# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_LIOMe_lc-50ax
_database_code_depnum_ccdc_archive 'CCDC 1517785'
# end Validation Reply Form

_audit_update_record             
;
2017-02-03 deposited with the CCDC.
2017-02-06 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT410_I                   
;
PROBLEM: Short Intra H...H Contact  H12A   ..  H25B    ..       1.76 Ang.  
RESPONSE: H-atoms in differnt parts of the disordered structure
;
_vrf_PLAT770_I                   
;
PROBLEM: Suspect C-H Bond in CIF:   C12A   --  H11C    ..       1.54 Ang.  
RESPONSE: H-atoms in differnt parts of the disordered structure
;
_vrf_PLAT771_I                   
;
PROBLEM: Suspect N-H Bond in CIF:   N4A    --  H27C    ..       1.49 Ang.  
RESPONSE: H-atoms in differnt parts of the disordered structure
;
_publcif_datablock.id            {66e62d46-ee85-4b30-9929-30e91597bbf5}

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H51 N8 O3'
_chemical_formula_weight         679.88

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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pna21
_symmetry_space_group_name_Hall  'P 2c -2n'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z'

_cell_length_a                   14.368(2)
_cell_length_b                   20.759(2)
_cell_length_c                   12.3557(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3685.3(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    5165
_cell_measurement_theta_min      4.42
_cell_measurement_theta_max      46.09

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1460
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.9839
_exptl_absorpt_correction_T_max  0.9947
_exptl_absorpt_process_details   
;
 [X-Red (Stoe & Cie, 2001) and X-Shape (Stoe & Cie, 1999)]
;

_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'STOE IPDS I'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24606
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_sigmaI/netI    0.0772
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.92
_diffrn_reflns_theta_max         23.98
_reflns_number_total             5630
_reflns_number_gt                2861
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_structure_solution    'SIR92 (Altomare 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Diamond (Brandenburg 2011)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1174P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5630
_refine_ls_number_parameters     488
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1097
_refine_ls_R_factor_gt           0.0629
_refine_ls_wR_factor_ref         0.1853
_refine_ls_wR_factor_gt          0.1620
_refine_ls_goodness_of_fit_ref   0.873
_refine_ls_restrained_S_all      0.879
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1A O 0.6200(8) 0.9756(5) 0.1784(11) 0.081(3) Uani 0.591(2) 1 d P A 1
O3A O 0.6051(5) 0.9591(4) 0.8597(6) 0.0525(17) Uani 0.591(2) 1 d P A 1
N3A N 0.6083(5) 1.1349(4) 0.5608(8) 0.0486(11) Uani 0.591(2) 1 d P A 1
N4A N 0.8980(5) 1.1582(4) 0.6425(7) 0.0459(18) Uani 0.591(2) 1 d P A 1
N5A N 0.8133(7) 1.1600(4) 0.3118(8) 0.053(2) Uani 0.591(2) 1 d P A 1
N6A N 0.6759(5) 0.7935(4) 0.5667(9) 0.0572(13) Uani 0.591(2) 1 d P A 1
N7A N 0.8705(7) 0.8147(5) 0.3016(9) 0.064(2) Uani 0.591(2) 1 d P A 1
N8A N 0.9702(6) 0.8132(4) 0.6332(8) 0.0523(19) Uani 0.591(2) 1 d P A 1
C3A C 0.6775(17) 0.8472(12) 0.5195(13) 0.054(3) Uani 0.591(2) 1 d P A 1
H3A H 0.6890 0.8495 0.4455 0.064 Uiso 0.591(2) 1 calc PR A 1
C4A C 0.6604(5) 0.9082(2) 0.5848(5) 0.0463(12) Uani 0.591(2) 1 d PG A 1
C5A C 0.6399(5) 0.9075(2) 0.6947(5) 0.0507(14) Uani 0.591(2) 1 d PG A 1
H5A H 0.6384 0.8687 0.7322 0.061 Uiso 0.591(2) 1 calc PR A 1
C6A C 0.6216(5) 0.9649(3) 0.7487(4) 0.0494(16) Uani 0.591(2) 1 d PG A 1
C7A C 0.6238(5) 1.0230(2) 0.6927(5) 0.0451(13) Uani 0.591(2) 1 d PG A 1
H7A H 0.6116 1.0614 0.7288 0.054 Uiso 0.591(2) 1 calc PR A 1
C8A C 0.6443(5) 1.0237(2) 0.5828(5) 0.0454(12) Uani 0.591(2) 1 d PG A 1
C9A C 0.6626(5) 0.9663(3) 0.5288(4) 0.0426(15) Uani 0.591(2) 1 d PG A 1
H9A H 0.6763 0.9667 0.4552 0.051 Uiso 0.591(2) 1 calc PR A 1
C10A C 0.6397(8) 1.0837(6) 0.5182(10) 0.0420(14) Uani 0.591(2) 1 d P A 1
H10A H 0.6597 1.0839 0.4466 0.050 Uiso 0.591(2) 1 calc PR A 1
C12A C 0.6590(7) 1.2457(5) 0.5351(12) 0.0501(15) Uani 0.591(2) 1 d P A 1
H12A H 0.6582 1.2478 0.6135 0.060 Uiso 0.591(2) 1 calc PR A 1
H12B H 0.6360 1.2863 0.5071 0.060 Uiso 0.591(2) 1 calc PR A 1
C13A C 0.8751(5) 0.7094(4) 0.3741(9) 0.055(3) Uani 0.591(2) 1 d P A 1
H13A H 0.9049 0.6677 0.3667 0.066 Uiso 0.591(2) 1 calc PR A 1
H13B H 0.8164 0.7077 0.3356 0.066 Uiso 0.591(2) 1 calc PR A 1
C16A C 0.8414(4) 0.9285(3) 0.3019(6) 0.044(2) Uani 0.591(2) 1 d PG A 1
C17A C 0.7549(5) 0.9223(2) 0.2528(6) 0.051(2) Uani 0.591(2) 1 d PG A 1
H17A H 0.7320 0.8816 0.2355 0.061 Uiso 0.591(2) 1 calc PR A 1
C18A C 0.7025(4) 0.9768(3) 0.2294(7) 0.057(2) Uani 0.591(2) 1 d PG A 1
C19A C 0.7366(4) 1.0375(3) 0.2553(6) 0.054(2) Uani 0.591(2) 1 d PG A 1
H19A H 0.7015 1.0740 0.2397 0.065 Uiso 0.591(2) 1 calc PR A 1
C20A C 0.8231(5) 1.0437(2) 0.3044(6) 0.045(2) Uani 0.591(2) 1 d PG A 1
C21A C 0.8756(4) 0.9892(3) 0.3278(6) 0.050(2) Uani 0.591(2) 1 d PG A 1
H21A H 0.9335 0.9933 0.3607 0.060 Uiso 0.591(2) 1 calc PR A 1
C22A C 0.8705(11) 1.1020(8) 0.333(2) 0.0420(14) Uani 0.591(2) 1 d P A 1
H22A H 0.9303 1.1033 0.3620 0.050 Uiso 0.591(2) 1 calc PR A 1
C28A C 0.9270(5) 1.0432(4) 0.6269(8) 0.046(2) Uani 0.591(2) 1 d P A 1
C29A C 1.0125(6) 1.0519(4) 0.5725(7) 0.0424(19) Uani 0.591(2) 1 d P A 1
H29A H 1.0332 1.0931 0.5551 0.051 Uiso 0.591(2) 1 calc PR A 1
C30A C 1.0660(6) 0.9978(4) 0.5448(7) 0.044(2) Uani 0.591(2) 1 d P A 1
C31A C 1.0360(5) 0.9366(4) 0.5701(7) 0.044(2) Uani 0.591(2) 1 d P A 1
H31A H 1.0720 0.9013 0.5501 0.053 Uiso 0.591(2) 1 calc PR A 1
C32A C 0.9533(6) 0.9269(4) 0.6247(8) 0.050(2) Uani 0.591(2) 1 d P A 1
C33A C 0.8984(7) 0.9798(5) 0.6470(10) 0.048(2) Uani 0.591(2) 1 d P A 1
H33A H 0.8398 0.9730 0.6768 0.057 Uiso 0.591(2) 1 calc PR A 1
C37A C 0.5675(9) 0.9161(6) 0.1655(13) 0.098(4) Uani 0.591(2) 1 d P A 1
H37A H 0.5052 0.9259 0.1427 0.147 Uiso 0.591(2) 1 calc PR A 1
H37B H 0.5656 0.8935 0.2332 0.147 Uiso 0.591(2) 1 calc PR A 1
H37C H 0.5971 0.8895 0.1119 0.147 Uiso 0.591(2) 1 calc PR A 1
C38A C 0.5949(8) 1.0168(6) 0.9188(8) 0.060(2) Uani 0.591(2) 1 d P A 1
H38A H 0.5845 1.0068 0.9937 0.090 Uiso 0.591(2) 1 calc PR A 1
H38B H 0.5429 1.0406 0.8911 0.090 Uiso 0.591(2) 1 calc PR A 1
H38C H 0.6505 1.0421 0.9120 0.090 Uiso 0.591(2) 1 calc PR A 1
C39A C 1.1757(10) 1.0683(7) 0.4545(11) 0.060(2) Uani 0.591(2) 1 d P A 1
H39A H 1.2355 1.0656 0.4200 0.090 Uiso 0.591(2) 1 calc PR A 1
H39B H 1.1792 1.0977 0.5144 0.090 Uiso 0.591(2) 1 calc PR A 1
H39C H 1.1304 1.0835 0.4034 0.090 Uiso 0.591(2) 1 calc PR A 1
C36 C 0.9130(7) 0.7051(5) 0.5806(10) 0.161(6) Uani 1 1 d D A 1
H36A H 0.9723 0.6931 0.5489 0.194 Uiso 1 1 calc R A 1
H36B H 0.8875 0.6669 0.6147 0.194 Uiso 1 1 calc R A 1
O1B O 0.6050(13) 0.9561(8) 0.1373(19) 0.081(3) Uani 0.409(2) 1 d P A 2
O3B O 0.6049(7) 0.9777(6) 0.7979(9) 0.0525(17) Uani 0.409(2) 1 d PD A 2
N3B N 0.6002(8) 1.1374(7) 0.4224(11) 0.0486(11) Uani 0.409(2) 1 d P A 2
N4B N 0.8172(8) 1.1592(7) 0.6758(11) 0.0459(18) Uani 0.409(2) 1 d P A 2
N5B N 0.8915(10) 1.1531(7) 0.3377(11) 0.053(2) Uani 0.409(2) 1 d P A 2
N6B N 0.6707(8) 0.7917(6) 0.4359(13) 0.0572(13) Uani 0.409(2) 1 d P A 2
N7B N 0.9685(9) 0.8099(7) 0.3609(13) 0.064(2) Uani 0.409(2) 1 d P A 2
N8B N 0.8698(10) 0.8147(7) 0.6975(12) 0.0523(19) Uani 0.409(2) 1 d P A 2
C3B C 0.676(3) 0.8496(19) 0.4683(19) 0.054(3) Uani 0.409(2) 1 d P A 2
H3B H 0.6920 0.8549 0.5407 0.064 Uiso 0.409(2) 1 calc PR A 2
C4B C 0.6614(7) 0.9087(4) 0.4076(7) 0.0463(12) Uani 0.409(2) 1 d PG A 2
C5B C 0.6416(7) 0.9065(3) 0.2975(7) 0.0507(14) Uani 0.409(2) 1 d PG A 2
H5B H 0.6414 0.8673 0.2612 0.061 Uiso 0.409(2) 1 calc PR A 2
C6B C 0.6222(7) 0.9631(4) 0.2416(6) 0.0494(16) Uani 0.409(2) 1 d PG A 2
C7B C 0.6225(7) 1.0217(3) 0.2958(8) 0.0451(13) Uani 0.409(2) 1 d PG A 2
H7B H 0.6095 1.0596 0.2584 0.054 Uiso 0.409(2) 1 calc PR A 2
C8B C 0.6422(7) 1.0239(3) 0.4058(8) 0.0454(12) Uani 0.409(2) 1 d PG A 2
C9B C 0.6616(8) 0.9674(4) 0.4617(6) 0.0426(15) Uani 0.409(2) 1 d PG A 2
H9B H 0.6748 0.9688 0.5354 0.051 Uiso 0.409(2) 1 calc PR A 2
C10B C 0.6343(13) 1.0858(9) 0.4611(14) 0.0420(14) Uani 0.409(2) 1 d P A 2
H10B H 0.6563 1.0877 0.5318 0.050 Uiso 0.409(2) 1 calc PR A 2
C12B C 0.6613(11) 1.2456(8) 0.4556(17) 0.0501(15) Uani 0.409(2) 1 d P A 2
H12C H 0.6604 1.2459 0.3771 0.060 Uiso 0.409(2) 1 calc PR A 2
H12D H 0.6390 1.2870 0.4810 0.060 Uiso 0.409(2) 1 calc PR A 2
C13B C 0.9305(9) 0.7059(6) 0.4230(14) 0.055(3) Uani 0.409(2) 1 d PD A 2
H13C H 0.9203 0.6630 0.3944 0.066 Uiso 0.409(2) 1 calc PR A 2
H13D H 0.9899 0.7062 0.4604 0.066 Uiso 0.409(2) 1 calc PR A 2
C16B C 0.9521(7) 0.9282(3) 0.3683(9) 0.044(2) Uani 0.409(2) 1 d PG A 2
C17B C 1.0374(7) 0.9383(4) 0.4187(9) 0.051(2) Uani 0.409(2) 1 d PG A 2
H17B H 1.0744 0.9033 0.4377 0.061 Uiso 0.409(2) 1 calc PR A 2
C18B C 1.0673(6) 1.0006(5) 0.4406(10) 0.057(2) Uani 0.409(2) 1 d PG A 2
C19B C 1.0120(7) 1.0528(3) 0.4121(10) 0.054(2) Uani 0.409(2) 1 d PG A 2
H19B H 1.0320 1.0945 0.4268 0.065 Uiso 0.409(2) 1 calc PR A 2
C20B C 0.9267(7) 1.0428(4) 0.3617(9) 0.045(2) Uani 0.409(2) 1 d PG A 2
C21B C 0.8968(6) 0.9804(5) 0.3398(9) 0.050(2) Uani 0.409(2) 1 d PG A 2
H21B H 0.8397 0.9737 0.3061 0.060 Uiso 0.409(2) 1 calc PR A 2
C22B C 0.8545(16) 1.1097(13) 0.326(3) 0.0420(14) Uani 0.409(2) 1 d P A 2
H22B H 0.7938 1.1067 0.2999 0.050 Uiso 0.409(2) 1 calc PR A 2
C28B C 0.8206(6) 1.0430(4) 0.6869(9) 0.046(2) Uani 0.409(2) 1 d PG A 2
C29B C 0.7340(6) 1.0383(4) 0.7364(8) 0.0424(19) Uani 0.409(2) 1 d PG A 2
H29B H 0.7004 1.0754 0.7524 0.051 Uiso 0.409(2) 1 calc PR A 2
C30B C 0.6975(5) 0.9782(4) 0.7619(8) 0.044(2) Uani 0.409(2) 1 d PGD A 2
C31B C 0.7476(6) 0.9227(4) 0.7380(9) 0.044(2) Uani 0.409(2) 1 d PG A 2
H31B H 0.7232 0.8825 0.7550 0.053 Uiso 0.409(2) 1 calc PR A 2
C32B C 0.8343(6) 0.9274(4) 0.6885(10) 0.050(2) Uani 0.409(2) 1 d PG A 2
C33B C 0.8707(5) 0.9875(5) 0.6630(10) 0.048(2) Uani 0.409(2) 1 d PG A 2
H33B H 0.9287 0.9906 0.6299 0.057 Uiso 0.409(2) 1 calc PR A 2
C37B C 0.6000(13) 1.0182(8) 0.075(2) 0.098(4) Uani 0.409(2) 1 d P A 2
H37D H 0.5908 1.0092 0.0000 0.147 Uiso 0.409(2) 1 calc PR A 2
H37E H 0.6570 1.0417 0.0849 0.147 Uiso 0.409(2) 1 calc PR A 2
H37F H 0.5489 1.0435 0.1020 0.147 Uiso 0.409(2) 1 calc PR A 2
C38B C 0.5616(11) 0.9143(7) 0.8058(13) 0.060(2) Uani 0.409(2) 1 d PD A 2
H38D H 0.4999 0.9187 0.8346 0.090 Uiso 0.409(2) 1 calc PR A 2
H38E H 0.5979 0.8874 0.8528 0.090 Uiso 0.409(2) 1 calc PR A 2
H38F H 0.5585 0.8951 0.7352 0.090 Uiso 0.409(2) 1 calc PR A 2
C39B C 1.1841(15) 1.0661(10) 0.5237(17) 0.060(2) Uani 0.409(2) 1 d P A 2
H39D H 1.2425 1.0608 0.5604 0.090 Uiso 0.409(2) 1 calc PR A 2
H39E H 1.1407 1.0873 0.5707 0.090 Uiso 0.409(2) 1 calc PR A 2
H39F H 1.1932 1.0916 0.4597 0.090 Uiso 0.409(2) 1 calc PR A 2
O2 O 1.14834(15) 1.00416(11) 0.4940(6) 0.0591(7) Uani 1 1 d . . .
N1 N 0.85520(18) 0.72268(13) 0.4994(7) 0.0598(10) Uani 1 1 d . . .
N2 N 0.75865(18) 1.23430(13) 0.4954(7) 0.0543(8) Uani 1 1 d . . .
C1 C 0.7657(2) 0.6956(2) 0.5141(12) 0.101(3) Uani 1 1 d . A .
H1A H 0.7613 0.6804 0.5882 0.121 Uiso 1 1 calc R . .
H1B H 0.7608 0.6581 0.4674 0.121 Uiso 1 1 calc R . .
C2 C 0.6843(2) 0.73792(17) 0.4926(10) 0.0709(13) Uani 1 1 d . . .
H2A H 0.6885 0.7539 0.4190 0.085 Uiso 0.591(2) 1 calc PR A 1
H2B H 0.6280 0.7123 0.4978 0.085 Uiso 0.591(2) 1 calc PR A 1
H2C H 0.6403 0.7088 0.4585 0.085 Uiso 0.409(2) 1 d PR A 2
H2D H 0.6585 0.7468 0.5636 0.085 Uiso 0.409(2) 1 d PR A 2
C11 C 0.5990(2) 1.19248(15) 0.4976(8) 0.0506(9) Uani 1 1 d . . .
H11A H 0.5347 1.2065 0.4998 0.061 Uiso 0.591(2) 1 calc PR A 1
H11B H 0.6143 1.1827 0.4229 0.061 Uiso 0.591(2) 1 calc PR A 1
H11C H 0.6198 1.1796 0.5691 0.061 Uiso 0.409(2) 1 d PR A 2
H11D H 0.5360 1.2088 0.5039 0.061 Uiso 0.409(2) 1 d PR A 2
C14 C 0.9324(4) 0.7569(4) 0.3261(6) 0.062(2) Uani 1 1 d . . .
H14A H 0.9600 0.7405 0.2599 0.075 Uiso 0.591(2) 1 calc PR A 1
H14B H 0.9820 0.7691 0.3752 0.075 Uiso 0.591(2) 1 calc PR A 1
H14C H 0.9812 0.7365 0.2840 0.075 Uiso 0.409(2) 1 d PR A 2
H14D H 0.8839 0.7688 0.2753 0.075 Uiso 0.409(2) 1 d PR A 2
C15 C 0.9076(5) 0.8667(4) 0.3313(6) 0.067(2) Uani 1 1 d . . .
H15A H 0.9674 0.8716 0.2957 0.080 Uiso 0.591(2) 1 calc PR A 1
H15B H 0.9184 0.8655 0.4088 0.080 Uiso 0.591(2) 1 calc PR A 1
H15C H 0.8987 0.8681 0.2535 0.080 Uiso 0.409(2) 1 d PR A 2
H15D H 0.8472 0.8616 0.3652 0.080 Uiso 0.409(2) 1 d PR A 2
C23 C 0.8528(6) 1.2171(4) 0.3344(10) 0.114(4) Uani 1 1 d . . .
H23A H 0.8661 1.2392 0.2669 0.136 Uiso 0.591(2) 1 calc PR A 1
H23B H 0.9116 1.2096 0.3708 0.136 Uiso 0.591(2) 1 calc PR A 1
H23C H 0.9048 1.2446 0.3146 0.136 Uiso 0.409(2) 1 d PR A 2
H23D H 0.8154 1.2137 0.2693 0.136 Uiso 0.409(2) 1 d PR A 2
H24 C 0.7966(7) 1.2582(3) 0.4008(5) 0.087(3) Uani 1 1 d . A .
H24A H 0.8341 1.2954 0.4199 0.105 Uiso 1 1 calc R . .
H24B H 0.7457 1.2738 0.3564 0.105 Uiso 1 1 calc R . .
C25 C 0.8068(6) 1.2580(4) 0.5928(6) 0.083(3) Uani 1 1 d . A .
H25A H 0.8610 1.2824 0.5701 0.100 Uiso 1 1 calc R . .
H25B H 0.7656 1.2874 0.6303 0.100 Uiso 1 1 calc R . .
C26 C 0.8366(6) 1.2098(5) 0.6682(7) 0.101(4) Uani 1 1 d . . .
H26A H 0.8650 1.2327 0.7281 0.122 Uiso 0.591(2) 1 calc PR A 1
H26B H 0.7804 1.1900 0.6963 0.122 Uiso 0.591(2) 1 calc PR A 1
H26C H 0.9034 1.2070 0.6575 0.122 Uiso 0.409(2) 1 d PR A 2
H26D H 0.8281 1.2291 0.7389 0.122 Uiso 0.409(2) 1 d PR A 2
C27 C 0.8651(5) 1.1014(4) 0.6563(5) 0.0584(18) Uani 1 1 d . . .
H27A H 0.8083 1.0981 0.6142 0.070 Uiso 0.591(2) 1 calc PR A 1
H27B H 0.8478 1.0972 0.7319 0.070 Uiso 0.591(2) 1 calc PR A 1
H27C H 0.8779 1.0989 0.5793 0.070 Uiso 0.409(2) 1 d PR A 2
H27D H 0.9247 1.1037 0.6930 0.070 Uiso 0.409(2) 1 d PR A 2
C34 C 0.9083(6) 0.8662(4) 0.6544(6) 0.076(3) Uani 1 1 d . . .
H34A H 0.8921 0.8668 0.7306 0.091 Uiso 0.591(2) 1 calc PR A 1
H34B H 0.8515 0.8608 0.6129 0.091 Uiso 0.591(2) 1 calc PR A 1
H34C H 0.9156 0.8625 0.5766 0.091 Uiso 0.409(2) 1 d PR A 2
H34D H 0.9690 0.8730 0.6868 0.091 Uiso 0.409(2) 1 d PR A 2
C35 C 0.9309(5) 0.7531(4) 0.6654(6) 0.071(2) Uani 1 1 d . . .
H35A H 0.8725 0.7619 0.7018 0.085 Uiso 0.591(2) 1 calc PR A 1
H35B H 0.9722 0.7337 0.7183 0.085 Uiso 0.591(2) 1 calc PR A 1
H35C H 0.9925 0.7700 0.6505 0.085 Uiso 0.409(2) 1 d PR A 2
H35D H 0.9367 0.7286 0.7320 0.085 Uiso 0.409(2) 1 d PR A 2


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
O1A C18A 1.343(11) . ?
O1A C37A 1.457(14) . ?
O3A C6A 1.397(9) . ?
O3A C38A 1.409(13) . ?
N3A C10A 1.269(14) . ?
N3A C11 1.434(10) . ?
N3A H11C 0.9471 . ?
N4A C27 1.282(10) . ?
N4A C26 1.423(11) . ?
N4A H26C 1.0336 . ?
N4A H27C 1.4866 . ?
N4A H27D 1.3482 . ?
N5A C23 1.344(12) . ?
N5A C22A 1.482(17) . ?
N5A H23D 1.2328 . ?
N6A C3A 1.26(3) . ?
N6A C2 1.478(12) . ?
N6A H2D 1.0022 . ?
N7A C15 1.261(12) . ?
N7A C14 1.523(12) . ?
N7A H14D 1.0243 . ?
N7A H15C 1.3225 . ?
N7A H15D 1.2959 . ?
N8A C35 1.427(11) . ?
N8A C34 1.438(12) . ?
N8A H34C 1.4679 . ?
N8A H34D 1.4072 . ?
N8A H35C 0.9760 . ?
C3A C4A 1.52(2) . ?
C3A H3A 0.9300 . ?
C4A C5A 1.3900 . ?
C4A C9A 1.3900 . ?
C5A C6A 1.3900 . ?
C5A H5A 0.9300 . ?
C6A C7A 1.3900 . ?
C7A C8A 1.3900 . ?
C7A H7A 0.9300 . ?
C8A C9A 1.3900 . ?
C8A C10A 1.482(12) . ?
C9A H9A 0.9300 . ?
C10A H10A 0.9300 . ?
C12A C11 1.476(12) . ?
C12A N2 1.532(11) . ?
C12A H12A 0.9700 . ?
C12A H12B 0.9700 . ?
C12A H11C 1.5426 . ?
C13A C14 1.415(11) . ?
C13A N1 1.598(12) . ?
C13A H13A 0.9700 . ?
C13A H13B 0.9700 . ?
C16A C17A 1.3900 . ?
C16A C21A 1.3900 . ?
C16A C15 1.636(9) . ?
C17A C18A 1.3900 . ?
C17A H17A 0.9300 . ?
C18A C19A 1.3900 . ?
C19A C20A 1.3900 . ?
C19A H19A 0.9300 . ?
C20A C21A 1.3900 . ?
C20A C22A 1.43(2) . ?
C21A H21A 0.9300 . ?
C22A H22A 0.9300 . ?
C28A C33A 1.402(11) . ?
C28A C29A 1.413(10) . ?
C28A C27 1.542(11) . ?
C28A H27C 1.4752 . ?
C28A H27D 1.4973 . ?
C29A C30A 1.403(10) . ?
C29A H29A 0.9300 . ?
C30A O2 1.345(9) . ?
C30A C31A 1.378(10) . ?
C31A C32A 1.382(10) . ?
C31A H31A 0.9300 . ?
C32A C33A 1.380(12) . ?
C32A C34 1.463(11) . ?
C32A H34C 1.5596 . ?
C32A H34D 1.3754 . ?
C33A H33A 0.9300 . ?
C37A H37A 0.9600 . ?
C37A H37B 0.9600 . ?
C37A H37C 0.9600 . ?
C38A H38A 0.9600 . ?
C38A H38B 0.9600 . ?
C38A H38C 0.9600 . ?
C39A O2 1.471(14) . ?
C39A H39A 0.9600 . ?
C39A H39B 0.9600 . ?
C39A H39C 0.9600 . ?
C36 N1 1.352(10) . ?
C36 C35 1.469(12) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
O1B C6B 1.32(2) . ?
O1B C37B 1.50(3) . ?
O3B C30B 1.403(11) . ?
O3B C38B 1.458(14) . ?
N3B C10B 1.27(2) . ?
N3B C11 1.473(15) . ?
N4B C26 1.090(15) . ?
N4B C27 1.405(15) . ?
N5B C22B 1.06(3) . ?
N5B C23 1.442(16) . ?
N6B C3B 1.27(4) . ?
N6B C2 1.333(15) . ?
N7B C14 1.290(14) . ?
N7B C15 1.514(15) . ?
N8B C34 1.316(15) . ?
N8B C35 1.601(16) . ?
C3B C4B 1.45(4) . ?
C3B H3B 0.9300 . ?
C4B C5B 1.3900 . ?
C4B C9B 1.3900 . ?
C5B C6B 1.3900 . ?
C5B H5B 0.9300 . ?
C6B C7B 1.3900 . ?
C7B C8B 1.3900 . ?
C7B H7B 0.9300 . ?
C8B C9B 1.3900 . ?
C8B C10B 1.460(19) . ?
C9B H9B 0.9300 . ?
C10B H10B 0.9300 . ?
C12B N2 1.501(18) . ?
C12B C11 1.511(17) . ?
C12B H12C 0.9700 . ?
C12B H12D 0.9700 . ?
C13B N1 1.478(16) . ?
C13B C14 1.599(17) . ?
C13B H13C 0.9700 . ?
C13B H13D 0.9700 . ?
C16B C17B 1.3900 . ?
C16B C21B 1.3900 . ?
C16B C15 1.498(10) . ?
C17B C18B 1.3900 . ?
C17B H17B 0.9300 . ?
C18B O2 1.340(8) . ?
C18B C19B 1.3900 . ?
C19B C20B 1.3900 . ?
C19B H19B 0.9300 . ?
C20B C21B 1.3900 . ?
C20B C22B 1.79(2) . ?
C21B H21B 0.9300 . ?
C22B H22B 0.9300 . ?
C28B C29B 1.3900 . ?
C28B C33B 1.3900 . ?
C28B C27 1.422(11) . ?
C29B C30B 1.3900 . ?
C29B H29B 0.9300 . ?
C30B C31B 1.3900 . ?
C31B C32B 1.3900 . ?
C31B H31B 0.9300 . ?
C32B C33B 1.3900 . ?
C32B C34 1.710(11) . ?
C33B H33B 0.9300 . ?
C37B H37D 0.9600 . ?
C37B H37E 0.9600 . ?
C37B H37F 0.9600 . ?
C38B H38D 0.9600 . ?
C38B H38E 0.9600 . ?
C38B H38F 0.9600 . ?
C39B O2 1.43(2) . ?
C39B H39D 0.9600 . ?
C39B H39E 0.9600 . ?
C39B H39F 0.9600 . ?
N1 C1 1.415(5) . ?
N2 H24 1.382(9) . ?
N2 C25 1.474(10) . ?
C1 C2 1.488(6) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 H11C 0.9700 . ?
C11 H11D 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 H14C 0.9700 . ?
C14 H14D 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 H15C 0.9700 . ?
C15 H15D 0.9700 . ?
C23 H24 1.433(11) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C23 H23C 0.9700 . ?
C23 H23D 0.9700 . ?
H24 H24A 0.9700 . ?
H24 H24B 0.9700 . ?
C25 C26 1.432(12) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 H26C 0.9700 . ?
C26 H26D 0.9700 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 H27C 0.9700 . ?
C27 H27D 0.9700 . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C34 H34C 0.9700 . ?
C34 H34D 0.9700 . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C35 H35C 0.9700 . ?
C35 H35D 0.9700 . ?

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
C18A O1A C37A 121.5(10) . . ?
C6A O3A C38A 117.0(8) . . ?
C10A N3A C11 120.3(9) . . ?
C10A N3A H11C 143.4 . . ?
C11 N3A H11C 42.2 . . ?
C27 N4A C26 115.7(8) . . ?
C27 N4A H26C 155.0 . . ?
C26 N4A H26C 43.0 . . ?
C27 N4A H27C 40.2 . . ?
C26 N4A H27C 128.3 . . ?
H26C N4A H27C 157.1 . . ?
C27 N4A H27D 43.2 . . ?
C26 N4A H27D 134.8 . . ?
H26C N4A H27D 136.0 . . ?
H27C N4A H27D 66.6 . . ?
C23 N5A C22A 116.4(11) . . ?
C23 N5A H23D 44.0 . . ?
C22A N5A H23D 142.8 . . ?
C3A N6A C2 113.7(12) . . ?
C3A N6A H2D 147.5 . . ?
C2 N6A H2D 40.6 . . ?
C15 N7A C14 111.7(8) . . ?
C15 N7A H14D 144.1 . . ?
C14 N7A H14D 38.9 . . ?
C15 N7A H15C 44.0 . . ?
C14 N7A H15C 124.8 . . ?
H14D N7A H15C 125.4 . . ?
C15 N7A H15D 44.6 . . ?
C14 N7A H15D 128.5 . . ?
H14D N7A H15D 160.1 . . ?
H15C N7A H15D 73.7 . . ?
C35 N8A C34 111.9(8) . . ?
C35 N8A H34C 122.1 . . ?
C34 N8A H34C 39.0 . . ?
C35 N8A H34D 129.4 . . ?
C34 N8A H34D 39.8 . . ?
H34C N8A H34D 66.6 . . ?
C35 N8A H35C 42.7 . . ?
C34 N8A H35C 149.9 . . ?
H34C N8A H35C 157.1 . . ?
H34D N8A H35C 135.3 . . ?
N6A C3A C4A 119.2(14) . . ?
N6A C3A H3A 120.4 . . ?
C4A C3A H3A 120.4 . . ?
C5A C4A C9A 120.0 . . ?
C5A C4A C3A 122.9(9) . . ?
C9A C4A C3A 117.0(9) . . ?
C4A C5A C6A 120.0 . . ?
C4A C5A H5A 120.0 . . ?
C6A C5A H5A 120.0 . . ?
C7A C6A C5A 120.0 . . ?
C7A C6A O3A 124.5(5) . . ?
C5A C6A O3A 115.4(5) . . ?
C6A C7A C8A 120.0 . . ?
C6A C7A H7A 120.0 . . ?
C8A C7A H7A 120.0 . . ?
C9A C8A C7A 120.0 . . ?
C9A C8A C10A 118.1(6) . . ?
C7A C8A C10A 121.7(6) . . ?
C8A C9A C4A 120.0 . . ?
C8A C9A H9A 120.0 . . ?
C4A C9A H9A 120.0 . . ?
N3A C10A C8A 119.8(10) . . ?
N3A C10A H10A 120.1 . . ?
C8A C10A H10A 120.1 . . ?
C11 C12A N2 109.2(8) . . ?
C11 C12A H12A 109.8 . . ?
N2 C12A H12A 109.8 . . ?
C11 C12A H12B 109.8 . . ?
N2 C12A H12B 109.8 . . ?
H12A C12A H12B 108.3 . . ?
C11 C12A H11C 37.4 . . ?
N2 C12A H11C 106.9 . . ?
H12A C12A H11C 76.3 . . ?
H12B C12A H11C 138.3 . . ?
C14 C13A N1 113.0(7) . . ?
C14 C13A H13A 109.0 . . ?
N1 C13A H13A 109.0 . . ?
C14 C13A H13B 109.0 . . ?
N1 C13A H13B 109.0 . . ?
H13A C13A H13B 107.8 . . ?
C17A C16A C21A 120.0 . . ?
C17A C16A C15 123.0(5) . . ?
C21A C16A C15 117.0(5) . . ?
C16A C17A C18A 120.0 . . ?
C16A C17A H17A 120.0 . . ?
C18A C17A H17A 120.0 . . ?
O1A C18A C19A 115.8(6) . . ?
O1A C18A C17A 124.1(6) . . ?
C19A C18A C17A 120.0 . . ?
C20A C19A C18A 120.0 . . ?
C20A C19A H19A 120.0 . . ?
C18A C19A H19A 120.0 . . ?
C21A C20A C19A 120.0 . . ?
C21A C20A C22A 112.2(7) . . ?
C19A C20A C22A 127.7(7) . . ?
C20A C21A C16A 120.0 . . ?
C20A C21A H21A 120.0 . . ?
C16A C21A H21A 120.0 . . ?
C20A C22A N5A 112.2(12) . . ?
C20A C22A H22A 123.9 . . ?
N5A C22A H22A 123.9 . . ?
C33A C28A C29A 117.3(7) . . ?
C33A C28A C27 121.7(7) . . ?
C29A C28A C27 120.9(7) . . ?
C33A C28A H27C 131.8 . . ?
C29A C28A H27C 97.2 . . ?
C27 C28A H27C 37.4 . . ?
C33A C28A H27D 133.2 . . ?
C29A C28A H27D 99.9 . . ?
C27 C28A H27D 37.2 . . ?
H27C C28A H27D 63.3 . . ?
C30A C29A C28A 119.4(7) . . ?
C30A C29A H29A 120.3 . . ?
C28A C29A H29A 120.3 . . ?
O2 C30A C31A 118.1(7) . . ?
O2 C30A C29A 121.2(7) . . ?
C31A C30A C29A 120.8(7) . . ?
C30A C31A C32A 121.0(7) . . ?
C30A C31A H31A 119.5 . . ?
C32A C31A H31A 119.5 . . ?
C33A C32A C31A 118.2(8) . . ?
C33A C32A C34 112.5(8) . . ?
C31A C32A C34 129.0(9) . . ?
C33A C32A H34C 124.0 . . ?
C31A C32A H34C 103.8 . . ?
C34 C32A H34C 37.3 . . ?
C33A C32A H34D 129.0 . . ?
C31A C32A H34D 104.5 . . ?
C34 C32A H34D 39.8 . . ?
H34C C32A H34D 64.7 . . ?
C32A C33A C28A 123.0(8) . . ?
C32A C33A H33A 118.5 . . ?
C28A C33A H33A 118.5 . . ?
O1A C37A H37A 109.5 . . ?
O1A C37A H37B 109.5 . . ?
H37A C37A H37B 109.5 . . ?
O1A C37A H37C 109.5 . . ?
H37A C37A H37C 109.5 . . ?
H37B C37A H37C 109.5 . . ?
O3A C38A H38A 109.5 . . ?
O3A C38A H38B 109.5 . . ?
H38A C38A H38B 109.5 . . ?
O3A C38A H38C 109.5 . . ?
H38A C38A H38C 109.5 . . ?
H38B C38A H38C 109.5 . . ?
O2 C39A H39A 109.5 . . ?
O2 C39A H39B 109.5 . . ?
H39A C39A H39B 109.5 . . ?
O2 C39A H39C 109.5 . . ?
H39A C39A H39C 109.5 . . ?
H39B C39A H39C 109.5 . . ?
N1 C36 C35 117.0(7) . . ?
N1 C36 H36A 108.0 . . ?
C35 C36 H36A 108.0 . . ?
N1 C36 H36B 108.0 . . ?
C35 C36 H36B 108.0 . . ?
H36A C36 H36B 107.3 . . ?
C6B O1B C37B 114.3(15) . . ?
C30B O3B C38B 115.6(10) . . ?
C10B N3B C11 114.9(13) . . ?
C26 N4B C27 133.0(12) . . ?
C22B N5B C23 126.0(16) . . ?
C3B N6B C2 128.2(18) . . ?
C14 N7B C15 110.6(11) . . ?
C34 N8B C35 108.5(10) . . ?
N6B C3B C4B 129(2) . . ?
N6B C3B H3B 115.6 . . ?
C4B C3B H3B 115.6 . . ?
C5B C4B C9B 120.0 . . ?
C5B C4B C3B 120.5(13) . . ?
C9B C4B C3B 119.4(13) . . ?
C6B C5B C4B 120.0 . . ?
C6B C5B H5B 120.0 . . ?
C4B C5B H5B 120.0 . . ?
O1B C6B C5B 115.5(10) . . ?
O1B C6B C7B 124.5(10) . . ?
C5B C6B C7B 120.0 . . ?
C8B C7B C6B 120.0 . . ?
C8B C7B H7B 120.0 . . ?
C6B C7B H7B 120.0 . . ?
C9B C8B C7B 120.0 . . ?
C9B C8B C10B 121.8(9) . . ?
C7B C8B C10B 118.1(9) . . ?
C8B C9B C4B 120.0 . . ?
C8B C9B H9B 120.0 . . ?
C4B C9B H9B 120.0 . . ?
N3B C10B C8B 126.6(15) . . ?
N3B C10B H10B 116.7 . . ?
C8B C10B H10B 116.7 . . ?
N2 C12B C11 109.0(12) . . ?
N2 C12B H12C 109.9 . . ?
C11 C12B H12C 109.9 . . ?
N2 C12B H12D 109.9 . . ?
C11 C12B H12D 109.9 . . ?
H12C C12B H12D 108.3 . . ?
N1 C13B C14 109.6(8) . . ?
N1 C13B H13C 109.8 . . ?
C14 C13B H13C 109.8 . . ?
N1 C13B H13D 109.8 . . ?
C14 C13B H13D 109.8 . . ?
H13C C13B H13D 108.2 . . ?
C17B C16B C21B 120.0 . . ?
C17B C16B C15 129.8(7) . . ?
C21B C16B C15 110.1(7) . . ?
C16B C17B C18B 120.0 . . ?
C16B C17B H17B 120.0 . . ?
C18B C17B H17B 120.0 . . ?
O2 C18B C19B 125.3(7) . . ?
O2 C18B C17B 114.6(7) . . ?
C19B C18B C17B 120.0 . . ?
C18B C19B C20B 120.0 . . ?
C18B C19B H19B 120.0 . . ?
C20B C19B H19B 120.0 . . ?
C21B C20B C19B 120.0 . . ?
C21B C20B C22B 119.6(12) . . ?
C19B C20B C22B 120.4(12) . . ?
C20B C21B C16B 120.0 . . ?
C20B C21B H21B 120.0 . . ?
C16B C21B H21B 120.0 . . ?
N5B C22B C20B 109.5(18) . . ?
N5B C22B H22B 125.2 . . ?
C20B C22B H22B 125.2 . . ?
C29B C28B C33B 120.0 . . ?
C29B C28B C27 125.4(7) . . ?
C33B C28B C27 114.6(7) . . ?
C28B C29B C30B 120.0 . . ?
C28B C29B H29B 120.0 . . ?
C30B C29B H29B 120.0 . . ?
C31B C30B C29B 120.0 . . ?
C31B C30B O3B 123.6(7) . . ?
C29B C30B O3B 115.9(7) . . ?
C30B C31B C32B 120.0 . . ?
C30B C31B H31B 120.0 . . ?
C32B C31B H31B 120.0 . . ?
C33B C32B C31B 120.0 . . ?
C33B C32B C34 112.1(6) . . ?
C31B C32B C34 127.9(6) . . ?
C32B C33B C28B 120.0 . . ?
C32B C33B H33B 120.0 . . ?
C28B C33B H33B 120.0 . . ?
O1B C37B H37D 109.5 . . ?
O1B C37B H37E 109.5 . . ?
H37D C37B H37E 109.5 . . ?
O1B C37B H37F 109.5 . . ?
H37D C37B H37F 109.5 . . ?
H37E C37B H37F 109.5 . . ?
O3B C38B H38D 109.5 . . ?
O3B C38B H38E 109.5 . . ?
H38D C38B H38E 109.5 . . ?
O3B C38B H38F 109.5 . . ?
H38D C38B H38F 109.5 . . ?
H38E C38B H38F 109.5 . . ?
O2 C39B H39D 109.5 . . ?
O2 C39B H39E 109.5 . . ?
H39D C39B H39E 109.5 . . ?
O2 C39B H39F 109.5 . . ?
H39D C39B H39F 109.5 . . ?
H39E C39B H39F 109.5 . . ?
C18B O2 C30A 57.4(5) . . ?
C18B O2 C39B 119.2(10) . . ?
C30A O2 C39B 106.5(10) . . ?
C18B O2 C39A 96.9(8) . . ?
C30A O2 C39A 118.6(7) . . ?
C39B O2 C39A 34.6(6) . . ?
C36 N1 C1 110.8(9) . . ?
C36 N1 C13B 87.7(6) . . ?
C1 N1 C13B 130.8(8) . . ?
C36 N1 C13A 124.1(7) . . ?
C1 N1 C13A 102.6(7) . . ?
C13B N1 C13A 37.8(6) . . ?
H24 N2 C25 112.7(3) . . ?
H24 N2 C12B 92.0(9) . . ?
C25 N2 C12B 130.8(9) . . ?
H24 N2 C12A 125.8(8) . . ?
C25 N2 C12A 97.2(7) . . ?
C12B N2 C12A 37.8(4) . . ?
N1 C1 C2 117.2(5) . . ?
N1 C1 H1A 108.0 . . ?
C2 C1 H1A 108.0 . . ?
N1 C1 H1B 108.0 . . ?
C2 C1 H1B 108.0 . . ?
H1A C1 H1B 107.2 . . ?
N6B C2 N6A 70.1(5) . . ?
N6B C2 C1 134.7(8) . . ?
N6A C2 C1 114.5(8) . . ?
N6B C2 H2A 39.6 . . ?
N6A C2 H2A 108.6 . . ?
C1 C2 H2A 108.6 . . ?
N6B C2 H2B 111.9 . . ?
N6A C2 H2B 108.6 . . ?
C1 C2 H2B 108.6 . . ?
H2A C2 H2B 107.6 . . ?
N6B C2 H2C 101.4 . . ?
N6A C2 H2C 134.6 . . ?
C1 C2 H2C 102.8 . . ?
H2A C2 H2C 81.2 . . ?
H2B C2 H2C 31.2 . . ?
N6B C2 H2D 105.2 . . ?
N6A C2 H2D 42.3 . . ?
C1 C2 H2D 104.5 . . ?
H2A C2 H2D 143.9 . . ?
H2B C2 H2D 74.1 . . ?
H2C C2 H2D 105.2 . . ?
N3A C11 N3B 72.3(4) . . ?
N3A C11 C12A 113.5(8) . . ?
N3B C11 C12A 140.6(8) . . ?
N3A C11 C12B 137.7(8) . . ?
N3B C11 C12B 110.1(11) . . ?
C12A C11 C12B 38.4(5) . . ?
N3A C11 H11A 108.9 . . ?
N3B C11 H11A 105.1 . . ?
C12A C11 H11A 108.9 . . ?
C12B C11 H11A 110.8 . . ?
N3A C11 H11B 108.9 . . ?
N3B C11 H11B 40.1 . . ?
C12A C11 H11B 108.9 . . ?
C12B C11 H11B 72.1 . . ?
H11A C11 H11B 107.7 . . ?
N3A C11 H11C 41.0 . . ?
N3B C11 H11C 110.9 . . ?
C12A C11 H11C 75.0 . . ?
C12B C11 H11C 109.4 . . ?
H11A C11 H11C 110.5 . . ?
H11B C11 H11C 137.7 . . ?
N3A C11 H11D 109.5 . . ?
N3B C11 H11D 109.4 . . ?
C12A C11 H11D 105.0 . . ?
C12B C11 H11D 109.0 . . ?
H11A C11 H11D 4.3 . . ?
H11B C11 H11D 111.1 . . ?
H11C C11 H11D 108.1 . . ?
N7B C14 C13A 133.5(11) . . ?
N7B C14 N7A 68.3(8) . . ?
C13A C14 N7A 107.0(6) . . ?
N7B C14 C13B 108.8(10) . . ?
C13A C14 C13B 38.2(6) . . ?
N7A C14 C13B 131.3(8) . . ?
N7B C14 H14A 114.5 . . ?
C13A C14 H14A 110.3 . . ?
N7A C14 H14A 110.3 . . ?
C13B C14 H14A 114.0 . . ?
N7B C14 H14B 43.3 . . ?
C13A C14 H14B 110.3 . . ?
N7A C14 H14B 110.3 . . ?
C13B C14 H14B 73.6 . . ?
H14A C14 H14B 108.6 . . ?
N7B C14 H14C 105.0 . . ?
C13A C14 H14C 110.0 . . ?
N7A C14 H14C 131.2 . . ?
C13B C14 H14C 97.2 . . ?
H14A C14 H14C 25.8 . . ?
H14B C14 H14C 85.3 . . ?
N7B C14 H14D 106.7 . . ?
C13A C14 H14D 91.8 . . ?
N7A C14 H14D 41.5 . . ?
C13B C14 H14D 129.9 . . ?
H14A C14 H14D 80.7 . . ?
H14B C14 H14D 150.0 . . ?
H14C C14 H14D 106.5 . . ?
N7A C15 C16B 179.1(10) . . ?
N7A C15 N7B 69.3(8) . . ?
C16B C15 N7B 110.1(8) . . ?
N7A C15 C16A 111.1(7) . . ?
C16B C15 C16A 69.5(5) . . ?
N7B C15 C16A 178.8(9) . . ?
N7A C15 H15A 109.4 . . ?
C16B C15 H15A 70.9 . . ?
N7B C15 H15A 71.3 . . ?
C16A C15 H15A 109.4 . . ?
N7A C15 H15B 109.4 . . ?
C16B C15 H15B 69.7 . . ?
N7B C15 H15B 69.5 . . ?
C16A C15 H15B 109.4 . . ?
H15A C15 H15B 108.0 . . ?
N7A C15 H15C 71.4 . . ?
C16B C15 H15C 109.5 . . ?
N7B C15 H15C 109.8 . . ?
C16A C15 H15C 71.4 . . ?
H15A C15 H15C 70.4 . . ?
H15B C15 H15C 178.4 . . ?
N7A C15 H15D 69.6 . . ?
C16B C15 H15D 110.1 . . ?
N7B C15 H15D 109.1 . . ?
C16A C15 H15D 70.2 . . ?
H15A C15 H15D 178.5 . . ?
H15B C15 H15D 73.4 . . ?
H15C C15 H15D 108.2 . . ?
N5A C23 H24 113.9(8) . . ?
N5A C23 N5B 49.8(7) . . ?
H24 C23 N5B 138.6(10) . . ?
N5A C23 H23A 108.8 . . ?
H24 C23 H23A 108.8 . . ?
N5B C23 H23A 112.6 . . ?
N5A C23 H23B 108.8 . . ?
H24 C23 H23B 108.8 . . ?
N5B C23 H23B 60.1 . . ?
H23A C23 H23B 107.7 . . ?
N5A C23 H23C 142.3 . . ?
H24 C23 H23C 103.2 . . ?
N5B C23 H23C 104.6 . . ?
H23A C23 H23C 49.8 . . ?
H23B C23 H23C 62.7 . . ?
N5A C23 H23D 61.9 . . ?
H24 C23 H23D 101.9 . . ?
N5B C23 H23D 99.8 . . ?
H23A C23 H23D 55.3 . . ?
H23B C23 H23D 148.8 . . ?
H23C C23 H23D 105.1 . . ?
N2 H24 C23 119.5(6) . . ?
N2 H24 H24A 107.4 . . ?
C23 H24 H24A 107.4 . . ?
N2 H24 H24B 107.4 . . ?
C23 H24 H24B 107.4 . . ?
H24A H24 H24B 107.0 . . ?
C26 C25 N2 116.0(6) . . ?
C26 C25 H25A 108.3 . . ?
N2 C25 H25A 108.3 . . ?
C26 C25 H25B 108.3 . . ?
N2 C25 H25B 108.3 . . ?
H25A C25 H25B 107.4 . . ?
N4B C26 N4A 56.9(8) . . ?
N4B C26 C25 130.7(10) . . ?
N4A C26 C25 124.5(9) . . ?
N4B C26 H26A 120.9 . . ?
N4A C26 H26A 106.2 . . ?
C25 C26 H26A 106.2 . . ?
N4B C26 H26B 49.4 . . ?
N4A C26 H26B 106.2 . . ?
C25 C26 H26B 106.2 . . ?
H26A C26 H26B 106.4 . . ?
N4B C26 H26C 102.1 . . ?
N4A C26 H26C 46.6 . . ?
C25 C26 H26C 104.4 . . ?
H26A C26 H26C 73.6 . . ?
H26B C26 H26C 148.0 . . ?
N4B C26 H26D 106.8 . . ?
N4A C26 H26D 126.2 . . ?
C25 C26 H26D 105.0 . . ?
H26A C26 H26D 33.0 . . ?
H26B C26 H26D 75.2 . . ?
H26C C26 H26D 105.8 . . ?
N4A C27 N4B 54.4(7) . . ?
N4A C27 C28B 170.3(8) . . ?
N4B C27 C28B 117.6(9) . . ?
N4A C27 C28A 118.4(7) . . ?
N4B C27 C28A 172.6(9) . . ?
C28B C27 C28A 69.8(6) . . ?
N4A C27 H27A 107.7 . . ?
N4B C27 H27A 74.9 . . ?
C28B C27 H27A 72.8 . . ?
C28A C27 H27A 107.7 . . ?
N4A C27 H27B 107.7 . . ?
N4B C27 H27B 77.6 . . ?
C28B C27 H27B 63.4 . . ?
C28A C27 H27B 107.7 . . ?
H27A C27 H27B 107.1 . . ?
N4A C27 H27C 81.3 . . ?
N4B C27 H27C 107.9 . . ?
C28B C27 H27C 107.5 . . ?
C28A C27 H27C 67.5 . . ?
H27A C27 H27C 68.4 . . ?
H27B C27 H27C 170.9 . . ?
N4A C27 H27D 72.0 . . ?
N4B C27 H27D 108.1 . . ?
C28B C27 H27D 108.3 . . ?
C28A C27 H27D 68.9 . . ?
H27A C27 H27D 175.3 . . ?
H27B C27 H27D 77.3 . . ?
H27C C27 H27D 107.1 . . ?
N8B C34 N8A 73.3(8) . . ?
N8B C34 C32A 170.7(10) . . ?
N8A C34 C32A 109.9(8) . . ?
N8B C34 C32B 104.0(9) . . ?
N8A C34 C32B 176.1(8) . . ?
C32A C34 C32B 72.3(6) . . ?
N8B C34 H34A 61.2 . . ?
N8A C34 H34A 109.7 . . ?
C32A C34 H34A 109.7 . . ?
C32B C34 H34A 66.4 . . ?
N8B C34 H34B 76.6 . . ?
N8A C34 H34B 109.7 . . ?
C32A C34 H34B 109.7 . . ?
C32B C34 H34B 72.0 . . ?
H34A C34 H34B 108.2 . . ?
N8B C34 H34C 112.5 . . ?
N8A C34 H34C 72.2 . . ?
C32A C34 H34C 76.8 . . ?
C32B C34 H34C 111.6 . . ?
H34A C34 H34C 171.4 . . ?
H34B C34 H34C 63.7 . . ?
N8B C34 H34D 109.2 . . ?
N8A C34 H34D 68.4 . . ?
C32A C34 H34D 65.2 . . ?
C32B C34 H34D 110.4 . . ?
H34A C34 H34D 79.2 . . ?
H34B C34 H34D 172.4 . . ?
H34C C34 H34D 109.0 . . ?
N8A C35 C36 117.6(8) . . ?
N8A C35 N8B 65.6(7) . . ?
C36 C35 N8B 128.5(8) . . ?
N8A C35 H35A 107.9 . . ?
C36 C35 H35A 107.9 . . ?
N8B C35 H35A 42.3 . . ?
N8A C35 H35B 107.9 . . ?
C36 C35 H35B 107.9 . . ?
N8B C35 H35B 120.0 . . ?
H35A C35 H35B 107.2 . . ?
N8A C35 H35C 43.0 . . ?
C36 C35 H35C 105.6 . . ?
N8B C35 H35C 105.0 . . ?
H35A C35 H35C 144.1 . . ?
H35B C35 H35C 73.7 . . ?
N8A C35 H35D 131.3 . . ?
C36 C35 H35D 105.4 . . ?
N8B C35 H35D 104.8 . . ?
H35A C35 H35D 77.3 . . ?
H35B C35 H35D 32.8 . . ?
H35C C35 H35D 105.8 . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        23.98
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.188
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.044
####################################################################### 
# 
# 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_Ni2LAThio-ClO4-4_lc169psq
_database_code_depnum_ccdc_archive 'CCDC 1517782'


