# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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. 
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data_p17463final
_database_code_depnum_ccdc_archive 'CCDC 1824471'
_audit_update_record             
;
2018-02-16 deposited with the CCDC.
2018-06-22 downloaded from the CCDC.
;
_audit_creation_date             2017-12-14
_audit_creation_method           
;
Olex2 1.2
(compiled Aug 10 2017 17:28:52 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        
'5-azoniaspiro[4.4]nonane 10-phenyl-9-phosphatriptycene-10-borate'
_chemical_formula_moiety         'C24 H17 B P, C4 H8 O, C8 H16 N'
_chemical_formula_sum            'C36 H41 B N O P'
_chemical_formula_weight         545.48
_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'
B B 0.0013 0.0007 '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'
P P 0.1023 0.0942 '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                   10.0854(10)
_cell_length_b                   17.8383(16)
_cell_length_c                   16.1920(16)
_cell_angle_alpha                90
_cell_angle_beta                 96.009(4)
_cell_angle_gamma                90
_cell_volume                     2897.0(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9836
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.486
_cell_measurement_theta_min      2.329
_shelx_estimated_absorpt_T_max   0.981
_shelx_estimated_absorpt_T_min   0.957
_exptl_absorpt_coefficient_mu    0.125
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0911 before and 0.0577 after correction.
The Ratio of minimum to maximum transmission is 0.9052.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0800
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            90574
_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         27.502
_diffrn_reflns_theta_min         2.277
_diffrn_ambient_temperature      100(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 AXS D8 Venture Kappa'
_diffrn_measurement_method       ?
_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                5485
_reflns_number_total             6642
_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 v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         1.394
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         6642
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0409
_refine_ls_restrained_S_all      1.065
_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)+(0.0653P)²+1.4278P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1214
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C25(H25A,
 H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B),
 C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23),
  C24(H24)
;
_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
P1 P 0.84527(4) 0.11914(2) 0.42215(2) 0.01367(10) Uani 1 1 d . . . . .
C1 C 0.93395(14) 0.26619(8) 0.45068(9) 0.0123(3) Uani 1 1 d . . . . .
C2 C 0.95154(14) 0.20010(8) 0.40487(9) 0.0132(3) Uani 1 1 d . . . . .
C3 C 1.03726(15) 0.19712(9) 0.34269(9) 0.0170(3) Uani 1 1 d . . . . .
H3 H 1.047814 0.151493 0.313825 0.020 Uiso 1 1 calc R . . . .
C4 C 1.10733(15) 0.26059(9) 0.32274(10) 0.0192(3) Uani 1 1 d . . . . .
H4 H 1.167180 0.258496 0.281228 0.023 Uiso 1 1 calc R . . . .
C5 C 1.08834(15) 0.32724(9) 0.36461(10) 0.0181(3) Uani 1 1 d . . . . .
H5 H 1.133637 0.371375 0.350493 0.022 Uiso 1 1 calc R . . . .
C6 C 1.00321(15) 0.32969(8) 0.42718(9) 0.0152(3) Uani 1 1 d . . . . .
H6 H 0.991732 0.375862 0.454792 0.018 Uiso 1 1 calc R . . . .
C7 C 0.68700(15) 0.24040(8) 0.45986(9) 0.0123(3) Uani 1 1 d . . . . .
C8 C 0.68839(15) 0.17249(8) 0.41464(9) 0.0128(3) Uani 1 1 d . . . . .
C9 C 0.57852(15) 0.14751(8) 0.36298(9) 0.0159(3) Uani 1 1 d . . . . .
H9 H 0.583133 0.101331 0.334201 0.019 Uiso 1 1 calc R . . . .
C10 C 0.46163(15) 0.18972(9) 0.35307(9) 0.0178(3) Uani 1 1 d . . . . .
H10 H 0.385515 0.172174 0.319018 0.021 Uiso 1 1 calc R . . . .
C11 C 0.45891(15) 0.25798(8) 0.39408(9) 0.0170(3) Uani 1 1 d . . . . .
H11 H 0.380783 0.288031 0.386974 0.020 Uiso 1 1 calc R . . . .
C12 C 0.56994(15) 0.28297(8) 0.44573(9) 0.0146(3) Uani 1 1 d . . . . .
H12 H 0.565917 0.330354 0.472128 0.018 Uiso 1 1 calc R . . . .
C13 C 0.81852(15) 0.33437(7) 0.58063(9) 0.0123(3) Uani 1 1 d . . . . .
C14 C 0.70280(15) 0.35271(8) 0.61755(9) 0.0147(3) Uani 1 1 d . . . . .
H14 H 0.625259 0.322967 0.604631 0.018 Uiso 1 1 calc R . . . .
C15 C 0.69664(16) 0.41265(8) 0.67234(10) 0.0167(3) Uani 1 1 d . . . . .
H15 H 0.615462 0.423542 0.694790 0.020 Uiso 1 1 calc R . . . .
C16 C 0.80858(16) 0.45648(8) 0.69422(9) 0.0173(3) Uani 1 1 d . . . . .
H16 H 0.804446 0.498087 0.730479 0.021 Uiso 1 1 calc R . . . .
C17 C 0.92656(15) 0.43824(8) 0.66202(10) 0.0165(3) Uani 1 1 d . . . . .
H17 H 1.004761 0.466814 0.677352 0.020 Uiso 1 1 calc R . . . .
C18 C 0.93098(15) 0.37825(8) 0.60734(9) 0.0142(3) Uani 1 1 d . . . . .
H18 H 1.013567 0.366400 0.587147 0.017 Uiso 1 1 calc R . . . .
C19 C 0.85790(14) 0.18678(7) 0.57661(9) 0.0114(3) Uani 1 1 d . . . . .
C20 C 0.87061(14) 0.11777(7) 0.53561(9) 0.0123(3) Uani 1 1 d . . . . .
C21 C 0.89394(14) 0.05070(8) 0.57899(9) 0.0145(3) Uani 1 1 d . . . . .
H21 H 0.903955 0.005310 0.549582 0.017 Uiso 1 1 calc R . . . .
C22 C 0.90254(15) 0.05024(8) 0.66518(10) 0.0166(3) Uani 1 1 d . . . . .
H22 H 0.917173 0.004577 0.694944 0.020 Uiso 1 1 calc R . . . .
C23 C 0.88954(15) 0.11718(8) 0.70746(10) 0.0163(3) Uani 1 1 d . . . . .
H23 H 0.894295 0.117275 0.766363 0.020 Uiso 1 1 calc R . . . .
C24 C 0.86947(14) 0.18439(8) 0.66355(9) 0.0135(3) Uani 1 1 d . . . . .
H24 H 0.863502 0.229819 0.693569 0.016 Uiso 1 1 calc R . . . .
B1 B 0.82477(16) 0.26221(8) 0.51958(10) 0.0113(3) Uani 1 1 d . . . . .
O1 O 0.36648(13) 0.39641(6) 0.61611(8) 0.0280(3) Uani 1 1 d . . . . .
C33 C 0.35277(19) 0.42697(9) 0.53376(12) 0.0285(4) Uani 1 1 d . . . . .
H33A H 0.317463 0.388646 0.493016 0.034 Uiso 1 1 calc R . . . .
H33B H 0.440094 0.444546 0.518542 0.034 Uiso 1 1 calc R . . . .
C34 C 0.25660(19) 0.49174(9) 0.53493(11) 0.0272(4) Uani 1 1 d . . . . .
H34A H 0.162929 0.474698 0.524496 0.033 Uiso 1 1 calc R . . . .
H34B H 0.273852 0.530385 0.493496 0.033 Uiso 1 1 calc R . . . .
C35 C 0.2879(2) 0.52064(9) 0.62285(12) 0.0296(4) Uani 1 1 d . . . . .
H35A H 0.367811 0.553182 0.627942 0.036 Uiso 1 1 calc R . . . .
H35B H 0.211621 0.548698 0.641396 0.036 Uiso 1 1 calc R . . . .
C36 C 0.31287(18) 0.44847(10) 0.67128(11) 0.0275(4) Uani 1 1 d . . . . .
H36A H 0.376954 0.457001 0.721001 0.033 Uiso 1 1 calc R . . . .
H36B H 0.228648 0.429048 0.689428 0.033 Uiso 1 1 calc R . . . .
N1 N 0.29264(12) 0.16385(7) 0.60756(8) 0.0142(3) Uani 1 1 d . . . . .
C25 C 0.27035(17) 0.12222(9) 0.52676(10) 0.0205(3) Uani 1 1 d . . . . .
H25A H 0.274868 0.156698 0.479231 0.025 Uiso 1 1 calc R . . . .
H25B H 0.182340 0.097092 0.521135 0.025 Uiso 1 1 calc R . . . .
C26 C 0.44220(16) 0.17323(9) 0.61920(10) 0.0209(3) Uani 1 1 d . . . . .
H26A H 0.473730 0.183306 0.678119 0.025 Uiso 1 1 calc R . . . .
H26B H 0.470520 0.214948 0.584739 0.025 Uiso 1 1 calc R . . . .
C27 C 0.49618(18) 0.09845(11) 0.59118(12) 0.0289(4) Uani 1 1 d . . . . .
H27A H 0.518197 0.064804 0.639291 0.035 Uiso 1 1 calc R . . . .
H27B H 0.577379 0.106234 0.562788 0.035 Uiso 1 1 calc R . . . .
C28 C 0.38269(17) 0.06482(9) 0.53067(11) 0.0242(4) Uani 1 1 d . . . . .
H28A H 0.412774 0.057088 0.475026 0.029 Uiso 1 1 calc R . . . .
H28B H 0.352983 0.016142 0.551618 0.029 Uiso 1 1 calc R . . . .
C29 C 0.24371(17) 0.12219(8) 0.67950(10) 0.0191(3) Uani 1 1 d . . . . .
H29A H 0.307394 0.082352 0.699649 0.023 Uiso 1 1 calc R . . . .
H29B H 0.155591 0.099135 0.663116 0.023 Uiso 1 1 calc R . . . .
C30 C 0.23371(17) 0.18181(9) 0.74632(10) 0.0200(3) Uani 1 1 d . . . . .
H30A H 0.314854 0.181862 0.786425 0.024 Uiso 1 1 calc R . . . .
H30B H 0.155177 0.172631 0.776829 0.024 Uiso 1 1 calc R . . . .
C31 C 0.21938(18) 0.25682(9) 0.69893(10) 0.0234(4) Uani 1 1 d . . . . .
H31A H 0.135651 0.282401 0.709412 0.028 Uiso 1 1 calc R . . . .
H31B H 0.295391 0.290332 0.716460 0.028 Uiso 1 1 calc R . . . .
C32 C 0.21753(17) 0.23668(8) 0.60759(10) 0.0210(3) Uani 1 1 d . . . . .
H32A H 0.124925 0.230476 0.581522 0.025 Uiso 1 1 calc R . . . .
H32B H 0.262058 0.275931 0.577216 0.025 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
P1 C2 1.8373(15) . ?
P1 C8 1.8394(15) . ?
P1 C20 1.8282(15) . ?
C1 C2 1.4139(19) . ?
C1 C6 1.404(2) . ?
C1 B1 1.649(2) . ?
C2 C3 1.395(2) . ?
C3 H3 0.9500 . ?
C3 C4 1.391(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.392(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.396(2) . ?
C6 H6 0.9500 . ?
C7 C8 1.4164(19) . ?
C7 C12 1.402(2) . ?
C7 B1 1.654(2) . ?
C8 C9 1.390(2) . ?
C9 H9 0.9500 . ?
C9 C10 1.394(2) . ?
C10 H10 0.9500 . ?
C10 C11 1.389(2) . ?
C11 H11 0.9500 . ?
C11 C12 1.399(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.405(2) . ?
C13 C18 1.408(2) . ?
C13 B1 1.628(2) . ?
C14 H14 0.9500 . ?
C14 C15 1.395(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.388(2) . ?
C16 H16 0.9500 . ?
C16 C17 1.387(2) . ?
C17 H17 0.9500 . ?
C17 C18 1.393(2) . ?
C18 H18 0.9500 . ?
C19 C20 1.4110(19) . ?
C19 C24 1.401(2) . ?
C19 B1 1.646(2) . ?
C20 C21 1.3948(19) . ?
C21 H21 0.9500 . ?
C21 C22 1.389(2) . ?
C22 H22 0.9500 . ?
C22 C23 1.389(2) . ?
C23 H23 0.9500 . ?
C23 C24 1.398(2) . ?
C24 H24 0.9500 . ?
O1 C33 1.434(2) . ?
O1 C36 1.433(2) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.510(2) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.516(3) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.515(2) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
N1 C25 1.5008(19) . ?
N1 C26 1.510(2) . ?
N1 C29 1.5077(19) . ?
N1 C32 1.5038(19) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C28 1.523(2) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.527(2) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.548(3) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.528(2) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.542(2) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.520(2) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?

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 P1 C8 95.44(6) . . ?
C20 P1 C2 98.11(6) . . ?
C20 P1 C8 95.87(7) . . ?
C2 C1 B1 116.64(12) . . ?
C6 C1 C2 115.93(13) . . ?
C6 C1 B1 127.19(12) . . ?
C1 C2 P1 117.92(11) . . ?
C3 C2 P1 119.70(11) . . ?
C3 C2 C1 122.12(13) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 C2 120.33(14) . . ?
C4 C3 H3 119.8 . . ?
C3 C4 H4 120.5 . . ?
C3 C4 C5 118.90(14) . . ?
C5 C4 H4 120.5 . . ?
C4 C5 H5 119.8 . . ?
C4 C5 C6 120.45(14) . . ?
C6 C5 H5 119.8 . . ?
C1 C6 H6 118.9 . . ?
C5 C6 C1 122.20(14) . . ?
C5 C6 H6 118.9 . . ?
C8 C7 B1 116.76(12) . . ?
C12 C7 C8 115.63(13) . . ?
C12 C7 B1 127.55(12) . . ?
C7 C8 P1 117.60(11) . . ?
C9 C8 P1 120.00(11) . . ?
C9 C8 C7 122.34(13) . . ?
C8 C9 H9 119.7 . . ?
C8 C9 C10 120.50(14) . . ?
C10 C9 H9 119.7 . . ?
C9 C10 H10 120.7 . . ?
C11 C10 C9 118.51(14) . . ?
C11 C10 H10 120.7 . . ?
C10 C11 H11 119.6 . . ?
C10 C11 C12 120.72(14) . . ?
C12 C11 H11 119.6 . . ?
C7 C12 H12 118.9 . . ?
C11 C12 C7 122.19(14) . . ?
C11 C12 H12 118.9 . . ?
C14 C13 C18 114.72(13) . . ?
C14 C13 B1 121.96(13) . . ?
C18 C13 B1 123.01(13) . . ?
C13 C14 H14 118.5 . . ?
C15 C14 C13 122.92(14) . . ?
C15 C14 H14 118.5 . . ?
C14 C15 H15 119.8 . . ?
C16 C15 C14 120.32(14) . . ?
C16 C15 H15 119.8 . . ?
C15 C16 H16 120.7 . . ?
C17 C16 C15 118.60(13) . . ?
C17 C16 H16 120.7 . . ?
C16 C17 H17 119.8 . . ?
C16 C17 C18 120.34(14) . . ?
C18 C17 H17 119.8 . . ?
C13 C18 H18 118.5 . . ?
C17 C18 C13 122.96(14) . . ?
C17 C18 H18 118.5 . . ?
C20 C19 B1 118.18(12) . . ?
C24 C19 C20 116.37(12) . . ?
C24 C19 B1 125.39(12) . . ?
C19 C20 P1 116.81(10) . . ?
C21 C20 P1 121.07(11) . . ?
C21 C20 C19 122.03(13) . . ?
C20 C21 H21 120.0 . . ?
C22 C21 C20 120.03(13) . . ?
C22 C21 H21 120.0 . . ?
C21 C22 H22 120.3 . . ?
C21 C22 C23 119.38(13) . . ?
C23 C22 H22 120.3 . . ?
C22 C23 H23 119.9 . . ?
C22 C23 C24 120.19(14) . . ?
C24 C23 H23 119.9 . . ?
C19 C24 H24 119.0 . . ?
C23 C24 C19 121.97(13) . . ?
C23 C24 H24 119.0 . . ?
C1 B1 C7 101.20(11) . . ?
C13 B1 C1 116.60(12) . . ?
C13 B1 C7 117.21(12) . . ?
C13 B1 C19 108.91(11) . . ?
C19 B1 C1 107.70(11) . . ?
C19 B1 C7 104.15(11) . . ?
C36 O1 C33 109.10(12) . . ?
O1 C33 H33A 110.5 . . ?
O1 C33 H33B 110.5 . . ?
O1 C33 C34 106.19(14) . . ?
H33A C33 H33B 108.7 . . ?
C34 C33 H33A 110.5 . . ?
C34 C33 H33B 110.5 . . ?
C33 C34 H34A 111.4 . . ?
C33 C34 H34B 111.4 . . ?
C33 C34 C35 101.62(15) . . ?
H34A C34 H34B 109.3 . . ?
C35 C34 H34A 111.4 . . ?
C35 C34 H34B 111.4 . . ?
C34 C35 H35A 111.4 . . ?
C34 C35 H35B 111.4 . . ?
H35A C35 H35B 109.3 . . ?
C36 C35 C34 101.78(13) . . ?
C36 C35 H35A 111.4 . . ?
C36 C35 H35B 111.4 . . ?
O1 C36 C35 106.34(14) . . ?
O1 C36 H36A 110.5 . . ?
O1 C36 H36B 110.5 . . ?
C35 C36 H36A 110.5 . . ?
C35 C36 H36B 110.5 . . ?
H36A C36 H36B 108.7 . . ?
C25 N1 C26 102.72(12) . . ?
C25 N1 C29 113.47(12) . . ?
C25 N1 C32 113.47(12) . . ?
C29 N1 C26 111.20(12) . . ?
C32 N1 C26 113.64(12) . . ?
C32 N1 C29 102.71(12) . . ?
N1 C25 H25A 110.8 . . ?
N1 C25 H25B 110.8 . . ?
N1 C25 C28 104.69(13) . . ?
H25A C25 H25B 108.9 . . ?
C28 C25 H25A 110.8 . . ?
C28 C25 H25B 110.8 . . ?
N1 C26 H26A 110.9 . . ?
N1 C26 H26B 110.9 . . ?
N1 C26 C27 104.40(12) . . ?
H26A C26 H26B 108.9 . . ?
C27 C26 H26A 110.9 . . ?
C27 C26 H26B 110.9 . . ?
C26 C27 H27A 110.7 . . ?
C26 C27 H27B 110.7 . . ?
C26 C27 C28 105.28(14) . . ?
H27A C27 H27B 108.8 . . ?
C28 C27 H27A 110.7 . . ?
C28 C27 H27B 110.7 . . ?
C25 C28 C27 105.27(13) . . ?
C25 C28 H28A 110.7 . . ?
C25 C28 H28B 110.7 . . ?
C27 C28 H28A 110.7 . . ?
C27 C28 H28B 110.7 . . ?
H28A C28 H28B 108.8 . . ?
N1 C29 H29A 110.8 . . ?
N1 C29 H29B 110.8 . . ?
N1 C29 C30 104.79(12) . . ?
H29A C29 H29B 108.9 . . ?
C30 C29 H29A 110.8 . . ?
C30 C29 H29B 110.8 . . ?
C29 C30 H30A 110.7 . . ?
C29 C30 H30B 110.7 . . ?
C29 C30 C31 105.15(13) . . ?
H30A C30 H30B 108.8 . . ?
C31 C30 H30A 110.7 . . ?
C31 C30 H30B 110.7 . . ?
C30 C31 H31A 110.6 . . ?
C30 C31 H31B 110.6 . . ?
H31A C31 H31B 108.7 . . ?
C32 C31 C30 105.67(12) . . ?
C32 C31 H31A 110.6 . . ?
C32 C31 H31B 110.6 . . ?
N1 C32 C31 104.45(12) . . ?
N1 C32 H32A 110.9 . . ?
N1 C32 H32B 110.9 . . ?
C31 C32 H32A 110.9 . . ?
C31 C32 H32B 110.9 . . ?
H32A C32 H32B 108.9 . . ?

