# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_as660_p-1
_database_code_depnum_ccdc_archive 'CCDC 1895464'
loop_
_audit_author_name
_audit_author_address
"Ala'aeddeen Swidan"
;University of Windsor
Canada
;
_audit_update_record             
;
2019-02-04 deposited with the CCDC.	2019-05-03 downloaded from the CCDC.
;

_audit_creation_date             2018-10-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_publ_section_exptl              
;
Any special experimental details
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '4(C33 H25 Cl Ge N5), 4(Cl3 Ge), C H2 Cl2'
_chemical_formula_sum            'C133 H102 Cl18 Ge8 N20'
_chemical_formula_weight         3199.16
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   14.1393(9)
_cell_length_b                   15.1768(9)
_cell_length_c                   16.3072(11)
_cell_angle_alpha                86.094(2)
_cell_angle_beta                 74.051(2)
_cell_angle_gamma                76.567(2)
_cell_volume                     3272.6(4)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9114
_cell_measurement_temperature    170
_cell_measurement_theta_max      30.390
_cell_measurement_theta_min      2.937
_shelx_estimated_absorpt_T_max   0.752
_shelx_estimated_absorpt_T_min   0.651
_exptl_absorpt_coefficient_mu    2.238
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6357
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0750 before and 0.0555 after correction. The Ratio of minimum to maximum transmission is 0.8520. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1602
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.135
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            224637
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.593
_diffrn_reflns_theta_min         2.936
_diffrn_ambient_temperature      170.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX3 Photon 100'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                15518
_reflns_number_total             20073
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       APEX3
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         1.359
_refine_diff_density_min         -1.112
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     820
_refine_ls_number_reflns         20073
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0375
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0366P)²+3.9033P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0973
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl9-C67 = Cl10-C67
 1.771 with sigma of 0.01
 Cl9-Cl10
 2.916 with sigma of 0.03
3. Uiso/Uaniso restraints and constraints
Cl9 \\sim Cl10 \\sim C67: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
4. Rigid body (RIGU) restrains
 Cl9, Cl10, C67
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: Cl9(0.5) Cl10(0.5) C67(0.5) H67A(0.5) H67B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C53(H53A,H53B), C20(H20A,H20B), C27(H27A,H27B), C60(H60A,H60B), C67(H67A,H67B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C38(H38), C4(H4), C5(H5), C35(H35), C36(H36), C42(H42),
 C43(H43), C44(H44), C59(H59), C9(H9), C11(H11), C48(H48), C15(H15), C37(H37),
 C51(H51), C50(H50), C49(H49), C66(H66), C58(H58), C55(H55), C57(H57), C26(H26),
  C22(H22), C56(H56), C16(H16), C62(H62), C18(H18), C17(H17), C65(H65),
 C64(H64), C63(H63), C29(H29), C33(H33), C24(H24), C25(H25), C23(H23), C10(H10),
  C32(H32), C30(H30), C31(H31)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.00294(2) 0.84173(2) 0.75051(2) 0.02260(5) Uani 1 1 d . . . . .
Ge4 Ge 0.44104(2) 1.67118(2) 0.70282(2) 0.04355(8) Uani 1 1 d . . . . .
Ge2 Ge 0.00975(2) 1.34122(2) 0.74267(2) 0.01971(5) Uani 1 1 d . . . . .
Ge3 Ge 0.42229(2) 1.18132(2) 0.67477(2) 0.03069(6) Uani 1 1 d . . . . .
Cl2 Cl -0.11767(4) 1.46787(4) 0.77693(3) 0.02596(10) Uani 1 1 d . . . . .
Cl4 Cl 0.49983(4) 1.07778(4) 0.56883(4) 0.03545(13) Uani 1 1 d . . . . .
Cl5 Cl 0.42383(5) 1.07615(5) 0.78469(4) 0.03692(13) Uani 1 1 d . . . . .
Cl1 Cl -0.13092(4) 0.96381(4) 0.77359(4) 0.03586(13) Uani 1 1 d . . . . .
Cl3 Cl 0.25863(4) 1.18377(4) 0.66845(4) 0.03324(12) Uani 1 1 d . . . . .
Cl8 Cl 0.51329(6) 1.58277(6) 0.58424(5) 0.0591(2) Uani 1 1 d . . . . .
N2 N 0.13824(12) 1.40054(11) 0.70186(11) 0.0192(3) Uani 1 1 d . . . . .
N3 N 0.04852(13) 1.36968(12) 0.85842(11) 0.0227(3) Uani 1 1 d . . . . .
N0AA N 0.02536(13) 1.38214(11) 0.60624(11) 0.0202(3) Uani 1 1 d . . . . .
N7 N 0.13018(13) 1.39806(11) 0.47867(10) 0.0203(3) Uani 1 1 d . . . . .
C41 C 0.18098(15) 1.40847(13) 0.61727(13) 0.0206(4) Uani 1 1 d . . . . .
C40 C 0.11580(15) 1.39538(13) 0.56524(12) 0.0190(4) Uani 1 1 d . . . . .
C45 C 0.18895(16) 1.41162(13) 0.75853(13) 0.0226(4) Uani 1 1 d . . . . .
N6 N 0.14815(13) 0.90456(12) 0.49585(11) 0.0228(3) Uani 1 1 d . . . . .
N5 N 0.03687(13) 0.87975(12) 0.61668(11) 0.0221(3) Uani 1 1 d . . . . .
N4 N 0.13494(13) 0.89739(11) 0.72381(11) 0.0205(3) Uani 1 1 d . . . . .
C8 C 0.18618(15) 0.90732(13) 0.64133(13) 0.0219(4) Uani 1 1 d . . . . .
C7 C 0.12721(15) 0.89749(13) 0.58253(13) 0.0216(4) Uani 1 1 d . . . . .
C2 C -0.09643(17) 0.85527(14) 0.55024(14) 0.0260(4) Uani 1 1 d . . . . .
H2 H -0.143741 0.844577 0.601748 0.031 Uiso 1 1 calc R . . . .
C1 C -0.00374(16) 0.87278(13) 0.55020(13) 0.0222(4) Uani 1 1 d . . . . .
C6 C 0.06576(16) 0.88802(13) 0.47379(13) 0.0223(4) Uani 1 1 d . . . . .
C3 C -0.11624(18) 0.85421(15) 0.47200(16) 0.0304(5) Uani 1 1 d . . . . .
H3 H -0.178718 0.842826 0.469606 0.037 Uiso 1 1 calc R . . . .
C34 C -0.02298(15) 1.37450(13) 0.54479(12) 0.0199(4) Uani 1 1 d . . . . .
C38 C 0.01485(17) 1.38164(14) 0.38883(13) 0.0248(4) Uani 1 1 d . . . . .
H38 H 0.059558 1.387943 0.334499 0.030 Uiso 1 1 calc R . . . .
C4 C -0.04567(19) 0.86968(15) 0.39559(15) 0.0302(5) Uani 1 1 d . . . . .
H4 H -0.062127 0.868631 0.343016 0.036 Uiso 1 1 calc R . . . .
C5 C 0.04654(18) 0.88629(14) 0.39471(14) 0.0277(4) Uani 1 1 d . . . . .
H5 H 0.094202 0.895983 0.343059 0.033 Uiso 1 1 calc R . . . .
C39 C 0.04246(15) 1.38475(13) 0.46457(12) 0.0204(4) Uani 1 1 d . . . . .
C53 C 0.21935(16) 1.40345(14) 0.40693(13) 0.0242(4) Uani 1 1 d . . . . .
H53A H 0.265157 1.432297 0.426661 0.029 Uiso 1 1 calc R . . . .
H53B H 0.197397 1.441672 0.360949 0.029 Uiso 1 1 calc R . . . .
C35 C -0.11960(16) 1.36142(14) 0.55239(14) 0.0252(4) Uani 1 1 d . . . . .
H35 H -0.164364 1.354317 0.606493 0.030 Uiso 1 1 calc R . . . .
C20 C 0.23887(17) 0.91947(15) 0.43102(14) 0.0273(4) Uani 1 1 d . . . . .
H20A H 0.277801 0.949781 0.457680 0.033 Uiso 1 1 calc R . . . .
H20B H 0.218330 0.959903 0.385717 0.033 Uiso 1 1 calc R . . . .
C36 C -0.14713(18) 1.35929(15) 0.47776(15) 0.0279(4) Uani 1 1 d . . . . .
H36 H -0.212580 1.351118 0.480666 0.033 Uiso 1 1 calc R . . . .
C42 C 0.27594(17) 1.42857(16) 0.58801(15) 0.0285(4) Uani 1 1 d . . . . .
H42 H 0.305355 1.434358 0.528629 0.034 Uiso 1 1 calc R . . . .
C43 C 0.32664(17) 1.43995(17) 0.64610(16) 0.0323(5) Uani 1 1 d . . . . .
H43 H 0.391138 1.454245 0.626907 0.039 Uiso 1 1 calc R . . . .
C44 C 0.28391(17) 1.43062(16) 0.73203(16) 0.0306(5) Uani 1 1 d . . . . .
H44 H 0.319012 1.437124 0.772475 0.037 Uiso 1 1 calc R . . . .
Cl7 Cl 0.27535(5) 1.68059(4) 0.70185(5) 0.04460(16) Uani 1 1 d . . . . .
Cl6 Cl 0.44746(8) 1.55005(6) 0.79742(6) 0.0612(2) Uani 1 1 d . . . . .
N8 N 0.01994(13) 0.87950(12) 0.87172(11) 0.0244(4) Uani 1 1 d . . . . .
N9 N 0.11780(15) 0.89811(13) 0.95248(12) 0.0267(4) Uani 1 1 d . . . . .
N10 N 0.15115(14) 1.41263(12) 0.92195(12) 0.0256(4) Uani 1 1 d . . . . .
C54 C 0.27560(16) 1.31010(15) 0.37210(14) 0.0260(4) Uani 1 1 d . . . . .
C59 C 0.32230(17) 1.24631(15) 0.42170(15) 0.0291(5) Uani 1 1 d . . . . .
H59 H 0.320513 1.261564 0.477727 0.035 Uiso 1 1 calc R . . . .
C12 C 0.17709(16) 0.90484(14) 0.78718(13) 0.0229(4) Uani 1 1 d . . . . .
C13 C 0.10891(16) 0.89304(14) 0.87161(13) 0.0233(4) Uani 1 1 d . . . . .
C19 C -0.03344(17) 0.87428(15) 0.95577(14) 0.0271(4) Uani 1 1 d . . . . .
C9 C 0.28251(17) 0.92456(16) 0.62078(14) 0.0285(4) Uani 1 1 d . . . . .
H9 H 0.318533 0.930196 0.562912 0.034 Uiso 1 1 calc R . . . .
C11 C 0.27234(17) 0.92357(16) 0.76975(15) 0.0301(5) Uani 1 1 d . . . . .
H11 H 0.301077 0.929598 0.814765 0.036 Uiso 1 1 calc R . . . .
C14 C 0.02645(18) 0.88711(14) 1.00720(14) 0.0285(5) Uani 1 1 d . . . . .
C27 C 0.2042(2) 0.90264(16) 0.98481(16) 0.0330(5) Uani 1 1 d . . . . .
H27A H 0.182043 0.948338 1.030697 0.040 Uiso 1 1 calc R . . . .
H27B H 0.257010 0.921837 0.938171 0.040 Uiso 1 1 calc R . . . .
C52 C 0.00873(17) 1.36318(14) 0.94555(13) 0.0242(4) Uani 1 1 d . . . . .
C60 C 0.23006(19) 1.44921(15) 0.94119(16) 0.0299(5) Uani 1 1 d . . . . .
H60A H 0.198516 1.493887 0.987807 0.036 Uiso 1 1 calc R . . . .
H60B H 0.262613 1.481369 0.890207 0.036 Uiso 1 1 calc R . . . .
C46 C 0.13203(16) 1.39863(14) 0.84684(13) 0.0233(4) Uani 1 1 d . . . . .
C48 C 0.0519(2) 1.39348(15) 1.07466(15) 0.0329(5) Uani 1 1 d . . . . .
H48 H 0.095619 1.411523 1.101948 0.039 Uiso 1 1 calc R . . . .
C47 C 0.07251(18) 1.39009(14) 0.98581(13) 0.0258(4) Uani 1 1 d . . . . .
C15 C -0.0079(2) 0.88806(16) 1.09623(15) 0.0360(5) Uani 1 1 d . . . . .
H15 H 0.032370 0.897975 1.131209 0.043 Uiso 1 1 calc R . . . .
C37 C -0.08073(18) 1.36892(15) 0.39754(14) 0.0276(4) Uani 1 1 d . . . . .
H37 H -0.102525 1.366570 0.347731 0.033 Uiso 1 1 calc R . . . .
C51 C -0.07906(18) 1.33743(14) 0.99212(14) 0.0279(4) Uani 1 1 d . . . . .
H51 H -0.122172 1.318183 0.964934 0.034 Uiso 1 1 calc R . . . .
C61 C 0.30919(17) 1.37743(15) 0.96702(14) 0.0261(4) Uani 1 1 d . . . . .
C50 C -0.1004(2) 1.34128(16) 1.08028(14) 0.0333(5) Uani 1 1 d . . . . .
H50 H -0.159979 1.324794 1.114395 0.040 Uiso 1 1 calc R . . . .
C49 C -0.0360(2) 1.36899(16) 1.12015(15) 0.0352(5) Uani 1 1 d . . . . .
H49 H -0.053605 1.370952 1.180672 0.042 Uiso 1 1 calc R . . . .
C66 C 0.33873(19) 1.39087(18) 1.03845(16) 0.0355(5) Uani 1 1 d . . . . .
H66 H 0.307064 1.444330 1.071170 0.043 Uiso 1 1 calc R . . . .
C58 C 0.37163(19) 1.16039(17) 0.39030(18) 0.0385(6) Uani 1 1 d . . . . .
H58 H 0.403444 1.117094 0.424819 0.046 Uiso 1 1 calc R . . . .
C55 C 0.2799(2) 1.28766(19) 0.28991(16) 0.0417(6) Uani 1 1 d . . . . .
H55 H 0.249041 1.331233 0.254997 0.050 Uiso 1 1 calc R . . . .
C57 C 0.3746(2) 1.1377(2) 0.3092(2) 0.0495(7) Uani 1 1 d . . . . .
H57 H 0.407681 1.078533 0.287945 0.059 Uiso 1 1 calc R . . . .
C21 C 0.30508(17) 0.83106(17) 0.39177(15) 0.0311(5) Uani 1 1 d . . . . .
C26 C 0.33551(19) 0.75924(17) 0.44242(19) 0.0398(6) Uani 1 1 d . . . . .
H26 H 0.317357 0.766406 0.502550 0.048 Uiso 1 1 calc R . . . .
C22 C 0.3358(2) 0.8219(3) 0.30396(18) 0.0536(9) Uani 1 1 d . . . . .
H22 H 0.317764 0.871296 0.268080 0.064 Uiso 1 1 calc R . . . .
C56 C 0.3294(3) 1.2012(2) 0.25860(19) 0.0548(8) Uani 1 1 d . . . . .
H56 H 0.332048 1.185813 0.202374 0.066 Uiso 1 1 calc R . . . .
C16 C -0.1038(2) 0.87373(17) 1.13010(16) 0.0412(6) Uani 1 1 d . . . . .
H16 H -0.130060 0.873665 1.190334 0.049 Uiso 1 1 calc R . . . .
C62 C 0.3549(2) 1.29831(18) 0.92059(18) 0.0402(6) Uani 1 1 d . . . . .
H62 H 0.334673 1.287635 0.871917 0.048 Uiso 1 1 calc R . . . .
C18 C -0.13036(18) 0.85930(16) 0.99103(16) 0.0334(5) Uani 1 1 d . . . . .
H18 H -0.171032 0.849634 0.956303 0.040 Uiso 1 1 calc R . . . .
C17 C -0.1640(2) 0.85926(17) 1.07917(17) 0.0397(6) Uani 1 1 d . . . . .
H17 H -0.229399 0.849186 1.105728 0.048 Uiso 1 1 calc R . . . .
C65 C 0.4136(2) 1.3277(2) 1.0629(2) 0.0526(8) Uani 1 1 d . . . . .
H65 H 0.433302 1.337601 1.112119 0.063 Uiso 1 1 calc R . . . .
C64 C 0.4597(2) 1.2500(2) 1.0153(2) 0.0565(9) Uani 1 1 d . . . . .
H64 H 0.512087 1.206768 1.031222 0.068 Uiso 1 1 calc R . . . .
C63 C 0.4300(2) 1.2349(2) 0.9450(2) 0.0505(8) Uani 1 1 d . . . . .
H63 H 0.461070 1.180853 0.913090 0.061 Uiso 1 1 calc R . . . .
C28 C 0.24736(18) 0.81186(16) 1.01897(15) 0.0301(5) Uani 1 1 d . . . . .
C29 C 0.30080(19) 0.73999(18) 0.96511(17) 0.0360(5) Uani 1 1 d . . . . .
H29 H 0.313815 0.747995 0.905066 0.043 Uiso 1 1 calc R . . . .
C33 C 0.2295(2) 0.79856(19) 1.10709(17) 0.0387(6) Uani 1 1 d . . . . .
H33 H 0.194795 0.847990 1.144504 0.046 Uiso 1 1 calc R . . . .
C24 C 0.4202(2) 0.6663(3) 0.3203(3) 0.0743(14) Uani 1 1 d . . . . .
H24 H 0.457552 0.609428 0.295847 0.089 Uiso 1 1 calc R . . . .
C25 C 0.3924(2) 0.6765(2) 0.4065(3) 0.0590(10) Uani 1 1 d . . . . .
H25 H 0.411836 0.627310 0.442061 0.071 Uiso 1 1 calc R . . . .
C23 C 0.3944(2) 0.7378(4) 0.2687(3) 0.0771(15) Uani 1 1 d . . . . .
H23 H 0.416239 0.730613 0.208524 0.093 Uiso 1 1 calc R . . . .
C10 C 0.32464(18) 0.93331(17) 0.68547(15) 0.0322(5) Uani 1 1 d . . . . .
H10 H 0.389849 0.946069 0.672409 0.039 Uiso 1 1 calc R . . . .
