C52 C -0.0429(3) 1.1472(3) -0.0705(3) 0.0786(11) Uani 1 1 d . . . . .
H52A H -0.065116 1.194497 -0.106599 0.118 Uiso 1 1 calc GR . . . .
H52B H -0.107062 1.115938 -0.059733 0.118 Uiso 1 1 calc GR . . . .
H52C H -0.016934 1.102377 -0.103787 0.118 Uiso 1 1 calc GR . . . .
C53 C 0.0849(4) 1.1193(3) 0.0796(3) 0.125(2) Uani 1 1 d . . . . .
H53A H 0.105919 1.071053 0.045864 0.187 Uiso 1 1 calc GR . . . .
H53B H 0.021644 1.092231 0.093958 0.187 Uiso 1 1 calc GR . . . .
H53C H 0.148292 1.147939 0.136335 0.187 Uiso 1 1 calc GR . . . .
K2 K 0.23339(5) 1.28689(4) 0.32151(4) 0.04293(17) Uani 1 1 d . . . . .
O1 O 0.41663(19) 1.2374(2) 0.31000(18) 0.0815(8) Uani 1 1 d D . . . .
C25 C 0.5139(4) 1.2282(4) 0.3800(3) 0.1181(18) Uani 1 1 d D . . . .
H25A H 0.505643 1.165655 0.394307 0.142 Uiso 1 1 calc R . . . .
H25B H 0.530763 1.273579 0.436023 0.142 Uiso 1 1 calc R . . . .
C26 C 0.6023(4) 1.2450(7) 0.3441(4) 0.193(4) Uani 1 1 d D . . . .
H26A H 0.637071 1.311243 0.358645 0.232 Uiso 1 1 calc R . . B 1
H26B H 0.660875 1.210153 0.370207 0.232 Uiso 1 1 calc R . . B 1
C28 C 0.4257(3) 1.2080(4) 0.2272(3) 0.1115(18) Uani 1 1 d D . . . .
H28A H 0.395541 1.247897 0.183217 0.134 Uiso 1 1 calc R . . C .
H28B H 0.383936 1.143994 0.200627 0.134 Uiso 1 1 calc R . . C .
C27 C 0.5476(4) 1.2142(6) 0.2483(5) 0.202(4) Uani 1 1 d D . . D 1
H27A H 0.562041 1.153364 0.229978 0.243 Uiso 1 1 calc R . . D 1
H27B H 0.574352 1.258202 0.215396 0.243 Uiso 1 1 calc R . . D 1
K1 K 0.000000 1.000000 0.500000 0.0355(2) Uani 1 2 d S T P . .
N1 N 0.12913(16) 1.12626(14) 0.34621(14) 0.0352(5) Uani 1 1 d D . . . .
N2 N 0.1661(3) 1.1840(2) 0.4219(2) 0.0277(7) Uani 0.8 1 d . . . A 1
N3 N 0.1476(3) 1.1556(2) 0.4903(2) 0.0278(8) Uani 0.8 1 d . . . A 1
C1 C 0.07044(19) 1.03501(16) 0.33546(15) 0.0284(5) Uani 1 1 d . . . . .
C2 C -0.0466(2) 1.01449(17) 0.29635(16) 0.0328(6) Uani 1 1 d . . . . .
C3 C -0.1020(2) 0.92377(18) 0.28259(18) 0.0404(6) Uani 1 1 d . . . . .
H3 H -0.181227 0.909133 0.256578 0.048 Uiso 1 1 calc R . . . .
C4 C -0.0447(2) 0.85520(18) 0.3057(2) 0.0457(7) Uani 1 1 d . . . . .
H4 H -0.083995 0.794010 0.296990 0.055 Uiso 1 1 calc R . . . .
C5 C 0.0704(2) 0.87580(18) 0.34183(19) 0.0422(6) Uani 1 1 d . . . . .
H5 H 0.109886 0.827933 0.356669 0.051 Uiso 1 1 calc R . . . .
C6 C 0.1299(2) 0.96494(16) 0.35694(16) 0.0324(6) Uani 1 1 d . . . . .
C7 C -0.1115(2) 1.08840(19) 0.27000(19) 0.0412(6) Uani 1 1 d . . . . .
H7 H -0.057531 1.145507 0.275286 0.049 Uiso 1 1 calc R . . . .
C9 C -0.1701(3) 1.1094(2) 0.3353(3) 0.0755(11) Uani 1 1 d . . . . .
H9A H -0.223594 1.054269 0.331229 0.113 Uiso 1 1 calc GR . . . .
H9B H -0.209553 1.159146 0.318592 0.113 Uiso 1 1 calc GR . . . .
H9C H -0.114527 1.128113 0.397789 0.113 Uiso 1 1 calc GR . . . .
C8 C -0.1951(3) 1.0625(3) 0.1723(3) 0.0891(13) Uani 1 1 d . . . . .
H8A H -0.155635 1.054007 0.131112 0.134 Uiso 1 1 calc GR . . . .
H8B H -0.236602 1.111592 0.157889 0.134 Uiso 1 1 calc GR . . . .
H8C H -0.247233 1.005202 0.164868 0.134 Uiso 1 1 calc GR . . . .
C10 C 0.2562(2) 0.98639(19) 0.39244(19) 0.0422(7) Uani 1 1 d . . . . .
H10 H 0.282199 1.051992 0.424589 0.051 Uiso 1 1 calc R . . . .
C12 C 0.3110(2) 0.9284(2) 0.4599(2) 0.0611(9) Uani 1 1 d . . . . .
H12A H 0.283913 0.933159 0.509757 0.092 Uiso 1 1 calc GR . . . .
H12B H 0.392132 0.950396 0.484621 0.092 Uiso 1 1 calc GR . . . .
H12C H 0.292417 0.864125 0.429025 0.092 Uiso 1 1 calc GR . . . .
C11 C 0.2930(3) 0.9780(3) 0.3115(2) 0.0680(10) Uani 1 1 d . . . . .
H11A H 0.374668 0.993932 0.333867 0.102 Uiso 1 1 calc GR . . . .
H11B H 0.261445 1.020025 0.271572 0.102 Uiso 1 1 calc GR . . . .
H11C H 0.266561 0.914777 0.277171 0.102 Uiso 1 1 calc GR . . . .
C13 C 0.1940(4) 1.2282(3) 0.5691(3) 0.0317(9) Uani 0.8 1 d . . . A 1
C14 C 0.2917(2) 1.22294(19) 0.64238(18) 0.0425(7) Uani 1 1 d . . . . .
C15 C 0.3301(2) 1.2848(2) 0.7246(2) 0.0538(8) Uani 1 1 d . . . . .
H15 H 0.391779 1.276888 0.774913 0.065 Uiso 1 1 calc R . . . .
C16 C 0.2798(3) 1.3569(2) 0.7334(3) 0.0678(11) Uani 1 1 d . . . . .
H16 H 0.306230 1.398448 0.789982 0.081 Uiso 1 1 calc R . . . .
C17 C 0.1914(3) 1.3698(2) 0.6613(3) 0.0653(10) Uani 1 1 d . U . . .
H17 H 0.160544 1.422526 0.667167 0.078 Uiso 0.8 1 calc R . . E 1
H17A H 0.144028 1.408099 0.671904 0.078 Uiso 0.2 1 calc R . . F 2
C18 C 0.1440(5) 1.3032(3) 0.5754(3) 0.0433(12) Uani 0.8 1 d . . . A 1
C19 C 0.3527(2) 1.1476(2) 0.62970(19) 0.0485(7) Uani 1 1 d . . . . .
H19 H 0.295531 1.092585 0.589314 0.058 Uiso 1 1 calc R . . . .
C21 C 0.4205(3) 1.1180(3) 0.7170(2) 0.0686(10) Uani 1 1 d . . . . .
H21A H 0.482957 1.168435 0.754828 0.103 Uiso 1 1 calc GR . . . .
H21B H 0.449446 1.064266 0.701668 0.103 Uiso 1 1 calc GR . . . .
H21C H 0.372849 1.102110 0.750568 0.103 Uiso 1 1 calc GR . . . .
C20 C 0.4288(2) 1.1782(2) 0.5798(2) 0.0587(9) Uani 1 1 d . . . . .
H20A H 0.384157 1.193829 0.521928 0.088 Uiso 1 1 calc GR . . . .
H20B H 0.464994 1.128153 0.567853 0.088 Uiso 1 1 calc GR . . . .
H20C H 0.485849 1.232199 0.617872 0.088 Uiso 1 1 calc GR . . . .
C22 C 0.0464(4) 1.3183(3) 0.4963(4) 0.0564(13) Uani 0.8 1 d . . . A 1
H22 H 0.021607 1.263798 0.445736 0.068 Uiso 0.8 1 calc R . . A 1
C23 C -0.0504(3) 1.3301(3) 0.5241(3) 0.0858(12) Uani 1 1 d . U . . .
H23A H -0.112361 1.339728 0.471796 0.129 Uiso 0.8 1 calc R . . A 1
H23B H -0.074664 1.274736 0.544833 0.129 Uiso 0.8 1 calc R . . A 1
H23C H -0.026843 1.383295 0.573746 0.129 Uiso 0.8 1 calc R . . A 1
H23D H -0.108308 1.348189 0.474675 0.129 Uiso 0.2 1 calc R . . A 2
H23E H -0.067888 1.263288 0.519430 0.129 Uiso 0.2 1 calc R . . A 2
H23F H -0.047398 1.360585 0.582991 0.129 Uiso 0.2 1 calc R . . A 2
C24 C 0.0787(6) 1.4048(4) 0.4608(5) 0.0858(18) Uani 0.8 1 d . . . A 1
H24A H 0.096219 1.459275 0.507961 0.129 Uiso 0.8 1 calc GR . . A 1
H24B H 0.016227 1.409559 0.406140 0.129 Uiso 0.8 1 calc GR . . A 1
H24C H 0.144145 1.400626 0.445529 0.129 Uiso 0.8 1 calc GR . . A 1
N5A N 0.1461(9) 1.3922(7) 0.1453(9) 0.031(4) Uani 0.3 1 d D . . A 2
N6A N 0.2105(6) 1.3328(4) 0.1537(5) 0.0350(16) Uani 0.3 1 d D . . A 2
C45A C 0.2274(9) 1.3051(7) 0.0704(7) 0.034(2) Uani 0.3 1 d . . . A 2
C50A C 0.3246(10) 1.3486(8) 0.0622(8) 0.040(3) Uani 0.3 1 d . . . A 2
C54A C 0.4040(11) 1.4305(9) 0.1343(8) 0.060(3) Uani 0.3 1 d . . . A 2
H54A H 0.380443 1.433061 0.187475 0.072 Uiso 0.3 1 calc R . . A 2
C55A C 0.3841(16) 1.5160(11) 0.0974(13) 0.066(5) Uani 0.3 1 d . . . A 2
H55D H 0.440962 1.568640 0.138668 0.099 Uiso 0.3 1 calc GR . . A 2
H55E H 0.309971 1.525645 0.092325 0.099 Uiso 0.3 1 calc GR . . A 2
H55F H 0.388461 1.509981 0.037073 0.099 Uiso 0.3 1 calc GR . . A 2
C56A C 0.5203(10) 1.4199(10) 0.1683(10) 0.098(5) Uani 0.3 1 d . . . A 2
H56D H 0.543192 1.406914 0.116832 0.146 Uiso 0.3 1 calc GR . . A 2
H56E H 0.527225 1.369041 0.201802 0.146 Uiso 0.3 1 calc GR . . A 2
H56F H 0.568141 1.476823 0.209139 0.146 Uiso 0.3 1 calc GR . . A 2
N2A N 0.1469(10) 1.1479(9) 0.4460(9) 0.026(3) Uani 0.2 1 d D . . A 2
N3A N 0.2028(9) 1.2326(6) 0.4785(7) 0.037(3) Uani 0.2 1 d D . . A 2
C13A C 0.2242(15) 1.2635(10) 0.5712(11) 0.027(3) Uani 0.2 1 d . U . A 2
C18A C 0.175(2) 1.3361(12) 0.5913(18) 0.044(4) Uani 0.2 1 d . U . A 2
C22A C 0.080(2) 1.3627(13) 0.5155(15) 0.058(4) Uani 0.2 1 d . U . A 2
H22A H 0.073938 1.322495 0.458380 0.070 Uiso 0.2 1 calc R . . A 2
C24A C 0.127(3) 1.4611(16) 0.506(2) 0.107(10) Uani 0.2 1 d . U . A 2
H24D H 0.128436 1.505880 0.556794 0.160 Uiso 0.2 1 calc GR . . A 2
H24E H 0.079756 1.474545 0.448255 0.160 Uiso 0.2 1 calc GR . . A 2
H24F H 0.203363 1.464765 0.508008 0.160 Uiso 0.2 1 calc GR . . A 2
O2 O 0.4264(7) 1.4055(6) 0.4705(5) 0.124(2) Uani 0.5 1 d D U . A -1
C29 C 0.4120(10) 1.4384(7) 0.5552(6) 0.120(3) Uani 0.5 1 d D U . A -1
H29A H 0.332304 1.429084 0.546763 0.144 Uiso 0.5 1 calc R . . A -1
H29B H 0.452526 1.408775 0.605658 0.144 Uiso 0.5 1 calc R . . A -1
C30 C 0.4597(14) 1.5302(9) 0.5693(9) 0.166(5) Uani 0.5 1 d D U . A -1
H30A H 0.498979 1.555322 0.635319 0.200 Uiso 0.5 1 calc R . . A -1
H30B H 0.401681 1.565587 0.543433 0.200 Uiso 0.5 1 calc R . . A -1
C31 C 0.5399(15) 1.5361(8) 0.5227(11) 0.159(5) Uani 0.5 1 d D U . A -1
H31A H 0.601265 1.503848 0.548515 0.191 Uiso 0.5 1 calc R . . A -1
H31B H 0.570358 1.600167 0.521069 0.191 Uiso 0.5 1 calc R . . A -1
C32 C 0.4554(14) 1.4851(9) 0.4324(9) 0.138(4) Uani 0.5 1 d D U . A -1
H32A H 0.392394 1.516059 0.407358 0.165 Uiso 0.5 1 calc R . . A -1
H32B H 0.488393 1.470826 0.386727 0.165 Uiso 0.5 1 calc R . . A -1
C57 C 0.3666(11) 0.9560(12) 0.0836(9) 0.162(7) Uani 0.5 1 d D U . G -1
H57A H 0.397652 0.988524 0.147172 0.243 Uiso 0.5 1 calc GR . . G -1
H57B H 0.357281 0.889637 0.082032 0.243 Uiso 0.5 1 calc GR . . G -1
H57C H 0.293912 0.970833 0.051794 0.243 Uiso 0.5 1 calc GR . . G -1
C58 C 0.4517(11) 0.9879(10) 0.0333(10) 0.119(5) Uani 0.5 1 d D U . G -1
C63 C 0.4645(17) 1.0737(13) 0.0140(16) 0.127(6) Uani 0.5 1 d D U . G -1
H63 H 0.423117 1.115116 0.029899 0.152 Uiso 0.5 1 calc R . . G -1
C62 C 0.5369(16) 1.1030(16) -0.0286(16) 0.141(7) Uani 0.5 1 d D U . G -1
H62 H 0.548209 1.163469 -0.040550 0.169 Uiso 0.5 1 calc R . . G -1
C61 C 0.5905(17) 1.0371(17) -0.0520(16) 0.145(8) Uani 0.5 1 d D U . G -1
H61 H 0.637802 1.050970 -0.084063 0.174 Uiso 0.5 1 calc R . . G -1
C60 C 0.5759(16) 0.9507(15) -0.0290(15) 0.128(6) Uani 0.5 1 d D U . G -1
H60 H 0.615655 0.907807 -0.044755 0.153 Uiso 0.5 1 calc R . . G -1
C59 C 0.5059(15) 0.9235(14) 0.0160(15) 0.118(6) Uani 0.5 1 d D U . G -1
H59 H 0.497621 0.864940 0.032712 0.141 Uiso 0.5 1 calc R . . G -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
K3 N6 2.812(5) . ?
K3 N6 2.812(5) 2_585 ?
K3 C33 3.148(2) 2_585 ?
K3 C38 3.223(2) 2_585 ?
K3 C37 3.328(3) 2_585 ?
K3 C36 3.378(3) 2_585 ?
K3 C35 3.335(3) 2_585 ?
K3 C34 3.229(2) 2_585 ?
K3 N5A 3.213(12) 2_585 ?
K3 N5A 3.213(12) . ?
N4 N5 1.238(6) . ?
N4 C33 1.422(3) . ?
N4 K2 2.778(2) . ?
N4 N5A 1.520(12) . ?
N5 N6 1.317(6) . ?
N5 K2 2.656(4) . ?
N6 C45 1.424(6) . ?
C33 C38 1.404(4) . ?
C33 C34 1.406(3) . ?
C38 C37 1.389(4) . ?
C38 C42 1.510(4) . ?
C37 C36 1.378(4) . ?
C36 C35 1.371(4) . ?
C35 C34 1.388(4) . ?
C34 C39 1.510(4) . ?
C42 C43 1.517(5) . ?
C42 C44 1.511(4) . ?
C39 C40 1.518(4) . ?
C39 C41 1.535(4) . ?
C45 C50 1.393(7) . ?
C45 C46 1.487(5) . ?
C50 C49 1.498(6) . ?
C50 C54 1.520(9) . ?
C49 C48 1.358(5) . ?
C49 C50A 1.183(12) . ?
C48 C47 1.375(5) . ?
C47 C46 1.383(4) . ?
C46 C51 1.498(4) . ?
C46 C45A 1.259(10) . ?
C54 C55 1.516(7) . ?
C54 C56 1.511(10) . ?
C51 C52 1.535(5) . ?
C51 C53 1.533(6) . ?
K2 O1 2.677(2) . ?
K2 N1 2.729(2) . ?
K2 N2 2.632(3) . ?
K2 N6A 2.771(7) . ?
K2 N2A 3.387(15) . ?
K2 N3A 2.867(11) . ?
K2 O2 2.929(7) . ?
O1 C25 1.404(5) . ?
O1 C28 1.395(4) . ?
C25 C26 1.468(7) . ?
C26 C27 1.421(7) . ?
C28 C27 1.496(6) . ?
K1 N3 2.856(3) 2_576 ?
K1 N3 2.857(3) . ?
K1 C1 3.155(2) 2_576 ?
K1 C2 3.131(2) 2_576 ?
K1 C3 3.231(3) 2_576 ?
K1 C4 3.374(3) 2_576 ?
K1 C5 3.426(3) 2_576 ?
K1 C6 3.338(2) 2_576 ?
K1 N2A 3.120(15) 2_576 ?
K1 N2A 3.120(15) . ?
N1 N2 1.286(4) . ?
N1 C1 1.424(3) . ?
N1 N2A 1.512(13) . ?
N2 N3 1.305(4) . ?
N3 C13 1.437(5) . ?
C1 C2 1.403(3) . ?
C1 C6 1.403(3) . ?
C2 C3 1.394(3) . ?
C2 C7 1.506(4) . ?
C3 C4 1.371(4) . ?
C4 C5 1.380(4) . ?
C5 C6 1.388(3) . ?
C6 C10 1.515(3) . ?
C7 C9 1.528(4) . ?
C7 C8 1.515(4) . ?
C10 C12 1.514(4) . ?
C10 C11 1.531(4) . ?
C13 C14 1.415(6) . ?
C13 C18 1.393(7) . ?
C14 C15 1.391(4) . ?
C14 C19 1.511(4) . ?
C14 C13A 1.434(19) . ?
C15 C16 1.365(5) . ?
C16 C17 1.369(5) . ?
C17 C18 1.464(6) . ?
C17 C18A 1.10(2) . ?
C18 C22 1.514(8) . ?
C19 C21 1.522(4) . ?
C19 C20 1.536(4) . ?
C22 C23 1.512(6) . ?
C22 C24 1.538(7) . ?
C23 C22A 1.77(2) . ?
N5A N6A 1.303(12) . ?
N6A C45A 1.448(11) . ?
C45A C50A 1.399(15) . ?
C50A C54A 1.530(16) . ?
C54A C55A 1.49(2) . ?
C54A C56A 1.465(19) . ?
N2A N3A 1.307(13) . ?
N3A C13A 1.410(18) . ?
C13A C18A 1.41(3) . ?
C18A C22A 1.53(3) . ?
C22A C24A 1.55(3) . ?
O2 C29 1.470(10) . ?
O2 C32 1.464(13) . ?
C29 C30 1.379(12) . ?
C30 C31 1.487(15) . ?
C31 C32 1.495(12) . ?
C57 C58 1.64(2) . ?
C58 C63 1.358(12) . ?
C58 C59 1.339(12) . ?
C63 C62 1.402(12) . ?
C62 C61 1.383(13) . ?
C61 C60 1.393(13) . ?
C60 C59 1.396(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N6 K3 N6 180.00(16) . 2_585 ?
N6 K3 C33 51.72(9) 2_585 2_585 ?
N6 K3 C33 128.28(9) . 2_585 ?
N6 K3 C38 67.78(9) 2_585 2_585 ?
N6 K3 C38 112.22(9) . 2_585 ?
N6 K3 C37 88.21(9) . 2_585 ?
N6 K3 C37 91.79(9) 2_585 2_585 ?
N6 K3 C36 78.11(9) . 2_585 ?
N6 K3 C36 101.89(9) 2_585 2_585 ?
N6 K3 C35 89.51(10) 2_585 2_585 ?
N6 K3 C35 90.49(10) . 2_585 ?
N6 K3 C34 114.75(10) . 2_585 ?
N6 K3 C34 65.25(10) 2_585 2_585 ?
N6 K3 N5A 169.14(19) . 2_585 ?
N6 K3 N5A 10.86(19) 2_585 2_585 ?
C33 K3 C38 25.43(7) 2_585 2_585 ?
C33 K3 C37 43.55(7) 2_585 2_585 ?
C33 K3 C36 50.25(7) 2_585 2_585 ?
C33 K3 C35 43.42(7) 2_585 2_585 ?
C33 K3 C34 25.43(6) 2_585 2_585 ?
C33 K3 N5A 40.9(2) 2_585 2_585 ?
C33 K3 N5A 139.1(2) 2_585 . ?
C38 K3 C37 24.42(7) 2_585 2_585 ?
C38 K3 C36 42.67(7) 2_585 2_585 ?
C38 K3 C35 50.02(7) 2_585 2_585 ?
C38 K3 C34 44.30(7) 2_585 2_585 ?
C37 K3 C36 23.70(7) 2_585 2_585 ?
C37 K3 C35 41.86(8) 2_585 2_585 ?
C35 K3 C36 23.56(7) 2_585 2_585 ?
C34 K3 C37 50.19(7) 2_585 2_585 ?
C34 K3 C36 42.64(8) 2_585 2_585 ?
C34 K3 C35 24.35(7) 2_585 2_585 ?
N5A K3 N5A 180.0 2_585 . ?
N5 N4 C33 123.4(3) . . ?
N5 N4 K2 71.4(2) . . ?
C33 N4 K2 164.64(16) . . ?
C33 N4 N5A 98.0(4) . . ?
N5A N4 K2 96.9(4) . . ?
N4 N5 N6 116.9(5) . . ?
N4 N5 K2 82.4(2) . . ?
N6 N5 K2 160.5(5) . . ?
N5 N6 K3 133.9(4) . . ?
N5 N6 C45 108.9(5) . . ?
C45 N6 K3 117.0(3) . . ?
C38 C33 N4 119.9(2) . . ?
C38 C33 C34 119.9(2) . . ?
C34 C33 N4 120.0(2) . . ?
C33 C38 C42 121.0(2) . . ?
C37 C38 C33 119.1(2) . . ?
C37 C38 C42 119.9(3) . . ?
C36 C37 C38 120.8(3) . . ?
C35 C36 C37 119.9(3) . . ?
C36 C35 C34 121.4(3) . . ?
C33 C34 C39 120.4(2) . . ?
C35 C34 C33 118.7(3) . . ?
C35 C34 C39 120.9(2) . . ?
C38 C42 C43 111.2(3) . . ?
C38 C42 C44 111.0(3) . . ?
C44 C42 C43 111.7(4) . . ?
C34 C39 C40 113.6(3) . . ?
C34 C39 C41 110.0(2) . . ?
C40 C39 C41 110.2(3) . . ?
N6 C45 C46 122.7(4) . . ?
C50 C45 N6 119.2(4) . . ?
C50 C45 C46 118.1(4) . . ?
C45 C50 C49 117.1(5) . . ?
C45 C50 C54 119.4(5) . . ?
C49 C50 C54 123.3(5) . . ?
C48 C49 C50 121.8(4) . . ?
C50A C49 C48 112.6(7) . . ?
C49 C48 C47 120.4(3) . . ?
C48 C47 C46 121.0(3) . . ?
C45 C46 C51 119.7(3) . . ?
C47 C46 C45 120.5(3) . . ?
C47 C46 C51 119.7(3) . . ?
C45A C46 C47 108.0(5) . . ?
C45A C46 C51 125.5(5) . . ?
C55 C54 C50 114.9(5) . . ?
C56 C54 C50 110.9(7) . . ?
C56 C54 C55 107.9(5) . . ?
C46 C51 C52 112.5(3) . . ?
C46 C51 C53 110.8(4) . . ?
C53 C51 C52 110.1(3) . . ?
N4 K2 N2A 126.8(2) . . ?
N4 K2 N3A 122.2(2) . . ?
N4 K2 O2 102.69(19) . . ?
N5 K2 N4 26.21(13) . . ?
N5 K2 O1 103.57(14) . . ?
N5 K2 N1 127.67(15) . . ?
N5 K2 O2 110.4(2) . . ?
O1 K2 N4 126.41(8) . . ?
O1 K2 N1 100.28(8) . . ?
O1 K2 N6A 82.02(15) . . ?
O1 K2 N2A 106.4(2) . . ?
O1 K2 N3A 109.3(2) . . ?
O1 K2 O2 72.59(17) . . ?
N1 K2 N4 124.14(7) . . ?
N1 K2 N6A 125.02(15) . . ?
N1 K2 N2A 25.88(19) . . ?
N1 K2 N3A 48.07(18) . . ?
N1 K2 O2 121.00(17) . . ?
N2 K2 N4 125.73(8) . . ?
N2 K2 N5 143.37(15) . . ?
N2 K2 O1 107.65(9) . . ?
N2 K2 N1 27.67(8) . . ?
N2 K2 O2 96.97(17) . . ?
N6A K2 N4 49.40(14) . . ?
N6A K2 N2A 149.7(2) . . ?
N6A K2 N3A 166.9(3) . . ?
N3A K2 N2A 22.2(2) . . ?
C25 O1 K2 129.2(2) . . ?
C28 O1 K2 123.1(2) . . ?
C28 O1 C25 107.6(3) . . ?
O1 C25 C26 105.0(4) . . ?
C27 C26 C25 104.9(5) . . ?
O1 C28 C27 106.0(4) . . ?
C26 C27 C28 106.2(4) . . ?
N3 K1 N3 180.0 2_576 . ?
N3 K1 C1 128.05(7) . 2_576 ?
N3 K1 C1 51.95(7) 2_576 2_576 ?
N3 K1 C2 69.69(8) 2_576 2_576 ?
N3 K1 C2 110.31(8) . 2_576 ?
N3 K1 C3 94.00(8) 2_576 2_576 ?
N3 K1 C3 86.00(8) . 2_576 ?
N3 K1 C4 101.65(7) 2_576 2_576 ?
N3 K1 C4 78.35(7) . 2_576 ?
N3 K1 C5 86.96(7) 2_576 2_576 ?
N3 K1 C5 93.04(7) . 2_576 ?
N3 K1 C6 63.32(7) 2_576 2_576 ?
N3 K1 C6 116.68(7) . 2_576 ?
N3 K1 N2A 167.5(2) . 2_576 ?
N3 K1 N2A 12.5(2) 2_576 2_576 ?
C1 K1 C3 44.20(6) 2_576 2_576 ?
C1 K1 C4 50.27(6) 2_576 2_576 ?
C1 K1 C5 42.53(6) 2_576 2_576 ?
C1 K1 C6 24.74(6) 2_576 2_576 ?
C2 K1 C1 25.79(6) 2_576 2_576 ?
C2 K1 C3 25.26(6) 2_576 2_576 ?
C2 K1 C4 43.34(7) 2_576 2_576 ?
C2 K1 C5 49.89(7) 2_576 2_576 ?
C2 K1 C6 44.07(6) 2_576 2_576 ?
C3 K1 C4 23.83(7) 2_576 2_576 ?
C3 K1 C5 41.69(7) 2_576 2_576 ?
C3 K1 C6 50.01(6) 2_576 2_576 ?
C4 K1 C5 23.40(6) 2_576 2_576 ?
C6 K1 C4 42.16(6) 2_576 2_576 ?
C6 K1 C5 23.64(6) 2_576 2_576 ?
N2A K1 N2A 180.0 . 2_576 ?
N2 N1 K2 71.94(17) . . ?
N2 N1 C1 122.7(2) . . ?
C1 N1 K2 165.39(15) . . ?
C1 N1 N2A 92.4(5) . . ?
N2A N1 K2 102.1(5) . . ?
N1 N2 K2 80.39(17) . . ?
N1 N2 N3 117.0(3) . . ?
N3 N2 K2 162.6(2) . . ?
N2 N3 K1 132.2(2) . . ?
N2 N3 C13 109.8(3) . . ?
C13 N3 K1 116.4(2) . . ?
C2 C1 N1 119.6(2) . . ?
C6 C1 N1 119.8(2) . . ?
C6 C1 C2 120.4(2) . . ?
C1 C2 C7 121.1(2) . . ?
C3 C2 C1 118.5(2) . . ?
C3 C2 C7 120.4(2) . . ?
C4 C3 C2 121.5(2) . . ?
C3 C4 C5 119.5(2) . . ?
C4 C5 C6 121.4(3) . . ?
C1 C6 C10 120.2(2) . . ?
C5 C6 C1 118.6(2) . . ?
C5 C6 C10 121.2(2) . . ?
C2 C7 C9 110.5(2) . . ?
C2 C7 C8 111.7(2) . . ?
C8 C7 C9 110.5(3) . . ?
C6 C10 C11 109.0(2) . . ?
C12 C10 C6 114.1(2) . . ?
C12 C10 C11 111.2(2) . . ?
C14 C13 N3 119.4(4) . . ?
C18 C13 N3 121.4(4) . . ?
C18 C13 C14 119.2(4) . . ?
C13 C14 C19 118.4(3) . . ?
C15 C14 C13 120.9(3) . . ?
C15 C14 C19 120.7(3) . . ?
C15 C14 C13A 109.0(6) . . ?
C13A C14 C19 125.7(6) . . ?
C16 C15 C14 120.4(3) . . ?
C15 C16 C17 120.6(3) . . ?
C16 C17 C18 120.8(4) . . ?
C18A C17 C16 120.7(14) . . ?
C13 C18 C17 117.6(5) . . ?
C13 C18 C22 122.1(4) . . ?
C17 C18 C22 120.2(4) . . ?
C14 C19 C21 115.2(3) . . ?
C14 C19 C20 109.0(3) . . ?
C21 C19 C20 109.6(2) . . ?
C18 C22 C23 111.1(4) . . ?
C18 C22 C24 111.4(5) . . ?
C23 C22 C24 107.7(4) . . ?
N4 N5A K3 107.2(5) . . ?
N6A N5A K3 142.3(8) . . ?
N6A N5A N4 110.2(9) . . ?
N5A N6A K2 103.3(7) . . ?
N5A N6A C45A 112.2(9) . . ?
C45A N6A K2 143.3(6) . . ?
C46 C45A N6A 116.5(7) . . ?
C46 C45A C50A 125.3(8) . . ?
C50A C45A N6A 118.2(9) . . ?
C49 C50A C45A 123.3(10) . . ?
C49 C50A C54A 115.4(10) . . ?
C45A C50A C54A 120.8(10) . . ?
C55A C54A C50A 108.0(12) . . ?
C56A C54A C50A 113.1(12) . . ?
C56A C54A C55A 115.5(11) . . ?
K1 N2A K2 161.1(4) . . ?
N1 N2A K2 52.0(5) . . ?
N1 N2A K1 112.3(6) . . ?
N3A N2A K2 55.9(8) . . ?
N3A N2A K1 138.0(9) . . ?
N3A N2A N1 107.9(12) . . ?
N2A N3A K2 101.9(9) . . ?
N2A N3A C13A 114.5(11) . . ?
C13A N3A K2 143.6(7) . . ?
N3A C13A C14 122.3(13) . . ?
C18A C13A C14 120.9(15) . . ?
C18A C13A N3A 116.8(18) . . ?
C17 C18A C13A 123(2) . . ?
C17 C18A C22A 115.9(19) . . ?
C13A C18A C22A 120(2) . . ?
C18A C22A C23 111.9(13) . . ?
C18A C22A C24A 106(2) . . ?
C24A C22A C23 123.7(15) . . ?
C29 O2 K2 117.6(6) . . ?
C32 O2 K2 104.8(7) . . ?
C32 O2 C29 108.6(9) . . ?
C30 C29 O2 99.4(8) . . ?
C29 C30 C31 106.8(10) . . ?
C30 C31 C32 94.4(10) . . ?
O2 C32 C31 92.8(10) . . ?
C63 C58 C57 120.7(12) . . ?
C59 C58 C57 114.2(12) . . ?
C59 C58 C63 125.2(12) . . ?
C58 C63 C62 121.9(13) . . ?
C61 C62 C63 115.0(13) . . ?
C62 C61 C60 120.6(13) . . ?
C61 C60 C59 123.6(13) . . ?
C58 C59 C60 113.6(12) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_8
_database_code_depnum_ccdc_archive 'CCDC 1972001'
loop_
_audit_author_name
_audit_author_address
'Alasdair McKay'
;Monash University
Australia
;
_audit_update_record             
;
2019-12-14 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_audit_creation_date             2019-12-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
''
alasdair.mckay@monash.edu
_chemical_name_common            ?
_chemical_name_systematic        '[Tl(N3Dipp2)]2'
_chemical_formula_moiety         'C48 H68 N6 Tl2'
_chemical_formula_sum            'C48 H68 N6 Tl2'
_chemical_formula_weight         1137.82
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   13.5767(5)
_cell_length_b                   20.2026(7)
_cell_length_c                   35.6666(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9782.8(6)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9883
_cell_measurement_temperature    180
_cell_measurement_theta_max      28.655
_cell_measurement_theta_min      2.490
_shelx_estimated_absorpt_T_max   0.437
_shelx_estimated_absorpt_T_min   0.437
_exptl_absorpt_coefficient_mu    6.617
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0667 before and 0.0440 after correction. The Ratio of minimum to maximum transmission is 0.8008. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4480
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            45357
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         1.158
_diffrn_ambient_temperature      180.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.828
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.983
_reflns_number_gt                15910
_reflns_number_total             21417
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.001
_refine_diff_density_min         -1.668
_refine_diff_density_rms         0.114
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.454(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1042
_refine_ls_number_reflns         21417
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0379
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0148P)²+2.7129P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0554
_refine_ls_wR_factor_ref         0.0615
_refine_special_details          'Refined as a 2-component inversion twin.,Twin'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.546(7)
 0.454(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C19(H19), C82(H82), C70(H70), C91(H91), C7(H7), C58(H58), C94(H94), C43(H43),
 C46(H46), C22(H22), C79(H79), C67(H67), C10(H10), C34(H34), C31(H31), C55(H55)
3.b Aromatic/amide H refined with riding coordinates:
 C87(H87), C63(H63), C17(H17), C88(H88), C16(H16), C65(H65), C15(H15), C3(H3),
 C64(H64), C40(H40), C89(H89), C39(H39), C41(H41), C29(H29), C5(H5), C75(H75),
 C77(H77), C76(H76), C4(H4), C53(H53), C51(H51), C28(H28), C52(H52), C27(H27)
3.c Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C), C20(H20A,H20B,H20C), C71(H71A,H71B,H71C), C72(H72A,H72B,
 H72C), C32(H32A,H32B,H32C), C21(H21A,H21B,H21C), C84(H84A,H84B,H84C), C96(H96A,
 H96B,H96C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C93(H93A,H93B,H93C),
 C47(H47A,H47B,H47C), C9(H9A,H9B,H9C), C83(H83A,H83B,H83C), C95(H95A,H95B,H95C),
  C35(H35A,H35B,H35C), C45(H45A,H45B,H45C), C81(H81A,H81B,H81C), C69(H69A,H69B,
 H69C), C36(H36A,H36B,H36C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C80(H80A,
 H80B,H80C), C33(H33A,H33B,H33C), C68(H68A,H68B,H68C), C24(H24A,H24B,H24C),
 C92(H92A,H92B,H92C), C44(H44A,H44B,H44C), C23(H23A,H23B,H23C), C57(H57A,H57B,
 H57C), C8(H8A,H8B,H8C), C56(H56A,H56B,H56C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tl3 Tl 0.57799(3) 0.72475(2) 0.83060(2) 0.03313(10) Uani 1 1 d . . . . .
Tl1 Tl 0.93762(3) 0.76175(2) 0.58227(2) 0.03212(9) Uani 1 1 d . . . . .
Tl4 Tl 0.47592(3) 0.76194(2) 0.91718(2) 0.03291(9) Uani 1 1 d . . . . .
Tl2 Tl 1.03120(3) 0.72679(2) 0.67034(2) 0.03178(9) Uani 1 1 d . . . . .
N6 N 0.9486(6) 0.6459(3) 0.6166(2) 0.0242(18) Uani 1 1 d . . . . .
N10 N 0.3921(6) 0.7113(3) 0.85236(17) 0.0268(18) Uani 1 1 d . . . . .
N5 N 0.8627(6) 0.6511(3) 0.63291(19) 0.0276(18) Uani 1 1 d . . . . .
N12 N 0.4852(6) 0.6467(3) 0.88265(19) 0.0274(19) Uani 1 1 d . . . . .
N1 N 1.1290(5) 0.7647(4) 0.60712(17) 0.0283(17) Uani 1 1 d . . . . .
C85 C 0.4985(7) 0.5831(4) 0.9018(2) 0.025(2) Uani 1 1 d . . . . .
N9 N 0.5768(6) 0.8396(4) 0.87068(19) 0.030(2) Uani 1 1 d . . . . .
N11 N 0.4013(6) 0.6522(4) 0.86602(19) 0.0237(18) Uani 1 1 d . . . . .
N3 N 1.0361(6) 0.8417(3) 0.62992(18) 0.0235(18) Uani 1 1 d . . . . .
N7 N 0.6707(5) 0.7626(4) 0.89341(17) 0.0249(17) Uani 1 1 d . . . . .
N2 N 1.1218(6) 0.8286(4) 0.61498(18) 0.025(2) Uani 1 1 d . . . . .
N8 N 0.6623(6) 0.8261(4) 0.88700(19) 0.0271(18) Uani 1 1 d . . . . .
C62 C 0.5319(7) 0.9342(4) 0.8322(3) 0.031(2) Uani 1 1 d . . . . .
C66 C 0.5506(7) 0.9500(4) 0.8995(3) 0.030(2) Uani 1 1 d . . . . .
C87 C 0.5907(8) 0.4840(5) 0.9111(3) 0.048(3) Uani 1 1 d . . . . .
H87 H 0.645924 0.456922 0.905316 0.058 Uiso 1 1 calc R . . . .
C19 C 1.0270(7) 0.9274(5) 0.5622(3) 0.034(2) Uani 1 1 d . . . . .
H19 H 1.040751 0.878854 0.563909 0.040 Uiso 1 1 calc R . . . .
C13 C 1.0181(7) 0.9116(4) 0.6337(2) 0.025(2) Uani 1 1 d . . . . .
C1 C 1.2242(7) 0.7440(4) 0.5957(2) 0.029(2) Uani 1 1 d . . . . .
C61 C 0.5561(7) 0.9092(5) 0.8679(3) 0.030(2) Uani 1 1 d . . . . .
C42 C 1.0479(8) 0.5479(5) 0.6075(3) 0.033(3) Uani 1 1 d . . . . .
N4 N 0.8486(5) 0.7119(3) 0.64587(19) 0.0275(18) Uani 1 1 d . . . . .
C82 C 0.2769(8) 0.8270(5) 0.8620(3) 0.047(3) Uani 1 1 d . . . . .
H82 H 0.349799 0.825749 0.866048 0.056 Uiso 1 1 calc R . . . .
C78 C 0.2540(7) 0.7776(5) 0.8319(3) 0.040(2) Uani 1 1 d . . . . .
C73 C 0.3088(7) 0.7190(4) 0.8276(2) 0.033(2) Uani 1 1 d . . . . .
C38 C 0.8967(8) 0.5619(5) 0.5707(3) 0.040(3) Uani 1 1 d . . . . .
C63 C 0.5056(7) 1.0002(5) 0.8293(3) 0.042(3) Uani 1 1 d . . . . .
H63 H 0.490316 1.017937 0.805352 0.051 Uiso 1 1 calc R . . . .
C2 C 1.2358(9) 0.7067(5) 0.5628(3) 0.044(3) Uani 1 1 d . . . . .
C17 C 0.9771(7) 1.0034(4) 0.6737(3) 0.038(2) Uani 1 1 d . . . . .
H17 H 0.964004 1.021033 0.697866 0.045 Uiso 1 1 calc R . . . .
C48 C 1.0881(9) 0.5505(5) 0.6761(3) 0.060(3) Uani 1 1 d . . . . .
H48A H 1.018248 0.561313 0.679396 0.091 Uiso 1 1 calc GR . . . .
H48B H 1.127146 0.573960 0.695005 0.091 Uiso 1 1 calc GR . . . .
H48C H 1.097481 0.502667 0.679035 0.091 Uiso 1 1 calc GR . . . .
C20 C 0.9362(8) 0.9357(5) 0.5380(3) 0.044(3) Uani 1 1 d . . . . .
H20A H 0.880189 0.913380 0.549813 0.066 Uiso 1 1 calc GR . . . .
H20B H 0.948232 0.916275 0.513211 0.066 Uiso 1 1 calc GR . . . .
H20C H 0.921347 0.982957 0.535163 0.066 Uiso 1 1 calc GR . . . .
C86 C 0.5800(8) 0.5443(5) 0.8936(3) 0.034(3) Uani 1 1 d . . . . .
C70 C 0.5694(7) 0.9249(5) 0.9394(2) 0.033(3) Uani 1 1 d . . . . .
H70 H 0.583509 0.876354 0.938010 0.040 Uiso 1 1 calc R . . . .
C14 C 1.0088(7) 0.9521(5) 0.6019(3) 0.030(2) Uani 1 1 d . . . . .
C88 C 0.5222(9) 0.4625(5) 0.9367(3) 0.051(3) Uani 1 1 d . . . . .
H88 H 0.528635 0.419853 0.947710 0.061 Uiso 1 1 calc R . . . .
C16 C 0.9692(8) 1.0439(5) 0.6427(3) 0.044(3) Uani 1 1 d . . . . .
H16 H 0.952500 1.089276 0.645547 0.053 Uiso 1 1 calc R . . . .
C65 C 0.5237(8) 1.0163(5) 0.8946(3) 0.039(3) Uani 1 1 d . . . . .
H65 H 0.521258 1.044714 0.915802 0.047 Uiso 1 1 calc R . . . .
C90 C 0.4306(7) 0.5644(5) 0.9298(3) 0.036(2) Uani 1 1 d . . . . .
C91 C 0.6532(8) 0.5675(5) 0.8641(3) 0.044(3) Uani 1 1 d . . . . .
H91 H 0.651794 0.616967 0.864284 0.053 Uiso 1 1 calc R . . . .
C18 C 1.0034(7) 0.9382(4) 0.6703(3) 0.032(2) Uani 1 1 d . . . . .
C71 C 0.4802(8) 0.9344(5) 0.9641(3) 0.047(3) Uani 1 1 d . . . . .
H71A H 0.468273 0.981872 0.967678 0.071 Uiso 1 1 calc GR . . . .
H71B H 0.491744 0.913489 0.988490 0.071 Uiso 1 1 calc GR . . . .
H71C H 0.422572 0.914188 0.952161 0.071 Uiso 1 1 calc GR . . . .
C7 C 1.1471(8) 0.6896(5) 0.5395(3) 0.040(3) Uani 1 1 d . . . . .
H7 H 1.089672 0.685801 0.556903 0.048 Uiso 1 1 calc R . . . .
C58 C 0.6809(8) 0.6866(5) 0.9619(3) 0.044(3) Uani 1 1 d . . . . .
H58 H 0.625856 0.683590 0.943291 0.053 Uiso 1 1 calc R . . . .
C94 C 0.3475(8) 0.6072(5) 0.9437(2) 0.037(3) Uani 1 1 d . . . . .
H94 H 0.352186 0.650190 0.929932 0.044 Uiso 1 1 calc R . . . .
C43 C 0.8124(8) 0.6032(5) 0.5561(3) 0.046(3) Uani 1 1 d . . . . .
H43 H 0.815165 0.646926 0.569243 0.055 Uiso 1 1 calc R . . . .
C15 C 0.9859(7) 1.0178(5) 0.6075(3) 0.032(2) Uani 1 1 d . . . . .
H15 H 0.981482 1.046252 0.586376 0.039 Uiso 1 1 calc R . . . .
C49 C 0.7653(7) 0.7448(4) 0.9063(3) 0.034(2) Uani 1 1 d . . . . .
C6 C 1.3060(7) 0.7574(5) 0.6199(3) 0.040(2) Uani 1 1 d . . . . .
C72 C 0.6596(8) 0.9590(5) 0.9563(3) 0.049(3) Uani 1 1 d . . . . .
H72A H 0.717905 0.948405 0.941225 0.073 Uiso 1 1 calc GR . . . .
H72B H 0.669418 0.943579 0.982031 0.073 Uiso 1 1 calc GR . . . .
H72C H 0.649292 1.007056 0.956305 0.073 Uiso 1 1 calc GR . . . .
C46 C 1.1216(8) 0.5717(5) 0.6367(3) 0.044(3) Uani 1 1 d . . . . .
H46 H 1.119910 0.621169 0.636219 0.053 Uiso 1 1 calc R . . . .
C32 C 0.8514(9) 0.6172(5) 0.7486(3) 0.059(3) Uani 1 1 d . . . . .
H32A H 0.889534 0.657902 0.752194 0.088 Uiso 1 1 calc GR . . . .
H32B H 0.894180 0.578753 0.752635 0.088 Uiso 1 1 calc GR . . . .
H32C H 0.796855 0.616055 0.766575 0.088 Uiso 1 1 calc GR . . . .
C25 C 0.7646(7) 0.7177(4) 0.6696(2) 0.031(2) Uani 1 1 d . . . . .
C21 C 1.1173(8) 0.9598(5) 0.5447(3) 0.050(3) Uani 1 1 d . . . . .
H21A H 1.124965 0.944249 0.518841 0.075 Uiso 1 1 calc GR . . . .
H21B H 1.176038 0.947937 0.559225 0.075 Uiso 1 1 calc GR . . . .
H21C H 1.109105 1.007967 0.544806 0.075 Uiso 1 1 calc GR . . . .
C3 C 1.3305(10) 0.6903(5) 0.5523(4) 0.055(3) Uani 1 1 d . . . . .
H3 H 1.340696 0.667809 0.529178 0.066 Uiso 1 1 calc R . . . .
C54 C 0.7728(8) 0.7068(5) 0.9404(3) 0.036(3) Uani 1 1 d . . . . .
C37 C 0.9642(8) 0.5837(5) 0.5984(3) 0.037(3) Uani 1 1 d . . . . .
C22 C 1.0138(9) 0.8939(5) 0.7049(3) 0.046(3) Uani 1 1 d . . . . .
H22 H 1.057778 0.856096 0.697988 0.055 Uiso 1 1 calc R . . . .
C84 C 0.2284(8) 0.8070(5) 0.8992(3) 0.056(3) Uani 1 1 d . . . . .
H84A H 0.156727 0.811198 0.896951 0.084 Uiso 1 1 calc GR . . . .
H84B H 0.252066 0.836062 0.919263 0.084 Uiso 1 1 calc GR . . . .
H84C H 0.245426 0.761041 0.905082 0.084 Uiso 1 1 calc GR . . . .
C64 C 0.5010(8) 1.0411(5) 0.8603(3) 0.042(3) Uani 1 1 d . . . . .
H64 H 0.482053 1.086096 0.857644 0.050 Uiso 1 1 calc R . . . .
C79 C 0.3454(8) 0.6118(5) 0.7920(2) 0.039(3) Uani 1 1 d . . . . .
H79 H 0.406099 0.615571 0.807683 0.047 Uiso 1 1 calc R . . . .
C30 C 0.7059(7) 0.7750(5) 0.6643(3) 0.039(2) Uani 1 1 d . . . . .
C40 C 0.9936(10) 0.4635(6) 0.5640(3) 0.061(4) Uani 1 1 d . . . . .
H40 H 1.002030 0.420995 0.553085 0.074 Uiso 1 1 calc R . . . .
C67 C 0.5406(8) 0.8914(5) 0.7971(3) 0.040(3) Uani 1 1 d . . . . .
H67 H 0.524653 0.844947 0.804596 0.048 Uiso 1 1 calc R . . . .
C10 C 1.2948(8) 0.7869(5) 0.6584(3) 0.043(3) Uani 1 1 d . . . . .
H10 H 1.222900 0.794177 0.662956 0.052 Uiso 1 1 calc R . . . .
C96 C 0.2465(8) 0.5787(6) 0.9354(3) 0.061(3) Uani 1 1 d . . . . .
H96A H 0.239544 0.571839 0.908280 0.091 Uiso 1 1 calc GR . . . .
H96B H 0.195675 0.609605 0.944013 0.091 Uiso 1 1 calc GR . . . .
H96C H 0.238884 0.536309 0.948382 0.091 Uiso 1 1 calc GR . . . .
C89 C 0.4439(8) 0.5027(6) 0.9466(3) 0.049(3) Uani 1 1 d . . . . .
H89 H 0.398513 0.488164 0.965174 0.058 Uiso 1 1 calc R . . . .
C39 C 0.9164(10) 0.5002(6) 0.5547(3) 0.058(4) Uani 1 1 d . . . . .
H39 H 0.872237 0.483717 0.536275 0.069 Uiso 1 1 calc R . . . .
C59 C 0.6886(9) 0.6200(5) 0.9809(3) 0.059(3) Uani 1 1 d . . . . .
H59A H 0.710310 0.586762 0.962723 0.088 Uiso 1 1 calc GR . . . .
H59B H 0.624053 0.607477 0.990963 0.088 Uiso 1 1 calc GR . . . .
H59C H 0.736395 0.622719 1.001451 0.088 Uiso 1 1 calc GR . . . .
C60 C 0.6522(8) 0.7401(5) 0.9907(3) 0.055(3) Uani 1 1 d . . . . .
H60A H 0.703843 0.743540 1.009831 0.083 Uiso 1 1 calc GR . . . .
H60B H 0.589804 0.727959 1.002692 0.083 Uiso 1 1 calc GR . . . .
H60C H 0.644801 0.782801 0.977994 0.083 Uiso 1 1 calc GR . . . .
C74 C 0.2842(8) 0.6733(5) 0.8000(3) 0.039(3) Uani 1 1 d . . . . .
C93 C 0.6200(8) 0.5455(5) 0.8252(3) 0.059(3) Uani 1 1 d . . . . .
H93A H 0.619450 0.497082 0.824032 0.088 Uiso 1 1 calc GR . . . .
H93B H 0.665657 0.562958 0.806382 0.088 Uiso 1 1 calc GR . . . .
H93C H 0.553628 0.562469 0.820333 0.088 Uiso 1 1 calc GR . . . .
C41 C 1.0623(8) 0.4870(5) 0.5898(3) 0.051(3) Uani 1 1 d . . . . .
H41 H 1.119242 0.461506 0.595302 0.061 Uiso 1 1 calc R . . . .
C47 C 1.2265(9) 0.5518(6) 0.6305(3) 0.064(4) Uani 1 1 d . . . . .
H47A H 1.232696 0.503713 0.633264 0.096 Uiso 1 1 calc GR . . . .
H47B H 1.268645 0.573929 0.648889 0.096 Uiso 1 1 calc GR . . . .
H47C H 1.246726 0.564674 0.605115 0.096 Uiso 1 1 calc GR . . . .
C9 C 1.1578(9) 0.6226(5) 0.5189(3) 0.059(3) Uani 1 1 d . . . . .
H9A H 1.211776 0.625317 0.500764 0.088 Uiso 1 1 calc GR . . . .
H9B H 1.096273 0.612235 0.505790 0.088 Uiso 1 1 calc GR . . . .
H9C H 1.172024 0.587641 0.537218 0.088 Uiso 1 1 calc GR . . . .
C34 C 0.7287(8) 0.8240(5) 0.6328(3) 0.042(3) Uani 1 1 d . . . . .
H34 H 0.801710 0.824520 0.629198 0.050 Uiso 1 1 calc R . . . .
C29 C 0.6268(8) 0.7844(6) 0.6880(3) 0.049(3) Uani 1 1 d . . . . .
H29 H 0.586420 0.822350 0.684881 0.059 Uiso 1 1 calc R . . . .
C31 C 0.8103(8) 0.6154(5) 0.7086(3) 0.042(3) Uani 1 1 d . . . . .
H31 H 0.867714 0.617039 0.691008 0.050 Uiso 1 1 calc R . . . .
C83 C 0.2493(10) 0.8996(5) 0.8532(4) 0.084(5) Uani 1 1 d . . . . .
H83A H 0.276780 0.912163 0.828763 0.126 Uiso 1 1 calc GR . . . .
H83B H 0.276294 0.928679 0.872646 0.126 Uiso 1 1 calc GR . . . .
H83C H 0.177495 0.904117 0.852514 0.126 Uiso 1 1 calc GR . . . .
C95 C 0.3595(8) 0.6228(6) 0.9854(3) 0.055(3) Uani 1 1 d . . . . .
H95A H 0.352706 0.581997 1.000023 0.083 Uiso 1 1 calc GR . . . .
H95B H 0.308678 0.654463 0.993129 0.083 Uiso 1 1 calc GR . . . .
H95C H 0.424762 0.642034 0.989801 0.083 Uiso 1 1 calc GR . . . .
C5 C 1.3983(9) 0.7382(6) 0.6070(3) 0.062(3) Uani 1 1 d . . . . .
H5 H 1.454916 0.748079 0.621627 0.074 Uiso 1 1 calc R . . . .
C75 C 0.2034(9) 0.6857(7) 0.7779(3) 0.058(3) Uani 1 1 d . . . . .
H75 H 0.185388 0.654059 0.759424 0.070 Uiso 1 1 calc R . . . .
C35 C 0.6958(9) 0.8951(5) 0.6411(3) 0.071(4) Uani 1 1 d . . . . .
H35A H 0.624480 0.898792 0.637580 0.107 Uiso 1 1 calc GR . . . .
H35B H 0.729550 0.925622 0.624065 0.107 Uiso 1 1 calc GR . . . .
H35C H 0.712524 0.906368 0.667103 0.107 Uiso 1 1 calc GR . . . .
C45 C 0.7116(8) 0.5720(6) 0.5651(3) 0.068(4) Uani 1 1 d . . . . .
H45A H 0.706717 0.528703 0.552809 0.101 Uiso 1 1 calc GR . . . .
H45B H 0.659000 0.600938 0.555850 0.101 Uiso 1 1 calc GR . . . .
H45C H 0.704983 0.566444 0.592252 0.101 Uiso 1 1 calc GR . . . .
C81 C 0.2943(10) 0.5487(6) 0.8039(3) 0.086(5) Uani 1 1 d . . . . .
H81A H 0.274299 0.552331 0.830221 0.129 Uiso 1 1 calc GR . . . .
H81B H 0.339561 0.511274 0.800977 0.129 Uiso 1 1 calc GR . . . .
H81C H 0.235948 0.541606 0.788230 0.129 Uiso 1 1 calc GR . . . .
C69 C 0.4701(10) 0.9103(6) 0.7658(3) 0.077(4) Uani 1 1 d . . . . .
H69A H 0.404185 0.917402 0.776172 0.115 Uiso 1 1 calc GR . . . .
H69B H 0.467663 0.874515 0.747202 0.115 Uiso 1 1 calc GR . . . .
H69C H 0.493073 0.951016 0.753680 0.115 Uiso 1 1 calc GR . . . .
C50 C 0.8505(8) 0.7573(5) 0.8851(3) 0.042(3) Uani 1 1 d . . . . .
C77 C 0.1731(9) 0.7874(6) 0.8085(3) 0.061(4) Uani 1 1 d . . . . .
H77 H 0.134657 0.826410 0.811191 0.073 Uiso 1 1 calc R . . . .
C36 C 0.6825(8) 0.7995(6) 0.5965(2) 0.055(3) Uani 1 1 d . . . . .
H36A H 0.708173 0.755368 0.590545 0.083 Uiso 1 1 calc GR . . . .
H36B H 0.698664 0.830100 0.576113 0.083 Uiso 1 1 calc GR . . . .
H36C H 0.610781 0.797121 0.599462 0.083 Uiso 1 1 calc GR . . . .
C26 C 0.7451(7) 0.6727(5) 0.6994(3) 0.034(3) Uani 1 1 d . . . . .
C11 C 1.3324(8) 0.7373(6) 0.6887(3) 0.072(4) Uani 1 1 d . . . . .
H11A H 1.291873 0.697153 0.688084 0.109 Uiso 1 1 calc GR . . . .
H11B H 1.327967 0.757739 0.713516 0.109 Uiso 1 1 calc GR . . . .
H11C H 1.401151 0.725671 0.683395 0.109 Uiso 1 1 calc GR . . . .
C76 C 0.1480(9) 0.7417(7) 0.7815(3) 0.074(4) Uani 1 1 d . . . . .
H76 H 0.092892 0.749055 0.765678 0.089 Uiso 1 1 calc R . . . .
C12 C 1.3458(9) 0.8533(5) 0.6620(3) 0.072(4) Uani 1 1 d . . . . .
H12A H 1.413697 0.849529 0.652932 0.107 Uiso 1 1 calc GR . . . .
H12B H 1.346213 0.867027 0.688360 0.107 Uiso 1 1 calc GR . . . .
H12C H 1.310479 0.886332 0.647024 0.107 Uiso 1 1 calc GR . . . .
C80 C 0.3797(9) 0.6079(6) 0.7514(3) 0.062(3) Uani 1 1 d . . . . .
H80A H 0.323460 0.597725 0.735215 0.093 Uiso 1 1 calc GR . . . .
H80B H 0.429451 0.573042 0.748998 0.093 Uiso 1 1 calc GR . . . .
H80C H 0.408320 0.650472 0.743999 0.093 Uiso 1 1 calc GR . . . .
C4 C 1.4095(9) 0.7054(6) 0.5739(4) 0.065(4) Uani 1 1 d . . . . .
H4 H 1.473551 0.692859 0.565911 0.078 Uiso 1 1 calc R . . . .
C33 C 0.7577(10) 0.5495(6) 0.7021(4) 0.084(5) Uani 1 1 d . . . . .
H33A H 0.802599 0.512971 0.707920 0.127 Uiso 1 1 calc GR . . . .
H33B H 0.736893 0.546474 0.675865 0.127 Uiso 1 1 calc GR . . . .
H33C H 0.699741 0.546905 0.718446 0.127 Uiso 1 1 calc GR . . . .
C68 C 0.6445(10) 0.8918(6) 0.7838(3) 0.080(4) Uani 1 1 d . . . . .
H68A H 0.661502 0.936098 0.774734 0.121 Uiso 1 1 calc GR . . . .
H68B H 0.652185 0.859682 0.763458 0.121 Uiso 1 1 calc GR . . . .
H68C H 0.688246 0.879821 0.804625 0.121 Uiso 1 1 calc GR . . . .
C24 C 1.0617(12) 0.9304(6) 0.7377(3) 0.105(6) Uani 1 1 d . . . . .
H24A H 1.126462 0.946999 0.729955 0.157 Uiso 1 1 calc GR . . . .
H24B H 1.069585 0.899957 0.758842 0.157 Uiso 1 1 calc GR . . . .
H24C H 1.019914 0.967624 0.745179 0.157 Uiso 1 1 calc GR . . . .
C92 C 0.7612(8) 0.5465(6) 0.8708(3) 0.063(4) Uani 1 1 d . . . . .
H92A H 0.780808 0.558764 0.896369 0.094 Uiso 1 1 calc GR . . . .
H92B H 0.804005 0.569058 0.852766 0.094 Uiso 1 1 calc GR . . . .
H92C H 0.767314 0.498535 0.867681 0.094 Uiso 1 1 calc GR . . . .
C44 C 0.8235(9) 0.6166(6) 0.5142(3) 0.067(4) Uani 1 1 d . . . . .
H44A H 0.883698 0.642179 0.509747 0.100 Uiso 1 1 calc GR . . . .
H44B H 0.766442 0.641641 0.505172 0.100 Uiso 1 1 calc GR . . . .
H44C H 0.827583 0.574384 0.500672 0.100 Uiso 1 1 calc GR . . . .
C53 C 0.8651(10) 0.6884(6) 0.9529(3) 0.056(3) Uani 1 1 d . . . . .
H53 H 0.870701 0.663979 0.975523 0.068 Uiso 1 1 calc R . . . .
C23 C 0.9156(10) 0.8654(6) 0.7162(3) 0.080(4) Uani 1 1 d . . . . .
H23A H 0.875947 0.899712 0.728376 0.119 Uiso 1 1 calc GR . . . .
H23B H 0.925882 0.828565 0.733655 0.119 Uiso 1 1 calc GR . . . .
H23C H 0.881024 0.849239 0.693849 0.119 Uiso 1 1 calc GR . . . .
C57 C 0.9009(10) 0.8511(5) 0.8421(3) 0.089(5) Uani 1 1 d . . . . .
H57A H 0.870857 0.884142 0.858667 0.134 Uiso 1 1 calc GR . . . .
H57B H 0.897317 0.866383 0.816116 0.134 Uiso 1 1 calc GR . . . .
H57C H 0.970011 0.844682 0.849228 0.134 Uiso 1 1 calc GR . . . .
C8 C 1.1238(8) 0.7450(5) 0.5116(2) 0.057(3) Uani 1 1 d . . . . .
H8A H 1.119285 0.787270 0.525007 0.086 Uiso 1 1 calc GR . . . .
H8B H 1.060994 0.735680 0.499181 0.086 Uiso 1 1 calc GR . . . .
H8C H 1.176320 0.747586 0.492810 0.086 Uiso 1 1 calc GR . . . .
C51 C 0.9414(8) 0.7376(6) 0.8998(4) 0.065(3) Uani 1 1 d . . . . .
H51 H 0.999769 0.747192 0.886145 0.078 Uiso 1 1 calc R . . . .
C28 C 0.6049(8) 0.7395(6) 0.7163(3) 0.053(3) Uani 1 1 d . . . . .
H28 H 0.549267 0.746452 0.731957 0.063 Uiso 1 1 calc R . . . .
C52 C 0.9488(10) 0.7046(6) 0.9334(4) 0.071(4) Uani 1 1 d . . . . .
H52 H 1.011660 0.692981 0.943122 0.085 Uiso 1 1 calc R . . . .
C27 C 0.6636(8) 0.6853(5) 0.7216(3) 0.046(3) Uani 1 1 d . . . . .
H27 H 0.647890 0.655200 0.741155 0.055 Uiso 1 1 calc R . . . .
C55 C 0.8463(8) 0.7863(5) 0.8459(3) 0.054(3) Uani 1 1 d . . . . .
H55 H 0.775445 0.795543 0.840311 0.065 Uiso 1 1 calc R . . . .
C56 C 0.8816(11) 0.7380(6) 0.8170(3) 0.102(5) Uani 1 1 d . . . . .
H56A H 0.953192 0.733206 0.818964 0.153 Uiso 1 1 calc GR . . . .
H56B H 0.864474 0.754347 0.791957 0.153 Uiso 1 1 calc GR . . . .
H56C H 0.850084 0.695018 0.821178 0.153 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tl3 Tl4 3.4673(5) . ?
Tl3 N10 2.654(7) . ?
Tl3 N12 2.742(7) . ?
Tl3 N9 2.726(7) . ?
Tl3 N7 2.681(7) . ?
Tl1 Tl2 3.4612(5) . ?
Tl1 N6 2.645(7) . ?
Tl1 N1 2.746(7) . ?
Tl1 N3 2.699(7) . ?
Tl1 N4 2.761(7) . ?
Tl4 N10 2.773(7) . ?
Tl4 N12 2.637(7) . ?
Tl4 N9 2.663(8) . ?
Tl4 N7 2.777(7) . ?
Tl2 N6 2.757(7) . ?
Tl2 N1 2.727(7) . ?
Tl2 N3 2.734(7) . ?
Tl2 N4 2.646(7) . ?
N6 N5 1.307(9) . ?
N6 C37 1.431(11) . ?
N10 N11 1.295(9) . ?
N10 C73 1.443(11) . ?
N5 N4 1.326(9) . ?
N12 C85 1.466(11) . ?
N12 N11 1.289(9) . ?
N1 N2 1.324(9) . ?
N1 C1 1.418(11) . ?
C85 C86 1.386(13) . ?
C85 C90 1.411(12) . ?
N9 N8 1.327(10) . ?
N9 C61 1.438(12) . ?
N3 N2 1.307(9) . ?
N3 C13 1.438(11) . ?
N7 N8 1.308(10) . ?
N7 C49 1.411(11) . ?
C62 C61 1.409(12) . ?
C62 C63 1.384(12) . ?
C62 C67 1.527(13) . ?
C66 C61 1.396(12) . ?
C66 C70 1.535(12) . ?
C66 C65 1.400(12) . ?
C87 C86 1.375(12) . ?
C87 C88 1.376(14) . ?
C19 C20 1.516(13) . ?
C19 C14 1.522(12) . ?
C19 C21 1.524(13) . ?
C13 C14 1.403(12) . ?
C13 C18 1.426(12) . ?
C1 C2 1.403(13) . ?
C1 C6 1.431(12) . ?
C42 C46 1.523(14) . ?
C42 C37 1.385(14) . ?
C42 C41 1.398(13) . ?
N4 C25 1.424(11) . ?
C82 C78 1.499(14) . ?
C82 C84 1.535(13) . ?
C82 C83 1.547(13) . ?
C78 C73 1.407(12) . ?
C78 C77 1.393(13) . ?
C73 C74 1.391(12) . ?
C38 C43 1.509(15) . ?
C38 C37 1.418(14) . ?
C38 C39 1.396(13) . ?
C63 C64 1.380(13) . ?
C2 C7 1.504(14) . ?
C2 C3 1.380(14) . ?
C17 C16 1.380(13) . ?
C17 C18 1.370(11) . ?
C48 C46 1.538(14) . ?
C86 C91 1.522(14) . ?
C70 C71 1.510(13) . ?
C70 C72 1.529(13) . ?
C14 C15 1.379(12) . ?
C88 C89 1.385(14) . ?
C16 C15 1.379(13) . ?
C65 C64 1.356(13) . ?
C90 C94 1.505(13) . ?
C90 C89 1.394(13) . ?
C91 C93 1.523(14) . ?
C91 C92 1.545(14) . ?
C18 C22 1.531(13) . ?
C7 C9 1.548(13) . ?
C7 C8 1.530(13) . ?
C58 C54 1.520(14) . ?
C58 C59 1.510(13) . ?
C58 C60 1.543(13) . ?
C94 C96 1.517(14) . ?
C94 C95 1.530(12) . ?
C43 C45 1.540(14) . ?
C43 C44 1.528(14) . ?
C49 C54 1.440(13) . ?
C49 C50 1.405(13) . ?
C6 C10 1.507(13) . ?
C6 C5 1.391(14) . ?
C46 C47 1.496(14) . ?
C32 C31 1.534(12) . ?
C25 C30 1.417(12) . ?
C25 C26 1.424(12) . ?
C3 C4 1.356(15) . ?
C54 C53 1.381(14) . ?
C22 C24 1.527(14) . ?
C22 C23 1.507(16) . ?
C79 C74 1.521(13) . ?
C79 C81 1.513(14) . ?
C79 C80 1.521(12) . ?
C30 C34 1.530(13) . ?
C30 C29 1.378(12) . ?
C40 C39 1.327(16) . ?
C40 C41 1.392(15) . ?
C67 C69 1.520(14) . ?
C67 C68 1.487(15) . ?
C10 C11 1.559(12) . ?
C10 C12 1.515(12) . ?
C74 C75 1.373(14) . ?
C34 C35 1.534(13) . ?
C34 C36 1.522(12) . ?
C29 C28 1.389(14) . ?
C31 C26 1.494(14) . ?
C31 C33 1.528(14) . ?
C5 C4 1.361(15) . ?
C75 C76 1.366(15) . ?
C50 C51 1.399(14) . ?
C50 C55 1.518(13) . ?
C77 C76 1.376(16) . ?
C26 C27 1.384(13) . ?
C53 C52 1.371(16) . ?
C57 C55 1.510(14) . ?
C51 C52 1.376(16) . ?
C28 C27 1.368(14) . ?
C55 C56 1.497(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N10 Tl3 Tl4 51.82(14) . . ?
N10 Tl3 N12 46.1(2) . . ?
N10 Tl3 N9 85.9(2) . . ?
N10 Tl3 N7 103.4(2) . . ?
N12 Tl3 Tl4 48.56(15) . . ?
N9 Tl3 Tl4 49.16(15) . . ?
N9 Tl3 N12 97.6(2) . . ?
N7 Tl3 Tl4 51.79(15) . . ?
N7 Tl3 N12 79.3(2) . . ?
N7 Tl3 N9 47.3(2) . . ?
N6 Tl1 Tl2 51.59(16) . . ?
N6 Tl1 N1 79.4(2) . . ?
N6 Tl1 N3 102.1(2) . . ?
N6 Tl1 N4 47.3(2) . . ?
N1 Tl1 Tl2 50.52(13) . . ?
N1 Tl1 N4 99.0(2) . . ?
N3 Tl1 Tl2 50.87(14) . . ?
N3 Tl1 N1 46.8(2) . . ?
N3 Tl1 N4 85.3(2) . . ?
N4 Tl1 Tl2 48.75(15) . . ?
N10 Tl4 Tl3 48.80(15) . . ?
N10 Tl4 N7 97.9(2) . . ?
N12 Tl4 Tl3 51.21(15) . . ?
N12 Tl4 N10 45.9(2) . . ?
N12 Tl4 N9 101.8(2) . . ?
N12 Tl4 N7 79.4(2) . . ?
N9 Tl4 Tl3 50.75(16) . . ?
N9 Tl4 N10 84.8(2) . . ?
N9 Tl4 N7 46.9(2) . . ?
N7 Tl4 Tl3 49.34(13) . . ?
N6 Tl2 Tl1 48.74(15) . . ?
N1 Tl2 Tl1 51.03(14) . . ?
N1 Tl2 N6 77.9(2) . . ?
N1 Tl2 N3 46.7(2) . . ?
N3 Tl2 Tl1 49.99(14) . . ?
N3 Tl2 N6 98.4(2) . . ?
N4 Tl2 Tl1 51.68(15) . . ?
N4 Tl2 N6 47.3(2) . . ?
N4 Tl2 N1 102.5(2) . . ?
N4 Tl2 N3 86.9(2) . . ?
Tl1 N6 Tl2 79.66(19) . . ?
N5 N6 Tl1 94.9(5) . . ?
N5 N6 Tl2 90.4(5) . . ?
N5 N6 C37 113.8(8) . . ?
C37 N6 Tl1 125.2(6) . . ?
C37 N6 Tl2 140.9(6) . . ?
Tl3 N10 Tl4 79.4(2) . . ?
N11 N10 Tl3 96.5(5) . . ?
N11 N10 Tl4 89.3(5) . . ?
N11 N10 C73 113.9(7) . . ?
C73 N10 Tl3 123.7(5) . . ?
C73 N10 Tl4 142.3(5) . . ?
N6 N5 N4 111.0(7) . . ?
Tl4 N12 Tl3 80.23(19) . . ?
C85 N12 Tl3 139.7(6) . . ?
C85 N12 Tl4 124.2(5) . . ?
N11 N12 Tl3 92.6(5) . . ?
N11 N12 Tl4 95.5(5) . . ?
N11 N12 C85 113.5(7) . . ?
Tl2 N1 Tl1 78.45(18) . . ?
N2 N1 Tl1 91.1(5) . . ?
N2 N1 Tl2 93.6(5) . . ?
N2 N1 C1 114.6(7) . . ?
C1 N1 Tl1 139.8(6) . . ?
C1 N1 Tl2 126.7(5) . . ?
C86 C85 N12 119.7(8) . . ?
C86 C85 C90 121.2(9) . . ?
C90 C85 N12 118.9(8) . . ?
Tl4 N9 Tl3 80.1(2) . . ?
N8 N9 Tl3 92.8(5) . . ?
N8 N9 Tl4 93.2(5) . . ?
N8 N9 C61 113.8(8) . . ?
C61 N9 Tl3 142.9(6) . . ?
C61 N9 Tl4 121.2(5) . . ?
N12 N11 N10 109.7(7) . . ?
Tl1 N3 Tl2 79.14(18) . . ?
N2 N3 Tl1 93.6(5) . . ?
N2 N3 Tl2 93.7(5) . . ?
N2 N3 C13 112.9(7) . . ?
C13 N3 Tl1 124.2(5) . . ?
C13 N3 Tl2 141.3(5) . . ?
Tl3 N7 Tl4 78.87(19) . . ?
N8 N7 Tl3 95.3(5) . . ?
N8 N7 Tl4 88.6(5) . . ?
N8 N7 C49 112.6(7) . . ?
C49 N7 Tl3 128.9(5) . . ?
C49 N7 Tl4 140.0(6) . . ?
N3 N2 N1 110.5(7) . . ?
N7 N8 N9 110.8(7) . . ?
C61 C62 C67 121.3(8) . . ?
C63 C62 C61 118.2(9) . . ?
C63 C62 C67 120.3(9) . . ?
C61 C66 C70 123.0(8) . . ?
C61 C66 C65 118.6(9) . . ?
C65 C66 C70 118.4(8) . . ?
C86 C87 C88 120.6(10) . . ?
C20 C19 C14 111.3(8) . . ?
C20 C19 C21 111.9(8) . . ?
C14 C19 C21 111.8(9) . . ?
C14 C13 N3 120.8(8) . . ?
C14 C13 C18 120.4(8) . . ?
C18 C13 N3 118.6(8) . . ?
N1 C1 C6 118.5(8) . . ?
C2 C1 N1 120.1(9) . . ?
C2 C1 C6 121.2(9) . . ?
C62 C61 N9 117.3(8) . . ?
C66 C61 N9 122.1(8) . . ?
C66 C61 C62 120.3(9) . . ?
C37 C42 C46 122.4(9) . . ?
C37 C42 C41 117.9(10) . . ?
C41 C42 C46 119.7(10) . . ?
Tl2 N4 Tl1 79.58(19) . . ?
N5 N4 Tl1 89.3(5) . . ?
N5 N4 Tl2 94.9(5) . . ?
N5 N4 C25 113.6(7) . . ?
C25 N4 Tl1 143.9(6) . . ?
C25 N4 Tl2 123.0(5) . . ?
C78 C82 C84 110.8(9) . . ?
C78 C82 C83 115.8(9) . . ?
C84 C82 C83 108.7(9) . . ?
C73 C78 C82 121.9(9) . . ?
C77 C78 C82 119.9(10) . . ?
C77 C78 C73 118.2(10) . . ?
C78 C73 N10 116.1(8) . . ?
C74 C73 N10 123.4(8) . . ?
C74 C73 C78 120.5(9) . . ?
C37 C38 C43 124.0(9) . . ?
C39 C38 C43 119.9(10) . . ?
C39 C38 C37 115.9(11) . . ?
C64 C63 C62 121.9(10) . . ?
C1 C2 C7 119.7(9) . . ?
C3 C2 C1 117.5(11) . . ?
C3 C2 C7 122.7(10) . . ?
C18 C17 C16 121.3(9) . . ?
C85 C86 C91 119.5(9) . . ?
C87 C86 C85 119.4(10) . . ?
C87 C86 C91 121.1(9) . . ?
C71 C70 C66 111.4(8) . . ?
C71 C70 C72 110.9(8) . . ?
C72 C70 C66 110.4(8) . . ?
C13 C14 C19 123.0(8) . . ?
C15 C14 C19 119.2(8) . . ?
C15 C14 C13 117.7(8) . . ?
C87 C88 C89 120.3(10) . . ?
C15 C16 C17 119.3(9) . . ?
C64 C65 C66 121.6(9) . . ?
C85 C90 C94 124.7(9) . . ?
C89 C90 C85 117.4(9) . . ?
C89 C90 C94 117.9(9) . . ?
C86 C91 C93 110.3(9) . . ?
C86 C91 C92 115.3(9) . . ?
C93 C91 C92 110.0(9) . . ?
C13 C18 C22 120.3(8) . . ?
C17 C18 C13 118.7(9) . . ?
C17 C18 C22 121.0(9) . . ?
C2 C7 C9 112.8(9) . . ?
C2 C7 C8 110.9(9) . . ?
C8 C7 C9 110.6(8) . . ?
C54 C58 C60 110.8(9) . . ?
C59 C58 C54 114.2(9) . . ?
C59 C58 C60 109.9(8) . . ?
C90 C94 C96 113.3(9) . . ?
C90 C94 C95 111.1(8) . . ?
C96 C94 C95 111.4(9) . . ?
C38 C43 C45 112.1(10) . . ?
C38 C43 C44 111.0(9) . . ?
C44 C43 C45 111.3(9) . . ?
C14 C15 C16 122.5(9) . . ?
N7 C49 C54 118.4(9) . . ?
C50 C49 N7 121.9(9) . . ?
C50 C49 C54 119.4(9) . . ?
C1 C6 C10 123.1(9) . . ?
C5 C6 C1 116.6(10) . . ?
C5 C6 C10 120.2(10) . . ?
C42 C46 C48 110.1(9) . . ?
C47 C46 C42 116.0(9) . . ?
C47 C46 C48 110.1(10) . . ?
C30 C25 N4 116.1(8) . . ?
C30 C25 C26 121.0(9) . . ?
C26 C25 N4 122.6(8) . . ?
C4 C3 C2 121.8(12) . . ?
C49 C54 C58 120.7(9) . . ?
C53 C54 C58 120.6(10) . . ?
C53 C54 C49 118.7(10) . . ?
C42 C37 N6 118.2(9) . . ?
C42 C37 C38 122.1(9) . . ?
C38 C37 N6 119.6(9) . . ?
C24 C22 C18 112.0(9) . . ?
C23 C22 C18 110.9(10) . . ?
C23 C22 C24 110.9(10) . . ?
C65 C64 C63 119.4(10) . . ?
C74 C79 C80 112.9(8) . . ?
C81 C79 C74 112.6(10) . . ?
C81 C79 C80 111.3(9) . . ?
C25 C30 C34 120.7(8) . . ?
C29 C30 C25 118.0(9) . . ?
C29 C30 C34 121.3(9) . . ?
C39 C40 C41 120.2(11) . . ?
C69 C67 C62 114.3(9) . . ?
C68 C67 C62 109.4(9) . . ?
C68 C67 C69 111.2(9) . . ?
C6 C10 C11 110.1(8) . . ?
C6 C10 C12 112.4(9) . . ?
C12 C10 C11 111.2(9) . . ?
C88 C89 C90 120.9(10) . . ?
C40 C39 C38 123.3(12) . . ?
C73 C74 C79 122.9(9) . . ?
C75 C74 C73 118.5(10) . . ?
C75 C74 C79 118.5(10) . . ?
C40 C41 C42 120.3(10) . . ?
C30 C34 C35 113.9(8) . . ?
C36 C34 C30 109.4(8) . . ?
C36 C34 C35 110.5(9) . . ?
C30 C29 C28 121.5(10) . . ?
C26 C31 C32 113.7(8) . . ?
C26 C31 C33 111.3(9) . . ?
C33 C31 C32 109.3(9) . . ?
C4 C5 C6 121.5(12) . . ?
C76 C75 C74 122.4(12) . . ?
C49 C50 C55 122.3(10) . . ?
C51 C50 C49 118.3(10) . . ?
C51 C50 C55 119.2(11) . . ?
C76 C77 C78 121.2(11) . . ?
C25 C26 C31 123.3(9) . . ?
C27 C26 C25 117.3(10) . . ?
C27 C26 C31 119.4(9) . . ?
C75 C76 C77 119.1(11) . . ?
C3 C4 C5 121.0(12) . . ?
C52 C53 C54 121.7(12) . . ?
C52 C51 C50 121.9(12) . . ?
C27 C28 C29 119.9(10) . . ?
C53 C52 C51 119.7(11) . . ?
C28 C27 C26 122.3(10) . . ?
C57 C55 C50 113.4(9) . . ?
C56 C55 C50 111.9(9) . . ?
C56 C55 C57 110.2(10) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.546(7)
2 0.454(7)

