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

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

data_compound1
_database_code_depnum_ccdc_archive 'CCDC 1510942'
_audit_update_record             
;
2016-11-28 deposited with the CCDC.
2017-01-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        Compound1
_chemical_name_common            ?
_chemical_melting_point          443
_chemical_formula_moiety         'C16 H18 Ge N4, C F3 O3 S, C F3 O3 S, C H2 Cl2'
_chemical_formula_sum            'C19 H20 Cl2 F6 Ge N4 O6 S2'
_chemical_formula_weight         722.00

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   8.4372(5)
_cell_length_b                   13.0507(8)
_cell_length_c                   13.3070(8)
_cell_angle_alpha                69.771(3)
_cell_angle_beta                 85.531(3)
_cell_angle_gamma                81.999(3)
_cell_volume                     1360.79(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8667
_cell_measurement_theta_min      3.54
_cell_measurement_theta_max      72.57

_exptl_crystal_description       Needles
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_exptl_absorpt_coefficient_mu    5.561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.177
_exptl_absorpt_correction_T_max  0.211
_exptl_absorpt_process_details   'SADABS;Universitat Gottingen,1997'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Fine-focus sealed tube'
_diffrn_measurement_device_type  micro-focus
_diffrn_measurement_method       'D8 venture APEX-II'
_diffrn_detector_area_resol_mean 'CMOS-Photon 100'
_diffrn_reflns_number            14142
_diffrn_reflns_av_unetI/netI     0.0604
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.541
_diffrn_reflns_theta_max         72.741
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             5317
_reflns_number_gt                4222
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0459P)²+5.4409P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5317
_refine_ls_number_parameters     363
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0613
_refine_ls_wR_factor_ref         0.1417
_refine_ls_wR_factor_gt          0.1298
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.092
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge01 Ge 0.08294(6) 0.26835(4) 0.06685(4) 0.01588(15) Uani 1 1 d . . . . .
S2 S 0.60548(14) 0.11174(9) 0.16842(9) 0.0190(2) Uani 1 1 d . . . . .
S1 S 0.92421(14) 0.34686(9) 0.77538(9) 0.0201(3) Uani 1 1 d . . . . .
Cl2 Cl 0.50106(19) 0.33722(14) 0.55195(13) 0.0463(4) Uani 1 1 d . . . . .
Cl1 Cl 0.7572(2) 0.28630(16) 0.41106(14) 0.0602(5) Uani 1 1 d . . . . .
F5 F 1.0252(5) 0.2902(3) 0.6086(3) 0.0514(10) Uani 1 1 d . . . . .
O3 O 0.5179(5) 0.2067(3) 0.1851(3) 0.0360(10) Uani 1 1 d . . . . .
F4 F 1.2122(4) 0.2949(3) 0.7067(3) 0.0515(10) Uani 1 1 d . . . . .
O6 O 0.9923(5) 0.4094(3) 0.8277(3) 0.0307(8) Uani 1 1 d . . . . .
F6 F 1.0885(5) 0.4454(3) 0.6021(3) 0.0520(10) Uani 1 1 d . . . . .
O2 O 0.7358(4) 0.1314(3) 0.0899(3) 0.0304(8) Uani 1 1 d . . . . .
O5 O 0.7806(4) 0.4014(3) 0.7181(3) 0.0321(9) Uani 1 1 d . . . . .
O1 O 0.5079(4) 0.0317(3) 0.1649(3) 0.0341(9) Uani 1 1 d . . . . .
N2 N 0.2550(4) 0.2014(3) -0.0220(3) 0.0156(8) Uani 1 1 d . . . . .
O4 O 0.9215(5) 0.2327(3) 0.8367(3) 0.0345(9) Uani 1 1 d . . . . .
F1 F 0.7957(5) -0.0516(3) 0.2910(3) 0.0626(12) Uani 1 1 d . . . . .
N3 N 0.1240(4) 0.0980(3) 0.1489(3) 0.0166(8) Uani 1 1 d . . . . .
F2 F 0.6041(5) 0.0154(4) 0.3762(3) 0.0700(14) Uani 1 1 d . . . . .
N1 N 0.2514(4) 0.3935(3) -0.0040(3) 0.0154(8) Uani 1 1 d . . . . .
N4 N 0.1679(5) 0.2471(3) 0.2229(3) 0.0184(8) Uani 1 1 d . . . . .
F3 F 0.8091(5) 0.1022(5) 0.3115(4) 0.0756(16) Uani 1 1 d . . . . .
C11 C 0.1155(6) 0.0429(4) 0.0718(4) 0.0199(10) Uani 1 1 d . . . . .
H11A H 0.0102 0.0599 0.0414 0.024 Uiso 1 1 calc R U . . .
H11B H 0.1380 -0.0362 0.1054 0.024 Uiso 1 1 calc R U . . .
C10 C 0.2260(5) 0.4967(4) -0.0047(4) 0.0190(10) Uani 1 1 d . . . . .
H10 H 0.1478 0.5143 0.0419 0.023 Uiso 1 1 calc R U . . .
C2 C 0.1668(5) 0.0579(4) 0.2447(4) 0.0177(9) Uani 1 1 d . . . . .
C8 C 0.4240(6) 0.5530(4) -0.1422(4) 0.0220(10) Uani 1 1 d . . . . .
H8 H 0.4829 0.6068 -0.1879 0.026 Uiso 1 1 calc R U . . .
C6 C 0.3595(5) 0.3687(4) -0.0748(4) 0.0164(9) Uani 1 1 d . . . . .
C5 C 0.3667(5) 0.2552(4) -0.0761(4) 0.0166(9) Uani 1 1 d . . . . .
C7 C 0.4497(6) 0.4469(4) -0.1451(4) 0.0209(10) Uani 1 1 d . . . . .
H7 H 0.5252 0.4283 -0.1927 0.025 Uiso 1 1 calc R U . . .
C1 C 0.1866(6) 0.1431(4) 0.2927(4) 0.0196(10) Uani 1 1 d . . . . .
C9 C 0.3110(6) 0.5787(4) -0.0715(4) 0.0202(10) Uani 1 1 d . . . . .
H9 H 0.2924 0.6496 -0.0687 0.024 Uiso 1 1 calc R U . . .
C12 C 0.2435(6) 0.0874(4) -0.0147(4) 0.0198(10) Uani 1 1 d . . . . .
H12A H 0.3458 0.0427 0.0042 0.024 Uiso 1 1 calc R U . . .
H12B H 0.2139 0.0857 -0.0830 0.024 Uiso 1 1 calc R U . . .
C4 C 0.4990(6) 0.2117(4) -0.1370(4) 0.0211(10) Uani 1 1 d . . . . .
H4A H 0.4776 0.1421 -0.1391 0.032 Uiso 1 1 calc R U . . .
H4B H 0.5983 0.2023 -0.1024 0.032 Uiso 1 1 calc R U . . .
H4C H 0.5064 0.2627 -0.2088 0.032 Uiso 1 1 calc R U . . .
C17 C 1.0701(6) 0.3445(5) 0.6676(4) 0.0290(12) Uani 1 1 d . . . . .
C3 C 0.1979(6) -0.0613(4) 0.3097(4) 0.0248(11) Uani 1 1 d . . . . .
H3A H 0.1748 -0.1047 0.2684 0.037 Uiso 1 1 calc R U . . .
H3B H 0.1307 -0.0768 0.3735 0.037 Uiso 1 1 calc R U . . .
H3C H 0.3082 -0.0792 0.3289 0.037 Uiso 1 1 calc R U . . .
C16 C 0.1787(6) 0.3301(4) 0.2576(4) 0.0228(10) Uani 1 1 d . . . . .
H16 H 0.1598 0.4019 0.2104 0.027 Uiso 1 1 calc R U . . .
C13 C 0.2225(6) 0.1203(4) 0.3974(4) 0.0250(11) Uani 1 1 d . . . . .
H13 H 0.2340 0.0481 0.4443 0.030 Uiso 1 1 calc R U . . .
C14 C 0.2416(6) 0.2062(4) 0.4327(4) 0.0277(11) Uani 1 1 d . . . . .
H14 H 0.2703 0.1921 0.5027 0.033 Uiso 1 1 calc R U . . .
C15 C 0.2175(6) 0.3125(4) 0.3625(4) 0.0264(11) Uani 1 1 d . . . . .
H15 H 0.2269 0.3715 0.3847 0.032 Uiso 1 1 calc R U . . .
C18 C 0.7092(7) 0.0426(6) 0.2926(5) 0.0414(15) Uani 1 1 d . . . . .
C19 C 0.6748(8) 0.3795(6) 0.4766(6) 0.0479(16) Uani 1 1 d . . . . .
H19A H 0.7534 0.3848 0.5235 0.058 Uiso 1 1 calc R U . . .
H19B H 0.6494 0.4519 0.4237 0.058 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge01 N2 2.088(4) . ?
Ge01 N3 2.102(4) . ?
Ge01 N4 2.163(4) . ?
Ge01 N1 2.224(4) . ?
S2 O3 1.429(4) . ?
S2 O1 1.432(4) . ?
S2 O2 1.443(4) . ?
S2 C18 1.813(6) . ?
S1 O4 1.432(4) . ?
S1 O6 1.437(4) . ?
S1 O5 1.444(4) . ?
S1 C17 1.822(5) . ?
Cl2 C19 1.753(7) . ?
Cl1 C19 1.768(7) . ?
F5 C17 1.329(7) . ?
F4 C17 1.333(6) . ?
F6 C17 1.327(6) . ?
N2 C5 1.277(6) . ?
N2 C12 1.474(6) . ?
F1 C18 1.346(7) . ?
N3 C2 1.260(6) . ?
N3 C11 1.453(6) . ?
F2 C18 1.345(7) . ?
N1 C10 1.331(6) . ?
N1 C6 1.349(6) . ?
N4 C16 1.333(6) . ?
N4 C1 1.349(6) . ?
F3 C18 1.315(8) . ?
C11 C12 1.532(6) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C10 C9 1.381(7) . ?
C10 H10 0.9300 . ?
C2 C3 1.493(6) . ?
C2 C1 1.494(6) . ?
C8 C9 1.377(7) . ?
C8 C7 1.386(6) . ?
C8 H8 0.9300 . ?
C6 C7 1.393(6) . ?
C6 C5 1.480(6) . ?
C5 C4 1.492(6) . ?
C7 H7 0.9300 . ?
C1 C13 1.369(7) . ?
C9 H9 0.9300 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C16 C15 1.391(7) . ?
C16 H16 0.9300 . ?
C13 C14 1.390(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.376(7) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ge01 N3 72.31(14) . . ?
N2 Ge01 N4 111.55(15) . . ?
N3 Ge01 N4 73.21(15) . . ?
N2 Ge01 N1 73.90(14) . . ?
N3 Ge01 N1 131.37(14) . . ?
N4 Ge01 N1 88.15(14) . . ?
O3 S2 O1 114.3(2) . . ?
O3 S2 O2 116.3(2) . . ?
O1 S2 O2 115.1(2) . . ?
O3 S2 C18 103.3(3) . . ?
O1 S2 C18 102.7(3) . . ?
O2 S2 C18 102.4(3) . . ?
O4 S1 O6 115.2(2) . . ?
O4 S1 O5 115.5(2) . . ?
O6 S1 O5 114.8(2) . . ?
O4 S1 C17 103.2(2) . . ?
O6 S1 C17 103.0(2) . . ?
O5 S1 C17 102.6(2) . . ?
C5 N2 C12 122.2(4) . . ?
C5 N2 Ge01 121.6(3) . . ?
C12 N2 Ge01 116.1(3) . . ?
C2 N3 C11 129.1(4) . . ?
C2 N3 Ge01 122.7(3) . . ?
C11 N3 Ge01 107.6(3) . . ?
C10 N1 C6 118.8(4) . . ?
C10 N1 Ge01 124.8(3) . . ?
C6 N1 Ge01 113.6(3) . . ?
C16 N4 C1 119.2(4) . . ?
C16 N4 Ge01 123.8(3) . . ?
C1 N4 Ge01 116.3(3) . . ?
N3 C11 C12 104.9(4) . . ?
N3 C11 H11A 110.8 . . ?
C12 C11 H11A 110.8 . . ?
N3 C11 H11B 110.8 . . ?
C12 C11 H11B 110.8 . . ?
H11A C11 H11B 108.8 . . ?
N1 C10 C9 122.8(4) . . ?
N1 C10 H10 118.6 . . ?
C9 C10 H10 118.6 . . ?
N3 C2 C3 126.6(4) . . ?
N3 C2 C1 113.3(4) . . ?
C3 C2 C1 120.1(4) . . ?
C9 C8 C7 119.9(4) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
N1 C6 C7 121.8(4) . . ?
N1 C6 C5 114.8(4) . . ?
C7 C6 C5 123.2(4) . . ?
N2 C5 C6 115.0(4) . . ?
N2 C5 C4 125.1(4) . . ?
C6 C5 C4 119.9(4) . . ?
C8 C7 C6 118.2(4) . . ?
C8 C7 H7 120.9 . . ?
C6 C7 H7 120.9 . . ?
N4 C1 C13 121.8(4) . . ?
N4 C1 C2 114.0(4) . . ?
C13 C1 C2 124.3(4) . . ?
C8 C9 C10 118.5(4) . . ?
C8 C9 H9 120.8 . . ?
C10 C9 H9 120.8 . . ?
N2 C12 C11 107.6(4) . . ?
N2 C12 H12A 110.2 . . ?
C11 C12 H12A 110.2 . . ?
N2 C12 H12B 110.2 . . ?
C11 C12 H12B 110.2 . . ?
H12A C12 H12B 108.5 . . ?
C5 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C5 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
F6 C17 F5 107.2(5) . . ?
F6 C17 F4 108.4(5) . . ?
F5 C17 F4 107.4(5) . . ?
F6 C17 S1 111.4(4) . . ?
F5 C17 S1 111.5(4) . . ?
F4 C17 S1 110.9(4) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N4 C16 C15 121.9(4) . . ?
N4 C16 H16 119.0 . . ?
C15 C16 H16 119.0 . . ?
C1 C13 C14 119.3(5) . . ?
C1 C13 H13 120.4 . . ?
C14 C13 H13 120.4 . . ?
C15 C14 C13 119.0(5) . . ?
C15 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
C14 C15 C16 118.8(5) . . ?
C14 C15 H15 120.6 . . ?
C16 C15 H15 120.6 . . ?
F3 C18 F2 108.4(5) . . ?
F3 C18 F1 106.8(5) . . ?
F2 C18 F1 106.9(6) . . ?
F3 C18 S2 113.0(5) . . ?
F2 C18 S2 110.7(4) . . ?
F1 C18 S2 110.9(4) . . ?
Cl2 C19 Cl1 111.4(4) . . ?
Cl2 C19 H19A 109.4 . . ?
Cl1 C19 H19A 109.4 . . ?
Cl2 C19 H19B 109.4 . . ?
Cl1 C19 H19B 109.4 . . ?
H19A C19 H19B 108.0 . . ?