_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_p17423final
_database_code_depnum_ccdc_archive 'CCDC 1824473'
_audit_update_record             
;
2018-02-16 deposited with the CCDC.
2018-06-22 downloaded from the CCDC.
;
_audit_creation_date             2017-12-14
_audit_creation_method           
;
Olex2 1.2
(compiled Aug 10 2017 17:28:52 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        cis-[PtMe2[PTB]2][NEt4]2
_chemical_formula_moiety         'C50 H40 B2 P2 Pt, 2(C8 H20 N)'
_chemical_formula_sum            'C66 H80 B2 N2 P2 Pt'
_chemical_formula_weight         1179.97
_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'
B B 0.0013 0.0007 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 '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           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   16.7080(8)
_cell_length_b                   22.4099(11)
_cell_length_c                   16.7415(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6268.4(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9422
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.370
_cell_measurement_theta_min      2.721
_shelx_estimated_absorpt_T_max   0.955
_shelx_estimated_absorpt_T_min   0.666
_exptl_absorpt_coefficient_mu    2.328
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6033
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1083 before and 0.0686 after correction.
The Ratio of minimum to maximum transmission is 0.8091.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1159
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            99373
_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         27.512
_diffrn_reflns_theta_min         2.433
_diffrn_ambient_temperature      100(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 AXS D8 Venture Kappa'
_diffrn_measurement_method       ?
_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                5314
_reflns_number_total             7201
_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 v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         5.629
_refine_diff_density_min         -2.337
_refine_diff_density_rms         0.151
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         7201
_refine_ls_number_restraints     312
_refine_ls_R_factor_all          0.1027
_refine_ls_R_factor_gt           0.0735
_refine_ls_restrained_S_all      1.066
_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)+(0.0454P)²+66.0340P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1530
_refine_ls_wR_factor_ref         0.1630
_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
Uanis(C33) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
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.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C28(H28A,H28B), C30(H30A,H30B), C32(H32A,H32B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(HC), C4(HD), C5(HE), C6(HF), C10(HG), C11(HH), C12(HI), C13(HJ), C16(HK),
 C17(HL), C18(HM), C19(HN), C21(HO), C22(HP), C23(HQ), C24(HR), C25(HS)
4.c Idealised Me refined as rotating group:
 C1(H,HA,HB), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C),
 C33(H33A,H33B,H33C)
;
_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
Pt1 Pt 0.500000 0.80754(2) 0.750000 0.03066(13) Uani 1 2 d S TU P . .
P1 P 0.54920(9) 0.74386(8) 0.65474(10) 0.0248(4) Uani 1 1 d . U . . .
C1 C 0.4507(5) 0.8787(4) 0.8159(5) 0.0427(19) Uani 1 1 d . U . . .
H H 0.416606 0.902904 0.780888 0.064 Uiso 1 1 calc GR . . . .
HA H 0.493919 0.903548 0.837310 0.064 Uiso 1 1 calc GR . . . .
HB H 0.418584 0.862830 0.859984 0.064 Uiso 1 1 calc GR . . . .
C2 C 0.5159(3) 0.6667(3) 0.6375(4) 0.0230(12) Uani 1 1 d . U . . .
C3 C 0.4495(4) 0.6433(4) 0.6770(4) 0.0331(15) Uani 1 1 d . U . . .
HC H 0.416926 0.668360 0.709268 0.040 Uiso 1 1 calc R . . . .
C4 C 0.4314(4) 0.5831(4) 0.6688(4) 0.0361(16) Uani 1 1 d . U . . .
HD H 0.387036 0.566422 0.696388 0.043 Uiso 1 1 calc R . . . .
C5 C 0.4781(4) 0.5479(4) 0.6204(5) 0.0360(16) Uani 1 1 d . U . . .
HE H 0.466670 0.506532 0.615925 0.043 Uiso 1 1 calc R . . . .
C6 C 0.5419(4) 0.5721(3) 0.5779(4) 0.0286(14) Uani 1 1 d . U . . .
HF H 0.572371 0.546983 0.543839 0.034 Uiso 1 1 calc R . . . .
C7 C 0.5621(4) 0.6325(3) 0.5842(4) 0.0254(13) Uani 1 1 d . U . . .
C8 C 0.5472(4) 0.7646(3) 0.5491(4) 0.0256(13) Uani 1 1 d . U . . .
C9 C 0.5907(3) 0.7264(3) 0.4985(4) 0.0239(13) Uani 1 1 d . U . . .
C10 C 0.5851(4) 0.7380(3) 0.4160(4) 0.0284(14) Uani 1 1 d . U . . .
HG H 0.612974 0.712988 0.379591 0.034 Uiso 1 1 calc R . . . .
C11 C 0.5402(5) 0.7847(3) 0.3866(4) 0.0349(16) Uani 1 1 d . U . . .
HH H 0.539183 0.791903 0.330664 0.042 Uiso 1 1 calc R . . . .
C12 C 0.4969(5) 0.8212(4) 0.4364(5) 0.0439(19) Uani 1 1 d . U . . .
HI H 0.465062 0.852565 0.415426 0.053 Uiso 1 1 calc R . . . .
C13 C 0.5008(4) 0.8110(3) 0.5191(4) 0.0365(15) Uani 1 1 d . U . . .
HJ H 0.471580 0.835851 0.554641 0.044 Uiso 1 1 calc R . . . .
C14 C 0.6914(4) 0.6890(3) 0.6121(4) 0.0279(14) Uani 1 1 d . U . . .
C15 C 0.6547(4) 0.7282(3) 0.6673(4) 0.0273(14) Uani 1 1 d . U . . .
C16 C 0.6937(4) 0.7477(4) 0.7358(4) 0.044(2) Uani 1 1 d . U . . .
HK H 0.667433 0.773789 0.772072 0.053 Uiso 1 1 calc R . . . .
C17 C 0.7717(5) 0.7287(5) 0.7510(6) 0.066(3) Uani 1 1 d . U . . .
HL H 0.799738 0.743242 0.796291 0.079 Uiso 1 1 calc R . . . .
C18 C 0.8075(5) 0.6892(5) 0.7005(5) 0.059(3) Uani 1 1 d . U . . .
HM H 0.859599 0.674800 0.712528 0.071 Uiso 1 1 calc R . . . .
C19 C 0.7690(4) 0.6694(4) 0.6312(4) 0.0386(19) Uani 1 1 d . U . . .
HN H 0.795577 0.642280 0.596602 0.046 Uiso 1 1 calc R . . . .
C20 C 0.6808(4) 0.6305(3) 0.4665(4) 0.0236(13) Uani 1 1 d . U . . .
C21 C 0.7608(4) 0.6412(3) 0.4454(4) 0.0310(15) Uani 1 1 d . U . . .
HO H 0.791032 0.668586 0.476524 0.037 Uiso 1 1 calc R . . . .
C22 C 0.7983(4) 0.6133(4) 0.3801(4) 0.0356(17) Uani 1 1 d . U . . .
HP H 0.852722 0.621935 0.368625 0.043 Uiso 1 1 calc R . . . .
C23 C 0.7578(5) 0.5741(4) 0.3331(5) 0.0421(18) Uani 1 1 d . U . . .
HQ H 0.783239 0.554012 0.290047 0.051 Uiso 1 1 calc R . . . .
C24 C 0.6769(5) 0.5646(4) 0.3511(5) 0.049(2) Uani 1 1 d . U . . .
HR H 0.646257 0.538439 0.318633 0.058 Uiso 1 1 calc R . . . .
C25 C 0.6412(5) 0.5923(4) 0.4143(5) 0.0398(18) Uani 1 1 d . U . . .
HS H 0.585953 0.585000 0.423248 0.048 Uiso 1 1 calc R . . . .
B1 B 0.6357(4) 0.6679(4) 0.5364(4) 0.0247(14) Uani 1 1 d . U . . .
N1 N 0.7051(4) 0.6118(4) 1.0510(5) 0.0559(19) Uani 1 1 d . U . A 1
C26 C 0.6440(7) 0.6473(5) 0.9998(9) 0.090(4) Uani 1 1 d . U . A 1
H26A H 0.592045 0.647874 1.028206 0.108 Uiso 1 1 calc R . . A 1
H26B H 0.635867 0.625765 0.948754 0.108 Uiso 1 1 calc R . . A 1
C27 C 0.6691(8) 0.7137(5) 0.9804(9) 0.092(4) Uani 1 1 d . U . A 1
H27A H 0.721659 0.713956 0.954407 0.138 Uiso 1 1 calc GR . . A 1
H27B H 0.671855 0.736721 1.030160 0.138 Uiso 1 1 calc GR . . A 1
H27C H 0.629410 0.731762 0.944725 0.138 Uiso 1 1 calc GR . . A 1
C28 C 0.7868(7) 0.6214(7) 1.0192(7) 0.090(4) Uani 1 1 d . U . A 1
H28A H 0.825974 0.602689 1.055888 0.108 Uiso 1 1 calc R . . A 1
H28B H 0.798048 0.664728 1.017733 0.108 Uiso 1 1 calc R . . A 1
C29 C 0.7987(10) 0.5947(8) 0.9330(8) 0.121(6) Uani 1 1 d . U . A 1
H29A H 0.807760 0.551627 0.936815 0.181 Uiso 1 1 calc GR . . A 1
H29B H 0.844943 0.613699 0.907542 0.181 Uiso 1 1 calc GR . . A 1
H29C H 0.750619 0.602296 0.900961 0.181 Uiso 1 1 calc GR . . A 1
C30 C 0.6746(7) 0.5539(5) 1.0542(7) 0.070(3) Uani 1 1 d . U . A 1
H30A H 0.676804 0.536298 0.999999 0.084 Uiso 1 1 calc R . . A 1
H30B H 0.617714 0.555739 1.070470 0.084 Uiso 1 1 calc R . . A 1
C31 C 0.7221(6) 0.5110(4) 1.1151(7) 0.067(3) Uani 1 1 d . U . A 1
H31A H 0.778925 0.521938 1.115509 0.100 Uiso 1 1 calc GR . . A 1
H31B H 0.716433 0.469460 1.097806 0.100 Uiso 1 1 calc GR . . A 1
H31C H 0.699925 0.515592 1.168889 0.100 Uiso 1 1 calc GR . . A 1
C32 C 0.7052(9) 0.6438(7) 1.1330(8) 0.098(4) Uani 1 1 d . U . A 1
H32A H 0.723820 0.685435 1.125917 0.117 Uiso 1 1 calc R . . A 1
H32B H 0.742993 0.623372 1.169326 0.117 Uiso 1 1 calc R . . A 1
C33 C 0.6196(11) 0.6442(8) 1.1715(11) 0.132(5) Uani 1 1 d . U . A 1
H33A H 0.617891 0.615463 1.215592 0.198 Uiso 1 1 calc GR . . A 1
H33B H 0.579836 0.633059 1.131091 0.198 Uiso 1 1 calc GR . . A 1
H33C H 0.607620 0.684198 1.191778 0.198 Uiso 1 1 calc GR . . 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
Pt1 P1 2.2926(18) . ?
Pt1 P1 2.2926(18) 3_656 ?
Pt1 C1 2.107(8) 3_656 ?
Pt1 C1 2.107(8) . ?
P1 C2 1.839(7) . ?
P1 C8 1.828(7) . ?
P1 C15 1.810(7) . ?
C1 H 0.9800 . ?
C1 HA 0.9800 . ?
C1 HB 0.9800 . ?
C2 C3 1.394(9) . ?
C2 C7 1.408(9) . ?
C3 HC 0.9500 . ?
C3 C4 1.390(11) . ?
C4 HD 0.9500 . ?
C4 C5 1.373(11) . ?
C5 HE 0.9500 . ?
C5 C6 1.391(9) . ?
C6 HF 0.9500 . ?
C6 C7 1.399(10) . ?
C7 B1 1.667(10) . ?
C8 C9 1.408(9) . ?
C8 C13 1.390(10) . ?
C9 C10 1.410(9) . ?
C9 B1 1.639(11) . ?
C10 HG 0.9500 . ?
C10 C11 1.379(10) . ?
C11 HH 0.9500 . ?
C11 C12 1.373(11) . ?
C12 HI 0.9500 . ?
C12 C13 1.405(11) . ?
C13 HJ 0.9500 . ?
C14 C15 1.413(10) . ?
C14 C19 1.406(9) . ?
C14 B1 1.642(10) . ?
C15 C16 1.390(9) . ?
C16 HK 0.9500 . ?
C16 C17 1.393(12) . ?
C17 HL 0.9500 . ?
C17 C18 1.363(13) . ?
C18 HM 0.9500 . ?
C18 C19 1.398(10) . ?
C19 HN 0.9500 . ?
C20 C21 1.404(9) . ?
C20 C25 1.390(10) . ?
C20 B1 1.624(10) . ?
C21 HO 0.9500 . ?
C21 C22 1.407(10) . ?
C22 HP 0.9500 . ?
C22 C23 1.359(11) . ?
C23 HQ 0.9500 . ?
C23 C24 1.402(11) . ?
C24 HR 0.9500 . ?
C24 C25 1.363(11) . ?
C25 HS 0.9500 . ?
N1 C26 1.552(12) . ?
N1 C28 1.481(13) . ?
N1 C30 1.395(13) . ?
N1 C32 1.548(14) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.581(16) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.574(17) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.610(14) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.57(2) . ?
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
P1 Pt1 P1 103.00(9) . 3_656 ?
C1 Pt1 P1 88.1(2) . 3_656 ?
C1 Pt1 P1 167.3(2) . . ?
C1 Pt1 P1 88.1(2) 3_656 . ?
C1 Pt1 P1 167.3(2) 3_656 3_656 ?
C1 Pt1 C1 81.6(5) 3_656 . ?
C2 P1 Pt1 125.9(2) . . ?
C8 P1 Pt1 120.5(2) . . ?
C8 P1 C2 94.7(3) . . ?
C15 P1 Pt1 112.9(2) . . ?
C15 P1 C2 97.5(3) . . ?
C15 P1 C8 100.4(3) . . ?
Pt1 C1 H 109.5 . . ?
Pt1 C1 HA 109.5 . . ?
Pt1 C1 HB 109.5 . . ?
H C1 HA 109.5 . . ?
H C1 HB 109.5 . . ?
HA C1 HB 109.5 . . ?
C3 C2 P1 121.3(5) . . ?
C3 C2 C7 122.2(7) . . ?
C7 C2 P1 116.5(4) . . ?
C2 C3 HC 120.3 . . ?
C4 C3 C2 119.4(7) . . ?
C4 C3 HC 120.3 . . ?
C3 C4 HD 120.3 . . ?
C5 C4 C3 119.5(6) . . ?
C5 C4 HD 120.3 . . ?
C4 C5 HE 119.6 . . ?
C4 C5 C6 120.9(7) . . ?
C6 C5 HE 119.6 . . ?
C5 C6 HF 119.2 . . ?
C5 C6 C7 121.6(7) . . ?
C7 C6 HF 119.2 . . ?
C2 C7 B1 116.7(6) . . ?
C6 C7 C2 116.2(6) . . ?
C6 C7 B1 127.1(6) . . ?
C9 C8 P1 114.7(5) . . ?
C13 C8 P1 123.4(5) . . ?
C13 C8 C9 121.7(6) . . ?
C8 C9 C10 116.3(6) . . ?
C8 C9 B1 119.4(6) . . ?
C10 C9 B1 123.9(6) . . ?
C9 C10 HG 119.1 . . ?
C11 C10 C9 121.8(7) . . ?
C11 C10 HG 119.1 . . ?
C10 C11 HH 119.3 . . ?
C12 C11 C10 121.4(7) . . ?
C12 C11 HH 119.3 . . ?
C11 C12 HI 120.7 . . ?
C11 C12 C13 118.6(7) . . ?
C13 C12 HI 120.7 . . ?
C8 C13 C12 120.2(7) . . ?
C8 C13 HJ 119.9 . . ?
C12 C13 HJ 119.9 . . ?
C15 C14 B1 116.0(6) . . ?
C19 C14 C15 116.4(6) . . ?
C19 C14 B1 127.4(7) . . ?
C14 C15 P1 117.8(5) . . ?
C16 C15 P1 119.4(5) . . ?
C16 C15 C14 122.1(6) . . ?
C15 C16 HK 120.3 . . ?
C15 C16 C17 119.5(7) . . ?
C17 C16 HK 120.3 . . ?
C16 C17 HL 120.1 . . ?
C18 C17 C16 119.8(7) . . ?
C18 C17 HL 120.1 . . ?
C17 C18 HM 119.4 . . ?
C17 C18 C19 121.2(8) . . ?
C19 C18 HM 119.4 . . ?
C14 C19 HN 119.5 . . ?
C18 C19 C14 120.9(7) . . ?
C18 C19 HN 119.5 . . ?
C21 C20 B1 122.4(6) . . ?
C25 C20 C21 113.5(6) . . ?
C25 C20 B1 123.4(6) . . ?
C20 C21 HO 118.5 . . ?
C20 C21 C22 122.9(7) . . ?
C22 C21 HO 118.5 . . ?
C21 C22 HP 119.4 . . ?
C23 C22 C21 121.1(7) . . ?
C23 C22 HP 119.4 . . ?
C22 C23 HQ 121.5 . . ?
C22 C23 C24 116.9(7) . . ?
C24 C23 HQ 121.5 . . ?
C23 C24 HR 119.3 . . ?
C25 C24 C23 121.3(8) . . ?
C25 C24 HR 119.3 . . ?
C20 C25 HS 118.0 . . ?
C24 C25 C20 124.1(7) . . ?
C24 C25 HS 118.0 . . ?
C9 B1 C7 103.2(5) . . ?
C9 B1 C14 109.1(6) . . ?
C14 B1 C7 100.7(5) . . ?
C20 B1 C7 116.3(6) . . ?
C20 B1 C9 110.2(5) . . ?
C20 B1 C14 116.3(5) . . ?
C26 N1 C32 104.7(9) . . ?
C28 N1 C26 109.5(9) . . ?
C28 N1 C32 104.5(8) . . ?
C30 N1 C26 104.9(7) . . ?
C30 N1 C28 119.0(10) . . ?
C30 N1 C32 113.4(10) . . ?
N1 C26 H26A 108.6 . . ?
N1 C26 H26B 108.5 . . ?
N1 C26 C27 114.9(9) . . ?
H26A C26 H26B 107.5 . . ?
C27 C26 H26A 108.5 . . ?
C27 C26 H26B 108.5 . . ?
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 . . ?
N1 C28 H28A 109.0 . . ?
N1 C28 H28B 109.0 . . ?
N1 C28 C29 113.0(10) . . ?
H28A C28 H28B 107.8 . . ?
C29 C28 H28A 109.0 . . ?
C29 C28 H28B 109.0 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N1 C30 H30A 108.9 . . ?
N1 C30 H30B 108.9 . . ?
N1 C30 C31 113.5(8) . . ?
H30A C30 H30B 107.7 . . ?
C31 C30 H30A 108.9 . . ?
C31 C30 H30B 108.9 . . ?
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 . . ?
N1 C32 H32A 109.3 . . ?
N1 C32 H32B 109.3 . . ?
N1 C32 C33 111.5(11) . . ?
H32A C32 H32B 108.0 . . ?
C33 C32 H32A 109.3 . . ?
C33 C32 H32B 109.3 . . ?
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 . . ?

_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 0.055 0.250 16.6 0.0 ?
2 0.000 -0.055 0.750 16.6 0.0 ?
3 0.000 0.500 -0.611 476.0 142.3 ?
4 0.500 0.000 -0.856 476.0 142.3 ?
5 0.500 0.445 0.750 16.6 0.0 ?
6 0.500 0.555 0.250 16.6 0.0 ?


_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_mkt_a
_database_code_depnum_ccdc_archive 'CCDC 1824475'
_audit_update_record             
;
2018-02-16 deposited with the CCDC.
2018-06-22 downloaded from the CCDC.
;
_audit_creation_date             2018-02-15
_audit_creation_method           
;
Olex2 1.2
(compiled Aug 10 2017 17:28:52 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        PTBCo(Br)3(NEt4)2
_chemical_formula_moiety         'C24 H17 B Br3 Co P, 2(C8 H20 N)'
_chemical_formula_sum            'C40 H57 B Br3 Co N2 P'
_chemical_formula_weight         906.31
_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 0.0181 0.0091 '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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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                   13.5630(10)
_cell_length_b                   16.1347(13)
_cell_length_c                   18.6380(16)
_cell_angle_alpha                90
_cell_angle_beta                 95.679(4)
_cell_angle_gamma                90
_cell_volume                     4058.6(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9827
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      79.475
_cell_measurement_theta_min      3.631
_shelx_estimated_absorpt_T_max   0.425
_shelx_estimated_absorpt_T_min   0.307
_exptl_absorpt_coefficient_mu    7.362
_exptl_absorpt_correction_T_max  0.357
_exptl_absorpt_correction_T_min  0.266
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1263 before and 0.0953 after correction.
The Ratio of minimum to maximum transmission is 0.7059.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1852
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0856
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            55074
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         79.934
_diffrn_reflns_theta_min         2.382
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'Apex Duo II'
_diffrn_measurement_method       ?
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7710
_reflns_number_total             8674
_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 V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 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    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         4.819
_refine_diff_density_min         -1.387
_refine_diff_density_rms         0.346
_refine_ls_extinction_coef       0.0022(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   2.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         8674
_refine_ls_number_restraints     393
_refine_ls_R_factor_all          0.1737
_refine_ls_R_factor_gt           0.1602
_refine_ls_restrained_S_all      2.025
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4098
_refine_ls_wR_factor_ref         0.4362
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.706(4)
 0.294(4)
2. 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
3. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
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 Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C35(H35A,H35B), C37(H37A,H37B), C39(H39A,H39B), C25(H25A,
 H25B), C27(H27A,H27B), C29(H29A,H29B), C31(H31A,H31B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C22(H22), C23(H23), C24(H24),
  C21(H21)
5.c Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C40(H40A,H40B,
 H40C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C32(H32A,
 H32B,H32C)
;
_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
Br1 Br 1.07020(12) 0.69087(13) 0.49768(11) 0.0386(6) Uani 1 1 d . U . . .
Br2 Br 1.06694(11) 0.88664(9) 0.63398(8) 0.0231(4) Uani 1 1 d . U . . .
Br3 Br 1.09263(13) 0.66168(10) 0.71302(11) 0.0349(5) Uani 1 1 d . U . . .
Co1 Co 1.03003(17) 0.74280(15) 0.61141(14) 0.0218(6) Uani 1 1 d . U . . .
P1 P 0.8554(2) 0.7409(2) 0.60155(19) 0.0173(7) Uani 1 1 d . U . . .
N2 N 0.7316(10) 0.5524(8) 0.8460(7) 0.025(2) Uani 1 1 d . U . . .
C1 C 0.7965(10) 0.7724(8) 0.6798(7) 0.017(2) Uani 1 1 d . U . . .
C2 C 0.6930(10) 0.7734(8) 0.6735(7) 0.017(2) Uani 1 1 d . U . . .
C3 C 0.6472(11) 0.7934(8) 0.7358(8) 0.020(2) Uani 1 1 d . U . . .
H3 H 0.576944 0.791876 0.734035 0.024 Uiso 1 1 calc R . . . .
C4 C 0.7016(12) 0.8150(9) 0.7992(8) 0.023(3) Uani 1 1 d . U . . .
H4 H 0.667903 0.830786 0.839326 0.028 Uiso 1 1 calc R . . . .
C5 C 0.8037(12) 0.8145(9) 0.8061(8) 0.024(3) Uani 1 1 d . U . . .
H5 H 0.840152 0.828601 0.850630 0.029 Uiso 1 1 calc R . . . .
C6 C 0.8528(11) 0.7924(8) 0.7455(7) 0.020(2) Uani 1 1 d . U . . .
H6 H 0.923166 0.791029 0.748837 0.024 Uiso 1 1 calc R . . . .
C7 C 0.6794(10) 0.6526(8) 0.5820(7) 0.017(2) Uani 1 1 d . U . . .
C8 C 0.7856(10) 0.6456(8) 0.5830(8) 0.018(2) Uani 1 1 d . U . . .
C9 C 0.8333(10) 0.5717(9) 0.5678(7) 0.020(2) Uani 1 1 d . U . . .
H9 H 0.902789 0.571196 0.564523 0.024 Uiso 1 1 calc R . . . .
C10 C 0.7790(12) 0.4997(8) 0.5576(7) 0.022(3) Uani 1 1 d . U . . .
H10 H 0.811057 0.448890 0.548714 0.027 Uiso 1 1 calc R . . . .
C11 C 0.6762(13) 0.5021(9) 0.5603(8) 0.026(3) Uani 1 1 d . U . . .
H11 H 0.637944 0.453001 0.552647 0.031 Uiso 1 1 calc R . . . .
C12 C 0.6307(11) 0.5763(9) 0.5742(8) 0.024(3) Uani 1 1 d . U . . .
H12 H 0.561520 0.575302 0.578693 0.029 Uiso 1 1 calc R . . . .
C13 C 0.7908(9) 0.8061(7) 0.5336(7) 0.014(2) Uani 1 1 d . U . . .
C14 C 0.6844(10) 0.8036(9) 0.5324(7) 0.017(2) Uani 1 1 d . U . . .
C15 C 0.6317(11) 0.8488(9) 0.4781(8) 0.022(3) Uani 1 1 d . U . . .
H15 H 0.561370 0.847888 0.474747 0.026 Uiso 1 1 calc R . . . .
C16 C 0.6789(13) 0.8964(11) 0.4276(9) 0.029(3) Uani 1 1 d . U . . .
H16 H 0.641049 0.926204 0.390591 0.035 Uiso 1 1 calc R . . . .
C17 C 0.7824(13) 0.8985(10) 0.4334(9) 0.028(3) Uani 1 1 d . U . . .
H17 H 0.814717 0.931347 0.400533 0.033 Uiso 1 1 calc R . . . .
C18 C 0.8378(11) 0.8547(8) 0.4849(8) 0.021(2) Uani 1 1 d . U . . .
H18 H 0.908090 0.857019 0.487912 0.025 Uiso 1 1 calc R . . . .
C19 C 0.5163(10) 0.7607(9) 0.5845(8) 0.020(2) Uani 1 1 d . U . . .
C20 C 0.4764(11) 0.8328(9) 0.6132(8) 0.024(3) Uani 1 1 d . U . . .
H20 H 0.520133 0.870488 0.639425 0.028 Uiso 1 1 calc R . . . .
C22 C 0.3101(11) 0.7961(10) 0.5656(9) 0.026(3) Uani 1 1 d . U . . .
H22 H 0.240851 0.806801 0.560467 0.031 Uiso 1 1 calc R . . . .
C23 C 0.3454(12) 0.7308(11) 0.5368(9) 0.029(3) Uani 1 1 d . U . . .
H23 H 0.300649 0.695032 0.509335 0.035 Uiso 1 1 calc R . . . .
C24 C 0.4490(12) 0.7095(10) 0.5444(9) 0.030(3) Uani 1 1 d . U . . .
H24 H 0.471296 0.660879 0.522151 0.035 Uiso 1 1 calc R . . . .
C33 C 0.7985(15) 0.4968(11) 0.8960(10) 0.036(3) Uani 1 1 d . U . . .
H33A H 0.819889 0.449102 0.867944 0.043 Uiso 1 1 calc R . . . .
H33B H 0.759580 0.474708 0.933972 0.043 Uiso 1 1 calc R . . . .
C34 C 0.8907(14) 0.5403(16) 0.9322(9) 0.043(5) Uani 1 1 d . U . . .
H34A H 0.941386 0.543381 0.898323 0.064 Uiso 1 1 calc GR . . . .
H34B H 0.916638 0.508873 0.975020 0.064 Uiso 1 1 calc GR . . . .
H34C H 0.873143 0.596384 0.946561 0.064 Uiso 1 1 calc GR . . . .
C35 C 0.7937(14) 0.5979(10) 0.7937(10) 0.032(3) Uani 1 1 d . U . . .
H35A H 0.749261 0.632258 0.760495 0.038 Uiso 1 1 calc R . . . .
H35B H 0.840796 0.635464 0.821549 0.038 Uiso 1 1 calc R . . . .
C36 C 0.8496(14) 0.5409(11) 0.7509(9) 0.033(3) Uani 1 1 d . U . . .
H36A H 0.806695 0.521677 0.708846 0.050 Uiso 1 1 calc GR . . . .
H36B H 0.872354 0.493237 0.780700 0.050 Uiso 1 1 calc GR . . . .
H36C H 0.906971 0.569946 0.734877 0.050 Uiso 1 1 calc GR . . . .
C37 C 0.6868(14) 0.6173(12) 0.8895(10) 0.036(3) Uani 1 1 d . U . . .
H37A H 0.651331 0.657885 0.856477 0.043 Uiso 1 1 calc R . . . .
H37B H 0.740456 0.647227 0.918728 0.043 Uiso 1 1 calc R . . . .
C38 C 0.6135(16) 0.5812(15) 0.9405(10) 0.045(4) Uani 1 1 d . U . . .
H38A H 0.545365 0.594426 0.921354 0.067 Uiso 1 1 calc GR . . . .
H38B H 0.627279 0.605449 0.988596 0.067 Uiso 1 1 calc GR . . . .
H38C H 0.621518 0.520880 0.943511 0.067 Uiso 1 1 calc GR . . . .
C39 C 0.6563(15) 0.4959(12) 0.8069(11) 0.039(4) Uani 1 1 d . U . . .
H39A H 0.624198 0.463009 0.842931 0.046 Uiso 1 1 calc R . . . .
H39B H 0.690984 0.456799 0.777138 0.046 Uiso 1 1 calc R . . . .
C40 C 0.5737(14) 0.5423(13) 0.7570(11) 0.041(4) Uani 1 1 d . U . . .
H40A H 0.597156 0.597904 0.745849 0.061 Uiso 1 1 calc GR . . . .
H40B H 0.513568 0.546940 0.781811 0.061 Uiso 1 1 calc GR . . . .
H40C H 0.558993 0.511097 0.712090 0.061 Uiso 1 1 calc GR . . . .
B1 B 0.6329(13) 0.7448(9) 0.5941(8) 0.019(2) Uani 1 1 d . U . . .
N1 N 0.7704(10) 0.6085(8) 0.3379(7) 0.025(2) Uani 1 1 d . U . . .
C25 C 0.7832(13) 0.6660(10) 0.2731(9) 0.029(3) Uani 1 1 d . U . . .
H25A H 0.821792 0.636207 0.238761 0.035 Uiso 1 1 calc R . . . .
H25B H 0.717028 0.678127 0.247951 0.035 Uiso 1 1 calc R . . . .
C26 C 0.8349(14) 0.7475(10) 0.2934(11) 0.035(4) Uani 1 1 d . U . . .
H26A H 0.851771 0.775609 0.249623 0.053 Uiso 1 1 calc GR . . . .
H26B H 0.895504 0.736572 0.325075 0.053 Uiso 1 1 calc GR . . . .
H26C H 0.790619 0.782822 0.318518 0.053 Uiso 1 1 calc GR . . . .
C27 C 0.8711(12) 0.5939(11) 0.3810(9) 0.031(3) Uani 1 1 d . U . . .
H27A H 0.892294 0.646201 0.405570 0.037 Uiso 1 1 calc R . . . .
H27B H 0.862305 0.552206 0.418791 0.037 Uiso 1 1 calc R . . . .
C28 C 0.9528(12) 0.5651(10) 0.3385(11) 0.034(4) Uani 1 1 d . U . . .
H28A H 0.944759 0.590312 0.290472 0.050 Uiso 1 1 calc GR . . . .
H28B H 0.950159 0.504608 0.333905 0.050 Uiso 1 1 calc GR . . . .
H28C H 1.016796 0.581515 0.363434 0.050 Uiso 1 1 calc GR . . . .
C29 C 0.7278(12) 0.5289(10) 0.3061(9) 0.027(3) Uani 1 1 d . U . . .
H29A H 0.776331 0.504574 0.275708 0.033 Uiso 1 1 calc R . . . .
H29B H 0.667410 0.542363 0.273934 0.033 Uiso 1 1 calc R . . . .
C30 C 0.7012(16) 0.4632(13) 0.3597(12) 0.045(4) Uani 1 1 d . U . . .
H30A H 0.668643 0.416411 0.333501 0.067 Uiso 1 1 calc GR . . . .
H30B H 0.656138 0.487135 0.392117 0.067 Uiso 1 1 calc GR . . . .
H30C H 0.761588 0.443871 0.387918 0.067 Uiso 1 1 calc GR . . . .
C31 C 0.7052(11) 0.6473(11) 0.3904(9) 0.029(3) Uani 1 1 d . U . . .
H31A H 0.706266 0.611326 0.433434 0.035 Uiso 1 1 calc R . . . .
H31B H 0.734162 0.701420 0.406265 0.035 Uiso 1 1 calc R . . . .
C32 C 0.5990(11) 0.6609(12) 0.3608(9) 0.031(3) Uani 1 1 d . U . . .
H32A H 0.596990 0.692045 0.315579 0.047 Uiso 1 1 calc GR . . . .
H32B H 0.564598 0.692299 0.395844 0.047 Uiso 1 1 calc GR . . . .
H32C H 0.566376 0.607186 0.351904 0.047 Uiso 1 1 calc GR . . . .
C21 C 0.3761(12) 0.8510(10) 0.6045(8) 0.027(3) Uani 1 1 d . U . . .
H21 H 0.352038 0.900119 0.624778 0.032 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
Br1 Co1 2.392(3) . ?
Br2 Co1 2.402(3) . ?
Br3 Co1 2.388(3) . ?
Co1 P1 2.358(4) . ?
P1 C1 1.804(14) . ?
P1 C8 1.820(14) . ?
P1 C13 1.805(13) . ?
N2 C33 1.53(2) . ?
N2 C35 1.54(2) . ?
N2 C37 1.49(2) . ?
N2 C39 1.50(2) . ?
C1 C2 1.397(19) . ?
C1 C6 1.415(17) . ?
C2 C3 1.41(2) . ?
C2 B1 1.68(2) . ?
C3 H3 0.9500 . ?
C3 C4 1.37(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.38(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.41(2) . ?
C6 H6 0.9500 . ?
C7 C8 1.444(18) . ?
C7 C12 1.398(19) . ?
C7 B1 1.641(19) . ?
C8 C9 1.398(19) . ?
C9 H9 0.9500 . ?
C9 C10 1.38(2) . ?
C10 H10 0.9500 . ?
C10 C11 1.40(2) . ?
C11 H11 0.9500 . ?
C11 C12 1.38(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.443(17) . ?
C13 C18 1.399(19) . ?
C14 C15 1.387(19) . ?
C14 B1 1.69(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.42(2) . ?
C16 H16 0.9500 . ?
C16 C17 1.40(2) . ?
C17 H17 0.9500 . ?
C17 C18 1.36(2) . ?
C18 H18 0.9500 . ?
C19 C20 1.41(2) . ?
C19 C24 1.39(2) . ?
C19 B1 1.59(2) . ?
C20 H20 0.9500 . ?
C20 C21 1.39(2) . ?
C22 H22 0.9500 . ?
C22 C23 1.30(2) . ?
C22 C21 1.41(2) . ?
C23 H23 0.9500 . ?
C23 C24 1.44(2) . ?
C24 H24 0.9500 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.53(3) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.47(2) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.56(3) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.57(3) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
N1 C25 1.55(2) . ?
N1 C27 1.53(2) . ?
N1 C29 1.51(2) . ?
N1 C31 1.516(19) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.52(2) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.50(2) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.52(2) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.506(19) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C21 H21 0.9500 . ?