_audit_update_record             
;
2017-01-25 deposited with the CCDC.
2017-02-06 downloaded from the CCDC.
;
# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.001 0.000 0.000 144.7 53.3
2 0.000 0.500 0.500 264.1 45.7
3 0.132 0.432 0.977 17.5 2.0
4 0.395 0.847 0.125 8.1 0.7
5 0.604 0.153 0.875 8.0 -0.4
6 0.867 0.568 0.022 17.4 3.5
_platon_squeeze_details          
;
two half molecules of disordered perchlorate anions
the given sum formula, density, mu, F000 are calculated includimg the squeezed
 ClO4-unit
;
_publcif_datablock.id            {d2728094-fd2c-4065-b2e4-50713b5107f5}

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H60 N12 Ni2 O2 S3, 4(Cl O4)'
_chemical_formula_sum            'C38 H61 Cl4 N12 Ni2 O18 S3'
_chemical_formula_weight         1329.35

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.1796(10)
_cell_length_b                   15.2919(14)
_cell_length_c                   21.793(2)
_cell_angle_alpha                101.454(8)
_cell_angle_beta                 103.465(9)
_cell_angle_gamma                102.672(8)
_cell_volume                     3105.3(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    8000
_cell_measurement_theta_min      4.3
_cell_measurement_theta_max      52.2

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_F_000             1280
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    0.897
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.733
_exptl_absorpt_correction_T_max  0.837

_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       'ω and π scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         8000
_diffrn_standards_interval_count .5
_diffrn_standards_interval_time  .5
_diffrn_reflns_number            22448
_diffrn_reflns_av_unetI/netI     0.1208
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.501
_diffrn_reflns_theta_max         26.659
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measured_fraction_theta_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_point_group_measured_fraction_full 0.972
_reflns_number_total             10966
_reflns_number_gt                6005
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_structure_solution    'SIR92 (Altomare 1994)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Diamond (Brandenburg 2011)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10966
_refine_ls_number_parameters     669
_refine_ls_number_restraints     40
_refine_ls_R_factor_all          0.1619
_refine_ls_R_factor_gt           0.1246
_refine_ls_wR_factor_ref         0.3818
_refine_ls_wR_factor_gt          0.3355
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000

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
Ni3 Ni 0.60942(12) 0.36528(9) 0.14662(7) 0.0676(4) Uani 1 1 d . . . . .
H3B H 0.567(9) 0.071(9) 0.416(4) 0.10(4) Uiso 1 1 d D . . . .
Ni4 Ni 0.91763(11) -0.03637(8) 0.30037(6) 0.0610(3) Uani 1 1 d . . . . .
S2 S 0.5659(3) 0.25817(18) 0.43563(12) 0.0730(7) Uani 1 1 d . . . . .
H6B H 0.391(6) 0.299(3) 0.076(3) 0.026(15) Uiso 1 1 d D . . . .
H5B H 0.705(9) 0.2319(17) 0.175(4) 0.06(2) Uiso 1 1 d D . . . .
S3 S 1.05860(17) 0.25675(13) 0.28352(10) 0.0509(4) Uani 1 1 d . . . . .
N3A N 0.7476(6) 0.2974(4) 0.1918(3) 0.0466(13) Uani 1 1 d D . . . .
N3C N 0.7470(6) -0.1522(4) 0.2773(3) 0.0521(14) Uani 1 1 d . . . . .
N3E N 0.4264(6) 0.2525(4) 0.0916(3) 0.0485(13) Uani 1 1 d D . . . .
N3F N 0.5188(6) 0.3560(4) 0.2243(3) 0.0467(13) Uani 1 1 d . . . . .
N3G N 0.9840(6) -0.0955(5) 0.2235(3) 0.0517(14) Uani 1 1 d . . . . .
N3H N 0.8664(6) 0.0399(5) 0.3807(3) 0.0499(13) Uani 1 1 d . . . . .
N3I N 0.7864(6) 0.0251(4) 0.2415(3) 0.0441(12) Uani 1 1 d D . . . .
H500 H 0.847040 0.079336 0.234499 0.053 Uiso 1 1 calc DR U . . .
O3J O 0.4849(7) 0.4496(5) 0.1098(4) 0.0722(18) Uani 1 1 d . . . . .
N3M N 0.7667(7) 0.4905(5) 0.1949(5) 0.066(2) Uani 1 1 d . . . . .
N3U N 0.6454(7) 0.0884(6) 0.4550(3) 0.0570(16) Uani 1 1 d D . . . .
N4J N 0.5190(11) 0.4097(6) 0.3745(5) 0.086(3) Uani 1 1 d D . . . .
H1B H 0.596588 0.394613 0.379732 0.103 Uiso 1 1 calc DR U . . .
O37 O 1.0251(6) -0.1085(4) 0.3605(3) 0.0558(13) Uani 1 1 d . . . . .
H37 H 0.966(9) -0.153(8) 0.365(5) 0.084 Uiso 1 1 calc R U . . .
C1AA C 0.9757(7) 0.2572(5) 0.2034(4) 0.0552(18) Uani 1 1 d . . . . .
C12B C 0.7257(12) 0.3592(7) 0.0233(6) 0.084 Uani 1 1 d D . . . .
N11B N 0.6826(7) 0.3587(6) 0.0662(4) 0.066(2) Uani 1 1 d . . . . .
C1G C 0.8442(11) 0.5584(7) 0.2140(7) 0.082(3) Uani 1 1 d . . . . .
C3K C 0.4225(7) 0.1683(5) 0.0447(4) 0.0505(16) Uani 1 1 d . . . . .
H3KA H 0.447372 0.185648 0.007541 0.061 Uiso 1 1 calc R U . A 1
H3KB H 0.326797 0.128309 0.028889 0.061 Uiso 1 1 calc R U . A 1
C3L C 0.7351(7) 0.3097(5) 0.2583(4) 0.0485(15) Uani 1 1 d . . . . .
H3LA H 0.787452 0.372409 0.284123 0.058 Uiso 1 1 calc R U . . .
H3LB H 0.775399 0.266817 0.278509 0.058 Uiso 1 1 calc R U . . .
C3O C 1.0721(8) 0.1325(5) 0.1912(5) 0.0560(18) Uani 1 1 d . . . . .
H3O H 1.093215 0.082288 0.167737 0.067 Uiso 1 1 calc R U . . .
C3P C 0.4274(10) 0.3951(7) 0.4143(5) 0.071(3) Uani 1 1 d . . . . .
H3PA H 0.331598 0.366172 0.386643 0.086 Uiso 1 1 calc R U . . .
H3PB H 0.430451 0.454418 0.441509 0.086 Uiso 1 1 calc R U . . .
C3Q C 0.3363(7) 0.2345(5) 0.1341(4) 0.0502(16) Uani 1 1 d . . . . .
H3QA H 0.349471 0.180615 0.149223 0.060 Uiso 1 1 calc R U . . .
H3QB H 0.238726 0.219907 0.108719 0.060 Uiso 1 1 calc R U . . .
C3R C 0.5500(17) -0.3042(9) 0.2526(11) 0.133(7) Uani 1 1 d . . . . .
H3RA H 0.461431 -0.293881 0.233690 0.200 Uiso 1 1 calc R U . . .
H3RB H 0.548367 -0.322140 0.292214 0.200 Uiso 1 1 calc R U . . .
H3RC H 0.565964 -0.352681 0.222226 0.200 Uiso 1 1 calc R U . . .
C3S C 0.7996(7) 0.1081(5) 0.3512(3) 0.0437(14) Uani 1 1 d . . . . .
H3SA H 0.745882 0.132709 0.378303 0.052 Uiso 1 1 calc R U . . .
H3SB H 0.872537 0.159670 0.349527 0.052 Uiso 1 1 calc R U . . .
C3T C 0.7392(9) 0.0286(6) 0.4697(4) 0.0573(18) Uani 1 1 d . . . . .
H3TA H 0.694510 -0.018693 0.487914 0.069 Uiso 1 1 calc R U . . .
H3TB H 0.826475 0.066089 0.502187 0.069 Uiso 1 1 calc R U . . .
C3V C 0.6981(9) -0.0374(6) 0.1755(4) 0.059(2) Uani 1 1 d . . . . .
H3VA H 0.623126 -0.083653 0.181197 0.070 Uiso 1 1 calc R U . B 1
H3VB H 0.755875 -0.069658 0.155536 0.070 Uiso 1 1 calc R U . B 1
C3X C 1.1122(7) 0.1609(5) 0.2578(4) 0.0489(15) Uani 1 1 d . . . . .
C3Y C 0.7044(7) 0.0586(5) 0.2832(4) 0.0457(14) Uani 1 1 d . . . . .
H3YA H 0.632414 0.006547 0.284950 0.055 Uiso 1 1 calc R U . . .
H3YB H 0.658247 0.100732 0.264985 0.055 Uiso 1 1 calc R U . . .
C4A C 0.4694(13) 0.3354(7) 0.4559(5) 0.078(3) Uani 1 1 d . . . . .
C4B C 0.9942(7) 0.1880(6) 0.1609(5) 0.0569(18) Uani 1 1 d . . . . .
H4B H 0.959601 0.176913 0.115769 0.068 Uiso 1 1 calc R U . . .
C4C C 1.0647(18) -0.1742(19) 0.1292(8) 0.180(12) Uani 1 1 d . . . . .
H4CA H 1.011157 -0.170055 0.087902 0.270 Uiso 1 1 calc R U . . .
H4CB H 1.052270 -0.238330 0.129038 0.270 Uiso 1 1 calc R U . . .
H4CC H 1.162520 -0.144638 0.136388 0.270 Uiso 1 1 calc R U . . .
C4D C 0.8936(8) 0.3237(5) 0.1899(5) 0.060(2) Uani 1 1 d . . . . .
H4DA H 0.941796 0.383175 0.221586 0.072 Uiso 1 1 calc R U . . .
H4DB H 0.893391 0.332367 0.147030 0.072 Uiso 1 1 calc R U . . .
C4F C 0.5509(10) 0.2095(7) 0.4980(5) 0.064(2) Uani 1 1 d . . . . .
C4H C 0.6616(9) -0.2196(6) 0.2669(5) 0.062(2) Uani 1 1 d . . . . .
C4I C 1.0034(8) 0.0910(6) 0.4305(4) 0.0568(18) Uani 1 1 d . . . . .
H4IA H 1.038557 0.048392 0.452987 0.068 Uiso 1 1 calc R U . . .
H4IB H 0.989123 0.139062 0.462630 0.068 Uiso 1 1 calc R U . . .
C4M C 0.6240(12) 0.1391(8) 0.5145(5) 0.072(2) Uani 1 1 d . . . . .
H4MA H 0.713916 0.169612 0.547262 0.087 Uiso 1 1 calc R U . . .
H4MB H 0.567560 0.096395 0.532106 0.087 Uiso 1 1 calc R U . . .
C4N C 0.4702(11) 0.2507(8) 0.5318(6) 0.078(3) Uani 1 1 d . . . . .
H4N H 0.444877 0.232318 0.566624 0.093 Uiso 1 1 calc R U . . .
C4O C 0.5460(9) 0.4483(5) 0.2717(4) 0.0569(18) Uani 1 1 d . . . . .
H4OA H 0.527529 0.492168 0.246436 0.068 Uiso 1 1 calc R U . . .
H4OB H 0.645344 0.469174 0.295287 0.068 Uiso 1 1 calc R U . . .
C4Q C 1.0166(10) -0.1280(8) 0.1813(5) 0.074(3) Uani 1 1 d . . . . .
C4U C 0.4640(13) 0.4547(6) 0.3220(6) 0.078(3) Uani 1 1 d . . . . .
H4UA H 0.473630 0.519419 0.341660 0.094 Uiso 1 1 calc R U . . .
H4UB H 0.365036 0.423851 0.300688 0.094 Uiso 1 1 calc R U . . .
C4V C 0.4304(12) 0.3236(7) 0.5075(6) 0.084(3) Uani 1 1 d . . . . .
H4V H 0.380834 0.359908 0.526696 0.101 Uiso 1 1 calc R U . . .
C24 C 0.9557(13) 0.6524(8) 0.2471(7) 0.092(4) Uani 1 1 d . . . . .
H24A H 1.037041 0.653041 0.231875 0.138 Uiso 1 1 calc R U . . .
H24B H 0.981982 0.661443 0.293655 0.138 Uiso 1 1 calc R U . . .
H24C H 0.917632 0.701466 0.236428 0.138 Uiso 1 1 calc R U . . .
C38 C 1.1112(8) 0.1348(6) 0.4006(4) 0.0567(18) Uani 1 1 d . . . . .
H38A H 1.089092 0.188814 0.388713 0.068 Uiso 1 1 calc R U . . .
H38B H 1.203143 0.155319 0.432595 0.068 Uiso 1 1 calc R U . . .
N39 N 1.1149(6) 0.0681(4) 0.3415(3) 0.0478(13) Uani 1 1 d . . . . .
H501 H 1.177747 0.033776 0.360111 0.057 Uiso 1 1 calc R U . . .
C41 C 0.3665(7) 0.3153(5) 0.1925(4) 0.0539(18) Uani 1 1 d . . . . .
H41A H 0.326206 0.362620 0.178739 0.065 Uiso 1 1 calc R U . . .
H41B H 0.321906 0.294555 0.223904 0.065 Uiso 1 1 calc R U . . .
C45 C 0.5825(8) 0.2927(5) 0.2579(4) 0.0510(16) Uani 1 1 d . . . . .
H45A H 0.531413 0.228602 0.235182 0.061 Uiso 1 1 calc R U . . .
H45B H 0.576520 0.304069 0.302382 0.061 Uiso 1 1 calc R U . . .
C46 C 1.1958(7) 0.1173(6) 0.3025(4) 0.0543(17) Uani 1 1 d . . . . .
H46A H 1.276991 0.165173 0.332614 0.065 Uiso 1 1 calc R U . . .
H46B H 1.230157 0.073015 0.276678 0.065 Uiso 1 1 calc R U . . .
C47 C 0.7717(8) -0.0185(6) 0.4076(4) 0.0534(17) Uani 1 1 d . . . . .
H47A H 0.811934 -0.067935 0.417117 0.064 Uiso 1 1 calc R U . . .
H47B H 0.683086 -0.047358 0.373663 0.064 Uiso 1 1 calc R U . . .
Cl50 Cl 0.1105(3) 0.3090(2) 0.58213(16) 0.0845(7) Uani 1 1 d D . . . .
O500 O -0.0272(12) 0.2878(12) 0.5897(9) 0.177(6) Uani 1 1 d D . . . .
O501 O 0.2030(14) 0.3907(8) 0.6204(8) 0.175(7) Uani 1 1 d D . . . .
O502 O 0.0965(17) 0.3155(8) 0.5146(5) 0.143(5) Uani 1 1 d D . . . .
O503 O 0.1553(11) 0.2288(6) 0.5879(5) 0.097(2) Uani 1 1 d D . . . .
Cl60 Cl 0.3399(2) 0.88186(19) 0.30737(13) 0.0729(6) Uani 1 1 d D . . . .
O600 O 0.3487(12) 0.8932(11) 0.2456(5) 0.153(6) Uani 1 1 d D . . . .
O601 O 0.4509(8) 0.8479(6) 0.3360(5) 0.102(3) Uani 1 1 d D . . . .
O602 O 0.2076(6) 0.8157(5) 0.2993(4) 0.0755(19) Uani 1 1 d D . . . .
O603 O 0.3475(7) 0.9683(5) 0.3508(4) 0.087(2) Uani 1 1 d D . . . .
Cl70 Cl 0.1646(7) 0.5143(5) 0.1511(4) 0.102(2) Uani 0.5 1 d D . P . .
O700 O 0.155(3) 0.498(2) 0.2132(10) 0.159(5) Uani 0.5 1 d D . P . .
O701 O 0.103(3) 0.5800(17) 0.1317(13) 0.159(5) Uani 0.5 1 d D . P . .
O702 O 0.3122(17) 0.535(2) 0.1572(13) 0.159(5) Uani 0.5 1 d D . P . .
O703 O 0.102(3) 0.4268(13) 0.1016(10) 0.159(5) Uani 0.5 1 d D . P . .
Cl80 Cl 0.6548(5) 0.6777(3) 0.07977(19) 0.0775(16) Uani 0.5 1 d . . P . .
O800 O 0.537700 0.738300 0.093204 0.157 Uani 0.5 1 d . . P . .
O801 O 0.732(2) 0.6870(14) 0.1398(6) 0.104(6) Uani 0.5 1 d . . P . .
O802 O 0.576(2) 0.5876(10) 0.0444(7) 0.109(7) Uani 0.5 1 d . . P . .
O803 O 0.7191(15) 0.7147(11) 0.0360(8) 0.087(5) Uani 0.5 1 d . . P . .
C805 C 0.781700 0.334549 -0.040100 0.1076(9) Uani 1 1 d D . . . .
H80A H 0.704393 0.296175 -0.076818 0.161 Uiso 1 1 calc R U . . .
H80B H 0.851477 0.301941 -0.030995 0.161 Uiso 1 1 calc R U . . .
H80C H 0.822344 0.390969 -0.050030 0.161 Uiso 1 1 calc R U . . .
S7A S 0.4942(2) 0.05539(14) 0.13068(10) 0.0478(5) Uani 0.889(4) 1 d . . P C 1
C1A C 0.6308(9) 0.1001(6) 0.0510(4) 0.0555(14) Uani 0.889(4) 1 d . . P C 1
H1A H 0.660637 0.125549 0.019563 0.067 Uiso 0.889(4) 1 calc R U P C 1
C2A C 0.6985(9) 0.0418(6) 0.0843(4) 0.0555(14) Uani 0.889(4) 1 d . . P C 1
H2A H 0.775922 0.024155 0.076159 0.067 Uiso 0.889(4) 1 calc R U P C 1
C30A C 0.5191(9) 0.1130(6) 0.0711(4) 0.0510(12) Uani 0.889(4) 1 d . . P C 1
C40A C 0.6341(8) 0.0152(5) 0.1299(3) 0.0510(12) Uani 0.889(4) 1 d . . P C 1
S7B S 0.6388(16) 0.0877(11) 0.0973(8) 0.0478(5) Uani 0.111(4) 1 d . . P C 2
C1B C 0.472(7) -0.030(4) 0.128(3) 0.0555(14) Uani 0.111(4) 1 d . . P C 2
H1BA H 0.441198 -0.078099 0.146418 0.067 Uiso 0.111(4) 1 calc R U P C 2
C2B C 0.370(7) 0.029(5) 0.087(3) 0.0555(14) Uani 0.111(4) 1 d . . P C 2
H2BA H 0.272682 0.012187 0.073903 0.067 Uiso 0.111(4) 1 calc R U P C 2
C30B C 0.460868 0.105545 0.078115 0.0510(12) Uani 0.111(4) 1 d . . P C 2
C40B C 0.6341(8) 0.0152(5) 0.1299(3) 0.0510(12) Uani 0.111(4) 1 d . . P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni3 N11B 2.051(8) . ?
Ni3 N3M 2.099(7) . ?
Ni3 N3A 2.105(6) . ?
Ni3 N3F 2.122(7) . ?
Ni3 O3J 2.138(6) . ?
Ni3 N3E 2.147(6) . ?
Ni4 N3G 2.068(7) . ?
Ni4 N3C 2.073(6) . ?
Ni4 N3I 2.133(6) . ?
Ni4 O37 2.137(5) . ?
Ni4 N39 2.138(6) . ?
Ni4 N3H 2.140(7) . ?
S2 C4F 1.696(10) . ?
S2 C4A 1.749(11) . ?
S3 C3X 1.712(8) . ?
S3 C1AA 1.755(9) . ?
N3A C3L 1.462(10) . ?
N3A C4D 1.465(9) . ?
N3A H5B 0.956(19) . ?
N3C C4H 1.137(10) . ?
N3E C3K 1.464(10) . ?
N3E C3Q 1.469(10) . ?
N3E H6B 0.950(19) . ?
N3F C41 1.476(9) . ?
N3F C45 1.492(9) . ?
N3F C4O 1.501(9) . ?
N3G C4Q 1.111(13) . ?
N3H C47 1.471(10) . ?
N3H C4I 1.488(9) . ?
N3H C3S 1.529(9) . ?
N3I C3Y 1.464(10) . ?
N3I C3V 1.505(9) . ?
N3I H500 0.9800 . ?
N3M C1G 1.091(12) . ?
N3U C4M 1.463(12) . ?
N3U C3T 1.486(10) . ?
N3U H3B 0.959(19) . ?
N4J C3P 1.426(16) . ?
N4J C4U 1.508(15) . ?
N4J H1B 0.8600 . ?
O37 H37 0.84(12) . ?
C1AA C4B 1.340(13) . ?
C1AA C4D 1.482(12) . ?
C12B N11B 1.121(13) . ?
C12B C805 1.622(12) . ?
C1G C24 1.539(14) . ?
C3K C30B 1.383(8) . ?
C3K C30A 1.518(11) . ?
C3K H3KA 0.9700 . ?
C3K H3KB 0.9700 . ?
C3L C45 1.515(10) . ?
C3L H3LA 0.9700 . ?
C3L H3LB 0.9700 . ?
C3O C3X 1.363(12) . ?
C3O C4B 1.435(12) . ?
C3O H3O 0.9300 . ?
C3P C4A 1.470(15) . ?
C3P H3PA 0.9700 . ?
C3P H3PB 0.9700 . ?
C3Q C41 1.507(11) . ?
C3Q H3QA 0.9700 . ?
C3Q H3QB 0.9700 . ?
C3R C4H 1.446(15) . ?
C3R H3RA 0.9600 . ?
C3R H3RB 0.9600 . ?
C3R H3RC 0.9600 . ?
C3S C3Y 1.508(9) . ?
C3S H3SA 0.9700 . ?
C3S H3SB 0.9700 . ?
C3T C47 1.545(12) . ?
C3T H3TA 0.9700 . ?
C3T H3TB 0.9700 . ?
C3V C40B 1.518(10) . ?
C3V C40A 1.518(10) . ?
C3V H3VA 0.9700 . ?
C3V H3VB 0.9700 . ?
C3X C46 1.497(10) . ?
C3Y H3YA 0.9700 . ?
C3Y H3YB 0.9700 . ?
C4A C4V 1.309(19) . ?
C4B H4B 0.9300 . ?
C4C C4Q 1.456(18) . ?
C4C H4CA 0.9600 . ?
C4C H4CB 0.9600 . ?
C4C H4CC 0.9600 . ?
C4D H4DA 0.9700 . ?
C4D H4DB 0.9700 . ?
C4F C4N 1.392(15) . ?
C4F C4M 1.491(13) . ?
C4I C38 1.502(12) . ?
C4I H4IA 0.9700 . ?
C4I H4IB 0.9700 . ?
C4M H4MA 0.9700 . ?
C4M H4MB 0.9700 . ?
C4N C4V 1.422(16) . ?
C4N H4N 0.9300 . ?
C4O C4U 1.526(15) . ?
C4O H4OA 0.9700 . ?
C4O H4OB 0.9700 . ?
C4U H4UA 0.9700 . ?
C4U H4UB 0.9700 . ?
C4V H4V 0.9300 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C38 N39 1.490(11) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
N39 C46 1.508(10) . ?
N39 H501 0.9800 . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
Cl50 O501 1.360(10) . ?
Cl50 O503 1.418(8) . ?
Cl50 O500 1.423(11) . ?
Cl50 O502 1.471(10) . ?
Cl60 O600 1.410(10) . ?
Cl60 O601 1.413(8) . ?
Cl60 O603 1.441(8) . ?
Cl60 O602 1.446(6) . ?
Cl70 O701 1.379(14) . ?
Cl70 O702 1.434(14) . ?
Cl70 O700 1.446(15) . ?
Cl70 O703 1.447(15) . ?
Cl80 O801 1.322(12) . ?
Cl80 O802 1.394(13) . ?
Cl80 O803 1.414(15) . ?
Cl80 O800 1.704(7) . ?
C805 H80A 0.9600 . ?
C805 H80B 0.9600 . ?
C805 H80C 0.9600 . ?
S7A C40A 1.672(8) . ?
S7A C30A 1.743(9) . ?
C1A C30A 1.349(13) . ?
C1A C2A 1.445(14) . ?
C1A H1A 0.9300 . ?
C2A C40A 1.388(13) . ?
C2A H2A 0.9300 . ?
S7B C40B 1.429(19) . ?
S7B C30B 1.854(16) . ?
C1B C40B 1.63(7) . ?
C1B C2B 1.72(11) . ?
C1B H1BA 0.9300 . ?
C2B C30B 1.41(7) . ?
C2B H2BA 0.9300 . ?

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
N11B Ni3 N3M 89.5(3) . . ?
N11B Ni3 N3A 94.1(3) . . ?
N3M Ni3 N3A 87.3(2) . . ?
N11B Ni3 N3F 173.3(3) . . ?
N3M Ni3 N3F 97.1(3) . . ?
N3A Ni3 N3F 85.0(2) . . ?
N11B Ni3 O3J 88.1(3) . . ?
N3M Ni3 O3J 85.9(3) . . ?
N3A Ni3 O3J 172.9(3) . . ?
N3F Ni3 O3J 93.5(3) . . ?
N11B Ni3 N3E 90.7(3) . . ?
N3M Ni3 N3E 169.9(3) . . ?
N3A Ni3 N3E 102.7(2) . . ?
N3F Ni3 N3E 83.1(2) . . ?
O3J Ni3 N3E 84.0(3) . . ?
N3G Ni4 N3C 91.2(3) . . ?
N3G Ni4 N3I 93.1(3) . . ?
N3C Ni4 N3I 88.6(2) . . ?
N3G Ni4 O37 89.9(3) . . ?
N3C Ni4 O37 84.7(2) . . ?
N3I Ni4 O37 172.7(2) . . ?
N3G Ni4 N39 91.2(2) . . ?
N3C Ni4 N39 166.3(3) . . ?
N3I Ni4 N39 104.7(2) . . ?
O37 Ni4 N39 81.8(2) . . ?
N3G Ni4 N3H 173.2(3) . . ?
N3C Ni4 N3H 95.4(3) . . ?
N3I Ni4 N3H 85.6(2) . . ?
O37 Ni4 N3H 92.2(2) . . ?
N39 Ni4 N3H 82.7(2) . . ?
C4F S2 C4A 93.4(5) . . ?
C3X S3 C1AA 93.0(4) . . ?
C3L N3A C4D 113.1(6) . . ?
C3L N3A Ni3 104.7(4) . . ?
C4D N3A Ni3 117.7(5) . . ?
C3L N3A H5B 100(6) . . ?
C4D N3A H5B 112(6) . . ?
Ni3 N3A H5B 108(5) . . ?
C4H N3C Ni4 174.0(7) . . ?
C3K N3E C3Q 113.2(6) . . ?
C3K N3E Ni3 126.5(5) . . ?
C3Q N3E Ni3 108.7(5) . . ?
C3K N3E H6B 120(4) . . ?
C3Q N3E H6B 98(4) . . ?
Ni3 N3E H6B 85(4) . . ?
C41 N3F C45 112.0(6) . . ?
C41 N3F C4O 110.2(6) . . ?
C45 N3F C4O 110.5(6) . . ?
C41 N3F Ni3 105.3(5) . . ?
C45 N3F Ni3 105.6(5) . . ?
C4O N3F Ni3 113.2(5) . . ?
C4Q N3G Ni4 178.5(7) . . ?
C47 N3H C4I 111.8(6) . . ?
C47 N3H C3S 112.3(6) . . ?
C4I N3H C3S 109.9(6) . . ?
C47 N3H Ni4 113.8(5) . . ?
C4I N3H Ni4 105.6(5) . . ?
C3S N3H Ni4 102.8(4) . . ?
C3Y N3I C3V 113.8(6) . . ?
C3Y N3I Ni4 103.8(4) . . ?
C3V N3I Ni4 115.1(4) . . ?
C3Y N3I H500 107.9 . . ?
C3V N3I H500 107.9 . . ?
Ni4 N3I H500 107.9 . . ?
C1G N3M Ni3 172.3(10) . . ?
C4M N3U C3T 111.4(7) . . ?
C4M N3U H3B 116(8) . . ?
C3T N3U H3B 123(8) . . ?
C3P N4J C4U 112.3(9) . . ?
C3P N4J H1B 123.9 . . ?
C4U N4J H1B 123.9 . . ?
Ni4 O37 H37 109.5 . . ?
C4B C1AA C4D 128.6(8) . . ?
C4B C1AA S3 109.5(7) . . ?
C4D C1AA S3 121.8(7) . . ?
N11B C12B C805 166.9(10) . . ?
C12B N11B Ni3 176.9(9) . . ?
N3M C1G C24 174.8(14) . . ?
C30B C3K N3E 109.3(6) . . ?
N3E C3K C30A 115.2(6) . . ?
N3E C3K H3KA 108.5 . . ?
C30A C3K H3KA 108.5 . . ?
N3E C3K H3KB 108.5 . . ?
C30A C3K H3KB 108.5 . . ?
H3KA C3K H3KB 107.5 . . ?
N3A C3L C45 110.9(6) . . ?
N3A C3L H3LA 109.5 . . ?
C45 C3L H3LA 109.5 . . ?
N3A C3L H3LB 109.5 . . ?
C45 C3L H3LB 109.5 . . ?
H3LA C3L H3LB 108.1 . . ?
C3X C3O C4B 113.3(8) . . ?
C3X C3O H3O 123.4 . . ?
C4B C3O H3O 123.4 . . ?
N4J C3P C4A 110.5(9) . . ?
N4J C3P H3PA 109.5 . . ?
C4A C3P H3PA 109.5 . . ?
N4J C3P H3PB 109.5 . . ?
C4A C3P H3PB 109.5 . . ?
H3PA C3P H3PB 108.1 . . ?
N3E C3Q C41 113.2(6) . . ?
N3E C3Q H3QA 108.9 . . ?
C41 C3Q H3QA 108.9 . . ?
N3E C3Q H3QB 108.9 . . ?
C41 C3Q H3QB 108.9 . . ?
H3QA C3Q H3QB 107.7 . . ?
C4H C3R H3RA 109.5 . . ?
C4H C3R H3RB 109.5 . . ?
H3RA C3R H3RB 109.5 . . ?
C4H C3R H3RC 109.5 . . ?
H3RA C3R H3RC 109.5 . . ?
H3RB C3R H3RC 109.5 . . ?
C3Y C3S N3H 109.3(6) . . ?
C3Y C3S H3SA 109.8 . . ?
N3H C3S H3SA 109.8 . . ?
C3Y C3S H3SB 109.8 . . ?
N3H C3S H3SB 109.8 . . ?
H3SA C3S H3SB 108.3 . . ?
N3U C3T C47 111.3(7) . . ?
N3U C3T H3TA 109.4 . . ?
C47 C3T H3TA 109.4 . . ?
N3U C3T H3TB 109.4 . . ?
C47 C3T H3TB 109.4 . . ?
H3TA C3T H3TB 108.0 . . ?
N3I C3V C40B 112.8(6) . . ?
N3I C3V C40A 112.8(6) . . ?
N3I C3V H3VA 109.0 . . ?
C40A C3V H3VA 109.0 . . ?
N3I C3V H3VB 109.0 . . ?
C40A C3V H3VB 109.0 . . ?
H3VA C3V H3VB 107.8 . . ?
C3O C3X C46 125.3(8) . . ?
C3O C3X S3 110.3(6) . . ?
C46 C3X S3 124.3(6) . . ?
N3I C3Y C3S 109.9(5) . . ?
N3I C3Y H3YA 109.7 . . ?
C3S C3Y H3YA 109.7 . . ?
N3I C3Y H3YB 109.7 . . ?
C3S C3Y H3YB 109.7 . . ?
H3YA C3Y H3YB 108.2 . . ?
C4V C4A C3P 127.1(11) . . ?
C4V C4A S2 110.2(8) . . ?
C3P C4A S2 122.3(9) . . ?
C1AA C4B C3O 113.9(8) . . ?
C1AA C4B H4B 123.1 . . ?
C3O C4B H4B 123.1 . . ?
C4Q C4C H4CA 109.5 . . ?
C4Q C4C H4CB 109.5 . . ?
H4CA C4C H4CB 109.5 . . ?
C4Q C4C H4CC 109.5 . . ?
H4CA C4C H4CC 109.5 . . ?
H4CB C4C H4CC 109.5 . . ?
N3A C4D C1AA 116.0(6) . . ?
N3A C4D H4DA 108.3 . . ?
C1AA C4D H4DA 108.3 . . ?
N3A C4D H4DB 108.3 . . ?
C1AA C4D H4DB 108.3 . . ?
H4DA C4D H4DB 107.4 . . ?
C4N C4F C4M 127.7(10) . . ?
C4N C4F S2 109.0(8) . . ?
C4M C4F S2 123.1(8) . . ?
N3C C4H C3R 178.3(12) . . ?
N3H C4I C38 112.2(6) . . ?
N3H C4I H4IA 109.2 . . ?
C38 C4I H4IA 109.2 . . ?
N3H C4I H4IB 109.2 . . ?
C38 C4I H4IB 109.2 . . ?
H4IA C4I H4IB 107.9 . . ?
N3U C4M C4F 108.6(8) . . ?
N3U C4M H4MA 110.0 . . ?
C4F C4M H4MA 110.0 . . ?
N3U C4M H4MB 110.0 . . ?
C4F C4M H4MB 110.0 . . ?
H4MA C4M H4MB 108.4 . . ?
C4F C4N C4V 113.0(11) . . ?
C4F C4N H4N 123.5 . . ?
C4V C4N H4N 123.5 . . ?
N3F C4O C4U 118.6(7) . . ?
N3F C4O H4OA 107.7 . . ?
C4U C4O H4OA 107.7 . . ?
N3F C4O H4OB 107.7 . . ?
C4U C4O H4OB 107.7 . . ?
H4OA C4O H4OB 107.1 . . ?
N3G C4Q C4C 175.8(16) . . ?
N4J C4U C4O 110.0(9) . . ?
N4J C4U H4UA 109.7 . . ?
C4O C4U H4UA 109.7 . . ?
N4J C4U H4UB 109.7 . . ?
C4O C4U H4UB 109.7 . . ?
H4UA C4U H4UB 108.2 . . ?
C4A C4V C4N 114.2(10) . . ?
C4A C4V H4V 122.9 . . ?
C4N C4V H4V 122.9 . . ?
C1G C24 H24A 109.5 . . ?
C1G C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C1G C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N39 C38 C4I 111.3(6) . . ?
N39 C38 H38A 109.4 . . ?
C4I C38 H38A 109.4 . . ?
N39 C38 H38B 109.4 . . ?
C4I C38 H38B 109.4 . . ?
H38A C38 H38B 108.0 . . ?
C38 N39 C46 111.2(6) . . ?
C38 N39 Ni4 109.9(5) . . ?
C46 N39 Ni4 124.7(5) . . ?
C38 N39 H501 102.6 . . ?
C46 N39 H501 102.6 . . ?
Ni4 N39 H501 102.6 . . ?
N3F C41 C3Q 111.8(6) . . ?
N3F C41 H41A 109.2 . . ?
C3Q C41 H41A 109.2 . . ?
N3F C41 H41B 109.2 . . ?
C3Q C41 H41B 109.2 . . ?
H41A C41 H41B 107.9 . . ?
N3F C45 C3L 109.5(6) . . ?
N3F C45 H45A 109.8 . . ?
C3L C45 H45A 109.8 . . ?
N3F C45 H45B 109.8 . . ?
C3L C45 H45B 109.8 . . ?
H45A C45 H45B 108.2 . . ?
C3X C46 N39 114.2(6) . . ?
C3X C46 H46A 108.7 . . ?
N39 C46 H46A 108.7 . . ?
C3X C46 H46B 108.7 . . ?
N39 C46 H46B 108.7 . . ?
H46A C46 H46B 107.6 . . ?
N3H C47 C3T 117.9(7) . . ?
N3H C47 H47A 107.8 . . ?
C3T C47 H47A 107.8 . . ?
N3H C47 H47B 107.8 . . ?
C3T C47 H47B 107.8 . . ?
H47A C47 H47B 107.2 . . ?
O501 Cl50 O503 115.0(8) . . ?
O501 Cl50 O500 117.3(10) . . ?
O503 Cl50 O500 104.2(8) . . ?
O501 Cl50 O502 105.1(9) . . ?
O503 Cl50 O502 107.3(6) . . ?
O500 Cl50 O502 107.5(9) . . ?
O600 Cl60 O601 110.0(7) . . ?
O600 Cl60 O603 111.4(8) . . ?
O601 Cl60 O603 108.7(5) . . ?
O600 Cl60 O602 109.2(6) . . ?
O601 Cl60 O602 108.8(5) . . ?
O603 Cl60 O602 108.6(5) . . ?
O701 Cl70 O702 114.0(15) . . ?
O701 Cl70 O700 116.3(14) . . ?
O702 Cl70 O700 104.1(14) . . ?
O701 Cl70 O703 108.9(15) . . ?
O702 Cl70 O703 104.9(14) . . ?
O700 Cl70 O703 107.8(15) . . ?
O801 Cl80 O802 116.0(11) . . ?
O801 Cl80 O803 119.2(11) . . ?
O802 Cl80 O803 105.0(10) . . ?
O801 Cl80 O800 102.5(10) . . ?
O802 Cl80 O800 106.6(11) . . ?
O803 Cl80 O800 106.6(7) . . ?
C12B C805 H80A 109.5 . . ?
C12B C805 H80B 109.5 . . ?
H80A C805 H80B 109.5 . . ?
C12B C805 H80C 109.5 . . ?
H80A C805 H80C 109.5 . . ?
H80B C805 H80C 109.5 . . ?
C40A S7A C30A 92.4(4) . . ?
C30A C1A C2A 111.8(9) . . ?
C30A C1A H1A 124.1 . . ?
C2A C1A H1A 124.1 . . ?
C40A C2A C1A 111.9(8) . . ?
C40A C2A H2A 124.0 . . ?
C1A C2A H2A 124.0 . . ?
C1A C30A C3K 125.3(9) . . ?
C1A C30A S7A 111.7(7) . . ?
C3K C30A S7A 123.0(7) . . ?
C2A C40A C3V 120.5(8) . . ?
C2A C40A S7A 112.1(6) . . ?
C3V C40A S7A 127.2(7) . . ?
C40B S7B C30B 107.3(10) . . ?
C40B C1B C2B 107(5) . . ?
C40B C1B H1BA 126.6 . . ?
C2B C1B H1BA 126.6 . . ?
C30B C2B C1B 108(5) . . ?
C30B C2B H2BA 125.9 . . ?
C1B C2B H2BA 125.9 . . ?
C3K C30B C2B 127(3) . . ?
C3K C30B S7B 124.5(6) . . ?
C2B C30B S7B 106(3) . . ?
S7B C40B C3V 154.2(9) . . ?
S7B C40B C1B 110(3) . . ?
C3V C40B C1B 95(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3X S3 C1AA C4B -1.6(6) . . . . ?
C3X S3 C1AA C4D 175.4(6) . . . . ?
C3Q N3E C3K C30B -56.9(7) . . . . ?
Ni3 N3E C3K C30B 81.7(7) . . . . ?
C3Q N3E C3K C30A -83.0(8) . . . . ?
Ni3 N3E C3K C30A 55.6(9) . . . . ?
C4D N3A C3L C45 173.1(6) . . . . ?
Ni3 N3A C3L C45 43.8(6) . . . . ?
C4U N4J C3P C4A 169.0(8) . . . . ?
C3K N3E C3Q C41 165.7(6) . . . . ?
Ni3 N3E C3Q C41 19.9(7) . . . . ?
C47 N3H C3S C3Y -81.3(8) . . . . ?
C4I N3H C3S C3Y 153.5(6) . . . . ?
Ni4 N3H C3S C3Y 41.5(6) . . . . ?
C4M N3U C3T C47 -175.2(8) . . . . ?
C3Y N3I C3V C40B 73.9(9) . . . . ?
Ni4 N3I C3V C40B -166.4(6) . . . . ?
C3Y N3I C3V C40A 73.9(9) . . . . ?
Ni4 N3I C3V C40A -166.4(6) . . . . ?
C4B C3O C3X C46 -179.3(6) . . . . ?
C4B C3O C3X S3 -1.4(8) . . . . ?
C1AA S3 C3X C3O 1.7(5) . . . . ?
C1AA S3 C3X C46 179.6(6) . . . . ?
C3V N3I C3Y C3S 171.4(6) . . . . ?
Ni4 N3I C3Y C3S 45.5(6) . . . . ?
N3H C3S C3Y N3I -62.0(7) . . . . ?
N4J C3P C4A C4V 164.1(11) . . . . ?
N4J C3P C4A S2 -23.8(12) . . . . ?
C4F S2 C4A C4V 0.4(9) . . . . ?
C4F S2 C4A C3P -172.9(9) . . . . ?
C4D C1AA C4B C3O -175.7(7) . . . . ?
S3 C1AA C4B C3O 1.1(8) . . . . ?
C3X C3O C4B C1AA 0.2(9) . . . . ?
C3L N3A C4D C1AA 75.6(9) . . . . ?
Ni3 N3A C4D C1AA -162.1(6) . . . . ?
C4B C1AA C4D N3A 92.9(11) . . . . ?
S3 C1AA C4D N3A -83.5(8) . . . . ?
C4A S2 C4F C4N 1.6(8) . . . . ?
C4A S2 C4F C4M -174.3(9) . . . . ?
C47 N3H C4I C38 168.1(7) . . . . ?
C3S N3H C4I C38 -66.5(8) . . . . ?
Ni4 N3H C4I C38 43.7(8) . . . . ?
C3T N3U C4M C4F 170.1(8) . . . . ?
C4N C4F C4M N3U 157.0(10) . . . . ?
S2 C4F C4M N3U -27.9(12) . . . . ?
C4M C4F C4N C4V 172.5(10) . . . . ?
S2 C4F C4N C4V -3.2(12) . . . . ?
C41 N3F C4O C4U 50.8(10) . . . . ?
C45 N3F C4O C4U -73.6(10) . . . . ?
Ni3 N3F C4O C4U 168.3(7) . . . . ?
C3P N4J C4U C4O -166.9(8) . . . . ?
N3F C4O C4U N4J 73.6(10) . . . . ?
C3P C4A C4V C4N 170.5(10) . . . . ?
S2 C4A C4V C4N -2.3(13) . . . . ?
C4F C4N C4V C4A 3.7(15) . . . . ?
N3H C4I C38 N39 -46.6(9) . . . . ?
C4I C38 N39 C46 166.3(6) . . . . ?
C4I C38 N39 Ni4 24.1(7) . . . . ?
C45 N3F C41 C3Q -69.8(9) . . . . ?
C4O N3F C41 C3Q 166.8(6) . . . . ?
Ni3 N3F C41 C3Q 44.5(7) . . . . ?
N3E C3Q C41 N3F -44.7(9) . . . . ?
C41 N3F C45 C3L 150.9(6) . . . . ?
C4O N3F C45 C3L -85.8(8) . . . . ?
Ni3 N3F C45 C3L 36.8(6) . . . . ?
N3A C3L C45 N3F -56.8(8) . . . . ?
C3O C3X C46 N39 -111.9(8) . . . . ?
S3 C3X C46 N39 70.6(8) . . . . ?
C38 N39 C46 C3X -82.3(8) . . . . ?
Ni4 N39 C46 C3X 53.3(9) . . . . ?
C4I N3H C47 C3T 54.9(9) . . . . ?
C3S N3H C47 C3T -69.3(8) . . . . ?
Ni4 N3H C47 C3T 174.5(5) . . . . ?
N3U C3T C47 N3H 72.1(9) . . . . ?
C30A C1A C2A C40A -1.4(9) . . . . ?
C2A C1A C30A C3K -178.2(7) . . . . ?
C2A C1A C30A S7A 0.2(8) . . . . ?
N3E C3K C30A C1A -114.6(8) . . . . ?
N3E C3K C30A S7A 67.2(8) . . . . ?
C40A S7A C30A C1A 0.8(6) . . . . ?
C40A S7A C30A C3K 179.3(6) . . . . ?
C1A C2A C40A C3V -173.3(6) . . . . ?
C1A C2A C40A S7A 2.0(8) . . . . ?
N3I C3V C40A C2A 96.8(9) . . . . ?
N3I C3V C40A S7A -77.8(9) . . . . ?
C30A S7A C40A C2A -1.6(6) . . . . ?
C30A S7A C40A C3V 173.3(7) . . . . ?
C40B C1B C2B C30B -10(3) . . . . ?
N3E C3K C30B C2B 100(3) . . . . ?
N3E C3K C30B S7B -99.3(8) . . . . ?
C1B C2B C30B C3K 176.7(12) . . . . ?
C1B C2B C30B S7B 13(3) . . . . ?
C40B S7B C30B C3K -177.9(7) . . . . ?
C40B S7B C30B C2B -14(3) . . . . ?
C30B S7B C40B C3V -154.6(17) . . . . ?
C30B S7B C40B C1B 7.0(13) . . . . ?
N3I C3V C40B S7B 50(2) . . . . ?
N3I C3V C40B C1B -112.4(15) . . . . ?
C2B C1B C40B S7B 0.2(14) . . . . ?
C2B C1B C40B C3V 172.2(15) . . . . ?