_refine_diff_density_max         0.877
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.128

####################################################################### 
# 
# 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_CompoundLGeClOTf
_database_code_depnum_ccdc_archive 'CCDC 1510943'
_audit_update_record             
;
2016-11-28 deposited with the CCDC.
2017-01-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          403
_chemical_formula_moiety         'C17 H18 Cl F3 Ge N4 O3 S'
_chemical_formula_sum            'C17 H18 Cl F3 Ge N4 O3 S'
_chemical_formula_weight         523.45

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   20.5748(10)
_cell_length_b                   13.4785(7)
_cell_length_c                   14.7382(8)
_cell_angle_alpha                90
_cell_angle_beta                 99.802(3)
_cell_angle_gamma                90
_cell_volume                     4027.5(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9929
_cell_measurement_theta_min      4.36
_cell_measurement_theta_max      72.44

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.33
_exptl_absorpt_coefficient_mu    4.775
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.178
_exptl_absorpt_correction_T_max  0.207
_exptl_absorpt_process_details   'SADABS;Universitat Gottingen,1997'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Fine-focused sealed tube'
_diffrn_measurement_device_type  'D8 Venture APEX-II'
_diffrn_measurement_method       'CMOS-Photon 100'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36440
_diffrn_reflns_av_unetI/netI     0.0912
_diffrn_reflns_av_R_equivalents  0.1057
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.938
_diffrn_reflns_theta_max         72.714
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             7885
_reflns_number_gt                5009
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0417P)²+24.7087P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7885
_refine_ls_number_parameters     545
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1342
_refine_ls_R_factor_gt           0.0772
_refine_ls_wR_factor_ref         0.1635
_refine_ls_wR_factor_gt          0.1397
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.78148(4) 0.50205(6) 0.38415(5) 0.01713(19) Uani 1 1 d . . . . .
Ge2 Ge 0.28311(4) 0.00832(6) 0.35073(5) 0.0182(2) Uani 1 1 d . . . . .
Cl2 Cl 0.29767(8) -0.02136(11) 0.50543(11) 0.0204(4) Uani 1 1 d . . . . .
Cl1 Cl 0.80065(8) 0.53299(12) 0.53854(11) 0.0210(4) Uani 1 1 d . . . . .
S2 S 0.08781(9) 0.31158(12) 0.13384(12) 0.0204(4) Uani 1 1 d . . . . .
S1 S 0.40900(9) 0.68934(12) 0.36574(13) 0.0228(4) Uani 1 1 d . . . . .
F1 F 0.3923(2) 0.5232(3) 0.2709(3) 0.0378(11) Uani 1 1 d . . . . .
F5 F 0.1541(2) 0.4653(3) 0.0902(3) 0.0346(11) Uani 1 1 d . . . . .
F4 F 0.1924(2) 0.4047(3) 0.2229(3) 0.0402(12) Uani 1 1 d . . . . .
F6 F 0.1029(2) 0.4913(3) 0.2035(3) 0.0366(11) Uani 1 1 d . . . . .
F3 F 0.3113(2) 0.6260(3) 0.2399(3) 0.0421(12) Uani 1 1 d . . . . .
F2 F 0.3251(2) 0.5437(3) 0.3664(4) 0.0458(13) Uani 1 1 d . . . . .
O6 O 0.0320(2) 0.3502(4) 0.0718(3) 0.0246(11) Uani 1 1 d . . . . .
O3 O 0.4342(2) 0.7366(3) 0.2918(4) 0.0294(12) Uani 1 1 d . . . . .
O4 O 0.1313(3) 0.2503(3) 0.0912(4) 0.0344(14) Uani 1 1 d . . . . .
O5 O 0.0733(3) 0.2767(4) 0.2198(3) 0.0307(12) Uani 1 1 d . . . . .
O2 O 0.3637(3) 0.7483(4) 0.4071(4) 0.0377(14) Uani 1 1 d . . . . .
N6 N 0.3026(3) 0.1679(4) 0.3768(4) 0.0180(12) Uani 1 1 d . . . . .
O1 O 0.4569(3) 0.6358(4) 0.4297(3) 0.0332(13) Uani 1 1 d . . . . .
N2 N 0.6834(3) 0.4417(4) 0.3857(4) 0.0184(12) Uani 1 1 d . . . . .
N5 N 0.1856(3) 0.0673(4) 0.3631(4) 0.0193(13) Uani 1 1 d . . . . .
N3 N 0.6980(3) 0.6351(4) 0.3801(4) 0.0191(13) Uani 1 1 d . . . . .
N4 N 0.9014(3) 0.4608(4) 0.3991(4) 0.0186(12) Uani 1 1 d . . . . .
N7 N 0.4048(3) 0.0479(4) 0.3837(4) 0.0187(13) Uani 1 1 d . . . . .
N8 N 0.1991(3) -0.1236(4) 0.3382(4) 0.0207(13) Uani 1 1 d . . . . .
N1 N 0.8014(3) 0.3446(4) 0.4235(4) 0.0204(13) Uani 1 1 d . . . . .
C5 C 0.6293(3) 0.4905(5) 0.3667(4) 0.0183(14) Uani 1 1 d . . . . .
C22 C 0.1317(3) 0.0174(5) 0.3517(4) 0.0192(15) Uani 1 1 d . . . . .
C24 C 0.1373(3) -0.0905(5) 0.3302(4) 0.0176(15) Uani 1 1 d . . . . .
C20 C 0.3593(4) 0.2095(5) 0.3984(5) 0.0201(15) Uani 1 1 d . . . . .
C12 C 0.6362(3) 0.6000(5) 0.3577(4) 0.0158(14) Uani 1 1 d . . . . .
C16 C 0.7082(3) 0.7324(5) 0.3758(5) 0.0219(16) Uani 1 1 d . . . . .
H16 H 0.7510 0.7563 0.3922 0.026 Uiso 1 1 calc R U . . .
C7 C 0.9154(3) 0.3637(5) 0.4174(4) 0.0175(15) Uani 1 1 d . . . . .
C13 C 0.5838(3) 0.6634(5) 0.3274(5) 0.0204(15) Uani 1 1 d . . . . .
H13 H 0.5415 0.6379 0.3102 0.024 Uiso 1 1 calc R U . . .
C6 C 0.5632(3) 0.4442(5) 0.3550(5) 0.0246(16) Uani 1 1 d . . . . .
H6A H 0.5616 0.3888 0.3136 0.037 Uiso 1 1 calc R U . . .
H6B H 0.5304 0.4920 0.3300 0.037 Uiso 1 1 calc R U . . .
H6C H 0.5547 0.4216 0.4136 0.037 Uiso 1 1 calc R U . . .
C1 C 0.6819(3) 0.3334(5) 0.3897(5) 0.0239(17) Uani 1 1 d . . . . .
H1A H 0.6777 0.3064 0.3279 0.029 Uiso 1 1 calc R U . . .
H1B H 0.6441 0.3119 0.4158 0.029 Uiso 1 1 calc R U . . .
C29 C 0.4179(3) 0.1442(5) 0.4036(4) 0.0184(15) Uani 1 1 d . . . . .
C30 C 0.4826(3) 0.1802(5) 0.4218(5) 0.0232(16) Uani 1 1 d . . . . .
H30 H 0.4909 0.2464 0.4373 0.028 Uiso 1 1 calc R U . . .
C3 C 0.8583(3) 0.3028(5) 0.4329(4) 0.0156(14) Uani 1 1 d . . . . .
C11 C 0.9499(3) 0.5203(5) 0.3819(4) 0.0185(15) Uani 1 1 d . . . . .
H11 H 0.9401 0.5864 0.3675 0.022 Uiso 1 1 calc R U . . .
C26 C 0.0933(4) -0.2522(5) 0.2939(5) 0.0274(17) Uani 1 1 d . . . . .
H26 H 0.0578 -0.2954 0.2791 0.033 Uiso 1 1 calc R U . . .
C8 C 0.9786(3) 0.3260(5) 0.4216(5) 0.0207(16) Uani 1 1 d . . . . .
H8 H 0.9873 0.2593 0.4349 0.025 Uiso 1 1 calc R U . . .
C18 C 0.1863(3) 0.1717(5) 0.3912(5) 0.0214(16) Uani 1 1 d . . . . .
H18A H 0.1925 0.1761 0.4578 0.026 Uiso 1 1 calc R U . . .
H18B H 0.1444 0.2025 0.3663 0.026 Uiso 1 1 calc R U . . .
C14 C 0.5943(4) 0.7643(5) 0.3226(5) 0.0264(17) Uani 1 1 d . . . . .
H14 H 0.5595 0.8075 0.3028 0.032 Uiso 1 1 calc R U . . .
C15 C 0.6577(4) 0.7993(5) 0.3481(5) 0.0238(16) Uani 1 1 d . . . . .
H15 H 0.6665 0.8670 0.3466 0.029 Uiso 1 1 calc R U . . .
C33 C 0.4549(3) -0.0130(5) 0.3789(4) 0.0219(16) Uani 1 1 d . . . . .
H33 H 0.4457 -0.0793 0.3646 0.026 Uiso 1 1 calc R U . . .
C17 C 0.3562(4) 0.5902(5) 0.3074(5) 0.0285(18) Uani 1 1 d . . . . .
C28 C 0.2088(4) -0.2196(5) 0.3235(5) 0.0246(16) Uani 1 1 d . . . . .
H28 H 0.2518 -0.2423 0.3271 0.030 Uiso 1 1 calc R U . . .
C4 C 0.8706(3) 0.1957(5) 0.4547(5) 0.0230(16) Uani 1 1 d . . . . .
H4A H 0.8337 0.1684 0.4783 0.035 Uiso 1 1 calc R U . . .
H4B H 0.9098 0.1890 0.5001 0.035 Uiso 1 1 calc R U . . .
H4C H 0.8762 0.1607 0.3998 0.035 Uiso 1 1 calc R U . . .
C27 C 0.1573(4) -0.2871(5) 0.3029(5) 0.0247(16) Uani 1 1 d . . . . .
H27 H 0.1657 -0.3541 0.2952 0.030 Uiso 1 1 calc R U . . .
C25 C 0.0823(3) -0.1514(5) 0.3074(5) 0.0227(16) Uani 1 1 d . . . . .
H25 H 0.0398 -0.1258 0.3014 0.027 Uiso 1 1 calc R U . . .