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
Br1 Co1 Br2 115.58(13) . . ?
Br3 Co1 Br1 114.62(12) . . ?
Br3 Co1 Br2 109.82(11) . . ?
P1 Co1 Br1 103.98(13) . . ?
P1 Co1 Br2 102.50(12) . . ?
P1 Co1 Br3 109.28(14) . . ?
C1 P1 Co1 117.1(5) . . ?
C1 P1 C8 97.4(7) . . ?
C1 P1 C13 100.4(6) . . ?
C8 P1 Co1 121.6(5) . . ?
C13 P1 Co1 117.4(4) . . ?
C13 P1 C8 98.8(6) . . ?
C33 N2 C35 109.7(13) . . ?
C37 N2 C33 109.3(13) . . ?
C37 N2 C35 106.7(12) . . ?
C37 N2 C39 113.3(14) . . ?
C39 N2 C33 106.0(13) . . ?
C39 N2 C35 111.8(14) . . ?
C2 C1 P1 117.2(10) . . ?
C2 C1 C6 121.5(13) . . ?
C6 C1 P1 121.3(11) . . ?
C1 C2 C3 117.1(12) . . ?
C1 C2 B1 117.8(12) . . ?
C3 C2 B1 125.0(13) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 C2 121.5(14) . . ?
C4 C3 H3 119.2 . . ?
C3 C4 H4 119.0 . . ?
C3 C4 C5 122.0(14) . . ?
C5 C4 H4 119.0 . . ?
C4 C5 H5 120.8 . . ?
C4 C5 C6 118.4(14) . . ?
C6 C5 H5 120.8 . . ?
C1 C6 H6 120.3 . . ?
C5 C6 C1 119.5(14) . . ?
C5 C6 H6 120.3 . . ?
C8 C7 B1 117.8(12) . . ?
C12 C7 C8 113.2(12) . . ?
C12 C7 B1 129.0(13) . . ?
C7 C8 P1 115.8(10) . . ?
C9 C8 P1 121.1(11) . . ?
C9 C8 C7 123.0(13) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 C8 119.6(13) . . ?
C10 C9 H9 120.2 . . ?
C9 C10 H10 120.3 . . ?
C9 C10 C11 119.5(13) . . ?
C11 C10 H10 120.3 . . ?
C10 C11 H11 120.2 . . ?
C12 C11 C10 119.7(14) . . ?
C12 C11 H11 120.2 . . ?
C7 C12 H12 117.8 . . ?
C11 C12 C7 124.5(14) . . ?
C11 C12 H12 117.8 . . ?
C14 C13 P1 114.2(9) . . ?
C18 C13 P1 124.1(10) . . ?
C18 C13 C14 121.7(12) . . ?
C13 C14 B1 119.0(11) . . ?
C15 C14 C13 116.0(13) . . ?
C15 C14 B1 124.9(12) . . ?
C14 C15 H15 118.8 . . ?
C14 C15 C16 122.4(14) . . ?
C16 C15 H15 118.8 . . ?
C15 C16 H16 120.7 . . ?
C17 C16 C15 118.6(14) . . ?
C17 C16 H16 120.7 . . ?
C16 C17 H17 119.2 . . ?
C18 C17 C16 121.6(15) . . ?
C18 C17 H17 119.2 . . ?
C13 C18 H18 120.2 . . ?
C17 C18 C13 119.6(14) . . ?
C17 C18 H18 120.2 . . ?
C20 C19 B1 120.2(13) . . ?
C24 C19 C20 115.9(13) . . ?
C24 C19 B1 123.7(13) . . ?
C19 C20 H20 118.7 . . ?
C21 C20 C19 122.6(14) . . ?
C21 C20 H20 118.7 . . ?
C23 C22 H22 120.6 . . ?
C23 C22 C21 118.8(14) . . ?
C21 C22 H22 120.6 . . ?
C22 C23 H23 118.3 . . ?
C22 C23 C24 123.5(15) . . ?
C24 C23 H23 118.3 . . ?
C19 C24 C23 119.5(15) . . ?
C19 C24 H24 120.3 . . ?
C23 C24 H24 120.3 . . ?
N2 C33 H33A 108.7 . . ?
N2 C33 H33B 108.7 . . ?
N2 C33 C34 114.3(15) . . ?
H33A C33 H33B 107.6 . . ?
C34 C33 H33A 108.7 . . ?
C34 C33 H33B 108.7 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N2 C35 H35A 109.0 . . ?
N2 C35 H35B 109.0 . . ?
H35A C35 H35B 107.8 . . ?
C36 C35 N2 112.9(14) . . ?
C36 C35 H35A 109.0 . . ?
C36 C35 H35B 109.0 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N2 C37 H37A 109.0 . . ?
N2 C37 H37B 109.0 . . ?
N2 C37 C38 112.8(15) . . ?
H37A C37 H37B 107.8 . . ?
C38 C37 H37A 109.0 . . ?
C38 C37 H37B 109.0 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N2 C39 H39A 108.7 . . ?
N2 C39 H39B 108.7 . . ?
N2 C39 C40 114.1(15) . . ?
H39A C39 H39B 107.6 . . ?
C40 C39 H39A 108.7 . . ?
C40 C39 H39B 108.7 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C2 B1 C14 104.3(11) . . ?
C7 B1 C2 102.1(10) . . ?
C7 B1 C14 103.0(11) . . ?
C19 B1 C2 116.3(12) . . ?
C19 B1 C7 121.4(12) . . ?
C19 B1 C14 107.8(10) . . ?
C27 N1 C25 109.8(13) . . ?
C29 N1 C25 105.8(12) . . ?
C29 N1 C27 111.2(12) . . ?
C29 N1 C31 112.4(13) . . ?
C31 N1 C25 112.0(12) . . ?
C31 N1 C27 105.8(11) . . ?
N1 C25 H25A 108.7 . . ?
N1 C25 H25B 108.7 . . ?
H25A C25 H25B 107.6 . . ?
C26 C25 N1 114.1(14) . . ?
C26 C25 H25A 108.7 . . ?
C26 C25 H25B 108.7 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N1 C27 H27A 108.3 . . ?
N1 C27 H27B 108.3 . . ?
H27A C27 H27B 107.4 . . ?
C28 C27 N1 116.1(14) . . ?
C28 C27 H27A 108.3 . . ?
C28 C27 H27B 108.3 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N1 C29 H29A 108.2 . . ?
N1 C29 H29B 108.2 . . ?
N1 C29 C30 116.2(15) . . ?
H29A C29 H29B 107.4 . . ?
C30 C29 H29A 108.2 . . ?
C30 C29 H29B 108.2 . . ?
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 . . ?
N1 C31 H31A 108.5 . . ?
N1 C31 H31B 108.5 . . ?
H31A C31 H31B 107.5 . . ?
C32 C31 N1 114.9(13) . . ?
C32 C31 H31A 108.5 . . ?
C32 C31 H31B 108.5 . . ?
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 . . ?
C20 C21 C22 119.6(15) . . ?
C20 C21 H21 120.2 . . ?
C22 C21 H21 120.2 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.706(4)
2 0.294(4)

####################################################################### 
# 
# 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_v18066
_database_code_depnum_ccdc_archive 'CCDC 1824472'
_audit_update_record             
;
2018-02-16 deposited with the CCDC.
2018-06-22 downloaded from the CCDC.
;
_audit_creation_date             2018-02-13
_audit_creation_method           
;
Olex2 1.2
(compiled Aug 10 2017 17:28:52 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        
'5-azoniaspiro[4.4]nonane 10-phenyl-9-phosphatriptycene-10-borate selenide'
_chemical_formula_moiety         'C24 H17 B P Se, C8 H16 N'
_chemical_formula_sum            'C32 H33 B N P Se'
_chemical_formula_weight         552.33
_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'
B B 0.0013 0.0007 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 '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           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'

_cell_length_a                   17.601(3)
_cell_length_b                   17.365(2)
_cell_length_c                   17.358(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5305.3(13)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9053
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.993
_cell_measurement_theta_min      2.314
_shelx_estimated_absorpt_T_max   0.919
_shelx_estimated_absorpt_T_min   0.807
_exptl_absorpt_coefficient_mu    1.498
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8510
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0780 before and 0.0625 after correction.
The Ratio of minimum to maximum transmission is 0.8510.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.057
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1514
_diffrn_reflns_av_unetI/netI     0.0685
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            198273
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.404
_diffrn_reflns_theta_min         2.314
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker AXS D8 Venture Kappa'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.946
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                18763
_reflns_number_total             22073
_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 v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         1.414
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 
;
 Flack x determined using 7530 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.004(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         22073
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0453
_refine_ls_restrained_S_all      1.024
_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)+(0.0642P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1133
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.419(6)
 0.581(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,
 H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C57(H57A,H57B),
 C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B),
  C63(H63A,H63B), C64(H64A,H64B)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23),
  C24(H24), C35(H35), C36(H36), C37(H37), C38(H38), C41(H41), C42(H42),
 C43(H43), C44(H44), C47(H47), C48(H48), C49(H49), C50(H50), C52(H52), C53(H53),
  C54(H54), C55(H55), C56(H56)
;
_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
Se1 Se 0.30642(2) -0.11452(2) 0.74092(2) 0.01819(7) Uani 1 1 d . . . . .
P1 P 0.34336(4) -0.02863(4) 0.66399(4) 0.01213(13) Uani 1 1 d . . . . .
C1 C 0.33567(17) -0.04891(16) 0.56283(16) 0.0131(5) Uani 1 1 d . . . . .
C2 C 0.36403(18) 0.01149(16) 0.51728(16) 0.0134(5) Uani 1 1 d . . . . .
C3 C 0.29790(16) 0.06485(17) 0.66831(17) 0.0143(5) Uani 1 1 d . . . . .
C4 C 0.32838(19) 0.11982(17) 0.61608(17) 0.0152(5) Uani 1 1 d . . . . .
C5 C 0.44078(17) 0.00171(16) 0.67290(16) 0.0132(5) Uani 1 1 d . . . . .
C6 C 0.46145(17) 0.06184(17) 0.62279(16) 0.0141(5) Uani 1 1 d . . . . .
C7 C 0.53351(19) 0.09376(18) 0.63596(17) 0.0172(5) Uani 1 1 d . . . . .
H7 H 0.549398 0.136277 0.605511 0.021 Uiso 1 1 calc R . . . .
C8 C 0.58259(19) 0.0653(2) 0.69214(18) 0.0208(6) Uani 1 1 d . . . . .
H8 H 0.631091 0.088225 0.699200 0.025 Uiso 1 1 calc R . . . .
C9 C 0.56080(19) 0.0034(2) 0.73785(19) 0.0218(6) Uani 1 1 d . . . . .
H9 H 0.594956 -0.017012 0.774968 0.026 Uiso 1 1 calc R . . . .
C10 C 0.48880(18) -0.02844(18) 0.72910(16) 0.0175(5) Uani 1 1 d . . . . .
H10 H 0.472714 -0.069935 0.760817 0.021 Uiso 1 1 calc R . . . .
C11 C 0.2984(2) 0.19408(19) 0.62308(19) 0.0204(6) Uani 1 1 d . . . . .
H11 H 0.316813 0.233626 0.590219 0.024 Uiso 1 1 calc R . . . .
C12 C 0.2420(2) 0.21183(19) 0.67696(19) 0.0238(7) Uani 1 1 d . . . . .
H12 H 0.223382 0.263068 0.680128 0.029 Uiso 1 1 calc R . . . .
C13 C 0.2130(2) 0.1564(2) 0.7256(2) 0.0240(7) Uani 1 1 d . . . . .
H13 H 0.173990 0.169129 0.761179 0.029 Uiso 1 1 calc R . . . .
C14 C 0.24145(19) 0.08161(19) 0.72198(17) 0.0192(6) Uani 1 1 d . . . . .
H14 H 0.222684 0.042777 0.755511 0.023 Uiso 1 1 calc R . . . .
C15 C 0.30212(19) -0.11493(18) 0.5335(2) 0.0181(6) Uani 1 1 d . . . . .
H15 H 0.283450 -0.153698 0.567121 0.022 Uiso 1 1 calc R . . . .
C16 C 0.2962(2) -0.1236(2) 0.4540(2) 0.0217(7) Uani 1 1 d . . . . .
H16 H 0.272668 -0.167829 0.432405 0.026 Uiso 1 1 calc R . . . .
C17 C 0.3255(2) -0.0660(2) 0.40667(18) 0.0238(7) Uani 1 1 d . . . . .
H17 H 0.322961 -0.072024 0.352338 0.029 Uiso 1 1 calc R . . . .
C18 C 0.3584(2) 0.00020(18) 0.43705(16) 0.0181(6) Uani 1 1 d . . . . .
H18 H 0.377404 0.038530 0.403096 0.022 Uiso 1 1 calc R . . . .
C19 C 0.4288(2) 0.14617(17) 0.49150(16) 0.0163(5) Uani 1 1 d . . . . .
C20 C 0.3848(2) 0.20180(19) 0.45326(18) 0.0191(6) Uani 1 1 d . . . . .
H20 H 0.334741 0.211587 0.471365 0.023 Uiso 1 1 calc R . . . .
C21 C 0.4113(2) 0.24332(19) 0.38977(18) 0.0245(7) Uani 1 1 d . . . . .
H21 H 0.379504 0.280410 0.365677 0.029 Uiso 1 1 calc R . . . .
C22 C 0.4840(2) 0.23036(19) 0.36196(17) 0.0238(7) Uani 1 1 d . . . . .
H22 H 0.502658 0.258891 0.319259 0.029 Uiso 1 1 calc R . . . .
C23 C 0.5293(2) 0.1752(2) 0.39726(18) 0.0236(7) Uani 1 1 d . . . . .
H23 H 0.579089 0.165325 0.378684 0.028 Uiso 1 1 calc R . . . .
C24 C 0.5009(2) 0.13434(19) 0.46027(18) 0.0197(6) Uani 1 1 d . . . . .
H24 H 0.532521 0.096338 0.483169 0.024 Uiso 1 1 calc R . . . .
B1 B 0.3973(2) 0.09006(18) 0.55880(18) 0.0141(6) Uani 1 1 d . . . . .
Se2 Se 0.29699(2) 0.39962(2) 0.27023(2) 0.01455(6) Uani 1 1 d . . . . .
P2 P 0.35370(4) 0.47892(4) 0.34173(4) 0.01041(12) Uani 1 1 d . . . . .
C33 C 0.34079(17) 0.47039(16) 0.44431(15) 0.0120(5) Uani 1 1 d . . . . .
C34 C 0.38252(17) 0.52578(16) 0.48570(15) 0.0123(5) Uani 1 1 d . . . . .
C35 C 0.37580(19) 0.52179(17) 0.56642(16) 0.0163(5) Uani 1 1 d . . . . .
H35 H 0.403613 0.556956 0.597448 0.020 Uiso 1 1 calc R . . . .
C36 C 0.3293(2) 0.46741(19) 0.60175(17) 0.0201(6) Uani 1 1 d . . . . .
H36 H 0.325803 0.466432 0.656358 0.024 Uiso 1 1 calc R . . . .
C37 C 0.2877(2) 0.4144(2) 0.55868(19) 0.0201(6) Uani 1 1 d . . . . .
H37 H 0.255565 0.378090 0.583441 0.024 Uiso 1 1 calc R . . . .
C38 C 0.29414(18) 0.41551(19) 0.47849(19) 0.0168(5) Uani 1 1 d . . . . .
H38 H 0.267119 0.379411 0.447825 0.020 Uiso 1 1 calc R . . . .
C39 C 0.33329(17) 0.57992(16) 0.32709(14) 0.0116(5) Uani 1 1 d . . . . .
C40 C 0.37632(17) 0.62944(16) 0.37496(15) 0.0124(5) Uani 1 1 d . . . . .
C41 C 0.36838(19) 0.70842(17) 0.35956(16) 0.0159(5) Uani 1 1 d . . . . .
H41 H 0.397382 0.744308 0.388563 0.019 Uiso 1 1 calc R . . . .
C42 C 0.3191(2) 0.73558(18) 0.30291(18) 0.0191(6) Uani 1 1 d . . . . .
H42 H 0.315586 0.789429 0.293920 0.023 Uiso 1 1 calc R . . . .
C43 C 0.27496(19) 0.68537(18) 0.25918(16) 0.0179(6) Uani 1 1 d . . . . .
H43 H 0.239873 0.704638 0.222339 0.022 Uiso 1 1 calc R . . . .
C44 C 0.28323(16) 0.60598(16) 0.27052(19) 0.0149(5) Uani 1 1 d . . . . .
H44 H 0.255189 0.570425 0.240155 0.018 Uiso 1 1 calc R . . . .
C45 C 0.45573(16) 0.48136(16) 0.33462(16) 0.0120(5) Uani 1 1 d . . . . .
C46 C 0.49060(17) 0.53951(16) 0.38050(15) 0.0121(5) Uani 1 1 d . . . . .
C47 C 0.56827(17) 0.54985(18) 0.36709(16) 0.0154(5) Uani 1 1 d . . . . .
H47 H 0.593947 0.590684 0.392569 0.018 Uiso 1 1 calc R . . . .
C48 C 0.60954(18) 0.50193(18) 0.31726(16) 0.0178(5) Uani 1 1 d . . . . .
H48 H 0.662515 0.510097 0.310679 0.021 Uiso 1 1 calc R . . . .
C49 C 0.57377(17) 0.44246(18) 0.27726(17) 0.0175(5) Uani 1 1 d . . . . .
H49 H 0.602282 0.408673 0.245366 0.021 Uiso 1 1 calc R . . . .
C50 C 0.49556(18) 0.43349(17) 0.28490(15) 0.0145(5) Uani 1 1 d . . . . .
H50 H 0.469634 0.394931 0.256335 0.017 Uiso 1 1 calc R . . . .
C51 C 0.47255(17) 0.64665(17) 0.50073(16) 0.0131(5) Uani 1 1 d . . . . .
C52 C 0.54344(19) 0.63224(18) 0.53511(17) 0.0167(5) Uani 1 1 d . . . . .
H52 H 0.574453 0.592442 0.514587 0.020 Uiso 1 1 calc R . . . .
C53 C 0.5700(2) 0.6741(2) 0.59821(17) 0.0205(6) Uani 1 1 d . . . . .
H53 H 0.618500 0.662682 0.619423 0.025 Uiso 1 1 calc R . . . .
C54 C 0.5262(2) 0.73240(19) 0.63023(18) 0.0210(6) Uani 1 1 d . . . . .
H54 H 0.544437 0.761266 0.672876 0.025 Uiso 1 1 calc R . . . .
C55 C 0.4552(2) 0.74778(19) 0.59884(18) 0.0204(6) Uani 1 1 d . . . . .
H55 H 0.423964 0.786802 0.620547 0.025 Uiso 1 1 calc R . . . .
C56 C 0.42975(19) 0.70567(18) 0.53523(16) 0.0164(5) Uani 1 1 d . . . . .
H56 H 0.381255 0.717501 0.514309 0.020 Uiso 1 1 calc R . . . .
B2 B 0.43406(19) 0.58935(19) 0.43769(18) 0.0117(5) Uani 1 1 d . . . . .
N1 N 0.57263(18) 0.36137(16) 0.55610(15) 0.0193(5) Uani 1 1 d . . . . .
C25 C 0.5699(2) 0.4199(2) 0.6201(2) 0.0253(7) Uani 1 1 d . . . . .
H25A H 0.545515 0.468190 0.602498 0.030 Uiso 1 1 calc R . . . .
H25B H 0.621593 0.431810 0.639149 0.030 Uiso 1 1 calc R . . . .
C26 C 0.5224(2) 0.3810(2) 0.6828(2) 0.0255(7) Uani 1 1 d . . . . .
H26A H 0.489042 0.418910 0.708657 0.031 Uiso 1 1 calc R . . . .
H26B H 0.555650 0.356818 0.721933 0.031 Uiso 1 1 calc R . . . .
C27 C 0.4746(2) 0.3193(2) 0.6409(2) 0.0228(6) Uani 1 1 d . . . . .
H27A H 0.488601 0.267028 0.658599 0.027 Uiso 1 1 calc R . . . .
H27B H 0.419704 0.327486 0.650416 0.027 Uiso 1 1 calc R . . . .
C28 C 0.4931(2) 0.3296(2) 0.55595(19) 0.0232(6) Uani 1 1 d . . . . .
H28A H 0.490960 0.279683 0.528411 0.028 Uiso 1 1 calc R . . . .
H28B H 0.457347 0.365969 0.531259 0.028 Uiso 1 1 calc R . . . .
C29 C 0.6315(2) 0.3001(2) 0.5710(2) 0.0252(7) Uani 1 1 d . . . . .
H29A H 0.618449 0.251765 0.543792 0.030 Uiso 1 1 calc R . . . .
H29B H 0.635988 0.289267 0.626823 0.030 Uiso 1 1 calc R . . . .
C30 C 0.7046(2) 0.3343(3) 0.5396(3) 0.0340(9) Uani 1 1 d . . . . .
H30A H 0.735172 0.294286 0.513381 0.041 Uiso 1 1 calc R . . . .
H30B H 0.735321 0.356678 0.581894 0.041 Uiso 1 1 calc R . . . .
C31 C 0.6806(3) 0.3974(3) 0.4822(3) 0.0419(11) Uani 1 1 d . . . . .
H31A H 0.697178 0.448784 0.500361 0.050 Uiso 1 1 calc R . . . .
H31B H 0.703027 0.387777 0.430787 0.050 Uiso 1 1 calc R . . . .
C32 C 0.5956(3) 0.3931(3) 0.4786(2) 0.0328(9) Uani 1 1 d . . . . .
H32A H 0.578936 0.358472 0.436594 0.039 Uiso 1 1 calc R . . . .
H32B H 0.573282 0.444746 0.470236 0.039 Uiso 1 1 calc R . . . .
N2 N 0.61195(17) 0.87698(16) 0.40733(16) 0.0191(5) Uani 1 1 d . . . . .
C57 C 0.5608(2) 0.8638(2) 0.4761(2) 0.0249(7) Uani 1 1 d . . . . .
H57A H 0.560524 0.808739 0.491004 0.030 Uiso 1 1 calc R . . . .
H57B H 0.508099 0.880054 0.464619 0.030 Uiso 1 1 calc R . . . .
C58 C 0.5950(3) 0.9131(2) 0.5397(2) 0.0291(8) Uani 1 1 d . . . . .
H58A H 0.625199 0.881115 0.575658 0.035 Uiso 1 1 calc R . . . .
H58B H 0.554624 0.939711 0.569188 0.035 Uiso 1 1 calc R . . . .
C59 C 0.6463(2) 0.9720(2) 0.4983(2) 0.0264(7) Uani 1 1 d . . . . .
H59A H 0.634259 1.025113 0.515089 0.032 Uiso 1 1 calc R . . . .
H59B H 0.700571 0.961518 0.509035 0.032 Uiso 1 1 calc R . . . .
C60 C 0.6291(2) 0.9617(2) 0.4130(2) 0.0265(7) Uani 1 1 d . . . . .
H60A H 0.584807 0.993063 0.397155 0.032 Uiso 1 1 calc R . . . .
H60B H 0.673419 0.975739 0.380845 0.032 Uiso 1 1 calc R . . . .
C61 C 0.6819(2) 0.8290(2) 0.4135(2) 0.0245(7) Uani 1 1 d . . . . .
H61A H 0.699047 0.825460 0.467719 0.029 Uiso 1 1 calc R . . . .
H61B H 0.723456 0.850957 0.382013 0.029 Uiso 1 1 calc R . . . .
C62 C 0.6587(2) 0.7505(2) 0.3834(2) 0.0292(8) Uani 1 1 d . . . . .
H62A H 0.644353 0.716067 0.426408 0.035 Uiso 1 1 calc R . . . .
H62B H 0.700967 0.726547 0.354365 0.035 Uiso 1 1 calc R . . . .
C63 C 0.5900(3) 0.7651(2) 0.3300(2) 0.0328(8) Uani 1 1 d . . . . .
H63A H 0.600903 0.747018 0.277017 0.039 Uiso 1 1 calc R . . . .
H63B H 0.544366 0.737961 0.349346 0.039 Uiso 1 1 calc R . . . .
C64 C 0.5777(3) 0.8521(2) 0.3310(2) 0.0298(8) Uani 1 1 d . . . . .
H64A H 0.604076 0.877074 0.287267 0.036 Uiso 1 1 calc R . . . .
H64B H 0.522974 0.864845 0.328646 0.036 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
Se1 P1 2.1050(8) . ?
P1 C1 1.796(3) . ?
P1 C3 1.811(3) . ?
P1 C5 1.801(3) . ?
C1 C2 1.405(4) . ?
C1 C15 1.387(4) . ?
C2 C18 1.410(4) . ?
C2 B1 1.650(4) . ?
C3 C4 1.422(4) . ?
C3 C14 1.393(4) . ?
C4 C11 1.399(4) . ?
C4 B1 1.652(5) . ?
C5 C6 1.407(4) . ?
C5 C10 1.393(4) . ?
C6 C7 1.403(4) . ?
C6 B1 1.658(4) . ?
C7 H7 0.9500 . ?
C7 C8 1.394(5) . ?
C8 H8 0.9500 . ?
C8 C9 1.389(5) . ?
C9 H9 0.9500 . ?
C9 C10 1.391(5) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C11 C12 1.397(5) . ?
C12 H12 0.9500 . ?
C12 C13 1.377(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.394(5) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C15 C16 1.392(5) . ?
C16 H16 0.9500 . ?
C16 C17 1.393(5) . ?
C17 H17 0.9500 . ?
C17 C18 1.390(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.406(4) . ?
C19 C24 1.395(5) . ?
C19 B1 1.619(4) . ?
C20 H20 0.9500 . ?
C20 C21 1.397(5) . ?
C21 H21 0.9500 . ?
C21 C22 1.387(6) . ?
C22 H22 0.9500 . ?
C22 C23 1.388(5) . ?
C23 H23 0.9500 . ?
C23 C24 1.396(4) . ?
C24 H24 0.9500 . ?
Se2 P2 2.1054(8) . ?
P2 C33 1.801(3) . ?
P2 C39 1.808(3) . ?
P2 C45 1.801(3) . ?
C33 C34 1.407(4) . ?
C33 C38 1.391(4) . ?
C34 C35 1.408(4) . ?
C34 B2 1.654(4) . ?
C35 H35 0.9500 . ?
C35 C36 1.392(4) . ?
C36 H36 0.9500 . ?
C36 C37 1.394(5) . ?
C37 H37 0.9500 . ?
C37 C38 1.397(4) . ?
C38 H38 0.9500 . ?
C39 C40 1.415(4) . ?
C39 C44 1.395(4) . ?
C40 C41 1.404(4) . ?
C40 B2 1.644(4) . ?
C41 H41 0.9500 . ?
C41 C42 1.393(4) . ?
C42 H42 0.9500 . ?
C42 C43 1.393(5) . ?
C43 H43 0.9500 . ?
C43 C44 1.400(4) . ?
C44 H44 0.9500 . ?
C45 C46 1.425(4) . ?
C45 C50 1.388(4) . ?
C46 C47 1.398(4) . ?
C46 B2 1.651(4) . ?
C47 H47 0.9500 . ?
C47 C48 1.403(4) . ?
C48 H48 0.9500 . ?
C48 C49 1.395(4) . ?
C49 H49 0.9500 . ?
C49 C50 1.392(4) . ?
C50 H50 0.9500 . ?
C51 C52 1.406(4) . ?
C51 C56 1.406(4) . ?
C51 B2 1.627(4) . ?
C52 H52 0.9500 . ?
C52 C53 1.396(4) . ?
C53 H53 0.9500 . ?
C53 C54 1.389(5) . ?
C54 H54 0.9500 . ?
C54 C55 1.390(5) . ?
C55 H55 0.9500 . ?
C55 C56 1.398(4) . ?
C56 H56 0.9500 . ?
N1 C25 1.507(4) . ?
N1 C28 1.504(5) . ?
N1 C29 1.508(4) . ?
N1 C32 1.508(4) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.530(5) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.543(5) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.521(5) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.519(5) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.541(6) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.499(7) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
N2 C57 1.512(4) . ?
N2 C60 1.505(4) . ?
N2 C61 1.491(5) . ?
N2 C64 1.518(4) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C57 C58 1.523(5) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C58 C59 1.542(6) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C59 C60 1.521(5) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C61 C62 1.515(5) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C62 C63 1.545(6) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C63 C64 1.525(5) . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?