_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_7(18c6)
_database_code_depnum_ccdc_archive 'CCDC 1972000'
loop_
_audit_author_name
_audit_author_address
'Alasdair McKay'
;Monash University
Australia
;
_audit_update_record             
;
2019-12-14 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_audit_creation_date             2019-04-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
''
alasdair.mckay@monash.edu
_chemical_name_common            '[K(18-crown-6)(N3Dipp2)]'
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H58 K N3 O6, 0.5(C7 H8)'
_chemical_formula_sum            'C39.50 H62 K N3 O6'
_chemical_formula_weight         714.02
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.9780(6)
_cell_length_b                   10.6630(9)
_cell_length_c                   21.8772(19)
_cell_angle_alpha                80.650(4)
_cell_angle_beta                 85.194(4)
_cell_angle_gamma                79.586(4)
_cell_volume                     2029.3(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6321
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.898
_cell_measurement_theta_min      2.304
_shelx_estimated_absorpt_T_max   0.991
_shelx_estimated_absorpt_T_min   0.942
_exptl_absorpt_coefficient_mu    0.177
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1407 before and 0.0651 after correction. The Ratio of minimum to maximum transmission is 0.8992. The λ/2 correction factor is 0.00150.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             774
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_unetI/netI     0.0681
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            33912
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.101
_diffrn_reflns_theta_min         2.048
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5834
_reflns_number_total             8950
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         8950
_refine_ls_number_restraints     122
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0490
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0470P)²+0.3885P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1260
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C38-C43 \\sim C43-C42 \\sim C42-C41 \\sim C41-C40 \\sim C40-C39 \\sim C39-C38
 with sigma of 0.02
 C38-C40 \\sim C38-C42 \\sim C39-C41 \\sim C43-C39 \\sim C42-C40 \\sim C43-C41
 with sigma of 0.04
 C37-C39 \\sim C37-C43
 with sigma of 0.04
3. Restrained planarity
 C37, C38, C43, C42, C41, C40, C39
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C37 \\sim C38 \\sim C43 \\sim C42 \\sim C41 \\sim C40 \\sim C39: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C37, C38, C43, C42, C41, C40, C39
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C37(0.5) H37A(0.5) H37B(0.5) H37C(0.5) C38(0.5) C43(0.5) H43(0.5)
 C42(0.5) H42(0.5) C41(0.5) H41(0.5) C40(0.5) H40(0.5) C39(0.5) H39(0.5)
7.a Ternary CH refined with riding coordinates:
 C10(H10), C7(H7), C22(H22), C19(H19)
7.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C36(H36A,H36B), C27(H27A,H27B), C26(H26A,H26B), C29(H29A,
 H29B), C28(H28A,H28B), C35(H35A,H35B), C33(H33A,H33B), C32(H32A,H32B),
 C30(H30A,H30B), C34(H34A,H34B), C31(H31A,H31B)
7.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C3(H3), C17(H17), C15(H15), C16(H16), C43(H43), C42(H42),
 C41(H41), C40(H40), C39(H39)
7.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C23(H23A,H23B,H23C), C9(H9A,H9B,
 H9C), C24(H24A,H24B,H24C), C20(H20A,H20B,H20C), C8(H8A,H8B,H8C), C21(H21A,H21B,
 H21C), C37(H37A,H37B,H37C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.58158(4) 0.53413(4) 0.23471(2) 0.02999(12) Uani 1 1 d . . . . .
O1 O 0.68651(14) 0.60971(16) 0.11023(6) 0.0439(4) Uani 1 1 d . . . . .
N2 N 0.21246(15) 0.68105(14) 0.23337(6) 0.0225(3) Uani 1 1 d . . . . .
N3 N 0.29288(15) 0.65285(14) 0.28282(6) 0.0236(3) Uani 1 1 d . . . . .
N1 N 0.29403(14) 0.66350(14) 0.18250(6) 0.0221(3) Uani 1 1 d . . . . .
O4 O 0.65317(15) 0.39192(16) 0.35574(7) 0.0510(4) Uani 1 1 d . . . . .
O3 O 0.74045(16) 0.63001(18) 0.32150(7) 0.0538(4) Uani 1 1 d . . . . .
O2 O 0.70345(15) 0.76355(15) 0.20313(7) 0.0475(4) Uani 1 1 d . . . . .
O6 O 0.60178(16) 0.36553(16) 0.14159(7) 0.0496(4) Uani 1 1 d . . . . .
O5 O 0.65954(17) 0.24185(15) 0.26234(8) 0.0541(4) Uani 1 1 d . . . . .
C1 C 0.20253(17) 0.68038(17) 0.13060(8) 0.0215(4) Uani 1 1 d . . . . .
C2 C 0.14642(19) 0.57474(18) 0.11638(8) 0.0270(4) Uani 1 1 d . . . . .
C13 C 0.20552(17) 0.68539(19) 0.33652(8) 0.0259(4) Uani 1 1 d . . . . .
C6 C 0.17877(18) 0.79875(18) 0.09050(8) 0.0262(4) Uani 1 1 d . . . . .
C5 C 0.1019(2) 0.8075(2) 0.03705(8) 0.0316(4) Uani 1 1 d . . . . .
H5 H 0.086978 0.886908 0.009616 0.038 Uiso 1 1 calc R . . . .
C18 C 0.13576(19) 0.8123(2) 0.34210(9) 0.0316(4) Uani 1 1 d . . . . .
C14 C 0.20042(19) 0.5866(2) 0.38776(8) 0.0321(5) Uani 1 1 d . . . . .
C4 C 0.0471(2) 0.7041(2) 0.02288(9) 0.0342(5) Uani 1 1 d . . . . .
H4 H -0.005338 0.711997 -0.013887 0.041 Uiso 1 1 calc R . . . .
C10 C 0.2239(2) 0.91852(18) 0.10659(9) 0.0326(5) Uani 1 1 d . . . . .
H10 H 0.290602 0.892149 0.142471 0.039 Uiso 1 1 calc R . . . .
C3 C 0.0689(2) 0.5889(2) 0.06261(9) 0.0332(5) Uani 1 1 d . . . . .
H3 H 0.030071 0.517609 0.053056 0.040 Uiso 1 1 calc R . . . .
C7 C 0.1632(2) 0.44785(19) 0.15996(9) 0.0363(5) Uani 1 1 d . . . . .
H7 H 0.237332 0.451168 0.191072 0.044 Uiso 1 1 calc R . . . .
C22 C 0.1498(2) 0.92149(19) 0.28932(9) 0.0357(5) Uani 1 1 d . . . . .
H22 H 0.126174 0.891962 0.250667 0.043 Uiso 1 1 calc R . . . .
C11 C 0.0828(2) 1.0095(2) 0.12665(10) 0.0395(5) Uani 1 1 d . . . . .
H11A H 0.018487 1.040591 0.091388 0.059 Uiso 1 1 calc GR . . . .
H11B H 0.113473 1.083063 0.140930 0.059 Uiso 1 1 calc GR . . . .
H11C H 0.025978 0.963251 0.160475 0.059 Uiso 1 1 calc GR . . . .
C19 C 0.2737(2) 0.4500(2) 0.38161(9) 0.0378(5) Uani 1 1 d . . . . .
H19 H 0.364384 0.455124 0.352057 0.045 Uiso 1 1 calc R . . . .
C17 C 0.0585(2) 0.8368(2) 0.39795(10) 0.0442(6) Uani 1 1 d . . . . .
H17 H 0.009423 0.922018 0.401967 0.053 Uiso 1 1 calc R . . . .
C15 C 0.1225(2) 0.6168(2) 0.44242(9) 0.0445(6) Uani 1 1 d . . . . .
H15 H 0.118265 0.550604 0.476988 0.053 Uiso 1 1 calc R . . . .
C16 C 0.0520(2) 0.7395(3) 0.44758(10) 0.0519(6) Uani 1 1 d . . . . .
H16 H -0.001590 0.757924 0.485290 0.062 Uiso 1 1 calc R . . . .
C12 C 0.3116(2) 0.9902(2) 0.05312(11) 0.0512(6) Uani 1 1 d . . . . .
H12A H 0.395712 0.929572 0.037323 0.077 Uiso 1 1 calc GR . . . .
H12B H 0.351614 1.058622 0.068047 0.077 Uiso 1 1 calc GR . . . .
H12C H 0.243428 1.028273 0.019753 0.077 Uiso 1 1 calc GR . . . .
C23 C 0.0392(3) 1.0459(2) 0.29589(11) 0.0546(6) Uani 1 1 d . . . . .
H23A H -0.064528 1.027566 0.302194 0.082 Uiso 1 1 calc GR . . . .
H23B H 0.047255 1.108436 0.258119 0.082 Uiso 1 1 calc GR . . . .
H23C H 0.063863 1.081765 0.331563 0.082 Uiso 1 1 calc GR . . . .
C25 C 0.6540(3) 0.7455(2) 0.10088(11) 0.0548(7) Uani 1 1 d . . . . .
H25A H 0.545693 0.775007 0.112243 0.066 Uiso 1 1 calc R . . . .
H25B H 0.674084 0.779304 0.056638 0.066 Uiso 1 1 calc R . . . .
C36 C 0.6076(3) 0.5556(3) 0.07016(10) 0.0570(7) Uani 1 1 d . . . . .
H36A H 0.632416 0.589695 0.026360 0.068 Uiso 1 1 calc R . . . .
H36B H 0.496818 0.578734 0.078638 0.068 Uiso 1 1 calc R . . . .
C27 C 0.8015(2) 0.7940(2) 0.24380(12) 0.0538(6) Uani 1 1 d . . . . .
H27A H 0.809205 0.886633 0.234237 0.065 Uiso 1 1 calc R . . . .
H27B H 0.904226 0.742968 0.238616 0.065 Uiso 1 1 calc R . . . .
C26 C 0.7516(2) 0.7945(2) 0.14023(11) 0.0534(7) Uani 1 1 d . . . . .
H26A H 0.858876 0.754472 0.133409 0.064 Uiso 1 1 calc R . . . .
H26B H 0.743630 0.889129 0.128980 0.064 Uiso 1 1 calc R . . . .
C9 C 0.2255(3) 0.3336(2) 0.12659(12) 0.0543(6) Uani 1 1 d . . . . .
H9A H 0.151480 0.323722 0.098016 0.081 Uiso 1 1 calc GR . . . .
H9B H 0.245040 0.255120 0.157046 0.081 Uiso 1 1 calc GR . . . .
H9C H 0.320353 0.348226 0.103167 0.081 Uiso 1 1 calc GR . . . .
C24 C 0.3115(2) 0.9479(2) 0.27990(11) 0.0515(6) Uani 1 1 d . . . . .
H24A H 0.339695 0.975895 0.317227 0.077 Uiso 1 1 calc GR . . . .
H24B H 0.318738 1.015908 0.244328 0.077 Uiso 1 1 calc GR . . . .
H24C H 0.380471 0.869073 0.272083 0.077 Uiso 1 1 calc GR . . . .
C20 C 0.3301(3) 0.3710(3) 0.44236(10) 0.0611(7) Uani 1 1 d . . . . .
H20A H 0.396016 0.417406 0.460441 0.092 Uiso 1 1 calc GR . . . .
H20B H 0.387296 0.287352 0.434291 0.092 Uiso 1 1 calc GR . . . .
H20C H 0.243226 0.357391 0.471383 0.092 Uiso 1 1 calc GR . . . .
C8 C 0.0119(3) 0.4322(2) 0.19528(11) 0.0558(7) Uani 1 1 d . . . . .
H8A H -0.021153 0.504020 0.218853 0.084 Uiso 1 1 calc GR . . . .
H8B H 0.024109 0.350635 0.223868 0.084 Uiso 1 1 calc GR . . . .
H8C H -0.064382 0.432027 0.165777 0.084 Uiso 1 1 calc GR . . . .
C29 C 0.6746(3) 0.5941(3) 0.38145(11) 0.0656(8) Uani 1 1 d . . . . .
H29A H 0.562825 0.618668 0.381554 0.079 Uiso 1 1 calc R . . . .
H29B H 0.712175 0.638444 0.411918 0.079 Uiso 1 1 calc R . . . .
C28 C 0.7401(3) 0.7639(3) 0.30787(13) 0.0642(8) Uani 1 1 d . . . . .
H28A H 0.802985 0.790361 0.336957 0.077 Uiso 1 1 calc R . . . .
H28B H 0.635301 0.811442 0.312484 0.077 Uiso 1 1 calc R . . . .
C35 C 0.6540(3) 0.4140(3) 0.08124(11) 0.0623(8) Uani 1 1 d . . . . .
H35A H 0.610646 0.374949 0.050241 0.075 Uiso 1 1 calc R . . . .
H35B H 0.765920 0.391567 0.076918 0.075 Uiso 1 1 calc R . . . .
C33 C 0.5883(3) 0.1880(2) 0.22060(15) 0.0673(8) Uani 1 1 d . . . . .
H33A H 0.477186 0.216945 0.224335 0.081 Uiso 1 1 calc R . . . .
H33B H 0.609094 0.092766 0.230302 0.081 Uiso 1 1 calc R . . . .
C21 C 0.1684(3) 0.3820(3) 0.35333(14) 0.0671(8) Uani 1 1 d . . . . .
H21A H 0.079534 0.372374 0.381771 0.101 Uiso 1 1 calc GR . . . .
H21B H 0.221961 0.296580 0.346110 0.101 Uiso 1 1 calc GR . . . .
H21C H 0.135754 0.432856 0.313820 0.101 Uiso 1 1 calc GR . . . .
C32 C 0.6179(3) 0.1992(3) 0.32539(14) 0.0718(9) Uani 1 1 d . . . . .
H32A H 0.643336 0.103996 0.334377 0.086 Uiso 1 1 calc R . . . .
H32B H 0.507175 0.224520 0.333205 0.086 Uiso 1 1 calc R . . . .
C30 C 0.7171(3) 0.4536(3) 0.39794(11) 0.0706(9) Uani 1 1 d . . . . .
H30A H 0.828943 0.428976 0.395688 0.085 Uiso 1 1 calc R . . . .
H30B H 0.678897 0.426047 0.440893 0.085 Uiso 1 1 calc R . . . .
C34 C 0.6471(3) 0.2298(3) 0.15667(14) 0.0689(8) Uani 1 1 d . . . . .
H34A H 0.759187 0.207468 0.153812 0.083 Uiso 1 1 calc R . . . .
H34B H 0.606360 0.185236 0.127114 0.083 Uiso 1 1 calc R . . . .
C31 C 0.6995(3) 0.2572(3) 0.36604(13) 0.0732(9) Uani 1 1 d . . . . .
H31A H 0.676832 0.222824 0.410000 0.088 Uiso 1 1 calc R . . . .
H31B H 0.810230 0.235474 0.356898 0.088 Uiso 1 1 calc R . . . .
C37 C 0.2448(10) 1.0022(11) 0.4859(5) 0.067(3) Uani 0.5 1 d D U P A -1
H37A H 0.235139 0.922870 0.470525 0.101 Uiso 0.5 1 calc GR . P A -1
H37B H 0.204080 1.077071 0.456164 0.101 Uiso 0.5 1 calc GR . P A -1
H37C H 0.187995 1.005702 0.526031 0.101 Uiso 0.5 1 calc GR . P A -1
C38 C 0.4078(6) 1.0036(4) 0.4936(2) 0.0435(11) Uani 0.5 1 d D U P A -1
C43 C 0.5166(10) 0.9357(15) 0.4577(7) 0.046(2) Uani 0.5 1 d D U P A -1
H43 H 0.487614 0.888464 0.428720 0.055 Uiso 0.5 1 calc R . P A -1
C42 C 0.6678(6) 0.9367(5) 0.4642(2) 0.0518(12) Uani 0.5 1 d D U P A -1
H42 H 0.743909 0.890838 0.439389 0.062 Uiso 0.5 1 calc R . P A -1
C41 C 0.7070(11) 1.0041(10) 0.5064(5) 0.064(2) Uani 0.5 1 d D U P A -1
H41 H 0.811509 1.002513 0.511270 0.077 Uiso 0.5 1 calc R . P A -1
C40 C 0.6016(8) 1.0738(5) 0.5421(2) 0.0622(14) Uani 0.5 1 d D U P A -1
H40 H 0.630714 1.122816 0.570243 0.075 Uiso 0.5 1 calc R . P A -1
C39 C 0.4504(12) 1.0700(15) 0.5354(7) 0.051(2) Uani 0.5 1 d D U P A -1
H39 H 0.374601 1.114790 0.560706 0.061 Uiso 0.5 1 calc R . P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
K1 O1 2.8435(14) . ?
K1 N2 3.4002(14) . ?
K1 N3 2.8667(14) . ?
K1 N1 2.9270(14) . ?
K1 O4 2.8898(15) . ?
K1 O3 2.8803(16) . ?
K1 O2 2.8197(15) . ?
K1 O6 2.9027(16) . ?
K1 O5 3.0395(17) . ?
O1 C25 1.409(3) . ?
O1 C36 1.421(3) . ?
N2 N3 1.3147(18) . ?
N2 N1 1.3006(19) . ?
N3 C13 1.413(2) . ?
N1 C1 1.426(2) . ?
O4 C30 1.427(3) . ?
O4 C31 1.408(3) . ?
O3 C29 1.416(3) . ?
O3 C28 1.410(3) . ?
O2 C27 1.414(3) . ?
O2 C26 1.412(3) . ?
O6 C35 1.412(3) . ?
O6 C34 1.423(3) . ?
O5 C33 1.405(3) . ?
O5 C32 1.421(3) . ?
C1 C2 1.402(3) . ?
C1 C6 1.408(2) . ?
C2 C3 1.390(2) . ?
C2 C7 1.514(3) . ?
C13 C18 1.405(3) . ?
C13 C14 1.412(3) . ?
C6 C5 1.389(2) . ?
C6 C10 1.509(3) . ?
C5 C4 1.374(3) . ?
C18 C22 1.515(3) . ?
C18 C17 1.392(3) . ?
C14 C19 1.508(3) . ?
C14 C15 1.388(3) . ?
C4 C3 1.377(3) . ?
C10 C11 1.530(3) . ?
C10 C12 1.531(3) . ?
C7 C9 1.518(3) . ?
C7 C8 1.528(3) . ?
C22 C23 1.526(3) . ?
C22 C24 1.520(3) . ?
C19 C20 1.526(3) . ?
C19 C21 1.515(3) . ?
C17 C16 1.380(3) . ?
C15 C16 1.365(3) . ?
C25 C26 1.490(3) . ?
C36 C35 1.477(4) . ?
C27 C28 1.470(3) . ?
C29 C30 1.469(4) . ?
C33 C34 1.481(4) . ?
C32 C31 1.470(4) . ?
C37 C38 1.490(9) . ?
C38 C43 1.376(10) . ?
C38 C39 1.361(10) . ?
C43 C42 1.379(8) . ?
C42 C41 1.362(9) . ?
C41 C40 1.367(10) . ?
C40 C39 1.386(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 K1 N2 101.57(4) . . ?
O1 K1 N3 120.99(4) . . ?
O1 K1 N1 80.40(4) . . ?
O1 K1 O4 147.26(4) . . ?
O1 K1 O3 111.49(5) . . ?
O1 K1 O6 58.46(5) . . ?
O1 K1 O5 107.38(5) . . ?
N3 K1 N2 22.19(3) . . ?
N3 K1 N1 44.16(4) . . ?
N3 K1 O4 91.21(4) . . ?
N3 K1 O3 91.93(4) . . ?
N3 K1 O6 120.91(4) . . ?
N3 K1 O5 117.19(4) . . ?
N1 K1 N2 22.14(3) . . ?
N1 K1 O5 121.52(4) . . ?
O4 K1 N2 111.17(4) . . ?
O4 K1 N1 132.07(4) . . ?
O4 K1 O6 112.06(5) . . ?
O4 K1 O5 55.93(5) . . ?
O3 K1 N2 110.57(4) . . ?
O3 K1 N1 125.32(5) . . ?
O3 K1 O4 57.18(5) . . ?
O3 K1 O6 146.66(4) . . ?
O3 K1 O5 105.86(5) . . ?
O2 K1 O1 60.22(5) . . ?
O2 K1 N2 95.55(4) . . ?
O2 K1 N3 95.96(4) . . ?
O2 K1 N1 90.65(4) . . ?
O2 K1 O4 114.84(5) . . ?
O2 K1 O3 57.91(5) . . ?
O2 K1 O6 118.24(5) . . ?
O2 K1 O5 144.51(4) . . ?
O6 K1 N2 102.73(4) . . ?
O6 K1 N1 86.20(4) . . ?
O6 K1 O5 56.16(5) . . ?
O5 K1 N2 119.92(4) . . ?
C25 O1 K1 104.98(12) . . ?
C25 O1 C36 112.24(18) . . ?
C36 O1 K1 108.57(12) . . ?
N3 N2 K1 55.43(8) . . ?
N1 N2 K1 58.01(8) . . ?
N1 N2 N3 112.80(13) . . ?
N2 N3 K1 102.38(9) . . ?
N2 N3 C13 111.87(13) . . ?
C13 N3 K1 145.65(10) . . ?
N2 N1 K1 99.85(9) . . ?
N2 N1 C1 111.81(12) . . ?
C1 N1 K1 144.88(10) . . ?
C30 O4 K1 118.48(15) . . ?
C31 O4 K1 122.61(15) . . ?
C31 O4 C30 111.8(2) . . ?
C29 O3 K1 107.24(13) . . ?
C28 O3 K1 113.37(14) . . ?
C28 O3 C29 112.1(2) . . ?
C27 O2 K1 119.17(13) . . ?
C26 O2 K1 116.11(13) . . ?
C26 O2 C27 112.15(16) . . ?
C35 O6 K1 116.43(14) . . ?
C35 O6 C34 112.6(2) . . ?
C34 O6 K1 121.26(14) . . ?
C33 O5 K1 109.09(13) . . ?
C33 O5 C32 112.8(2) . . ?
C32 O5 K1 109.78(14) . . ?
C2 C1 N1 119.47(15) . . ?
C2 C1 C6 119.55(16) . . ?
C6 C1 N1 120.75(15) . . ?
C1 C2 C7 121.02(16) . . ?
C3 C2 C1 119.18(17) . . ?
C3 C2 C7 119.75(17) . . ?
C18 C13 N3 122.58(16) . . ?
C18 C13 C14 119.81(16) . . ?
C14 C13 N3 117.39(16) . . ?
C1 C6 C10 121.63(16) . . ?
C5 C6 C1 119.01(17) . . ?
C5 C6 C10 119.19(16) . . ?
C4 C5 C6 121.60(18) . . ?
C13 C18 C22 120.68(16) . . ?
C17 C18 C13 118.74(18) . . ?
C17 C18 C22 120.54(19) . . ?
C13 C14 C19 119.86(16) . . ?
C15 C14 C13 118.91(19) . . ?
C15 C14 C19 121.19(18) . . ?
C5 C4 C3 119.23(17) . . ?
C6 C10 C11 109.83(15) . . ?
C6 C10 C12 113.08(17) . . ?
C11 C10 C12 109.51(17) . . ?
C4 C3 C2 121.42(19) . . ?
C2 C7 C9 112.34(18) . . ?
C2 C7 C8 109.98(16) . . ?
C9 C7 C8 111.59(18) . . ?
C18 C22 C23 114.29(17) . . ?
C18 C22 C24 111.04(16) . . ?
C24 C22 C23 110.24(19) . . ?
C14 C19 C20 113.56(19) . . ?
C14 C19 C21 111.03(17) . . ?
C21 C19 C20 110.6(2) . . ?
C16 C17 C18 121.2(2) . . ?
C16 C15 C14 121.4(2) . . ?
C15 C16 C17 119.9(2) . . ?
O1 C25 C26 108.76(18) . . ?
O1 C36 C35 108.34(19) . . ?
O2 C27 C28 108.62(17) . . ?
O2 C26 C25 108.89(17) . . ?
O3 C29 C30 107.8(2) . . ?
O3 C28 C27 108.6(2) . . ?
O6 C35 C36 109.24(19) . . ?
O5 C33 C34 109.0(2) . . ?
O5 C32 C31 109.6(2) . . ?
O4 C30 C29 108.98(19) . . ?
O6 C34 C33 108.7(2) . . ?
O4 C31 C32 108.8(2) . . ?
C43 C38 C37 119.0(7) . . ?
C39 C38 C37 121.2(7) . . ?
C39 C38 C43 119.8(6) . . ?
C38 C43 C42 119.5(8) . . ?
C41 C42 C43 119.3(8) . . ?
C42 C41 C40 122.5(7) . . ?
C41 C40 C39 117.2(8) . . ?
C38 C39 C40 121.6(9) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_7(DME)2
_database_code_depnum_ccdc_archive 'CCDC 1971999'
loop_
_audit_author_name
_audit_author_address
'Alasdair McKay'
;Monash University
Australia
;
_audit_update_record             
;
2019-12-14 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_audit_creation_date             2019-04-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
''
alasdair.mckay@monash.edu
_chemical_name_common            '[K(DME)2(N3Dipp2)]'
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H54 K N3 O4'
_chemical_formula_sum            'C32 H54 K N3 O4'
_chemical_formula_weight         583.88
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.2751(5)
_cell_length_b                   15.4085(5)
_cell_length_c                   16.3889(6)
_cell_angle_alpha                90
_cell_angle_beta                 108.5830(10)
_cell_angle_gamma                90
_cell_volume                     3416.9(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9248
_cell_measurement_temperature    150
_cell_measurement_theta_max      24.808
_cell_measurement_theta_min      2.289
_shelx_estimated_absorpt_T_max   0.927
_shelx_estimated_absorpt_T_min   0.927
_exptl_absorpt_coefficient_mu    0.192
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.0742 before and 0.0521 after correction. The Ratio of minimum to maximum transmission is 0.9317. The λ/2 correction factor is 0.00150.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.135
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            41517
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.021
_diffrn_reflns_theta_min         2.644
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5083
_reflns_number_total             6705
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         6705
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0422
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0416P)²+1.6294P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1088
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C13(H13), C10(H10), C25(H25), C22(H22)
2.b Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C30(H30A,H30B), C33(H33A,H33B), C29(H29A,H29B)
2.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C7(H7), C6(H6), C20(H20), C18(H18), C19(H19)
2.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C11(H11A,H11B,H11C), C14(H14A,H14B,H14C), C12(H12A,H12B,
 H12C), C31(H31A,H31B,H31C), C28(H28A,H28B,H28C), C23(H23A,H23B,H23C), C35(H35A,
 H35B,H35C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C32(H32A,H32B,H32C),
 C24(H24A,H24B,H24C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.45443(3) 0.95576(3) 0.24534(3) 0.02843(12) Uani 1 1 d . . . . .
N3 N 0.62535(11) 0.85789(9) 0.30193(9) 0.0250(3) Uani 1 1 d . . . . .
N1 N 0.52026(10) 0.82045(9) 0.36716(9) 0.0229(3) Uani 1 1 d . . . . .
O2 O 0.31689(10) 0.90034(9) 0.09467(9) 0.0386(3) Uani 1 1 d . . . . .
N2 N 0.60736(10) 0.80618(9) 0.35796(9) 0.0219(3) Uani 1 1 d . . . . .
O1 O 0.25888(10) 0.90559(9) 0.24267(9) 0.0366(3) Uani 1 1 d . . . . .
O4 O 0.58886(9) 1.08785(8) 0.22764(8) 0.0335(3) Uani 1 1 d . . . . .
O3 O 0.38735(10) 1.10403(9) 0.14871(10) 0.0409(4) Uani 1 1 d . . . . .
C4 C 0.49824(12) 0.75591(11) 0.41993(11) 0.0205(4) Uani 1 1 d . . . . .
C5 C 0.48529(12) 0.66838(11) 0.39372(11) 0.0225(4) Uani 1 1 d . . . . .
C9 C 0.48237(12) 0.78205(11) 0.49694(11) 0.0222(4) Uani 1 1 d . . . . .
C13 C 0.49326(14) 0.87649(11) 0.52415(12) 0.0278(4) Uani 1 1 d . . . . .
H13 H 0.486983 0.912052 0.471633 0.033 Uiso 1 1 calc R . . . .
C8 C 0.46045(13) 0.71935(11) 0.54917(12) 0.0259(4) Uani 1 1 d . . . . .
H8 H 0.450720 0.736385 0.601600 0.031 Uiso 1 1 calc R . . . .
C7 C 0.45257(13) 0.63282(12) 0.52617(12) 0.0284(4) Uani 1 1 d . . . . .
H7 H 0.439349 0.590520 0.563239 0.034 Uiso 1 1 calc R . . . .
C10 C 0.49225(14) 0.63923(12) 0.30683(12) 0.0280(4) Uani 1 1 d . . . . .
H10 H 0.485156 0.692225 0.270122 0.034 Uiso 1 1 calc R . . . .
C16 C 0.72230(13) 0.85035(11) 0.29692(12) 0.0245(4) Uani 1 1 d . . . . .
C6 C 0.46407(13) 0.60816(11) 0.44884(12) 0.0259(4) Uani 1 1 d . . . . .
H6 H 0.457332 0.548659 0.432834 0.031 Uiso 1 1 calc R . . . .
C20 C 0.89611(15) 0.88248(13) 0.34763(15) 0.0380(5) Uani 1 1 d . . . . .
H20 H 0.953764 0.899391 0.392646 0.046 Uiso 1 1 calc R . . . .
C21 C 0.80680(13) 0.87558(11) 0.36441(12) 0.0282(4) Uani 1 1 d . . . . .
C34 C 0.54982(15) 1.14419(13) 0.15715(12) 0.0344(5) Uani 1 1 d . . . . .
H34A H 0.542932 1.113112 0.102679 0.041 Uiso 1 1 calc R . . . .
H34B H 0.594962 1.193989 0.161440 0.041 Uiso 1 1 calc R . . . .
C30 C 0.22264(16) 0.87182(15) 0.09512(14) 0.0452(5) Uani 1 1 d . . . . .
H30A H 0.197654 0.825890 0.051323 0.054 Uiso 1 1 calc R . . . .
H30B H 0.175290 0.920792 0.081048 0.054 Uiso 1 1 calc R . . . .
C17 C 0.73028(14) 0.82811(12) 0.21584(12) 0.0306(4) Uani 1 1 d . . . . .
C25 C 0.80138(15) 0.89639(13) 0.45333(13) 0.0347(5) Uani 1 1 d . . . . .
H25 H 0.730148 0.906732 0.446591 0.042 Uiso 1 1 calc R . . . .
C15 C 0.41349(16) 0.90708(13) 0.56127(13) 0.0373(5) Uani 1 1 d . . . . .
H15A H 0.348209 0.892052 0.521445 0.056 Uiso 1 1 calc GR . . . .
H15B H 0.418129 0.970135 0.569372 0.056 Uiso 1 1 calc GR . . . .
H15C H 0.422926 0.878690 0.616830 0.056 Uiso 1 1 calc GR . . . .
C11 C 0.59169(15) 0.59936(14) 0.31496(14) 0.0408(5) Uani 1 1 d . . . . .
H11A H 0.644144 0.641215 0.341835 0.061 Uiso 1 1 calc GR . . . .
H11B H 0.594205 0.584026 0.257659 0.061 Uiso 1 1 calc GR . . . .
H11C H 0.601123 0.547019 0.350638 0.061 Uiso 1 1 calc GR . . . .
C18 C 0.82066(17) 0.83743(13) 0.20238(14) 0.0408(5) Uani 1 1 d . . . . .
H18 H 0.826068 0.824331 0.147413 0.049 Uiso 1 1 calc R . . . .
C22 C 0.63948(16) 0.79713(13) 0.14423(12) 0.0376(5) Uani 1 1 d . . . . .
H22 H 0.594609 0.768446 0.172072 0.045 Uiso 1 1 calc R . . . .
C33 C 0.45144(15) 1.17573(13) 0.15770(14) 0.0371(5) Uani 1 1 d . . . . .
H33A H 0.458261 1.206293 0.212428 0.044 Uiso 1 1 calc R . . . .
H33B H 0.423985 1.216988 0.109706 0.044 Uiso 1 1 calc R . . . .
C19 C 0.90278(16) 0.86531(14) 0.26706(16) 0.0447(6) Uani 1 1 d . . . . .
H19 H 0.963868 0.872709 0.256310 0.054 Uiso 1 1 calc R . . . .
C29 C 0.23192(16) 0.83721(14) 0.18242(14) 0.0440(5) Uani 1 1 d . . . . .
H29A H 0.168194 0.811867 0.182433 0.053 Uiso 1 1 calc R . . . .
H29B H 0.282771 0.791053 0.198168 0.053 Uiso 1 1 calc R . . . .
C14 C 0.59604(16) 0.89307(14) 0.58792(15) 0.0426(5) Uani 1 1 d . . . . .
H14A H 0.603985 0.860022 0.640789 0.064 Uiso 1 1 calc GR . . . .
H14B H 0.603829 0.955123 0.601498 0.064 Uiso 1 1 calc GR . . . .
H14C H 0.646253 0.874699 0.562373 0.064 Uiso 1 1 calc GR . . . .
C12 C 0.40942(17) 0.57653(15) 0.25955(14) 0.0457(6) Uani 1 1 d . . . . .
H12A H 0.415253 0.562411 0.203068 0.068 Uiso 1 1 calc GR . . . .
H12B H 0.345193 0.603831 0.251978 0.068 Uiso 1 1 calc GR . . . .
H12C H 0.414828 0.523230 0.293382 0.068 Uiso 1 1 calc GR . . . .
C31 C 0.31283(19) 0.93642(16) 0.01408(14) 0.0513(6) Uani 1 1 d . . . . .
H31A H 0.294377 0.891198 -0.030233 0.077 Uiso 1 1 calc GR . . . .
H31B H 0.377767 0.960002 0.017622 0.077 Uiso 1 1 calc GR . . . .
H31C H 0.263544 0.983002 -0.000881 0.077 Uiso 1 1 calc GR . . . .
C28 C 0.25337(17) 0.88114(15) 0.32402(15) 0.0464(6) Uani 1 1 d . . . . .
H28A H 0.186080 0.861806 0.317961 0.070 Uiso 1 1 calc GR . . . .
H28B H 0.270275 0.930946 0.363185 0.070 Uiso 1 1 calc GR . . . .
H28C H 0.299909 0.833698 0.347392 0.070 Uiso 1 1 calc GR . . . .
C23 C 0.58334(18) 0.87237(15) 0.09162(14) 0.0477(6) Uani 1 1 d . . . . .
H23A H 0.569290 0.915538 0.130078 0.072 Uiso 1 1 calc GR . . . .
H23B H 0.521067 0.851282 0.051115 0.072 Uiso 1 1 calc GR . . . .
H23C H 0.623301 0.899026 0.059597 0.072 Uiso 1 1 calc GR . . . .
C35 C 0.68930(15) 1.06863(14) 0.23984(15) 0.0427(5) Uani 1 1 d . . . . .
H35A H 0.694641 1.036217 0.190063 0.064 Uiso 1 1 calc GR . . . .
H35B H 0.715973 1.033563 0.291998 0.064 Uiso 1 1 calc GR . . . .
H35C H 0.726861 1.122813 0.245898 0.064 Uiso 1 1 calc GR . . . .
C26 C 0.8567(2) 0.97774(15) 0.49291(16) 0.0577(7) Uani 1 1 d . . . . .
H26A H 0.840353 0.992870 0.544860 0.087 Uiso 1 1 calc GR . . . .
H26B H 0.837607 1.025528 0.451432 0.087 Uiso 1 1 calc GR . . . .
H26C H 0.927963 0.967519 0.508064 0.087 Uiso 1 1 calc GR . . . .
C27 C 0.8338(2) 0.82009(16) 0.51270(16) 0.0641(7) Uani 1 1 d . . . . .
H27A H 0.796463 0.768476 0.485874 0.096 Uiso 1 1 calc GR . . . .
H27B H 0.821564 0.832177 0.567129 0.096 Uiso 1 1 calc GR . . . .
H27C H 0.904533 0.809821 0.523820 0.096 Uiso 1 1 calc GR . . . .
C32 C 0.28947(16) 1.12908(16) 0.14087(17) 0.0521(6) Uani 1 1 d . . . . .
H32A H 0.289664 1.163484 0.191219 0.078 Uiso 1 1 calc GR . . . .
H32B H 0.248702 1.077173 0.137347 0.078 Uiso 1 1 calc GR . . . .
H32C H 0.262285 1.163934 0.088625 0.078 Uiso 1 1 calc GR . . . .
C24 C 0.6630(2) 0.73036(17) 0.08430(16) 0.0700(8) Uani 1 1 d . . . . .
H24A H 0.699540 0.758577 0.050168 0.105 Uiso 1 1 calc GR . . . .
H24B H 0.601238 0.706180 0.045716 0.105 Uiso 1 1 calc GR . . . .
H24C H 0.703223 0.683589 0.118682 0.105 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
K1 N3 2.7650(15) . ?
K1 N1 2.8320(14) . ?
K1 O2 2.7553(14) . ?
K1 N2 3.3041(15) . ?
K1 O1 2.8833(14) . ?
K1 O4 2.8747(13) . ?
K1 O3 2.7709(14) . ?
N3 N2 1.3017(19) . ?
N3 C16 1.417(2) . ?
N1 N2 1.3177(19) . ?
N1 C4 1.417(2) . ?
O2 C30 1.418(2) . ?
O2 C31 1.417(2) . ?
O1 C29 1.411(2) . ?
O1 C28 1.412(2) . ?
O4 C34 1.410(2) . ?
O4 C35 1.414(2) . ?
O3 C33 1.412(2) . ?
O3 C32 1.415(2) . ?
C4 C5 1.410(2) . ?
C4 C9 1.410(2) . ?
C5 C10 1.526(2) . ?
C5 C6 1.394(2) . ?
C9 C13 1.515(2) . ?
C9 C8 1.391(2) . ?
C13 C15 1.527(3) . ?
C13 C14 1.527(3) . ?
C8 C7 1.380(3) . ?
C7 C6 1.382(3) . ?
C10 C11 1.513(3) . ?
C10 C12 1.532(3) . ?
C16 C21 1.407(3) . ?
C16 C17 1.411(3) . ?
C20 C21 1.391(3) . ?
C20 C19 1.379(3) . ?
C21 C25 1.518(3) . ?
C34 C33 1.489(3) . ?
C30 C29 1.493(3) . ?
C17 C18 1.384(3) . ?
C17 C22 1.522(3) . ?
C25 C26 1.513(3) . ?
C25 C27 1.502(3) . ?
C18 C19 1.375(3) . ?
C22 C23 1.513(3) . ?
C22 C24 1.532(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 K1 N1 45.81(4) . . ?
N3 K1 N2 22.61(4) . . ?
N3 K1 O1 127.26(4) . . ?
N3 K1 O4 82.75(4) . . ?
N3 K1 O3 138.47(4) . . ?
N1 K1 N2 23.20(4) . . ?
N1 K1 O1 85.15(4) . . ?
N1 K1 O4 120.67(4) . . ?
O2 K1 N3 115.61(5) . . ?
O2 K1 N1 112.66(4) . . ?
O2 K1 N2 116.08(4) . . ?
O2 K1 O1 59.56(4) . . ?
O2 K1 O4 115.91(4) . . ?
O2 K1 O3 74.07(4) . . ?
O1 K1 N2 106.59(4) . . ?
O4 K1 N2 101.93(4) . . ?
O4 K1 O1 149.60(4) . . ?
O3 K1 N1 170.59(4) . . ?
O3 K1 N2 160.20(4) . . ?
O3 K1 O1 93.20(4) . . ?
O3 K1 O4 58.59(4) . . ?
N2 N3 K1 102.66(10) . . ?
N2 N3 C16 113.99(14) . . ?
C16 N3 K1 143.04(11) . . ?
N2 N1 K1 98.94(9) . . ?
N2 N1 C4 110.70(13) . . ?
C4 N1 K1 149.14(10) . . ?
C30 O2 K1 119.86(12) . . ?
C31 O2 K1 121.30(13) . . ?
C31 O2 C30 111.68(17) . . ?
N3 N2 K1 54.74(8) . . ?
N3 N2 N1 112.58(14) . . ?
N1 N2 K1 57.85(8) . . ?
C29 O1 K1 104.93(11) . . ?
C29 O1 C28 112.13(16) . . ?
C28 O1 K1 113.73(12) . . ?
C34 O4 K1 114.60(11) . . ?
C34 O4 C35 111.28(15) . . ?
C35 O4 K1 121.12(11) . . ?
C33 O3 K1 119.41(11) . . ?
C33 O3 C32 112.60(16) . . ?
C32 O3 K1 115.34(12) . . ?
C5 C4 N1 121.22(15) . . ?
C5 C4 C9 120.21(15) . . ?
C9 C4 N1 118.41(15) . . ?
C4 C5 C10 121.64(15) . . ?
C6 C5 C4 118.29(16) . . ?
C6 C5 C10 120.06(15) . . ?
C4 C9 C13 120.46(15) . . ?
C8 C9 C4 118.97(16) . . ?
C8 C9 C13 120.52(15) . . ?
C9 C13 C15 113.22(15) . . ?
C9 C13 C14 110.37(15) . . ?
C15 C13 C14 110.58(16) . . ?
C7 C8 C9 121.16(16) . . ?
C8 C7 C6 119.52(16) . . ?
C5 C10 C12 112.83(15) . . ?
C11 C10 C5 112.06(16) . . ?
C11 C10 C12 109.85(17) . . ?
C21 C16 N3 122.70(15) . . ?
C21 C16 C17 120.07(16) . . ?
C17 C16 N3 116.60(16) . . ?
C7 C6 C5 121.67(16) . . ?
C19 C20 C21 121.4(2) . . ?
C16 C21 C25 121.33(16) . . ?
C20 C21 C16 118.41(18) . . ?
C20 C21 C25 120.25(18) . . ?
O4 C34 C33 108.86(15) . . ?
O2 C30 C29 108.74(17) . . ?
C16 C17 C22 119.85(16) . . ?
C18 C17 C16 118.93(19) . . ?
C18 C17 C22 121.19(18) . . ?
C26 C25 C21 114.04(17) . . ?
C27 C25 C21 110.92(17) . . ?
C27 C25 C26 111.1(2) . . ?
C19 C18 C17 121.24(19) . . ?
C17 C22 C24 113.48(19) . . ?
C23 C22 C17 111.44(17) . . ?
C23 C22 C24 109.50(18) . . ?
O3 C33 C34 108.98(16) . . ?
C18 C19 C20 119.74(19) . . ?
O1 C29 C30 108.97(17) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_6(15c5)
_database_code_depnum_ccdc_archive 'CCDC 1971997'
loop_
_audit_author_name
_audit_author_address
'Alasdair McKay'
;Monash University
Australia
;
_audit_update_record             
;
2019-12-14 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_audit_creation_date             2019-04-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
''
alasdair.mckay@monash.edu
_chemical_name_common            ?
_chemical_name_systematic        '[Na(N3Dipp2)(15-crown-5)]'
_chemical_formula_moiety         'C34 H54 N3 Na O5, C7 H8'
_chemical_formula_sum            'C41 H62 N3 Na O5'
_chemical_formula_weight         699.92
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.0109(15)
_cell_length_b                   16.0444(13)
_cell_length_c                   18.2255(18)
_cell_angle_alpha                90
_cell_angle_beta                 86.298(4)
_cell_angle_gamma                90
_cell_volume                     4088.5(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1346
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      19.456
_cell_measurement_theta_min      2.886
_shelx_estimated_absorpt_T_max   0.996
_shelx_estimated_absorpt_T_min   0.988
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6115
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1267 before and 0.0735 after correction. The Ratio of minimum to maximum transmission is 0.8196. The λ/2 correction factor is 0.00150.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1501
_diffrn_reflns_av_unetI/netI     0.1981
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33867
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         2.185
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3645
_reflns_number_total             9014
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         9014
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2016
_refine_ls_R_factor_gt           0.0703
_refine_ls_restrained_S_all      0.960
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0545P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1380
_refine_ls_wR_factor_ref         0.1868
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C22(H22), C19(H19), C10(H10), C7(H7)
2.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C27(H27A,H27B), C34(H34A,
 H34B), C32(H32A,H32B), C33(H33A,H33B), C31(H31A,H31B), C26(H26A,H26B),
 C25(H25A,H25B)
2.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C17(H17), C16(H16), C4(H4), C5(H5), C3(H3), C41(H41), C37(H37),
 C39(H39), C38(H38), C40(H40)
2.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C21(H21A,H21B,H21C), C24(H24A,H24B,H24C), C9(H9A,H9B,
 H9C), C11(H11A,H11B,H11C), C8(H8A,H8B,H8C), C20(H20A,H20B,H20C), C12(H12A,H12B,
 H12C), C35(H35A,H35B,H35C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Na1 Na 0.57109(10) 0.54150(6) 0.75412(6) 0.0262(3) Uani 1 1 d . . . . .
O3 O 0.52361(19) 0.62441(13) 0.86846(11) 0.0352(7) Uani 1 1 d . . . . .
O5 O 0.62712(19) 0.63178(12) 0.65488(12) 0.0362(7) Uani 1 1 d . . . . .
O2 O 0.40819(18) 0.52176(14) 0.80057(13) 0.0385(7) Uani 1 1 d . . . . .
N2 N 0.62341(19) 0.36192(14) 0.74666(13) 0.0212(7) Uani 1 1 d . . . . .
O4 O 0.69960(19) 0.63714(13) 0.79334(12) 0.0363(7) Uani 1 1 d . . . . .
O1 O 0.4394(2) 0.58121(14) 0.66263(13) 0.0432(7) Uani 1 1 d . . . . .
N3 N 0.61215(19) 0.40544(14) 0.80761(13) 0.0217(7) Uani 1 1 d . . . . .
N1 N 0.6063(2) 0.40658(14) 0.68862(13) 0.0215(7) Uani 1 1 d . . . . .
C1 C 0.6245(3) 0.35963(17) 0.62232(16) 0.0221(8) Uani 1 1 d . . . . .
C14 C 0.7111(2) 0.38983(17) 0.91101(16) 0.0208(8) Uani 1 1 d . . . . .
C18 C 0.5820(2) 0.28891(18) 0.89679(16) 0.0237(8) Uani 1 1 d . . . . .
C13 C 0.6351(2) 0.35897(18) 0.87100(15) 0.0210(8) Uani 1 1 d . . . . .
C22 C 0.4971(3) 0.25766(18) 0.85738(18) 0.0277(9) Uani 1 1 d . . . . .
H22 H 0.516970 0.256599 0.803682 0.033 Uiso 1 1 calc R . . . .
C15 C 0.7350(3) 0.34840(19) 0.97392(16) 0.0263(8) Uani 1 1 d . . . . .
H15 H 0.786710 0.368218 1.000274 0.032 Uiso 1 1 calc R . . . .
C2 C 0.5676(3) 0.29061(18) 0.60453(17) 0.0250(8) Uani 1 1 d . . . . .
C17 C 0.6093(3) 0.25035(19) 0.96115(16) 0.0269(8) Uani 1 1 d . . . . .
H17 H 0.574519 0.203030 0.979318 0.032 Uiso 1 1 calc R . . . .
C19 C 0.7678(3) 0.46425(18) 0.88166(17) 0.0256(8) Uani 1 1 d . . . . .
H19 H 0.722211 0.502435 0.858323 0.031 Uiso 1 1 calc R . . . .
C6 C 0.6983(3) 0.38696(18) 0.57219(16) 0.0240(8) Uani 1 1 d . . . . .
C16 C 0.6849(3) 0.27882(19) 0.99899(17) 0.0290(9) Uani 1 1 d . . . . .
H16 H 0.702450 0.250744 1.041996 0.035 Uiso 1 1 calc R . . . .
C10 C 0.7586(3) 0.46274(19) 0.58698(17) 0.0292(9) Uani 1 1 d . . . . .
H10 H 0.726043 0.493569 0.629209 0.035 Uiso 1 1 calc R . . . .
C7 C 0.4796(3) 0.26481(19) 0.65212(18) 0.0314(9) Uani 1 1 d . . . . .
H7 H 0.475958 0.300588 0.697138 0.038 Uiso 1 1 calc R . . . .
C4 C 0.6670(3) 0.2703(2) 0.49290(18) 0.0346(10) Uani 1 1 d . . . . .
H4 H 0.683837 0.237945 0.450332 0.042 Uiso 1 1 calc R . . . .
C36 C 0.3970(3) 0.8993(2) 0.69921(19) 0.0357(9) Uani 1 1 d . . . . .
C28 C 0.4680(3) 0.5670(2) 0.91178(19) 0.0397(10) Uani 1 1 d . . . . .
H28A H 0.451224 0.590631 0.961109 0.048 Uiso 1 1 calc R . . . .
H28B H 0.504052 0.514633 0.917736 0.048 Uiso 1 1 calc R . . . .
C5 C 0.7190(3) 0.34119(19) 0.50782(17) 0.0307(9) Uani 1 1 d . . . . .
H5 H 0.769289 0.358876 0.473900 0.037 Uiso 1 1 calc R . . . .
C3 C 0.5914(3) 0.2471(2) 0.53976(18) 0.0338(10) Uani 1 1 d . . . . .
H3 H 0.554249 0.200042 0.527828 0.041 Uiso 1 1 calc R . . . .
C29 C 0.6050(3) 0.6563(2) 0.90299(19) 0.0419(11) Uani 1 1 d . . . . .
H29A H 0.639912 0.610154 0.925440 0.050 Uiso 1 1 calc R . . . .
H29B H 0.584269 0.696292 0.942175 0.050 Uiso 1 1 calc R . . . .
C23 C 0.4664(3) 0.1691(2) 0.87904(19) 0.0433(11) Uani 1 1 d . . . . .
H23A H 0.520631 0.131058 0.869977 0.065 Uiso 1 1 calc GR . . . .
H23B H 0.413733 0.151697 0.849692 0.065 Uiso 1 1 calc GR . . . .
H23C H 0.445261 0.167817 0.931336 0.065 Uiso 1 1 calc GR . . . .
C41 C 0.4050(3) 0.9465(2) 0.7620(2) 0.0455(11) Uani 1 1 d . . . . .
H41 H 0.403045 1.005657 0.759749 0.055 Uiso 1 1 calc R . . . .
C30 C 0.6684(3) 0.6988(2) 0.8454(2) 0.0457(11) Uani 1 1 d . . . . .
H30A H 0.632728 0.743191 0.821243 0.055 Uiso 1 1 calc R . . . .
H30B H 0.723918 0.724267 0.867769 0.055 Uiso 1 1 calc R . . . .
C21 C 0.8153(3) 0.5141(2) 0.94054(19) 0.0412(10) Uani 1 1 d . . . . .
H21A H 0.768311 0.525956 0.981364 0.062 Uiso 1 1 calc GR . . . .
H21B H 0.839933 0.566661 0.919438 0.062 Uiso 1 1 calc GR . . . .
H21C H 0.868280 0.481758 0.958662 0.062 Uiso 1 1 calc GR . . . .
C27 C 0.3792(3) 0.5504(2) 0.87248(19) 0.0451(11) Uani 1 1 d . . . . .
H27A H 0.339616 0.507601 0.899112 0.054 Uiso 1 1 calc R . . . .
H27B H 0.340951 0.602011 0.869651 0.054 Uiso 1 1 calc R . . . .
C34 C 0.4957(3) 0.5797(2) 0.59433(19) 0.0447(11) Uani 1 1 d . . . . .
H34A H 0.454555 0.587661 0.552713 0.054 Uiso 1 1 calc R . . . .
H34B H 0.529470 0.525768 0.587932 0.054 Uiso 1 1 calc R . . . .
C24 C 0.4130(3) 0.3170(2) 0.8674(2) 0.0469(11) Uani 1 1 d . . . . .
H24A H 0.390508 0.318793 0.919389 0.070 Uiso 1 1 calc GR . . . .
H24B H 0.361112 0.297601 0.838062 0.070 Uiso 1 1 calc GR . . . .
H24C H 0.432980 0.372905 0.851104 0.070 Uiso 1 1 calc GR . . . .
C9 C 0.3875(3) 0.2785(2) 0.61198(19) 0.0464(11) Uani 1 1 d . . . . .
H9A H 0.382364 0.337374 0.598609 0.070 Uiso 1 1 calc GR . . . .
H9B H 0.332016 0.262499 0.644391 0.070 Uiso 1 1 calc GR . . . .
H9C H 0.389630 0.244208 0.567388 0.070 Uiso 1 1 calc GR . . . .
C32 C 0.6840(3) 0.7007(2) 0.6736(2) 0.0459(11) Uani 1 1 d . . . . .
H32A H 0.642873 0.746157 0.694328 0.055 Uiso 1 1 calc R . . . .
H32B H 0.720710 0.721991 0.629237 0.055 Uiso 1 1 calc R . . . .
C33 C 0.5659(3) 0.6496(2) 0.59739(19) 0.0472(12) Uani 1 1 d . . . . .
H33A H 0.603829 0.654433 0.549852 0.057 Uiso 1 1 calc R . . . .
H33B H 0.531852 0.702856 0.607303 0.057 Uiso 1 1 calc R . . . .
C31 C 0.7512(3) 0.6718(2) 0.7293(2) 0.0423(10) Uani 1 1 d . . . . .
H31A H 0.794913 0.629114 0.706831 0.051 Uiso 1 1 calc R . . . .
H31B H 0.790376 0.719457 0.744304 0.051 Uiso 1 1 calc R . . . .
C26 C 0.3342(3) 0.5191(3) 0.7513(2) 0.0530(12) Uani 1 1 d . . . . .
H26A H 0.295690 0.570809 0.755467 0.064 Uiso 1 1 calc R . . . .
H26B H 0.291475 0.471102 0.763048 0.064 Uiso 1 1 calc R . . . .
C37 C 0.4020(3) 0.8143(2) 0.7044(2) 0.0494(11) Uani 1 1 d . . . . .
H37 H 0.395087 0.781538 0.661714 0.059 Uiso 1 1 calc R . . . .
C11 C 0.8567(3) 0.4367(2) 0.6098(2) 0.0480(11) Uani 1 1 d . . . . .
H11A H 0.849286 0.398436 0.651633 0.072 Uiso 1 1 calc GR . . . .
H11B H 0.892246 0.486173 0.623841 0.072 Uiso 1 1 calc GR . . . .
H11C H 0.891722 0.408771 0.568486 0.072 Uiso 1 1 calc GR . . . .
C25 C 0.3797(3) 0.5106(2) 0.6750(2) 0.0487(11) Uani 1 1 d . . . . .
H25A H 0.417910 0.458687 0.670559 0.058 Uiso 1 1 calc R . . . .
H25B H 0.330181 0.508772 0.638705 0.058 Uiso 1 1 calc R . . . .
C8 C 0.4846(3) 0.17344(19) 0.6768(2) 0.0517(12) Uani 1 1 d . . . . .
H8A H 0.483121 0.136886 0.633805 0.078 Uiso 1 1 calc GR . . . .
H8B H 0.429812 0.160978 0.711203 0.078 Uiso 1 1 calc GR . . . .
H8C H 0.544067 0.164183 0.701113 0.078 Uiso 1 1 calc GR . . . .
C20 C 0.8427(3) 0.4378(2) 0.8221(2) 0.0461(11) Uani 1 1 d . . . . .
H20A H 0.889427 0.401007 0.843360 0.069 Uiso 1 1 calc GR . . . .
H20B H 0.875338 0.487248 0.801287 0.069 Uiso 1 1 calc GR . . . .
H20C H 0.811511 0.408049 0.783204 0.069 Uiso 1 1 calc GR . . . .
C12 C 0.7682(3) 0.5222(2) 0.52204(19) 0.0513(12) Uani 1 1 d . . . . .
H12A H 0.805004 0.495374 0.481024 0.077 Uiso 1 1 calc GR . . . .
H12B H 0.801376 0.572922 0.536357 0.077 Uiso 1 1 calc GR . . . .
H12C H 0.704502 0.536821 0.506855 0.077 Uiso 1 1 calc GR . . . .
C39 C 0.4239(3) 0.8208(3) 0.8306(2) 0.0651(14) Uani 1 1 d . . . . .
H39 H 0.434583 0.793540 0.875630 0.078 Uiso 1 1 calc R . . . .
C38 C 0.4165(3) 0.7755(3) 0.7693(3) 0.0656(14) Uani 1 1 d . . . . .
H38 H 0.421416 0.716468 0.771175 0.079 Uiso 1 1 calc R . . . .
C40 C 0.4161(3) 0.9061(3) 0.8291(2) 0.0632(14) Uani 1 1 d . . . . .
H40 H 0.418243 0.937488 0.873159 0.076 Uiso 1 1 calc R . . . .
C35 C 0.3854(4) 0.9413(3) 0.6259(2) 0.0678(14) Uani 1 1 d . . . . .
H35A H 0.370206 1.000387 0.633934 0.102 Uiso 1 1 calc GR . . . .
H35B H 0.333471 0.914433 0.601257 0.102 Uiso 1 1 calc GR . . . .
H35C H 0.445118 0.936397 0.595085 0.102 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Na1 O3 2.525(2) . ?
Na1 O5 2.409(2) . ?
Na1 O2 2.403(3) . ?
Na1 N2 2.974(3) . ?
Na1 O4 2.505(3) . ?
Na1 O1 2.643(3) . ?
Na1 N3 2.474(2) . ?
Na1 N1 2.506(2) . ?
O3 C28 1.414(4) . ?
O3 C29 1.432(4) . ?
O5 C32 1.417(4) . ?
O5 C33 1.425(4) . ?
O2 C27 1.423(4) . ?
O2 C26 1.415(4) . ?
N2 N3 1.313(3) . ?
N2 N1 1.313(3) . ?
O4 C30 1.420(4) . ?
O4 C31 1.444(4) . ?
O1 C34 1.430(4) . ?
O1 C25 1.418(4) . ?
N3 C13 1.429(3) . ?
N1 C1 1.433(4) . ?
C1 C2 1.415(4) . ?
C1 C6 1.405(4) . ?
C14 C13 1.418(4) . ?
C14 C15 1.385(4) . ?
C14 C19 1.513(4) . ?
C18 C13 1.411(4) . ?
C18 C22 1.514(4) . ?
C18 C17 1.401(4) . ?
C22 H22 1.0000 . ?
C22 C23 1.529(4) . ?
C22 C24 1.517(5) . ?
C15 H15 0.9500 . ?
C15 C16 1.380(4) . ?
C2 C7 1.519(5) . ?
C2 C3 1.394(4) . ?
C17 H17 0.9500 . ?
C17 C16 1.379(4) . ?
C19 H19 1.0000 . ?
C19 C21 1.525(4) . ?
C19 C20 1.520(5) . ?
C6 C10 1.515(4) . ?
C6 C5 1.398(4) . ?
C16 H16 0.9500 . ?
C10 H10 1.0000 . ?
C10 C11 1.519(5) . ?
C10 C12 1.520(4) . ?
C7 H7 1.0000 . ?
C7 C9 1.539(5) . ?
C7 C8 1.536(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.388(4) . ?
C4 C3 1.369(5) . ?
C36 C41 1.384(5) . ?
C36 C37 1.369(5) . ?
C36 C35 1.515(5) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C27 1.498(5) . ?
C5 H5 0.9500 . ?
C3 H3 0.9500 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.495(5) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C41 H41 0.9500 . ?
C41 C40 1.401(5) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C33 1.494(5) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C31 1.501(5) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C25 1.498(5) . ?
C37 H37 0.9500 . ?
C37 C38 1.364(5) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C39 H39 0.9500 . ?
C39 C38 1.342(6) . ?
C39 C40 1.374(6) . ?
C38 H38 0.9500 . ?
C40 H40 0.9500 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Na1 N2 126.81(8) . . ?
O3 Na1 O1 103.67(9) . . ?
O5 Na1 O3 111.02(8) . . ?
O5 Na1 N2 118.74(9) . . ?
O5 Na1 O4 68.93(8) . . ?
O5 Na1 O1 65.68(9) . . ?
O5 Na1 N3 138.91(10) . . ?
O5 Na1 N1 96.73(9) . . ?
O2 Na1 O3 65.49(9) . . ?
O2 Na1 O5 126.85(9) . . ?
O2 Na1 N2 96.55(8) . . ?
O2 Na1 O4 131.61(9) . . ?
O2 Na1 O1 64.44(9) . . ?
O2 Na1 N3 89.12(9) . . ?
O2 Na1 N1 101.95(9) . . ?
O4 Na1 O3 66.28(8) . . ?
O4 Na1 N2 115.27(8) . . ?
O4 Na1 O1 125.18(8) . . ?
O4 Na1 N1 122.84(10) . . ?
O1 Na1 N2 112.62(8) . . ?
N3 Na1 O3 101.26(8) . . ?
N3 Na1 N2 25.86(7) . . ?
N3 Na1 O4 103.79(9) . . ?
N3 Na1 O1 130.61(9) . . ?
N3 Na1 N1 51.81(8) . . ?
N1 Na1 O3 151.84(9) . . ?
N1 Na1 N2 25.96(7) . . ?
N1 Na1 O1 91.80(8) . . ?
C28 O3 Na1 102.93(18) . . ?
C28 O3 C29 114.4(3) . . ?
C29 O3 Na1 112.1(2) . . ?
C32 O5 Na1 116.72(19) . . ?
C32 O5 C33 113.3(3) . . ?
C33 O5 Na1 119.3(2) . . ?
C27 O2 Na1 119.3(2) . . ?
C26 O2 Na1 119.9(2) . . ?
C26 O2 C27 114.6(3) . . ?
N3 N2 Na1 55.27(13) . . ?
N1 N2 Na1 56.68(13) . . ?
N1 N2 N3 111.9(2) . . ?
C30 O4 Na1 114.9(2) . . ?
C30 O4 C31 112.9(3) . . ?
C31 O4 Na1 109.68(18) . . ?
C34 O1 Na1 100.2(2) . . ?
C25 O1 Na1 97.8(2) . . ?
C25 O1 C34 114.3(3) . . ?
N2 N3 Na1 98.87(16) . . ?
N2 N3 C13 112.7(2) . . ?
C13 N3 Na1 148.13(18) . . ?
N2 N1 Na1 97.37(16) . . ?
N2 N1 C1 111.2(2) . . ?
C1 N1 Na1 151.03(18) . . ?
C2 C1 N1 122.2(3) . . ?
C6 C1 N1 117.9(3) . . ?
C6 C1 C2 119.8(3) . . ?
C13 C14 C19 119.3(3) . . ?
C15 C14 C13 119.2(3) . . ?
C15 C14 C19 121.4(3) . . ?
C13 C18 C22 121.3(3) . . ?
C17 C18 C13 117.7(3) . . ?
C17 C18 C22 121.1(3) . . ?
C14 C13 N3 116.7(3) . . ?
C18 C13 N3 122.9(3) . . ?
C18 C13 C14 120.2(3) . . ?
C18 C22 H22 107.0 . . ?
C18 C22 C23 113.7(3) . . ?
C18 C22 C24 111.3(3) . . ?
C23 C22 H22 107.0 . . ?
C24 C22 H22 107.0 . . ?
C24 C22 C23 110.4(3) . . ?
C14 C15 H15 119.4 . . ?
C16 C15 C14 121.2(3) . . ?
C16 C15 H15 119.4 . . ?
C1 C2 C7 122.1(3) . . ?
C3 C2 C1 118.6(3) . . ?
C3 C2 C7 119.2(3) . . ?
C18 C17 H17 118.9 . . ?
C16 C17 C18 122.2(3) . . ?
C16 C17 H17 118.9 . . ?
C14 C19 H19 107.3 . . ?
C14 C19 C21 114.1(3) . . ?
C14 C19 C20 110.8(3) . . ?
C21 C19 H19 107.3 . . ?
C20 C19 H19 107.3 . . ?
C20 C19 C21 109.7(3) . . ?
C1 C6 C10 122.0(3) . . ?
C5 C6 C1 119.0(3) . . ?
C5 C6 C10 118.9(3) . . ?
C15 C16 H16 120.2 . . ?
C17 C16 C15 119.5(3) . . ?
C17 C16 H16 120.2 . . ?
C6 C10 H10 107.6 . . ?
C6 C10 C11 110.7(3) . . ?
C6 C10 C12 112.8(3) . . ?
C11 C10 H10 107.6 . . ?
C11 C10 C12 110.5(3) . . ?
C12 C10 H10 107.6 . . ?
C2 C7 H7 108.0 . . ?
C2 C7 C9 111.4(3) . . ?
C2 C7 C8 112.1(3) . . ?
C9 C7 H7 108.0 . . ?
C8 C7 H7 108.0 . . ?
C8 C7 C9 109.3(3) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C3 C4 C5 119.7(3) . . ?
C41 C36 C35 120.4(3) . . ?
C37 C36 C41 118.7(3) . . ?
C37 C36 C35 120.9(3) . . ?
O3 C28 H28A 110.3 . . ?
O3 C28 H28B 110.3 . . ?
O3 C28 C27 107.1(3) . . ?
H28A C28 H28B 108.6 . . ?
C27 C28 H28A 110.3 . . ?
C27 C28 H28B 110.3 . . ?
C6 C5 H5 119.6 . . ?
C4 C5 C6 120.8(3) . . ?
C4 C5 H5 119.6 . . ?
C2 C3 H3 119.1 . . ?
C4 C3 C2 121.7(3) . . ?
C4 C3 H3 119.1 . . ?
O3 C29 H29A 110.1 . . ?
O3 C29 H29B 110.1 . . ?
O3 C29 C30 108.0(3) . . ?
H29A C29 H29B 108.4 . . ?
C30 C29 H29A 110.1 . . ?
C30 C29 H29B 110.1 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C36 C41 H41 120.4 . . ?
C36 C41 C40 119.2(4) . . ?
C40 C41 H41 120.4 . . ?
O4 C30 C29 107.2(3) . . ?
O4 C30 H30A 110.3 . . ?
O4 C30 H30B 110.3 . . ?
C29 C30 H30A 110.3 . . ?
C29 C30 H30B 110.3 . . ?
H30A C30 H30B 108.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O2 C27 C28 107.6(3) . . ?
O2 C27 H27A 110.2 . . ?
O2 C27 H27B 110.2 . . ?
C28 C27 H27A 110.2 . . ?
C28 C27 H27B 110.2 . . ?
H27A C27 H27B 108.5 . . ?
O1 C34 H34A 110.5 . . ?
O1 C34 H34B 110.5 . . ?
O1 C34 C33 106.4(3) . . ?
H34A C34 H34B 108.6 . . ?
C33 C34 H34A 110.5 . . ?
C33 C34 H34B 110.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O5 C32 H32A 110.1 . . ?
O5 C32 H32B 110.1 . . ?
O5 C32 C31 108.0(3) . . ?
H32A C32 H32B 108.4 . . ?
C31 C32 H32A 110.1 . . ?
C31 C32 H32B 110.1 . . ?
O5 C33 C34 107.8(3) . . ?
O5 C33 H33A 110.1 . . ?
O5 C33 H33B 110.1 . . ?
C34 C33 H33A 110.1 . . ?
C34 C33 H33B 110.1 . . ?
H33A C33 H33B 108.5 . . ?
O4 C31 C32 111.3(3) . . ?
O4 C31 H31A 109.4 . . ?
O4 C31 H31B 109.4 . . ?
C32 C31 H31A 109.4 . . ?
C32 C31 H31B 109.4 . . ?
H31A C31 H31B 108.0 . . ?
O2 C26 H26A 110.1 . . ?
O2 C26 H26B 110.1 . . ?
O2 C26 C25 107.8(3) . . ?
H26A C26 H26B 108.5 . . ?
C25 C26 H26A 110.1 . . ?
C25 C26 H26B 110.1 . . ?
C36 C37 H37 119.1 . . ?
C38 C37 C36 121.8(4) . . ?
C38 C37 H37 119.1 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O1 C25 C26 106.6(3) . . ?
O1 C25 H25A 110.4 . . ?
O1 C25 H25B 110.4 . . ?
C26 C25 H25A 110.4 . . ?
C26 C25 H25B 110.4 . . ?
H25A C25 H25B 108.6 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C38 C39 H39 119.6 . . ?
C38 C39 C40 120.8(4) . . ?
C40 C39 H39 119.6 . . ?
C37 C38 H38 120.1 . . ?
C39 C38 C37 119.8(4) . . ?
C39 C38 H38 120.1 . . ?
C41 C40 H40 120.2 . . ?
C39 C40 C41 119.5(4) . . ?
C39 C40 H40 120.2 . . ?
C36 C35 H35A 109.5 . . ?
C36 C35 H35B 109.5 . . ?
C36 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_11
_database_code_depnum_ccdc_archive 'CCDC 1972004'
loop_
_audit_author_name
_audit_author_address
'Alasdair McKay'
;Monash University
Australia
;
_audit_update_record             
;
2019-12-14 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT029_11                  
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.924 Why?
RESPONSE: Data was weak and incomplete (92% to theta = 25 degrees). The quality of this structure is poor and is included as confirmation of connectivity and for provision of unit cell parameters only.
;
_vrf_PLAT342_11                  
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02748 Ang.
RESPONSE: Data was weak and incomplete (92% to theta = 25 degree). The quality of this structure is poor and is included as confirmation of connectivity and for provision of unit cell parameters only.
;
_vrf_PLAT911_11                  
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.597        355 Report
RESPONSE: Data was weak and incomplete (92% to theta = 25 degrees). The quality of this structure is poor and is included as confirmation of connectivity and for provision of unit cell parameters only.
;
# Added during the CSD deposition process: Saturday 14 December 2019 01:17 PM
# end Validation Reply Form