C19 C 0.2412(3) 0.2252(5) 0.3565(5) 0.0213(16) Uani 1 1 d . . . . .
H19A H 0.2295 0.2352 0.2906 0.026 Uiso 1 1 calc R U . . .
H19B H 0.2476 0.2899 0.3857 0.026 Uiso 1 1 calc R U . . .
C10 C 1.0145(3) 0.4880(5) 0.3844(4) 0.0214(15) Uani 1 1 d . . . . .
H10 H 1.0471 0.5313 0.3722 0.026 Uiso 1 1 calc R U . . .
C32 C 0.5202(4) 0.0174(5) 0.3943(5) 0.0231(16) Uani 1 1 d . . . . .
H32 H 0.5538 -0.0275 0.3898 0.028 Uiso 1 1 calc R U . . .
C9 C 1.0286(4) 0.3892(5) 0.4058(5) 0.0236(16) Uani 1 1 d . . . . .
H9 H 1.0714 0.3656 0.4095 0.028 Uiso 1 1 calc R U . . .
C23 C 0.0668(4) 0.0615(6) 0.3636(5) 0.0292(18) Uani 1 1 d . . . . .
H23A H 0.0707 0.0901 0.4239 0.044 Uiso 1 1 calc R U . . .
H23B H 0.0337 0.0106 0.3565 0.044 Uiso 1 1 calc R U . . .
H23C H 0.0545 0.1120 0.3180 0.044 Uiso 1 1 calc R U . . .
C2 C 0.7436(4) 0.2954(5) 0.4471(5) 0.0298(18) Uani 1 1 d . . . . .
H2A H 0.7419 0.3067 0.5117 0.036 Uiso 1 1 calc R U . . .
H2B H 0.7471 0.2245 0.4378 0.036 Uiso 1 1 calc R U . . .
C21 C 0.3709(4) 0.3186(5) 0.4158(5) 0.0299(18) Uani 1 1 d . . . . .
H21A H 0.3823 0.3493 0.3619 0.045 Uiso 1 1 calc R U . . .
H21B H 0.4062 0.3276 0.4668 0.045 Uiso 1 1 calc R U . . .
H21C H 0.3314 0.3486 0.4299 0.045 Uiso 1 1 calc R U . . .
C31 C 0.5344(4) 0.1154(5) 0.4164(5) 0.0270(17) Uani 1 1 d . . . . .
H31 H 0.5778 0.1376 0.4275 0.032 Uiso 1 1 calc R U . . .
C34 C 0.1371(4) 0.4239(5) 0.1649(5) 0.0248(17) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 N2 2.180(6) . ?
Ge1 N1 2.220(5) . ?
Ge1 Cl1 2.2807(18) . ?
Ge2 N5 2.195(6) . ?
Ge2 N6 2.210(5) . ?
Ge2 Cl2 2.2837(17) . ?
S2 O5 1.430(5) . ?
S2 O6 1.438(5) . ?
S2 O4 1.439(5) . ?
S2 C34 1.837(7) . ?
S1 O3 1.434(5) . ?
S1 O2 1.436(5) . ?
S1 O1 1.437(5) . ?
S1 C17 1.840(8) . ?
F1 C17 1.339(8) . ?
F5 C34 1.333(8) . ?
F4 C34 1.327(8) . ?
F6 C34 1.334(8) . ?
F3 C17 1.329(8) . ?
F2 C17 1.322(8) . ?
N6 C20 1.285(8) . ?
N6 C19 1.467(8) . ?
N2 C5 1.283(8) . ?
N2 C1 1.461(8) . ?
N5 C22 1.282(8) . ?
N5 C18 1.467(8) . ?
N3 C16 1.332(8) . ?
N3 C12 1.344(8) . ?
N4 C11 1.339(8) . ?
N4 C7 1.356(8) . ?
N7 C33 1.328(8) . ?
N7 C29 1.348(8) . ?
N8 C28 1.332(8) . ?
N8 C24 1.333(8) . ?
N1 C3 1.284(8) . ?
N1 C2 1.454(9) . ?
C5 C6 1.479(9) . ?
C5 C12 1.490(9) . ?
C22 C24 1.497(9) . ?
C22 C23 1.499(9) . ?
C24 C25 1.391(9) . ?
C20 C29 1.484(9) . ?
C20 C21 1.505(9) . ?
C12 C13 1.389(9) . ?
C16 C15 1.384(9) . ?
C16 H16 0.9300 . ?
C7 C8 1.388(9) . ?
C7 C3 1.483(9) . ?
C13 C14 1.381(9) . ?
C13 H13 0.9300 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C1 C2 1.492(9) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C29 C30 1.400(9) . ?
C30 C31 1.391(10) . ?
C30 H30 0.9300 . ?
C3 C4 1.491(9) . ?
C11 C10 1.392(9) . ?
C11 H11 0.9300 . ?
C26 C27 1.385(10) . ?
C26 C25 1.397(10) . ?
C26 H26 0.9300 . ?
C8 C9 1.387(9) . ?
C8 H8 0.9300 . ?
C18 C19 1.501(9) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C14 C15 1.378(10) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C33 C32 1.384(10) . ?
C33 H33 0.9300 . ?
C28 C27 1.390(10) . ?
C28 H28 0.9300 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C27 H27 0.9300 . ?
C25 H25 0.9300 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C10 C9 1.387(10) . ?
C10 H10 0.9300 . ?
C32 C31 1.380(10) . ?
C32 H32 0.9300 . ?
C9 H9 0.9300 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C31 H31 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ge1 N1 76.7(2) . . ?
N2 Ge1 Cl1 93.48(15) . . ?
N1 Ge1 Cl1 85.47(15) . . ?
N5 Ge2 N6 77.0(2) . . ?
N5 Ge2 Cl2 86.96(15) . . ?
N6 Ge2 Cl2 90.45(15) . . ?
O5 S2 O6 114.7(3) . . ?
O5 S2 O4 115.9(3) . . ?
O6 S2 O4 114.8(3) . . ?
O5 S2 C34 103.9(3) . . ?
O6 S2 C34 102.0(3) . . ?
O4 S2 C34 102.9(3) . . ?
O3 S1 O2 114.9(3) . . ?
O3 S1 O1 115.2(3) . . ?
O2 S1 O1 115.0(3) . . ?
O3 S1 C17 103.2(3) . . ?
O2 S1 C17 103.1(3) . . ?
O1 S1 C17 103.0(3) . . ?
C20 N6 C19 122.3(6) . . ?
C20 N6 Ge2 126.7(5) . . ?
C19 N6 Ge2 110.7(4) . . ?
C5 N2 C1 119.9(6) . . ?
C5 N2 Ge1 125.2(5) . . ?
C1 N2 Ge1 113.5(4) . . ?
C22 N5 C18 120.5(6) . . ?
C22 N5 Ge2 125.5(5) . . ?
C18 N5 Ge2 113.9(4) . . ?
C16 N3 C12 119.0(6) . . ?
C11 N4 C7 118.4(6) . . ?
C33 N7 C29 118.6(6) . . ?
C28 N8 C24 118.5(6) . . ?
C3 N1 C2 122.7(6) . . ?
C3 N1 Ge1 124.9(5) . . ?
C2 N1 Ge1 112.1(4) . . ?
N2 C5 C6 123.7(6) . . ?
N2 C5 C12 115.8(6) . . ?
C6 C5 C12 120.5(6) . . ?
N5 C22 C24 116.2(6) . . ?
N5 C22 C23 122.9(6) . . ?
C24 C22 C23 120.8(6) . . ?
N8 C24 C25 123.2(6) . . ?
N8 C24 C22 114.4(6) . . ?
C25 C24 C22 122.4(6) . . ?
N6 C20 C29 116.7(6) . . ?
N6 C20 C21 125.4(7) . . ?
C29 C20 C21 117.9(6) . . ?
N3 C12 C13 120.8(6) . . ?
N3 C12 C5 115.3(6) . . ?
C13 C12 C5 123.9(6) . . ?
N3 C16 C15 122.7(6) . . ?
N3 C16 H16 118.7 . . ?
C15 C16 H16 118.7 . . ?
N4 C7 C8 121.9(6) . . ?
N4 C7 C3 114.7(6) . . ?
C8 C7 C3 123.4(6) . . ?
C14 C13 C12 120.2(7) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 C1 C2 110.1(6) . . ?
N2 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
N2 C1 H1B 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.2 . . ?
N7 C29 C30 121.5(6) . . ?
N7 C29 C20 115.5(6) . . ?
C30 C29 C20 122.9(6) . . ?
C31 C30 C29 119.0(6) . . ?
C31 C30 H30 120.5 . . ?
C29 C30 H30 120.5 . . ?
N1 C3 C7 118.1(6) . . ?
N1 C3 C4 124.5(6) . . ?
C7 C3 C4 117.4(6) . . ?
N4 C11 C10 123.2(6) . . ?
N4 C11 H11 118.4 . . ?
C10 C11 H11 118.4 . . ?
C27 C26 C25 119.4(7) . . ?
C27 C26 H26 120.3 . . ?
C25 C26 H26 120.3 . . ?
C9 C8 C7 118.9(6) . . ?
C9 C8 H8 120.5 . . ?
C7 C8 H8 120.5 . . ?
N5 C18 C19 109.7(6) . . ?
N5 C18 H18A 109.7 . . ?
C19 C18 H18A 109.7 . . ?
N5 C18 H18B 109.7 . . ?
C19 C18 H18B 109.7 . . ?
H18A C18 H18B 108.2 . . ?
C15 C14 C13 118.2(7) . . ?
C15 C14 H14 120.9 . . ?
C13 C14 H14 120.9 . . ?
C14 C15 C16 119.0(6) . . ?
C14 C15 H15 120.5 . . ?
C16 C15 H15 120.5 . . ?
N7 C33 C32 123.3(6) . . ?
N7 C33 H33 118.4 . . ?
C32 C33 H33 118.4 . . ?
F2 C17 F3 108.2(7) . . ?
F2 C17 F1 108.0(6) . . ?
F3 C17 F1 107.8(6) . . ?
F2 C17 S1 110.5(5) . . ?
F3 C17 S1 111.4(5) . . ?
F1 C17 S1 110.7(5) . . ?
N8 C28 C27 122.8(7) . . ?
N8 C28 H28 118.6 . . ?
C27 C28 H28 118.6 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C26 C27 C28 118.4(7) . . ?
C26 C27 H27 120.8 . . ?
C28 C27 H27 120.8 . . ?
C24 C25 C26 117.6(7) . . ?
C24 C25 H25 121.2 . . ?
C26 C25 H25 121.2 . . ?
N6 C19 C18 110.4(5) . . ?
N6 C19 H19A 109.6 . . ?
C18 C19 H19A 109.6 . . ?
N6 C19 H19B 109.6 . . ?
C18 C19 H19B 109.6 . . ?
H19A C19 H19B 108.1 . . ?
C9 C10 C11 117.9(6) . . ?
C9 C10 H10 121.1 . . ?
C11 C10 H10 121.1 . . ?
C31 C32 C33 118.9(7) . . ?
C31 C32 H32 120.6 . . ?
C33 C32 H32 120.6 . . ?
C8 C9 C10 119.7(7) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N1 C2 C1 111.1(6) . . ?
N1 C2 H2A 109.4 . . ?
C1 C2 H2A 109.4 . . ?
N1 C2 H2B 109.4 . . ?
C1 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C32 C31 C30 118.7(7) . . ?
C32 C31 H31 120.6 . . ?
C30 C31 H31 120.6 . . ?
F4 C34 F5 107.3(6) . . ?
F4 C34 F6 108.4(6) . . ?
F5 C34 F6 107.4(6) . . ?
F4 C34 S2 112.1(5) . . ?
F5 C34 S2 110.5(5) . . ?
F6 C34 S2 111.0(5) . . ?