_refine_diff_density_max         2.369
_refine_diff_density_min         -1.858
_refine_diff_density_rms         0.159


_refine_special_details          ', SQUEEZE'
####################################################################### 
# 
# 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_LIF_lc-27a
_database_code_depnum_ccdc_archive 'CCDC 1517784'


_audit_update_record             
;
2017-01-10 deposited with the CCDC.
2017-02-06 downloaded from the CCDC.
;
_publcif_datablock.id            {0f572e16-c84f-4356-bae3-ad4ddf93468d}

_audit_creation_date             2016-07-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H39 F3 N8'
_chemical_formula_sum            'C36 H39 F3 N8'
_chemical_formula_weight         640.44
_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 0.0030 0.0020 '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'
F F 0.0170 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 '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           9
_space_group_name_H-M_alt        'C 1 c 1'
_space_group_name_Hall           'C -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   15.888(3)
_cell_length_b                   13.4639(18)
_cell_length_c                   16.442(3)
_cell_angle_alpha                90
_cell_angle_beta                 102.98(2)
_cell_angle_gamma                90
_cell_volume                     3427.3(10)
_cell_formula_units_Z            4
_cell_oxdiff_measurement_reflns_used 6757
_exptl_absorpt_correction_T_min  0.9682
_exptl_absorpt_correction_T_max  0.9937
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    6746
_cell_measurement_theta_min      2.9056
_cell_measurement_theta_max      36.5984

_exptl_absorpt_coefficient_mu    0.087

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_radiation_wavelength     0.7107
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_detector_area_resol_mean 8.4171
_diffrn_reflns_av_R_equivalents  0.0748
_diffrn_reflns_av_unetI/netI     0.2518
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17944
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.220
_diffrn_reflns_theta_min         2.527
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_method       'ω scans'
_diffrn_source                   ?
_reflns_Friedel_coverage         0.939
_reflns_Friedel_fraction_full    0.964
_reflns_Friedel_fraction_max     0.926
_reflns_number_gt                11896
_reflns_number_total             17944
_reflns_special_details          
;
 _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_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details 
;
 Flack x determined using 621 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.7(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.782
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         7944
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.2070
_refine_ls_R_factor_gt           0.0793
_refine_ls_restrained_S_all      0.782
_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)+(0.1025P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2261
_refine_ls_wR_factor_ref         0.2570
_refine_special_details          
;
 Refined as a 5-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.4571 0.22245 0.17525 0.09637 0.04883
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:
 C1(H1A,H1B), C2(H2A,H2B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B),
 C14(H14A,H14B), C22(H22A,H22B), C23(H23A,H23B), C25(H25A,H25B), C26(H26A,H26B),
  C35(H35A,H35B), C36(H36A,H36B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C9(H9), C10(H10), C15(H15), C17(H17), C19(H19),
 C24(H24), C21(H21), C27(H27), C29(H29), C31(H31), C33(H33), C34(H34)
3.c Fitted hexagon refined as free rotating group:
 C4(C5,C6,C7,C8,C9), C16(C17,C18,C19,C20,C24), C28(C29,C30,C31,C32,C33)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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
F1 F -0.2835(5) 0.7613(6) -0.4248(5) 0.060(2) Uani 1 1 d . . . . .
F2 F -0.4361(5) 0.7128(7) 0.0514(4) 0.058(2) Uani 1 1 d . . . . .
F3 F -0.3486(6) 0.1586(7) -0.2177(6) 0.074(3) Uani 1 1 d . . . . .
N1 N -0.6786(7) 0.5435(10) -0.3557(7) 0.054(3) Uani 1 1 d . . . . .
N2 N -0.5990(7) 0.7221(9) -0.2540(7) 0.048(3) Uani 1 1 d . . . . .
N3 N -0.6007(8) 0.3920(10) -0.2175(9) 0.059(4) Uani 1 1 d . . . . .
N4 N -0.5322(7) 0.5190(11) -0.4458(7) 0.061(4) Uani 1 1 d . . . . .
N5 N -0.0206(6) 0.5414(9) -0.0437(7) 0.046(3) Uani 1 1 d . . . . .
N6 N -0.1466(8) 0.3844(11) -0.0145(8) 0.064(4) Uani 1 1 d . . . . .
N7 N -0.1541(7) 0.7094(9) -0.0394(7) 0.051(3) Uani 1 1 d . . . . .
N8 N -0.0819(7) 0.5271(10) -0.2309(7) 0.051(3) Uani 1 1 d . . . . .
C1 C -0.6845(8) 0.5310(12) -0.4453(7) 0.045(4) Uani 1 1 d . . . . .
H1A H -0.6830 0.5957 -0.4709 0.055 Uiso 1 1 calc R . . . .
H1B H -0.7392 0.4999 -0.4706 0.055 Uiso 1 1 calc R . . . .
C2 C -0.6103(9) 0.4669(12) -0.4622(9) 0.054(4) Uani 1 1 d . . . . .
H2A H -0.6043 0.4080 -0.4274 0.065 Uiso 1 1 calc R . . . .
H2B H -0.6240 0.4458 -0.5201 0.065 Uiso 1 1 calc R . . . .
C3 C -0.4720(9) 0.4883(10) -0.3889(9) 0.045(4) Uani 1 1 d . . . . .
H3 H -0.4825 0.4337 -0.3580 0.055 Uiso 1 1 calc R . . . .
C4 C -0.3820(4) 0.5349(7) -0.3670(5) 0.051(4) Uani 1 1 d . . . . .
C5 C -0.3734(5) 0.6255(7) -0.4048(4) 0.052(4) Uani 1 1 d G . . . .
H5 H -0.4206 0.6536 -0.4414 0.062 Uiso 1 1 calc R . . . .
C6 C -0.2943(6) 0.6742(5) -0.3879(5) 0.044(4) Uani 1 1 d G . . . .
C7 C -0.2237(4) 0.6323(6) -0.3332(5) 0.040(3) Uani 1 1 d G . . . .
H7 H -0.1707 0.6649 -0.3219 0.049 Uiso 1 1 calc R . . . .
C8 C -0.2323(4) 0.5416(6) -0.2954(4) 0.037(3) Uani 1 1 d G . . . .
C9 C -0.3114(6) 0.4929(5) -0.3123(5) 0.045(4) Uani 1 1 d G . . . .
H9 H -0.3172 0.4323 -0.2870 0.055 Uiso 1 1 calc R . . . .
C10 C -0.1596(9) 0.4919(12) -0.2422(8) 0.049(4) Uani 1 1 d . . . . .
H10 H -0.1688 0.4333 -0.2155 0.059 Uiso 1 1 calc R . . . .
C11 C -0.0126(10) 0.4719(12) -0.1802(8) 0.052(4) Uani 1 1 d . . . . .
H11A H 0.0293 0.4542 -0.2124 0.062 Uiso 1 1 calc R . . . .
H11B H -0.0347 0.4112 -0.1609 0.062 Uiso 1 1 calc R . . . .
C12 C 0.0318(8) 0.5381(12) -0.1028(8) 0.049(4) Uani 1 1 d . . . . .
H12A H 0.0878 0.5106 -0.0770 0.059 Uiso 1 1 calc R . . . .
H12B H 0.0404 0.6049 -0.1216 0.059 Uiso 1 1 calc R . . . .
C13 C -0.7225(8) 0.6387(11) -0.3406(8) 0.044(4) Uani 1 1 d . . . . .
H13A H -0.7447 0.6321 -0.2905 0.052 Uiso 1 1 calc R . . . .
H13B H -0.7710 0.6510 -0.3871 0.052 Uiso 1 1 calc R . . . .
C14 C -0.6612(10) 0.7255(12) -0.3309(8) 0.053(4) Uani 1 1 d . . . . .
H14A H -0.6318 0.7253 -0.3766 0.064 Uiso 1 1 calc R . . . .
H14B H -0.6938 0.7868 -0.3339 0.064 Uiso 1 1 calc R . . . .
C15 C -0.5209(8) 0.7090(10) -0.2523(8) 0.040(3) Uani 1 1 d . . . . .
H15 H -0.5040 0.7009 -0.3025 0.048 Uiso 1 1 calc R . . . .
C16 C -0.4532(4) 0.7058(7) -0.1722(4) 0.034(3) Uani 1 1 d . . . . .
C17 C -0.4767(4) 0.7082(7) -0.0957(5) 0.041(3) Uani 1 1 d G . . . .
H17 H -0.5347 0.7113 -0.0938 0.049 Uiso 1 1 calc R . . . .
C18 C -0.4134(5) 0.7060(7) -0.0220(4) 0.042(3) Uani 1 1 d G . . . .
C19 C -0.3267(5) 0.7014(7) -0.0248(4) 0.039(3) Uani 1 1 d G . . . .
H19 H -0.2844 0.7000 0.0246 0.047 Uiso 1 1 calc R . . . .
C20 C -0.3032(4) 0.6990(7) -0.1012(5) 0.043(3) Uani 1 1 d G . . . .
C24 C -0.3665(5) 0.7012(7) -0.1749(4) 0.041(3) Uani 1 1 d G . . . .
H24 H -0.3508 0.6996 -0.2261 0.049 Uiso 1 1 calc R . . . .
C21 C -0.2135(9) 0.6998(10) -0.1035(8) 0.046(4) Uani 1 1 d . . . . .
H21 H -0.1987 0.6929 -0.1548 0.056 Uiso 1 1 calc R . . . .
C22 C -0.0604(8) 0.7167(11) -0.0441(10) 0.052(4) Uani 1 1 d . . . . .
H22A H -0.0567 0.7126 -0.1021 0.062 Uiso 1 1 calc R . . . .
H22B H -0.0382 0.7811 -0.0231 0.062 Uiso 1 1 calc R . . . .
C23 C -0.0077(8) 0.6414(12) 0.0019(8) 0.046(4) Uani 1 1 d . . . . .
H23A H -0.0217 0.6343 0.0561 0.055 Uiso 1 1 calc R . . . .
H23B H 0.0525 0.6608 0.0109 0.055 Uiso 1 1 calc R . . . .
C25 C -0.7224(11) 0.4609(13) -0.3196(10) 0.069(5) Uani 1 1 d . . . . .
H25A H -0.7188 0.4001 -0.3502 0.083 Uiso 1 1 calc R . . . .
H25B H -0.7830 0.4769 -0.3254 0.083 Uiso 1 1 calc R . . . .
C26 C -0.6802(11) 0.4452(15) -0.2275(10) 0.073(5) Uani 1 1 d . . . . .
H26A H -0.6693 0.5091 -0.2000 0.087 Uiso 1 1 calc R . . . .
H26B H -0.7193 0.4084 -0.2011 0.087 Uiso 1 1 calc R . . . .
C27 C -0.5348(10) 0.4333(12) -0.1792(10) 0.058(4) Uani 1 1 d . . . . .
H27 H -0.5394 0.4969 -0.1586 0.069 Uiso 1 1 calc R . . . .
C28 C -0.4472(4) 0.3863(7) -0.1642(5) 0.051(4) Uani 1 1 d . . . . .
C29 C -0.4386(5) 0.2953(7) -0.2013(5) 0.051(4) Uani 1 1 d G . . . .
H29 H -0.4863 0.2658 -0.2361 0.061 Uiso 1 1 calc R . . . .
C30 C -0.3587(7) 0.2483(5) -0.1863(6) 0.053(4) Uani 1 1 d G . . . .
C31 C -0.2874(5) 0.2924(7) -0.1342(6) 0.052(4) Uani 1 1 d G . . . .
H31 H -0.2340 0.2610 -0.1242 0.063 Uiso 1 1 calc R . . . .
C32 C -0.2961(5) 0.3835(7) -0.0972(5) 0.042(3) Uani 1 1 d G . . . .
C33 C -0.3760(6) 0.4305(5) -0.1122(5) 0.047(4) Uani 1 1 d G . . . .
H33 H -0.3818 0.4914 -0.0873 0.056 Uiso 1 1 calc R . . . .
C34 C -0.2204(10) 0.4268(13) -0.0341(8) 0.055(4) Uani 1 1 d . . . . .
H34 H -0.2280 0.4868 -0.0086 0.066 Uiso 1 1 calc R . . . .
C35 C -0.0792(10) 0.4312(13) 0.0486(9) 0.062(5) Uani 1 1 d . . . . .
H35A H -0.0604 0.3862 0.0951 0.075 Uiso 1 1 calc R . . . .
H35B H -0.1017 0.4908 0.0693 0.075 Uiso 1 1 calc R . . . .
C36 C -0.0047(9) 0.4573(12) 0.0116(9) 0.054(4) Uani 1 1 d . . . . .
H36A H 0.0450 0.4714 0.0564 0.064 Uiso 1 1 calc R . . . .
H36B H 0.0094 0.4003 -0.0189 0.064 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
F1 C6 1.348(10) . ?
F2 C18 1.338(8) . ?
F3 C30 1.336(10) . ?
N1 C1 1.465(15) . ?
N1 C13 1.506(18) . ?
N1 C25 1.503(19) . ?
N2 C14 1.420(16) . ?
N2 C15 1.246(15) . ?
N3 C26 1.43(2) . ?
N3 C27 1.228(19) . ?
N4 C2 1.398(18) . ?
N4 C3 1.249(17) . ?
N5 C12 1.414(15) . ?
N5 C23 1.532(19) . ?
N5 C36 1.440(17) . ?
N6 C34 1.279(18) . ?
N6 C35 1.456(18) . ?
N7 C21 1.253(15) . ?
N7 C22 1.511(15) . ?
N8 C10 1.296(16) . ?
N8 C11 1.431(18) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.535(18) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3 0.9300 . ?
C3 C4 1.528(15) . ?
C4 C5 1.3900 . ?
C4 C9 1.3900 . ?
C5 H5 0.9300 . ?
C5 C6 1.3900 . ?
C6 C7 1.3900 . ?
C7 H7 0.9300 . ?
C7 C8 1.3900 . ?
C8 C9 1.3900 . ?
C8 C10 1.447(16) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.583(19) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.51(2) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 H15 0.9300 . ?
C15 C16 1.503(13) . ?
C16 C17 1.3900 . ?
C16 C24 1.3900 . ?
C17 H17 0.9300 . ?
C17 C18 1.3900 . ?
C18 C19 1.3900 . ?
C19 H19 0.9300 . ?
C19 C20 1.3900 . ?
C20 C24 1.3900 . ?
C20 C21 1.435(15) . ?
C24 H24 0.9300 . ?
C21 H21 0.9300 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.421(19) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.53(2) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 H27 0.9300 . ?
C27 C28 1.497(16) . ?
C28 C29 1.3900 . ?
C28 C33 1.3900 . ?
C29 H29 0.9300 . ?
C29 C30 1.3900 . ?
C30 C31 1.3900 . ?
C31 H31 0.9300 . ?
C31 C32 1.3900 . ?
C32 C33 1.3900 . ?
C32 C34 1.517(16) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C35 C36 1.488(19) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?

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 N1 C13 109.6(11) . . ?
C1 N1 C25 112.4(12) . . ?
C25 N1 C13 107.0(11) . . ?
C15 N2 C14 121.0(12) . . ?
C27 N3 C26 117.6(16) . . ?
C3 N4 C2 118.4(14) . . ?
C12 N5 C23 109.2(11) . . ?
C12 N5 C36 111.3(11) . . ?
C36 N5 C23 113.3(11) . . ?
C34 N6 C35 118.2(14) . . ?
C21 N7 C22 121.9(12) . . ?
C10 N8 C11 118.5(13) . . ?
N1 C1 H1A 109.3 . . ?
N1 C1 H1B 109.3 . . ?
N1 C1 C2 111.6(11) . . ?
H1A C1 H1B 108.0 . . ?
C2 C1 H1A 109.3 . . ?
C2 C1 H1B 109.3 . . ?
N4 C2 C1 111.6(13) . . ?
N4 C2 H2A 109.3 . . ?
N4 C2 H2B 109.3 . . ?
C1 C2 H2A 109.3 . . ?
C1 C2 H2B 109.3 . . ?
H2A C2 H2B 108.0 . . ?
N4 C3 H3 118.0 . . ?
N4 C3 C4 124.0(13) . . ?
C4 C3 H3 118.0 . . ?
C5 C4 C3 115.8(9) . . ?
C5 C4 C9 120.0 . . ?
C9 C4 C3 124.2(9) . . ?
C4 C5 H5 120.0 . . ?
C4 C5 C6 120.0 . . ?
C6 C5 H5 120.0 . . ?
F1 C6 C5 121.4(7) . . ?
F1 C6 C7 118.6(7) . . ?
C7 C6 C5 120.0 . . ?
C6 C7 H7 120.0 . . ?
C8 C7 C6 120.0 . . ?
C8 C7 H7 120.0 . . ?
C7 C8 C9 120.0 . . ?
C7 C8 C10 122.1(9) . . ?
C9 C8 C10 117.8(9) . . ?
C4 C9 H9 120.0 . . ?
C8 C9 C4 120.0 . . ?
C8 C9 H9 120.0 . . ?
N8 C10 C8 121.5(13) . . ?
N8 C10 H10 119.3 . . ?
C8 C10 H10 119.3 . . ?
N8 C11 H11A 109.9 . . ?
N8 C11 H11B 109.9 . . ?
N8 C11 C12 108.8(12) . . ?
H11A C11 H11B 108.3 . . ?
C12 C11 H11A 109.9 . . ?
C12 C11 H11B 109.9 . . ?
N5 C12 C11 110.2(11) . . ?
N5 C12 H12A 109.6 . . ?
N5 C12 H12B 109.6 . . ?
C11 C12 H12A 109.6 . . ?
C11 C12 H12B 109.6 . . ?
H12A C12 H12B 108.1 . . ?
N1 C13 H13A 109.3 . . ?
N1 C13 H13B 109.3 . . ?
N1 C13 C14 111.4(10) . . ?
H13A C13 H13B 108.0 . . ?
C14 C13 H13A 109.3 . . ?
C14 C13 H13B 109.3 . . ?
N2 C14 C13 111.9(12) . . ?
N2 C14 H14A 109.2 . . ?
N2 C14 H14B 109.2 . . ?
C13 C14 H14A 109.2 . . ?
C13 C14 H14B 109.2 . . ?
H14A C14 H14B 107.9 . . ?
N2 C15 H15 118.8 . . ?
N2 C15 C16 122.5(12) . . ?
C16 C15 H15 118.8 . . ?
C17 C16 C15 120.5(8) . . ?
C17 C16 C24 120.0 . . ?
C24 C16 C15 119.5(8) . . ?
C16 C17 H17 120.0 . . ?
C16 C17 C18 120.0 . . ?
C18 C17 H17 120.0 . . ?
F2 C18 C17 119.8(6) . . ?
F2 C18 C19 120.1(6) . . ?
C19 C18 C17 120.0 . . ?
C18 C19 H19 120.0 . . ?
C18 C19 C20 120.0 . . ?
C20 C19 H19 120.0 . . ?
C19 C20 C21 119.5(8) . . ?
C24 C20 C19 120.0 . . ?
C24 C20 C21 120.4(8) . . ?
C16 C24 H24 120.0 . . ?
C20 C24 C16 120.0 . . ?
C20 C24 H24 120.0 . . ?
N7 C21 C20 123.0(12) . . ?
N7 C21 H21 118.5 . . ?
C20 C21 H21 118.5 . . ?
N7 C22 H22A 108.9 . . ?
N7 C22 H22B 108.9 . . ?
H22A C22 H22B 107.7 . . ?
C23 C22 N7 113.3(11) . . ?
C23 C22 H22A 108.9 . . ?
C23 C22 H22B 108.9 . . ?
N5 C23 H23A 109.3 . . ?
N5 C23 H23B 109.3 . . ?
C22 C23 N5 111.6(11) . . ?
C22 C23 H23A 109.3 . . ?
C22 C23 H23B 109.3 . . ?
H23A C23 H23B 108.0 . . ?
N1 C25 H25A 109.5 . . ?
N1 C25 H25B 109.5 . . ?
N1 C25 C26 110.8(12) . . ?
H25A C25 H25B 108.1 . . ?
C26 C25 H25A 109.5 . . ?
C26 C25 H25B 109.5 . . ?
N3 C26 C25 111.3(14) . . ?
N3 C26 H26A 109.4 . . ?
N3 C26 H26B 109.4 . . ?
C25 C26 H26A 109.4 . . ?
C25 C26 H26B 109.4 . . ?
H26A C26 H26B 108.0 . . ?
N3 C27 H27 118.4 . . ?
N3 C27 C28 123.2(15) . . ?
C28 C27 H27 118.4 . . ?
C29 C28 C27 118.7(10) . . ?
C29 C28 C33 120.0 . . ?
C33 C28 C27 121.3(10) . . ?
C28 C29 H29 120.0 . . ?
C28 C29 C30 120.0 . . ?
C30 C29 H29 120.0 . . ?
F3 C30 C29 121.7(9) . . ?
F3 C30 C31 118.2(9) . . ?
C31 C30 C29 120.0 . . ?
C30 C31 H31 120.0 . . ?
C30 C31 C32 120.0 . . ?
C32 C31 H31 120.0 . . ?
C31 C32 C33 120.0 . . ?
C31 C32 C34 119.8(10) . . ?
C33 C32 C34 119.9(10) . . ?
C28 C33 H33 120.0 . . ?
C32 C33 C28 120.0 . . ?
C32 C33 H33 120.0 . . ?
N6 C34 C32 122.8(14) . . ?
N6 C34 H34 118.6 . . ?
C32 C34 H34 118.6 . . ?
N6 C35 H35A 109.7 . . ?
N6 C35 H35B 109.7 . . ?
N6 C35 C36 109.7(12) . . ?
H35A C35 H35B 108.2 . . ?
C36 C35 H35A 109.7 . . ?
C36 C35 H35B 109.7 . . ?
N5 C36 C35 113.7(12) . . ?
N5 C36 H36A 108.8 . . ?
N5 C36 H36B 108.8 . . ?
C35 C36 H36A 108.8 . . ?
C35 C36 H36B 108.8 . . ?
H36A C36 H36B 107.7 . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.4571
2 0.22245
3 0.17525
4 0.09637
5 0.04883
####################################################################### 
# 
# 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_Tren-Ni-CH3CN-2-ClO4-3_upa_fm435
_database_code_depnum_ccdc_archive 'CCDC 1517786'

_audit_update_record             
;
2017-02-03 deposited with the CCDC.
2017-02-06 downloaded from the CCDC.
;
_publcif_datablock.id            {b245eeae-109b-4e98-8083-0e4b39bab528}

_audit_creation_date             2016-11-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10 H24 N6 Ni, 2(Cl O4)'
_chemical_formula_sum            'C10 H24 Cl2 N6 Ni O8'
_chemical_formula_weight         485.96
_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 0.0181 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'
Cl Cl 0.3639 0.7018 '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'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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           36
_space_group_name_H-M_alt        'C m c 21'
_space_group_name_Hall           'C 2c -2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   31.9793(9)
_cell_length_b                   10.8558(3)
_cell_length_c                   11.0677(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3842.27(19)
_cell_formula_units_Z            8
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    6746
_cell_measurement_theta_min      2.9056
_cell_measurement_theta_max      36.5984
_shelx_estimated_absorpt_T_max   0.638
_shelx_estimated_absorpt_T_min   0.467
_exptl_absorpt_coefficient_mu    4.502
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_special_details           ?
_exptl_transmission_factor_max   0.638
_exptl_transmission_factor_min   0.467
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4184
_diffrn_reflns_point_group_measured_fraction_full 0.681
_diffrn_reflns_point_group_measured_fraction_max 0.648
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.189
_diffrn_reflns_theta_min         4.301
_diffrn_ambient_temperature      110.15
_diffrn_detector_area_resol_mean 8.4171
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.273
_reflns_Friedel_fraction_full    0.331
_reflns_Friedel_fraction_max     0.294
_reflns_number_gt                2581
_reflns_number_total             2652
_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_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.949
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         2652
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0493
_refine_ls_restrained_S_all      1.184
_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)+(0.0359P)²+39.5549P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1364
_refine_ls_wR_factor_ref         0.1381
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N3(H3A,H3B), N4(H4A,H4B), C1(H1A,H1B), C2(H2C,H2D), C3(H3C,H3D),
 C4(H4C,H4D), C5(H5A,H5B), C6(H6A,H6B)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C)
;
_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
Ni1 Ni 0.11934(3) 0.13554(10) 0.22903(13) 0.0183(3) Uani 1 1 d . . . . .
N1 N 0.13509(18) 0.3183(5) 0.1939(7) 0.0228(14) Uani 1 1 d . . . . .
N2 N 0.1111(2) 0.1959(6) 0.4077(7) 0.0266(15) Uani 1 1 d . . . . .
H2A H 0.0825 0.1762 0.4356 0.032 Uiso 1 1 calc R . . . .
H2B H 0.1313 0.1539 0.4616 0.032 Uiso 1 1 calc R . . . .
N3 N 0.05994(19) 0.1908(5) 0.1768(7) 0.0232(14) Uani 1 1 d . . . . .
H3A H 0.0454 0.1226 0.1347 0.028 Uiso 1 1 calc R . . . .
H3B H 0.0432 0.2145 0.2484 0.028 Uiso 1 1 calc R . . . .
N4 N 0.1416(2) 0.1091(7) 0.0493(7) 0.0298(16) Uani 1 1 d . . . . .
H4A H 0.1639 0.0456 0.0490 0.036 Uiso 1 1 calc R . . . .
H4B H 0.1185 0.0801 -0.0028 0.036 Uiso 1 1 calc R . . . .
N5 N 0.0991(2) -0.0452(6) 0.2499(7) 0.0243(15) Uani 1 1 d . . . . .
N6 N 0.1803(2) 0.0847(6) 0.2851(7) 0.0236(14) Uani 1 1 d . . . . .
C1 C 0.1488(3) 0.3696(7) 0.3132(9) 0.0255(18) Uani 1 1 d . . . . .
H1A H 0.1501 0.4606 0.3086 0.031 Uiso 1 1 calc R . . . .
H1B H 0.1771 0.3387 0.3332 0.031 Uiso 1 1 calc R . . . .
C2 C 0.1180(3) 0.3311(8) 0.4112(9) 0.0301(18) Uani 1 1 d . . . . .
H2C H 0.1291 0.3549 0.4913 0.036 Uiso 1 1 calc R . . . .
H2D H 0.0911 0.3742 0.3989 0.036 Uiso 1 1 calc R . . . .
C3 C 0.0976(2) 0.3847(6) 0.1469(9) 0.0228(16) Uani 1 1 d . . . . .
H3C H 0.1065 0.4430 0.0831 0.027 Uiso 1 1 calc R . . . .
H3D H 0.0849 0.4331 0.2132 0.027 Uiso 1 1 calc R . . . .
C4 C 0.0648(3) 0.2969(8) 0.0951(9) 0.0291(19) Uani 1 1 d . . . . .
H4C H 0.0377 0.3403 0.0865 0.035 Uiso 1 1 calc R . . . .
H4D H 0.0736 0.2682 0.0141 0.035 Uiso 1 1 calc R . . . .
C5 C 0.1696(3) 0.3153(8) 0.1051(9) 0.030(2) Uani 1 1 d . . . . .
H5A H 0.1956 0.2871 0.1451 0.035 Uiso 1 1 calc R . . . .
H5B H 0.1745 0.3993 0.0732 0.035 Uiso 1 1 calc R . . . .
C6 C 0.1587(3) 0.2281(9) 0.0008(9) 0.037(2) Uani 1 1 d . . . . .
H6A H 0.1377 0.2673 -0.0523 0.044 Uiso 1 1 calc R . . . .
H6B H 0.1841 0.2115 -0.0478 0.044 Uiso 1 1 calc R . . . .
C7 C 0.0831(2) -0.1368(7) 0.2352(9) 0.0241(15) Uani 1 1 d . . . . .
C8 C 0.0629(3) -0.2563(7) 0.2172(10) 0.035(2) Uani 1 1 d . . . . .
H8A H 0.0440 -0.2516 0.1476 0.053 Uiso 1 1 calc GR . . . .
H8B H 0.0468 -0.2780 0.2896 0.053 Uiso 1 1 calc GR . . . .
H8C H 0.0842 -0.3194 0.2024 0.053 Uiso 1 1 calc GR . . . .
C9 C 0.2119(2) 0.0654(7) 0.3255(8) 0.0207(16) Uani 1 1 d . . . . .
C10 C 0.2527(2) 0.0398(8) 0.3803(10) 0.030(2) Uani 1 1 d . . . . .
H10A H 0.2742 0.0396 0.3174 0.045 Uiso 1 1 calc GR . . . .
H10B H 0.2519 -0.0409 0.4199 0.045 Uiso 1 1 calc GR . . . .
H10C H 0.2591 0.1035 0.4401 0.045 Uiso 1 1 calc GR . . . .
Cl1 Cl 0.20192(5) 0.24686(17) 0.6463(2) 0.0243(4) Uani 1 1 d . . . . .
O1 O 0.1693(2) 0.3222(7) 0.6949(8) 0.050(2) Uani 1 1 d . . . . .
O2 O 0.22776(17) 0.1997(5) 0.7426(6) 0.0321(14) Uani 1 1 d . . . . .
O3 O 0.2275(2) 0.3153(7) 0.5645(8) 0.054(2) Uani 1 1 d . . . . .
O4 O 0.1831(2) 0.1450(6) 0.5823(6) 0.0368(15) Uani 1 1 d . . . . .
Cl2 Cl 0.5000 0.0526(2) 0.9121(3) 0.0247(6) Uani 1 2 d S T P . .
O5 O 0.5000 0.0697(11) 1.0387(12) 0.064(3) Uani 1 2 d S T P . .
O6 O 0.5000 0.1666(11) 0.8510(14) 0.062(4) Uani 1 2 d S T P . .
O7 O 0.53634(19) -0.0179(6) 0.8797(9) 0.048(2) Uani 1 1 d . . . . .
Cl3 Cl 0.0000 -0.0019(2) 0.4409(3) 0.0215(5) Uani 1 2 d S T P . .
O8 O 0.03708(19) 0.0402(6) 0.5024(7) 0.0390(17) Uani 1 1 d . . . . .
O9 O 0.0000 0.0397(9) 0.3198(9) 0.034(2) Uani 1 2 d S T P . .
O10 O 0.0000 -0.1352(8) 0.4418(10) 0.038(2) Uani 1 2 d S T P . .


_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
Ni1 N1 2.083(6) . ?
Ni1 N2 2.100(8) . ?
Ni1 N3 2.074(6) . ?
Ni1 N4 2.132(8) . ?
Ni1 N5 2.078(6) . ?
Ni1 N6 2.118(6) . ?
N1 C1 1.498(12) . ?
N1 C3 1.493(9) . ?
N1 C5 1.477(11) . ?
N2 H2A 0.9900 . ?
N2 H2B 0.9900 . ?
N2 C2 1.485(11) . ?
N3 H3A 0.9900 . ?
N3 H3B 0.9900 . ?
N3 C4 1.472(10) . ?
N4 H4A 0.9900 . ?
N4 H4B 0.9900 . ?
N4 C6 1.501(12) . ?
N5 C7 1.131(10) . ?
N6 C9 1.126(10) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.523(13) . ?
C2 H2C 0.9900 . ?
C2 H2D 0.9900 . ?
C3 H3C 0.9900 . ?
C3 H3D 0.9900 . ?
C3 C4 1.529(11) . ?
C4 H4C 0.9900 . ?
C4 H4D 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.533(14) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.464(10) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.464(10) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
Cl1 O1 1.429(7) . ?
Cl1 O2 1.443(6) . ?
Cl1 O3 1.429(7) . ?
Cl1 O4 1.444(7) . ?
Cl2 O5 1.413(14) . ?
Cl2 O6 1.410(12) . ?
Cl2 O7 1.437(6) 3_655 ?
Cl2 O7 1.437(6) . ?
Cl3 O8 1.442(6) . ?
Cl3 O8 1.442(6) 3 ?
Cl3 O9 1.415(10) . ?
Cl3 O10 1.447(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
N1 Ni1 N2 84.8(3) . . ?
N1 Ni1 N4 82.7(3) . . ?
N1 Ni1 N6 94.6(2) . . ?
N2 Ni1 N4 164.2(3) . . ?
N2 Ni1 N6 85.5(3) . . ?
N3 Ni1 N1 83.9(2) . . ?
N3 Ni1 N2 93.3(3) . . ?
N3 Ni1 N4 94.9(3) . . ?
N3 Ni1 N5 91.1(2) . . ?
N3 Ni1 N6 178.2(3) . . ?
N5 Ni1 N1 174.1(3) . . ?
N5 Ni1 N2 98.7(3) . . ?
N5 Ni1 N4 94.6(3) . . ?
N5 Ni1 N6 90.4(3) . . ?
N6 Ni1 N4 86.0(3) . . ?
C1 N1 Ni1 105.1(5) . . ?
C3 N1 Ni1 109.3(4) . . ?
C3 N1 C1 111.2(6) . . ?
C5 N1 Ni1 106.5(5) . . ?
C5 N1 C1 112.1(6) . . ?
C5 N1 C3 112.2(7) . . ?
Ni1 N2 H2A 110.0 . . ?
Ni1 N2 H2B 110.0 . . ?
H2A N2 H2B 108.4 . . ?
C2 N2 Ni1 108.3(6) . . ?
C2 N2 H2A 110.0 . . ?
C2 N2 H2B 110.0 . . ?
Ni1 N3 H3A 110.2 . . ?
Ni1 N3 H3B 110.2 . . ?
H3A N3 H3B 108.5 . . ?
C4 N3 Ni1 107.5(5) . . ?
C4 N3 H3A 110.2 . . ?
C4 N3 H3B 110.2 . . ?
Ni1 N4 H4A 109.7 . . ?
Ni1 N4 H4B 109.7 . . ?
H4A N4 H4B 108.2 . . ?
C6 N4 Ni1 109.8(5) . . ?
C6 N4 H4A 109.7 . . ?
C6 N4 H4B 109.7 . . ?
C7 N5 Ni1 162.8(7) . . ?
C9 N6 Ni1 172.5(7) . . ?
N1 C1 H1A 109.7 . . ?
N1 C1 H1B 109.7 . . ?
N1 C1 C2 109.6(6) . . ?
H1A C1 H1B 108.2 . . ?
C2 C1 H1A 109.7 . . ?
C2 C1 H1B 109.7 . . ?
N2 C2 C1 110.5(7) . . ?
N2 C2 H2C 109.6 . . ?
N2 C2 H2D 109.6 . . ?
C1 C2 H2C 109.6 . . ?
C1 C2 H2D 109.6 . . ?
H2C C2 H2D 108.1 . . ?
N1 C3 H3C 109.1 . . ?
N1 C3 H3D 109.1 . . ?
N1 C3 C4 112.4(6) . . ?
H3C C3 H3D 107.9 . . ?
C4 C3 H3C 109.1 . . ?
C4 C3 H3D 109.1 . . ?
N3 C4 C3 109.2(7) . . ?
N3 C4 H4C 109.8 . . ?
N3 C4 H4D 109.8 . . ?
C3 C4 H4C 109.8 . . ?
C3 C4 H4D 109.8 . . ?
H4C C4 H4D 108.3 . . ?
N1 C5 H5A 109.6 . . ?
N1 C5 H5B 109.6 . . ?
N1 C5 C6 110.2(7) . . ?
H5A C5 H5B 108.1 . . ?
C6 C5 H5A 109.6 . . ?
C6 C5 H5B 109.6 . . ?
N4 C6 C5 110.2(7) . . ?
N4 C6 H6A 109.6 . . ?
N4 C6 H6B 109.6 . . ?
C5 C6 H6A 109.6 . . ?
C5 C6 H6B 109.6 . . ?
H6A C6 H6B 108.1 . . ?
N5 C7 C8 179.2(10) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N6 C9 C10 178.9(10) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O1 Cl1 O2 110.0(5) . . ?
O1 Cl1 O4 108.6(4) . . ?
O2 Cl1 O4 109.2(4) . . ?
O3 Cl1 O1 111.0(5) . . ?
O3 Cl1 O2 108.9(4) . . ?
O3 Cl1 O4 109.0(5) . . ?
O5 Cl2 O7 108.5(5) . . ?
O5 Cl2 O7 108.5(5) . 3_655 ?
O6 Cl2 O5 111.1(9) . . ?
O6 Cl2 O7 110.3(5) . . ?
O6 Cl2 O7 110.3(5) . 3_655 ?
O7 Cl2 O7 107.9(6) 3_655 . ?
O8 Cl3 O8 110.6(6) 3 . ?
O8 Cl3 O10 108.3(4) . . ?
O8 Cl3 O10 108.3(4) 3 . ?
O9 Cl3 O8 110.2(4) . . ?
O9 Cl3 O8 110.2(4) . 3 ?
O9 Cl3 O10 109.0(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 N1 C1 C2 -45.4(7) . . . . ?
Ni1 N1 C3 C4 -20.8(9) . . . . ?
Ni1 N1 C5 C6 48.1(8) . . . . ?
Ni1 N2 C2 C1 -29.3(8) . . . . ?
Ni1 N3 C4 C3 -43.6(8) . . . . ?
Ni1 N4 C6 C5 20.6(8) . . . . ?
N1 C1 C2 N2 51.3(9) . . . . ?
N1 C3 C4 N3 43.5(10) . . . . ?
N1 C5 C6 N4 -46.3(9) . . . . ?
C1 N1 C3 C4 -136.5(7) . . . . ?
C1 N1 C5 C6 162.6(7) . . . . ?
C3 N1 C1 C2 72.8(8) . . . . ?
C3 N1 C5 C6 -71.4(8) . . . . ?
C5 N1 C1 C2 -160.7(6) . . . . ?
C5 N1 C3 C4 97.1(8) . . . . ?