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 P1 Se1 117.26(10) . . ?
C1 P1 C3 100.54(13) . . ?
C1 P1 C5 102.31(14) . . ?
C3 P1 Se1 118.18(10) . . ?
C5 P1 Se1 116.55(10) . . ?
C5 P1 C3 98.91(13) . . ?
C2 C1 P1 112.2(2) . . ?
C15 C1 P1 123.6(2) . . ?
C15 C1 C2 124.2(3) . . ?
C1 C2 C18 115.3(3) . . ?
C1 C2 B1 119.8(2) . . ?
C18 C2 B1 124.8(3) . . ?
C4 C3 P1 114.1(2) . . ?
C14 C3 P1 122.0(2) . . ?
C14 C3 C4 123.7(3) . . ?
C3 C4 B1 116.8(2) . . ?
C11 C4 C3 114.9(3) . . ?
C11 C4 B1 128.2(3) . . ?
C6 C5 P1 114.2(2) . . ?
C10 C5 P1 121.9(2) . . ?
C10 C5 C6 123.7(3) . . ?
C5 C6 B1 117.2(3) . . ?
C7 C6 C5 115.2(3) . . ?
C7 C6 B1 127.4(3) . . ?
C6 C7 H7 118.9 . . ?
C8 C7 C6 122.3(3) . . ?
C8 C7 H7 118.9 . . ?
C7 C8 H8 119.9 . . ?
C9 C8 C7 120.2(3) . . ?
C9 C8 H8 119.9 . . ?
C8 C9 H9 120.1 . . ?
C8 C9 C10 119.8(3) . . ?
C10 C9 H9 120.1 . . ?
C5 C10 H10 120.7 . . ?
C9 C10 C5 118.7(3) . . ?
C9 C10 H10 120.7 . . ?
C4 C11 H11 119.0 . . ?
C12 C11 C4 122.0(3) . . ?
C12 C11 H11 119.0 . . ?
C11 C12 H12 119.4 . . ?
C13 C12 C11 121.3(3) . . ?
C13 C12 H12 119.4 . . ?
C12 C13 H13 120.3 . . ?
C12 C13 C14 119.4(3) . . ?
C14 C13 H13 120.3 . . ?
C3 C14 C13 118.7(3) . . ?
C3 C14 H14 120.6 . . ?
C13 C14 H14 120.6 . . ?
C1 C15 H15 120.5 . . ?
C1 C15 C16 119.0(3) . . ?
C16 C15 H15 120.5 . . ?
C15 C16 H16 120.7 . . ?
C15 C16 C17 118.6(3) . . ?
C17 C16 H16 120.7 . . ?
C16 C17 H17 119.2 . . ?
C18 C17 C16 121.6(3) . . ?
C18 C17 H17 119.2 . . ?
C2 C18 H18 119.4 . . ?
C17 C18 C2 121.3(3) . . ?
C17 C18 H18 119.4 . . ?
C20 C19 B1 124.4(3) . . ?
C24 C19 C20 114.8(3) . . ?
C24 C19 B1 120.2(3) . . ?
C19 C20 H20 118.6 . . ?
C21 C20 C19 122.9(3) . . ?
C21 C20 H20 118.6 . . ?
C20 C21 H21 120.0 . . ?
C22 C21 C20 120.0(3) . . ?
C22 C21 H21 120.0 . . ?
C21 C22 H22 120.4 . . ?
C21 C22 C23 119.2(3) . . ?
C23 C22 H22 120.4 . . ?
C22 C23 H23 120.3 . . ?
C22 C23 C24 119.5(3) . . ?
C24 C23 H23 120.3 . . ?
C19 C24 C23 123.7(3) . . ?
C19 C24 H24 118.2 . . ?
C23 C24 H24 118.2 . . ?
C2 B1 C4 105.1(2) . . ?
C2 B1 C6 106.9(2) . . ?
C4 B1 C6 100.9(2) . . ?
C19 B1 C2 107.7(2) . . ?
C19 B1 C4 119.8(3) . . ?
C19 B1 C6 115.3(3) . . ?
C33 P2 Se2 117.98(10) . . ?
C33 P2 C39 101.17(12) . . ?
C39 P2 Se2 117.21(9) . . ?
C45 P2 Se2 116.60(10) . . ?
C45 P2 C33 101.27(13) . . ?
C45 P2 C39 99.53(13) . . ?
C34 C33 P2 112.5(2) . . ?
C38 C33 P2 123.5(2) . . ?
C38 C33 C34 124.0(3) . . ?
C33 C34 C35 115.5(3) . . ?
C33 C34 B2 119.0(2) . . ?
C35 C34 B2 125.5(3) . . ?
C34 C35 H35 119.3 . . ?
C36 C35 C34 121.4(3) . . ?
C36 C35 H35 119.3 . . ?
C35 C36 H36 119.3 . . ?
C35 C36 C37 121.4(3) . . ?
C37 C36 H36 119.3 . . ?
C36 C37 H37 120.6 . . ?
C36 C37 C38 118.9(3) . . ?
C38 C37 H37 120.6 . . ?
C33 C38 C37 118.8(3) . . ?
C33 C38 H38 120.6 . . ?
C37 C38 H38 120.6 . . ?
C40 C39 P2 113.6(2) . . ?
C44 C39 P2 122.6(2) . . ?
C44 C39 C40 123.7(3) . . ?
C39 C40 B2 117.5(2) . . ?
C41 C40 C39 115.4(3) . . ?
C41 C40 B2 127.0(3) . . ?
C40 C41 H41 119.1 . . ?
C42 C41 C40 121.8(3) . . ?
C42 C41 H41 119.1 . . ?
C41 C42 H42 119.3 . . ?
C43 C42 C41 121.3(3) . . ?
C43 C42 H42 119.3 . . ?
C42 C43 H43 120.6 . . ?
C42 C43 C44 118.8(3) . . ?
C44 C43 H43 120.6 . . ?
C39 C44 C43 118.9(3) . . ?
C39 C44 H44 120.5 . . ?
C43 C44 H44 120.5 . . ?
C46 C45 P2 114.1(2) . . ?
C50 C45 P2 122.1(2) . . ?
C50 C45 C46 123.7(3) . . ?
C45 C46 B2 116.6(2) . . ?
C47 C46 C45 114.8(3) . . ?
C47 C46 B2 128.5(3) . . ?
C46 C47 H47 118.9 . . ?
C46 C47 C48 122.2(3) . . ?
C48 C47 H47 118.9 . . ?
C47 C48 H48 119.6 . . ?
C49 C48 C47 120.8(3) . . ?
C49 C48 H48 119.6 . . ?
C48 C49 H49 120.6 . . ?
C50 C49 C48 118.8(3) . . ?
C50 C49 H49 120.6 . . ?
C45 C50 C49 119.5(3) . . ?
C45 C50 H50 120.3 . . ?
C49 C50 H50 120.3 . . ?
C52 C51 C56 115.1(3) . . ?
C52 C51 B2 123.1(3) . . ?
C56 C51 B2 120.6(3) . . ?
C51 C52 H52 118.7 . . ?
C53 C52 C51 122.6(3) . . ?
C53 C52 H52 118.7 . . ?
C52 C53 H53 119.8 . . ?
C54 C53 C52 120.5(3) . . ?
C54 C53 H53 119.8 . . ?
C53 C54 H54 120.6 . . ?
C53 C54 C55 118.9(3) . . ?
C55 C54 H54 120.6 . . ?
C54 C55 H55 120.1 . . ?
C54 C55 C56 119.8(3) . . ?
C56 C55 H55 120.1 . . ?
C51 C56 H56 118.4 . . ?
C55 C56 C51 123.1(3) . . ?
C55 C56 H56 118.4 . . ?
C40 B2 C34 106.1(2) . . ?
C40 B2 C46 101.3(2) . . ?
C46 B2 C34 106.5(2) . . ?
C51 B2 C34 107.3(2) . . ?
C51 B2 C40 116.4(2) . . ?
C51 B2 C46 118.3(3) . . ?
C25 N1 C29 111.8(3) . . ?
C25 N1 C32 114.8(3) . . ?
C28 N1 C25 102.7(3) . . ?
C28 N1 C29 112.4(3) . . ?
C28 N1 C32 112.5(3) . . ?
C29 N1 C32 103.1(3) . . ?
N1 C25 H25A 110.9 . . ?
N1 C25 H25B 110.9 . . ?
N1 C25 C26 104.1(3) . . ?
H25A C25 H25B 109.0 . . ?
C26 C25 H25A 110.9 . . ?
C26 C25 H25B 110.9 . . ?
C25 C26 H26A 110.6 . . ?
C25 C26 H26B 110.6 . . ?
C25 C26 C27 105.6(3) . . ?
H26A C26 H26B 108.7 . . ?
C27 C26 H26A 110.6 . . ?
C27 C26 H26B 110.6 . . ?
C26 C27 H27A 110.7 . . ?
C26 C27 H27B 110.7 . . ?
H27A C27 H27B 108.8 . . ?
C28 C27 C26 105.0(3) . . ?
C28 C27 H27A 110.7 . . ?
C28 C27 H27B 110.7 . . ?
N1 C28 C27 103.9(3) . . ?
N1 C28 H28A 111.0 . . ?
N1 C28 H28B 111.0 . . ?
C27 C28 H28A 111.0 . . ?
C27 C28 H28B 111.0 . . ?
H28A C28 H28B 109.0 . . ?
N1 C29 H29A 110.9 . . ?
N1 C29 H29B 110.9 . . ?
N1 C29 C30 104.2(3) . . ?
H29A C29 H29B 108.9 . . ?
C30 C29 H29A 110.9 . . ?
C30 C29 H29B 110.9 . . ?
C29 C30 H30A 110.5 . . ?
C29 C30 H30B 110.5 . . ?
C29 C30 C31 106.1(3) . . ?
H30A C30 H30B 108.7 . . ?
C31 C30 H30A 110.5 . . ?
C31 C30 H30B 110.5 . . ?
C30 C31 H31A 110.7 . . ?
C30 C31 H31B 110.7 . . ?
H31A C31 H31B 108.8 . . ?
C32 C31 C30 105.4(3) . . ?
C32 C31 H31A 110.7 . . ?
C32 C31 H31B 110.7 . . ?
N1 C32 H32A 110.9 . . ?
N1 C32 H32B 110.9 . . ?
C31 C32 N1 104.4(3) . . ?
C31 C32 H32A 110.9 . . ?
C31 C32 H32B 110.9 . . ?
H32A C32 H32B 108.9 . . ?
C57 N2 C64 114.2(3) . . ?
C60 N2 C57 102.5(3) . . ?
C60 N2 C64 114.5(3) . . ?
C61 N2 C57 110.5(3) . . ?
C61 N2 C60 112.1(3) . . ?
C61 N2 C64 103.4(3) . . ?
N2 C57 H57A 110.8 . . ?
N2 C57 H57B 110.8 . . ?
N2 C57 C58 104.6(3) . . ?
H57A C57 H57B 108.9 . . ?
C58 C57 H57A 110.8 . . ?
C58 C57 H57B 110.8 . . ?
C57 C58 H58A 110.7 . . ?
C57 C58 H58B 110.7 . . ?
C57 C58 C59 105.4(3) . . ?
H58A C58 H58B 108.8 . . ?
C59 C58 H58A 110.7 . . ?
C59 C58 H58B 110.7 . . ?
C58 C59 H59A 110.7 . . ?
C58 C59 H59B 110.7 . . ?
H59A C59 H59B 108.8 . . ?
C60 C59 C58 105.0(3) . . ?
C60 C59 H59A 110.7 . . ?
C60 C59 H59B 110.7 . . ?
N2 C60 C59 102.7(3) . . ?
N2 C60 H60A 111.2 . . ?
N2 C60 H60B 111.2 . . ?
C59 C60 H60A 111.2 . . ?
C59 C60 H60B 111.2 . . ?
H60A C60 H60B 109.1 . . ?
N2 C61 H61A 110.8 . . ?
N2 C61 H61B 110.8 . . ?
N2 C61 C62 104.8(3) . . ?
H61A C61 H61B 108.9 . . ?
C62 C61 H61A 110.8 . . ?
C62 C61 H61B 110.8 . . ?
C61 C62 H62A 110.6 . . ?
C61 C62 H62B 110.6 . . ?
C61 C62 C63 105.7(3) . . ?
H62A C62 H62B 108.7 . . ?
C63 C62 H62A 110.6 . . ?
C63 C62 H62B 110.6 . . ?
C62 C63 H63A 110.7 . . ?
C62 C63 H63B 110.7 . . ?
H63A C63 H63B 108.8 . . ?
C64 C63 C62 105.4(3) . . ?
C64 C63 H63A 110.7 . . ?
C64 C63 H63B 110.7 . . ?
N2 C64 C63 103.7(3) . . ?
N2 C64 H64A 111.0 . . ?
N2 C64 H64B 111.0 . . ?
C63 C64 H64A 111.0 . . ?
C63 C64 H64B 111.0 . . ?
H64A C64 H64B 109.0 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.419(6)
2 0.581(6)