_audit_creation_date             2019-12-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
''
alasdair.mckay@monash.edu
_chemical_name_common            ?
_chemical_name_systematic        '[GaI(N3Dipp2)]2'
_chemical_formula_moiety         'C48 H68 Ga2 I2 N6'
_chemical_formula_sum            'C48 H68 Ga2 I2 N6'
_chemical_formula_weight         1122.32
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.764(3)
_cell_length_b                   11.169(3)
_cell_length_c                   12.729(5)
_cell_angle_alpha                96.760(17)
_cell_angle_beta                 114.864(10)
_cell_angle_gamma                105.707(12)
_cell_volume                     1288.8(7)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    1935
_cell_measurement_temperature    150
_cell_measurement_theta_max      20.10
_cell_measurement_theta_min      2.23
_shelx_estimated_absorpt_T_max   0.935
_shelx_estimated_absorpt_T_min   0.772
_exptl_absorpt_coefficient_mu    2.279
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5339
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1241 before and 0.0632 after correction. The Ratio of minimum to maximum transmission is 0.7156. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             566
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1076
_diffrn_reflns_av_unetI/netI     0.1663
_diffrn_reflns_Laue_measured_fraction_full 0.924
_diffrn_reflns_Laue_measured_fraction_max 0.922
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11441
_diffrn_reflns_point_group_measured_fraction_full 0.924
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.121
_diffrn_reflns_theta_min         2.112
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.924
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2037
_reflns_number_total             4243
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.944
_refine_diff_density_min         -1.734
_refine_diff_density_rms         0.174
_refine_ls_extinction_coef       0.0112(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         4243
_refine_ls_number_restraints     314
_refine_ls_R_factor_all          0.1809
_refine_ls_R_factor_gt           0.0890
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1028P)²+1.8361P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2015
_refine_ls_wR_factor_ref         0.2382
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C24A-C22 \\sim C24-C22 \\sim C23A-C22 \\sim C23-C22
 with sigma of 0.02
 C21-C19 \\sim C21A-C19
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C24A \\sim C22 \\sim C24 \\sim C23A \\sim C23: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C21 \\sim C19 \\sim C21A \\sim C20: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 N3, I1, Ga1, N1, N2, C1, C13, C2, C6, C14, C18, C7, C3, C10, C5, C15, C19,
 C17, C22, C8, C9, C4, C12, C11, C16, C20, C21, C21A, C23, C24, C24A, C23A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H22A)=Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C23A)=Sof(H23D)=
 Sof(H23E)=Sof(H23F)=1-FVAR(1)
 Sof(H22)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24)=Sof(H24A)=Sof(H24B)=
 Sof(H24C)=FVAR(1)
 Sof(H19A)=Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(2)
 Sof(H19)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C22(H22), C22(H22A), C19(H19), C19(H19A), C7(H7), C10(H10)
6.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C15(H15), C16(H16), C3(H3), C4(H4), C5(H5)
6.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C23(H23A,H23B,H23C), C12(H12A,H12B,H12C), C24(H24A,H24B,
 H24C), C11(H11A,H11B,H11C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C9(H9A,
 H9B,H9C), C24A(H24D,H24E,H24F), C23A(H23D,H23E,H23F), C21A(H21D,H21E,H21F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.17199(12) -0.00777(12) 0.45968(8) 0.0746(6) Uani 1 1 d . U . . .
Ga1 Ga 0.43051(16) -0.00713(13) 0.55478(10) 0.0398(5) Uani 1 1 d . U . . .
N1 N 0.4446(11) -0.1150(9) 0.6719(8) 0.043(3) Uani 1 1 d . U . . .
N3 N 0.5217(12) 0.0863(9) 0.7289(8) 0.043(3) Uani 1 1 d . U . . .
N2 N 0.5076(11) -0.0177(9) 0.7665(8) 0.040(3) Uani 1 1 d . U . . .
C14 C 0.5055(16) 0.2364(12) 0.8764(10) 0.047(3) Uani 1 1 d . U . . .
C13 C 0.5790(14) 0.2102(12) 0.8146(9) 0.039(3) Uani 1 1 d . U . . .
C18 C 0.7071(14) 0.3003(12) 0.8272(10) 0.041(3) Uani 1 1 d . U . . .
C17 C 0.7592(15) 0.4184(12) 0.9064(10) 0.049(3) Uani 1 1 d . U . . .
H17 H 0.846651 0.481765 0.918578 0.059 Uiso 1 1 calc R . . . .
C15 C 0.5643(16) 0.3570(13) 0.9538(11) 0.061(4) Uani 1 1 d . U . . .
H15 H 0.516997 0.377619 0.998071 0.073 Uiso 1 1 calc R . . . .
C22 C 0.7829(14) 0.2665(14) 0.7558(11) 0.058(3) Uani 1 1 d D U . . .
H22 H 0.752782 0.170613 0.729604 0.069 Uiso 0.737(14) 1 calc R . P A 1
H22A H 0.714977 0.195813 0.680208 0.069 Uiso 0.263(14) 1 calc R . P A 2
C1 C 0.4196(18) -0.2421(13) 0.6899(10) 0.056(3) Uani 1 1 d . U . . .
C16 C 0.6886(17) 0.4480(14) 0.9690(12) 0.063(4) Uani 1 1 d . U . . .
H16 H 0.726234 0.531166 1.022197 0.075 Uiso 1 1 calc R . . . .
C19 C 0.3630(17) 0.1435(14) 0.8604(12) 0.062(3) Uani 1 1 d D U . . .
H19 H 0.342068 0.053965 0.816752 0.075 Uiso 0.56(4) 1 calc R . P B 1
H19A H 0.341202 0.068316 0.796016 0.075 Uiso 0.44(4) 1 calc R . P B 2
C2 C 0.521(2) -0.3016(15) 0.6944(12) 0.071(4) Uani 1 1 d . U . . .
C7 C 0.659(2) -0.2349(17) 0.6891(16) 0.087(4) Uani 1 1 d . U . . .
H7 H 0.639627 -0.167817 0.645176 0.104 Uiso 1 1 calc R . . . .
C6 C 0.287(2) -0.3004(16) 0.6957(13) 0.081(4) Uani 1 1 d . U . . .
C10 C 0.177(2) -0.243(2) 0.6839(16) 0.102(5) Uani 1 1 d . U . . .
H10 H 0.215714 -0.153272 0.677774 0.122 Uiso 1 1 calc R . . . .
C3 C 0.492(3) -0.4285(18) 0.7101(15) 0.108(6) Uani 1 1 d . U . . .
H3 H 0.558839 -0.471537 0.715871 0.130 Uiso 1 1 calc R . . . .
C8 C 0.791(2) -0.163(2) 0.8155(17) 0.133(8) Uani 1 1 d . U . . .
H8A H 0.765340 -0.101797 0.857666 0.199 Uiso 1 1 calc GR . . . .
H8B H 0.875613 -0.115148 0.807109 0.199 Uiso 1 1 calc GR . . . .
H8C H 0.814410 -0.224960 0.861411 0.199 Uiso 1 1 calc GR . . . .
C23 C 0.730(2) 0.3213(19) 0.6394(15) 0.062(5) Uani 0.737(14) 1 d D U P A 1
H23A H 0.625656 0.273843 0.585680 0.093 Uiso 0.737(14) 1 calc GR . P A 1
H23B H 0.786091 0.310315 0.597259 0.093 Uiso 0.737(14) 1 calc GR . P A 1
H23C H 0.746927 0.413088 0.664458 0.093 Uiso 0.737(14) 1 calc GR . P A 1
C4 C 0.369(3) -0.4867(19) 0.7166(16) 0.121(7) Uani 1 1 d . U . . .
H4 H 0.351516 -0.571605 0.726651 0.146 Uiso 1 1 calc R . . . .
C12 C 0.159(2) -0.230(2) 0.7963(18) 0.139(9) Uani 1 1 d . U . . .
H12A H 0.109401 -0.315705 0.800338 0.209 Uiso 1 1 calc GR . . . .
H12B H 0.100191 -0.175929 0.793816 0.209 Uiso 1 1 calc GR . . . .
H12C H 0.255508 -0.190280 0.867288 0.209 Uiso 1 1 calc GR . . . .
C5 C 0.265(3) -0.4285(18) 0.7095(15) 0.114(6) Uani 1 1 d . U . . .
H5 H 0.180549 -0.475195 0.713857 0.137 Uiso 1 1 calc R . . . .
C24 C 0.9540(17) 0.329(2) 0.8179(17) 0.061(5) Uani 0.737(14) 1 d D U P A 1
H24A H 0.982996 0.422905 0.832399 0.091 Uiso 0.737(14) 1 calc GR . P A 1
H24B H 0.989655 0.295948 0.765602 0.091 Uiso 0.737(14) 1 calc GR . P A 1
H24C H 0.996319 0.307200 0.894509 0.091 Uiso 0.737(14) 1 calc GR . P A 1
C11 C 0.032(2) -0.314(2) 0.5674(17) 0.125(8) Uani 1 1 d . U . . .
H11A H 0.051666 -0.326152 0.499352 0.187 Uiso 1 1 calc GR . . . .
H11B H -0.032116 -0.263206 0.554546 0.187 Uiso 1 1 calc GR . . . .
H11C H -0.017076 -0.398532 0.574256 0.187 Uiso 1 1 calc GR . . . .
C20 C 0.2351(18) 0.1882(17) 0.7989(15) 0.081(4) Uani 1 1 d . U . . .
H20A H 0.252350 0.270397 0.849529 0.121 Uiso 1 1 calc GR . . . .
H20B H 0.144546 0.123392 0.786579 0.121 Uiso 1 1 calc GR . . . .
H20C H 0.225974 0.199496 0.721166 0.121 Uiso 1 1 calc GR . . . .
C21 C 0.348(4) 0.145(4) 0.978(2) 0.079(8) Uani 0.56(4) 1 d D U P B 1
H21A H 0.433072 0.131565 1.039576 0.119 Uiso 0.56(4) 1 calc GR . P B 1
H21B H 0.258408 0.075264 0.961042 0.119 Uiso 0.56(4) 1 calc GR . P B 1
H21C H 0.344547 0.227891 1.008215 0.119 Uiso 0.56(4) 1 calc GR . P B 1
C9 C 0.693(3) -0.326(2) 0.617(2) 0.146(9) Uani 1 1 d . U . . .
H9A H 0.744050 -0.374337 0.667948 0.218 Uiso 1 1 calc GR . . . .
H9B H 0.756323 -0.275823 0.588021 0.218 Uiso 1 1 calc GR . . . .
H9C H 0.602131 -0.385588 0.548418 0.218 Uiso 1 1 calc GR . . . .
C24A C 0.889(5) 0.220(5) 0.861(3) 0.054(7) Uani 0.263(14) 1 d D U P A 2
H24D H 0.965568 0.294817 0.925659 0.081 Uiso 0.263(14) 1 calc GR . P A 2
H24E H 0.933673 0.170101 0.828713 0.081 Uiso 0.263(14) 1 calc GR . P A 2
H24F H 0.831777 0.164963 0.891562 0.081 Uiso 0.263(14) 1 calc GR . P A 2
C23A C 0.878(6) 0.387(3) 0.736(5) 0.059(7) Uani 0.263(14) 1 d D U P A 2
H23D H 0.813573 0.421153 0.677285 0.089 Uiso 0.263(14) 1 calc GR . P A 2
H23E H 0.939544 0.360924 0.705600 0.089 Uiso 0.263(14) 1 calc GR . P A 2
H23F H 0.940642 0.453575 0.812185 0.089 Uiso 0.263(14) 1 calc GR . P A 2
C21A C 0.410(5) 0.090(4) 0.975(3) 0.068(8) Uani 0.44(4) 1 d D U P B 2
H21D H 0.452958 0.025212 0.964562 0.103 Uiso 0.44(4) 1 calc GR . P B 2
H21E H 0.324167 0.050504 0.984688 0.103 Uiso 0.44(4) 1 calc GR . P B 2
H21F H 0.482807 0.161059 1.045758 0.103 Uiso 0.44(4) 1 calc GR . P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 Ga1 2.5227(19) . ?
Ga1 Ga1 2.426(3) 2_656 ?
Ga1 N1 2.007(10) . ?
Ga1 N3 2.009(9) . ?
N1 N2 1.302(12) . ?
N1 C1 1.437(16) . ?
N3 N2 1.303(13) . ?
N3 C13 1.450(14) . ?
C14 C13 1.388(17) . ?
C14 C15 1.374(17) . ?
C14 C19 1.516(19) . ?
C13 C18 1.402(17) . ?
C18 C17 1.371(16) . ?
C18 C22 1.531(17) . ?
C17 C16 1.381(18) . ?
C15 C16 1.364(18) . ?
C22 C23 1.607(17) . ?
C22 C24 1.567(17) . ?
C22 C24A 1.60(2) . ?
C22 C23A 1.57(2) . ?
C1 C2 1.40(2) . ?
C1 C6 1.44(2) . ?
C19 C20 1.52(2) . ?
C19 C21 1.57(2) . ?
C19 C21A 1.57(2) . ?
C2 C7 1.51(2) . ?
C2 C3 1.42(2) . ?
C7 C8 1.55(2) . ?
C7 C9 1.51(2) . ?
C6 C10 1.45(3) . ?
C6 C5 1.43(3) . ?
C10 C12 1.52(3) . ?
C10 C11 1.54(2) . ?
C3 C4 1.35(3) . ?
C4 C5 1.41(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Ga1 Ga1 I1 121.54(8) 2_656 . ?
N1 Ga1 I1 106.9(3) . . ?
N1 Ga1 Ga1 122.8(3) . 2_656 ?
N1 Ga1 N3 62.7(4) . . ?
N3 Ga1 I1 105.9(3) . . ?
N3 Ga1 Ga1 122.4(3) . 2_656 ?
N2 N1 Ga1 95.4(7) . . ?
N2 N1 C1 117.6(9) . . ?
C1 N1 Ga1 147.0(7) . . ?
N2 N3 Ga1 95.2(6) . . ?
N2 N3 C13 118.8(9) . . ?
C13 N3 Ga1 145.7(8) . . ?
N1 N2 N3 106.7(9) . . ?
C13 C14 C19 124.5(12) . . ?
C15 C14 C13 117.1(13) . . ?
C15 C14 C19 118.4(12) . . ?
C14 C13 N3 120.3(12) . . ?
C14 C13 C18 123.2(11) . . ?
C18 C13 N3 116.4(11) . . ?
C13 C18 C22 121.0(11) . . ?
C17 C18 C13 116.2(11) . . ?
C17 C18 C22 122.8(13) . . ?
C18 C17 C16 122.1(13) . . ?
C16 C15 C14 121.8(13) . . ?
C18 C22 C23 107.8(11) . . ?
C18 C22 C24 117.2(12) . . ?
C18 C22 C24A 93.0(19) . . ?
C18 C22 C23A 114(2) . . ?
C24 C22 C23 103.4(14) . . ?
C23A C22 C24A 109(3) . . ?
N1 C1 C6 115.9(14) . . ?
C2 C1 N1 118.5(15) . . ?
C2 C1 C6 125.5(16) . . ?
C15 C16 C17 119.5(13) . . ?
C14 C19 C20 112.1(13) . . ?
C14 C19 C21 115.3(16) . . ?
C14 C19 C21A 104.2(19) . . ?
C20 C19 C21 95(2) . . ?
C20 C19 C21A 131(2) . . ?
C1 C2 C7 122.9(14) . . ?
C1 C2 C3 117.5(19) . . ?
C3 C2 C7 119.5(17) . . ?
C2 C7 C8 112.5(17) . . ?
C2 C7 C9 112.0(17) . . ?
C9 C7 C8 112.0(17) . . ?
C1 C6 C10 126.0(18) . . ?
C5 C6 C1 113(2) . . ?
C5 C6 C10 121(2) . . ?
C6 C10 C12 111(2) . . ?
C6 C10 C11 111.9(17) . . ?
C12 C10 C11 113.5(17) . . ?
C4 C3 C2 119(2) . . ?
C3 C4 C5 124(2) . . ?
C4 C5 C6 121(2) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_13
_database_code_depnum_ccdc_archive 'CCDC 1972005'
loop_
_audit_author_name
_audit_author_address
'Alasdair McKay'
;Monash University
Australia
;
_audit_update_record             
;
2019-12-14 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_audit_creation_date             2019-12-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
''
alasdair.mckay@monash.edu
_chemical_name_common            ?
_chemical_name_systematic        '[GaCl(N3Dipp2)2]'
_chemical_formula_moiety         'C48 H68 Cl Ga N6'
_chemical_formula_sum            'C48 H68 Cl Ga N6'
_chemical_formula_weight         834.25
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.315(3)
_cell_length_b                   16.444(3)
_cell_length_c                   21.068(4)
_cell_angle_alpha                90
_cell_angle_beta                 109.614(9)
_cell_angle_gamma                90
_cell_volume                     4671.6(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4406
_cell_measurement_temperature    150
_cell_measurement_theta_max      24.45
_cell_measurement_theta_min      2.40
_shelx_estimated_absorpt_T_max   0.935
_shelx_estimated_absorpt_T_min   0.935
_exptl_absorpt_coefficient_mu    0.684
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6324
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1106 before and 0.0690 after correction. The Ratio of minimum to maximum transmission is 0.8476. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       cube
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0913
_diffrn_reflns_av_unetI/netI     0.1055
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            39262
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         1.510
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5967
_reflns_number_total             10285
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         10285
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1154
_refine_ls_R_factor_gt           0.0544
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0469P)²+1.2732P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1134
_refine_ls_wR_factor_ref         0.1359
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C22(H22), C10(H10), C19(H19), C46(H46), C43(H43), C7(H7), C34(H34), C31(H31)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C28(H28), C27(H27), C29(H29), C3(H3), C17(H17), C4(H4),
 C39(H39), C5(H5), C41(H41), C40(H40)
2.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C24(H24A,H24B,
 H24C), C11(H11A,H11B,H11C), C21(H21A,H21B,H21C), C44(H44A,H44B,H44C), C12(H12A,
 H12B,H12C), C48(H48A,H48B,H48C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C20(H20A,H20B,H20C), C36(H36A,H36B,H36C),
 C35(H35A,H35B,H35C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ga1 Ga 0.24238(2) 0.22498(2) 0.41328(2) 0.02513(11) Uani 1 1 d . . . . .
Cl1 Cl 0.22665(6) 0.22712(5) 0.51179(4) 0.0385(2) Uani 1 1 d . . . . .
C13 C 0.4978(2) 0.22922(18) 0.47019(14) 0.0257(7) Uani 1 1 d . . . . .
C25 C 0.2572(2) 0.40193(18) 0.35038(16) 0.0267(7) Uani 1 1 d . . . . .
C18 C 0.5489(2) 0.27012(19) 0.43408(15) 0.0298(7) Uani 1 1 d . . . . .
C6 C 0.2605(2) 0.02606(19) 0.29139(16) 0.0318(8) Uani 1 1 d . . . . .
C22 C 0.5044(2) 0.2840(2) 0.35979(16) 0.0350(8) Uani 1 1 d . . . . .
H22 H 0.430634 0.280883 0.347465 0.042 Uiso 1 1 calc R . . . .
C30 C 0.2594(2) 0.4187(2) 0.28600(16) 0.0339(8) Uani 1 1 d . . . . .
C37 C -0.0078(2) 0.22945(19) 0.33558(16) 0.0299(7) Uani 1 1 d . . . . .
C14 C 0.5404(2) 0.2132(2) 0.53899(15) 0.0347(8) Uani 1 1 d . . . . .
C15 C 0.6383(3) 0.2383(2) 0.57047(17) 0.0429(9) Uani 1 1 d . . . . .
H15 H 0.669778 0.228109 0.617197 0.051 Uiso 1 1 calc R . . . .
C2 C 0.2074(2) -0.0081(2) 0.38656(17) 0.0347(8) Uani 1 1 d . . . . .
C16 C 0.6896(3) 0.2772(2) 0.53546(19) 0.0470(10) Uani 1 1 d . . . . .
H16 H 0.756412 0.293214 0.557791 0.056 Uiso 1 1 calc R . . . .
C42 C -0.0505(2) 0.1778(2) 0.28069(18) 0.0377(8) Uani 1 1 d . . . . .
C26 C 0.3003(2) 0.4530(2) 0.40514(17) 0.0341(8) Uani 1 1 d . . . . .
C10 C 0.3093(3) 0.0809(2) 0.25430(16) 0.0381(9) Uani 1 1 d . . . . .
H10 H 0.331040 0.131499 0.281618 0.046 Uiso 1 1 calc R . . . .
C19 C 0.4857(3) 0.1676(3) 0.57706(17) 0.0485(10) Uani 1 1 d . . . . .
H19 H 0.413125 0.174796 0.552386 0.058 Uiso 1 1 calc R . . . .
C46 C 0.0052(3) 0.1498(2) 0.23589(17) 0.0404(9) Uani 1 1 d . . . . .
H46 H 0.077513 0.152860 0.262763 0.048 Uiso 1 1 calc R . . . .
C38 C -0.0608(3) 0.2596(2) 0.37460(18) 0.0391(9) Uani 1 1 d . . . . .
C28 C 0.3528(3) 0.5398(2) 0.3321(2) 0.0465(10) Uani 1 1 d . . . . .
H28 H 0.386815 0.587137 0.325957 0.056 Uiso 1 1 calc R . . . .
C27 C 0.3480(3) 0.5224(2) 0.3936(2) 0.0456(10) Uani 1 1 d . . . . .
H27 H 0.377847 0.558545 0.429971 0.055 Uiso 1 1 calc R . . . .
C29 C 0.3087(3) 0.4891(2) 0.27835(19) 0.0428(9) Uani 1 1 d . . . . .
H29 H 0.311956 0.502410 0.235257 0.051 Uiso 1 1 calc R . . . .
C43 C -0.0154(3) 0.3159(2) 0.43404(16) 0.0429(9) Uani 1 1 d . . . . .
H43 H 0.057446 0.319355 0.442057 0.051 Uiso 1 1 calc R . . . .
C3 C 0.1700(3) -0.0814(2) 0.35491(19) 0.0455(10) Uani 1 1 d . . . . .
H3 H 0.137995 -0.117917 0.375893 0.055 Uiso 1 1 calc R . . . .
C17 C 0.6458(2) 0.2931(2) 0.46884(18) 0.0414(9) Uani 1 1 d . . . . .
H17 H 0.682609 0.320677 0.445363 0.050 Uiso 1 1 calc R . . . .
C23 C 0.5364(3) 0.2165(2) 0.32281(19) 0.0558(11) Uani 1 1 d . . . . .
H23A H 0.608377 0.219198 0.332971 0.084 Uiso 1 1 calc GR . . . .
H23B H 0.502927 0.222926 0.274190 0.084 Uiso 1 1 calc GR . . . .
H23C H 0.518773 0.163829 0.337297 0.084 Uiso 1 1 calc GR . . . .
C7 C 0.2007(3) 0.0107(2) 0.45513(18) 0.0434(9) Uani 1 1 d . . . . .
H7 H 0.240905 0.060726 0.472375 0.052 Uiso 1 1 calc R . . . .
C34 C 0.2094(3) 0.3649(2) 0.22583(16) 0.0425(9) Uani 1 1 d . . . . .
H34 H 0.184756 0.315243 0.242677 0.051 Uiso 1 1 calc R . . . .
C31 C 0.2920(3) 0.4364(2) 0.47298(17) 0.0451(10) Uani 1 1 d . . . . .
H31 H 0.266017 0.379825 0.471988 0.054 Uiso 1 1 calc R . . . .
C4 C 0.1786(3) -0.1015(2) 0.2939(2) 0.0469(10) Uani 1 1 d . . . . .
H4 H 0.153341 -0.151884 0.273145 0.056 Uiso 1 1 calc R . . . .
C39 C -0.1601(3) 0.2370(3) 0.3567(2) 0.0642(13) Uani 1 1 d . . . . .
H39 H -0.199015 0.256887 0.382097 0.077 Uiso 1 1 calc R . . . .
C5 C 0.2237(3) -0.0489(2) 0.26299(18) 0.0426(9) Uani 1 1 d . . . . .
H5 H 0.230140 -0.063904 0.221097 0.051 Uiso 1 1 calc R . . . .
C45 C -0.0291(4) 0.2840(4) 0.4978(2) 0.0905(17) Uani 1 1 d . . . . .
H45A H -0.099858 0.283707 0.492271 0.136 Uiso 1 1 calc GR . . . .
H45B H 0.006545 0.319068 0.535781 0.136 Uiso 1 1 calc GR . . . .
H45C H -0.002906 0.228497 0.506494 0.136 Uiso 1 1 calc GR . . . .
C47 C -0.0143(3) 0.2105(3) 0.1778(2) 0.0757(15) Uani 1 1 d . . . . .
H47A H -0.084637 0.208958 0.150186 0.113 Uiso 1 1 calc GR . . . .
H47B H 0.026095 0.196072 0.150033 0.113 Uiso 1 1 calc GR . . . .
H47C H 0.003202 0.265414 0.196056 0.113 Uiso 1 1 calc GR . . . .
C24 C 0.5298(3) 0.3671(2) 0.33807(18) 0.0487(10) Uani 1 1 d . . . . .
H24A H 0.512512 0.409495 0.364845 0.073 Uiso 1 1 calc GR . . . .
H24B H 0.492337 0.375577 0.290227 0.073 Uiso 1 1 calc GR . . . .
H24C H 0.601023 0.369573 0.345162 0.073 Uiso 1 1 calc GR . . . .
C11 C 0.4001(3) 0.0413(2) 0.2464(2) 0.0616(12) Uani 1 1 d . . . . .
H11A H 0.448315 0.029678 0.290993 0.092 Uiso 1 1 calc GR . . . .
H11B H 0.429855 0.078076 0.221949 0.092 Uiso 1 1 calc GR . . . .
H11C H 0.380920 -0.009592 0.221127 0.092 Uiso 1 1 calc GR . . . .
C41 C -0.1490(3) 0.1579(3) 0.2651(2) 0.0645(13) Uani 1 1 d . . . . .
H41 H -0.180187 0.123992 0.227417 0.077 Uiso 1 1 calc R . . . .
C21 C 0.5068(4) 0.1994(4) 0.6477(2) 0.108(2) Uani 1 1 d . . . . .
H21A H 0.577993 0.195071 0.672713 0.162 Uiso 1 1 calc GR . . . .
H21B H 0.469781 0.167287 0.670450 0.162 Uiso 1 1 calc GR . . . .
H21C H 0.486422 0.256499 0.645818 0.162 Uiso 1 1 calc GR . . . .
C44 C -0.0588(3) 0.4009(2) 0.4172(2) 0.0657(13) Uani 1 1 d . . . . .
H44A H -0.130173 0.399182 0.409658 0.099 Uiso 1 1 calc GR . . . .
H44B H -0.047725 0.420598 0.376446 0.099 Uiso 1 1 calc GR . . . .
H44C H -0.026483 0.437670 0.454827 0.099 Uiso 1 1 calc GR . . . .
C40 C -0.2022(3) 0.1865(3) 0.3032(3) 0.0841(17) Uani 1 1 d . . . . .
H40 H -0.269686 0.171140 0.292302 0.101 Uiso 1 1 calc R . . . .
C12 C 0.2371(3) 0.1056(3) 0.18484(19) 0.0691(13) Uani 1 1 d . . . . .
H12A H 0.210574 0.056732 0.158360 0.104 Uiso 1 1 calc GR . . . .
H12B H 0.272289 0.138632 0.161321 0.104 Uiso 1 1 calc GR . . . .
H12C H 0.182517 0.137364 0.190519 0.104 Uiso 1 1 calc GR . . . .
C48 C -0.0167(3) 0.0632(3) 0.2119(3) 0.0833(17) Uani 1 1 d . . . . .
H48A H -0.007451 0.027331 0.250684 0.125 Uiso 1 1 calc GR . . . .
H48B H 0.028379 0.046704 0.188037 0.125 Uiso 1 1 calc GR . . . .
H48C H -0.085417 0.059199 0.181315 0.125 Uiso 1 1 calc GR . . . .
C9 C 0.0957(3) 0.0288(3) 0.4508(2) 0.0789(15) Uani 1 1 d . . . . .
H9A H 0.068340 0.071257 0.417023 0.118 Uiso 1 1 calc GR . . . .
H9B H 0.094867 0.047423 0.494736 0.118 Uiso 1 1 calc GR . . . .
H9C H 0.055557 -0.020664 0.437679 0.118 Uiso 1 1 calc GR . . . .
C8 C 0.2443(4) -0.0579(3) 0.5059(2) 0.0860(17) Uani 1 1 d . . . . .
H8A H 0.201577 -0.105987 0.493266 0.129 Uiso 1 1 calc GR . . . .
H8B H 0.248307 -0.039999 0.551070 0.129 Uiso 1 1 calc GR . . . .
H8C H 0.310823 -0.071530 0.505637 0.129 Uiso 1 1 calc GR . . . .
C32 C 0.2179(4) 0.4931(3) 0.4871(2) 0.0806(15) Uani 1 1 d . . . . .
H32A H 0.241638 0.549289 0.489066 0.121 Uiso 1 1 calc GR . . . .
H32B H 0.210500 0.478623 0.530241 0.121 Uiso 1 1 calc GR . . . .
H32C H 0.153683 0.488153 0.451009 0.121 Uiso 1 1 calc GR . . . .
C33 C 0.3917(3) 0.4401(3) 0.5297(2) 0.0790(15) Uani 1 1 d . . . . .
H33A H 0.436887 0.400041 0.521303 0.119 Uiso 1 1 calc GR . . . .
H33B H 0.382318 0.428030 0.572676 0.119 Uiso 1 1 calc GR . . . .
H33C H 0.420030 0.494688 0.531473 0.119 Uiso 1 1 calc GR . . . .
C20 C 0.5085(4) 0.0767(3) 0.5777(3) 0.0902(17) Uani 1 1 d . . . . .
H20A H 0.492983 0.057294 0.531279 0.135 Uiso 1 1 calc GR . . . .
H20B H 0.468278 0.046976 0.599502 0.135 Uiso 1 1 calc GR . . . .
H20C H 0.579000 0.067542 0.602617 0.135 Uiso 1 1 calc GR . . . .
N5 N 0.11663(18) 0.31997(16) 0.33617(12) 0.0259(6) Uani 1 1 d . . . . .
N2 N 0.38173(18) 0.13379(15) 0.40957(12) 0.0261(6) Uani 1 1 d . . . . .
N4 N 0.21312(17) 0.32834(15) 0.36285(11) 0.0245(6) Uani 1 1 d . . . . .
N1 N 0.28577(18) 0.12219(15) 0.38436(12) 0.0265(6) Uani 1 1 d . . . . .
N6 N 0.09495(17) 0.24882(15) 0.35262(11) 0.0239(6) Uani 1 1 d . . . . .
N3 N 0.39600(18) 0.20551(15) 0.43604(12) 0.0252(6) Uani 1 1 d . . . . .
C1 C 0.2511(2) 0.04497(19) 0.35324(15) 0.0273(7) Uani 1 1 d . . . . .
C36 C 0.2804(4) 0.3372(3) 0.1902(2) 0.0833(16) Uani 1 1 d . . . . .
H36A H 0.244886 0.302678 0.151735 0.125 Uiso 1 1 calc GR . . . .
H36B H 0.334944 0.306256 0.221668 0.125 Uiso 1 1 calc GR . . . .
H36C H 0.307178 0.384837 0.174198 0.125 Uiso 1 1 calc GR . . . .
C35 C 0.1213(4) 0.4066(3) 0.1765(2) 0.0917(18) Uani 1 1 d . . . . .
H35A H 0.076809 0.425679 0.200020 0.138 Uiso 1 1 calc GR . . . .
H35B H 0.085810 0.368281 0.141002 0.138 Uiso 1 1 calc GR . . . .
H35C H 0.143861 0.453119 0.156412 0.138 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ga1 Cl1 2.1617(9) . ?
Ga1 N4 1.973(3) . ?
Ga1 N1 1.967(3) . ?
Ga1 N6 2.105(2) . ?
Ga1 N3 2.112(2) . ?
C13 C18 1.392(4) . ?
C13 C14 1.396(4) . ?
C13 N3 1.446(4) . ?
C25 C30 1.395(4) . ?
C25 C26 1.393(4) . ?
C25 N4 1.429(4) . ?
C18 C22 1.496(4) . ?
C18 C17 1.387(4) . ?
C6 C10 1.509(5) . ?
C6 C5 1.395(5) . ?
C6 C1 1.389(4) . ?
C22 C23 1.512(5) . ?
C22 C24 1.524(5) . ?
C30 C29 1.392(5) . ?
C30 C34 1.515(5) . ?
C37 C42 1.399(4) . ?
C37 C38 1.385(5) . ?
C37 N6 1.428(4) . ?
C14 C15 1.398(5) . ?
C14 C19 1.496(5) . ?
C15 C16 1.362(5) . ?
C2 C3 1.394(5) . ?
C2 C7 1.512(5) . ?
C2 C1 1.393(5) . ?
C16 C17 1.357(5) . ?
C42 C46 1.499(5) . ?
C42 C41 1.375(5) . ?
C26 C27 1.392(5) . ?
C26 C31 1.499(5) . ?
C10 C11 1.513(5) . ?
C10 C12 1.536(5) . ?
C19 C21 1.509(5) . ?
C19 C20 1.530(6) . ?
C46 C47 1.530(5) . ?
C46 C48 1.509(5) . ?
C38 C43 1.517(5) . ?
C38 C39 1.393(5) . ?
C28 C27 1.351(5) . ?
C28 C29 1.377(5) . ?
C43 C45 1.515(5) . ?
C43 C44 1.523(5) . ?
C3 C4 1.373(5) . ?
C7 C9 1.504(5) . ?
C7 C8 1.535(5) . ?
C34 C36 1.523(5) . ?
C34 C35 1.504(5) . ?
C31 C32 1.514(5) . ?
C31 C33 1.524(5) . ?
C4 C5 1.367(5) . ?
C39 C40 1.367(6) . ?
C41 C40 1.362(6) . ?
N5 N4 1.312(3) . ?
N5 N6 1.287(3) . ?
N2 N1 1.310(3) . ?
N2 N3 1.291(3) . ?
N1 C1 1.439(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Ga1 Cl1 115.54(7) . . ?
N4 Ga1 N6 61.60(10) . . ?
N4 Ga1 N3 105.63(10) . . ?
N1 Ga1 Cl1 117.19(8) . . ?
N1 Ga1 N4 127.26(10) . . ?
N1 Ga1 N6 109.18(10) . . ?
N1 Ga1 N3 61.77(10) . . ?
N6 Ga1 Cl1 99.99(7) . . ?
N6 Ga1 N3 157.15(10) . . ?
N3 Ga1 Cl1 102.74(7) . . ?
C18 C13 C14 122.2(3) . . ?
C18 C13 N3 119.0(3) . . ?
C14 C13 N3 118.8(3) . . ?
C30 C25 N4 120.1(3) . . ?
C26 C25 C30 122.5(3) . . ?
C26 C25 N4 117.3(3) . . ?
C13 C18 C22 121.9(3) . . ?
C17 C18 C13 117.3(3) . . ?
C17 C18 C22 120.7(3) . . ?
C5 C6 C10 118.7(3) . . ?
C1 C6 C10 124.0(3) . . ?
C1 C6 C5 117.3(3) . . ?
C18 C22 C23 109.3(3) . . ?
C18 C22 C24 112.9(3) . . ?
C23 C22 C24 111.0(3) . . ?
C25 C30 C34 122.6(3) . . ?
C29 C30 C25 117.1(3) . . ?
C29 C30 C34 120.3(3) . . ?
C42 C37 N6 118.1(3) . . ?
C38 C37 C42 122.2(3) . . ?
C38 C37 N6 119.6(3) . . ?
C13 C14 C15 117.1(3) . . ?
C13 C14 C19 121.8(3) . . ?
C15 C14 C19 121.1(3) . . ?
C16 C15 C14 121.3(3) . . ?
C3 C2 C7 119.7(3) . . ?
C1 C2 C3 117.8(3) . . ?
C1 C2 C7 122.5(3) . . ?
C17 C16 C15 120.3(3) . . ?
C37 C42 C46 121.9(3) . . ?
C41 C42 C37 118.1(3) . . ?
C41 C42 C46 119.8(3) . . ?
C25 C26 C31 121.7(3) . . ?
C27 C26 C25 117.2(3) . . ?
C27 C26 C31 121.1(3) . . ?
C6 C10 C11 111.3(3) . . ?
C6 C10 C12 111.8(3) . . ?
C11 C10 C12 109.7(3) . . ?
C14 C19 C21 112.8(4) . . ?
C14 C19 C20 110.2(3) . . ?
C21 C19 C20 111.0(4) . . ?
C42 C46 C47 108.1(3) . . ?
C42 C46 C48 113.9(3) . . ?
C48 C46 C47 112.7(3) . . ?
C37 C38 C43 122.7(3) . . ?
C37 C38 C39 117.2(3) . . ?
C39 C38 C43 120.1(3) . . ?
C27 C28 C29 120.3(4) . . ?
C28 C27 C26 121.8(4) . . ?
C28 C29 C30 121.2(4) . . ?
C38 C43 C44 109.9(3) . . ?
C45 C43 C38 111.9(4) . . ?
C45 C43 C44 111.1(4) . . ?
C4 C3 C2 121.0(4) . . ?
C16 C17 C18 121.8(4) . . ?
C2 C7 C8 111.9(3) . . ?
C9 C7 C2 111.4(3) . . ?
C9 C7 C8 110.6(4) . . ?
C30 C34 C36 112.4(3) . . ?
C35 C34 C30 111.3(3) . . ?
C35 C34 C36 109.9(4) . . ?
C26 C31 C32 111.1(3) . . ?
C26 C31 C33 112.7(3) . . ?
C32 C31 C33 110.8(3) . . ?
C5 C4 C3 119.9(3) . . ?
C40 C39 C38 120.8(4) . . ?
C4 C5 C6 121.7(4) . . ?
C40 C41 C42 120.5(4) . . ?
C41 C40 C39 121.2(4) . . ?
N6 N5 N4 107.1(2) . . ?
N3 N2 N1 107.5(2) . . ?
C25 N4 Ga1 143.24(19) . . ?
N5 N4 Ga1 98.22(18) . . ?
N5 N4 C25 118.5(2) . . ?
N2 N1 Ga1 98.42(18) . . ?
N2 N1 C1 117.9(2) . . ?
C1 N1 Ga1 143.4(2) . . ?
C37 N6 Ga1 148.1(2) . . ?
N5 N6 Ga1 92.83(17) . . ?
N5 N6 C37 117.1(2) . . ?
C13 N3 Ga1 150.6(2) . . ?
N2 N3 Ga1 92.22(17) . . ?
N2 N3 C13 116.6(2) . . ?
C6 C1 C2 122.3(3) . . ?
C6 C1 N1 119.8(3) . . ?
C2 C1 N1 117.9(3) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_15
_database_code_depnum_ccdc_archive 'CCDC 1972007'
loop_
_audit_author_name
_audit_author_address
'Alasdair McKay'
;Monash University
Australia
;
_audit_update_record             
;
2019-12-14 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_audit_creation_date             2019-12-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
''
alasdair.mckay@monash.edu
_chemical_name_common            ?
_chemical_name_systematic        '[InH(N3Dipp2)2]'
_chemical_formula_moiety         'C48 H69 In N6'
_chemical_formula_sum            'C48 H69 In N6'
_chemical_formula_weight         844.91
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.667(5)
_cell_length_b                   16.510(6)
_cell_length_c                   21.164(6)
_cell_angle_alpha                90
_cell_angle_beta                 109.752(11)
_cell_angle_gamma                90
_cell_volume                     4823(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9778
_cell_measurement_temperature    150
_cell_measurement_theta_max      26.095
_cell_measurement_theta_min      2.388
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.526
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1233 before and 0.0587 after correction. The Ratio of minimum to maximum transmission is 0.8919. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       cube
_exptl_crystal_F_000             1792
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            46764
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         1.475
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8315
_reflns_number_total             10632
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.32B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.32B (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         10632
_refine_ls_number_restraints     311
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0330
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0416P)²+1.5584P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0935
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C11-C12 \\sim C11A-C12A
 with sigma of 0.04
 C10-C11 \\sim C10-C12 \\sim C10-C11A \\sim C10-C12A
 with sigma of 0.02
 C9-C8 \\sim C9A-C8A
 with sigma of 0.04
 C7-C9 \\sim C7-C8 \\sim C7-C9A \\sim C7-C8A
 with sigma of 0.02
 C36-C35 \\sim C35A-C36A
 with sigma of 0.04
 C34-C36 \\sim C34-C35 \\sim C34-C35A \\sim C34-C36A
 with sigma of 0.02
 C45-C44 \\sim C44A-C45A
 with sigma of 0.04
 C43-C45 \\sim C43-C44 \\sim C43-C44A \\sim C43-C45A
 with sigma of 0.02
 C20-C21 \\sim C21A-C20A
 with sigma of 0.04
 C19-C20 \\sim C19-C21 \\sim C19-C21A \\sim C19-C20A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C10 \\sim C12A \\sim C12 \\sim C11A \\sim C11: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C7 \\sim C9 \\sim C9A \\sim C8 \\sim C8A: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C34 \\sim C36 \\sim C36A \\sim C35 \\sim C35A: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C43 \\sim C45A \\sim C45 \\sim C44A \\sim C44: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C19 \\sim C21 \\sim C21A \\sim C20 \\sim C20A: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 C10, C12A, C12, C11A, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7, C9, C9A, C8, C8A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C34, C36, C36A, C35, C35A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C43, C45A, C45, C44A, C44
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C19, C21, C21A, C20, C20A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H10A)=Sof(C11A)=Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(C12A)=Sof(H12D)=
 Sof(H12E)=Sof(H12F)=1-FVAR(1)
 Sof(H10)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C12)=Sof(H12A)=Sof(H12B)=
 Sof(H12C)=FVAR(1)
 Sof(H7B)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=
 Sof(H8AC)=1-FVAR(2)
 Sof(H7A)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C8)=Sof(H8A)=Sof(H8B)=
 Sof(H8C)=FVAR(2)
 Sof(H34A)=Sof(C35A)=Sof(H35D)=Sof(H35E)=Sof(H35F)=Sof(C36A)=Sof(H36D)=
 Sof(H36E)=Sof(H36F)=1-FVAR(3)
 Sof(H34)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C35)=Sof(H35A)=Sof(H35B)=
 Sof(H35C)=FVAR(3)
 Sof(H43A)=Sof(C44A)=Sof(H44D)=Sof(H44E)=Sof(H44F)=Sof(C45A)=Sof(H45D)=
 Sof(H45E)=Sof(H45F)=1-FVAR(4)
 Sof(H43)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=Sof(C44)=Sof(H44A)=Sof(H44B)=
 Sof(H44C)=FVAR(4)
 Sof(H19A)=Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C20A)=Sof(H20D)=
 Sof(H20E)=Sof(H20F)=1-FVAR(5)
 Sof(H19)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C21)=Sof(H21A)=Sof(H21B)=
 Sof(H21C)=FVAR(5)
6.a Ternary CH refined with riding coordinates:
 C7(H7A), C7(H7B), C10(H10), C10(H10A), C34(H34), C34(H34A), C31(H31),
 C46(H46), C43(H43), C43(H43A), C22(H22), C19(H19), C19(H19A)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C3(H3), C29(H29), C28(H28), C27(H27), C39(H39), C40(H40),
 C41(H41), C16(H16), C15(H15), C17(H17)
6.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C36(H36A,H36B,
 H36C), C45(H45A,H45B,H45C), C44(H44A,H44B,H44C), C48(H48A,H48B,H48C), C47(H47A,
 H47B,H47C), C33(H33A,H33B,H33C), C32(H32A,H32B,H32C), C24(H24A,H24B,H24C),
 C23(H23A,H23B,H23C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C8(H8A,H8B,H8C),
  C35(H35A,H35B,H35C), C11A(H11D,H11E,H11F), C12A(H12D,H12E,H12F), C9A(H9AA,
 H9AB,H9AC), C8A(H8AA,H8AB,H8AC), C35A(H35D,H35E,H35F), C36A(H36D,H36E,H36F),
 C44A(H44D,H44E,H44F), C45A(H45D,H45E,H45F), C21A(H21D,H21E,H21F), C20A(H20D,
 H20E,H20F)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
In1 In 0.25633(2) 0.27280(2) 0.07439(2) 0.04222(6) Uani 1 1 d . . . . .
N2 N 0.38201(12) 0.17612(12) 0.16845(9) 0.0428(4) Uani 1 1 d . . . . .
C5 C 0.6546(2) 0.2534(3) 0.1473(2) 0.0932(11) Uani 1 1 d . . . . .
H5 H 0.691870 0.234050 0.121470 0.112 Uiso 1 1 calc R . . . .
N1 N 0.40500(12) 0.24522(11) 0.15018(9) 0.0420(4) Uani 1 1 d . . . . .
C4 C 0.6981(2) 0.3015(3) 0.2015(2) 0.1048(13) Uani 1 1 d . . . . .
H4 H 0.765098 0.313762 0.213489 0.126 Uiso 1 1 calc R . . . .
N6 N 0.20960(12) 0.38314(11) 0.11219(9) 0.0463(4) Uani 1 1 d . . . . .
C3 C 0.6460(2) 0.3321(2) 0.23839(18) 0.0829(10) Uani 1 1 d . . . . .
H3 H 0.676836 0.366719 0.275267 0.099 Uiso 1 1 calc R . . . .
N3 N 0.28932(12) 0.16511(11) 0.13995(9) 0.0442(4) Uani 1 1 d . . . . .
C2 C 0.54927(16) 0.31358(16) 0.22318(13) 0.0551(6) Uani 1 1 d . . . . .
N5 N 0.11691(12) 0.37055(12) 0.09053(9) 0.0452(4) Uani 1 1 d . . . . .
C7 C 0.49437(19) 0.34634(17) 0.26603(13) 0.0628(7) Uani 1 1 d D U . . .
H7A H 0.423975 0.333890 0.244036 0.075 Uiso 0.53(4) 1 calc R . P A 1
H7B H 0.424410 0.346393 0.237370 0.075 Uiso 0.47(4) 1 calc R . P A 2
N4 N 0.09962(12) 0.29956(11) 0.06375(9) 0.0411(4) Uani 1 1 d . . . . .
C9 C 0.5081(17) 0.4384(6) 0.2695(11) 0.093(4) Uani 0.53(4) 1 d D U P A 1
H9A H 0.577381 0.451088 0.287669 0.139 Uiso 0.53(4) 1 calc GR . P A 1
H9B H 0.475359 0.461550 0.298752 0.139 Uiso 0.53(4) 1 calc GR . P A 1
H9C H 0.480326 0.461407 0.224371 0.139 Uiso 0.53(4) 1 calc GR . P A 1
C6 C 0.55713(19) 0.23175(17) 0.12863(15) 0.0625(7) Uani 1 1 d . . . . .
C10 C 0.5100(2) 0.1793(2) 0.06805(14) 0.0794(9) Uani 1 1 d D U . . .
H10 H 0.438474 0.187262 0.055474 0.095 Uiso 0.44(4) 1 calc R . P B 1
H10A H 0.442165 0.167936 0.066189 0.095 Uiso 0.56(4) 1 calc R . P B 2
C11 C 0.530(2) 0.0884(8) 0.0856(11) 0.109(5) Uani 0.44(4) 1 d D U P B 1
H11A H 0.599362 0.077393 0.096311 0.163 Uiso 0.44(4) 1 calc GR . P B 1
H11B H 0.492789 0.055293 0.047085 0.163 Uiso 0.44(4) 1 calc GR . P B 1
H11C H 0.510874 0.075022 0.124406 0.163 Uiso 0.44(4) 1 calc GR . P B 1
C12 C 0.536(3) 0.196(2) 0.0048(12) 0.149(8) Uani 0.44(4) 1 d D U P B 1
H12A H 0.534579 0.254090 -0.003331 0.224 Uiso 0.44(4) 1 calc GR . P B 1
H12B H 0.488103 0.168890 -0.033738 0.224 Uiso 0.44(4) 1 calc GR . P B 1
H12C H 0.600367 0.174291 0.010957 0.224 Uiso 0.44(4) 1 calc GR . P B 1
C30 C -0.04146(18) 0.29192(17) -0.03880(13) 0.0586(6) Uani 1 1 d . . . . .
C29 C -0.1370(2) 0.2689(2) -0.07021(16) 0.0767(9) Uani 1 1 d . . . . .
H29 H -0.166523 0.277094 -0.117158 0.092 Uiso 1 1 calc R . . . .
C28 C -0.1893(2) 0.2345(2) -0.03472(18) 0.0811(9) Uani 1 1 d . . . . .
H28 H -0.254904 0.219655 -0.057067 0.097 Uiso 1 1 calc R . . . .
C27 C -0.1482(2) 0.22122(18) 0.03230(17) 0.0726(8) Uani 1 1 d . . . . .
H27 H -0.185694 0.196944 0.056018 0.087 Uiso 1 1 calc R . . . .
C26 C -0.05252(17) 0.24231(16) 0.06705(13) 0.0537(6) Uani 1 1 d . . . . .
C25 C -0.00008(15) 0.27906(13) 0.03083(11) 0.0445(5) Uani 1 1 d . . . . .
C34 C 0.0163(2) 0.3315(2) -0.07758(14) 0.0817(9) Uani 1 1 d D U . . .
H34 H 0.086422 0.319287 -0.054194 0.098 Uiso 0.814(14) 1 calc R . P C 1
H34A H 0.077757 0.351133 -0.043437 0.098 Uiso 0.186(14) 1 calc R . P C 2
C36 C 0.0019(5) 0.4244(3) -0.0770(4) 0.119(2) Uani 0.814(14) 1 d D U P C 1
H36A H -0.067014 0.437268 -0.097704 0.178 Uiso 0.814(14) 1 calc GR . P C 1
H36B H 0.038615 0.450710 -0.102317 0.178 Uiso 0.814(14) 1 calc GR . P C 1
H36C H 0.025148 0.444021 -0.030549 0.178 Uiso 0.814(14) 1 calc GR . P C 1
C31 C -0.0087(2) 0.22692(19) 0.14158(15) 0.0682(8) Uani 1 1 d . . . . .
H31 H 0.062942 0.234490 0.154208 0.082 Uiso 1 1 calc R . . . .
C39 C 0.2748(2) 0.55280(19) 0.23419(16) 0.0762(9) Uani 1 1 d . . . . .
H39 H 0.268725 0.568987 0.275670 0.091 Uiso 1 1 calc R . . . .
C40 C 0.3221(2) 0.6017(2) 0.20372(18) 0.0861(10) Uani 1 1 d . . . . .
H40 H 0.350269 0.650703 0.225000 0.103 Uiso 1 1 calc R . . . .
C41 C 0.3298(2) 0.58153(19) 0.14268(18) 0.0819(9) Uani 1 1 d . . . . .
H41 H 0.362646 0.616974 0.122203 0.098 Uiso 1 1 calc R . . . .
C42 C 0.29018(19) 0.50977(17) 0.11062(15) 0.0640(7) Uani 1 1 d . . . . .
C46 C 0.2983(2) 0.48894(19) 0.04311(16) 0.0777(8) Uani 1 1 d . . . . .
H46 H 0.253725 0.442228 0.025079 0.093 Uiso 1 1 calc R . . . .
C37 C 0.24437(16) 0.45905(15) 0.14369(13) 0.0527(6) Uani 1 1 d . . . . .
C38 C 0.23514(18) 0.47958(17) 0.20553(14) 0.0616(7) Uani 1 1 d . . . . .
C43 C 0.1868(2) 0.4248(2) 0.24277(16) 0.0762(8) Uani 1 1 d D U . . .
H43 H 0.166952 0.373545 0.216524 0.091 Uiso 0.55(2) 1 calc R . P D 1
H43A H 0.141687 0.389727 0.207332 0.091 Uiso 0.45(2) 1 calc R . P D 2
C45 C 0.2568(8) 0.4023(8) 0.3156(4) 0.101(3) Uani 0.55(2) 1 d D U P D 1
H45A H 0.319027 0.383691 0.313221 0.151 Uiso 0.55(2) 1 calc GR . P D 1
H45B H 0.227568 0.359139 0.334140 0.151 Uiso 0.55(2) 1 calc GR . P D 1
H45C H 0.267285 0.450191 0.344549 0.151 Uiso 0.55(2) 1 calc GR . P D 1
C44 C 0.0983(11) 0.4632(10) 0.2497(9) 0.115(5) Uani 0.55(2) 1 d D U P D 1
H44A H 0.115280 0.516114 0.271498 0.172 Uiso 0.55(2) 1 calc GR . P D 1
H44B H 0.072265 0.428355 0.277029 0.172 Uiso 0.55(2) 1 calc GR . P D 1
H44C H 0.049398 0.470281 0.205150 0.172 Uiso 0.55(2) 1 calc GR . P D 1
C22 C 0.2950(2) 0.1304(2) 0.27934(14) 0.0736(8) Uani 1 1 d . . . . .
H22 H 0.315660 0.180868 0.261763 0.088 Uiso 1 1 calc R . . . .
C16 C 0.1515(2) -0.0415(2) 0.1747(2) 0.0901(11) Uani 1 1 d . . . . .
H16 H 0.117221 -0.087691 0.181382 0.108 Uiso 1 1 calc R . . . .
C15 C 0.1552(2) -0.02590(19) 0.1120(2) 0.0822(10) Uani 1 1 d . . . . .
H15 H 0.124634 -0.062151 0.076257 0.099 Uiso 1 1 calc R . . . .
C17 C 0.1963(2) 0.0080(2) 0.22760(19) 0.0812(10) Uani 1 1 d . . . . .
H17 H 0.193745 -0.004785 0.270733 0.097 Uiso 1 1 calc R . . . .
C18 C 0.24553(17) 0.07692(17) 0.21953(14) 0.0610(7) Uani 1 1 d . . . . .
C13 C 0.24735(15) 0.09266(15) 0.15446(13) 0.0501(6) Uani 1 1 d . . . . .
C14 C 0.20258(18) 0.04163(16) 0.09973(15) 0.0635(7) Uani 1 1 d . . . . .
C19 C 0.2086(2) 0.0570(2) 0.03089(16) 0.0792(9) Uani 1 1 d D U . . .
H19 H 0.252658 0.104708 0.036862 0.095 Uiso 0.61(3) 1 calc R . P E 1
H19A H 0.222618 0.115698 0.027177 0.095 Uiso 0.39(3) 1 calc R . P E 2
C1 C 0.50565(15) 0.26259(14) 0.16830(12) 0.0460(5) Uani 1 1 d . . . . .
C48 C 0.2647(5) 0.5573(3) -0.0084(2) 0.166(2) Uani 1 1 d . . . . .
H48A H 0.198520 0.573134 -0.012710 0.249 Uiso 1 1 calc GR . . . .
H48B H 0.266216 0.538536 -0.051989 0.249 Uiso 1 1 calc GR . . . .
H48C H 0.307984 0.603974 0.006470 0.249 Uiso 1 1 calc GR . . . .
C47 C 0.3987(3) 0.4603(3) 0.0494(2) 0.1395(18) Uani 1 1 d . . . . .
H47A H 0.443651 0.506214 0.061087 0.209 Uiso 1 1 calc GR . . . .
H47B H 0.397801 0.437058 0.006614 0.209 Uiso 1 1 calc GR . . . .
H47C H 0.419798 0.419036 0.084663 0.209 Uiso 1 1 calc GR . . . .
C33 C -0.0254(3) 0.1416(3) 0.1607(2) 0.1124(14) Uani 1 1 d . . . . .
H33A H -0.094756 0.133224 0.151845 0.169 Uiso 1 1 calc GR . . . .
H33B H 0.010201 0.133086 0.208543 0.169 Uiso 1 1 calc GR . . . .
H33C H -0.002500 0.103119 0.134138 0.169 Uiso 1 1 calc GR . . . .
C32 C -0.0450(4) 0.2905(3) 0.1795(2) 0.1253(16) Uani 1 1 d . . . . .
H32A H -0.111050 0.276778 0.177330 0.188 Uiso 1 1 calc GR . . . .
H32B H -0.045045 0.343715 0.159060 0.188 Uiso 1 1 calc GR . . . .
H32C H -0.002440 0.291748 0.226500 0.188 Uiso 1 1 calc GR . . . .
C24 C 0.2295(3) 0.1563(3) 0.3188(2) 0.1349(17) Uani 1 1 d . . . . .
H24A H 0.179858 0.193735 0.291572 0.202 Uiso 1 1 calc GR . . . .
H24B H 0.268545 0.183422 0.360373 0.202 Uiso 1 1 calc GR . . . .
H24C H 0.198289 0.108476 0.329790 0.202 Uiso 1 1 calc GR . . . .
C23 C 0.3851(3) 0.0918(3) 0.3270(2) 0.1335(18) Uani 1 1 d . . . . .
H23A H 0.367389 0.042604 0.346150 0.200 Uiso 1 1 calc GR . . . .
H23B H 0.417260 0.129834 0.363201 0.200 Uiso 1 1 calc GR . . . .
H23C H 0.429096 0.077652 0.302720 0.200 Uiso 1 1 calc GR . . . .
C20 C 0.2561(12) -0.0099(10) 0.0022(11) 0.118(4) Uani 0.61(3) 1 d D U P E 1
H20A H 0.315582 -0.028335 0.036938 0.177 Uiso 0.61(3) 1 calc GR . P E 1
H20B H 0.271937 0.011473 -0.036076 0.177 Uiso 0.61(3) 1 calc GR . P E 1
H20C H 0.211215 -0.055548 -0.012673 0.177 Uiso 0.61(3) 1 calc GR . P E 1
C21 C 0.1141(8) 0.0833(13) -0.0224(6) 0.112(4) Uani 0.61(3) 1 d D U P E 1
H21A H 0.066262 0.039630 -0.029957 0.168 Uiso 0.61(3) 1 calc GR . P E 1
H21B H 0.125778 0.095139 -0.064348 0.168 Uiso 0.61(3) 1 calc GR . P E 1
H21C H 0.089453 0.131912 -0.007027 0.168 Uiso 0.61(3) 1 calc GR . P E 1
C8 C 0.5287(17) 0.3113(17) 0.3370(8) 0.117(5) Uani 0.53(4) 1 d D U P A 1
H8A H 0.532721 0.252172 0.334706 0.175 Uiso 0.53(4) 1 calc GR . P A 1
H8B H 0.482583 0.325907 0.359564 0.175 Uiso 0.53(4) 1 calc GR . P A 1
H8C H 0.592671 0.333285 0.362343 0.175 Uiso 0.53(4) 1 calc GR . P A 1
C35 C -0.0116(6) 0.3020(7) -0.1494(3) 0.145(4) Uani 0.814(14) 1 d D U P C 1
H35A H 0.005557 0.244636 -0.149698 0.217 Uiso 0.814(14) 1 calc GR . P C 1
H35B H 0.023105 0.333641 -0.173258 0.217 Uiso 0.814(14) 1 calc GR . P C 1
H35C H -0.081582 0.308531 -0.171853 0.217 Uiso 0.814(14) 1 calc GR . P C 1
H1 H 0.2676(18) 0.2685(14) -0.0024(13) 0.060(7) Uiso 1 1 d . . . . .
C11A C 0.5615(15) 0.0997(10) 0.0739(12) 0.131(6) Uani 0.56(4) 1 d D U P B 2
H11D H 0.628068 0.109028 0.075267 0.197 Uiso 0.56(4) 1 calc GR . P B 2
H11E H 0.527520 0.065693 0.035162 0.197 Uiso 0.56(4) 1 calc GR . P B 2
H11F H 0.562429 0.072326 0.115257 0.197 Uiso 0.56(4) 1 calc GR . P B 2
C12A C 0.505(2) 0.2270(15) 0.0052(8) 0.150(6) Uani 0.56(4) 1 d D U P B 2
H12D H 0.468522 0.277320 0.003708 0.225 Uiso 0.56(4) 1 calc GR . P B 2
H12E H 0.471662 0.194459 -0.034736 0.225 Uiso 0.56(4) 1 calc GR . P B 2
H12F H 0.570340 0.239937 0.006171 0.225 Uiso 0.56(4) 1 calc GR . P B 2
C9A C 0.517(2) 0.4305(9) 0.2954(15) 0.107(6) Uani 0.47(4) 1 d D U P A 2
H9AA H 0.580467 0.430666 0.330696 0.161 Uiso 0.47(4) 1 calc GR . P A 2
H9AB H 0.467256 0.446684 0.314643 0.161 Uiso 0.47(4) 1 calc GR . P A 2
H9AC H 0.516716 0.468781 0.260046 0.161 Uiso 0.47(4) 1 calc GR . P A 2
C8A C 0.5049(10) 0.2839(10) 0.3226(6) 0.078(3) Uani 0.47(4) 1 d D U P A 2
H8AA H 0.487749 0.229923 0.302935 0.117 Uiso 0.47(4) 1 calc GR . P A 2
H8AB H 0.461630 0.298709 0.347294 0.117 Uiso 0.47(4) 1 calc GR . P A 2
H8AC H 0.572054 0.283582 0.353370 0.117 Uiso 0.47(4) 1 calc GR . P A 2
C35A C 0.046(3) 0.2611(14) -0.1176(18) 0.127(10) Uani 0.186(14) 1 d D U P C 2
H35D H 0.091509 0.224506 -0.085829 0.191 Uiso 0.186(14) 1 calc GR . P C 2
H35E H 0.076437 0.284319 -0.148041 0.191 Uiso 0.186(14) 1 calc GR . P C 2
H35F H -0.012154 0.230770 -0.143610 0.191 Uiso 0.186(14) 1 calc GR . P C 2
C36A C -0.024(2) 0.4014(18) -0.1244(19) 0.143(11) Uani 0.186(14) 1 d D U P C 2
H36D H -0.090399 0.389575 -0.152552 0.214 Uiso 0.186(14) 1 calc GR . P C 2
H36E H 0.016156 0.409609 -0.152964 0.214 Uiso 0.186(14) 1 calc GR . P C 2
H36F H -0.022228 0.450567 -0.098158 0.214 Uiso 0.186(14) 1 calc GR . P C 2
C44A C 0.1228(15) 0.4692(15) 0.2746(9) 0.133(7) Uani 0.45(2) 1 d D U P D 2
H44D H 0.163176 0.493325 0.317160 0.200 Uiso 0.45(2) 1 calc GR . P D 2
H44E H 0.077042 0.431006 0.282911 0.200 Uiso 0.45(2) 1 calc GR . P D 2
H44F H 0.086980 0.512010 0.244221 0.200 Uiso 0.45(2) 1 calc GR . P D 2
C45A C 0.2535(12) 0.3702(12) 0.2872(13) 0.166(8) Uani 0.45(2) 1 d D U P D 2
H45D H 0.299835 0.350965 0.266323 0.249 Uiso 0.45(2) 1 calc GR . P D 2
H45E H 0.218176 0.323989 0.296577 0.249 Uiso 0.45(2) 1 calc GR . P D 2
H45F H 0.288493 0.398189 0.329285 0.249 Uiso 0.45(2) 1 calc GR . P D 2
C21A C 0.1074(10) 0.038(2) -0.0205(8) 0.118(6) Uani 0.39(3) 1 d D U P E 2
H21D H 0.095392 -0.020802 -0.020511 0.178 Uiso 0.39(3) 1 calc GR . P E 2
H21E H 0.105077 0.054551 -0.065382 0.178 Uiso 0.39(3) 1 calc GR . P E 2
H21F H 0.057750 0.066742 -0.008097 0.178 Uiso 0.39(3) 1 calc GR . P E 2
C20A C 0.2907(19) 0.008(2) 0.0232(17) 0.144(10) Uani 0.39(3) 1 d D U P E 2
H20D H 0.349003 0.016469 0.062499 0.216 Uiso 0.39(3) 1 calc GR . P E 2
H20E H 0.303287 0.025262 -0.017355 0.216 Uiso 0.39(3) 1 calc GR . P E 2
H20F H 0.273374 -0.049525 0.019606 0.216 Uiso 0.39(3) 1 calc GR . P E 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
In1 N1 2.2739(18) . ?
In1 N6 2.1906(19) . ?
In1 N3 2.2061(19) . ?
In1 N4 2.2758(18) . ?
In1 H1 1.69(3) . ?
N2 N1 1.286(3) . ?
N2 N3 1.300(2) . ?
C5 H5 0.9500 . ?
C5 C4 1.362(5) . ?
C5 C6 1.395(4) . ?
N1 C1 1.423(3) . ?
C4 H4 0.9500 . ?
C4 C3 1.361(5) . ?
N6 N5 1.296(2) . ?
N6 C37 1.430(3) . ?
C3 H3 0.9500 . ?
C3 C2 1.379(3) . ?
N3 C13 1.425(3) . ?
C2 C7 1.502(4) . ?
C2 C1 1.402(3) . ?
N5 N4 1.289(3) . ?
C7 H7A 1.0000 . ?
C7 H7B 1.0000 . ?
C7 C9 1.531(10) . ?
C7 C8 1.528(10) . ?
C7 C9A 1.513(11) . ?
C7 C8A 1.547(10) . ?
N4 C25 1.432(3) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C6 C10 1.508(4) . ?
C6 C1 1.401(3) . ?
C10 H10 1.0000 . ?
C10 H10A 1.0000 . ?
C10 C11 1.550(12) . ?
C10 C12 1.531(11) . ?
C10 C11A 1.500(10) . ?
C10 C12A 1.526(10) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C30 C29 1.386(4) . ?
C30 C25 1.407(3) . ?
C30 C34 1.512(4) . ?
C29 H29 0.9500 . ?
C29 C28 1.366(5) . ?
C28 H28 0.9500 . ?
C28 C27 1.358(5) . ?
C27 H27 0.9500 . ?
C27 C26 1.390(4) . ?
C26 C25 1.395(3) . ?
C26 C31 1.510(4) . ?
C34 H34 1.0000 . ?
C34 H34A 1.0000 . ?
C34 C36 1.549(6) . ?
C34 C35 1.516(6) . ?
C34 C35A 1.583(14) . ?
C34 C36A 1.505(14) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C31 H31 1.0000 . ?
C31 C33 1.508(5) . ?
C31 C32 1.523(5) . ?
C39 H39 0.9500 . ?
C39 C40 1.361(5) . ?
C39 C38 1.389(4) . ?
C40 H40 0.9500 . ?
C40 C41 1.376(5) . ?
C41 H41 0.9500 . ?
C41 C42 1.391(4) . ?
C42 C46 1.513(4) . ?
C42 C37 1.400(4) . ?
C46 H46 1.0000 . ?
C46 C48 1.530(5) . ?
C46 C47 1.508(5) . ?
C37 C38 1.402(4) . ?
C38 C43 1.523(4) . ?
C43 H43 1.0000 . ?
C43 H43A 1.0000 . ?
C43 C45 1.581(7) . ?
C43 C44 1.495(9) . ?
C43 C44A 1.516(11) . ?
C43 C45A 1.426(11) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C22 H22 1.0000 . ?
C22 C18 1.513(4) . ?
C22 C24 1.532(5) . ?
C22 C23 1.507(4) . ?
C16 H16 0.9500 . ?
C16 C15 1.370(5) . ?
C16 C17 1.363(5) . ?
C15 H15 0.9500 . ?
C15 C14 1.384(4) . ?
C17 H17 0.9500 . ?
C17 C18 1.388(4) . ?
C18 C13 1.411(4) . ?
C13 C14 1.403(4) . ?
C14 C19 1.510(4) . ?
C19 H19 1.0000 . ?
C19 H19A 1.0000 . ?
C19 C20 1.537(9) . ?
C19 C21 1.525(8) . ?
C19 C21A 1.548(10) . ?
C19 C20A 1.504(12) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C11A H11D 0.9800 . ?
C11A H11E 0.9800 . ?
C11A H11F 0.9800 . ?
C12A H12D 0.9800 . ?
C12A H12E 0.9800 . ?
C12A H12F 0.9800 . ?
C9A H9AA 0.9800 . ?
C9A H9AB 0.9800 . ?
C9A H9AC 0.9800 . ?
C8A H8AA 0.9800 . ?
C8A H8AB 0.9800 . ?
C8A H8AC 0.9800 . ?
C35A H35D 0.9800 . ?
C35A H35E 0.9800 . ?
C35A H35F 0.9800 . ?
C36A H36D 0.9800 . ?
C36A H36E 0.9800 . ?
C36A H36F 0.9800 . ?
C44A H44D 0.9800 . ?
C44A H44E 0.9800 . ?
C44A H44F 0.9800 . ?
C45A H45D 0.9800 . ?
C45A H45E 0.9800 . ?
C45A H45F 0.9800 . ?
C21A H21D 0.9800 . ?
C21A H21E 0.9800 . ?
C21A H21F 0.9800 . ?
C20A H20D 0.9800 . ?
C20A H20E 0.9800 . ?
C20A H20F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 In1 N4 143.55(6) . . ?
N1 In1 H1 106.7(9) . . ?
N6 In1 N1 104.64(7) . . ?
N6 In1 N3 118.02(7) . . ?
N6 In1 N4 56.26(7) . . ?
N6 In1 H1 122.1(8) . . ?
N3 In1 N1 56.00(6) . . ?
N3 In1 N4 102.61(6) . . ?
N3 In1 H1 119.9(8) . . ?
N4 In1 H1 109.7(9) . . ?
N1 N2 N3 108.91(17) . . ?
C4 C5 H5 118.9 . . ?
C4 C5 C6 122.1(3) . . ?
C6 C5 H5 118.9 . . ?
N2 N1 In1 95.93(12) . . ?
N2 N1 C1 116.83(18) . . ?
C1 N1 In1 144.07(15) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 C5 120.3(3) . . ?
C3 C4 H4 119.8 . . ?
N5 N6 In1 99.07(13) . . ?
N5 N6 C37 118.13(18) . . ?
C37 N6 In1 142.44(15) . . ?
C4 C3 H3 119.4 . . ?
C4 C3 C2 121.1(3) . . ?
C2 C3 H3 119.4 . . ?
N2 N3 In1 98.72(13) . . ?
N2 N3 C13 118.51(17) . . ?
C13 N3 In1 142.46(13) . . ?
C3 C2 C7 119.9(2) . . ?
C3 C2 C1 118.1(2) . . ?
C1 C2 C7 121.9(2) . . ?
N4 N5 N6 109.16(17) . . ?
C2 C7 H7A 108.9 . . ?
C2 C7 H7B 106.5 . . ?
C2 C7 C9 107.3(10) . . ?
C2 C7 C8 113.1(7) . . ?
C2 C7 C9A 119.6(11) . . ?
C2 C7 C8A 107.1(6) . . ?
C9 C7 H7A 108.9 . . ?
C8 C7 H7A 108.9 . . ?
C8 C7 C9 109.5(9) . . ?
C9A C7 H7B 106.5 . . ?
C9A C7 C8A 110.0(9) . . ?
C8A C7 H7B 106.5 . . ?
N5 N4 In1 95.22(12) . . ?
N5 N4 C25 116.48(17) . . ?
C25 N4 In1 146.46(14) . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C5 C6 C10 121.3(3) . . ?
C5 C6 C1 116.4(3) . . ?
C1 C6 C10 122.2(2) . . ?
C6 C10 H10 106.8 . . ?
C6 C10 H10A 107.8 . . ?
C6 C10 C11 110.9(9) . . ?
C6 C10 C12 117.7(15) . . ?
C6 C10 C12A 108.6(10) . . ?
C11 C10 H10 106.8 . . ?
C12 C10 H10 106.8 . . ?
C12 C10 C11 107.3(11) . . ?
C11A C10 C6 111.1(8) . . ?
C11A C10 H10A 107.8 . . ?
C11A C10 C12A 113.7(8) . . ?
C12A C10 H10A 107.8 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C29 C30 C25 118.0(3) . . ?
C29 C30 C34 121.3(2) . . ?
C25 C30 C34 120.7(2) . . ?
C30 C29 H29 119.5 . . ?
C28 C29 C30 121.0(3) . . ?
C28 C29 H29 119.5 . . ?
C29 C28 H28 119.7 . . ?
C27 C28 C29 120.5(3) . . ?
C27 C28 H28 119.7 . . ?
C28 C27 H27 119.2 . . ?
C28 C27 C26 121.6(3) . . ?
C26 C27 H27 119.2 . . ?
C27 C26 C25 117.6(2) . . ?
C27 C26 C31 120.5(2) . . ?
C25 C26 C31 121.9(2) . . ?
C30 C25 N4 118.8(2) . . ?
C26 C25 N4 119.8(2) . . ?
C26 C25 C30 121.2(2) . . ?
C30 C34 H34 108.4 . . ?
C30 C34 H34A 106.4 . . ?
C30 C34 C36 108.7(3) . . ?
C30 C34 C35 113.3(4) . . ?
C30 C34 C35A 106.1(11) . . ?
C36 C34 H34 108.4 . . ?
C35 C34 H34 108.4 . . ?
C35 C34 C36 109.6(5) . . ?
C35A C34 H34A 106.4 . . ?
C36A C34 C30 121.7(14) . . ?
C36A C34 H34A 106.4 . . ?
C36A C34 C35A 109.1(15) . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C26 C31 H31 107.2 . . ?
C26 C31 C32 109.5(3) . . ?
C33 C31 C26 112.8(3) . . ?
C33 C31 H31 107.2 . . ?
C33 C31 C32 112.6(3) . . ?
C32 C31 H31 107.2 . . ?
C40 C39 H39 119.5 . . ?
C40 C39 C38 121.0(3) . . ?
C38 C39 H39 119.5 . . ?
C39 C40 H40 119.4 . . ?
C39 C40 C41 121.3(3) . . ?
C41 C40 H40 119.4 . . ?
C40 C41 H41 119.7 . . ?
C40 C41 C42 120.7(3) . . ?
C42 C41 H41 119.7 . . ?
C41 C42 C46 120.0(3) . . ?
C41 C42 C37 117.2(3) . . ?
C37 C42 C46 122.7(2) . . ?
C42 C46 H46 106.6 . . ?
C42 C46 C48 113.3(3) . . ?
C48 C46 H46 106.6 . . ?
C47 C46 C42 112.0(3) . . ?
C47 C46 H46 106.6 . . ?
C47 C46 C48 111.3(4) . . ?
C42 C37 N6 116.5(2) . . ?
C42 C37 C38 122.4(2) . . ?
C38 C37 N6 121.0(2) . . ?
C39 C38 C37 117.4(3) . . ?
C39 C38 C43 119.4(3) . . ?
C37 C38 C43 123.2(2) . . ?
C38 C43 H43 108.3 . . ?
C38 C43 H43A 105.2 . . ?
C38 C43 C45 112.4(5) . . ?
C45 C43 H43 108.3 . . ?
C44 C43 C38 111.7(6) . . ?
C44 C43 H43 108.3 . . ?
C44 C43 C45 107.7(7) . . ?
C44A C43 C38 114.1(10) . . ?
C44A C43 H43A 105.2 . . ?
C45A C43 C38 112.4(7) . . ?
C45A C43 H43A 105.2 . . ?
C45A C43 C44A 113.7(10) . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C18 C22 H22 107.2 . . ?
C18 C22 C24 114.1(3) . . ?
C24 C22 H22 107.2 . . ?
C23 C22 H22 107.2 . . ?
C23 C22 C18 112.1(3) . . ?
C23 C22 C24 108.8(3) . . ?
C15 C16 H16 119.4 . . ?
C17 C16 H16 119.4 . . ?
C17 C16 C15 121.1(3) . . ?
C16 C15 H15 119.3 . . ?
C16 C15 C14 121.3(3) . . ?
C14 C15 H15 119.3 . . ?
C16 C17 H17 119.4 . . ?
C16 C17 C18 121.1(3) . . ?
C18 C17 H17 119.4 . . ?
C17 C18 C22 119.9(3) . . ?
C17 C18 C13 117.0(3) . . ?
C13 C18 C22 123.2(2) . . ?
C18 C13 N3 121.1(2) . . ?
C14 C13 N3 116.2(2) . . ?
C14 C13 C18 122.5(2) . . ?
C15 C14 C13 117.0(3) . . ?
C15 C14 C19 120.8(3) . . ?
C13 C14 C19 122.2(2) . . ?
C14 C19 H19 104.8 . . ?
C14 C19 H19A 108.6 . . ?
C14 C19 C20 116.3(9) . . ?
C14 C19 C21 115.2(6) . . ?
C14 C19 C21A 106.8(8) . . ?
C20 C19 H19 104.8 . . ?
C21 C19 H19 104.8 . . ?
C21 C19 C20 109.4(7) . . ?
C21A C19 H19A 108.6 . . ?
C20A C19 C14 108.9(14) . . ?
C20A C19 H19A 108.6 . . ?
C20A C19 C21A 115.2(11) . . ?
C2 C1 N1 119.0(2) . . ?
C6 C1 N1 119.0(2) . . ?
C6 C1 C2 121.8(2) . . ?
C46 C48 H48A 109.5 . . ?
C46 C48 H48B 109.5 . . ?
C46 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C10 C11A H11D 109.5 . . ?
C10 C11A H11E 109.5 . . ?
C10 C11A H11F 109.5 . . ?
H11D C11A H11E 109.5 . . ?
H11D C11A H11F 109.5 . . ?
H11E C11A H11F 109.5 . . ?
C10 C12A H12D 109.5 . . ?
C10 C12A H12E 109.5 . . ?
C10 C12A H12F 109.5 . . ?
H12D C12A H12E 109.5 . . ?
H12D C12A H12F 109.5 . . ?
H12E C12A H12F 109.5 . . ?
C7 C9A H9AA 109.5 . . ?
C7 C9A H9AB 109.5 . . ?
C7 C9A H9AC 109.5 . . ?
H9AA C9A H9AB 109.5 . . ?
H9AA C9A H9AC 109.5 . . ?
H9AB C9A H9AC 109.5 . . ?
C7 C8A H8AA 109.5 . . ?
C7 C8A H8AB 109.5 . . ?
C7 C8A H8AC 109.5 . . ?
H8AA C8A H8AB 109.5 . . ?
H8AA C8A H8AC 109.5 . . ?
H8AB C8A H8AC 109.5 . . ?
C34 C35A H35D 109.5 . . ?
C34 C35A H35E 109.5 . . ?
C34 C35A H35F 109.5 . . ?
H35D C35A H35E 109.5 . . ?
H35D C35A H35F 109.5 . . ?
H35E C35A H35F 109.5 . . ?
C34 C36A H36D 109.5 . . ?
C34 C36A H36E 109.5 . . ?
C34 C36A H36F 109.5 . . ?
H36D C36A H36E 109.5 . . ?
H36D C36A H36F 109.5 . . ?
H36E C36A H36F 109.5 . . ?
C43 C44A H44D 109.5 . . ?
C43 C44A H44E 109.5 . . ?
C43 C44A H44F 109.5 . . ?
H44D C44A H44E 109.5 . . ?
H44D C44A H44F 109.5 . . ?
H44E C44A H44F 109.5 . . ?
C43 C45A H45D 109.5 . . ?
C43 C45A H45E 109.5 . . ?
C43 C45A H45F 109.5 . . ?
H45D C45A H45E 109.5 . . ?
H45D C45A H45F 109.5 . . ?
H45E C45A H45F 109.5 . . ?
C19 C21A H21D 109.5 . . ?
C19 C21A H21E 109.5 . . ?
C19 C21A H21F 109.5 . . ?
H21D C21A H21E 109.5 . . ?
H21D C21A H21F 109.5 . . ?
H21E C21A H21F 109.5 . . ?
C19 C20A H20D 109.5 . . ?
C19 C20A H20E 109.5 . . ?
C19 C20A H20F 109.5 . . ?
H20D C20A H20E 109.5 . . ?
H20D C20A H20F 109.5 . . ?
H20E C20A H20F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
In1 N1 C1 C2 104.8(3) . . . . ?
In1 N1 C1 C6 -71.8(3) . . . . ?
In1 N6 N5 N4 5.18(18) . . . . ?
In1 N6 C37 C42 56.4(3) . . . . ?
In1 N6 C37 C38 -121.7(3) . . . . ?
In1 N3 C13 C18 -122.5(2) . . . . ?
In1 N3 C13 C14 53.2(3) . . . . ?
In1 N4 C25 C30 -64.9(3) . . . . ?
In1 N4 C25 C26 111.1(3) . . . . ?
N2 N1 C1 C2 -101.6(3) . . . . ?
N2 N1 C1 C6 81.7(3) . . . . ?
N2 N3 C13 C18 65.5(3) . . . . ?
N2 N3 C13 C14 -118.8(2) . . . . ?
C5 C4 C3 C2 1.7(7) . . . . ?
C5 C6 C10 C11 82.9(13) . . . . ?
C5 C6 C10 C12 -41.2(17) . . . . ?
C5 C6 C10 C11A 57.8(13) . . . . ?
C5 C6 C10 C12A -67.9(13) . . . . ?
C5 C6 C1 N1 177.5(3) . . . . ?
C5 C6 C1 C2 1.0(4) . . . . ?
N1 N2 N3 In1 6.33(17) . . . . ?
N1 N2 N3 C13 -178.57(19) . . . . ?
C4 C5 C6 C10 179.3(4) . . . . ?
C4 C5 C6 C1 0.5(6) . . . . ?
C4 C3 C2 C7 178.3(4) . . . . ?
C4 C3 C2 C1 -0.3(5) . . . . ?
N6 N5 N4 In1 -4.95(17) . . . . ?
N6 N5 N4 C25 -173.63(18) . . . . ?
N6 C37 C38 C39 177.1(2) . . . . ?
N6 C37 C38 C43 -1.2(4) . . . . ?
C3 C2 C7 C9 53.9(9) . . . . ?
C3 C2 C7 C8 -67.0(15) . . . . ?
C3 C2 C7 C9A 36.2(15) . . . . ?
C3 C2 C7 C8A -89.6(7) . . . . ?
C3 C2 C1 N1 -177.6(3) . . . . ?
C3 C2 C1 C6 -1.1(4) . . . . ?
N3 N2 N1 In1 -6.10(17) . . . . ?
N3 N2 N1 C1 -170.85(18) . . . . ?
N3 C13 C14 C15 -175.3(2) . . . . ?
N3 C13 C14 C19 7.1(3) . . . . ?
N5 N6 C37 C42 -114.9(2) . . . . ?
N5 N6 C37 C38 67.1(3) . . . . ?
N5 N4 C25 C30 94.3(3) . . . . ?
N5 N4 C25 C26 -89.6(3) . . . . ?
C7 C2 C1 N1 3.8(4) . . . . ?
C7 C2 C1 C6 -179.6(3) . . . . ?
C6 C5 C4 C3 -1.8(7) . . . . ?
C10 C6 C1 N1 -1.3(4) . . . . ?
C10 C6 C1 C2 -177.8(3) . . . . ?
C30 C29 C28 C27 -0.8(5) . . . . ?
C29 C30 C25 N4 177.6(2) . . . . ?
C29 C30 C25 C26 1.6(4) . . . . ?
C29 C30 C34 C36 89.4(5) . . . . ?
C29 C30 C34 C35 -32.7(7) . . . . ?
C29 C30 C34 C35A -76.8(17) . . . . ?
C29 C30 C34 C36A 49(2) . . . . ?
C29 C28 C27 C26 0.3(5) . . . . ?
C28 C27 C26 C25 1.0(4) . . . . ?
C28 C27 C26 C31 180.0(3) . . . . ?
C27 C26 C25 N4 -178.0(2) . . . . ?
C27 C26 C25 C30 -2.0(4) . . . . ?
C27 C26 C31 C33 49.6(4) . . . . ?
C27 C26 C31 C32 -76.6(4) . . . . ?
C25 C30 C29 C28 -0.2(5) . . . . ?
C25 C30 C34 C36 -89.2(4) . . . . ?
C25 C30 C34 C35 148.7(6) . . . . ?
C25 C30 C34 C35A 104.6(17) . . . . ?
C25 C30 C34 C36A -130(2) . . . . ?
C25 C26 C31 C33 -131.5(3) . . . . ?
C25 C26 C31 C32 102.3(3) . . . . ?
C34 C30 C29 C28 -178.8(3) . . . . ?
C34 C30 C25 N4 -3.8(4) . . . . ?
C34 C30 C25 C26 -179.7(3) . . . . ?
C31 C26 C25 N4 3.1(4) . . . . ?
C31 C26 C25 C30 179.0(3) . . . . ?
C39 C40 C41 C42 -0.7(5) . . . . ?
C39 C38 C43 C45 -56.4(6) . . . . ?
C39 C38 C43 C44 64.8(10) . . . . ?
C39 C38 C43 C44A 42.6(10) . . . . ?
C39 C38 C43 C45A -88.8(14) . . . . ?
C40 C39 C38 C37 -1.1(4) . . . . ?
C40 C39 C38 C43 177.2(3) . . . . ?
C40 C41 C42 C46 179.3(3) . . . . ?
C40 C41 C42 C37 -1.3(4) . . . . ?
C41 C42 C46 C48 -51.2(5) . . . . ?
C41 C42 C46 C47 75.7(4) . . . . ?
C41 C42 C37 N6 -176.0(2) . . . . ?
C41 C42 C37 C38 2.0(4) . . . . ?
C42 C37 C38 C39 -0.9(4) . . . . ?
C42 C37 C38 C43 -179.2(2) . . . . ?
C46 C42 C37 N6 3.4(4) . . . . ?
C46 C42 C37 C38 -178.5(3) . . . . ?
C37 N6 N5 N4 179.8(2) . . . . ?
C37 C42 C46 C48 129.3(4) . . . . ?
C37 C42 C46 C47 -103.7(4) . . . . ?
C37 C38 C43 C45 121.9(6) . . . . ?
C37 C38 C43 C44 -116.9(9) . . . . ?
C37 C38 C43 C44A -139.1(10) . . . . ?
C37 C38 C43 C45A 89.5(14) . . . . ?
C38 C39 C40 C41 1.9(5) . . . . ?
C22 C18 C13 N3 -5.8(4) . . . . ?
C22 C18 C13 C14 178.8(2) . . . . ?
C16 C15 C14 C13 0.6(4) . . . . ?
C16 C15 C14 C19 178.2(3) . . . . ?
C16 C17 C18 C22 -179.6(3) . . . . ?
C16 C17 C18 C13 -0.3(4) . . . . ?
C15 C16 C17 C18 1.3(5) . . . . ?
C15 C14 C19 C20 -58.0(9) . . . . ?
C15 C14 C19 C21 72.1(10) . . . . ?
C15 C14 C19 C21A 42.6(14) . . . . ?
C15 C14 C19 C20A -82.4(17) . . . . ?
C17 C16 C15 C14 -1.4(5) . . . . ?
C17 C18 C13 N3 175.0(2) . . . . ?
C17 C18 C13 C14 -0.5(4) . . . . ?
C18 C13 C14 C15 0.3(4) . . . . ?
C18 C13 C14 C19 -177.3(2) . . . . ?
C13 C14 C19 C20 119.5(8) . . . . ?
C13 C14 C19 C21 -110.4(10) . . . . ?
C13 C14 C19 C21A -140.0(13) . . . . ?
C13 C14 C19 C20A 95.1(17) . . . . ?
C1 C2 C7 C9 -127.6(9) . . . . ?
C1 C2 C7 C8 111.5(14) . . . . ?
C1 C2 C7 C9A -145.2(15) . . . . ?
C1 C2 C7 C8A 88.9(7) . . . . ?
C1 C6 C10 C11 -98.4(12) . . . . ?
C1 C6 C10 C12 137.6(17) . . . . ?
C1 C6 C10 C11A -123.4(13) . . . . ?
C1 C6 C10 C12A 110.9(13) . . . . ?
C24 C22 C18 C17 -51.8(4) . . . . ?
C24 C22 C18 C13 128.9(3) . . . . ?
C23 C22 C18 C17 72.4(4) . . . . ?
C23 C22 C18 C13 -106.8(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_16
_database_code_depnum_ccdc_archive 'CCDC 1972008'
loop_
_audit_author_name
_audit_author_address
'Alasdair McKay'
;Monash University
Australia
;
_audit_update_record             
;
2019-12-14 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_audit_creation_date             2019-12-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
''
alasdair.mckay@monash.edu
_chemical_name_common            ?
_chemical_name_systematic        '[TlCl(N3Dipp2)2]'
_chemical_formula_moiety         'C48 H68 Cl N6 Tl'
_chemical_formula_sum            'C48 H68 Cl N6 Tl'
_chemical_formula_weight         968.90
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.6044(6)
_cell_length_b                   16.5465(9)
_cell_length_c                   21.0726(11)
_cell_angle_alpha                90
_cell_angle_beta                 109.055(2)
_cell_angle_gamma                90
_cell_volume                     4813.2(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9988
_cell_measurement_temperature    150
_cell_measurement_theta_max      26.955
_cell_measurement_theta_min      2.881
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.448
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.1346 before and 0.0651 after correction. The Ratio of minimum to maximum transmission is 0.7839. The λ/2 correction factor is 0.00150.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       cube
_exptl_crystal_F_000             1984
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            86173
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.137
_diffrn_reflns_theta_min         1.475
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8772
_reflns_number_total             10514
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         10514
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0244
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0155P)²+3.4126P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0497
_refine_ls_wR_factor_ref         0.0532
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C43(H43), C46(H46), C31(H31), C22(H22), C7(H7), C19(H19), C10(H10), C34(H34)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C17(H17), C39(H39), C28(H28), C41(H41), C4(H4), C27(H27),
 C40(H40), C3(H3), C5(H5), C29(H29)
2.c Idealised Me refined as rotating group:
 C45(H45A,H45B,H45C), C8(H8A,H8B,H8C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C48(H48A,H48B,H48C), C47(H47A,
 H47B,H47C), C44(H44A,H44B,H44C), C12(H12A,H12B,H12C), C9(H9A,H9B,H9C),
 C32(H32A,H32B,H32C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C11(H11A,H11B,
 H11C), C33(H33A,H33B,H33C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tl1 Tl 0.24993(2) 0.26312(2) 0.42484(2) 0.02133(4) Uani 1 1 d . . . . .
Cl4 Cl 0.22563(5) 0.25648(4) 0.53374(3) 0.03780(16) Uani 1 1 d . . . . .
C1 C 0.25521(17) 0.45766(14) 0.36151(13) 0.0259(6) Uani 1 1 d . . . . .
N5 N 0.12362(13) 0.15671(11) 0.33496(9) 0.0185(4) Uani 1 1 d . . . . .
C26 C 0.26740(18) 0.04815(15) 0.29586(13) 0.0266(6) Uani 1 1 d . . . . .
C25 C 0.25824(16) 0.06925(14) 0.35814(12) 0.0211(5) Uani 1 1 d . . . . .
N3 N 0.41190(13) 0.30530(11) 0.44527(9) 0.0183(4) Uani 1 1 d . . . . .
C37 C -0.00206(17) 0.24817(13) 0.32489(12) 0.0195(5) Uani 1 1 d . . . . .
N6 N 0.09887(14) 0.22836(11) 0.34679(9) 0.0193(4) Uani 1 1 d . . . . .
C14 C 0.56913(19) 0.25855(15) 0.44218(13) 0.0254(5) Uani 1 1 d . . . . .
N2 N 0.38919(13) 0.37614(11) 0.41961(9) 0.0201(4) Uani 1 1 d . . . . .
N4 N 0.21361(13) 0.14302(11) 0.36711(9) 0.0200(4) Uani 1 1 d . . . . .
C42 C -0.05888(18) 0.22114(15) 0.36333(12) 0.0248(5) Uani 1 1 d . . . . .
C15 C 0.6665(2) 0.24282(16) 0.47699(14) 0.0335(6) Uani 1 1 d . . . . .
H15 H 0.706757 0.222476 0.453204 0.040 Uiso 1 1 calc R . . . .
C2 C 0.27082(18) 0.47909(15) 0.30130(13) 0.0295(6) Uani 1 1 d . . . . .
C45 C 0.0212(2) 0.26319(18) 0.17424(15) 0.0409(7) Uani 1 1 d . . . . .
H45A H 0.038446 0.209913 0.195030 0.061 Uiso 1 1 calc GR . . . .
H45B H 0.067619 0.278572 0.151674 0.061 Uiso 1 1 calc GR . . . .
H45C H -0.044106 0.261118 0.141330 0.061 Uiso 1 1 calc GR . . . .
C43 C 0.02390(18) 0.32552(15) 0.22833(12) 0.0274(6) Uani 1 1 d . . . . .
H43 H 0.092021 0.327719 0.259787 0.033 Uiso 1 1 calc R . . . .
C16 C 0.7053(2) 0.25602(17) 0.54454(15) 0.0355(7) Uani 1 1 d . . . . .
H16 H 0.771899 0.245140 0.567060 0.043 Uiso 1 1 calc R . . . .
C17 C 0.64783(19) 0.28517(17) 0.58019(13) 0.0331(6) Uani 1 1 d . . . . .
H17 H 0.675325 0.293844 0.627170 0.040 Uiso 1 1 calc R . . . .
C18 C 0.55047(17) 0.30192(14) 0.54817(12) 0.0234(5) Uani 1 1 d . . . . .
C46 C -0.01590(19) 0.17034(16) 0.42592(12) 0.0288(6) Uani 1 1 d . . . . .
H46 H 0.055898 0.178260 0.441097 0.035 Uiso 1 1 calc R . . . .
C13 C 0.51257(16) 0.28915(14) 0.47867(11) 0.0193(5) Uani 1 1 d . . . . .
C31 C 0.22452(19) 0.09789(17) 0.23310(13) 0.0322(6) Uani 1 1 d . . . . .
H31 H 0.202540 0.150362 0.246759 0.039 Uiso 1 1 calc R . . . .
C8 C 0.2858(3) 0.3540(2) 0.2385(2) 0.0667(11) Uani 1 1 d . . . . .
H8A H 0.260554 0.323957 0.269223 0.100 Uiso 1 1 calc GR . . . .
H8B H 0.332206 0.320266 0.225803 0.100 Uiso 1 1 calc GR . . . .
H8C H 0.232230 0.368808 0.198138 0.100 Uiso 1 1 calc GR . . . .
C39 C -0.13748(18) 0.31705(16) 0.24900(13) 0.0325(6) Uani 1 1 d . . . . .
H39 H -0.164947 0.350019 0.210558 0.039 Uiso 1 1 calc R . . . .
C28 C 0.3576(2) -0.06938(18) 0.34967(17) 0.0435(8) Uani 1 1 d . . . . .
H28 H 0.392458 -0.116942 0.346694 0.052 Uiso 1 1 calc R . . . .
C41 C -0.1564(2) 0.24229(17) 0.34091(14) 0.0341(6) Uani 1 1 d . . . . .
H41 H -0.196990 0.224217 0.365223 0.041 Uiso 1 1 calc R . . . .
C22 C 0.48684(19) 0.33581(16) 0.58613(12) 0.0296(6) Uani 1 1 d . . . . .
H22 H 0.418400 0.320428 0.560832 0.036 Uiso 1 1 calc R . . . .
C7 C 0.3358(2) 0.42958(16) 0.27268(14) 0.0347(6) Uani 1 1 d . . . . .
H7 H 0.391439 0.411139 0.312011 0.042 Uiso 1 1 calc R . . . .
C4 C 0.1607(2) 0.59104(17) 0.29271(15) 0.0444(8) Uani 1 1 d . . . . .
H4 H 0.127816 0.636846 0.268701 0.053 Uiso 1 1 calc R . . . .
C19 C 0.5285(2) 0.24516(18) 0.36692(14) 0.0401(7) Uani 1 1 d . . . . .
H19 H 0.456637 0.252065 0.352701 0.048 Uiso 1 1 calc R . . . .
C10 C 0.1790(2) 0.47868(17) 0.45389(14) 0.0383(7) Uani 1 1 d . . . . .
H10 H 0.228405 0.436726 0.475930 0.046 Uiso 1 1 calc R . . . .
N1 N 0.29668(14) 0.38564(12) 0.39649(10) 0.0236(4) Uani 1 1 d . . . . .
C30 C 0.29786(18) 0.02161(15) 0.41587(13) 0.0276(6) Uani 1 1 d . . . . .
C27 C 0.31797(19) -0.02270(17) 0.29367(15) 0.0367(7) Uani 1 1 d . . . . .
H27 H 0.325110 -0.039027 0.252317 0.044 Uiso 1 1 calc R . . . .
C6 C 0.19440(19) 0.50163(15) 0.38814(13) 0.0312(6) Uani 1 1 d . . . . .
C20 C 0.5497(3) 0.1600(2) 0.34780(16) 0.0717(12) Uani 1 1 d . . . . .
H20A H 0.619960 0.151920 0.361190 0.108 Uiso 1 1 calc GR . . . .
H20B H 0.521139 0.152885 0.299128 0.108 Uiso 1 1 calc GR . . . .
H20C H 0.521713 0.120411 0.370792 0.108 Uiso 1 1 calc GR . . . .
C21 C 0.5693(3) 0.3099(2) 0.33110(16) 0.0622(11) Uani 1 1 d . . . . .
H21A H 0.555468 0.363680 0.345171 0.093 Uiso 1 1 calc GR . . . .
H21B H 0.538840 0.304371 0.282417 0.093 Uiso 1 1 calc GR . . . .
H21C H 0.639479 0.302810 0.342866 0.093 Uiso 1 1 calc GR . . . .
C34 C 0.2881(2) 0.04566(17) 0.48281(13) 0.0344(6) Uani 1 1 d . . . . .
H34 H 0.242525 0.092596 0.474348 0.041 Uiso 1 1 calc R . . . .
C38 C -0.03953(17) 0.29812(15) 0.26869(12) 0.0245(5) Uani 1 1 d . . . . .
C40 C -0.1955(2) 0.28890(18) 0.28419(15) 0.0386(7) Uani 1 1 d . . . . .
H40 H -0.262572 0.301596 0.269396 0.046 Uiso 1 1 calc R . . . .
C3 C 0.2222(2) 0.54749(17) 0.26819(14) 0.0369(7) Uani 1 1 d . . . . .
H3 H 0.231700 0.564391 0.227718 0.044 Uiso 1 1 calc R . . . .
C24 C 0.5119(3) 0.3005(2) 0.65627(15) 0.0606(10) Uani 1 1 d . . . . .
H24A H 0.507059 0.241461 0.653383 0.091 Uiso 1 1 calc GR . . . .
H24B H 0.466688 0.321323 0.677949 0.091 Uiso 1 1 calc GR . . . .
H24C H 0.578165 0.315954 0.682754 0.091 Uiso 1 1 calc GR . . . .
C5 C 0.1465(2) 0.56872(17) 0.35179(15) 0.0396(7) Uani 1 1 d . . . . .
H5 H 0.103778 0.599247 0.368060 0.048 Uiso 1 1 calc R . . . .
C23 C 0.4922(2) 0.42802(19) 0.58811(17) 0.0512(8) Uani 1 1 d . . . . .
H23A H 0.559167 0.444952 0.611231 0.077 Uiso 1 1 calc GR . . . .
H23B H 0.450153 0.449053 0.612204 0.077 Uiso 1 1 calc GR . . . .
H23C H 0.470851 0.449205 0.542164 0.077 Uiso 1 1 calc GR . . . .
C29 C 0.34766(19) -0.04823(17) 0.40971(16) 0.0396(7) Uani 1 1 d . . . . .
H29 H 0.375072 -0.081646 0.447875 0.048 Uiso 1 1 calc R . . . .
C48 C -0.0354(2) 0.08091(18) 0.40995(15) 0.0478(8) Uani 1 1 d . . . . .
H48A H -0.105192 0.070668 0.396483 0.072 Uiso 1 1 calc GR . . . .
H48B H -0.002003 0.048739 0.449858 0.072 Uiso 1 1 calc GR . . . .
H48C H -0.011400 0.065796 0.373232 0.072 Uiso 1 1 calc GR . . . .
C47 C -0.0508(2) 0.1952(2) 0.48375(15) 0.0492(8) Uani 1 1 d . . . . .
H47A H -0.039097 0.253095 0.492588 0.074 Uiso 1 1 calc GR . . . .
H47B H -0.015411 0.164438 0.524033 0.074 Uiso 1 1 calc GR . . . .
H47C H -0.120268 0.184108 0.471835 0.074 Uiso 1 1 calc GR . . . .
C44 C -0.0011(2) 0.40910(19) 0.19799(18) 0.0543(9) Uani 1 1 d . . . . .
H44A H -0.065120 0.407803 0.163414 0.081 Uiso 1 1 calc GR . . . .
H44B H 0.047484 0.425928 0.177767 0.081 Uiso 1 1 calc GR . . . .
H44C H -0.001861 0.447541 0.233195 0.081 Uiso 1 1 calc GR . . . .
C12 C 0.1948(4) 0.5498(2) 0.5023(2) 0.0910(16) Uani 1 1 d . . . . .
H12A H 0.259939 0.571847 0.510653 0.136 Uiso 1 1 calc GR . . . .
H12B H 0.187923 0.531497 0.544737 0.136 Uiso 1 1 calc GR . . . .
H12C H 0.146574 0.591845 0.482577 0.136 Uiso 1 1 calc GR . . . .
C9 C 0.3795(3) 0.4771(2) 0.22829(16) 0.0558(9) Uani 1 1 d . . . . .
H9A H 0.328105 0.493449 0.187229 0.084 Uiso 1 1 calc GR . . . .
H9B H 0.426751 0.443431 0.216560 0.084 Uiso 1 1 calc GR . . . .
H9C H 0.411841 0.525373 0.252330 0.084 Uiso 1 1 calc GR . . . .
C32 C 0.1361(2) 0.0562(2) 0.18547(17) 0.0576(9) Uani 1 1 d . . . . .
H32A H 0.154480 0.002544 0.173953 0.086 Uiso 1 1 calc GR . . . .
H32B H 0.110371 0.088485 0.144512 0.086 Uiso 1 1 calc GR . . . .
H32C H 0.086500 0.050540 0.207193 0.086 Uiso 1 1 calc GR . . . .
C35 C 0.3849(2) 0.0740(2) 0.53185(16) 0.0615(10) Uani 1 1 d . . . . .
H35A H 0.430646 0.028725 0.542826 0.092 Uiso 1 1 calc GR . . . .
H35B H 0.375299 0.094051 0.572985 0.092 Uiso 1 1 calc GR . . . .
H35C H 0.410997 0.117536 0.511201 0.092 Uiso 1 1 calc GR . . . .
C36 C 0.2437(3) -0.0222(2) 0.51263(18) 0.0602(10) Uani 1 1 d . . . . .
H36A H 0.181523 -0.038369 0.480091 0.090 Uiso 1 1 calc GR . . . .
H36B H 0.233491 -0.003001 0.553795 0.090 Uiso 1 1 calc GR . . . .
H36C H 0.287758 -0.068636 0.523091 0.090 Uiso 1 1 calc GR . . . .
C11 C 0.0799(3) 0.4408(3) 0.4414(2) 0.0686(11) Uani 1 1 d . . . . .
H11A H 0.029856 0.482489 0.426079 0.103 Uiso 1 1 calc GR . . . .
H11B H 0.076802 0.416661 0.483069 0.103 Uiso 1 1 calc GR . . . .
H11C H 0.069252 0.398873 0.406876 0.103 Uiso 1 1 calc GR . . . .
C33 C 0.2987(3) 0.1170(3) 0.1988(2) 0.0776(13) Uani 1 1 d . . . . .
H33A H 0.353987 0.145101 0.230442 0.116 Uiso 1 1 calc GR . . . .
H33B H 0.269055 0.151674 0.159792 0.116 Uiso 1 1 calc GR . . . .
H33C H 0.320870 0.066668 0.184168 0.116 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tl1 Cl4 2.4364(7) . ?
Tl1 N3 2.3672(18) . ?
Tl1 N6 2.3523(19) . ?
Tl1 N4 2.2998(19) . ?
Tl1 N1 2.2802(19) . ?
C1 C2 1.406(4) . ?
C1 N1 1.428(3) . ?
C1 C6 1.399(4) . ?
N5 N6 1.287(3) . ?
N5 N4 1.287(3) . ?
C26 C25 1.406(4) . ?
C26 C31 1.509(4) . ?
C26 C27 1.394(4) . ?
C25 N4 1.425(3) . ?
C25 C30 1.406(3) . ?
N3 N2 1.288(3) . ?
N3 C13 1.433(3) . ?
C37 N6 1.431(3) . ?
C37 C42 1.408(3) . ?
C37 C38 1.401(3) . ?
C14 C15 1.395(4) . ?
C14 C13 1.395(3) . ?
C14 C19 1.517(4) . ?
N2 N1 1.288(3) . ?
C42 C46 1.517(3) . ?
C42 C41 1.390(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.367(4) . ?
C2 C7 1.520(4) . ?
C2 C3 1.396(4) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C45 C43 1.528(4) . ?
C43 H43 1.0000 . ?
C43 C38 1.517(3) . ?
C43 C44 1.517(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.383(4) . ?
C17 H17 0.9500 . ?
C17 C18 1.388(3) . ?
C18 C13 1.402(3) . ?
C18 C22 1.518(3) . ?
C46 H46 1.0000 . ?
C46 C48 1.524(4) . ?
C46 C47 1.523(4) . ?
C31 H31 1.0000 . ?
C31 C32 1.518(4) . ?
C31 C33 1.518(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C8 C7 1.507(4) . ?
C39 H39 0.9500 . ?
C39 C38 1.389(3) . ?
C39 C40 1.376(4) . ?
C28 H28 0.9500 . ?
C28 C27 1.371(4) . ?
C28 C29 1.366(4) . ?
C41 H41 0.9500 . ?
C41 C40 1.380(4) . ?
C22 H22 1.0000 . ?
C22 C24 1.519(4) . ?
C22 C23 1.528(4) . ?
C7 H7 1.0000 . ?
C7 C9 1.513(4) . ?
C4 H4 0.9500 . ?
C4 C3 1.376(4) . ?
C4 C5 1.378(4) . ?
C19 H19 1.0000 . ?
C19 C20 1.525(4) . ?
C19 C21 1.537(5) . ?
C10 H10 1.0000 . ?
C10 C6 1.523(4) . ?
C10 C12 1.525(4) . ?
C10 C11 1.518(5) . ?
C30 C34 1.517(4) . ?
C30 C29 1.394(4) . ?
C27 H27 0.9500 . ?
C6 C5 1.399(4) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C34 H34 1.0000 . ?
C34 C35 1.528(4) . ?
C34 C36 1.530(4) . ?
C40 H40 0.9500 . ?
C3 H3 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C5 H5 0.9500 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C29 H29 0.9500 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Tl1 Cl4 106.63(5) . . ?
N6 Tl1 Cl4 104.82(5) . . ?
N6 Tl1 N3 148.50(6) . . ?
N4 Tl1 Cl4 112.33(5) . . ?
N4 Tl1 N3 113.27(6) . . ?
N4 Tl1 N6 54.35(6) . . ?
N1 Tl1 Cl4 115.79(5) . . ?
N1 Tl1 N3 54.45(6) . . ?
N1 Tl1 N6 109.08(7) . . ?
N1 Tl1 N4 131.82(7) . . ?
C2 C1 N1 120.7(2) . . ?
C6 C1 C2 122.8(2) . . ?
C6 C1 N1 116.4(2) . . ?
N4 N5 N6 111.30(18) . . ?
C25 C26 C31 123.0(2) . . ?
C27 C26 C25 116.9(2) . . ?
C27 C26 C31 120.1(2) . . ?
C26 C25 N4 121.6(2) . . ?
C30 C25 C26 122.1(2) . . ?
C30 C25 N4 116.3(2) . . ?
N2 N3 Tl1 94.98(13) . . ?
N2 N3 C13 117.27(18) . . ?
C13 N3 Tl1 147.00(14) . . ?
C42 C37 N6 118.7(2) . . ?
C38 C37 N6 119.0(2) . . ?
C38 C37 C42 122.2(2) . . ?
N5 N6 Tl1 95.86(13) . . ?
N5 N6 C37 118.24(18) . . ?
C37 N6 Tl1 143.27(15) . . ?
C15 C14 C19 120.4(2) . . ?
C13 C14 C15 117.6(2) . . ?
C13 C14 C19 122.0(2) . . ?
N1 N2 N3 111.38(18) . . ?
N5 N4 Tl1 98.39(13) . . ?
N5 N4 C25 120.91(18) . . ?
C25 N4 Tl1 140.69(15) . . ?
C37 C42 C46 121.5(2) . . ?
C41 C42 C37 117.1(2) . . ?
C41 C42 C46 121.5(2) . . ?
C14 C15 H15 119.3 . . ?
C16 C15 C14 121.5(2) . . ?
C16 C15 H15 119.3 . . ?
C1 C2 C7 121.9(2) . . ?
C3 C2 C1 116.7(3) . . ?
C3 C2 C7 121.4(2) . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
C45 C43 H43 107.3 . . ?
C38 C43 C45 110.2(2) . . ?
C38 C43 H43 107.3 . . ?
C38 C43 C44 113.7(2) . . ?
C44 C43 C45 110.9(2) . . ?
C44 C43 H43 107.3 . . ?
C15 C16 H16 119.9 . . ?
C15 C16 C17 120.2(3) . . ?
C17 C16 H16 119.9 . . ?
C16 C17 H17 119.6 . . ?
C16 C17 C18 120.8(2) . . ?
C18 C17 H17 119.6 . . ?
C17 C18 C13 118.0(2) . . ?
C17 C18 C22 121.6(2) . . ?
C13 C18 C22 120.3(2) . . ?
C42 C46 H46 107.4 . . ?
C42 C46 C48 110.6(2) . . ?
C42 C46 C47 113.2(2) . . ?
C48 C46 H46 107.4 . . ?
C47 C46 H46 107.4 . . ?
C47 C46 C48 110.6(2) . . ?
C14 C13 N3 119.6(2) . . ?
C14 C13 C18 121.8(2) . . ?
C18 C13 N3 118.5(2) . . ?
C26 C31 H31 107.6 . . ?
C26 C31 C32 110.6(2) . . ?
C26 C31 C33 112.0(3) . . ?
C32 C31 H31 107.6 . . ?
C32 C31 C33 111.4(3) . . ?
C33 C31 H31 107.6 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
C38 C39 H39 119.4 . . ?
C40 C39 H39 119.4 . . ?
C40 C39 C38 121.2(2) . . ?
C27 C28 H28 119.7 . . ?
C29 C28 H28 119.7 . . ?
C29 C28 C27 120.7(3) . . ?
C42 C41 H41 119.2 . . ?
C40 C41 C42 121.5(3) . . ?
C40 C41 H41 119.2 . . ?
C18 C22 H22 107.6 . . ?
C18 C22 C24 112.1(2) . . ?
C18 C22 C23 110.4(2) . . ?
C24 C22 H22 107.6 . . ?
C24 C22 C23 111.3(3) . . ?
C23 C22 H22 107.6 . . ?
C2 C7 H7 106.2 . . ?
C8 C7 C2 111.6(2) . . ?
C8 C7 H7 106.2 . . ?
C8 C7 C9 111.8(3) . . ?
C9 C7 C2 114.1(2) . . ?
C9 C7 H7 106.2 . . ?
C3 C4 H4 119.7 . . ?
C3 C4 C5 120.5(3) . . ?
C5 C4 H4 119.7 . . ?
C14 C19 H19 108.1 . . ?
C14 C19 C20 111.6(2) . . ?
C14 C19 C21 109.3(3) . . ?
C20 C19 H19 108.1 . . ?
C20 C19 C21 111.7(3) . . ?
C21 C19 H19 108.1 . . ?
C6 C10 H10 107.3 . . ?
C6 C10 C12 112.4(3) . . ?
C12 C10 H10 107.3 . . ?
C11 C10 H10 107.3 . . ?
C11 C10 C6 111.1(3) . . ?
C11 C10 C12 111.2(3) . . ?
C1 N1 Tl1 139.85(15) . . ?
N2 N1 Tl1 99.16(13) . . ?
N2 N1 C1 120.88(19) . . ?
C25 C30 C34 121.4(2) . . ?
C29 C30 C25 117.7(2) . . ?
C29 C30 C34 121.0(2) . . ?
C26 C27 H27 119.2 . . ?
C28 C27 C26 121.7(3) . . ?
C28 C27 H27 119.2 . . ?
C1 C6 C10 122.5(2) . . ?
C5 C6 C1 117.5(3) . . ?
C5 C6 C10 120.0(3) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C30 C34 H34 107.3 . . ?
C30 C34 C35 111.2(2) . . ?
C30 C34 C36 111.8(2) . . ?
C35 C34 H34 107.3 . . ?
C35 C34 C36 111.7(3) . . ?
C36 C34 H34 107.3 . . ?
C37 C38 C43 120.6(2) . . ?
C39 C38 C37 117.7(2) . . ?
C39 C38 C43 121.5(2) . . ?
C39 C40 C41 120.2(2) . . ?
C39 C40 H40 119.9 . . ?
C41 C40 H40 119.9 . . ?
C2 C3 H3 119.2 . . ?
C4 C3 C2 121.6(3) . . ?
C4 C3 H3 119.2 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C4 C5 C6 120.8(3) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C28 C29 C30 121.0(3) . . ?
C28 C29 H29 119.5 . . ?
C30 C29 H29 119.5 . . ?
C46 C48 H48A 109.5 . . ?
C46 C48 H48B 109.5 . . ?
C46 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tl1 N3 N2 N1 -1.39(18) . . . . ?
Tl1 N3 C13 C14 104.0(3) . . . . ?
Tl1 N3 C13 C18 -73.6(3) . . . . ?
C1 C2 C7 C8 77.7(3) . . . . ?
C1 C2 C7 C9 -154.3(3) . . . . ?
C1 C2 C3 C4 -1.0(4) . . . . ?
C1 C6 C5 C4 -1.2(4) . . . . ?
C26 C25 N4 Tl1 -114.9(2) . . . . ?
C26 C25 N4 N5 63.6(3) . . . . ?
C26 C25 C30 C34 179.4(2) . . . . ?
C26 C25 C30 C29 0.2(4) . . . . ?
C25 C26 C31 C32 -106.2(3) . . . . ?
C25 C26 C31 C33 128.9(3) . . . . ?
C25 C26 C27 C28 -0.5(4) . . . . ?
C25 C30 C34 C35 -108.5(3) . . . . ?
C25 C30 C34 C36 125.8(3) . . . . ?
C25 C30 C29 C28 0.1(4) . . . . ?
N3 N2 N1 Tl1 1.46(19) . . . . ?
N3 N2 N1 C1 -175.5(2) . . . . ?
C37 C42 C46 C48 -97.2(3) . . . . ?
C37 C42 C46 C47 138.0(3) . . . . ?
C37 C42 C41 C40 -1.1(4) . . . . ?
N6 N5 N4 Tl1 3.11(18) . . . . ?
N6 N5 N4 C25 -175.98(19) . . . . ?
N6 C37 C42 C46 -1.4(3) . . . . ?
N6 C37 C42 C41 179.3(2) . . . . ?
N6 C37 C38 C43 4.8(3) . . . . ?
N6 C37 C38 C39 -179.3(2) . . . . ?
C14 C15 C16 C17 0.4(4) . . . . ?
N2 N3 C13 C14 -89.3(3) . . . . ?
N2 N3 C13 C18 93.1(3) . . . . ?
N4 N5 N6 Tl1 -3.02(18) . . . . ?
N4 N5 N6 C37 -168.85(19) . . . . ?
N4 C25 C30 C34 3.4(3) . . . . ?
N4 C25 C30 C29 -175.8(2) . . . . ?
C42 C37 N6 Tl1 -77.4(3) . . . . ?
C42 C37 N6 N5 78.6(3) . . . . ?
C42 C37 C38 C43 -179.6(2) . . . . ?
C42 C37 C38 C39 -3.7(4) . . . . ?
C42 C41 C40 C39 -1.3(5) . . . . ?
C15 C14 C13 N3 -179.2(2) . . . . ?
C15 C14 C13 C18 -1.7(4) . . . . ?
C15 C14 C19 C20 53.3(4) . . . . ?
C15 C14 C19 C21 -70.6(3) . . . . ?
C15 C16 C17 C18 -0.4(4) . . . . ?
C2 C1 N1 Tl1 -113.5(3) . . . . ?
C2 C1 N1 N2 61.8(3) . . . . ?
C2 C1 C6 C10 -179.1(2) . . . . ?
C2 C1 C6 C5 1.2(4) . . . . ?
C45 C43 C38 C37 87.5(3) . . . . ?
C45 C43 C38 C39 -88.3(3) . . . . ?
C16 C17 C18 C13 -0.6(4) . . . . ?
C16 C17 C18 C22 -178.5(2) . . . . ?
C17 C18 C13 N3 179.2(2) . . . . ?
C17 C18 C13 C14 1.7(4) . . . . ?
C17 C18 C22 C24 -37.0(4) . . . . ?
C17 C18 C22 C23 87.7(3) . . . . ?
C46 C42 C41 C40 179.6(3) . . . . ?
C13 N3 N2 N1 -174.16(19) . . . . ?
C13 C14 C15 C16 0.6(4) . . . . ?
C13 C14 C19 C20 -128.8(3) . . . . ?
C13 C14 C19 C21 107.2(3) . . . . ?
C13 C18 C22 C24 145.1(3) . . . . ?
C13 C18 C22 C23 -90.2(3) . . . . ?
C31 C26 C25 N4 -4.9(4) . . . . ?
C31 C26 C25 C30 179.3(2) . . . . ?
C31 C26 C27 C28 -179.9(2) . . . . ?
C41 C42 C46 C48 82.0(3) . . . . ?
C41 C42 C46 C47 -42.8(3) . . . . ?
C22 C18 C13 N3 -2.8(3) . . . . ?
C22 C18 C13 C14 179.6(2) . . . . ?
C7 C2 C3 C4 177.8(3) . . . . ?
C19 C14 C15 C16 178.6(3) . . . . ?
C19 C14 C13 N3 2.9(4) . . . . ?
C19 C14 C13 C18 -179.6(2) . . . . ?
C10 C6 C5 C4 179.1(3) . . . . ?
N1 C1 C2 C7 -3.1(4) . . . . ?
N1 C1 C2 C3 175.8(2) . . . . ?
N1 C1 C6 C10 4.9(4) . . . . ?
N1 C1 C6 C5 -174.9(2) . . . . ?
C30 C25 N4 Tl1 61.1(3) . . . . ?
C30 C25 N4 N5 -120.3(2) . . . . ?
C27 C26 C25 N4 175.8(2) . . . . ?
C27 C26 C25 C30 0.0(4) . . . . ?
C27 C26 C31 C32 73.1(3) . . . . ?
C27 C26 C31 C33 -51.8(4) . . . . ?
C27 C28 C29 C30 -0.7(4) . . . . ?
C6 C1 C2 C7 -178.9(2) . . . . ?
C6 C1 C2 C3 -0.1(4) . . . . ?
C6 C1 N1 Tl1 62.5(3) . . . . ?
C6 C1 N1 N2 -122.1(2) . . . . ?
C34 C30 C29 C28 -179.1(3) . . . . ?
C38 C37 N6 Tl1 98.4(3) . . . . ?
C38 C37 N6 N5 -105.6(2) . . . . ?
C38 C37 C42 C46 -177.1(2) . . . . ?
C38 C37 C42 C41 3.7(4) . . . . ?
C38 C39 C40 C41 1.3(4) . . . . ?
C40 C39 C38 C37 1.1(4) . . . . ?
C40 C39 C38 C43 177.0(3) . . . . ?
C3 C2 C7 C8 -101.1(3) . . . . ?
C3 C2 C7 C9 26.9(4) . . . . ?
C3 C4 C5 C6 0.2(4) . . . . ?
C5 C4 C3 C2 1.0(4) . . . . ?
C29 C28 C27 C26 0.9(4) . . . . ?
C29 C30 C34 C35 70.7(3) . . . . ?
C29 C30 C34 C36 -55.0(4) . . . . ?
C44 C43 C38 C37 -147.3(3) . . . . ?
C44 C43 C38 C39 36.9(4) . . . . ?
C12 C10 C6 C1 128.7(3) . . . . ?
C12 C10 C6 C5 -51.6(4) . . . . ?
C11 C10 C6 C1 -105.9(3) . . . . ?
C11 C10 C6 C5 73.8(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_9
_database_code_depnum_ccdc_archive 'CCDC 1972002'
loop_
_audit_author_name
_audit_author_address
'Alasdair McKay'
;Monash University
Australia
;
_audit_update_record             
;
2019-12-14 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_audit_creation_date             2019-04-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
''
alasdair.mckay@monash.edu
_chemical_name_common            ?
_chemical_name_systematic        '[InCl(N3Dipp2)2]'
_chemical_formula_moiety         'C48 H68 Cl In N6'
_chemical_formula_sum            'C48 H68 Cl In N6'
_chemical_formula_weight         879.35
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.5014(4)
_cell_length_b                   16.4263(4)
_cell_length_c                   21.0903(6)
_cell_angle_alpha                90
_cell_angle_beta                 109.584(3)
_cell_angle_gamma                90
_cell_volume                     4733.2(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    45596
_cell_measurement_temperature    112(2)
_cell_measurement_theta_max      29.0144
_cell_measurement_theta_min      2.8854
_shelx_estimated_absorpt_T_max   0.943
_shelx_estimated_absorpt_T_min   0.943
_exptl_absorpt_coefficient_mu    0.593
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       cube
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            59913
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         2.894
_diffrn_ambient_temperature      112(2)
_diffrn_detector_area_resol_mean 8.4171
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -11.00  102.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.0069   77.0000   60.0000 113