C32 C 0.2618(2) 0.7144(2) 1.14031(19) 0.0447(7) Uani 1 1 d . . . . .
H32 H 0.246604 0.705308 1.200315 0.054 Uiso 1 1 calc R . . . .
C30 C 0.3355(2) 0.6558(2) 0.9992(2) 0.0472(7) Uani 1 1 d . . . . .
H30 H 0.372761 0.606645 0.962167 0.057 Uiso 1 1 calc R . . . .
C31 C 0.3160(2) 0.6435(2) 1.0862(2) 0.0485(7) Uani 1 1 d . . . . .
H31 H 0.340094 0.586016 1.108930 0.058 Uiso 1 1 calc R . . . .
Cl9 Cl 0.3931(4) 0.9888(4) 1.0600(3) 0.152(2) Uani 0.5 1 d D U P A -1
Cl10 Cl 0.5972(3) 1.0047(2) 0.9817(3) 0.0952(11) Uani 0.5 1 d D U P A -1
C67 C 0.4926(8) 0.9828(9) 0.9609(6) 0.135(4) Uani 0.5 1 d D U P A -1
H67A H 0.509181 0.921750 0.935651 0.162 Uiso 0.5 1 calc R . P A -1
H67B H 0.469614 1.027763 0.919544 0.162 Uiso 0.5 1 calc R . P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 Cl1 2.2872(6) . ?
Ge1 N5 2.1696(17) . ?
Ge1 N4 2.1499(17) . ?
Ge1 N8 2.1847(19) . ?
Ge4 Cl8 2.2835(8) . ?
Ge4 Cl7 2.3182(8) . ?
Ge4 Cl6 2.3195(10) . ?
Ge2 Cl2 2.2884(5) . ?
Ge2 N2 2.1373(17) . ?
Ge2 N3 2.1999(17) . ?
Ge2 N0AA 2.2338(17) . ?
Ge3 Cl4 2.2768(6) . ?
Ge3 Cl5 2.3187(7) . ?
Ge3 Cl3 2.3361(6) . ?
N2 C41 1.355(3) . ?
N2 C45 1.355(3) . ?
N3 C52 1.383(3) . ?
N3 C46 1.315(3) . ?
N0AA C40 1.324(2) . ?
N0AA C34 1.383(3) . ?
N7 C40 1.369(2) . ?
N7 C39 1.382(3) . ?
N7 C53 1.480(2) . ?
C41 C40 1.465(3) . ?
C41 C42 1.394(3) . ?
C45 C44 1.384(3) . ?
C45 C46 1.469(3) . ?
N6 C7 1.364(3) . ?
N6 C6 1.389(3) . ?
N6 C20 1.473(3) . ?
N5 C7 1.328(3) . ?
N5 C1 1.379(3) . ?
N4 C8 1.358(3) . ?
N4 C12 1.350(3) . ?
C8 C7 1.468(3) . ?
C8 C9 1.392(3) . ?
C2 C1 1.396(3) . ?
C2 C3 1.381(3) . ?
C1 C6 1.402(3) . ?
C6 C5 1.392(3) . ?
C3 C4 1.410(3) . ?
C34 C39 1.402(3) . ?
C34 C35 1.397(3) . ?
C38 C39 1.401(3) . ?
C38 C37 1.377(3) . ?
C4 C5 1.380(3) . ?
C53 C54 1.517(3) . ?
C35 C36 1.380(3) . ?
C20 C21 1.514(3) . ?
C36 C37 1.406(3) . ?
C42 C43 1.376(3) . ?
C43 C44 1.377(3) . ?
N8 C13 1.320(3) . ?
N8 C19 1.378(3) . ?
N9 C13 1.368(3) . ?
N9 C14 1.392(3) . ?
N9 C27 1.474(3) . ?
N10 C60 1.468(3) . ?
N10 C46 1.365(3) . ?
N10 C47 1.389(3) . ?
C54 C59 1.385(3) . ?
C54 C55 1.387(3) . ?
C59 C58 1.386(3) . ?
C12 C13 1.475(3) . ?
C12 C11 1.390(3) . ?
C19 C14 1.396(3) . ?
C19 C18 1.398(3) . ?
C9 C10 1.373(3) . ?
C11 C10 1.386(3) . ?
C14 C15 1.399(3) . ?
C27 C28 1.508(3) . ?
C52 C47 1.394(3) . ?
C52 C51 1.392(3) . ?
C60 C61 1.499(3) . ?
C48 C47 1.399(3) . ?
C48 C49 1.380(4) . ?
C15 C16 1.378(4) . ?
C51 C50 1.388(3) . ?
C61 C66 1.383(3) . ?
C61 C62 1.388(3) . ?
C50 C49 1.403(4) . ?
C66 C65 1.382(4) . ?
C58 C57 1.377(4) . ?
C55 C56 1.393(4) . ?
C57 C56 1.383(5) . ?
C21 C26 1.382(4) . ?
C21 C22 1.384(4) . ?
C26 C25 1.393(4) . ?
C22 C23 1.413(5) . ?
C16 C17 1.401(4) . ?
C62 C63 1.384(4) . ?
C18 C17 1.384(3) . ?
C65 C64 1.381(4) . ?
C64 C63 1.373(4) . ?
C28 C29 1.384(3) . ?
C28 C33 1.398(3) . ?
C29 C30 1.394(4) . ?
C33 C32 1.380(4) . ?
C24 C25 1.360(6) . ?
C24 C23 1.370(7) . ?
C32 C31 1.378(5) . ?
C30 C31 1.377(5) . ?
Cl9 C67 1.820(8) . ?
Cl10 C67 1.713(8) . ?

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
N5 Ge1 Cl1 87.50(5) . . ?
N5 Ge1 N8 140.60(7) . . ?
N4 Ge1 Cl1 105.49(5) . . ?
N4 Ge1 N5 73.08(7) . . ?
N4 Ge1 N8 72.02(7) . . ?
N8 Ge1 Cl1 84.68(5) . . ?
Cl8 Ge4 Cl7 96.15(3) . . ?
Cl8 Ge4 Cl6 94.36(3) . . ?
Cl7 Ge4 Cl6 95.04(3) . . ?
N2 Ge2 Cl2 100.90(5) . . ?
N2 Ge2 N3 73.14(7) . . ?
N2 Ge2 N0AA 72.53(6) . . ?
N3 Ge2 Cl2 85.73(5) . . ?
N3 Ge2 N0AA 142.82(7) . . ?
N0AA Ge2 Cl2 87.09(4) . . ?
Cl4 Ge3 Cl5 94.93(2) . . ?
Cl4 Ge3 Cl3 95.28(2) . . ?
Cl5 Ge3 Cl3 95.94(2) . . ?
C41 N2 Ge2 119.19(13) . . ?
C41 N2 C45 119.49(18) . . ?
C45 N2 Ge2 119.79(14) . . ?
C52 N3 Ge2 136.68(15) . . ?
C46 N3 Ge2 116.47(14) . . ?
C46 N3 C52 106.82(18) . . ?
C40 N0AA Ge2 114.11(13) . . ?
C40 N0AA C34 106.77(16) . . ?
C34 N0AA Ge2 136.30(13) . . ?
C40 N7 C39 106.26(16) . . ?
C40 N7 C53 132.22(18) . . ?
C39 N7 C53 121.22(17) . . ?
N2 C41 C40 112.39(17) . . ?
N2 C41 C42 120.77(19) . . ?
C42 C41 C40 126.83(19) . . ?
N0AA C40 N7 111.99(18) . . ?
N0AA C40 C41 117.12(17) . . ?
N7 C40 C41 130.82(18) . . ?
N2 C45 C44 121.5(2) . . ?
N2 C45 C46 111.81(18) . . ?
C44 C45 C46 126.6(2) . . ?
C7 N6 C6 106.41(17) . . ?
C7 N6 C20 131.51(19) . . ?
C6 N6 C20 121.94(18) . . ?
C7 N5 Ge1 116.46(14) . . ?
C7 N5 C1 106.95(17) . . ?
C1 N5 Ge1 134.98(14) . . ?
C8 N4 Ge1 118.97(14) . . ?
C12 N4 Ge1 119.73(13) . . ?
C12 N4 C8 119.96(18) . . ?
N4 C8 C7 111.49(17) . . ?
N4 C8 C9 120.9(2) . . ?
C9 C8 C7 127.61(19) . . ?
N6 C7 C8 131.05(18) . . ?
N5 C7 N6 111.82(19) . . ?
N5 C7 C8 117.13(18) . . ?
C3 C2 C1 117.0(2) . . ?
N5 C1 C2 130.77(19) . . ?
N5 C1 C6 108.17(18) . . ?
C2 C1 C6 121.0(2) . . ?
N6 C6 C1 106.63(18) . . ?
N6 C6 C5 131.16(19) . . ?
C5 C6 C1 122.2(2) . . ?
C2 C3 C4 121.4(2) . . ?
N0AA C34 C39 108.06(18) . . ?
N0AA C34 C35 130.95(18) . . ?
C35 C34 C39 120.98(19) . . ?
C37 C38 C39 116.25(19) . . ?
C5 C4 C3 122.1(2) . . ?
C4 C5 C6 116.2(2) . . ?
N7 C39 C34 106.91(17) . . ?
N7 C39 C38 131.10(19) . . ?
C38 C39 C34 121.98(19) . . ?
N7 C53 C54 111.12(17) . . ?
C36 C35 C34 117.0(2) . . ?
N6 C20 C21 111.37(18) . . ?
C35 C36 C37 121.7(2) . . ?
C43 C42 C41 119.3(2) . . ?
C42 C43 C44 120.0(2) . . ?
C43 C44 C45 118.9(2) . . ?
C13 N8 Ge1 116.93(14) . . ?
C13 N8 C19 107.07(19) . . ?
C19 N8 Ge1 134.25(16) . . ?
C13 N9 C14 106.03(19) . . ?
C13 N9 C27 131.96(19) . . ?
C14 N9 C27 121.63(19) . . ?
C46 N10 C60 132.1(2) . . ?
C46 N10 C47 105.78(18) . . ?
C47 N10 C60 121.99(18) . . ?
C59 C54 C53 120.8(2) . . ?
C59 C54 C55 119.3(2) . . ?
C55 C54 C53 119.9(2) . . ?
C54 C59 C58 120.6(2) . . ?
N4 C12 C13 111.44(18) . . ?
N4 C12 C11 121.13(19) . . ?
C11 C12 C13 127.4(2) . . ?
N8 C13 N9 111.93(18) . . ?
N8 C13 C12 116.04(19) . . ?
N9 C13 C12 131.9(2) . . ?
N8 C19 C14 108.3(2) . . ?
N8 C19 C18 130.3(2) . . ?
C14 C19 C18 121.4(2) . . ?
C10 C9 C8 119.0(2) . . ?
C10 C11 C12 118.8(2) . . ?
N9 C14 C19 106.66(19) . . ?
N9 C14 C15 131.3(2) . . ?
C19 C14 C15 122.0(2) . . ?
N9 C27 C28 110.89(19) . . ?
N3 C52 C47 108.0(2) . . ?
N3 C52 C51 130.5(2) . . ?
C51 C52 C47 121.4(2) . . ?
N10 C60 C61 112.89(18) . . ?
N3 C46 C45 117.43(18) . . ?
N3 C46 N10 112.42(19) . . ?
N10 C46 C45 130.1(2) . . ?
C49 C48 C47 115.8(2) . . ?
N10 C47 C52 106.95(18) . . ?
N10 C47 C48 130.8(2) . . ?
C52 C47 C48 122.2(2) . . ?
C16 C15 C14 115.9(3) . . ?
C38 C37 C36 122.1(2) . . ?
C50 C51 C52 116.6(2) . . ?
C66 C61 C60 119.1(2) . . ?
C66 C61 C62 118.9(2) . . ?
C62 C61 C60 121.9(2) . . ?
C51 C50 C49 121.5(2) . . ?
C48 C49 C50 122.4(2) . . ?
C65 C66 C61 121.0(2) . . ?
C57 C58 C59 120.1(2) . . ?
C54 C55 C56 120.0(3) . . ?
C58 C57 C56 119.8(3) . . ?
C26 C21 C20 120.9(2) . . ?
C26 C21 C22 119.5(3) . . ?
C22 C21 C20 119.6(3) . . ?
C21 C26 C25 120.9(3) . . ?
C21 C22 C23 118.7(4) . . ?
C57 C56 C55 120.2(3) . . ?
C15 C16 C17 122.6(2) . . ?
C63 C62 C61 120.2(2) . . ?
C17 C18 C19 116.6(3) . . ?
C18 C17 C16 121.5(2) . . ?
C66 C65 C64 119.5(3) . . ?
C63 C64 C65 120.2(3) . . ?
C64 C63 C62 120.2(3) . . ?
C29 C28 C27 121.4(2) . . ?
C29 C28 C33 119.1(2) . . ?
C33 C28 C27 119.5(2) . . ?
C28 C29 C30 119.8(3) . . ?
C32 C33 C28 120.7(3) . . ?
C25 C24 C23 120.2(3) . . ?
C24 C25 C26 119.8(4) . . ?
C24 C23 C22 120.7(3) . . ?
C9 C10 C11 120.2(2) . . ?
C31 C32 C33 119.8(3) . . ?
C31 C30 C29 120.4(3) . . ?
C30 C31 C32 120.2(3) . . ?
Cl10 C67 Cl9 109.0(5) . . ?

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

data_as722_p-1_new
_database_code_depnum_ccdc_archive 'CCDC 1895472'
loop_
_audit_author_name
_audit_author_address
"Ala'aeddeen Swidan"
;University of Windsor
Canada
;
_audit_update_record             
;
2019-02-04 deposited with the CCDC.	2019-05-03 downloaded from the CCDC.
;

_audit_creation_date             2019-01-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(Cl3 Ge), C66 H50 N10 Ni, 1.5(C4 H8 O)'
_chemical_formula_sum            'C72 H62 Cl6 Ge2 N10 Ni O1.50'
_chemical_formula_weight         1507.90
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

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

_cell_length_a                   13.6605(8)
_cell_length_b                   14.1678(9)
_cell_length_c                   19.8848(14)
_cell_angle_alpha                82.572(2)
_cell_angle_beta                 76.130(2)
_cell_angle_gamma                62.991(2)
_cell_volume                     3327.9(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9874
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      32.126
_cell_measurement_theta_min      2.914
_shelx_estimated_absorpt_T_max   0.738
_shelx_estimated_absorpt_T_min   0.627
_exptl_absorpt_coefficient_mu    1.473
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.6353
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0593 before and 0.0395 after correction. The Ratio of minimum to maximum transmission is 0.8509. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       cubic
_exptl_crystal_F_000             1540
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.22
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            44388
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.877
_diffrn_reflns_theta_min         2.821
_diffrn_ambient_temperature      170.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX3 Photon 100'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12245
_reflns_number_total             15560
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       APEX3
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.878
_refine_diff_density_min         -1.016
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     893
_refine_ls_number_reflns         15560
_refine_ls_number_restraints     174
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0403
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0366P)²+6.0569P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.1055
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C1A-C1B \\sim C1B-C1C \\sim C1C-C1D
 with sigma of 0.02
 O2-C1A \\sim O2-C1D
 with sigma of 0.02
 O2-C1B \\sim O2-C1C
 with sigma of 0.04
 C1B-C1D \\sim C1A-C1C
 with sigma of 0.04
 C1E-C1F \\sim C1F-C1G \\sim C1G-C1H
 with sigma of 0.02
 O1-C1E \\sim O1-C1H
 with sigma of 0.02
 O1-C1F \\sim O1-C1G
 with sigma of 0.04
 C1F-C1H \\sim C1E-C1G
 with sigma of 0.04
 O2-C1A \\sim O2-C0AA
 with sigma of 0.02
 O2-C1D \\sim O2-C3AA
 with sigma of 0.02
 C1A-C1B \\sim C0AA-C1AA
 with sigma of 0.02
 C1B-C1C \\sim C1AA-C2AA
 with sigma of 0.02
 C1C-C1D \\sim C2AA-C3AA
 with sigma of 0.02
 O2-C1B \\sim O2-C1AA
 with sigma of 0.04
 O2-C1C \\sim O2-C2AA
 with sigma of 0.04
 C1A-C1C \\sim C0AA-C2AA
 with sigma of 0.04
 C1B-C1D \\sim C1AA-C3AA
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O2 \\sim C1A \\sim C1B \\sim C1C \\sim C1D: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O1 \\sim C1E \\sim C1F \\sim C1G \\sim C1H: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 O1, C1H, C1G, C1E, C1F
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C1A, C1B, C1C, C0AA, O2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C3AA, C2AA, C1AA, C0AA, O2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=Sof(C1AA)=Sof(H1AC)=Sof(H1AD)=Sof(C2AA)=
 Sof(H2AA)=Sof(H2AB)=Sof(C3AA)=Sof(H3AA)=Sof(H3AB)=1-FVAR(1)
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(C1C)=Sof(H1CA)=
 Sof(H1CB)=Sof(C1D)=Sof(H1DA)=Sof(H1DB)=FVAR(1)
 Fixed Sof: O1(0.5) C1E(0.5) H1EA(0.5) H1EB(0.5) C1F(0.5) H1FA(0.5) H1FB(0.5)
 C1G(0.5) H1GA(0.5) H1GB(0.5) C1H(0.5) H1HA(0.5) H1HB(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C60(H60A,H60B), C53(H53A,H53B), C20(H20A,H20B), C1A(H1AA,
 H1AB), C1B(H1BA,H1BB), C1C(H1CA,H1CB), C1D(H1DA,H1DB), C1E(H1EA,H1EB),
 C1F(H1FA,H1FB), C1G(H1GA,H1GB), C1H(H1HA,H1HB), C0AA(H0AA,H0AB), C1AA(H1AC,
 H1AD), C2AA(H2AA,H2AB), C3AA(H3AA,H3AB)
6.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C42(H42), C9(H9), C10(H10), C51(H51), C43(H43), C2(H2), C18(H18),
 C48(H48), C44(H44), C49(H49), C17(H17), C16(H16), C15(H15), C3(H3), C5(H5),
 C33(H33), C50(H50), C35(H35), C66(H66), C4(H4), C36(H36), C63(H63), C55(H55),
 C64(H64), C38(H38), C37(H37), C26(H26), C62(H62), C32(H32), C31(H31), C22(H22),
  C29(H29), C56(H56), C65(H65), C23(H23), C30(H30), C24(H24), C25(H25),
 C59(H59), C57(H57), C58(H58)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge2 Ge 0.86132(2) 0.03104(2) 0.46721(2) 0.02651(7) Uani 1 1 d . . . . .