_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_LIMe_lc-48
_database_code_depnum_ccdc_archive 'CCDC 1517787'
# end Validation Reply Form

#Added by publCIF (Do 17. Nov 08:55:23 2016)


_audit_update_record             
;
2017-02-03 deposited with the CCDC.
2017-02-06 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT410_I                   
;
PROBLEM: Short Intra H...H Contact  H15A   ..  H30B    ..       1.66 Ang.  
RESPONSE: H-atoms in different parts of the disordered structure
;
_publcif_datablock.id            {fb2c7a0f-1e6a-4f73-aa71-1263c903c4ab}
_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H48 N8'
_chemical_formula_sum            'C39 H48 N8'
_chemical_formula_weight         628.8618

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'
N N 0.0061 0.0033 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pna21
_symmetry_space_group_name_Hall  'P 2c -2n'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z'

_cell_length_a                   14.4185(18)
_cell_length_b                   20.046(3)
_cell_length_c                   12.574(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3634.3(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    2745
_cell_measurement_theta_min      5.6
_cell_measurement_theta_max      47.3

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1160
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.9500
_exptl_absorpt_correction_T_max  0.9925
_exptl_absorpt_process_details   
;
 [X-Red (Stoe & Cie, 2001) and X-Shape (Stoe & Cie, 1999)]
;

_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'STOE IPDS I'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26225
_diffrn_reflns_av_R_equivalents  0.1620
_diffrn_reflns_av_sigmaI/netI    0.3868
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.83
_diffrn_reflns_theta_max         28.25
_reflns_number_total             8835
_reflns_number_gt                4308
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_structure_solution    'SIR92 (Altomare 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond (Brandenburg 2011)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'


_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0729P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8835
_refine_ls_number_parameters     452
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.3006
_refine_ls_R_factor_gt           0.0595
_refine_ls_wR_factor_ref         0.1933
_refine_ls_wR_factor_gt          0.1318
_refine_ls_goodness_of_fit_ref   0.540
_refine_ls_restrained_S_all      0.540
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N3A N -0.8822(11) -0.6564(8) 0.4462(12) 0.0613(10) Uani 0.458(4) 1 d P A 1
N15A N -0.9725(10) -0.3126(9) 0.4675(12) 0.0636(10) Uani 0.458(4) 1 d P A 1
N17A N -0.5868(11) -0.6377(8) 0.5389(13) 0.0613(10) Uani 0.458(4) 1 d P A 1
N27A N -0.6872(9) -0.2835(8) 0.5562(9) 0.0636(10) Uani 0.458(4) 1 d P A 1
N32A N -0.7884(8) -0.6612(8) 0.7891(10) 0.0613(10) Uani 0.458(4) 1 d P A 1
N42A N -0.8809(10) -0.3017(8) 0.7931(12) 0.0636(10) Uani 0.458(4) 1 d P A 1
C9A C -1.0368(8) -0.4418(5) 0.5280(9) 0.051(4) Uani 0.458(4) 1 d PG A 1
H9A H -1.0757 -0.4064 0.5453 0.062 Uiso 0.458(4) 1 calc PR A 1
C10A C -0.9524(8) -0.4297(4) 0.4783(9) 0.060(2) Uani 0.458(4) 1 d PG A 1
C11A C -0.8942(7) -0.4826(5) 0.4525(10) 0.039(5) Uani 0.458(4) 1 d PG A 1
H11A H -0.8377 -0.4745 0.4193 0.047 Uiso 0.458(4) 1 calc PR A 1
C5A C -0.9206(7) -0.5476(5) 0.4763(10) 0.060(2) Uani 0.458(4) 1 d PG A 1
C6A C -1.0050(8) -0.5597(5) 0.5260(10) 0.067(5) Uani 0.458(4) 1 d PG A 1
H6A H -1.0227 -0.6032 0.5419 0.080 Uiso 0.458(4) 1 calc PR A 1
C7A C -1.0632(6) -0.5068(6) 0.5518(9) 0.060(2) Uani 0.458(4) 1 d PG A 1
C25A C -0.6593(10) -0.4665(5) 0.5784(6) 0.061(7) Uani 0.458(4) 1 d PG A 1
H25A H -0.6698 -0.4688 0.6512 0.073 Uiso 0.458(4) 1 calc PR A 1
C19A C -0.6389(9) -0.5241(4) 0.5215(8) 0.047(4) Uani 0.458(4) 1 d PG A 1
C20A C -0.6232(8) -0.5207(4) 0.4126(8) 0.035(4) Uani 0.458(4) 1 d PG A 1
H20A H -0.6095 -0.5593 0.3746 0.043 Uiso 0.458(4) 1 calc PR A 1
C21A C -0.6278(9) -0.4596(6) 0.3605(6) 0.072(7) Uani 0.458(4) 1 d PG A 1
C23A C -0.6481(9) -0.4020(4) 0.4174(8) 0.051(5) Uani 0.458(4) 1 d PG A 1
H23A H -0.6512 -0.3611 0.3825 0.061 Uiso 0.458(4) 1 calc PR A 1
C24A C -0.6639(9) -0.4054(4) 0.5263(8) 0.044(4) Uani 0.458(4) 1 d PG A 1
C40A C -0.8709(7) -0.4831(6) 0.7643(9) 0.044(5) Uani 0.458(4) 1 d PG A 1
H40A H -0.9254 -0.4882 0.7256 0.053 Uiso 0.458(4) 1 calc PR A 1
C34A C -0.8179(9) -0.5387(4) 0.7902(10) 0.073(5) Uani 0.458(4) 1 d PG A 1
C35A C -0.7364(8) -0.5312(5) 0.8480(9) 0.062(2) Uani 0.458(4) 1 d PG A 1
H35A H -0.7010 -0.5684 0.8654 0.074 Uiso 0.458(4) 1 calc PR A 1
C38A C -0.7079(7) -0.4680(6) 0.8799(9) 0.054(5) Uani 0.458(4) 1 d PG A 1
C39A C -0.7608(8) -0.4124(5) 0.8540(9) 0.062(2) Uani 0.458(4) 1 d PG A 1
H39A H -0.7417 -0.3702 0.8753 0.074 Uiso 0.458(4) 1 calc PR A 1
C36A C -0.8424(8) -0.4200(5) 0.7962(10) 0.064(4) Uani 0.458(4) 1 d PG A 1
C37A C -0.6108(17) -0.4719(11) 0.947(3) 0.076(2) Uani 0.458(4) 1 d P A 1
H37A H -0.5909 -0.5175 0.9516 0.114 Uiso 0.458(4) 1 calc PR A 1
H37B H -0.6203 -0.4543 1.0169 0.114 Uiso 0.458(4) 1 calc PR A 1
H37C H -0.5642 -0.4461 0.9110 0.114 Uiso 0.458(4) 1 calc PR A 1
C8A C -1.151(2) -0.5158(18) 0.617(2) 0.076(2) Uani 0.458(4) 1 d P A 1
H8AA H -1.1802 -0.4733 0.6270 0.114 Uiso 0.458(4) 1 calc PR A 1
H8AB H -1.1354 -0.5346 0.6849 0.114 Uiso 0.458(4) 1 calc PR A 1
H8AC H -1.1924 -0.5452 0.5801 0.114 Uiso 0.458(4) 1 calc PR A 1
C22A C -0.6277(16) -0.4628(14) 0.243(2) 0.076(2) Uani 0.458(4) 1 d P A 1
H22A H -0.6404 -0.4193 0.2141 0.114 Uiso 0.458(4) 1 calc PR A 1
H22B H -0.6745 -0.4935 0.2190 0.114 Uiso 0.458(4) 1 calc PR A 1
H22C H -0.5680 -0.4776 0.2181 0.114 Uiso 0.458(4) 1 calc PR A 1
C9B C -0.8768(7) -0.4867(7) 0.4310(8) 0.078(8) Uani 0.542(4) 1 d PG A 2
H9B H -0.9330 -0.4929 0.4659 0.093 Uiso 0.542(4) 1 calc PR A 2
C10B C -0.8475(8) -0.4227(5) 0.4048(8) 0.060(2) Uani 0.542(4) 1 d PG A 2
C11B C -0.7635(8) -0.4134(5) 0.3527(8) 0.071(4) Uani 0.542(4) 1 d PG A 2
H11B H -0.7439 -0.3706 0.3352 0.085 Uiso 0.542(4) 1 calc PR A 2
C5B C -0.7088(7) -0.4681(6) 0.3266(8) 0.074(6) Uani 0.542(4) 1 d PG A 2
C7B C -0.7381(8) -0.5321(5) 0.3527(8) 0.070(4) Uani 0.542(4) 1 d PG A 2
H7B H -0.7015 -0.5687 0.3353 0.084 Uiso 0.542(4) 1 calc PR A 2
C6B C -0.8221(9) -0.5414(5) 0.4049(8) 0.060(2) Uani 0.542(4) 1 d PG A 2
C24B C -0.6656(8) -0.4025(4) 0.6725(8) 0.049(4) Uani 0.542(4) 1 d PG A 2
C25B C -0.6601(8) -0.4625(5) 0.6174(6) 0.052(5) Uani 0.542(4) 1 d PG A 2
H25B H -0.6722 -0.4636 0.5448 0.063 Uiso 0.542(4) 1 calc PR A 2
C20B C -0.6366(7) -0.5208(4) 0.6709(8) 0.039(3) Uani 0.542(4) 1 d PG A 2
C23B C -0.6186(7) -0.5191(4) 0.7795(8) 0.080(6) Uani 0.542(4) 1 d PG A 2
H23B H -0.6029 -0.5581 0.8152 0.096 Uiso 0.542(4) 1 calc PR A 2
C19B C -0.6241(8) -0.4591(6) 0.8345(6) 0.060(4) Uani 0.542(4) 1 d PG A 2
C21B C -0.6476(7) -0.4008(4) 0.7811(8) 0.061(5) Uani 0.542(4) 1 d PG A 2
H21B H -0.6513 -0.3607 0.8179 0.074 Uiso 0.542(4) 1 calc PR A 2
C40B C -0.8977(6) -0.4831(6) 0.7471(9) 0.109(9) Uani 0.542(4) 1 d PG A 2
H40B H -0.8418 -0.4750 0.7817 0.130 Uiso 0.542(4) 1 calc PR A 2
C39B C -0.9545(7) -0.4302(5) 0.7181(8) 0.056(3) Uani 0.542(4) 1 d PG A 2
C38B C -1.0381(6) -0.4423(5) 0.6664(8) 0.062(2) Uani 0.542(4) 1 d PG A 2
H38B H -1.0761 -0.4069 0.6470 0.074 Uiso 0.542(4) 1 calc PR A 2
C34B C -1.0648(6) -0.5074(5) 0.6437(9) 0.069(4) Uani 0.542(4) 1 d PG A 2
C35B C -1.0079(7) -0.5604(4) 0.6728(9) 0.062(2) Uani 0.542(4) 1 d PG A 2
H35B H -1.0258 -0.6039 0.6576 0.074 Uiso 0.542(4) 1 calc PR A 2
C36B C -0.9244(6) -0.5482(5) 0.7245(9) 0.059(4) Uani 0.542(4) 1 d PG A 2
N42B N -0.9771(8) -0.3093(8) 0.7256(11) 0.0636(10) Uani 0.542(4) 1 d P A 2
N17B N -0.5966(9) -0.6373(7) 0.6570(11) 0.0613(10) Uani 0.542(4) 1 d P A 2
N15B N -0.8871(8) -0.3079(7) 0.3901(10) 0.0636(10) Uani 0.542(4) 1 d P A 2
N3B N -0.8156(7) -0.6590(7) 0.4127(10) 0.0613(10) Uani 0.542(4) 1 d P A 2
N27B N -0.6868(8) -0.2868(7) 0.6638(9) 0.0636(10) Uani 0.542(4) 1 d P A 2
N32B N -0.8874(8) -0.6675(6) 0.7355(9) 0.0613(10) Uani 0.542(4) 1 d P A 2
C37B C -0.6015(16) -0.4472(9) 0.947(2) 0.076(2) Uani 0.542(4) 1 d P A 2
H37D H -0.6063 -0.4004 0.9617 0.114 Uiso 0.542(4) 1 calc PR A 2
H37E H -0.5393 -0.4620 0.9604 0.114 Uiso 0.542(4) 1 calc PR A 2
H37F H -0.6439 -0.4715 0.9908 0.114 Uiso 0.542(4) 1 calc PR A 2
C8B C -1.156(2) -0.5212(15) 0.5807(16) 0.076(2) Uani 0.542(4) 1 d P A 2
H8B1 H -1.1881 -0.4800 0.5693 0.114 Uiso 0.542(4) 1 calc PR A 2
H8B2 H -1.1943 -0.5512 0.6206 0.114 Uiso 0.542(4) 1 calc PR A 2
H8B3 H -1.1407 -0.5410 0.5134 0.114 Uiso 0.542(4) 1 calc PR A 2
C22B C -0.6087(13) -0.4515(12) 0.270(2) 0.076(2) Uani 0.542(4) 1 d P A 2
H22D H -0.6029 -0.4042 0.2602 0.114 Uiso 0.542(4) 1 calc PR A 2
H22E H -0.6054 -0.4735 0.2025 0.114 Uiso 0.542(4) 1 calc PR A 2
H22F H -0.5593 -0.4670 0.3150 0.114 Uiso 0.542(4) 1 calc PR A 2
N1 N -0.8684(2) -0.21426(19) 0.5987(10) 0.0745(12) Uani 1 1 d . . .
N2 N -0.7438(3) -0.73916(19) 0.5986(9) 0.0698(11) Uani 1 1 d . . .
C1 C -0.7889(9) -0.7668(7) 0.5037(11) 0.131(5) Uani 1 1 d . A .
H1A H -0.7422 -0.7888 0.4607 0.158 Uiso 1 1 calc R . .
H1B H -0.8332 -0.8004 0.5261 0.158 Uiso 1 1 calc R . .
C2 C -0.8370(9) -0.7180(5) 0.4377(9) 0.124(5) Uani 1 1 d . . .
H2A H -0.7914 -0.7090 0.3828 0.149 Uiso 0.458(4) 1 calc PR A 1
H2B H -0.8836 -0.7452 0.4031 0.149 Uiso 0.458(4) 1 calc PR A 1
H2C H -0.8461 -0.7405 0.3702 0.149 Uiso 0.542(4) 1 calc PR A 2
H2D H -0.8981 -0.7142 0.4693 0.149 Uiso 0.542(4) 1 calc PR A 2
C4 C -0.8544(7) -0.6029(4) 0.4347(8) 0.067(3) Uani 1 1 d . . .
H4A H -0.7974 -0.5938 0.4033 0.080 Uiso 0.458(4) 1 calc PR A 1
H4B H -0.9089 -0.6042 0.4741 0.080 Uiso 0.542(4) 1 calc PR A 2
C12 C -0.9151(7) -0.3617(5) 0.4390(8) 0.068(3) Uani 1 1 d . . .
H12A H -0.8604 -0.3559 0.4008 0.082 Uiso 0.458(4) 1 calc PR A 1
H12B H -0.9652 -0.3646 0.4854 0.082 Uiso 0.542(4) 1 calc PR A 2
C13 C -0.9415(7) -0.2465(5) 0.4298(6) 0.069(3) Uani 1 1 d . . .
H13A H -0.9833 -0.2299 0.3755 0.083 Uiso 0.458(4) 1 calc PR A 1
H13B H -0.8797 -0.2495 0.3998 0.083 Uiso 0.458(4) 1 calc PR A 1
H13C H -1.0052 -0.2620 0.4277 0.083 Uiso 0.542(4) 1 calc PR A 2
H13D H -0.9361 -0.2157 0.3706 0.083 Uiso 0.542(4) 1 calc PR A 2
C14 C -0.9416(5) -0.1978(4) 0.5301(7) 0.0986(14) Uani 1 1 d . A .
H14A H -0.9348 -0.1520 0.5064 0.118 Uiso 1 1 calc R . .
H14B H -1.0001 -0.2016 0.5676 0.118 Uiso 1 1 calc R . .
C15 C -0.6452(4) -0.7522(3) 0.6027(18) 0.148(4) Uani 1 1 d . A .
H15A H -0.6314 -0.7730 0.6706 0.178 Uiso 1 1 calc R . .
H15B H -0.6304 -0.7844 0.5476 0.178 Uiso 1 1 calc R . .
C16 C -0.5852(3) -0.6965(3) 0.5902(10) 0.0668(17) Uani 1 1 d . . .
H16A H -0.5722 -0.6837 0.6631 0.080 Uiso 0.458(4) 1 calc PR A 1
H16B H -0.5283 -0.7168 0.5647 0.080 Uiso 0.458(4) 1 calc PR A 1
H16C H -0.5900 -0.6821 0.5168 0.080 Uiso 0.542(4) 1 calc PR A 2
H16D H -0.5223 -0.7125 0.6004 0.080 Uiso 0.542(4) 1 calc PR A 2
C18 C -0.6278(3) -0.5858(2) 0.5991(11) 0.0657(15) Uani 1 1 d . . .
H18A H -0.6449 -0.5876 0.6704 0.079 Uiso 0.458(4) 1 calc PR A 1
H18B H -0.6423 -0.5878 0.5271 0.079 Uiso 0.542(4) 1 calc PR A 2
C26 C -0.6841(3) -0.3431(2) 0.6011(12) 0.0600(13) Uani 1 1 d . . .
H26A H -0.6934 -0.3483 0.6738 0.072 Uiso 0.458(4) 1 calc PR A 1
H26B H -0.6922 -0.3444 0.5278 0.072 Uiso 0.542(4) 1 calc PR A 2
C28 C -0.6991(3) -0.2271(2) 0.6096(14) 0.095(3) Uani 1 1 d . . .
H28A H -0.6456 -0.1994 0.5940 0.115 Uiso 0.458(4) 1 calc PR A 1
H28B H -0.6950 -0.2386 0.6844 0.115 Uiso 0.458(4) 1 calc PR A 1
H28C H -0.6808 -0.2370 0.5371 0.115 Uiso 0.542(4) 1 calc PR A 2
H28D H -0.6512 -0.1980 0.6376 0.115 Uiso 0.542(4) 1 calc PR A 2
C29 C -0.7805(3) -0.1840(3) 0.5986(14) 0.0986(14) Uani 1 1 d . A .
H29A H -0.7791 -0.1518 0.6561 0.118 Uiso 1 1 calc R . .
H29B H -0.7742 -0.1593 0.5327 0.118 Uiso 1 1 calc R . .
C30 C -0.7826(11) -0.7625(5) 0.6920(11) 0.169(7) Uani 1 1 d . A .
H30A H -0.8256 -0.7974 0.6717 0.203 Uiso 1 1 calc R . .
H30B H -0.7328 -0.7842 0.7307 0.203 Uiso 1 1 calc R . .
C31 C -0.8265(8) -0.7252(7) 0.7616(11) 0.133(5) Uani 1 1 d . . .
H31A H -0.8322 -0.7509 0.8267 0.160 Uiso 0.458(4) 1 calc PR A 1
H31B H -0.8888 -0.7179 0.7349 0.160 Uiso 0.458(4) 1 calc PR A 1
H31C H -0.7793 -0.7081 0.8093 0.160 Uiso 0.542(4) 1 calc PR A 2
H31D H -0.8642 -0.7555 0.8033 0.160 Uiso 0.542(4) 1 calc PR A 2
C33 C -0.8567(7) -0.6092(5) 0.7579(7) 0.076(3) Uani 1 1 d . . .
H33A H -0.9133 -0.6170 0.7245 0.091 Uiso 0.458(4) 1 calc PR A 1
H33B H -0.7998 -0.6024 0.7909 0.091 Uiso 0.542(4) 1 calc PR A 2
C41 C -0.9127(7) -0.3637(6) 0.7562(9) 0.081(3) Uani 1 1 d . . .
H41A H -0.9656 -0.3708 0.7154 0.097 Uiso 0.458(4) 1 calc PR A 1
H41B H -0.8567 -0.3585 0.7921 0.097 Uiso 0.542(4) 1 calc PR A 2
C43 C -0.9456(6) -0.2494(5) 0.7599(9) 0.095(4) Uani 1 1 d . . .
H43A H -0.9889 -0.2668 0.7079 0.114 Uiso 0.458(4) 1 calc PR A 1
H43B H -0.9805 -0.2333 0.8207 0.114 Uiso 0.458(4) 1 calc PR A 1
H43C H -0.9114 -0.2606 0.8240 0.114 Uiso 0.542(4) 1 calc PR A 2
H43D H -1.0014 -0.2272 0.7846 0.114 Uiso 0.542(4) 1 calc PR A 2
C44 C -0.8936(5) -0.1975(4) 0.7158(8) 0.0986(14) Uani 1 1 d . A .
H44A H -0.8374 -0.1910 0.7567 0.118 Uiso 1 1 calc R . .
H44B H -0.9292 -0.1564 0.7181 0.118 Uiso 1 1 calc R . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
N3A C4 1.154(16) . ?
N3A C2 1.400(18) . ?
N15A C12 1.336(17) . ?
N15A C13 1.477(18) . ?
N17A C16 1.345(16) . ?
N17A C18 1.416(17) . ?
N27A C26 1.321(17) . ?
N27A C28 1.327(16) . ?
N32A C31 1.438(18) . ?
N32A C33 1.487(16) . ?
N42A C41 1.403(18) . ?
N42A C43 1.464(17) . ?
C9A C10A 1.3900 . ?
C9A C7A 1.3900 . ?
C9A H9A 0.9300 . ?
C10A C11A 1.3900 . ?
C10A C12 1.546(13) . ?
C11A C5A 1.3900 . ?
C11A H11A 0.9300 . ?
C5A C6A 1.3900 . ?
C5A C4 1.554(12) . ?
C6A C7A 1.3900 . ?
C6A H6A 0.9300 . ?
C7A C8A 1.52(3) . ?
C25A C19A 1.3900 . ?
C25A C24A 1.3900 . ?
C25A H25A 0.9300 . ?
C19A C20A 1.3900 . ?
C19A C18 1.583(12) . ?
C20A C21A 1.3900 . ?
C20A H20A 0.9300 . ?
C21A C23A 1.3900 . ?
C21A C22A 1.49(3) . ?
C23A C24A 1.3900 . ?
C23A H23A 0.9300 . ?
C24A C26 1.592(12) . ?
C40A C34A 1.3900 . ?
C40A C36A 1.3900 . ?
C40A H40A 0.9300 . ?
C34A C35A 1.3900 . ?
C34A C33 1.573(12) . ?
C35A C38A 1.3900 . ?
C35A H35A 0.9300 . ?
C38A C39A 1.3900 . ?
C38A C37A 1.63(3) . ?
C39A C36A 1.3900 . ?
C39A H39A 0.9300 . ?
C36A C41 1.598(14) . ?
C37A H37A 0.9600 . ?
C37A H37B 0.9600 . ?
C37A H37C 0.9600 . ?
C8A H8AA 0.9600 . ?
C8A H8AB 0.9600 . ?
C8A H8AC 0.9600 . ?
C22A H22A 0.9600 . ?
C22A H22B 0.9600 . ?
C22A H22C 0.9600 . ?
C9B C10B 1.3900 . ?
C9B C6B 1.3900 . ?
C9B H9B 0.9300 . ?
C10B C11B 1.3900 . ?
C10B C12 1.621(13) . ?
C11B C5B 1.3900 . ?
C11B H11B 0.9300 . ?
C5B C7B 1.3900 . ?
C5B C22B 1.64(2) . ?
C7B C6B 1.3900 . ?
C7B H7B 0.9300 . ?
C6B C4 1.371(13) . ?
C24B C25B 1.3900 . ?
C24B C21B 1.3900 . ?
C24B C26 1.515(13) . ?
C25B C20B 1.3900 . ?
C25B H25B 0.9300 . ?
C20B C23B 1.3900 . ?
C20B C18 1.590(10) . ?
C23B C19B 1.3900 . ?
C23B H23B 0.9300 . ?
C19B C21B 1.3900 . ?
C19B C37B 1.46(2) . ?
C21B H21B 0.9300 . ?
C40B C39B 1.3900 . ?
C40B C36B 1.3900 . ?
C40B H40B 0.9300 . ?
C39B C38B 1.3900 . ?
C39B C41 1.540(14) . ?
C38B C34B 1.3900 . ?
C38B H38B 0.9300 . ?
C34B C35B 1.3900 . ?
C34B C8B 1.56(3) . ?
C35B C36B 1.3900 . ?
C35B H35B 0.9300 . ?
C36B C33 1.619(13) . ?
N42B C43 1.354(16) . ?
N42B C41 1.483(16) . ?
N17B C18 1.340(14) . ?
N17B C16 1.464(15) . ?
N15B C12 1.307(15) . ?
N15B C13 1.543(15) . ?
N3B C2 1.262(16) . ?
N3B C4 1.284(14) . ?
N27B C26 1.376(16) . ?
N27B C28 1.389(14) . ?
N32B C33 1.281(14) . ?
N32B C31 1.489(15) . ?
C37B H37D 0.9600 . ?
C37B H37E 0.9600 . ?
C37B H37F 0.9600 . ?
C8B H8B1 0.9600 . ?
C8B H8B2 0.9600 . ?
C8B H8B3 0.9600 . ?
C22B H22D 0.9600 . ?
C22B H22E 0.9600 . ?
C22B H22F 0.9600 . ?
N1 C14 1.402(9) . ?
N1 C29 1.405(5) . ?
N1 C44 1.553(12) . ?
N2 C30 1.382(12) . ?
N2 C15 1.447(6) . ?
N2 C1 1.466(13) . ?
C1 C2 1.458(16) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C4 H4A 0.9300 . ?
C4 H4B 0.9300 . ?
C12 H12A 0.9300 . ?
C12 H12B 0.9300 . ?
C13 C14 1.594(11) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 H13C 0.9700 . ?
C13 H13D 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.420(7) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 H16C 0.9700 . ?
C16 H16D 0.9700 . ?
C18 H18A 0.9300 . ?
C18 H18B 0.9300 . ?
C26 H26A 0.9300 . ?
C26 H26B 0.9300 . ?
C28 C29 1.464(6) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 H28C 0.9700 . ?
C28 H28D 0.9700 . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C31 1.313(16) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C31 H31C 0.9700 . ?
C31 H31D 0.9700 . ?
C33 H33A 0.9300 . ?
C33 H33B 0.9300 . ?
C41 H41A 0.9300 . ?
C41 H41B 0.9300 . ?
C43 C44 1.397(13) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C43 H43C 0.9700 . ?
C43 H43D 0.9700 . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?

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
C4 N3A C2 130.3(15) . . ?
C12 N15A C13 112.9(12) . . ?
C16 N17A C18 113.2(13) . . ?
C26 N27A C28 123.9(12) . . ?
C31 N32A C33 108.0(10) . . ?
C41 N42A C43 109.4(12) . . ?
C10A C9A C7A 120.0 . . ?
C10A C9A H9A 120.0 . . ?
C7A C9A H9A 120.0 . . ?
C11A C10A C9A 120.0 . . ?
C11A C10A C12 112.8(8) . . ?
C9A C10A C12 127.0(8) . . ?
C10A C11A C5A 120.0 . . ?
C10A C11A H11A 120.0 . . ?
C5A C11A H11A 120.0 . . ?
C6A C5A C11A 120.0 . . ?
C6A C5A C4 124.4(8) . . ?
C11A C5A C4 115.4(8) . . ?
C7A C6A C5A 120.0 . . ?
C7A C6A H6A 120.0 . . ?
C5A C6A H6A 120.0 . . ?
C6A C7A C9A 120.0 . . ?
C6A C7A C8A 122.5(16) . . ?
C9A C7A C8A 117.1(16) . . ?
C19A C25A C24A 120.0 . . ?
C19A C25A H25A 120.0 . . ?
C24A C25A H25A 120.0 . . ?
C20A C19A C25A 120.0 . . ?
C20A C19A C18 129.0(8) . . ?
C25A C19A C18 110.7(8) . . ?
C19A C20A C21A 120.0 . . ?
C19A C20A H20A 120.0 . . ?
C21A C20A H20A 120.0 . . ?
C20A C21A C23A 120.0 . . ?
C20A C21A C22A 115.7(13) . . ?
C23A C21A C22A 123.3(13) . . ?
C24A C23A C21A 120.0 . . ?
C24A C23A H23A 120.0 . . ?
C21A C23A H23A 120.0 . . ?
C23A C24A C25A 120.0 . . ?
C23A C24A C26 125.0(8) . . ?
C25A C24A C26 114.9(8) . . ?
C34A C40A C36A 120.0 . . ?
C34A C40A H40A 120.0 . . ?
C36A C40A H40A 120.0 . . ?
C35A C34A C40A 120.0 . . ?
C35A C34A C33 122.3(9) . . ?
C40A C34A C33 117.6(9) . . ?
C34A C35A C38A 120.0 . . ?
C34A C35A H35A 120.0 . . ?
C38A C35A H35A 120.0 . . ?
C35A C38A C39A 120.0 . . ?
C35A C38A C37A 111.0(11) . . ?
C39A C38A C37A 129.0(11) . . ?
C38A C39A C36A 120.0 . . ?
C38A C39A H39A 120.0 . . ?
C36A C39A H39A 120.0 . . ?
C39A C36A C40A 120.0 . . ?
C39A C36A C41 128.6(8) . . ?
C40A C36A C41 111.4(8) . . ?
C38A C37A H37A 109.5 . . ?
C38A C37A H37B 109.5 . . ?
H37A C37A H37B 109.5 . . ?
C38A C37A H37C 109.5 . . ?
H37A C37A H37C 109.5 . . ?
H37B C37A H37C 109.5 . . ?
C7A C8A H8AA 109.5 . . ?
C7A C8A H8AB 109.5 . . ?
H8AA C8A H8AB 109.5 . . ?
C7A C8A H8AC 109.5 . . ?
H8AA C8A H8AC 109.5 . . ?
H8AB C8A H8AC 109.5 . . ?
C21A C22A H22A 109.5 . . ?
C21A C22A H22B 109.5 . . ?
H22A C22A H22B 109.5 . . ?
C21A C22A H22C 109.5 . . ?
H22A C22A H22C 109.5 . . ?
H22B C22A H22C 109.5 . . ?
C10B C9B C6B 120.0 . . ?
C10B C9B H9B 120.0 . . ?
C6B C9B H9B 120.0 . . ?
C11B C10B C9B 120.0 . . ?
C11B C10B C12 123.2(9) . . ?
C9B C10B C12 116.8(9) . . ?
C10B C11B C5B 120.0 . . ?
C10B C11B H11B 120.0 . . ?
C5B C11B H11B 120.0 . . ?
C11B C5B C7B 120.0 . . ?
C11B C5B C22B 116.1(11) . . ?
C7B C5B C22B 123.8(11) . . ?
C5B C7B C6B 120.0 . . ?
C5B C7B H7B 120.0 . . ?
C6B C7B H7B 120.0 . . ?
C4 C6B C7B 123.1(10) . . ?
C4 C6B C9B 116.9(10) . . ?
C7B C6B C9B 120.0 . . ?
C25B C24B C21B 120.0 . . ?
C25B C24B C26 113.3(9) . . ?
C21B C24B C26 126.5(9) . . ?
C24B C25B C20B 120.0 . . ?
C24B C25B H25B 120.0 . . ?
C20B C25B H25B 120.0 . . ?
C25B C20B C23B 120.0 . . ?
C25B C20B C18 115.7(8) . . ?
C23B C20B C18 124.2(8) . . ?
C19B C23B C20B 120.0 . . ?
C19B C23B H23B 120.0 . . ?
C20B C23B H23B 120.0 . . ?
C23B C19B C21B 120.0 . . ?
C23B C19B C37B 127.3(11) . . ?
C21B C19B C37B 112.5(11) . . ?
C19B C21B C24B 120.0 . . ?
C19B C21B H21B 120.0 . . ?
C24B C21B H21B 120.0 . . ?
C39B C40B C36B 120.0 . . ?
C39B C40B H40B 120.0 . . ?
C36B C40B H40B 120.0 . . ?
C38B C39B C40B 120.0 . . ?
C38B C39B C41 129.5(8) . . ?
C40B C39B C41 110.4(8) . . ?
C34B C38B C39B 120.0 . . ?
C34B C38B H38B 120.0 . . ?
C39B C38B H38B 120.0 . . ?
C35B C34B C38B 120.0 . . ?
C35B C34B C8B 119.6(13) . . ?
C38B C34B C8B 120.3(13) . . ?
C34B C35B C36B 120.0 . . ?
C34B C35B H35B 120.0 . . ?
C36B C35B H35B 120.0 . . ?
C35B C36B C40B 120.0 . . ?
C35B C36B C33 120.8(8) . . ?
C40B C36B C33 119.2(8) . . ?
C43 N42B C41 111.1(11) . . ?
C18 N17B C16 110.6(11) . . ?
C12 N15B C13 110.5(11) . . ?
C2 N3B C4 131.3(13) . . ?
C26 N27B C28 115.4(11) . . ?
C33 N32B C31 117.2(11) . . ?
C19B C37B H37D 109.5 . . ?
C19B C37B H37E 109.5 . . ?
H37D C37B H37E 109.5 . . ?
C19B C37B H37F 109.5 . . ?
H37D C37B H37F 109.5 . . ?
H37E C37B H37F 109.5 . . ?
C34B C8B H8B1 109.5 . . ?
C34B C8B H8B2 109.5 . . ?
H8B1 C8B H8B2 109.5 . . ?
C34B C8B H8B3 109.5 . . ?
H8B1 C8B H8B3 109.5 . . ?
H8B2 C8B H8B3 109.5 . . ?
C5B C22B H22D 109.5 . . ?
C5B C22B H22E 109.5 . . ?
H22D C22B H22E 109.5 . . ?
C5B C22B H22F 109.5 . . ?
H22D C22B H22F 109.5 . . ?
H22E C22B H22F 109.5 . . ?
C14 N1 C29 125.2(9) . . ?
C14 N1 C44 110.9(6) . . ?
C29 N1 C44 96.8(10) . . ?
C30 N2 C15 107.8(12) . . ?
C30 N2 C1 112.6(6) . . ?
C15 N2 C1 113.4(12) . . ?
C2 C1 N2 114.9(10) . . ?
C2 C1 H1A 108.5 . . ?
N2 C1 H1A 108.5 . . ?
C2 C1 H1B 108.5 . . ?
N2 C1 H1B 108.5 . . ?
H1A C1 H1B 107.5 . . ?
N3B C2 N3A 46.1(8) . . ?
N3B C2 C1 130.9(11) . . ?
N3A C2 C1 140.3(11) . . ?
N3B C2 H2A 58.9 . . ?
N3A C2 H2A 102.0 . . ?
C1 C2 H2A 102.0 . . ?
N3B C2 H2B 125.8 . . ?
N3A C2 H2B 102.0 . . ?
C1 C2 H2B 102.0 . . ?
H2A C2 H2B 104.8 . . ?
N3B C2 H2C 104.5 . . ?
N3A C2 H2C 114.4 . . ?
C1 C2 H2C 104.5 . . ?
H2A C2 H2C 63.6 . . ?
H2B C2 H2C 41.5 . . ?
N3B C2 H2D 104.5 . . ?
N3A C2 H2D 58.4 . . ?
C1 C2 H2D 104.5 . . ?
H2A C2 H2D 153.2 . . ?
H2B C2 H2D 66.2 . . ?
H2C C2 H2D 105.7 . . ?
N3A C4 N3B 50.7(9) . . ?
N3A C4 C6B 171.4(13) . . ?
N3B C4 C6B 125.5(12) . . ?
N3A C4 C5A 114.0(13) . . ?
N3B C4 C5A 164.5(12) . . ?
C6B C4 C5A 70.0(8) . . ?
N3A C4 H4A 123.0 . . ?
N3B C4 H4A 72.4 . . ?
C6B C4 H4A 53.5 . . ?
C5A C4 H4A 123.0 . . ?
N3A C4 H4B 67.2 . . ?
N3B C4 H4B 117.3 . . ?
C6B C4 H4B 117.3 . . ?
C5A C4 H4B 47.2 . . ?
H4A C4 H4B 168.2 . . ?
N15B C12 N15A 73.0(11) . . ?
N15B C12 C10A 170.6(11) . . ?
N15A C12 C10A 110.4(11) . . ?
N15B C12 C10B 108.2(10) . . ?
N15A C12 C10B 178.6(12) . . ?
C10A C12 C10B 68.3(8) . . ?
N15B C12 H12A 52.5 . . ?
N15A C12 H12A 124.8 . . ?
C10A C12 H12A 124.8 . . ?
C10B C12 H12A 56.6 . . ?
N15B C12 H12B 125.9 . . ?
N15A C12 H12B 52.9 . . ?
C10A C12 H12B 58.3 . . ?
C10B C12 H12B 125.9 . . ?
H12A C12 H12B 171.6 . . ?
N15A C13 N15B 62.7(9) . . ?
N15A C13 C14 107.2(8) . . ?
N15B C13 C14 138.1(8) . . ?
N15A C13 H13A 110.3 . . ?
N15B C13 H13A 111.2 . . ?
C14 C13 H13A 110.3 . . ?
N15A C13 H13B 110.3 . . ?
N15B C13 H13B 49.9 . . ?
C14 C13 H13B 110.3 . . ?
H13A C13 H13B 108.5 . . ?
N15A C13 H13C 55.6 . . ?
N15B C13 H13C 102.6 . . ?
C14 C13 H13C 102.6 . . ?
H13A C13 H13C 60.1 . . ?
H13B C13 H13C 147.1 . . ?
N15A C13 H13D 147.3 . . ?
N15B C13 H13D 102.6 . . ?
C14 C13 H13D 102.6 . . ?
H13A C13 H13D 44.8 . . ?
H13B C13 H13D 70.6 . . ?
H13C C13 H13D 104.9 . . ?
N1 C14 C13 110.0(6) . . ?
N1 C14 H14A 109.7 . . ?
C13 C14 H14A 109.7 . . ?
N1 C14 H14B 109.7 . . ?
C13 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
C16 C15 N2 116.9(5) . . ?
C16 C15 H15A 108.1 . . ?
N2 C15 H15A 108.1 . . ?
C16 C15 H15B 108.1 . . ?
N2 C15 H15B 108.1 . . ?
H15A C15 H15B 107.3 . . ?
N17A C16 C15 137.1(11) . . ?
N17A C16 N17B 64.0(5) . . ?
C15 C16 N17B 120.4(11) . . ?
N17A C16 H16A 102.9 . . ?
C15 C16 H16A 102.9 . . ?
N17B C16 H16A 42.6 . . ?
N17A C16 H16B 102.9 . . ?
C15 C16 H16B 102.9 . . ?
N17B C16 H16B 128.6 . . ?
H16A C16 H16B 105.0 . . ?
N17A C16 H16C 44.0 . . ?
C15 C16 H16C 107.2 . . ?
N17B C16 H16C 107.2 . . ?
H16A C16 H16C 146.4 . . ?
H16B C16 H16C 82.5 . . ?
N17A C16 H16D 111.6 . . ?
C15 C16 H16D 107.2 . . ?
N17B C16 H16D 107.2 . . ?
H16A C16 H16D 77.4 . . ?
H16B C16 H16D 27.8 . . ?
H16C C16 H16D 106.9 . . ?
N17B C18 N17A 65.4(5) . . ?
N17B C18 C19A 165.8(9) . . ?
N17A C18 C19A 106.6(12) . . ?
N17B C18 C20B 110.5(12) . . ?
N17A C18 C20B 159.8(8) . . ?
C19A C18 C20B 72.6(4) . . ?
N17B C18 H18A 62.4 . . ?
N17A C18 H18A 126.7 . . ?
C19A C18 H18A 126.7 . . ?
C20B C18 H18A 57.6 . . ?
N17B C18 H18B 124.8 . . ?
N17A C18 H18B 62.7 . . ?
C19A C18 H18B 53.9 . . ?
C20B C18 H18B 124.8 . . ?
H18A C18 H18B 151.2 . . ?
N27A C26 N27B 60.3(5) . . ?
N27A C26 C24B 165.8(11) . . ?
N27B C26 C24B 108.1(12) . . ?
N27A C26 C24A 117.6(13) . . ?
N27B C26 C24A 170.8(8) . . ?
C24B C26 C24A 72.6(4) . . ?
N27A C26 H26A 121.2 . . ?
N27B C26 H26A 61.7 . . ?
C24B C26 H26A 49.7 . . ?
C24A C26 H26A 121.2 . . ?
N27A C26 H26B 66.2 . . ?
N27B C26 H26B 126.0 . . ?
C24B C26 H26B 126.0 . . ?
C24A C26 H26B 54.2 . . ?
H26A C26 H26B 162.4 . . ?
N27A C28 N27B 59.8(5) . . ?
N27A C28 C29 124.0(12) . . ?
N27B C28 C29 131.1(10) . . ?
N27A C28 H28A 106.3 . . ?
N27B C28 H28A 119.3 . . ?
C29 C28 H28A 106.3 . . ?
N27A C28 H28B 106.3 . . ?
N27B C28 H28B 46.6 . . ?
C29 C28 H28B 106.3 . . ?
H28A C28 H28B 106.4 . . ?
N27A C28 H28C 46.7 . . ?
N27B C28 H28C 104.5 . . ?
C29 C28 H28C 104.5 . . ?
H28A C28 H28C 73.1 . . ?
H28B C28 H28C 147.8 . . ?
N27A C28 H28D 127.1 . . ?
N27B C28 H28D 104.5 . . ?
C29 C28 H28D 104.5 . . ?
H28A C28 H28D 33.2 . . ?
H28B C28 H28D 75.4 . . ?
H28C C28 H28D 105.6 . . ?
N1 C29 C28 117.9(5) . . ?
N1 C29 H29A 107.8 . . ?
C28 C29 H29A 107.8 . . ?
N1 C29 H29B 107.8 . . ?
C28 C29 H29B 107.8 . . ?
H29A C29 H29B 107.2 . . ?
C31 C30 N2 124.7(9) . . ?
C31 C30 H30A 106.2 . . ?
N2 C30 H30A 106.2 . . ?
C31 C30 H30B 106.2 . . ?
N2 C30 H30B 106.2 . . ?
H30A C30 H30B 106.4 . . ?
C30 C31 N32A 119.0(11) . . ?
C30 C31 N32B 125.4(12) . . ?
N32A C31 N32B 65.4(8) . . ?
C30 C31 H31A 107.6 . . ?
N32A C31 H31A 107.6 . . ?
N32B C31 H31A 123.2 . . ?
C30 C31 H31B 107.6 . . ?
N32A C31 H31B 107.6 . . ?
N32B C31 H31B 42.3 . . ?
H31A C31 H31B 107.0 . . ?
C30 C31 H31C 106.0 . . ?
N32A C31 H31C 42.9 . . ?
N32B C31 H31C 106.0 . . ?
H31A C31 H31C 74.0 . . ?
H31B C31 H31C 144.1 . . ?
C30 C31 H31D 106.0 . . ?
N32A C31 H31D 130.0 . . ?
N32B C31 H31D 106.0 . . ?
H31A C31 H31D 33.2 . . ?
H31B C31 H31D 76.2 . . ?
H31C C31 H31D 106.3 . . ?
N32B C33 N32A 69.3(9) . . ?
N32B C33 C34A 177.5(11) . . ?
N32A C33 C34A 109.0(10) . . ?
N32B C33 C36B 115.1(10) . . ?
N32A C33 C36B 175.4(10) . . ?
C34A C33 C36B 66.7(8) . . ?
N32B C33 H33A 56.2 . . ?
N32A C33 H33A 125.5 . . ?
C34A C33 H33A 125.5 . . ?
C36B C33 H33A 58.8 . . ?
N32B C33 H33B 122.5 . . ?
N32A C33 H33B 53.2 . . ?
C34A C33 H33B 55.8 . . ?
C36B C33 H33B 122.5 . . ?
H33A C33 H33B 178.7 . . ?
N42A C41 N42B 68.8(10) . . ?
N42A C41 C39B 175.9(11) . . ?
N42B C41 C39B 108.1(10) . . ?
N42A C41 C36A 108.3(10) . . ?
N42B C41 C36A 176.3(12) . . ?
C39B C41 C36A 74.7(7) . . ?
N42A C41 H41A 125.9 . . ?
N42B C41 H41A 57.1 . . ?
C39B C41 H41A 51.3 . . ?
C36A C41 H41A 125.9 . . ?
N42A C41 H41B 57.2 . . ?
N42B C41 H41B 125.9 . . ?
C39B C41 H41B 125.9 . . ?
C36A C41 H41B 51.3 . . ?
H41A C41 H41B 174.8 . . ?
N42B C43 C44 135.5(11) . . ?
N42B C43 N42A 70.7(10) . . ?
C44 C43 N42A 107.8(9) . . ?
N42B C43 H43A 41.4 . . ?
C44 C43 H43A 110.1 . . ?
N42A C43 H43A 110.1 . . ?
N42B C43 H43B 111.8 . . ?
C44 C43 H43B 110.1 . . ?
N42A C43 H43B 110.1 . . ?
H43A C43 H43B 108.5 . . ?
N42B C43 H43C 103.3 . . ?
C44 C43 H43C 103.3 . . ?
N42A C43 H43C 43.5 . . ?
H43A C43 H43C 143.5 . . ?
H43B C43 H43C 71.8 . . ?
N42B C43 H43D 103.3 . . ?
C44 C43 H43D 103.3 . . ?
N42A C43 H43D 140.0 . . ?
H43A C43 H43D 81.2 . . ?
H43B C43 H43D 33.4 . . ?
H43C C43 H43D 105.2 . . ?
C43 C44 N1 109.9(7) . . ?
C43 C44 H44A 109.7 . . ?
N1 C44 H44A 109.7 . . ?
C43 C44 H44B 109.7 . . ?
N1 C44 H44B 109.7 . . ?
H44A C44 H44B 108.2 . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        28.25
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.161
_refine_diff_density_rms         0.038
####################################################################### 
# 
# 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_LAOH_FM645s
_database_code_depnum_ccdc_archive 'CCDC 1517780'