#__ type_ start__ end____ width___ exp.time_
  2 omega   -9.00  112.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.0069   77.0000  -60.0000 121

#__ type_ start__ end____ width___ exp.time_
  3 omega  -18.00  113.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.0069   77.0000 -180.0000 131

#__ type_ start__ end____ width___ exp.time_
  4 omega  -61.00   31.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.2881   77.0000   90.0000 92

#__ type_ start__ end____ width___ exp.time_
  5 omega  -51.00  -14.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.2881   77.0000   30.0000 37

#__ type_ start__ end____ width___ exp.time_
  6 omega   30.00   67.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.2881   77.0000   30.0000 37

#__ type_ start__ end____ width___ exp.time_
  7 omega  -54.00   51.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.2881   77.0000  -60.0000 105

#__ type_ start__ end____ width___ exp.time_
  8 omega  -64.00   34.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.2881   77.0000 -150.0000 98
;
_diffrn_measurement_device_type  'XcaliburTM2, Oxford Diffraction'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0256362000
_diffrn_orient_matrix_UB_12      0.0015103000
_diffrn_orient_matrix_UB_13      0.0232970000
_diffrn_orient_matrix_UB_21      -0.0403754000
_diffrn_orient_matrix_UB_22      0.0184461000
_diffrn_orient_matrix_UB_23      -0.0247280000
_diffrn_orient_matrix_UB_31      -0.0200823000
_diffrn_orient_matrix_UB_32      -0.0389761000
_diffrn_orient_matrix_UB_33      -0.0108508000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8639
_reflns_number_total             10392
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39)'
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.717
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         10392
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0275
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0258P)²+3.1989P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0613
_refine_ls_wR_factor_ref         0.0667
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C19(H19), C22(H22), C31(H31), C34(H34), C43(H43), C46(H46)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C15(H15), C16(H16), C17(H17), C27(H27), C28(H28),
 C29(H29), C39(H39), C40(H40), C41(H41)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
In1 In 0.25292(2) 0.76586(2) 0.57530(2) 0.01493(4) Uani 1 1 d . . . . .
Cl1 Cl 0.27605(3) 0.76111(3) 0.47012(2) 0.02514(10) Uani 1 1 d . . . . .
N1 N 0.20916(11) 0.88216(9) 0.60579(8) 0.0188(3) Uani 1 1 d . . . . .
N2 N 0.11472(11) 0.87302(9) 0.58121(7) 0.0166(3) Uani 1 1 d . . . . .
N3 N 0.09447(10) 0.80181(9) 0.55383(7) 0.0147(3) Uani 1 1 d . . . . .
N4 N 0.28361(10) 0.65157(9) 0.63223(7) 0.0154(3) Uani 1 1 d . . . . .
N5 N 0.37684(10) 0.66280(9) 0.66360(7) 0.0156(3) Uani 1 1 d . . . . .
N6 N 0.40157(10) 0.73443(9) 0.64920(7) 0.0150(3) Uani 1 1 d . . . . .
C1 C 0.24791(13) 0.95666(11) 0.63950(9) 0.0204(4) Uani 1 1 d . . . . .
C2 C 0.30664(14) 1.00293(12) 0.61210(10) 0.0250(4) Uani 1 1 d . . . . .
C3 C 0.35258(15) 1.07159(12) 0.64779(11) 0.0309(5) Uani 1 1 d . . . . .
H3 H 0.394098 1.103419 0.631066 0.037 Uiso 1 1 calc R . . . .
C4 C 0.33875(16) 1.09391(13) 0.70674(11) 0.0333(5) Uani 1 1 d . . . . .
H4 H 0.371075 1.140641 0.730498 0.040 Uiso 1 1 calc R . . . .
C5 C 0.27829(15) 1.04895(13) 0.73160(11) 0.0296(5) Uani 1 1 d . . . . .
H5 H 0.268083 1.066180 0.771735 0.036 Uiso 1 1 calc R . . . .
C6 C 0.23177(14) 0.97879(12) 0.69924(10) 0.0237(4) Uani 1 1 d . . . . .
C7 C 0.32079(16) 0.98040(12) 0.54621(11) 0.0295(5) Uani 1 1 d . . . . .
H7 H 0.271743 0.937186 0.524612 0.035 Uiso 1 1 calc R . . . .
C8 C 0.42163(18) 0.94444(17) 0.55777(14) 0.0471(6) Uani 1 1 d . . . . .
H8A H 0.471637 0.985841 0.577666 0.071 Uiso 1 1 calc GR . . . .
H8B H 0.426510 0.926428 0.514712 0.071 Uiso 1 1 calc GR . . . .
H8C H 0.431792 0.897865 0.588395 0.071 Uiso 1 1 calc GR . . . .
C9 C 0.3010(3) 1.05218(17) 0.49738(14) 0.0613(8) Uani 1 1 d . . . . .
H9A H 0.234944 1.073177 0.489829 0.092 Uiso 1 1 calc GR . . . .
H9B H 0.306446 1.034092 0.454484 0.092 Uiso 1 1 calc GR . . . .
H9C H 0.349019 1.095290 0.516500 0.092 Uiso 1 1 calc GR . . . .
C10 C 0.16704(15) 0.92831(13) 0.72792(11) 0.0280(4) Uani 1 1 d . . . . .
H10 H 0.112171 0.907149 0.688570 0.034 Uiso 1 1 calc R . . . .
C11 C 0.2206(2) 0.85505(16) 0.76536(17) 0.0558(8) Uani 1 1 d . . . . .
H11A H 0.247844 0.823940 0.736161 0.084 Uiso 1 1 calc GR . . . .
H11B H 0.174990 0.820650 0.778732 0.084 Uiso 1 1 calc GR . . . .
H11C H 0.273692 0.872847 0.805572 0.084 Uiso 1 1 calc GR . . . .
C12 C 0.1204(2) 0.97656(15) 0.77050(12) 0.0433(6) Uani 1 1 d . . . . .
H12A H 0.072754 0.942287 0.781731 0.065 Uiso 1 1 calc GR . . . .
H12B H 0.087176 1.024382 0.745279 0.065 Uiso 1 1 calc GR . . . .
H12C H 0.171167 0.994211 0.812019 0.065 Uiso 1 1 calc GR . . . .
C13 C -0.00752(13) 0.78477(11) 0.52095(9) 0.0168(4) Uani 1 1 d . . . . .
C14 C -0.04840(13) 0.79984(11) 0.45170(9) 0.0187(4) Uani 1 1 d . . . . .
C15 C -0.14715(14) 0.78303(13) 0.42038(10) 0.0256(4) Uani 1 1 d . . . . .
H15 H -0.176538 0.792871 0.373506 0.031 Uiso 1 1 calc R . . . .
C16 C -0.20320(14) 0.75225(13) 0.45632(11) 0.0269(5) Uani 1 1 d . . . . .
H16 H -0.270843 0.741694 0.434286 0.032 Uiso 1 1 calc R . . . .
C17 C -0.16121(14) 0.73686(12) 0.52397(10) 0.0242(4) Uani 1 1 d . . . . .
H17 H -0.200329 0.715217 0.548165 0.029 Uiso 1 1 calc R . . . .
C18 C -0.06253(13) 0.75233(11) 0.55775(9) 0.0197(4) Uani 1 1 d . . . . .
C19 C 0.01298(14) 0.83623(13) 0.41312(9) 0.0236(4) Uani 1 1 d . . . . .
H19 H 0.082503 0.819764 0.436588 0.028 Uiso 1 1 calc R . . . .
C20 C -0.01666(18) 0.80503(17) 0.34124(11) 0.0415(6) Uani 1 1 d . . . . .
H20A H -0.014096 0.745406 0.341535 0.062 Uiso 1 1 calc GR . . . .
H20B H 0.028408 0.826531 0.319594 0.062 Uiso 1 1 calc GR . . . .
H20C H -0.083420 0.823017 0.316230 0.062 Uiso 1 1 calc GR . . . .
C21 C 0.00843(17) 0.92927(14) 0.41444(12) 0.0378(5) Uani 1 1 d . . . . .
H21A H -0.059598 0.947087 0.393793 0.057 Uiso 1 1 calc GR . . . .
H21B H 0.048219 0.951974 0.389232 0.057 Uiso 1 1 calc GR . . . .
H21C H 0.033740 0.948325 0.461139 0.057 Uiso 1 1 calc GR . . . .
C22 C -0.01954(16) 0.73591(14) 0.63276(10) 0.0291(5) Uani 1 1 d . . . . .
H22 H 0.053035 0.742826 0.646546 0.035 Uiso 1 1 calc R . . . .
C23 C -0.0400(2) 0.64933(17) 0.64984(12) 0.0508(7) Uani 1 1 d . . . . .
H23A H -0.110887 0.640976 0.636669 0.076 Uiso 1 1 calc GR . . . .
H23B H -0.009889 0.640399 0.698376 0.076 Uiso 1 1 calc GR . . . .
H23C H -0.012523 0.610818 0.625491 0.076 Uiso 1 1 calc GR . . . .
C24 C -0.05835(19) 0.79879(19) 0.67093(12) 0.0483(7) Uani 1 1 d . . . . .
H24A H -0.045177 0.853685 0.657893 0.073 Uiso 1 1 calc GR . . . .
H24B H -0.025693 0.791533 0.719437 0.073 Uiso 1 1 calc GR . . . .
H24C H -0.129066 0.791473 0.659929 0.073 Uiso 1 1 calc GR . . . .
C25 C 0.24024(12) 0.57611(11) 0.64095(9) 0.0167(4) Uani 1 1 d . . . . .
C26 C 0.20125(13) 0.52756(11) 0.58344(10) 0.0210(4) Uani 1 1 d . . . . .
C27 C 0.15189(14) 0.45681(12) 0.58918(11) 0.0279(5) Uani 1 1 d . . . . .
H27 H 0.124683 0.422976 0.550906 0.034 Uiso 1 1 calc R . . . .
C28 C 0.14197(15) 0.43517(13) 0.64981(12) 0.0310(5) Uani 1 1 d . . . . .
H28 H 0.107210 0.387113 0.652781 0.037 Uiso 1 1 calc R . . . .
C29 C 0.18213(14) 0.48279(12) 0.70590(11) 0.0267(4) Uani 1 1 d . . . . .
H29 H 0.175671 0.466564 0.747441 0.032 Uiso 1 1 calc R . . . .
C30 C 0.23215(13) 0.55444(11) 0.70308(9) 0.0197(4) Uani 1 1 d . . . . .
C31 C 0.21184(15) 0.55051(12) 0.51657(10) 0.0251(4) Uani 1 1 d . . . . .
H31 H 0.257834 0.597788 0.524989 0.030 Uiso 1 1 calc R . . . .
C32 C 0.11443(17) 0.57839(17) 0.46625(12) 0.0424(6) Uani 1 1 d . . . . .
H32A H 0.067708 0.533140 0.456370 0.064 Uiso 1 1 calc GR . . . .
H32B H 0.124304 0.596144 0.424629 0.064 Uiso 1 1 calc GR . . . .
H32C H 0.088703 0.623802 0.485430 0.064 Uiso 1 1 calc GR . . . .
C33 C 0.25666(18) 0.48175(15) 0.48767(12) 0.0402(6) Uani 1 1 d . . . . .
H33A H 0.319551 0.465757 0.520716 0.060 Uiso 1 1 calc GR . . . .
H33B H 0.266916 0.500478 0.446425 0.060 Uiso 1 1 calc GR . . . .
H33C H 0.212236 0.434901 0.477348 0.060 Uiso 1 1 calc GR . . . .
C34 C 0.27705(14) 0.60430(13) 0.76648(10) 0.0248(4) Uani 1 1 d . . . . .
H34 H 0.300077 0.656844 0.753056 0.030 Uiso 1 1 calc R . . . .
C35 C 0.20309(19) 0.62468(19) 0.80134(13) 0.0499(7) Uani 1 1 d . . . . .
H35A H 0.147148 0.653315 0.769777 0.075 Uiso 1 1 calc GR . . . .
H35B H 0.234175 0.659527 0.840391 0.075 Uiso 1 1 calc GR . . . .
H35C H 0.180480 0.574278 0.816216 0.075 Uiso 1 1 calc GR . . . .
C36 C 0.36580(17) 0.56115(15) 0.81440(12) 0.0403(6) Uani 1 1 d . . . . .
H36A H 0.346006 0.508064 0.826722 0.060 Uiso 1 1 calc GR . . . .
H36B H 0.393774 0.594202 0.855030 0.060 Uiso 1 1 calc GR . . . .
H36C H 0.414880 0.553363 0.792373 0.060 Uiso 1 1 calc GR . . . .
C37 C 0.50396(13) 0.75297(10) 0.67233(9) 0.0163(4) Uani 1 1 d . . . . .
C38 C 0.54229(13) 0.80224(11) 0.72938(9) 0.0186(4) Uani 1 1 d . . . . .
C39 C 0.64133(14) 0.82106(12) 0.75000(10) 0.0249(4) Uani 1 1 d . . . . .
H39 H 0.669125 0.854367 0.788526 0.030 Uiso 1 1 calc R . . . .
C40 C 0.69990(14) 0.79195(14) 0.71521(11) 0.0291(5) Uani 1 1 d . . . . .
H40 H 0.767797 0.804401 0.730500 0.035 Uiso 1 1 calc R . . . .
C41 C 0.66028(14) 0.74479(13) 0.65825(10) 0.0262(4) Uani 1 1 d . . . . .
H41 H 0.701361 0.725731 0.634543 0.031 Uiso 1 1 calc R . . . .
C42 C 0.56153(13) 0.72477(11) 0.63504(9) 0.0191(4) Uani 1 1 d . . . . .
C43 C 0.47862(13) 0.82994(12) 0.76948(9) 0.0213(4) Uani 1 1 d . . . . .
H43 H 0.409653 0.832374 0.737814 0.026 Uiso 1 1 calc R . . . .
C44 C 0.50462(17) 0.91411(14) 0.80059(13) 0.0385(6) Uani 1 1 d . . . . .
H44A H 0.570231 0.912764 0.834462 0.058 Uiso 1 1 calc GR . . . .
H44B H 0.456936 0.930288 0.821947 0.058 Uiso 1 1 calc GR . . . .
H44C H 0.503427 0.953446 0.765391 0.058 Uiso 1 1 calc GR . . . .
C45 C 0.48202(16) 0.76675(14) 0.82305(10) 0.0302(5) Uani 1 1 d . . . . .
H45A H 0.464359 0.713282 0.801824 0.045 Uiso 1 1 calc GR . . . .
H45B H 0.435605 0.781861 0.845773 0.045 Uiso 1 1 calc GR . . . .
H45C H 0.548269 0.764429 0.856036 0.045 Uiso 1 1 calc GR . . . .
C46 C 0.51818(14) 0.67285(12) 0.57258(9) 0.0218(4) Uani 1 1 d . . . . .
H46 H 0.445648 0.680936 0.556850 0.026 Uiso 1 1 calc R . . . .
C47 C 0.55337(18) 0.69712(17) 0.51479(11) 0.0395(6) Uani 1 1 d . . . . .
H47A H 0.542804 0.755570 0.506062 0.059 Uiso 1 1 calc GR . . . .
H47B H 0.516663 0.666540 0.474293 0.059 Uiso 1 1 calc GR . . . .
H47C H 0.623289 0.684845 0.526855 0.059 Uiso 1 1 calc GR . . . .
C48 C 0.53757(19) 0.58273(13) 0.58963(11) 0.0380(5) Uani 1 1 d . . . . .
H48A H 0.608165 0.572355 0.604323 0.057 Uiso 1 1 calc GR . . . .
H48B H 0.504571 0.549852 0.549675 0.057 Uiso 1 1 calc GR . . . .
H48C H 0.512416 0.568135 0.625841 0.057 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
In1 Cl1 2.3532(5) . ?
In1 N1 2.1771(15) . ?
In1 N3 2.2663(14) . ?
In1 N4 2.1922(15) . ?
In1 N6 2.2562(14) . ?
N1 N2 1.300(2) . ?
N1 C1 1.432(2) . ?
N2 N3 1.294(2) . ?
N3 C13 1.435(2) . ?
N4 N5 1.304(2) . ?
N4 C25 1.429(2) . ?
N5 N6 1.295(2) . ?
N6 C37 1.432(2) . ?
C1 C2 1.402(3) . ?
C1 C6 1.404(3) . ?
C2 C3 1.395(3) . ?
C2 C7 1.517(3) . ?
C3 C4 1.374(3) . ?
C4 C5 1.377(3) . ?
C5 C6 1.393(3) . ?
C6 C10 1.522(3) . ?
C7 C8 1.519(3) . ?
C7 C9 1.528(3) . ?
C10 C11 1.504(3) . ?
C10 C12 1.516(3) . ?
C13 C14 1.402(2) . ?
C13 C18 1.392(3) . ?
C14 C15 1.389(3) . ?
C14 C19 1.516(3) . ?
C15 C16 1.380(3) . ?
C16 C17 1.374(3) . ?
C17 C18 1.392(3) . ?
C18 C22 1.517(3) . ?
C19 C20 1.520(3) . ?
C19 C21 1.530(3) . ?
C22 C23 1.521(3) . ?
C22 C24 1.528(3) . ?
C25 C26 1.402(3) . ?
C25 C30 1.400(3) . ?
C26 C27 1.391(3) . ?
C26 C31 1.517(3) . ?
C27 C28 1.380(3) . ?
C28 C29 1.374(3) . ?
C29 C30 1.394(3) . ?
C30 C34 1.516(3) . ?
C31 C32 1.525(3) . ?
C31 C33 1.528(3) . ?
C34 C35 1.527(3) . ?
C34 C36 1.519(3) . ?
C37 C38 1.401(3) . ?
C37 C42 1.404(3) . ?
C38 C39 1.389(3) . ?
C38 C43 1.516(3) . ?
C39 C40 1.381(3) . ?
C40 C41 1.382(3) . ?
C41 C42 1.389(3) . ?
C42 C46 1.517(3) . ?
C43 C44 1.523(3) . ?
C43 C45 1.523(3) . ?
C46 C47 1.524(3) . ?
C46 C48 1.527(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 In1 Cl1 117.08(4) . . ?
N1 In1 N3 56.90(5) . . ?
N1 In1 N4 127.98(6) . . ?
N1 In1 N6 107.60(5) . . ?
N3 In1 Cl1 106.00(4) . . ?
N4 In1 Cl1 114.90(4) . . ?
N4 In1 N3 109.80(5) . . ?
N4 In1 N6 56.91(5) . . ?
N6 In1 Cl1 103.80(4) . . ?
N6 In1 N3 150.18(5) . . ?
N2 N1 In1 98.81(10) . . ?
N2 N1 C1 118.83(14) . . ?
C1 N1 In1 142.35(12) . . ?
N3 N2 N1 109.48(14) . . ?
N2 N3 In1 94.77(10) . . ?
N2 N3 C13 115.79(14) . . ?
C13 N3 In1 149.03(11) . . ?
N5 N4 In1 98.18(10) . . ?
N5 N4 C25 118.91(14) . . ?
C25 N4 In1 142.73(11) . . ?
N6 N5 N4 109.33(14) . . ?
N5 N6 In1 95.41(10) . . ?
N5 N6 C37 116.77(14) . . ?
C37 N6 In1 145.92(11) . . ?
C2 C1 N1 116.73(17) . . ?
C2 C1 C6 122.44(17) . . ?
C6 C1 N1 120.73(18) . . ?
C1 C2 C7 122.18(17) . . ?
C3 C2 C1 117.51(19) . . ?
C3 C2 C7 120.31(19) . . ?
C4 C3 C2 121.1(2) . . ?
C3 C4 C5 120.40(19) . . ?
C4 C5 C6 121.5(2) . . ?
C1 C6 C10 121.75(17) . . ?
C5 C6 C1 117.05(19) . . ?
C5 C6 C10 121.20(19) . . ?
C2 C7 C8 111.49(18) . . ?
C2 C7 C9 112.13(19) . . ?
C8 C7 C9 111.2(2) . . ?
C11 C10 C6 111.48(17) . . ?
C11 C10 C12 111.2(2) . . ?
C12 C10 C6 114.05(18) . . ?
C14 C13 N3 118.46(16) . . ?
C18 C13 N3 119.71(16) . . ?
C18 C13 C14 121.82(17) . . ?
C13 C14 C19 120.63(16) . . ?
C15 C14 C13 117.97(17) . . ?
C15 C14 C19 121.36(17) . . ?
C16 C15 C14 120.99(18) . . ?
C17 C16 C15 120.01(18) . . ?
C16 C17 C18 121.32(18) . . ?
C13 C18 C22 122.50(17) . . ?
C17 C18 C13 117.88(17) . . ?
C17 C18 C22 119.59(17) . . ?
C14 C19 C20 112.45(17) . . ?
C14 C19 C21 110.33(17) . . ?
C20 C19 C21 110.83(18) . . ?
C18 C22 C23 111.63(17) . . ?
C18 C22 C24 109.50(19) . . ?
C23 C22 C24 111.8(2) . . ?
C26 C25 N4 116.69(16) . . ?
C30 C25 N4 121.29(16) . . ?
C30 C25 C26 121.92(17) . . ?
C25 C26 C31 121.71(17) . . ?
C27 C26 C25 118.03(18) . . ?
C27 C26 C31 120.26(18) . . ?
C28 C27 C26 120.79(19) . . ?
C29 C28 C27 120.35(19) . . ?
C28 C29 C30 121.35(19) . . ?
C25 C30 C34 122.82(17) . . ?
C29 C30 C25 117.55(18) . . ?
C29 C30 C34 119.61(17) . . ?
C26 C31 C32 111.27(17) . . ?
C26 C31 C33 112.10(18) . . ?
C32 C31 C33 111.28(18) . . ?
C30 C34 C35 112.32(18) . . ?
C30 C34 C36 110.63(17) . . ?
C36 C34 C35 110.92(19) . . ?
C38 C37 N6 118.88(16) . . ?
C38 C37 C42 122.18(16) . . ?
C42 C37 N6 118.86(16) . . ?
C37 C38 C43 120.79(16) . . ?
C39 C38 C37 117.93(17) . . ?
C39 C38 C43 121.19(17) . . ?
C40 C39 C38 120.82(18) . . ?
C39 C40 C41 120.36(18) . . ?
C40 C41 C42 121.21(18) . . ?
C37 C42 C46 121.38(16) . . ?
C41 C42 C37 117.46(17) . . ?
C41 C42 C46 121.15(17) . . ?
C38 C43 C44 113.81(17) . . ?
C38 C43 C45 109.58(16) . . ?
C45 C43 C44 110.94(17) . . ?
C42 C46 C47 113.26(17) . . ?
C42 C46 C48 110.51(16) . . ?
C47 C46 C48 110.94(18) . . ?

_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_PLAT910_9                   
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         11 Note  
RESPONSE: This reflection was found to be an outlier and was omitted from the 
final refinement.
;
# end Validation Reply Form
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_14
_database_code_depnum_ccdc_archive 'CCDC 1972006'
loop_
_audit_author_name
_audit_author_address
'Alasdair McKay'
;Monash University
Australia
;
_audit_update_record             
;
2019-12-14 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_audit_creation_date             2019-12-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
''
alasdair.mckay@monash.edu
_chemical_name_common            ?
_chemical_name_systematic        '[GaH(N3Dipp2)2]'
_chemical_formula_moiety         'C48 H69 Ga N6'
_chemical_formula_sum            'C48 H69 Ga N6'
_chemical_formula_weight         799.81
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.6502(6)
_cell_length_b                   16.1245(6)
_cell_length_c                   20.9328(8)
_cell_angle_alpha                90
_cell_angle_beta                 110.465(2)
_cell_angle_gamma                90
_cell_volume                     4632.8(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.863
_cell_measurement_theta_min      2.431
_shelx_estimated_absorpt_T_max   0.940
_shelx_estimated_absorpt_T_min   0.940
_exptl_absorpt_coefficient_mu    0.631
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1246 before and 0.0633 after correction. The Ratio of minimum to maximum transmission is 0.9052. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       cube
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39795
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         1.484
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7539
_reflns_number_total             10201
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.766
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         10201
_refine_ls_number_restraints     153
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0571
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0772P)²+5.0281P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1535
_refine_ls_wR_factor_ref         0.1675
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Others
 Sof(C11B)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C12B)=Sof(H12A)=Sof(H12B)=
 Sof(H12C)=Sof(H10A)=1-FVAR(1)
 Sof(H10)=Sof(C11A)=Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(C12A)=Sof(H12D)=
 Sof(H12E)=Sof(H12F)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10A), C10(H10), C19(H19), C22(H22), C31(H31), C34(H34), C43(H43),
  C46(H46)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C15(H15), C16(H16), C17(H17), C27(H27), C28(H28),
 C29(H29), C39(H39), C40(H40), C41(H41)
4.c Idealised Me refined as rotating group:
 C11B(H11A,H11B,H11C), C12B(H12A,H12B,H12C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C), C11A(H11D,H11E,H11F), C12A(H12D,H12E,H12F)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ga1 Ga 0.83151(2) 0.72130(2) 0.58456(2) 0.02911(12) Uani 1 1 d . U . . .
N1 N 0.96671(17) 0.70342(14) 0.56797(11) 0.0262(5) Uani 1 1 d . U . . .
C1 C 1.0326(2) 0.72577(18) 0.53340(15) 0.0307(6) Uani 1 1 d . U . . .
C11B C 0.901(2) 0.6080(17) 0.3800(17) 0.090(10) Uani 0.249(17) 1 d . U P A 2
H11A H 0.923365 0.625922 0.343289 0.135 Uiso 0.249(17) 1 calc GR . P A 2
H11B H 0.833337 0.588725 0.360491 0.135 Uiso 0.249(17) 1 calc GR . P A 2
H11C H 0.942305 0.562693 0.405528 0.135 Uiso 0.249(17) 1 calc GR . P A 2
C12B C 0.8363(19) 0.7528(17) 0.3823(15) 0.091(11) Uani 0.249(17) 1 d . U P A 2
H12A H 0.871216 0.784957 0.358447 0.137 Uiso 0.249(17) 1 calc GR . P A 2
H12B H 0.820566 0.788606 0.414856 0.137 Uiso 0.249(17) 1 calc GR . P A 2
H12C H 0.775979 0.730680 0.349182 0.137 Uiso 0.249(17) 1 calc GR . P A 2
N2 N 0.97704(16) 0.63022(14) 0.59462(11) 0.0270(5) Uani 1 1 d . U . . .
C2 C 1.1212(2) 0.7628(2) 0.56988(16) 0.0364(7) Uani 1 1 d . U . . .
N3 N 0.90582(17) 0.61858(14) 0.61805(12) 0.0279(5) Uani 1 1 d . U . . .
C3 C 1.1816(3) 0.7868(2) 0.5339(2) 0.0503(9) Uani 1 1 d . U . . .
H3 H 1.242961 0.811502 0.557749 0.060 Uiso 1 1 calc R . . . .
N4 N 0.75007(16) 0.74188(15) 0.65002(12) 0.0265(5) Uani 1 1 d . U . . .
C4 C 1.1535(3) 0.7752(3) 0.4651(2) 0.0585(10) Uani 1 1 d . U . . .
H4 H 1.195616 0.791405 0.441644 0.070 Uiso 1 1 calc R . . . .
N5 N 0.78868(16) 0.81403(15) 0.66808(12) 0.0271(5) Uani 1 1 d . U . . .
C5 C 1.0658(3) 0.7406(3) 0.43002(19) 0.0552(10) Uani 1 1 d . U . . .
H5 H 1.046989 0.734171 0.382024 0.066 Uiso 1 1 calc R . . . .
N6 N 0.85705(16) 0.82285(14) 0.64119(11) 0.0262(5) Uani 1 1 d . U . . .
C6 C 1.0024(3) 0.7143(2) 0.46278(16) 0.0417(7) Uani 1 1 d . U . . .
C7 C 1.1547(2) 0.7744(2) 0.64578(17) 0.0399(7) Uani 1 1 d . U . . .
H7 H 1.096133 0.769183 0.659622 0.048 Uiso 1 1 calc R . . . .
C8 C 1.1979(4) 0.8594(3) 0.6675(2) 0.0683(12) Uani 1 1 d . U . . .
H8A H 1.212004 0.866415 0.716564 0.102 Uiso 1 1 calc GR . . . .
H8B H 1.151373 0.901911 0.642427 0.102 Uiso 1 1 calc GR . . . .
H8C H 1.258289 0.864913 0.657731 0.102 Uiso 1 1 calc GR . . . .
C9 C 1.2232(4) 0.7062(3) 0.6799(2) 0.0862(16) Uani 1 1 d . U . . .
H9A H 1.196617 0.653059 0.658711 0.129 Uiso 1 1 calc GR . . . .
H9B H 1.231539 0.704650 0.728421 0.129 Uiso 1 1 calc GR . . . .
H9C H 1.286416 0.715925 0.674957 0.129 Uiso 1 1 calc GR . . . .
C10 C 0.9061(3) 0.6747(3) 0.42399(18) 0.0559(10) Uani 1 1 d . U . . .
H10A H 0.878222 0.654883 0.458569 0.067 Uiso 0.249(17) 1 calc R . P A 2
H10 H 0.859683 0.687000 0.448178 0.067 Uiso 0.751(17) 1 calc R . P A 1
C13 C 0.9004(2) 0.53983(18) 0.64860(15) 0.0310(6) Uani 1 1 d . U . . .
C14 C 0.9684(2) 0.51938(19) 0.71237(15) 0.0347(7) Uani 1 1 d . U . . .
C15 C 0.9587(3) 0.4426(2) 0.74005(18) 0.0446(8) Uani 1 1 d . U . . .
H15 H 1.005085 0.426492 0.782708 0.054 Uiso 1 1 calc R . . . .
C16 C 0.8835(3) 0.3898(2) 0.70697(19) 0.0529(9) Uani 1 1 d . U . . .
H16 H 0.877359 0.338452 0.727337 0.063 Uiso 1 1 calc R . . . .
C17 C 0.8166(3) 0.4113(2) 0.6441(2) 0.0510(9) Uani 1 1 d . U . . .
H17 H 0.765036 0.374249 0.621387 0.061 Uiso 1 1 calc R . . . .
C18 C 0.8239(3) 0.4866(2) 0.61350(17) 0.0421(7) Uani 1 1 d . U . . .
C19 C 1.0514(2) 0.5761(2) 0.75160(16) 0.0399(7) Uani 1 1 d . U . . .
H19 H 1.044826 0.628703 0.725020 0.048 Uiso 1 1 calc R . . . .
C20 C 1.1498(3) 0.5379(3) 0.7596(3) 0.0810(15) Uani 1 1 d . U . . .
H20A H 1.158123 0.486303 0.785767 0.122 Uiso 1 1 calc GR . . . .
H20B H 1.201811 0.576805 0.783642 0.122 Uiso 1 1 calc GR . . . .
H20C H 1.152718 0.525907 0.714433 0.122 Uiso 1 1 calc GR . . . .
C21 C 1.0493(3) 0.5983(3) 0.8219(2) 0.0673(12) Uani 1 1 d . U . . .
H21A H 0.990706 0.630844 0.816837 0.101 Uiso 1 1 calc GR . . . .
H21B H 1.107281 0.630987 0.846796 0.101 Uiso 1 1 calc GR . . . .
H21C H 1.048691 0.547360 0.847267 0.101 Uiso 1 1 calc GR . . . .
C22 C 0.7518(3) 0.5076(2) 0.54357(19) 0.0513(9) Uani 1 1 d . U . . .
H22 H 0.774830 0.559341 0.527608 0.062 Uiso 1 1 calc R . . . .
C23 C 0.7458(4) 0.4387(4) 0.4914(2) 0.0905(17) Uani 1 1 d . U . . .
H23A H 0.811380 0.425778 0.491859 0.136 Uiso 1 1 calc GR . . . .
H23B H 0.705275 0.457503 0.445716 0.136 Uiso 1 1 calc GR . . . .
H23C H 0.716820 0.388896 0.503263 0.136 Uiso 1 1 calc GR . . . .
C24 C 0.6510(4) 0.5246(4) 0.5460(3) 0.0873(16) Uani 1 1 d . U . . .
H24A H 0.625605 0.474036 0.559822 0.131 Uiso 1 1 calc GR . . . .
H24B H 0.607203 0.541825 0.500799 0.131 Uiso 1 1 calc GR . . . .
H24C H 0.655109 0.568780 0.579057 0.131 Uiso 1 1 calc GR . . . .
C25 C 0.6646(2) 0.72386(18) 0.66536(15) 0.0298(6) Uani 1 1 d . U . . .
C26 C 0.6725(2) 0.67212(19) 0.72058(16) 0.0355(7) Uani 1 1 d . U . . .
C27 C 0.5890(3) 0.6524(2) 0.7337(2) 0.0552(10) Uani 1 1 d . U . . .
H27 H 0.593017 0.618168 0.771592 0.066 Uiso 1 1 calc R . . . .
C28 C 0.4992(3) 0.6823(3) 0.6918(3) 0.0746(14) Uani 1 1 d . U . . .
H28 H 0.441987 0.668099 0.700852 0.090 Uiso 1 1 calc R . . . .
C29 C 0.4928(3) 0.7319(3) 0.6379(2) 0.0620(11) Uani 1 1 d . U . . .
H29 H 0.430651 0.751954 0.609963 0.074 Uiso 1 1 calc R . . . .
C30 C 0.5746(2) 0.7541(2) 0.62222(18) 0.0404(7) Uani 1 1 d . U . . .
C31 C 0.7702(2) 0.6413(2) 0.76767(16) 0.0363(7) Uani 1 1 d . U . . .
H31 H 0.817212 0.647004 0.742971 0.044 Uiso 1 1 calc R . . . .
C32 C 0.7683(3) 0.5505(3) 0.7864(3) 0.0739(14) Uani 1 1 d . U . . .
H32A H 0.723068 0.542827 0.811027 0.111 Uiso 1 1 calc GR . . . .
H32B H 0.833801 0.533112 0.815387 0.111 Uiso 1 1 calc GR . . . .
H32C H 0.746865 0.516858 0.744731 0.111 Uiso 1 1 calc GR . . . .
C33 C 0.8053(3) 0.6968(4) 0.8295(2) 0.0801(15) Uani 1 1 d . U . . .
H33A H 0.805897 0.754499 0.814960 0.120 Uiso 1 1 calc GR . . . .
H33B H 0.871296 0.680365 0.858255 0.120 Uiso 1 1 calc GR . . . .
H33C H 0.761478 0.691606 0.855563 0.120 Uiso 1 1 calc GR . . . .
C34 C 0.5646(2) 0.8066(2) 0.56023(18) 0.0485(8) Uani 1 1 d . U . . .
H34 H 0.631902 0.819716 0.561435 0.058 Uiso 1 1 calc R . . . .
C35 C 0.5143(5) 0.7581(4) 0.4954(2) 0.0953(18) Uani 1 1 d . U . . .
H35A H 0.551485 0.707587 0.495305 0.143 Uiso 1 1 calc GR . . . .
H35B H 0.510526 0.792261 0.455799 0.143 Uiso 1 1 calc GR . . . .
H35C H 0.448407 0.743108 0.493059 0.143 Uiso 1 1 calc GR . . . .
C36 C 0.5143(4) 0.8877(3) 0.5611(3) 0.0884(17) Uani 1 1 d . U . . .
H36A H 0.445766 0.877327 0.554768 0.133 Uiso 1 1 calc GR . . . .
H36B H 0.518206 0.923124 0.524078 0.133 Uiso 1 1 calc GR . . . .
H36C H 0.546103 0.915443 0.604899 0.133 Uiso 1 1 calc GR . . . .
C37 C 0.9133(2) 0.89706(18) 0.65490(15) 0.0300(6) Uani 1 1 d . U . . .
C38 C 0.9030(2) 0.9501(2) 0.60006(17) 0.0398(7) Uani 1 1 d . U . . .
C39 C 0.9620(3) 1.0201(2) 0.6119(2) 0.0500(9) Uani 1 1 d . U . . .
H39 H 0.955853 1.057263 0.575404 0.060 Uiso 1 1 calc R . . . .
C40 C 1.0287(3) 1.0365(2) 0.6751(2) 0.0513(9) Uani 1 1 d . U . . .
H40 H 1.068806 1.084319 0.681865 0.062 Uiso 1 1 calc R . . . .
C41 C 1.0380(2) 0.9840(2) 0.7290(2) 0.0453(8) Uani 1 1 d . U . . .
H41 H 1.084462 0.996233 0.772719 0.054 Uiso 1 1 calc R . . . .
C42 C 0.9802(2) 0.9130(2) 0.72039(17) 0.0361(7) Uani 1 1 d . U . . .
C43 C 0.8266(3) 0.9352(2) 0.53072(17) 0.0503(9) Uani 1 1 d . U . . .
H43 H 0.803105 0.876943 0.530261 0.060 Uiso 1 1 calc R . . . .
C44 C 0.7400(3) 0.9914(4) 0.5191(3) 0.0879(16) Uani 1 1 d . U . . .
H44A H 0.715828 0.985453 0.557062 0.132 Uiso 1 1 calc GR . . . .
H44B H 0.688340 0.976074 0.476391 0.132 Uiso 1 1 calc GR . . . .
H44C H 0.759421 1.049034 0.516454 0.132 Uiso 1 1 calc GR . . . .
C45 C 0.8672(4) 0.9427(5) 0.4735(2) 0.100(2) Uani 1 1 d . U . . .
H45A H 0.875164 1.001369 0.464496 0.150 Uiso 1 1 calc GR . . . .
H45B H 0.822025 0.916669 0.432156 0.150 Uiso 1 1 calc GR . . . .
H45C H 0.930484 0.914732 0.486715 0.150 Uiso 1 1 calc GR . . . .
C46 C 0.9898(2) 0.8579(2) 0.78108(17) 0.0431(8) Uani 1 1 d . U . . .
H46 H 0.952903 0.805717 0.763122 0.052 Uiso 1 1 calc R . . . .
C47 C 0.9437(3) 0.8982(3) 0.8277(2) 0.0661(12) Uani 1 1 d . U . . .
H47A H 0.978794 0.949359 0.846673 0.099 Uiso 1 1 calc GR . . . .
H47B H 0.946903 0.860043 0.864831 0.099 Uiso 1 1 calc GR . . . .
H47C H 0.875406 0.911297 0.801638 0.099 Uiso 1 1 calc GR . . . .
C48 C 1.0951(3) 0.8333(3) 0.8219(2) 0.0641(11) Uani 1 1 d . U . . .
H48A H 1.122587 0.802841 0.792299 0.096 Uiso 1 1 calc GR . . . .
H48B H 1.096281 0.797913 0.860245 0.096 Uiso 1 1 calc GR . . . .
H48C H 1.133889 0.883276 0.839233 0.096 Uiso 1 1 calc GR . . . .
C11A C 0.9221(5) 0.5777(5) 0.4245(5) 0.077(2) Uani 0.751(17) 1 d . U P A 1
H11D H 0.971932 0.565053 0.404649 0.115 Uiso 0.751(17) 1 calc GR . P A 1
H11E H 0.860786 0.550612 0.397695 0.115 Uiso 0.751(17) 1 calc GR . P A 1
H11F H 0.943465 0.557336 0.471582 0.115 Uiso 0.751(17) 1 calc GR . P A 1
C12A C 0.8626(5) 0.7050(8) 0.3521(4) 0.093(4) Uani 0.751(17) 1 d . U P A 1
H12D H 0.850908 0.764841 0.352171 0.140 Uiso 0.751(17) 1 calc GR . P A 1
H12E H 0.800821 0.676306 0.329188 0.140 Uiso 0.751(17) 1 calc GR . P A 1
H12F H 0.907663 0.693753 0.327832 0.140 Uiso 0.751(17) 1 calc GR . P A 1
H H 0.751(2) 0.7230(18) 0.5148(16) 0.031(8) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ga1 N1 2.147(2) . ?
Ga1 N3 1.971(2) . ?
Ga1 N4 2.134(2) . ?
Ga1 N6 1.979(2) . ?
Ga1 H 1.52(3) . ?
N1 C1 1.440(4) . ?
N1 N2 1.292(3) . ?
C1 C2 1.390(4) . ?
C1 C6 1.399(4) . ?
C11B H11A 0.9800 . ?
C11B H11B 0.9800 . ?
C11B H11C 0.9800 . ?
C11B C10 1.400(19) . ?
C12B H12A 0.9800 . ?
C12B H12B 0.9800 . ?
C12B H12C 0.9800 . ?
C12B C10 1.66(2) . ?
N2 N3 1.312(3) . ?
C2 C3 1.401(4) . ?
C2 C7 1.502(5) . ?
N3 C13 1.436(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.366(6) . ?
N4 N5 1.291(3) . ?
N4 C25 1.427(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.356(6) . ?
N5 N6 1.317(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.400(5) . ?
N6 C37 1.424(4) . ?
C6 C10 1.502(5) . ?
C7 H7 1.0000 . ?
C7 C8 1.511(5) . ?
C7 C9 1.493(6) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 1.0000 . ?
C10 H10 1.0000 . ?
C10 C11A 1.580(9) . ?
C10 C12A 1.497(7) . ?
C13 C14 1.398(4) . ?
C13 C18 1.399(5) . ?
C14 C15 1.395(4) . ?
C14 C19 1.514(5) . ?
C15 H15 0.9500 . ?
C15 C16 1.372(5) . ?
C16 H16 0.9500 . ?
C16 C17 1.383(5) . ?
C17 H17 0.9500 . ?
C17 C18 1.393(5) . ?
C18 C22 1.514(5) . ?
C19 H19 1.0000 . ?
C19 C20 1.522(5) . ?
C19 C21 1.525(5) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22 1.0000 . ?
C22 C23 1.540(6) . ?
C22 C24 1.520(6) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.397(4) . ?
C25 C30 1.400(4) . ?
C26 C27 1.382(4) . ?
C26 C31 1.510(4) . ?
C27 H27 0.9500 . ?
C27 C28 1.387(5) . ?
C28 H28 0.9500 . ?
C28 C29 1.359(6) . ?
C29 H29 0.9500 . ?
C29 C30 1.396(5) . ?
C30 C34 1.513(5) . ?
C31 H31 1.0000 . ?
C31 C32 1.519(5) . ?
C31 C33 1.509(5) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34 1.0000 . ?
C34 C35 1.516(6) . ?
C34 C36 1.505(6) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.397(4) . ?
C37 C42 1.402(4) . ?
C38 C39 1.390(5) . ?
C38 C43 1.510(5) . ?
C39 H39 0.9500 . ?
C39 C40 1.368(6) . ?
C40 H40 0.9500 . ?
C40 C41 1.380(5) . ?
C41 H41 0.9500 . ?
C41 C42 1.397(5) . ?
C42 C46 1.516(5) . ?
C43 H43 1.0000 . ?
C43 C44 1.508(6) . ?
C43 C45 1.517(6) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46 1.0000 . ?
C46 C47 1.514(5) . ?
C46 C48 1.531(5) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C11A H11D 0.9800 . ?
C11A H11E 0.9800 . ?
C11A H11F 0.9800 . ?
C12A H12D 0.9800 . ?
C12A H12E 0.9800 . ?
C12A H12F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ga1 H 107.4(12) . . ?
N3 Ga1 N1 61.22(9) . . ?
N3 Ga1 N4 105.39(9) . . ?
N3 Ga1 N6 121.12(10) . . ?
N3 Ga1 H 120.2(11) . . ?
N4 Ga1 N1 151.56(9) . . ?
N4 Ga1 H 101.0(12) . . ?
N6 Ga1 N1 102.48(9) . . ?
N6 Ga1 N4 61.17(9) . . ?
N6 Ga1 H 118.7(11) . . ?
C1 N1 Ga1 150.02(18) . . ?
N2 N1 Ga1 91.62(16) . . ?
N2 N1 C1 116.6(2) . . ?
C2 C1 N1 119.5(3) . . ?
C2 C1 C6 121.8(3) . . ?
C6 C1 N1 118.5(3) . . ?
H11A C11B H11B 109.5 . . ?
H11A C11B H11C 109.5 . . ?
H11B C11B H11C 109.5 . . ?
C10 C11B H11A 109.5 . . ?
C10 C11B H11B 109.5 . . ?
C10 C11B H11C 109.5 . . ?
H12A C12B H12B 109.5 . . ?
H12A C12B H12C 109.5 . . ?
H12B C12B H12C 109.5 . . ?
C10 C12B H12A 109.5 . . ?
C10 C12B H12B 109.5 . . ?
C10 C12B H12C 109.5 . . ?
N1 N2 N3 107.7(2) . . ?
C1 C2 C3 117.8(3) . . ?
C1 C2 C7 122.1(3) . . ?
C3 C2 C7 120.0(3) . . ?
N2 N3 Ga1 99.16(16) . . ?
N2 N3 C13 117.9(2) . . ?
C13 N3 Ga1 142.31(19) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 C2 121.0(4) . . ?
C4 C3 H3 119.5 . . ?
N5 N4 Ga1 92.41(16) . . ?
N5 N4 C25 116.5(2) . . ?
C25 N4 Ga1 147.60(19) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 C3 120.4(3) . . ?
C5 C4 H4 119.8 . . ?
N4 N5 N6 107.0(2) . . ?
C4 C5 H5 119.2 . . ?
C4 C5 C6 121.6(3) . . ?
C6 C5 H5 119.2 . . ?
N5 N6 Ga1 98.85(16) . . ?
N5 N6 C37 118.5(2) . . ?
C37 N6 Ga1 142.27(18) . . ?
C1 C6 C5 117.3(3) . . ?
C1 C6 C10 121.2(3) . . ?
C5 C6 C10 121.5(3) . . ?
C2 C7 H7 107.5 . . ?
C2 C7 C8 112.3(3) . . ?
C8 C7 H7 107.5 . . ?
C9 C7 C2 109.3(3) . . ?
C9 C7 H7 107.5 . . ?
C9 C7 C8 112.6(4) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11B C10 C12B 110.8(15) . . ?
C11B C10 C6 120.5(12) . . ?
C11B C10 H10A 106.8 . . ?
C12B C10 H10A 106.8 . . ?
C6 C10 C12B 104.5(8) . . ?
C6 C10 H10A 106.8 . . ?
C6 C10 H10 108.6 . . ?
C6 C10 C11A 108.0(4) . . ?
C11A C10 H10 108.6 . . ?
C12A C10 C6 113.2(5) . . ?
C12A C10 H10 108.6 . . ?
C12A C10 C11A 109.9(5) . . ?
C14 C13 N3 120.1(3) . . ?
C14 C13 C18 122.0(3) . . ?
C18 C13 N3 117.9(3) . . ?
C13 C14 C19 123.0(3) . . ?
C15 C14 C13 117.6(3) . . ?
C15 C14 C19 119.4(3) . . ?
C14 C15 H15 119.3 . . ?
C16 C15 C14 121.4(3) . . ?
C16 C15 H15 119.3 . . ?
C15 C16 H16 119.9 . . ?
C15 C16 C17 120.1(3) . . ?
C17 C16 H16 119.9 . . ?
C16 C17 H17 119.6 . . ?
C16 C17 C18 120.9(3) . . ?
C18 C17 H17 119.6 . . ?
C13 C18 C22 122.0(3) . . ?
C17 C18 C13 118.0(3) . . ?
C17 C18 C22 120.0(3) . . ?
C14 C19 H19 107.9 . . ?
C14 C19 C20 111.4(3) . . ?
C14 C19 C21 112.5(3) . . ?
C20 C19 H19 107.9 . . ?
C20 C19 C21 109.1(3) . . ?
C21 C19 H19 107.9 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C18 C22 H22 107.9 . . ?
C18 C22 C23 111.8(3) . . ?
C18 C22 C24 111.4(3) . . ?
C23 C22 H22 107.9 . . ?
C24 C22 H22 107.9 . . ?
C24 C22 C23 109.8(4) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 N4 118.9(3) . . ?
C26 C25 C30 121.9(3) . . ?
C30 C25 N4 119.1(3) . . ?
C25 C26 C31 121.5(3) . . ?
C27 C26 C25 118.7(3) . . ?
C27 C26 C31 119.8(3) . . ?
C26 C27 H27 119.9 . . ?
C26 C27 C28 120.2(4) . . ?
C28 C27 H27 119.9 . . ?
C27 C28 H28 119.8 . . ?
C29 C28 C27 120.4(3) . . ?
C29 C28 H28 119.8 . . ?
C28 C29 H29 119.0 . . ?
C28 C29 C30 122.0(3) . . ?
C30 C29 H29 119.0 . . ?
C25 C30 C34 122.3(3) . . ?
C29 C30 C25 116.9(3) . . ?
C29 C30 C34 120.8(3) . . ?
C26 C31 H31 107.4 . . ?
C26 C31 C32 112.8(3) . . ?
C32 C31 H31 107.4 . . ?
C33 C31 C26 109.0(3) . . ?
C33 C31 H31 107.4 . . ?
C33 C31 C32 112.5(4) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C30 C34 H34 107.3 . . ?
C30 C34 C35 110.5(4) . . ?
C35 C34 H34 107.3 . . ?
C36 C34 C30 112.1(3) . . ?
C36 C34 H34 107.3 . . ?
C36 C34 C35 111.8(4) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38 C37 N6 117.4(3) . . ?
C38 C37 C42 121.9(3) . . ?
C42 C37 N6 120.6(3) . . ?
C37 C38 C43 121.6(3) . . ?
C39 C38 C37 118.0(3) . . ?
C39 C38 C43 120.4(3) . . ?
C38 C39 H39 119.4 . . ?
C40 C39 C38 121.2(3) . . ?
C40 C39 H39 119.4 . . ?
C39 C40 H40 119.8 . . ?
C39 C40 C41 120.4(3) . . ?
C41 C40 H40 119.8 . . ?
C40 C41 H41 119.5 . . ?
C40 C41 C42 120.9(3) . . ?
C42 C41 H41 119.5 . . ?
C37 C42 C46 122.7(3) . . ?
C41 C42 C37 117.5(3) . . ?
C41 C42 C46 119.8(3) . . ?
C38 C43 H43 107.2 . . ?
C38 C43 C45 112.5(4) . . ?
C44 C43 C38 111.0(3) . . ?
C44 C43 H43 107.2 . . ?
C44 C43 C45 111.5(4) . . ?
C45 C43 H43 107.2 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C42 C46 H46 107.4 . . ?
C42 C46 C48 113.6(3) . . ?
C47 C46 C42 110.9(3) . . ?
C47 C46 H46 107.4 . . ?
C47 C46 C48 110.0(3) . . ?
C48 C46 H46 107.4 . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C46 C48 H48A 109.5 . . ?
C46 C48 H48B 109.5 . . ?
C46 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C10 C11A H11D 109.5 . . ?
C10 C11A H11E 109.5 . . ?
C10 C11A H11F 109.5 . . ?
H11D C11A H11E 109.5 . . ?
H11D C11A H11F 109.5 . . ?
H11E C11A H11F 109.5 . . ?
C10 C12A H12D 109.5 . . ?
C10 C12A H12E 109.5 . . ?
C10 C12A H12F 109.5 . . ?
H12D C12A H12E 109.5 . . ?
H12D C12A H12F 109.5 . . ?
H12E C12A H12F 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_10
_database_code_depnum_ccdc_archive 'CCDC 1972003'
loop_
_audit_author_name
_audit_author_address
'Alasdair McKay'
;Monash University
Australia
;
_audit_update_record             
;
2019-12-14 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_audit_creation_date             2019-04-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
''
alasdair.mckay@monash.edu
_chemical_name_common            ?
_chemical_name_systematic        '[InI(N3Dipp2)2]'
_chemical_formula_moiety         'C48 H66 I In N6'
_chemical_formula_sum            'C48 H66 I In N6'
_chemical_formula_weight         968.78
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 S O2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.375(3)
_cell_length_b                   16.586(3)
_cell_length_c                   21.259(4)
_cell_angle_alpha                90
_cell_angle_beta                 109.19(3)
_cell_angle_gamma                90
_cell_volume                     4786.8(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2450
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.9851
_cell_measurement_theta_min      2.8293
_shelx_estimated_absorpt_T_max   0.891
_shelx_estimated_absorpt_T_min   0.891
_exptl_absorpt_coefficient_mu    1.176
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       cube
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1254
_diffrn_reflns_av_unetI/netI     0.1553
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28650
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.681
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.878
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 8.4171
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -12.00  107.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       21.0069   65.0000  169.0000 119