Ni1 Ni 0.53897(2) 0.32491(2) 0.71958(2) 0.01512(7) Uani 1 1 d . . . . .
Ge1 Ge 0.93118(3) -0.23912(3) 0.82033(2) 0.04280(10) Uani 1 1 d . . . . .
Cl6 Cl 0.86251(5) 0.09594(5) 0.35379(4) 0.03047(15) Uani 1 1 d . . . . .
Cl5 Cl 0.67839(6) 0.05206(6) 0.48743(4) 0.03291(15) Uani 1 1 d . . . . .
Cl4 Cl 0.94899(6) -0.14335(5) 0.44013(4) 0.03790(17) Uani 1 1 d . . . . .
Cl2 Cl 0.96593(9) -0.32829(8) 0.72330(5) 0.0592(3) Uani 1 1 d . . . . .
Cl1 Cl 0.74091(8) -0.16278(10) 0.83975(5) 0.0705(3) Uani 1 1 d . . . . .
Cl3 Cl 0.95423(9) -0.37990(10) 0.89892(6) 0.0669(3) Uani 1 1 d . . . . .
N3 N 0.41572(16) 0.47425(15) 0.74150(10) 0.0158(4) Uani 1 1 d . . . . .
N8 N 0.66015(16) 0.17520(15) 0.69673(10) 0.0167(4) Uani 1 1 d . . . . .
N9 N 0.45306(17) 0.11252(16) 0.65127(11) 0.0192(4) Uani 1 1 d . . . . .
N5 N 0.55703(16) 0.40714(14) 0.62496(10) 0.0163(4) Uani 1 1 d . . . . .
N6 N 0.67656(17) 0.32789(16) 0.74498(10) 0.0195(4) Uani 1 1 d . . . . .
N4 N 0.51896(17) 0.56714(15) 0.57382(10) 0.0188(4) Uani 1 1 d . . . . .
N10 N 0.45138(17) 0.25614(15) 0.68781(10) 0.0181(4) Uani 1 1 d . . . . .
N7 N 0.85798(18) 0.24058(17) 0.75095(12) 0.0242(4) Uani 1 1 d . . . . .
N1 N 0.46932(17) 0.31095(16) 0.82422(10) 0.0195(4) Uani 1 1 d . . . . .
N2 N 0.34047(19) 0.38885(17) 0.91813(11) 0.0242(5) Uani 1 1 d . . . . .
C8 C 0.3421(2) 0.49174(19) 0.80247(12) 0.0191(5) Uani 1 1 d . . . . .
C40 C 0.7695(2) 0.23685(19) 0.73337(12) 0.0192(5) Uani 1 1 d . . . . .
C41 C 0.7633(2) 0.14778(19) 0.70610(12) 0.0191(5) Uani 1 1 d . . . . .
C52 C 0.3441(2) 0.28068(19) 0.68181(12) 0.0189(5) Uani 1 1 d . . . . .
C46 C 0.5144(2) 0.15518(18) 0.66965(12) 0.0180(5) Uani 1 1 d . . . . .
C45 C 0.6344(2) 0.10588(19) 0.67325(12) 0.0183(5) Uani 1 1 d . . . . .
C14 C 0.6108(2) 0.49409(19) 0.53045(12) 0.0196(5) Uani 1 1 d . . . . .
C13 C 0.4907(2) 0.51030(18) 0.62942(12) 0.0172(4) Uani 1 1 d . . . . .
C39 C 0.8189(2) 0.3408(2) 0.77615(13) 0.0249(5) Uani 1 1 d . . . . .
C11 C 0.3029(2) 0.64448(19) 0.69832(14) 0.0227(5) Uani 1 1 d . . . . .
H11 H 0.289481 0.695911 0.661617 0.027 Uiso 1 1 calc R . . . .
C34 C 0.7048(2) 0.3944(2) 0.77256(13) 0.0216(5) Uani 1 1 d . . . . .
C12 C 0.39906(19) 0.54885(18) 0.69056(12) 0.0169(4) Uani 1 1 d . . . . .
C42 C 0.8486(2) 0.0459(2) 0.69240(14) 0.0257(5) Uani 1 1 d . . . . .
H42 H 0.921737 0.026199 0.699716 0.031 Uiso 1 1 calc R . . . .
C1 C 0.4906(2) 0.23964(19) 0.87922(13) 0.0215(5) Uani 1 1 d . . . . .
C9 C 0.2459(2) 0.5873(2) 0.81435(14) 0.0239(5) Uani 1 1 d . . . . .
H9 H 0.194610 0.600299 0.857723 0.029 Uiso 1 1 calc R . . . .
C19 C 0.6346(2) 0.39438(19) 0.56320(12) 0.0184(5) Uani 1 1 d . . . . .
C7 C 0.3807(2) 0.39829(19) 0.84913(12) 0.0201(5) Uani 1 1 d . . . . .
C47 C 0.3433(2) 0.19157(19) 0.65920(13) 0.0204(5) Uani 1 1 d . . . . .
C61 C 0.4594(2) -0.06210(19) 0.69333(13) 0.0221(5) Uani 1 1 d . . . . .
C10 C 0.2269(2) 0.6628(2) 0.76130(14) 0.0257(5) Uani 1 1 d . . . . .
H10 H 0.160985 0.728172 0.768025 0.031 Uiso 1 1 calc R . . . .
C51 C 0.2446(2) 0.3745(2) 0.69548(14) 0.0245(5) Uani 1 1 d . . . . .
H51 H 0.243401 0.434924 0.712177 0.029 Uiso 1 1 calc R . . . .
C43 C 0.8232(2) -0.0258(2) 0.66765(14) 0.0272(6) Uani 1 1 d . . . . .
H43 H 0.880051 -0.095554 0.657172 0.033 Uiso 1 1 calc R . . . .
C2 C 0.5727(2) 0.1352(2) 0.88232(14) 0.0259(5) Uani 1 1 d . . . . .
H2 H 0.626239 0.101329 0.842176 0.031 Uiso 1 1 calc R . . . .
C27 C 0.4890(2) 0.68160(19) 0.56694(14) 0.0248(5) Uani 1 1 d . . . . .
H27A H 0.420001 0.720579 0.601446 0.030 Uiso 1 1 calc R . . . .
H27B H 0.473613 0.707800 0.520186 0.030 Uiso 1 1 calc R . . . .
C18 C 0.7259(2) 0.3032(2) 0.53320(14) 0.0252(5) Uani 1 1 d . . . . .
H18 H 0.743212 0.235400 0.554997 0.030 Uiso 1 1 calc R . . . .
C48 C 0.2466(2) 0.1918(2) 0.64717(14) 0.0259(5) Uani 1 1 d . . . . .
H48 H 0.247171 0.130991 0.631487 0.031 Uiso 1 1 calc R . . . .
C28 C 0.5829(2) 0.70242(19) 0.57793(13) 0.0233(5) Uani 1 1 d . . . . .
C44 C 0.7161(2) 0.0030(2) 0.65805(14) 0.0243(5) Uani 1 1 d . . . . .
H44 H 0.698753 -0.046345 0.641437 0.029 Uiso 1 1 calc R . . . .
C49 C 0.1498(2) 0.2860(2) 0.65944(15) 0.0299(6) Uani 1 1 d . . . . .
H49 H 0.082127 0.290358 0.651216 0.036 Uiso 1 1 calc R . . . .
C54 C 0.9760(2) 0.0797(2) 0.81295(14) 0.0282(6) Uani 1 1 d . . . . .
C6 C 0.4104(2) 0.2878(2) 0.93883(13) 0.0249(5) Uani 1 1 d . . . . .
C17 C 0.7899(2) 0.3159(2) 0.47052(14) 0.0289(6) Uani 1 1 d . . . . .
H17 H 0.852585 0.255550 0.448961 0.035 Uiso 1 1 calc R . . . .
C60 C 0.4847(2) 0.00378(19) 0.63183(13) 0.0213(5) Uani 1 1 d . . . . .
H60A H 0.565917 -0.030760 0.611152 0.026 Uiso 1 1 calc R . . . .
H60B H 0.443244 0.006991 0.596348 0.026 Uiso 1 1 calc R . . . .
C16 C 0.7643(2) 0.4164(2) 0.43790(14) 0.0277(6) Uani 1 1 d . . . . .
H16 H 0.809677 0.421800 0.394552 0.033 Uiso 1 1 calc R . . . .
C15 C 0.6753(2) 0.5070(2) 0.46718(13) 0.0244(5) Uani 1 1 d . . . . .
H15 H 0.658729 0.574728 0.445402 0.029 Uiso 1 1 calc R . . . .
C3 C 0.5730(3) 0.0833(2) 0.94598(15) 0.0323(6) Uani 1 1 d . . . . .
H3 H 0.628384 0.012520 0.949874 0.039 Uiso 1 1 calc R . . . .
C5 C 0.4101(3) 0.2351(2) 1.00331(14) 0.0328(6) Uani 1 1 d . . . . .
H5 H 0.355850 0.268119 1.043431 0.039 Uiso 1 1 calc R . . . .
C33 C 0.6255(3) 0.7611(2) 0.52974(15) 0.0305(6) Uani 1 1 d . . . . .
H33 H 0.594612 0.789395 0.489563 0.037 Uiso 1 1 calc R . . . .
C50 C 0.1487(2) 0.3757(2) 0.68382(15) 0.0300(6) Uani 1 1 d . . . . .
H50 H 0.080134 0.438488 0.692381 0.036 Uiso 1 1 calc R . . . .
C35 C 0.6394(3) 0.4984(2) 0.79553(14) 0.0289(6) Uani 1 1 d . . . . .
H35 H 0.561752 0.534934 0.794480 0.035 Uiso 1 1 calc R . . . .
C53 C 0.9710(2) 0.1555(2) 0.75185(15) 0.0273(6) Uani 1 1 d . . . . .
H53A H 1.021794 0.187659 0.752326 0.033 Uiso 1 1 calc R . . . .
H53B H 0.998884 0.115254 0.708677 0.033 Uiso 1 1 calc R . . . .
C66 C 0.3775(2) -0.0953(2) 0.69550(15) 0.0291(6) Uani 1 1 d . . . . .
H66 H 0.337796 -0.075955 0.658879 0.035 Uiso 1 1 calc R . . . .
C21 C 0.2700(2) 0.5585(2) 0.97751(13) 0.0289(6) Uani 1 1 d . . . . .
C4 C 0.4924(3) 0.1332(2) 1.00558(15) 0.0343(7) Uani 1 1 d . . . . .
H4 H 0.495398 0.095025 1.048569 0.041 Uiso 1 1 calc R . . . .
C36 C 0.6931(3) 0.5454(2) 0.81982(16) 0.0364(7) Uani 1 1 d . . . . .
H36 H 0.651257 0.616053 0.835569 0.044 Uiso 1 1 calc R . . . .
C20 C 0.2465(2) 0.4688(2) 0.96425(14) 0.0304(6) Uani 1 1 d . . . . .
H20A H 0.229486 0.434149 1.009043 0.036 Uiso 1 1 calc R . . . .
H20B H 0.179183 0.498383 0.943419 0.036 Uiso 1 1 calc R . . . .
C63 C 0.4927(3) -0.1536(2) 0.80234(16) 0.0383(7) Uani 1 1 d . . . . .
H63 H 0.532433 -0.173677 0.838972 0.046 Uiso 1 1 calc R . . . .
C55 C 0.8834(2) 0.0729(2) 0.85544(15) 0.0317(6) Uani 1 1 d . . . . .
H55 H 0.810685 0.119148 0.847102 0.038 Uiso 1 1 calc R . . . .
C64 C 0.4113(3) -0.1862(2) 0.80421(17) 0.0411(8) Uani 1 1 d . . . . .
H64 H 0.395043 -0.228822 0.841990 0.049 Uiso 1 1 calc R . . . .
C38 C 0.8720(3) 0.3892(2) 0.80082(16) 0.0344(6) Uani 1 1 d . . . . .
H38 H 0.949254 0.352915 0.802950 0.041 Uiso 1 1 calc R . . . .
C37 C 0.8071(3) 0.4921(3) 0.82189(17) 0.0384(7) Uani 1 1 d . . . . .
H37 H 0.840718 0.527958 0.838319 0.046 Uiso 1 1 calc R . . . .
C26 C 0.3754(3) 0.5559(2) 0.95954(16) 0.0356(7) Uani 1 1 d . . . . .
H26 H 0.437251 0.495818 0.937119 0.043 Uiso 1 1 calc R . . . .
C62 C 0.5169(3) -0.0917(2) 0.74730(15) 0.0306(6) Uani 1 1 d . . . . .
H62 H 0.573018 -0.069300 0.746422 0.037 Uiso 1 1 calc R . . . .
C32 C 0.7129(3) 0.7789(3) 0.53946(18) 0.0400(7) Uani 1 1 d . . . . .
H32 H 0.741950 0.818798 0.505821 0.048 Uiso 1 1 calc R . . . .
C31 C 0.7578(3) 0.7388(2) 0.59790(18) 0.0407(7) Uani 1 1 d . . . . .
H31 H 0.817847 0.750794 0.604483 0.049 Uiso 1 1 calc R . . . .
C22 C 0.1798(3) 0.6475(3) 1.01003(17) 0.0413(7) Uani 1 1 d . . . . .
H22 H 0.106795 0.650584 1.022079 0.050 Uiso 1 1 calc R . . . .
C29 C 0.6287(3) 0.6627(2) 0.63673(16) 0.0349(7) Uani 1 1 d . . . . .
H29 H 0.600257 0.622334 0.670318 0.042 Uiso 1 1 calc R . . . .
C56 C 0.8944(3) -0.0002(3) 0.91010(17) 0.0404(7) Uani 1 1 d . . . . .
H56 H 0.829621 -0.003723 0.938815 0.049 Uiso 1 1 calc R . . . .
C65 C 0.3535(3) -0.1570(2) 0.75116(17) 0.0387(7) Uani 1 1 d . . . . .
H65 H 0.296904 -0.179036 0.752626 0.046 Uiso 1 1 calc R . . . .
C23 C 0.1965(4) 0.7317(3) 1.0248(2) 0.0533(10) Uani 1 1 d . . . . .
H23 H 0.135027 0.792005 1.047343 0.064 Uiso 1 1 calc R . . . .
C30 C 0.7150(3) 0.6811(3) 0.64689(18) 0.0434(8) Uani 1 1 d . . . . .
H30 H 0.745067 0.654089 0.687487 0.052 Uiso 1 1 calc R . . . .
C24 C 0.3018(4) 0.7279(3) 1.0070(2) 0.0518(10) Uani 1 1 d . . . . .
H24 H 0.312853 0.785547 1.017440 0.062 Uiso 1 1 calc R . . . .
C25 C 0.3917(3) 0.6409(3) 0.97406(18) 0.0454(8) Uani 1 1 d . . . . .
H25 H 0.464178 0.638946 0.961321 0.054 Uiso 1 1 calc R . . . .
C59 C 1.0811(3) 0.0105(3) 0.8258(2) 0.0604(11) Uani 1 1 d . . . . .
H59 H 1.146077 0.013362 0.796893 0.073 Uiso 1 1 calc R . . . .
C57 C 0.9987(3) -0.0674(3) 0.9227(2) 0.0578(10) Uani 1 1 d . . . . .
H57 H 1.006459 -0.116927 0.960506 0.069 Uiso 1 1 calc R . . . .
C58 C 1.0925(4) -0.0626(4) 0.8802(3) 0.0830(17) Uani 1 1 d . . . . .
H58 H 1.165129 -0.109664 0.888342 0.100 Uiso 1 1 calc R . . . .
O2 O 0.2729(5) 0.1025(4) 0.9109(3) 0.169(2) Uani 1 1 d D U . . .