_refine_diff_density_max         0.802
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.145

####################################################################### 
# 
# 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_Compound3
_database_code_depnum_ccdc_archive 'CCDC 1510944'
_audit_update_record             
;
2016-11-28 deposited with the CCDC.
2017-01-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        Compound3
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C37 H36 Au F15 Ge2 N8 O15 S5'
_chemical_formula_sum            'C37 H36 Au F15 Ge2 N8 O15 S5'
_chemical_formula_weight         1620.18

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -4.4197 7.2980 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   12.421(3)
_cell_length_b                   12.980(3)
_cell_length_c                   17.648(4)
_cell_angle_alpha                85.383(5)
_cell_angle_beta                 72.526(5)
_cell_angle_gamma                75.017(5)
_cell_volume                     2621.8(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9588
_cell_measurement_theta_min      3.52
_cell_measurement_theta_max      73.00

_exptl_crystal_description       Neddles
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.052
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.37
_exptl_absorpt_coefficient_mu    9.527
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.018
_exptl_absorpt_correction_T_max  0.029
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   'SADABS;Universitat Gottingen,1997'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Single-focused sealed tube'
_diffrn_measurement_device_type  'D8 venture APEX-II'
_diffrn_measurement_method       'CMOS-Photon 100'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29573
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.625
_diffrn_reflns_theta_max         73.011
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             10213
_reflns_number_gt                10067
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0568P)²+5.0961P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10213
_refine_ls_number_parameters     752
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0364
_refine_ls_wR_factor_ref         0.0970
_refine_ls_wR_factor_gt          0.0965
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.095
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Au1 Au 0.33390(2) 0.33038(2) 0.74104(2) 0.00758(6) Uani 1 1 d . . . . .
Ge1 Ge 0.41066(3) 0.31536(3) 0.85110(2) 0.00600(9) Uani 1 1 d . . . . .
Ge2 Ge 0.27882(3) 0.30189(3) 0.62751(2) 0.00597(9) Uani 1 1 d . . . . .
S3 S 0.72068(7) 0.18947(7) 0.63003(5) 0.00997(16) Uani 1 1 d . . . . .
S2 S 0.09242(7) 0.20215(7) 0.84602(5) 0.01094(17) Uani 1 1 d . . . . .
S1 S 0.17377(7) 0.60640(7) 0.75512(5) 0.01222(17) Uani 1 1 d . . . . .
S5 S 0.23599(7) 0.27355(7) 0.39772(5) 0.01151(17) Uani 1 1 d . . . . .
S4 S 0.48331(10) 0.77038(8) 0.93689(6) 0.0193(2) Uani 1 1 d . . . . .
F5 F -0.0684(2) 0.1442(2) 0.96244(15) 0.0283(6) Uani 1 1 d . . . . .
F4 F 0.1064(2) 0.0497(2) 0.95175(16) 0.0276(6) Uani 1 1 d . . . . .
F7 F 0.8851(2) 0.0200(2) 0.56828(17) 0.0289(6) Uani 1 1 d . . . . .
F1 F 0.1030(2) 0.7465(2) 0.87054(15) 0.0277(6) Uani 1 1 d . . . . .
F9 F 0.7417(2) 0.0592(2) 0.51835(16) 0.0278(6) Uani 1 1 d . . . . .
F11 F 0.1757(3) 0.2903(2) 0.26638(16) 0.0303(6) Uani 1 1 d . . . . .
F6 F 0.0173(2) 0.0274(2) 0.86916(18) 0.0298(6) Uani 1 1 d . . . . .
F10 F 0.2387(2) 0.1283(2) 0.30117(17) 0.0303(6) Uani 1 1 d . . . . .
O6 O 0.0028(2) 0.2484(2) 0.80734(17) 0.0179(6) Uani 1 1 d . . . . .
O4 O 0.2007(2) 0.1421(2) 0.79359(16) 0.0184(6) Uani 1 1 d . . . . .
F15 F 0.4058(3) 0.7311(2) 0.82188(19) 0.0340(7) Uani 1 1 d . . . . .
F2 F 0.0207(2) 0.7920(2) 0.77761(18) 0.0315(6) Uani 1 1 d . . . . .
F12 F 0.0676(2) 0.2184(2) 0.36398(17) 0.0301(6) Uani 1 1 d . . . . .
O8 O 0.6699(3) 0.1172(2) 0.68784(16) 0.0183(6) Uani 1 1 d . . . . .
O2 O 0.2779(2) 0.5678(2) 0.78016(18) 0.0208(6) Uani 1 1 d . . . . .
O7 O 0.8016(3) 0.2359(2) 0.65044(19) 0.0219(6) Uani 1 1 d . . . . .
O3 O 0.1955(3) 0.6195(3) 0.67030(17) 0.0211(6) Uani 1 1 d . . . . .
O5 O 0.1046(3) 0.2721(2) 0.90072(18) 0.0197(6) Uani 1 1 d . . . . .
N6 N 0.1691(3) 0.4260(2) 0.59465(17) 0.0090(6) Uani 1 1 d . . . . .
F3 F 0.1983(2) 0.8005(2) 0.75789(17) 0.0288(6) Uani 1 1 d . . . . .
F8 F 0.8700(3) 0.1521(3) 0.48771(17) 0.0431(8) Uani 1 1 d . . . . .
O15 O 0.1604(3) 0.3795(2) 0.4168(2) 0.0255(7) Uani 1 1 d . . . . .
N2 N 0.3447(3) 0.2091(2) 0.92734(18) 0.0097(6) Uani 1 1 d . . . . .
O9 O 0.6389(3) 0.2626(2) 0.59595(19) 0.0207(6) Uani 1 1 d . . . . .
N5 N 0.3808(3) 0.3429(2) 0.52237(17) 0.0083(6) Uani 1 1 d . . . . .
O14 O 0.3541(2) 0.2709(2) 0.35271(17) 0.0182(6) Uani 1 1 d . . . . .
N3 N 0.5487(3) 0.1969(2) 0.85219(17) 0.0074(5) Uani 1 1 d . . . . .
O11 O 0.4779(3) 0.8703(2) 0.97051(18) 0.0266(7) Uani 1 1 d . . . . .
O1 O 0.0797(3) 0.5573(2) 0.79395(19) 0.0249(7) Uani 1 1 d . . . . .
N7 N 0.1463(2) 0.2417(2) 0.63295(17) 0.0085(6) Uani 1 1 d . . . . .
F14 F 0.4631(4) 0.8761(3) 0.80837(18) 0.0541(10) Uani 1 1 d . . . . .
N4 N 0.5418(3) 0.3943(2) 0.82617(17) 0.0089(6) Uani 1 1 d . . . . .
N8 N 0.3578(2) 0.1402(2) 0.61505(17) 0.0075(5) Uani 1 1 d . . . . .
N1 N 0.3114(3) 0.4087(2) 0.94659(18) 0.0104(6) Uani 1 1 d . . . . .
O13 O 0.2244(3) 0.1991(3) 0.46274(18) 0.0270(7) Uani 1 1 d . . . . .
F13 F 0.3011(3) 0.8684(3) 0.8931(3) 0.0642(13) Uani 1 1 d . . . . .
C21 C 0.3345(3) 0.4404(3) 0.4957(2) 0.0095(7) Uani 1 1 d . . . . .
C12 C 0.6454(3) 0.3325(3) 0.8296(2) 0.0094(7) Uani 1 1 d . . . . .
C22 C 0.2086(3) 0.4846(3) 0.5370(2) 0.0095(7) Uani 1 1 d . . . . .
C13 C 0.7432(3) 0.3725(3) 0.8113(2) 0.0135(7) Uani 1 1 d . . . . .
H13 H 0.8136 0.3299 0.8161 0.016 Uiso 1 1 calc R U . . .
C25 C 0.0359(3) 0.3177(3) 0.6311(2) 0.0113(7) Uani 1 1 d . . . . .
H25A H -0.0282 0.3024 0.6740 0.014 Uiso 1 1 calc R U . . .
H25B H 0.0203 0.3124 0.5811 0.014 Uiso 1 1 calc R U . . .