#__ type_ start__ end____ width___ exp.time_
  2 omega  -75.00   51.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       21.0069  -77.0000  -90.0000 126

#__ type_ start__ end____ width___ exp.time_
  3 omega -120.00  -32.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.4444  179.0000  -90.0000 88

#__ type_ start__ end____ width___ exp.time_
  4 omega  -16.00   14.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.4444  -77.0000  150.0000 30

#__ type_ start__ end____ width___ exp.time_
  5 omega -103.00  -74.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.4444  -77.0000  150.0000 29
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0293542000
_diffrn_orient_matrix_UB_12      -0.0353692000
_diffrn_orient_matrix_UB_13      0.0051572000
_diffrn_orient_matrix_UB_21      -0.0364703000
_diffrn_orient_matrix_UB_22      -0.0198619000
_diffrn_orient_matrix_UB_23      -0.0257831000
_diffrn_orient_matrix_UB_31      0.0224603000
_diffrn_orient_matrix_UB_32      0.0135710000
_diffrn_orient_matrix_UB_33      -0.0232839000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4430
_reflns_number_total             9062
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.528
_refine_diff_density_min         -1.782
_refine_diff_density_rms         0.158
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         9062
_refine_ls_number_restraints     499
_refine_ls_R_factor_all          0.1797
_refine_ls_R_factor_gt           0.0905
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0921P)²+18.0010P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2067
_refine_ls_wR_factor_ref         0.2658
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C36A-C34 \\sim C36B-C34 \\sim C35A-C34 \\sim C35B-C34
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C35B \\sim C34 \\sim C36B: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C35A \\sim C34 \\sim C36A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C35B)=Sof(H35D)=Sof(H35E)=Sof(H35F)=Sof(C36B)=Sof(H36D)=Sof(H36E)=
 Sof(H36F)=1-FVAR(1)
 Sof(C35A)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C36A)=Sof(H36A)=Sof(H36B)=
 Sof(H36C)=FVAR(1)
 Sof(C11B)=Sof(H11D)=Sof(H11E)=Sof(H11F)=1-FVAR(2)
 Sof(C11A)=Sof(H11A)=Sof(H11B)=Sof(H11C)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C19(H19), C22(H22), C31(H31), C43(H43), C46(H46)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C15(H15), C16(H16), C17(H17), C27(H27), C28(H28),
 C29(H29), C39(H39), C40(H40), C41(H41)
6.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11A(H11A,H11B,H11C), C11B(H11D,H11E,H11F),
 C12(H12A,H12B,H12C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C),
 C35A(H35A,H35B,H35C), C35B(H35D,H35E,H35F), C36A(H36A,H36B,H36C), C36B(H36D,
 H36E,H36F), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.20826(6) 0.23891(6) 0.54247(4) 0.0589(3) Uani 1 1 d . U . . .
In1 In 0.23716(5) 0.23439(6) 0.42360(4) 0.0371(3) Uani 1 1 d . U . . .
N1 N 0.2814(5) 0.1191(6) 0.3915(4) 0.037(2) Uani 1 1 d . U . . .
N2 N 0.3782(5) 0.1311(6) 0.4161(4) 0.034(2) Uani 1 1 d . U . . .
N3 N 0.3953(5) 0.2007(6) 0.4413(4) 0.0315(19) Uani 1 1 d . U . . .
N4 N 0.2121(6) 0.3481(6) 0.3678(4) 0.039(2) Uani 1 1 d . U . . .
N5 N 0.1203(6) 0.3374(6) 0.3383(4) 0.034(2) Uani 1 1 d . U . . .
N6 N 0.0944(6) 0.2665(6) 0.3496(4) 0.034(2) Uani 1 1 d . U . . .
C1 C 0.2476(7) 0.0453(8) 0.3588(5) 0.040(2) Uani 1 1 d . U . . .
C2 C 0.1921(8) -0.0056(8) 0.3868(6) 0.047(3) Uani 1 1 d . U . . .
C3 C 0.1530(9) -0.0753(8) 0.3538(6) 0.053(3) Uani 1 1 d . U . . .
H3 H 0.113538 -0.109254 0.370753 0.064 Uiso 1 1 calc R . . . .
C4 C 0.1712(9) -0.0962(8) 0.2959(6) 0.056(3) Uani 1 1 d . U . . .
H4 H 0.143709 -0.144388 0.273199 0.067 Uiso 1 1 calc R . . . .
C5 C 0.2283(8) -0.0484(8) 0.2710(5) 0.046(3) Uani 1 1 d . U . . .
H5 H 0.239230 -0.064524 0.231183 0.055 Uiso 1 1 calc R . . . .
C6 C 0.2700(7) 0.0213(8) 0.3009(5) 0.042(2) Uani 1 1 d . U . . .
C7 C 0.1729(9) 0.0177(8) 0.4518(6) 0.055(3) Uani 1 1 d . U . . .
H7 H 0.220336 0.061156 0.474333 0.066 Uiso 1 1 calc R . . . .
C8 C 0.0680(9) 0.0497(10) 0.4379(7) 0.073(4) Uani 1 1 d . U . . .
H8A H 0.056550 0.095375 0.407030 0.109 Uiso 1 1 calc GR . . . .
H8B H 0.059842 0.067487 0.479796 0.109 Uiso 1 1 calc GR . . . .
H8C H 0.020451 0.006862 0.418153 0.109 Uiso 1 1 calc GR . . . .
C9 C 0.1918(15) -0.0554(10) 0.4979(7) 0.099(6) Uani 1 1 d . U . . .
H9A H 0.154150 -0.101588 0.473706 0.149 Uiso 1 1 calc GR . . . .
H9B H 0.171136 -0.043160 0.536400 0.149 Uiso 1 1 calc GR . . . .
H9C H 0.262195 -0.068403 0.513084 0.149 Uiso 1 1 calc GR . . . .
C10 C 0.3309(8) 0.0766(8) 0.2697(6) 0.050(3) Uani 1 1 d . U . . .
C11A C 0.260(2) 0.0998(19) 0.1958(14) 0.065(10) Uani 0.53(3) 1 d . U P A 1
H11A H 0.287743 0.145837 0.179219 0.098 Uiso 0.53(3) 1 calc GR . P A 1
H11B H 0.194483 0.114199 0.197351 0.098 Uiso 0.53(3) 1 calc GR . P A 1
H11C H 0.254092 0.053653 0.166034 0.098 Uiso 0.53(3) 1 calc GR . P A 1
C11B C 0.2822(19) 0.153(2) 0.2372(15) 0.056(9) Uani 0.47(3) 1 d . U P A 2
H11D H 0.324500 0.180184 0.215696 0.084 Uiso 0.47(3) 1 calc GR . P A 2
H11E H 0.271843 0.188879 0.270998 0.084 Uiso 0.47(3) 1 calc GR . P A 2
H11F H 0.218608 0.140430 0.203643 0.084 Uiso 0.47(3) 1 calc GR . P A 2
C12 C 0.4004(12) 0.0299(11) 0.2456(9) 0.102(6) Uani 1 1 d . U . . .
H12A H 0.368958 -0.020299 0.225010 0.153 Uiso 1 1 calc GR . . . .
H12B H 0.459685 0.017388 0.283200 0.153 Uiso 1 1 calc GR . . . .
H12C H 0.418622 0.061906 0.212647 0.153 Uiso 1 1 calc GR . . . .
C13 C 0.4974(7) 0.2171(8) 0.4745(5) 0.040(3) Uani 1 1 d . U . . .
C14 C 0.5391(8) 0.1974(9) 0.5411(5) 0.049(3) Uani 1 1 d . U . . .
C15 C 0.6382(8) 0.2172(9) 0.5712(6) 0.061(4) Uani 1 1 d . U . . .
H15 H 0.669439 0.206352 0.617177 0.073 Uiso 1 1 calc R . . . .
C16 C 0.6900(9) 0.2514(9) 0.5360(6) 0.062(4) Uani 1 1 d . U . . .
H16 H 0.758242 0.260793 0.557805 0.075 Uiso 1 1 calc R . . . .
C17 C 0.6502(8) 0.2734(9) 0.4704(6) 0.059(4) Uani 1 1 d . U . . .
H17 H 0.688703 0.298849 0.447371 0.070 Uiso 1 1 calc R . . . .
C18 C 0.5504(7) 0.2569(8) 0.4390(6) 0.045(3) Uani 1 1 d . U . . .
C19 C 0.4802(9) 0.1589(9) 0.5779(6) 0.058(3) Uani 1 1 d . U . . .
H19 H 0.409554 0.172366 0.553863 0.070 Uiso 1 1 calc R . . . .
C20 C 0.5045(11) 0.1893(11) 0.6494(6) 0.078(5) Uani 1 1 d . U . . .
H20A H 0.573186 0.176386 0.674722 0.117 Uiso 1 1 calc GR . . . .
H20B H 0.460948 0.163129 0.670324 0.117 Uiso 1 1 calc GR . . . .
H20C H 0.494994 0.247818 0.649108 0.117 Uiso 1 1 calc GR . . . .
C21 C 0.4900(10) 0.0670(10) 0.5763(7) 0.079(4) Uani 1 1 d . U . . .
H21A H 0.457306 0.047441 0.530924 0.118 Uiso 1 1 calc GR . . . .
H21B H 0.459115 0.042550 0.606498 0.118 Uiso 1 1 calc GR . . . .
H21C H 0.559896 0.052341 0.590611 0.118 Uiso 1 1 calc GR . . . .
C22 C 0.5071(9) 0.2790(9) 0.3661(6) 0.058(3) Uani 1 1 d . U . . .
H22 H 0.434189 0.271472 0.352887 0.069 Uiso 1 1 calc R . . . .
C23 C 0.5248(12) 0.3640(10) 0.3520(8) 0.093(5) Uani 1 1 d . U . . .
H23A H 0.494788 0.399732 0.376651 0.140 Uiso 1 1 calc GR . . . .
H23B H 0.495434 0.374404 0.304157 0.140 Uiso 1 1 calc GR . . . .
H23C H 0.595846 0.374116 0.365914 0.140 Uiso 1 1 calc GR . . . .
C24 C 0.5442(11) 0.2218(11) 0.3237(7) 0.081(4) Uani 1 1 d . U . . .
H24A H 0.612346 0.235608 0.327999 0.122 Uiso 1 1 calc GR . . . .
H24B H 0.502649 0.226678 0.276949 0.122 Uiso 1 1 calc GR . . . .
H24C H 0.541630 0.166294 0.338792 0.122 Uiso 1 1 calc GR . . . .
C25 C 0.2559(7) 0.4222(7) 0.3601(5) 0.037(2) Uani 1 1 d . U . . .
C26 C 0.2986(7) 0.4686(8) 0.4164(6) 0.045(3) Uani 1 1 d . U . . .
C27 C 0.3469(8) 0.5419(9) 0.4085(7) 0.056(3) Uani 1 1 d . U . . .
H27 H 0.374149 0.576988 0.445275 0.067 Uiso 1 1 calc R . . . .
C28 C 0.3532(8) 0.5605(9) 0.3475(8) 0.063(3) Uani 1 1 d . U . . .
H28 H 0.389170 0.607135 0.343518 0.076 Uiso 1 1 calc R . . . .
C29 C 0.3110(9) 0.5159(9) 0.2930(7) 0.059(3) Uani 1 1 d . U . . .
H29 H 0.315055 0.532479 0.251222 0.071 Uiso 1 1 calc R . . . .
C30 C 0.2605(9) 0.4444(8) 0.2976(6) 0.052(3) Uani 1 1 d . U . . .
C31 C 0.2890(8) 0.4448(9) 0.4813(6) 0.053(3) Uani 1 1 d . U . . .
H31 H 0.248418 0.394542 0.474445 0.063 Uiso 1 1 calc R . . . .
C32 C 0.3914(10) 0.4266(12) 0.5321(7) 0.094(6) Uani 1 1 d . U . . .
H32A H 0.426066 0.388077 0.512756 0.140 Uiso 1 1 calc GR . . . .
H32B H 0.383627 0.403419 0.572523 0.140 Uiso 1 1 calc GR . . . .
H32C H 0.429517 0.476606 0.543383 0.140 Uiso 1 1 calc GR . . . .
C33 C 0.2381(11) 0.5097(11) 0.5086(8) 0.084(5) Uani 1 1 d . U . . .
H33A H 0.177313 0.526277 0.473838 0.126 Uiso 1 1 calc GR . . . .
H33B H 0.281961 0.556286 0.522651 0.126 Uiso 1 1 calc GR . . . .
H33C H 0.222241 0.488332 0.546813 0.126 Uiso 1 1 calc GR . . . .
C34 C 0.2152(10) 0.3963(9) 0.2350(6) 0.069(3) Uani 1 1 d D U . . .
C35A C 0.2962(19) 0.384(2) 0.2029(14) 0.087(7) Uani 0.500(18) 1 d D U P B 1
H35A H 0.357204 0.366874 0.236968 0.131 Uiso 0.500(18) 1 calc GR . P B 1
H35B H 0.307805 0.435491 0.183490 0.131 Uiso 0.500(18) 1 calc GR . P B 1
H35C H 0.275068 0.343410 0.167909 0.131 Uiso 0.500(18) 1 calc GR . P B 1
C35B C 0.2470(18) 0.3120(13) 0.2300(11) 0.052(5) Uani 0.500(18) 1 d D U P B 2
H35D H 0.201420 0.286568 0.190118 0.078 Uiso 0.500(18) 1 calc GR . P B 2
H35E H 0.246937 0.281753 0.269576 0.078 Uiso 0.500(18) 1 calc GR . P B 2
H35F H 0.313549 0.312113 0.226972 0.078 Uiso 0.500(18) 1 calc GR . P B 2
C36A C 0.130(2) 0.441(2) 0.1891(14) 0.076(8) Uani 0.500(18) 1 d D U P B 1
H36A H 0.088684 0.403651 0.155885 0.114 Uiso 0.500(18) 1 calc GR . P B 1
H36B H 0.154509 0.483528 0.166491 0.114 Uiso 0.500(18) 1 calc GR . P B 1
H36C H 0.091597 0.465126 0.214525 0.114 Uiso 0.500(18) 1 calc GR . P B 1
C36B C 0.178(2) 0.4383(19) 0.1682(11) 0.067(7) Uani 0.500(18) 1 d D U P B 2
H36D H 0.232930 0.447677 0.151557 0.100 Uiso 0.500(18) 1 calc GR . P B 2
H36E H 0.148063 0.489969 0.173197 0.100 Uiso 0.500(18) 1 calc GR . P B 2
H36F H 0.128433 0.404290 0.136561 0.100 Uiso 0.500(18) 1 calc GR . P B 2
C37 C -0.0101(7) 0.2489(6) 0.3277(5) 0.032(2) Uani 1 1 d . U . . .
C38 C -0.0704(7) 0.2804(7) 0.3634(5) 0.037(2) Uani 1 1 d . U . . .
C39 C -0.1698(8) 0.2586(8) 0.3385(6) 0.048(3) Uani 1 1 d . U . . .
H39 H -0.212920 0.278323 0.360555 0.057 Uiso 1 1 calc R . . . .
C40 C -0.2066(9) 0.2123(9) 0.2862(7) 0.057(4) Uani 1 1 d . U . . .
H40 H -0.275161 0.200726 0.270654 0.069 Uiso 1 1 calc R . . . .
C41 C -0.1459(8) 0.1800(8) 0.2532(6) 0.051(3) Uani 1 1 d . U . . .
H41 H -0.173086 0.145480 0.216004 0.061 Uiso 1 1 calc R . . . .
C42 C -0.0459(7) 0.1980(7) 0.2743(5) 0.037(2) Uani 1 1 d . U . . .
C43 C -0.0304(8) 0.3349(8) 0.4220(5) 0.043(3) Uani 1 1 d . U . . .
H43 H 0.042819 0.328165 0.438367 0.051 Uiso 1 1 calc R . . . .
C44 C -0.0675(9) 0.3115(10) 0.4798(6) 0.067(4) Uani 1 1 d . U . . .
H44A H -0.137976 0.323347 0.467359 0.101 Uiso 1 1 calc GR . . . .
H44B H -0.031414 0.342431 0.519585 0.101 Uiso 1 1 calc GR . . . .
H44C H -0.056553 0.253730 0.489093 0.101 Uiso 1 1 calc GR . . . .
C45 C -0.0516(9) 0.4231(8) 0.4043(6) 0.055(3) Uani 1 1 d . U . . .
H45A H -0.023087 0.438189 0.369960 0.083 Uiso 1 1 calc GR . . . .
H45B H -0.022346 0.456237 0.444073 0.083 Uiso 1 1 calc GR . . . .
H45C H -0.122949 0.431743 0.387440 0.083 Uiso 1 1 calc GR . . . .
C46 C 0.0171(7) 0.1651(7) 0.2337(5) 0.042(3) Uani 1 1 d . U . . .
H46 H 0.087363 0.168309 0.263132 0.050 Uiso 1 1 calc R . . . .
C47 C 0.0068(9) 0.2194(10) 0.1740(6) 0.069(4) Uani 1 1 d . U . . .
H47A H 0.054188 0.202650 0.152244 0.103 Uiso 1 1 calc GR . . . .
H47B H 0.019943 0.275405 0.188979 0.103 Uiso 1 1 calc GR . . . .
H47C H -0.060176 0.215097 0.142266 0.103 Uiso 1 1 calc GR . . . .
C48 C -0.0028(10) 0.0783(9) 0.2131(7) 0.075(4) Uani 1 1 d . U . . .
H48A H 0.003025 0.045179 0.252328 0.112 Uiso 1 1 calc GR . . . .
H48B H 0.045122 0.060053 0.192337 0.112 Uiso 1 1 calc GR . . . .
H48C H -0.069508 0.073268 0.181057 0.112 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 In1 2.6933(12) . ?
In1 N1 2.194(9) . ?
In1 N3 2.249(8) . ?
In1 N4 2.195(10) . ?
In1 N6 2.201(8) . ?
N1 N2 1.331(10) . ?
N1 C1 1.413(15) . ?
N2 N3 1.263(12) . ?
N3 C13 1.430(12) . ?
N4 N5 1.274(11) . ?
N4 C25 1.414(14) . ?
N5 N6 1.281(12) . ?
N6 C37 1.449(12) . ?
C1 C2 1.421(16) . ?
C1 C6 1.427(15) . ?
C2 C3 1.374(17) . ?
C2 C7 1.543(17) . ?
C3 C4 1.384(17) . ?
C4 C5 1.366(17) . ?
C5 C6 1.360(16) . ?
C6 C10 1.559(17) . ?
C7 C8 1.534(17) . ?
C7 C9 1.526(19) . ?
C10 C11A 1.61(3) . ?
C10 C11B 1.50(3) . ?
C10 C12 1.481(17) . ?
C13 C14 1.382(15) . ?
C13 C18 1.401(16) . ?
C14 C15 1.396(16) . ?
C14 C19 1.473(18) . ?
C15 C16 1.342(19) . ?
C16 C17 1.372(18) . ?
C17 C18 1.396(15) . ?
C18 C22 1.515(17) . ?
C19 C20 1.530(16) . ?
C19 C21 1.53(2) . ?
C22 C23 1.48(2) . ?
C22 C24 1.520(19) . ?
C25 C26 1.385(15) . ?
C25 C30 1.402(16) . ?
C26 C27 1.436(18) . ?
C26 C31 1.485(17) . ?
C27 C28 1.364(18) . ?
C28 C29 1.340(18) . ?
C29 C30 1.411(18) . ?
C30 C34 1.504(19) . ?
C31 C32 1.543(16) . ?
C31 C33 1.519(18) . ?
C34 C35A 1.544(18) . ?
C34 C35B 1.486(18) . ?
C34 C36A 1.486(18) . ?
C34 C36B 1.512(17) . ?
C37 C38 1.427(15) . ?
C37 C42 1.372(15) . ?
C38 C39 1.398(14) . ?
C38 C43 1.493(15) . ?
C39 C40 1.310(16) . ?
C40 C41 1.394(16) . ?
C41 C42 1.390(14) . ?
C42 C46 1.541(15) . ?
C43 C44 1.540(16) . ?
C43 C45 1.516(17) . ?
C46 C47 1.525(16) . ?
C46 C48 1.504(17) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 In1 I1 117.8(2) . . ?
N1 In1 N3 57.0(3) . . ?
N1 In1 N4 126.4(3) . . ?
N1 In1 N6 106.6(3) . . ?
N3 In1 I1 108.0(2) . . ?
N4 In1 I1 115.8(2) . . ?
N4 In1 N3 106.3(3) . . ?
N4 In1 N6 57.1(3) . . ?
N6 In1 I1 105.6(2) . . ?
N6 In1 N3 146.5(3) . . ?
N2 N1 In1 96.9(7) . . ?
N2 N1 C1 117.9(9) . . ?
C1 N1 In1 145.2(6) . . ?
N3 N2 N1 109.7(8) . . ?
N2 N3 In1 96.4(6) . . ?
N2 N3 C13 114.2(9) . . ?
C13 N3 In1 148.4(7) . . ?
N5 N4 In1 96.0(7) . . ?
N5 N4 C25 119.5(9) . . ?
C25 N4 In1 144.0(7) . . ?
N4 N5 N6 110.7(9) . . ?
N5 N6 In1 95.5(6) . . ?
N5 N6 C37 117.4(9) . . ?
C37 N6 In1 143.7(7) . . ?
N1 C1 C2 117.2(10) . . ?
N1 C1 C6 121.9(11) . . ?
C2 C1 C6 120.9(12) . . ?
C1 C2 C7 121.2(11) . . ?
C3 C2 C1 118.5(12) . . ?
C3 C2 C7 120.3(12) . . ?
C2 C3 C4 120.0(13) . . ?
C5 C4 C3 120.8(13) . . ?
C6 C5 C4 122.8(12) . . ?
C1 C6 C10 121.4(11) . . ?
C5 C6 C1 116.7(12) . . ?
C5 C6 C10 121.6(11) . . ?
C8 C7 C2 111.7(10) . . ?
C9 C7 C2 109.2(11) . . ?
C9 C7 C8 110.8(12) . . ?
C6 C10 C11A 106.9(12) . . ?
C11B C10 C6 116.7(13) . . ?
C12 C10 C6 112.2(12) . . ?
C12 C10 C11A 94.2(16) . . ?
C12 C10 C11B 123.2(16) . . ?
C14 C13 N3 119.3(10) . . ?
C14 C13 C18 122.2(10) . . ?
C18 C13 N3 118.4(10) . . ?
C13 C14 C15 116.5(12) . . ?
C13 C14 C19 121.0(10) . . ?
C15 C14 C19 122.5(11) . . ?
C16 C15 C14 121.0(12) . . ?
C15 C16 C17 123.8(11) . . ?
C16 C17 C18 116.9(12) . . ?
C13 C18 C22 123.6(10) . . ?
C17 C18 C13 119.4(11) . . ?
C17 C18 C22 116.9(11) . . ?
C14 C19 C20 113.7(12) . . ?
C14 C19 C21 110.3(11) . . ?
C20 C19 C21 110.9(12) . . ?
C18 C22 C24 110.5(12) . . ?
C23 C22 C18 113.4(12) . . ?
C23 C22 C24 111.0(12) . . ?
C26 C25 N4 118.2(11) . . ?
C26 C25 C30 121.8(12) . . ?
C30 C25 N4 119.9(10) . . ?
C25 C26 C27 117.6(12) . . ?
C25 C26 C31 120.2(11) . . ?
C27 C26 C31 122.0(11) . . ?
C28 C27 C26 119.2(12) . . ?
C29 C28 C27 123.0(15) . . ?
C28 C29 C30 120.1(14) . . ?
C25 C30 C29 118.2(12) . . ?
C25 C30 C34 123.9(12) . . ?
C29 C30 C34 117.9(12) . . ?
C26 C31 C32 110.1(10) . . ?
C26 C31 C33 111.7(12) . . ?
C33 C31 C32 109.9(11) . . ?
C30 C34 C35A 106.8(16) . . ?
C30 C34 C36B 120.3(17) . . ?
C35B C34 C30 120.6(13) . . ?
C35B C34 C36B 112.8(18) . . ?
C36A C34 C30 109.9(17) . . ?
C36A C34 C35A 110(2) . . ?
C38 C37 N6 120.1(9) . . ?
C42 C37 N6 117.3(9) . . ?
C42 C37 C38 122.5(9) . . ?
C37 C38 C43 122.1(9) . . ?
C39 C38 C37 115.3(10) . . ?
C39 C38 C43 122.6(10) . . ?
C40 C39 C38 123.4(12) . . ?
C39 C40 C41 120.5(11) . . ?
C42 C41 C40 120.5(11) . . ?
C37 C42 C41 117.8(10) . . ?
C37 C42 C46 123.4(9) . . ?
C41 C42 C46 118.6(10) . . ?
C38 C43 C44 111.9(10) . . ?
C38 C43 C45 112.7(9) . . ?
C45 C43 C44 110.3(11) . . ?
C47 C46 C42 110.1(9) . . ?
C48 C46 C42 114.3(10) . . ?
C48 C46 C47 111.4(11) . . ?