C1A C 0.1465(11) 0.1870(10) 0.9348(8) 0.166(8) Uani 0.617(10) 1 d D U P A 1
H1AA H 0.094318 0.163142 0.923991 0.199 Uiso 0.617(10) 1 calc R . P A 1
H1AB H 0.128555 0.198308 0.985249 0.199 Uiso 0.617(10) 1 calc R . P A 1
C1B C 0.1388(11) 0.2785(10) 0.8979(9) 0.160(8) Uani 0.617(10) 1 d D U P A 1
H1BA H 0.113169 0.336438 0.930407 0.192 Uiso 0.617(10) 1 calc R . P A 1
H1BB H 0.083014 0.299634 0.868332 0.192 Uiso 0.617(10) 1 calc R . P A 1
C1C C 0.2491(7) 0.2618(6) 0.8543(4) 0.065(2) Uani 0.617(10) 1 d D U P A 1
H1CA H 0.241354 0.305365 0.810989 0.077 Uiso 0.617(10) 1 calc R . P A 1
H1CB H 0.294877 0.276372 0.879457 0.077 Uiso 0.617(10) 1 calc R . P A 1
C1D C 0.2920(10) 0.1569(8) 0.8419(4) 0.095(4) Uani 0.617(10) 1 d D U P A 1
H1DA H 0.373196 0.128205 0.821174 0.114 Uiso 0.617(10) 1 calc R . P A 1
H1DB H 0.253601 0.145737 0.809414 0.114 Uiso 0.617(10) 1 calc R . P A 1
O1 O 0.9549(5) 0.4769(5) 0.5893(3) 0.0651(15) Uani 0.5 1 d D U P B -1
C1E C 1.0364(13) 0.5121(14) 0.5530(6) 0.068(3) Uani 0.5 1 d D U P B -1
H1EA H 1.112911 0.453719 0.550327 0.081 Uiso 0.5 1 calc R . P B -1
H1EB H 1.030630 0.571628 0.577396 0.081 Uiso 0.5 1 calc R . P B -1
C1F C 1.0141(8) 0.5472(8) 0.4822(5) 0.068(2) Uani 0.5 1 d D U P B -1
H1FA H 1.085012 0.524323 0.447123 0.082 Uiso 0.5 1 calc R . P B -1
H1FB H 0.971455 0.625175 0.478996 0.082 Uiso 0.5 1 calc R . P B -1
C1G C 0.9459(17) 0.4934(18) 0.4727(6) 0.090(4) Uani 0.5 1 d D U P B -1
H1GA H 0.874919 0.545872 0.459374 0.108 Uiso 0.5 1 calc R . P B -1
H1GB H 0.988301 0.440205 0.435924 0.108 Uiso 0.5 1 calc R . P B -1
C1H C 0.9220(10) 0.4407(8) 0.5406(5) 0.075(3) Uani 0.5 1 d D U P B -1
H1HA H 0.840937 0.459166 0.554411 0.090 Uiso 0.5 1 calc R . P B -1
H1HB H 0.964553 0.362790 0.537045 0.090 Uiso 0.5 1 calc R . P B -1
C0AA C 0.267(2) 0.133(2) 0.8348(8) 0.192(15) Uani 0.383(10) 1 d D U P A 2
H0AA H 0.325320 0.155874 0.811272 0.231 Uiso 0.383(10) 1 calc R . P A 2
H0AB H 0.273725 0.074042 0.809367 0.231 Uiso 0.383(10) 1 calc R . P A 2
C1AA C 0.1573(14) 0.2191(11) 0.8412(10) 0.127(7) Uani 0.383(10) 1 d D U P A 2
H1AC H 0.146699 0.259048 0.796743 0.153 Uiso 0.383(10) 1 calc R . P A 2
H1AD H 0.098459 0.194077 0.856986 0.153 Uiso 0.383(10) 1 calc R . P A 2
C2AA C 0.1559(12) 0.2806(10) 0.8910(9) 0.085(5) Uani 0.383(10) 1 d D U P A 2
H2AA H 0.082011 0.342664 0.902790 0.102 Uiso 0.383(10) 1 calc R . P A 2
H2AB H 0.215282 0.305080 0.875775 0.102 Uiso 0.383(10) 1 calc R . P A 2
C3AA C 0.1784(14) 0.2033(12) 0.9499(9) 0.113(5) Uani 0.383(10) 1 d D U P A 2
H3AA H 0.111273 0.192516 0.972914 0.135 Uiso 0.383(10) 1 calc R . P A 2
H3AB H 0.205054 0.225054 0.984582 0.135 Uiso 0.383(10) 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge2 Cl6 2.3221(8) . ?
Ge2 Cl5 2.3170(8) . ?
Ge2 Cl4 2.2752(8) . ?
Ni1 N3 2.0377(19) . ?
Ni1 N8 2.0360(19) . ?
Ni1 N5 2.1047(19) . ?
Ni1 N6 2.079(2) . ?
Ni1 N10 2.088(2) . ?
Ni1 N1 2.095(2) . ?
Ge1 Cl2 2.2782(10) . ?
Ge1 Cl1 2.2690(10) . ?
Ge1 Cl3 2.3192(12) . ?
N3 C8 1.345(3) . ?
N3 C12 1.345(3) . ?
N8 C41 1.334(3) . ?
N8 C45 1.348(3) . ?
N9 C46 1.365(3) . ?
N9 C47 1.391(3) . ?
N9 C60 1.476(3) . ?
N5 C13 1.326(3) . ?
N5 C19 1.387(3) . ?
N6 C40 1.333(3) . ?
N6 C34 1.380(3) . ?
N4 C14 1.386(3) . ?
N4 C13 1.366(3) . ?
N4 C27 1.477(3) . ?
N10 C52 1.376(3) . ?
N10 C46 1.335(3) . ?
N7 C40 1.361(3) . ?
N7 C39 1.385(3) . ?
N7 C53 1.467(3) . ?
N1 C1 1.379(3) . ?
N1 C7 1.324(3) . ?
N2 C7 1.364(3) . ?
N2 C6 1.387(3) . ?
N2 C20 1.468(3) . ?
C8 C9 1.390(3) . ?
C8 C7 1.475(3) . ?
C40 C41 1.480(3) . ?
C41 C42 1.392(3) . ?
C52 C47 1.400(3) . ?
C52 C51 1.401(3) . ?
C46 C45 1.478(3) . ?
C45 C44 1.391(3) . ?
C14 C19 1.404(3) . ?
C14 C15 1.396(3) . ?
C13 C12 1.471(3) . ?
C39 C34 1.405(4) . ?
C39 C38 1.396(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.387(3) . ?
C11 C10 1.389(4) . ?
C34 C35 1.400(4) . ?
C42 H42 0.9500 . ?
C42 C43 1.388(4) . ?
C1 C2 1.398(4) . ?
C1 C6 1.407(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.383(4) . ?
C19 C18 1.400(3) . ?
C47 C48 1.396(4) . ?
C61 C60 1.510(3) . ?
C61 C66 1.387(4) . ?
C61 C62 1.390(4) . ?
C10 H10 0.9500 . ?
C51 H51 0.9500 . ?
C51 C50 1.377(4) . ?
C43 H43 0.9500 . ?
C43 C44 1.384(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.379(4) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.508(4) . ?
C18 H18 0.9500 . ?
C18 C17 1.383(4) . ?
C48 H48 0.9500 . ?
C48 C49 1.384(4) . ?
C28 C33 1.383(4) . ?
C28 C29 1.392(4) . ?
C44 H44 0.9500 . ?
C49 H49 0.9500 . ?
C49 C50 1.410(4) . ?
C54 C53 1.507(4) . ?
C54 C55 1.379(4) . ?
C54 C59 1.385(4) . ?
C6 C5 1.398(4) . ?
C17 H17 0.9500 . ?
C17 C16 1.409(4) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C16 H16 0.9500 . ?
C16 C15 1.379(4) . ?
C15 H15 0.9500 . ?
C3 H3 0.9500 . ?
C3 C4 1.414(4) . ?
C5 H5 0.9500 . ?
C5 C4 1.373(4) . ?
C33 H33 0.9500 . ?
C33 C32 1.387(4) . ?
C50 H50 0.9500 . ?
C35 H35 0.9500 . ?
C35 C36 1.383(4) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C66 H66 0.9500 . ?
C66 C65 1.389(4) . ?
C21 C20 1.512(4) . ?
C21 C26 1.382(4) . ?
C21 C22 1.394(4) . ?
C4 H4 0.9500 . ?
C36 H36 0.9500 . ?
C36 C37 1.396(5) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C63 H63 0.9500 . ?
C63 C64 1.375(5) . ?
C63 C62 1.385(4) . ?
C55 H55 0.9500 . ?
C55 C56 1.387(4) . ?
C64 H64 0.9500 . ?
C64 C65 1.378(5) . ?
C38 H38 0.9500 . ?
C38 C37 1.376(4) . ?
C37 H37 0.9500 . ?
C26 H26 0.9500 . ?
C26 C25 1.395(4) . ?
C62 H62 0.9500 . ?
C32 H32 0.9500 . ?
C32 C31 1.380(5) . ?
C31 H31 0.9500 . ?
C31 C30 1.384(5) . ?
C22 H22 0.9500 . ?
C22 C23 1.391(5) . ?
C29 H29 0.9500 . ?
C29 C30 1.380(4) . ?
C56 H56 0.9500 . ?
C56 C57 1.370(5) . ?
C65 H65 0.9500 . ?
C23 H23 0.9500 . ?
C23 C24 1.374(6) . ?
C30 H30 0.9500 . ?
C24 H24 0.9500 . ?
C24 C25 1.380(5) . ?
C25 H25 0.9500 . ?
C59 H59 0.9500 . ?
C59 C58 1.383(6) . ?
C57 H57 0.9500 . ?
C57 C58 1.381(6) . ?
C58 H58 0.9500 . ?
O2 C1A 1.586(11) . ?
O2 C1D 1.512(9) . ?
O2 C0AA 1.531(15) . ?
O2 C3AA 1.562(14) . ?
C1A H1AA 0.9900 . ?
C1A H1AB 0.9900 . ?
C1A C1B 1.378(11) . ?
C1B H1BA 0.9900 . ?
C1B H1BB 0.9900 . ?
C1B C1C 1.476(11) . ?
C1C H1CA 0.9900 . ?
C1C H1CB 0.9900 . ?
C1C C1D 1.359(10) . ?
C1D H1DA 0.9900 . ?
C1D H1DB 0.9900 . ?
O1 C1E 1.426(12) . ?
O1 C1H 1.396(10) . ?
C1E H1EA 0.9900 . ?
C1E H1EB 0.9900 . ?
C1E C1F 1.485(11) . ?
C1F H1FA 0.9900 . ?
C1F H1FB 0.9900 . ?
C1F C1G 1.501(13) . ?
C1G H1GA 0.9900 . ?
C1G H1GB 0.9900 . ?
C1G C1H 1.495(12) . ?
C1H H1HA 0.9900 . ?
C1H H1HB 0.9900 . ?
C0AA H0AA 0.9900 . ?
C0AA H0AB 0.9900 . ?
C0AA C1AA 1.424(14) . ?
C1AA H1AC 0.9900 . ?
C1AA H1AD 0.9900 . ?
C1AA C2AA 1.393(13) . ?
C2AA H2AA 0.9900 . ?
C2AA H2AB 0.9900 . ?
C2AA C3AA 1.484(13) . ?
C3AA H3AA 0.9900 . ?
C3AA H3AB 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl5 Ge2 Cl6 94.28(3) . . ?
Cl4 Ge2 Cl6 95.97(3) . . ?
Cl4 Ge2 Cl5 97.52(3) . . ?
N3 Ni1 N5 77.72(7) . . ?
N3 Ni1 N6 102.93(8) . . ?
N3 Ni1 N10 101.18(8) . . ?
N3 Ni1 N1 77.19(8) . . ?
N8 Ni1 N3 178.88(8) . . ?
N8 Ni1 N5 102.06(7) . . ?
N8 Ni1 N6 78.16(8) . . ?
N8 Ni1 N10 77.74(8) . . ?
N8 Ni1 N1 103.05(8) . . ?
N6 Ni1 N5 92.49(8) . . ?
N6 Ni1 N10 155.82(8) . . ?
N6 Ni1 N1 91.48(8) . . ?
N10 Ni1 N5 94.43(8) . . ?
N10 Ni1 N1 92.01(8) . . ?
N1 Ni1 N5 154.86(8) . . ?
Cl2 Ge1 Cl3 97.42(4) . . ?
Cl1 Ge1 Cl2 97.87(4) . . ?
Cl1 Ge1 Cl3 97.52(4) . . ?
C8 N3 Ni1 119.30(15) . . ?
C12 N3 Ni1 118.75(15) . . ?
C12 N3 C8 121.1(2) . . ?
C41 N8 Ni1 118.94(16) . . ?
C41 N8 C45 121.6(2) . . ?
C45 N8 Ni1 119.50(16) . . ?
C46 N9 C47 106.6(2) . . ?
C46 N9 C60 131.0(2) . . ?
C47 N9 C60 122.3(2) . . ?
C13 N5 Ni1 112.52(15) . . ?
C13 N5 C19 105.79(19) . . ?
C19 N5 Ni1 139.22(16) . . ?
C40 N6 Ni1 113.42(16) . . ?
C40 N6 C34 106.1(2) . . ?
C34 N6 Ni1 140.47(17) . . ?
C14 N4 C27 121.7(2) . . ?
C13 N4 C14 106.16(19) . . ?
C13 N4 C27 129.5(2) . . ?
C52 N10 Ni1 139.74(16) . . ?
C46 N10 Ni1 113.78(16) . . ?
C46 N10 C52 106.4(2) . . ?
C40 N7 C39 106.6(2) . . ?
C40 N7 C53 129.3(2) . . ?
C39 N7 C53 123.8(2) . . ?
C1 N1 Ni1 139.76(17) . . ?
C7 N1 Ni1 113.71(16) . . ?
C7 N1 C1 106.4(2) . . ?
C7 N2 C6 106.3(2) . . ?
C7 N2 C20 128.6(2) . . ?
C6 N2 C20 125.1(2) . . ?
N3 C8 C9 120.8(2) . . ?
N3 C8 C7 110.1(2) . . ?
C9 C8 C7 129.1(2) . . ?
N6 C40 N7 112.3(2) . . ?
N6 C40 C41 118.3(2) . . ?
N7 C40 C41 129.4(2) . . ?
N8 C41 C40 111.1(2) . . ?
N8 C41 C42 121.2(2) . . ?
C42 C41 C40 127.6(2) . . ?
N10 C52 C47 109.0(2) . . ?
N10 C52 C51 130.7(2) . . ?
C47 C52 C51 120.2(2) . . ?
N9 C46 C45 129.8(2) . . ?
N10 C46 N9 111.8(2) . . ?
N10 C46 C45 118.4(2) . . ?
N8 C45 C46 110.6(2) . . ?
N8 C45 C44 120.1(2) . . ?
C44 C45 C46 129.3(2) . . ?
N4 C14 C19 106.4(2) . . ?
N4 C14 C15 131.4(2) . . ?
C15 C14 C19 122.2(2) . . ?
N5 C13 N4 112.8(2) . . ?
N5 C13 C12 118.5(2) . . ?
N4 C13 C12 128.7(2) . . ?
N7 C39 C34 106.3(2) . . ?
N7 C39 C38 132.0(3) . . ?
C38 C39 C34 121.8(3) . . ?
C12 C11 H11 121.0 . . ?
C12 C11 C10 118.1(2) . . ?
C10 C11 H11 121.0 . . ?
N6 C34 C39 108.8(2) . . ?
N6 C34 C35 130.5(2) . . ?
C35 C34 C39 120.7(2) . . ?
N3 C12 C13 110.5(2) . . ?
N3 C12 C11 120.9(2) . . ?
C11 C12 C13 128.5(2) . . ?
C41 C42 H42 121.2 . . ?
C43 C42 C41 117.7(2) . . ?
C43 C42 H42 121.2 . . ?
N1 C1 C2 130.8(2) . . ?
N1 C1 C6 108.6(2) . . ?
C2 C1 C6 120.6(2) . . ?
C8 C9 H9 120.9 . . ?
C10 C9 C8 118.2(2) . . ?
C10 C9 H9 120.9 . . ?
N5 C19 C14 108.8(2) . . ?
N5 C19 C18 130.6(2) . . ?
C18 C19 C14 120.5(2) . . ?
N1 C7 N2 112.5(2) . . ?
N1 C7 C8 118.6(2) . . ?
N2 C7 C8 128.8(2) . . ?
N9 C47 C52 106.2(2) . . ?
N9 C47 C48 131.0(2) . . ?
C48 C47 C52 122.8(2) . . ?
C66 C61 C60 119.0(2) . . ?
C66 C61 C62 119.1(2) . . ?
C62 C61 C60 121.9(2) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 C11 120.9(2) . . ?
C9 C10 H10 119.6 . . ?
C52 C51 H51 121.2 . . ?
C50 C51 C52 117.5(2) . . ?
C50 C51 H51 121.2 . . ?
C42 C43 H43 119.6 . . ?
C44 C43 C42 120.9(2) . . ?
C44 C43 H43 119.6 . . ?
C1 C2 H2 121.3 . . ?
C3 C2 C1 117.3(3) . . ?
C3 C2 H2 121.3 . . ?
N4 C27 H27A 109.5 . . ?
N4 C27 H27B 109.5 . . ?
N4 C27 C28 110.8(2) . . ?
H27A C27 H27B 108.1 . . ?
C28 C27 H27A 109.5 . . ?
C28 C27 H27B 109.5 . . ?
C19 C18 H18 121.4 . . ?
C17 C18 C19 117.3(2) . . ?
C17 C18 H18 121.4 . . ?
C47 C48 H48 122.0 . . ?
C49 C48 C47 116.0(2) . . ?
C49 C48 H48 122.0 . . ?
C33 C28 C27 120.8(2) . . ?
C33 C28 C29 118.6(3) . . ?
C29 C28 C27 120.6(2) . . ?
C45 C44 H44 120.7 . . ?
C43 C44 C45 118.6(2) . . ?
C43 C44 H44 120.7 . . ?
C48 C49 H49 119.1 . . ?
C48 C49 C50 121.9(3) . . ?
C50 C49 H49 119.1 . . ?
C55 C54 C53 124.3(2) . . ?
C55 C54 C59 118.2(3) . . ?
C59 C54 C53 117.5(3) . . ?
N2 C6 C1 106.3(2) . . ?
N2 C6 C5 131.6(3) . . ?
C5 C6 C1 122.1(2) . . ?
C18 C17 H17 119.2 . . ?
C18 C17 C16 121.6(2) . . ?
C16 C17 H17 119.2 . . ?
N9 C60 C61 112.0(2) . . ?
N9 C60 H60A 109.2 . . ?
N9 C60 H60B 109.2 . . ?
C61 C60 H60A 109.2 . . ?
C61 C60 H60B 109.2 . . ?
H60A C60 H60B 107.9 . . ?
C17 C16 H16 119.1 . . ?
C15 C16 C17 121.8(2) . . ?
C15 C16 H16 119.1 . . ?
C14 C15 H15 121.7 . . ?
C16 C15 C14 116.6(2) . . ?
C16 C15 H15 121.7 . . ?
C2 C3 H3 119.3 . . ?
C2 C3 C4 121.3(3) . . ?
C4 C3 H3 119.3 . . ?
C6 C5 H5 121.8 . . ?
C4 C5 C6 116.5(3) . . ?
C4 C5 H5 121.8 . . ?
C28 C33 H33 119.7 . . ?
C28 C33 C32 120.7(3) . . ?
C32 C33 H33 119.7 . . ?
C51 C50 C49 121.5(3) . . ?
C51 C50 H50 119.2 . . ?
C49 C50 H50 119.2 . . ?
C34 C35 H35 121.6 . . ?
C36 C35 C34 116.9(3) . . ?
C36 C35 H35 121.6 . . ?
N7 C53 C54 113.7(2) . . ?
N7 C53 H53A 108.8 . . ?