_audit_update_record             
;
2017-01-10 deposited with the CCDC.
2017-02-06 downloaded from the CCDC.
;
_publcif_datablock.id            {461670f7-4ba5-4a51-9fe2-e3d85a867d97}

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C36 H61 N8 O3, 2(Cl O4), 2(C2 H3 N), 4(Cl), 4(H2 O)'

_chemical_formula_sum            'C40 H75 Cl6 N10 O15'
_chemical_formula_weight         1148.8

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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.1345(2)
_cell_length_b                   14.5818(3)
_cell_length_c                   18.3859(4)
_cell_angle_alpha                107.412(2)
_cell_angle_beta                 101.170(2)
_cell_angle_gamma                102.173(2)
_cell_volume                     2676.69(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    10235
_cell_measurement_theta_min      .320
_cell_measurement_theta_max      .492

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_F_000             1214
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_absorpt_coefficient_mu    3.540
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.58476
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4372
_diffrn_reflns_number            51557
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.316
_diffrn_reflns_theta_max         76.360
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             9971
_reflns_number_gt                9177
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SIR92 (Altomare 1994)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Diamond (Brandenburg 2011)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0755P)²+5.5911P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9971
_refine_ls_number_parameters     655
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0571
_refine_ls_wR_factor_ref         0.1532
_refine_ls_wR_factor_gt          0.1496
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
O90 O 0.8791(4) 0.5752(4) 0.3782(3) 0.0649(7) Uani 0.740(3) 1 d . . P A 1
O91 O 0.7355(4) 0.5639(4) 0.2619(3) 0.0649(7) Uani 0.740(3) 1 d . . P A 1
O92 O 0.8463(4) 0.7170(4) 0.3569(3) 0.0649(7) Uani 0.740(3) 1 d . . P A 1
O93 O 0.7974(11) 0.5187(12) 0.3192(7) 0.0649(7) Uani 0.260(3) 1 d . . P A 2
O95 O 0.8874(11) 0.6609(12) 0.4247(8) 0.0649(7) Uani 0.260(3) 1 d . . P A 2
O94 O 0.8109(12) 0.6812(12) 0.3058(8) 0.0649(7) Uani 0.260(3) 1 d . . P A 2
Cl1 Cl 0.37089(5) 1.03973(4) 0.27714(3) 0.01739(13) Uani 1 1 d . . . . .
Cl2 Cl 0.71346(6) 1.23472(5) 0.43088(3) 0.02007(14) Uani 1 1 d . . . . .
Cl3 Cl 0.30393(6) 0.91013(5) 0.01025(4) 0.02196(14) Uani 1 1 d . . . . .
Cl4 Cl 0.37619(7) 0.46462(5) 0.07426(4) 0.02630(15) Uani 1 1 d . . . . .
Cl5 Cl 0.08464(6) 1.29922(5) 0.28807(4) 0.02662(15) Uani 1 1 d . . . . .
Cl6 Cl 0.78509(6) 0.61840(7) 0.34788(5) 0.03745(19) Uani 1 1 d . . . . .
O1 O 0.26230(17) 0.80516(13) 0.19117(11) 0.0201(4) Uani 1 1 d G . . . .
H1C H 0.270946 0.801651 0.145565 0.030 Uiso 1 1 d G U . . .
H1D H 0.285365 0.866307 0.221518 0.030 Uiso 1 1 d G U . . .
O2 O -0.09012(18) 1.01516(15) 0.34643(11) 0.0220(4) Uani 1 1 d . . . . .
H2 H -0.070392 1.076359 0.358984 0.033 Uiso 1 1 calc R U . . .
O3 O 0.55611(17) 1.09266(14) 0.61951(11) 0.0210(4) Uani 1 1 d . . . . .
H3 H 0.548080 1.042284 0.631461 0.031 Uiso 1 1 calc R U . . .
O4 O 0.3782(3) 0.8872(2) -0.04289(17) 0.0587(8) Uani 1 1 d . . . . .
O5 O 0.6375(2) 0.75641(14) -0.00453(11) 0.0240(4) Uani 1 1 d . . . . .
H5 H 0.622561 0.695305 -0.018082 0.036 Uiso 1 1 calc R U . . .
O6 O 0.3510(2) 1.01254(17) 0.06175(14) 0.0379(5) Uani 1 1 d . . . . .
O7 O -0.0271(2) 1.21374(17) 0.40448(13) 0.0307(4) Uani 1 1 d G . . . .
H7A H 0.002909 1.242255 0.375104 0.046 Uiso 1 1 d G U . . .
H7B H -0.101359 1.219949 0.404244 0.046 Uiso 1 1 d G U . . .
O8 O 0.1795(3) 0.8948(3) -0.0323(3) 0.138(3) Uani 1 1 d . . . . .
O9 O 0.6784(2) 0.61170(19) 0.37835(16) 0.0446(6) Uani 1 1 d . . . . .
O10 O -0.0801(2) 0.6474(2) -0.03014(13) 0.0399(6) Uani 1 1 d G . . . .
H10C H -0.158983 0.619757 -0.054214 0.060 Uiso 1 1 d G U . . .
H10D H -0.039500 0.657483 -0.063032 0.060 Uiso 1 1 d G U . . .
N11 N 0.45083(19) 1.27329(15) 0.24103(12) 0.0155(4) Uani 1 1 d . . . . .
N12 N 0.4321(2) 1.25587(15) 0.40176(12) 0.0153(4) Uani 1 1 d . . . . .
H12A H 0.410362 1.201005 0.358614 0.018 Uiso 1 1 calc R U . . .
H12B H 0.510827 1.263506 0.429488 0.018 Uiso 1 1 calc R U . . .
N13 N 0.58577(19) 1.10391(15) 0.19381(12) 0.0166(4) Uani 1 1 d . . . . .
H13A H 0.554270 1.079190 0.141301 0.020 Uiso 1 1 calc R U . . .
H13B H 0.521837 1.090260 0.214986 0.020 Uiso 1 1 calc R U . . .
N1 N 0.11441(19) 0.81333(15) 0.43854(12) 0.0162(4) Uani 1 1 d . . . . .
H1A H 0.175051 0.808761 0.475580 0.019 Uiso 1 1 calc R U . . .
H1B H 0.040891 0.771795 0.435420 0.019 Uiso 1 1 calc R U . . .
N2 N 0.39913(19) 0.66280(16) 0.21420(12) 0.0158(4) Uani 1 1 d . . . . .
H2A H 0.355840 0.708054 0.218103 0.019 Uiso 1 1 calc R U . . .
H2B H 0.373888 0.620726 0.164125 0.019 Uiso 1 1 calc R U . . .
N3 N 0.1537(2) 0.62712(15) 0.26020(12) 0.0160(4) Uani 1 1 d . . . . .
H3A H 0.185187 0.679334 0.239494 0.019 Uiso 1 1 calc R U . . .
N4 N 0.0044(2) 0.67144(16) 0.12523(12) 0.0178(4) Uani 1 1 d . . . . .
H4A H 0.009864 0.668519 0.076968 0.021 Uiso 1 1 calc R U . . .
H4B H 0.076491 0.714068 0.160016 0.021 Uiso 1 1 calc R U . . .
N5 N 0.1862(2) 1.13671(16) 0.17754(12) 0.0167(4) Uani 1 1 d . . . . .
H5A H 0.158982 1.173756 0.215339 0.020 Uiso 1 1 calc R U . . .
H5B H 0.246369 1.115008 0.200817 0.020 Uiso 1 1 calc R U . . .
O13 O 0.0588(3) 0.68274(19) -0.13134(14) 0.0431(6) Uani 1 1 d G . . . .
H13C H 0.094768 0.742511 -0.099204 0.065 Uiso 1 1 d G U . . .
H13D H 0.019214 0.683742 -0.175431 0.065 Uiso 1 1 d G U . . .
C1 C 0.2290(2) 0.99948(18) 0.48638(14) 0.0154(5) Uani 1 1 d . . . . .
C2 C 0.3421(2) 1.15585(19) 0.47910(14) 0.0173(5) Uani 1 1 d . . . . .
C3 C -0.0621(2) 0.9737(2) 0.27696(14) 0.0177(5) Uani 1 1 d . . . . .
C4 C 0.6018(2) 0.88221(19) 0.22143(14) 0.0167(5) Uani 1 1 d . . . . .
H4 H 0.593904 0.911603 0.271993 0.020 Uiso 1 1 calc R U . . .
C5 C 0.4503(2) 1.15861(18) 0.53303(14) 0.0169(5) Uani 1 1 d . . . . .
H5C H 0.524478 1.211270 0.548275 0.020 Uiso 1 1 calc R U . . .
C6 C -0.0926(2) 0.8698(2) 0.24563(15) 0.0186(5) Uani 1 1 d . . . . .
H6 H -0.129033 0.831262 0.272257 0.022 Uiso 1 1 calc R U . . .
C7 C 0.5731(2) 0.77839(19) 0.18786(14) 0.0157(5) Uani 1 1 d . . . . .
C8 C 0.0195(2) 0.98488(19) 0.16666(15) 0.0176(5) Uani 1 1 d . . . . .
N9 N 0.2085(2) 0.6312(2) 0.04550(15) 0.0319(6) Uani 1 1 d . . . . .
C10 C 0.3412(2) 1.2431(2) 0.45090(15) 0.0195(5) Uani 1 1 d . . . . .
H10A H 0.255431 1.233182 0.419827 0.023 Uiso 1 1 calc R U . . .
H10B H 0.363419 1.304237 0.496654 0.023 Uiso 1 1 calc R U . . .
C11 C 0.4474(2) 1.08235(19) 0.56428(14) 0.0166(5) Uani 1 1 d . . . . .
C12 C 0.5826(2) 0.73325(18) 0.11133(14) 0.0166(5) Uani 1 1 d . . . . .
H12 H 0.562850 0.663823 0.088700 0.020 Uiso 1 1 calc R U . . .
C13 C 0.6424(2) 0.94222(18) 0.17934(14) 0.0159(5) Uani 1 1 d . . . . .
C14 C 0.3372(2) 1.00340(18) 0.54203(14) 0.0160(5) Uani 1 1 d . . . . .
H14 H 0.335203 0.953480 0.563941 0.019 Uiso 1 1 calc R U . . .
C15 C -0.0684(2) 0.82368(19) 0.17458(15) 0.0182(5) Uani 1 1 d . . . . .
N16 N 0.3679(3) 0.5625(2) 0.44106(15) 0.0319(6) Uani 1 1 d . . . . .
C17 C 0.6222(2) 0.79404(19) 0.06949(14) 0.0172(5) Uani 1 1 d . . . . .
C18 C 0.4305(2) 1.34542(19) 0.37764(14) 0.0177(5) Uani 1 1 d . . . . .
H18A H 0.464061 1.405872 0.424508 0.021 Uiso 1 1 calc R U . . .
H18B H 0.342936 1.340996 0.353484 0.021 Uiso 1 1 calc R U . . .
C19 C 0.6423(2) 1.21548(18) 0.22094(15) 0.0180(5) Uani 1 1 d . . . . .
H19A H 0.713979 1.229893 0.199372 0.022 Uiso 1 1 calc R U . . .
H19B H 0.674272 1.242284 0.278296 0.022 Uiso 1 1 calc R U . . .
C20 C 0.1041(2) 0.91874(19) 0.46450(14) 0.0174(5) Uani 1 1 d . . . . .
H20A H 0.069633 0.929789 0.509943 0.021 Uiso 1 1 calc R U . . .
H20B H 0.043764 0.925482 0.422045 0.021 Uiso 1 1 calc R U . . .
C21 C 0.2324(2) 1.07576(19) 0.45517(14) 0.0175(5) Uani 1 1 d . . . . .
H21 H 0.160694 1.073092 0.418031 0.021 Uiso 1 1 calc R U . . .
C22 C 0.5089(2) 1.35293(18) 0.31968(14) 0.0172(5) Uani 1 1 d . . . . .
H22A H 0.518224 1.417750 0.313735 0.021 Uiso 1 1 calc R U . . .
H22B H 0.593560 1.349018 0.341227 0.021 Uiso 1 1 calc R U . . .
C23 C -0.0117(2) 0.8812(2) 0.13473(15) 0.0184(5) Uani 1 1 d . . . . .
H23 H 0.004897 0.849979 0.087192 0.022 Uiso 1 1 calc R U . . .
C24 C 0.6525(2) 0.89793(19) 0.10338(15) 0.0177(5) Uani 1 1 d . . . . .
H24 H 0.679457 0.937804 0.075168 0.021 Uiso 1 1 calc R U . . .
C25 C 0.3419(2) 1.29587(18) 0.19651(14) 0.0169(5) Uani 1 1 d . . . . .
H25A H 0.373545 1.339640 0.169494 0.020 Uiso 1 1 calc R U . . .
H25B H 0.301196 1.331164 0.233480 0.020 Uiso 1 1 calc R U . . .
C26 C 0.6849(2) 1.05472(19) 0.21774(16) 0.0200(5) Uani 1 1 d . . . . .
H26A H 0.706986 1.072442 0.274860 0.024 Uiso 1 1 calc R U . . .
H26B H 0.761459 1.081017 0.203980 0.024 Uiso 1 1 calc R U . . .
C27 C 0.5462(2) 1.26707(19) 0.19550(15) 0.0175(5) Uani 1 1 d . . . . .
H27A H 0.591684 1.334443 0.201156 0.021 Uiso 1 1 calc R U . . .
H27B H 0.501941 1.231100 0.139797 0.021 Uiso 1 1 calc R U . . .
C28 C 0.1444(2) 0.77918(19) 0.36064(14) 0.0181(5) Uani 1 1 d . . . . .
H28A H 0.220600 0.826734 0.361476 0.022 Uiso 1 1 calc R U . . .
H28B H 0.074249 0.775969 0.318527 0.022 Uiso 1 1 calc R U . . .
C29 C 0.3707(2) 0.60600(19) 0.26729(14) 0.0177(5) Uani 1 1 d . . . . .
H29A H 0.400329 0.651697 0.321945 0.021 Uiso 1 1 calc R U . . .
H29B H 0.416586 0.555769 0.262096 0.021 Uiso 1 1 calc R U . . .
C31 C -0.0063(2) 1.03124(19) 0.23784(15) 0.0185(5) Uani 1 1 d . . . . .
H31 H 0.014059 1.100818 0.259047 0.022 Uiso 1 1 calc R U . . .
C32 C 0.2436(2) 1.20122(19) 0.13597(14) 0.0179(5) Uani 1 1 d . . . . .
H32A H 0.177072 1.219066 0.105375 0.021 Uiso 1 1 calc R U . . .
H32B H 0.284237 1.164402 0.099754 0.021 Uiso 1 1 calc R U . . .
C33 C 0.0181(2) 0.57559(19) 0.21637(15) 0.0194(5) Uani 1 1 d . . . . .
H33A H -0.035278 0.611485 0.241982 0.023 Uiso 1 1 calc R U . . .
H33B H -0.003983 0.508332 0.217910 0.023 Uiso 1 1 calc R U . . .
C34 C 0.0766(2) 1.04793(19) 0.12301(14) 0.0185(5) Uani 1 1 d . . . . .
H34A H 0.106116 1.006794 0.082185 0.022 Uiso 1 1 calc R U . . .
H34B H 0.010973 1.071253 0.097229 0.022 Uiso 1 1 calc R U . . .
C35 C 0.5397(2) 0.7148(2) 0.23629(15) 0.0186(5) Uani 1 1 d . . . . .
H35A H 0.585824 0.664666 0.229228 0.022 Uiso 1 1 calc R U . . .
H35B H 0.567646 0.756885 0.291941 0.022 Uiso 1 1 calc R U . . .
C36 C -0.0083(3) 0.56958(19) 0.13070(15) 0.0205(5) Uani 1 1 d . . . . .
H36A H 0.051284 0.540210 0.106599 0.025 Uiso 1 1 calc R U . . .
H36B H -0.094112 0.526470 0.101616 0.025 Uiso 1 1 calc R U . . .
C37 C 0.1659(2) 0.67543(19) 0.34495(14) 0.0180(5) Uani 1 1 d . . . . .
H37A H 0.250415 0.682182 0.376025 0.022 Uiso 1 1 calc R U . . .
H37B H 0.103518 0.634045 0.360915 0.022 Uiso 1 1 calc R U . . .
C38 C 0.2292(2) 0.55527(19) 0.24705(15) 0.0186(5) Uani 1 1 d . . . . .
H38A H 0.199515 0.511309 0.191868 0.022 Uiso 1 1 calc R U . . .
H38B H 0.215229 0.514137 0.279169 0.022 Uiso 1 1 calc R U . . .
C40 C -0.1063(2) 0.7105(2) 0.14122(16) 0.0206(5) Uani 1 1 d . . . . .
H40A H -0.139085 0.684462 0.178460 0.025 Uiso 1 1 calc R U . . .
H40B H -0.174191 0.686579 0.092253 0.025 Uiso 1 1 calc R U . . .
O41 O 0.3120(6) 0.8485(3) 0.0549(3) 0.1110(19) Uani 1 1 d . . . . .
C42 C 0.2745(3) 0.5337(2) 0.45514(16) 0.0285(6) Uani 1 1 d . . . . .
C43 C 0.2615(3) 0.6286(2) -0.00158(18) 0.0288(6) Uani 1 1 d . . . . .
C44 C 0.3286(3) 0.6225(3) -0.06272(19) 0.0364(7) Uani 1 1 d . . . . .
H44A H 0.268127 0.605245 -0.113097 0.055 Uiso 1 1 calc R U . . .
H44B H 0.372353 0.572056 -0.065025 0.055 Uiso 1 1 calc R U . . .
H44C H 0.389398 0.686212 -0.050325 0.055 Uiso 1 1 calc R U . . .
C45 C 0.1548(4) 0.4994(3) 0.4727(2) 0.0436(8) Uani 1 1 d . . . . .
H45A H 0.086653 0.470195 0.424463 0.065 Uiso 1 1 calc R U . . .
H45B H 0.137856 0.555269 0.508322 0.065 Uiso 1 1 calc R U . . .
H45C H 0.160985 0.450101 0.496993 0.065 Uiso 1 1 calc R 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
O90 Cl6 1.438(4) . ?
O91 Cl6 1.470(5) . ?
O92 Cl6 1.399(5) . ?
O93 Cl6 1.436(15) . ?
O95 Cl6 1.494(12) . ?
O94 Cl6 1.385(13) . ?
Cl3 O8 1.388(3) . ?
Cl3 O41 1.391(3) . ?
Cl3 O4 1.408(3) . ?
Cl3 O6 1.426(2) . ?
Cl6 O9 1.405(2) . ?
O1 H1C 0.8501 . ?
O1 H1D 0.8499 . ?
O2 C3 1.366(3) . ?
O2 H2 0.8200 . ?
O3 C11 1.369(3) . ?
O3 H3 0.8200 . ?
O5 C17 1.365(3) . ?
O5 H5 0.8200 . ?
O7 H7A 0.8498 . ?
O7 H7B 0.8499 . ?
O10 H10C 0.8500 . ?
O10 H10D 0.8505 . ?
N11 C22 1.474(3) . ?
N11 C27 1.475(3) . ?
N11 C25 1.481(3) . ?
N12 C10 1.500(3) . ?
N12 C18 1.502(3) . ?
N12 H12A 0.8900 . ?
N12 H12B 0.8900 . ?
N13 C19 1.501(3) . ?
N13 C26 1.504(3) . ?
N13 H13A 0.8900 . ?
N13 H13B 0.8900 . ?
N1 C28 1.497(3) . ?
N1 C20 1.503(3) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N2 C29 1.494(3) . ?
N2 C35 1.503(3) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N3 C38 1.470(3) . ?
N3 C37 1.471(3) . ?
N3 C33 1.477(3) . ?
N3 H3A 0.9800 . ?
N4 C36 1.497(3) . ?
N4 C40 1.506(3) . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N5 C32 1.498(3) . ?
N5 C34 1.501(3) . ?
N5 H5A 0.8900 . ?
N5 H5B 0.8900 . ?
O13 H13C 0.8498 . ?
O13 H13D 0.8501 . ?
C1 C21 1.393(4) . ?
C1 C14 1.400(3) . ?
C1 C20 1.514(3) . ?
C2 C5 1.388(3) . ?
C2 C21 1.390(4) . ?
C2 C10 1.512(3) . ?
C3 C31 1.387(4) . ?
C3 C6 1.389(4) . ?
C4 C7 1.391(3) . ?
C4 C13 1.394(4) . ?
C4 H4 0.9300 . ?
C5 C11 1.394(4) . ?
C5 H5C 0.9300 . ?
C6 C15 1.385(4) . ?
C6 H6 0.9300 . ?
C7 C12 1.399(3) . ?
C7 C35 1.507(3) . ?
C8 C23 1.386(4) . ?
C8 C31 1.397(4) . ?
C8 C34 1.512(3) . ?
N9 C43 1.135(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C14 1.388(3) . ?
C12 C17 1.395(3) . ?
C12 H12 0.9300 . ?
C13 C24 1.390(4) . ?
C13 C26 1.505(3) . ?
C14 H14 0.9300 . ?
C15 C23 1.401(4) . ?
C15 C40 1.509(4) . ?
N16 C42 1.145(4) . ?
C17 C24 1.391(4) . ?
C18 C22 1.516(3) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C27 1.511(3) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 H21 0.9300 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C32 1.521(3) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C37 1.532(3) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C38 1.512(3) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C31 H31 0.9300 . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 C36 1.517(4) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C42 C45 1.454(5) . ?
C43 C44 1.457(4) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?

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
O8 Cl3 O41 112.7(4) . . ?
O8 Cl3 O4 109.3(3) . . ?
O41 Cl3 O4 106.6(2) . . ?
O8 Cl3 O6 107.46(18) . . ?
O41 Cl3 O6 109.4(2) . . ?
O4 Cl3 O6 111.51(16) . . ?
O94 Cl6 O9 121.4(5) . . ?
O92 Cl6 O9 112.6(2) . . ?
O94 Cl6 O93 119.0(8) . . ?
O9 Cl6 O93 106.9(5) . . ?
O92 Cl6 O90 108.6(3) . . ?
O9 Cl6 O90 115.5(2) . . ?
O92 Cl6 O91 105.6(3) . . ?
O9 Cl6 O91 106.3(2) . . ?
O90 Cl6 O91 107.7(3) . . ?
O94 Cl6 O95 107.0(8) . . ?
O9 Cl6 O95 98.4(5) . . ?
O93 Cl6 O95 99.9(8) . . ?
H1C O1 H1D 109.4 . . ?
C3 O2 H2 109.5 . . ?
C11 O3 H3 109.5 . . ?
C17 O5 H5 109.5 . . ?
H7A O7 H7B 109.5 . . ?
H10C O10 H10D 109.4 . . ?
C22 N11 C27 109.88(19) . . ?
C22 N11 C25 110.05(19) . . ?
C27 N11 C25 108.61(18) . . ?
C10 N12 C18 111.05(19) . . ?
C10 N12 H12A 109.4 . . ?
C18 N12 H12A 109.4 . . ?
C10 N12 H12B 109.4 . . ?
C18 N12 H12B 109.4 . . ?
H12A N12 H12B 108.0 . . ?
C19 N13 C26 110.87(19) . . ?
C19 N13 H13A 109.5 . . ?
C26 N13 H13A 109.5 . . ?
C19 N13 H13B 109.5 . . ?
C26 N13 H13B 109.5 . . ?
H13A N13 H13B 108.1 . . ?
C28 N1 C20 114.72(19) . . ?
C28 N1 H1A 108.6 . . ?
C20 N1 H1A 108.6 . . ?
C28 N1 H1B 108.6 . . ?
C20 N1 H1B 108.6 . . ?
H1A N1 H1B 107.6 . . ?
C29 N2 C35 110.71(19) . . ?
C29 N2 H2A 109.5 . . ?
C35 N2 H2A 109.5 . . ?
C29 N2 H2B 109.5 . . ?
C35 N2 H2B 109.5 . . ?
H2A N2 H2B 108.1 . . ?
C38 N3 C37 111.80(19) . . ?
C38 N3 C33 109.76(19) . . ?
C37 N3 C33 110.14(19) . . ?
C38 N3 H3A 108.4 . . ?
C37 N3 H3A 108.4 . . ?
C33 N3 H3A 108.4 . . ?
C36 N4 C40 112.6(2) . . ?
C36 N4 H4A 109.1 . . ?
C40 N4 H4A 109.1 . . ?
C36 N4 H4B 109.1 . . ?
C40 N4 H4B 109.1 . . ?
H4A N4 H4B 107.8 . . ?
C32 N5 C34 113.20(19) . . ?
C32 N5 H5A 108.9 . . ?
C34 N5 H5A 108.9 . . ?
C32 N5 H5B 108.9 . . ?
C34 N5 H5B 108.9 . . ?
H5A N5 H5B 107.8 . . ?
H13C O13 H13D 109.5 . . ?
C21 C1 C14 119.7(2) . . ?
C21 C1 C20 118.8(2) . . ?
C14 C1 C20 121.3(2) . . ?
C5 C2 C21 119.8(2) . . ?
C5 C2 C10 119.9(2) . . ?
C21 C2 C10 120.2(2) . . ?
O2 C3 C31 122.5(2) . . ?
O2 C3 C6 117.3(2) . . ?
C31 C3 C6 120.2(2) . . ?
C7 C4 C13 120.1(2) . . ?
C7 C4 H4 120.0 . . ?
C13 C4 H4 120.0 . . ?
C2 C5 C11 119.9(2) . . ?
C2 C5 H5C 120.1 . . ?
C11 C5 H5C 120.1 . . ?
C15 C6 C3 119.7(2) . . ?
C15 C6 H6 120.1 . . ?
C3 C6 H6 120.1 . . ?
C4 C7 C12 120.5(2) . . ?
C4 C7 C35 119.6(2) . . ?
C12 C7 C35 119.8(2) . . ?
C23 C8 C31 119.9(2) . . ?
C23 C8 C34 120.2(2) . . ?
C31 C8 C34 119.8(2) . . ?
N12 C10 C2 113.3(2) . . ?
N12 C10 H10A 108.9 . . ?
C2 C10 H10A 108.9 . . ?
N12 C10 H10B 108.9 . . ?
C2 C10 H10B 108.9 . . ?
H10A C10 H10B 107.7 . . ?
O3 C11 C14 123.0(2) . . ?
O3 C11 C5 116.3(2) . . ?
C14 C11 C5 120.6(2) . . ?
C17 C12 C7 118.9(2) . . ?
C17 C12 H12 120.5 . . ?
C7 C12 H12 120.5 . . ?
C24 C13 C4 119.8(2) . . ?
C24 C13 C26 119.6(2) . . ?
C4 C13 C26 120.5(2) . . ?
C11 C14 C1 119.5(2) . . ?
C11 C14 H14 120.2 . . ?
C1 C14 H14 120.2 . . ?
C6 C15 C23 120.5(2) . . ?
C6 C15 C40 118.2(2) . . ?
C23 C15 C40 121.3(2) . . ?
O5 C17 C24 116.6(2) . . ?
O5 C17 C12 122.8(2) . . ?
C24 C17 C12 120.6(2) . . ?
N12 C18 C22 112.3(2) . . ?
N12 C18 H18A 109.2 . . ?
C22 C18 H18A 109.2 . . ?
N12 C18 H18B 109.2 . . ?
C22 C18 H18B 109.2 . . ?
H18A C18 H18B 107.9 . . ?
N13 C19 C27 112.3(2) . . ?
N13 C19 H19A 109.1 . . ?
C27 C19 H19A 109.1 . . ?
N13 C19 H19B 109.1 . . ?
C27 C19 H19B 109.1 . . ?
H19A C19 H19B 107.9 . . ?
N1 C20 C1 114.6(2) . . ?
N1 C20 H20A 108.6 . . ?
C1 C20 H20A 108.6 . . ?
N1 C20 H20B 108.6 . . ?
C1 C20 H20B 108.6 . . ?
H20A C20 H20B 107.6 . . ?
C2 C21 C1 120.5(2) . . ?
C2 C21 H21 119.7 . . ?
C1 C21 H21 119.7 . . ?
N11 C22 C18 112.8(2) . . ?
N11 C22 H22A 109.0 . . ?
C18 C22 H22A 109.0 . . ?
N11 C22 H22B 109.0 . . ?
C18 C22 H22B 109.0 . . ?
H22A C22 H22B 107.8 . . ?
C8 C23 C15 119.5(2) . . ?
C8 C23 H23 120.2 . . ?
C15 C23 H23 120.2 . . ?
C13 C24 C17 120.1(2) . . ?
C13 C24 H24 119.9 . . ?
C17 C24 H24 119.9 . . ?
N11 C25 C32 112.0(2) . . ?
N11 C25 H25A 109.2 . . ?
C32 C25 H25A 109.2 . . ?
N11 C25 H25B 109.2 . . ?
C32 C25 H25B 109.2 . . ?
H25A C25 H25B 107.9 . . ?
N13 C26 C13 113.7(2) . . ?
N13 C26 H26A 108.8 . . ?
C13 C26 H26A 108.8 . . ?
N13 C26 H26B 108.8 . . ?
C13 C26 H26B 108.8 . . ?
H26A C26 H26B 107.7 . . ?
N11 C27 C19 113.9(2) . . ?
N11 C27 H27A 108.8 . . ?
C19 C27 H27A 108.8 . . ?
N11 C27 H27B 108.8 . . ?
C19 C27 H27B 108.8 . . ?
H27A C27 H27B 107.7 . . ?
N1 C28 C37 109.7(2) . . ?
N1 C28 H28A 109.7 . . ?
C37 C28 H28A 109.7 . . ?
N1 C28 H28B 109.7 . . ?
C37 C28 H28B 109.7 . . ?
H28A C28 H28B 108.2 . . ?
N2 C29 C38 111.3(2) . . ?
N2 C29 H29A 109.4 . . ?
C38 C29 H29A 109.4 . . ?
N2 C29 H29B 109.4 . . ?
C38 C29 H29B 109.4 . . ?
H29A C29 H29B 108.0 . . ?
C3 C31 C8 120.1(2) . . ?
C3 C31 H31 119.9 . . ?
C8 C31 H31 119.9 . . ?
N5 C32 C25 109.77(19) . . ?
N5 C32 H32A 109.7 . . ?
C25 C32 H32A 109.7 . . ?
N5 C32 H32B 109.7 . . ?
C25 C32 H32B 109.7 . . ?
H32A C32 H32B 108.2 . . ?
N3 C33 C36 111.6(2) . . ?
N3 C33 H33A 109.3 . . ?
C36 C33 H33A 109.3 . . ?
N3 C33 H33B 109.3 . . ?
C36 C33 H33B 109.3 . . ?
H33A C33 H33B 108.0 . . ?
N5 C34 C8 112.1(2) . . ?
N5 C34 H34A 109.2 . . ?
C8 C34 H34A 109.2 . . ?
N5 C34 H34B 109.2 . . ?
C8 C34 H34B 109.2 . . ?
H34A C34 H34B 107.9 . . ?
N2 C35 C7 113.08(19) . . ?
N2 C35 H35A 109.0 . . ?
C7 C35 H35A 109.0 . . ?
N2 C35 H35B 109.0 . . ?
C7 C35 H35B 109.0 . . ?
H35A C35 H35B 107.8 . . ?
N4 C36 C33 111.1(2) . . ?
N4 C36 H36A 109.4 . . ?
C33 C36 H36A 109.4 . . ?
N4 C36 H36B 109.4 . . ?
C33 C36 H36B 109.4 . . ?
H36A C36 H36B 108.0 . . ?
N3 C37 C28 110.1(2) . . ?
N3 C37 H37A 109.6 . . ?
C28 C37 H37A 109.6 . . ?
N3 C37 H37B 109.6 . . ?
C28 C37 H37B 109.6 . . ?
H37A C37 H37B 108.2 . . ?
N3 C38 C29 112.8(2) . . ?
N3 C38 H38A 109.0 . . ?
C29 C38 H38A 109.0 . . ?
N3 C38 H38B 109.0 . . ?
C29 C38 H38B 109.0 . . ?
H38A C38 H38B 107.8 . . ?
N4 C40 C15 112.0(2) . . ?
N4 C40 H40A 109.2 . . ?
C15 C40 H40A 109.2 . . ?
N4 C40 H40B 109.2 . . ?
C15 C40 H40B 109.2 . . ?
H40A C40 H40B 107.9 . . ?
N16 C42 C45 178.5(3) . . ?
N9 C43 C44 178.5(3) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C42 C45 H45A 109.5 . . ?
C42 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C42 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?

_refine_diff_density_max         1.574
_refine_diff_density_min         -1.038
_refine_diff_density_rms         0.083

####################################################################### 
# 
# 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_Ni2LAOH-Me-ClO4-2_jo-007
_database_code_depnum_ccdc_archive 'CCDC 1517781'

_audit_update_record             
;
2017-01-25 deposited with the CCDC.
2017-02-06 downloaded from the CCDC.
;
_publcif_datablock.id            {87e2ab00-862c-4229-9c9c-bf9d653d4f73}

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H57 N8 Ni2 O3, 2(Cl O4), 2(C2 H3 N)'
_chemical_formula_sum            'C43 H63 Cl2 N10 Ni2 O11'
_chemical_formula_weight         1083.81

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1480 0.1590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3390 1.1120 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

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                   13.2094(10)
_cell_length_b                   14.0369(6)
_cell_length_c                   25.4984(19)
_cell_angle_alpha                90
_cell_angle_beta                 92.086(9)
_cell_angle_gamma                90
_cell_volume                     4724.8(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    8000
_cell_measurement_theta_min      5.9
_cell_measurement_theta_max      56.2