_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_PLAT973_10                  
;
PROBLEM: Check Calcd Positive Resid. Density on       In1       2.26 eA-3  
RESPONSE: Several peaks of electron density are located proximate to In. It is
suspect that this is the result of a fourier truncation.
;
_vrf_PLAT910_10                  
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         11 Note  
RESPONSE: A reflection was found to be an outlier and was thus omitted from 
the final refinement.
;
# end Validation Reply Form
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_22
_database_code_depnum_ccdc_archive 'CCDC 1972013'
loop_
_audit_author_name
_audit_author_address
'Alasdair McKay'
;Monash University
Australia
;
_audit_update_record             
;
2019-12-14 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_audit_creation_date             2019-12-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
''
alasdair.mckay@monash.edu
_chemical_name_common            ?
_chemical_name_systematic        '[SnCl(N3Dipp2).W(CO)5]'
_chemical_formula_moiety         'C29 H34 Cl N3 O5 Sn W'
_chemical_formula_sum            'C29 H34 Cl N3 O5 Sn W'
_chemical_formula_weight         842.58
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.6676(7)
_cell_length_b                   11.0404(7)
_cell_length_c                   15.4465(11)
_cell_angle_alpha                73.901(3)
_cell_angle_beta                 71.850(3)
_cell_angle_gamma                72.069(3)
_cell_volume                     1611.28(19)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9221
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.960
_cell_measurement_theta_min      2.191
_shelx_estimated_absorpt_T_max   0.717
_shelx_estimated_absorpt_T_min   0.554
_exptl_absorpt_coefficient_mu    4.464
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5674
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0824 before and 0.0406 after correction. The Ratio of minimum to maximum transmission is 0.7611. The λ/2 correction factor is 0.00150.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24732
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.972
_diffrn_reflns_theta_min         1.979
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6607
_reflns_number_total             6965
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         6965
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0169
_refine_ls_R_factor_gt           0.0153
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0083P)²+0.8371P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0345
_refine_ls_wR_factor_ref         0.0352
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C22(H22), C10(H10), C19(H19)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C15(H15), C17(H17), C16(H16), C4(H4)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C23(H23A,H23B,H23C), C12(H12A,H12B,H12C), C11(H11A,H11B,
 H11C), C24(H24A,H24B,H24C), C9(H9A,H9B,H9C), C21(H21A,H21B,H21C), C20(H20A,
 H20B,H20C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.79210(2) 0.84135(2) 0.51851(2) 0.01873(3) Uani 1 1 d . . . . .
Sn1 Sn 0.95004(2) 0.73129(2) 0.64011(2) 0.01730(4) Uani 1 1 d . . . . .
O5 O 0.61985(17) 0.96746(17) 0.37048(12) 0.0409(4) Uani 1 1 d . . . . .
Cl1 Cl 1.18465(5) 0.71539(6) 0.60011(4) 0.03330(13) Uani 1 1 d . . . . .
O4 O 0.89948(16) 0.57710(15) 0.44336(10) 0.0326(4) Uani 1 1 d . . . . .
N3 N 0.95686(15) 0.55139(15) 0.74688(11) 0.0155(3) Uani 1 1 d . . . . .
N2 N 0.92977(15) 0.60398(15) 0.81822(11) 0.0155(3) Uani 1 1 d . . . . .
N1 N 0.91606(15) 0.72886(15) 0.78894(11) 0.0164(3) Uani 1 1 d . . . . .
O2 O 0.66855(18) 1.10239(16) 0.59817(12) 0.0409(4) Uani 1 1 d . . . . .
O1 O 1.02806(16) 0.96860(16) 0.37730(11) 0.0352(4) Uani 1 1 d . . . . .
C13 C 0.98258(19) 0.41244(18) 0.76297(13) 0.0170(4) Uani 1 1 d . . . . .
C26 C 0.9458(2) 0.9194(2) 0.42838(14) 0.0241(4) Uani 1 1 d . . . . .
C28 C 0.8634(2) 0.6726(2) 0.46911(14) 0.0231(4) Uani 1 1 d . . . . .
C6 C 0.7511(2) 0.89016(19) 0.87293(13) 0.0205(4) Uani 1 1 d . . . . .
C1 C 0.88193(19) 0.80677(18) 0.85696(13) 0.0171(4) Uani 1 1 d . . . . .
C25 C 0.7141(2) 1.0087(2) 0.57030(15) 0.0264(5) Uani 1 1 d . . . . .
C5 C 0.7199(2) 0.9720(2) 0.93443(14) 0.0259(5) Uani 1 1 d . . . . .
H5 H 0.633269 1.031407 0.944785 0.031 Uiso 1 1 calc R . . . .
C18 C 0.8813(2) 0.3583(2) 0.75996(14) 0.0214(4) Uani 1 1 d . . . . .
C2 C 0.97838(19) 0.80204(19) 0.90279(13) 0.0192(4) Uani 1 1 d . . . . .
C14 C 1.1099(2) 0.33617(19) 0.77542(14) 0.0207(4) Uani 1 1 d . . . . .
C3 C 0.9399(2) 0.8831(2) 0.96603(15) 0.0260(5) Uani 1 1 d . . . . .
H3 H 1.002075 0.879823 0.999766 0.031 Uiso 1 1 calc R . . . .
C7 C 1.1215(2) 0.7132(2) 0.88477(14) 0.0222(4) Uani 1 1 d . . . . .
H7 H 1.119998 0.643312 0.855744 0.027 Uiso 1 1 calc R . . . .
C15 C 1.1325(2) 0.2020(2) 0.78746(15) 0.0266(5) Uani 1 1 d . . . . .
H15 H 1.217673 0.147700 0.796493 0.032 Uiso 1 1 calc R . . . .
C29 C 0.6823(2) 0.9210(2) 0.42408(15) 0.0265(5) Uani 1 1 d . . . . .
C17 C 0.9093(2) 0.2243(2) 0.77297(15) 0.0281(5) Uani 1 1 d . . . . .
H17 H 0.841864 0.184977 0.772587 0.034 Uiso 1 1 calc R . . . .
C16 C 1.0337(2) 0.1467(2) 0.78651(15) 0.0297(5) Uani 1 1 d . . . . .
H16 H 1.051044 0.054998 0.795176 0.036 Uiso 1 1 calc R . . . .
C22 C 0.7456(2) 0.4411(2) 0.74243(16) 0.0297(5) Uani 1 1 d . . . . .
H22 H 0.750573 0.534069 0.725569 0.036 Uiso 1 1 calc R . . . .
C10 C 0.6443(2) 0.8820(2) 0.83003(16) 0.0318(5) Uani 1 1 d . . . . .
H10 H 0.691864 0.862578 0.766717 0.038 Uiso 1 1 calc R . . . .
C4 C 0.8133(2) 0.9684(2) 0.98085(15) 0.0286(5) Uani 1 1 d . . . . .
H4 H 0.790255 1.024683 1.023051 0.034 Uiso 1 1 calc R . . . .
C8 C 1.2219(2) 0.7887(3) 0.81638(19) 0.0413(6) Uani 1 1 d . . . . .
H8A H 1.191634 0.828632 0.758924 0.062 Uiso 1 1 calc GR . . . .
H8B H 1.312015 0.729425 0.802319 0.062 Uiso 1 1 calc GR . . . .
H8C H 1.226837 0.856660 0.843848 0.062 Uiso 1 1 calc GR . . . .
C23 C 0.7168(3) 0.4108(3) 0.66048(19) 0.0437(6) Uani 1 1 d . . . . .
H23A H 0.793519 0.418446 0.605932 0.066 Uiso 1 1 calc GR . . . .
H23B H 0.633942 0.472371 0.646230 0.066 Uiso 1 1 calc GR . . . .
H23C H 0.704533 0.322102 0.676909 0.066 Uiso 1 1 calc GR . . . .
C12 C 0.5814(2) 0.7693(3) 0.8872(2) 0.0473(7) Uani 1 1 d . . . . .
H12A H 0.653029 0.688694 0.890974 0.071 Uiso 1 1 calc GR . . . .
H12B H 0.516214 0.761387 0.857468 0.071 Uiso 1 1 calc GR . . . .
H12C H 0.534305 0.785356 0.949956 0.071 Uiso 1 1 calc GR . . . .
C11 C 0.5338(2) 1.0079(3) 0.81836(17) 0.0461(7) Uani 1 1 d . . . . .
H11A H 0.477192 1.023246 0.879686 0.069 Uiso 1 1 calc GR . . . .
H11B H 0.477023 1.000317 0.781869 0.069 Uiso 1 1 calc GR . . . .
H11C H 0.576187 1.080630 0.786038 0.069 Uiso 1 1 calc GR . . . .
C24 C 0.6304(2) 0.4258(3) 0.8300(2) 0.0492(7) Uani 1 1 d . . . . .
H24A H 0.622056 0.335664 0.847581 0.074 Uiso 1 1 calc GR . . . .
H24B H 0.544840 0.484030 0.817742 0.074 Uiso 1 1 calc GR . . . .
H24C H 0.650232 0.447728 0.880785 0.074 Uiso 1 1 calc GR . . . .
C9 C 1.1687(3) 0.6481(3) 0.97371(18) 0.0507(7) Uani 1 1 d . . . . .
H9A H 1.175874 0.714409 1.001759 0.076 Uiso 1 1 calc GR . . . .
H9B H 1.257824 0.587469 0.959115 0.076 Uiso 1 1 calc GR . . . .
H9C H 1.102939 0.600503 1.017490 0.076 Uiso 1 1 calc GR . . . .
C27 C 0.6317(2) 0.7730(2) 0.60909(16) 0.0289(5) Uani 1 1 d . . . . .
O3 O 0.54029(17) 0.73685(18) 0.65834(14) 0.0482(5) Uani 1 1 d . . . . .
C19 C 1.2231(2) 0.3945(2) 0.77337(15) 0.0262(5) Uani 1 1 d . . . . .
H19 H 1.188862 0.491158 0.761176 0.031 Uiso 1 1 calc R . . . .
C21 C 1.2599(3) 0.3522(2) 0.86707(18) 0.0403(6) Uani 1 1 d . . . . .
H21A H 1.178241 0.375708 0.916227 0.060 Uiso 1 1 calc GR . . . .
H21B H 1.328056 0.395937 0.865423 0.060 Uiso 1 1 calc GR . . . .
H21C H 1.296922 0.257906 0.879683 0.060 Uiso 1 1 calc GR . . . .
C20 C 1.3480(2) 0.3594(3) 0.69428(19) 0.0430(6) Uani 1 1 d . . . . .
H20A H 1.382106 0.264780 0.703617 0.065 Uiso 1 1 calc GR . . . .
H20B H 1.419104 0.398624 0.693900 0.065 Uiso 1 1 calc GR . . . .
H20C H 1.322662 0.392529 0.634725 0.065 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 Sn1 2.6998(2) . ?
W1 C26 2.037(2) . ?
W1 C28 2.046(2) . ?
W1 C25 2.051(2) . ?
W1 C29 1.998(2) . ?
W1 C27 2.042(2) . ?
Sn1 Cl1 2.3458(5) . ?
Sn1 N3 2.1998(15) . ?
Sn1 N1 2.2067(15) . ?
O5 C29 1.136(3) . ?
O4 C28 1.142(2) . ?
N3 N2 1.299(2) . ?
N3 C13 1.436(2) . ?
N2 N1 1.303(2) . ?
N1 C1 1.431(2) . ?
O2 C25 1.139(3) . ?
O1 C26 1.146(3) . ?
C13 C18 1.404(3) . ?
C13 C14 1.399(3) . ?
C6 C1 1.406(3) . ?
C6 C5 1.387(3) . ?
C6 C10 1.520(3) . ?
C1 C2 1.401(3) . ?
C5 C4 1.383(3) . ?
C18 C17 1.386(3) . ?
C18 C22 1.515(3) . ?
C2 C3 1.390(3) . ?
C2 C7 1.528(3) . ?
C14 C15 1.393(3) . ?
C14 C19 1.523(3) . ?
C3 C4 1.381(3) . ?
C7 C8 1.522(3) . ?
C7 C9 1.523(3) . ?
C15 C16 1.376(3) . ?
C17 C16 1.383(3) . ?
C22 C23 1.533(3) . ?
C22 C24 1.528(3) . ?
C10 C12 1.521(4) . ?
C10 C11 1.529(3) . ?
C27 O3 1.140(3) . ?
C19 C21 1.527(3) . ?
C19 C20 1.532(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C26 W1 Sn1 89.16(6) . . ?
C26 W1 C28 93.01(8) . . ?
C26 W1 C25 88.99(8) . . ?
C26 W1 C27 176.92(8) . . ?
C28 W1 Sn1 88.01(5) . . ?
C28 W1 C25 177.92(8) . . ?
C25 W1 Sn1 92.58(6) . . ?
C29 W1 Sn1 177.54(6) . . ?
C29 W1 C26 88.92(8) . . ?
C29 W1 C28 90.54(8) . . ?
C29 W1 C25 88.93(8) . . ?
C29 W1 C27 89.70(9) . . ?
C27 W1 Sn1 92.28(6) . . ?
C27 W1 C28 89.76(8) . . ?
C27 W1 C25 88.23(8) . . ?
Cl1 Sn1 W1 123.537(16) . . ?
N3 Sn1 W1 130.97(4) . . ?
N3 Sn1 Cl1 95.46(4) . . ?
N3 Sn1 N1 57.24(6) . . ?
N1 Sn1 W1 133.06(4) . . ?
N1 Sn1 Cl1 96.32(4) . . ?
N2 N3 Sn1 97.39(11) . . ?
N2 N3 C13 117.71(15) . . ?
C13 N3 Sn1 144.84(12) . . ?
N3 N2 N1 108.41(15) . . ?
N2 N1 Sn1 96.95(11) . . ?
N2 N1 C1 117.75(15) . . ?
C1 N1 Sn1 145.21(12) . . ?
C18 C13 N3 118.41(17) . . ?
C14 C13 N3 119.23(16) . . ?
C14 C13 C18 122.24(18) . . ?
O1 C26 W1 176.93(19) . . ?
O4 C28 W1 177.80(19) . . ?
C1 C6 C10 120.49(18) . . ?
C5 C6 C1 117.94(18) . . ?
C5 C6 C10 121.37(18) . . ?
C6 C1 N1 117.50(16) . . ?
C2 C1 N1 120.35(17) . . ?
C2 C1 C6 122.11(18) . . ?
O2 C25 W1 178.56(19) . . ?
C4 C5 C6 120.87(19) . . ?
C13 C18 C22 122.34(18) . . ?
C17 C18 C13 117.66(19) . . ?
C17 C18 C22 120.00(18) . . ?
C1 C2 C7 122.45(17) . . ?
C3 C2 C1 117.42(18) . . ?
C3 C2 C7 120.13(17) . . ?
C13 C14 C19 122.63(18) . . ?
C15 C14 C13 117.46(18) . . ?
C15 C14 C19 119.88(18) . . ?
C4 C3 C2 121.42(19) . . ?
C8 C7 C2 110.33(17) . . ?
C8 C7 C9 110.1(2) . . ?
C9 C7 C2 112.58(18) . . ?
C16 C15 C14 121.27(19) . . ?
O5 C29 W1 179.36(19) . . ?
C16 C17 C18 121.16(19) . . ?
C15 C16 C17 120.2(2) . . ?
C18 C22 C23 111.34(19) . . ?
C18 C22 C24 111.21(19) . . ?
C24 C22 C23 111.14(19) . . ?
C6 C10 C12 109.68(19) . . ?
C6 C10 C11 113.9(2) . . ?
C12 C10 C11 110.5(2) . . ?
C3 C4 C5 120.18(19) . . ?
O3 C27 W1 178.4(2) . . ?
C14 C19 C21 111.05(18) . . ?
C14 C19 C20 110.90(18) . . ?
C21 C19 C20 111.28(19) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_GisoRh(CO)2
_database_code_depnum_ccdc_archive 'CCDC 1976266'
loop_
_audit_author_name
_audit_author_address
'Alasdair McKay'
;Monash University
Australia
;
_audit_update_record             
;
2020-01-08 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_audit_creation_date             2020-01-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
''
alasdair.mckay@monash.edu
_chemical_name_common            ?
_chemical_name_systematic        '[(Giso)Rh(CO2)]'
_chemical_formula_moiety         'C39 H56 N3 O2 Rh'
_chemical_formula_sum            'C39 H56 N3 O2 Rh'
_chemical_formula_weight         701.77
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.4904(4)
_cell_length_b                   18.2900(8)
_cell_length_c                   20.8209(7)
_cell_angle_alpha                90
_cell_angle_beta                 99.416(2)
_cell_angle_gamma                90
_cell_volume                     3565.4(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9883
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.09
_cell_measurement_theta_min      2.23
_shelx_estimated_absorpt_T_max   0.980
_shelx_estimated_absorpt_T_min   0.917
_exptl_absorpt_coefficient_mu    0.516
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6580
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.0694 before and 0.0536 after correction. The Ratio of minimum to maximum transmission is 0.8826. The λ/2 correction factor is 0.00150.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27965
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.132
_diffrn_reflns_theta_min         1.491
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6659
_reflns_number_total             7766
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         7766
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0280
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0217P)²+2.0990P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0689
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C22(H22), C16(H16), C12(H12), C34(H34), C9(H9), C37(H37)
2.b Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C17(H17A,H17B), C27(H27A,H27B), C25(H25A,H25B), C19(H19A,
 H19B), C18(H18A,H18B), C26(H26A,H26B), C24(H24A,H24B), C20(H20A,H20B),
 C21(H21A,H21B)
2.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C30(H30), C5(H5), C31(H31), C32(H32), C6(H6)
2.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C10(H10A,H10B,H10C), C38(H38A,H38B,
 H38C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C11(H11A,H11B,H11C), C39(H39A,
 H39B,H39C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.72021(2) 0.20222(2) 0.76393(2) 0.01391(5) Uani 1 1 d . . . . .
N1 N 0.55141(16) 0.16679(8) 0.69601(6) 0.0127(3) Uani 1 1 d . . . . .
C1 C 0.8506(2) 0.21873(12) 0.83859(10) 0.0250(5) Uani 1 1 d . . . . .
N2 N 0.34868(16) 0.10526(8) 0.72899(6) 0.0134(3) Uani 1 1 d . . . . .
N3 N 0.56079(16) 0.14912(8) 0.80008(6) 0.0137(3) Uani 1 1 d . . . . .
O2 O 0.90305(17) 0.29262(8) 0.69026(7) 0.0333(4) Uani 1 1 d . . . . .
C28 C 0.52726(19) 0.15394(10) 0.86437(8) 0.0140(4) Uani 1 1 d . . . . .
C7 C 0.6335(2) 0.04062(11) 0.56625(9) 0.0197(4) Uani 1 1 d . . . . .
H7 H 0.661588 -0.008541 0.560761 0.024 Uiso 1 1 calc R . . . .
C33 C 0.4427(2) 0.21102(10) 0.88241(9) 0.0172(4) Uani 1 1 d . . . . .
O1 O 0.93039(18) 0.22568(11) 0.88538(7) 0.0475(5) Uani 1 1 d . . . . .
C3 C 0.56723(18) 0.13670(9) 0.63425(8) 0.0122(3) Uani 1 1 d . . . . .
C22 C 0.3000(2) 0.06216(10) 0.78165(8) 0.0157(4) Uani 1 1 d . . . . .
H22 H 0.386037 0.056780 0.816106 0.019 Uiso 1 1 calc R . . . .
C23 C 0.1867(2) 0.09812(11) 0.81546(8) 0.0201(4) Uani 1 1 d . . . . .
H23A H 0.093784 0.098647 0.785849 0.024 Uiso 1 1 calc R . . . .
H23B H 0.214263 0.149285 0.826870 0.024 Uiso 1 1 calc R . . . .
C15 C 0.47975(19) 0.13811(9) 0.74163(8) 0.0125(3) Uani 1 1 d . . . . .
C8 C 0.61158(19) 0.06402(10) 0.62745(8) 0.0149(4) Uani 1 1 d . . . . .
C16 C 0.26002(19) 0.11549(10) 0.66357(8) 0.0156(4) Uani 1 1 d . . . . .
H16 H 0.307228 0.155243 0.641852 0.019 Uiso 1 1 calc R . . . .
C30 C 0.5642(2) 0.10776(11) 0.97402(8) 0.0215(4) Uani 1 1 d . . . . .
H30 H 0.605675 0.073271 1.005670 0.026 Uiso 1 1 calc R . . . .
C2 C 0.8348(2) 0.25590(11) 0.71686(9) 0.0202(4) Uani 1 1 d . . . . .
C29 C 0.5949(2) 0.10381(10) 0.91058(8) 0.0161(4) Uani 1 1 d . . . . .
C5 C 0.5754(2) 0.15853(11) 0.52074(8) 0.0208(4) Uani 1 1 d . . . . .
H5 H 0.563749 0.190378 0.484207 0.025 Uiso 1 1 calc R . . . .
C4 C 0.5516(2) 0.18512(10) 0.58086(8) 0.0153(4) Uani 1 1 d . . . . .
C31 C 0.4742(2) 0.16113(11) 0.99120(9) 0.0242(4) Uani 1 1 d . . . . .
H31 H 0.451848 0.162071 1.034032 0.029 Uiso 1 1 calc R . . . .
C32 C 0.4169(2) 0.21291(11) 0.94653(9) 0.0229(4) Uani 1 1 d . . . . .
H32 H 0.358679 0.250617 0.959522 0.028 Uiso 1 1 calc R . . . .
C17 C 0.1098(2) 0.14279(11) 0.66728(9) 0.0215(4) Uani 1 1 d . . . . .
H17A H 0.115980 0.186843 0.695233 0.026 Uiso 1 1 calc R . . . .
H17B H 0.057385 0.104678 0.687558 0.026 Uiso 1 1 calc R . . . .
C12 C 0.6444(2) 0.01185(10) 0.68501(9) 0.0174(4) Uani 1 1 d . . . . .
H12 H 0.590361 0.029149 0.719515 0.021 Uiso 1 1 calc R . . . .
C6 C 0.6154(2) 0.08716(11) 0.51329(9) 0.0228(4) Uani 1 1 d . . . . .
H6 H 0.630499 0.069952 0.471903 0.027 Uiso 1 1 calc R . . . .
C27 C 0.2541(2) -0.01591(11) 0.76167(9) 0.0236(4) Uani 1 1 d . . . . .
H27A H 0.327885 -0.039377 0.740050 0.028 Uiso 1 1 calc R . . . .
H27B H 0.163541 -0.014807 0.730400 0.028 Uiso 1 1 calc R . . . .
C34 C 0.7024(2) 0.04858(10) 0.89350(8) 0.0190(4) Uani 1 1 d . . . . .
H34 H 0.745025 0.069848 0.856806 0.023 Uiso 1 1 calc R . . . .
C25 C 0.1297(2) -0.02320(12) 0.86013(10) 0.0306(5) Uani 1 1 d . . . . .
H25A H 0.032858 -0.023703 0.833796 0.037 Uiso 1 1 calc R . . . .
H25B H 0.125984 -0.050882 0.900681 0.037 Uiso 1 1 calc R . . . .
C19 C 0.0251(2) 0.09735(13) 0.55289(9) 0.0272(5) Uani 1 1 d . . . . .
H19A H -0.032196 0.057041 0.567120 0.033 Uiso 1 1 calc R . . . .
H19B H -0.020692 0.112667 0.508786 0.033 Uiso 1 1 calc R . . . .
C18 C 0.0268(2) 0.16151(12) 0.59960(9) 0.0278(5) Uani 1 1 d . . . . .
H18A H -0.072595 0.174788 0.603522 0.033 Uiso 1 1 calc R . . . .
H18B H 0.071469 0.204305 0.581875 0.033 Uiso 1 1 calc R . . . .
C26 C 0.2337(3) -0.06029(12) 0.82224(10) 0.0301(5) Uani 1 1 d . . . . .
H26A H 0.197383 -0.109586 0.808613 0.036 Uiso 1 1 calc R . . . .
H26B H 0.327107 -0.066210 0.850849 0.036 Uiso 1 1 calc R . . . .
C14 C 0.6006(2) -0.06739(11) 0.66892(10) 0.0294(5) Uani 1 1 d . . . . .
H14A H 0.499671 -0.069005 0.648960 0.044 Uiso 1 1 calc GR . . . .
H14B H 0.614762 -0.096475 0.708992 0.044 Uiso 1 1 calc GR . . . .
H14C H 0.659200 -0.087449 0.638512 0.044 Uiso 1 1 calc GR . . . .
C13 C 0.8030(2) 0.01520(12) 0.71294(10) 0.0277(5) Uani 1 1 d . . . . .
H13A H 0.858810 -0.000911 0.679868 0.042 Uiso 1 1 calc GR . . . .
H13B H 0.823032 -0.016890 0.751037 0.042 Uiso 1 1 calc GR . . . .
H13C H 0.829259 0.065539 0.725871 0.042 Uiso 1 1 calc GR . . . .
C24 C 0.1733(2) 0.05515(12) 0.87710(9) 0.0270(5) Uani 1 1 d . . . . .
H24A H 0.265855 0.055653 0.906966 0.032 Uiso 1 1 calc R . . . .
H24B H 0.100955 0.078569 0.899641 0.032 Uiso 1 1 calc R . . . .
C9 C 0.5103(2) 0.26485(10) 0.58692(9) 0.0218(4) Uani 1 1 d . . . . .
H9 H 0.518020 0.276483 0.634291 0.026 Uiso 1 1 calc R . . . .
C10 C 0.3567(2) 0.27890(12) 0.55475(12) 0.0370(6) Uani 1 1 d . . . . .
H10A H 0.345937 0.266914 0.508330 0.055 Uiso 1 1 calc GR . . . .
H10B H 0.333181 0.330531 0.559836 0.055 Uiso 1 1 calc GR . . . .
H10C H 0.292063 0.248293 0.575399 0.055 Uiso 1 1 calc GR . . . .
C38 C 0.2476(3) 0.30588(13) 0.84598(13) 0.0386(6) Uani 1 1 d . . . . .
H38A H 0.177330 0.266833 0.847171 0.058 Uiso 1 1 calc GR . . . .
H38B H 0.213084 0.339583 0.810275 0.058 Uiso 1 1 calc GR . . . .
H38C H 0.261235 0.332555 0.887356 0.058 Uiso 1 1 calc GR . . . .
C20 C 0.1750(2) 0.07018(12) 0.55025(9) 0.0257(5) Uani 1 1 d . . . . .
H20A H 0.229629 0.108912 0.531973 0.031 Uiso 1 1 calc R . . . .
H20B H 0.170119 0.027095 0.521186 0.031 Uiso 1 1 calc R . . . .
C37 C 0.3896(2) 0.27260(11) 0.83530(9) 0.0227(4) Uani 1 1 d . . . . .
H37 H 0.376439 0.252264 0.790134 0.027 Uiso 1 1 calc R . . . .
C35 C 0.6357(2) -0.02417(12) 0.86981(11) 0.0309(5) Uani 1 1 d . . . . .
H35A H 0.587608 -0.045486 0.903584 0.046 Uiso 1 1 calc GR . . . .
H35B H 0.710546 -0.057540 0.860410 0.046 Uiso 1 1 calc GR . . . .
H35C H 0.566093 -0.016359 0.830150 0.046 Uiso 1 1 calc GR . . . .
C36 C 0.8251(2) 0.03499(13) 0.94930(10) 0.0298(5) Uani 1 1 d . . . . .
H36A H 0.865410 0.081897 0.966057 0.045 Uiso 1 1 calc GR . . . .
H36B H 0.899291 0.006010 0.933487 0.045 Uiso 1 1 calc GR . . . .
H36C H 0.789572 0.008315 0.984208 0.045 Uiso 1 1 calc GR . . . .
C21 C 0.2521(2) 0.04923(11) 0.61817(8) 0.0196(4) Uani 1 1 d . . . . .
H21A H 0.349743 0.031927 0.615405 0.024 Uiso 1 1 calc R . . . .
H21B H 0.200068 0.008971 0.635804 0.024 Uiso 1 1 calc R . . . .
C11 C 0.6107(2) 0.31601(12) 0.55810(11) 0.0311(5) Uani 1 1 d . . . . .
H11A H 0.709762 0.305021 0.577229 0.047 Uiso 1 1 calc GR . . . .
H11B H 0.588725 0.366801 0.567727 0.047 Uiso 1 1 calc GR . . . .
H11C H 0.598048 0.309051 0.510832 0.047 Uiso 1 1 calc GR . . . .
C39 C 0.5027(2) 0.33278(12) 0.84013(12) 0.0338(5) Uani 1 1 d . . . . .
H39A H 0.516199 0.354280 0.883819 0.051 Uiso 1 1 calc GR . . . .
H39B H 0.471273 0.370751 0.807734 0.051 Uiso 1 1 calc GR . . . .
H39C H 0.593184 0.311878 0.831923 0.051 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 N1 2.0604(14) . ?
Rh1 C1 1.847(2) . ?
Rh1 N3 2.0423(14) . ?
Rh1 C2 1.859(2) . ?
N1 C3 1.429(2) . ?
N1 C15 1.361(2) . ?
C1 O1 1.139(2) . ?
N2 C22 1.484(2) . ?
N2 C15 1.368(2) . ?
N2 C16 1.491(2) . ?
N3 C28 1.428(2) . ?
N3 C15 1.344(2) . ?
O2 C2 1.138(2) . ?
C28 C33 1.405(3) . ?
C28 C29 1.406(2) . ?
C7 C8 1.392(2) . ?
C7 C6 1.381(3) . ?
C33 C32 1.397(3) . ?
C33 C37 1.524(3) . ?
C3 C8 1.409(2) . ?
C3 C4 1.410(2) . ?
C22 C23 1.527(3) . ?
C22 C27 1.530(3) . ?
C23 C24 1.528(2) . ?
C8 C12 1.524(2) . ?
C16 C17 1.525(3) . ?
C16 C21 1.531(2) . ?
C30 C29 1.401(2) . ?
C30 C31 1.382(3) . ?
C29 C34 1.518(3) . ?
C5 C4 1.395(2) . ?
C5 C6 1.375(3) . ?
C4 C9 1.520(3) . ?
C31 C32 1.376(3) . ?
C17 C18 1.536(3) . ?
C12 C14 1.530(3) . ?
C12 C13 1.524(3) . ?
C27 C26 1.539(3) . ?
C34 C35 1.520(3) . ?
C34 C36 1.525(3) . ?
C25 C26 1.520(3) . ?
C25 C24 1.517(3) . ?
C19 C18 1.523(3) . ?
C19 C20 1.516(3) . ?
C9 C10 1.524(3) . ?
C9 C11 1.526(3) . ?
C38 C37 1.528(3) . ?
C20 C21 1.531(3) . ?
C37 C39 1.529(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Rh1 N1 165.48(7) . . ?
C1 Rh1 N3 101.68(7) . . ?
C1 Rh1 C2 89.31(8) . . ?
N3 Rh1 N1 64.13(5) . . ?
C2 Rh1 N1 105.10(7) . . ?
C2 Rh1 N3 167.95(7) . . ?
C3 N1 Rh1 123.67(11) . . ?
C15 N1 Rh1 93.63(10) . . ?
C15 N1 C3 128.16(15) . . ?
O1 C1 Rh1 176.9(2) . . ?
C22 N2 C16 122.96(14) . . ?
C15 N2 C22 118.33(14) . . ?
C15 N2 C16 118.70(14) . . ?
C28 N3 Rh1 127.45(11) . . ?
C15 N3 Rh1 94.95(10) . . ?
C15 N3 C28 132.49(15) . . ?
C33 C28 N3 121.40(16) . . ?
C33 C28 C29 121.24(15) . . ?
C29 C28 N3 117.02(16) . . ?
C6 C7 C8 121.58(18) . . ?
C28 C33 C37 121.36(15) . . ?
C32 C33 C28 118.12(17) . . ?
C32 C33 C37 120.36(17) . . ?
C8 C3 N1 122.07(15) . . ?
C8 C3 C4 120.54(15) . . ?
C4 C3 N1 117.04(15) . . ?
N2 C22 C23 116.09(15) . . ?
N2 C22 C27 113.81(14) . . ?
C23 C22 C27 109.69(15) . . ?
C22 C23 C24 109.12(16) . . ?
N1 C15 N2 125.29(15) . . ?
N3 C15 N1 107.27(15) . . ?
N3 C15 N2 127.43(15) . . ?
C7 C8 C3 118.30(16) . . ?
C7 C8 C12 119.05(16) . . ?
C3 C8 C12 122.55(15) . . ?
N2 C16 C17 112.80(14) . . ?
N2 C16 C21 115.34(15) . . ?
C17 C16 C21 109.78(15) . . ?
C31 C30 C29 120.90(18) . . ?
O2 C2 Rh1 175.57(17) . . ?
C28 C29 C34 121.52(15) . . ?
C30 C29 C28 117.99(17) . . ?
C30 C29 C34 120.45(16) . . ?
C6 C5 C4 121.35(17) . . ?
C3 C4 C9 122.15(15) . . ?
C5 C4 C3 118.48(17) . . ?
C5 C4 C9 119.37(16) . . ?
C32 C31 C30 120.27(17) . . ?
C31 C32 C33 121.15(18) . . ?
C16 C17 C18 111.71(15) . . ?
C8 C12 C14 114.07(16) . . ?
C13 C12 C8 109.70(16) . . ?
C13 C12 C14 109.75(16) . . ?
C5 C6 C7 119.70(16) . . ?
C22 C27 C26 109.75(16) . . ?
C29 C34 C35 113.49(17) . . ?
C29 C34 C36 112.87(15) . . ?
C35 C34 C36 109.26(17) . . ?
C24 C25 C26 111.52(17) . . ?
C20 C19 C18 111.36(17) . . ?
C19 C18 C17 111.36(17) . . ?
C25 C26 C27 111.69(18) . . ?
C25 C24 C23 110.32(16) . . ?
C4 C9 C10 111.49(17) . . ?
C4 C9 C11 111.68(17) . . ?
C10 C9 C11 109.74(17) . . ?
C19 C20 C21 110.98(15) . . ?
C33 C37 C38 114.05(17) . . ?
C33 C37 C39 109.56(17) . . ?
C38 C37 C39 109.28(18) . . ?
C20 C21 C16 109.88(16) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Hexane'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_PisoRh(CO)2
_database_code_depnum_ccdc_archive 'CCDC 1976265'
loop_
_audit_author_name
_audit_author_address
'Alasdair McKay'
;Monash University
Australia
;
_audit_update_record             
;
2020-01-08 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_audit_creation_date             2020-01-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
''
alasdair.mckay@monash.edu
_chemical_name_common            ?
_chemical_name_systematic        '[(Piso)Rh(CO)2]'
_chemical_formula_moiety         'C31 H43 N2 O2 Rh'
_chemical_formula_sum            'C31 H43 N2 O2 Rh'
_chemical_formula_weight         578.58
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.2807(4)
_cell_length_b                   10.9865(4)
_cell_length_c                   14.6713(5)
_cell_angle_alpha                70.8800(11)
_cell_angle_beta                 79.7465(13)
_cell_angle_gamma                74.6877(15)
_cell_volume                     1502.48(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.102
_cell_measurement_theta_min      2.506
_shelx_estimated_absorpt_T_max   0.943
_shelx_estimated_absorpt_T_min   0.885
_exptl_absorpt_coefficient_mu    0.596
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.1383 before and 0.0525 after correction. The Ratio of minimum to maximum transmission is 0.8884. The λ/2 correction factor is 0.00150.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21909
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         3.043
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5501
_reflns_number_total             5884
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         5884
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0242
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0222P)²+0.6833P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0625
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C26(H26), C29(H29), C12(H12), C9(H9)
2.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C22(H22), C5(H5), C23(H23), C7(H7), C6(H6)
2.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C28(H28A,H28B,H28C), C10(H10A,H10B,
 H10C), C13(H13A,H13B,H13C), C27(H27A,H27B,H27C), C14(H14A,H14B,H14C), C19(H19A,
 H19B,H19C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C11(H11A,H11B,H11C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.21091(2) 0.63894(2) 0.37720(2) 0.02068(6) Uani 1 1 d . . . . .
C20 C 0.25042(18) 0.55314(17) 0.18412(12) 0.0198(4) Uani 1 1 d . . . . .
C15 C 0.26169(16) 0.77071(17) 0.20252(12) 0.0189(3) Uani 1 1 d . . . . .
C24 C 0.1406(2) 0.43743(19) 0.11824(14) 0.0288(4) Uani 1 1 d . . . . .
H24 H 0.061480 0.427565 0.098863 0.035 Uiso 1 1 calc R . . . .
C3 C 0.25552(18) 0.92956(17) 0.29688(12) 0.0213(4) Uani 1 1 d . . . . .
C16 C 0.29012(18) 0.85081(17) 0.09657(13) 0.0234(4) Uani 1 1 d . . . . .
C21 C 0.37447(18) 0.46389(18) 0.17458(13) 0.0230(4) Uani 1 1 d . . . . .
C25 C 0.13162(18) 0.53916(18) 0.15747(13) 0.0231(4) Uani 1 1 d . . . . .
C22 C 0.3773(2) 0.36341(19) 0.13567(14) 0.0292(4) Uani 1 1 d . . . . .
H22 H 0.460408 0.302205 0.128706 0.035 Uiso 1 1 calc R . . . .
C8 C 0.13428(19) 1.02126(18) 0.30689(13) 0.0256(4) Uani 1 1 d . . . . .
C30 C -0.0905(2) 0.6766(2) 0.09041(16) 0.0399(5) Uani 1 1 d . . . . .
H30A H -0.038947 0.723944 0.033015 0.060 Uiso 1 1 calc GR . . . .
H30B H -0.174912 0.736803 0.105158 0.060 Uiso 1 1 calc GR . . . .
H30C H -0.111791 0.602150 0.077751 0.060 Uiso 1 1 calc GR . . . .
C4 C 0.37856(19) 0.94438(19) 0.31565(14) 0.0275(4) Uani 1 1 d . . . . .
C26 C 0.50144(19) 0.4689(2) 0.21164(15) 0.0304(4) Uani 1 1 d . . . . .
H26 H 0.490224 0.560238 0.215747 0.036 Uiso 1 1 calc R . . . .
C29 C -0.00600(18) 0.6250(2) 0.17689(14) 0.0287(4) Uani 1 1 d . . . . .
H29 H 0.008966 0.702954 0.191237 0.034 Uiso 1 1 calc R . . . .
C5 C 0.3778(2) 1.0525(2) 0.34477(16) 0.0385(5) Uani 1 1 d . . . . .
H5 H 0.460235 1.063789 0.358183 0.046 Uiso 1 1 calc R . . . .
C23 C 0.2623(2) 0.3508(2) 0.10706(15) 0.0330(5) Uani 1 1 d . . . . .
H23 H 0.266830 0.282382 0.079606 0.040 Uiso 1 1 calc R . . . .
C7 C 0.1399(2) 1.1286(2) 0.33578(16) 0.0365(5) Uani 1 1 d . . . . .
H7 H 0.059065 1.192565 0.342608 0.044 Uiso 1 1 calc R . . . .
C31 C -0.0832(2) 0.5479(2) 0.26626(16) 0.0422(5) Uani 1 1 d . . . . .
H31A H -0.098089 0.470184 0.254206 0.063 Uiso 1 1 calc GR . . . .
H31B H -0.170851 0.604381 0.280111 0.063 Uiso 1 1 calc GR . . . .
H31C H -0.030370 0.519445 0.321896 0.063 Uiso 1 1 calc GR . . . .
C12 C -0.0007(2) 1.0041(2) 0.29070(16) 0.0354(5) Uani 1 1 d . . . . .
H12 H 0.017685 0.932160 0.259418 0.042 Uiso 1 1 calc R . . . .
C9 C 0.5102(2) 0.8440(2) 0.30677(16) 0.0384(5) Uani 1 1 d . . . . .
H9 H 0.493979 0.785745 0.271930 0.046 Uiso 1 1 calc R . . . .
C28 C 0.5170(2) 0.3736(3) 0.31316(16) 0.0436(6) Uani 1 1 d . . . . .
H28A H 0.434820 0.393754 0.355921 0.065 Uiso 1 1 calc GR . . . .
H28B H 0.595100 0.382895 0.338096 0.065 Uiso 1 1 calc GR . . . .
H28C H 0.531249 0.282855 0.310847 0.065 Uiso 1 1 calc GR . . . .
C10 C 0.6243(2) 0.9095(3) 0.2475(2) 0.0566(7) Uani 1 1 d . . . . .
H10A H 0.639662 0.970565 0.278355 0.085 Uiso 1 1 calc GR . . . .
H10B H 0.599246 0.958341 0.181799 0.085 Uiso 1 1 calc GR . . . .
H10C H 0.707424 0.841620 0.244272 0.085 Uiso 1 1 calc GR . . . .
C6 C 0.2600(2) 1.1435(2) 0.35453(17) 0.0430(6) Uani 1 1 d . . . . .
H6 H 0.261475 1.217211 0.374347 0.052 Uiso 1 1 calc R . . . .
C13 C -0.0802(3) 1.1290(3) 0.22436(19) 0.0560(7) Uani 1 1 d . . . . .
H13A H -0.105255 1.199148 0.255897 0.084 Uiso 1 1 calc GR . . . .
H13B H -0.162488 1.111194 0.211253 0.084 Uiso 1 1 calc GR . . . .
H13C H -0.024226 1.157125 0.163211 0.084 Uiso 1 1 calc GR . . . .
C27 C 0.6302(2) 0.4399(3) 0.14420(18) 0.0480(6) Uani 1 1 d . . . . .
H27A H 0.648460 0.347929 0.143761 0.072 Uiso 1 1 calc GR . . . .
H27B H 0.706958 0.454385 0.167388 0.072 Uiso 1 1 calc GR . . . .
H27C H 0.617590 0.498923 0.078351 0.072 Uiso 1 1 calc GR . . . .
C14 C -0.0853(2) 0.9621(3) 0.38805(18) 0.0513(6) Uani 1 1 d . . . . .
H14A H -0.035496 0.878947 0.429004 0.077 Uiso 1 1 calc GR . . . .
H14B H -0.171492 0.949655 0.376871 0.077 Uiso 1 1 calc GR . . . .
H14C H -0.103139 1.030690 0.420534 0.077 Uiso 1 1 calc GR . . . .
N1 N 0.25157(16) 0.81023(14) 0.28048(11) 0.0238(3) Uani 1 1 d . . . . .
N2 N 0.24136(15) 0.64816(15) 0.23267(10) 0.0222(3) Uani 1 1 d . . . . .
C2 C 0.1701(2) 0.4752(2) 0.44232(14) 0.0284(4) Uani 1 1 d . . . . .
C1 C 0.1934(2) 0.67538(19) 0.49411(15) 0.0300(4) Uani 1 1 d . . . . .
O1 O 0.18402(17) 0.70213(16) 0.56367(11) 0.0454(4) Uani 1 1 d . . . . .
O2 O 0.14167(16) 0.37701(14) 0.48208(11) 0.0430(4) Uani 1 1 d . . . . .
C19 C 0.2994(2) 0.9919(2) 0.08544(15) 0.0377(5) Uani 1 1 d . . . . .
H19A H 0.318409 1.038031 0.016664 0.057 Uiso 1 1 calc GR . . . .
H19B H 0.372547 0.989004 0.121307 0.057 Uiso 1 1 calc GR . . . .
H19C H 0.213321 1.038810 0.111219 0.057 Uiso 1 1 calc GR . . . .
C17 C 0.4270(2) 0.7830(2) 0.05392(17) 0.0446(6) Uani 1 1 d . . . . .
H17A H 0.420826 0.696810 0.051191 0.067 Uiso 1 1 calc GR . . . .
H17B H 0.497652 0.770830 0.095014 0.067 Uiso 1 1 calc GR . . . .
H17C H 0.449801 0.838238 -0.011632 0.067 Uiso 1 1 calc GR . . . .
C18 C 0.1785(3) 0.8586(3) 0.03802(17) 0.0487(6) Uani 1 1 d . . . . .
H18A H 0.177196 0.769536 0.038566 0.073 Uiso 1 1 calc GR . . . .
H18B H 0.195583 0.912715 -0.028955 0.073 Uiso 1 1 calc GR . . . .
H18C H 0.090818 0.898727 0.066697 0.073 Uiso 1 1 calc GR . . . .
C11 C 0.5505(3) 0.7575(4) 0.4057(2) 0.0831(11) Uani 1 1 d . . . . .
H11A H 0.567371 0.812038 0.441625 0.125 Uiso 1 1 calc GR . . . .
H11B H 0.633040 0.690776 0.398321 0.125 Uiso 1 1 calc GR . . . .
H11C H 0.477177 0.713649 0.441402 0.125 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 N1 2.0457(15) . ?
Rh1 N2 2.0603(14) . ?
Rh1 C2 1.858(2) . ?
Rh1 C1 1.854(2) . ?
C20 C21 1.405(2) . ?
C20 C25 1.406(2) . ?
C20 N2 1.421(2) . ?
C15 C16 1.534(2) . ?
C15 N1 1.329(2) . ?
C15 N2 1.333(2) . ?
C24 C25 1.392(2) . ?
C24 C23 1.378(3) . ?
C3 C8 1.400(3) . ?
C3 C4 1.402(3) . ?
C3 N1 1.420(2) . ?
C16 C19 1.531(2) . ?
C16 C17 1.538(3) . ?
C16 C18 1.521(3) . ?
C21 C22 1.391(2) . ?
C21 C26 1.521(3) . ?
C25 C29 1.517(3) . ?
C22 C23 1.377(3) . ?
C8 C7 1.395(3) . ?
C8 C12 1.517(3) . ?
C30 C29 1.532(3) . ?
C4 C5 1.386(3) . ?
C4 C9 1.519(3) . ?
C26 C28 1.521(3) . ?
C26 C27 1.533(3) . ?
C29 C31 1.525(3) . ?
C5 C6 1.371(3) . ?
C7 C6 1.373(3) . ?
C12 C13 1.521(3) . ?
C12 C14 1.533(3) . ?
C9 C10 1.524(3) . ?
C9 C11 1.512(4) . ?
C2 O2 1.133(2) . ?
C1 O1 1.133(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Rh1 N2 63.11(6) . . ?
C2 Rh1 N1 168.16(7) . . ?
C2 Rh1 N2 105.25(7) . . ?
C1 Rh1 N1 101.51(7) . . ?
C1 Rh1 N2 164.61(7) . . ?
C1 Rh1 C2 90.14(8) . . ?
C21 C20 C25 120.88(15) . . ?
C21 C20 N2 119.38(15) . . ?
C25 C20 N2 119.25(15) . . ?
N1 C15 C16 126.74(15) . . ?
N1 C15 N2 107.61(15) . . ?
N2 C15 C16 125.64(15) . . ?
C23 C24 C25 121.05(17) . . ?
C8 C3 C4 121.28(16) . . ?
C8 C3 N1 119.37(16) . . ?
C4 C3 N1 118.78(16) . . ?
C15 C16 C17 109.18(16) . . ?
C19 C16 C15 112.96(15) . . ?
C19 C16 C17 107.02(16) . . ?
C18 C16 C15 109.98(15) . . ?
C18 C16 C19 108.16(17) . . ?
C18 C16 C17 109.46(18) . . ?
C20 C21 C26 121.90(16) . . ?
C22 C21 C20 118.22(16) . . ?
C22 C21 C26 119.74(17) . . ?
C20 C25 C29 121.88(16) . . ?
C24 C25 C20 118.44(17) . . ?
C24 C25 C29 119.53(16) . . ?
C23 C22 C21 121.37(18) . . ?
C3 C8 C12 122.06(16) . . ?
C7 C8 C3 117.77(17) . . ?
C7 C8 C12 120.13(18) . . ?
C3 C4 C9 121.64(17) . . ?
C5 C4 C3 118.40(18) . . ?
C5 C4 C9 119.95(18) . . ?
C21 C26 C28 110.37(16) . . ?
C21 C26 C27 112.87(17) . . ?
C28 C26 C27 110.08(18) . . ?
C25 C29 C30 113.08(16) . . ?
C25 C29 C31 109.49(17) . . ?
C31 C29 C30 110.19(17) . . ?
C6 C5 C4 121.02(19) . . ?
C22 C23 C24 120.00(17) . . ?
C6 C7 C8 121.24(19) . . ?
C8 C12 C13 112.27(18) . . ?
C8 C12 C14 110.13(18) . . ?
C13 C12 C14 109.95(19) . . ?
C4 C9 C10 112.1(2) . . ?
C11 C9 C4 110.8(2) . . ?
C11 C9 C10 111.0(2) . . ?
C5 C6 C7 120.28(18) . . ?
C15 N1 Rh1 95.04(11) . . ?
C15 N1 C3 135.14(15) . . ?
C3 N1 Rh1 129.66(11) . . ?
C20 N2 Rh1 132.48(12) . . ?
C15 N2 Rh1 94.24(10) . . ?
C15 N2 C20 133.03(15) . . ?
O2 C2 Rh1 178.19(18) . . ?
O1 C1 Rh1 177.37(18) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Hexane'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_18
_database_code_depnum_ccdc_archive 'CCDC 1972010'
loop_
_audit_author_name
_audit_author_address
'Alasdair McKay'
;Monash University
Australia
;
_audit_update_record             
;
2019-12-14 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_audit_creation_date             2019-12-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
''
alasdair.mckay@monash.edu
_chemical_name_common            ?
_chemical_name_systematic        '[TlCl(DippForm)2]'
_chemical_formula_moiety         'C50 H70 Cl N4 Tl'
_chemical_formula_sum            'C50 H70 Cl N4 Tl'
_chemical_formula_weight         966.92
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.5473(4)
_cell_length_b                   16.5705(6)
_cell_length_c                   21.2327(8)
_cell_angle_alpha                90
_cell_angle_beta                 109.1370(10)
_cell_angle_gamma                90
_cell_volume                     4835.4(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.981
_cell_measurement_theta_min      2.373
_shelx_estimated_absorpt_T_max   0.771
_shelx_estimated_absorpt_T_min   0.684
_exptl_absorpt_coefficient_mu    3.431
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1411 before and 0.0675 after correction. The Ratio of minimum to maximum transmission is 0.8925. The λ/2 correction factor is 0.00150.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1984
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            42717
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         2.660
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8749
_reflns_number_total             10671
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         10671
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0281
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0209P)²+1.9269P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0696
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C11-C10 \\sim C11A-C10 \\sim C12A-C10 \\sim C12-C10
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C10 \\sim C12A \\sim C11A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C10 \\sim C12 \\sim C11: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
4. Rigid body (RIGU) restrains
 C10, C12A, C11A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C10, C12, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H10A)=Sof(C11A)=Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(C12A)=Sof(H12D)=
 Sof(H12E)=Sof(H12F)=1-FVAR(1)
 Sof(H10)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C11)=Sof(H11A)=Sof(H11B)=
 Sof(H11C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C48(H48), C7(H7), C35(H35), C10(H10), C10(H10A), C23(H23), C32(H32), C20(H20),
  C45(H45)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C43(H43), C30(H30), C42(H42), C18(H18), C41(H41), C29(H29), C16(H16),
 C3(H3), C4(H4), C28(H28), C17(H17)
6.c Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C49(H49A,H49B,H49C), C36(H36A,H36B,H36C), C24(H24A,H24B,
 H24C), C22(H22A,H22B,H22C), C21(H21A,H21B,H21C), C25(H25A,H25B,H25C), C37(H37A,
 H37B,H37C), C9(H9A,H9B,H9C), C46(H46A,H46B,H46C), C8(H8A,H8B,H8C), C47(H47A,
 H47B,H47C), C12(H12A,H12B,H12C), C34(H34A,H34B,H34C), C33(H33A,H33B,H33C),
 C11(H11A,H11B,H11C), C11A(H11D,H11E,H11F), C12A(H12D,H12E,H12F)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tl1 Tl 0.73623(2) 0.27532(2) 0.41545(2) 0.02401(5) Uani 1 1 d . . . . .
Cl1 Cl 0.71673(6) 0.27205(6) 0.52456(4) 0.0431(2) Uani 1 1 d . . . . .
N3 N 0.79135(16) 0.39010(14) 0.38558(12) 0.0248(5) Uani 1 1 d . . . . .
N2 N 0.58036(16) 0.24400(14) 0.34484(12) 0.0217(5) Uani 1 1 d . . . . .
N1 N 0.70234(15) 0.15693(14) 0.35968(11) 0.0227(5) Uani 1 1 d . . . . .
N4 N 0.90465(16) 0.30041(14) 0.43924(12) 0.0219(5) Uani 1 1 d . . . . .
C14 C 0.4811(2) 0.26653(17) 0.32813(15) 0.0243(6) Uani 1 1 d . . . . .
C26 C 0.7546(2) 0.46526(17) 0.35290(16) 0.0265(7) Uani 1 1 d . . . . .
C13 C 0.6094(2) 0.17303(18) 0.33311(14) 0.0233(6) Uani 1 1 d . . . . .
C44 C 1.0534(2) 0.23506(18) 0.43693(16) 0.0277(7) Uani 1 1 d . . . . .
C39 C 1.0014(2) 0.27440(17) 0.47278(15) 0.0244(6) Uani 1 1 d . . . . .
C6 C 0.7601(2) 0.07018(19) 0.28646(16) 0.0308(7) Uani 1 1 d . . . . .
C38 C 0.8829(2) 0.37117(18) 0.41182(14) 0.0236(6) Uani 1 1 d . . . . .
C1 C 0.75209(19) 0.08815(17) 0.34919(15) 0.0242(6) Uani 1 1 d . . . . .
C31 C 0.7648(2) 0.48401(18) 0.29162(16) 0.0303(7) Uani 1 1 d . . . . .
C19 C 0.4416(2) 0.31940(18) 0.27389(16) 0.0283(7) Uani 1 1 d . . . . .
C48 C 1.0099(2) 0.2221(2) 0.36289(17) 0.0338(8) Uani 1 1 d . . . . .
H48 H 0.937600 0.225258 0.351145 0.041 Uiso 1 1 calc R . . . .
C15 C 0.4254(2) 0.2395(2) 0.36674(17) 0.0333(8) Uani 1 1 d . . . . .
C5 C 0.8166(2) 0.0038(2) 0.28152(18) 0.0384(8) Uani 1 1 d . . . . .
H5 H 0.823472 -0.009166 0.239710 0.046 Uiso 1 1 calc R . . . .
C7 C 0.7893(2) 0.0593(2) 0.47214(16) 0.0372(8) Uani 1 1 d . . . . .
H7 H 0.765261 0.116154 0.469760 0.045 Uiso 1 1 calc R . . . .
C43 C 1.1483(2) 0.2100(2) 0.47102(19) 0.0389(8) Uani 1 1 d . . . . .
H43 H 1.185091 0.183752 0.447434 0.047 Uiso 1 1 calc R . . . .
C35 C 0.8122(2) 0.4274(2) 0.25445(17) 0.0354(8) Uani 1 1 d . . . . .
H35 H 0.833748 0.377642 0.282043 0.043 Uiso 1 1 calc R . . . .
C40 C 1.0421(2) 0.28555(18) 0.54215(16) 0.0309(7) Uani 1 1 d . . . . .
C10 C 0.7103(2) 0.1211(2) 0.22513(16) 0.0387(8) Uani 1 1 d D U . . .
H10 H 0.681298 0.168088 0.241517 0.046 Uiso 0.531(10) 1 calc R . P A 1
H10A H 0.644691 0.133929 0.228229 0.046 Uiso 0.469(10) 1 calc R . P A 2
C2 C 0.7999(2) 0.04054(18) 0.40544(16) 0.0284(7) Uani 1 1 d . . . . .
C23 C 0.5023(2) 0.34915(19) 0.23314(16) 0.0328(7) Uani 1 1 d . . . . .
H23 H 0.572074 0.344863 0.261675 0.039 Uiso 1 1 calc R . . . .
C30 C 0.7287(2) 0.5583(2) 0.26293(17) 0.0381(8) Uani 1 1 d . . . . .
H30 H 0.736395 0.573230 0.221755 0.046 Uiso 1 1 calc R . . . .
C27 C 0.7082(2) 0.51761(19) 0.38526(17) 0.0331(7) Uani 1 1 d . . . . .
C42 C 1.1892(2) 0.2230(2) 0.53882(19) 0.0435(9) Uani 1 1 d . . . . .
H42 H 1.254464 0.206926 0.561324 0.052 Uiso 1 1 calc R . . . .
C18 C 0.3445(2) 0.3393(2) 0.25691(19) 0.0425(9) Uani 1 1 d . . . . .
H18 H 0.316345 0.373845 0.219856 0.051 Uiso 1 1 calc R . . . .
C41 C 1.1367(2) 0.2588(2) 0.57331(18) 0.0395(8) Uani 1 1 d . . . . .
H41 H 1.165311 0.265655 0.620108 0.047 Uiso 1 1 calc R . . . .
C29 C 0.6821(2) 0.6103(2) 0.29308(19) 0.0446(9) Uani 1 1 d . . . . .
H29 H 0.657068 0.660169 0.272405 0.053 Uiso 1 1 calc R . . . .
C16 C 0.3282(3) 0.2630(2) 0.3470(2) 0.0442(9) Uani 1 1 d . . . . .
H16 H 0.288714 0.245494 0.372257 0.053 Uiso 1 1 calc R . . . .
C3 C 0.8536(2) -0.0255(2) 0.39649(19) 0.0385(8) Uani 1 1 d . . . . .
H3 H 0.885120 -0.059049 0.433551 0.046 Uiso 1 1 calc R . . . .
C32 C 0.6974(3) 0.4976(2) 0.45136(19) 0.0459(9) Uani 1 1 d . . . . .
H32 H 0.739060 0.449273 0.469035 0.055 Uiso 1 1 calc R . . . .
C20 C 0.4687(2) 0.1878(2) 0.42813(16) 0.0393(8) Uani 1 1 d . . . . .
H20 H 0.540590 0.185408 0.437355 0.047 Uiso 1 1 calc R . . . .
C4 C 0.8623(2) -0.0430(2) 0.3362(2) 0.0427(9) Uani 1 1 d . . . . .
H4 H 0.900217 -0.088009 0.331838 0.051 Uiso 1 1 calc R . . . .
C50 C 1.0409(3) 0.2890(2) 0.3256(2) 0.0531(11) Uani 1 1 d . . . . .
H50A H 1.022857 0.341308 0.339606 0.080 Uiso 1 1 calc GR . . . .
H50B H 1.008415 0.282067 0.277576 0.080 Uiso 1 1 calc GR . . . .
H50C H 1.111594 0.286898 0.335483 0.080 Uiso 1 1 calc GR . . . .
C49 C 1.0341(3) 0.1395(2) 0.34077(19) 0.0528(10) Uani 1 1 d . . . . .
H49A H 1.104173 0.136079 0.348402 0.079 Uiso 1 1 calc GR . . . .
H49B H 0.998462 0.132029 0.293211 0.079 Uiso 1 1 calc GR . . . .
H49C H 1.015180 0.097319 0.366464 0.079 Uiso 1 1 calc GR . . . .
C28 C 0.6719(2) 0.5900(2) 0.35279(19) 0.0424(9) Uani 1 1 d . . . . .
H28 H 0.639247 0.626273 0.372911 0.051 Uiso 1 1 calc R . . . .
C45 C 0.9840(2) 0.3256(2) 0.58039(17) 0.0413(8) Uani 1 1 d . . . . .
H45 H 0.913498 0.317142 0.555017 0.050 Uiso 1 1 calc R . . . .
C36 C 0.7397(3) 0.4021(3) 0.1867(2) 0.0780(15) Uani 1 1 d . . . . .
H36A H 0.683811 0.375034 0.193548 0.117 Uiso 1 1 calc GR . . . .
H36B H 0.771632 0.365087 0.164393 0.117 Uiso 1 1 calc GR . . . .
H36C H 0.717299 0.450077 0.158866 0.117 Uiso 1 1 calc GR . . . .
C17 C 0.2879(3) 0.3106(2) 0.2921(2) 0.0520(10) Uani 1 1 d . . . . .
H17 H 0.220665 0.323739 0.278524 0.062 Uiso 1 1 calc R . . . .
C24 C 0.4878(3) 0.2940(3) 0.1735(2) 0.0614(12) Uani 1 1 d . . . . .
H24A H 0.504145 0.238461 0.188956 0.092 Uiso 1 1 calc GR . . . .
H24B H 0.530080 0.311545 0.148458 0.092 Uiso 1 1 calc GR . . . .
H24C H 0.419697 0.296429 0.144564 0.092 Uiso 1 1 calc GR . . . .
C22 C 0.4513(4) 0.2237(3) 0.4894(2) 0.0762(16) Uani 1 1 d . . . . .
H22A H 0.479738 0.277849 0.497791 0.114 Uiso 1 1 calc GR . . . .
H22B H 0.481690 0.189236 0.528175 0.114 Uiso 1 1 calc GR . . . .
H22C H 0.381135 0.227055 0.481644 0.114 Uiso 1 1 calc GR . . . .
C21 C 0.4297(3) 0.1015(2) 0.4164(2) 0.0606(12) Uani 1 1 d . . . . .
H21A H 0.360399 0.101349 0.411749 0.091 Uiso 1 1 calc GR . . . .
H21B H 0.465511 0.067578 0.454260 0.091 Uiso 1 1 calc GR . . . .
H21C H 0.438088 0.080260 0.375521 0.091 Uiso 1 1 calc GR . . . .
C25 C 0.4825(3) 0.4375(3) 0.2131(3) 0.0736(15) Uani 1 1 d . . . . .
H25A H 0.415866 0.443163 0.182338 0.110 Uiso 1 1 calc GR . . . .
H25B H 0.528487 0.455735 0.191183 0.110 Uiso 1 1 calc GR . . . .
H25C H 0.490454 0.470252 0.252971 0.110 Uiso 1 1 calc GR . . . .
C37 C 0.9002(3) 0.4646(2) 0.2430(2) 0.0588(11) Uani 1 1 d . . . . .
H37A H 0.880070 0.511576 0.213718 0.088 Uiso 1 1 calc GR . . . .
H37B H 0.930837 0.424748 0.222089 0.088 Uiso 1 1 calc GR . . . .
H37C H 0.946874 0.481462 0.285808 0.088 Uiso 1 1 calc GR . . . .
C9 C 0.8853(3) 0.0561(4) 0.5288(2) 0.101(2) Uani 1 1 d . . . . .
H9A H 0.912983 0.001819 0.531570 0.151 Uiso 1 1 calc GR . . . .
H9B H 0.874382 0.069130 0.570827 0.151 Uiso 1 1 calc GR . . . .
H9C H 0.930502 0.095380 0.520649 0.151 Uiso 1 1 calc GR . . . .
C46 C 1.0036(3) 0.4175(3) 0.5842(2) 0.0660(12) Uani 1 1 d . . . . .
H46A H 1.072671 0.427501 0.607955 0.099 Uiso 1 1 calc GR . . . .
H46B H 0.964211 0.443645 0.607959 0.099 Uiso 1 1 calc GR . . . .
H46C H 0.986196 0.439609 0.538948 0.099 Uiso 1 1 calc GR . . . .
C8 C 0.7133(4) 0.0065(3) 0.4856(3) 0.0907(18) Uani 1 1 d . . . . .
H8A H 0.656117 0.003047 0.445285 0.136 Uiso 1 1 calc GR . . . .
H8B H 0.694294 0.029841 0.521926 0.136 Uiso 1 1 calc GR . . . .
H8C H 0.740019 -0.047632 0.498295 0.136 Uiso 1 1 calc GR . . . .
C47 C 1.0037(4) 0.2916(3) 0.6493(2) 0.0781(15) Uani 1 1 d . . . . .
H47A H 0.989256 0.233646 0.646236 0.117 Uiso 1 1 calc GR . . . .
H47B H 0.962404 0.318900 0.671058 0.117 Uiso 1 1 calc GR . . . .
H47C H 1.072269 0.299965 0.675599 0.117 Uiso 1 1 calc GR . . . .
C12 C 0.7892(6) 0.1578(6) 0.1977(4) 0.056(3) Uani 0.531(10) 1 d D U P A 1
H12A H 0.836176 0.189059 0.232945 0.084 Uiso 0.531(10) 1 calc GR . P A 1
H12B H 0.757626 0.193085 0.159751 0.084 Uiso 0.531(10) 1 calc GR . P A 1
H12C H 0.823073 0.114018 0.183320 0.084 Uiso 0.531(10) 1 calc GR . P A 1
C34 C 0.7328(5) 0.5641(3) 0.5024(3) 0.113(2) Uani 1 1 d . . . . .
H34A H 0.799947 0.578211 0.506527 0.169 Uiso 1 1 calc GR . . . .
H34B H 0.730335 0.545430 0.545628 0.169 Uiso 1 1 calc GR . . . .
H34C H 0.691095 0.611616 0.488156 0.169 Uiso 1 1 calc GR . . . .
C33 C 0.5935(3) 0.4740(4) 0.4440(3) 0.108(2) Uani 1 1 d . . . . .
H33A H 0.550897 0.520940 0.429465 0.162 Uiso 1 1 calc GR . . . .
H33B H 0.590571 0.454818 0.486940 0.162 Uiso 1 1 calc GR . . . .
H33C H 0.572093 0.430862 0.410760 0.162 Uiso 1 1 calc GR . . . .
C11 C 0.6303(6) 0.0830(6) 0.1744(4) 0.058(3) Uani 0.531(10) 1 d D U P A 1
H11A H 0.653120 0.033328 0.159404 0.086 Uiso 0.531(10) 1 calc GR . P A 1
H11B H 0.604938 0.119893 0.136571 0.086 Uiso 0.531(10) 1 calc GR . P A 1
H11C H 0.578542 0.070101 0.192923 0.086 Uiso 0.531(10) 1 calc GR . P A 1
C11A C 0.6889(9) 0.0713(6) 0.1584(4) 0.060(3) Uani 0.469(10) 1 d D U P A 2
H11D H 0.749177 0.065109 0.147736 0.089 Uiso 0.469(10) 1 calc GR . P A 2
H11E H 0.640569 0.099894 0.121975 0.089 Uiso 0.469(10) 1 calc GR . P A 2
H11F H 0.663695 0.017871 0.164036 0.089 Uiso 0.469(10) 1 calc GR . P A 2
C12A C 0.7542(7) 0.1987(5) 0.2223(5) 0.051(3) Uani 0.469(10) 1 d D U P A 2
H12D H 0.759293 0.229469 0.262684 0.076 Uiso 0.469(10) 1 calc GR . P A 2
H12E H 0.713768 0.228495 0.183090 0.076 Uiso 0.469(10) 1 calc GR . P A 2
H12F H 0.819245 0.190717 0.219050 0.076 Uiso 0.469(10) 1 calc GR . P A 2
H13 H 0.5637(18) 0.1297(17) 0.3043(13) 0.018(7) Uiso 1 1 d . . . . .
H38 H 0.929(2) 0.4052(17) 0.4126(14) 0.019(8) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tl1 Cl1 2.4251(8) . ?
Tl1 N3 2.235(2) . ?
Tl1 N2 2.330(2) . ?
Tl1 N1 2.261(2) . ?
Tl1 N4 2.371(2) . ?
N3 C26 1.441(4) . ?
N3 C38 1.302(4) . ?
N2 C14 1.419(4) . ?
N2 C13 1.301(4) . ?
N1 C13 1.311(3) . ?
N1 C1 1.407(4) . ?
N4 C39 1.420(4) . ?
N4 C38 1.301(4) . ?
C14 C19 1.411(4) . ?
C14 C15 1.402(4) . ?
C26 C31 1.392(4) . ?
C26 C27 1.409(4) . ?
C44 C39 1.398(4) . ?
C44 C48 1.505(5) . ?
C44 C43 1.395(4) . ?
C39 C40 1.408(4) . ?
C6 C1 1.406(4) . ?
C6 C5 1.398(4) . ?
C6 C10 1.521(5) . ?
C1 C2 1.410(4) . ?
C31 C35 1.528(5) . ?
C31 C30 1.398(4) . ?
C19 C23 1.507(4) . ?
C19 C18 1.378(4) . ?
C48 C50 1.515(5) . ?
C48 C49 1.525(5) . ?
C15 C16 1.393(5) . ?
C15 C20 1.514(5) . ?
C5 C4 1.373(5) . ?
C7 C2 1.506(4) . ?
C7 C9 1.516(5) . ?
C7 C8 1.510(5) . ?
C43 C42 1.383(5) . ?
C35 C36 1.538(5) . ?
C35 C37 1.511(5) . ?
C40 C41 1.390(5) . ?
C40 C45 1.504(5) . ?
C10 C12 1.570(7) . ?
C10 C11 1.446(7) . ?
C10 C11A 1.581(8) . ?
C10 C12A 1.446(8) . ?
C2 C3 1.393(4) . ?
C23 C24 1.519(5) . ?
C23 C25 1.525(5) . ?
C30 C29 1.377(5) . ?
C27 C32 1.499(5) . ?
C27 C28 1.398(4) . ?
C42 C41 1.356(5) . ?
C18 C17 1.366(5) . ?
C29 C28 1.365(5) . ?
C16 C17 1.370(5) . ?
C3 C4 1.358(5) . ?
C32 C34 1.512(6) . ?
C32 C33 1.519(6) . ?
C20 C22 1.526(5) . ?
C20 C21 1.528(5) . ?
C45 C46 1.546(5) . ?
C45 C47 1.507(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Tl1 Cl1 117.08(7) . . ?
N3 Tl1 N2 111.77(8) . . ?
N3 Tl1 N1 128.80(9) . . ?
N3 Tl1 N4 57.95(8) . . ?
N2 Tl1 Cl1 102.46(6) . . ?
N2 Tl1 N4 153.63(8) . . ?
N1 Tl1 Cl1 114.04(6) . . ?
N1 Tl1 N2 58.04(8) . . ?
N1 Tl1 N4 107.25(8) . . ?
N4 Tl1 Cl1 103.70(6) . . ?
C26 N3 Tl1 139.60(18) . . ?
C38 N3 Tl1 94.90(18) . . ?
C38 N3 C26 125.5(2) . . ?
C14 N2 Tl1 142.94(19) . . ?
C13 N2 Tl1 90.92(17) . . ?
C13 N2 C14 123.9(2) . . ?
C13 N1 Tl1 93.78(18) . . ?
C13 N1 C1 127.5(2) . . ?
C1 N1 Tl1 138.68(17) . . ?
C39 N4 Tl1 147.01(18) . . ?
C38 N4 Tl1 88.86(17) . . ?
C38 N4 C39 123.6(2) . . ?
C19 C14 N2 118.4(3) . . ?
C15 C14 N2 120.4(3) . . ?
C15 C14 C19 121.1(3) . . ?
C31 C26 N3 120.4(3) . . ?
C31 C26 C27 122.2(3) . . ?
C27 C26 N3 117.3(3) . . ?
N2 C13 N1 117.1(3) . . ?
C39 C44 C48 121.2(3) . . ?
C43 C44 C39 118.4(3) . . ?
C43 C44 C48 120.3(3) . . ?
C44 C39 N4 119.5(3) . . ?
C44 C39 C40 120.9(3) . . ?
C40 C39 N4 119.5(3) . . ?
C1 C6 C10 121.9(3) . . ?
C5 C6 C1 118.1(3) . . ?
C5 C6 C10 120.0(3) . . ?
N4 C38 N3 118.2(3) . . ?
N1 C1 C2 117.1(3) . . ?
C6 C1 N1 121.9(3) . . ?
C6 C1 C2 120.9(3) . . ?
C26 C31 C35 123.4(3) . . ?
C26 C31 C30 117.6(3) . . ?
C30 C31 C35 119.0(3) . . ?
C14 C19 C23 120.9(3) . . ?
C18 C19 C14 118.1(3) . . ?
C18 C19 C23 120.9(3) . . ?
C44 C48 C50 110.3(3) . . ?
C44 C48 C49 112.9(3) . . ?
C50 C48 C49 111.0(3) . . ?
C14 C15 C20 121.8(3) . . ?
C16 C15 C14 117.4(3) . . ?
C16 C15 C20 120.8(3) . . ?
C4 C5 C6 121.0(3) . . ?
C2 C7 C9 112.8(3) . . ?
C2 C7 C8 111.4(3) . . ?
C8 C7 C9 111.8(4) . . ?
C42 C43 C44 120.6(3) . . ?
C31 C35 C36 111.3(3) . . ?
C37 C35 C31 112.5(3) . . ?
C37 C35 C36 108.6(3) . . ?
C39 C40 C45 120.3(3) . . ?
C41 C40 C39 117.8(3) . . ?
C41 C40 C45 121.8(3) . . ?
C6 C10 C12 109.3(4) . . ?
C6 C10 C11A 112.1(4) . . ?
C11 C10 C6 115.9(4) . . ?
C11 C10 C12 113.6(5) . . ?
C12A C10 C6 115.9(4) . . ?
C12A C10 C11A 112.7(6) . . ?
C1 C2 C7 120.5(3) . . ?
C3 C2 C1 117.8(3) . . ?
C3 C2 C7 121.7(3) . . ?
C19 C23 C24 109.5(3) . . ?
C19 C23 C25 112.4(3) . . ?
C24 C23 C25 112.5(3) . . ?
C29 C30 C31 121.4(3) . . ?
C26 C27 C32 122.3(3) . . ?
C28 C27 C26 116.8(3) . . ?
C28 C27 C32 120.9(3) . . ?
C41 C42 C43 120.2(3) . . ?
C17 C18 C19 121.5(3) . . ?
C42 C41 C40 121.9(3) . . ?
C28 C29 C30 119.8(3) . . ?
C17 C16 C15 121.7(3) . . ?
C4 C3 C2 121.8(3) . . ?
C27 C32 C34 113.2(3) . . ?
C27 C32 C33 111.5(3) . . ?
C34 C32 C33 110.8(4) . . ?
C15 C20 C22 112.0(3) . . ?
C15 C20 C21 111.2(3) . . ?
C22 C20 C21 110.3(3) . . ?
C3 C4 C5 120.5(3) . . ?
C29 C28 C27 122.1(3) . . ?
C40 C45 C46 109.7(3) . . ?
C40 C45 C47 113.4(3) . . ?
C47 C45 C46 110.2(3) . . ?
C18 C17 C16 120.0(3) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_21
_database_code_depnum_ccdc_archive 'CCDC 1972012'
loop_
_audit_author_name
_audit_author_address
'Alasdair McKay'
;Monash University
Australia
;
_audit_update_record             
;
2019-12-14 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_audit_creation_date             2019-12-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
''
alasdair.mckay@monash.edu
_chemical_name_common            ?
_chemical_name_systematic        '[SnBr(N3Dipp2)(IEt)]'
_chemical_formula_moiety         'C31 H46 Br N5 Sn'
_chemical_formula_sum            'C31 H46 Br N5 Sn'
_chemical_formula_weight         687.33
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   17.1551(13)
_cell_length_b                   21.1932(16)
_cell_length_c                   21.6061(17)
_cell_angle_alpha                87.943(2)
_cell_angle_beta                 68.502(2)
_cell_angle_gamma                69.665(2)
_cell_volume                     6815.6(9)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9780
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.307
_cell_measurement_theta_min      2.501
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.948
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0657 before and 0.0440 after correction. The Ratio of minimum to maximum transmission is 0.9042. The λ/2 correction factor is 0.00150.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2816
_exptl_crystal_recrystallization_method 
'Grown from diethyl ether at room temperature'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            132490
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.388
_diffrn_reflns_theta_min         1.018
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                19988
_reflns_number_total             27861
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.575
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1430
_refine_ls_number_reflns         27861
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0391
_refine_ls_restrained_S_all      1.099
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0337P)²+11.3684P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0981
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C24 \\sim C24A \\sim C22 \\sim C23 \\sim C23A: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
3. Rigid body (RIGU) restrains
 C24, C24A, C22, C23, C23A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H22A)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C23A)=Sof(H23D)=
 Sof(H23E)=Sof(H23F)=1-FVAR(1)
 Sof(H22)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24)=Sof(H24D)=Sof(H24E)=
 Sof(H24F)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C7(H7), C112(H112), C10(H10), C84(H84), C22(H22), C22(H22A), C115(H115),
 C38(H38), C69(H69), C41(H41), C100(H100), C72(H72), C50(H50), C81(H81),
 C19(H19), C103(H103), C53(H53)
5.b Secondary CH2 refined with riding coordinates:
 C92(H92A,H92B), C119(H11D,H11E), C57(H57A,H57B), C61(H61A,H61B), C88(H88A,
 H88B), C30(H30A,H30B), C123(H12D,H12E), C26(H26A,H26B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C108(H108), C5(H5), C34(H34), C91(H91), C90(H90), C28(H28), C36(H36),
 C110(H110), C59(H59), C4(H4), C29(H29), C17(H17), C60(H60), C35(H35),
 C121(H121), C79(H79), C109(H109), C77(H77), C98(H98), C122(H122), C48(H48),
 C67(H67), C78(H78), C65(H65), C15(H15), C66(H66), C16(H16), C96(H96), C47(H47),
  C46(H46), C97(H97)
5.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C93(H93A,H93B,H93C), C114(H11F,H11G,H11H), C8(H8A,H8B,
 H8C), C9(H9A,H9B,H9C), C120(H12F,H12G,H12H), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C), C113(H11I,H11J,H11K), C117(H11L,H11M,H11N), C43(H43A,H43B,H43C),
 C58(H58A,H58B,H58C), C70(H70A,H70B,H70C), C40(H40A,H40B,H40C), C85(H85A,H85B,
 H85C), C27(H27A,H27B,H27C), C124(H12I,H12J,H12K), C101(H10A,H10B,H10C),
 C39(H39A,H39B,H39C), C89(H89A,H89B,H89C), C105(H10D,H10E,H10F), C86(H86A,H86B,
 H86C), C62(H62A,H62B,H62C), C42(H42A,H42B,H42C), C21(H21A,H21B,H21C), C83(H83A,
 H83B,H83C), C71(H71A,H71B,H71C), C116(H11O,H11P,H11Q), C74(H74A,H74B,H74C),
 C102(H10G,H10H,H10I), C104(H10J,H10K,H10L), C73(H73A,H73B,H73C), C82(H82A,H82B,
 H82C), C20(H20A,H20B,H20C), C52(H52A,H52B,H52C), C51(H51A,H51B,H51C), C54(H54A,
 H54B,H54C), C55(H55A,H55B,H55C), C23(H23A,H23B,H23C), C24A(H24A,H24B,H24C),
 C23A(H23D,H23E,H23F), C24(H24D,H24E,H24F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.13207(2) 0.70670(2) 1.15920(2) 0.02415(7) Uani 1 1 d . . . . .
Sn3 Sn 0.49471(2) 0.69114(2) 0.69012(2) 0.02385(7) Uani 1 1 d . . . . .
Sn2 Sn 0.02652(2) 0.80639(2) 0.76425(2) 0.02402(7) Uani 1 1 d . . . . .
Sn4 Sn 0.40795(2) 0.79711(2) 0.28712(2) 0.02413(7) Uani 1 1 d . . . . .
Br1 Br 0.24711(3) 0.73189(2) 1.04392(2) 0.03322(10) Uani 1 1 d . . . . .
Br4 Br 0.28081(3) 0.78564(2) 0.40329(2) 0.03251(10) Uani 1 1 d . . . . .
Br3 Br 0.46597(3) 0.57184(2) 0.70435(2) 0.03423(10) Uani 1 1 d . . . . .
Br2 Br 0.03833(3) 0.93127(2) 0.75908(2) 0.03236(10) Uani 1 1 d . . . . .
N1 N 0.0282(2) 0.74738(15) 1.11681(14) 0.0209(7) Uani 1 1 d . . . . .
N18 N 0.5074(2) 0.74885(16) 0.33258(15) 0.0233(7) Uani 1 1 d . . . . .
N15 N 0.3155(2) 0.72765(16) 0.83424(16) 0.0254(7) Uani 1 1 d . . . . .
N17 N 0.5850(2) 0.72853(16) 0.28122(16) 0.0245(7) Uani 1 1 d . . . . .
N2 N -0.0486(2) 0.75978(15) 1.16863(15) 0.0228(7) Uani 1 1 d . . . . .
N11 N 0.5327(2) 0.76226(16) 0.75307(16) 0.0258(7) Uani 1 1 d . . . . .
N8 N -0.0143(2) 0.73811(16) 0.69931(16) 0.0257(7) Uani 1 1 d . . . . .
N3 N -0.0351(2) 0.75966(15) 1.22315(15) 0.0213(7) Uani 1 1 d . . . . .
N12 N 0.5940(2) 0.71128(17) 0.76210(16) 0.0282(8) Uani 1 1 d . . . . .
N16 N 0.5701(2) 0.73133(15) 0.22683(16) 0.0237(7) Uani 1 1 d . . . . .
N7 N -0.0818(2) 0.78906(17) 0.69911(16) 0.0285(8) Uani 1 1 d . . . . .
N6 N -0.0757(2) 0.84484(16) 0.71936(16) 0.0263(7) Uani 1 1 d . . . . .
N5 N 0.1459(2) 0.79170(16) 1.27053(16) 0.0264(7) Uani 1 1 d . . . . .
N19 N 0.3967(2) 0.64744(16) 0.25059(17) 0.0281(8) Uani 1 1 d . . . . .
N9 N 0.1985(2) 0.78481(17) 0.61524(16) 0.0297(8) Uani 1 1 d . . . . .
N13 N 0.5860(2) 0.65474(16) 0.74573(16) 0.0258(7) Uani 1 1 d . . . . .
N4 N 0.1218(2) 0.86295(16) 1.20072(16) 0.0260(7) Uani 1 1 d . . . . .
N20 N 0.3788(2) 0.71831(17) 0.17939(16) 0.0289(8) Uani 1 1 d . . . . .
N14 N 0.2948(2) 0.79975(16) 0.76455(16) 0.0278(7) Uani 1 1 d . . . . .
N10 N 0.2263(2) 0.70768(16) 0.67916(17) 0.0294(8) Uani 1 1 d . . . . .
C1 C 0.0237(2) 0.73767(19) 1.05309(18) 0.0223(8) Uani 1 1 d . . . . .
C32 C -0.1537(3) 0.90515(19) 0.7338(2) 0.0273(9) Uani 1 1 d . . . . .
C13 C -0.1127(2) 0.7673(2) 1.28283(19) 0.0255(9) Uani 1 1 d . . . . .
C2 C 0.0426(3) 0.6719(2) 1.02653(19) 0.0253(9) Uani 1 1 d . . . . .
C63 C 0.5344(3) 0.8277(2) 0.7673(2) 0.0281(9) Uani 1 1 d . . . . .
C106 C 0.5115(2) 0.7572(2) 0.39686(18) 0.0247(8) Uani 1 1 d . . . . .
C75 C 0.6577(3) 0.5937(2) 0.7446(2) 0.0332(10) Uani 1 1 d . . . . .
C94 C 0.6490(3) 0.7107(2) 0.16633(19) 0.0275(9) Uani 1 1 d . . . . .
C118 C 0.3948(2) 0.71007(19) 0.2365(2) 0.0258(9) Uani 1 1 d . . . . .
C44 C -0.0094(3) 0.6737(2) 0.6756(2) 0.0287(9) Uani 1 1 d . . . . .
C25 C 0.1318(2) 0.7980(2) 1.21274(19) 0.0245(8) Uani 1 1 d . . . . .
C6 C 0.0016(3) 0.7937(2) 1.01775(19) 0.0264(9) Uani 1 1 d . . . . .
C33 C -0.2206(3) 0.9212(2) 0.7987(2) 0.0322(10) Uani 1 1 d . . . . .
C87 C 0.3564(2) 0.74249(19) 0.77205(19) 0.0243(8) Uani 1 1 d . . . . .
C56 C 0.1617(3) 0.76505(19) 0.67516(19) 0.0262(9) Uani 1 1 d . . . . .
C76 C 0.6548(3) 0.5643(2) 0.8044(2) 0.0346(10) Uani 1 1 d . . . . .
C92 C 0.3562(3) 0.6697(2) 0.8664(2) 0.0290(9) Uani 1 1 d . . . . .
H92A H 0.362516 0.686616 0.905759 0.035 Uiso 1 1 calc R . . . .
H92B H 0.416882 0.642173 0.834543 0.035 Uiso 1 1 calc R . . . .
C18 C -0.1469(3) 0.7155(2) 1.2969(2) 0.0318(10) Uani 1 1 d . . . . .
C3 C 0.0401(3) 0.6640(2) 0.9634(2) 0.0313(9) Uani 1 1 d . . . . .
H3 H 0.053756 0.620044 0.944106 0.038 Uiso 1 1 calc R . . . .
C37 C -0.1607(3) 0.9487(2) 0.6840(2) 0.0292(9) Uani 1 1 d . . . . .
C111 C 0.5285(3) 0.7015(2) 0.43330(19) 0.0283(9) Uani 1 1 d . . . . .
C108 C 0.4944(3) 0.8305(2) 0.4874(2) 0.0349(10) Uani 1 1 d . . . . .
H108 H 0.481972 0.874210 0.506572 0.042 Uiso 1 1 calc R . . . .
C5 C -0.0010(3) 0.7827(2) 0.9554(2) 0.0326(10) Uani 1 1 d . . . . .
H5 H -0.016502 0.820117 0.931057 0.039 Uiso 1 1 calc R . . . .
C107 C 0.4957(3) 0.8225(2) 0.4229(2) 0.0292(9) Uani 1 1 d . . . . .
C68 C 0.4771(3) 0.8639(2) 0.8292(2) 0.0336(10) Uani 1 1 d . . . . .
C64 C 0.5883(3) 0.8541(2) 0.7169(2) 0.0348(10) Uani 1 1 d . . . . .