N7 C53 H53B 108.8 . . ?
C54 C53 H53A 108.8 . . ?
C54 C53 H53B 108.8 . . ?
H53A C53 H53B 107.7 . . ?
C61 C66 H66 119.9 . . ?
C61 C66 C65 120.1(3) . . ?
C65 C66 H66 119.9 . . ?
C26 C21 C20 123.5(3) . . ?
C26 C21 C22 119.1(3) . . ?
C22 C21 C20 117.4(3) . . ?
C3 C4 H4 118.9 . . ?
C5 C4 C3 122.1(3) . . ?
C5 C4 H4 118.9 . . ?
C35 C36 H36 119.0 . . ?
C35 C36 C37 122.0(3) . . ?
C37 C36 H36 119.0 . . ?
N2 C20 C21 113.1(2) . . ?
N2 C20 H20A 109.0 . . ?
N2 C20 H20B 109.0 . . ?
C21 C20 H20A 109.0 . . ?
C21 C20 H20B 109.0 . . ?
H20A C20 H20B 107.8 . . ?
C64 C63 H63 119.8 . . ?
C64 C63 C62 120.3(3) . . ?
C62 C63 H63 119.8 . . ?
C54 C55 H55 119.4 . . ?
C54 C55 C56 121.2(3) . . ?
C56 C55 H55 119.4 . . ?
C63 C64 H64 120.1 . . ?
C63 C64 C65 119.8(3) . . ?
C65 C64 H64 120.1 . . ?
C39 C38 H38 121.6 . . ?
C37 C38 C39 116.7(3) . . ?
C37 C38 H38 121.6 . . ?
C36 C37 H37 119.1 . . ?
C38 C37 C36 121.9(3) . . ?
C38 C37 H37 119.1 . . ?
C21 C26 H26 119.7 . . ?
C21 C26 C25 120.6(3) . . ?
C25 C26 H26 119.7 . . ?
C61 C62 H62 119.8 . . ?
C63 C62 C61 120.3(3) . . ?
C63 C62 H62 119.8 . . ?
C33 C32 H32 119.9 . . ?
C31 C32 C33 120.1(3) . . ?
C31 C32 H32 119.9 . . ?
C32 C31 H31 120.1 . . ?
C32 C31 C30 119.8(3) . . ?
C30 C31 H31 120.1 . . ?
C21 C22 H22 119.9 . . ?
C23 C22 C21 120.1(3) . . ?
C23 C22 H22 119.9 . . ?
C28 C29 H29 119.6 . . ?
C30 C29 C28 120.9(3) . . ?
C30 C29 H29 119.6 . . ?
C55 C56 H56 120.0 . . ?
C57 C56 C55 120.0(3) . . ?
C57 C56 H56 120.0 . . ?
C66 C65 H65 119.8 . . ?
C64 C65 C66 120.3(3) . . ?
C64 C65 H65 119.8 . . ?
C22 C23 H23 119.9 . . ?
C24 C23 C22 120.1(3) . . ?
C24 C23 H23 119.9 . . ?
C31 C30 H30 120.0 . . ?
C29 C30 C31 120.0(3) . . ?
C29 C30 H30 120.0 . . ?
C23 C24 H24 119.8 . . ?
C23 C24 C25 120.4(3) . . ?
C25 C24 H24 119.8 . . ?
C26 C25 H25 120.2 . . ?
C24 C25 C26 119.6(3) . . ?
C24 C25 H25 120.2 . . ?
C54 C59 H59 119.6 . . ?
C58 C59 C54 120.9(4) . . ?
C58 C59 H59 119.6 . . ?
C56 C57 H57 120.2 . . ?
C56 C57 C58 119.6(4) . . ?
C58 C57 H57 120.2 . . ?
C59 C58 H58 119.9 . . ?
C57 C58 C59 120.1(4) . . ?
C57 C58 H58 119.9 . . ?
C1D O2 C1A 95.0(7) . . ?
C0AA O2 C3AA 103.0(10) . . ?
O2 C1A H1AA 110.7 . . ?
O2 C1A H1AB 110.7 . . ?
H1AA C1A H1AB 108.8 . . ?
C1B C1A O2 105.1(8) . . ?
C1B C1A H1AA 110.7 . . ?
C1B C1A H1AB 110.7 . . ?
C1A C1B H1BA 109.6 . . ?
C1A C1B H1BB 109.6 . . ?
C1A C1B C1C 110.2(9) . . ?
H1BA C1B H1BB 108.1 . . ?
C1C C1B H1BA 109.6 . . ?
C1C C1B H1BB 109.6 . . ?
C1B C1C H1CA 111.9 . . ?
C1B C1C H1CB 111.9 . . ?
H1CA C1C H1CB 109.6 . . ?
C1D C1C C1B 99.6(8) . . ?
C1D C1C H1CA 111.9 . . ?
C1D C1C H1CB 111.9 . . ?
O2 C1D H1DA 110.4 . . ?
O2 C1D H1DB 110.4 . . ?
C1C C1D O2 106.8(6) . . ?
C1C C1D H1DA 110.4 . . ?
C1C C1D H1DB 110.4 . . ?
H1DA C1D H1DB 108.6 . . ?
C1H O1 C1E 107.9(8) . . ?
O1 C1E H1EA 110.1 . . ?
O1 C1E H1EB 110.1 . . ?
O1 C1E C1F 107.8(8) . . ?
H1EA C1E H1EB 108.5 . . ?
C1F C1E H1EA 110.1 . . ?
C1F C1E H1EB 110.1 . . ?
C1E C1F H1FA 111.0 . . ?
C1E C1F H1FB 111.1 . . ?
C1E C1F C1G 103.5(8) . . ?
H1FA C1F H1FB 109.0 . . ?
C1G C1F H1FA 111.0 . . ?
C1G C1F H1FB 111.1 . . ?
C1F C1G H1GA 110.4 . . ?
C1F C1G H1GB 110.4 . . ?
H1GA C1G H1GB 108.6 . . ?
C1H C1G C1F 106.6(9) . . ?
C1H C1G H1GA 110.4 . . ?
C1H C1G H1GB 110.4 . . ?
O1 C1H C1G 107.2(8) . . ?
O1 C1H H1HA 110.3 . . ?
O1 C1H H1HB 110.3 . . ?
C1G C1H H1HA 110.3 . . ?
C1G C1H H1HB 110.3 . . ?
H1HA C1H H1HB 108.5 . . ?
O2 C0AA H0AA 111.5 . . ?
O2 C0AA H0AB 111.5 . . ?
H0AA C0AA H0AB 109.3 . . ?
C1AA C0AA O2 101.4(12) . . ?
C1AA C0AA H0AA 111.5 . . ?
C1AA C0AA H0AB 111.5 . . ?
C0AA C1AA H1AC 111.3 . . ?
C0AA C1AA H1AD 111.3 . . ?
H1AC C1AA H1AD 109.2 . . ?
C2AA C1AA C0AA 102.5(15) . . ?
C2AA C1AA H1AC 111.3 . . ?
C2AA C1AA H1AD 111.3 . . ?
C1AA C2AA H2AA 111.6 . . ?
C1AA C2AA H2AB 111.6 . . ?
C1AA C2AA C3AA 100.9(12) . . ?
H2AA C2AA H2AB 109.4 . . ?
C3AA C2AA H2AA 111.6 . . ?
C3AA C2AA H2AB 111.6 . . ?
O2 C3AA H3AA 111.7 . . ?
O2 C3AA H3AB 111.7 . . ?
C2AA C3AA O2 100.2(11) . . ?
C2AA C3AA H3AA 111.7 . . ?
C2AA C3AA H3AB 111.7 . . ?
H3AA C3AA H3AB 109.5 . . ?

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

data_as662_p-1
_database_code_depnum_ccdc_archive 'CCDC 1895465'
loop_
_audit_author_name
_audit_author_address
"Ala'aeddeen Swidan"
;University of Windsor
Canada
;
_audit_update_record             
;
2019-02-04 deposited with the CCDC.	2019-05-03 downloaded from the CCDC.
;

_audit_creation_date             2018-10-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C33 H25 Cl N5 Sn, Cl3 Sn'
_chemical_formula_sum            'C33 H27 Cl4 N5 Sn2'
_chemical_formula_weight         872.77
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   7.4012(4)
_cell_length_b                   13.5942(8)
_cell_length_c                   16.4392(9)
_cell_angle_alpha                80.1799(19)
_cell_angle_beta                 87.4275(19)
_cell_angle_gamma                79.968(2)
_cell_volume                     1604.65(16)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9674
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      30.52
_cell_measurement_theta_min      3.083
_shelx_estimated_absorpt_T_max   0.802
_shelx_estimated_absorpt_T_min   0.645
_exptl_absorpt_coefficient_mu    1.923
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0588 before and 0.0470 after correction. The Ratio of minimum to maximum transmission is 0.8926. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0119
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            107568
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.588
_diffrn_reflns_theta_min         2.956
_diffrn_ambient_temperature      170.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX3 Photon 100'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9075
_reflns_number_total             9854
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       APEX3
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         0.466
_refine_diff_density_min         -1.108
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         9854
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0220
_refine_ls_restrained_S_all      1.192
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0218P)²+1.2988P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0526
_refine_ls_wR_factor_ref         0.0553
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C27(H27A,H27B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C11(H11), C4(H4), C3(H3), C26(H26), C22(H22), C9(H9),
 C15(H15), C18(H18), C16(H16), C17(H17), C25(H25), C24(H24), C29(H29), C23(H23),
  C33(H33), C30(H30), C10(H10), C32(H32), C31(H31)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.34940(2) 0.00431(2) 0.25757(2) 0.01582(3) Uani 1 1 d . . . . .
Sn2 Sn 0.66222(2) -0.45548(2) 0.28381(2) 0.02319(3) Uani 1 1 d . . . . .
Cl1 Cl 0.07624(6) 0.13773(3) 0.23325(2) 0.02383(8) Uani 1 1 d . . . . .
Cl4 Cl 0.93592(7) -0.48066(4) 0.19131(3) 0.03310(10) Uani 1 1 d . . . . .
Cl3 Cl 0.84064(7) -0.49952(4) 0.41227(3) 0.03074(9) Uani 1 1 d . . . . .
Cl2 Cl 0.66072(6) -0.26951(3) 0.27129(3) 0.03021(9) Uani 1 1 d . . . . .
N2 N 0.21948(17) -0.14594(10) 0.28820(8) 0.0158(2) Uani 1 1 d . . . . .
N6 N 0.20131(18) -0.13577(10) 0.51033(8) 0.0159(2) Uani 1 1 d . . . . .
N1 N 0.25270(18) -0.02930(10) 0.39564(8) 0.0156(2) Uani 1 1 d . . . . .
C7 C 0.2214(2) -0.12204(11) 0.42628(9) 0.0153(3) Uani 1 1 d . . . . .
C1 C 0.2568(2) 0.02039(11) 0.46205(9) 0.0150(2) Uani 1 1 d . . . . .
C8 C 0.2047(2) -0.19062(11) 0.36753(9) 0.0165(3) Uani 1 1 d . . . . .
C2 C 0.2830(2) 0.11921(12) 0.46453(10) 0.0192(3) Uani 1 1 d . . . . .
H2 H 0.306980 0.163908 0.415746 0.023 Uiso 1 1 calc R . . . .
N3 N 0.25694(18) -0.04465(10) 0.13881(8) 0.0179(2) Uani 1 1 d . . . . .
N4 N 0.18547(19) -0.15813(11) 0.06811(9) 0.0203(3) Uani 1 1 d . . . . .
C12 C 0.2015(2) -0.19749(12) 0.22636(10) 0.0177(3) Uani 1 1 d . . . . .
C21 C 0.3675(2) -0.27737(11) 0.60744(10) 0.0178(3) Uani 1 1 d . . . . .
C6 C 0.2225(2) -0.04557(11) 0.53426(9) 0.0153(3) Uani 1 1 d . . . . .
C19 C 0.2581(2) -0.00348(12) 0.05591(9) 0.0187(3) Uani 1 1 d . . . . .
C20 C 0.1822(2) -0.22624(12) 0.57275(10) 0.0184(3) Uani 1 1 d . . . . .
H20A H 0.127225 -0.274542 0.546970 0.022 Uiso 1 1 calc R . . . .
H20B H 0.099278 -0.205672 0.618059 0.022 Uiso 1 1 calc R . . . .
C5 C 0.2117(2) -0.01572(12) 0.61181(9) 0.0189(3) Uani 1 1 d . . . . .
H5 H 0.188389 -0.060384 0.660729 0.023 Uiso 1 1 calc R . . . .
C11 C 0.1739(2) -0.29752(13) 0.24273(11) 0.0243(3) Uani 1 1 d . . . . .
H11 H 0.165544 -0.333804 0.198892 0.029 Uiso 1 1 calc R . . . .
C4 C 0.2368(2) 0.08242(13) 0.61348(10) 0.0196(3) Uani 1 1 d . . . . .
H4 H 0.229773 0.105701 0.665015 0.023 Uiso 1 1 calc R . . . .
C13 C 0.2149(2) -0.13643(12) 0.14408(10) 0.0180(3) Uani 1 1 d . . . . .
C3 C 0.2723(2) 0.14900(12) 0.54123(10) 0.0205(3) Uani 1 1 d . . . . .
H3 H 0.289312 0.215660 0.545289 0.025 Uiso 1 1 calc R . . . .
C26 C 0.4946(2) -0.33435(12) 0.56104(10) 0.0215(3) Uani 1 1 d . . . . .
H26 H 0.462008 -0.344805 0.508319 0.026 Uiso 1 1 calc R . . . .
C22 C 0.4167(3) -0.26461(13) 0.68547(10) 0.0246(3) Uani 1 1 d . . . . .
H22 H 0.329957 -0.228407 0.718683 0.029 Uiso 1 1 calc R . . . .
C9 C 0.1733(2) -0.29002(12) 0.38740(11) 0.0225(3) Uani 1 1 d . . . . .
H9 H 0.161993 -0.320692 0.443390 0.027 Uiso 1 1 calc R . . . .
C14 C 0.2139(2) -0.07440(13) 0.01090(10) 0.0204(3) Uani 1 1 d . . . . .
C15 C 0.2008(2) -0.05498(15) -0.07525(11) 0.0262(3) Uani 1 1 d . . . . .
H15 H 0.170719 -0.103388 -0.105494 0.031 Uiso 1 1 calc R . . . .
C18 C 0.2931(2) 0.09093(13) 0.01638(10) 0.0228(3) Uani 1 1 d . . . . .
H18 H 0.324823 0.139149 0.046399 0.027 Uiso 1 1 calc R . . . .
C16 C 0.2343(2) 0.03875(16) -0.11351(11) 0.0282(4) Uani 1 1 d . . . . .
H16 H 0.226722 0.055402 -0.171919 0.034 Uiso 1 1 calc R . . . .
C28 C 0.3162(3) -0.30838(13) 0.00774(10) 0.0234(3) Uani 1 1 d . . . . .
C17 C 0.2793(2) 0.11061(15) -0.06879(11) 0.0267(3) Uani 1 1 d . . . . .
H17 H 0.300697 0.174281 -0.097851 0.032 Uiso 1 1 calc R . . . .
C25 C 0.6683(3) -0.37583(13) 0.59136(12) 0.0274(3) Uani 1 1 d . . . . .
H25 H 0.753362 -0.415137 0.559624 0.033 Uiso 1 1 calc R . . . .
C24 C 0.7179(3) -0.36001(14) 0.66794(13) 0.0300(4) Uani 1 1 d . . . . .
H24 H 0.837787 -0.387051 0.688064 0.036 Uiso 1 1 calc R . . . .
C29 C 0.4848(3) -0.32060(14) 0.04544(11) 0.0272(3) Uani 1 1 d . . . . .
H29 H 0.492482 -0.294220 0.094861 0.033 Uiso 1 1 calc R . . . .
C27 C 0.1451(3) -0.24959(14) 0.04122(11) 0.0252(3) Uani 1 1 d . . . . .
H27A H 0.050820 -0.230092 -0.002093 0.030 Uiso 1 1 calc R . . . .
H27B H 0.095397 -0.292920 0.088497 0.030 Uiso 1 1 calc R . . . .
C23 C 0.5923(3) -0.30471(14) 0.71487(11) 0.0287(4) Uani 1 1 d . . . . .
H23 H 0.625950 -0.294058 0.767368 0.034 Uiso 1 1 calc R . . . .
C33 C 0.3057(3) -0.34981(15) -0.06358(11) 0.0324(4) Uani 1 1 d . . . . .
H33 H 0.191013 -0.342674 -0.089602 0.039 Uiso 1 1 calc R . . . .
C30 C 0.6422(3) -0.37099(15) 0.01161(14) 0.0352(4) Uani 1 1 d . . . . .
H30 H 0.757322 -0.378123 0.037206 0.042 Uiso 1 1 calc R . . . .
C10 C 0.1589(3) -0.34329(13) 0.32401(12) 0.0255(3) Uani 1 1 d . . . . .
H10 H 0.138695 -0.411405 0.336370 0.031 Uiso 1 1 calc R . . . .
C32 C 0.4624(4) -0.40136(16) -0.09645(13) 0.0416(5) Uani 1 1 d . . . . .
H32 H 0.454337 -0.430336 -0.144544 0.050 Uiso 1 1 calc R . . . .
C31 C 0.6299(4) -0.41094(16) -0.05999(14) 0.0409(5) Uani 1 1 d . . . . .
H31 H 0.737171 -0.444873 -0.083794 0.049 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
Sn1 Cl1 2.4667(4) . ?
Sn1 N2 2.3750(13) . ?
Sn1 N1 2.3424(13) . ?
Sn1 N3 2.3335(13) . ?
Sn2 Cl4 2.4885(5) . ?
Sn2 Cl3 2.4709(5) . ?
Sn2 Cl2 2.4994(5) . ?
N2 C8 1.3496(19) . ?
N2 C12 1.3526(19) . ?
N6 C7 1.3674(19) . ?
N6 C6 1.3856(19) . ?
N6 C20 1.4840(19) . ?
N1 C7 1.3309(19) . ?
N1 C1 1.3823(19) . ?
C7 C8 1.475(2) . ?