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_F_000             2276
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    0.981
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6989
_exptl_absorpt_correction_T_max  0.9092
_exptl_absorpt_process_details   
;
 [X-Red (Stoe & Cie, 2001) and X-Shape (Stoe & Cie, 1999)]
;
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'STOE IPDS I'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            42885
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         3.010
_diffrn_reflns_theta_max         28.132
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             10314
_reflns_number_gt                7729
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_structure_solution    'SIR92 (Altomare 1994)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Diamond (Brandenburg 2011)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1241P)²+4.6433P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_extinction_coef       0.0111(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         10314
_refine_ls_number_parameters     612
_refine_ls_number_restraints     50
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0713
_refine_ls_wR_factor_ref         0.2061
_refine_ls_wR_factor_gt          0.1941
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.117
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Cl1 Cl -0.31418(9) -0.13425(8) -0.46700(4) 0.0412(2) Uani 1 1 d D . . . .
O4 O -0.3322(3) -0.1071(3) -0.41441(15) 0.0560(9) Uani 1 1 d D . . . .
O5 O -0.3974(4) -0.1901(4) -0.4859(2) 0.0829(16) Uani 1 1 d D . . . .
O6 O -0.3042(3) -0.0516(3) -0.49865(18) 0.0621(11) Uani 1 1 d D . . . .
O7 O -0.2210(4) -0.1868(4) -0.46626(19) 0.0685(12) Uani 1 1 d D . . . .
Cl2A Cl -0.37614(8) -0.29503(13) -0.18261(5) 0.0571(4) Uani 0.555(6) 1 d D . P
A 1
O8A O -0.2704(4) -0.2981(10) -0.1789(6) 0.0724(9) Uani 0.555(6) 1 d D . P A 1
O1A O -0.4231(7) -0.2377(7) -0.1466(3) 0.0724(9) Uani 0.555(6) 1 d D . P A 1
O9A O -0.4100(6) -0.2803(7) -0.2351(2) 0.0724(9) Uani 0.555(6) 1 d D . P A 1
O10A O -0.4079(6) -0.3959(5) -0.1742(4) 0.0724(9) Uani 0.555(6) 1 d D . P A 1
Cl2B Cl -0.37614(8) -0.29503(13) -0.18261(5) 0.0571(4) Uani 0.445(6) 1 d D . P
A 2
O8B O -0.2717(5) -0.3115(12) -0.1804(7) 0.0724(9) Uani 0.445(6) 1 d D . P A 2
O1B O -0.4079(8) -0.2681(9) -0.1326(3) 0.0724(9) Uani 0.445(6) 1 d D . P A 2
O9B O -0.3800(7) -0.1972(6) -0.2086(4) 0.0724(9) Uani 0.445(6) 1 d D . P A 2
O10B O -0.4379(7) -0.3451(7) -0.2170(4) 0.0724(9) Uani 0.445(6) 1 d D . P A 2
Ni1 Ni -0.28283(3) -0.74441(3) -0.18585(2) 0.02469(14) Uani 1 1 d . . . . .
Ni2 Ni 0.01613(3) -0.75942(3) -0.16730(2) 0.02372(14) Uani 1 1 d . . . . .
O1 O -0.05101(19) -0.62995(18) -0.17628(10) 0.0267(5) Uani 1 1 d . . . . .
C60 C -0.1113(3) -0.5169(3) -0.11380(15) 0.0285(7) Uani 1 1 d . . . . .
O2 O -0.13847(17) -0.80801(18) -0.16125(10) 0.0244(5) Uani 1 1 d . . . . .
O3 O -0.19700(19) -0.6599(2) -0.23053(10) 0.0278(5) Uani 1 1 d . . . . .
N1 N 0.1529(2) -0.6839(2) -0.15939(13) 0.0265(6) Uani 1 1 d . . . . .
H404 H 0.182847 -0.697202 -0.124429 0.032 Uiso 1 1 calc R U . . .
N2 N 0.0379(2) -0.8019(2) -0.08602(12) 0.0260(6) Uani 1 1 d . . . . .
H403 H 0.064357 -0.746541 -0.066490 0.031 Uiso 1 1 calc R U . . .
N3 N -0.0147(2) -0.7758(2) -0.25226(12) 0.0262(6) Uani 1 1 d . . . . .
H401 H -0.083158 -0.802805 -0.253607 0.031 Uiso 1 1 calc R U . . .
N4 N 0.1130(2) -0.8758(2) -0.18099(13) 0.0272(6) Uani 1 1 d . . . . .
N5 N -0.4079(2) -0.6838(2) -0.22746(13) 0.0290(6) Uani 1 1 d . . . . .
H400 H -0.444047 -0.735263 -0.246142 0.035 Uiso 1 1 calc R U . . .
N6 N -0.2473(2) -0.6431(2) -0.12165(12) 0.0276(6) Uani 1 1 d . . . . .
H405 H -0.184183 -0.669393 -0.106351 0.033 Uiso 1 1 calc R U . . .
N9 N -0.3166(2) -0.8786(2) -0.22228(13) 0.0283(6) Uani 1 1 d . . . . .
H402 H -0.337550 -0.865322 -0.258815 0.034 Uiso 1 1 calc R U . . .
N10 N -0.3935(2) -0.7861(2) -0.13314(13) 0.0294(6) Uani 1 1 d . . . . .
C1 C -0.2205(3) -0.5397(3) -0.12827(16) 0.0308(7) Uani 1 1 d . . . . .
H1 H -0.263825 -0.501587 -0.106664 0.037 Uiso 1 1 calc R U . . .
H2 H -0.234263 -0.521683 -0.164555 0.037 Uiso 1 1 calc R U . . .
C2 C -0.1496(3) -0.6867(3) -0.36953(15) 0.0331(8) Uani 1 1 d . . . . .
H3 H -0.097690 -0.702875 -0.391535 0.040 Uiso 1 1 calc R U . . .
C3 C -0.3228(3) -0.6433(3) -0.35810(16) 0.0346(8) Uani 1 1 d . . . . .
H4 H -0.386933 -0.629442 -0.372340 0.041 Uiso 1 1 calc R U . . .
C4 C -0.0328(3) -0.5608(2) -0.14002(14) 0.0254(6) Uani 1 1 d . . . . .
C5 C -0.0846(3) -0.4503(3) -0.07501(15) 0.0305(7) Uani 1 1 d . . . . .
H5 H -0.135536 -0.420110 -0.057049 0.037 Uiso 1 1 calc R U . . .
C6 C -0.2456(3) -0.6671(3) -0.39147(16) 0.0355(8) Uani 1 1 d . . . . .
C7 C -0.0238(3) -0.6966(3) -0.29144(15) 0.0293(7) Uani 1 1 d . . . . .
H6 H 0.022216 -0.709029 -0.319415 0.035 Uiso 1 1 calc R U . . .
H7 H -0.002505 -0.637729 -0.274445 0.035 Uiso 1 1 calc R U . . .
C8 C 0.0430(4) -0.3605(3) -0.01840(18) 0.0402(9) Uani 1 1 d . . . . .
H8 H 0.113103 -0.368507 -0.008110 0.060 Uiso 1 1 calc R U . . .
H9 H 0.001749 -0.373894 0.010952 0.060 Uiso 1 1 calc R U . . .
H10 H 0.031493 -0.296147 -0.029851 0.060 Uiso 1 1 calc R U . . .
C9 C -0.3062(3) -0.6400(3) -0.30401(15) 0.0298(7) Uani 1 1 d . . . . .
C10 C -0.1525(3) -1.0818(3) -0.09777(17) 0.0337(8) Uani 1 1 d . . . . .
C11 C 0.0705(3) -0.9260(3) -0.22799(15) 0.0298(7) Uani 1 1 d . . . . .
H11 H 0.009123 -0.959325 -0.219069 0.036 Uiso 1 1 calc R U . . .
H12 H 0.118846 -0.972816 -0.239634 0.036 Uiso 1 1 calc R U . . .
C12 C 0.0683(3) -0.5360(3) -0.13030(15) 0.0288(7) Uani 1 1 d . . . . .
C13 C -0.3183(3) -0.6578(3) -0.07893(15) 0.0336(8) Uani 1 1 d . . . . .
H13 H -0.375360 -0.614757 -0.083350 0.040 Uiso 1 1 calc R U . . .
H14 H -0.284374 -0.644357 -0.045365 0.040 Uiso 1 1 calc R U . . .
C14 C 0.1149(3) -0.9369(3) -0.13409(16) 0.0314(7) Uani 1 1 d . . . . .
H15 H 0.173793 -0.978210 -0.134150 0.038 Uiso 1 1 calc R U . . .
H16 H 0.054830 -0.976707 -0.134536 0.038 Uiso 1 1 calc R U . . .
C15 C -0.1449(3) -0.8959(2) -0.14081(14) 0.0251(6) Uani 1 1 d . . . . .
C16 C 0.0158(3) -0.4277(3) -0.06243(16) 0.0338(8) Uani 1 1 d . . . . .
C17 C -0.1108(3) -1.0068(3) -0.06913(15) 0.0321(7) Uani 1 1 d . . . . .
H17 H -0.085564 -1.018097 -0.035177 0.039 Uiso 1 1 calc R U . . .
C18 C -0.4723(3) -0.6502(3) -0.18523(17) 0.0346(8) Uani 1 1 d . . . . .
H18 H -0.536651 -0.627488 -0.199938 0.041 Uiso 1 1 calc R U . . .
H19 H -0.439370 -0.598238 -0.166263 0.041 Uiso 1 1 calc R U . . .
C19 C -0.1890(3) -0.9716(3) -0.16986(15) 0.0282(7) Uani 1 1 d . . . . .
C20 C -0.1923(3) -1.0627(3) -0.14860(16) 0.0316(7) Uani 1 1 d . . . . .
H20 H -0.221352 -1.111933 -0.168359 0.038 Uiso 1 1 calc R U . . .
C21 C -0.3554(3) -0.7599(3) -0.07992(15) 0.0337(8) Uani 1 1 d . . . . .
H21 H -0.300338 -0.802116 -0.069154 0.040 Uiso 1 1 calc R U . . .
H22 H -0.409151 -0.767271 -0.055324 0.040 Uiso 1 1 calc R U . . .
C22 C -0.1292(3) -0.6828(3) -0.31534(14) 0.0272(7) Uani 1 1 d . . . . .
C23 C 0.2168(3) -0.7291(3) -0.19834(17) 0.0312(7) Uani 1 1 d . . . . .
H23 H 0.285434 -0.704827 -0.194569 0.037 Uiso 1 1 calc R U . . .
H24 H 0.190868 -0.714286 -0.233480 0.037 Uiso 1 1 calc R U . . .
C24 C 0.1452(3) -0.5790(3) -0.16564(16) 0.0306(7) Uani 1 1 d . . . . .
H24A H 0.126407 -0.564231 -0.201860 0.037 Uiso 1 1 calc R U . . .
H24B H 0.210954 -0.550610 -0.157709 0.037 Uiso 1 1 calc R U . . .
C25 C 0.0468(3) -0.8557(3) -0.27192(15) 0.0307(7) Uani 1 1 d . . . . .
H25 H 0.109445 -0.831155 -0.285362 0.037 Uiso 1 1 calc R U . . .
H26 H 0.009898 -0.887639 -0.300405 0.037 Uiso 1 1 calc R U . . .
C26 C 0.2166(3) -0.8368(3) -0.18990(16) 0.0305(7) Uani 1 1 d . . . . .
H27 H 0.243808 -0.867582 -0.220387 0.037 Uiso 1 1 calc R U . . .
H28 H 0.260748 -0.852022 -0.159832 0.037 Uiso 1 1 calc R U . . .
C27 C 0.0923(3) -0.4701(3) -0.09090(16) 0.0320(7) Uani 1 1 d . . . . .
H29 H 0.159688 -0.454137 -0.083506 0.038 Uiso 1 1 calc R U . . .
C28 C -0.4071(3) -0.8902(3) -0.13882(17) 0.0338(8) Uani 1 1 d . . . . .
H30 H -0.470952 -0.908998 -0.124277 0.041 Uiso 1 1 calc R U . . .
H31 H -0.352993 -0.923119 -0.119534 0.041 Uiso 1 1 calc R U . . .
C29 C -0.4896(3) -0.7340(3) -0.14814(17) 0.0342(8) Uani 1 1 d . . . . .
H32 H -0.519952 -0.710415 -0.116596 0.041 Uiso 1 1 calc R U . . .
H33 H -0.536883 -0.778196 -0.164978 0.041 Uiso 1 1 calc R U . . .
C30 C -0.2093(3) -0.6609(3) -0.28305(14) 0.0269(7) Uani 1 1 d . . . . .
C200 C -0.2336(3) -0.9497(3) -0.22348(15) 0.0283(7) Uani 1 1 d . . . . .
H20K H -0.180677 -0.925707 -0.245303 0.034 Uiso 1 1 calc R U . . .
H20L H -0.259556 -1.008085 -0.239299 0.034 Uiso 1 1 calc R U . . .
C201 C -0.1548(4) -1.1825(3) -0.0755(2) 0.0449(10) Uani 1 1 d . . . . .
H20C H -0.096012 -1.216761 -0.085989 0.067 Uiso 1 1 calc R U . . .
H20D H -0.214745 -1.214610 -0.088634 0.067 Uiso 1 1 calc R U . . .
H20E H -0.155269 -1.179593 -0.037911 0.067 Uiso 1 1 calc R U . . .
C202 C -0.1056(3) -0.9149(3) -0.08964(14) 0.0286(7) Uani 1 1 d . . . . .
C203 C -0.0549(3) -0.8344(3) -0.05997(14) 0.0298(7) Uani 1 1 d . . . . .
H20M H -0.101805 -0.781580 -0.057665 0.036 Uiso 1 1 calc R U . . .
H20N H -0.036965 -0.855246 -0.024564 0.036 Uiso 1 1 calc R U . . .
C204 C 0.1186(3) -0.8757(3) -0.08482(16) 0.0333(8) Uani 1 1 d . . . . .
H20A H 0.110952 -0.916212 -0.054388 0.040 Uiso 1 1 calc R U . . .
H20B H 0.184283 -0.844953 -0.081357 0.040 Uiso 1 1 calc R U . . .
C205 C -0.3856(3) -0.6083(3) -0.26631(16) 0.0327(8) Uani 1 1 d . . . . .
H20F H -0.361884 -0.551671 -0.247881 0.039 Uiso 1 1 calc R U . . .
H20G H -0.447363 -0.592029 -0.286004 0.039 Uiso 1 1 calc R U . . .
C206 C -0.2651(4) -0.6709(5) -0.45031(18) 0.0521(12) Uani 1 1 d . . . . .
H20H H -0.234941 -0.616443 -0.466272 0.078 Uiso 1 1 calc R U . . .
H20I H -0.336836 -0.670720 -0.457976 0.078 Uiso 1 1 calc R U . . .
H20J H -0.236063 -0.728041 -0.463974 0.078 Uiso 1 1 calc R U . . .
C220 C -0.4063(3) -0.9180(3) -0.19637(18) 0.0364(8) Uani 1 1 d . . . . .
H22A H -0.405876 -0.986929 -0.199278 0.044 Uiso 1 1 calc R U . . .
H22B H -0.467497 -0.894665 -0.214195 0.044 Uiso 1 1 calc R U . . .
N300 N -0.3747(5) -0.4317(5) -0.4414(3) 0.086(2) Uani 1 1 d . . . . .
C300 C -0.4093(6) -0.3926(6) -0.5411(3) 0.0722(18) Uani 1 1 d . . . . .
H3C H -0.481591 -0.386071 -0.549125 0.108 Uiso 1 1 d R U . . .
H3B H -0.379749 -0.448535 -0.563065 0.108 Uiso 1 1 d R U . . .
H3A H -0.376485 -0.327462 -0.552175 0.108 Uiso 1 1 d R U . . .
C301 C -0.3890(5) -0.4149(5) -0.4855(3) 0.0629(15) Uani 1 1 d . . . . .
N301 N -0.6620(5) -0.3980(5) -0.1602(2) 0.0704(16) Uani 1 1 d . . . . .
C302 C -0.5566(6) -0.3979(6) -0.0738(2) 0.074(2) Uani 1 1 d . . . . .
H4C H -0.486066 -0.413807 -0.077717 0.111 Uiso 1 1 d R U . . .
H4B H -0.555403 -0.334498 -0.057823 0.111 Uiso 1 1 d R U . . .
H4A H -0.583422 -0.439307 -0.047450 0.111 Uiso 1 1 d R U . . .
C303 C -0.6146(5) -0.3984(4) -0.1229(2) 0.0542(13) 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
Cl1 O5 1.421(5) . ?
Cl1 O6 1.422(4) . ?
Cl1 O4 1.423(4) . ?
Cl1 O7 1.434(4) . ?
Cl2A O1A 1.385(6) . ?
Cl2A O8A 1.397(6) . ?
Cl2A O9A 1.410(6) . ?
Cl2A O10A 1.495(6) . ?
Cl2B O10B 1.369(6) . ?
Cl2B O8B 1.398(6) . ?
Cl2B O1B 1.407(6) . ?
Cl2B O9B 1.524(7) . ?
Ni1 O3 2.021(3) . ?
Ni1 N10 2.104(3) . ?
Ni1 N5 2.109(3) . ?
Ni1 N9 2.140(3) . ?
Ni1 O2 2.177(2) . ?
Ni1 N6 2.206(3) . ?
Ni2 O1 2.032(3) . ?
Ni2 N1 2.097(3) . ?
Ni2 N4 2.112(3) . ?
Ni2 O2 2.164(2) . ?
Ni2 N2 2.166(3) . ?
Ni2 N3 2.202(3) . ?
O1 C4 1.356(4) . ?
C60 C5 1.397(5) . ?
C60 C4 1.397(5) . ?
C60 C1 1.510(5) . ?
O2 C15 1.343(4) . ?
O3 C30 1.343(4) . ?
N1 C23 1.470(5) . ?
N1 C24 1.485(5) . ?
N1 H404 0.9800 . ?
N2 C204 1.487(5) . ?
N2 C203 1.487(5) . ?
N2 H403 0.9800 . ?
N3 C25 1.483(5) . ?
N3 C7 1.497(5) . ?
N3 H401 0.9800 . ?
N4 C14 1.472(5) . ?
N4 C11 1.484(5) . ?
N4 C26 1.498(5) . ?
N5 C18 1.474(5) . ?
N5 C205 1.487(5) . ?
N5 H400 0.9800 . ?
N6 C13 1.477(5) . ?
N6 C1 1.505(5) . ?
N6 H405 0.9800 . ?
N9 C200 1.484(5) . ?
N9 C220 1.484(5) . ?
N9 H402 0.9800 . ?
N10 C21 1.476(5) . ?
N10 C28 1.479(5) . ?
N10 C29 1.503(5) . ?
C1 H1 0.9700 . ?
C1 H2 0.9700 . ?
C2 C6 1.394(6) . ?
C2 C22 1.399(5) . ?
C2 H3 0.9300 . ?
C3 C9 1.389(5) . ?
C3 C6 1.392(6) . ?
C3 H4 0.9300 . ?
C4 C12 1.394(5) . ?
C5 C16 1.389(6) . ?
C5 H5 0.9300 . ?
C6 C206 1.514(6) . ?
C7 C22 1.512(5) . ?
C7 H6 0.9700 . ?
C7 H7 0.9700 . ?
C8 C16 1.500(5) . ?
C8 H8 0.9600 . ?
C8 H9 0.9600 . ?
C8 H10 0.9600 . ?
C9 C30 1.401(5) . ?
C9 C205 1.514(6) . ?
C10 C17 1.383(6) . ?
C10 C20 1.407(6) . ?
C10 C201 1.524(6) . ?
C11 C25 1.517(6) . ?
C11 H11 0.9700 . ?
C11 H12 0.9700 . ?
C12 C27 1.394(5) . ?
C12 C24 1.508(5) . ?
C13 C21 1.514(6) . ?
C13 H13 0.9700 . ?
C13 H14 0.9700 . ?
C14 C204 1.521(6) . ?
C14 H15 0.9700 . ?
C14 H16 0.9700 . ?
C15 C19 1.410(5) . ?
C15 C202 1.412(5) . ?
C16 C27 1.399(6) . ?
C17 C202 1.395(5) . ?
C17 H17 0.9300 . ?
C18 C29 1.531(6) . ?
C18 H18 0.9700 . ?
C18 H19 0.9700 . ?
C19 C20 1.389(5) . ?
C19 C200 1.501(5) . ?
C20 H20 0.9300 . ?
C21 H21 0.9700 . ?
C21 H22 0.9700 . ?
C22 C30 1.398(5) . ?
C23 C26 1.527(5) . ?
C23 H23 0.9700 . ?
C23 H24 0.9700 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 H25 0.9700 . ?
C25 H26 0.9700 . ?
C26 H27 0.9700 . ?
C26 H28 0.9700 . ?
C27 H29 0.9300 . ?
C28 C220 1.519(6) . ?
C28 H30 0.9700 . ?
C28 H31 0.9700 . ?
C29 H32 0.9700 . ?
C29 H33 0.9700 . ?
C200 H20K 0.9700 . ?
C200 H20L 0.9700 . ?
C201 H20C 0.9600 . ?
C201 H20D 0.9600 . ?
C201 H20E 0.9600 . ?
C202 C203 1.503(5) . ?
C203 H20M 0.9700 . ?
C203 H20N 0.9700 . ?
C204 H20A 0.9700 . ?
C204 H20B 0.9700 . ?
C205 H20F 0.9700 . ?
C205 H20G 0.9700 . ?
C206 H20H 0.9600 . ?
C206 H20I 0.9600 . ?
C206 H20J 0.9600 . ?
C220 H22A 0.9700 . ?
C220 H22B 0.9700 . ?
N300 C301 1.157(10) . ?
C300 C301 1.466(11) . ?
C300 H3C 0.9731 . ?
C300 H3B 1.0490 . ?
C300 H3A 1.0550 . ?
N301 C303 1.120(7) . ?
C302 C303 1.444(8) . ?
C302 H4C 0.9669 . ?
C302 H4B 0.9780 . ?
C302 H4A 0.9655 . ?

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
O5 Cl1 O6 110.2(3) . . ?
O5 Cl1 O4 108.2(3) . . ?
O6 Cl1 O4 109.8(3) . . ?
O5 Cl1 O7 112.0(3) . . ?
O6 Cl1 O7 109.2(3) . . ?
O4 Cl1 O7 107.4(3) . . ?
O1A Cl2A O8A 116.4(6) . . ?
O1A Cl2A O9A 114.2(5) . . ?
O8A Cl2A O9A 110.5(7) . . ?
O1A Cl2A O10A 108.7(5) . . ?
O8A Cl2A O10A 104.2(6) . . ?
O9A Cl2A O10A 101.2(5) . . ?
O10B Cl2B O8B 120.3(8) . . ?
O10B Cl2B O1B 121.8(6) . . ?
O8B Cl2B O1B 109.5(8) . . ?
O10B Cl2B O9B 100.1(6) . . ?
O8B Cl2B O9B 100.6(7) . . ?
O1B Cl2B O9B 98.3(6) . . ?
O3 Ni1 N10 160.07(13) . . ?
O3 Ni1 N5 85.69(12) . . ?
N10 Ni1 N5 83.35(13) . . ?
O3 Ni1 N9 112.61(12) . . ?
N10 Ni1 N9 83.92(13) . . ?
N5 Ni1 N9 89.41(13) . . ?
O3 Ni1 O2 84.24(10) . . ?
N10 Ni1 O2 108.87(11) . . ?
N5 Ni1 O2 166.37(12) . . ?
N9 Ni1 O2 86.02(11) . . ?
O3 Ni1 N6 86.06(11) . . ?
N10 Ni1 N6 80.73(13) . . ?
N5 Ni1 N6 104.75(13) . . ?
N9 Ni1 N6 157.64(13) . . ?
O2 Ni1 N6 83.70(11) . . ?
O1 Ni2 N1 85.98(11) . . ?
O1 Ni2 N4 159.70(12) . . ?
N1 Ni2 N4 83.19(12) . . ?
O1 Ni2 O2 83.15(10) . . ?
N1 Ni2 O2 164.59(11) . . ?
N4 Ni2 O2 110.32(11) . . ?
O1 Ni2 N2 113.35(11) . . ?
N1 Ni2 N2 87.87(12) . . ?
N4 Ni2 N2 83.40(12) . . ?
O2 Ni2 N2 86.45(11) . . ?
O1 Ni2 N3 85.30(11) . . ?
N1 Ni2 N3 105.97(12) . . ?
N4 Ni2 N3 81.26(12) . . ?
O2 Ni2 N3 84.03(11) . . ?
N2 Ni2 N3 157.86(12) . . ?
C4 O1 Ni2 119.9(2) . . ?
C5 C60 C4 117.4(3) . . ?
C5 C60 C1 122.0(3) . . ?
C4 C60 C1 120.5(3) . . ?
C15 O2 Ni2 113.0(2) . . ?
C15 O2 Ni1 114.9(2) . . ?
Ni2 O2 Ni1 132.01(12) . . ?
C30 O3 Ni1 120.4(2) . . ?
C23 N1 C24 113.2(3) . . ?
C23 N1 Ni2 103.4(2) . . ?
C24 N1 Ni2 115.8(2) . . ?
C23 N1 H404 108.0 . . ?
C24 N1 H404 108.0 . . ?
Ni2 N1 H404 108.0 . . ?
C204 N2 C203 112.2(3) . . ?
C204 N2 Ni2 106.4(2) . . ?
C203 N2 Ni2 115.4(2) . . ?
C204 N2 H403 107.5 . . ?
C203 N2 H403 107.5 . . ?
Ni2 N2 H403 107.5 . . ?
C25 N3 C7 111.6(3) . . ?
C25 N3 Ni2 109.1(2) . . ?
C7 N3 Ni2 125.9(2) . . ?
C25 N3 H401 102.2 . . ?
C7 N3 H401 102.2 . . ?
Ni2 N3 H401 102.2 . . ?
C14 N4 C11 111.9(3) . . ?
C14 N4 C26 110.4(3) . . ?
C11 N4 C26 111.9(3) . . ?
C14 N4 Ni2 108.0(2) . . ?
C11 N4 Ni2 106.7(2) . . ?
C26 N4 Ni2 107.7(2) . . ?
C18 N5 C205 113.1(3) . . ?
C18 N5 Ni1 102.9(2) . . ?
C205 N5 Ni1 116.9(2) . . ?
C18 N5 H400 107.8 . . ?
C205 N5 H400 107.8 . . ?
Ni1 N5 H400 107.8 . . ?
C13 N6 C1 112.1(3) . . ?
C13 N6 Ni1 109.5(2) . . ?
C1 N6 Ni1 125.7(2) . . ?
C13 N6 H405 102.0 . . ?
C1 N6 H405 102.0 . . ?
Ni1 N6 H405 102.0 . . ?
C200 N9 C220 111.2(3) . . ?
C200 N9 Ni1 117.3(2) . . ?
C220 N9 Ni1 107.0(2) . . ?
C200 N9 H402 107.0 . . ?
C220 N9 H402 107.0 . . ?
Ni1 N9 H402 107.0 . . ?
C21 N10 C28 111.9(3) . . ?
C21 N10 C29 111.7(3) . . ?
C28 N10 C29 110.9(3) . . ?
C21 N10 Ni1 107.3(2) . . ?
C28 N10 Ni1 107.3(2) . . ?
C29 N10 Ni1 107.6(2) . . ?
N6 C1 C60 113.8(3) . . ?
N6 C1 H1 108.8 . . ?
C60 C1 H1 108.8 . . ?
N6 C1 H2 108.8 . . ?
C60 C1 H2 108.8 . . ?
H1 C1 H2 107.7 . . ?
C6 C2 C22 121.9(4) . . ?
C6 C2 H3 119.1 . . ?
C22 C2 H3 119.1 . . ?
C9 C3 C6 121.5(4) . . ?
C9 C3 H4 119.3 . . ?
C6 C3 H4 119.3 . . ?
O1 C4 C12 116.4(3) . . ?
O1 C4 C60 121.7(3) . . ?
C12 C4 C60 121.9(3) . . ?
C16 C5 C60 122.1(4) . . ?
C16 C5 H5 119.0 . . ?
C60 C5 H5 119.0 . . ?
C3 C6 C2 118.5(4) . . ?
C3 C6 C206 120.8(4) . . ?
C2 C6 C206 120.7(4) . . ?
N3 C7 C22 114.5(3) . . ?
N3 C7 H6 108.6 . . ?
C22 C7 H6 108.6 . . ?
N3 C7 H7 108.6 . . ?
C22 C7 H7 108.6 . . ?
H6 C7 H7 107.6 . . ?
C16 C8 H8 109.5 . . ?
C16 C8 H9 109.5 . . ?
H8 C8 H9 109.5 . . ?
C16 C8 H10 109.5 . . ?
H8 C8 H10 109.5 . . ?
H9 C8 H10 109.5 . . ?
C3 C9 C30 118.7(4) . . ?
C3 C9 C205 123.5(3) . . ?
C30 C9 C205 117.6(3) . . ?
C17 C10 C20 118.0(4) . . ?
C17 C10 C201 121.5(4) . . ?
C20 C10 C201 120.5(4) . . ?
N4 C11 C25 110.4(3) . . ?
N4 C11 H11 109.6 . . ?
C25 C11 H11 109.6 . . ?
N4 C11 H12 109.6 . . ?
C25 C11 H12 109.6 . . ?
H11 C11 H12 108.1 . . ?
C4 C12 C27 119.0(4) . . ?
C4 C12 C24 117.1(3) . . ?
C27 C12 C24 123.7(3) . . ?
N6 C13 C21 109.5(3) . . ?
N6 C13 H13 109.8 . . ?
C21 C13 H13 109.8 . . ?
N6 C13 H14 109.8 . . ?
C21 C13 H14 109.8 . . ?
H13 C13 H14 108.2 . . ?
N4 C14 C204 109.9(3) . . ?
N4 C14 H15 109.7 . . ?
C204 C14 H15 109.7 . . ?
N4 C14 H16 109.7 . . ?
C204 C14 H16 109.7 . . ?
H15 C14 H16 108.2 . . ?
O2 C15 C19 121.3(3) . . ?
O2 C15 C202 120.4(3) . . ?
C19 C15 C202 118.3(3) . . ?
C5 C16 C27 119.0(4) . . ?
C5 C16 C8 121.1(4) . . ?
C27 C16 C8 119.9(4) . . ?
C10 C17 C202 122.0(4) . . ?
C10 C17 H17 119.0 . . ?
C202 C17 H17 119.0 . . ?
N5 C18 C29 108.0(3) . . ?
N5 C18 H18 110.1 . . ?
C29 C18 H18 110.1 . . ?
N5 C18 H19 110.1 . . ?
C29 C18 H19 110.1 . . ?
H18 C18 H19 108.4 . . ?
C20 C19 C15 120.4(3) . . ?
C20 C19 C200 121.8(3) . . ?
C15 C19 C200 117.7(3) . . ?
C19 C20 C10 121.3(4) . . ?
C19 C20 H20 119.4 . . ?
C10 C20 H20 119.4 . . ?
N10 C21 C13 110.5(3) . . ?
N10 C21 H21 109.6 . . ?
C13 C21 H21 109.6 . . ?
N10 C21 H22 109.6 . . ?
C13 C21 H22 109.6 . . ?
H21 C21 H22 108.1 . . ?
C30 C22 C2 117.9(3) . . ?
C30 C22 C7 119.7(3) . . ?
C2 C22 C7 122.3(3) . . ?
N1 C23 C26 109.1(3) . . ?
N1 C23 H23 109.9 . . ?
C26 C23 H23 109.9 . . ?
N1 C23 H24 109.9 . . ?
C26 C23 H24 109.9 . . ?
H23 C23 H24 108.3 . . ?
N1 C24 C12 112.2(3) . . ?
N1 C24 H24A 109.2 . . ?
C12 C24 H24A 109.2 . . ?
N1 C24 H24B 109.2 . . ?
C12 C24 H24B 109.2 . . ?
H24A C24 H24B 107.9 . . ?
N3 C25 C11 110.1(3) . . ?
N3 C25 H25 109.6 . . ?
C11 C25 H25 109.6 . . ?
N3 C25 H26 109.6 . . ?
C11 C25 H26 109.6 . . ?
H25 C25 H26 108.2 . . ?
N4 C26 C23 112.9(3) . . ?
N4 C26 H27 109.0 . . ?
C23 C26 H27 109.0 . . ?
N4 C26 H28 109.0 . . ?
C23 C26 H28 109.0 . . ?
H27 C26 H28 107.8 . . ?
C12 C27 C16 120.4(4) . . ?
C12 C27 H29 119.8 . . ?
C16 C27 H29 119.8 . . ?
N10 C28 C220 110.1(3) . . ?
N10 C28 H30 109.6 . . ?
C220 C28 H30 109.6 . . ?
N10 C28 H31 109.6 . . ?
C220 C28 H31 109.6 . . ?
H30 C28 H31 108.2 . . ?
N10 C29 C18 112.8(3) . . ?
N10 C29 H32 109.0 . . ?
C18 C29 H32 109.0 . . ?
N10 C29 H33 109.0 . . ?
C18 C29 H33 109.0 . . ?
H32 C29 H33 107.8 . . ?
O3 C30 C22 121.5(3) . . ?
O3 C30 C9 117.0(3) . . ?
C22 C30 C9 121.5(3) . . ?
N9 C200 C19 112.6(3) . . ?
N9 C200 H20K 109.1 . . ?
C19 C200 H20K 109.1 . . ?
N9 C200 H20L 109.1 . . ?
C19 C200 H20L 109.1 . . ?
H20K C200 H20L 107.8 . . ?
C10 C201 H20C 109.5 . . ?
C10 C201 H20D 109.5 . . ?
H20C C201 H20D 109.5 . . ?
C10 C201 H20E 109.5 . . ?
H20C C201 H20E 109.5 . . ?
H20D C201 H20E 109.5 . . ?
C17 C202 C15 119.9(3) . . ?
C17 C202 C203 122.3(3) . . ?
C15 C202 C203 117.7(3) . . ?
N2 C203 C202 111.4(3) . . ?
N2 C203 H20M 109.3 . . ?
C202 C203 H20M 109.3 . . ?
N2 C203 H20N 109.3 . . ?
C202 C203 H20N 109.3 . . ?
H20M C203 H20N 108.0 . . ?
N2 C204 C14 112.0(3) . . ?
N2 C204 H20A 109.2 . . ?
C14 C204 H20A 109.2 . . ?
N2 C204 H20B 109.2 . . ?
C14 C204 H20B 109.2 . . ?
H20A C204 H20B 107.9 . . ?
N5 C205 C9 111.9(3) . . ?
N5 C205 H20F 109.2 . . ?
C9 C205 H20F 109.2 . . ?
N5 C205 H20G 109.2 . . ?
C9 C205 H20G 109.2 . . ?
H20F C205 H20G 107.9 . . ?
C6 C206 H20H 109.5 . . ?
C6 C206 H20I 109.5 . . ?
H20H C206 H20I 109.5 . . ?
C6 C206 H20J 109.5 . . ?
H20H C206 H20J 109.5 . . ?
H20I C206 H20J 109.5 . . ?
N9 C220 C28 111.6(3) . . ?
N9 C220 H22A 109.3 . . ?
C28 C220 H22A 109.3 . . ?
N9 C220 H22B 109.3 . . ?
C28 C220 H22B 109.3 . . ?
H22A C220 H22B 108.0 . . ?
C301 C300 H3C 111.6 . . ?
C301 C300 H3B 107.3 . . ?
H3C C300 H3B 109.8 . . ?
C301 C300 H3A 112.4 . . ?
H3C C300 H3A 105.8 . . ?
H3B C300 H3A 109.9 . . ?
N300 C301 C300 178.7(8) . . ?
C303 C302 H4C 113.1 . . ?
C303 C302 H4B 111.5 . . ?
H4C C302 H4B 104.6 . . ?
C303 C302 H4A 113.8 . . ?
H4C C302 H4A 108.2 . . ?
H4B C302 H4A 105.0 . . ?
N301 C303 C302 178.0(8) . . ?

_refine_diff_density_max         1.132
_refine_diff_density_min         -1.292
_refine_diff_density_rms         0.122

####################################################################### 
# 
# 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_Ni2LAF-N3-ClO4-3_lc179
_database_code_depnum_ccdc_archive 'CCDC 1517783'


_audit_update_record             
;
2017-02-03 deposited with the CCDC.
2017-02-06 downloaded from the CCDC.
;
_publcif_datablock.id            {81537af2-2642-41fd-823e-282f2707f93b}
_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'2(C40 H60 F3 N12 Ni2 O), 6(Cl O4), 1.68(C2 H6 O), 5(C2 H3 N), (H2 O)'
_chemical_formula_sum            'C93.36 H147.08 Cl6 F6 N29 Ni4 O28.68'
_chemical_formula_weight         2696.14

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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   67.725(3)
_cell_length_b                   12.0716(7)
_cell_length_c                   29.6586(15)
_cell_angle_alpha                90
_cell_angle_beta                 90.888(5)
_cell_angle_gamma                90
_cell_volume                     24245(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6856
_cell_measurement_theta_min      2.9356
_cell_measurement_theta_max      35.5984