C16 C 0.5340(3) 0.4939(3) 0.7981(2) 0.0103(7) Uani 1 1 d . . . . .
H16 H 0.4630 0.5345 0.7930 0.012 Uiso 1 1 calc R U . . .
C18 C 0.5615(3) 0.3407(3) 0.4244(2) 0.0156(8) Uani 1 1 d . . . . .
H18 H 0.6384 0.3051 0.4004 0.019 Uiso 1 1 calc R U . . .
C5 C 0.2388(3) 0.3587(3) 1.0014(2) 0.0111(7) Uani 1 1 d . . . . .
C17 C 0.4920(3) 0.2941(3) 0.4863(2) 0.0112(7) Uani 1 1 d . . . . .
H17 H 0.5233 0.2265 0.5036 0.013 Uiso 1 1 calc R U . . .
C24 C 0.0493(3) 0.4300(3) 0.6408(2) 0.0125(7) Uani 1 1 d . . . . .
H24A H -0.0050 0.4838 0.6200 0.015 Uiso 1 1 calc R U . . .
H24B H 0.0364 0.4452 0.6962 0.015 Uiso 1 1 calc R U . . .
C9 C 0.5290(3) 0.0892(3) 0.8653(2) 0.0114(7) Uani 1 1 d . . . . .
H9A H 0.5684 0.0507 0.9027 0.014 Uiso 1 1 calc R U . . .
H9B H 0.5595 0.0501 0.8157 0.014 Uiso 1 1 calc R U . . .
C10 C 0.6462(3) 0.2181(3) 0.8459(2) 0.0094(7) Uani 1 1 d . . . . .
C28 C 0.2814(3) 0.0790(3) 0.6262(2) 0.0097(7) Uani 1 1 d . . . . .
C6 C 0.2666(3) 0.2423(3) 0.9924(2) 0.0120(7) Uani 1 1 d . . . . .
C26 C 0.1620(3) 0.1399(3) 0.6309(2) 0.0098(7) Uani 1 1 d . . . . .
O12 O 0.4144(5) 0.7051(3) 0.9888(2) 0.0545(13) Uani 1 1 d . . . . .
O10 O 0.5983(3) 0.7142(3) 0.8934(2) 0.0432(10) Uani 1 1 d . . . . .
C7 C 0.2085(4) 0.1747(3) 1.0552(3) 0.0218(9) Uani 1 1 d . . . . .
H7A H 0.2452 0.1009 1.0428 0.033 Uiso 1 1 calc R U . . .
H7B H 0.1278 0.1888 1.0577 0.033 Uiso 1 1 calc R U . . .
H7C H 0.2152 0.1907 1.1055 0.033 Uiso 1 1 calc R U . . .
C15 C 0.6295(3) 0.5384(3) 0.7765(2) 0.0154(7) Uani 1 1 d . . . . .
H15 H 0.6232 0.6074 0.7564 0.019 Uiso 1 1 calc R U . . .
C32 C 0.4657(3) 0.0958(3) 0.6206(2) 0.0126(7) Uani 1 1 d . . . . .
H32 H 0.5164 0.1391 0.6162 0.015 Uiso 1 1 calc R U . . .
C23 C 0.1430(3) 0.5851(3) 0.5094(2) 0.0154(7) Uani 1 1 d . . . . .
H23A H 0.0610 0.5914 0.5318 0.023 Uiso 1 1 calc R U . . .
H23B H 0.1623 0.5846 0.4525 0.023 Uiso 1 1 calc R U . . .
H23C H 0.1631 0.6445 0.5259 0.023 Uiso 1 1 calc R U . . .
C20 C 0.3997(3) 0.4913(3) 0.4345(2) 0.0132(7) Uani 1 1 d . . . . .
H20 H 0.3667 0.5584 0.4176 0.016 Uiso 1 1 calc R U . . .
C4 C 0.1459(3) 0.4149(3) 1.0601(2) 0.0188(8) Uani 1 1 d . . . . .
H4 H 0.0969 0.3795 1.0970 0.023 Uiso 1 1 calc R U . . .
C8 C 0.3968(3) 0.1000(3) 0.8985(2) 0.0145(7) Uani 1 1 d . . . . .
H8A H 0.3656 0.0862 0.8571 0.017 Uiso 1 1 calc R U . . .
H8B H 0.3807 0.0495 0.9415 0.017 Uiso 1 1 calc R U . . .
C11 C 0.7528(3) 0.1364(3) 0.8500(2) 0.0171(8) Uani 1 1 d . . . . .
H11A H 0.7427 0.1096 0.9034 0.026 Uiso 1 1 calc R U . . .
H11B H 0.8182 0.1679 0.8347 0.026 Uiso 1 1 calc R U . . .
H11C H 0.7666 0.0789 0.8146 0.026 Uiso 1 1 calc R U . . .
C14 C 0.7343(3) 0.4770(3) 0.7855(2) 0.0164(8) Uani 1 1 d . . . . .
H14 H 0.7984 0.5061 0.7744 0.020 Uiso 1 1 calc R U . . .
C30 C 0.4270(3) -0.0763(3) 0.6419(2) 0.0145(7) Uani 1 1 d . . . . .
H30 H 0.4509 -0.1494 0.6496 0.017 Uiso 1 1 calc R U . . .
C19 C 0.5155(3) 0.4409(3) 0.3985(2) 0.0160(8) Uani 1 1 d . . . . .
H19 H 0.5613 0.4742 0.3574 0.019 Uiso 1 1 calc R U . . .
C1 C 0.2950(4) 0.5145(3) 0.9520(2) 0.0176(8) Uani 1 1 d . . . . .
H1 H 0.3470 0.5481 0.9161 0.021 Uiso 1 1 calc R U . . .
C29 C 0.3134(3) -0.0298(3) 0.6395(2) 0.0124(7) Uani 1 1 d . . . . .
H29 H 0.2601 -0.0712 0.6466 0.015 Uiso 1 1 calc R U . . .
C36 C 0.1767(3) 0.2246(3) 0.3287(2) 0.0158(8) Uani 1 1 d . . . . .
C34 C 0.0341(3) 0.1003(3) 0.9102(2) 0.0168(8) Uani 1 1 d . . . . .
C35 C 0.8096(4) 0.1015(3) 0.5472(2) 0.0177(8) Uani 1 1 d . . . . .
C33 C 0.1206(4) 0.7440(3) 0.7922(2) 0.0172(8) Uani 1 1 d . . . . .
C27 C 0.0683(3) 0.0879(3) 0.6339(3) 0.0218(9) Uani 1 1 d . . . . .
H27A H -0.0007 0.1202 0.6747 0.033 Uiso 1 1 calc R U . . .
H27B H 0.0924 0.0133 0.6453 0.033 Uiso 1 1 calc R U . . .
H27C H 0.0522 0.0962 0.5835 0.033 Uiso 1 1 calc R U . . .
C37 C 0.4100(4) 0.8138(3) 0.8608(3) 0.0264(10) Uani 1 1 d . . . . .
C31 C 0.5033(3) -0.0124(3) 0.6328(2) 0.0136(7) Uani 1 1 d . . . . .
H31 H 0.5791 -0.0418 0.6348 0.016 Uiso 1 1 calc R U . . .
C2 C 0.2034(4) 0.5750(3) 1.0092(3) 0.0232(9) Uani 1 1 d . . . . .
H2 H 0.1936 0.6483 1.0114 0.028 Uiso 1 1 calc R U . . .
C3 C 0.1266(4) 0.5251(4) 1.0632(2) 0.0222(9) Uani 1 1 d . . . . .
H3 H 0.0628 0.5648 1.1011 0.027 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Au1 Ge1 2.3823(6) . ?
Au1 Ge2 2.3857(6) . ?
Ge1 N3 1.989(3) . ?
Ge1 N2 2.002(3) . ?
Ge1 N1 2.034(3) . ?
Ge1 N4 2.063(3) . ?
Ge2 N7 1.972(3) . ?
Ge2 N6 1.994(3) . ?
Ge2 N5 2.027(3) . ?
Ge2 N8 2.072(3) . ?
S3 O7 1.438(3) . ?
S3 O9 1.439(3) . ?
S3 O8 1.444(3) . ?
S3 C35 1.818(4) . ?
S2 O5 1.442(3) . ?
S2 O4 1.449(3) . ?
S2 O6 1.452(3) . ?
S2 C34 1.822(4) . ?
S1 O1 1.441(3) . ?
S1 O3 1.443(3) . ?
S1 O2 1.446(3) . ?
S1 C33 1.836(4) . ?
S5 O14 1.436(3) . ?
S5 O13 1.438(3) . ?
S5 O15 1.450(3) . ?
S5 C36 1.826(4) . ?
S4 O10 1.433(4) . ?
S4 O12 1.439(4) . ?
S4 O11 1.447(3) . ?
S4 C37 1.816(5) . ?
F5 C34 1.341(5) . ?
F4 C34 1.337(5) . ?
F7 C35 1.331(5) . ?
F1 C33 1.335(5) . ?
F9 C35 1.347(5) . ?
F11 C36 1.337(5) . ?
F6 C34 1.329(5) . ?
F10 C36 1.330(5) . ?
F15 C37 1.340(5) . ?
F2 C33 1.327(5) . ?
F12 C36 1.331(5) . ?
N6 C22 1.273(5) . ?
N6 C24 1.456(5) . ?
F3 C33 1.335(5) . ?
F8 C35 1.329(5) . ?
N2 C6 1.280(5) . ?
N2 C8 1.459(5) . ?
N5 C17 1.341(5) . ?
N5 C21 1.358(5) . ?
N3 C10 1.282(5) . ?
N3 C9 1.469(4) . ?
N7 C26 1.287(5) . ?
N7 C25 1.474(4) . ?
F14 C37 1.317(6) . ?
N4 C16 1.338(5) . ?
N4 C12 1.345(5) . ?
N8 C32 1.346(4) . ?
N8 C28 1.350(5) . ?
N1 C1 1.342(5) . ?
N1 C5 1.359(5) . ?
F13 C37 1.327(6) . ?
C21 C20 1.376(5) . ?
C21 C22 1.492(5) . ?
C12 C13 1.382(5) . ?
C12 C10 1.488(5) . ?
C22 C23 1.480(5) . ?
C13 C14 1.384(6) . ?
C13 H13 0.9300 . ?
C25 C24 1.537(5) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C16 C15 1.389(5) . ?
C16 H16 0.9300 . ?
C18 C17 1.379(5) . ?
C18 C19 1.380(6) . ?
C18 H18 0.9300 . ?
C5 C4 1.380(5) . ?
C5 C6 1.471(5) . ?
C17 H17 0.9300 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C9 C8 1.541(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.484(5) . ?
C28 C29 1.385(5) . ?