C1 C2 1.398(2) . ?
C1 C6 1.403(2) . ?
C8 C9 1.392(2) . ?
C2 C3 1.384(2) . ?
N3 C19 1.382(2) . ?
N3 C13 1.325(2) . ?
N4 C13 1.366(2) . ?
N4 C14 1.388(2) . ?
N4 C27 1.469(2) . ?
C12 C11 1.389(2) . ?
C12 C13 1.470(2) . ?
C21 C20 1.514(2) . ?
C21 C26 1.396(2) . ?
C21 C22 1.395(2) . ?
C6 C5 1.397(2) . ?
C19 C14 1.400(2) . ?
C19 C18 1.397(2) . ?
C5 C4 1.384(2) . ?
C11 C10 1.383(3) . ?
C4 C3 1.410(2) . ?
C26 C25 1.388(2) . ?
C22 C23 1.393(3) . ?
C9 C10 1.384(2) . ?
C14 C15 1.400(2) . ?
C15 C16 1.380(3) . ?
C18 C17 1.385(2) . ?
C16 C17 1.409(3) . ?
C28 C29 1.390(3) . ?
C28 C27 1.510(2) . ?
C28 C33 1.395(2) . ?
C25 C24 1.388(3) . ?
C24 C23 1.384(3) . ?
C29 C30 1.389(3) . ?
C33 C32 1.385(3) . ?
C30 C31 1.391(3) . ?
C32 C31 1.377(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Sn1 Cl1 102.62(3) . . ?
N1 Sn1 Cl1 88.16(3) . . ?
N1 Sn1 N2 67.25(4) . . ?
N3 Sn1 Cl1 83.95(3) . . ?
N3 Sn1 N2 67.94(5) . . ?
N3 Sn1 N1 131.37(5) . . ?
Cl4 Sn2 Cl2 93.169(18) . . ?
Cl3 Sn2 Cl4 94.549(17) . . ?
Cl3 Sn2 Cl2 94.289(17) . . ?
C8 N2 Sn1 119.49(10) . . ?
C8 N2 C12 119.95(13) . . ?
C12 N2 Sn1 118.78(10) . . ?
C7 N6 C6 106.49(12) . . ?
C7 N6 C20 132.35(13) . . ?
C6 N6 C20 120.82(13) . . ?
C7 N1 Sn1 118.62(10) . . ?
C7 N1 C1 106.75(12) . . ?
C1 N1 Sn1 132.93(10) . . ?
N6 C7 C8 130.28(13) . . ?
N1 C7 N6 111.78(13) . . ?
N1 C7 C8 117.86(13) . . ?
N1 C1 C2 130.39(14) . . ?
N1 C1 C6 108.24(13) . . ?
C2 C1 C6 121.34(14) . . ?
N2 C8 C7 112.40(13) . . ?
N2 C8 C9 121.18(14) . . ?
C9 C8 C7 126.41(14) . . ?
C3 C2 C1 117.00(14) . . ?
C19 N3 Sn1 133.59(11) . . ?
C13 N3 Sn1 118.78(10) . . ?
C13 N3 C19 106.94(13) . . ?
C13 N4 C14 106.59(13) . . ?
C13 N4 C27 132.44(15) . . ?
C14 N4 C27 120.83(14) . . ?
N2 C12 C11 121.22(15) . . ?
N2 C12 C13 112.79(13) . . ?
C11 C12 C13 125.99(15) . . ?
C26 C21 C20 120.93(14) . . ?
C22 C21 C20 120.12(15) . . ?
C22 C21 C26 118.90(15) . . ?
N6 C6 C1 106.72(13) . . ?
N6 C6 C5 131.46(14) . . ?
C5 C6 C1 121.80(14) . . ?
N3 C19 C14 108.25(14) . . ?
N3 C19 C18 130.59(15) . . ?
C18 C19 C14 121.16(15) . . ?
N6 C20 C21 110.53(12) . . ?
C4 C5 C6 116.37(14) . . ?
C10 C11 C12 118.77(16) . . ?
C5 C4 C3 122.18(15) . . ?
N3 C13 N4 111.68(14) . . ?
N3 C13 C12 118.52(14) . . ?
N4 C13 C12 129.77(15) . . ?
C2 C3 C4 121.32(15) . . ?
C25 C26 C21 120.51(16) . . ?
C23 C22 C21 120.30(17) . . ?
C10 C9 C8 118.73(16) . . ?
N4 C14 C19 106.53(14) . . ?
N4 C14 C15 131.06(16) . . ?
C19 C14 C15 122.39(17) . . ?
C16 C15 C14 115.91(17) . . ?
C17 C18 C19 116.59(16) . . ?
C15 C16 C17 122.15(16) . . ?
C29 C28 C27 121.51(15) . . ?
C29 C28 C33 119.14(18) . . ?
C33 C28 C27 119.34(17) . . ?
C18 C17 C16 121.79(18) . . ?
C26 C25 C24 120.16(18) . . ?
C23 C24 C25 119.78(17) . . ?
C30 C29 C28 120.67(18) . . ?
N4 C27 C28 110.74(14) . . ?
C24 C23 C22 120.30(17) . . ?
C32 C33 C28 120.0(2) . . ?
C29 C30 C31 119.5(2) . . ?
C11 C10 C9 120.10(15) . . ?
C31 C32 C33 120.54(19) . . ?
C32 C31 C30 120.1(2) . . ?

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

data_as890_test
_database_code_depnum_ccdc_archive 'CCDC 1895466'
loop_
_audit_author_name
_audit_author_address
"Ala'aeddeen Swidan"
;University of Windsor
Canada
;
_audit_update_record             
;
2019-02-04 deposited with the CCDC.	2019-05-03 downloaded from the CCDC.
;
_audit_creation_date             2018-10-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C37 H21 Cl F12 Ge N5, Cl3 Ge'
_chemical_formula_sum            'C37 H21 Cl4 F12 Ge2 N5'
_chemical_formula_weight         1050.57
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   8.9182(8)
_cell_length_b                   14.4073(13)
_cell_length_c                   16.3208(14)
_cell_angle_alpha                73.936(3)
_cell_angle_beta                 80.147(3)
_cell_angle_gamma                75.525(3)
_cell_volume                     1939.4(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9231
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      29.183
_cell_measurement_theta_min      3.071
_shelx_estimated_absorpt_T_max   0.831
_shelx_estimated_absorpt_T_min   0.465
_exptl_absorpt_coefficient_mu    1.921
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5486
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0892 before and 0.0651 after correction. The Ratio of minimum to maximum transmission is 0.7356. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.799
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            88406
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.225
_diffrn_reflns_theta_min         2.832
_diffrn_ambient_temperature      170.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX3 Photon 100'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9187
_reflns_number_total             10430
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       APEX3
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.673
_refine_diff_density_min         -1.170
_refine_diff_density_rms         0.152
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         10430
_refine_ls_number_restraints     72
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0632
_refine_ls_restrained_S_all      1.102
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0657P)²+14.8977P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1738
_refine_ls_wR_factor_ref         0.1787
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 F4'-F6' \\sim F4'-F5' \\sim F6'-F5' \\sim F5-F4 \\sim F5-F6 \\sim F4-F6
 with sigma of 0.04
 C35-C25 \\sim C35-F4' \\sim C35-F6' \\sim C35-F5' \\sim C35-F5 \\sim C35-F4
\\sim C35-F6
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C35, F4', F6', F5'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C35, F5, F4, F6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(F5)=Sof(F4)=Sof(F6)=1-FVAR(1)
 Sof(F4')=Sof(F6')=Sof(F5')=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C20(H20A,H20B)
5.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C17(H17), C9(H9), C18(H18), C2(H2), C11(H11), C5(H5), C15(H15),
 C4(H4), C16(H16), C26(H26), C29(H29), C22(H22), C3(H3), C31(H31), C33(H33),
 C24(H24)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.46861(5) 0.58943(3) 0.74628(3) 0.01748(11) Uani 1 1 d . . . . .
Ge2 Ge 0.16833(6) 0.44130(4) 0.76555(3) 0.02621(13) Uani 1 1 d . . . . .
Cl1 Cl 0.26348(12) 0.71983(9) 0.73471(8) 0.0262(2) Uani 1 1 d . . . . .
Cl2 Cl 0.06089(15) 0.49425(9) 0.88542(8) 0.0288(2) Uani 1 1 d . . . . .
Cl3 Cl -0.05772(16) 0.45818(10) 0.70740(9) 0.0349(3) Uani 1 1 d . . . . .
Cl4 Cl 0.1918(2) 0.27797(10) 0.82621(10) 0.0454(4) Uani 1 1 d . . . . .
F10 F 0.5183(4) 1.1325(2) 0.4131(2) 0.0398(8) Uani 1 1 d . . . . .
F2 F 0.6118(5) 1.1605(2) 0.8179(3) 0.0483(9) Uani 1 1 d . . . . .
F12 F 0.3810(4) 1.0305(3) 0.4133(3) 0.0517(11) Uani 1 1 d . . . . .
N2 N 0.6587(4) 0.6638(2) 0.6996(2) 0.0147(6) Uani 1 1 d . . . . .
F11 F 0.4820(5) 1.1115(3) 0.2935(3) 0.0495(10) Uani 1 1 d . . . . .
N3 N 0.4939(4) 0.6283(3) 0.5984(2) 0.0172(6) Uani 1 1 d . . . . .
F8 F 1.1992(4) 0.9008(3) 0.3340(3) 0.0473(9) Uani 1 1 d . . . . .
F3 F 0.4989(5) 1.0603(3) 0.7913(3) 0.0574(12) Uani 1 1 d . . . . .
N5 N 0.6373(4) 0.6762(3) 0.4736(2) 0.0169(6) Uani 1 1 d . . . . .
N1 N 0.5156(4) 0.6360(3) 0.8530(2) 0.0184(7) Uani 1 1 d . . . . .
N4 N 0.6736(4) 0.6856(3) 0.9162(2) 0.0184(7) Uani 1 1 d . . . . .
F9 F 1.0896(5) 1.0479(3) 0.3385(4) 0.0701(15) Uani 1 1 d . . . . .
F1 F 0.4754(5) 1.0782(4) 0.9180(3) 0.0732(16) Uani 1 1 d . . . . .
F7 F 1.1220(5) 0.9334(4) 0.4547(3) 0.0626(13) Uani 1 1 d . . . . .
C19 C 0.4200(5) 0.6216(3) 0.5322(3) 0.0176(7) Uani 1 1 d . . . . .
C14 C 0.5076(5) 0.6522(3) 0.4544(3) 0.0164(7) Uani 1 1 d . . . . .
C8 C 0.7327(5) 0.6818(3) 0.7574(3) 0.0160(7) Uani 1 1 d . . . . .
C13 C 0.6214(5) 0.6598(3) 0.5614(3) 0.0160(7) Uani 1 1 d . . . . .
C12 C 0.7194(5) 0.6777(3) 0.6168(3) 0.0163(7) Uani 1 1 d . . . . .
C10 C 0.9350(5) 0.7277(3) 0.6487(3) 0.0220(8) Uani 1 1 d . . . . .
H10 H 1.029497 0.750315 0.630690 0.026 Uiso 1 1 calc R . . . .
C17 C 0.2375(5) 0.5924(4) 0.4568(3) 0.0239(9) Uani 1 1 d . . . . .
H17 H 0.145558 0.570695 0.456360 0.029 Uiso 1 1 calc R . . . .
C1 C 0.4513(5) 0.6340(3) 0.9362(3) 0.0201(8) Uani 1 1 d . . . . .
C9 C 0.8714(5) 0.7154(3) 0.7338(3) 0.0210(8) Uani 1 1 d . . . . .
H9 H 0.920932 0.729353 0.774706 0.025 Uiso 1 1 calc R . . . .
C7 C 0.6477(5) 0.6665(3) 0.8430(3) 0.0165(7) Uani 1 1 d . . . . .
C18 C 0.2823(5) 0.5906(3) 0.5351(3) 0.0212(8) Uani 1 1 d . . . . .
H18 H 0.222177 0.569175 0.587862 0.025 Uiso 1 1 calc R . . . .
C6 C 0.5493(5) 0.6658(3) 0.9769(3) 0.0197(8) Uani 1 1 d . . . . .
C27 C 0.7638(5) 0.7050(3) 0.4094(3) 0.0191(8) Uani 1 1 d . . . . .
H27A H 0.749272 0.693903 0.354311 0.023 Uiso 1 1 calc R . . . .
H27B H 0.863664 0.661670 0.427463 0.023 Uiso 1 1 calc R . . . .
C2 C 0.3129(6) 0.6074(4) 0.9807(3) 0.0276(10) Uani 1 1 d . . . . .
H2 H 0.247092 0.583885 0.954709 0.033 Uiso 1 1 calc R . . . .
C28 C 0.7742(5) 0.8114(3) 0.3952(3) 0.0177(7) Uani 1 1 d . . . . .
C11 C 0.8605(5) 0.7071(3) 0.5901(3) 0.0209(8) Uani 1 1 d . . . . .
H11 H 0.905442 0.713012 0.532277 0.025 Uiso 1 1 calc R . . . .
C5 C 0.5131(6) 0.6758(4) 1.0607(3) 0.0264(9) Uani 1 1 d . . . . .
H5 H 0.578888 0.698579 1.087285 0.032 Uiso 1 1 calc R . . . .
C15 C 0.4610(5) 0.6562(3) 0.3759(3) 0.0228(8) Uani 1 1 d . . . . .
H15 H 0.520086 0.678739 0.323072 0.027 Uiso 1 1 calc R . . . .
C20 C 0.8140(5) 0.7079(3) 0.9365(3) 0.0197(8) Uani 1 1 d . . . . .
H20A H 0.906945 0.669127 0.909002 0.024 Uiso 1 1 calc R . . . .
H20B H 0.818094 0.684987 0.999289 0.024 Uiso 1 1 calc R . . . .
C4 C 0.3747(6) 0.6505(4) 1.1033(3) 0.0305(10) Uani 1 1 d . . . . .
H4 H 0.345089 0.656030 1.160783 0.037 Uiso 1 1 calc R . . . .
C16 C 0.3245(6) 0.6255(4) 0.3790(3) 0.0261(9) Uani 1 1 d . . . . .
H16 H 0.288940 0.626999 0.326865 0.031 Uiso 1 1 calc R . . . .
C30 C 0.9286(5) 0.9324(3) 0.3750(3) 0.0222(8) Uani 1 1 d . . . . .
C21 C 0.8245(5) 0.8153(3) 0.9088(3) 0.0190(8) Uani 1 1 d . . . . .
C26 C 0.9691(5) 0.8357(4) 0.9075(3) 0.0248(9) Uani 1 1 d . . . . .
H26 H 1.056653 0.782960 0.920385 0.030 Uiso 1 1 calc R . . . .
C29 C 0.9182(5) 0.8350(3) 0.3852(3) 0.0200(8) Uani 1 1 d . . . . .
H29 H 1.010272 0.784621 0.385343 0.024 Uiso 1 1 calc R . . . .
C22 C 0.6965(5) 0.8926(3) 0.8891(3) 0.0203(8) Uani 1 1 d . . . . .
H22 H 0.597226 0.879224 0.889605 0.024 Uiso 1 1 calc R . . . .
C3 C 0.2775(6) 0.6171(4) 1.0642(3) 0.0308(10) Uani 1 1 d . . . . .
H3 H 0.184156 0.600563 1.095982 0.037 Uiso 1 1 calc R . . . .
C32 C 0.6527(5) 0.9831(3) 0.3786(3) 0.0222(8) Uani 1 1 d . . . . .
C31 C 0.7956(5) 1.0075(3) 0.3716(3) 0.0236(9) Uani 1 1 d . . . . .
H31 H 0.802556 1.074007 0.364628 0.028 Uiso 1 1 calc R . . . .
C25 C 0.9865(6) 0.9331(4) 0.8874(3) 0.0276(10) Uani 1 1 d D . . . .
C33 C 0.6399(5) 0.8861(3) 0.3903(3) 0.0187(8) Uani 1 1 d . . . . .
H33 H 0.540697 0.870870 0.394911 0.022 Uiso 1 1 calc R . . . .
C34 C 0.5747(6) 1.0723(4) 0.8492(3) 0.0283(10) Uani 1 1 d . . . . .
C24 C 0.8588(6) 1.0109(4) 0.8680(3) 0.0277(10) Uani 1 1 d . . . . .
H24 H 0.870111 1.077490 0.854456 0.033 Uiso 1 1 calc R . . . .
C37 C 0.5080(6) 1.0640(4) 0.3739(4) 0.0298(10) Uani 1 1 d . . . . .
C36 C 1.0841(6) 0.9539(4) 0.3762(4) 0.0318(11) Uani 1 1 d . . . . .
C23 C 0.7154(5) 0.9901(3) 0.8685(3) 0.0234(9) Uani 1 1 d . . . . .
C35 C 1.1398(6) 0.9536(4) 0.8870(4) 0.0388(12) Uani 1 1 d D U . . .
F4' F 1.2565(12) 0.8879(9) 0.8581(12) 0.085(5) Uani 0.500(17) 1 d D U P A 1
F6' F 1.1726(15) 0.9628(17) 0.9560(7) 0.102(8) Uani 0.500(17) 1 d D U P A 1
F5' F 1.1661(12) 1.0368(8) 0.8251(8) 0.074(5) Uani 0.500(17) 1 d D U P A 1
F5 F 1.2370(17) 0.9436(17) 0.8228(8) 0.104(8) Uani 0.500(17) 1 d D U P A 2
F4 F 1.2113(14) 0.8908(8) 0.9558(8) 0.078(4) Uani 0.500(17) 1 d D U P A 2
F6 F 1.1317(11) 1.0388(7) 0.9068(10) 0.074(5) Uani 0.500(17) 1 d D U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 Cl1 2.2618(12) . ?
Ge1 N2 2.149(3) . ?
Ge1 N3 2.307(4) . ?
Ge1 N1 2.168(4) . ?
Ge2 Cl2 2.2685(13) . ?
Ge2 Cl3 2.3034(13) . ?
Ge2 Cl4 2.2576(16) . ?
F10 C37 1.343(6) . ?