####################################################################### 
# 
# 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_p17305_final
_database_code_depnum_ccdc_archive 'CCDC 1824474'
_audit_update_record             
;
2018-02-16 deposited with the CCDC.
2018-06-22 downloaded from the CCDC.
;
_audit_creation_date             2018-02-16
_audit_creation_method           
;
Olex2 1.2
(compiled Aug 10 2017 17:28:52 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        
'Tetrakis(ethylammonium) 10-phenyl-9-phosphatriptycene-10-borate'
_chemical_formula_moiety         'C24 H17 B P, C8 H20 N'
_chemical_formula_sum            'C32 H37 B N P'
_chemical_formula_weight         477.40
_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'
B B 0.0013 0.0007 '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'
P P 0.1023 0.0942 '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                   18.893(2)
_cell_length_b                   15.0154(15)
_cell_length_c                   20.461(2)
_cell_angle_alpha                90
_cell_angle_beta                 114.845(4)
_cell_angle_gamma                90
_cell_volume                     5267.4(9)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.502
_cell_measurement_theta_min      2.356
_shelx_estimated_absorpt_T_max   0.981
_shelx_estimated_absorpt_T_min   0.961
_exptl_absorpt_coefficient_mu    0.126
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0947 before and 0.0726 after correction.
The Ratio of minimum to maximum transmission is 0.9250.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0798
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_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            205507
_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         27.504
_diffrn_reflns_theta_min         2.356
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker AXS D8 Venture Kappa'
_diffrn_measurement_method       ?
_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                9771
_reflns_number_total             12103
_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 v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.846
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.251
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     639
_refine_ls_number_reflns         12103
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0441
_refine_ls_restrained_S_all      1.251
_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)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1560
_refine_ls_wR_factor_ref         0.1646
_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 Secondary CH2 refined with riding coordinates:
 C014(H01D,H01F), C01F(H01N,H01O), C01H(H01P,H01Q), C01I(H01S,H01T), C01P(H1AA,
 HE), C01Q(H2AA,HF), C01S(H3AA,HG), C01W(H6AA,HN)
2.b Aromatic/amide H refined with riding coordinates:
 C005(H005), C009(H009), C00B(H00B), C00F(H00F), C00G(H00G), C00I(H00I),
 C00K(H00K), C00L(H00L), C00M(H00M), C00P(H00P), C00Q(H00Q), C00S(H00S),
 C00T(H00T), C00U(H00U), C00X(H00X), C00Y(H00Y), C00Z(H00Z), C010(H010),
 C011(H011), C012(H012), C013(H013), C015(H015), C016(H016), C017(H017),
 C019(H019), C01A(H01A), C01B(H01B), C01C(H01C), C01E(H01E), C01G(H01G),
 C01J(H01J), C01L(H01L), C01M(H01M), C01R(H01R)
2.c Idealised Me refined as rotating group:
 C018(H01,H,HA), C01D(H01H,H01I,H01K), C01K(H0AA,HB,HC), C01N(H01U,H01V,H01W),
 C01O(H01X,H01Y,HD), C01T(H4AA,HH,HI), C01U(H5AA,HJ,HK), C01V(H01Z,HL,HM)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
P001 P 0.06881(2) 0.11503(2) 0.44697(2) 0.01592(11) Uani 1 1 d . . . . .
P002 P 0.55333(2) 0.11278(2) 0.93070(2) 0.01708(11) Uani 1 1 d . . . . .
N003 N -0.07947(7) 0.18139(8) 0.07777(6) 0.0136(2) Uani 1 1 d . . . . .
N004 N 0.42015(7) 0.19002(8) 0.57348(6) 0.0129(2) Uani 1 1 d . . . . .
C005 C 0.14454(8) 0.20134(10) 0.29909(7) 0.0153(3) Uani 1 1 d . . . . .
H005 H 0.151574 0.256705 0.280138 0.018 Uiso 1 1 calc R . . . .
C006 C 0.62486(8) 0.38106(9) 0.86309(7) 0.0136(3) Uani 1 1 d . . . . .
C007 C -0.01217(8) 0.19234(10) 0.39817(7) 0.0151(3) Uani 1 1 d . . . . .
C008 C 0.50406(8) 0.28322(9) 0.87446(6) 0.0122(3) Uani 1 1 d . . . . .
C009 C 0.64632(8) 0.21133(9) 0.79902(7) 0.0139(3) Uani 1 1 d . . . . .
H009 H 0.657989 0.268172 0.785648 0.017 Uiso 1 1 calc R . . . .
C00A C 0.47902(8) 0.19931(9) 0.88756(7) 0.0138(3) Uani 1 1 d . . . . .
C00B C 0.40117(9) 0.18140(10) 0.87164(7) 0.0169(3) Uani 1 1 d . . . . .
H00B H 0.386154 0.123456 0.879575 0.020 Uiso 1 1 calc R . . . .
C00C C 0.61510(8) 0.20625(9) 0.84996(7) 0.0121(3) Uani 1 1 d . . . . .
C00D C 0.14213(8) 0.28152(9) 0.47704(7) 0.0148(3) Uani 1 1 d . . . . .
C00E C 0.62122(9) 0.18758(10) 0.99982(7) 0.0171(3) Uani 1 1 d . . . . .
C00F C 0.70340(9) 0.40770(9) 0.89325(8) 0.0175(3) Uani 1 1 d . . . . .
H00F H 0.738427 0.379303 0.936172 0.021 Uiso 1 1 calc R . . . .
C00G C 0.66084(8) 0.13545(10) 0.76727(7) 0.0166(3) Uani 1 1 d . . . . .
H00G H 0.682223 0.141284 0.732949 0.020 Uiso 1 1 calc R . . . .
C00H C 0.00580(8) 0.27569(9) 0.37691(7) 0.0139(3) Uani 1 1 d . . . . .
C00I C -0.05620(8) 0.33683(10) 0.34897(7) 0.0158(3) Uani 1 1 d . . . . .
H00I H -0.046052 0.395473 0.337691 0.019 Uiso 1 1 calc R . . . .
C00J C 0.11835(8) 0.20120(9) 0.35396(7) 0.0132(3) Uani 1 1 d . . . . .
C00K C 0.44677(8) 0.35008(9) 0.84993(7) 0.0137(3) Uani 1 1 d . . . . .
H00K H 0.461510 0.408736 0.843395 0.016 Uiso 1 1 calc R . . . .
C00L C 0.34545(9) 0.24802(10) 0.84420(7) 0.0189(3) Uani 1 1 d . . . . .
H00L H 0.292052 0.235705 0.831979 0.023 Uiso 1 1 calc R . . . .
C00M C 0.16053(9) 0.12280(10) 0.27158(7) 0.0181(3) Uani 1 1 d . . . . .
H00M H 0.178181 0.125411 0.234464 0.022 Uiso 1 1 calc R . . . .
C00N C 0.13209(8) 0.20090(9) 0.50755(7) 0.0158(3) Uani 1 1 d . . . . .
C00O C 0.63892(8) 0.27075(10) 0.97790(7) 0.0149(3) Uani 1 1 d . . . . .
C00P C 0.64415(9) 0.05102(10) 0.78561(7) 0.0191(3) Uani 1 1 d . . . . .
H00P H 0.654332 -0.000783 0.764302 0.023 Uiso 1 1 calc R . . . .
C00Q C -0.08836(9) 0.16874(10) 0.38539(7) 0.0187(3) Uani 1 1 d . . . . .
H00Q H -0.098861 0.111215 0.398539 0.022 Uiso 1 1 calc R . . . .
C00R C 0.11865(9) 0.37721(9) 0.35359(7) 0.0158(3) Uani 1 1 d . . . . .
C00S C 0.15081(9) 0.04058(10) 0.29810(7) 0.0196(3) Uani 1 1 d . . . . .
H00S H 0.161897 -0.012982 0.279497 0.024 Uiso 1 1 calc R . . . .
C00T C 0.36887(8) 0.33284(10) 0.83488(7) 0.0173(3) Uani 1 1 d . . . . .
H00T H 0.331585 0.379533 0.818121 0.021 Uiso 1 1 calc R . . . .
C00U C 0.12465(9) 0.03797(10) 0.35220(7) 0.0178(3) Uani 1 1 d . . . . .
H00U H 0.117715 -0.017695 0.370797 0.021 Uiso 1 1 calc R . . . .
C00V C 0.10855(8) 0.11697(9) 0.37926(7) 0.0148(3) Uani 1 1 d . . . . .
C00W C 0.59794(8) 0.12055(9) 0.86671(7) 0.0147(3) Uani 1 1 d . . . . .
C00X C -0.13209(9) 0.31396(11) 0.33734(7) 0.0201(3) Uani 1 1 d . . . . .
H00X H -0.172558 0.356919 0.318183 0.024 Uiso 1 1 calc R . . . .
C00Y C -0.14904(9) 0.22945(11) 0.35338(7) 0.0211(3) Uani 1 1 d . . . . .
H00Y H -0.201282 0.212954 0.342745 0.025 Uiso 1 1 calc R . . . .
C00Z C 0.57688(9) 0.42603(10) 0.79901(7) 0.0186(3) Uani 1 1 d . . . . .
H00Z H 0.523262 0.410407 0.775763 0.022 Uiso 1 1 calc R . . . .
C010 C 0.18275(9) 0.34937(10) 0.52525(8) 0.0199(3) Uani 1 1 d . . . . .
H010 H 0.189828 0.405002 0.506696 0.024 Uiso 1 1 calc R . . . .
C011 C 0.19684(9) 0.40469(10) 0.37810(8) 0.0183(3) Uani 1 1 d . . . . .
H011 H 0.234537 0.377892 0.420494 0.022 Uiso 1 1 calc R . . . .
C012 C 0.68414(9) 0.32933(11) 1.03292(7) 0.0212(3) Uani 1 1 d . . . . .
H012 H 0.696628 0.386342 1.020564 0.025 Uiso 1 1 calc R . . . .
C013 C 0.16250(9) 0.18884(11) 0.58200(7) 0.0216(3) Uani 1 1 d . . . . .
H013 H 0.154979 0.133795 0.601090 0.026 Uiso 1 1 calc R . . . .
C014 C -0.10731(9) 0.27378(10) 0.04649(7) 0.0194(3) Uani 1 1 d . . . . .
H01D H -0.129120 0.269769 -0.006679 0.023 Uiso 1 1 calc R . . . .
H01F H -0.150141 0.292083 0.059402 0.023 Uiso 1 1 calc R . . . .
C015 C 0.61238(9) 0.04396(10) 0.83556(7) 0.0181(3) Uani 1 1 d . . . . .
H015 H 0.600478 -0.013003 0.848511 0.022 Uiso 1 1 calc R . . . .
C016 C 0.73245(9) 0.47364(10) 0.86337(8) 0.0220(3) Uani 1 1 d . . . . .
H016 H 0.786151 0.489103 0.885848 0.026 Uiso 1 1 calc R . . . .
C017 C 0.20396(9) 0.25733(12) 0.62858(8) 0.0261(4) Uani 1 1 d . . . . .
H017 H 0.225505 0.248871 0.679264 0.031 Uiso 1 1 calc R . . . .
C018 C 0.31669(9) 0.09130(11) 0.47913(7) 0.0236(3) Uani 1 1 d . . . . .
H01 H 0.294414 0.143799 0.449011 0.035 Uiso 1 1 calc GR . . . .
H H 0.274906 0.049106 0.473397 0.035 Uiso 1 1 calc GR . . . .
HA H 0.354346 0.062795 0.464395 0.035 Uiso 1 1 calc GR . . . .
C019 C 0.68293(10) 0.51700(10) 0.80058(8) 0.0241(3) Uani 1 1 d . . . . .
H019 H 0.702222 0.562532 0.780175 0.029 Uiso 1 1 calc R . . . .
C01A C 0.64820(9) 0.16458(11) 1.07240(8) 0.0246(4) Uani 1 1 d . . . . .
H01A H 0.635188 0.108266 1.085483 0.030 Uiso 1 1 calc R . . . .
C01B C 0.21320(9) 0.33755(11) 0.59996(8) 0.0260(4) Uani 1 1 d . . . . .
H01B H 0.240378 0.384953 0.631163 0.031 Uiso 1 1 calc R . . . .
C01C C 0.22178(9) 0.46878(10) 0.34370(8) 0.0231(3) Uani 1 1 d . . . . .
H01C H 0.275363 0.484657 0.362526 0.028 Uiso 1 1 calc R . . . .
C01D C -0.19065(9) 0.10177(11) -0.02544(7) 0.0224(3) Uani 1 1 d . . . . .
H01H H -0.208216 0.158077 -0.051492 0.034 Uiso 1 1 calc GR . . . .
H01I H -0.235753 0.063070 -0.035269 0.034 Uiso 1 1 calc GR . . . .
H01K H -0.154356 0.072278 -0.041373 0.034 Uiso 1 1 calc GR . . . .
C01E C 0.09052(10) 0.48527(11) 0.25501(8) 0.0245(3) Uani 1 1 d . . . . .
H01E H 0.053202 0.512834 0.212808 0.029 Uiso 1 1 calc R . . . .
C01F C -0.04065(9) 0.18481(11) 0.15970(7) 0.0206(3) Uani 1 1 d . . . . .
H01N H -0.027220 0.123307 0.178218 0.025 Uiso 1 1 calc R . . . .
H01O H 0.008738 0.218542 0.174885 0.025 Uiso 1 1 calc R . . . .
C01G C 0.06684(9) 0.41988(10) 0.29028(7) 0.0194(3) Uani 1 1 d . . . . .
H01G H 0.013337 0.403507 0.270590 0.023 Uiso 1 1 calc R . . . .
C01H C -0.02011(9) 0.14937(10) 0.05101(8) 0.0195(3) Uani 1 1 d . . . . .
H01P H 0.023454 0.192586 0.066256 0.023 Uiso 1 1 calc R . . . .
H01Q H -0.044984 0.148475 -0.002298 0.023 Uiso 1 1 calc R . . . .
C01I C -0.14977(9) 0.12020(10) 0.05483(7) 0.0187(3) Uani 1 1 d . . . . .
H01S H -0.132776 0.062716 0.080357 0.022 Uiso 1 1 calc R . . . .
H01T H -0.187957 0.146902 0.070563 0.022 Uiso 1 1 calc R . . . .
C01J C 0.16819(10) 0.50993(10) 0.28146(9) 0.0254(4) Uani 1 1 d . . . . .
H01J H 0.184705 0.554092 0.257639 0.030 Uiso 1 1 calc R . . . .
C01K C 0.41344(10) 0.23817(11) 0.69081(7) 0.0256(4) Uani 1 1 d . . . . .
H0AA H 0.368861 0.198719 0.681308 0.038 Uiso 1 1 calc GR . . . .
HB H 0.394556 0.297667 0.671756 0.038 Uiso 1 1 calc GR . . . .
HC H 0.445171 0.241987 0.742860 0.038 Uiso 1 1 calc GR . . . .
C01L C 0.60515(10) 0.49260(10) 0.76843(8) 0.0232(3) Uani 1 1 d . . . . .
H01L H 0.570753 0.521212 0.725358 0.028 Uiso 1 1 calc R . . . .
C01M C 0.71140(10) 0.30590(13) 1.10569(8) 0.0294(4) Uani 1 1 d . . . . .
H01M H 0.742158 0.347032 1.141718 0.035 Uiso 1 1 calc R . . . .
C01N C -0.08928(10) 0.22681(11) 0.19442(7) 0.0259(4) Uani 1 1 d . . . . .
H01U H -0.138333 0.193913 0.180082 0.039 Uiso 1 1 calc GR . . . .
H01V H -0.100562 0.288901 0.178713 0.039 Uiso 1 1 calc GR . . . .
H01W H -0.060409 0.224782 0.246933 0.039 Uiso 1 1 calc GR . . . .
C01O C -0.04549(10) 0.34550(11) 0.07115(9) 0.0280(4) Uani 1 1 d . . . . .
H01X H -0.068171 0.401775 0.047277 0.042 Uiso 1 1 calc GR . . . .
H01Y H -0.002606 0.328349 0.058724 0.042 Uiso 1 1 calc GR . . . .
HD H -0.025596 0.352886 0.123438 0.042 Uiso 1 1 calc GR . . . .
C01P C 0.38043(10) 0.27665(10) 0.53785(8) 0.0236(3) Uani 1 1 d . . . . .
H1AA H 0.355699 0.267556 0.485044 0.028 Uiso 1 1 calc R . . . .
HE H 0.338320 0.289633 0.553216 0.028 Uiso 1 1 calc R . . . .
C01Q C 0.47867(9) 0.16509(10) 0.54397(8) 0.0219(3) Uani 1 1 d . . . . .
H2AA H 0.518017 0.213149 0.556045 0.026 Uiso 1 1 calc R . . . .
HF H 0.451265 0.161847 0.490814 0.026 Uiso 1 1 calc R . . . .
C01R C 0.69415(10) 0.22387(13) 1.12575(8) 0.0318(4) Uani 1 1 d . . . . .
H01R H 0.713309 0.208066 1.175180 0.038 Uiso 1 1 calc R . . . .
C01S C 0.46257(9) 0.20123(11) 0.65443(7) 0.0236(3) Uani 1 1 d . . . . .
H3AA H 0.507599 0.241405 0.664972 0.028 Uiso 1 1 calc R . . . .
HG H 0.483405 0.142554 0.676006 0.028 Uiso 1 1 calc R . . . .
C01T C 0.52060(10) 0.07773(11) 0.57164(8) 0.0269(4) Uani 1 1 d . . . . .
H4AA H 0.556586 0.066355 0.549338 0.040 Uiso 1 1 calc GR . . . .
HH H 0.482369 0.029340 0.559432 0.040 Uiso 1 1 calc GR . . . .
HI H 0.549978 0.080949 0.624051 0.040 Uiso 1 1 calc GR . . . .
C01U C 0.43275(11) 0.35656(11) 0.55398(9) 0.0312(4) Uani 1 1 d . . . . .
H5AA H 0.401636 0.409275 0.531047 0.047 Uiso 1 1 calc GR . . . .
HJ H 0.472102 0.346892 0.535247 0.047 Uiso 1 1 calc GR . . . .
HK H 0.458678 0.365715 0.606195 0.047 Uiso 1 1 calc GR . . . .
C01V C 0.01291(10) 0.05739(11) 0.07807(8) 0.0266(4) Uani 1 1 d . . . . .
H01Z H 0.049656 0.040689 0.057749 0.040 Uiso 1 1 calc GR . . . .
HL H -0.029713 0.013956 0.063147 0.040 Uiso 1 1 calc GR . . . .
HM H 0.040053 0.058265 0.130744 0.040 Uiso 1 1 calc GR . . . .
C01W C 0.35761(9) 0.11949(10) 0.55754(8) 0.0211(3) Uani 1 1 d . . . . .
H6AA H 0.317912 0.142257 0.573046 0.025 Uiso 1 1 calc R . . . .
HN H 0.381677 0.066173 0.586962 0.025 Uiso 1 1 calc R . . . .
B01X B 0.59687(9) 0.29232(10) 0.89078(8) 0.0124(3) Uani 1 1 d . . . . .
B01Y B 0.09673(9) 0.29063(10) 0.38878(8) 0.0135(3) Uani 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
P001 C007 1.8444(15) . ?
P001 C00N 1.8393(15) . ?
P001 C00V 1.8324(15) . ?
P002 C00A 1.8431(14) . ?
P002 C00E 1.8392(16) . ?
P002 C00W 1.8345(15) . ?
N003 C014 1.5258(18) . ?
N003 C01F 1.5224(16) . ?
N003 C01H 1.5182(18) . ?
N003 C01I 1.5182(18) . ?
N004 C01P 1.5255(18) . ?
N004 C01Q 1.5126(18) . ?
N004 C01S 1.5162(16) . ?
N004 C01W 1.5166(18) . ?
C005 H005 0.9500 . ?
C005 C00J 1.4043(18) . ?
C005 C00M 1.393(2) . ?
C006 C00F 1.405(2) . ?
C006 C00Z 1.4136(19) . ?
C006 B01X 1.621(2) . ?
C007 C00H 1.4124(19) . ?
C007 C00Q 1.396(2) . ?
C008 C00A 1.4106(19) . ?
C008 C00K 1.4053(19) . ?
C008 B01X 1.647(2) . ?
C009 H009 0.9500 . ?
C009 C00C 1.3991(18) . ?
C009 C00G 1.3947(19) . ?
C00A C00B 1.392(2) . ?
C00B H00B 0.9500 . ?
C00B C00L 1.388(2) . ?
C00C C00W 1.4043(19) . ?
C00C B01X 1.652(2) . ?
C00D C00N 1.4109(19) . ?
C00D C010 1.4012(19) . ?
C00D B01Y 1.6474(19) . ?
C00E C00O 1.414(2) . ?
C00E C01A 1.3959(19) . ?
C00F H00F 0.9500 . ?
C00F C016 1.392(2) . ?
C00G H00G 0.9500 . ?
C00G C00P 1.395(2) . ?
C00H C00I 1.4068(19) . ?
C00H B01Y 1.646(2) . ?
C00I H00I 0.9500 . ?
C00I C00X 1.394(2) . ?
C00J C00V 1.4079(19) . ?
C00J B01Y 1.650(2) . ?
C00K H00K 0.9500 . ?
C00K C00T 1.395(2) . ?
C00L H00L 0.9500 . ?
C00L C00T 1.388(2) . ?
C00M H00M 0.9500 . ?
C00M C00S 1.391(2) . ?
C00N C013 1.3957(18) . ?
C00O C012 1.4010(19) . ?
C00O B01X 1.6503(19) . ?
C00P H00P 0.9500 . ?
C00P C015 1.390(2) . ?
C00Q H00Q 0.9500 . ?
C00Q C00Y 1.394(2) . ?
C00R C011 1.408(2) . ?
C00R C01G 1.4076(19) . ?
C00R B01Y 1.622(2) . ?
C00S H00S 0.9500 . ?
C00S C00U 1.389(2) . ?
C00T H00T 0.9500 . ?
C00U H00U 0.9500 . ?
C00U C00V 1.3957(19) . ?
C00W C015 1.3961(19) . ?
C00X H00X 0.9500 . ?
C00X C00Y 1.382(2) . ?
C00Y H00Y 0.9500 . ?
C00Z H00Z 0.9500 . ?
C00Z C01L 1.399(2) . ?
C010 H010 0.9500 . ?
C010 C01B 1.400(2) . ?
C011 H011 0.9500 . ?
C011 C01C 1.386(2) . ?
C012 H012 0.9500 . ?
C012 C01M 1.401(2) . ?
C013 H013 0.9500 . ?
C013 C017 1.397(2) . ?
C014 H01D 0.9900 . ?
C014 H01F 0.9900 . ?
C014 C01O 1.511(2) . ?
C015 H015 0.9500 . ?
C016 H016 0.9500 . ?
C016 C019 1.393(2) . ?
C017 H017 0.9500 . ?
C017 C01B 1.382(2) . ?
C018 H01 0.9800 . ?
C018 H 0.9800 . ?
C018 HA 0.9800 . ?
C018 C01W 1.5195(18) . ?
C019 H019 0.9500 . ?
C019 C01L 1.383(2) . ?
C01A H01A 0.9500 . ?
C01A C01R 1.393(2) . ?
C01B H01B 0.9500 . ?
C01C H01C 0.9500 . ?
C01C C01J 1.395(2) . ?
C01D H01H 0.9800 . ?
C01D H01I 0.9800 . ?
C01D H01K 0.9800 . ?
C01D C01I 1.5180(18) . ?
C01E H01E 0.9500 . ?
C01E C01G 1.398(2) . ?
C01E C01J 1.384(2) . ?
C01F H01N 0.9900 . ?
C01F H01O 0.9900 . ?
C01F C01N 1.515(2) . ?
C01G H01G 0.9500 . ?
C01H H01P 0.9900 . ?
C01H H01Q 0.9900 . ?
C01H C01V 1.521(2) . ?
C01I H01S 0.9900 . ?
C01I H01T 0.9900 . ?
C01J H01J 0.9500 . ?
C01K H0AA 0.9800 . ?
C01K HB 0.9800 . ?
C01K HC 0.9800 . ?
C01K C01S 1.518(2) . ?
C01L H01L 0.9500 . ?
C01M H01M 0.9500 . ?
C01M C01R 1.380(3) . ?
C01N H01U 0.9800 . ?
C01N H01V 0.9800 . ?
C01N H01W 0.9800 . ?
C01O H01X 0.9800 . ?
C01O H01Y 0.9800 . ?
C01O HD 0.9800 . ?
C01P H1AA 0.9900 . ?
C01P HE 0.9900 . ?
C01P C01U 1.500(2) . ?
C01Q H2AA 0.9900 . ?
C01Q HF 0.9900 . ?
C01Q C01T 1.514(2) . ?
C01R H01R 0.9500 . ?
C01S H3AA 0.9900 . ?
C01S HG 0.9900 . ?
C01T H4AA 0.9800 . ?
C01T HH 0.9800 . ?
C01T HI 0.9800 . ?
C01U H5AA 0.9800 . ?
C01U HJ 0.9800 . ?
C01U HK 0.9800 . ?
C01V H01Z 0.9800 . ?
C01V HL 0.9800 . ?
C01V HM 0.9800 . ?
C01W H6AA 0.9900 . ?
C01W HN 0.9900 . ?

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
C00N P001 C007 94.59(6) . . ?
C00V P001 C007 95.22(6) . . ?
C00V P001 C00N 98.14(7) . . ?
C00E P002 C00A 94.73(6) . . ?
C00W P002 C00A 95.71(6) . . ?
C00W P002 C00E 97.41(7) . . ?
C01F N003 C014 110.67(11) . . ?
C01H N003 C014 108.26(11) . . ?
C01H N003 C01F 108.71(11) . . ?
C01I N003 C014 108.54(11) . . ?
C01I N003 C01F 108.37(11) . . ?
C01I N003 C01H 112.31(11) . . ?
C01Q N004 C01P 108.40(11) . . ?
C01Q N004 C01S 108.91(11) . . ?
C01Q N004 C01W 112.05(11) . . ?
C01S N004 C01P 110.82(11) . . ?
C01S N004 C01W 108.59(11) . . ?
C01W N004 C01P 108.08(11) . . ?
C00J C005 H005 119.0 . . ?
C00M C005 H005 119.0 . . ?
C00M C005 C00J 122.05(13) . . ?
C00F C006 C00Z 114.76(13) . . ?
C00F C006 B01X 121.34(12) . . ?
C00Z C006 B01X 122.72(13) . . ?
C00H C007 P001 118.18(11) . . ?
C00Q C007 P001 119.80(11) . . ?
C00Q C007 C00H 121.98(13) . . ?
C00A C008 B01X 116.69(12) . . ?
C00K C008 C00A 115.88(13) . . ?
C00K C008 B01X 127.43(12) . . ?
C00C C009 H009 119.0 . . ?
C00G C009 H009 119.0 . . ?
C00G C009 C00C 121.97(13) . . ?
C008 C00A P002 118.15(11) . . ?
C00B C00A P002 119.54(11) . . ?
C00B C00A C008 122.26(13) . . ?
C00A C00B H00B 119.9 . . ?
C00L C00B C00A 120.16(14) . . ?
C00L C00B H00B 119.9 . . ?
C009 C00C C00W 116.40(12) . . ?
C009 C00C B01X 125.23(12) . . ?
C00W C00C B01X 118.37(12) . . ?
C00N C00D B01Y 116.83(12) . . ?
C010 C00D C00N 116.61(12) . . ?
C010 C00D B01Y 126.17(13) . . ?
C00O C00E P002 118.48(10) . . ?
C01A C00E P002 119.48(12) . . ?
C01A C00E C00O 121.79(14) . . ?
C006 C00F H00F 118.4 . . ?
C016 C00F C006 123.25(14) . . ?
C016 C00F H00F 118.4 . . ?
C009 C00G H00G 119.8 . . ?
C009 C00G C00P 120.41(13) . . ?
C00P C00G H00G 119.8 . . ?
C007 C00H B01Y 116.51(12) . . ?
C00I C00H C007 115.88(13) . . ?
C00I C00H B01Y 127.60(13) . . ?
C00H C00I H00I 119.0 . . ?
C00X C00I C00H 121.98(14) . . ?
C00X C00I H00I 119.0 . . ?
C005 C00J C00V 116.12(13) . . ?
C005 C00J B01Y 125.33(12) . . ?
C00V C00J B01Y 118.53(12) . . ?
C008 C00K H00K 119.0 . . ?
C00T C00K C008 121.94(13) . . ?
C00T C00K H00K 119.0 . . ?
C00B C00L H00L 120.5 . . ?
C00T C00L C00B 119.05(14) . . ?
C00T C00L H00L 120.5 . . ?
C005 C00M H00M 119.8 . . ?
C00S C00M C005 120.46(13) . . ?
C00S C00M H00M 119.8 . . ?
C00D C00N P001 118.26(10) . . ?
C013 C00N P001 119.84(12) . . ?
C013 C00N C00D 121.61(13) . . ?
C00E C00O B01X 116.45(12) . . ?
C012 C00O C00E 116.44(12) . . ?
C012 C00O B01X 126.80(13) . . ?
C00G C00P H00P 120.6 . . ?
C015 C00P C00G 118.90(13) . . ?
C015 C00P H00P 120.6 . . ?
C007 C00Q H00Q 120.0 . . ?
C00Y C00Q C007 120.10(14) . . ?
C00Y C00Q H00Q 120.0 . . ?
C011 C00R B01Y 120.15(13) . . ?
C01G C00R C011 114.48(13) . . ?
C01G C00R B01Y 124.40(13) . . ?
C00M C00S H00S 120.5 . . ?
C00U C00S C00M 119.01(13) . . ?
C00U C00S H00S 120.5 . . ?
C00K C00T H00T 119.7 . . ?
C00L C00T C00K 120.51(13) . . ?
C00L C00T H00T 119.7 . . ?
C00S C00U H00U 119.9 . . ?
C00S C00U C00V 120.13(14) . . ?
C00V C00U H00U 119.9 . . ?
C00J C00V P001 116.82(10) . . ?
C00U C00V P001 120.88(11) . . ?
C00U C00V C00J 122.23(13) . . ?
C00C C00W P002 117.05(10) . . ?
C015 C00W P002 120.66(11) . . ?
C015 C00W C00C 122.28(13) . . ?
C00I C00X H00X 119.7 . . ?
C00Y C00X C00I 120.67(14) . . ?
C00Y C00X H00X 119.7 . . ?
C00Q C00Y H00Y 120.5 . . ?
C00X C00Y C00Q 119.04(14) . . ?
C00X C00Y H00Y 120.5 . . ?
C006 C00Z H00Z 118.7 . . ?
C01L C00Z C006 122.66(14) . . ?
C01L C00Z H00Z 118.7 . . ?
C00D C010 H010 119.0 . . ?
C01B C010 C00D 121.92(15) . . ?
C01B C010 H010 119.0 . . ?
C00R C011 H011 118.2 . . ?
C01C C011 C00R 123.52(14) . . ?
C01C C011 H011 118.2 . . ?
C00O C012 H012 119.2 . . ?
C01M C012 C00O 121.62(16) . . ?
C01M C012 H012 119.2 . . ?
C00N C013 H013 119.8 . . ?
C00N C013 C017 120.31(15) . . ?
C017 C013 H013 119.8 . . ?
N003 C014 H01D 108.5 . . ?
N003 C014 H01F 108.5 . . ?
H01D C014 H01F 107.5 . . ?
C01O C014 N003 115.22(13) . . ?
C01O C014 H01D 108.5 . . ?
C01O C014 H01F 108.5 . . ?
C00P C015 C00W 120.04(14) . . ?
C00P C015 H015 120.0 . . ?
C00W C015 H015 120.0 . . ?
C00F C016 H016 119.9 . . ?
C00F C016 C019 120.11(14) . . ?
C019 C016 H016 119.9 . . ?
C013 C017 H017 120.4 . . ?
C01B C017 C013 119.13(13) . . ?
C01B C017 H017 120.4 . . ?
H01 C018 H 109.5 . . ?
H01 C018 HA 109.5 . . ?
H C018 HA 109.5 . . ?
C01W C018 H01 109.5 . . ?
C01W C018 H 109.5 . . ?
C01W C018 HA 109.5 . . ?
C016 C019 H019 120.6 . . ?
C01L C019 C016 118.85(14) . . ?
C01L C019 H019 120.6 . . ?
C00E C01A H01A 119.9 . . ?
C01R C01A C00E 120.29(16) . . ?
C01R C01A H01A 119.9 . . ?
C010 C01B H01B 119.8 . . ?
C017 C01B C010 120.40(14) . . ?
C017 C01B H01B 119.8 . . ?
C011 C01C H01C 120.0 . . ?
C011 C01C C01J 120.00(15) . . ?
C01J C01C H01C 120.0 . . ?
H01H C01D H01I 109.5 . . ?
H01H C01D H01K 109.5 . . ?
H01I C01D H01K 109.5 . . ?
C01I C01D H01H 109.5 . . ?
C01I C01D H01I 109.5 . . ?
C01I C01D H01K 109.5 . . ?
C01G C01E H01E 119.9 . . ?
C01J C01E H01E 119.9 . . ?
C01J C01E C01G 120.16(14) . . ?
N003 C01F H01N 108.5 . . ?
N003 C01F H01O 108.5 . . ?
H01N C01F H01O 107.5 . . ?
C01N C01F N003 115.09(12) . . ?
C01N C01F H01N 108.5 . . ?
C01N C01F H01O 108.5 . . ?
C00R C01G H01G 118.5 . . ?
C01E C01G C00R 123.02(14) . . ?
C01E C01G H01G 118.5 . . ?
N003 C01H H01P 108.7 . . ?
N003 C01H H01Q 108.7 . . ?
N003 C01H C01V 114.11(12) . . ?
H01P C01H H01Q 107.6 . . ?
C01V C01H H01P 108.7 . . ?
C01V C01H H01Q 108.7 . . ?
N003 C01I H01S 108.5 . . ?
N003 C01I H01T 108.5 . . ?
C01D C01I N003 115.23(12) . . ?
C01D C01I H01S 108.5 . . ?
C01D C01I H01T 108.5 . . ?
H01S C01I H01T 107.5 . . ?
C01C C01J H01J 120.6 . . ?
C01E C01J C01C 118.82(14) . . ?
C01E C01J H01J 120.6 . . ?
H0AA C01K HB 109.5 . . ?
H0AA C01K HC 109.5 . . ?
HB C01K HC 109.5 . . ?
C01S C01K H0AA 109.5 . . ?
C01S C01K HB 109.5 . . ?
C01S C01K HC 109.5 . . ?
C00Z C01L H01L 119.8 . . ?
C019 C01L C00Z 120.37(14) . . ?
C019 C01L H01L 119.8 . . ?
C012 C01M H01M 119.6 . . ?
C01R C01M C012 120.87(15) . . ?
C01R C01M H01M 119.6 . . ?
C01F C01N H01U 109.5 . . ?
C01F C01N H01V 109.5 . . ?
C01F C01N H01W 109.5 . . ?
H01U C01N H01V 109.5 . . ?
H01U C01N H01W 109.5 . . ?
H01V C01N H01W 109.5 . . ?
C014 C01O H01X 109.5 . . ?
C014 C01O H01Y 109.5 . . ?
C014 C01O HD 109.5 . . ?
H01X C01O H01Y 109.5 . . ?
H01X C01O HD 109.5 . . ?
H01Y C01O HD 109.5 . . ?
N004 C01P H1AA 108.4 . . ?
N004 C01P HE 108.4 . . ?
H1AA C01P HE 107.5 . . ?
C01U C01P N004 115.50(14) . . ?
C01U C01P H1AA 108.4 . . ?
C01U C01P HE 108.4 . . ?
N004 C01Q H2AA 108.6 . . ?
N004 C01Q HF 108.6 . . ?
N004 C01Q C01T 114.87(12) . . ?
H2AA C01Q HF 107.5 . . ?
C01T C01Q H2AA 108.6 . . ?
C01T C01Q HF 108.6 . . ?
C01A C01R H01R 120.5 . . ?
C01M C01R C01A 118.98(14) . . ?
C01M C01R H01R 120.5 . . ?
N004 C01S C01K 115.15(13) . . ?
N004 C01S H3AA 108.5 . . ?
N004 C01S HG 108.5 . . ?
C01K C01S H3AA 108.5 . . ?
C01K C01S HG 108.5 . . ?
H3AA C01S HG 107.5 . . ?
C01Q C01T H4AA 109.5 . . ?
C01Q C01T HH 109.5 . . ?
C01Q C01T HI 109.5 . . ?
H4AA C01T HH 109.5 . . ?
H4AA C01T HI 109.5 . . ?
HH C01T HI 109.5 . . ?
C01P C01U H5AA 109.5 . . ?
C01P C01U HJ 109.5 . . ?
C01P C01U HK 109.5 . . ?
H5AA C01U HJ 109.5 . . ?
H5AA C01U HK 109.5 . . ?
HJ C01U HK 109.5 . . ?
C01H C01V H01Z 109.5 . . ?
C01H C01V HL 109.5 . . ?
C01H C01V HM 109.5 . . ?
H01Z C01V HL 109.5 . . ?
H01Z C01V HM 109.5 . . ?
HL C01V HM 109.5 . . ?
N004 C01W C018 115.24(12) . . ?
N004 C01W H6AA 108.5 . . ?
N004 C01W HN 108.5 . . ?
C018 C01W H6AA 108.5 . . ?
C018 C01W HN 108.5 . . ?
H6AA C01W HN 107.5 . . ?
C006 B01X C008 118.24(12) . . ?
C006 B01X C00C 107.37(11) . . ?
C006 B01X C00O 117.33(12) . . ?
C008 B01X C00C 105.24(11) . . ?
C008 B01X C00O 101.01(10) . . ?
C00O B01X C00C 106.53(11) . . ?
C00D B01Y C00J 107.25(11) . . ?
C00H B01Y C00D 100.42(11) . . ?
C00H B01Y C00J 104.94(11) . . ?
C00R B01Y C00D 116.15(12) . . ?
C00R B01Y C00H 119.28(12) . . ?
C00R B01Y C00J 107.75(11) . . ?