C28 C26 1.470(5) . ?
C6 C7 1.486(5) . ?
C26 C27 1.477(5) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C15 C14 1.387(6) . ?
C15 H15 0.9300 . ?
C32 C31 1.382(5) . ?
C32 H32 0.9300 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C20 C19 1.390(6) . ?
C20 H20 0.9300 . ?
C4 C3 1.391(6) . ?
C4 H4 0.9300 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C14 H14 0.9300 . ?
C30 C31 1.381(5) . ?
C30 C29 1.395(5) . ?
C30 H30 0.9300 . ?
C19 H19 0.9300 . ?
C1 C2 1.381(6) . ?
C1 H1 0.9300 . ?
C29 H29 0.9300 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C31 H31 0.9300 . ?
C2 C3 1.382(6) . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Ge1 Au1 Ge2 166.538(16) . . ?
N3 Ge1 N2 75.82(12) . . ?
N3 Ge1 N1 124.03(12) . . ?
N2 Ge1 N1 78.37(12) . . ?
N3 Ge1 N4 77.98(12) . . ?
N2 Ge1 N4 141.03(12) . . ?
N1 Ge1 N4 93.30(12) . . ?
N3 Ge1 Au1 118.64(8) . . ?
N2 Ge1 Au1 107.99(8) . . ?
N1 Ge1 Au1 116.32(9) . . ?
N4 Ge1 Au1 109.75(8) . . ?
N7 Ge2 N6 78.02(12) . . ?
N7 Ge2 N5 121.48(12) . . ?
N6 Ge2 N5 78.30(12) . . ?
N7 Ge2 N8 78.23(12) . . ?
N6 Ge2 N8 146.65(12) . . ?
N5 Ge2 N8 94.71(12) . . ?
N7 Ge2 Au1 123.73(9) . . ?
N6 Ge2 Au1 115.40(9) . . ?
N5 Ge2 Au1 114.79(8) . . ?
N8 Ge2 Au1 97.25(8) . . ?
O7 S3 O9 114.86(18) . . ?
O7 S3 O8 116.05(19) . . ?
O9 S3 O8 114.02(18) . . ?
O7 S3 C35 104.50(18) . . ?
O9 S3 C35 102.49(19) . . ?
O8 S3 C35 102.47(18) . . ?
O5 S2 O4 115.28(18) . . ?
O5 S2 O6 114.74(18) . . ?
O4 S2 O6 114.39(17) . . ?
O5 S2 C34 103.56(19) . . ?
O4 S2 C34 103.57(18) . . ?
O6 S2 C34 103.05(17) . . ?
O1 S1 O3 115.00(19) . . ?
O1 S1 O2 115.3(2) . . ?
O3 S1 O2 114.19(18) . . ?
O1 S1 C33 104.22(18) . . ?
O3 S1 C33 103.40(18) . . ?
O2 S1 C33 102.48(18) . . ?
O14 S5 O13 114.47(18) . . ?
O14 S5 O15 114.96(19) . . ?
O13 S5 O15 114.5(2) . . ?
O14 S5 C36 104.17(18) . . ?
O13 S5 C36 104.00(19) . . ?
O15 S5 C36 102.70(18) . . ?
O10 S4 O12 115.0(3) . . ?
O10 S4 O11 114.2(2) . . ?
O12 S4 O11 115.2(2) . . ?
O10 S4 C37 103.9(2) . . ?
O12 S4 C37 103.9(3) . . ?
O11 S4 C37 102.48(19) . . ?
C22 N6 C24 129.7(3) . . ?
C22 N6 Ge2 119.4(2) . . ?
C24 N6 Ge2 110.8(2) . . ?
C6 N2 C8 128.9(3) . . ?
C6 N2 Ge1 119.1(3) . . ?
C8 N2 Ge1 112.1(2) . . ?
C17 N5 C21 118.8(3) . . ?
C17 N5 Ge2 126.9(2) . . ?
C21 N5 Ge2 113.2(2) . . ?
C10 N3 C9 123.9(3) . . ?
C10 N3 Ge1 119.5(2) . . ?
C9 N3 Ge1 116.4(2) . . ?
C26 N7 C25 123.2(3) . . ?
C26 N7 Ge2 119.4(2) . . ?
C25 N7 Ge2 117.2(2) . . ?
C16 N4 C12 119.8(3) . . ?
C16 N4 Ge1 125.2(2) . . ?
C12 N4 Ge1 114.4(2) . . ?
C32 N8 C28 119.4(3) . . ?
C32 N8 Ge2 124.1(2) . . ?
C28 N8 Ge2 113.4(2) . . ?
C1 N1 C5 119.0(3) . . ?
C1 N1 Ge1 126.7(3) . . ?
C5 N1 Ge1 112.8(2) . . ?
N5 C21 C20 121.7(3) . . ?
N5 C21 C22 114.3(3) . . ?
C20 C21 C22 124.0(3) . . ?
N4 C12 C13 121.4(3) . . ?
N4 C12 C10 113.9(3) . . ?
C13 C12 C10 124.4(3) . . ?
N6 C22 C23 127.0(3) . . ?
N6 C22 C21 112.4(3) . . ?
C23 C22 C21 120.6(3) . . ?
C12 C13 C14 118.7(3) . . ?
C12 C13 H13 120.6 . . ?
C14 C13 H13 120.6 . . ?
N7 C25 C24 107.1(3) . . ?
N7 C25 H25A 110.3 . . ?
C24 C25 H25A 110.3 . . ?
N7 C25 H25B 110.3 . . ?
C24 C25 H25B 110.3 . . ?
H25A C25 H25B 108.5 . . ?
N4 C16 C15 121.7(3) . . ?
N4 C16 H16 119.2 . . ?
C15 C16 H16 119.2 . . ?
C17 C18 C19 119.1(4) . . ?
C17 C18 H18 120.4 . . ?
C19 C18 H18 120.4 . . ?
N1 C5 C4 121.5(4) . . ?
N1 C5 C6 115.0(3) . . ?
C4 C5 C6 123.5(4) . . ?
N5 C17 C18 122.2(3) . . ?
N5 C17 H17 118.9 . . ?
C18 C17 H17 118.9 . . ?
N6 C24 C25 103.7(3) . . ?
N6 C24 H24A 111.0 . . ?
C25 C24 H24A 111.0 . . ?
N6 C24 H24B 111.0 . . ?
C25 C24 H24B 111.0 . . ?
H24A C24 H24B 109.0 . . ?
N3 C9 C8 108.2(3) . . ?
N3 C9 H9A 110.1 . . ?
C8 C9 H9A 110.1 . . ?
N3 C9 H9B 110.1 . . ?
C8 C9 H9B 110.1 . . ?
H9A C9 H9B 108.4 . . ?
N3 C10 C11 123.9(3) . . ?
N3 C10 C12 113.8(3) . . ?
C11 C10 C12 122.3(3) . . ?
N8 C28 C29 121.4(3) . . ?
N8 C28 C26 113.8(3) . . ?
C29 C28 C26 124.5(3) . . ?
N2 C6 C5 112.8(3) . . ?
N2 C6 C7 126.1(4) . . ?
C5 C6 C7 121.1(3) . . ?
N7 C26 C28 114.4(3) . . ?
N7 C26 C27 123.1(3) . . ?
C28 C26 C27 122.4(3) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C14 C15 C16 118.3(4) . . ?
C14 C15 H15 120.9 . . ?
C16 C15 H15 120.9 . . ?
N8 C32 C31 121.8(3) . . ?
N8 C32 H32 119.1 . . ?
C31 C32 H32 119.1 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C20 C19 119.1(4) . . ?
C21 C20 H20 120.4 . . ?
C19 C20 H20 120.4 . . ?
C5 C4 C3 119.1(4) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
N2 C8 C9 106.6(3) . . ?
N2 C8 H8A 110.4 . . ?
C9 C8 H8A 110.4 . . ?
N2 C8 H8B 110.4 . . ?
C9 C8 H8B 110.4 . . ?
H8A C8 H8B 108.6 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C14 C15 119.8(4) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
C31 C30 C29 119.2(3) . . ?
C31 C30 H30 120.4 . . ?
C29 C30 H30 120.4 . . ?
C18 C19 C20 119.1(4) . . ?
C18 C19 H19 120.5 . . ?
C20 C19 H19 120.5 . . ?
N1 C1 C2 122.1(4) . . ?
N1 C1 H1 119.0 . . ?
C2 C1 H1 119.0 . . ?
C28 C29 C30 118.9(3) . . ?
C28 C29 H29 120.6 . . ?
C30 C29 H29 120.6 . . ?
F10 C36 F12 107.8(3) . . ?
F10 C36 F11 107.8(3) . . ?
F12 C36 F11 107.6(3) . . ?
F10 C36 S5 111.9(3) . . ?
F12 C36 S5 110.8(3) . . ?
F11 C36 S5 110.8(3) . . ?
F6 C34 F4 107.7(3) . . ?
F6 C34 F5 107.8(3) . . ?
F4 C34 F5 107.5(3) . . ?
F6 C34 S2 112.0(3) . . ?
F4 C34 S2 111.0(3) . . ?
F5 C34 S2 110.6(3) . . ?
F8 C35 F7 107.4(3) . . ?
F8 C35 F9 107.5(4) . . ?
F7 C35 F9 106.6(3) . . ?
F8 C35 S3 112.4(3) . . ?
F7 C35 S3 112.4(3) . . ?
F9 C35 S3 110.2(3) . . ?
F2 C33 F3 108.4(3) . . ?
F2 C33 F1 107.7(3) . . ?
F3 C33 F1 107.5(3) . . ?
F2 C33 S1 111.4(3) . . ?
F3 C33 S1 110.5(3) . . ?
F1 C33 S1 111.1(3) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
F14 C37 F13 107.8(4) . . ?
F14 C37 F15 108.1(4) . . ?
F13 C37 F15 107.5(4) . . ?
F14 C37 S4 111.1(3) . . ?
F13 C37 S4 110.4(4) . . ?
F15 C37 S4 111.8(3) . . ?
C30 C31 C32 119.2(3) . . ?
C30 C31 H31 120.4 . . ?
C32 C31 H31 120.4 . . ?
C1 C2 C3 119.2(4) . . ?
C1 C2 H2 120.4 . . ?
C3 C2 H2 120.4 . . ?
C2 C3 C4 119.0(4) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?