F2 C34 1.334(6) . ?
F12 C37 1.335(6) . ?
N2 C8 1.352(5) . ?
N2 C12 1.347(5) . ?
F11 C37 1.330(7) . ?
N3 C19 1.393(5) . ?
N3 C13 1.317(5) . ?
F8 C36 1.330(6) . ?
F3 C34 1.322(7) . ?
N5 C14 1.394(5) . ?
N5 C13 1.374(5) . ?
N5 C27 1.460(5) . ?
N1 C1 1.376(6) . ?
N1 C7 1.328(5) . ?
N4 C7 1.365(5) . ?
N4 C6 1.385(6) . ?
N4 C20 1.478(5) . ?
F9 C36 1.332(6) . ?
F1 C34 1.314(6) . ?
F7 C36 1.317(7) . ?
C19 C14 1.393(6) . ?
C19 C18 1.398(6) . ?
C14 C15 1.394(6) . ?
C8 C9 1.394(6) . ?
C8 C7 1.457(6) . ?
C13 C12 1.469(5) . ?
C12 C11 1.389(6) . ?
C10 H10 0.9500 . ?
C10 C9 1.387(6) . ?
C10 C11 1.384(6) . ?
C17 H17 0.9500 . ?
C17 C18 1.393(6) . ?
C17 C16 1.398(7) . ?
C1 C6 1.408(6) . ?
C1 C2 1.405(6) . ?
C9 H9 0.9500 . ?
C18 H18 0.9500 . ?
C6 C5 1.389(6) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.510(6) . ?
C2 H2 0.9500 . ?
C2 C3 1.383(7) . ?
C28 C29 1.381(6) . ?
C28 C33 1.393(6) . ?
C11 H11 0.9500 . ?
C5 H5 0.9500 . ?
C5 C4 1.389(7) . ?
C15 H15 0.9500 . ?
C15 C16 1.385(7) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.509(6) . ?
C4 H4 0.9500 . ?
C4 C3 1.399(8) . ?
C16 H16 0.9500 . ?
C30 C29 1.391(6) . ?
C30 C31 1.389(6) . ?
C30 C36 1.499(6) . ?
C21 C26 1.388(6) . ?
C21 C22 1.393(6) . ?
C26 H26 0.9500 . ?
C26 C25 1.391(7) . ?
C29 H29 0.9500 . ?
C22 H22 0.9500 . ?
C22 C23 1.396(6) . ?
C3 H3 0.9500 . ?
C32 C31 1.383(6) . ?
C32 C33 1.388(6) . ?
C32 C37 1.505(6) . ?
C31 H31 0.9500 . ?
C25 C24 1.394(7) . ?
C25 C35 1.468(6) . ?
C33 H33 0.9500 . ?
C34 C23 1.505(6) . ?
C24 H24 0.9500 . ?
C24 C23 1.382(7) . ?
C35 F4' 1.337(10) . ?
C35 F6' 1.259(9) . ?
C35 F5' 1.380(9) . ?
C35 F5 1.257(10) . ?
C35 F4 1.371(9) . ?
C35 F6 1.336(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
Cl1 Ge1 N3 85.51(9) . . ?
N2 Ge1 Cl1 100.74(9) . . ?
N2 Ge1 N3 71.73(13) . . ?
N2 Ge1 N1 73.47(13) . . ?
N1 Ge1 Cl1 85.73(10) . . ?
N1 Ge1 N3 141.72(13) . . ?
Cl2 Ge2 Cl3 98.48(5) . . ?
Cl4 Ge2 Cl2 96.87(6) . . ?
Cl4 Ge2 Cl3 94.70(6) . . ?
C8 N2 Ge1 118.3(3) . . ?
C12 N2 Ge1 120.9(3) . . ?
C12 N2 C8 119.9(4) . . ?
C19 N3 Ge1 139.3(3) . . ?
C13 N3 Ge1 114.5(3) . . ?
C13 N3 C19 106.0(3) . . ?
C14 N5 C27 123.5(3) . . ?
C13 N5 C14 105.6(3) . . ?
C13 N5 C27 130.7(4) . . ?
C1 N1 Ge1 136.7(3) . . ?
C7 N1 Ge1 116.2(3) . . ?
C7 N1 C1 106.7(4) . . ?
C7 N4 C6 106.9(3) . . ?
C7 N4 C20 129.3(4) . . ?
C6 N4 C20 123.1(4) . . ?
N3 C19 C14 108.8(4) . . ?
N3 C19 C18 130.2(4) . . ?
C14 C19 C18 121.0(4) . . ?
N5 C14 C15 131.1(4) . . ?
C19 C14 N5 106.7(4) . . ?
C19 C14 C15 122.2(4) . . ?
N2 C8 C9 121.7(4) . . ?
N2 C8 C7 112.4(3) . . ?
C9 C8 C7 125.8(4) . . ?
N3 C13 N5 112.9(4) . . ?
N3 C13 C12 117.6(4) . . ?
N5 C13 C12 129.4(4) . . ?
N2 C12 C13 113.3(4) . . ?
N2 C12 C11 120.9(4) . . ?
C11 C12 C13 125.8(4) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C11 C10 C9 119.9(4) . . ?
C18 C17 H17 119.2 . . ?
C18 C17 C16 121.7(4) . . ?
C16 C17 H17 119.2 . . ?
N1 C1 C6 108.7(4) . . ?
N1 C1 C2 130.7(4) . . ?
C2 C1 C6 120.6(4) . . ?
C8 C9 H9 120.9 . . ?
C10 C9 C8 118.1(4) . . ?
C10 C9 H9 120.9 . . ?
N1 C7 N4 111.7(4) . . ?
N1 C7 C8 117.2(4) . . ?
N4 C7 C8 130.8(4) . . ?
C19 C18 H18 121.6 . . ?
C17 C18 C19 116.8(4) . . ?
C17 C18 H18 121.6 . . ?
N4 C6 C1 105.9(4) . . ?
N4 C6 C5 131.4(4) . . ?
C5 C6 C1 122.6(4) . . ?
N5 C27 H27A 108.8 . . ?
N5 C27 H27B 108.8 . . ?
N5 C27 C28 113.9(3) . . ?
H27A C27 H27B 107.7 . . ?
C28 C27 H27A 108.8 . . ?
C28 C27 H27B 108.8 . . ?
C1 C2 H2 121.7 . . ?
C3 C2 C1 116.5(5) . . ?
C3 C2 H2 121.7 . . ?
C29 C28 C27 119.7(4) . . ?
C29 C28 C33 119.8(4) . . ?
C33 C28 C27 120.5(4) . . ?
C12 C11 H11 120.3 . . ?
C10 C11 C12 119.3(4) . . ?
C10 C11 H11 120.3 . . ?
C6 C5 H5 122.0 . . ?
C4 C5 C6 115.9(4) . . ?
C4 C5 H5 122.0 . . ?
C14 C15 H15 121.7 . . ?
C16 C15 C14 116.7(4) . . ?
C16 C15 H15 121.7 . . ?
N4 C20 H20A 108.4 . . ?
N4 C20 H20B 108.4 . . ?
N4 C20 C21 115.6(3) . . ?
H20A C20 H20B 107.4 . . ?
C21 C20 H20A 108.4 . . ?
C21 C20 H20B 108.4 . . ?
C5 C4 H4 119.0 . . ?
C5 C4 C3 122.1(5) . . ?
C3 C4 H4 119.0 . . ?
C17 C16 H16 119.2 . . ?
C15 C16 C17 121.6(4) . . ?
C15 C16 H16 119.2 . . ?
C29 C30 C36 118.9(4) . . ?
C31 C30 C29 120.8(4) . . ?
C31 C30 C36 120.1(4) . . ?
C26 C21 C20 116.8(4) . . ?
C26 C21 C22 119.9(4) . . ?
C22 C21 C20 123.3(4) . . ?
C21 C26 H26 119.8 . . ?
C21 C26 C25 120.3(4) . . ?
C25 C26 H26 119.8 . . ?
C28 C29 C30 120.1(4) . . ?
C28 C29 H29 120.0 . . ?
C30 C29 H29 120.0 . . ?
C21 C22 H22 120.3 . . ?
C21 C22 C23 119.3(4) . . ?
C23 C22 H22 120.3 . . ?
C2 C3 C4 122.2(5) . . ?
C2 C3 H3 118.9 . . ?
C4 C3 H3 118.9 . . ?
C31 C32 C33 121.6(4) . . ?
C31 C32 C37 118.8(4) . . ?
C33 C32 C37 119.5(4) . . ?
C30 C31 H31 120.8 . . ?
C32 C31 C30 118.4(4) . . ?
C32 C31 H31 120.8 . . ?
C26 C25 C24 120.2(4) . . ?
C26 C25 C35 119.7(5) . . ?
C24 C25 C35 120.1(5) . . ?
C28 C33 H33 120.4 . . ?
C32 C33 C28 119.3(4) . . ?
C32 C33 H33 120.4 . . ?
F2 C34 C23 112.4(4) . . ?
F3 C34 F2 106.3(5) . . ?
F3 C34 C23 111.8(4) . . ?
F1 C34 F2 106.9(5) . . ?
F1 C34 F3 107.2(5) . . ?
F1 C34 C23 111.8(4) . . ?
C25 C24 H24 120.4 . . ?
C23 C24 C25 119.2(4) . . ?
C23 C24 H24 120.4 . . ?
F10 C37 C32 111.3(4) . . ?
F12 C37 F10 105.6(5) . . ?
F12 C37 C32 112.4(4) . . ?
F11 C37 F10 106.6(4) . . ?
F11 C37 F12 108.1(5) . . ?
F11 C37 C32 112.4(5) . . ?
F8 C36 F9 105.2(5) . . ?
F8 C36 C30 112.5(5) . . ?
F9 C36 C30 112.3(4) . . ?
F7 C36 F8 105.9(5) . . ?
F7 C36 F9 108.5(5) . . ?
F7 C36 C30 112.0(4) . . ?
C22 C23 C34 118.3(4) . . ?
C24 C23 C22 121.1(4) . . ?
C24 C23 C34 120.5(4) . . ?
F4' C35 C25 112.5(7) . . ?
F4' C35 F5' 97.8(9) . . ?
F6' C35 C25 117.5(6) . . ?
F6' C35 F4' 108.0(11) . . ?
F6' C35 F5' 106.1(10) . . ?
F5' C35 C25 112.9(6) . . ?
F5 C35 C25 116.9(7) . . ?
F5 C35 F4 104.9(11) . . ?
F5 C35 F6 111.6(10) . . ?
F4 C35 C25 110.1(6) . . ?
F6 C35 C25 113.3(6) . . ?
F6 C35 F4 98.2(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_as723_p-1_new
_database_code_depnum_ccdc_archive 'CCDC 1895467'
loop_
_audit_author_name
_audit_author_address
"Ala'aeddeen Swidan"
;University of Windsor
Canada
;
_audit_update_record             
;
2019-02-04 deposited with the CCDC.	2019-05-03 downloaded from the CCDC.
;

_audit_creation_date             2019-01-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C37 H21 Cl F12 N5 Sn, Cl3 Sn'
_chemical_formula_sum            'C37 H21 Cl4 F12 N5 Sn2'
_chemical_formula_weight         1142.77
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   9.1861(13)
_cell_length_b                   13.4274(18)
_cell_length_c                   17.478(2)
_cell_angle_alpha                75.357(4)
_cell_angle_beta                 80.979(4)
_cell_angle_gamma                79.243(4)
_cell_volume                     2035.5(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9550
_cell_measurement_temperature    170.2
_cell_measurement_theta_max      33.02
_cell_measurement_theta_min      3.09
_shelx_estimated_absorpt_T_max   0.644
_shelx_estimated_absorpt_T_min   0.628
_exptl_absorpt_coefficient_mu    1.581
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6508
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0843 before and 0.0651 after correction. The Ratio of minimum to maximum transmission is 0.8718. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.865
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1108
_exptl_crystal_size_max          0.325
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.305
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            99263
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.965
_diffrn_ambient_temperature      170.2
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX3 Photon 100'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8163
_reflns_number_total             9248
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       APEX3
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         2.616
_refine_diff_density_min         -2.031
_refine_diff_density_rms         0.192
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         9248
_refine_ls_number_restraints     150
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0617
_refine_ls_restrained_S_all      1.139
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0345P)²+32.9559P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1484
_refine_ls_wR_factor_ref         0.1594
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C34-F3 \\sim C34-F3A
 with sigma of 0.02
 C34-F10 \\sim C34-F10A
 with sigma of 0.02
 C34-F12 \\sim C34-F12A
 with sigma of 0.02
 F2-C0AA \\sim F2A-C0AA
 with sigma of 0.02
 C0AA-F11 \\sim C0AA-F11A
 with sigma of 0.02
 C0AA-F13 \\sim C0AA-F13A
 with sigma of 0.02
 F2-F11 \\sim F2-F13 \\sim F11-F13 \\sim F13A-F2A \\sim F13A-F11A \\sim F2A-F11A
 with sigma of 0.04
 C0AA-C30 \\sim C0AA-F2 \\sim C0AA-F11 \\sim C0AA-F13 \\sim C0AA-F13A \\sim
C0AA-F2A \\sim C0AA-F11A
 with sigma of 0.02
 F3-F10 \\sim F3-F12 \\sim F10-F12 \\sim F10A-F12A \\sim F10A-F3A \\sim F12A-F3A
 with sigma of 0.04
 C34-C23 \\sim C34-F3 \\sim C34-F10 \\sim C34-F12 \\sim C34-F10A \\sim C34-F12A
\\sim C34-F3A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F6A) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
4. Rigid body (RIGU) restrains
 C34
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C34, F3, F10, F12, F10A, F12A, F3A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 F2, C0AA, F11, F13, F13A, F2A, F11A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(F10A)=Sof(F12A)=Sof(F3A)=1-FVAR(1)
 Sof(F3)=Sof(F10)=Sof(F12)=FVAR(1)
 Sof(F13A)=Sof(F2A)=Sof(F11A)=1-FVAR(2)
 Sof(F2)=Sof(F11)=Sof(F13)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C20(H20A,H20B)
6.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C17(H17), C5(H5), C11(H11), C2(H2), C3(H3), C15(H15),
 C18(H18), C4(H4), C16(H16), C33(H33), C29(H29), C22(H22), C26(H26), C24(H24),
 C31(H31)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.41464(5) 0.06866(3) 0.75513(3) 0.02067(11) Uani 1 1 d . . . . .
Sn2 Sn 1.06231(5) -0.18733(4) 0.82027(3) 0.02933(13) Uani 1 1 d . . . . .
Cl1 Cl 0.22130(17) 0.22226(13) 0.74724(10) 0.0282(3) Uani 1 1 d . . . . .
Cl2 Cl 1.08614(19) -0.03948(13) 0.87769(11) 0.0317(3) Uani 1 1 d . . . . .
Cl3 Cl 1.3248(2) -0.20986(15) 0.76899(11) 0.0354(4) Uani 1 1 d . . . . .
Cl4 Cl 0.9804(2) -0.06701(16) 0.69623(13) 0.0417(4) Uani 1 1 d . . . . .
N4 N 0.6010(6) 0.1566(4) 0.5001(3) 0.0187(10) Uani 1 1 d . . . . .
N3 N 0.6359(5) 0.1494(4) 0.7072(3) 0.0166(9) Uani 1 1 d . . . . .
N5 N 0.4530(6) 0.1248(4) 0.6144(3) 0.0208(10) Uani 1 1 d . . . . .
N2 N 0.6751(6) 0.1699(4) 0.9077(3) 0.0207(10) Uani 1 1 d . . . . .
N1 N 0.4961(6) 0.1307(4) 0.8532(3) 0.0225(10) Uani 1 1 d . . . . .
C13 C 0.5855(6) 0.1481(4) 0.5802(4) 0.0177(11) Uani 1 1 d . . . . .
C9 C 0.8463(7) 0.2104(5) 0.7355(4) 0.0250(13) Uani 1 1 d . . . . .
H9 H 0.898965 0.225649 0.772716 0.030 Uiso 1 1 calc R . . . .
C10 C 0.9011(7) 0.2260(5) 0.6558(4) 0.0290(14) Uani 1 1 d . . . . .
H10 H 0.993197 0.251494 0.637743 0.035 Uiso 1 1 calc R . . . .
C12 C 0.6893(7) 0.1667(4) 0.6302(4) 0.0179(11) Uani 1 1 d . . . . .
C19 C 0.3778(7) 0.1172(5) 0.5539(4) 0.0221(12) Uani 1 1 d . . . . .
C27 C 0.7290(7) 0.1774(5) 0.4397(4) 0.0201(11) Uani 1 1 d . . . . .
H27A H 0.719283 0.150634 0.393266 0.024 Uiso 1 1 calc R . . . .
H27B H 0.821508 0.138830 0.462094 0.024 Uiso 1 1 calc R . . . .
C28 C 0.7435(7) 0.2916(5) 0.4119(4) 0.0210(12) Uani 1 1 d . . . . .
C1 C 0.4463(7) 0.1274(4) 0.9318(4) 0.0207(12) Uani 1 1 d . . . . .
C20 C 0.8201(7) 0.1859(5) 0.9234(4) 0.0226(12) Uani 1 1 d . . . . .
H20A H 0.899490 0.149558 0.890368 0.027 Uiso 1 1 calc R . . . .
H20B H 0.832905 0.153250 0.979889 0.027 Uiso 1 1 calc R . . . .
C8 C 0.7110(7) 0.1715(4) 0.7600(4) 0.0196(11) Uani 1 1 d . . . . .
C14 C 0.4681(7) 0.1372(5) 0.4819(4) 0.0221(12) Uani 1 1 d . . . . .
C17 C 0.1894(7) 0.0908(5) 0.4860(4) 0.0286(14) Uani 1 1 d . . . . .
H17 H 0.092894 0.074991 0.485783 0.034 Uiso 1 1 calc R . . . .
C6 C 0.5567(7) 0.1538(5) 0.9670(4) 0.0220(12) Uani 1 1 d . . . . .
C7 C 0.6328(7) 0.1562(5) 0.8402(4) 0.0206(11) Uani 1 1 d . . . . .