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_F_000             11237
_exptl_transmission_factor_min   0.438
_exptl_transmission_factor_max   0.589
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    2.695
_shelx_estimated_absorpt_T_min   0.438
_shelx_estimated_absorpt_T_max   0.589
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 10.4372
_diffrn_reflns_number            44869
_diffrn_reflns_av_unetI/netI     0.2757
_diffrn_reflns_av_R_equivalents  0.1394
_diffrn_reflns_limit_h_min       -85
_diffrn_reflns_limit_h_max       64
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         3.272
_diffrn_reflns_theta_max         76.428
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             22018
_reflns_number_gt                7862
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SIR92 (Altomare 1994)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Diamond (Brandenburg 2011)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1110P)²+246.1918P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         22018
_refine_ls_number_parameters     1506
_refine_ls_number_restraints     41
_refine_ls_R_factor_all          0.2438
_refine_ls_R_factor_gt           0.1332
_refine_ls_wR_factor_ref         0.4318
_refine_ls_wR_factor_gt          0.3473
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Ni1 Ni 0.30720(2) 0.55503(15) 0.44232(7) 0.0306(4) Uani 1 1 d . . . . .
O80 O 0.50132(19) 0.6762(14) 0.6644(6) 0.092(4) Uani 1 1 d D . . . .
H801 H 0.493(2) 0.617(12) 0.676(6) 0.110 Uiso 1 1 d D U . . .
H800 H 0.493(2) 0.709(15) 0.642(5) 0.110 Uiso 1 1 d D U . . .
O1 O 0.53560(19) 0.9792(11) 0.3386(5) 0.078(4) Uani 1 1 d . . . . .
Cl1 Cl 0.37016(4) 0.5965(2) 0.56465(11) 0.0403(6) Uani 1 1 d . . . . .
Ni2 Ni 0.33504(3) 0.64427(15) 0.24475(7) 0.0326(4) Uani 1 1 d . . . . .
O2 O 0.53074(19) 1.1756(11) 0.3545(6) 0.090(5) Uani 1 1 d . . . . .
Cl2 Cl 0.52409(5) 1.0618(4) 0.36285(14) 0.0602(9) Uani 1 1 d . . . . .
Ni3 Ni 0.58844(3) 0.94832(15) 0.46986(7) 0.0333(4) Uani 1 1 d . . . . .
O3 O 0.50487(16) 1.0590(12) 0.3476(5) 0.085(4) Uani 1 1 d . . . . .
Cl3 Cl 0.37882(4) 0.7882(2) 0.71666(11) 0.0391(6) Uani 1 1 d . . . . .
Ni4 Ni 0.55923(3) 0.86208(17) 0.66647(7) 0.0370(5) Uani 1 1 d D . . . .
O4 O 0.4290(2) 0.7455(12) 0.2793(6) 0.114(7) Uani 1 1 d . . . . .
Cl4 Cl 0.41814(4) 0.7091(3) 0.24273(13) 0.0493(8) Uani 1 1 d . . . . .
N6 N 0.33466(12) 0.4885(7) 0.4676(4) 0.037(2) Uani 1 1 d . . . . .
H6A H 0.342026 0.548762 0.482277 0.044 Uiso 1 1 calc R U . . .
O6 O 0.38979(16) 0.6331(10) 0.5636(7) 0.110(6) Uani 1 1 d . . . . .
N1AA N 0.29777(13) 0.5227(7) 0.5075(4) 0.034(2) Uani 1 1 d . . . . .
N2AA N 0.57920(15) 0.9306(9) 0.5336(3) 0.041(2) Uani 1 1 d . . . . .
N14 N 0.31247(13) 0.7178(7) 0.4673(4) 0.035(2) Uani 1 1 d . . . . .
H14A H 0.301566 0.763038 0.455394 0.042 Uiso 1 1 calc R U . . .
O14 O 0.38963(15) 0.7463(8) 0.7554(4) 0.058(3) Uani 1 1 d . . . . .
N3AA N 0.34249(15) 0.6753(8) 0.1774(4) 0.039(2) Uani 1 1 d . . . . .
N4AA N 0.59824(14) 0.9773(8) 0.4049(3) 0.036(2) Uani 1 1 d . . . . .
N3 N 0.54757(14) 0.8325(10) 0.7294(4) 0.045(3) Uani 1 1 d . . . . .
N5AA N 0.29065(14) 0.4042(7) 0.4268(4) 0.035(2) Uani 1 1 d . . . . .
H5AA H 0.278573 0.432514 0.412232 0.042 Uiso 1 1 calc R U . . .
C507 C 0.5308(6) 0.429(4) 0.6672(17) 0.3443(3) Uani 1 1 d D U . . .
H5A7 H 0.543128 0.389198 0.666547 0.516 Uiso 1 1 calc R U . . .
H5B7 H 0.533412 0.506285 0.671744 0.516 Uiso 1 1 calc R U . . .
H5C7 H 0.522983 0.401313 0.691410 0.516 Uiso 1 1 calc R U . . .
C509 C 0.5199(6) 0.413(4) 0.6232(16) 0.3443(3) Uani 1 1 d D U . . .
H50A H 0.527564 0.440688 0.598258 0.413 Uiso 1 1 calc R U . . .
H50B H 0.517064 0.335002 0.618058 0.413 Uiso 1 1 calc R U . . .
O510 O 0.5028(5) 0.472(2) 0.6278(14) 0.3443(3) Uani 1 1 d D U . . .
H510 H 0.493453 0.435895 0.618056 0.516 Uiso 1 1 calc R U . . .
N22 N 0.57124(15) 1.0969(8) 0.4569(4) 0.043(3) Uani 1 1 d . . . . .
H22A H 0.557889 1.068048 0.451430 0.052 Uiso 1 1 calc R U . . .
O22 O 0.32146(15) 0.1350(9) 0.4836(3) 0.054(2) Uani 1 1 d . . . . .
O21 O 0.3182(2) 0.1918(9) 0.5582(4) 0.082(4) Uani 1 1 d . . . . .
C21 C 0.5771(2) 0.5285(14) 0.3778(6) 0.061(4) Uani 1 1 d . . . . .
Cl20 Cl 0.32578(4) 0.1049(2) 0.53112(12) 0.0445(7) Uani 1 1 d . . . . .
C20 C 0.27095(16) 0.9527(10) 0.4789(5) 0.040(3) Uani 1 1 d . . . . .
N23 N 0.56781(15) 0.6929(9) 0.6702(4) 0.040(2) Uani 1 1 d . . . . .
H23 H 0.558097 0.654520 0.651015 0.048 Uiso 1 1 calc R U . . .
C23 C 0.22883(18) 0.4214(13) 0.3992(6) 0.056(4) Uani 1 1 d . . . . .
O23 O 0.3161(3) 0.0046(11) 0.5389(7) 0.138(8) Uani 1 1 d . . . . .
N8AA N 0.31968(14) 0.5065(8) 0.2140(4) 0.040(2) Uani 1 1 d . . . . .
H8AA H 0.305850 0.530455 0.213778 0.048 Uiso 1 1 calc R U . . .
N26 N 0.56987(17) 0.8960(10) 0.6056(4) 0.050(3) Uani 1 1 d . . . . .
Cl26 Cl 0.26394(5) 0.4203(4) 0.64357(15) 0.0630(10) Uani 1 1 d . . . . .
C25 C 0.5321(3) 0.7560(17) 0.4081(10) 0.120(11) Uani 1 1 d . . . . .
H25A H 0.533353 0.759381 0.375950 0.180 Uiso 1 1 calc R U . . .
H25B H 0.519827 0.788792 0.416664 0.180 Uiso 1 1 calc R U . . .
H25C H 0.532498 0.680119 0.417744 0.180 Uiso 1 1 calc R U . . .
O24 O 0.3458(2) 0.102(2) 0.5358(6) 0.159(10) Uani 1 1 d . . . . .
N7 N 0.57460(12) 0.9109(7) 0.5689(4) 0.034(2) Uani 1 1 d . . . . .
O7 O 0.5265(2) 1.0437(14) 0.4108(4) 0.094(5) Uani 1 1 d . . . . .
N6AA N 0.36455(14) 0.5864(8) 0.2498(4) 0.038(2) Uani 1 1 d . . . . .
H6AA H 0.372940 0.650930 0.256039 0.045 Uiso 1 1 calc R U . . .
N449 N 0.34195(14) 0.8138(8) 0.2551(4) 0.036(2) Uani 1 1 d . . . . .
H449 H 0.329275 0.852849 0.255814 0.044 Uiso 1 1 calc R U . . .
N33 N 0.32185(11) 0.5933(7) 0.3432(4) 0.033(2) Uani 1 1 d . . . . .
C32 C 0.2974(3) 1.0522(15) 0.2381(8) 0.076(5) Uani 1 1 d . . . . .
O30 O 0.2494(4) 0.495(3) 0.6537(11) 0.233(15) Uani 1 1 d . . . . .
C30 C 0.27236(19) 1.0714(10) 0.4692(5) 0.046(3) Uani 1 1 d . . . . .
H30A H 0.285796 1.095250 0.473111 0.069 Uiso 1 1 calc R U . . .
H30B H 0.264082 1.111861 0.489374 0.069 Uiso 1 1 calc R U . . .
H30C H 0.268112 1.084974 0.438630 0.069 Uiso 1 1 calc R U . . .
C1CA C 0.34195(18) 0.7983(10) 0.1724(4) 0.0396(15) Uani 1 1 d . . . . .
H1CA H 0.328356 0.823210 0.170041 0.047 Uiso 1 1 calc R U . . .
H1CB H 0.348644 0.819743 0.145077 0.047 Uiso 1 1 calc R U . . .
N37 N 0.32754(18) 0.6067(10) 0.3078(4) 0.046(3) Uani 1 1 d . . . . .
C37 C 0.2803(2) 1.1102(13) 0.2568(9) 0.101(9) Uani 1 1 d . . . . .
H37A H 0.274009 1.153453 0.233568 0.151 Uiso 1 1 calc R U . . .
H37B H 0.284656 1.158143 0.280841 0.151 Uiso 1 1 calc R U . . .
H37C H 0.271136 1.057011 0.268252 0.151 Uiso 1 1 calc R U . . .
C36 C 0.1656(2) 0.6393(15) 0.3675(7) 0.076(5) Uani 1 1 d . . . . .
H36A H 0.156654 0.692746 0.379890 0.113 Uiso 1 1 d R U . . .
H36B H 0.166274 0.575781 0.386954 0.113 Uiso 1 1 d R U . . .
H36C H 0.160860 0.617014 0.338187 0.113 Uiso 1 1 d R U . . .
C35 C 0.1849(2) 0.6882(13) 0.3642(6) 0.061(4) Uani 1 1 d . . . . .
N34 N 0.2007(3) 0.7212(15) 0.3610(7) 0.093(6) Uani 1 1 d . . . . .
N38 N 0.53922(14) 1.0022(9) 0.6679(4) 0.044(3) Uani 1 1 d . . . . .
H38 H 0.528103 0.977912 0.648773 0.053 Uiso 1 1 calc R U . . .
N39 N 0.27892(13) 0.6324(8) 0.4209(4) 0.039(2) Uani 1 1 d . . . . .
N7AA N 0.59966(14) 0.7851(8) 0.4603(4) 0.039(2) Uani 1 1 d . . . . .
H7AA H 0.588094 0.738061 0.454611 0.047 Uiso 1 1 calc R U . . .
N41 N 0.61678(13) 1.0180(9) 0.4882(4) 0.043(2) Uani 1 1 d . . . . .
H41 H 0.626393 0.957349 0.487604 0.051 Uiso 1 1 calc R U . . .
N40 N 0.3115(2) 1.0091(15) 0.2237(6) 0.089(6) Uani 1 1 d . . . . .
N5 N 0.56087(14) 0.8678(8) 0.4459(4) 0.046(3) Uani 1 1 d . . . . .
O5 O 0.35933(15) 0.6461(9) 0.5281(4) 0.061(3) Uani 1 1 d . . . . .
N44 N 0.58413(13) 0.9243(8) 0.7041(3) 0.037(2) Uani 1 1 d . . . . .
H44 H 0.592470 0.860341 0.711532 0.044 Uiso 1 1 calc R U . . .
C43 C 0.5793(3) 0.4307(14) 0.3490(6) 0.064(4) Uani 1 1 d . . . . .
H43A H 0.580185 0.453547 0.318038 0.096 Uiso 1 1 calc R U . . .
H43B H 0.568142 0.382875 0.352402 0.096 Uiso 1 1 calc R U . . .
H43C H 0.591161 0.391618 0.357548 0.096 Uiso 1 1 calc R U . . .
C42 C 0.2752(3) 0.706(2) 0.2898(8) 0.112(9) Uani 1 1 d . . . . .
H42A H 0.264893 0.694747 0.267574 0.168 Uiso 1 1 calc R U . . .
H42B H 0.270265 0.751159 0.313766 0.168 Uiso 1 1 calc R U . . .
H42C H 0.279324 0.635601 0.301681 0.168 Uiso 1 1 calc R U . . .
N46 N 0.31690(15) 0.5774(9) 0.3791(4) 0.042(2) Uani 1 1 d . . . . .
N45 N 0.5751(3) 0.6033(12) 0.3997(6) 0.080(5) Uani 1 1 d . . . . .
C8AA C 0.36072(15) 0.4977(9) 0.4074(5) 0.037(3) Uani 1 1 d . . . . .
C6EA C 0.35196(17) 0.8521(10) 0.2128(4) 0.036(2) Uani 1 1 d . . . . .
H6EA H 0.365816 0.831770 0.213934 0.043 Uiso 1 1 calc R U . . .
H6EB H 0.351065 0.932088 0.210301 0.043 Uiso 1 1 calc R U . . .
C8EA C 0.38561(15) 0.6299(9) 0.3928(4) 0.032(2) Uani 1 1 d . . . . .
C9AA C 0.31352(15) 0.4656(9) 0.5337(4) 0.034(2) Uani 1 1 d . . . . .
H9AA H 0.307584 0.410527 0.553125 0.041 Uiso 1 1 calc R U . . .
H9AB H 0.320326 0.519026 0.552828 0.041 Uiso 1 1 calc R U . . .
C0BA C 0.52828(17) 0.8942(14) 0.7322(6) 0.057(4) Uani 1 1 d . . . . .
H0BA H 0.518084 0.854502 0.715537 0.069 Uiso 1 1 calc R U . . .
H0BB H 0.524306 0.899204 0.763454 0.069 Uiso 1 1 calc R U . . .
C9EA C 0.30298(16) 0.3851(9) 0.2704(5) 0.036(3) Uani 1 1 d . . . . .
C6 C 0.62575(17) 0.8975(9) 0.6566(5) 0.037(3) Uani 1 1 d . . . . .
H6 H 0.627257 0.860865 0.684049 0.045 Uiso 1 1 calc R U . . .
C1BA C 0.59805(15) 0.6898(9) 0.5734(4) 0.035(2) Uani 1 1 d . . . . .
H1BA H 0.605287 0.750229 0.583913 0.041 Uiso 1 1 calc R U . . .
C0FA C 0.30715(15) 0.3566(9) 0.3152(4) 0.033(2) Uani 1 1 d . . . . .
H0FA H 0.320201 0.344159 0.324047 0.040 Uiso 1 1 calc R U . . .
C2FA C 0.29219(17) 0.3461(9) 0.3473(5) 0.038(3) Uani 1 1 d . . . . .
C7 C 0.3245(2) 0.5028(10) 0.1659(5) 0.046(3) Uani 1 1 d . . . . .
H7A H 0.313796 0.468375 0.148954 0.055 Uiso 1 1 calc R U . . .
H7B H 0.336363 0.459143 0.161657 0.055 Uiso 1 1 calc R U . . .
C59 C 0.32649(16) 0.9649(9) 0.3312(5) 0.039(3) Uani 1 1 d . . . . .
H59 H 0.325699 1.007318 0.305090 0.047 Uiso 1 1 calc R U . . .
C3FA C 0.32901(14) 0.8406(9) 0.4124(4) 0.033(2) Uani 1 1 d . . . . .
C2BA C 0.36313(18) 0.6359(10) 0.1699(4) 0.0396(15) Uani 1 1 d . . . . .
H2BA H 0.372109 0.698313 0.172334 0.047 Uiso 1 1 calc R U . . .
H2BB H 0.364046 0.606325 0.139575 0.047 Uiso 1 1 calc R U . . .
C4FA C 0.31580(15) 0.9279(8) 0.4078(4) 0.031(2) Uani 1 1 d . . . . .
H4FA H 0.307669 0.946878 0.431527 0.037 Uiso 1 1 calc R U . . .
C8 C 0.30981(18) 0.7152(10) 0.5180(4) 0.041(3) Uani 1 1 d . . . . .
H8A H 0.306348 0.788321 0.528881 0.049 Uiso 1 1 calc R U . . .
H8B H 0.321974 0.692138 0.532897 0.049 Uiso 1 1 calc R U . . .
O8 O 0.39881(15) 0.7576(8) 0.2448(5) 0.079(4) Uani 1 1 d . . . . .
C2CA C 0.34115(14) 0.8141(8) 0.3753(4) 0.031(2) Uani 1 1 d . . . . .
H2CA H 0.350075 0.755726 0.377642 0.038 Uiso 1 1 calc R U . . .
O29 O 0.2566(4) 0.3356(13) 0.6160(8) 0.173(11) Uani 1 1 d . . . . .
N29 N 0.27014(17) 0.8600(9) 0.4849(5) 0.051(3) Uani 1 1 d . . . . .
O28 O 0.2736(4) 0.3835(18) 0.6824(7) 0.173(11) Uani 1 1 d . . . . .
N28 N 0.24163(18) 0.4426(12) 0.4230(5) 0.068(4) Uani 1 1 d . . . . .
O27 O 0.2773(4) 0.482(2) 0.6205(10) 0.227(15) Uani 1 1 d . . . . .
C27 C 0.2132(2) 0.3882(17) 0.3679(5) 0.071(5) Uani 1 1 d . . . . .
H27A H 0.207886 0.452542 0.352939 0.106 Uiso 1 1 calc R U . . .
H27B H 0.202855 0.351899 0.384128 0.106 Uiso 1 1 calc R U . . .
H27C H 0.218379 0.338238 0.345861 0.106 Uiso 1 1 calc R U . . .
C4CA C 0.33978(14) 0.8746(9) 0.3357(4) 0.033(2) Uani 1 1 d . . . . .
C3BA C 0.61150(16) 0.7275(10) 0.4962(4) 0.039(3) Uani 1 1 d . . . . .
H3BA H 0.619216 0.781871 0.512928 0.047 Uiso 1 1 calc R U . . .
H3BB H 0.620605 0.676418 0.482250 0.047 Uiso 1 1 calc R U . . .
C4BA C 0.29336(17) 0.6334(9) 0.5279(5) 0.042(3) Uani 1 1 d . . . . .
H4BA H 0.292005 0.625518 0.560206 0.050 Uiso 1 1 calc R U . . .
H4BB H 0.280961 0.661247 0.515580 0.050 Uiso 1 1 calc R U . . .
C5BA C 0.62205(16) 1.0086(9) 0.5734(4) 0.035(2) Uani 1 1 d . . . . .
C6BA C 0.58704(16) 0.6280(9) 0.6037(5) 0.037(3) Uani 1 1 d . . . . .
C73 C 0.34842(16) 0.4272(9) 0.4386(5) 0.045(3) Uani 1 1 d . . . . .
H73A H 0.340842 0.375118 0.420406 0.054 Uiso 1 1 calc R U . . .
H73B H 0.357306 0.384479 0.457771 0.054 Uiso 1 1 calc R U . . .
O72 O 0.4874(4) 0.483(4) 0.5384(12) 0.20(2) Uani 0.68(2) 1 d D . P . .
H72F H 0.491151 0.457607 0.514365 0.298 Uiso 0.68(2) 1 calc R U P . .
C70 C 0.58278(16) 1.0446(10) 0.3820(5) 0.044(3) Uani 1 1 d . . . . .
H70A H 0.571311 0.998839 0.375544 0.053 Uiso 1 1 calc R U . . .
H70B H 0.587717 1.072596 0.353712 0.053 Uiso 1 1 calc R U . . .
C75 C 0.28334(16) 0.3581(9) 0.4705(4) 0.036(2) Uani 1 1 d . . . . .
H75A H 0.293134 0.308587 0.483644 0.043 Uiso 1 1 calc R U . . .
H75B H 0.271256 0.316628 0.465328 0.043 Uiso 1 1 calc R U . . .
C74 C 0.4710(8) 0.549(5) 0.5308(12) 0.22(4) Uani 0.68(2) 1 d D . P . .
H74A H 0.460308 0.507205 0.516794 0.260 Uiso 0.68(2) 1 calc R U P . .
H74B H 0.474081 0.612326 0.512083 0.260 Uiso 0.68(2) 1 calc R U P . .
C7BA C 0.59850(16) 0.6641(9) 0.5288(5) 0.037(3) Uani 1 1 d . . . . .
C77 C 0.29669(16) 0.3149(10) 0.3964(4) 0.038(3) Uani 1 1 d . . . . .
H77A H 0.289701 0.247367 0.403928 0.046 Uiso 1 1 calc R U . . .
H77B H 0.310731 0.301164 0.400280 0.046 Uiso 1 1 calc R U . . .
C76 C 0.4661(5) 0.583(3) 0.5775(12) 0.119(16) Uani 0.68(2) 1 d D . P . .
H76A H 0.454638 0.630250 0.576695 0.179 Uiso 0.68(2) 1 calc R U P . .
H76B H 0.463376 0.518722 0.595314 0.179 Uiso 0.68(2) 1 calc R U P . .
H76C H 0.477021 0.622865 0.590647 0.179 Uiso 0.68(2) 1 calc R U P . .
C5CA C 0.58798(16) 0.5744(10) 0.5124(4) 0.039(3) Uani 1 1 d . . . . .
H5CA H 0.588294 0.555522 0.482054 0.046 Uiso 1 1 calc R U . . .
C79 C 0.55547(16) 1.1476(10) 0.5692(5) 0.044(3) Uani 1 1 d . . . . .
H79 H 0.568302 1.155876 0.580334 0.053 Uiso 1 1 calc R U . . .
C6CA C 0.61101(15) 0.9761(9) 0.6494(5) 0.037(3) Uani 1 1 d . . . . .
C7CA C 0.31476(16) 0.9862(8) 0.3681(5) 0.036(3) Uani 1 1 d . . . . .
C8CA C 0.63796(15) 0.8772(10) 0.6209(4) 0.036(3) Uani 1 1 d . . . . .
C10 C 0.32778(18) 0.6211(10) 0.1489(4) 0.0396(15) Uani 1 1 d . . . . .
H10A H 0.332237 0.619272 0.118006 0.047 Uiso 1 1 calc R U . . .
H10B H 0.315467 0.662007 0.149675 0.047 Uiso 1 1 calc R U . . .
O10 O 0.41712(19) 0.5918(9) 0.2450(6) 0.095(5) Uani 1 1 d . . . . .
C0DA C 0.57565(17) 0.9632(12) 0.7468(5) 0.047(3) Uani 1 1 d . . . . .
H0DA H 0.568414 1.031526 0.741604 0.057 Uiso 1 1 calc R U . . .
H0DB H 0.586165 0.978017 0.768508 0.057 Uiso 1 1 calc R U . . .
C87 C 0.32840(16) 0.4093(9) 0.5034(4) 0.032(2) Uani 1 1 d . . . . .
H87A H 0.339815 0.385873 0.521084 0.038 Uiso 1 1 calc R U . . .
H87B H 0.322488 0.344197 0.489547 0.038 Uiso 1 1 calc R U . . .
C11 C 0.5637(2) 0.6537(12) 0.7153(5) 0.053(3) Uani 1 1 d . . . . .
H11A H 0.575015 0.667950 0.734783 0.064 Uiso 1 1 calc R U . . .
H11B H 0.561565 0.574213 0.714401 0.064 Uiso 1 1 calc R U . . .
O11 O 0.36962(16) 0.4777(8) 0.5590(4) 0.058(3) Uani 1 1 d . . . . .
C1DA C 0.38486(15) 0.6102(9) 0.3478(5) 0.038(3) Uani 1 1 d . . . . .
H1DC H 0.392937 0.649688 0.328443 0.045 Uiso 1 1 calc R U . . .
C12 C 0.28356(18) 0.4032(10) 0.2575(5) 0.044(3) Uani 1 1 d . . . . .
H12 H 0.280472 0.422183 0.227803 0.053 Uiso 1 1 calc R U . . .
O12 O 0.3619(3) 0.6222(14) 0.6053(5) 0.137(8) Uani 1 1 d . . . . .
C91 C 0.31889(18) 0.3940(9) 0.2350(5) 0.040(3) Uani 1 1 d . . . . .
H91A H 0.331616 0.377378 0.248886 0.049 Uiso 1 1 calc R U . . .
H91B H 0.316384 0.339292 0.211673 0.049 Uiso 1 1 calc R U . . .
C2DA C 0.37369(15) 0.5760(10) 0.4240(5) 0.041(3) Uani 1 1 d . . . . .
H2DA H 0.374485 0.592287 0.454653 0.049 Uiso 1 1 calc R U . . .
C13 C 0.60941(15) 1.0319(10) 0.6085(5) 0.039(3) Uani 1 1 d . . . . .
H13 H 0.599712 1.085757 0.604613 0.046 Uiso 1 1 calc R U . . .
O13 O 0.3907(2) 0.7669(11) 0.6777(5) 0.088(4) Uani 1 1 d . . . . .
C8BA C 0.60054(19) 0.8690(11) 0.3848(5) 0.048(3) Uani 1 1 d . . . . .
H8BA H 0.608285 0.875632 0.357696 0.057 Uiso 1 1 calc R U . . .
H8BB H 0.587643 0.840258 0.376171 0.057 Uiso 1 1 calc R U . . .
C3DA C 0.33086(15) 0.7793(9) 0.4559(4) 0.034(2) Uani 1 1 d . . . . .
H3DA H 0.333938 0.831382 0.479877 0.041 Uiso 1 1 calc R U . . .
H3DB H 0.341727 0.727194 0.454077 0.041 Uiso 1 1 calc R U . . .
C14 C 0.57664(17) 0.5360(9) 0.5880(5) 0.045(3) Uani 1 1 d . . . . .
H14 H 0.569619 0.490871 0.607446 0.054 Uiso 1 1 calc R U . . .
C156 C 0.2648(2) 0.6736(10) 0.4132(5) 0.043(3) Uani 1 1 d . . . . .
C15 C 0.5681(2) 1.1849(11) 0.4899(6) 0.053(4) Uani 1 1 d . . . . .
H15A H 0.564836 1.252818 0.474014 0.063 Uiso 1 1 calc R U . . .
H15B H 0.580342 1.197333 0.506611 0.063 Uiso 1 1 calc R U . . .
O15 O 0.36059(15) 0.7366(9) 0.7125(5) 0.083(5) Uani 1 1 d . . . . .
C5DA C 0.37204(16) 0.5310(10) 0.3308(5) 0.039(3) Uani 1 1 d . . . . .
C6DA C 0.62161(17) 1.0933(11) 0.4510(4) 0.043(3) Uani 1 1 d . . . . .
H6DA H 0.635382 1.115046 0.453254 0.051 Uiso 1 1 calc R U . . .
H6DB H 0.613555 1.159536 0.452614 0.051 Uiso 1 1 calc R U . . .
C7DA C 0.63686(16) 0.9311(9) 0.5792(5) 0.039(3) Uani 1 1 d . . . . .
H7DA H 0.645718 0.915501 0.556450 0.046 Uiso 1 1 calc R U . . .
C9BA C 0.55168(18) 1.1589(9) 0.5233(5) 0.043(3) Uani 1 1 d . . . . .
C0CA C 0.54031(18) 1.1243(11) 0.5989(5) 0.045(3) Uani 1 1 d . . . . .
C16 C 0.35341(16) 0.8513(10) 0.2965(4) 0.037(3) Uani 1 1 d . . . . .
H16A H 0.360744 0.917936 0.289398 0.044 Uiso 1 1 calc R U . . .
H16B H 0.362829 0.794354 0.305174 0.044 Uiso 1 1 calc R U . . .
O16 O 0.37687(15) 0.9062(7) 0.7198(4) 0.060(3) Uani 1 1 d . . . . .
C17 C 0.57697(18) 1.1401(10) 0.4117(5) 0.045(3) Uani 1 1 d . . . . .
H17A H 0.587960 1.191099 0.415082 0.053 Uiso 1 1 calc R U . . .
H17B H 0.565960 1.179745 0.398028 0.053 Uiso 1 1 calc R U . . .
C8DA C 0.57719(18) 0.5145(10) 0.5418(5) 0.041(3) Uani 1 1 d . . . . .
C9DA C 0.56186(17) 0.8756(13) 0.7653(5) 0.051(3) Uani 1 1 d . . . . .
H9DA H 0.554439 0.906879 0.789905 0.061 Uiso 1 1 calc R U . . .
H9DB H 0.569622 0.814345 0.777138 0.061 Uiso 1 1 calc R U . . .
C0EA C 0.61775(17) 1.0345(11) 0.4068(5) 0.046(3) Uani 1 1 d . . . . .
H0EA H 0.618311 1.087980 0.382408 0.055 Uiso 1 1 calc R U . . .
H0EB H 0.628106 0.980336 0.402063 0.055 Uiso 1 1 calc R U . . .
C19 C 0.27285(17) 0.3633(11) 0.3345(5) 0.043(3) Uani 1 1 d . . . . .
H19 H 0.262706 0.355839 0.355082 0.052 Uiso 1 1 calc R U . . .
O19 O 0.4287(3) 0.7429(18) 0.2048(6) 0.145(8) Uani 1 1 d . . . . .
C1B C 0.59728(16) 1.0110(10) 0.6873(4) 0.040(3) Uani 1 1 d . . . . .
H1BB H 0.605309 1.037833 0.712349 0.048 Uiso 1 1 calc R U . . .
H1BC H 0.589234 1.072371 0.676628 0.048 Uiso 1 1 calc R U . . .
C1C C 0.35990(15) 0.4761(9) 0.3606(5) 0.039(3) Uani 1 1 d . . . . .
H1C H 0.350994 0.423757 0.349466 0.046 Uiso 1 1 calc R U . . .
C1D C 0.6107(2) 0.7875(12) 0.4171(5) 0.049(3) Uani 1 1 d . . . . .
H1DA H 0.610837 0.714118 0.403804 0.059 Uiso 1 1 calc R U . . .
H1DB H 0.624216 0.810380 0.422790 0.059 Uiso 1 1 calc R U . . .
C1E C 0.62018(16) 1.0795(10) 0.5313(4) 0.038(3) Uani 1 1 d . . . . .
H1EA H 0.609345 1.130915 0.535236 0.045 Uiso 1 1 calc R U . . .
H1EB H 0.632157 1.122899 0.528526 0.045 Uiso 1 1 calc R U . . .
C1F C 0.58742(16) 0.6528(10) 0.6535(4) 0.040(3) Uani 1 1 d . . . . .
H1FA H 0.591173 0.586326 0.669865 0.047 Uiso 1 1 calc R U . . .
H1FB H 0.597366 0.708847 0.659729 0.047 Uiso 1 1 calc R U . . .
C1G C 0.52109(18) 1.1101(12) 0.5828(5) 0.051(3) Uani 1 1 d . . . . .
H1G H 0.510838 1.091719 0.601909 0.062 Uiso 1 1 calc R U . . .
C1H C 0.37095(17) 0.4970(9) 0.2814(5) 0.040(3) Uani 1 1 d . . . . .
H1HA H 0.383863 0.470944 0.272468 0.048 Uiso 1 1 calc R U . . .
H1HB H 0.361829 0.435371 0.278290 0.048 Uiso 1 1 calc R U . . .
C1I C 0.27952(16) 0.4545(9) 0.5025(5) 0.041(3) Uani 1 1 d . . . . .
H1IA H 0.268803 0.499774 0.490735 0.049 Uiso 1 1 calc R U . . .
H1IB H 0.275714 0.426236 0.531768 0.049 Uiso 1 1 calc R U . . .
C1J C 0.53061(19) 1.0086(13) 0.7130(6) 0.059(4) Uani 1 1 d . . . . .
H1JA H 0.517828 1.044739 0.711037 0.071 Uiso 1 1 calc R U . . .
H1JB H 0.539110 1.052389 0.732649 0.071 Uiso 1 1 calc R U . . .
C155 C 0.2456(2) 0.7264(13) 0.4027(6) 0.062(4) Uani 1 1 d . . . . .
H15C H 0.237477 0.676031 0.385593 0.093 Uiso 1 1 calc R U . . .
H15D H 0.247727 0.792464 0.385399 0.093 Uiso 1 1 calc R U . . .
H15E H 0.239125 0.745175 0.430235 0.093 Uiso 1 1 calc R U . . .
C1K C 0.54394(19) 1.1135(11) 0.6498(5) 0.046(3) Uani 1 1 d . . . . .
H1KA H 0.557702 1.129869 0.656415 0.056 Uiso 1 1 calc R U . . .
H1KB H 0.535996 1.168243 0.665093 0.056 Uiso 1 1 calc R U . . .
C1L C 0.53307(18) 1.1482(10) 0.5054(5) 0.046(3) Uani 1 1 d . . . . .
H1L H 0.530528 1.155735 0.474625 0.056 Uiso 1 1 calc R U . . .
C1M C 0.3695(2) 0.5461(10) 0.2040(5) 0.049(3) Uani 1 1 d . . . . .
H1MA H 0.362678 0.477229 0.197531 0.059 Uiso 1 1 calc R U . . .
H1MB H 0.383636 0.532891 0.202047 0.059 Uiso 1 1 calc R U . . .
C4EA C 0.26879(16) 0.3929(12) 0.2886(5) 0.048(3) Uani 1 1 d . . . . .
C5EA C 0.5179(2) 1.1250(12) 0.5362(6) 0.055(4) Uani 1 1 d . . . . .
C60 C 0.5485(2) 0.8168(13) 0.4295(7) 0.068(5) Uani 1 1 d . . . . .
F3 F 0.39909(10) 0.7041(6) 0.4096(3) 0.0434(17) Uani 1 1 d . . . . .
F1 F 0.65278(10) 0.8007(6) 0.6271(3) 0.0453(18) Uani 1 1 d . . . . .
F4 F 0.30226(11) 1.0743(6) 0.3647(3) 0.052(2) Uani 1 1 d . . . . .
F2 F 0.49912(11) 1.1142(8) 0.5203(4) 0.068(3) Uani 1 1 d . . . . .
F8 F 0.56673(13) 0.4239(7) 0.5272(3) 0.064(2) Uani 1 1 d . . . . .
F9 F 0.24984(11) 0.4096(9) 0.2768(4) 0.073(3) Uani 1 1 d . . . . .
O666 O 0.53290(12) 0.7817(8) 0.6288(3) 0.047(2) Uani 1 1 d D . . . .
H666 H 0.5233(9) 0.749(9) 0.6411(11) 0.070 Uiso 1 1 d D U . . .
O677 O 0.30353(13) 0.7218(8) 0.2369(4) 0.053(2) Uani 1 1 d . . . . .
H667 H 0.298537 0.726397 0.207563 0.064 Uiso 1 1 calc R U . . .
C66 C 0.54548(18) 0.7093(13) 0.7353(5) 0.055(4) Uani 1 1 d . . . . .
H66A H 0.533602 0.683401 0.719937 0.065 Uiso 1 1 calc R U . . .
H66B H 0.544525 0.691256 0.767043 0.065 Uiso 1 1 calc R U . . .
C666 C 0.5273(2) 0.8092(14) 0.5812(6) 0.065(4) Uani 1 1 d D . . . .
H66C H 0.513096 0.815525 0.578366 0.078 Uiso 1 1 calc R U . . .
H66D H 0.533080 0.879870 0.573030 0.078 Uiso 1 1 calc R U . . .
C667 C 0.5345(3) 0.7214(17) 0.5500(7) 0.083(6) Uani 1 1 d . . . . .
H66E H 0.530805 0.649930 0.561302 0.125 Uiso 1 1 calc R U . . .
H66F H 0.548614 0.725595 0.548067 0.125 Uiso 1 1 calc R U . . .
H66G H 0.528678 0.732217 0.520624 0.125 Uiso 1 1 calc R U . . .
C677 C 0.2917(2) 0.7604(18) 0.2692(8) 0.095(8) Uani 1 1 d . . . . .
H677 H 0.286475 0.829691 0.257541 0.113 Uiso 1 1 calc R U . . .
H678 H 0.300487 0.780256 0.294075 0.113 Uiso 1 1 calc R 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
Ni1 N46 2.015(12) . ?
Ni1 N1AA 2.081(11) . ?
Ni1 N14 2.128(9) . ?
Ni1 N6 2.150(9) . ?
Ni1 N5AA 2.183(9) . ?
Ni1 N39 2.215(10) . ?
O80 H801 0.96(2) . ?
O80 H800 0.96(2) . ?
O1 Cl2 1.462(13) . ?
Cl1 O12 1.372(15) . ?
Cl1 O6 1.401(11) . ?
Cl1 O5 1.432(9) . ?
Cl1 O11 1.445(9) . ?
Ni2 N37 1.998(11) . ?
Ni2 N3AA 2.102(11) . ?
Ni2 N449 2.120(9) . ?
Ni2 N6AA 2.120(10) . ?
Ni2 N8AA 2.157(10) . ?
Ni2 O677 2.339(9) . ?
O2 Cl2 1.467(14) . ?
Cl2 O3 1.372(11) . ?
Cl2 O7 1.444(13) . ?
Ni3 N2AA 2.013(10) . ?
Ni3 N4AA 2.077(10) . ?
Ni3 N7AA 2.133(10) . ?
Ni3 N41 2.158(9) . ?
Ni3 N22 2.170(10) . ?
Ni3 N5 2.212(10) . ?
Cl3 O15 1.387(10) . ?
Cl3 O16 1.433(9) . ?
Cl3 O13 1.443(13) . ?
Cl3 O14 1.444(9) . ?
Ni4 N26 1.995(11) . ?
Ni4 N3 2.068(11) . ?
Ni4 N23 2.125(11) . ?
Ni4 N44 2.143(9) . ?
Ni4 N38 2.168(10) . ?
Ni4 O666 2.303(9) . ?
O4 Cl4 1.371(12) . ?
Cl4 O19 1.402(17) . ?
Cl4 O10 1.419(12) . ?
Cl4 O8 1.436(11) . ?
N6 C73 1.478(15) . ?
N6 C87 1.493(14) . ?
N6 H6A 0.9800 . ?
N1AA C9AA 1.482(14) . ?
N1AA C1I 1.491(13) . ?
N1AA C4BA 1.498(14) . ?
N2AA N7 1.122(15) . ?
N14 C3DA 1.493(13) . ?
N14 C8 1.517(16) . ?
N14 H14A 0.9800 . ?
N3AA C10 1.452(15) . ?
N3AA C1CA 1.492(15) . ?
N3AA C2BA 1.497(15) . ?
N4AA C8BA 1.448(16) . ?
N4AA C70 1.481(15) . ?
N4AA C0EA 1.491(14) . ?
N3 C66 1.504(19) . ?
N3 C0BA 1.507(15) . ?
N3 C9DA 1.519(16) . ?
N5AA C77 1.468(14) . ?
N5AA C75 1.503(15) . ?
N5AA H5AA 0.9800 . ?
C507 C509 1.503(19) . ?
C507 H5A7 0.9600 . ?
C507 H5B7 0.9600 . ?
C507 H5C7 0.9600 . ?
C509 O510 1.372(18) . ?
C509 H50A 0.9700 . ?
C509 H50B 0.9700 . ?
O510 H510 0.8200 . ?
N22 C15 1.461(17) . ?
N22 C17 1.495(18) . ?
N22 H22A 0.9800 . ?
O22 Cl20 1.480(11) . ?
O21 Cl20 1.422(11) . ?
C21 N45 1.12(2) . ?
C21 C43 1.47(2) . ?
Cl20 O24 1.363(14) . ?
Cl20 O23 1.397(14) . ?
C20 N29 1.134(17) . ?
C20 C30 1.466(15) . ?
N23 C11 1.450(18) . ?
N23 C1F 1.506(13) . ?
N23 H23 0.9800 . ?
C23 N28 1.14(2) . ?
C23 C27 1.456(19) . ?
N8AA C7 1.469(17) . ?
N8AA C91 1.496(14) . ?
N8AA H8AA 0.9800 . ?
N26 N7 1.154(15) . ?
Cl26 O27 1.36(2) . ?
Cl26 O30 1.37(2) . ?
Cl26 O28 1.388(15) . ?
Cl26 O29 1.396(17) . ?
C25 C60 1.47(2) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
N6AA C1M 1.487(17) . ?
N6AA C1H 1.490(16) . ?
N6AA H6AA 0.9800 . ?
N449 C6EA 1.508(15) . ?
N449 C16 1.512(14) . ?
N449 H449 0.9800 . ?
N33 N37 1.136(15) . ?
N33 N46 1.137(15) . ?
C32 N40 1.17(3) . ?
C32 C37 1.47(2) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C1CA C6EA 1.514(15) . ?
C1CA H1CA 0.9700 . ?
C1CA H1CB 0.9700 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C36 C35 1.44(2) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C35 N34 1.14(2) . ?
N38 C1J 1.469(19) . ?
N38 C1K 1.483(17) . ?
N38 H38 0.9800 . ?
N39 C156 1.101(17) . ?
N7AA C1D 1.493(17) . ?
N7AA C3BA 1.494(15) . ?
N7AA H7AA 0.9800 . ?
N41 C6DA 1.470(16) . ?
N41 C1E 1.493(16) . ?
N41 H41 0.9800 . ?
N5 C60 1.14(2) . ?
N44 C1B 1.466(15) . ?
N44 C0DA 1.476(17) . ?
N44 H44 0.9800 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C42 C677 1.44(3) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C8AA C2DA 1.377(18) . ?
C8AA C1C 1.412(19) . ?
C8AA C73 1.516(16) . ?
C6EA H6EA 0.9700 . ?
C6EA H6EB 0.9700 . ?
C8EA C1DA 1.355(18) . ?
C8EA F3 1.368(13) . ?
C8EA C2DA 1.400(17) . ?
C9AA C87 1.522(15) . ?
C9AA H9AA 0.9700 . ?
C9AA H9AB 0.9700 . ?
C0BA C1J 1.50(2) . ?
C0BA H0BA 0.9700 . ?
C0BA H0BB 0.9700 . ?
C9EA C12 1.382(17) . ?
C9EA C0FA 1.396(18) . ?
C9EA C91 1.520(16) . ?
C6 C8CA 1.376(17) . ?
C6 C6CA 1.391(16) . ?
C6 H6 0.9300 . ?
C1BA C7BA 1.359(18) . ?
C1BA C6BA 1.394(16) . ?
C1BA H1BA 0.9300 . ?
C0FA C2FA 1.407(16) . ?
C0FA H0FA 0.9300 . ?
C2FA C19 1.374(17) . ?
C2FA C77 1.531(18) . ?
C7 C10 1.531(16) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C59 C7CA 1.386(18) . ?
C59 C4CA 1.419(15) . ?
C59 H59 0.9300 . ?
C3FA C4FA 1.388(15) . ?
C3FA C2CA 1.419(16) . ?
C3FA C3DA 1.492(16) . ?
C2BA C1M 1.540(19) . ?
C2BA H2BA 0.9700 . ?
C2BA H2BB 0.9700 . ?
C4FA C7CA 1.371(17) . ?
C4FA H4FA 0.9300 . ?
C8 C4BA 1.521(16) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C2CA C4CA 1.384(17) . ?
C2CA H2CA 0.9300 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C4CA C16 1.524(16) . ?
C3BA C7BA 1.523(16) . ?
C3BA H3BA 0.9700 . ?
C3BA H3BB 0.9700 . ?
C4BA H4BA 0.9700 . ?
C4BA H4BB 0.9700 . ?
C5BA C7DA 1.380(16) . ?
C5BA C13 1.387(17) . ?
C5BA C1E 1.517(17) . ?
C6BA C14 1.391(17) . ?
C6BA C1F 1.507(18) . ?
C73 H73A 0.9700 . ?
C73 H73B 0.9700 . ?
O72 C74 1.381(18) . ?
O72 H72F 0.8200 . ?
C70 C17 1.506(19) . ?
C70 H70A 0.9700 . ?
C70 H70B 0.9700 . ?
C75 C1I 1.526(16) . ?
C75 H75A 0.9700 . ?
C75 H75B 0.9700 . ?
C74 C76 1.489(18) . ?
C74 H74A 0.9700 . ?
C74 H74B 0.9700 . ?
C7BA C5CA 1.380(17) . ?
C77 H77A 0.9700 . ?
C77 H77B 0.9700 . ?
C76 H76A 0.9600 . ?
C76 H76B 0.9600 . ?
C76 H76C 0.9600 . ?
C5CA C8DA 1.355(18) . ?
C5CA H5CA 0.9300 . ?
C79 C9BA 1.39(2) . ?
C79 C0CA 1.390(19) . ?
C79 H79 0.9300 . ?
C6CA C13 1.390(18) . ?
C6CA C1B 1.530(16) . ?
C7CA F4 1.362(12) . ?
C8CA F1 1.374(12) . ?
C8CA C7DA 1.399(18) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C0DA C9DA 1.519(19) . ?
C0DA H0DA 0.9700 . ?
C0DA H0DB 0.9700 . ?
C87 H87A 0.9700 . ?
C87 H87B 0.9700 . ?
C11 C66 1.530(19) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C1DA C5DA 1.381(17) . ?
C1DA H1DC 0.9300 . ?
C12 C4EA 1.378(18) . ?
C12 H12 0.9300 . ?
C91 H91A 0.9700 . ?
C91 H91B 0.9700 . ?
C2DA H2DA 0.9300 . ?
C13 H13 0.9300 . ?
C8BA C1D 1.528(18) . ?
C8BA H8BA 0.9700 . ?
C8BA H8BB 0.9700 . ?
C3DA H3DA 0.9700 . ?
C3DA H3DB 0.9700 . ?
C14 C8DA 1.39(2) . ?
C14 H14 0.9300 . ?
C156 C155 1.475(18) . ?
C15 C9BA 1.535(19) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C5DA C1C 1.384(18) . ?
C5DA C1H 1.524(18) . ?
C6DA C0EA 1.511(18) . ?
C6DA H6DA 0.9700 . ?
C6DA H6DB 0.9700 . ?
C7DA H7DA 0.9300 . ?
C9BA C1L 1.367(17) . ?
C0CA C1G 1.390(18) . ?
C0CA C1K 1.531(19) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C8DA F8 1.370(14) . ?
C9DA H9DA 0.9700 . ?
C9DA H9DB 0.9700 . ?
C0EA H0EA 0.9700 . ?
C0EA H0EB 0.9700 . ?
C19 C4EA 1.43(2) . ?
C19 H19 0.9300 . ?
C1B H1BB 0.9700 . ?
C1B H1BC 0.9700 . ?
C1C H1C 0.9300 . ?
C1D H1DA 0.9700 . ?
C1D H1DB 0.9700 . ?
C1E H1EA 0.9700 . ?
C1E H1EB 0.9700 . ?
C1F H1FA 0.9700 . ?
C1F H1FB 0.9700 . ?
C1G C5EA 1.41(2) . ?
C1G H1G 0.9300 . ?
C1H H1HA 0.9700 . ?
C1H H1HB 0.9700 . ?
C1I H1IA 0.9700 . ?
C1I H1IB 0.9700 . ?
C1J H1JA 0.9700 . ?
C1J H1JB 0.9700 . ?
C155 H15C 0.9600 . ?
C155 H15D 0.9600 . ?
C155 H15E 0.9600 . ?
C1K H1KA 0.9700 . ?
C1K H1KB 0.9700 . ?
C1L C5EA 1.41(2) . ?
C1L H1L 0.9300 . ?
C1M H1MA 0.9700 . ?
C1M H1MB 0.9700 . ?
C4EA F9 1.340(14) . ?
C5EA F2 1.354(15) . ?
O666 C666 1.495(18) . ?
O666 H666 0.852(9) . ?
O677 C677 1.34(2) . ?
O677 H667 0.9300 . ?
C66 H66A 0.9700 . ?
C66 H66B 0.9700 . ?
C666 C667 1.49(2) . ?
C666 H66C 0.9700 . ?
C666 H66D 0.9700 . ?
C667 H66E 0.9600 . ?
C667 H66F 0.9600 . ?
C667 H66G 0.9600 . ?
C677 H677 0.9700 . ?
C677 H678 0.9700 . ?