_refine_diff_density_max         1.402
_refine_diff_density_min         -1.968
_refine_diff_density_rms         0.178

####################################################################### 
# 
# 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_CompoundLGeClGeCl3
_database_code_depnum_ccdc_archive 'CCDC 1510945'
_audit_update_record             
;
2016-11-28 deposited with the CCDC.
2017-01-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H18 Cl Ge N4, Cl3 Ge'
_chemical_formula_sum            'C16 H18 Cl4 Ge2 N4'
_chemical_formula_weight         553.32

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'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   8.872(3)
_cell_length_b                   10.214(4)
_cell_length_c                   12.585(5)
_cell_angle_alpha                90.296(7)
_cell_angle_beta                 93.135(8)
_cell_angle_gamma                107.603(7)
_cell_volume                     1085.1(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8548
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      27.86

_exptl_crystal_description       'needle shape'
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.25
_exptl_absorpt_coefficient_mu    3.271
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.300
_exptl_absorpt_correction_T_max  0.340
_exptl_absorpt_process_details   'SADABS;Universitat Gottingen,1997'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focused sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21205
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.621
_diffrn_reflns_theta_max         29.140
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5806
_reflns_number_gt                4506
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0423P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5806
_refine_ls_number_parameters     237
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0340
_refine_ls_wR_factor_ref         0.0949
_refine_ls_wR_factor_gt          0.0884
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.41685(3) 0.49036(2) 0.33619(2) 0.04407(8) Uani 1 1 d . . . . .
Ge2 Ge 0.11426(3) 0.08002(2) 0.17679(2) 0.05418(9) Uani 1 1 d . . . . .
Cl1 Cl 0.19332(7) 0.43419(6) 0.22632(5) 0.05232(14) Uani 1 1 d . . . . .
Cl2 Cl -0.11743(8) 0.03044(7) 0.26341(7) 0.0706(2) Uani 1 1 d . . . . .
Cl3 Cl 0.27277(9) 0.07264(7) 0.32999(6) 0.0726(2) Uani 1 1 d . . . . .
Cl4 Cl 0.09033(9) -0.14327(7) 0.12130(7) 0.0805(2) Uani 1 1 d . . . . .
N2 N 0.3773(2) 0.67257(16) 0.40444(15) 0.0447(4) Uani 1 1 d . . . . .
N1 N 0.5175(2) 0.65356(17) 0.21992(15) 0.0465(4) Uani 1 1 d . . . . .
N3 N 0.2284(2) 0.42972(18) 0.47637(15) 0.0466(4) Uani 1 1 d . . . . .
N4 N 0.5608(2) 0.4079(2) 0.18121(15) 0.0504(4) Uani 1 1 d . . . . .
C7 C 0.2173(2) 0.5389(2) 0.53264(16) 0.0418(5) Uani 1 1 d . . . . .
C5 C 0.3037(2) 0.6741(2) 0.48933(18) 0.0446(5) Uani 1 1 d . . . . .
C12 C 0.6409(2) 0.5151(2) 0.12552(17) 0.0468(5) Uani 1 1 d . . . . .
C3 C 0.5989(3) 0.6447(2) 0.13970(18) 0.0457(5) Uani 1 1 d . . . . .
C8 C 0.1311(3) 0.5230(3) 0.62341(18) 0.0525(5) Uani 1 1 d . . . . .
H8 H 0.1220 0.5994 0.6598 0.063 Uiso 1 1 calc R U . . .
C11 C 0.1567(3) 0.3032(2) 0.5106(2) 0.0584(6) Uani 1 1 d . . . . .
H11 H 0.1631 0.2276 0.4717 0.070 Uiso 1 1 calc R U . . .
C1 C 0.4705(3) 0.8000(2) 0.3578(2) 0.0577(6) Uani 1 1 d . . . . .
H1A H 0.5782 0.8268 0.3891 0.069 Uiso 1 1 calc R U . . .
H1B H 0.4250 0.8730 0.3723 0.069 Uiso 1 1 calc R U . . .
C9 C 0.0600(3) 0.3933(3) 0.6585(2) 0.0609(6) Uani 1 1 d . . . . .
H9 H 0.0033 0.3809 0.7196 0.073 Uiso 1 1 calc R U . . .
C2 C 0.4712(3) 0.7780(2) 0.2392(2) 0.0586(6) Uani 1 1 d . . . . .
H2A H 0.3666 0.7671 0.2061 0.070 Uiso 1 1 calc R U . . .
H2B H 0.5456 0.8567 0.2086 0.070 Uiso 1 1 calc R U . . .
C13 C 0.7575(3) 0.5070(3) 0.0579(2) 0.0655(7) Uani 1 1 d . . . . .
H13 H 0.8106 0.5827 0.0192 0.079 Uiso 1 1 calc R U . . .
C16 C 0.5965(3) 0.2897(3) 0.1730(2) 0.0597(6) Uani 1 1 d . . . . .
H16 H 0.5415 0.2153 0.2121 0.072 Uiso 1 1 calc R U . . .
C10 C 0.0731(3) 0.2815(3) 0.6025(2) 0.0631(7) Uani 1 1 d . . . . .
H10 H 0.0269 0.1929 0.6258 0.076 Uiso 1 1 calc R U . . .
C6 C 0.3057(3) 0.8046(3) 0.5463(2) 0.0626(7) Uani 1 1 d . . . . .
H6A H 0.4086 0.8460 0.5809 0.094 Uiso 1 1 calc R U . . .
H6B H 0.2274 0.7839 0.5985 0.094 Uiso 1 1 calc R U . . .
H6C H 0.2826 0.8670 0.4959 0.094 Uiso 1 1 calc R U . . .
C15 C 0.7128(3) 0.2741(3) 0.1079(2) 0.0678(7) Uani 1 1 d . . . . .
H15 H 0.7355 0.1911 0.1042 0.081 Uiso 1 1 calc R U . . .
C4 C 0.6535(3) 0.7572(3) 0.0616(2) 0.0646(7) Uani 1 1 d . . . . .
H4A H 0.5780 0.8074 0.0545 0.097 Uiso 1 1 calc R U . . .
H4B H 0.6627 0.7179 -0.0063 0.097 Uiso 1 1 calc R U . . .
H4C H 0.7547 0.8182 0.0865 0.097 Uiso 1 1 calc R U . . .
C14 C 0.7930(3) 0.3843(3) 0.0496(3) 0.0767(9) Uani 1 1 d . . . . .
H14 H 0.8702 0.3765 0.0050 0.092 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 N2 2.1764(16) . ?
Ge1 N1 2.2327(19) . ?
Ge1 Cl1 2.2754(9) . ?
Ge2 Cl2 2.3001(10) . ?
Ge2 Cl4 2.3257(10) . ?
Ge2 Cl3 2.3386(10) . ?
N2 C5 1.285(3) . ?
N2 C1 1.460(3) . ?
N1 C3 1.291(3) . ?
N1 C2 1.472(3) . ?
N3 C11 1.341(3) . ?
N3 C7 1.350(2) . ?
N4 C12 1.337(3) . ?
N4 C16 1.342(3) . ?
C7 C8 1.392(3) . ?
C7 C5 1.484(3) . ?
C5 C6 1.505(3) . ?
C12 C13 1.396(3) . ?
C12 C3 1.491(3) . ?
C3 C4 1.499(3) . ?
C8 C9 1.371(4) . ?
C8 H8 0.9300 . ?
C11 C10 1.390(4) . ?
C11 H11 0.9300 . ?
C1 C2 1.510(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C9 C10 1.377(4) . ?
C9 H9 0.9300 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C13 C14 1.387(4) . ?
C13 H13 0.9300 . ?
C16 C15 1.397(4) . ?
C16 H16 0.9300 . ?
C10 H10 0.9300 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C15 C14 1.376(4) . ?
C15 H15 0.9300 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C14 H14 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ge1 N1 76.39(7) . . ?
N2 Ge1 Cl1 94.88(5) . . ?
N1 Ge1 Cl1 85.86(5) . . ?
Cl2 Ge2 Cl4 97.25(3) . . ?
Cl2 Ge2 Cl3 94.74(4) . . ?
Cl4 Ge2 Cl3 94.31(3) . . ?
C5 N2 C1 121.13(18) . . ?
C5 N2 Ge1 124.54(15) . . ?
C1 N2 Ge1 113.19(13) . . ?
C3 N1 C2 120.73(19) . . ?
C3 N1 Ge1 127.28(15) . . ?
C2 N1 Ge1 111.86(14) . . ?
C11 N3 C7 118.7(2) . . ?
C12 N4 C16 118.5(2) . . ?
N3 C7 C8 121.6(2) . . ?
N3 C7 C5 114.36(18) . . ?
C8 C7 C5 124.01(19) . . ?
N2 C5 C7 116.96(17) . . ?
N2 C5 C6 123.1(2) . . ?
C7 C5 C6 120.0(2) . . ?
N4 C12 C13 122.2(2) . . ?
N4 C12 C3 116.23(18) . . ?
C13 C12 C3 121.6(2) . . ?
N1 C3 C12 117.5(2) . . ?
N1 C3 C4 123.6(2) . . ?
C12 C3 C4 118.9(2) . . ?
C9 C8 C7 119.2(2) . . ?
C9 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
N3 C11 C10 122.1(2) . . ?
N3 C11 H11 119.0 . . ?
C10 C11 H11 119.0 . . ?
N2 C1 C2 109.00(18) . . ?
N2 C1 H1A 109.9 . . ?
C2 C1 H1A 109.9 . . ?
N2 C1 H1B 109.9 . . ?
C2 C1 H1B 109.9 . . ?
H1A C1 H1B 108.3 . . ?
C8 C9 C10 119.4(2) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
N1 C2 C1 108.48(19) . . ?
N1 C2 H2A 110.0 . . ?
C1 C2 H2A 110.0 . . ?
N1 C2 H2B 110.0 . . ?
C1 C2 H2B 110.0 . . ?
H2A C2 H2B 108.4 . . ?
C14 C13 C12 118.9(3) . . ?
C14 C13 H13 120.6 . . ?
C12 C13 H13 120.6 . . ?
N4 C16 C15 122.6(3) . . ?
N4 C16 H16 118.7 . . ?
C15 C16 H16 118.7 . . ?
C9 C10 C11 119.0(2) . . ?
C9 C10 H10 120.5 . . ?
C11 C10 H10 120.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C14 C15 C16 118.5(2) . . ?
C14 C15 H15 120.8 . . ?
C16 C15 H15 120.8 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C15 C14 C13 119.3(2) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?

_refine_diff_density_max         0.390
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.081

####################################################################### 
# 
# 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_Compound2
_database_code_depnum_ccdc_archive 'CCDC 1510946'
_audit_update_record             
;
2016-11-28 deposited with the CCDC.
2017-01-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        Compound2
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H39 Ag F15 Ge2 N9 O15 S5'
_chemical_formula_sum            'C39 H39 Ag F15 Ge2 N9 O15 S5'
_chemical_formula_weight         1572.14

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   14.699(2)
_cell_length_b                   15.176(3)
_cell_length_c                   15.433(3)
_cell_angle_alpha                112.989(6)
_cell_angle_beta                 103.063(6)
_cell_angle_gamma                106.078(6)
_cell_volume                     2819.6(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9931
_cell_measurement_theta_min      3.36
_cell_measurement_theta_max      73.14