C5 C 0.5371(8) 0.1601(5) 1.0460(4) 0.0264(13) Uani 1 1 d . . . . .
H5 H 0.611370 0.179704 1.068990 0.032 Uiso 1 1 calc R . . . .
C11 C 0.8220(7) 0.2046(5) 0.6022(4) 0.0247(13) Uani 1 1 d . . . . .
H11 H 0.858434 0.215852 0.547226 0.030 Uiso 1 1 calc R . . . .
C2 C 0.3132(7) 0.1010(5) 0.9767(4) 0.0263(13) Uani 1 1 d . . . . .
H2 H 0.239235 0.080700 0.953969 0.032 Uiso 1 1 calc R . . . .
C3 C 0.2949(8) 0.1059(5) 1.0551(4) 0.0303(14) Uani 1 1 d . . . . .
H3 H 0.206040 0.088218 1.087401 0.036 Uiso 1 1 calc R . . . .
C15 C 0.4236(8) 0.1364(5) 0.4096(4) 0.0270(13) Uani 1 1 d . . . . .
H15 H 0.486053 0.151559 0.360752 0.032 Uiso 1 1 calc R . . . .
C21 C 0.8409(7) 0.2993(5) 0.9065(4) 0.0219(12) Uani 1 1 d . . . . .
C18 C 0.2349(8) 0.0924(5) 0.5573(4) 0.0273(13) Uani 1 1 d . . . . .
H18 H 0.172431 0.077462 0.606197 0.033 Uiso 1 1 calc R . . . .
C4 C 0.4039(8) 0.1365(6) 1.0894(4) 0.0316(15) Uani 1 1 d . . . . .
H4 H 0.385062 0.140831 1.143519 0.038 Uiso 1 1 calc R . . . .
C16 C 0.2826(8) 0.1120(6) 0.4136(4) 0.0317(15) Uani 1 1 d . . . . .
H16 H 0.247295 0.109426 0.366002 0.038 Uiso 1 1 calc R . . . .
C33 C 0.6189(7) 0.3682(5) 0.4022(4) 0.0286(14) Uani 1 1 d . . . . .
H33 H 0.521935 0.349179 0.412861 0.034 Uiso 1 1 calc R . . . .
C29 C 0.8846(7) 0.3201(5) 0.3955(4) 0.0241(13) Uani 1 1 d . . . . .
H29 H 0.970058 0.267788 0.400951 0.029 Uiso 1 1 calc R . . . .
C22 C 0.9819(8) 0.3210(5) 0.9083(4) 0.0289(14) Uani 1 1 d . . . . .
H22 H 1.061798 0.265254 0.919064 0.035 Uiso 1 1 calc R . . . .
C23 C 1.0083(8) 0.4230(6) 0.8945(5) 0.0364(17) Uani 1 1 d D . . . .
C26 C 0.7241(8) 0.3805(5) 0.8903(4) 0.0290(14) Uani 1 1 d . . . . .
H26 H 0.627240 0.365970 0.889129 0.035 Uiso 1 1 calc R . . . .
C32 C 0.6356(9) 0.4721(5) 0.3771(5) 0.0376(17) Uani 1 1 d . . . . .
C30 C 0.9024(8) 0.4269(6) 0.3704(5) 0.0368(17) Uani 1 1 d D . . . .
C24 C 0.8877(9) 0.5049(6) 0.8778(5) 0.0396(18) Uani 1 1 d . . . . .
H24 H 0.903438 0.575145 0.868071 0.048 Uiso 1 1 calc R . . . .
C25 C 0.7485(9) 0.4835(5) 0.8757(6) 0.0375(18) Uani 1 1 d . . . . .
C31 C 0.7751(9) 0.5018(6) 0.3620(6) 0.0404(19) Uani 1 1 d . . . . .
H31 H 0.784436 0.573650 0.345749 0.048 Uiso 1 1 calc R . . . .
C34 C 1.1536(8) 0.4467(6) 0.8949(5) 0.0518(17) Uani 1 1 d D U . . .
C35 C 0.6210(12) 0.5699(7) 0.8574(8) 0.061(3) Uani 1 1 d . . . . .
F1 F 0.6640(7) 0.6603(4) 0.8261(5) 0.082(2) Uani 1 1 d . . . . .
F2 F 1.059(3) 0.5520(11) 0.3225(19) 0.090(7) Uani 0.54(4) 1 d D U P A 1
F3 F 1.154(2) 0.5176(12) 0.9351(10) 0.076(5) Uani 0.63(2) 1 d D U P B 1
F5 F 0.5424(10) 0.5536(6) 0.8071(8) 0.132(5) Uani 1 1 d . . . . .
C0AA C 1.0490(9) 0.4541(6) 0.3597(5) 0.0591(19) Uani 1 1 d D U . . .
F8 F 0.5317(11) 0.5806(7) 0.9206(7) 0.145(5) Uani 1 1 d . . . . .
F10 F 1.2085(14) 0.4976(16) 0.8202(6) 0.092(5) Uani 0.63(2) 1 d D U P B 1
F11 F 1.116(2) 0.427(3) 0.4265(9) 0.093(6) Uani 0.54(4) 1 d D U P A 1
F12 F 1.2597(13) 0.3688(8) 0.9126(17) 0.119(7) Uani 0.63(2) 1 d D U P B 1
F13 F 1.144(2) 0.3973(15) 0.3125(14) 0.071(4) Uani 0.54(4) 1 d D U P A 1
C1AA C 0.5010(10) 0.5550(7) 0.3674(8) 0.064(3) Uani 1 1 d . . . . .
F10A F 1.2630(19) 0.419(2) 0.8429(15) 0.085(6) Uani 0.37(2) 1 d D U P B 2
F12A F 1.208(2) 0.3841(15) 0.9649(11) 0.065(5) Uani 0.37(2) 1 d D U P B 2
F3A F 1.166(4) 0.5381(13) 0.9062(17) 0.066(6) Uani 0.37(2) 1 d D U P B 2
F13A F 1.164(2) 0.3833(14) 0.348(2) 0.081(7) Uani 0.46(4) 1 d D U P A 2
F2A F 1.064(4) 0.5401(13) 0.2994(12) 0.059(5) Uani 0.46(4) 1 d D U P A 2
F11A F 1.072(3) 0.490(3) 0.4227(11) 0.091(7) Uani 0.46(4) 1 d D U P A 2
F15A F 0.4941(9) 0.6084(6) 0.2944(5) 0.093(3) Uani 1 1 d . . . C 2
F6A F 0.3785(8) 0.5207(6) 0.4012(6) 0.107(3) Uani 1 1 d . U . D 2
F4A F 0.5096(8) 0.6280(5) 0.4084(5) 0.087(2) Uani 1 1 d . . . E 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 Cl1 2.4480(16) . ?
Sn1 N3 2.416(5) . ?
Sn1 N5 2.373(5) . ?
Sn1 N1 2.356(5) . ?
Sn2 Cl2 2.4969(17) . ?
Sn2 Cl3 2.4279(18) . ?
Sn2 Cl4 2.483(2) . ?
N4 C13 1.364(8) . ?
N4 C27 1.469(7) . ?
N4 C14 1.394(8) . ?
N3 C12 1.335(8) . ?
N3 C8 1.352(7) . ?
N5 C13 1.325(8) . ?
N5 C19 1.385(8) . ?
N2 C20 1.465(8) . ?
N2 C6 1.387(8) . ?
N2 C7 1.363(8) . ?
N1 C1 1.370(8) . ?
N1 C7 1.334(8) . ?
C13 C12 1.480(8) . ?
C9 H9 0.9500 . ?
C9 C10 1.382(10) . ?
C9 C8 1.401(9) . ?
C10 H10 0.9500 . ?
C10 C11 1.383(9) . ?
C12 C11 1.381(8) . ?
C19 C14 1.389(9) . ?
C19 C18 1.403(9) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.511(8) . ?
C28 C33 1.389(9) . ?
C28 C29 1.386(8) . ?
C1 C6 1.404(9) . ?
C1 C2 1.398(9) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.518(8) . ?
C8 C7 1.456(9) . ?
C14 C15 1.389(9) . ?
C17 H17 0.9500 . ?
C17 C18 1.381(10) . ?
C17 C16 1.408(11) . ?
C6 C5 1.386(9) . ?
C5 H5 0.9500 . ?
C5 C4 1.381(10) . ?
C11 H11 0.9500 . ?
C2 H2 0.9500 . ?
C2 C3 1.371(10) . ?
C3 H3 0.9500 . ?
C3 C4 1.412(11) . ?
C15 H15 0.9500 . ?
C15 C16 1.382(10) . ?
C21 C22 1.386(9) . ?
C21 C26 1.387(9) . ?
C18 H18 0.9500 . ?
C4 H4 0.9500 . ?
C16 H16 0.9500 . ?
C33 H33 0.9500 . ?
C33 C32 1.383(9) . ?
C29 H29 0.9500 . ?
C29 C30 1.423(9) . ?
C22 H22 0.9500 . ?
C22 C23 1.390(10) . ?
C23 C24 1.416(11) . ?
C23 C34 1.430(8) . ?
C26 H26 0.9500 . ?
C26 C25 1.395(9) . ?
C32 C31 1.379(11) . ?
C32 C1AA 1.501(11) . ?
C30 C31 1.394(11) . ?
C30 C0AA 1.432(8) . ?
C24 H24 0.9500 . ?
C24 C25 1.370(10) . ?
C25 C35 1.498(11) . ?
C31 H31 0.9500 . ?
C34 F3 1.320(11) . ?
C34 F10 1.378(11) . ?
C34 F12 1.300(10) . ?
C34 F10A 1.311(12) . ?
C34 F12A 1.404(12) . ?
C34 F3A 1.318(13) . ?
C35 F1 1.305(11) . ?
C35 F5 1.303(14) . ?
C35 F8 1.291(15) . ?
F2 C0AA 1.325(12) . ?
C0AA F11 1.343(12) . ?
C0AA F13 1.368(12) . ?
C0AA F13A 1.312(12) . ?
C0AA F2A 1.363(12) . ?
C0AA F11A 1.365(13) . ?
C1AA F15A 1.300(14) . ?
C1AA F6A 1.294(11) . ?
C1AA F4A 1.372(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Sn1 Cl1 100.93(12) . . ?
N5 Sn1 Cl1 84.85(13) . . ?
N5 Sn1 N3 66.49(17) . . ?
N1 Sn1 Cl1 84.67(13) . . ?
N1 Sn1 N3 67.31(18) . . ?
N1 Sn1 N5 129.43(18) . . ?
Cl3 Sn2 Cl2 92.55(6) . . ?
Cl3 Sn2 Cl4 94.81(7) . . ?
Cl4 Sn2 Cl2 92.01(6) . . ?
C13 N4 C27 130.4(5) . . ?
C13 N4 C14 107.0(5) . . ?
C14 N4 C27 122.6(5) . . ?
C12 N3 Sn1 120.8(4) . . ?
C12 N3 C8 119.8(5) . . ?
C8 N3 Sn1 119.2(4) . . ?
C13 N5 Sn1 118.8(4) . . ?
C13 N5 C19 106.1(5) . . ?
C19 N5 Sn1 133.2(4) . . ?
C6 N2 C20 122.7(5) . . ?
C7 N2 C20 129.9(5) . . ?
C7 N2 C6 107.0(5) . . ?
C1 N1 Sn1 133.1(4) . . ?
C7 N1 Sn1 118.3(4) . . ?
C7 N1 C1 106.9(5) . . ?
N4 C13 C12 129.6(5) . . ?
N5 C13 N4 111.8(5) . . ?
N5 C13 C12 118.6(5) . . ?
C10 C9 H9 120.9 . . ?
C10 C9 C8 118.3(6) . . ?
C8 C9 H9 120.9 . . ?
C9 C10 H10 119.9 . . ?
C9 C10 C11 120.1(6) . . ?
C11 C10 H10 119.9 . . ?
N3 C12 C13 112.4(5) . . ?
N3 C12 C11 122.0(5) . . ?
C11 C12 C13 125.5(6) . . ?
N5 C19 C14 109.5(5) . . ?
N5 C19 C18 129.8(6) . . ?
C14 C19 C18 120.7(6) . . ?
N4 C27 H27A 108.9 . . ?
N4 C27 H27B 108.9 . . ?
N4 C27 C28 113.6(5) . . ?
H27A C27 H27B 107.7 . . ?
C28 C27 H27A 108.9 . . ?
C28 C27 H27B 108.9 . . ?
C33 C28 C27 121.5(6) . . ?
C29 C28 C27 119.0(6) . . ?
C29 C28 C33 119.5(6) . . ?
N1 C1 C6 108.7(6) . . ?
N1 C1 C2 130.4(6) . . ?
C2 C1 C6 120.9(6) . . ?
N2 C20 H20A 108.6 . . ?
N2 C20 H20B 108.6 . . ?
N2 C20 C21 114.5(5) . . ?
H20A C20 H20B 107.6 . . ?
C21 C20 H20A 108.6 . . ?
C21 C20 H20B 108.6 . . ?
N3 C8 C9 121.0(6) . . ?
N3 C8 C7 113.3(5) . . ?
C9 C8 C7 125.6(6) . . ?
C19 C14 N4 105.6(5) . . ?
C19 C14 C15 123.3(6) . . ?
C15 C14 N4 131.1(6) . . ?
C18 C17 H17 119.2 . . ?
C18 C17 C16 121.6(6) . . ?
C16 C17 H17 119.2 . . ?
N2 C6 C1 106.0(5) . . ?
C5 C6 N2 131.7(6) . . ?
C5 C6 C1 122.3(6) . . ?
N2 C7 C8 129.3(6) . . ?
N1 C7 N2 111.3(5) . . ?
N1 C7 C8 119.3(5) . . ?
C6 C5 H5 121.8 . . ?
C4 C5 C6 116.4(6) . . ?
C4 C5 H5 121.8 . . ?
C10 C11 H11 120.7 . . ?
C12 C11 C10 118.7(6) . . ?
C12 C11 H11 120.7 . . ?
C1 C2 H2 121.7 . . ?
C3 C2 C1 116.6(6) . . ?
C3 C2 H2 121.7 . . ?
C2 C3 H3 118.9 . . ?
C2 C3 C4 122.2(6) . . ?
C4 C3 H3 118.9 . . ?
C14 C15 H15 122.2 . . ?
C16 C15 C14 115.6(6) . . ?
C16 C15 H15 122.2 . . ?
C22 C21 C20 118.1(6) . . ?
C22 C21 C26 119.6(6) . . ?
C26 C21 C20 122.3(6) . . ?
C19 C18 H18 121.7 . . ?
C17 C18 C19 116.7(6) . . ?
C17 C18 H18 121.7 . . ?
C5 C4 C3 121.5(7) . . ?
C5 C4 H4 119.2 . . ?
C3 C4 H4 119.2 . . ?
C17 C16 H16 118.9 . . ?
C15 C16 C17 122.2(6) . . ?
C15 C16 H16 118.9 . . ?
C28 C33 H33 119.9 . . ?
C32 C33 C28 120.2(6) . . ?
C32 C33 H33 119.9 . . ?
C28 C29 H29 119.7 . . ?
C28 C29 C30 120.6(6) . . ?
C30 C29 H29 119.7 . . ?
C21 C22 H22 119.4 . . ?
C21 C22 C23 121.1(6) . . ?
C23 C22 H22 119.4 . . ?
C22 C23 C24 118.4(7) . . ?
C22 C23 C34 121.8(7) . . ?
C24 C23 C34 119.8(7) . . ?
C21 C26 H26 119.9 . . ?
C21 C26 C25 120.2(6) . . ?
C25 C26 H26 119.9 . . ?
C33 C32 C1AA 120.2(7) . . ?
C31 C32 C33 121.0(7) . . ?
C31 C32 C1AA 118.8(7) . . ?
C29 C30 C0AA 119.2(7) . . ?
C31 C30 C29 118.5(6) . . ?
C31 C30 C0AA 122.2(7) . . ?
C23 C24 H24 119.7 . . ?
C25 C24 C23 120.5(7) . . ?
C25 C24 H24 119.7 . . ?
C26 C25 C35 119.2(7) . . ?
C24 C25 C26 120.2(7) . . ?
C24 C25 C35 120.6(7) . . ?
C32 C31 C30 120.2(7) . . ?
C32 C31 H31 119.9 . . ?
C30 C31 H31 119.9 . . ?
F3 C34 C23 113.8(11) . . ?
F3 C34 F10 99.8(10) . . ?
F10 C34 C23 111.0(8) . . ?
F12 C34 C23 117.4(8) . . ?
F12 C34 F3 110.6(13) . . ?
F12 C34 F10 102.1(11) . . ?
F10A C34 C23 119.5(11) . . ?
F10A C34 F12A 99.0(13) . . ?
F10A C34 F3A 109.7(15) . . ?
F12A C34 C23 107.0(10) . . ?
F3A C34 C23 118.9(16) . . ?
F3A C34 F12A 98.2(14) . . ?
F1 C35 C25 113.0(8) . . ?
F5 C35 C25 111.7(8) . . ?
F5 C35 F1 106.5(10) . . ?
F8 C35 C25 111.7(10) . . ?
F8 C35 F1 106.3(9) . . ?
F8 C35 F5 107.4(11) . . ?
F2 C0AA C30 115.2(14) . . ?
F2 C0AA F11 110.8(14) . . ?
F2 C0AA F13 103.8(13) . . ?
F11 C0AA C30 114.0(10) . . ?
F11 C0AA F13 101.3(11) . . ?
F13 C0AA C30 110.4(12) . . ?
F13A C0AA C30 118.6(12) . . ?
F13A C0AA F2A 106.9(15) . . ?
F13A C0AA F11A 107.0(13) . . ?
F2A C0AA C30 111.8(17) . . ?
F2A C0AA F11A 100.4(14) . . ?
F11A C0AA C30 110.6(11) . . ?
F15A C1AA C32 113.3(9) . . ?
F15A C1AA F4A 103.8(8) . . ?
F6A C1AA C32 112.8(7) . . ?
F6A C1AA F15A 114.0(10) . . ?
F6A C1AA F4A 102.5(10) . . ?
F4A C1AA C32 109.3(9) . . ?