_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_p17612
_database_code_depnum_ccdc_archive 'CCDC 1824478'
_audit_update_record             
;
2018-02-16 deposited with the CCDC.
2018-06-22 downloaded from the CCDC.
;
_audit_creation_date             2017-12-14
_audit_creation_method           
;
Olex2 1.2
(compiled Aug 10 2017 17:28:52 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        '[Fe(PTB)Br3][NEt4]2'
_chemical_formula_moiety         'C24 H17 B Br3 Fe P, 2(C8 H20 N)'
_chemical_formula_sum            'C40 H57 B Br3 Fe N2 P'
_chemical_formula_weight         903.23
_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'
B B 0.0013 0.0007 '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'
Fe Fe 0.3463 0.8444 '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'
P P 0.1023 0.0942 '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                   13.5457(11)
_cell_length_b                   16.1351(13)
_cell_length_c                   18.6839(15)
_cell_angle_alpha                90
_cell_angle_beta                 95.303(4)
_cell_angle_gamma                90
_cell_volume                     4066.1(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9826
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.147
_cell_measurement_theta_min      2.525
_shelx_estimated_absorpt_T_max   0.461
_shelx_estimated_absorpt_T_min   0.317
_exptl_absorpt_coefficient_mu    3.388
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5246
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0817 before and 0.0588 after correction.
The Ratio of minimum to maximum transmission is 0.7034.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.27
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 0.999
_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       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            195212
_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         29.193
_diffrn_reflns_theta_min         2.319
_diffrn_ambient_temperature      100(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 AXS D8 Venture Kappa'
_diffrn_measurement_method       ?
_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                9461
_reflns_number_total             10966
_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 v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.945
_refine_diff_density_min         -1.063
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         10966
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0340
_refine_ls_restrained_S_all      1.044
_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)+(0.0384P)²+8.4466P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0885
_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 Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C35(H35A,H35B), C37(H37A,H37B), C39(H39A,H39B), C25(H25A,
 H25B), C27(H27A,H27B), C29(H29A,H29B), C31(H31A,H31B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23),
  C24(H24)
2.c Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C40(H40A,H40B,
 H40C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C32(H32A,
 H32B,H32C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
Br1 Br 1.07006(2) 0.68836(2) 0.49688(2) 0.03022(8) Uani 1 1 d . . . . .
Br2 Br 1.06697(2) 0.88799(2) 0.63591(2) 0.01602(6) Uani 1 1 d . . . . .
Br3 Br 1.09487(2) 0.66170(2) 0.71772(2) 0.02561(7) Uani 1 1 d . . . . .
Fe1 Fe 1.03416(2) 0.74059(2) 0.61250(2) 0.01559(7) Uani 1 1 d . . . . .
P1 P 0.85386(4) 0.74005(3) 0.60167(3) 0.01056(10) Uani 1 1 d . . . . .
C1 C 0.78873(16) 0.80577(13) 0.53408(11) 0.0108(4) Uani 1 1 d . . . . .
C2 C 0.68468(16) 0.80293(13) 0.53298(11) 0.0108(4) Uani 1 1 d . . . . .
C3 C 0.63180(17) 0.84794(14) 0.47786(12) 0.0147(4) Uani 1 1 d . . . . .
H3 H 0.561393 0.846488 0.473922 0.018 Uiso 1 1 calc R . . . .
C4 C 0.67950(19) 0.89482(15) 0.42860(13) 0.0183(5) Uani 1 1 d . . . . .
H4 H 0.641388 0.924283 0.391679 0.022 Uiso 1 1 calc R . . . .
C5 C 0.78238(19) 0.89870(15) 0.43317(13) 0.0179(5) Uani 1 1 d . . . . .
H5 H 0.814644 0.932192 0.400601 0.021 Uiso 1 1 calc R . . . .
C6 C 0.83777(17) 0.85306(14) 0.48591(12) 0.0145(4) Uani 1 1 d . . . . .
H6 H 0.908157 0.854132 0.489030 0.017 Uiso 1 1 calc R . . . .
C7 C 0.78219(16) 0.64533(13) 0.58223(11) 0.0111(4) Uani 1 1 d . . . . .
C8 C 0.67834(16) 0.65216(13) 0.58275(11) 0.0113(4) Uani 1 1 d . . . . .
C9 C 0.62569(18) 0.57751(14) 0.57414(12) 0.0150(4) Uani 1 1 d . . . . .
H9 H 0.555977 0.578071 0.576704 0.018 Uiso 1 1 calc R . . . .
C10 C 0.67238(19) 0.50229(14) 0.56191(13) 0.0181(5) Uani 1 1 d . . . . .
H10 H 0.634030 0.453050 0.556090 0.022 Uiso 1 1 calc R . . . .
C11 C 0.77439(19) 0.49866(14) 0.55815(12) 0.0178(5) Uani 1 1 d . . . . .
H11 H 0.805644 0.447849 0.547964 0.021 Uiso 1 1 calc R . . . .
C12 C 0.82982(17) 0.57097(14) 0.56960(12) 0.0141(4) Uani 1 1 d . . . . .
H12 H 0.899817 0.569557 0.568796 0.017 Uiso 1 1 calc R . . . .
C13 C 0.69018(16) 0.77354(13) 0.67294(12) 0.0115(4) Uani 1 1 d . . . . .
C14 C 0.79471(17) 0.77341(13) 0.68039(11) 0.0115(4) Uani 1 1 d . . . . .
C15 C 0.85083(18) 0.79306(14) 0.74454(12) 0.0141(4) Uani 1 1 d . . . . .
H15 H 0.921190 0.791949 0.747186 0.017 Uiso 1 1 calc R . . . .
C16 C 0.80262(19) 0.81436(14) 0.80477(12) 0.0172(4) Uani 1 1 d . . . . .
H16 H 0.839683 0.829197 0.848553 0.021 Uiso 1 1 calc R . . . .
C17 C 0.69956(19) 0.81355(14) 0.79981(12) 0.0171(4) Uani 1 1 d . . . . .
H17 H 0.666084 0.827269 0.840703 0.021 Uiso 1 1 calc R . . . .
C18 C 0.64507(18) 0.79289(14) 0.73564(12) 0.0145(4) Uani 1 1 d . . . . .
H18 H 0.574785 0.791807 0.734073 0.017 Uiso 1 1 calc R . . . .
C19 C 0.51551(16) 0.76131(14) 0.58514(12) 0.0135(4) Uani 1 1 d . . . . .
C20 C 0.47522(18) 0.83382(15) 0.61293(12) 0.0159(4) Uani 1 1 d . . . . .
H20 H 0.518647 0.871476 0.639191 0.019 Uiso 1 1 calc R . . . .
C21 C 0.37447(19) 0.85261(16) 0.60354(13) 0.0200(5) Uani 1 1 d . . . . .
H21 H 0.350640 0.902097 0.623463 0.024 Uiso 1 1 calc R . . . .
C22 C 0.30877(19) 0.79932(18) 0.56520(15) 0.0237(5) Uani 1 1 d . . . . .
H22 H 0.239636 0.810568 0.560408 0.028 Uiso 1 1 calc R . . . .
C23 C 0.34586(19) 0.72964(17) 0.53415(15) 0.0245(5) Uani 1 1 d . . . . .
H23 H 0.302272 0.693583 0.506213 0.029 Uiso 1 1 calc R . . . .
C24 C 0.44705(18) 0.71193(16) 0.54361(14) 0.0191(5) Uani 1 1 d . . . . .
H24 H 0.470638 0.664157 0.520827 0.023 Uiso 1 1 calc R . . . .
B1 B 0.63442(17) 0.74641(14) 0.59404(13) 0.0094(4) Uani 1 1 d . . . . .
N1 N 0.73204(15) 0.55245(12) 0.84647(10) 0.0147(4) Uani 1 1 d . . . . .
C33 C 0.7944(2) 0.59793(17) 0.79426(15) 0.0247(5) Uani 1 1 d . . . . .
H33A H 0.749906 0.632134 0.761229 0.030 Uiso 1 1 calc R . . . .
H33B H 0.840960 0.635816 0.822035 0.030 Uiso 1 1 calc R . . . .
C34 C 0.8531(2) 0.54025(18) 0.75017(14) 0.0266(6) Uani 1 1 d . . . . .
H34A H 0.807345 0.506786 0.718393 0.040 Uiso 1 1 calc GR . . . .
H34B H 0.894335 0.503691 0.782409 0.040 Uiso 1 1 calc GR . . . .
H34C H 0.895595 0.572986 0.721219 0.040 Uiso 1 1 calc GR . . . .
C35 C 0.8008(2) 0.49696(17) 0.89544(15) 0.0260(5) Uani 1 1 d . . . . .
H35A H 0.762335 0.473658 0.933279 0.031 Uiso 1 1 calc R . . . .
H35B H 0.822612 0.450034 0.866629 0.031 Uiso 1 1 calc R . . . .
C36 C 0.8918(2) 0.5399(2) 0.93130(16) 0.0329(7) Uani 1 1 d . . . . .
H36A H 0.937111 0.553529 0.895061 0.049 Uiso 1 1 calc GR . . . .
H36B H 0.925294 0.502990 0.967474 0.049 Uiso 1 1 calc GR . . . .
H36C H 0.871859 0.590881 0.954541 0.049 Uiso 1 1 calc GR . . . .
C37 C 0.6851(2) 0.61742(17) 0.88985(16) 0.0268(6) Uani 1 1 d . . . . .
H37A H 0.647707 0.656462 0.856665 0.032 Uiso 1 1 calc R . . . .
H37B H 0.738081 0.649201 0.917759 0.032 Uiso 1 1 calc R . . . .
C38 C 0.6145(2) 0.5815(2) 0.94198(16) 0.0358(7) Uani 1 1 d . . . . .
H38A H 0.563970 0.547384 0.915141 0.054 Uiso 1 1 calc GR . . . .
H38B H 0.582402 0.626930 0.965778 0.054 Uiso 1 1 calc GR . . . .
H38C H 0.652356 0.547322 0.978208 0.054 Uiso 1 1 calc GR . . . .
C39 C 0.6573(2) 0.49667(18) 0.80683(16) 0.0290(6) Uani 1 1 d . . . . .
H39A H 0.625538 0.462331 0.842154 0.035 Uiso 1 1 calc R . . . .
H39B H 0.692144 0.458810 0.775920 0.035 Uiso 1 1 calc R . . . .
C40 C 0.5756(2) 0.5434(2) 0.75953(16) 0.0353(7) Uani 1 1 d . . . . .
H40A H 0.606470 0.581920 0.727705 0.053 Uiso 1 1 calc GR . . . .
H40B H 0.533981 0.574419 0.790348 0.053 Uiso 1 1 calc GR . . . .
H40C H 0.534683 0.503450 0.730561 0.053 Uiso 1 1 calc GR . . . .
N2 N 0.77070(14) 0.60741(13) 0.33943(10) 0.0143(4) Uani 1 1 d . . . . .
C25 C 0.70391(18) 0.64555(17) 0.39150(13) 0.0189(5) Uani 1 1 d . . . . .
H25A H 0.704288 0.609176 0.434195 0.023 Uiso 1 1 calc R . . . .
H25B H 0.732316 0.699597 0.407844 0.023 Uiso 1 1 calc R . . . .
C26 C 0.59719(19) 0.65910(19) 0.36150(15) 0.0250(5) Uani 1 1 d . . . . .
H26A H 0.595443 0.696326 0.319953 0.038 Uiso 1 1 calc GR . . . .
H26B H 0.559900 0.683917 0.398586 0.038 Uiso 1 1 calc GR . . . .
H26C H 0.567286 0.605804 0.346567 0.038 Uiso 1 1 calc GR . . . .
C27 C 0.72718(18) 0.52716(15) 0.30734(13) 0.0179(4) Uani 1 1 d . . . . .
H27A H 0.666758 0.540773 0.275593 0.022 Uiso 1 1 calc R . . . .
H27B H 0.775560 0.502437 0.276940 0.022 Uiso 1 1 calc R . . . .
C28 C 0.7005(2) 0.46266(17) 0.36125(16) 0.0282(6) Uani 1 1 d . . . . .
H28A H 0.672042 0.413969 0.335651 0.042 Uiso 1 1 calc GR . . . .
H28B H 0.651910 0.485933 0.391425 0.042 Uiso 1 1 calc GR . . . .
H28C H 0.760255 0.446354 0.391554 0.042 Uiso 1 1 calc GR . . . .
C29 C 0.78283(19) 0.66488(15) 0.27645(13) 0.0182(5) Uani 1 1 d . . . . .
H29A H 0.820754 0.635246 0.241539 0.022 Uiso 1 1 calc R . . . .
H29B H 0.716283 0.676975 0.252225 0.022 Uiso 1 1 calc R . . . .
C30 C 0.8343(2) 0.74629(17) 0.29517(16) 0.0267(6) Uani 1 1 d . . . . .
H30A H 0.842237 0.777356 0.250989 0.040 Uiso 1 1 calc GR . . . .
H30B H 0.899674 0.735467 0.320478 0.040 Uiso 1 1 calc GR . . . .
H30C H 0.794409 0.778791 0.326161 0.040 Uiso 1 1 calc GR . . . .
C31 C 0.86967(18) 0.59191(17) 0.38239(13) 0.0203(5) Uani 1 1 d . . . . .
H31A H 0.890840 0.643722 0.407729 0.024 Uiso 1 1 calc R . . . .
H31B H 0.860039 0.549519 0.419415 0.024 Uiso 1 1 calc R . . . .
C32 C 0.95223(19) 0.56349(17) 0.33909(16) 0.0240(5) Uani 1 1 d . . . . .
H32A H 0.964086 0.605628 0.303088 0.036 Uiso 1 1 calc GR . . . .
H32B H 0.933318 0.511195 0.314905 0.036 Uiso 1 1 calc GR . . . .
H32C H 1.012836 0.555218 0.371184 0.036 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
Br1 Fe1 2.4098(5) . ?
Br2 Fe1 2.4515(4) . ?
Br3 Fe1 2.4211(5) . ?
Fe1 P1 2.4320(7) . ?
P1 C1 1.814(2) . ?
P1 C7 1.829(2) . ?
P1 C14 1.820(2) . ?
C1 C2 1.409(3) . ?
C1 C6 1.394(3) . ?
C2 C3 1.402(3) . ?
C2 B1 1.655(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.395(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.390(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.393(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.412(3) . ?
C7 C12 1.393(3) . ?
C8 C9 1.401(3) . ?
C8 B1 1.654(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.397(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.391(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.393(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.410(3) . ?
C13 C18 1.405(3) . ?
C13 B1 1.652(3) . ?
C14 C15 1.395(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.395(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.391(4) . ?
C17 H17 0.9500 . ?
C17 C18 1.389(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.410(3) . ?
C19 C24 1.402(3) . ?
C19 B1 1.622(3) . ?
C20 H20 0.9500 . ?
C20 C21 1.393(3) . ?
C21 H21 0.9500 . ?
C21 C22 1.388(4) . ?
C22 H22 0.9500 . ?
C22 C23 1.381(4) . ?
C23 H23 0.9500 . ?
C23 C24 1.395(3) . ?
C24 H24 0.9500 . ?
N1 C33 1.535(3) . ?
N1 C35 1.532(3) . ?
N1 C37 1.502(3) . ?
N1 C39 1.498(3) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.516(4) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.515(4) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.540(4) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.547(4) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
N2 C25 1.519(3) . ?
N2 C27 1.523(3) . ?
N2 C29 1.519(3) . ?
N2 C31 1.518(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.517(3) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.515(4) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.513(4) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.511(4) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 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
Br1 Fe1 Br2 116.800(18) . . ?
Br1 Fe1 Br3 117.549(18) . . ?
Br1 Fe1 P1 102.031(19) . . ?
Br3 Fe1 Br2 108.834(16) . . ?
Br3 Fe1 P1 109.20(2) . . ?
P1 Fe1 Br2 100.511(18) . . ?
C1 P1 Fe1 118.41(7) . . ?
C1 P1 C7 97.77(10) . . ?
C1 P1 C14 99.65(10) . . ?
C7 P1 Fe1 122.01(7) . . ?
C14 P1 Fe1 116.45(8) . . ?
C14 P1 C7 98.19(10) . . ?
C2 C1 P1 114.37(16) . . ?
C6 C1 P1 122.63(17) . . ?
C6 C1 C2 123.0(2) . . ?
C1 C2 B1 118.86(18) . . ?
C3 C2 C1 115.9(2) . . ?
C3 C2 B1 125.24(19) . . ?
C2 C3 H3 119.0 . . ?
C4 C3 C2 122.0(2) . . ?
C4 C3 H3 119.0 . . ?
C3 C4 H4 119.8 . . ?
C5 C4 C3 120.5(2) . . ?
C5 C4 H4 119.8 . . ?
C4 C5 H5 120.3 . . ?
C4 C5 C6 119.4(2) . . ?
C6 C5 H5 120.3 . . ?
C1 C6 H6 120.4 . . ?
C5 C6 C1 119.2(2) . . ?
C5 C6 H6 120.4 . . ?
C8 C7 P1 116.38(16) . . ?
C12 C7 P1 120.53(17) . . ?
C12 C7 C8 123.1(2) . . ?
C7 C8 B1 116.30(18) . . ?
C9 C8 C7 115.4(2) . . ?
C9 C8 B1 128.30(19) . . ?
C8 C9 H9 118.9 . . ?
C10 C9 C8 122.1(2) . . ?
C10 C9 H9 118.9 . . ?
C9 C10 H10 119.6 . . ?
C11 C10 C9 120.8(2) . . ?
C11 C10 H10 119.6 . . ?
C10 C11 H11 120.6 . . ?
C10 C11 C12 118.7(2) . . ?
C12 C11 H11 120.6 . . ?
C7 C12 C11 119.7(2) . . ?
C7 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C14 C13 B1 117.37(18) . . ?
C18 C13 C14 115.3(2) . . ?
C18 C13 B1 127.2(2) . . ?
C13 C14 P1 115.71(16) . . ?
C15 C14 P1 121.05(17) . . ?
C15 C14 C13 123.2(2) . . ?
C14 C15 H15 120.3 . . ?
C16 C15 C14 119.4(2) . . ?
C16 C15 H15 120.3 . . ?
C15 C16 H16 120.5 . . ?
C17 C16 C15 119.1(2) . . ?
C17 C16 H16 120.5 . . ?
C16 C17 H17 119.7 . . ?
C18 C17 C16 120.7(2) . . ?
C18 C17 H17 119.7 . . ?
C13 C18 H18 118.8 . . ?
C17 C18 C13 122.4(2) . . ?
C17 C18 H18 118.8 . . ?
C20 C19 B1 120.0(2) . . ?
C24 C19 C20 114.6(2) . . ?
C24 C19 B1 124.9(2) . . ?
C19 C20 H20 118.6 . . ?
C21 C20 C19 122.8(2) . . ?
C21 C20 H20 118.6 . . ?
C20 C21 H21 119.9 . . ?
C22 C21 C20 120.3(2) . . ?
C22 C21 H21 119.9 . . ?
C21 C22 H22 120.6 . . ?
C23 C22 C21 118.7(2) . . ?
C23 C22 H22 120.6 . . ?
C22 C23 H23 119.8 . . ?
C22 C23 C24 120.3(2) . . ?
C24 C23 H23 119.8 . . ?
C19 C24 H24 118.5 . . ?
C23 C24 C19 123.1(2) . . ?
C23 C24 H24 118.5 . . ?
C8 B1 C2 104.06(16) . . ?
C13 B1 C2 106.60(17) . . ?
C13 B1 C8 102.56(16) . . ?
C19 B1 C2 108.39(17) . . ?
C19 B1 C8 119.27(18) . . ?
C19 B1 C13 114.83(17) . . ?
C35 N1 C33 108.6(2) . . ?
C37 N1 C33 107.13(19) . . ?
C37 N1 C35 110.5(2) . . ?
C39 N1 C33 111.1(2) . . ?
C39 N1 C35 106.8(2) . . ?
C39 N1 C37 112.7(2) . . ?
N1 C33 H33A 108.9 . . ?
N1 C33 H33B 108.9 . . ?
H33A C33 H33B 107.7 . . ?
C34 C33 N1 113.5(2) . . ?
C34 C33 H33A 108.9 . . ?
C34 C33 H33B 108.9 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N1 C35 H35A 108.5 . . ?
N1 C35 H35B 108.5 . . ?
H35A C35 H35B 107.5 . . ?
C36 C35 N1 114.9(2) . . ?
C36 C35 H35A 108.5 . . ?
C36 C35 H35B 108.5 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N1 C37 H37A 108.9 . . ?
N1 C37 H37B 108.9 . . ?
N1 C37 C38 113.4(2) . . ?
H37A C37 H37B 107.7 . . ?
C38 C37 H37A 108.9 . . ?
C38 C37 H37B 108.9 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N1 C39 H39A 108.8 . . ?
N1 C39 H39B 108.8 . . ?
N1 C39 C40 113.9(2) . . ?
H39A C39 H39B 107.7 . . ?
C40 C39 H39A 108.8 . . ?
C40 C39 H39B 108.8 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C25 N2 C27 111.40(18) . . ?
C25 N2 C29 111.25(19) . . ?
C29 N2 C27 106.24(17) . . ?
C31 N2 C25 106.10(18) . . ?
C31 N2 C27 111.03(19) . . ?
C31 N2 C29 110.90(19) . . ?
N2 C25 H25A 108.5 . . ?
N2 C25 H25B 108.5 . . ?
H25A C25 H25B 107.5 . . ?
C26 C25 N2 115.2(2) . . ?
C26 C25 H25A 108.5 . . ?
C26 C25 H25B 108.5 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N2 C27 H27A 108.4 . . ?
N2 C27 H27B 108.4 . . ?
H27A C27 H27B 107.5 . . ?
C28 C27 N2 115.5(2) . . ?
C28 C27 H27A 108.4 . . ?
C28 C27 H27B 108.4 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N2 C29 H29A 108.4 . . ?
N2 C29 H29B 108.4 . . ?
H29A C29 H29B 107.5 . . ?
C30 C29 N2 115.6(2) . . ?
C30 C29 H29A 108.4 . . ?
C30 C29 H29B 108.4 . . ?
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 . . ?
N2 C31 H31A 108.4 . . ?
N2 C31 H31B 108.4 . . ?
H31A C31 H31B 107.5 . . ?
C32 C31 N2 115.3(2) . . ?
C32 C31 H31A 108.4 . . ?
C32 C31 H31B 108.4 . . ?
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 . . ?