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
N46 Ni1 N1AA 176.8(4) . . ?
N46 Ni1 N14 98.3(4) . . ?
N1AA Ni1 N14 84.4(4) . . ?
N46 Ni1 N6 94.7(4) . . ?
N1AA Ni1 N6 83.2(4) . . ?
N14 Ni1 N6 94.8(4) . . ?
N46 Ni1 N5AA 95.1(4) . . ?
N1AA Ni1 N5AA 82.9(4) . . ?
N14 Ni1 N5AA 157.8(3) . . ?
N6 Ni1 N5AA 101.6(3) . . ?
N46 Ni1 N39 88.3(4) . . ?
N1AA Ni1 N39 93.9(4) . . ?
N14 Ni1 N39 81.4(4) . . ?
N6 Ni1 N39 175.5(4) . . ?
N5AA Ni1 N39 81.5(4) . . ?
H801 O80 H800 103(3) . . ?
O12 Cl1 O6 110.3(13) . . ?
O12 Cl1 O5 111.2(10) . . ?
O6 Cl1 O5 109.0(8) . . ?
O12 Cl1 O11 108.5(9) . . ?
O6 Cl1 O11 109.4(7) . . ?
O5 Cl1 O11 108.4(7) . . ?
N37 Ni2 N3AA 177.0(4) . . ?
N37 Ni2 N449 98.2(4) . . ?
N3AA Ni2 N449 84.8(4) . . ?
N37 Ni2 N6AA 96.5(5) . . ?
N3AA Ni2 N6AA 83.4(4) . . ?
N449 Ni2 N6AA 95.9(4) . . ?
N37 Ni2 N8AA 95.3(4) . . ?
N3AA Ni2 N8AA 81.8(4) . . ?
N449 Ni2 N8AA 155.4(4) . . ?
N6AA Ni2 N8AA 102.9(4) . . ?
N37 Ni2 O677 86.5(5) . . ?
N3AA Ni2 O677 93.8(4) . . ?
N449 Ni2 O677 80.1(3) . . ?
N6AA Ni2 O677 175.3(4) . . ?
N8AA Ni2 O677 80.4(4) . . ?
O3 Cl2 O7 114.3(9) . . ?
O3 Cl2 O1 109.3(9) . . ?
O7 Cl2 O1 109.2(9) . . ?
O3 Cl2 O2 105.1(8) . . ?
O7 Cl2 O2 106.1(10) . . ?
O1 Cl2 O2 112.8(8) . . ?
N2AA Ni3 N4AA 176.3(4) . . ?
N2AA Ni3 N7AA 98.2(4) . . ?
N4AA Ni3 N7AA 85.0(4) . . ?
N2AA Ni3 N41 95.3(4) . . ?
N4AA Ni3 N41 82.6(4) . . ?
N7AA Ni3 N41 94.4(4) . . ?
N2AA Ni3 N22 94.6(4) . . ?
N4AA Ni3 N22 82.8(4) . . ?
N7AA Ni3 N22 158.7(4) . . ?
N41 Ni3 N22 101.3(4) . . ?
N2AA Ni3 N5 89.0(5) . . ?
N4AA Ni3 N5 93.2(4) . . ?
N7AA Ni3 N5 81.5(4) . . ?
N41 Ni3 N5 174.4(4) . . ?
N22 Ni3 N5 81.8(4) . . ?
O15 Cl3 O16 111.6(7) . . ?
O15 Cl3 O13 111.0(10) . . ?
O16 Cl3 O13 106.4(8) . . ?
O15 Cl3 O14 110.6(7) . . ?
O16 Cl3 O14 110.0(6) . . ?
O13 Cl3 O14 107.0(8) . . ?
N26 Ni4 N3 177.8(5) . . ?
N26 Ni4 N23 98.2(4) . . ?
N3 Ni4 N23 84.0(4) . . ?
N26 Ni4 N44 96.1(5) . . ?
N3 Ni4 N44 84.2(4) . . ?
N23 Ni4 N44 95.6(4) . . ?
N26 Ni4 N38 95.3(5) . . ?
N3 Ni4 N38 82.5(4) . . ?
N23 Ni4 N38 156.8(4) . . ?
N44 Ni4 N38 101.7(4) . . ?
N26 Ni4 O666 86.3(4) . . ?
N3 Ni4 O666 93.5(4) . . ?
N23 Ni4 O666 80.2(4) . . ?
N44 Ni4 O666 175.4(4) . . ?
N38 Ni4 O666 81.9(4) . . ?
O4 Cl4 O19 105.6(13) . . ?
O4 Cl4 O10 107.9(9) . . ?
O19 Cl4 O10 110.8(12) . . ?
O4 Cl4 O8 108.2(9) . . ?
O19 Cl4 O8 113.0(10) . . ?
O10 Cl4 O8 111.1(7) . . ?
C73 N6 C87 106.4(9) . . ?
C73 N6 Ni1 122.2(9) . . ?
C87 N6 Ni1 103.5(6) . . ?
C73 N6 H6A 108.0 . . ?
C87 N6 H6A 108.0 . . ?
Ni1 N6 H6A 108.0 . . ?
C9AA N1AA C1I 112.5(9) . . ?
C9AA N1AA C4BA 110.4(10) . . ?
C1I N1AA C4BA 111.2(9) . . ?
C9AA N1AA Ni1 110.3(7) . . ?
C1I N1AA Ni1 106.2(8) . . ?
C4BA N1AA Ni1 105.9(7) . . ?
N7 N2AA Ni3 173.7(10) . . ?
C3DA N14 C8 110.3(9) . . ?
C3DA N14 Ni1 121.1(7) . . ?
C8 N14 Ni1 107.7(6) . . ?
C3DA N14 H14A 105.5 . . ?
C8 N14 H14A 105.5 . . ?
Ni1 N14 H14A 105.5 . . ?
C10 N3AA C1CA 112.1(10) . . ?
C10 N3AA C2BA 113.8(10) . . ?
C1CA N3AA C2BA 108.8(9) . . ?
C10 N3AA Ni2 107.4(7) . . ?
C1CA N3AA Ni2 105.4(7) . . ?
C2BA N3AA Ni2 108.8(8) . . ?
C8BA N4AA C70 112.7(11) . . ?
C8BA N4AA C0EA 109.4(10) . . ?
C70 N4AA C0EA 112.5(10) . . ?
C8BA N4AA Ni3 105.5(8) . . ?
C70 N4AA Ni3 106.5(7) . . ?
C0EA N4AA Ni3 109.9(8) . . ?
C66 N3 C0BA 113.5(11) . . ?
C66 N3 C9DA 108.5(11) . . ?
C0BA N3 C9DA 109.6(11) . . ?
C66 N3 Ni4 108.3(9) . . ?
C0BA N3 Ni4 108.0(9) . . ?
C9DA N3 Ni4 108.9(8) . . ?
C77 N5AA C75 110.9(9) . . ?
C77 N5AA Ni1 126.5(7) . . ?
C75 N5AA Ni1 107.5(7) . . ?
C77 N5AA H5AA 103.0 . . ?
C75 N5AA H5AA 103.0 . . ?
Ni1 N5AA H5AA 103.0 . . ?
C509 C507 H5A7 109.5 . . ?
C509 C507 H5B7 109.5 . . ?
H5A7 C507 H5B7 109.5 . . ?
C509 C507 H5C7 109.5 . . ?
H5A7 C507 H5C7 109.5 . . ?
H5B7 C507 H5C7 109.5 . . ?
O510 C509 C507 105(2) . . ?
O510 C509 H50A 110.8 . . ?
C507 C509 H50A 110.8 . . ?
O510 C509 H50B 110.8 . . ?
C507 C509 H50B 110.8 . . ?
H50A C509 H50B 108.9 . . ?
C509 O510 H510 109.5 . . ?
C15 N22 C17 112.9(10) . . ?
C15 N22 Ni3 124.4(9) . . ?
C17 N22 Ni3 107.5(7) . . ?
C15 N22 H22A 103.1 . . ?
C17 N22 H22A 103.1 . . ?
Ni3 N22 H22A 103.1 . . ?
N45 C21 C43 179(2) . . ?
O24 Cl20 O23 115.3(14) . . ?
O24 Cl20 O21 109.3(12) . . ?
O23 Cl20 O21 111.8(11) . . ?
O24 Cl20 O22 106.6(10) . . ?
O23 Cl20 O22 106.5(9) . . ?
O21 Cl20 O22 106.8(7) . . ?
N29 C20 C30 177.4(17) . . ?
C11 N23 C1F 112.6(10) . . ?
C11 N23 Ni4 107.8(8) . . ?
C1F N23 Ni4 122.2(8) . . ?
C11 N23 H23 104.1 . . ?
C1F N23 H23 104.1 . . ?
Ni4 N23 H23 104.1 . . ?
N28 C23 C27 176.4(18) . . ?
C7 N8AA C91 112.8(10) . . ?
C7 N8AA Ni2 108.7(7) . . ?
C91 N8AA Ni2 122.9(8) . . ?
C7 N8AA H8AA 103.3 . . ?
C91 N8AA H8AA 103.3 . . ?
Ni2 N8AA H8AA 103.3 . . ?
N7 N26 Ni4 174.1(11) . . ?
O27 Cl26 O30 103.7(19) . . ?
O27 Cl26 O28 106.4(17) . . ?
O30 Cl26 O28 111.0(17) . . ?
O27 Cl26 O29 109.8(17) . . ?
O30 Cl26 O29 111.2(16) . . ?
O28 Cl26 O29 114.2(12) . . ?
C60 C25 H25A 109.5 . . ?
C60 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C60 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N2AA N7 N26 176.8(13) . . ?
C1M N6AA C1H 105.6(9) . . ?
C1M N6AA Ni2 105.7(8) . . ?
C1H N6AA Ni2 123.2(7) . . ?
C1M N6AA H6AA 107.1 . . ?
C1H N6AA H6AA 107.1 . . ?
Ni2 N6AA H6AA 107.1 . . ?
C6EA N449 C16 110.6(9) . . ?
C6EA N449 Ni2 106.1(7) . . ?
C16 N449 Ni2 121.0(7) . . ?
C6EA N449 H449 106.0 . . ?
C16 N449 H449 106.0 . . ?
Ni2 N449 H449 106.0 . . ?
N37 N33 N46 177.0(12) . . ?
N40 C32 C37 178(2) . . ?
C20 C30 H30A 109.5 . . ?
C20 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C20 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N3AA C1CA C6EA 109.8(10) . . ?
N3AA C1CA H1CA 109.7 . . ?
C6EA C1CA H1CA 109.7 . . ?
N3AA C1CA H1CB 109.7 . . ?
C6EA C1CA H1CB 109.7 . . ?
H1CA C1CA H1CB 108.2 . . ?
N33 N37 Ni2 173.1(11) . . ?
C32 C37 H37A 109.5 . . ?
C32 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C32 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C35 C36 H36A 109.1 . . ?
C35 C36 H36B 109.3 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 110.0 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N34 C35 C36 176(2) . . ?
C1J N38 C1K 111.9(11) . . ?
C1J N38 Ni4 108.4(8) . . ?
C1K N38 Ni4 124.1(8) . . ?
C1J N38 H38 103.3 . . ?
C1K N38 H38 103.3 . . ?
Ni4 N38 H38 103.3 . . ?
C156 N39 Ni1 175.0(12) . . ?
C1D N7AA C3BA 110.6(9) . . ?
C1D N7AA Ni3 106.2(7) . . ?
C3BA N7AA Ni3 121.5(8) . . ?
C1D N7AA H7AA 105.8 . . ?
C3BA N7AA H7AA 105.8 . . ?
Ni3 N7AA H7AA 105.8 . . ?
C6DA N41 C1E 107.6(10) . . ?
C6DA N41 Ni3 105.0(8) . . ?
C1E N41 Ni3 122.3(7) . . ?
C6DA N41 H41 107.0 . . ?
C1E N41 H41 107.0 . . ?
Ni3 N41 H41 107.0 . . ?
C60 N5 Ni3 169.5(12) . . ?
C1B N44 C0DA 108.1(10) . . ?
C1B N44 Ni4 123.4(8) . . ?
C0DA N44 Ni4 104.2(7) . . ?
C1B N44 H44 106.7 . . ?
C0DA N44 H44 106.7 . . ?
Ni4 N44 H44 106.7 . . ?
C21 C43 H43A 109.5 . . ?
C21 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C21 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C677 C42 H42A 109.5 . . ?
C677 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C677 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N33 N46 Ni1 177.3(10) . . ?
C2DA C8AA C1C 119.7(11) . . ?
C2DA C8AA C73 121.3(13) . . ?
C1C C8AA C73 118.9(11) . . ?
N449 C6EA C1CA 108.9(9) . . ?
N449 C6EA H6EA 109.9 . . ?
C1CA C6EA H6EA 109.9 . . ?
N449 C6EA H6EB 109.9 . . ?
C1CA C6EA H6EB 109.9 . . ?
H6EA C6EA H6EB 108.3 . . ?
C1DA C8EA F3 119.3(10) . . ?
C1DA C8EA C2DA 123.9(11) . . ?
F3 C8EA C2DA 116.8(11) . . ?
N1AA C9AA C87 112.0(10) . . ?
N1AA C9AA H9AA 109.2 . . ?
C87 C9AA H9AA 109.2 . . ?
N1AA C9AA H9AB 109.2 . . ?
C87 C9AA H9AB 109.2 . . ?
H9AA C9AA H9AB 107.9 . . ?
C1J C0BA N3 109.7(11) . . ?
C1J C0BA H0BA 109.7 . . ?
N3 C0BA H0BA 109.7 . . ?
C1J C0BA H0BB 109.7 . . ?
N3 C0BA H0BB 109.7 . . ?
H0BA C0BA H0BB 108.2 . . ?
C12 C9EA C0FA 118.8(11) . . ?
C12 C9EA C91 118.6(12) . . ?
C0FA C9EA C91 122.6(10) . . ?
C8CA C6 C6CA 116.2(12) . . ?
C8CA C6 H6 121.9 . . ?
C6CA C6 H6 121.9 . . ?
C7BA C1BA C6BA 121.7(11) . . ?
C7BA C1BA H1BA 119.1 . . ?
C6BA C1BA H1BA 119.1 . . ?
C9EA C0FA C2FA 121.9(10) . . ?
C9EA C0FA H0FA 119.0 . . ?
C2FA C0FA H0FA 119.0 . . ?
C19 C2FA C0FA 119.6(13) . . ?
C19 C2FA C77 118.3(11) . . ?
C0FA C2FA C77 122.1(10) . . ?
N8AA C7 C10 109.1(10) . . ?
N8AA C7 H7A 109.9 . . ?
C10 C7 H7A 109.9 . . ?
N8AA C7 H7B 109.9 . . ?
C10 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
C7CA C59 C4CA 116.0(11) . . ?
C7CA C59 H59 122.0 . . ?
C4CA C59 H59 122.0 . . ?
C4FA C3FA C2CA 118.4(11) . . ?
C4FA C3FA C3DA 120.5(11) . . ?
C2CA C3FA C3DA 121.1(10) . . ?
N3AA C2BA C1M 112.4(10) . . ?
N3AA C2BA H2BA 109.1 . . ?
C1M C2BA H2BA 109.1 . . ?
N3AA C2BA H2BB 109.1 . . ?
C1M C2BA H2BB 109.1 . . ?
H2BA C2BA H2BB 107.9 . . ?
C7CA C4FA C3FA 119.9(10) . . ?
C7CA C4FA H4FA 120.0 . . ?
C3FA C4FA H4FA 120.0 . . ?
N14 C8 C4BA 107.6(10) . . ?
N14 C8 H8A 110.2 . . ?
C4BA C8 H8A 110.2 . . ?
N14 C8 H8B 110.2 . . ?
C4BA C8 H8B 110.2 . . ?
H8A C8 H8B 108.5 . . ?
C4CA C2CA C3FA 120.4(9) . . ?
C4CA C2CA H2CA 119.8 . . ?
C3FA C2CA H2CA 119.8 . . ?
C23 C27 H27A 109.5 . . ?
C23 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C23 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C2CA C4CA C59 121.3(11) . . ?
C2CA C4CA C16 121.2(10) . . ?
C59 C4CA C16 117.4(11) . . ?
N7AA C3BA C7BA 112.1(9) . . ?
N7AA C3BA H3BA 109.2 . . ?
C7BA C3BA H3BA 109.2 . . ?
N7AA C3BA H3BB 109.2 . . ?
C7BA C3BA H3BB 109.2 . . ?
H3BA C3BA H3BB 107.9 . . ?
N1AA C4BA C8 110.5(9) . . ?
N1AA C4BA H4BA 109.6 . . ?
C8 C4BA H4BA 109.6 . . ?
N1AA C4BA H4BB 109.6 . . ?
C8 C4BA H4BB 109.6 . . ?
H4BA C4BA H4BB 108.1 . . ?
C7DA C5BA C13 119.9(12) . . ?
C7DA C5BA C1E 122.5(11) . . ?
C13 C5BA C1E 117.3(11) . . ?
C14 C6BA C1BA 119.0(13) . . ?
C14 C6BA C1F 119.2(12) . . ?
C1BA C6BA C1F 121.7(11) . . ?
N6 C73 C8AA 115.6(9) . . ?
N6 C73 H73A 108.4 . . ?
C8AA C73 H73A 108.4 . . ?
N6 C73 H73B 108.4 . . ?
C8AA C73 H73B 108.4 . . ?
H73A C73 H73B 107.4 . . ?
C74 O72 H72F 109.5 . . ?
N4AA C70 C17 109.9(11) . . ?
N4AA C70 H70A 109.7 . . ?
C17 C70 H70A 109.7 . . ?
N4AA C70 H70B 109.7 . . ?
C17 C70 H70B 109.7 . . ?
H70A C70 H70B 108.2 . . ?
N5AA C75 C1I 108.4(9) . . ?
N5AA C75 H75A 110.0 . . ?
C1I C75 H75A 110.0 . . ?
N5AA C75 H75B 110.0 . . ?
C1I C75 H75B 110.0 . . ?
H75A C75 H75B 108.4 . . ?
O72 C74 C76 102(3) . . ?
O72 C74 H74A 111.5 . . ?
C76 C74 H74A 111.5 . . ?
O72 C74 H74B 111.5 . . ?
C76 C74 H74B 111.5 . . ?
H74A C74 H74B 109.3 . . ?
C1BA C7BA C5CA 120.1(12) . . ?
C1BA C7BA C3BA 121.6(11) . . ?
C5CA C7BA C3BA 118.2(12) . . ?
N5AA C77 C2FA 110.5(10) . . ?
N5AA C77 H77A 109.6 . . ?
C2FA C77 H77A 109.6 . . ?
N5AA C77 H77B 109.6 . . ?
C2FA C77 H77B 109.6 . . ?
H77A C77 H77B 108.1 . . ?
C74 C76 H76A 109.5 . . ?
C74 C76 H76B 109.5 . . ?
H76A C76 H76B 109.5 . . ?
C74 C76 H76C 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
C8DA C5CA C7BA 118.3(12) . . ?
C8DA C5CA H5CA 120.9 . . ?
C7BA C5CA H5CA 120.9 . . ?
C9BA C79 C0CA 120.8(11) . . ?
C9BA C79 H79 119.6 . . ?
C0CA C79 H79 119.6 . . ?
C13 C6CA C6 120.8(12) . . ?
C13 C6CA C1B 117.9(11) . . ?
C6 C6CA C1B 121.1(12) . . ?
F4 C7CA C4FA 119.2(11) . . ?
F4 C7CA C59 116.7(11) . . ?
C4FA C7CA C59 124.0(10) . . ?
F1 C8CA C6 117.7(11) . . ?
F1 C8CA C7DA 117.3(11) . . ?
C6 C8CA C7DA 124.9(11) . . ?
N3AA C10 C7 109.3(11) . . ?
N3AA C10 H10A 109.8 . . ?
C7 C10 H10A 109.8 . . ?
N3AA C10 H10B 109.8 . . ?
C7 C10 H10B 109.8 . . ?
H10A C10 H10B 108.3 . . ?
N44 C0DA C9DA 109.7(12) . . ?
N44 C0DA H0DA 109.7 . . ?
C9DA C0DA H0DA 109.7 . . ?
N44 C0DA H0DB 109.7 . . ?
C9DA C0DA H0DB 109.7 . . ?
H0DA C0DA H0DB 108.2 . . ?
N6 C87 C9AA 109.4(9) . . ?
N6 C87 H87A 109.8 . . ?
C9AA C87 H87A 109.8 . . ?
N6 C87 H87B 109.8 . . ?
C9AA C87 H87B 109.8 . . ?
H87A C87 H87B 108.2 . . ?
N23 C11 C66 112.5(12) . . ?
N23 C11 H11A 109.1 . . ?
C66 C11 H11A 109.1 . . ?
N23 C11 H11B 109.1 . . ?
C66 C11 H11B 109.1 . . ?
H11A C11 H11B 107.8 . . ?
C8EA C1DA C5DA 119.6(11) . . ?
C8EA C1DA H1DC 120.2 . . ?
C5DA C1DA H1DC 120.2 . . ?
C4EA C12 C9EA 119.8(13) . . ?
C4EA C12 H12 120.1 . . ?
C9EA C12 H12 120.1 . . ?
N8AA C91 C9EA 112.5(9) . . ?
N8AA C91 H91A 109.1 . . ?
C9EA C91 H91A 109.1 . . ?
N8AA C91 H91B 109.1 . . ?
C9EA C91 H91B 109.1 . . ?
H91A C91 H91B 107.8 . . ?
C8AA C2DA C8EA 116.9(13) . . ?
C8AA C2DA H2DA 121.6 . . ?
C8EA C2DA H2DA 121.6 . . ?
C5BA C13 C6CA 121.1(11) . . ?
C5BA C13 H13 119.5 . . ?
C6CA C13 H13 119.5 . . ?
N4AA C8BA C1D 111.9(12) . . ?
N4AA C8BA H8BA 109.2 . . ?
C1D C8BA H8BA 109.2 . . ?
N4AA C8BA H8BB 109.2 . . ?
C1D C8BA H8BB 109.2 . . ?
H8BA C8BA H8BB 107.9 . . ?
C3FA C3DA N14 112.5(9) . . ?
C3FA C3DA H3DA 109.1 . . ?
N14 C3DA H3DA 109.1 . . ?
C3FA C3DA H3DB 109.1 . . ?
N14 C3DA H3DB 109.1 . . ?
H3DA C3DA H3DB 107.8 . . ?
C6BA C14 C8DA 117.1(12) . . ?
C6BA C14 H14 121.4 . . ?
C8DA C14 H14 121.4 . . ?
N39 C156 C155 178.7(16) . . ?
N22 C15 C9BA 113.4(11) . . ?
N22 C15 H15A 108.9 . . ?
C9BA C15 H15A 108.9 . . ?
N22 C15 H15B 108.9 . . ?
C9BA C15 H15B 108.9 . . ?
H15A C15 H15B 107.7 . . ?
C1DA C5DA C1C 118.4(12) . . ?
C1DA C5DA C1H 123.9(12) . . ?
C1C C5DA C1H 117.6(11) . . ?
N41 C6DA C0EA 108.9(11) . . ?
N41 C6DA H6DA 109.9 . . ?
C0EA C6DA H6DA 109.9 . . ?
N41 C6DA H6DB 109.9 . . ?
C0EA C6DA H6DB 109.9 . . ?
H6DA C6DA H6DB 108.3 . . ?
C5BA C7DA C8CA 117.1(12) . . ?
C5BA C7DA H7DA 121.4 . . ?
C8CA C7DA H7DA 121.4 . . ?
C1L C9BA C79 121.9(13) . . ?
C1L C9BA C15 116.2(14) . . ?
C79 C9BA C15 121.9(12) . . ?
C1G C0CA C79 120.3(13) . . ?
C1G C0CA C1K 117.6(13) . . ?
C79 C0CA C1K 122.1(11) . . ?
N449 C16 C4CA 111.5(9) . . ?
N449 C16 H16A 109.3 . . ?
C4CA C16 H16A 109.3 . . ?
N449 C16 H16B 109.3 . . ?
C4CA C16 H16B 109.3 . . ?
H16A C16 H16B 108.0 . . ?
N22 C17 C70 109.3(10) . . ?
N22 C17 H17A 109.8 . . ?
C70 C17 H17A 109.8 . . ?
N22 C17 H17B 109.8 . . ?
C70 C17 H17B 109.8 . . ?
H17A C17 H17B 108.3 . . ?
C5CA C8DA F8 120.3(12) . . ?
C5CA C8DA C14 123.7(12) . . ?
F8 C8DA C14 116.0(12) . . ?
C0DA C9DA N3 112.0(12) . . ?
C0DA C9DA H9DA 109.2 . . ?
N3 C9DA H9DA 109.2 . . ?
C0DA C9DA H9DB 109.2 . . ?
N3 C9DA H9DB 109.2 . . ?
H9DA C9DA H9DB 107.9 . . ?
N4AA C0EA C6DA 113.0(11) . . ?
N4AA C0EA H0EA 109.0 . . ?
C6DA C0EA H0EA 109.0 . . ?
N4AA C0EA H0EB 109.0 . . ?
C6DA C0EA H0EB 109.0 . . ?
H0EA C0EA H0EB 107.8 . . ?
C2FA C19 C4EA 118.0(12) . . ?
C2FA C19 H19 121.0 . . ?
C4EA C19 H19 121.0 . . ?
N44 C1B C6CA 115.6(10) . . ?
N44 C1B H1BB 108.4 . . ?
C6CA C1B H1BB 108.4 . . ?
N44 C1B H1BC 108.4 . . ?
C6CA C1B H1BC 108.4 . . ?
H1BB C1B H1BC 107.4 . . ?
C5DA C1C C8AA 121.5(11) . . ?
C5DA C1C H1C 119.2 . . ?
C8AA C1C H1C 119.2 . . ?
N7AA C1D C8BA 109.0(10) . . ?
N7AA C1D H1DA 109.9 . . ?
C8BA C1D H1DA 109.9 . . ?
N7AA C1D H1DB 109.9 . . ?
C8BA C1D H1DB 109.9 . . ?
H1DA C1D H1DB 108.3 . . ?
N41 C1E C5BA 115.7(10) . . ?
N41 C1E H1EA 108.3 . . ?
C5BA C1E H1EA 108.3 . . ?
N41 C1E H1EB 108.3 . . ?
C5BA C1E H1EB 108.3 . . ?
H1EA C1E H1EB 107.4 . . ?
N23 C1F C6BA 112.7(10) . . ?
N23 C1F H1FA 109.1 . . ?
C6BA C1F H1FA 109.1 . . ?
N23 C1F H1FB 109.1 . . ?
C6BA C1F H1FB 109.1 . . ?
H1FA C1F H1FB 107.8 . . ?
C0CA C1G C5EA 116.8(14) . . ?
C0CA C1G H1G 121.6 . . ?
C5EA C1G H1G 121.6 . . ?
N6AA C1H C5DA 114.8(9) . . ?
N6AA C1H H1HA 108.6 . . ?
C5DA C1H H1HA 108.6 . . ?
N6AA C1H H1HB 108.6 . . ?
C5DA C1H H1HB 108.6 . . ?
H1HA C1H H1HB 107.5 . . ?
N1AA C1I C75 109.5(9) . . ?
N1AA C1I H1IA 109.8 . . ?
C75 C1I H1IA 109.8 . . ?
N1AA C1I H1IB 109.8 . . ?
C75 C1I H1IB 109.8 . . ?
H1IA C1I H1IB 108.2 . . ?
N38 C1J C0BA 110.1(12) . . ?
N38 C1J H1JA 109.6 . . ?
C0BA C1J H1JA 109.6 . . ?
N38 C1J H1JB 109.6 . . ?
C0BA C1J H1JB 109.6 . . ?
H1JA C1J H1JB 108.2 . . ?
C156 C155 H15C 109.5 . . ?
C156 C155 H15D 109.5 . . ?
H15C C155 H15D 109.5 . . ?
C156 C155 H15E 109.5 . . ?
H15C C155 H15E 109.5 . . ?
H15D C155 H15E 109.5 . . ?
N38 C1K C0CA 113.7(11) . . ?
N38 C1K H1KA 108.8 . . ?
C0CA C1K H1KA 108.8 . . ?
N38 C1K H1KB 108.8 . . ?
C0CA C1K H1KB 108.8 . . ?
H1KA C1K H1KB 107.7 . . ?
C9BA C1L C5EA 116.3(14) . . ?
C9BA C1L H1L 121.9 . . ?
C5EA C1L H1L 121.9 . . ?
N6AA C1M C2BA 107.7(10) . . ?
N6AA C1M H1MA 110.2 . . ?
C2BA C1M H1MA 110.2 . . ?
N6AA C1M H1MB 110.2 . . ?
C2BA C1M H1MB 110.2 . . ?
H1MA C1M H1MB 108.5 . . ?
F9 C4EA C12 120.9(14) . . ?
F9 C4EA C19 117.1(12) . . ?
C12 C4EA C19 122.0(11) . . ?
F2 C5EA C1G 117.4(14) . . ?
F2 C5EA C1L 118.8(14) . . ?
C1G C5EA C1L 123.9(12) . . ?
N5 C60 C25 177.4(18) . . ?
C666 O666 Ni4 123.1(9) . . ?
C666 O666 H666 109(2) . . ?
Ni4 O666 H666 126(2) . . ?
C677 O677 Ni2 128.4(11) . . ?
C677 O677 H667 115.8 . . ?
Ni2 O677 H667 115.8 . . ?
N3 C66 C11 108.1(11) . . ?
N3 C66 H66A 110.1 . . ?
C11 C66 H66A 110.1 . . ?
N3 C66 H66B 110.1 . . ?
C11 C66 H66B 110.1 . . ?
H66A C66 H66B 108.4 . . ?
C667 C666 O666 110.4(13) . . ?
C667 C666 H66C 109.6 . . ?
O666 C666 H66C 109.6 . . ?
C667 C666 H66D 109.6 . . ?
O666 C666 H66D 109.6 . . ?
H66C C666 H66D 108.1 . . ?
C666 C667 H66E 109.5 . . ?
C666 C667 H66F 109.5 . . ?
H66E C667 H66F 109.5 . . ?
C666 C667 H66G 109.5 . . ?
H66E C667 H66G 109.5 . . ?
H66F C667 H66G 109.5 . . ?
O677 C677 C42 128(2) . . ?
O677 C677 H677 105.2 . . ?
C42 C677 H677 105.2 . . ?
O677 C677 H678 105.2 . . ?
C42 C677 H678 105.2 . . ?
H677 C677 H678 105.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 N3AA C1CA C6EA 160.4(10) . . . . ?
C2BA N3AA C1CA C6EA -72.8(12) . . . . ?
Ni2 N3AA C1CA C6EA 43.8(11) . . . . ?
C16 N449 C6EA C1CA 171.2(9) . . . . ?
Ni2 N449 C6EA C1CA 38.2(10) . . . . ?
N3AA C1CA C6EA N449 -56.8(13) . . . . ?
C1I N1AA C9AA C87 97.2(12) . . . . ?
C4BA N1AA C9AA C87 -137.8(10) . . . . ?
Ni1 N1AA C9AA C87 -21.2(11) . . . . ?
C66 N3 C0BA C1J -163.6(12) . . . . ?
C9DA N3 C0BA C1J 74.9(15) . . . . ?
Ni4 N3 C0BA C1J -43.6(14) . . . . ?
C12 C9EA C0FA C2FA -0.2(17) . . . . ?
C91 C9EA C0FA C2FA -178.4(10) . . . . ?
C9EA C0FA C2FA C19 0.6(17) . . . . ?
C9EA C0FA C2FA C77 -180.0(10) . . . . ?
C91 N8AA C7 C10 -172.3(10) . . . . ?
Ni2 N8AA C7 C10 -32.4(12) . . . . ?
C10 N3AA C2BA C1M -96.4(12) . . . . ?
C1CA N3AA C2BA C1M 137.8(11) . . . . ?
Ni2 N3AA C2BA C1M 23.4(11) . . . . ?
C2CA C3FA C4FA C7CA -0.1(16) . . . . ?
C3DA C3FA C4FA C7CA 177.6(10) . . . . ?
C3DA N14 C8 C4BA -169.0(9) . . . . ?
Ni1 N14 C8 C4BA -35.0(10) . . . . ?
C4FA C3FA C2CA C4CA 0.2(15) . . . . ?
C3DA C3FA C2CA C4CA -177.5(10) . . . . ?
C3FA C2CA C4CA C59 0.8(16) . . . . ?
C3FA C2CA C4CA C16 176.8(9) . . . . ?
C7CA C59 C4CA C2CA -1.7(16) . . . . ?
C7CA C59 C4CA C16 -177.9(10) . . . . ?
C1D N7AA C3BA C7BA -146.5(11) . . . . ?
Ni3 N7AA C3BA C7BA 88.0(11) . . . . ?
C9AA N1AA C4BA C8 74.0(13) . . . . ?
C1I N1AA C4BA C8 -160.3(11) . . . . ?
Ni1 N1AA C4BA C8 -45.4(12) . . . . ?
N14 C8 C4BA N1AA 54.8(13) . . . . ?
C7BA C1BA C6BA C14 1.6(16) . . . . ?
C7BA C1BA C6BA C1F 176.6(10) . . . . ?
C87 N6 C73 C8AA -164.9(10) . . . . ?
Ni1 N6 C73 C8AA 76.8(12) . . . . ?
C2DA C8AA C73 N6 61.0(15) . . . . ?
C1C C8AA C73 N6 -123.9(12) . . . . ?
C8BA N4AA C70 C17 163.6(10) . . . . ?
C0EA N4AA C70 C17 -72.1(13) . . . . ?
Ni3 N4AA C70 C17 48.3(10) . . . . ?
C77 N5AA C75 C1I 173.6(9) . . . . ?
Ni1 N5AA C75 C1I 31.6(10) . . . . ?
C6BA C1BA C7BA C5CA -0.4(16) . . . . ?
C6BA C1BA C7BA C3BA -176.3(10) . . . . ?
N7AA C3BA C7BA C1BA -118.0(12) . . . . ?
N7AA C3BA C7BA C5CA 66.0(13) . . . . ?
C75 N5AA C77 C2FA 145.9(9) . . . . ?
Ni1 N5AA C77 C2FA -81.0(11) . . . . ?
C19 C2FA C77 N5AA -62.4(14) . . . . ?
C0FA C2FA C77 N5AA 118.1(11) . . . . ?
C1BA C7BA C5CA C8DA 0.7(17) . . . . ?
C3BA C7BA C5CA C8DA 176.7(10) . . . . ?
C8CA C6 C6CA C13 -1.8(17) . . . . ?
C8CA C6 C6CA C1B -176.4(10) . . . . ?
C3FA C4FA C7CA F4 -177.6(10) . . . . ?
C3FA C4FA C7CA C59 -1.0(18) . . . . ?
C4CA C59 C7CA F4 178.5(10) . . . . ?
C4CA C59 C7CA C4FA 1.9(18) . . . . ?
C6CA C6 C8CA F1 179.5(10) . . . . ?
C6CA C6 C8CA C7DA 1.7(18) . . . . ?
C1CA N3AA C10 C7 -162.1(10) . . . . ?
C2BA N3AA C10 C7 73.8(13) . . . . ?
Ni2 N3AA C10 C7 -46.8(11) . . . . ?
N8AA C7 C10 N3AA 53.9(14) . . . . ?
C1B N44 C0DA C9DA 179.9(10) . . . . ?
Ni4 N44 C0DA C9DA 47.1(11) . . . . ?
C73 N6 C87 C9AA -177.9(9) . . . . ?
Ni1 N6 C87 C9AA -47.9(9) . . . . ?
N1AA C9AA C87 N6 48.0(12) . . . . ?
C1F N23 C11 C66 170.6(11) . . . . ?
Ni4 N23 C11 C66 32.8(14) . . . . ?
F3 C8EA C1DA C5DA 176.5(9) . . . . ?
C2DA C8EA C1DA C5DA -1.5(17) . . . . ?
C0FA C9EA C12 C4EA 0.1(18) . . . . ?
C91 C9EA C12 C4EA 178.4(11) . . . . ?
C7 N8AA C91 C9EA -144.3(11) . . . . ?
Ni2 N8AA C91 C9EA 82.3(12) . . . . ?
C12 C9EA C91 N8AA 60.3(14) . . . . ?
C0FA C9EA C91 N8AA -121.5(12) . . . . ?
C1C C8AA C2DA C8EA -0.5(15) . . . . ?
C73 C8AA C2DA C8EA 174.5(10) . . . . ?
C1DA C8EA C2DA C8AA 0.8(17) . . . . ?
F3 C8EA C2DA C8AA -177.2(9) . . . . ?
C7DA C5BA C13 C6CA -1.9(17) . . . . ?
C1E C5BA C13 C6CA -175.6(10) . . . . ?
C6 C6CA C13 C5BA 1.9(17) . . . . ?
C1B C6CA C13 C5BA 176.7(10) . . . . ?
C70 N4AA C8BA C1D -159.8(10) . . . . ?
C0EA N4AA C8BA C1D 74.2(14) . . . . ?
Ni3 N4AA C8BA C1D -44.0(12) . . . . ?
C4FA C3FA C3DA N14 65.3(13) . . . . ?
C2CA C3FA C3DA N14 -117.1(10) . . . . ?
C8 N14 C3DA C3FA -146.8(10) . . . . ?
Ni1 N14 C3DA C3FA 86.2(11) . . . . ?
C1BA C6BA C14 C8DA -3.0(16) . . . . ?
C1F C6BA C14 C8DA -178.1(10) . . . . ?
C17 N22 C15 C9BA 145.5(12) . . . . ?
Ni3 N22 C15 C9BA -81.3(13) . . . . ?
C8EA C1DA C5DA C1C 1.7(16) . . . . ?
C8EA C1DA C5DA C1H -175.9(10) . . . . ?
C1E N41 C6DA C0EA -178.4(10) . . . . ?
Ni3 N41 C6DA C0EA -46.7(11) . . . . ?
C13 C5BA C7DA C8CA 1.6(17) . . . . ?
C1E C5BA C7DA C8CA 175.1(10) . . . . ?
F1 C8CA C7DA C5BA -179.5(10) . . . . ?
C6 C8CA C7DA C5BA -1.6(18) . . . . ?
C0CA C79 C9BA C1L 0.4(19) . . . . ?
C0CA C79 C9BA C15 179.9(11) . . . . ?
N22 C15 C9BA C1L -63.9(15) . . . . ?
N22 C15 C9BA C79 116.6(14) . . . . ?
C9BA C79 C0CA C1G 0.9(19) . . . . ?
C9BA C79 C0CA C1K -178.9(11) . . . . ?
C6EA N449 C16 C4CA 147.7(10) . . . . ?
Ni2 N449 C16 C4CA -87.4(10) . . . . ?
C2CA C4CA C16 N449 117.5(11) . . . . ?
C59 C4CA C16 N449 -66.3(13) . . . . ?
C15 N22 C17 C70 171.7(10) . . . . ?
Ni3 N22 C17 C70 30.8(11) . . . . ?
N4AA C70 C17 N22 -53.9(12) . . . . ?
C7BA C5CA C8DA F8 -179.1(11) . . . . ?
C7BA C5CA C8DA C14 -2.3(19) . . . . ?
C6BA C14 C8DA C5CA 3.4(19) . . . . ?
C6BA C14 C8DA F8 -179.6(10) . . . . ?
N44 C0DA C9DA N3 -48.0(14) . . . . ?
C66 N3 C9DA C0DA 139.8(11) . . . . ?
C0BA N3 C9DA C0DA -95.8(14) . . . . ?
Ni4 N3 C9DA C0DA 22.1(14) . . . . ?
C8BA N4AA C0EA C6DA -137.0(12) . . . . ?
C70 N4AA C0EA C6DA 96.9(14) . . . . ?
Ni3 N4AA C0EA C6DA -21.5(13) . . . . ?
N41 C6DA C0EA N4AA 47.2(14) . . . . ?
C0FA C2FA C19 C4EA -0.8(18) . . . . ?
C77 C2FA C19 C4EA 179.7(11) . . . . ?
C0DA N44 C1B C6CA 166.6(10) . . . . ?
Ni4 N44 C1B C6CA -71.8(12) . . . . ?
C13 C6CA C1B N44 120.1(12) . . . . ?
C6 C6CA C1B N44 -65.1(14) . . . . ?
C1DA C5DA C1C C8AA -1.4(16) . . . . ?
C1H C5DA C1C C8AA 176.3(10) . . . . ?
C2DA C8AA C1C C5DA 0.8(16) . . . . ?
C73 C8AA C1C C5DA -174.3(10) . . . . ?
C3BA N7AA C1D C8BA -166.9(11) . . . . ?
Ni3 N7AA C1D C8BA -33.2(12) . . . . ?
N4AA C8BA C1D N7AA 54.0(15) . . . . ?
C6DA N41 C1E C5BA -162.3(10) . . . . ?
Ni3 N41 C1E C5BA 76.2(12) . . . . ?
C7DA C5BA C1E N41 61.7(14) . . . . ?
C13 C5BA C1E N41 -124.7(11) . . . . ?
C11 N23 C1F C6BA 144.1(11) . . . . ?
Ni4 N23 C1F C6BA -85.1(12) . . . . ?
C14 C6BA C1F N23 -70.7(14) . . . . ?
C1BA C6BA C1F N23 114.2(12) . . . . ?
C79 C0CA C1G C5EA -2(2) . . . . ?
C1K C0CA C1G C5EA 177.3(12) . . . . ?
C1M N6AA C1H C5DA 165.5(10) . . . . ?
Ni2 N6AA C1H C5DA -73.2(12) . . . . ?
C1DA C5DA C1H N6AA -63.9(14) . . . . ?
C1C C5DA C1H N6AA 118.5(11) . . . . ?
C9AA N1AA C1I C75 -71.0(13) . . . . ?
C4BA N1AA C1I C75 164.5(10) . . . . ?
Ni1 N1AA C1I C75 49.7(10) . . . . ?
N5AA C75 C1I N1AA -55.3(13) . . . . ?
C1K N38 C1J C0BA -173.4(10) . . . . ?
Ni4 N38 C1J C0BA -32.9(12) . . . . ?
N3 C0BA C1J N38 51.6(15) . . . . ?
C1J N38 C1K C0CA -143.5(11) . . . . ?
Ni4 N38 C1K C0CA 83.4(12) . . . . ?
C1G C0CA C1K N38 62.2(15) . . . . ?
C79 C0CA C1K N38 -118.0(13) . . . . ?
C79 C9BA C1L C5EA 0.0(18) . . . . ?
C15 C9BA C1L C5EA -179.5(12) . . . . ?
C1H N6AA C1M C2BA 179.8(9) . . . . ?
Ni2 N6AA C1M C2BA 47.8(10) . . . . ?
N3AA C2BA C1M N6AA -48.7(13) . . . . ?
C9EA C12 C4EA F9 -179.7(12) . . . . ?
C9EA C12 C4EA C19 0(2) . . . . ?
C2FA C19 C4EA F9 -179.9(12) . . . . ?
C2FA C19 C4EA C12 1(2) . . . . ?
C0CA C1G C5EA F2 -178.4(12) . . . . ?
C0CA C1G C5EA C1L 3(2) . . . . ?
C9BA C1L C5EA F2 179.6(12) . . . . ?
C9BA C1L C5EA C1G -2(2) . . . . ?
C0BA N3 C66 C11 159.8(12) . . . . ?
C9DA N3 C66 C11 -78.1(14) . . . . ?
Ni4 N3 C66 C11 39.9(13) . . . . ?
N23 C11 C66 N3 -49.6(16) . . . . ?
Ni4 O666 C666 C667 101.2(15) . . . . ?
Ni2 O677 C677 C42 -100(2) . . . . ?

_refine_diff_density_max         1.434
_refine_diff_density_min         -1.134
_refine_diff_density_rms         0.122

####################################################################### 
# 
# 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_LAPy_lc-184sq
_database_code_depnum_ccdc_archive 'CCDC 1517950'

_audit_update_record             
;
2017-02-03 deposited with the CCDC.
2017-02-06 downloaded from the CCDC.
;
_vrf_PLAT430_I                   
;
PROBLEM: Short Inter D...A Contact  O106   ..  O106    ..       2.28 Ang.  
RESPONSE: two half disordered water molecules
;
# end Validation Reply Form

#Added by publCIF (Fr 6. Jan 14:32:12 2017)

# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.000 -0.007 373.2 53.0
2 0.500 0.455 0.250 122.3 21.4
3 0.500 0.545 0.750 122.0 19.7
_platon_squeeze_details          
;
structure contains 1 molecule of disordered acetonitril and positional
 disordered water
the sum formula, density, mu and F000 are calculated including these solvent
 molecules
;
_publcif_datablock.id            {c992c4f9-04bd-4e2f-8fda-7e61d0d5a082}

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H53 N11, 2(Cl), 3(H2 O) (C2H3N)'

_chemical_formula_sum            'C35 H62 Cl2 N12 O3'
_chemical_formula_weight         769.85

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   16.679(3)
_cell_length_b                   19.9817(18)
_cell_length_c                   14.9744(15)
_cell_angle_alpha                90
_cell_angle_beta                 120.298(10)
_cell_angle_gamma                90
_cell_volume                     4308.9(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    6746
_cell_measurement_theta_min      2.9056
_cell_measurement_theta_max      36.5984

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_F_000             1528
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    0.206
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.58476
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       'ω and π scans'
_diffrn_detector_area_resol_mean 8.4171
_diffrn_reflns_number            39717
_diffrn_reflns_av_unetI/netI     0.0726
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.911
_diffrn_reflns_theta_max         36.619
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.712
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.712
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.712
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6847
_reflns_number_gt                3791
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SIR92 (Altomare 1994)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Diamond (Brandenburg 2011)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6847
_refine_ls_number_parameters     245
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1431
_refine_ls_R_factor_gt           0.0851
_refine_ls_wR_factor_ref         0.2859
_refine_ls_wR_factor_gt          0.2644
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
N7 N 0.24666(16) 0.50202(12) 0.34224(19) 0.0300(5) Uani 1 1 d . . . . .
H7A H 0.249705 0.485655 0.288755 0.036 Uiso 1 1 calc R U . . .
H7B H 0.206547 0.476961 0.350148 0.036 Uiso 1 1 calc R U . . .
N8 N 0.07121(15) 0.51067(12) 0.19693(19) 0.0273(5) Uani 1 1 d . . . . .
N9 N -0.15750(15) 0.43574(13) 0.0539(2) 0.0294(5) Uani 1 1 d . . . . .
H1 H -0.186(2) 0.4569(18) -0.010(3) 0.035 Uiso 1 1 d . U . . .
N10 N 0.000000 0.26759(18) 0.250000 0.0341(8) Uani 1 2 d S T P . .
N11 N 0.30792(16) 0.37430(14) 0.4159(2) 0.0339(6) Uani 1 1 d . . . . .
N12 N 0.16454(18) 0.31224(13) 0.2255(2) 0.0355(6) Uani 1 1 d . . . . .
H12 H 0.170669 0.353791 0.218578 0.043 Uiso 1 1 d R U . . .
C18 C -0.2926(2) 0.36134(18) -0.0038(3) 0.0375(7) Uani 1 1 d . . . . .
H18A H -0.328134 0.393408 -0.058349 0.045 Uiso 1 1 calc R U . . .
H18B H -0.315378 0.316955 -0.031027 0.045 Uiso 1 1 calc R U . . .
C19 C -0.1906(2) 0.36631(16) 0.0274(2) 0.0350(7) Uani 1 1 d . . . . .
H19A H -0.153886 0.337586 0.086520 0.042 Uiso 1 1 calc R U . . .
H19B H -0.182750 0.351049 -0.029214 0.042 Uiso 1 1 calc R U . . .
C20 C 0.37746(19) 0.42620(17) 0.4380(2) 0.0374(7) Uani 1 1 d . . . . .
H20A H 0.396803 0.424060 0.386917 0.045 Uiso 1 1 calc R U . . .
H20B H 0.431558 0.418010 0.505436 0.045 Uiso 1 1 calc R U . . .
C21 C 0.3396(2) 0.49547(17) 0.4366(2) 0.0369(7) Uani 1 1 d . . . . .
H21A H 0.334562 0.501898 0.497789 0.044 Uiso 1 1 calc R U . . .
H21B H 0.381238 0.529257 0.436358 0.044 Uiso 1 1 calc R U . . .
C22 C 0.2102(2) 0.57084(16) 0.3172(3) 0.0358(7) Uani 1 1 d . . . . .
H22A H 0.249778 0.597734 0.301223 0.043 Uiso 1 1 calc R U . . .
H22B H 0.210601 0.590570 0.376635 0.043 Uiso 1 1 calc R U . . .
C23 C 0.11245(19) 0.57072(15) 0.2259(2) 0.0308(6) Uani 1 1 d . . . . .
C24 C 0.0683(2) 0.63060(16) 0.1791(3) 0.0357(7) Uani 1 1 d . . . . .
H24 H 0.098646 0.671471 0.201683 0.043 Uiso 1 1 calc R U . . .
C25 C -0.0221(2) 0.62699(16) 0.0979(2) 0.0370(7) Uani 1 1 d . . . . .
H25 H -0.053632 0.665823 0.064314 0.044 Uiso 1 1 calc R U . . .
C26 C -0.0652(2) 0.56612(16) 0.0671(2) 0.0328(6) Uani 1 1 d . . . . .
H26 H -0.126015 0.563364 0.012267 0.039 Uiso 1 1 calc R U . . .
C27 C -0.01730(18) 0.50824(14) 0.1184(2) 0.0268(5) Uani 1 1 d . . . . .
C28 C -0.05765(19) 0.43945(15) 0.0912(2) 0.0315(6) Uani 1 1 d . . . . .
H28A H -0.046521 0.421462 0.038217 0.038 Uiso 1 1 calc R U . . .
H28B H -0.025120 0.411159 0.151782 0.038 Uiso 1 1 calc R U . . .
C29 C 0.3240(2) 0.31378(18) 0.3730(3) 0.0425(8) Uani 1 1 d . . . . .
H29A H 0.370093 0.286524 0.429028 0.051 Uiso 1 1 calc R U . . .
H29B H 0.348784 0.326034 0.328953 0.051 Uiso 1 1 calc R U . . .
C30 C 0.2369(2) 0.27311(17) 0.3111(3) 0.0427(8) Uani 1 1 d . . . . .
H30A H 0.251172 0.233778 0.283669 0.051 Uiso 1 1 calc R U . . .
H30B H 0.214181 0.258209 0.355923 0.051 Uiso 1 1 calc R U . . .
C31 C 0.0825(2) 0.27352(17) 0.1545(3) 0.0384(7) Uani 1 1 d . . . . .
H31A H 0.099310 0.243333 0.115933 0.046 Uiso 1 1 calc R U . . .
H31B H 0.035942 0.304082 0.105356 0.046 Uiso 1 1 calc R U . . .
C32 C 0.0393(2) 0.23292(15) 0.2047(2) 0.0333(6) Uani 1 1 d . . . . .
C33 C 0.0404(2) 0.16346(16) 0.2037(3) 0.0376(7) Uani 1 1 d . . . . .
H33 H 0.068143 0.140812 0.171983 0.045 Uiso 1 1 calc R U . . .
C34 C 0.000000 0.1284(2) 0.250000 0.0385(10) Uani 1 2 d S T P . .
H34 H 0.000002 0.081865 0.250001 0.046 Uiso 1 2 calc R U P . .
Cl1 Cl 0.30828(6) 0.49290(5) 0.17611(6) 0.0464(3) Uani 1 1 d . . . . .
O105 O 0.7523(5) 0.6580(3) 0.8931(5) 0.0616(17) Uani 0.5 1 d D . P . .
H106 H 0.699(4) 0.678(4) 0.836(4) 0.074 Uiso 0.5 1 d D U P . .
H105 H 0.761(6) 0.690(3) 0.945(4) 0.074 Uiso 0.5 1 d D U P . .
O106 O 0.5196(4) 0.4490(3) 0.3348(4) 0.0600(16) Uani 0.5 1 d D . P . .
H107 H 0.568(4) 0.471(4) 0.328(6) 0.072 Uiso 0.5 1 d D U P . .
H108 H 0.479(4) 0.442(4) 0.262(2) 0.072 Uiso 0.5 1 d D U P . .


_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
N7 C22 1.473(4) . ?
N7 C21 1.485(4) . ?
N7 H7A 0.8900 . ?
N7 H7B 0.8900 . ?
N8 C23 1.342(4) . ?
N8 C27 1.346(4) . ?
N9 C28 1.467(3) . ?
N9 C19 1.472(4) . ?
N9 H1 0.93(4) . ?
N10 C32 1.348(4) . ?
N10 C32 1.348(4) 2 ?
N11 C29 1.456(4) . ?
N11 C20 1.464(4) . ?
N11 C18 1.484(4) 2 ?
N12 C31 1.461(4) . ?
N12 C30 1.466(4) . ?
N12 H12 0.8491 . ?
C18 C19 1.524(4) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.517(5) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.510(4) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.394(4) . ?
C24 C25 1.381(5) . ?
C24 H24 0.9300 . ?
C25 C26 1.369(5) . ?
C25 H25 0.9300 . ?
C26 C27 1.395(4) . ?
C26 H26 0.9300 . ?
C27 C28 1.494(4) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.507(5) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 C32 1.512(4) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C33 1.388(4) . ?
C33 C34 1.378(4) . ?
C33 H33 0.9300 . ?
C34 H34 0.9300 . ?
O105 H106 0.952(19) . ?
O105 H105 0.961(19) . ?
O106 H107 0.971(19) . ?
O106 H108 0.966(19) . ?

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
C22 N7 C21 115.0(2) . . ?
C22 N7 H7A 108.5 . . ?
C21 N7 H7A 108.5 . . ?
C22 N7 H7B 108.5 . . ?
C21 N7 H7B 108.5 . . ?
H7A N7 H7B 107.5 . . ?
C23 N8 C27 118.2(2) . . ?
C28 N9 C19 110.5(2) . . ?
C28 N9 H1 105(2) . . ?
C19 N9 H1 103(2) . . ?
C32 N10 C32 118.2(4) . 2 ?
C29 N11 C20 112.8(2) . . ?
C29 N11 C18 113.5(3) . 2 ?
C20 N11 C18 113.2(3) . 2 ?
C31 N12 C30 114.2(3) . . ?
C31 N12 H12 123.8 . . ?
C30 N12 H12 122.1 . . ?
N11 C18 C19 112.5(2) 2 . ?
N11 C18 H18A 109.1 2 . ?
C19 C18 H18A 109.1 . . ?
N11 C18 H18B 109.1 2 . ?
C19 C18 H18B 109.1 . . ?
H18A C18 H18B 107.8 . . ?
N9 C19 C18 110.7(3) . . ?
N9 C19 H19A 109.5 . . ?
C18 C19 H19A 109.5 . . ?
N9 C19 H19B 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 108.1 . . ?
N11 C20 C21 111.5(2) . . ?
N11 C20 H20A 109.3 . . ?
C21 C20 H20A 109.3 . . ?
N11 C20 H20B 109.3 . . ?
C21 C20 H20B 109.3 . . ?
H20A C20 H20B 108.0 . . ?
N7 C21 C20 108.7(3) . . ?
N7 C21 H21A 109.9 . . ?
C20 C21 H21A 109.9 . . ?
N7 C21 H21B 109.9 . . ?
C20 C21 H21B 109.9 . . ?
H21A C21 H21B 108.3 . . ?
N7 C22 C23 110.3(2) . . ?
N7 C22 H22A 109.6 . . ?
C23 C22 H22A 109.6 . . ?
N7 C22 H22B 109.6 . . ?
C23 C22 H22B 109.6 . . ?
H22A C22 H22B 108.1 . . ?
N8 C23 C24 123.4(3) . . ?
N8 C23 C22 115.9(3) . . ?
C24 C23 C22 120.6(3) . . ?
C25 C24 C23 117.6(3) . . ?
C25 C24 H24 121.2 . . ?
C23 C24 H24 121.2 . . ?
C26 C25 C24 119.9(3) . . ?
C26 C25 H25 120.1 . . ?
C24 C25 H25 120.1 . . ?
C25 C26 C27 119.5(3) . . ?
C25 C26 H26 120.2 . . ?
C27 C26 H26 120.2 . . ?
N8 C27 C26 121.5(3) . . ?
N8 C27 C28 114.6(2) . . ?
C26 C27 C28 123.9(3) . . ?
N9 C28 C27 114.8(2) . . ?
N9 C28 H28A 108.6 . . ?
C27 C28 H28A 108.6 . . ?
N9 C28 H28B 108.6 . . ?
C27 C28 H28B 108.6 . . ?
H28A C28 H28B 107.6 . . ?
N11 C29 C30 112.6(2) . . ?
N11 C29 H29A 109.1 . . ?
C30 C29 H29A 109.1 . . ?
N11 C29 H29B 109.1 . . ?
C30 C29 H29B 109.1 . . ?
H29A C29 H29B 107.8 . . ?
N12 C30 C29 111.3(3) . . ?
N12 C30 H30A 109.4 . . ?
C29 C30 H30A 109.4 . . ?
N12 C30 H30B 109.4 . . ?
C29 C30 H30B 109.4 . . ?
H30A C30 H30B 108.0 . . ?
N12 C31 C32 115.4(3) . . ?
N12 C31 H31A 108.4 . . ?
C32 C31 H31A 108.4 . . ?
N12 C31 H31B 108.4 . . ?
C32 C31 H31B 108.4 . . ?
H31A C31 H31B 107.5 . . ?
N10 C32 C33 122.1(3) . . ?
N10 C32 C31 116.6(3) . . ?
C33 C32 C31 121.2(3) . . ?
C34 C33 C32 119.3(3) . . ?
C34 C33 H33 120.3 . . ?
C32 C33 H33 120.3 . . ?
C33 C34 C33 118.9(4) 2 . ?
C33 C34 H34 120.5 2 . ?
C33 C34 H34 120.5 . . ?
H106 O105 H105 98(2) . . ?
H107 O106 H108 96(2) . . ?

_refine_diff_density_max         0.593
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.083