C7 C 0.0655(3) 0.60971(19) 1.0632(2) 0.0282(9) Uani 1 1 d . . . . .
H7 H 0.048859 0.625777 1.110890 0.034 Uiso 1 1 calc R . . . .
C80 C 0.7282(3) 0.5644(2) 0.6836(2) 0.0365(10) Uani 1 1 d . . . . .
C34 C -0.2915(3) 0.9829(2) 0.8131(2) 0.0367(10) Uani 1 1 d . . . . .
H34 H -0.336329 0.995220 0.856990 0.044 Uiso 1 1 calc R . . . .
C95 C 0.6817(3) 0.6449(2) 0.1359(2) 0.0339(10) Uani 1 1 d . . . . .
C91 C 0.2300(3) 0.7746(2) 0.8652(2) 0.0346(10) Uani 1 1 d . . . . .
H91 H 0.188458 0.774974 0.908885 0.042 Uiso 1 1 calc R . . . .
C99 C 0.6881(3) 0.7580(2) 0.1365(2) 0.0361(10) Uani 1 1 d . . . . .
C90 C 0.2172(3) 0.8197(2) 0.8212(2) 0.0352(10) Uani 1 1 d . . . . .
H90 H 0.164551 0.858142 0.827881 0.042 Uiso 1 1 calc R . . . .
C28 C 0.1280(3) 0.8964(2) 1.2512(2) 0.0327(10) Uani 1 1 d . . . . .
H28 H 0.122184 0.942487 1.254561 0.039 Uiso 1 1 calc R . . . .
C112 C 0.4798(3) 0.8842(2) 0.3846(2) 0.0344(10) Uani 1 1 d . . . . .
H112 H 0.494440 0.867829 0.337441 0.041 Uiso 1 1 calc R . . . .
C36 C -0.2345(3) 1.0095(2) 0.7015(2) 0.0345(10) Uani 1 1 d . . . . .
H36 H -0.240674 1.039719 0.668528 0.041 Uiso 1 1 calc R . . . .
C119 C 0.4129(3) 0.6158(2) 0.3083(2) 0.0330(10) Uani 1 1 d . . . . .
H11D H 0.414784 0.649570 0.337660 0.040 Uiso 1 1 calc R . . . .
H11E H 0.472068 0.578425 0.292520 0.040 Uiso 1 1 calc R . . . .
C45 C -0.0489(3) 0.6344(2) 0.7200(2) 0.0370(10) Uani 1 1 d . . . . .
C14 C -0.1484(3) 0.8258(2) 1.3269(2) 0.0341(10) Uani 1 1 d . . . . .
C57 C 0.1542(3) 0.8440(2) 0.5870(2) 0.0329(10) Uani 1 1 d . . . . .
H57A H 0.092668 0.868167 0.619749 0.039 Uiso 1 1 calc R . . . .
H57B H 0.149323 0.828835 0.546237 0.039 Uiso 1 1 calc R . . . .
C110 C 0.5286(3) 0.7119(2) 0.4963(2) 0.0337(10) Uani 1 1 d . . . . .
H110 H 0.541064 0.674452 0.521291 0.040 Uiso 1 1 calc R . . . .
C59 C 0.2846(3) 0.7398(2) 0.5811(2) 0.0374(11) Uani 1 1 d . . . . .
H59 H 0.323944 0.742391 0.537535 0.045 Uiso 1 1 calc R . . . .
C10 C -0.0205(3) 0.8654(2) 1.0465(2) 0.0305(9) Uani 1 1 d . . . . .
H10 H -0.013621 0.862062 1.090583 0.037 Uiso 1 1 calc R . . . .
C4 C 0.0183(3) 0.7189(2) 0.9288(2) 0.0351(10) Uani 1 1 d . . . . .
H4 H 0.016728 0.712509 0.886045 0.042 Uiso 1 1 calc R . . . .
C29 C 0.1437(3) 0.8518(2) 1.2947(2) 0.0351(10) Uani 1 1 d . . . . .
H29 H 0.151664 0.860061 1.334463 0.042 Uiso 1 1 calc R . . . .
C49 C 0.0422(3) 0.6499(2) 0.6086(2) 0.0370(10) Uani 1 1 d . . . . .
C84 C 0.7354(3) 0.5963(3) 0.6179(2) 0.0448(12) Uani 1 1 d . . . . .
H84 H 0.690485 0.643556 0.629611 0.054 Uiso 1 1 calc R . . . .
C22 C -0.1064(3) 0.6504(2) 1.2505(2) 0.0394(11) Uani 1 1 d . U . . .
H22 H -0.089943 0.665819 1.204749 0.047 Uiso 0.505(9) 1 calc R . P A 1
H22A H -0.048554 0.649159 1.215011 0.047 Uiso 0.495(9) 1 calc R . P A 2
C61 C 0.2177(3) 0.6659(2) 0.7353(2) 0.0359(10) Uani 1 1 d . . . . .
H61A H 0.177088 0.695451 0.777419 0.043 Uiso 1 1 calc R . . . .
H61B H 0.277309 0.643989 0.738137 0.043 Uiso 1 1 calc R . . . .
C115 C 0.5466(3) 0.6304(2) 0.4055(2) 0.0338(10) Uani 1 1 d . . . . .
H115 H 0.541723 0.633746 0.360705 0.041 Uiso 1 1 calc R . . . .
C17 C -0.2205(3) 0.7244(3) 1.3569(2) 0.0453(12) Uani 1 1 d . . . . .
H17 H -0.245929 0.690198 1.367521 0.054 Uiso 1 1 calc R . . . .
C88 C 0.3076(3) 0.8375(2) 0.7054(2) 0.0364(10) Uani 1 1 d . . . . .
H88A H 0.248696 0.861023 0.701826 0.044 Uiso 1 1 calc R . . . .
H88B H 0.346442 0.805161 0.664815 0.044 Uiso 1 1 calc R . . . .
C30 C 0.1578(3) 0.7302(2) 1.3056(2) 0.0308(9) Uani 1 1 d . . . . .
H30A H 0.188921 0.732146 1.335717 0.037 Uiso 1 1 calc R . . . .
H30B H 0.196452 0.690146 1.272361 0.037 Uiso 1 1 calc R . . . .
C60 C 0.3019(3) 0.6919(2) 0.6211(2) 0.0389(11) Uani 1 1 d . . . . .
H60 H 0.356090 0.654041 0.611428 0.047 Uiso 1 1 calc R . . . .
C38 C -0.2196(3) 0.8736(2) 0.8526(2) 0.0380(11) Uani 1 1 d . . . . .
H38 H -0.169634 0.829568 0.831686 0.046 Uiso 1 1 calc R . . . .
C31 C 0.0700(3) 0.7221(2) 1.3460(2) 0.0413(11) Uani 1 1 d . . . . .
H31A H 0.040030 0.718372 1.316206 0.062 Uiso 1 1 calc GR . . . .
H31B H 0.031613 0.761524 1.379162 0.062 Uiso 1 1 calc GR . . . .
H31C H 0.081320 0.681080 1.368917 0.062 Uiso 1 1 calc GR . . . .
C35 C -0.2979(3) 1.0263(2) 0.7651(2) 0.0368(11) Uani 1 1 d . . . . .
H35 H -0.346701 1.068329 0.776173 0.044 Uiso 1 1 calc R . . . .
C121 C 0.3827(3) 0.6169(2) 0.2028(2) 0.0376(11) Uani 1 1 d . . . . .
H121 H 0.380934 0.572629 0.201897 0.045 Uiso 1 1 calc R . . . .
C69 C 0.6488(3) 0.8158(3) 0.6488(2) 0.0451(12) Uani 1 1 d . . . . .
H69 H 0.627454 0.778816 0.643463 0.054 Uiso 1 1 calc R . . . .
C41 C -0.0908(3) 0.9315(2) 0.6134(2) 0.0338(10) Uani 1 1 d . . . . .
H41 H -0.045436 0.885694 0.610820 0.041 Uiso 1 1 calc R . . . .
C123 C 0.3730(3) 0.7784(2) 0.1428(2) 0.0355(10) Uani 1 1 d . . . . .
H12D H 0.336341 0.819409 0.175058 0.043 Uiso 1 1 calc R . . . .
H12E H 0.342019 0.777819 0.112220 0.043 Uiso 1 1 calc R . . . .
C79 C 0.7954(3) 0.5031(2) 0.6829(3) 0.0464(12) Uani 1 1 d . . . . .
H79 H 0.843050 0.481557 0.641851 0.056 Uiso 1 1 calc R . . . .
C93 C 0.2998(3) 0.6264(2) 0.8881(2) 0.0391(11) Uani 1 1 d . . . . .
H93A H 0.296122 0.607729 0.848883 0.059 Uiso 1 1 calc GR . . . .
H93B H 0.239343 0.653853 0.918974 0.059 Uiso 1 1 calc GR . . . .
H93C H 0.327168 0.589313 0.910726 0.059 Uiso 1 1 calc GR . . . .
C109 C 0.5110(3) 0.7757(2) 0.5233(2) 0.0367(10) Uani 1 1 d . . . . .
H109 H 0.510305 0.781868 0.566848 0.044 Uiso 1 1 calc R . . . .
C114 C 0.5406(4) 0.9237(3) 0.3828(3) 0.0497(13) Uani 1 1 d . . . . .
H11F H 0.534391 0.958686 0.352163 0.075 Uiso 1 1 calc GR . . . .
H11G H 0.603218 0.892588 0.367204 0.075 Uiso 1 1 calc GR . . . .
H11H H 0.522951 0.944959 0.427751 0.075 Uiso 1 1 calc GR . . . .
C8 C 0.0133(3) 0.5645(2) 1.0630(3) 0.0479(13) Uani 1 1 d . . . . .
H8A H 0.032230 0.544649 1.017203 0.072 Uiso 1 1 calc GR . . . .
H8B H -0.051079 0.591403 1.080127 0.072 Uiso 1 1 calc GR . . . .
H8C H 0.025223 0.528224 1.091516 0.072 Uiso 1 1 calc GR . . . .
C77 C 0.7242(3) 0.5039(2) 0.8011(3) 0.0440(12) Uani 1 1 d . . . . .
H77 H 0.724082 0.483217 0.840851 0.053 Uiso 1 1 calc R . . . .
C98 C 0.7637(3) 0.7357(3) 0.0774(3) 0.0505(13) Uani 1 1 d . . . . .
H98 H 0.792401 0.766460 0.057126 0.061 Uiso 1 1 calc R . . . .
C122 C 0.3720(3) 0.6603(2) 0.1579(2) 0.0370(11) Uani 1 1 d . . . . .
H122 H 0.361829 0.653000 0.118860 0.044 Uiso 1 1 calc R . . . .
C26 C 0.1034(3) 0.8948(2) 1.1438(2) 0.0310(9) Uani 1 1 d . . . . .
H26A H 0.042771 0.930400 1.160159 0.037 Uiso 1 1 calc R . . . .
H26B H 0.104278 0.860543 1.113424 0.037 Uiso 1 1 calc R . . . .
C9 C 0.1656(3) 0.5686(2) 1.0347(2) 0.0378(10) Uani 1 1 d . . . . .
H9A H 0.184084 0.552350 0.987779 0.057 Uiso 1 1 calc GR . . . .
H9B H 0.178556 0.529851 1.060310 0.057 Uiso 1 1 calc GR . . . .
H9C H 0.198821 0.597086 1.037604 0.057 Uiso 1 1 calc GR . . . .
C100 C 0.6379(3) 0.5944(2) 0.1668(2) 0.0459(13) Uani 1 1 d . . . . .
H100 H 0.580828 0.619551 0.204975 0.055 Uiso 1 1 calc R . . . .
C72 C 0.4175(3) 0.8343(2) 0.8830(2) 0.0458(12) Uani 1 1 d . . . . .
H72 H 0.410843 0.797428 0.860052 0.055 Uiso 1 1 calc R . . . .
C50 C -0.1037(4) 0.6595(3) 0.7932(2) 0.0487(13) Uani 1 1 d . . . . .
H50 H -0.089074 0.698651 0.803431 0.058 Uiso 1 1 calc R . . . .
C48 C 0.0528(3) 0.5859(2) 0.5859(2) 0.0472(12) Uani 1 1 d . . . . .
H48 H 0.087879 0.568908 0.540290 0.057 Uiso 1 1 calc R . . . .
C67 C 0.4759(3) 0.9285(2) 0.8410(2) 0.0443(12) Uani 1 1 d . . . . .
H67 H 0.436904 0.954443 0.882842 0.053 Uiso 1 1 calc R . . . .
C81 C 0.5816(3) 0.5963(2) 0.8717(2) 0.0416(11) Uani 1 1 d . . . . .
H81 H 0.539297 0.639182 0.864005 0.050 Uiso 1 1 calc R . . . .
C78 C 0.7929(3) 0.4739(2) 0.7410(3) 0.0504(14) Uani 1 1 d . . . . .
H78 H 0.839126 0.432475 0.739671 0.060 Uiso 1 1 calc R . . . .
C120 C 0.3407(3) 0.5883(2) 0.3480(3) 0.0450(12) Uani 1 1 d . . . . .
H12F H 0.337192 0.556065 0.318677 0.068 Uiso 1 1 calc GR . . . .
H12G H 0.282761 0.625652 0.366544 0.068 Uiso 1 1 calc GR . . . .
H12H H 0.355605 0.565302 0.384622 0.068 Uiso 1 1 calc GR . . . .
C19 C -0.1122(3) 0.8829(2) 1.3079(2) 0.0426(12) Uani 1 1 d . . . . .
H19 H -0.047389 0.862024 1.278178 0.051 Uiso 1 1 calc R . . . .
C65 C 0.5861(3) 0.9190(2) 0.7316(3) 0.0458(12) Uani 1 1 d . . . . .
H65 H 0.623581 0.937963 0.698732 0.055 Uiso 1 1 calc R . . . .
C15 C -0.2206(3) 0.8314(3) 1.3863(2) 0.0480(13) Uani 1 1 d . . . . .
H15 H -0.245602 0.870445 1.417356 0.058 Uiso 1 1 calc R . . . .
C11 C -0.1171(3) 0.9103(3) 1.0592(3) 0.0537(14) Uani 1 1 d . . . . .
H11A H -0.157982 0.890526 1.090511 0.081 Uiso 1 1 calc GR . . . .
H11B H -0.126464 0.913799 1.016948 0.081 Uiso 1 1 calc GR . . . .
H11C H -0.129043 0.955439 1.078461 0.081 Uiso 1 1 calc GR . . . .
C12 C 0.0450(3) 0.8972(2) 1.0019(2) 0.0424(11) Uani 1 1 d . . . . .
H12A H 0.106617 0.867439 0.994386 0.064 Uiso 1 1 calc GR . . . .
H12B H 0.032584 0.941228 1.023721 0.064 Uiso 1 1 calc GR . . . .
H12C H 0.037759 0.903245 0.958841 0.064 Uiso 1 1 calc GR . . . .
C103 C 0.6508(3) 0.8302(2) 0.1683(3) 0.0497(13) Uani 1 1 d . . . . .
H103 H 0.587569 0.839618 0.199873 0.060 Uiso 1 1 calc R . . . .
C113 C 0.3817(3) 0.9310(2) 0.4129(2) 0.0439(12) Uani 1 1 d . . . . .
H11I H 0.343509 0.905592 0.413307 0.066 Uiso 1 1 calc GR . . . .
H11J H 0.372447 0.968224 0.384912 0.066 Uiso 1 1 calc GR . . . .
H11K H 0.365932 0.949474 0.458613 0.066 Uiso 1 1 calc GR . . . .
C66 C 0.5308(3) 0.9552(2) 0.7925(3) 0.0477(13) Uani 1 1 d . . . . .
H66 H 0.530239 0.998991 0.801554 0.057 Uiso 1 1 calc R . . . .
C117 C 0.4771(4) 0.6019(2) 0.4495(3) 0.0526(14) Uani 1 1 d . . . . .
H11L H 0.416926 0.632745 0.454492 0.079 Uiso 1 1 calc GR . . . .
H11M H 0.481221 0.596970 0.493596 0.079 Uiso 1 1 calc GR . . . .
H11N H 0.488577 0.557557 0.428695 0.079 Uiso 1 1 calc GR . . . .
C43 C -0.0420(3) 0.9816(2) 0.5959(2) 0.0428(11) Uani 1 1 d . . . . .
H43A H -0.018294 0.984809 0.630121 0.064 Uiso 1 1 calc GR . . . .
H43B H -0.083961 1.026264 0.593924 0.064 Uiso 1 1 calc GR . . . .
H43C H 0.007670 0.966037 0.552280 0.064 Uiso 1 1 calc GR . . . .
C16 C -0.2564(3) 0.7814(3) 1.4005(2) 0.0532(14) Uani 1 1 d . . . . .
H16 H -0.306282 0.786435 1.440961 0.064 Uiso 1 1 calc R . . . .
C96 C 0.7564(3) 0.6261(3) 0.0764(2) 0.0472(12) Uani 1 1 d . . . . .
H96 H 0.779391 0.581462 0.055055 0.057 Uiso 1 1 calc R . . . .
C47 C 0.0127(4) 0.5469(3) 0.6292(3) 0.0577(15) Uani 1 1 d . . . . .
H47 H 0.020036 0.503157 0.613243 0.069 Uiso 1 1 calc R . . . .
C58 C 0.2047(3) 0.8919(2) 0.5696(2) 0.0431(11) Uani 1 1 d . . . . .
H58A H 0.206331 0.909360 0.610357 0.065 Uiso 1 1 calc GR . . . .
H58B H 0.174531 0.929675 0.549079 0.065 Uiso 1 1 calc GR . . . .
H58C H 0.266193 0.867894 0.538087 0.065 Uiso 1 1 calc GR . . . .
C70 C 0.6441(4) 0.8597(3) 0.5916(3) 0.0688(17) Uani 1 1 d . . . . .
H70A H 0.581461 0.880698 0.595635 0.103 Uiso 1 1 calc GR . . . .
H70B H 0.679828 0.831532 0.548712 0.103 Uiso 1 1 calc GR . . . .
H70C H 0.667837 0.895138 0.593748 0.103 Uiso 1 1 calc GR . . . .
C46 C -0.0377(4) 0.5708(3) 0.6949(3) 0.0524(14) Uani 1 1 d . . . . .
H46 H -0.065558 0.543632 0.724037 0.063 Uiso 1 1 calc R . . . .
C40 C -0.2017(4) 0.9007(3) 0.9084(2) 0.0540(14) Uani 1 1 d . . . . .
H40A H -0.198170 0.867630 0.941149 0.081 Uiso 1 1 calc GR . . . .
H40B H -0.250534 0.943387 0.930460 0.081 Uiso 1 1 calc GR . . . .
H40C H -0.144745 0.908373 0.889533 0.081 Uiso 1 1 calc GR . . . .
C85 C 0.7118(4) 0.5599(3) 0.5728(3) 0.0588(15) Uani 1 1 d . . . . .
H85A H 0.649842 0.561822 0.595526 0.088 Uiso 1 1 calc GR . . . .
H85B H 0.752621 0.512575 0.562196 0.088 Uiso 1 1 calc GR . . . .
H85C H 0.717459 0.581680 0.531419 0.088 Uiso 1 1 calc GR . . . .
C27 C 0.1720(3) 0.9259(2) 1.1057(2) 0.0447(12) Uani 1 1 d . . . . .
H27A H 0.231891 0.890543 1.088417 0.067 Uiso 1 1 calc GR . . . .
H27B H 0.171045 0.960038 1.135723 0.067 Uiso 1 1 calc GR . . . .
H27C H 0.157553 0.947296 1.068395 0.067 Uiso 1 1 calc GR . . . .
C124 C 0.4633(3) 0.7823(3) 0.1028(2) 0.0499(13) Uani 1 1 d . . . . .
H12I H 0.455479 0.823528 0.079921 0.075 Uiso 1 1 calc GR . . . .
H12J H 0.499233 0.742660 0.069568 0.075 Uiso 1 1 calc GR . . . .
H12K H 0.494169 0.783364 0.132755 0.075 Uiso 1 1 calc GR . . . .
C101 C 0.6962(4) 0.5392(3) 0.1950(3) 0.0652(16) Uani 1 1 d . . . . .
H10A H 0.664094 0.509234 0.216728 0.098 Uiso 1 1 calc GR . . . .
H10B H 0.709649 0.559953 0.227731 0.098 Uiso 1 1 calc GR . . . .
H10C H 0.752355 0.512973 0.158522 0.098 Uiso 1 1 calc GR . . . .
C39 C -0.3079(4) 0.8599(3) 0.8818(3) 0.0694(18) Uani 1 1 d . . . . .
H39A H -0.302078 0.824299 0.911833 0.104 Uiso 1 1 calc GR . . . .
H39B H -0.320792 0.845195 0.845275 0.104 Uiso 1 1 calc GR . . . .
H39C H -0.357021 0.901361 0.906738 0.104 Uiso 1 1 calc GR . . . .
C89 C 0.3491(4) 0.8885(3) 0.7076(3) 0.0586(15) Uani 1 1 d . . . . .
H89A H 0.352509 0.913981 0.668474 0.088 Uiso 1 1 calc GR . . . .
H89B H 0.409650 0.865281 0.707176 0.088 Uiso 1 1 calc GR . . . .
H89C H 0.312265 0.919761 0.748474 0.088 Uiso 1 1 calc GR . . . .
C105 C 0.7035(4) 0.8381(3) 0.2092(3) 0.0627(15) Uani 1 1 d . . . . .
H10D H 0.698411 0.807979 0.244775 0.094 Uiso 1 1 calc GR . . . .
H10E H 0.679220 0.885062 0.229043 0.094 Uiso 1 1 calc GR . . . .
H10F H 0.766859 0.826270 0.179991 0.094 Uiso 1 1 calc GR . . . .
C86 C 0.8279(4) 0.6011(3) 0.5802(3) 0.0737(19) Uani 1 1 d . . . . .
H86A H 0.826344 0.627278 0.542059 0.111 Uiso 1 1 calc GR . . . .
H86B H 0.872953 0.555464 0.564011 0.111 Uiso 1 1 calc GR . . . .
H86C H 0.843524 0.623485 0.610305 0.111 Uiso 1 1 calc GR . . . .
C97 C 0.7977(3) 0.6710(3) 0.0478(2) 0.0507(13) Uani 1 1 d . . . . .
H97 H 0.849668 0.657071 0.007605 0.061 Uiso 1 1 calc R . . . .
C62 C 0.1820(4) 0.6125(3) 0.7284(3) 0.0749(19) Uani 1 1 d . . . . .
H62A H 0.177363 0.586307 0.767085 0.112 Uiso 1 1 calc GR . . . .
H62B H 0.222720 0.582305 0.687375 0.112 Uiso 1 1 calc GR . . . .
H62C H 0.122445 0.633887 0.726383 0.112 Uiso 1 1 calc GR . . . .
C53 C 0.0835(4) 0.6945(3) 0.5609(2) 0.0552(15) Uani 1 1 d . . . . .
H53 H 0.093090 0.726249 0.588036 0.066 Uiso 1 1 calc R . . . .
C42 C -0.1322(4) 0.9285(3) 0.5621(3) 0.0575(14) Uani 1 1 d . . . . .
H42A H -0.162582 0.895760 0.573458 0.086 Uiso 1 1 calc GR . . . .
H42B H -0.084699 0.914601 0.517415 0.086 Uiso 1 1 calc GR . . . .
H42C H -0.175714 0.973330 0.562684 0.086 Uiso 1 1 calc GR . . . .
C21 C -0.1595(4) 0.9294(3) 1.2681(3) 0.0683(17) Uani 1 1 d . . . . .
H21A H -0.152913 0.903226 1.228784 0.103 Uiso 1 1 calc GR . . . .
H21B H -0.132956 0.964160 1.253508 0.103 Uiso 1 1 calc GR . . . .
H21C H -0.223337 0.951042 1.295927 0.103 Uiso 1 1 calc GR . . . .
C83 C 0.5277(4) 0.5510(3) 0.9028(3) 0.0585(15) Uani 1 1 d . . . . .
H83A H 0.503731 0.540292 0.871390 0.088 Uiso 1 1 calc GR . . . .
H83B H 0.477959 0.574774 0.944338 0.088 Uiso 1 1 calc GR . . . .
H83C H 0.566834 0.509084 0.912460 0.088 Uiso 1 1 calc GR . . . .
C71 C 0.7454(4) 0.7823(3) 0.6442(3) 0.0700(17) Uani 1 1 d . . . . .
H71A H 0.747591 0.750391 0.678070 0.105 Uiso 1 1 calc GR . . . .
H71B H 0.767353 0.817027 0.652071 0.105 Uiso 1 1 calc GR . . . .
H71C H 0.783216 0.758009 0.599639 0.105 Uiso 1 1 calc GR . . . .
C116 C 0.6410(4) 0.5827(3) 0.3953(3) 0.0656(16) Uani 1 1 d . . . . .
H11O H 0.651067 0.538074 0.375867 0.098 Uiso 1 1 calc GR . . . .
H11P H 0.647946 0.578416 0.438462 0.098 Uiso 1 1 calc GR . . . .
H11Q H 0.684767 0.600680 0.364973 0.098 Uiso 1 1 calc GR . . . .
C74 C 0.4646(5) 0.8014(3) 0.9301(3) 0.079(2) Uani 1 1 d . . . . .
H74A H 0.429543 0.777723 0.961515 0.118 Uiso 1 1 calc GR . . . .
H74B H 0.469966 0.836373 0.955054 0.118 Uiso 1 1 calc GR . . . .
H74C H 0.524637 0.768978 0.903979 0.118 Uiso 1 1 calc GR . . . .
C102 C 0.6133(3) 0.5635(3) 0.1172(3) 0.0590(15) Uani 1 1 d . . . . .
H10G H 0.575855 0.537509 0.140616 0.088 Uiso 1 1 calc GR . . . .
H10H H 0.668190 0.533525 0.082117 0.088 Uiso 1 1 calc GR . . . .
H10I H 0.580010 0.599709 0.096912 0.088 Uiso 1 1 calc GR . . . .
C104 C 0.6484(4) 0.8812(3) 0.1160(3) 0.078(2) Uani 1 1 d . . . . .
H10J H 0.612159 0.875627 0.091994 0.116 Uiso 1 1 calc GR . . . .
H10K H 0.709625 0.873215 0.084178 0.116 Uiso 1 1 calc GR . . . .
H10L H 0.621785 0.927308 0.138462 0.116 Uiso 1 1 calc GR . . . .
C73 C 0.3242(4) 0.8847(3) 0.9205(3) 0.0756(19) Uani 1 1 d . . . . .
H73A H 0.296265 0.904430 0.888640 0.113 Uiso 1 1 calc GR . . . .
H73B H 0.327986 0.920686 0.945279 0.113 Uiso 1 1 calc GR . . . .
H73C H 0.287957 0.861792 0.951863 0.113 Uiso 1 1 calc GR . . . .
C82 C 0.6177(4) 0.6148(3) 0.9207(3) 0.0677(17) Uani 1 1 d . . . . .
H82A H 0.567568 0.637762 0.962394 0.102 Uiso 1 1 calc GR . . . .
H82B H 0.650417 0.645036 0.900945 0.102 Uiso 1 1 calc GR . . . .
H82C H 0.658393 0.573609 0.930221 0.102 Uiso 1 1 calc GR . . . .
C20 C -0.1176(4) 0.9229(3) 1.3677(3) 0.0683(18) Uani 1 1 d . . . . .
H20A H -0.094102 0.891398 1.396467 0.102 Uiso 1 1 calc GR . . . .
H20B H -0.180234 0.951141 1.393204 0.102 Uiso 1 1 calc GR . . . .
H20C H -0.081748 0.951728 1.351796 0.102 Uiso 1 1 calc GR . . . .
C52 C -0.0812(6) 0.6065(3) 0.8399(3) 0.108(3) Uani 1 1 d . . . . .
H52A H -0.116000 0.626221 0.886433 0.162 Uiso 1 1 calc GR . . . .
H52B H -0.016917 0.591480 0.831236 0.162 Uiso 1 1 calc GR . . . .
H52C H -0.096072 0.567655 0.831888 0.162 Uiso 1 1 calc GR . . . .
C51 C -0.2027(4) 0.6853(4) 0.8062(3) 0.099(3) Uani 1 1 d . . . . .
H51A H -0.237308 0.701367 0.853706 0.148 Uiso 1 1 calc GR . . . .
H51B H -0.218608 0.648738 0.794026 0.148 Uiso 1 1 calc GR . . . .
H51C H -0.216371 0.722753 0.779227 0.148 Uiso 1 1 calc GR . . . .
C54 C 0.0178(5) 0.7373(3) 0.5300(3) 0.085(2) Uani 1 1 d . . . . .
H54A H -0.038962 0.764075 0.565623 0.128 Uiso 1 1 calc GR . . . .
H54B H 0.006673 0.707534 0.503135 0.128 Uiso 1 1 calc GR . . . .
H54C H 0.043443 0.767670 0.501352 0.128 Uiso 1 1 calc GR . . . .
C55 C 0.1740(5) 0.6546(4) 0.5078(3) 0.108(3) Uani 1 1 d . . . . .
H55A H 0.213624 0.626457 0.529168 0.162 Uiso 1 1 calc GR . . . .
H55B H 0.200655 0.685904 0.481859 0.162 Uiso 1 1 calc GR . . . .
H55C H 0.166183 0.625588 0.477921 0.162 Uiso 1 1 calc GR . . . .
C23 C -0.0213(6) 0.6037(4) 1.2509(5) 0.043(3) Uani 0.505(9) 1 d . U P A 1
H23A H 0.003078 0.565770 1.216261 0.065 Uiso 0.505(9) 1 calc GR . P A 1
H23B H -0.030849 0.586474 1.294771 0.065 Uiso 0.505(9) 1 calc GR . P A 1
H23C H 0.021075 0.627271 1.242002 0.065 Uiso 0.505(9) 1 calc GR . P A 1
C24A C -0.1632(7) 0.6466(6) 1.2202(6) 0.047(3) Uani 0.495(9) 1 d . U P A 2
H24A H -0.137334 0.602824 1.193137 0.071 Uiso 0.495(9) 1 calc GR . P A 2
H24B H -0.170913 0.683151 1.191393 0.071 Uiso 0.495(9) 1 calc GR . P A 2
H24C H -0.221720 0.650992 1.254560 0.071 Uiso 0.495(9) 1 calc GR . P A 2
C23A C -0.0853(8) 0.5899(5) 1.2963(6) 0.058(3) Uani 0.495(9) 1 d . U P A 2
H23D H -0.046834 0.547343 1.267557 0.087 Uiso 0.495(9) 1 calc GR . P A 2
H23E H -0.141746 0.585689 1.326265 0.087 Uiso 0.495(9) 1 calc GR . P A 2
H23F H -0.054615 0.599912 1.322840 0.087 Uiso 0.495(9) 1 calc GR . P A 2
C24 C -0.1706(7) 0.6119(6) 1.2514(6) 0.050(3) Uani 0.505(9) 1 d . U P A 1
H24D H -0.138835 0.574765 1.215258 0.074 Uiso 0.505(9) 1 calc GR . P A 1
H24E H -0.223772 0.643449 1.244912 0.074 Uiso 0.505(9) 1 calc GR . P A 1
H24F H -0.189133 0.593704 1.294471 0.074 Uiso 0.505(9) 1 calc GR . P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 Br1 2.7235(5) . ?
Sn1 N1 2.198(3) . ?
Sn1 N3 2.523(3) . ?
Sn1 C25 2.287(4) . ?
Sn3 Br3 2.7257(5) . ?
Sn3 N11 2.455(3) . ?
Sn3 N13 2.228(3) . ?
Sn3 C87 2.283(4) . ?
Sn2 Br2 2.7190(5) . ?
Sn2 N8 2.475(3) . ?
Sn2 N6 2.208(3) . ?
Sn2 C56 2.299(4) . ?
Sn4 Br4 2.7256(5) . ?
Sn4 N18 2.205(3) . ?
Sn4 N16 2.482(3) . ?
Sn4 C118 2.294(4) . ?
N1 N2 1.325(4) . ?
N1 C1 1.432(5) . ?
N18 N17 1.321(4) . ?
N18 C106 1.436(5) . ?
N15 C87 1.352(5) . ?
N15 C92 1.474(5) . ?
N15 C91 1.380(5) . ?
N17 N16 1.286(4) . ?
N2 N3 1.280(4) . ?
N11 N12 1.287(4) . ?
N11 C63 1.443(5) . ?
N8 N7 1.281(4) . ?
N8 C44 1.440(5) . ?
N3 C13 1.438(5) . ?
N12 N13 1.327(4) . ?
N16 C94 1.437(5) . ?
N7 N6 1.325(4) . ?
N6 C32 1.433(5) . ?
N5 C25 1.350(5) . ?
N5 C29 1.377(5) . ?
N5 C30 1.474(5) . ?
N19 C118 1.343(5) . ?
N19 C119 1.464(5) . ?
N19 C121 1.372(5) . ?
N9 C56 1.340(5) . ?
N9 C57 1.464(5) . ?
N9 C59 1.382(5) . ?
N13 C75 1.436(5) . ?
N4 C25 1.355(5) . ?
N4 C28 1.377(5) . ?
N4 C26 1.464(5) . ?
N20 C118 1.353(5) . ?
N20 C123 1.468(5) . ?
N20 C122 1.385(5) . ?
N14 C87 1.355(5) . ?
N14 C90 1.379(5) . ?
N14 C88 1.472(5) . ?
N10 C56 1.356(5) . ?
N10 C61 1.469(5) . ?
N10 C60 1.380(5) . ?
C1 C2 1.409(5) . ?
C1 C6 1.404(5) . ?
C32 C33 1.407(6) . ?
C32 C37 1.405(5) . ?
C13 C18 1.392(6) . ?
C13 C14 1.396(6) . ?
C2 C3 1.397(5) . ?
C2 C7 1.521(5) . ?
C63 C68 1.390(6) . ?
C63 C64 1.391(6) . ?
C106 C111 1.400(5) . ?
C106 C107 1.410(5) . ?
C75 C76 1.406(6) . ?
C75 C80 1.397(6) . ?
C94 C95 1.394(6) . ?
C94 C99 1.404(6) . ?
C44 C45 1.390(6) . ?
C44 C49 1.392(6) . ?
C6 C5 1.394(5) . ?
C6 C10 1.526(5) . ?
C33 C34 1.390(6) . ?
C33 C38 1.515(6) . ?
C76 C77 1.394(6) . ?
C76 C81 1.514(7) . ?
C92 H92A 0.9900 . ?
C92 H92B 0.9900 . ?
C92 C93 1.501(6) . ?
C18 C22 1.521(6) . ?
C18 C17 1.402(6) . ?
C3 H3 0.9500 . ?
C3 C4 1.376(6) . ?
C37 C36 1.399(6) . ?
C37 C41 1.513(6) . ?
C111 C110 1.388(6) . ?
C111 C115 1.526(6) . ?
C108 H108 0.9500 . ?
C108 C107 1.399(5) . ?
C108 C109 1.378(6) . ?
C5 H5 0.9500 . ?
C5 C4 1.368(6) . ?
C107 C112 1.519(6) . ?
C68 C72 1.522(6) . ?
C68 C67 1.393(6) . ?
C64 C69 1.509(6) . ?
C64 C65 1.407(6) . ?
C7 H7 1.0000 . ?
C7 C8 1.524(6) . ?
C7 C9 1.521(6) . ?
C80 C84 1.532(6) . ?
C80 C79 1.401(6) . ?
C34 H34 0.9500 . ?
C34 C35 1.369(6) . ?
C95 C100 1.515(6) . ?
C95 C96 1.389(6) . ?
C91 H91 0.9500 . ?
C91 C90 1.345(6) . ?
C99 C98 1.392(6) . ?
C99 C103 1.515(6) . ?
C90 H90 0.9500 . ?
C28 H28 0.9500 . ?
C28 C29 1.338(6) . ?
C112 H112 1.0000 . ?
C112 C114 1.538(6) . ?
C112 C113 1.524(6) . ?
C36 H36 0.9500 . ?
C36 C35 1.368(6) . ?
C119 H11D 0.9900 . ?
C119 H11E 0.9900 . ?
C119 C120 1.516(6) . ?
C45 C50 1.514(6) . ?
C45 C46 1.393(6) . ?
C14 C19 1.523(6) . ?
C14 C15 1.392(6) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C57 C58 1.506(6) . ?
C110 H110 0.9500 . ?
C110 C109 1.379(6) . ?
C59 H59 0.9500 . ?
C59 C60 1.334(6) . ?
C10 H10 1.0000 . ?
C10 C11 1.521(6) . ?
C10 C12 1.527(6) . ?
C4 H4 0.9500 . ?
C29 H29 0.9500 . ?
C49 C48 1.387(6) . ?
C49 C53 1.521(6) . ?
C84 H84 1.0000 . ?
C84 C85 1.506(7) . ?
C84 C86 1.533(7) . ?
C22 H22 1.0000 . ?
C22 H22A 1.0000 . ?
C22 C23 1.455(10) . ?
C22 C24A 1.382(11) . ?
C22 C23A 1.613(11) . ?
C22 C24 1.575(10) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C61 C62 1.496(7) . ?
C115 H115 1.0000 . ?
C115 C117 1.522(6) . ?
C115 C116 1.520(6) . ?
C17 H17 0.9500 . ?
C17 C16 1.365(7) . ?
C88 H88A 0.9900 . ?
C88 H88B 0.9900 . ?
C88 C89 1.496(6) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.505(6) . ?
C60 H60 0.9500 . ?
C38 H38 1.0000 . ?
C38 C40 1.523(7) . ?
C38 C39 1.540(6) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C35 H35 0.9500 . ?
C121 H121 0.9500 . ?
C121 C122 1.331(6) . ?
C69 H69 1.0000 . ?
C69 C70 1.530(7) . ?
C69 C71 1.525(7) . ?
C41 H41 1.0000 . ?
C41 C43 1.527(6) . ?
C41 C42 1.532(6) . ?
C123 H12D 0.9900 . ?
C123 H12E 0.9900 . ?
C123 C124 1.503(6) . ?
C79 H79 0.9500 . ?
C79 C78 1.371(7) . ?
C93 H93A 0.9800 . ?
C93 H93B 0.9800 . ?
C93 H93C 0.9800 . ?
C109 H109 0.9500 . ?
C114 H11F 0.9800 . ?
C114 H11G 0.9800 . ?
C114 H11H 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C77 H77 0.9500 . ?
C77 C78 1.378(7) . ?
C98 H98 0.9500 . ?
C98 C97 1.365(7) . ?
C122 H122 0.9500 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.512(6) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C100 H100 1.0000 . ?
C100 C101 1.523(7) . ?
C100 C102 1.527(7) . ?
C72 H72 1.0000 . ?
C72 C74 1.528(7) . ?
C72 C73 1.511(7) . ?
C50 H50 1.0000 . ?
C50 C52 1.526(7) . ?
C50 C51 1.509(8) . ?
C48 H48 0.9500 . ?
C48 C47 1.379(7) . ?
C67 H67 0.9500 . ?
C67 C66 1.383(7) . ?
C81 H81 1.0000 . ?
C81 C83 1.530(6) . ?
C81 C82 1.531(6) . ?
C78 H78 0.9500 . ?
C120 H12F 0.9800 . ?
C120 H12G 0.9800 . ?
C120 H12H 0.9800 . ?
C19 H19 1.0000 . ?
C19 C21 1.504(7) . ?
C19 C20 1.528(6) . ?
C65 H65 0.9500 . ?
C65 C66 1.369(7) . ?
C15 H15 0.9500 . ?
C15 C16 1.373(7) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C103 H103 1.0000 . ?
C103 C105 1.526(7) . ?
C103 C104 1.537(7) . ?
C113 H11I 0.9800 . ?
C113 H11J 0.9800 . ?
C113 H11K 0.9800 . ?
C66 H66 0.9500 . ?
C117 H11L 0.9800 . ?
C117 H11M 0.9800 . ?
C117 H11N 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C16 H16 0.9500 . ?
C96 H96 0.9500 . ?
C96 C97 1.378(7) . ?
C47 H47 0.9500 . ?
C47 C46 1.367(7) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?
C46 H46 0.9500 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C85 H85A 0.9800 . ?
C85 H85B 0.9800 . ?
C85 H85C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C124 H12I 0.9800 . ?
C124 H12J 0.9800 . ?
C124 H12K 0.9800 . ?
C101 H10A 0.9800 . ?
C101 H10B 0.9800 . ?
C101 H10C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C89 H89A 0.9800 . ?
C89 H89B 0.9800 . ?
C89 H89C 0.9800 . ?
C105 H10D 0.9800 . ?
C105 H10E 0.9800 . ?
C105 H10F 0.9800 . ?
C86 H86A 0.9800 . ?
C86 H86B 0.9800 . ?
C86 H86C 0.9800 . ?
C97 H97 0.9500 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C53 H53 1.0000 . ?
C53 C54 1.530(8) . ?
C53 C55 1.515(8) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C83 H83A 0.9800 . ?
C83 H83B 0.9800 . ?
C83 H83C 0.9800 . ?
C71 H71A 0.9800 . ?
C71 H71B 0.9800 . ?
C71 H71C 0.9800 . ?
C116 H11O 0.9800 . ?
C116 H11P 0.9800 . ?
C116 H11Q 0.9800 . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C102 H10G 0.9800 . ?
C102 H10H 0.9800 . ?
C102 H10I 0.9800 . ?
C104 H10J 0.9800 . ?
C104 H10K 0.9800 . ?
C104 H10L 0.9800 . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24A H24A 0.9800 . ?
C24A H24B 0.9800 . ?
C24A H24C 0.9800 . ?
C23A H23D 0.9800 . ?
C23A H23E 0.9800 . ?
C23A H23F 0.9800 . ?
C24 H24D 0.9800 . ?
C24 H24E 0.9800 . ?
C24 H24F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Sn1 Br1 86.61(8) . . ?
N1 Sn1 N3 53.14(10) . . ?
N1 Sn1 C25 105.76(12) . . ?
N3 Sn1 Br1 133.41(7) . . ?
C25 Sn1 Br1 88.55(10) . . ?
C25 Sn1 N3 82.26(11) . . ?
N11 Sn3 Br3 136.14(7) . . ?
N13 Sn3 Br3 88.63(8) . . ?
N13 Sn3 N11 53.77(11) . . ?
N13 Sn3 C87 103.99(13) . . ?
C87 Sn3 Br3 88.86(9) . . ?
C87 Sn3 N11 80.81(12) . . ?
N8 Sn2 Br2 135.07(7) . . ?
N6 Sn2 Br2 87.53(8) . . ?
N6 Sn2 N8 53.47(11) . . ?
N6 Sn2 C56 105.25(13) . . ?
C56 Sn2 Br2 89.81(10) . . ?
C56 Sn2 N8 81.54(12) . . ?
N18 Sn4 Br4 87.06(8) . . ?
N18 Sn4 N16 53.41(11) . . ?
N18 Sn4 C118 105.75(12) . . ?
N16 Sn4 Br4 133.91(7) . . ?
C118 Sn4 Br4 88.87(10) . . ?
C118 Sn4 N16 81.64(12) . . ?
N2 N1 Sn1 104.4(2) . . ?
N2 N1 C1 114.8(3) . . ?
C1 N1 Sn1 134.7(2) . . ?
N17 N18 Sn4 104.0(2) . . ?
N17 N18 C106 116.0(3) . . ?
C106 N18 Sn4 134.8(2) . . ?
C87 N15 C92 125.3(3) . . ?
C87 N15 C91 111.3(3) . . ?
C91 N15 C92 123.4(3) . . ?
N16 N17 N18 108.9(3) . . ?
N3 N2 N1 109.8(3) . . ?
N12 N11 Sn3 92.9(2) . . ?
N12 N11 C63 115.3(3) . . ?
C63 N11 Sn3 148.7(2) . . ?
N7 N8 Sn2 92.1(2) . . ?
N7 N8 C44 115.4(3) . . ?
C44 N8 Sn2 150.8(3) . . ?
N2 N3 Sn1 90.3(2) . . ?
N2 N3 C13 114.6(3) . . ?
C13 N3 Sn1 149.7(2) . . ?
N11 N12 N13 108.9(3) . . ?
N17 N16 Sn4 91.8(2) . . ?
N17 N16 C94 115.2(3) . . ?
C94 N16 Sn4 150.6(2) . . ?
N8 N7 N6 108.8(3) . . ?
N7 N6 Sn2 103.5(2) . . ?
N7 N6 C32 116.1(3) . . ?
C32 N6 Sn2 133.2(3) . . ?
C25 N5 C29 111.0(3) . . ?
C25 N5 C30 125.3(3) . . ?
C29 N5 C30 123.7(3) . . ?
C118 N19 C119 124.7(3) . . ?
C118 N19 C121 110.5(4) . . ?
C121 N19 C119 124.8(4) . . ?
C56 N9 C57 126.0(3) . . ?
C56 N9 C59 110.7(4) . . ?
C59 N9 C57 123.3(3) . . ?
N12 N13 Sn3 102.5(2) . . ?
N12 N13 C75 114.8(3) . . ?
C75 N13 Sn3 136.8(3) . . ?
C25 N4 C28 110.4(3) . . ?
C25 N4 C26 125.6(3) . . ?
C28 N4 C26 124.0(3) . . ?
C118 N20 C123 125.8(3) . . ?
C118 N20 C122 110.4(4) . . ?
C122 N20 C123 123.8(4) . . ?
C87 N14 C90 110.7(3) . . ?
C87 N14 C88 125.8(3) . . ?
C90 N14 C88 123.4(3) . . ?
C56 N10 C61 126.0(3) . . ?
C56 N10 C60 110.1(3) . . ?
C60 N10 C61 123.8(3) . . ?
C2 C1 N1 119.4(3) . . ?
C6 C1 N1 119.5(3) . . ?
C6 C1 C2 121.0(3) . . ?
C33 C32 N6 119.4(3) . . ?
C37 C32 N6 119.6(4) . . ?
C37 C32 C33 120.9(4) . . ?
C18 C13 N3 119.8(3) . . ?
C18 C13 C14 122.0(4) . . ?
C14 C13 N3 118.1(3) . . ?
C1 C2 C7 123.1(3) . . ?
C3 C2 C1 117.9(4) . . ?
C3 C2 C7 119.0(4) . . ?
C68 C63 N11 118.7(3) . . ?
C68 C63 C64 122.4(4) . . ?
C64 C63 N11 118.7(4) . . ?
C111 C106 N18 120.1(3) . . ?
C111 C106 C107 121.1(3) . . ?
C107 C106 N18 118.8(3) . . ?
C76 C75 N13 119.5(4) . . ?
C80 C75 N13 119.0(4) . . ?
C80 C75 C76 121.6(4) . . ?
C95 C94 N16 118.8(4) . . ?
C95 C94 C99 121.1(4) . . ?
C99 C94 N16 119.9(4) . . ?
N19 C118 Sn4 135.2(3) . . ?
N19 C118 N20 105.0(3) . . ?
N20 C118 Sn4 119.7(3) . . ?
C45 C44 N8 120.3(4) . . ?
C45 C44 C49 121.5(4) . . ?
C49 C44 N8 117.9(3) . . ?
N5 C25 Sn1 119.7(3) . . ?
N5 C25 N4 104.7(3) . . ?
N4 C25 Sn1 135.6(3) . . ?
C1 C6 C10 121.6(3) . . ?
C5 C6 C1 118.3(4) . . ?
C5 C6 C10 120.1(4) . . ?
C32 C33 C38 122.8(4) . . ?
C34 C33 C32 118.3(4) . . ?
C34 C33 C38 118.9(4) . . ?
N15 C87 Sn3 133.0(3) . . ?
N15 C87 N14 104.4(3) . . ?
N14 C87 Sn3 122.6(3) . . ?
N9 C56 Sn2 135.6(3) . . ?
N9 C56 N10 105.2(3) . . ?
N10 C56 Sn2 119.2(3) . . ?
C75 C76 C81 122.9(4) . . ?
C77 C76 C75 117.9(4) . . ?
C77 C76 C81 119.2(4) . . ?
N15 C92 H92A 109.4 . . ?
N15 C92 H92B 109.4 . . ?
N15 C92 C93 111.2(3) . . ?
H92A C92 H92B 108.0 . . ?
C93 C92 H92A 109.4 . . ?
C93 C92 H92B 109.4 . . ?
C13 C18 C22 122.5(4) . . ?
C13 C18 C17 117.5(4) . . ?
C17 C18 C22 119.9(4) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 C2 121.1(4) . . ?
C4 C3 H3 119.5 . . ?
C32 C37 C41 121.8(4) . . ?
C36 C37 C32 117.9(4) . . ?
C36 C37 C41 120.3(4) . . ?
C106 C111 C115 121.8(4) . . ?
C110 C111 C106 118.5(4) . . ?
C110 C111 C115 119.7(4) . . ?
C107 C108 H108 119.6 . . ?
C109 C108 H108 119.6 . . ?
C109 C108 C107 120.9(4) . . ?
C6 C5 H5 119.4 . . ?
C4 C5 C6 121.1(4) . . ?
C4 C5 H5 119.4 . . ?
C106 C107 C112 123.2(3) . . ?
C108 C107 C106 118.0(4) . . ?
C108 C107 C112 118.8(4) . . ?
C63 C68 C72 121.3(4) . . ?
C63 C68 C67 118.1(4) . . ?
C67 C68 C72 120.5(4) . . ?
C63 C64 C69 122.8(4) . . ?
C63 C64 C65 117.4(4) . . ?
C65 C64 C69 119.8(4) . . ?
C2 C7 H7 107.6 . . ?
C2 C7 C8 112.8(3) . . ?
C8 C7 H7 107.6 . . ?
C9 C7 C2 111.4(3) . . ?
C9 C7 H7 107.6 . . ?
C9 C7 C8 109.7(4) . . ?
C75 C80 C84 123.0(4) . . ?
C75 C80 C79 118.2(4) . . ?
C79 C80 C84 118.8(4) . . ?
C33 C34 H34 119.4 . . ?
C35 C34 C33 121.2(4) . . ?
C35 C34 H34 119.4 . . ?
C94 C95 C100 121.4(4) . . ?
C96 C95 C94 118.4(4) . . ?
C96 C95 C100 120.2(4) . . ?
N15 C91 H91 126.9 . . ?
C90 C91 N15 106.3(4) . . ?
C90 C91 H91 126.9 . . ?
C94 C99 C103 121.2(4) . . ?
C98 C99 C94 117.7(4) . . ?
C98 C99 C103 121.1(4) . . ?
N14 C90 H90 126.4 . . ?
C91 C90 N14 107.2(4) . . ?
C91 C90 H90 126.4 . . ?
N4 C28 H28 126.4 . . ?
C29 C28 N4 107.2(4) . . ?
C29 C28 H28 126.4 . . ?
C107 C112 H112 107.5 . . ?
C107 C112 C114 112.6(4) . . ?
C107 C112 C113 111.4(4) . . ?
C114 C112 H112 107.5 . . ?
C113 C112 H112 107.5 . . ?
C113 C112 C114 110.1(4) . . ?
C37 C36 H36 119.4 . . ?
C35 C36 C37 121.2(4) . . ?
C35 C36 H36 119.4 . . ?
N19 C119 H11D 109.3 . . ?
N19 C119 H11E 109.3 . . ?
N19 C119 C120 111.8(4) . . ?
H11D C119 H11E 107.9 . . ?
C120 C119 H11D 109.3 . . ?
C120 C119 H11E 109.3 . . ?
C44 C45 C50 121.7(4) . . ?
C44 C45 C46 117.8(4) . . ?
C46 C45 C50 120.4(4) . . ?
C13 C14 C19 120.2(4) . . ?
C15 C14 C13 117.9(4) . . ?
C15 C14 C19 121.8(4) . . ?
N9 C57 H57A 109.2 . . ?
N9 C57 H57B 109.2 . . ?
N9 C57 C58 112.0(4) . . ?
H57A C57 H57B 107.9 . . ?
C58 C57 H57A 109.2 . . ?
C58 C57 H57B 109.2 . . ?
C111 C110 H110 119.4 . . ?
C109 C110 C111 121.1(4) . . ?
C109 C110 H110 119.4 . . ?
N9 C59 H59 126.5 . . ?
C60 C59 N9 106.9(4) . . ?
C60 C59 H59 126.5 . . ?
C6 C10 H10 107.4 . . ?
C6 C10 C12 111.5(3) . . ?
C11 C10 C6 111.9(4) . . ?
C11 C10 H10 107.4 . . ?
C11 C10 C12 110.9(4) . . ?
C12 C10 H10 107.4 . . ?
C3 C4 H4 119.7 . . ?
C5 C4 C3 120.5(4) . . ?
C5 C4 H4 119.7 . . ?
N5 C29 H29 126.7 . . ?
C28 C29 N5 106.7(4) . . ?
C28 C29 H29 126.7 . . ?
C44 C49 C53 120.3(4) . . ?
C48 C49 C44 118.7(4) . . ?
C48 C49 C53 120.9(4) . . ?
C80 C84 H84 107.2 . . ?
C80 C84 C86 112.8(4) . . ?
C85 C84 C80 112.0(4) . . ?
C85 C84 H84 107.2 . . ?
C85 C84 C86 110.1(5) . . ?
C86 C84 H84 107.2 . . ?
C18 C22 H22 103.7 . . ?
C18 C22 H22A 108.8 . . ?
C18 C22 C23A 105.6(5) . . ?
C18 C22 C24 117.6(5) . . ?
C23 C22 C18 114.9(5) . . ?
C23 C22 H22 103.7 . . ?
C23 C22 C24 111.2(6) . . ?
C24A C22 C18 111.3(5) . . ?
C24A C22 H22A 108.8 . . ?
C24A C22 C23A 113.4(7) . . ?
C23A C22 H22A 108.8 . . ?
C24 C22 H22 103.7 . . ?
N10 C61 H61A 109.0 . . ?
N10 C61 H61B 109.0 . . ?
N10 C61 C62 112.8(4) . . ?
H61A C61 H61B 107.8 . . ?
C62 C61 H61A 109.0 . . ?
C62 C61 H61B 109.0 . . ?
C111 C115 H115 107.5 . . ?
C117 C115 C111 111.7(4) . . ?
C117 C115 H115 107.5 . . ?
C116 C115 C111 111.7(4) . . ?
C116 C115 H115 107.5 . . ?
C116 C115 C117 110.7(4) . . ?
C18 C17 H17 119.4 . . ?
C16 C17 C18 121.2(5) . . ?
C16 C17 H17 119.4 . . ?
N14 C88 H88A 109.0 . . ?
N14 C88 H88B 109.0 . . ?
N14 C88 C89 113.1(4) . . ?
H88A C88 H88B 107.8 . . ?
C89 C88 H88A 109.0 . . ?
C89 C88 H88B 109.0 . . ?
N5 C30 H30A 109.1 . . ?
N5 C30 H30B 109.1 . . ?
N5 C30 C31 112.5(3) . . ?
H30A C30 H30B 107.8 . . ?
C31 C30 H30A 109.1 . . ?
C31 C30 H30B 109.1 . . ?
N10 C60 H60 126.5 . . ?
C59 C60 N10 107.1(4) . . ?
C59 C60 H60 126.5 . . ?
C33 C38 H38 107.9 . . ?
C33 C38 C40 111.5(4) . . ?
C33 C38 C39 111.4(4) . . ?
C40 C38 H38 107.9 . . ?
C40 C38 C39 110.0(4) . . ?
C39 C38 H38 107.9 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C34 C35 H35 119.7 . . ?
C36 C35 C34 120.5(4) . . ?
C36 C35 H35 119.7 . . ?
N19 C121 H121 126.1 . . ?
C122 C121 N19 107.8(4) . . ?
C122 C121 H121 126.1 . . ?
C64 C69 H69 107.2 . . ?
C64 C69 C70 112.8(4) . . ?
C64 C69 C71 111.1(4) . . ?
C70 C69 H69 107.2 . . ?
C71 C69 H69 107.2 . . ?
C71 C69 C70 111.0(4) . . ?
C37 C41 H41 107.8 . . ?
C37 C41 C43 111.4(3) . . ?
C37 C41 C42 111.6(4) . . ?
C43 C41 H41 107.8 . . ?
C43 C41 C42 110.1(4) . . ?
C42 C41 H41 107.8 . . ?
N20 C123 H12D 109.0 . . ?
N20 C123 H12E 109.0 . . ?
N20 C123 C124 112.9(4) . . ?
H12D C123 H12E 107.8 . . ?
C124 C123 H12D 109.0 . . ?
C124 C123 H12E 109.0 . . ?
C80 C79 H79 119.7 . . ?
C78 C79 C80 120.6(5) . . ?
C78 C79 H79 119.7 . . ?
C92 C93 H93A 109.5 . . ?
C92 C93 H93B 109.5 . . ?
C92 C93 H93C 109.5 . . ?
H93A C93 H93B 109.5 . . ?
H93A C93 H93C 109.5 . . ?
H93B C93 H93C 109.5 . . ?
C108 C109 C110 120.3(4) . . ?
C108 C109 H109 119.8 . . ?
C110 C109 H109 119.8 . . ?
C112 C114 H11F 109.5 . . ?
C112 C114 H11G 109.5 . . ?
C112 C114 H11H 109.5 . . ?
H11F C114 H11G 109.5 . . ?
H11F C114 H11H 109.5 . . ?
H11G C114 H11H 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C76 C77 H77 119.6 . . ?
C78 C77 C76 120.9(4) . . ?
C78 C77 H77 119.6 . . ?
C99 C98 H98 119.1 . . ?
C97 C98 C99 121.9(5) . . ?
C97 C98 H98 119.1 . . ?
N20 C122 H122 126.8 . . ?
C121 C122 N20 106.3(4) . . ?
C121 C122 H122 126.8 . . ?
N4 C26 H26A 109.4 . . ?
N4 C26 H26B 109.4 . . ?
N4 C26 C27 111.4(3) . . ?
H26A C26 H26B 108.0 . . ?
C27 C26 H26A 109.4 . . ?
C27 C26 H26B 109.4 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C95 C100 H100 107.5 . . ?
C95 C100 C101 112.0(4) . . ?
C95 C100 C102 111.5(4) . . ?
C101 C100 H100 107.5 . . ?
C101 C100 C102 110.7(4) . . ?
C102 C100 H100 107.5 . . ?
C68 C72 H72 107.2 . . ?
C68 C72 C74 109.5(4) . . ?
C74 C72 H72 107.2 . . ?
C73 C72 C68 113.5(4) . . ?
C73 C72 H72 107.2 . . ?
C73 C72 C74 112.0(5) . . ?
C45 C50 H50 107.3 . . ?
C45 C50 C52 113.1(5) . . ?
C52 C50 H50 107.3 . . ?
C51 C50 C45 110.3(4) . . ?
C51 C50 H50 107.3 . . ?
C51 C50 C52 111.2(5) . . ?
C49 C48 H48 119.8 . . ?
C47 C48 C49 120.3(4) . . ?
C47 C48 H48 119.8 . . ?
C68 C67 H67 119.7 . . ?
C66 C67 C68 120.6(4) . . ?
C66 C67 H67 119.7 . . ?
C76 C81 H81 107.4 . . ?
C76 C81 C83 111.6(4) . . ?
C76 C81 C82 112.6(4) . . ?
C83 C81 H81 107.4 . . ?
C83 C81 C82 110.1(4) . . ?
C82 C81 H81 107.4 . . ?
C79 C78 C77 120.8(4) . . ?
C79 C78 H78 119.6 . . ?
C77 C78 H78 119.6 . . ?
C119 C120 H12F 109.5 . . ?
C119 C120 H12G 109.5 . . ?
C119 C120 H12H 109.5 . . ?
H12F C120 H12G 109.5 . . ?
H12F C120 H12H 109.5 . . ?
H12G C120 H12H 109.5 . . ?
C14 C19 H19 107.4 . . ?
C14 C19 C20 113.6(4) . . ?
C21 C19 C14 110.1(4) . . ?
C21 C19 H19 107.4 . . ?
C21 C19 C20 110.6(4) . . ?
C20 C19 H19 107.4 . . ?
C64 C65 H65 119.5 . . ?
C66 C65 C64 121.0(4) . . ?
C66 C65 H65 119.5 . . ?
C14 C15 H15 119.5 . . ?
C16 C15 C14 121.1(4) . . ?
C16 C15 H15 119.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C99 C103 H103 107.5 . . ?
C99 C103 C105 110.3(4) . . ?
C99 C103 C104 111.7(5) . . ?
C105 C103 H103 107.5 . . ?
C105 C103 C104 112.0(4) . . ?
C104 C103 H103 107.5 . . ?
C112 C113 H11I 109.5 . . ?
C112 C113 H11J 109.5 . . ?
C112 C113 H11K 109.5 . . ?
H11I C113 H11J 109.5 . . ?
H11I C113 H11K 109.5 . . ?
H11J C113 H11K 109.5 . . ?
C67 C66 H66 119.8 . . ?
C65 C66 C67 120.4(4) . . ?
C65 C66 H66 119.8 . . ?
C115 C117 H11L 109.5 . . ?
C115 C117 H11M 109.5 . . ?
C115 C117 H11N 109.5 . . ?
H11L C117 H11M 109.5 . . ?
H11L C117 H11N 109.5 . . ?
H11M C117 H11N 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C17 C16 C15 120.3(4) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C95 C96 H96 119.4 . . ?
C97 C96 C95 121.2(5) . . ?
C97 C96 H96 119.4 . . ?
C48 C47 H47 119.9 . . ?
C46 C47 C48 120.3(4) . . ?
C46 C47 H47 119.9 . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C69 C70 H70A 109.5 . . ?
C69 C70 H70B 109.5 . . ?
C69 C70 H70C 109.5 . . ?
H70A C70 H70B 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
C45 C46 H46 119.4 . . ?
C47 C46 C45 121.3(4) . . ?
C47 C46 H46 119.4 . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C84 C85 H85A 109.5 . . ?
C84 C85 H85B 109.5 . . ?
C84 C85 H85C 109.5 . . ?
H85A C85 H85B 109.5 . . ?
H85A C85 H85C 109.5 . . ?
H85B C85 H85C 109.5 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C123 C124 H12I 109.5 . . ?
C123 C124 H12J 109.5 . . ?
C123 C124 H12K 109.5 . . ?
H12I C124 H12J 109.5 . . ?
H12I C124 H12K 109.5 . . ?
H12J C124 H12K 109.5 . . ?
C100 C101 H10A 109.5 . . ?
C100 C101 H10B 109.5 . . ?
C100 C101 H10C 109.5 . . ?
H10A C101 H10B 109.5 . . ?
H10A C101 H10C 109.5 . . ?
H10B C101 H10C 109.5 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C88 C89 H89A 109.5 . . ?
C88 C89 H89B 109.5 . . ?
C88 C89 H89C 109.5 . . ?
H89A C89 H89B 109.5 . . ?
H89A C89 H89C 109.5 . . ?
H89B C89 H89C 109.5 . . ?
C103 C105 H10D 109.5 . . ?
C103 C105 H10E 109.5 . . ?
C103 C105 H10F 109.5 . . ?
H10D C105 H10E 109.5 . . ?
H10D C105 H10F 109.5 . . ?
H10E C105 H10F 109.5 . . ?
C84 C86 H86A 109.5 . . ?
C84 C86 H86B 109.5 . . ?
C84 C86 H86C 109.5 . . ?
H86A C86 H86B 109.5 . . ?
H86A C86 H86C 109.5 . . ?
H86B C86 H86C 109.5 . . ?
C98 C97 C96 119.6(4) . . ?
C98 C97 H97 120.2 . . ?
C96 C97 H97 120.2 . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62B 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C49 C53 H53 107.4 . . ?
C49 C53 C54 110.0(5) . . ?
C54 C53 H53 107.4 . . ?
C55 C53 C49 112.8(5) . . ?
C55 C53 H53 107.4 . . ?
C55 C53 C54 111.6(5) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C81 C83 H83A 109.5 . . ?
C81 C83 H83B 109.5 . . ?
C81 C83 H83C 109.5 . . ?
H83A C83 H83B 109.5 . . ?
H83A C83 H83C 109.5 . . ?
H83B C83 H83C 109.5 . . ?
C69 C71 H71A 109.5 . . ?
C69 C71 H71B 109.5 . . ?
C69 C71 H71C 109.5 . . ?
H71A C71 H71B 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
C115 C116 H11O 109.5 . . ?
C115 C116 H11P 109.5 . . ?
C115 C116 H11Q 109.5 . . ?
H11O C116 H11P 109.5 . . ?
H11O C116 H11Q 109.5 . . ?
H11P C116 H11Q 109.5 . . ?
C72 C74 H74A 109.5 . . ?
C72 C74 H74B 109.5 . . ?
C72 C74 H74C 109.5 . . ?
H74A C74 H74B 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
C100 C102 H10G 109.5 . . ?
C100 C102 H10H 109.5 . . ?
C100 C102 H10I 109.5 . . ?
H10G C102 H10H 109.5 . . ?
H10G C102 H10I 109.5 . . ?
H10H C102 H10I 109.5 . . ?
C103 C104 H10J 109.5 . . ?
C103 C104 H10K 109.5 . . ?
C103 C104 H10L 109.5 . . ?
H10J C104 H10K 109.5 . . ?
H10J C104 H10L 109.5 . . ?
H10K C104 H10L 109.5 . . ?
C72 C73 H73A 109.5 . . ?
C72 C73 H73B 109.5 . . ?
C72 C73 H73C 109.5 . . ?
H73A C73 H73B 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C81 C82 H82A 109.5 . . ?
C81 C82 H82B 109.5 . . ?
C81 C82 H82C 109.5 . . ?
H82A C82 H82B 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C50 C52 H52A 109.5 . . ?
C50 C52 H52B 109.5 . . ?
C50 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C53 C55 H55A 109.5 . . ?
C53 C55 H55B 109.5 . . ?
C53 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24A H24A 109.5 . . ?
C22 C24A H24B 109.5 . . ?
C22 C24A H24C 109.5 . . ?
H24A C24A H24B 109.5 . . ?
H24A C24A H24C 109.5 . . ?
H24B C24A H24C 109.5 . . ?
C22 C23A H23D 109.5 . . ?
C22 C23A H23E 109.5 . . ?
C22 C23A H23F 109.5 . . ?
H23D C23A H23E 109.5 . . ?
H23D C23A H23F 109.5 . . ?
H23E C23A H23F 109.5 . . ?
C22 C24 H24D 109.5 . . ?
C22 C24 H24E 109.5 . . ?
C22 C24 H24F 109.5 . . ?
H24D C24 H24E 109.5 . . ?
H24D C24 H24F 109.5 . . ?
H24E C24 H24F 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_17
_database_code_depnum_ccdc_archive 'CCDC 1972009'
loop_
_audit_author_name
_audit_author_address
'Alasdair McKay'
;Monash University
Australia
;
_audit_update_record             
;
2019-12-14 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_audit_creation_date             2019-12-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
''
alasdair.mckay@monash.edu
_chemical_name_common            ?
_chemical_name_systematic        '[TlBr(N3Dipp2)2]'
_chemical_formula_moiety         'C48 H68 Br N6 Tl'
_chemical_formula_sum            'C48 H68 Br N6 Tl'
_chemical_formula_weight         1013.36
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.570(3)
_cell_length_b                   16.835(3)
_cell_length_c                   21.235(4)
_cell_angle_alpha                90
_cell_angle_beta                 108.21(3)
_cell_angle_gamma                90
_cell_volume                     4947.6(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5214
_cell_measurement_temperature    150
_cell_measurement_theta_max      21.410
_cell_measurement_theta_min      2.354
_shelx_estimated_absorpt_T_max   0.887
_shelx_estimated_absorpt_T_min   0.661
_exptl_absorpt_coefficient_mu    4.108
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6259
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0535 before and 0.0440 after correction. The Ratio of minimum to maximum transmission is 0.8389. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       cube
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0610
_diffrn_reflns_av_unetI/netI     0.0949
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            33377
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         1.471
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5942
_reflns_number_total             10694
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.799
_refine_diff_density_min         -1.087
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         10694
_refine_ls_number_restraints     187
_refine_ls_R_factor_all          0.1294
_refine_ls_R_factor_gt           0.0591
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0717P)²+1.7544P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1352
_refine_ls_wR_factor_ref         0.1558
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C7-C8A \\sim C7-C9A \\sim C7-C9 \\sim C7-C8
 with sigma of 0.02
 C12A-C11A \\sim C12-C11
 with sigma of 0.04
 C10-C12A \\sim C10-C11A \\sim C10-C12 \\sim C10-C11
 with sigma of 0.02
 C34-C36A \\sim C34-C35A \\sim C34-C35 \\sim C34-C36
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C7 \\sim C8 \\sim C8A \\sim C9A \\sim C9: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C10 \\sim C11A \\sim C11 \\sim C12A \\sim C12: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C34 \\sim C36A \\sim C36 \\sim C35A \\sim C35: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C7, C8A, C8, C9, C9A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C10, C11A, C11, C12A, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C34, C36A, C36, C35A, C35
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H7B)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=
 Sof(H9AC)=1-FVAR(1)
 Sof(H7A)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C8)=Sof(H8A)=Sof(H8B)=
 Sof(H8C)=FVAR(1)
 Sof(H10A)=Sof(C12A)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C11A)=Sof(H11A)=
 Sof(H11B)=Sof(H11C)=1-FVAR(2)
 Sof(H10)=Sof(C12)=Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(C11)=Sof(H11D)=Sof(H11E)=
 Sof(H11F)=FVAR(2)
 Sof(H34A)=Sof(C36A)=Sof(H36A)=Sof(H36B)=Sof(H36C)=Sof(C35A)=Sof(H35A)=
 Sof(H35B)=Sof(H35C)=1-FVAR(3)
 Sof(H34)=Sof(C35)=Sof(H35D)=Sof(H35E)=Sof(H35F)=Sof(C36)=Sof(H36D)=Sof(H36E)=
 Sof(H36F)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C34(H34A), C34(H34), C31(H31), C46(H46), C10(H10A), C10(H10), C7(H7B),
 C7(H7A), C19(H19), C43(H43), C22(H22)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C28(H28), C27(H27), C41(H41), C29(H29), C16(H16), C5(H5), C17(H17),
 C3(H3), C15(H15), C39(H39), C40(H40)
6.c Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C45(H45A,H45B,H45C), C44(H44A,H44B,
 H44C), C32(H32A,H32B,H32C), C24(H24A,H24B,H24C), C21(H21A,H21B,H21C),
 C12A(H12A,H12B,H12C), C23(H23A,H23B,H23C), C8A(H8AA,H8AB,H8AC), C33(H33A,H33B,
 H33C), C11A(H11A,H11B,H11C), C20(H20A,H20B,H20C), C9A(H9AA,H9AB,H9AC),
 C36A(H36A,H36B,H36C), C35A(H35A,H35B,H35C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C),
 C12(H12D,H12E,H12F), C11(H11D,H11E,H11F), C35(H35D,H35E,H35F), C36(H36D,H36E,
 H36F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tl1 Tl 0.74163(2) 0.26645(2) 0.41962(2) 0.05201(13) Uani 1 1 d . . . . .
Br1 Br 0.71785(8) 0.26098(7) 0.53389(5) 0.0860(3) Uani 1 1 d . . . . .
N5 N 0.6180(4) 0.1607(4) 0.3342(3) 0.0409(14) Uani 1 1 d . . . . .
N2 N 0.8822(4) 0.3705(4) 0.4123(3) 0.0418(15) Uani 1 1 d . . . . .
N6 N 0.5942(4) 0.2310(4) 0.3457(3) 0.0396(13) Uani 1 1 d . . . . .
N1 N 0.7934(4) 0.3830(3) 0.3896(3) 0.0438(15) Uani 1 1 d . . . . .
N4 N 0.7077(5) 0.1478(4) 0.3621(3) 0.0466(15) Uani 1 1 d . . . . .
N3 N 0.9013(4) 0.3015(4) 0.4362(3) 0.0389(14) Uani 1 1 d . . . . .
C25 C 0.7519(5) 0.0758(4) 0.3528(4) 0.0420(18) Uani 1 1 d . . . . .
C37 C 0.4936(6) 0.2507(4) 0.3282(4) 0.047(2) Uani 1 1 d . . . . .
C30 C 0.7572(6) 0.0548(5) 0.2890(4) 0.053(2) Uani 1 1 d . . . . .
C13 C 1.0015(6) 0.2824(4) 0.4703(4) 0.047(2) Uani 1 1 d . . . . .
C34 C 0.7130(7) 0.1049(6) 0.2284(4) 0.078(3) Uani 1 1 d D U . . .
H34A H 0.691814 0.155926 0.243704 0.094 Uiso 0.521(14) 1 calc R . P A 2
H34 H 0.649971 0.117954 0.235517 0.094 Uiso 0.479(14) 1 calc R . P A 1
C42 C 0.4545(6) 0.3007(5) 0.2733(4) 0.057(2) Uani 1 1 d . . . . .
C6 C 0.7733(6) 0.4778(5) 0.2970(4) 0.059(2) Uani 1 1 d . . . . .
C1 C 0.7562(6) 0.4571(5) 0.3556(4) 0.057(2) Uani 1 1 d . . . . .
C31 C 0.7904(7) 0.0503(6) 0.4756(4) 0.070(3) Uani 1 1 d . . . . .
H31 H 0.751420 0.100195 0.470325 0.085 Uiso 1 1 calc R . . . .
C18 C 1.0535(6) 0.2439(5) 0.4349(5) 0.058(2) Uani 1 1 d . . . . .
C46 C 0.5151(6) 0.3311(5) 0.2319(4) 0.060(2) Uani 1 1 d . . . . .
H46 H 0.584578 0.325377 0.258794 0.072 Uiso 1 1 calc R . . . .
C10 C 0.8266(6) 0.4242(6) 0.2620(4) 0.069(2) Uani 1 1 d D U . . .
H10A H 0.879415 0.402989 0.300674 0.083 Uiso 0.37(3) 1 calc R . P B 2
H10 H 0.852295 0.376961 0.290556 0.083 Uiso 0.63(3) 1 calc R . P B 1
C4 C 0.6822(8) 0.5941(6) 0.2947(5) 0.083(3) Uani 1 1 d . . . . .
H4 H 0.654575 0.641740 0.272975 0.100 Uiso 1 1 calc R . . . .
C38 C 0.4364(6) 0.2214(5) 0.3646(4) 0.053(2) Uani 1 1 d . . . . .
C26 C 0.7972(6) 0.0305(5) 0.4082(4) 0.053(2) Uani 1 1 d . . . . .
C28 C 0.8520(7) -0.0590(6) 0.3402(6) 0.080(3) Uani 1 1 d . . . . .
H28 H 0.885622 -0.105862 0.335600 0.096 Uiso 1 1 calc R . . . .
C7 C 0.6895(7) 0.4849(6) 0.4522(5) 0.081(3) Uani 1 1 d D U . . .
H7B H 0.712093 0.428629 0.460774 0.097 Uiso 0.41(3) 1 calc R . P C 2
H7A H 0.739425 0.443897 0.473113 0.097 Uiso 0.59(3) 1 calc R . P C 1
C19 C 0.9829(7) 0.3371(7) 0.5752(5) 0.086(3) Uani 1 1 d . . . . .
H19 H 0.913496 0.327467 0.549600 0.103 Uiso 1 1 calc R . . . .
C2 C 0.7044(6) 0.5064(5) 0.3864(4) 0.059(2) Uani 1 1 d . . . . .
C27 C 0.8462(6) -0.0381(6) 0.3985(5) 0.070(3) Uani 1 1 d . . . . .
H27 H 0.876391 -0.070784 0.435656 0.084 Uiso 1 1 calc R . . . .
C41 C 0.3573(6) 0.3213(6) 0.2573(5) 0.076(3) Uani 1 1 d . . . . .
H41 H 0.329180 0.356213 0.221218 0.091 Uiso 1 1 calc R . . . .
C14 C 1.0418(6) 0.2986(5) 0.5385(4) 0.060(2) Uani 1 1 d . . . . .
C43 C 0.4774(6) 0.1690(6) 0.4237(4) 0.070(3) Uani 1 1 d . . . . .
H43 H 0.549361 0.173171 0.436974 0.084 Uiso 1 1 calc R . . . .
C22 C 1.0121(7) 0.2230(7) 0.3626(4) 0.077(3) Uani 1 1 d . . . . .
H22 H 0.941016 0.232951 0.350063 0.092 Uiso 1 1 calc R . . . .
C29 C 0.8098(7) -0.0133(6) 0.2871(5) 0.073(3) Uani 1 1 d . . . . .
H29 H 0.816351 -0.028626 0.245626 0.087 Uiso 1 1 calc R . . . .
C16 C 1.1897(7) 0.2408(7) 0.5341(6) 0.087(3) Uani 1 1 d . . . . .
H16 H 1.255430 0.227783 0.555913 0.105 Uiso 1 1 calc R . . . .
C5 C 0.7334(7) 0.5490(6) 0.2672(5) 0.072(3) Uani 1 1 d . . . . .
H5 H 0.743008 0.565105 0.226874 0.087 Uiso 1 1 calc R . . . .
C17 C 1.1502(7) 0.2238(6) 0.4701(5) 0.076(3) Uani 1 1 d . . . . .
H17 H 1.188136 0.197494 0.447354 0.091 Uiso 1 1 calc R . . . .
C3 C 0.6679(8) 0.5745(6) 0.3532(6) 0.084(3) Uani 1 1 d . . . . .
H3 H 0.631321 0.609209 0.371387 0.101 Uiso 1 1 calc R . . . .
C47 C 0.4975(10) 0.2797(7) 0.1714(6) 0.109(4) Uani 1 1 d . . . . .
H47A H 0.526102 0.227204 0.184450 0.164 Uiso 1 1 calc GR . . . .
H47B H 0.527028 0.304329 0.140596 0.164 Uiso 1 1 calc GR . . . .
H47C H 0.427752 0.274096 0.149617 0.164 Uiso 1 1 calc GR . . . .
C15 C 1.1366(7) 0.2765(6) 0.5686(5) 0.080(3) Uani 1 1 d . . . . .
H15 H 1.165566 0.286454 0.614547 0.096 Uiso 1 1 calc R . . . .
C39 C 0.3398(8) 0.2450(6) 0.3450(6) 0.087(3) Uani 1 1 d . . . . .
H39 H 0.299220 0.227323 0.369528 0.104 Uiso 1 1 calc R . . . .
C40 C 0.3034(8) 0.2919(7) 0.2928(7) 0.101(4) Uani 1 1 d . . . . .
H40 H 0.236719 0.304998 0.280100 0.122 Uiso 1 1 calc R . . . .
C48 C 0.4965(8) 0.4197(7) 0.2132(6) 0.113(4) Uani 1 1 d . . . . .
H48A H 0.433278 0.425564 0.179454 0.169 Uiso 1 1 calc GR . . . .
H48B H 0.546983 0.439515 0.195745 0.169 Uiso 1 1 calc GR . . . .
H48C H 0.497552 0.450307 0.252735 0.169 Uiso 1 1 calc GR . . . .
C45 C 0.4495(8) 0.0795(6) 0.4059(5) 0.097(3) Uani 1 1 d . . . . .
H45A H 0.381182 0.071435 0.401487 0.145 Uiso 1 1 calc GR . . . .
H45B H 0.489420 0.045210 0.441161 0.145 Uiso 1 1 calc GR . . . .
H45C H 0.460640 0.066249 0.363929 0.145 Uiso 1 1 calc GR . . . .
C44 C 0.4466(9) 0.1917(9) 0.4840(5) 0.127(5) Uani 1 1 d . . . . .
H44A H 0.464203 0.247094 0.496026 0.190 Uiso 1 1 calc GR . . . .
H44B H 0.479438 0.157086 0.521408 0.190 Uiso 1 1 calc GR . . . .
H44C H 0.376533 0.185312 0.473249 0.190 Uiso 1 1 calc GR . . . .
C32 C 0.8896(8) 0.0693(9) 0.5246(5) 0.128(5) Uani 1 1 d . . . . .
H32A H 0.920973 0.019901 0.544718 0.192 Uiso 1 1 calc GR . . . .
H32B H 0.881970 0.104585 0.559291 0.192 Uiso 1 1 calc GR . . . .
H32C H 0.929465 0.095461 0.501146 0.192 Uiso 1 1 calc GR . . . .
C24 C 1.0534(10) 0.2857(11) 0.3248(7) 0.159(7) Uani 1 1 d . . . . .
H24A H 1.023482 0.337406 0.326722 0.238 Uiso 1 1 calc GR . . . .
H24B H 1.039110 0.269348 0.278455 0.238 Uiso 1 1 calc GR . . . .
H24C H 1.123468 0.289776 0.345479 0.238 Uiso 1 1 calc GR . . . .
C21 C 0.9984(9) 0.4266(9) 0.5789(6) 0.132(5) Uani 1 1 d . . . . .
H21A H 1.061286 0.438957 0.573690 0.198 Uiso 1 1 calc GR . . . .
H21B H 0.996639 0.446026 0.622060 0.198 Uiso 1 1 calc GR . . . .
H21C H 0.947142 0.452358 0.543521 0.198 Uiso 1 1 calc GR . . . .
C12A C 0.884(4) 0.465(3) 0.2243(17) 0.092(12) Uani 0.37(3) 1 d D U P B 2
H12A H 0.858069 0.450280 0.177315 0.139 Uiso 0.37(3) 1 calc GR . P B 2
H12B H 0.951564 0.447873 0.241669 0.139 Uiso 0.37(3) 1 calc GR . P B 2
H12C H 0.879735 0.522283 0.229096 0.139 Uiso 0.37(3) 1 calc GR . P B 2
C23 C 1.0242(10) 0.1366(8) 0.3481(6) 0.131(5) Uani 1 1 d . . . . .
H23A H 1.067982 0.131972 0.321473 0.197 Uiso 1 1 calc GR . . . .
H23B H 0.961124 0.114044 0.323604 0.197 Uiso 1 1 calc GR . . . .
H23C H 1.051187 0.107749 0.389920 0.197 Uiso 1 1 calc GR . . . .
C8A C 0.5837(13) 0.482(3) 0.4453(19) 0.093(6) Uani 0.41(3) 1 d D U P C 2
H8AA H 0.560481 0.536372 0.448523 0.139 Uiso 0.41(3) 1 calc GR . P C 2
H8AB H 0.573824 0.449495 0.480713 0.139 Uiso 0.41(3) 1 calc GR . P C 2
H8AC H 0.547796 0.459596 0.402141 0.139 Uiso 0.41(3) 1 calc GR . P C 2
C33 C 0.7377(10) -0.0111(8) 0.5013(6) 0.134(5) Uani 1 1 d . . . . .
H33A H 0.673297 -0.019016 0.469365 0.201 Uiso 1 1 calc GR . . . .
H33B H 0.731451 0.006577 0.543733 0.201 Uiso 1 1 calc GR . . . .
H33C H 0.773695 -0.061171 0.507662 0.201 Uiso 1 1 calc GR . . . .
C11A C 0.779(3) 0.3507(19) 0.232(2) 0.091(12) Uani 0.37(3) 1 d D U P B 2
H11A H 0.738793 0.330942 0.257963 0.136 Uiso 0.37(3) 1 calc GR . P B 2
H11B H 0.828595 0.310913 0.232479 0.136 Uiso 0.37(3) 1 calc GR . P B 2
H11C H 0.739280 0.360971 0.186565 0.136 Uiso 0.37(3) 1 calc GR . P B 2
C20 C 0.9999(11) 0.3039(12) 0.6444(5) 0.165(7) Uani 1 1 d . . . . .
H20A H 0.977115 0.248859 0.641257 0.248 Uiso 1 1 calc GR . . . .
H20B H 0.964450 0.335926 0.667642 0.248 Uiso 1 1 calc GR . . . .
H20C H 1.069101 0.305590 0.668890 0.248 Uiso 1 1 calc GR . . . .
C9A C 0.764(3) 0.534(2) 0.5065(13) 0.103(7) Uani 0.41(3) 1 d D U P C 2
H9AA H 0.823160 0.540489 0.494855 0.155 Uiso 0.41(3) 1 calc GR . P C 2
H9AB H 0.777864 0.507115 0.549234 0.155 Uiso 0.41(3) 1 calc GR . P C 2
H9AC H 0.736276 0.586935 0.509648 0.155 Uiso 0.41(3) 1 calc GR . P C 2
C36A C 0.6246(14) 0.0659(14) 0.1829(11) 0.102(6) Uani 0.521(14) 1 d D U P A 2
H36A H 0.633952 0.008243 0.184076 0.153 Uiso 0.521(14) 1 calc GR . P A 2
H36B H 0.613283 0.085293 0.137611 0.153 Uiso 0.521(14) 1 calc GR . P A 2
H36C H 0.568647 0.078734 0.197366 0.153 Uiso 0.521(14) 1 calc GR . P A 2
C35A C 0.7964(14) 0.1253(15) 0.1998(10) 0.102(5) Uani 0.521(14) 1 d D U P A 2
H35A H 0.856165 0.134066 0.236356 0.152 Uiso 0.521(14) 1 calc GR . P A 2
H35B H 0.779958 0.173459 0.172712 0.152 Uiso 0.521(14) 1 calc GR . P A 2
H35C H 0.805568 0.081054 0.172347 0.152 Uiso 0.521(14) 1 calc GR . P A 2
C9 C 0.709(2) 0.5549(11) 0.5001(10) 0.101(6) Uani 0.59(3) 1 d D U P C 1
H9A H 0.769696 0.580475 0.501445 0.151 Uiso 0.59(3) 1 calc GR . P C 1
H9B H 0.712875 0.535904 0.544573 0.151 Uiso 0.59(3) 1 calc GR . P C 1
H9C H 0.655827 0.593388 0.485219 0.151 Uiso 0.59(3) 1 calc GR . P C 1
C8 C 0.5919(12) 0.4438(14) 0.4377(13) 0.087(5) Uani 0.59(3) 1 d D U P C 1
H8A H 0.552145 0.455645 0.392207 0.130 Uiso 0.59(3) 1 calc GR . P C 1
H8B H 0.559270 0.463082 0.468723 0.130 Uiso 0.59(3) 1 calc GR . P C 1
H8C H 0.601624 0.386282 0.443013 0.130 Uiso 0.59(3) 1 calc GR . P C 1
C12 C 0.909(2) 0.469(2) 0.2515(15) 0.117(10) Uani 0.63(3) 1 d D U P B 1
H12D H 0.884944 0.517905 0.227375 0.175 Uiso 0.63(3) 1 calc GR . P B 1
H12E H 0.939588 0.435877 0.225593 0.175 Uiso 0.63(3) 1 calc GR . P B 1
H12F H 0.956020 0.481244 0.294472 0.175 Uiso 0.63(3) 1 calc GR . P B 1
C11 C 0.7617(13) 0.3957(16) 0.1940(10) 0.096(7) Uani 0.63(3) 1 d D U P B 1
H11D H 0.702236 0.372849 0.198585 0.143 Uiso 0.63(3) 1 calc GR . P B 1
H11E H 0.795889 0.355217 0.176734 0.143 Uiso 0.63(3) 1 calc GR . P B 1
H11F H 0.745494 0.440707 0.163246 0.143 Uiso 0.63(3) 1 calc GR . P B 1
C35 C 0.7499(18) 0.1871(12) 0.2259(9) 0.099(6) Uani 0.479(14) 1 d D U P A 1
H35D H 0.745130 0.217369 0.264179 0.149 Uiso 0.479(14) 1 calc GR . P A 1
H35E H 0.711297 0.213172 0.184936 0.149 Uiso 0.479(14) 1 calc GR . P A 1
H35F H 0.817597 0.184727 0.227001 0.149 Uiso 0.479(14) 1 calc GR . P A 1
C36 C 0.675(2) 0.0636(15) 0.1612(8) 0.095(5) Uani 0.479(14) 1 d D U P A 1
H36D H 0.729545 0.048787 0.145780 0.143 Uiso 0.479(14) 1 calc GR . P A 1
H36E H 0.632103 0.099702 0.129014 0.143 Uiso 0.479(14) 1 calc GR . P A 1
H36F H 0.639273 0.015719 0.165548 0.143 Uiso 0.479(14) 1 calc GR . P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tl1 Br1 2.5579(10) . ?
Tl1 N6 2.307(6) . ?
Tl1 N1 2.264(6) . ?
Tl1 N4 2.312(6) . ?
Tl1 N3 2.318(5) . ?
N5 N6 1.278(8) . ?
N5 N4 1.274(8) . ?
N2 N1 1.249(7) . ?
N2 N3 1.264(8) . ?
N6 C37 1.434(10) . ?
N1 C1 1.459(10) . ?
N4 C25 1.415(9) . ?
N3 C13 1.448(9) . ?
C25 C30 1.426(10) . ?
C25 C26 1.385(10) . ?
C37 C42 1.406(11) . ?
C37 C38 1.392(10) . ?
C30 C34 1.506(12) . ?
C30 C29 1.387(12) . ?
C13 C18 1.383(11) . ?
C13 C14 1.410(11) . ?
C34 H34A 1.0000 . ?
C34 H34 1.0000 . ?
C34 C36A 1.498(14) . ?
C34 C35A 1.557(14) . ?
C34 C35 1.491(15) . ?
C34 C36 1.528(14) . ?
C42 C46 1.517(10) . ?
C42 C41 1.393(11) . ?
C6 C1 1.387(11) . ?
C6 C10 1.527(12) . ?
C6 C5 1.394(12) . ?
C1 C2 1.413(11) . ?
C31 H31 1.0000 . ?
C31 C26 1.503(11) . ?
C31 C32 1.527(13) . ?
C31 C33 1.489(13) . ?
C18 C22 1.505(13) . ?
C18 C17 1.414(12) . ?
C46 H46 1.0000 . ?
C46 C47 1.503(13) . ?
C46 C48 1.545(13) . ?
C10 H10A 1.0000 . ?
C10 H10 1.0000 . ?
C10 C12A 1.488(16) . ?
C10 C11A 1.459(16) . ?
C10 C12 1.486(13) . ?
C10 C11 1.535(13) . ?
C4 H4 0.9500 . ?
C4 C5 1.321(12) . ?
C4 C3 1.365(13) . ?
C38 C43 1.497(11) . ?
C38 C39 1.396(13) . ?
C26 C27 1.406(12) . ?
C28 H28 0.9500 . ?
C28 C27 1.315(12) . ?
C28 C29 1.345(13) . ?
C7 H7B 1.0000 . ?
C7 H7A 1.0000 . ?
C7 C2 1.523(12) . ?
C7 C8A 1.503(16) . ?
C7 C9A 1.553(16) . ?
C7 C9 1.526(14) . ?
C7 C8 1.523(14) . ?
C19 H19 1.0000 . ?
C19 C14 1.477(13) . ?
C19 C21 1.521(16) . ?
C19 C20 1.518(15) . ?
C2 C3 1.363(12) . ?
C27 H27 0.9500 . ?
C41 H41 0.9500 . ?
C41 C40 1.342(13) . ?
C14 C15 1.380(12) . ?
C43 H43 1.0000 . ?
C43 C45 1.576(13) . ?
C43 C44 1.531(12) . ?
C22 H22 1.0000 . ?
C22 C24 1.556(16) . ?
C22 C23 1.508(15) . ?
C29 H29 0.9500 . ?
C16 H16 0.9500 . ?
C16 C17 1.331(14) . ?
C16 C15 1.359(14) . ?
C5 H5 0.9500 . ?
C17 H17 0.9500 . ?
C3 H3 0.9500 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C15 H15 0.9500 . ?
C39 H39 0.9500 . ?
C39 C40 1.328(14) . ?
C40 H40 0.9500 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C12A H12A 0.9800 . ?
C12A H12B 0.9800 . ?
C12A H12C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C8A H8AA 0.9800 . ?
C8A H8AB 0.9800 . ?
C8A H8AC 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C11A H11A 0.9800 . ?
C11A H11B 0.9800 . ?
C11A H11C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C9A H9AA 0.9800 . ?
C9A H9AB 0.9800 . ?
C9A H9AC 0.9800 . ?
C36A H36A 0.9800 . ?
C36A H36B 0.9800 . ?
C36A H36C 0.9800 . ?
C35A H35A 0.9800 . ?
C35A H35B 0.9800 . ?
C35A H35C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C12 H12D 0.9800 . ?
C12 H12E 0.9800 . ?
C12 H12F 0.9800 . ?
C11 H11D 0.9800 . ?
C11 H11E 0.9800 . ?
C11 H11F 0.9800 . ?
C35 H35D 0.9800 . ?
C35 H35E 0.9800 . ?
C35 H35F 0.9800 . ?
C36 H36D 0.9800 . ?
C36 H36E 0.9800 . ?
C36 H36F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N6 Tl1 Br1 105.21(13) . . ?
N6 Tl1 N4 54.4(2) . . ?
N6 Tl1 N3 147.79(18) . . ?
N1 Tl1 Br1 116.99(15) . . ?
N1 Tl1 N6 110.7(2) . . ?
N1 Tl1 N4 129.4(2) . . ?
N1 Tl1 N3 54.2(2) . . ?