_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_nix4
_database_code_depnum_ccdc_archive 'CCDC 1824477'
_audit_update_record             
;
2018-02-16 deposited with the CCDC.
2018-06-22 downloaded from the CCDC.
;
_audit_creation_date             2018-02-15
_audit_creation_method           
;
Olex2 1.2
(compiled Aug 10 2017 17:28:52 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        PTBCo(Br)(NCMe)2(NEt4)
_chemical_formula_moiety         
'C52 H52 B2 Br Co N2 P2, C8 H20 N, 4(C2 H3 N), C2 H9 N'
_chemical_formula_sum            'C70 H93 B2 Br Co N8 P2'
_chemical_formula_weight         1268.92
_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 0.0181 0.0091 '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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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           64
_space_group_name_H-M_alt        'C m c e'
_space_group_name_Hall           '-C 2bc 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'x, -y-1/2, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'x+1/2, -y, z-1/2'
'-x+1/2, y+1/2, z'

_cell_length_a                   25.9634(18)
_cell_length_b                   17.7060(13)
_cell_length_c                   29.773(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     13686.8(17)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9957
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      55.955
_cell_measurement_theta_min      2.969
_shelx_estimated_absorpt_T_max   0.683
_shelx_estimated_absorpt_T_min   0.532
_exptl_absorpt_coefficient_mu    3.436
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.4289
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1144 before and 0.0823 after correction.
The Ratio of minimum to maximum transmission is 0.5694.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             5368
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.3423
_diffrn_reflns_av_unetI/netI     0.1213
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            49683
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        56.482
_diffrn_reflns_theta_max         56.482
_diffrn_reflns_theta_min         2.968
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Apex Duo II'
_diffrn_measurement_method       ?
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2652
_reflns_number_total             4624
_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 v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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         1.435
_refine_diff_density_min         -1.134
_refine_diff_density_rms         0.135
_refine_ls_extinction_coef       0.00002(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         4624
_refine_ls_number_restraints     375
_refine_ls_R_factor_all          0.2300
_refine_ls_R_factor_gt           0.1730
_refine_ls_restrained_S_all      1.016
_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)+(0.1714P)²+557.0297P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4104
_refine_ls_wR_factor_ref         0.4570
_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
Uanis(C26) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(N6)
\\sim Ueq, Uanis(C33) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
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
 Fixed Sof: H26A(1.5) H26B(1.5) H26C(1.5) H28A(1.5) H28B(1.5) H28C(1.5)
 H34A(1.5) H34B(1.5) H34C(1.5)
5.a Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C31(H31A,H31B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23),
  C24(H24)
5.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C32(H32A,H32B,
 H32C), C38(H38A,H38B,H38C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C)
;
_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
Br1 Br 0.500000 0.40698(17) 0.42347(11) 0.0772(10) Uani 1 2 d S TU P . .
Co1 Co 0.500000 0.3152(2) 0.36444(15) 0.0662(13) Uani 1 2 d S TU P . .
P1 P 0.41345(15) 0.3143(2) 0.36594(16) 0.0608(13) Uani 1 1 d . U . . .
N1 N 0.500000 0.2060(14) 0.3651(8) 0.081(6) Uani 1 2 d S TU P . .
N2 N 0.500000 0.3336(15) 0.3010(10) 0.086(6) Uani 1 2 d S TU P . .
N3 N 0.3475(6) 0.500000 0.500000 0.059(4) Uani 1 2 d S TU P . .
C1 C 0.3289(6) 0.2792(8) 0.4156(6) 0.058(3) Uani 1 1 d . U . . .
C2 C 0.3829(6) 0.2799(9) 0.4162(6) 0.061(4) Uani 1 1 d . U . . .
C3 C 0.4101(6) 0.2540(9) 0.4531(6) 0.062(4) Uani 1 1 d . U . . .
H3 H 0.446707 0.255735 0.453104 0.075 Uiso 1 1 calc R . . . .
C4 C 0.3836(6) 0.2251(10) 0.4907(6) 0.068(4) Uani 1 1 d . U . . .
H4 H 0.401838 0.204876 0.515616 0.081 Uiso 1 1 calc R . . . .
C5 C 0.3319(6) 0.2269(9) 0.4904(6) 0.065(4) Uani 1 1 d . U . . .
H5 H 0.313737 0.209500 0.516067 0.078 Uiso 1 1 calc R . . . .
C6 C 0.3042(6) 0.2534(8) 0.4537(6) 0.059(4) Uani 1 1 d . U . . .
H6 H 0.267601 0.253669 0.454838 0.071 Uiso 1 1 calc R . . . .
C7 C 0.3785(6) 0.2568(9) 0.3261(6) 0.062(4) Uani 1 1 d . U . . .
C8 C 0.3251(6) 0.2572(9) 0.3294(6) 0.061(4) Uani 1 1 d . U . . .
C9 C 0.2978(7) 0.2172(10) 0.2962(6) 0.075(5) Uani 1 1 d . U . . .
H9 H 0.261266 0.220699 0.295326 0.090 Uiso 1 1 calc R . . . .
C10 C 0.3231(7) 0.1724(11) 0.2646(7) 0.088(6) Uani 1 1 d . U . . .
H10 H 0.303607 0.144582 0.243278 0.106 Uiso 1 1 calc R . . . .
C11 C 0.3768(7) 0.1681(10) 0.2640(7) 0.085(6) Uani 1 1 d . U . . .
H11 H 0.393882 0.135820 0.243390 0.102 Uiso 1 1 calc R . . . .
C12 C 0.4050(7) 0.2122(10) 0.2945(6) 0.071(5) Uani 1 1 d . U . . .
H12 H 0.441612 0.212002 0.293760 0.085 Uiso 1 1 calc R . . . .
C13 C 0.2380(6) 0.3049(10) 0.3755(6) 0.065(4) Uani 1 1 d . U . . .
C14 C 0.2128(7) 0.2347(10) 0.3708(6) 0.071(5) Uani 1 1 d . U . . .
H14 H 0.232616 0.191100 0.363821 0.086 Uiso 1 1 calc R . . . .
C15 C 0.1586(7) 0.2273(11) 0.3760(7) 0.079(5) Uani 1 1 d . U . . .
H15 H 0.142148 0.180217 0.370828 0.095 Uiso 1 1 calc R . . . .
C16 C 0.1301(6) 0.2896(11) 0.3889(7) 0.080(5) Uani 1 1 d . U . . .
H16 H 0.093777 0.285797 0.391559 0.096 Uiso 1 1 calc R . . . .
C17 C 0.1544(6) 0.3570(11) 0.3978(7) 0.075(5) Uani 1 1 d . U . . .
H17 H 0.134932 0.398921 0.408269 0.090 Uiso 1 1 calc R . . . .
C18 C 0.2068(6) 0.3640(10) 0.3914(6) 0.069(5) Uani 1 1 d . U . . .
H18 H 0.222587 0.411109 0.398177 0.083 Uiso 1 1 calc R . . . .
C19 C 0.3235(6) 0.3945(9) 0.3567(5) 0.057(3) Uani 1 1 d . U . . .
C20 C 0.3780(6) 0.4026(9) 0.3557(5) 0.058(3) Uani 1 1 d . U . . .
C21 C 0.2969(7) 0.4583(9) 0.3431(6) 0.069(4) Uani 1 1 d . U . . .
H21 H 0.260376 0.456183 0.341838 0.083 Uiso 1 1 calc R . . . .
C22 C 0.3212(7) 0.5254(10) 0.3313(7) 0.075(5) Uani 1 1 d . U . . .
H22 H 0.301198 0.567787 0.322502 0.090 Uiso 1 1 calc R . . . .
C23 C 0.3717(7) 0.5307(10) 0.3323(7) 0.082(6) Uani 1 1 d . U . . .
H23 H 0.387847 0.577269 0.325150 0.098 Uiso 1 1 calc R . . . .
C24 C 0.4026(7) 0.4666(9) 0.3442(6) 0.065(4) Uani 1 1 d . U . . .
H24 H 0.439135 0.469255 0.343930 0.078 Uiso 1 1 calc R . . . .
C25 C 0.500000 0.3409(19) 0.2640(13) 0.093(9) Uani 1 2 d S TU P . .
C26 C 0.500000 0.339(2) 0.2159(10) 0.125(9) Uani 1 2 d S TU P . .
H26A H 0.500996 0.286389 0.205655 0.187 Uiso 3 2 calc GR . . A 1
H26B H 0.530309 0.365874 0.204511 0.187 Uiso 1.5 1 calc GR . . A 1
H26C H 0.468695 0.363345 0.204548 0.187 Uiso 1.5 1 calc GR . . A 1
C27 C 0.500000 0.142(2) 0.3637(13) 0.122(13) Uani 1 2 d S TU P . .
C28 C 0.500000 0.0582(17) 0.3592(11) 0.118(8) Uani 1 2 d S TU P . .
H28A H 0.485927 0.035486 0.386532 0.177 Uiso 1.5 1 calc GR . . . .
H28B H 0.535343 0.040430 0.354539 0.177 Uiso 1.5 1 calc GR . . . .
H28C H 0.478729 0.043702 0.333373 0.177 Uiso 1.5 1 calc GR . . . .
C29 C 0.3812(6) 0.4297(10) 0.4954(7) 0.073(5) Uani 1 1 d . U . . .
H29A H 0.358478 0.385479 0.490961 0.087 Uiso 1 1 calc R . . . .
H29B H 0.402446 0.435158 0.467938 0.087 Uiso 1 1 calc R . . . .
C30 C 0.4171(7) 0.4132(11) 0.5348(7) 0.079(5) Uani 1 1 d . U . . .
H30A H 0.434923 0.365221 0.529626 0.118 Uiso 1 1 calc GR . . . .
H30B H 0.396863 0.409838 0.562543 0.118 Uiso 1 1 calc GR . . . .
H30C H 0.442429 0.453927 0.537588 0.118 Uiso 1 1 calc GR . . . .
C31 C 0.3155(7) 0.5039(10) 0.4575(7) 0.074(5) Uani 1 1 d . U . . .
H31A H 0.296102 0.456058 0.454074 0.089 Uiso 1 1 calc R . . . .
H31B H 0.338745 0.508896 0.431342 0.089 Uiso 1 1 calc R . . . .
C32 C 0.2768(8) 0.5709(12) 0.4575(8) 0.094(7) Uani 1 1 d . U . . .
H32A H 0.260539 0.574832 0.427888 0.142 Uiso 1 1 calc GR . . . .
H32B H 0.295247 0.617873 0.464192 0.142 Uiso 1 1 calc GR . . . .
H32C H 0.250350 0.562238 0.480368 0.142 Uiso 1 1 calc GR . . . .
B1 B 0.3003(7) 0.3090(10) 0.3685(7) 0.060(3) Uani 1 1 d . U . . .
N4 N 0.1035(15) 0.4742(17) 0.3004(11) 0.202(14) Uani 1 1 d . U . . .
C37 C 0.1316(14) 0.4289(14) 0.2879(10) 0.134(10) Uani 1 1 d . U . . .
C38 C 0.1676(9) 0.3756(13) 0.2712(8) 0.106(7) Uani 1 1 d . U . . .
H38A H 0.181674 0.393595 0.242623 0.159 Uiso 1 1 calc GR . . . .
H38B H 0.150459 0.326943 0.266644 0.159 Uiso 1 1 calc GR . . . .
H38C H 0.195699 0.369487 0.292963 0.159 Uiso 1 1 calc GR . . . .
N5 N 0.500000 0.212(3) 0.5709(15) 0.173(11) Uani 1 2 d S TU P . .
C33 C 0.500000 0.160(3) 0.5506(19) 0.168(11) Uani 1 2 d S TU P . .
C34 C 0.500000 0.0980(17) 0.5155(12) 0.123(10) Uani 1 2 d S TU P . .
H34A H 0.515703 0.052394 0.528170 0.185 Uiso 1.5 1 calc GR . . . .
H34B H 0.519805 0.114531 0.489300 0.185 Uiso 1.5 1 calc GR . . . .
H34C H 0.464492 0.087052 0.506490 0.185 Uiso 1.5 1 calc GR . . . .
N6 N 0.5900(16) 0.027(2) 0.4422(13) 0.219(15) Uani 1 1 d . U . . .
C35 C 0.622(2) 0.058(2) 0.421(2) 0.24(2) Uani 1 1 d . U . . .
C36 C 0.6547(10) 0.0829(13) 0.3845(10) 0.123(8) Uani 1 1 d . U . . .
H36A H 0.642185 0.061553 0.356223 0.185 Uiso 1 1 calc GR . . . .
H36B H 0.690150 0.065999 0.389878 0.185 Uiso 1 1 calc GR . . . .
H36C H 0.653968 0.138196 0.382796 0.185 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
Br1 Co1 2.394(5) . ?
Co1 P1 2.248(4) . ?
Co1 P1 2.248(4) 12_655 ?
Co1 N1 1.93(3) . ?
Co1 N2 1.92(3) . ?
P1 C2 1.800(17) . ?
P1 C7 1.807(17) . ?
P1 C20 1.839(17) . ?
N1 C27 1.14(4) . ?
N2 C25 1.11(4) . ?
N3 C29 1.528(18) 4_566 ?
N3 C29 1.528(18) . ?
N3 C31 1.516(19) 4_566 ?
N3 C31 1.516(19) . ?
C1 C2 1.40(2) . ?
C1 C6 1.38(2) . ?
C1 B1 1.67(3) . ?
C2 C3 1.39(2) . ?
C3 H3 0.9500 . ?
C3 C4 1.41(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.34(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.39(2) . ?
C6 H6 0.9500 . ?
C7 C8 1.39(2) . ?
C7 C12 1.41(2) . ?
C8 C9 1.41(2) . ?
C8 B1 1.62(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.39(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.40(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.40(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.41(2) . ?
C13 C18 1.41(2) . ?
C13 B1 1.63(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.42(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.38(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.38(2) . ?
C17 H17 0.9500 . ?
C17 C18 1.38(2) . ?
C18 H18 0.9500 . ?
C19 C20 1.42(2) . ?
C19 C21 1.39(2) . ?
C19 B1 1.67(2) . ?
C20 C24 1.35(2) . ?
C21 H21 0.9500 . ?
C21 C22 1.39(2) . ?
C22 H22 0.9500 . ?
C22 C23 1.31(2) . ?
C23 H23 0.9500 . ?
C23 C24 1.43(2) . ?
C24 H24 0.9500 . ?
C25 C26 1.43(4) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.48(5) . ?
C28 H28A 0.98(6) 12_655 ?
C28 H28A 0.9800 . ?
C28 H28B 0.98(2) 12_655 ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C28 H28C 0.98(8) 12_655 ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.53(2) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.55(2) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
N4 C37 1.15(3) . ?
C37 C38 1.42(3) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
N5 C33 1.10(6) . ?
C33 C34 1.51(6) . ?
C34 H34A 0.98(7) 12_655 ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34B 0.98(8) 12_655 ?
C34 H34C 0.9800 . ?
C34 H34C 0.980(12) 12_655 ?
N6 C35 1.18(5) . ?
C35 C36 1.45(5) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 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
P1 Co1 Br1 89.44(16) . . ?
P1 Co1 Br1 89.44(16) 12_655 . ?
P1 Co1 P1 177.6(3) 12_655 . ?
N1 Co1 Br1 132.1(7) . . ?
N1 Co1 P1 89.58(15) . 12_655 ?
N1 Co1 P1 89.58(16) . . ?
N2 Co1 Br1 127.4(8) . . ?
N2 Co1 P1 91.18(17) . 12_655 ?
N2 Co1 P1 91.19(17) . . ?
N2 Co1 N1 100.4(11) . . ?
C2 P1 Co1 117.4(6) . . ?
C2 P1 C7 97.7(8) . . ?
C2 P1 C20 101.8(7) . . ?
C7 P1 Co1 119.5(6) . . ?
C7 P1 C20 96.8(7) . . ?
C20 P1 Co1 119.4(6) . . ?
C27 N1 Co1 177(3) . . ?
C25 N2 Co1 177(3) . . ?
C29 N3 C29 110.0(16) . 4_566 ?
C31 N3 C29 110.7(11) . 4_566 ?
C31 N3 C29 110.7(11) 4_566 . ?
C31 N3 C29 106.0(10) . . ?
C31 N3 C29 106.0(10) 4_566 4_566 ?
C31 N3 C31 113.5(19) . 4_566 ?
C2 C1 B1 116.9(15) . . ?
C6 C1 C2 117.2(15) . . ?
C6 C1 B1 125.8(14) . . ?
C1 C2 P1 115.7(13) . . ?
C3 C2 P1 123.1(12) . . ?
C3 C2 C1 121.2(16) . . ?
C2 C3 H3 120.0 . . ?
C2 C3 C4 120.0(16) . . ?
C4 C3 H3 120.0 . . ?
C3 C4 H4 120.8 . . ?
C5 C4 C3 118.3(17) . . ?
C5 C4 H4 120.8 . . ?
C4 C5 H5 118.9 . . ?
C4 C5 C6 122.1(17) . . ?
C6 C5 H5 118.9 . . ?
C1 C6 C5 121.0(15) . . ?
C1 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
C8 C7 P1 116.9(13) . . ?
C8 C7 C12 122.5(16) . . ?
C12 C7 P1 120.6(12) . . ?
C7 C8 C9 116.8(16) . . ?
C7 C8 B1 116.8(15) . . ?
C9 C8 B1 126.2(15) . . ?
C8 C9 H9 119.3 . . ?
C10 C9 C8 121.5(17) . . ?
C10 C9 H9 119.3 . . ?
C9 C10 H10 119.7 . . ?
C9 C10 C11 120.7(18) . . ?
C11 C10 H10 119.7 . . ?
C10 C11 H11 120.5 . . ?
C10 C11 C12 118.9(18) . . ?
C12 C11 H11 120.5 . . ?
C7 C12 H12 120.4 . . ?
C11 C12 C7 119.2(16) . . ?
C11 C12 H12 120.4 . . ?
C14 C13 B1 119.0(14) . . ?
C18 C13 C14 115.0(15) . . ?
C18 C13 B1 125.5(15) . . ?
C13 C14 H14 119.1 . . ?
C13 C14 C15 121.8(17) . . ?
C15 C14 H14 119.1 . . ?
C14 C15 H15 120.4 . . ?
C16 C15 C14 119.2(17) . . ?
C16 C15 H15 120.4 . . ?
C15 C16 H16 119.9 . . ?
C17 C16 C15 120.1(16) . . ?
C17 C16 H16 119.9 . . ?
C16 C17 H17 119.9 . . ?
C16 C17 C18 120.2(18) . . ?
C18 C17 H17 119.9 . . ?
C13 C18 H18 118.4 . . ?
C17 C18 C13 123.2(17) . . ?
C17 C18 H18 118.4 . . ?
C20 C19 B1 117.1(14) . . ?
C21 C19 C20 114.1(15) . . ?
C21 C19 B1 128.4(15) . . ?
C19 C20 P1 114.1(12) . . ?
C24 C20 P1 121.4(13) . . ?
C24 C20 C19 124.2(16) . . ?
C19 C21 H21 118.5 . . ?
C19 C21 C22 123.0(16) . . ?
C22 C21 H21 118.5 . . ?
C21 C22 H22 119.7 . . ?
C23 C22 C21 120.5(17) . . ?
C23 C22 H22 119.7 . . ?
C22 C23 H23 119.7 . . ?
C22 C23 C24 120.5(17) . . ?
C24 C23 H23 119.7 . . ?
C20 C24 C23 117.6(16) . . ?
C20 C24 H24 121.2 . . ?
C23 C24 H24 121.2 . . ?
N2 C25 C26 172(4) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N1 C27 C28 177(4) . . ?
C27 C28 H28A 109(2) . 12_655 ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5(5) . 12_655 ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109(2) . 12_655 ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28A 43.8 . 12_655 ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 12_655 12_655 ?
H28A C28 H28B 68.6 . 12_655 ?
H28A C28 H28C 109.5 12_655 12_655 ?
H28A C28 H28C 138.9 . 12_655 ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28A 68.6 . 12_655 ?
H28B C28 H28B 138.9 . 12_655 ?
H28B C28 H28C 43.8 . 12_655 ?
H28B C28 H28C 109.5 12_655 12_655 ?
H28B C28 H28C 109.5 . . ?
H28C C28 H28A 138.9 . 12_655 ?
H28C C28 H28B 43.8 . 12_655 ?
H28C C28 H28C 68.6 . 12_655 ?
N3 C29 H29A 108.3 . . ?
N3 C29 H29B 108.3 . . ?
H29A C29 H29B 107.4 . . ?
C30 C29 N3 115.9(14) . . ?
C30 C29 H29A 108.3 . . ?
C30 C29 H29B 108.3 . . ?
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 . . ?
N3 C31 H31A 109.0 . . ?
N3 C31 H31B 109.0 . . ?
N3 C31 C32 112.9(15) . . ?
H31A C31 H31B 107.8 . . ?
C32 C31 H31A 109.0 . . ?
C32 C31 H31B 109.0 . . ?
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 . . ?
C8 B1 C1 104.4(13) . . ?
C8 B1 C13 117.5(15) . . ?
C8 B1 C19 102.6(14) . . ?
C13 B1 C1 108.7(15) . . ?
C13 B1 C19 115.2(13) . . ?
C19 B1 C1 107.6(13) . . ?
N4 C37 C38 177(4) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N5 C33 C34 170(6) . . ?
C33 C34 H34A 109(3) . 12_655 ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109(3) . 12_655 ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
C33 C34 H34C 109.5(3) . 12_655 ?
H34A C34 H34A 49.2 . 12_655 ?
H34A C34 H34B 109.5 12_655 12_655 ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34B 140.3 . 12_655 ?
H34A C34 H34C 63.3 . 12_655 ?
H34A C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 12_655 12_655 ?
H34B C34 H34A 140.3 . 12_655 ?
H34B C34 H34B 63.3 . 12_655 ?
H34B C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 12_655 12_655 ?
H34B C34 H34C 49.2 . 12_655 ?
H34C C34 H34A 63.3 . 12_655 ?
H34C C34 H34B 49.2 . 12_655 ?
H34C C34 H34C 140.3 . 12_655 ?
N6 C35 C36 163(6) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?

_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 0.115 0.316 114.2 26.7 ?
2 0.000 -0.115 0.684 114.2 25.8 ?
3 0.000 0.385 0.816 114.2 26.1 ?
4 0.000 0.615 0.184 114.2 26.4 ?
5 0.172 0.000 0.000 19.4 1.2 ?
6 0.172 0.500 0.500 19.4 1.2 ?
7 0.250 0.020 0.250 21.3 2.6 ?
8 0.250 -0.020 0.750 21.3 2.6 ?
9 0.250 0.480 0.750 21.3 2.6 ?
10 0.250 0.520 0.250 21.3 2.6 ?
11 0.328 0.000 0.500 19.4 1.2 ?
12 0.328 0.500 0.000 19.4 1.2 ?
13 0.500 0.115 0.184 114.2 26.4 ?
14 0.500 0.385 0.684 114.2 25.8 ?
15 0.500 0.615 0.316 114.2 26.7 ?
16 0.500 0.885 0.816 114.2 26.1 ?
17 0.672 0.000 0.500 19.4 1.2 ?
18 0.672 0.500 0.000 19.4 1.2 ?
19 0.750 0.020 0.250 21.3 2.6 ?
20 0.750 -0.020 0.750 21.3 2.6 ?
21 0.750 0.480 0.750 21.3 2.6 ?
22 0.750 0.520 0.250 21.3 2.6 ?
23 0.828 0.000 0.000 19.4 1.2 ?
24 0.828 0.500 0.500 19.4 1.2 ?


_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. 
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data_p17640final
_database_code_depnum_ccdc_archive 'CCDC 1824476'
_audit_update_record             
;
2018-02-16 deposited with the CCDC.
2018-06-22 downloaded from the CCDC.
;
_audit_creation_date             2017-12-18
_audit_creation_method           
;
Olex2 1.2
(compiled Aug 10 2017 17:28:52 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        Co(PTB)2Br2
_chemical_formula_moiety         
'2(C48 H34 B2 Br2 Co P2), C20 H38 Co N2 O4, 2(C4 H8 O), 2(C8 H20 N), 2(C2 H3 N)'
_chemical_formula_sum            'C144 H168 B4 Br4 Co3 N6 O6 P4'
_chemical_formula_weight         2742.38
_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'
B B 0.0013 0.0007 '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'
Co Co 0.3494 0.9721 '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'
P P 0.1023 0.0942 '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                   22.776(2)
_cell_length_b                   11.6346(12)
_cell_length_c                   27.261(3)
_cell_angle_alpha                90
_cell_angle_beta                 113.332(3)
_cell_angle_gamma                90
_cell_volume                     6633.1(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9125
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.576
_cell_measurement_theta_min      2.303
_shelx_estimated_absorpt_T_max   0.891
_shelx_estimated_absorpt_T_min   0.688
_exptl_absorpt_coefficient_mu    1.682
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6622
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0891 before and 0.0659 after correction.
The Ratio of minimum to maximum transmission is 0.8881.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2846
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1050
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            219281
_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         27.508
_diffrn_reflns_theta_min         2.203
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker AXS D8 Venture Kappa'
_diffrn_measurement_method       ?
_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                11129
_reflns_number_total             15217
_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 v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         2.765
_refine_diff_density_min         -1.201
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     769
_refine_ls_number_reflns         15217
_refine_ls_number_restraints     765
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0610
_refine_ls_restrained_S_all      1.002
_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)+(0.0632P)²+28.7521P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1377
_refine_ls_wR_factor_ref         0.1536
_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
Uanis(O1) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C51)
\\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C70) \\sim Ueq,
Uanis(C71) \\sim Ueq, Uanis(C72) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
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.a Free rotating group:
 O3(C69,C70,C71,C72)
4.b Secondary CH2 refined with riding coordinates:
 C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B), C68(H68A,H68B), C69(H69A,
 H69B), C70(H70A,H70B), C71(H71A,H71B), C72(H72A,H72B), C49(H49A,H49B),
 C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C55(H55A,H55B),
  C57(H57A,H57B), C59(H59A,H59B)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23),
  C24(H24), C27(H27), C28(H28), C29(H29), C30(H30), C33(H33), C34(H34),
 C35(H35), C36(H36), C39(H39), C40(H40), C41(H41), C42(H42), C44(H44), C45(H45),
  C46(H46), C47(H47), C48(H48)
4.d Idealised Me refined as rotating group:
 C64(H64A,H64B,H64C), C54(H54A,H54B,H54C), C56(H56A,H56B,H56C), C58(H58A,H58B,
 H58C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C)
;
_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
Br1 Br 0.09117(2) 0.61901(4) 0.24263(2) 0.02255(11) Uani 1 1 d . U . . .
Br2 Br 0.25382(2) 0.80904(4) 0.30002(2) 0.02799(12) Uani 1 1 d . U . . .
Co1 Co 0.19815(3) 0.64098(5) 0.30602(2) 0.01607(12) Uani 1 1 d . U . . .
P1 P 0.26016(5) 0.48954(9) 0.29140(4) 0.0170(2) Uani 1 1 d . U . . .
P2 P 0.18047(5) 0.65153(9) 0.38628(4) 0.0164(2) Uani 1 1 d . U . . .
C1 C 0.34748(19) 0.4874(4) 0.31829(16) 0.0207(8) Uani 1 1 d . U . . .
C2 C 0.3740(2) 0.3881(4) 0.30470(17) 0.0226(9) Uani 1 1 d . U . . .
C3 C 0.4402(2) 0.3782(4) 0.32947(19) 0.0294(10) Uani 1 1 d . U . . .
H3 H 0.460230 0.311717 0.322972 0.035 Uiso 1 1 calc R . . . .
C4 C 0.4778(2) 0.4630(5) 0.3636(2) 0.0359(11) Uani 1 1 d . U . . .
H4 H 0.522796 0.452663 0.380265 0.043 Uiso 1 1 calc R . . . .
C5 C 0.4509(2) 0.5615(4) 0.37343(19) 0.0315(10) Uani 1 1 d . U . . .
H5 H 0.477112 0.620458 0.395336 0.038 Uiso 1 1 calc R . . . .
C6 C 0.3848(2) 0.5736(4) 0.35096(17) 0.0237(9) Uani 1 1 d . U . . .
H6 H 0.365370 0.640361 0.357920 0.028 Uiso 1 1 calc R . . . .
C7 C 0.2815(2) 0.2563(4) 0.29756(17) 0.0232(9) Uani 1 1 d . U . . .
C8 C 0.24896(19) 0.3453(3) 0.31184(17) 0.0195(8) Uani 1 1 d . U . . .
C9 C 0.2154(2) 0.3276(4) 0.34390(18) 0.0241(9) Uani 1 1 d . U . . .
H9 H 0.194978 0.390118 0.353193 0.029 Uiso 1 1 calc R . . . .
C10 C 0.2118(2) 0.2173(4) 0.36234(19) 0.0298(10) Uani 1 1 d . U . . .
H10 H 0.188226 0.203617 0.383749 0.036 Uiso 1 1 calc R . . . .
C11 C 0.2429(2) 0.1279(4) 0.3492(2) 0.0318(10) Uani 1 1 d . U . . .
H11 H 0.240537 0.052314 0.361460 0.038 Uiso 1 1 calc R . . . .
C12 C 0.2775(2) 0.1480(4) 0.31821(19) 0.0285(10) Uani 1 1 d . U . . .
H12 H 0.299442 0.085493 0.310655 0.034 Uiso 1 1 calc R . . . .
C13 C 0.2770(2) 0.3709(4) 0.21242(17) 0.0235(9) Uani 1 1 d . U . . .
C14 C 0.24572(19) 0.4676(4) 0.22181(16) 0.0191(8) Uani 1 1 d . U . . .
C15 C 0.2108(2) 0.5442(4) 0.18208(17) 0.0251(9) Uani 1 1 d . U . . .
H15 H 0.190980 0.608905 0.190407 0.030 Uiso 1 1 calc R . . . .
C16 C 0.2049(2) 0.5259(4) 0.12991(19) 0.0321(11) Uani 1 1 d . U . . .
H16 H 0.181672 0.578395 0.102351 0.039 Uiso 1 1 calc R . . . .
C17 C 0.2334(2) 0.4296(5) 0.1188(2) 0.0366(12) Uani 1 1 d . U . . .
H17 H 0.228662 0.415131 0.083101 0.044 Uiso 1 1 calc R . . . .
C18 C 0.2688(2) 0.3540(4) 0.15921(19) 0.0326(11) Uani 1 1 d . U . . .
H18 H 0.287975 0.288955 0.150483 0.039 Uiso 1 1 calc R . . . .
C19 C 0.3540(2) 0.1903(4) 0.24090(18) 0.0273(9) Uani 1 1 d . U . . .
C20 C 0.3217(2) 0.0859(4) 0.2233(2) 0.0355(11) Uani 1 1 d . U . . .
H20 H 0.282698 0.073695 0.227572 0.043 Uiso 1 1 calc R . . . .
C21 C 0.3441(3) -0.0007(5) 0.1999(2) 0.0464(13) Uani 1 1 d . U . . .
H21 H 0.321205 -0.070797 0.189284 0.056 Uiso 1 1 calc R . . . .
C22 C 0.4001(3) 0.0161(5) 0.1922(3) 0.0534(15) Uani 1 1 d . U . . .
H22 H 0.416488 -0.043171 0.177262 0.064 Uiso 1 1 calc R . . . .
C23 C 0.4314(3) 0.1187(5) 0.2065(2) 0.0473(14) Uani 1 1 d . U . . .
H23 H 0.469164 0.131243 0.200327 0.057 Uiso 1 1 calc R . . . .
C24 C 0.4090(2) 0.2052(5) 0.2298(2) 0.0360(11) Uani 1 1 d . U . . .
H24 H 0.431300 0.276314 0.238412 0.043 Uiso 1 1 calc R . . . .
C25 C 0.14901(18) 0.7901(3) 0.39654(15) 0.0169(8) Uani 1 1 d . U . . .
C26 C 0.14536(18) 0.8033(4) 0.44681(16) 0.0176(8) Uani 1 1 d . U . . .
C27 C 0.12932(19) 0.9136(4) 0.45786(17) 0.0210(8) Uani 1 1 d . U . . .
H27 H 0.128479 0.928286 0.491862 0.025 Uiso 1 1 calc R . . . .
C28 C 0.1146(2) 1.0023(4) 0.42088(18) 0.0236(9) Uani 1 1 d . U . . .
H28 H 0.104199 1.076148 0.429971 0.028 Uiso 1 1 calc R . . . .
C29 C 0.1149(2) 0.9838(4) 0.37071(18) 0.0244(9) Uani 1 1 d . U . . .
H29 H 0.102548 1.043507 0.344806 0.029 Uiso 1 1 calc R . . . .
C30 C 0.13345(19) 0.8779(3) 0.35871(16) 0.0193(8) Uani 1 1 d . U . . .
H30 H 0.135537 0.865079 0.325025 0.023 Uiso 1 1 calc R . . . .
C31 C 0.2506(2) 0.6463(3) 0.44914(16) 0.0199(8) Uani 1 1 d . U . . .
C32 C 0.2406(2) 0.6720(3) 0.49554(16) 0.0209(8) Uani 1 1 d . U . . .
C33 C 0.2962(2) 0.6861(4) 0.54211(18) 0.0283(10) Uani 1 1 d . U . . .
H33 H 0.292378 0.706797 0.574430 0.034 Uiso 1 1 calc R . . . .
C34 C 0.3569(2) 0.6706(4) 0.54217(19) 0.0342(11) Uani 1 1 d . U . . .
H34 H 0.393518 0.681273 0.574363 0.041 Uiso 1 1 calc R . . . .
C35 C 0.3645(2) 0.6399(4) 0.4962(2) 0.0357(11) Uani 1 1 d . U . . .
H35 H 0.406041 0.627132 0.497077 0.043 Uiso 1 1 calc R . . . .
C36 C 0.3113(2) 0.6279(4) 0.44884(19) 0.0282(10) Uani 1 1 d . U . . .
H36 H 0.315890 0.607614 0.416778 0.034 Uiso 1 1 calc R . . . .
C37 C 0.12722(19) 0.5568(3) 0.40292(16) 0.0186(8) Uani 1 1 d . U . . .
C38 C 0.1254(2) 0.5816(4) 0.45262(16) 0.0200(8) Uani 1 1 d . U . . .
C39 C 0.0880(2) 0.5087(4) 0.46905(17) 0.0268(10) Uani 1 1 d . U . . .
H39 H 0.085580 0.521712 0.502598 0.032 Uiso 1 1 calc R . . . .
C40 C 0.0542(2) 0.4170(4) 0.43748(18) 0.0304(10) Uani 1 1 d . U . . .
H40 H 0.029843 0.367883 0.450085 0.037 Uiso 1 1 calc R . . . .
C41 C 0.0557(2) 0.3971(4) 0.38780(18) 0.0264(9) Uani 1 1 d . U . . .
H41 H 0.031885 0.335620 0.366047 0.032 Uiso 1 1 calc R . . . .
C42 C 0.0924(2) 0.4681(4) 0.37034(16) 0.0206(8) Uani 1 1 d . U . . .
H42 H 0.093645 0.456182 0.336300 0.025 Uiso 1 1 calc R . . . .
C43 C 0.1499(2) 0.7044(4) 0.54046(17) 0.0235(9) Uani 1 1 d . U . . .
C44 C 0.1868(2) 0.6497(4) 0.58935(17) 0.0281(10) Uani 1 1 d . U . . .
H44 H 0.224185 0.608837 0.592369 0.034 Uiso 1 1 calc R . . . .
C45 C 0.1700(3) 0.6538(4) 0.63314(19) 0.0365(11) Uani 1 1 d . U . . .
H45 H 0.195958 0.616051 0.665359 0.044 Uiso 1 1 calc R . . . .
C46 C 0.1161(3) 0.7121(4) 0.6302(2) 0.0364(11) Uani 1 1 d . U . . .
H46 H 0.105534 0.717019 0.660486 0.044 Uiso 1 1 calc R . . . .
C47 C 0.0777(2) 0.7634(4) 0.5825(2) 0.0344(11) Uani 1 1 d . U . . .
H47 H 0.039688 0.802041 0.579578 0.041 Uiso 1 1 calc R . . . .
C48 C 0.0947(2) 0.7582(4) 0.53859(18) 0.0271(9) Uani 1 1 d . U . . .
H48 H 0.067311 0.793153 0.506063 0.033 Uiso 1 1 calc R . . . .
B1 B 0.3238(2) 0.2934(4) 0.2633(2) 0.0246(10) Uani 1 1 d . U . . .
B2 B 0.1655(2) 0.6919(4) 0.48759(18) 0.0209(9) Uani 1 1 d . U . . .
Co2 Co 0.500000 1.000000 0.500000 0.0300(2) Uani 1 2 d S TU P . .
O2 O 0.47771(18) 0.9662(3) 0.41977(15) 0.0441(9) Uani 1 1 d . U . . .
N3 N 0.40670(19) 0.9571(4) 0.48952(19) 0.0404(11) Uani 1 1 d . U . . .
C63 C 0.3547(2) 0.9527(4) 0.4837(2) 0.0393(13) Uani 1 1 d . U . . .
C64 C 0.2878(2) 0.9487(5) 0.4765(3) 0.0553(17) Uani 1 1 d . U . . .
H64A H 0.263584 0.901721 0.445084 0.083 Uiso 1 1 calc GR . . . .
H64B H 0.270315 1.026771 0.471211 0.083 Uiso 1 1 calc GR . . . .
H64C H 0.284635 0.914778 0.508213 0.083 Uiso 1 1 calc GR . . . .
C65 C 0.4264(4) 0.8996(8) 0.3842(3) 0.078(2) Uani 1 1 d . U . . .
H65A H 0.385509 0.941674 0.374472 0.093 Uiso 1 1 calc R . . . .
H65B H 0.423159 0.826014 0.401228 0.093 Uiso 1 1 calc R . . . .
C66 C 0.5120(7) 1.0130(12) 0.3899(4) 0.158(6) Uani 1 1 d . U . . .
H66A H 0.510291 1.098049 0.390190 0.190 Uiso 1 1 calc R . . . .
H66B H 0.557414 0.989173 0.406329 0.190 Uiso 1 1 calc R . . . .
C67 C 0.4835(5) 0.9719(8) 0.3362(3) 0.092(3) Uani 1 1 d . U . . .
H67A H 0.516659 0.942857 0.324452 0.110 Uiso 1 1 calc R . . . .
H67B H 0.459553 1.034298 0.311759 0.110 Uiso 1 1 calc R . . . .
C68 C 0.4395(4) 0.8778(7) 0.3361(3) 0.073(2) Uani 1 1 d . U . . .
H68A H 0.399577 0.880502 0.303393 0.088 Uiso 1 1 calc R . . . .
H68B H 0.459967 0.801849 0.338226 0.088 Uiso 1 1 calc R . . . .
O3 O 0.46575(16) 1.1692(3) 0.47837(16) 0.0492(10) Uani 1 1 d . U . A -1
C69 C 0.4141(3) 1.2031(5) 0.42929(15) 0.136(4) Uani 1 1 d G U . A -1
H69A H 0.380459 1.143321 0.417579 0.164 Uiso 1 1 calc R . . A -1
H69B H 0.430030 1.214668 0.400705 0.164 Uiso 1 1 calc R . . A -1
C70 C 0.3875(2) 1.3160(5) 0.4412(2) 0.0632(18) Uani 1 1 d G U . A -1
H70A H 0.354248 1.301709 0.455336 0.076 Uiso 1 1 calc R . . A -1
H70B H 0.369569 1.365201 0.409053 0.076 Uiso 1 1 calc R . . A -1
C71 C 0.4478(3) 1.3699(3) 0.4839(3) 0.124(4) Uani 1 1 d G U . A -1
H71A H 0.474198 1.409094 0.467553 0.149 Uiso 1 1 calc R . . A -1
H71B H 0.436827 1.425215 0.506572 0.149 Uiso 1 1 calc R . . A -1
C72 C 0.4819(3) 1.2636(5) 0.51584(19) 0.153(5) Uani 1 1 d G U . A -1
H72A H 0.528713 1.275766 0.531914 0.184 Uiso 1 1 calc R . . A -1
H72B H 0.467164 1.247558 0.544811 0.184 Uiso 1 1 calc R . . A -1
O1 O 0.2467(5) 0.3706(7) 0.5441(3) 0.132(3) Uani 1 1 d . U . . .
C49 C 0.3158(6) 0.3607(11) 0.5617(6) 0.133(4) Uani 1 1 d . U . . .
H49A H 0.337552 0.371163 0.600817 0.159 Uiso 1 1 calc R . . . .
H49B H 0.332466 0.418181 0.543650 0.159 Uiso 1 1 calc R . . . .
C50 C 0.3255(5) 0.2372(9) 0.5453(4) 0.094(2) Uani 1 1 d . U . . .
H50A H 0.361800 0.234389 0.534011 0.113 Uiso 1 1 calc R . . . .
H50B H 0.334138 0.183319 0.575466 0.113 Uiso 1 1 calc R . . . .
C51 C 0.2728(6) 0.2111(9) 0.5061(4) 0.121(4) Uani 1 1 d . U . . .
H51A H 0.256802 0.137271 0.514000 0.145 Uiso 1 1 calc R . . . .
H51B H 0.281212 0.200548 0.473442 0.145 Uiso 1 1 calc R . . . .
C52 C 0.2252(7) 0.2962(12) 0.4965(6) 0.164(5) Uani 1 1 d . U . . .
H52A H 0.183607 0.260294 0.490832 0.197 Uiso 1 1 calc R . . . .
H52B H 0.220134 0.341553 0.464285 0.197 Uiso 1 1 calc R . . . .
N1 N 0.07017(17) 0.2231(3) 0.17069(14) 0.0234(8) Uani 1 1 d . U . . .
C53 C 0.0187(2) 0.2393(4) 0.19209(18) 0.0267(10) Uani 1 1 d . U . . .
H53A H 0.000648 0.163012 0.194391 0.032 Uiso 1 1 calc R . . . .
H53B H -0.016206 0.285852 0.166124 0.032 Uiso 1 1 calc R . . . .
C54 C 0.0404(2) 0.2966(4) 0.24631(19) 0.0315(11) Uani 1 1 d . U . . .
H54A H 0.055378 0.374636 0.244018 0.047 Uiso 1 1 calc GR . . . .
H54B H 0.075427 0.252071 0.272409 0.047 Uiso 1 1 calc GR . . . .
H54C H 0.004632 0.300228 0.257593 0.047 Uiso 1 1 calc GR . . . .
C55 C 0.0985(2) 0.3388(4) 0.16505(18) 0.0267(9) Uani 1 1 d . U . . .
H55A H 0.115844 0.376920 0.200406 0.032 Uiso 1 1 calc R . . . .
H55B H 0.134653 0.324834 0.154375 0.032 Uiso 1 1 calc R . . . .
C56 C 0.0519(2) 0.4199(5) 0.1251(2) 0.0364(12) Uani 1 1 d . U . . .
H56A H 0.036799 0.385664 0.089326 0.055 Uiso 1 1 calc GR . . . .
H56B H 0.073327 0.492977 0.125146 0.055 Uiso 1 1 calc GR . . . .
H56C H 0.015443 0.433505 0.134804 0.055 Uiso 1 1 calc GR . . . .
C57 C 0.0373(2) 0.1648(4) 0.11683(18) 0.0317(11) Uani 1 1 d . U . . .
H57A H 0.019790 0.090428 0.122379 0.038 Uiso 1 1 calc R . . . .
H57B H 0.000829 0.213172 0.094316 0.038 Uiso 1 1 calc R . . . .
C58 C 0.0792(3) 0.1430(5) 0.0868(2) 0.0482(15) Uani 1 1 d . U . . .
H58A H 0.054140 0.105055 0.052836 0.072 Uiso 1 1 calc GR . . . .
H58B H 0.114998 0.093464 0.108215 0.072 Uiso 1 1 calc GR . . . .
H58C H 0.095735 0.216236 0.079880 0.072 Uiso 1 1 calc GR . . . .
C59 C 0.1249(2) 0.1516(4) 0.20840(19) 0.0308(10) Uani 1 1 d . U . . .
H59A H 0.156955 0.142064 0.192561 0.037 Uiso 1 1 calc R . . . .
H59B H 0.145713 0.194559 0.242262 0.037 Uiso 1 1 calc R . . . .
C60 C 0.1067(3) 0.0337(4) 0.2212(2) 0.0399(12) Uani 1 1 d . U . . .
H60A H 0.086001 -0.010004 0.188027 0.060 Uiso 1 1 calc GR . . . .
H60B H 0.076997 0.041823 0.238985 0.060 Uiso 1 1 calc GR . . . .
H60C H 0.145145 -0.006978 0.244825 0.060 Uiso 1 1 calc GR . . . .
N2 N 0.4271(3) 0.7218(5) 0.1633(2) 0.0644(16) Uani 1 1 d . U . . .
C61 C 0.3749(4) 0.6232(8) 0.2186(3) 0.090(3) Uani 1 1 d . U . . .
H61A H 0.348370 0.559466 0.198047 0.136 Uiso 1 1 calc GR . . . .
H61B H 0.348158 0.678129 0.227665 0.136 Uiso 1 1 calc GR . . . .
H61C H 0.408172 0.593299 0.251495 0.136 Uiso 1 1 calc GR . . . .
C62 C 0.4036(3) 0.6784(6) 0.1880(2) 0.0501(15) 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
Br1 Co1 2.3777(7) . ?
Br2 Co1 2.3711(7) . ?
Co1 P1 2.3883(12) . ?
Co1 P2 2.3797(11) . ?
P1 C1 1.827(4) . ?
P1 C8 1.818(4) . ?
P1 C14 1.810(4) . ?
P2 C25 1.831(4) . ?
P2 C31 1.823(4) . ?
P2 C37 1.824(4) . ?
C1 C2 1.419(6) . ?
C1 C6 1.386(6) . ?
C2 C3 1.391(6) . ?
C2 B1 1.666(7) . ?
C3 C4 1.394(7) . ?
C4 C5 1.375(7) . ?
C5 C6 1.389(6) . ?
C7 C8 1.415(6) . ?
C7 C12 1.398(6) . ?
C7 B1 1.643(6) . ?
C8 C9 1.386(6) . ?
C9 C10 1.392(6) . ?
C10 C11 1.384(7) . ?
C11 C12 1.383(7) . ?
C13 C14 1.408(6) . ?
C13 C18 1.401(6) . ?
C13 B1 1.643(7) . ?
C14 C15 1.385(6) . ?
C15 C16 1.391(6) . ?
C16 C17 1.387(7) . ?
C17 C18 1.391(7) . ?
C19 C20 1.403(7) . ?
C19 C24 1.412(6) . ?
C19 B1 1.617(6) . ?
C20 C21 1.394(7) . ?
C21 C22 1.384(8) . ?
C22 C23 1.367(9) . ?
C23 C24 1.391(7) . ?
C25 C26 1.414(5) . ?
C25 C30 1.393(6) . ?
C26 C27 1.399(6) . ?
C26 B2 1.650(6) . ?
C27 C28 1.388(6) . ?
C28 C29 1.387(6) . ?
C29 C30 1.383(6) . ?
C31 C32 1.403(6) . ?
C31 C36 1.404(6) . ?
C32 C33 1.403(6) . ?
C32 B2 1.653(7) . ?
C33 C34 1.393(7) . ?
C34 C35 1.377(7) . ?
C35 C36 1.384(7) . ?
C37 C38 1.402(6) . ?
C37 C42 1.387(6) . ?
C38 C39 1.395(6) . ?
C38 B2 1.644(6) . ?
C39 C40 1.395(6) . ?
C40 C41 1.388(6) . ?
C41 C42 1.387(6) . ?
C43 C44 1.414(6) . ?
C43 C48 1.387(7) . ?
C43 B2 1.622(6) . ?
C44 C45 1.391(6) . ?
C45 C46 1.376(8) . ?
C46 C47 1.382(8) . ?
C47 C48 1.399(6) . ?
Co2 O2 2.078(4) 3_676 ?
Co2 O2 2.078(4) . ?
Co2 N3 2.089(4) 3_676 ?
Co2 N3 2.089(4) . ?
Co2 O3 2.113(3) . ?
O2 C65 1.418(7) . ?
O2 C66 1.441(9) . ?
N3 C63 1.133(6) . ?
C63 C64 1.456(7) . ?
C65 C68 1.478(10) . ?
C66 C67 1.428(11) . ?
C67 C68 1.483(10) . ?
O3 C69 1.4431 . ?
O3 C72 1.4448 . ?
C69 C70 1.5346 . ?
C70 C71 1.5390 . ?
C71 C72 1.5347 . ?
O1 C49 1.457(14) . ?
O1 C52 1.473(13) . ?
C49 C50 1.545(15) . ?
C50 C51 1.288(13) . ?
C51 C52 1.414(14) . ?
N1 C53 1.515(5) . ?
N1 C55 1.526(6) . ?
N1 C57 1.518(5) . ?
N1 C59 1.513(6) . ?
C53 C54 1.515(6) . ?
C55 C56 1.512(6) . ?
C57 C58 1.503(7) . ?
C59 C60 1.513(7) . ?
N2 C62 1.133(7) . ?
C61 C62 1.402(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
Br1 Co1 P1 107.64(3) . . ?
Br1 Co1 P2 100.13(3) . . ?
Br2 Co1 Br1 117.43(3) . . ?
Br2 Co1 P1 103.25(3) . . ?
Br2 Co1 P2 108.10(3) . . ?
P2 Co1 P1 121.21(4) . . ?
C1 P1 Co1 124.38(15) . . ?
C8 P1 Co1 117.77(14) . . ?
C8 P1 C1 97.31(19) . . ?
C14 P1 Co1 113.89(14) . . ?
C14 P1 C1 97.80(19) . . ?
C14 P1 C8 101.63(19) . . ?
C25 P2 Co1 113.89(13) . . ?
C31 P2 Co1 117.30(14) . . ?
C31 P2 C25 97.81(18) . . ?
C31 P2 C37 99.60(19) . . ?
C37 P2 Co1 124.66(14) . . ?
C37 P2 C25 98.95(19) . . ?
C2 C1 P1 114.5(3) . . ?
C6 C1 P1 122.8(3) . . ?
C6 C1 C2 122.7(4) . . ?
C1 C2 B1 117.8(4) . . ?
C3 C2 C1 115.6(4) . . ?
C3 C2 B1 126.5(4) . . ?
C2 C3 C4 121.8(4) . . ?
C5 C4 C3 121.1(4) . . ?
C4 C5 C6 119.2(5) . . ?
C1 C6 C5 119.5(4) . . ?
C8 C7 B1 117.0(4) . . ?
C12 C7 C8 115.1(4) . . ?
C12 C7 B1 127.8(4) . . ?
C7 C8 P1 116.0(3) . . ?
C9 C8 P1 120.7(3) . . ?
C9 C8 C7 123.0(4) . . ?
C8 C9 C10 119.4(4) . . ?
C11 C10 C9 119.3(4) . . ?
C12 C11 C10 120.3(4) . . ?
C11 C12 C7 122.8(4) . . ?
C14 C13 B1 119.4(4) . . ?
C18 C13 C14 115.5(4) . . ?
C18 C13 B1 124.9(4) . . ?
C13 C14 P1 114.1(3) . . ?
C15 C14 P1 122.6(3) . . ?
C15 C14 C13 123.2(4) . . ?
C14 C15 C16 119.6(4) . . ?
C17 C16 C15 118.9(4) . . ?
C16 C17 C18 120.8(4) . . ?
C17 C18 C13 122.0(4) . . ?
C20 C19 C24 115.0(4) . . ?
C20 C19 B1 121.8(4) . . ?
C24 C19 B1 122.4(4) . . ?
C21 C20 C19 123.0(5) . . ?
C22 C21 C20 119.6(5) . . ?
C23 C22 C21 119.3(5) . . ?
C22 C23 C24 121.1(5) . . ?
C23 C24 C19 121.8(5) . . ?
C26 C25 P2 114.9(3) . . ?
C30 C25 P2 122.2(3) . . ?
C30 C25 C26 122.8(4) . . ?
C25 C26 B2 117.4(4) . . ?
C27 C26 C25 115.4(4) . . ?
C27 C26 B2 127.0(4) . . ?
C28 C27 C26 122.3(4) . . ?
C29 C28 C27 120.5(4) . . ?
C30 C29 C28 119.5(4) . . ?
C29 C30 C25 119.3(4) . . ?
C32 C31 P2 116.5(3) . . ?
C32 C31 C36 123.3(4) . . ?
C36 C31 P2 119.9(3) . . ?
C31 C32 C33 115.5(4) . . ?
C31 C32 B2 116.1(3) . . ?
C33 C32 B2 128.2(4) . . ?
C34 C33 C32 121.7(4) . . ?
C35 C34 C33 121.0(4) . . ?
C34 C35 C36 119.8(5) . . ?
C35 C36 C31 118.6(4) . . ?
C38 C37 P2 113.2(3) . . ?
C42 C37 P2 123.9(3) . . ?
C42 C37 C38 122.9(4) . . ?
C37 C38 B2 119.9(4) . . ?
C39 C38 C37 116.1(4) . . ?
C39 C38 B2 124.0(4) . . ?
C38 C39 C40 121.7(4) . . ?
C41 C40 C39 120.6(4) . . ?
C42 C41 C40 119.1(4) . . ?
C37 C42 C41 119.5(4) . . ?
C44 C43 B2 122.7(4) . . ?
C48 C43 C44 115.4(4) . . ?
C48 C43 B2 121.5(4) . . ?
C45 C44 C43 122.0(5) . . ?
C46 C45 C44 120.6(5) . . ?
C45 C46 C47 119.1(4) . . ?
C46 C47 C48 119.9(5) . . ?
C43 C48 C47 122.9(5) . . ?
C7 B1 C2 100.8(3) . . ?
C13 B1 C2 104.5(3) . . ?
C13 B1 C7 107.1(3) . . ?
C19 B1 C2 117.8(4) . . ?
C19 B1 C7 116.9(4) . . ?
C19 B1 C13 108.6(4) . . ?
C26 B2 C32 101.3(3) . . ?
C38 B2 C26 106.3(3) . . ?
C38 B2 C32 106.0(3) . . ?
C43 B2 C26 115.4(4) . . ?
C43 B2 C32 118.4(4) . . ?
C43 B2 C38 108.5(3) . . ?
O2 Co2 O2 180.0 . 3_676 ?
O2 Co2 N3 90.02(17) . 3_676 ?
O2 Co2 N3 89.98(17) 3_676 3_676 ?
O2 Co2 N3 89.98(17) . . ?
O2 Co2 N3 90.02(17) 3_676 . ?
O2 Co2 O3 91.53(16) 3_676 . ?
O2 Co2 O3 88.47(15) . . ?
N3 Co2 N3 180.0 3_676 . ?
N3 Co2 O3 86.64(16) . . ?
N3 Co2 O3 93.36(16) 3_676 . ?
C65 O2 Co2 127.9(4) . . ?
C65 O2 C66 107.8(6) . . ?
C66 O2 Co2 124.3(4) . . ?
C63 N3 Co2 168.8(4) . . ?
N3 C63 C64 179.2(7) . . ?
O2 C65 C68 107.4(6) . . ?
C67 C66 O2 108.9(7) . . ?
C66 C67 C68 106.4(7) . . ?
C65 C68 C67 104.2(6) . . ?
C69 O3 Co2 126.1(3) . . ?
C69 O3 C72 109.5 . . ?
C72 O3 Co2 123.3(3) . . ?
O3 C69 C70 106.4 . . ?
C69 C70 C71 101.5 . . ?
C72 C71 C70 101.5 . . ?
O3 C72 C71 106.4 . . ?
C49 O1 C52 100.6(10) . . ?
O1 C49 C50 103.8(9) . . ?
C51 C50 C49 105.4(10) . . ?
C50 C51 C52 112.6(10) . . ?
C51 C52 O1 106.5(10) . . ?
C53 N1 C55 110.6(3) . . ?
C53 N1 C57 105.5(3) . . ?
C57 N1 C55 111.2(3) . . ?
C59 N1 C53 111.2(3) . . ?
C59 N1 C55 106.6(3) . . ?
C59 N1 C57 111.7(4) . . ?
N1 C53 C54 115.2(4) . . ?
C56 C55 N1 114.8(4) . . ?
C58 C57 N1 115.2(4) . . ?
C60 C59 N1 115.3(4) . . ?
N2 C62 C61 179.2(9) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT413_p17640final         
;
PROBLEM: Short Inter XH3 .. XHn    H51A     ..H64B      .       1.86 Ang.  
RESPONSE: H51A belongs to a disordered THF solvent molecule whose carbon 
atoms have been restrained.
;