N4 Tl1 Br1 113.58(14) . . ?
N4 Tl1 N3 109.8(2) . . ?
N3 Tl1 Br1 106.97(13) . . ?
N4 N5 N6 111.6(6) . . ?
N1 N2 N3 112.4(6) . . ?
N5 N6 Tl1 96.9(4) . . ?
N5 N6 C37 118.7(6) . . ?
C37 N6 Tl1 140.9(5) . . ?
N2 N1 Tl1 98.2(4) . . ?
N2 N1 C1 121.0(6) . . ?
C1 N1 Tl1 140.9(5) . . ?
N5 N4 Tl1 96.7(4) . . ?
N5 N4 C25 121.8(6) . . ?
C25 N4 Tl1 141.5(5) . . ?
N2 N3 Tl1 95.1(4) . . ?
N2 N3 C13 117.8(6) . . ?
C13 N3 Tl1 145.7(4) . . ?
N4 C25 C30 120.5(7) . . ?
C26 C25 N4 118.1(7) . . ?
C26 C25 C30 121.2(7) . . ?
C42 C37 N6 118.1(7) . . ?
C38 C37 N6 121.0(7) . . ?
C38 C37 C42 121.0(8) . . ?
C25 C30 C34 122.5(8) . . ?
C29 C30 C25 115.4(8) . . ?
C29 C30 C34 122.1(8) . . ?
C18 C13 N3 118.1(7) . . ?
C18 C13 C14 121.8(8) . . ?
C14 C13 N3 120.0(7) . . ?
C30 C34 H34A 107.2 . . ?
C30 C34 H34 99.3 . . ?
C30 C34 C35A 106.2(11) . . ?
C30 C34 C36 118.5(13) . . ?
C36A C34 C30 110.9(12) . . ?
C36A C34 H34A 107.2 . . ?
C36A C34 C35A 117.6(13) . . ?
C35A C34 H34A 107.2 . . ?
C35 C34 C30 119.2(11) . . ?
C35 C34 H34 99.3 . . ?
C35 C34 C36 114.8(13) . . ?
C36 C34 H34 99.3 . . ?
C37 C42 C46 121.6(7) . . ?
C41 C42 C37 118.1(7) . . ?
C41 C42 C46 120.3(8) . . ?
C1 C6 C10 123.3(8) . . ?
C1 C6 C5 117.1(9) . . ?
C5 C6 C10 119.4(8) . . ?
C6 C1 N1 121.1(8) . . ?
C6 C1 C2 122.7(8) . . ?
C2 C1 N1 116.2(7) . . ?
C26 C31 H31 106.5 . . ?
C26 C31 C32 111.4(8) . . ?
C32 C31 H31 106.5 . . ?
C33 C31 H31 106.5 . . ?
C33 C31 C26 112.9(9) . . ?
C33 C31 C32 112.5(10) . . ?
C13 C18 C22 123.4(8) . . ?
C13 C18 C17 116.7(8) . . ?
C17 C18 C22 119.9(8) . . ?
C42 C46 H46 107.7 . . ?
C42 C46 C48 112.8(8) . . ?
C47 C46 C42 109.1(8) . . ?
C47 C46 H46 107.7 . . ?
C47 C46 C48 111.6(8) . . ?
C48 C46 H46 107.7 . . ?
C6 C10 H10A 100.9 . . ?
C6 C10 H10 109.0 . . ?
C6 C10 C11 112.6(10) . . ?
C12A C10 C6 117(3) . . ?
C12A C10 H10A 100.9 . . ?
C11A C10 C6 117.9(13) . . ?
C11A C10 H10A 100.9 . . ?
C11A C10 C12A 115.0(18) . . ?
C12 C10 C6 109.4(15) . . ?
C12 C10 H10 109.0 . . ?
C12 C10 C11 107.8(12) . . ?
C11 C10 H10 109.0 . . ?
C5 C4 H4 118.9 . . ?
C5 C4 C3 122.1(10) . . ?
C3 C4 H4 118.9 . . ?
C37 C38 C43 121.6(8) . . ?
C37 C38 C39 117.1(8) . . ?
C39 C38 C43 121.2(8) . . ?
C25 C26 C31 122.0(7) . . ?
C25 C26 C27 117.2(8) . . ?
C27 C26 C31 120.7(8) . . ?
C27 C28 H28 120.3 . . ?
C27 C28 C29 119.3(9) . . ?
C29 C28 H28 120.3 . . ?
C2 C7 H7B 105.1 . . ?
C2 C7 H7A 106.3 . . ?
C2 C7 C9A 106.7(15) . . ?
C2 C7 C9 112.3(11) . . ?
C2 C7 C8 108.4(12) . . ?
C8A C7 H7B 105.1 . . ?
C8A C7 C2 110.7(16) . . ?
C8A C7 C9A 122.7(19) . . ?
C9A C7 H7B 105.1 . . ?
C9 C7 H7A 106.3 . . ?
C8 C7 H7A 106.3 . . ?
C8 C7 C9 116.7(13) . . ?
C14 C19 H19 107.3 . . ?
C14 C19 C21 111.2(9) . . ?
C14 C19 C20 113.8(10) . . ?
C21 C19 H19 107.3 . . ?
C20 C19 H19 107.3 . . ?
C20 C19 C21 109.7(11) . . ?
C1 C2 C7 122.3(8) . . ?
C3 C2 C1 115.7(8) . . ?
C3 C2 C7 122.0(8) . . ?
C26 C27 H27 118.6 . . ?
C28 C27 C26 122.9(9) . . ?
C28 C27 H27 118.6 . . ?
C42 C41 H41 120.1 . . ?
C40 C41 C42 119.9(9) . . ?
C40 C41 H41 120.1 . . ?
C13 C14 C19 120.2(8) . . ?
C15 C14 C13 117.2(8) . . ?
C15 C14 C19 122.5(9) . . ?
C38 C43 H43 107.6 . . ?
C38 C43 C45 110.8(7) . . ?
C38 C43 C44 114.3(9) . . ?
C45 C43 H43 107.6 . . ?
C44 C43 H43 107.6 . . ?
C44 C43 C45 108.6(8) . . ?
C18 C22 H22 106.5 . . ?
C18 C22 C24 105.8(10) . . ?
C18 C22 C23 113.5(9) . . ?
C24 C22 H22 106.5 . . ?
C23 C22 H22 106.5 . . ?
C23 C22 C24 117.4(9) . . ?
C30 C29 H29 118.0 . . ?
C28 C29 C30 124.0(9) . . ?
C28 C29 H29 118.0 . . ?
C17 C16 H16 119.8 . . ?
C17 C16 C15 120.5(10) . . ?
C15 C16 H16 119.8 . . ?
C6 C5 H5 119.8 . . ?
C4 C5 C6 120.5(9) . . ?
C4 C5 H5 119.8 . . ?
C18 C17 H17 119.0 . . ?
C16 C17 C18 122.0(9) . . ?
C16 C17 H17 119.0 . . ?
C4 C3 H3 119.1 . . ?
C2 C3 C4 121.9(10) . . ?
C2 C3 H3 119.1 . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C14 C15 H15 119.1 . . ?
C16 C15 C14 121.8(9) . . ?
C16 C15 H15 119.1 . . ?
C38 C39 H39 119.3 . . ?
C40 C39 C38 121.4(9) . . ?
C40 C39 H39 119.3 . . ?
C41 C40 H40 118.7 . . ?
C39 C40 C41 122.5(10) . . ?
C39 C40 H40 118.7 . . ?
C46 C48 H48A 109.5 . . ?
C46 C48 H48B 109.5 . . ?
C46 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C10 C12A H12A 109.5 . . ?
C10 C12A H12B 109.5 . . ?
C10 C12A H12C 109.5 . . ?
H12A C12A H12B 109.5 . . ?
H12A C12A H12C 109.5 . . ?
H12B C12A H12C 109.5 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C7 C8A H8AA 109.5 . . ?
C7 C8A H8AB 109.5 . . ?
C7 C8A H8AC 109.5 . . ?
H8AA C8A H8AB 109.5 . . ?
H8AA C8A H8AC 109.5 . . ?
H8AB C8A H8AC 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C10 C11A H11A 109.5 . . ?
C10 C11A H11B 109.5 . . ?
C10 C11A H11C 109.5 . . ?
H11A C11A H11B 109.5 . . ?
H11A C11A H11C 109.5 . . ?
H11B C11A H11C 109.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C7 C9A H9AA 109.5 . . ?
C7 C9A H9AB 109.5 . . ?
C7 C9A H9AC 109.5 . . ?
H9AA C9A H9AB 109.5 . . ?
H9AA C9A H9AC 109.5 . . ?
H9AB C9A H9AC 109.5 . . ?
C34 C36A H36A 109.5 . . ?
C34 C36A H36B 109.5 . . ?
C34 C36A H36C 109.5 . . ?
H36A C36A H36B 109.5 . . ?
H36A C36A H36C 109.5 . . ?
H36B C36A H36C 109.5 . . ?
C34 C35A H35A 109.5 . . ?
C34 C35A H35B 109.5 . . ?
C34 C35A H35C 109.5 . . ?
H35A C35A H35B 109.5 . . ?
H35A C35A H35C 109.5 . . ?
H35B C35A H35C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C12 H12D 109.5 . . ?
C10 C12 H12E 109.5 . . ?
C10 C12 H12F 109.5 . . ?
H12D C12 H12E 109.5 . . ?
H12D C12 H12F 109.5 . . ?
H12E C12 H12F 109.5 . . ?
C10 C11 H11D 109.5 . . ?
C10 C11 H11E 109.5 . . ?
C10 C11 H11F 109.5 . . ?
H11D C11 H11E 109.5 . . ?
H11D C11 H11F 109.5 . . ?
H11E C11 H11F 109.5 . . ?
C34 C35 H35D 109.5 . . ?
C34 C35 H35E 109.5 . . ?
C34 C35 H35F 109.5 . . ?
H35D C35 H35E 109.5 . . ?
H35D C35 H35F 109.5 . . ?
H35E C35 H35F 109.5 . . ?
C34 C36 H36D 109.5 . . ?
C34 C36 H36E 109.5 . . ?
C34 C36 H36F 109.5 . . ?
H36D C36 H36E 109.5 . . ?
H36D C36 H36F 109.5 . . ?
H36E C36 H36F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Tl1 N6 C37 C42 99.7(9) . . . . ?
Tl1 N6 C37 C38 -80.1(10) . . . . ?
Tl1 N1 C1 C6 -116.1(8) . . . . ?
Tl1 N1 C1 C2 65.3(11) . . . . ?
Tl1 N4 C25 C30 -118.2(8) . . . . ?
Tl1 N4 C25 C26 56.0(10) . . . . ?
Tl1 N3 C13 C18 101.9(9) . . . . ?
Tl1 N3 C13 C14 -74.3(11) . . . . ?
N5 N6 C37 C42 -107.6(8) . . . . ?
N5 N6 C37 C38 72.6(9) . . . . ?
N5 N4 C25 C30 64.6(9) . . . . ?
N5 N4 C25 C26 -121.2(7) . . . . ?
N2 N1 C1 C6 63.1(10) . . . . ?
N2 N1 C1 C2 -115.5(8) . . . . ?
N2 N3 C13 C18 -96.0(8) . . . . ?
N2 N3 C13 C14 87.8(8) . . . . ?
N6 N5 N4 Tl1 5.9(5) . . . . ?
N6 N5 N4 C25 -175.9(6) . . . . ?
N6 C37 C42 C46 2.2(12) . . . . ?
N6 C37 C42 C41 -178.5(8) . . . . ?
N6 C37 C38 C43 0.7(12) . . . . ?
N6 C37 C38 C39 178.5(8) . . . . ?
N1 N2 N3 Tl1 -3.8(6) . . . . ?
N1 N2 N3 C13 -173.8(6) . . . . ?
N1 C1 C2 C7 1.1(12) . . . . ?
N1 C1 C2 C3 -178.4(8) . . . . ?
N4 N5 N6 Tl1 -5.9(5) . . . . ?
N4 N5 N6 C37 -169.0(6) . . . . ?
N4 C25 C30 C34 -2.9(11) . . . . ?
N4 C25 C30 C29 174.3(7) . . . . ?
N4 C25 C26 C31 7.5(11) . . . . ?
N4 C25 C26 C27 -175.9(7) . . . . ?
N3 N2 N1 Tl1 3.9(6) . . . . ?
N3 N2 N1 C1 -175.6(6) . . . . ?
N3 C13 C18 C22 1.8(12) . . . . ?
N3 C13 C18 C17 -178.1(7) . . . . ?
N3 C13 C14 C19 -1.6(12) . . . . ?
N3 C13 C14 C15 177.8(7) . . . . ?
C25 C30 C34 C36A -107.6(14) . . . . ?
C25 C30 C34 C35A 123.5(12) . . . . ?
C25 C30 C34 C35 63.2(16) . . . . ?
C25 C30 C34 C36 -148.8(14) . . . . ?
C25 C30 C29 C28 1.5(13) . . . . ?
C25 C26 C27 C28 1.6(13) . . . . ?
C37 C42 C46 C47 97.8(10) . . . . ?
C37 C42 C46 C48 -137.7(9) . . . . ?
C37 C42 C41 C40 -1.7(15) . . . . ?
C37 C38 C43 C45 -102.6(9) . . . . ?
C37 C38 C43 C44 134.4(9) . . . . ?
C37 C38 C39 C40 1.8(16) . . . . ?
C30 C25 C26 C31 -178.3(7) . . . . ?
C30 C25 C26 C27 -1.7(11) . . . . ?
C13 C18 C22 C24 102.8(10) . . . . ?
C13 C18 C22 C23 -127.1(10) . . . . ?
C13 C18 C17 C16 0.2(14) . . . . ?
C13 C14 C15 C16 0.3(14) . . . . ?
C34 C30 C29 C28 178.7(9) . . . . ?
C42 C37 C38 C43 -179.1(8) . . . . ?
C42 C37 C38 C39 -1.3(12) . . . . ?
C42 C41 C40 C39 2.3(19) . . . . ?
C6 C1 C2 C7 -177.5(8) . . . . ?
C6 C1 C2 C3 3.1(13) . . . . ?
C1 C6 C10 C12A -149(2) . . . . ?
C1 C6 C10 C11A 68(3) . . . . ?
C1 C6 C10 C12 -125.4(18) . . . . ?
C1 C6 C10 C11 114.7(15) . . . . ?
C1 C6 C5 C4 0.4(14) . . . . ?
C1 C2 C3 C4 -1.3(15) . . . . ?
C31 C26 C27 C28 178.2(9) . . . . ?
C18 C13 C14 C19 -177.7(9) . . . . ?
C18 C13 C14 C15 1.8(12) . . . . ?
C46 C42 C41 C40 177.6(10) . . . . ?
C10 C6 C1 N1 3.2(12) . . . . ?
C10 C6 C1 C2 -178.2(8) . . . . ?
C10 C6 C5 C4 176.2(9) . . . . ?
C38 C37 C42 C46 -178.1(8) . . . . ?
C38 C37 C42 C41 1.3(13) . . . . ?
C38 C39 C40 C41 -2(2) . . . . ?
C26 C25 C30 C34 -176.9(7) . . . . ?
C26 C25 C30 C29 0.3(11) . . . . ?
C7 C2 C3 C4 179.3(9) . . . . ?
C19 C14 C15 C16 179.7(10) . . . . ?
C27 C28 C29 C30 -1.8(15) . . . . ?
C41 C42 C46 C47 -81.6(11) . . . . ?
C41 C42 C46 C48 43.0(12) . . . . ?
C14 C13 C18 C22 177.9(8) . . . . ?
C14 C13 C18 C17 -2.0(12) . . . . ?
C43 C38 C39 C40 179.6(11) . . . . ?
C22 C18 C17 C16 -179.7(10) . . . . ?
C29 C30 C34 C36A 75.4(15) . . . . ?
C29 C30 C34 C35A -53.5(14) . . . . ?
C29 C30 C34 C35 -113.8(15) . . . . ?
C29 C30 C34 C36 34.2(17) . . . . ?
C29 C28 C27 C26 0.1(15) . . . . ?
C5 C6 C1 N1 178.8(7) . . . . ?
C5 C6 C1 C2 -2.7(13) . . . . ?
C5 C6 C10 C12A 36(2) . . . . ?
C5 C6 C10 C11A -107(3) . . . . ?
C5 C6 C10 C12 59.1(19) . . . . ?
C5 C6 C10 C11 -60.7(16) . . . . ?
C5 C4 C3 C2 -0.9(17) . . . . ?
C17 C18 C22 C24 -77.3(11) . . . . ?
C17 C18 C22 C23 52.8(13) . . . . ?
C17 C16 C15 C14 -2.0(16) . . . . ?
C3 C4 C5 C6 1.4(16) . . . . ?
C15 C16 C17 C18 1.8(16) . . . . ?
C39 C38 C43 C45 79.7(11) . . . . ?
C39 C38 C43 C44 -43.4(13) . . . . ?
C32 C31 C26 C25 -117.9(10) . . . . ?
C32 C31 C26 C27 65.7(12) . . . . ?
C21 C19 C14 C13 -95.1(11) . . . . ?
C21 C19 C14 C15 85.5(12) . . . . ?
C8A C7 C2 C1 -123(2) . . . . ?
C8A C7 C2 C3 57(2) . . . . ?
C33 C31 C26 C25 114.5(10) . . . . ?
C33 C31 C26 C27 -62.0(12) . . . . ?
C20 C19 C14 C13 140.5(10) . . . . ?
C20 C19 C14 C15 -38.9(15) . . . . ?
C9A C7 C2 C1 101.3(19) . . . . ?
C9A C7 C2 C3 -79(2) . . . . ?
C9 C7 C2 C1 134.5(15) . . . . ?
C9 C7 C2 C3 -46.1(18) . . . . ?
C8 C7 C2 C1 -95.1(14) . . . . ?
C8 C7 C2 C3 84.3(15) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_19
_database_code_depnum_ccdc_archive 'CCDC 1972011'
loop_
_audit_author_name
_audit_author_address
'Alasdair McKay'
;Monash University
Australia
;
_audit_update_record             
;
2019-12-14 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_audit_creation_date             2019-12-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
''
alasdair.mckay@monash.edu
_chemical_name_common            ?
_chemical_name_systematic        '[Ge(N3Dipp2)2]'
_chemical_formula_moiety         'C48 H68 Ge N6'
_chemical_formula_sum            'C48 H68 Ge N6'
_chemical_formula_weight         801.67
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.737(3)
_cell_length_b                   15.884(4)
_cell_length_c                   20.901(5)
_cell_angle_alpha                90
_cell_angle_beta                 110.220(7)
_cell_angle_gamma                90
_cell_volume                     4591.3(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9595
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.864
_cell_measurement_theta_min      2.439
_shelx_estimated_absorpt_T_max   0.966
_shelx_estimated_absorpt_T_min   0.920
_exptl_absorpt_coefficient_mu    0.705
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6067
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1211 before and 0.0728 after correction. The Ratio of minimum to maximum transmission is 0.8139. The λ/2 correction factor is 0.00150.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0696
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            75551
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.464
_diffrn_reflns_theta_min         1.480
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7037
_reflns_number_total             9441
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         9441
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0390
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0387P)²+3.0358P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.1038
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C20A \\sim C19 \\sim C21A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C20 \\sim C19 \\sim C21: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
3. Rigid body (RIGU) restrains
 C20A, C19, C21A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C20, C19, C21
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H19A)=Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C20A)=Sof(H20D)=
 Sof(H20E)=Sof(H20F)=1-FVAR(1)
 Sof(H19)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C20)=Sof(H20A)=Sof(H20B)=
 Sof(H20C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C22(H22), C34(H34), C46(H46), C43(H43), C19(H19), C19(H19A), C10(H10),
 C31(H31), C7(H7)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C4(H4), C29(H29), C27(H27), C17(H17), C41(H41), C28(H28),
 C15(H15), C16(H16), C39(H39), C40(H40)
5.c Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C47(H47A,H47B,H47C), C23(H23A,H23B,H23C), C36(H36A,H36B,
 H36C), C11(H11A,H11B,H11C), C45(H45A,H45B,H45C), C48(H48A,H48B,H48C), C24(H24A,
 H24B,H24C), C32(H32A,H32B,H32C), C9(H9A,H9B,H9C), C12(H12A,H12B,H12C),
 C44(H44A,H44B,H44C), C8(H8A,H8B,H8C), C33(H33A,H33B,H33C), C21(H21A,H21B,H21C),
  C20(H20A,H20B,H20C), C21A(H21D,H21E,H21F), C20A(H20D,H20E,H20F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.32285(2) 0.72158(2) 0.57356(2) 0.02759(8) Uani 1 1 d . . . . .
N6 N 0.25409(13) 0.73522(11) 0.65064(9) 0.0269(4) Uani 1 1 d . . . . .
N4 N 0.36115(12) 0.81545(11) 0.64142(9) 0.0264(4) Uani 1 1 d . . . . .
N1 N 0.40587(12) 0.62524(11) 0.62028(9) 0.0263(4) Uani 1 1 d . . . . .
N3 N 0.47063(12) 0.70830(11) 0.57091(9) 0.0261(4) Uani 1 1 d . . . . .
N2 N 0.47810(12) 0.63362(11) 0.59717(9) 0.0273(4) Uani 1 1 d . . . . .
N5 N 0.29205(13) 0.80895(11) 0.66776(9) 0.0277(4) Uani 1 1 d . . . . .
C13 C 0.53546(16) 0.72716(14) 0.53492(11) 0.0296(5) Uani 1 1 d . . . . .
C37 C 0.16670(16) 0.71959(14) 0.66385(11) 0.0305(5) Uani 1 1 d . . . . .
C1 C 0.39698(16) 0.54552(13) 0.64997(11) 0.0306(5) Uani 1 1 d . . . . .
C25 C 0.41507(16) 0.89182(13) 0.65238(11) 0.0295(5) Uani 1 1 d . . . . .
C18 C 0.62475(17) 0.76403(15) 0.57030(12) 0.0357(5) Uani 1 1 d . . . . .
C22 C 0.65860(17) 0.77742(16) 0.64629(13) 0.0407(6) Uani 1 1 d . . . . .
H22 H 0.600745 0.773252 0.660725 0.049 Uiso 1 1 calc R . . . .
C5 C 0.4530(2) 0.44622(16) 0.74083(13) 0.0467(7) Uani 1 1 d . . . . .
H5 H 0.498479 0.429495 0.783520 0.056 Uiso 1 1 calc R . . . .
C6 C 0.46366(17) 0.52414(14) 0.71396(12) 0.0349(5) Uani 1 1 d . . . . .
C42 C 0.17202(17) 0.66874(15) 0.71964(12) 0.0368(5) Uani 1 1 d . . . . .
C34 C 0.49425(18) 0.85349(17) 0.77859(12) 0.0432(6) Uani 1 1 d . . . . .
H34 H 0.459870 0.799288 0.761559 0.052 Uiso 1 1 calc R . . . .
C3 C 0.3135(2) 0.41540(17) 0.64504(14) 0.0511(7) Uani 1 1 d . . . . .
H3 H 0.262026 0.378134 0.622200 0.061 Uiso 1 1 calc R . . . .
C30 C 0.48255(17) 0.90907(15) 0.71717(13) 0.0361(5) Uani 1 1 d . . . . .
C46 C 0.26731(18) 0.63799(15) 0.76885(12) 0.0376(6) Uani 1 1 d . . . . .
H46 H 0.315676 0.641227 0.745156 0.045 Uiso 1 1 calc R . . . .
C38 C 0.07893(17) 0.75139(17) 0.61972(14) 0.0416(6) Uani 1 1 d . . . . .
C43 C 0.07174(19) 0.80418(17) 0.55775(13) 0.0457(6) Uani 1 1 d . . . . .
H43 H 0.139258 0.818271 0.560836 0.055 Uiso 1 1 calc R . . . .
C14 C 0.50517(18) 0.71312(16) 0.46462(12) 0.0387(6) Uani 1 1 d . . . . .
C4 C 0.3785(2) 0.39286(17) 0.70734(15) 0.0536(7) Uani 1 1 d . . . . .
H4 H 0.372038 0.340459 0.727244 0.064 Uiso 1 1 calc R . . . .
C2 C 0.32110(19) 0.49156(15) 0.61456(13) 0.0412(6) Uani 1 1 d . . . . .
C26 C 0.40106(19) 0.94682(15) 0.59758(13) 0.0402(6) Uani 1 1 d . . . . .
C29 C 0.53745(19) 0.98205(17) 0.72466(15) 0.0474(7) Uani 1 1 d . . . . .
H29 H 0.584132 0.995002 0.767900 0.057 Uiso 1 1 calc R . . . .
C19 C 0.4096(2) 0.6728(2) 0.42642(13) 0.0509(7) Uani 1 1 d . U . . .
H19 H 0.364187 0.684552 0.451487 0.061 Uiso 0.768(12) 1 calc R . P A 1
H19A H 0.383363 0.652066 0.461735 0.061 Uiso 0.232(12) 1 calc R . P A 2
C10 C 0.54651(18) 0.58116(16) 0.75394(12) 0.0421(6) Uani 1 1 d . . . . .
H10 H 0.539838 0.635558 0.728643 0.051 Uiso 1 1 calc R . . . .
C31 C 0.3232(2) 0.93282(17) 0.52854(13) 0.0515(7) Uani 1 1 d . . . . .
H31 H 0.296010 0.875293 0.529345 0.062 Uiso 1 1 calc R . . . .
C27 C 0.4573(2) 1.01902(16) 0.60834(16) 0.0517(7) Uani 1 1 d . . . . .
H27 H 0.448438 1.057433 0.571838 0.062 Uiso 1 1 calc R . . . .
C17 C 0.6843(2) 0.78509(18) 0.53380(15) 0.0501(7) Uani 1 1 d . . . . .
H17 H 0.745910 0.809244 0.557059 0.060 Uiso 1 1 calc R . . . .
C7 C 0.2497(2) 0.51141(17) 0.54401(14) 0.0536(7) Uani 1 1 d . . . . .
H7 H 0.269433 0.566166 0.529146 0.064 Uiso 1 1 calc R . . . .
C41 C 0.0872(2) 0.65017(19) 0.73088(17) 0.0608(8) Uani 1 1 d . . . . .
H41 H 0.089095 0.616338 0.768802 0.073 Uiso 1 1 calc R . . . .
C28 C 0.5256(2) 1.03584(17) 0.67080(17) 0.0535(7) Uani 1 1 d . . . . .
H28 H 0.564780 1.084746 0.676897 0.064 Uiso 1 1 calc R . . . .
C15 C 0.5678(2) 0.73629(19) 0.43097(14) 0.0531(7) Uani 1 1 d . . . . .
H15 H 0.548945 0.727358 0.383203 0.064 Uiso 1 1 calc R . . . .
C35 C 0.5994(2) 0.8327(2) 0.81883(15) 0.0631(8) Uani 1 1 d . . . . .
H35A H 0.628160 0.803591 0.789172 0.095 Uiso 1 1 calc GR . . . .
H35B H 0.602619 0.796357 0.857424 0.095 Uiso 1 1 calc GR . . . .
H35C H 0.635054 0.884924 0.835809 0.095 Uiso 1 1 calc GR . . . .
C47 C 0.2638(2) 0.5469(2) 0.7906(2) 0.0769(11) Uani 1 1 d . . . . .
H47A H 0.217642 0.541851 0.814795 0.115 Uiso 1 1 calc GR . . . .
H47B H 0.328116 0.529621 0.820900 0.115 Uiso 1 1 calc GR . . . .
H47C H 0.243214 0.510614 0.750226 0.115 Uiso 1 1 calc GR . . . .
C16 C 0.6562(2) 0.7718(2) 0.46521(16) 0.0595(8) Uani 1 1 d . . . . .
H16 H 0.697780 0.787133 0.441121 0.071 Uiso 1 1 calc R . . . .
C23 C 0.7030(3) 0.8629(2) 0.66716(17) 0.0691(9) Uani 1 1 d . . . . .
H23A H 0.762756 0.867285 0.656783 0.104 Uiso 1 1 calc GR . . . .
H23B H 0.717581 0.870712 0.716218 0.104 Uiso 1 1 calc GR . . . .
H23C H 0.657438 0.906473 0.642060 0.104 Uiso 1 1 calc GR . . . .
C36 C 0.4461(2) 0.8946(2) 0.82454(15) 0.0658(9) Uani 1 1 d . . . . .
H36A H 0.477887 0.948376 0.841484 0.099 Uiso 1 1 calc GR . . . .
H36B H 0.451980 0.857352 0.863157 0.099 Uiso 1 1 calc GR . . . .
H36C H 0.377612 0.904389 0.798520 0.099 Uiso 1 1 calc GR . . . .
C39 C -0.0040(2) 0.7300(2) 0.63327(18) 0.0652(9) Uani 1 1 d . . . . .
H39 H -0.064890 0.750270 0.604157 0.078 Uiso 1 1 calc R . . . .
C11 C 0.5453(2) 0.6003(2) 0.82490(14) 0.0663(9) Uani 1 1 d . . . . .
H11A H 0.485153 0.629570 0.821204 0.099 Uiso 1 1 calc GR . . . .
H11B H 0.600634 0.636078 0.849207 0.099 Uiso 1 1 calc GR . . . .
H11C H 0.549273 0.547519 0.850030 0.099 Uiso 1 1 calc GR . . . .
C45 C 0.0199(3) 0.8864(2) 0.5566(2) 0.0833(11) Uani 1 1 d . . . . .
H45A H -0.047888 0.875178 0.550890 0.125 Uiso 1 1 calc GR . . . .
H45B H 0.022944 0.921064 0.518654 0.125 Uiso 1 1 calc GR . . . .
H45C H 0.050878 0.916391 0.599680 0.125 Uiso 1 1 calc GR . . . .
C48 C 0.3007(3) 0.6970(3) 0.82940(17) 0.0839(12) Uani 1 1 d . . . . .
H48A H 0.306101 0.754226 0.813601 0.126 Uiso 1 1 calc GR . . . .
H48B H 0.363866 0.678558 0.860765 0.126 Uiso 1 1 calc GR . . . .
H48C H 0.253698 0.696367 0.853049 0.126 Uiso 1 1 calc GR . . . .
C40 C 0.0001(2) 0.6801(2) 0.6877(2) 0.0796(11) Uani 1 1 d . . . . .
H40 H -0.057723 0.666228 0.695723 0.096 Uiso 1 1 calc R . . . .
C24 C 0.7268(3) 0.7079(2) 0.68118(18) 0.0982(14) Uani 1 1 d . . . . .
H24A H 0.699391 0.653611 0.661548 0.147 Uiso 1 1 calc GR . . . .
H24B H 0.736680 0.708327 0.730005 0.147 Uiso 1 1 calc GR . . . .
H24C H 0.788997 0.716338 0.674730 0.147 Uiso 1 1 calc GR . . . .
C32 C 0.2408(2) 0.9943(2) 0.5154(2) 0.0809(11) Uani 1 1 d . . . . .
H32A H 0.214573 0.990992 0.552475 0.121 Uiso 1 1 calc GR . . . .
H32B H 0.189915 0.980422 0.472089 0.121 Uiso 1 1 calc GR . . . .
H32C H 0.264319 1.051528 0.512997 0.121 Uiso 1 1 calc GR . . . .
C9 C 0.2505(3) 0.4446(3) 0.49135(17) 0.0981(14) Uani 1 1 d . . . . .
H9A H 0.317116 0.435325 0.493141 0.147 Uiso 1 1 calc GR . . . .
H9B H 0.211097 0.463970 0.445671 0.147 Uiso 1 1 calc GR . . . .
H9C H 0.223942 0.391810 0.501554 0.147 Uiso 1 1 calc GR . . . .
C12 C 0.6429(2) 0.5422(3) 0.7595(2) 0.0834(11) Uani 1 1 d . . . . .
H12A H 0.652312 0.490047 0.786028 0.125 Uiso 1 1 calc GR . . . .
H12B H 0.695143 0.581740 0.782206 0.125 Uiso 1 1 calc GR . . . .
H12C H 0.643524 0.529611 0.713710 0.125 Uiso 1 1 calc GR . . . .
C44 C 0.0267(3) 0.7557(3) 0.49314(17) 0.0958(14) Uani 1 1 d . . . . .
H44A H 0.063823 0.704074 0.494636 0.144 Uiso 1 1 calc GR . . . .
H44B H 0.026765 0.790151 0.454270 0.144 Uiso 1 1 calc GR . . . .
H44C H -0.039988 0.741042 0.488191 0.144 Uiso 1 1 calc GR . . . .
C8 C 0.1480(3) 0.5217(3) 0.54455(19) 0.0903(12) Uani 1 1 d . . . . .
H8A H 0.125529 0.467992 0.556788 0.135 Uiso 1 1 calc GR . . . .
H8B H 0.105050 0.538989 0.499189 0.135 Uiso 1 1 calc GR . . . .
H8C H 0.147448 0.564676 0.578038 0.135 Uiso 1 1 calc GR . . . .
C33 C 0.3632(3) 0.9341(3) 0.47076(17) 0.1066(16) Uani 1 1 d . . . . .
H33A H 0.388829 0.990198 0.467464 0.160 Uiso 1 1 calc GR . . . .
H33B H 0.311522 0.920408 0.427815 0.160 Uiso 1 1 calc GR . . . .
H33C H 0.415154 0.892388 0.479670 0.160 Uiso 1 1 calc GR . . . .
C21 C 0.4252(4) 0.5757(4) 0.4258(4) 0.087(2) Uani 0.768(12) 1 d . U P A 1
H21A H 0.471750 0.563251 0.403092 0.130 Uiso 0.768(12) 1 calc GR . P A 1
H21B H 0.363492 0.548140 0.401205 0.130 Uiso 0.768(12) 1 calc GR . P A 1
H21C H 0.450206 0.554741 0.472792 0.130 Uiso 0.768(12) 1 calc GR . P A 1
C20 C 0.3647(4) 0.7052(6) 0.3543(3) 0.092(3) Uani 0.768(12) 1 d . U P A 1
H20A H 0.356665 0.766395 0.355238 0.139 Uiso 0.768(12) 1 calc GR . P A 1
H20B H 0.301386 0.678695 0.332684 0.139 Uiso 0.768(12) 1 calc GR . P A 1
H20C H 0.406827 0.691568 0.328386 0.139 Uiso 0.768(12) 1 calc GR . P A 1
C21A C 0.4064(16) 0.6032(12) 0.3831(11) 0.074(6) Uani 0.232(12) 1 d . U P A 2
H21D H 0.427125 0.621286 0.345433 0.111 Uiso 0.232(12) 1 calc GR . P A 2
H21E H 0.340215 0.581423 0.364726 0.111 Uiso 0.232(12) 1 calc GR . P A 2
H21F H 0.449769 0.558854 0.409148 0.111 Uiso 0.232(12) 1 calc GR . P A 2
C20A C 0.3374(12) 0.7490(12) 0.3856(11) 0.075(6) Uani 0.232(12) 1 d . U P A 2
H20D H 0.319378 0.783460 0.418252 0.112 Uiso 0.232(12) 1 calc GR . P A 2
H20E H 0.279019 0.724826 0.352168 0.112 Uiso 0.232(12) 1 calc GR . P A 2
H20F H 0.370670 0.784138 0.362118 0.112 Uiso 0.232(12) 1 calc GR . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 N6 2.1902(17) . ?
Ge1 N4 2.0001(18) . ?
Ge1 N1 1.9917(17) . ?
Ge1 N3 2.2078(18) . ?
N6 N5 1.294(2) . ?
N6 C37 1.429(3) . ?
N4 N5 1.318(2) . ?
N4 C25 1.425(3) . ?
N1 N2 1.319(2) . ?
N1 C1 1.436(3) . ?
N3 N2 1.296(2) . ?
N3 C13 1.437(3) . ?
C13 C18 1.396(3) . ?
C13 C14 1.398(3) . ?
C37 C42 1.398(3) . ?
C37 C38 1.398(3) . ?
C1 C6 1.401(3) . ?
C1 C2 1.400(3) . ?
C25 C30 1.403(3) . ?
C25 C26 1.398(3) . ?
C18 C22 1.506(3) . ?
C18 C17 1.388(3) . ?
C22 C23 1.505(4) . ?
C22 C24 1.502(4) . ?
C5 C6 1.390(3) . ?
C5 C4 1.372(4) . ?
C6 C10 1.518(3) . ?
C42 C46 1.507(3) . ?
C42 C41 1.381(3) . ?
C34 C30 1.518(3) . ?
C34 C35 1.522(4) . ?
C34 C36 1.524(4) . ?
C3 C4 1.371(4) . ?
C3 C2 1.390(3) . ?
C30 C29 1.391(3) . ?
C46 C47 1.523(4) . ?
C46 C48 1.514(4) . ?
C38 C43 1.516(4) . ?
C38 C39 1.389(4) . ?
C43 C45 1.510(4) . ?
C43 C44 1.496(4) . ?
C14 C19 1.501(4) . ?
C14 C15 1.389(4) . ?
C2 C7 1.519(4) . ?
C26 C31 1.518(4) . ?
C26 C27 1.387(4) . ?
C29 C28 1.375(4) . ?
C19 C21 1.560(7) . ?
C19 C20 1.511(5) . ?
C19 C21A 1.420(14) . ?
C19 C20A 1.643(17) . ?
C10 C11 1.520(4) . ?
C10 C12 1.517(4) . ?
C31 C32 1.508(4) . ?
C31 C33 1.516(4) . ?
C27 C28 1.371(4) . ?
C17 C16 1.364(4) . ?
C7 C9 1.532(5) . ?
C7 C8 1.512(4) . ?
C41 C40 1.373(4) . ?
C15 C16 1.372(4) . ?
C39 C40 1.370(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N6 Ge1 N3 137.65(6) . . ?
N4 Ge1 N6 59.57(7) . . ?
N4 Ge1 N3 92.87(7) . . ?
N1 Ge1 N6 94.44(7) . . ?
N1 Ge1 N4 104.49(7) . . ?
N1 Ge1 N3 59.65(7) . . ?
N5 N6 Ge1 91.57(12) . . ?
N5 N6 C37 115.86(17) . . ?
C37 N6 Ge1 143.31(14) . . ?
N5 N4 Ge1 99.69(13) . . ?
N5 N4 C25 117.91(17) . . ?
C25 N4 Ge1 138.92(14) . . ?
N2 N1 Ge1 100.35(12) . . ?
N2 N1 C1 116.94(17) . . ?
C1 N1 Ge1 139.21(14) . . ?
N2 N3 Ge1 90.98(12) . . ?
N2 N3 C13 115.98(17) . . ?
C13 N3 Ge1 146.44(14) . . ?
N3 N2 N1 106.64(16) . . ?
N6 N5 N4 106.13(16) . . ?
C18 C13 N3 119.05(19) . . ?
C18 C13 C14 121.6(2) . . ?
C14 C13 N3 119.2(2) . . ?
C42 C37 N6 117.8(2) . . ?
C38 C37 N6 120.0(2) . . ?
C38 C37 C42 122.1(2) . . ?
C6 C1 N1 119.2(2) . . ?
C2 C1 N1 119.1(2) . . ?
C2 C1 C6 121.7(2) . . ?
C30 C25 N4 119.4(2) . . ?
C26 C25 N4 119.0(2) . . ?
C26 C25 C30 121.6(2) . . ?
C13 C18 C22 121.7(2) . . ?
C17 C18 C13 118.0(2) . . ?
C17 C18 C22 120.2(2) . . ?
C23 C22 C18 112.7(2) . . ?
C24 C22 C18 109.3(2) . . ?
C24 C22 C23 111.8(3) . . ?
C4 C5 C6 121.7(2) . . ?
C1 C6 C10 123.1(2) . . ?
C5 C6 C1 117.5(2) . . ?
C5 C6 C10 119.4(2) . . ?
C37 C42 C46 121.8(2) . . ?
C41 C42 C37 118.2(2) . . ?
C41 C42 C46 120.0(2) . . ?
C30 C34 C35 112.9(2) . . ?
C30 C34 C36 110.0(2) . . ?
C35 C34 C36 110.6(2) . . ?
C4 C3 C2 121.4(3) . . ?
C25 C30 C34 122.6(2) . . ?
C29 C30 C25 117.5(2) . . ?
C29 C30 C34 119.9(2) . . ?
C42 C46 C47 113.1(2) . . ?
C42 C46 C48 109.1(2) . . ?
C48 C46 C47 111.9(3) . . ?
C37 C38 C43 122.6(2) . . ?
C39 C38 C37 117.1(2) . . ?
C39 C38 C43 120.2(2) . . ?
C45 C43 C38 112.2(2) . . ?
C44 C43 C38 111.4(3) . . ?
C44 C43 C45 111.6(3) . . ?
C13 C14 C19 121.8(2) . . ?
C15 C14 C13 117.6(2) . . ?
C15 C14 C19 120.6(2) . . ?
C3 C4 C5 119.8(2) . . ?
C1 C2 C7 123.0(2) . . ?
C3 C2 C1 117.8(2) . . ?
C3 C2 C7 119.1(2) . . ?
C25 C26 C31 122.4(2) . . ?
C27 C26 C25 118.2(2) . . ?
C27 C26 C31 119.2(2) . . ?
C28 C29 C30 121.4(3) . . ?
C14 C19 C21 108.2(3) . . ?
C14 C19 C20 113.1(3) . . ?
C14 C19 C20A 106.4(6) . . ?
C20 C19 C21 110.1(4) . . ?
C21A C19 C14 119.3(9) . . ?
C21A C19 C20A 111.7(10) . . ?
C6 C10 C11 112.2(2) . . ?
C12 C10 C6 110.6(2) . . ?
C12 C10 C11 109.5(2) . . ?
C32 C31 C26 112.0(2) . . ?
C32 C31 C33 110.9(3) . . ?
C33 C31 C26 112.4(3) . . ?
C28 C27 C26 121.1(3) . . ?
C16 C17 C18 121.3(3) . . ?
C2 C7 C9 112.3(3) . . ?
C8 C7 C2 111.8(3) . . ?
C8 C7 C9 109.5(3) . . ?
C40 C41 C42 120.6(3) . . ?
C27 C28 C29 120.1(3) . . ?
C16 C15 C14 121.5(3) . . ?
C17 C16 C15 120.0(2) . . ?
C40 C39 C38 121.4(3) . . ?
C39 C40 C41 120.6(3) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_23
_database_code_depnum_ccdc_archive 'CCDC 1972014'
loop_
_audit_author_name
_audit_author_address
'Alasdair McKay'
;Monash University
Australia
;
_audit_update_record             
;
2019-12-14 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_audit_creation_date             2019-12-14
_audit_creation_method           
;
Olex2 1.3-alpha
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
''
alasdair.mckay@monash.edu
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C29 H34 Cl2 K N3 O5 Sn W'
_chemical_formula_sum            'C29 H34 Cl2 K N3 O5 Sn W'
_chemical_formula_weight         917.13
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.3890(7)
_cell_length_b                   16.2162(8)
_cell_length_c                   18.0413(9)
_cell_angle_alpha                113.9600(10)
_cell_angle_beta                 93.105(2)
_cell_angle_gamma                91.697(2)
_cell_volume                     3568.6(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9881
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.387
_cell_measurement_theta_min      2.48
_shelx_estimated_absorpt_T_max   0.849
_shelx_estimated_absorpt_T_min   0.677
_exptl_absorpt_coefficient_mu    4.225
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6957
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0842 before and 0.0567 after correction. The Ratio of minimum to maximum transmission is 0.9333. The λ/2 correction factor is 0.00150.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1784
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            62536
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.429
_diffrn_reflns_theta_min         1.238
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9472
_reflns_number_total             14648
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max         3.719
_refine_diff_density_min         -3.898
_refine_diff_density_rms         0.158
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     792
_refine_ls_number_reflns         14648
_refine_ls_number_restraints     821
_refine_ls_R_factor_all          0.1082
_refine_ls_R_factor_gt           0.0561
_refine_ls_restrained_S_all      1.094
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0427P)²+37.3138P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1591
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
W2A \\sim Sn2A \\sim W2 \\sim Sn2: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(W2A)=Sof(Sn2A)=1-FVAR(1)
 Sof(W2)=Sof(Sn2)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C17(H17), C56(H56), C41(H41), C53(H53), C32(H32), C20(H20), C29(H29), C44(H44)
5.b Aromatic/amide H refined with riding coordinates:
 C49(H49), C13(H13), C37(H37), C14(H14), C51(H51), C26(H26), C27(H27),
 C39(H39), C50(H50), C25(H25), C15(H15), C38(H38)
5.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C34(H34A,H34B,H34C), C46(H46A,H46B,
 H46C), C42(H42A,H42B,H42C), C22(H22A,H22B,H22C), C43(H43A,H43B,H43C), C55(H55A,
 H55B,H55C), C33(H33A,H33B,H33C), C18(H18A,H18B,H18C), C58(H58A,H58B,H58C),
 C45(H45A,H45B,H45C), C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C57(H57A,H57B,
 H57C), C54(H54A,H54B,H54C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 1.24092(3) 0.45774(3) 1.02638(2) 0.04925(14) Uani 1 1 d . . . . .
W2 W 1.22278(8) 0.57615(5) 0.44267(4) 0.0561(3) Uani 0.781(3) 1 d . U P A 1
Sn1 Sn 1.17207(4) 0.36371(4) 0.86740(3) 0.03577(15) Uani 1 1 d . . . . .
Sn2 Sn 1.28882(7) 0.65678(9) 0.60503(7) 0.0337(3) Uani 0.781(3) 1 d . U P A 1
Cl1 Cl 1.2558(2) 0.45274(16) 0.79789(15) 0.0531(6) Uani 1 1 d . . . . .
Cl2 Cl 1.01373(18) 0.39704(17) 0.81952(18) 0.0574(6) Uani 1 1 d . . . . .
K1 K 1.0861(2) 0.58397(17) 0.80879(18) 0.0744(8) Uani 1 1 d . . . . .
Cl4 Cl 1.1882(2) 0.55648(18) 0.65561(17) 0.0651(7) Uani 1 1 d . . . . .
K2 K 1.3528(3) 0.4153(2) 0.6410(2) 0.0950(10) Uani 1 1 d . . . . .
Cl3 Cl 1.4415(2) 0.5997(2) 0.6410(3) 0.0877(10) Uani 1 1 d . . . . .
N6 N 1.2646(5) 0.7640(4) 0.7213(4) 0.0395(16) Uani 1 1 d . . . . .
N1 N 1.1031(5) 0.2096(4) 0.8320(4) 0.0369(15) Uani 1 1 d . . . . .
N5 N 1.3292(5) 0.8294(5) 0.7266(4) 0.0395(16) Uani 1 1 d . . . . .
N3 N 1.2084(5) 0.2453(4) 0.7656(4) 0.0355(15) Uani 1 1 d . . . . .
N2 N 1.1574(5) 0.1778(4) 0.7720(4) 0.0369(15) Uani 1 1 d . . . . .
N4 N 1.3807(6) 0.8024(5) 0.6649(4) 0.0409(16) Uani 1 1 d . . . . .
O2 O 1.0668(6) 0.3683(6) 1.0849(5) 0.081(2) Uani 1 1 d . . . . .
C47 C 1.2002(7) 0.7790(6) 0.7854(5) 0.0422(18) Uani 1 1 d . . . . .
O4 O 1.4197(6) 0.5447(7) 0.9676(6) 0.092(3) Uani 1 1 d . . . . .
C11 C 1.0470(7) 0.1435(5) 0.8498(5) 0.0404(18) Uani 1 1 d . . . . .
C35 C 1.4543(7) 0.8650(6) 0.6590(5) 0.0419(18) Uani 1 1 d . . . . .
C36 C 1.4300(8) 0.9102(6) 0.6098(6) 0.049(2) Uani 1 1 d . . . . .
C48 C 1.2405(8) 0.7875(6) 0.8619(6) 0.053(2) Uani 1 1 d . . . . .
C12 C 1.0912(8) 0.1031(6) 0.8969(6) 0.049(2) Uani 1 1 d . . . . .
C23 C 1.2722(7) 0.2262(5) 0.7008(5) 0.0430(18) Uani 1 1 d . . . . .
O1 O 1.2995(8) 0.5715(8) 1.2045(5) 0.109(4) Uani 1 1 d . . . . .
C24 C 1.2309(9) 0.2108(7) 0.6226(6) 0.057(2) Uani 1 1 d . . . . .
C52 C 1.0967(8) 0.7812(6) 0.7695(6) 0.053(2) Uani 1 1 d . . . . .
C2 C 1.1280(8) 0.4017(7) 1.0622(6) 0.056(3) Uani 1 1 d . . . . .
C17 C 1.1994(8) 0.1240(8) 0.9288(7) 0.061(2) Uani 1 1 d . . . . .
H17 H 1.224532 0.175492 0.916605 0.073 Uiso 1 1 calc R U . . .
O3 O 1.3873(7) 0.3085(8) 1.0245(7) 0.109(4) Uani 1 1 d . . . . .
C49 C 1.1719(10) 0.7990(7) 0.9219(7) 0.067(3) Uani 1 1 d . . . . .
H49 H 1.196730 0.806218 0.974620 0.080 Uiso 1 1 calc R U . . .
C16 C 0.9451(8) 0.1262(7) 0.8224(7) 0.059(2) Uani 1 1 d . . . . .
C28 C 1.3761(8) 0.2278(7) 0.7177(7) 0.060(2) Uani 1 1 d . . . . .
C40 C 1.5492(8) 0.8752(8) 0.6987(7) 0.063(3) Uani 1 1 d . . . . .
C56 C 1.0546(9) 0.7764(8) 0.6887(7) 0.068(3) Uani 1 1 d . . . . .
H56 H 1.098750 0.738817 0.646220 0.082 Uiso 1 1 calc R U . . .
C41 C 1.3268(8) 0.9009(7) 0.5690(7) 0.057(2) Uani 1 1 d . . . . .
H41 H 1.295437 0.841102 0.561565 0.068 Uiso 1 1 calc R U . . .
C4 C 1.3561(9) 0.5131(8) 0.9892(6) 0.061(3) Uani 1 1 d . . . . .
C53 C 1.3499(9) 0.7823(8) 0.8812(7) 0.067(3) Uani 1 1 d . . . . .
H53 H 1.387344 0.793492 0.839411 0.081 Uiso 1 1 calc R U . . .
C13 C 1.0336(9) 0.0407(7) 0.9138(6) 0.064(3) Uani 1 1 d . . . . .
H13 H 1.063390 0.010546 0.944121 0.077 Uiso 1 1 calc R U . . .
C37 C 1.5035(9) 0.9679(7) 0.6023(7) 0.066(3) Uani 1 1 d . . . . .
H37 H 1.488295 1.000881 0.570436 0.080 Uiso 1 1 calc R U . . .
C32 C 1.1201(10) 0.2109(8) 0.6030(7) 0.071(3) Uani 1 1 d . . . . .
H32 H 1.085471 0.217053 0.652569 0.085 Uiso 1 1 calc R U . . .
C14 C 0.9348(10) 0.0225(8) 0.8872(7) 0.074(3) Uani 1 1 d . . . . .
H14 H 0.896333 -0.019552 0.899934 0.089 Uiso 1 1 calc R U . . .
C3 C 1.3331(8) 0.3617(9) 1.0255(8) 0.070(3) Uani 1 1 d . . . . .
C51 C 1.0346(9) 0.7921(7) 0.8323(7) 0.066(3) Uani 1 1 d . . . . .
H51 H 0.964397 0.794059 0.823088 0.079 Uiso 1 1 calc R U . . .
C20 C 0.8989(9) 0.1654(9) 0.7662(9) 0.084(3) Uani 1 1 d . . . . .
H20 H 0.942918 0.218511 0.770961 0.101 Uiso 1 1 calc R U . . .
C26 C 1.3981(12) 0.1994(8) 0.5776(9) 0.084(3) Uani 1 1 d . . . . .
H26 H 1.441534 0.190555 0.535347 0.101 Uiso 1 1 calc R U . . .
O5 O 1.1143(9) 0.6124(7) 1.0110(7) 0.120(4) Uani 1 1 d . . . . .
C5 C 1.1573(10) 0.5564(8) 1.0193(7) 0.070(3) Uani 1 1 d . . . . .
C29 C 1.4199(8) 0.2430(9) 0.8016(8) 0.080(3) Uani 1 1 d . . . . .
H29 H 1.365402 0.263864 0.839754 0.096 Uiso 1 1 calc R U . . .
O10 O 1.2813(12) 0.3993(7) 0.4712(7) 0.144(5) Uani 1 1 d . . . . .
O7 O 1.4407(11) 0.6012(9) 0.3946(11) 0.161(6) Uani 1 1 d . . . . .
C27 C 1.4375(10) 0.2150(8) 0.6545(9) 0.081(3) Uani 1 1 d . . . . .
H27 H 1.508140 0.217147 0.664709 0.098 Uiso 1 1 calc R U . . .
C39 C 1.6204(9) 0.9328(9) 0.6862(8) 0.078(3) Uani 1 1 d . . . . .
H39 H 1.686420 0.939871 0.710969 0.094 Uiso 1 1 calc R U . . .
C50 C 1.0729(10) 0.8000(8) 0.9065(8) 0.073(3) Uani 1 1 d . . . . .
H50 H 1.029006 0.806401 0.947848 0.088 Uiso 1 1 calc R U . . .
C25 C 1.2974(11) 0.1965(8) 0.5618(7) 0.078(3) Uani 1 1 d . . . . .
H25 H 1.271371 0.184345 0.508165 0.093 Uiso 1 1 calc R U . . .
C15 C 0.8907(9) 0.0637(8) 0.8429(8) 0.072(3) Uani 1 1 d . . . . .
H15 H 0.821658 0.050157 0.825351 0.086 Uiso 1 1 calc R U . . .
C44 C 1.5754(9) 0.8314(9) 0.7562(8) 0.076(3) Uani 1 1 d . . . . .
H44 H 1.519060 0.787014 0.751032 0.091 Uiso 1 1 calc R U . . .
C38 C 1.5975(9) 0.9782(9) 0.6400(8) 0.078(3) Uani 1 1 d . . . . .
H38 H 1.646801 1.017661 0.633580 0.094 Uiso 1 1 calc R U . . .
C9 C 1.0836(13) 0.5760(12) 0.4765(12) 0.113(5) Uani 1 1 d . . . . .
C19 C 1.2126(11) 0.1545(11) 1.0211(8) 0.096(4) Uani 1 1 d . . . . .
H19A H 1.191700 0.104468 1.035137 0.144 Uiso 1 1 calc R U . . .
H19B H 1.171274 0.205846 1.047601 0.144 Uiso 1 1 calc R U . . .
H19C H 1.283106 0.172623 1.039703 0.144 Uiso 1 1 calc R U . . .
O6 O 1.1393(15) 0.4591(11) 0.2693(7) 0.199(8) Uani 1 1 d . . . . .
C21 C 0.8965(12) 0.0947(12) 0.6782(9) 0.107(5) Uani 1 1 d . . . . .
H21A H 0.842346 0.048839 0.668631 0.161 Uiso 1 1 calc R U . . .
H21B H 0.960690 0.065921 0.668679 0.161 Uiso 1 1 calc R U . . .
H21C H 0.885020 0.124281 0.640874 0.161 Uiso 1 1 calc R U . . .
C1 C 1.2758(12) 0.5320(11) 1.1391(8) 0.098(4) Uani 1 1 d . . . . .
O9 O 1.0004(10) 0.5822(10) 0.4986(10) 0.159(6) Uani 1 1 d . . . . .
C10 C 1.2581(14) 0.4639(10) 0.4606(8) 0.102(5) Uani 1 1 d . . . . .
C6 C 1.1695(18) 0.5002(13) 0.3355(10) 0.145(7) Uani 1 1 d . . . . .
C34 C 1.0795(13) 0.1233(11) 0.5341(10) 0.120(6) Uani 1 1 d . . . . .
H34A H 1.093436 0.072429 0.548589 0.179 Uiso 1 1 calc R U . . .
H34B H 1.111972 0.115403 0.484469 0.179 Uiso 1 1 calc R U . . .
H34C H 1.007035 0.125370 0.524904 0.179 Uiso 1 1 calc R U . . .
C46 C 1.5836(13) 0.9026(12) 0.8434(9) 0.119(6) Uani 1 1 d . . . . .
H46A H 1.640610 0.945277 0.850895 0.179 Uiso 1 1 calc R U . . .
H46B H 1.593674 0.873228 0.880927 0.179 Uiso 1 1 calc R U . . .
H46C H 1.521895 0.935230 0.854424 0.179 Uiso 1 1 calc R U . . .
C42 C 1.2627(11) 0.9739(10) 0.6233(11) 0.116(5) Uani 1 1 d . . . . .
H42A H 1.259483 0.969416 0.675680 0.174 Uiso 1 1 calc R U . . .
H42B H 1.194936 0.965976 0.597078 0.174 Uiso 1 1 calc R U . . .
H42C H 1.292261 1.033504 0.632186 0.174 Uiso 1 1 calc R U . . .
C22 C 0.7939(11) 0.1981(10) 0.7882(13) 0.128(6) Uani 1 1 d . . . . .
H22A H 0.795249 0.236493 0.846506 0.193 Uiso 1 1 calc R U . . .
H22B H 0.746787 0.145897 0.774834 0.193 Uiso 1 1 calc R U . . .
H22C H 0.772614 0.232956 0.757218 0.193 Uiso 1 1 calc R U . . .
C43 C 1.3267(12) 0.9036(15) 0.4868(10) 0.147(8) Uani 1 1 d . . . . .
H43A H 1.369007 0.955735 0.490504 0.220 Uiso 1 1 calc R U . . .
H43B H 1.258108 0.909048 0.468170 0.220 Uiso 1 1 calc R U . . .
H43C H 1.353016 0.847928 0.448169 0.220 Uiso 1 1 calc R U . . .
O8 O 1.1738(15) 0.7415(11) 0.4035(12) 0.230(10) Uani 1 1 d . . . . .
C55 C 1.3910(13) 0.8516(13) 0.9644(10) 0.135(7) Uani 1 1 d . . . . .
H55A H 1.377111 0.912499 0.969046 0.203 Uiso 1 1 calc R U . . .
H55B H 1.463490 0.846953 0.970562 0.203 Uiso 1 1 calc R U . . .
H55C H 1.358736 0.840096 1.006977 0.203 Uiso 1 1 calc R U . . .
C33 C 1.0965(13) 0.2916(11) 0.5846(11) 0.119(6) Uani 1 1 d . . . . .
H33A H 1.132817 0.289533 0.538255 0.178 Uiso 1 1 calc R U . . .
H33B H 1.117002 0.347393 0.632288 0.178 Uiso 1 1 calc R U . . .
H33C H 1.024289 0.290262 0.571503 0.178 Uiso 1 1 calc R U . . .
C18 C 1.2622(12) 0.0440(11) 0.8844(12) 0.130(7) Uani 1 1 d . . . . .
H18A H 1.259808 0.032070 0.826495 0.195 Uiso 1 1 calc R U . . .
H18B H 1.235285 -0.009585 0.890540 0.195 Uiso 1 1 calc R U . . .
H18C H 1.331684 0.057964 0.907445 0.195 Uiso 1 1 calc R U . . .
C58 C 1.0570(17) 0.8705(11) 0.6894(11) 0.141(7) Uani 1 1 d . . . . .
H58A H 1.006147 0.905753 0.724029 0.211 Uiso 1 1 calc R U . . .
H58B H 1.043137 0.865796 0.633872 0.211 Uiso 1 1 calc R U . . .
H58C H 1.123382 0.900636 0.710691 0.211 Uiso 1 1 calc R U . . .
C45 C 1.6703(13) 0.7810(14) 0.7387(13) 0.147(7) Uani 1 1 d . . . . .
H45A H 1.668987 0.741901 0.680541 0.221 Uiso 1 1 calc R U . . .
H45B H 1.675357 0.744053 0.770149 0.221 Uiso 1 1 calc R U . . .
H45C H 1.728290 0.824426 0.754028 0.221 Uiso 1 1 calc R U . . .
C31 C 1.5043(14) 0.3145(13) 0.8327(13) 0.171(9) Uani 1 1 d . . . . .
H31A H 1.483273 0.369115 0.827012 0.257 Uiso 1 1 calc R U . . .
H31B H 1.562645 0.292233 0.801243 0.257 Uiso 1 1 calc R U . . .
H31C H 1.522151 0.328730 0.890187 0.257 Uiso 1 1 calc R U . . .
C30 C 1.4552(16) 0.1568(12) 0.8039(10) 0.137(7) Uani 1 1 d . . . . .
H30A H 1.509102 0.134892 0.767246 0.206 Uiso 1 1 calc R U . . .
H30B H 1.399248 0.111131 0.786408 0.206 Uiso 1 1 calc R U . . .
H30C H 1.480153 0.168168 0.859437 0.206 Uiso 1 1 calc R U . . .
C57 C 0.9505(12) 0.7340(16) 0.6655(12) 0.151(8) Uani 1 1 d . . . . .
H57A H 0.949587 0.672979 0.664221 0.227 Uiso 1 1 calc R U . . .
H57B H 0.928443 0.730515 0.611532 0.227 Uiso 1 1 calc R U . . .
H57C H 0.905227 0.770651 0.705383 0.227 Uiso 1 1 calc R U . . .
C54 C 1.3716(13) 0.6875(11) 0.8736(14) 0.145(8) Uani 1 1 d . . . . .
H54A H 1.357461 0.682062 0.924243 0.218 Uiso 1 1 calc R U . . .
H54B H 1.442173 0.676742 0.863436 0.218 Uiso 1 1 calc R U . . .
H54C H 1.329031 0.642881 0.828390 0.218 Uiso 1 1 calc R U . . .
C7 C 1.3665(16) 0.5912(12) 0.4128(12) 0.122(6) Uani 1 1 d . . . . .
C8 C 1.1861(14) 0.6866(12) 0.4266(12) 0.133(6) Uani 1 1 d . . . . .
W2A W 1.2726(5) 0.5595(2) 0.4531(3) 0.143(2) Uani 0.219(3) 1 d . U P A 2
Sn2A Sn 1.3355(12) 0.6566(5) 0.6075(5) 0.163(3) Uani 0.219(3) 1 d . U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 Sn1 2.7349(7) . ?
W1 C2 2.007(11) . ?
W1 C4 2.038(11) . ?
W1 C3 2.011(14) . ?
W1 C5 2.022(13) . ?
W1 C1 1.918(13) . ?
W2 Sn2 2.7590(14) . ?
W2 C9 1.992(19) . ?
W2 C10 2.038(16) . ?
W2 C6 1.905(16) . ?
W2 C7 2.06(2) . ?
W2 C8 1.998(18) . ?
Sn1 Cl1 2.538(2) . ?
Sn1 Cl2 2.404(3) . ?
Sn1 N1 2.451(7) . ?
Sn1 N3 2.140(7) . ?
Sn2 Cl4 2.550(3) . ?
Sn2 Cl3 2.432(3) . ?
Sn2 N6 2.162(7) . ?
Sn2 N4 2.422(7) . ?
Cl1 K1 3.118(4) . ?
Cl1 K2 3.020(4) . ?
Cl2 K1 3.239(4) . ?
K1 Cl4 3.025(4) . ?
K1 K2 4.941(4) . ?
K1 O2 2.790(9) 2_767 ?
K1 C49 3.372(12) . ?
K1 C51 3.325(11) . ?
K1 C50 3.236(12) . ?
K1 O6 3.194(18) 2_766 ?
Cl4 K2 3.168(4) . ?
K2 Cl3 3.185(4) . ?
K2 C24 3.535(11) . ?
K2 C26 3.300(12) . ?
K2 O10 3.063(13) . ?
K2 O7 2.869(14) 2_866 ?
K2 C25 3.286(13) . ?
Cl3 Sn2A 1.914(12) . ?
N6 N5 1.319(9) . ?
N6 C47 1.425(11) . ?
N6 Sn2A 2.357(12) . ?
N1 N2 1.272(9) . ?
N1 C11 1.440(10) . ?
N5 N4 1.270(10) . ?
N3 N2 1.321(9) . ?
N3 C23 1.423(11) . ?
N4 C35 1.433(11) . ?
N4 Sn2A 2.211(11) . ?
O2 C2 1.151(12) . ?
C47 C48 1.405(13) . ?
C47 C52 1.405(14) . ?
O4 C4 1.145(12) . ?
C11 C12 1.387(13) . ?
C11 C16 1.406(14) . ?
C35 C36 1.393(13) . ?
C35 C40 1.395(14) . ?
C36 C41 1.504(14) . ?
C36 C37 1.387(13) . ?
C48 C49 1.415(15) . ?
C48 C53 1.500(16) . ?
C12 C17 1.506(15) . ?
C12 C13 1.393(13) . ?
C23 C24 1.407(14) . ?
C23 C28 1.406(14) . ?
O1 C1 1.112(14) . ?
C24 C32 1.506(16) . ?
C24 C25 1.399(15) . ?
C52 C56 1.505(15) . ?
C52 C51 1.397(14) . ?
C17 H17 1.0000 . ?
C17 C19 1.530(16) . ?
C17 C18 1.525(18) . ?
O3 C3 1.138(15) . ?
C49 H49 0.9500 . ?
C49 C50 1.342(17) . ?
C16 C20 1.514(16) . ?
C16 C15 1.409(14) . ?
C28 C29 1.513(17) . ?
C28 C27 1.392(15) . ?
C40 C39 1.404(16) . ?
C40 C44 1.511(16) . ?
C56 H56 1.0000 . ?
C56 C58 1.521(19) . ?
C56 C57 1.496(18) . ?
C41 H41 1.0000 . ?
C41 C42 1.519(18) . ?
C41 C43 1.501(17) . ?
C53 H53 1.0000 . ?
C53 C55 1.524(18) . ?
C53 C54 1.524(18) . ?
C13 H13 0.9500 . ?
C13 C14 1.364(17) . ?
C37 H37 0.9500 . ?
C37 C38 1.370(17) . ?
C32 H32 1.0000 . ?
C32 C34 1.519(18) . ?
C32 C33 1.513(17) . ?
C14 H14 0.9500 . ?
C14 C15 1.357(17) . ?
C51 H51 0.9500 . ?
C51 C50 1.360(17) . ?
C20 H20 1.0000 . ?
C20 C21 1.53(2) . ?
C20 C22 1.532(19) . ?
C26 H26 0.9500 . ?
C26 C27 1.377(19) . ?
C26 C25 1.359(19) . ?
O5 C5 1.144(14) . ?
C29 H29 1.0000 . ?
C29 C31 1.504(19) . ?
C29 C30 1.50(2) . ?
O10 C10 1.186(17) . ?
O7 C7 1.090(19) . ?
C27 H27 0.9500 . ?
C39 H39 0.9500 . ?
C39 C38 1.347(17) . ?
C50 H50 0.9500 . ?
C25 H25 0.9500 . ?
C15 H15 0.9500 . ?
C44 H44 1.0000 . ?
C44 C46 1.522(19) . ?
C44 C45 1.510(19) . ?
C38 H38 0.9500 . ?
C9 O9 1.20(2) . ?
C9 W2A 2.59(2) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
O6 C6 1.149(18) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C10 W2A 1.618(15) . ?
C6 W2A 2.298(17) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
O8 C8 1.137(18) . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C7 W2A 1.655(18) . ?
C8 W2A 2.588(19) . ?
W2A Sn2A 2.656(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 W1 Sn1 90.3(3) . . ?
C2 W1 C4 179.3(5) . . ?
C2 W1 C3 91.9(5) . . ?
C2 W1 C5 93.4(5) . . ?
C4 W1 Sn1 89.3(3) . . ?
C3 W1 Sn1 93.5(3) . . ?
C3 W1 C4 87.5(5) . . ?
C3 W1 C5 174.2(5) . . ?
C5 W1 Sn1 84.2(3) . . ?
C5 W1 C4 87.1(5) . . ?
C1 W1 Sn1 173.3(5) . . ?
C1 W1 C2 87.6(5) . . ?
C1 W1 C4 92.9(5) . . ?
C1 W1 C3 92.9(6) . . ?
C1 W1 C5 89.6(6) . . ?
C9 W2 Sn2 88.4(5) . . ?
C9 W2 C10 94.4(7) . . ?
C9 W2 C7 173.8(7) . . ?
C9 W2 C8 84.6(8) . . ?
C10 W2 Sn2 80.6(4) . . ?
C10 W2 C7 90.8(7) . . ?
C6 W2 Sn2 168.4(5) . . ?
C6 W2 C9 86.8(9) . . ?
C6 W2 C10 89.2(7) . . ?
C6 W2 C7 96.6(9) . . ?
C6 W2 C8 91.1(8) . . ?
C7 W2 Sn2 89.2(6) . . ?
C8 W2 Sn2 98.9(5) . . ?
C8 W2 C10 178.9(8) . . ?
C8 W2 C7 90.2(8) . . ?
Cl1 Sn1 W1 102.22(6) . . ?
Cl2 Sn1 W1 119.61(7) . . ?
Cl2 Sn1 Cl1 87.65(9) . . ?
Cl2 Sn1 N1 88.41(18) . . ?
N1 Sn1 W1 115.67(16) . . ?
N1 Sn1 Cl1 138.24(18) . . ?
N3 Sn1 W1 137.63(19) . . ?
N3 Sn1 Cl1 86.18(19) . . ?
N3 Sn1 Cl2 102.0(2) . . ?
N3 Sn1 N1 54.2(2) . . ?
Cl4 Sn2 W2 98.76(8) . . ?
Cl3 Sn2 W2 115.09(11) . . ?
Cl3 Sn2 Cl4 88.86(12) . . ?
N6 Sn2 W2 144.7(2) . . ?
N6 Sn2 Cl4 84.92(19) . . ?
N6 Sn2 Cl3 100.0(2) . . ?
N6 Sn2 N4 54.6(3) . . ?
N4 Sn2 W2 122.60(18) . . ?
N4 Sn2 Cl4 136.79(19) . . ?
N4 Sn2 Cl3 84.70(19) . . ?
Sn1 Cl1 K1 98.06(9) . . ?
Sn1 Cl1 K2 138.11(11) . . ?
K2 Cl1 K1 107.22(11) . . ?
Sn1 Cl2 K1 97.78(10) . . ?
Cl1 K1 Cl2 65.14(8) . . ?
Cl1 K1 K2 35.71(6) . . ?
Cl1 K1 C49 109.9(3) . . ?
Cl1 K1 C51 145.3(2) . . ?
Cl1 K1 C50 132.9(3) . . ?
Cl1 K1 O6 129.8(3) . 2_766 ?
Cl2 K1 K2 87.21(8) . . ?
Cl2 K1 C49 143.3(2) . . ?
Cl2 K1 C51 148.3(2) . . ?
Cl4 K1 Cl1 73.72(9) . . ?
Cl4 K1 Cl2 113.62(11) . . ?
Cl4 K1 K2 38.08(7) . . ?
Cl4 K1 C49 98.1(2) . . ?
Cl4 K1 C51 90.2(2) . . ?
Cl4 K1 C50 106.2(2) . . ?
Cl4 K1 O6 97.9(3) . 2_766 ?
O2 K1 Cl1 128.3(2) 2_767 . ?
O2 K1 Cl2 75.45(19) 2_767 . ?
O2 K1 Cl4 156.4(2) 2_767 . ?
O2 K1 K2 161.9(2) 2_767 . ?
O2 K1 C49 82.7(3) 2_767 . ?
O2 K1 C51 74.9(3) 2_767 . ?
O2 K1 C50 66.5(3) 2_767 . ?
O2 K1 O6 62.5(3) 2_767 2_766 ?
C49 K1 K2 109.4(2) . . ?
C51 K1 K2 123.1(2) . . ?
C51 K1 C49 41.1(3) . . ?
C50 K1 Cl2 140.1(2) . . ?
C50 K1 K2 128.9(2) . . ?
C50 K1 C49 23.3(3) . . ?
C50 K1 C51 23.9(3) . . ?
O6 K1 Cl2 74.5(3) 2_766 . ?
O6 K1 K2 118.0(3) 2_766 . ?
O6 K1 C49 120.4(4) 2_766 . ?
O6 K1 C51 82.0(4) 2_766 . ?
O6 K1 C50 97.3(4) 2_766 . ?
Sn2 Cl4 K1 135.70(12) . . ?
Sn2 Cl4 K2 97.66(11) . . ?
K1 Cl4 K2 105.84(11) . . ?
Cl1 K2 K1 37.07(7) . . ?
Cl1 K2 Cl4 73.07(9) . . ?
Cl1 K2 Cl3 109.77(13) . . ?
Cl1 K2 C24 72.62(18) . . ?
Cl1 K2 C26 102.6(2) . . ?
Cl1 K2 O10 135.5(3) . . ?
Cl1 K2 C25 95.3(2) . . ?
Cl4 K2 K1 36.08(6) . . ?
Cl4 K2 Cl3 66.61(9) . . ?
Cl4 K2 C24 108.4(2) . . ?
Cl4 K2 C26 145.7(3) . . ?
Cl4 K2 C25 121.9(3) . . ?
Cl3 K2 K1 88.96(9) . . ?
Cl3 K2 C24 172.8(2) . . ?
Cl3 K2 C26 141.4(3) . . ?
Cl3 K2 C25 154.9(2) . . ?
C24 K2 K1 89.41(18) . . ?
C26 K2 K1 129.5(2) . . ?
C26 K2 C24 41.1(3) . . ?
O10 K2 K1 102.3(3) . . ?
O10 K2 Cl4 70.3(3) . . ?
O10 K2 Cl3 77.6(2) . . ?
O10 K2 C24 95.9(3) . . ?
O10 K2 C26 94.0(4) . . ?
O10 K2 C25 83.5(3) . . ?
O7 K2 Cl1 130.6(4) 2_866 . ?
O7 K2 K1 150.5(4) 2_866 . ?
O7 K2 Cl4 136.3(3) 2_866 . ?
O7 K2 Cl3 70.3(3) 2_866 . ?
O7 K2 C24 113.6(3) 2_866 . ?
O7 K2 C26 72.8(4) 2_866 . ?
O7 K2 O10 93.7(5) 2_866 . ?
O7 K2 C25 94.8(4) 2_866 . ?
C25 K2 K1 111.3(2) . . ?
C25 K2 C24 23.3(3) . . ?
C25 K2 C26 23.8(3) . . ?
Sn2 Cl3 K2 99.77(13) . . ?
Sn2A Cl3 K2 108.5(4) . . ?
N5 N6 Sn2 103.5(5) . . ?
N5 N6 C47 119.0(7) . . ?
N5 N6 Sn2A 93.1(6) . . ?
C47 N6 Sn2 137.5(5) . . ?
C47 N6 Sn2A 146.6(6) . . ?
N2 N1 Sn1 91.6(5) . . ?
N2 N1 C11 115.5(7) . . ?
C11 N1 Sn1 152.1(5) . . ?
N4 N5 N6 109.5(7) . . ?
N2 N3 Sn1 105.1(5) . . ?
N2 N3 C23 119.0(6) . . ?
C23 N3 Sn1 135.8(5) . . ?
N1 N2 N3 108.9(6) . . ?
N5 N4 Sn2 92.4(5) . . ?
N5 N4 C35 117.7(7) . . ?
N5 N4 Sn2A 101.6(6) . . ?
C35 N4 Sn2 149.7(6) . . ?
C35 N4 Sn2A 139.9(7) . . ?
C2 O2 K1 139.9(8) . 2_767 ?
C48 C47 N6 119.8(9) . . ?
C48 C47 C52 121.3(9) . . ?
C52 C47 N6 118.9(8) . . ?
C12 C11 N1 120.6(8) . . ?
C12 C11 C16 121.6(8) . . ?
C16 C11 N1 117.7(8) . . ?
C36 C35 N4 118.4(8) . . ?
C36 C35 C40 122.1(9) . . ?
C40 C35 N4 119.4(9) . . ?
C35 C36 C41 121.9(8) . . ?
C37 C36 C35 117.6(10) . . ?
C37 C36 C41 120.4(9) . . ?
C47 C48 C49 116.8(10) . . ?
C47 C48 C53 123.5(9) . . ?
C49 C48 C53 119.7(10) . . ?
C11 C12 C17 121.7(8) . . ?
C11 C12 C13 118.6(10) . . ?
C13 C12 C17 119.7(9) . . ?
C24 C23 N3 119.7(9) . . ?
C28 C23 N3 118.7(9) . . ?
C28 C23 C24 121.5(9) . . ?
C23 C24 K2 89.3(6) . . ?
C23 C24 C32 122.8(9) . . ?
C32 C24 K2 110.4(7) . . ?
C25 C24 K2 68.3(6) . . ?
C25 C24 C23 117.4(11) . . ?
C25 C24 C32 119.8(11) . . ?
C47 C52 C56 120.9(9) . . ?
C51 C52 C47 117.9(10) . . ?
C51 C52 C56 121.1(10) . . ?
O2 C2 W1 176.6(10) . . ?
C12 C17 H17 107.2 . . ?
C12 C17 C19 112.4(10) . . ?
C12 C17 C18 110.7(11) . . ?
C19 C17 H17 107.2 . . ?
C18 C17 H17 107.2 . . ?
C18 C17 C19 111.7(12) . . ?
K1 C49 H49 111.1 . . ?
C48 C49 K1 87.1(6) . . ?
C48 C49 H49 119.0 . . ?
C50 C49 K1 72.6(7) . . ?
C50 C49 C48 122.0(11) . . ?
C50 C49 H49 119.0 . . ?
C11 C16 C20 121.3(9) . . ?
C11 C16 C15 116.9(10) . . ?
C15 C16 C20 121.5(10) . . ?
C23 C28 C29 121.3(10) . . ?
C27 C28 C23 117.7(11) . . ?
C27 C28 C29 121.1(11) . . ?
C35 C40 C39 117.0(11) . . ?
C35 C40 C44 122.9(10) . . ?
C39 C40 C44 120.0(11) . . ?
C52 C56 H56 107.9 . . ?
C52 C56 C58 109.9(10) . . ?
C58 C56 H56 107.9 . . ?
C57 C56 C52 113.4(12) . . ?
C57 C56 H56 107.9 . . ?
C57 C56 C58 109.8(14) . . ?
C36 C41 H41 107.7 . . ?
C36 C41 C42 110.1(10) . . ?
C42 C41 H41 107.7 . . ?
C43 C41 C36 113.5(10) . . ?
C43 C41 H41 107.7 . . ?
C43 C41 C42 109.8(13) . . ?
O4 C4 W1 178.9(10) . . ?
C48 C53 H53 107.4 . . ?
C48 C53 C55 114.5(12) . . ?
C48 C53 C54 110.3(10) . . ?
C55 C53 H53 107.4 . . ?
C55 C53 C54 109.6(13) . . ?
C54 C53 H53 107.4 . . ?
C12 C13 H13 119.7 . . ?
C14 C13 C12 120.6(11) . . ?
C14 C13 H13 119.7 . . ?
C36 C37 H37 119.4 . . ?
C38 C37 C36 121.3(11) . . ?
C38 C37 H37 119.4 . . ?
C24 C32 H32 107.5 . . ?
C24 C32 C34 112.3(11) . . ?
C24 C32 C33 110.6(11) . . ?
C34 C32 H32 107.5 . . ?
C33 C32 H32 107.5 . . ?
C33 C32 C34 111.2(12) . . ?
C13 C14 H14 119.5 . . ?
C15 C14 C13 120.9(10) . . ?
C15 C14 H14 119.5 . . ?
O3 C3 W1 178.1(11) . . ?
K1 C51 H51 108.8 . . ?
C52 C51 K1 87.3(6) . . ?
C52 C51 H51 119.4 . . ?
C50 C51 K1 74.4(7) . . ?
C50 C51 C52 121.3(11) . . ?
C50 C51 H51 119.4 . . ?
C16 C20 H20 108.0 . . ?
C16 C20 C21 109.2(11) . . ?
C16 C20 C22 112.6(13) . . ?
C21 C20 H20 108.0 . . ?
C22 C20 H20 108.0 . . ?
C22 C20 C21 110.8(12) . . ?
K2 C26 H26 102.9 . . ?
C27 C26 K2 89.7(8) . . ?
C27 C26 H26 119.9 . . ?
C25 C26 K2 77.5(7) . . ?
C25 C26 H26 119.9 . . ?
C25 C26 C27 120.2(12) . . ?
O5 C5 W1 175.1(12) . . ?
C28 C29 H29 107.6 . . ?
C31 C29 C28 113.0(14) . . ?
C31 C29 H29 107.6 . . ?
C31 C29 C30 109.4(14) . . ?
C30 C29 C28 111.4(11) . . ?
C30 C29 H29 107.6 . . ?
C10 O10 K2 120.8(10) . . ?
C7 O7 K2 163.6(16) . 2_866 ?
C28 C27 H27 119.3 . . ?
C26 C27 C28 121.4(13) . . ?
C26 C27 H27 119.3 . . ?
C40 C39 H39 119.2 . . ?
C38 C39 C40 121.6(12) . . ?
C38 C39 H39 119.2 . . ?
K1 C50 H50 104.5 . . ?
C49 C50 K1 84.1(7) . . ?
C49 C50 C51 120.8(11) . . ?
C49 C50 H50 119.6 . . ?
C51 C50 K1 81.7(7) . . ?
C51 C50 H50 119.6 . . ?
K2 C25 H25 103.4 . . ?
C24 C25 K2 88.4(7) . . ?
C24 C25 H25 119.1 . . ?
C26 C25 K2 78.7(8) . . ?
C26 C25 C24 121.8(12) . . ?
C26 C25 H25 119.1 . . ?
C16 C15 H15 119.3 . . ?
C14 C15 C16 121.4(11) . . ?
C14 C15 H15 119.3 . . ?
C40 C44 H44 107.8 . . ?
C40 C44 C46 109.6(11) . . ?
C46 C44 H44 107.8 . . ?
C45 C44 C40 113.8(13) . . ?
C45 C44 H44 107.8 . . ?
C45 C44 C46 109.8(13) . . ?
C37 C38 H38 119.8 . . ?
C39 C38 C37 120.4(11) . . ?
C39 C38 H38 119.8 . . ?
O9 C9 W2 175.5(16) . . ?
O9 C9 W2A 169.6(15) . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C6 O6 K1 129.9(19) . 2_766 ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O1 C1 W1 176.2(17) . . ?
O10 C10 W2 178.2(16) . . ?
O10 C10 W2A 157.8(18) . . ?
O6 C6 W2 175.3(17) . . ?
O6 C6 W2A 163(2) . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C53 C55 H55A 109.5 . . ?
C53 C55 H55B 109.5 . . ?
C53 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C56 C58 H58A 109.5 . . ?
C56 C58 H58B 109.5 . . ?
C56 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C56 C57 H57A 109.5 . . ?
C56 C57 H57B 109.5 . . ?
C56 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
O7 C7 W2 177(2) . . ?
O7 C7 W2A 163(2) . . ?
O8 C8 W2 167(2) . . ?
O8 C8 W2A 159(2) . . ?
C9 W2A Sn2A 95.3(5) . . ?
C10 W2A C9 86.0(8) . . ?
C10 W2A C6 88.3(8) . . ?
C10 W2A C7 126.3(10) . . ?
C10 W2A C8 146.4(8) . . ?
C10 W2A Sn2A 96.5(6) . . ?
C6 W2A C9 66.1(7) . . ?
C6 W2A C8 69.3(7) . . ?
C6 W2A Sn2A 160.4(7) . . ?
C7 W2A C9 143.8(9) . . ?
C7 W2A C6 95.7(9) . . ?
C7 W2A C8 82.1(9) . . ?
C7 W2A Sn2A 96.6(7) . . ?
C8 W2A C9 62.4(6) . . ?
C8 W2A Sn2A 97.4(5) . . ?
Cl3 Sn2A N6 110.8(4) . . ?
Cl3 Sn2A N4 104.7(6) . . ?
Cl3 Sn2A W2A 110.7(4) . . ?
N6 Sn2A W2A 135.0(6) . . ?
N4 Sn2A N6 55.0(3) . . ?
N4 Sn2A W2A 127.2(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Sn1 N1 N2 N3 -3.3(6) . . . . ?
Sn1 N1 C11 C12 -81.8(15) . . . . ?
Sn1 N1 C11 C16 94.2(13) . . . . ?
Sn1 N3 N2 N1 3.9(7) . . . . ?
Sn1 N3 C23 C24 -102.6(10) . . . . ?
Sn1 N3 C23 C28 74.1(11) . . . . ?
Sn2 N6 N5 N4 -2.7(8) . . . . ?
Sn2 N6 C47 C48 112.8(9) . . . . ?
Sn2 N6 C47 C52 -64.4(12) . . . . ?
Sn2 N4 C35 C36 74.0(14) . . . . ?
Sn2 N4 C35 C40 -102.4(13) . . . . ?
K1 C49 C50 C51 -76.7(11) . . . . ?
K1 C51 C50 C49 78.0(11) . . . . ?
K1 O6 C6 W2A 163(4) 2_766 . . . ?
K2 C24 C32 C34 133.4(10) . . . . ?
K2 C24 C32 C33 8.5(12) . . . . ?
K2 C24 C25 C26 75.6(11) . . . . ?
K2 C26 C27 C28 75.6(12) . . . . ?
K2 C26 C25 C24 -80.9(11) . . . . ?
K2 O10 C10 W2A 70(3) . . . . ?
K2 O7 C7 W2A 17(13) 2_866 . . . ?
N6 N5 N4 Sn2 2.3(7) . . . . ?
N6 N5 N4 C35 178.9(7) . . . . ?
N6 N5 N4 Sn2A -9.2(8) . . . . ?
N6 C47 C48 C49 -177.8(8) . . . . ?
N6 C47 C48 C53 0.5(14) . . . . ?
N6 C47 C52 C56 -5.7(13) . . . . ?
N6 C47 C52 C51 177.3(8) . . . . ?
N1 C11 C12 C17 -1.9(14) . . . . ?
N1 C11 C12 C13 178.9(9) . . . . ?
N1 C11 C16 C20 8.3(15) . . . . ?
N1 C11 C16 C15 -177.8(9) . . . . ?
N5 N6 C47 C48 -69.0(11) . . . . ?
N5 N6 C47 C52 113.8(9) . . . . ?
N5 N4 C35 C36 -99.2(10) . . . . ?
N5 N4 C35 C40 84.4(11) . . . . ?
N3 C23 C24 K2 112.1(7) . . . . ?
N3 C23 C24 C32 -1.8(14) . . . . ?
N3 C23 C24 C25 177.1(8) . . . . ?
N3 C23 C28 C29 4.2(14) . . . . ?
N3 C23 C28 C27 -175.7(9) . . . . ?
N2 N1 C11 C12 83.7(10) . . . . ?
N2 N1 C11 C16 -100.3(10) . . . . ?
N2 N3 C23 C24 79.9(10) . . . . ?
N2 N3 C23 C28 -103.4(10) . . . . ?
N4 C35 C36 C41 5.4(13) . . . . ?
N4 C35 C36 C37 -177.5(9) . . . . ?
N4 C35 C40 C39 175.7(10) . . . . ?
N4 C35 C40 C44 -7.5(16) . . . . ?
C47 N6 N5 N4 178.6(7) . . . . ?
C47 C48 C49 K1 68.8(8) . . . . ?
C47 C48 C49 C50 1.3(16) . . . . ?
C47 C48 C53 C55 138.2(12) . . . . ?
C47 C48 C53 C54 -97.6(14) . . . . ?
C47 C52 C56 C58 -85.7(14) . . . . ?
C47 C52 C56 C57 151.0(13) . . . . ?
C47 C52 C51 K1 -70.2(8) . . . . ?
C47 C52 C51 C50 -0.3(15) . . . . ?
C11 N1 N2 N3 -176.5(7) . . . . ?
C11 C12 C17 C19 125.8(11) . . . . ?
C11 C12 C17 C18 -108.5(13) . . . . ?
C11 C12 C13 C14 -2.5(16) . . . . ?
C11 C16 C20 C21 96.8(12) . . . . ?
C11 C16 C20 C22 -139.7(11) . . . . ?
C11 C16 C15 C14 0.2(18) . . . . ?
C35 C36 C41 C42 91.1(13) . . . . ?
C35 C36 C41 C43 -145.4(13) . . . . ?
C35 C36 C37 C38 1.9(17) . . . . ?
C35 C40 C39 C38 1.9(19) . . . . ?
C35 C40 C44 C46 -106.3(14) . . . . ?
C35 C40 C44 C45 130.4(14) . . . . ?
C36 C35 C40 C39 -0.6(16) . . . . ?
C36 C35 C40 C44 176.2(10) . . . . ?
C36 C37 C38 C39 -1(2) . . . . ?
C48 C47 C52 C56 177.2(9) . . . . ?
C48 C47 C52 C51 0.1(14) . . . . ?
C48 C49 C50 K1 75.1(10) . . . . ?
C48 C49 C50 C51 -1.6(18) . . . . ?
C12 C11 C16 C20 -175.7(11) . . . . ?
C12 C11 C16 C15 -1.9(15) . . . . ?
C12 C13 C14 C15 0.9(19) . . . . ?
C23 N3 N2 N1 -178.0(7) . . . . ?
C23 C24 C32 C34 -123.7(12) . . . . ?
C23 C24 C32 C33 111.4(13) . . . . ?
C23 C24 C25 K2 -77.2(8) . . . . ?
C23 C24 C25 C26 -1.6(17) . . . . ?
C23 C28 C29 C31 -130.8(13) . . . . ?
C23 C28 C29 C30 105.6(14) . . . . ?
C23 C28 C27 C26 -1.4(17) . . . . ?
C24 C23 C28 C29 -179.1(10) . . . . ?
C24 C23 C28 C27 1.0(15) . . . . ?
C52 C47 C48 C49 -0.6(13) . . . . ?
C52 C47 C48 C53 177.7(9) . . . . ?
C52 C51 C50 K1 -76.9(10) . . . . ?
C52 C51 C50 C49 1.1(18) . . . . ?
C17 C12 C13 C14 178.3(11) . . . . ?
C49 C48 C53 C55 -43.6(16) . . . . ?
C49 C48 C53 C54 80.6(15) . . . . ?
C16 C11 C12 C17 -177.8(10) . . . . ?
C16 C11 C12 C13 3.0(14) . . . . ?
C28 C23 C24 K2 -64.5(9) . . . . ?
C28 C23 C24 C32 -178.5(10) . . . . ?
C28 C23 C24 C25 0.5(14) . . . . ?
C40 C35 C36 C41 -178.3(10) . . . . ?
C40 C35 C36 C37 -1.2(15) . . . . ?
C40 C39 C38 C37 -1(2) . . . . ?
C56 C52 C51 K1 112.7(9) . . . . ?
C56 C52 C51 C50 -177.4(11) . . . . ?
C41 C36 C37 C38 179.0(11) . . . . ?
C53 C48 C49 K1 -109.6(9) . . . . ?
C53 C48 C49 C50 -177.0(11) . . . . ?
C13 C12 C17 C19 -55.1(14) . . . . ?
C13 C12 C17 C18 70.7(14) . . . . ?
C13 C14 C15 C16 0(2) . . . . ?
C37 C36 C41 C42 -85.9(13) . . . . ?
C37 C36 C41 C43 37.6(16) . . . . ?
C32 C24 C25 K2 101.8(9) . . . . ?
C32 C24 C25 C26 177.3(11) . . . . ?
C51 C52 C56 C58 91.2(15) . . . . ?
C51 C52 C56 C57 -32.1(17) . . . . ?
C20 C16 C15 C14 174.0(12) . . . . ?
C29 C28 C27 C26 178.7(12) . . . . ?
O10 C10 W2A C9 -160(3) . . . . ?
O10 C10 W2A C6 134(3) . . . . ?
O10 C10 W2A C7 38(4) . . . . ?
O10 C10 W2A C8 -179(3) . . . . ?
O10 C10 W2A Sn2A -65(3) . . . . ?
O7 C7 W2A C9 175(6) . . . . ?
O7 C7 W2A C10 -37(7) . . . . ?
O7 C7 W2A C6 -129(7) . . . . ?
O7 C7 W2A C8 163(7) . . . . ?
O7 C7 W2A Sn2A 66(7) . . . . ?
C27 C28 C29 C31 49.1(17) . . . . ?
C27 C28 C29 C30 -74.5(17) . . . . ?
C27 C26 C25 K2 82.2(12) . . . . ?
C27 C26 C25 C24 1.3(19) . . . . ?
C39 C40 C44 C46 70.5(16) . . . . ?
C39 C40 C44 C45 -52.9(18) . . . . ?
C25 C24 C32 C34 57.4(15) . . . . ?
C25 C24 C32 C33 -67.5(15) . . . . ?
C25 C26 C27 C28 0(2) . . . . ?
C15 C16 C20 C21 -76.8(15) . . . . ?
C15 C16 C20 C22 46.8(16) . . . . ?
C44 C40 C39 C38 -175.1(13) . . . . ?
Sn2A N6 N5 N4 8.4(7) . . . . ?
Sn2A N6 C47 C48 93.0(13) . . . . ?
Sn2A N6 C47 C52 -84.3(14) . . . . ?
Sn2A N4 C35 C36 93.2(12) . . . . ?
Sn2A N4 C35 C40 -83.3(13) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_PLAT430_23                  
;
PROBLEM: Short Inter D...A Contact  O9       ..O9       .       2.69 Ang.  
RESPONSE: These short contacts arise as this compound crystallises as a 
network polymer.
;
_vrf_PLAT971_23                  
;
PROBLEM: Check Calcd Resid. Dens.  0.73A   From W2A             3.32 eA-3  
RESPONSE: The Fourier difference map revealed large peaks of electron density 
proximal to W2 and Sn2. Twinning was investigated, but a suitable twin law was 
not found. W2 and Sn2 were modelled as disordered over two sites, with 
occupancies refining to 0.78/0.22. Residual peaks of electron density are noted 
proximate to these atoms. 
;
_vrf_PLAT972_23                  
;
PROBLEM: Check Calcd Resid. Dens.  0.31A   From W2A            -3.10 eA-3  
RESPONSE: The Fourier difference map revealed large peaks of electron density 
proximal to W2 and Sn2. Twinning was investigated, but a suitable twin law was 
not found. W2 and Sn2 were modelled as disordered over two sites, with 
occupancies refining to 0.78/0.22. Residual peaks of electron density are noted 
proximate to these atoms.
;
_vrf_PLAT974_23                  
;
PROBLEM: Check Calcd Negative Resid. Density on      Sn2A      -1.76 eA-3  
RESPONSE: The Fourier difference map revealed large peaks of electron density 
proximal to W2 and Sn2. Twinning was investigated, but a suitable twin law was 
not found. W2 and Sn2 were modelled as disordered over two sites, with 
occupancies refining to 0.78/0.22. Residual peaks of electron density are noted 
proximate to these atoms.
;
# end Validation Reply Form
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