_exptl_crystal_description       needles
_exptl_crystal_colour            'Pale Yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.852
_exptl_crystal_F_000             1564
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_exptl_absorpt_coefficient_mu    6.848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.174
_exptl_absorpt_correction_T_max  0.222
_exptl_absorpt_process_details   'SADABS;Universitat Gottingen,1997'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'D8 Venture APEX-II'
_diffrn_measurement_method       'CMOS-Photon 100'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24387
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.360
_diffrn_reflns_theta_max         73.391
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measured_fraction_theta_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_point_group_measured_fraction_full 0.976
_reflns_number_total             10814
_reflns_number_gt                9416
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0369P)²+28.8312P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10814
_refine_ls_number_parameters     780
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0571
_refine_ls_wR_factor_ref         0.1417
_refine_ls_wR_factor_gt          0.1360
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag 0.73993(3) 0.65826(3) 0.35045(3) 0.01358(11) Uani 1 1 d . . . . .
Ge1 Ge 0.91132(4) 0.67099(4) 0.33673(4) 0.00894(13) Uani 1 1 d . . . . .
Ge2 Ge 0.58536(4) 0.70258(4) 0.34732(4) 0.00900(13) Uani 1 1 d . . . . .
S1 S 0.65943(10) 0.40118(10) 0.25323(9) 0.0135(3) Uani 1 1 d . . . . .
S2 S 0.80846(10) 0.77509(10) 0.60593(10) 0.0140(3) Uani 1 1 d . . . . .
S3 S 0.23677(10) 0.17627(11) 0.78129(10) 0.0159(3) Uani 1 1 d . . . . .
S5 S 0.17848(11) 0.78049(11) 0.99359(10) 0.0177(3) Uani 1 1 d . . . . .
S4 S 0.29696(11) 0.79320(12) 0.41288(14) 0.0313(4) Uani 1 1 d . . . . .
F2 F 0.8987(3) 0.7504(3) 0.7564(3) 0.0232(7) Uani 1 1 d . . . . .
F7 F 0.2953(3) 0.6339(3) 0.2591(3) 0.0315(9) Uani 1 1 d . . . . .
F12 F 0.1780(3) 0.0110(3) 0.8047(3) 0.0357(9) Uani 1 1 d . . . . .
F3 F 0.9288(4) 0.9107(3) 0.7956(3) 0.0439(12) Uani 1 1 d . . . . .
F1 F 1.0014(3) 0.8295(4) 0.7061(3) 0.0391(10) Uani 1 1 d . . . . .
F4 F 0.4960(4) 0.2348(3) 0.1950(3) 0.0507(13) Uani 1 1 d . . . . .
O5 O 0.6078(3) 0.4637(3) 0.2992(3) 0.0222(9) Uani 1 1 d . . . . .
F10 F 0.3067(3) 0.1426(3) 0.9320(3) 0.0410(11) Uani 1 1 d . . . . .
O2 O 0.8319(3) 0.8612(3) 0.5844(3) 0.0215(9) Uani 1 1 d . . . . .
O8 O 0.3355(3) 0.2596(3) 0.8200(3) 0.0262(10) Uani 1 1 d . . . . .
O1 O 0.8136(4) 0.6827(3) 0.5345(3) 0.0242(9) Uani 1 1 d . . . . .
F5 F 0.4958(3) 0.2925(4) 0.0876(3) 0.0468(12) Uani 1 1 d . . . . .
O6 O 0.7087(3) 0.4392(3) 0.1961(3) 0.0244(9) Uani 1 1 d . . . . .
N3 N 1.0216(3) 0.7615(3) 0.4819(3) 0.0138(9) Uani 1 1 d . . . . .
N7 N 0.6043(3) 0.8194(3) 0.4823(3) 0.0119(9) Uani 1 1 d . . . . .
N8 N 0.4858(3) 0.6272(3) 0.3957(3) 0.0101(8) Uani 1 1 d . . . . .
N2 N 1.0029(3) 0.8003(3) 0.3412(3) 0.0116(9) Uani 1 1 d . . . . .
N5 N 0.4789(3) 0.6095(3) 0.1965(3) 0.0119(9) Uani 1 1 d . . . . .
F11 F 0.3253(4) 0.0515(4) 0.7942(4) 0.0498(12) Uani 1 1 d . . . . .
F6 F 0.5871(4) 0.2085(3) 0.1056(3) 0.0455(12) Uani 1 1 d . . . . .
N4 N 0.9776(3) 0.5728(3) 0.3580(3) 0.0119(9) Uani 1 1 d . . . . .
O11 O 0.2204(3) 0.8287(4) 0.4300(4) 0.0291(10) Uani 1 1 d . . . . .
O7 O 0.1947(4) 0.1093(4) 0.6732(3) 0.0349(12) Uani 1 1 d . . . . .
N1 N 0.9178(3) 0.6154(3) 0.1894(3) 0.0099(8) Uani 1 1 d . . . . .
O4 O 0.7177(4) 0.3732(4) 0.3177(4) 0.0348(12) Uani 1 1 d . . . . .
N6 N 0.5484(3) 0.8073(4) 0.3129(3) 0.0132(9) Uani 1 1 d . . . . .
O13 O 0.2380(4) 0.7217(4) 0.9664(4) 0.0392(12) Uani 1 1 d . . . . .
O9 O 0.1677(4) 0.2075(4) 0.8260(4) 0.0314(11) Uani 1 1 d . . . . .
O3 O 0.7211(3) 0.7541(4) 0.6335(4) 0.0319(11) Uani 1 1 d . . . . .
O12 O 0.2014(4) 0.8350(5) 1.1004(4) 0.0499(16) Uani 1 1 d . . . . .
O14 O 0.0716(4) 0.7294(5) 0.9309(4) 0.0445(15) Uani 1 1 d . . . . .
F8 F 0.1476(4) 0.6150(4) 0.2705(5) 0.084(2) Uani 1 1 d . . . . .
C28 C 0.4470(4) 0.6635(4) 0.1527(4) 0.0128(10) Uani 1 1 d . . . . .
C17 C 0.4223(4) 0.5253(4) 0.3443(4) 0.0143(11) Uani 1 1 d . . . . .
H17 H 0.4124 0.4863 0.2765 0.017 Uiso 1 1 calc R U . . .
C10 C 1.0817(4) 0.7267(5) 0.5170(4) 0.0154(11) Uani 1 1 d . . . . .
C26 C 0.4832(4) 0.7765(4) 0.2246(4) 0.0132(10) Uani 1 1 d . . . . .
C19 C 0.3871(4) 0.5336(5) 0.4896(4) 0.0184(12) Uani 1 1 d . . . . .
H19 H 0.3547 0.5019 0.5216 0.022 Uiso 1 1 calc R U . . .
C18 C 0.3713(4) 0.4765(4) 0.3890(4) 0.0169(11) Uani 1 1 d . . . . .
H18 H 0.3268 0.4060 0.3515 0.020 Uiso 1 1 calc R U . . .
C16 C 0.9456(5) 0.4702(4) 0.2929(4) 0.0191(12) Uani 1 1 d . . . . .
H16 H 0.8893 0.4387 0.2326 0.023 Uiso 1 1 calc R U . . .
F13 F 0.2125(5) 0.8441(6) 0.8648(5) 0.0733(18) Uani 1 1 d . . . . .
F15 F 0.3256(5) 0.9427(4) 1.0183(5) 0.079(2) Uani 1 1 d . . . . .
C21 C 0.5003(4) 0.6842(4) 0.4945(4) 0.0107(10) Uani 1 1 d . . . . .
C25 C 0.5933(4) 0.9173(4) 0.3954(4) 0.0155(11) Uani 1 1 d . . . . .
H25A H 0.5396 0.9401 0.4070 0.019 Uiso 1 1 calc R U . . .
H25B H 0.6359 0.9630 0.3773 0.019 Uiso 1 1 calc R U . . .
C5 C 0.9719(4) 0.6914(4) 0.1735(4) 0.0129(10) Uani 1 1 d . . . . .
C32 C 0.4601(4) 0.5086(4) 0.1385(4) 0.0135(10) Uani 1 1 d . . . . .
H32 H 0.4862 0.4734 0.1681 0.016 Uiso 1 1 calc R U . . .
C4 C 0.9771(4) 0.6735(4) 0.0808(4) 0.0158(11) Uani 1 1 d . . . . .
H4 H 1.0149 0.7277 0.0724 0.019 Uiso 1 1 calc R U . . .
C1 C 0.8641(4) 0.5183(4) 0.1097(4) 0.0127(10) Uani 1 1 d . . . . .
H1 H 0.8241 0.4658 0.1187 0.015 Uiso 1 1 calc R U . . .
C24 C 0.6575(4) 0.9212(4) 0.4913(4) 0.0170(11) Uani 1 1 d . . . . .
H24A H 0.7265 0.9316 0.4939 0.020 Uiso 1 1 calc R U . . .
H24B H 0.6610 0.9775 0.5520 0.020 Uiso 1 1 calc R U . . .
C30 C 0.3688(4) 0.5107(5) -0.0097(4) 0.0202(12) Uani 1 1 d . . . . .
H30 H 0.3314 0.4770 -0.0793 0.024 Uiso 1 1 calc R U . . .
C6 C 1.0222(4) 0.7974(4) 0.2647(4) 0.0128(10) Uani 1 1 d . . . . .
C12 C 1.0563(4) 0.6157(4) 0.4490(4) 0.0156(11) Uani 1 1 d . . . . .
C3 C 0.9241(4) 0.5720(5) -0.0002(4) 0.0175(11) Uani 1 1 d . . . . .
H3 H 0.9271 0.5565 -0.0638 0.021 Uiso 1 1 calc R U . . .
C2 C 0.8672(4) 0.4950(4) 0.0152(4) 0.0161(11) Uani 1 1 d . . . . .
H2 H 0.8307 0.4269 -0.0385 0.019 Uiso 1 1 calc R U . . .
C22 C 0.5653(4) 0.7980(4) 0.5407(4) 0.0145(11) Uani 1 1 d . . . . .
C7 C 1.0861(5) 0.8889(4) 0.2594(4) 0.0198(12) Uani 1 1 d . . . . .
H7A H 1.0441 0.9013 0.2120 0.030 Uiso 1 1 calc R U . . .
H7B H 1.1390 0.8745 0.2375 0.030 Uiso 1 1 calc R U . . .
H7C H 1.1165 0.9498 0.3254 0.030 Uiso 1 1 calc R U . . .
C8 C 1.0457(5) 0.8984(4) 0.4383(4) 0.0180(12) Uani 1 1 d . . . . .
H8A H 1.0106 0.9427 0.4332 0.022 Uiso 1 1 calc R U . . .
H8B H 1.1178 0.9362 0.4552 0.022 Uiso 1 1 calc R U . . .
C20 C 0.4527(4) 0.6401(4) 0.5433(4) 0.0158(11) Uani 1 1 d . . . . .
H20 H 0.4639 0.6803 0.6112 0.019 Uiso 1 1 calc R U . . .
C15 C 0.9945(5) 0.4097(5) 0.3132(5) 0.0239(13) Uani 1 1 d . . . . .
H15 H 0.9720 0.3394 0.2664 0.029 Uiso 1 1 calc R U . . .
C31 C 0.4022(4) 0.4563(5) 0.0352(4) 0.0187(12) Uani 1 1 d . . . . .
H31 H 0.3858 0.3854 -0.0036 0.022 Uiso 1 1 calc R U . . .
C29 C 0.3919(4) 0.6164(5) 0.0502(4) 0.0189(12) Uani 1 1 d . . . . .
H29 H 0.3704 0.6543 0.0214 0.023 Uiso 1 1 calc R U . . .
C34 C 0.5549(5) 0.2768(5) 0.1558(5) 0.0236(13) Uani 1 1 d . . . . .
F9 F 0.2095(6) 0.7143(6) 0.2221(4) 0.086(2) Uani 1 1 d . . . . .
C11 C 1.1709(5) 0.7862(5) 0.6161(4) 0.0249(13) Uani 1 1 d . . . . .
H11A H 1.1753 0.8560 0.6524 0.037 Uiso 1 1 calc R U . . .
H11B H 1.2326 0.7893 0.6038 0.037 Uiso 1 1 calc R U . . .
H11C H 1.1621 0.7514 0.6559 0.037 Uiso 1 1 calc R U . . .
C13 C 1.1066(5) 0.5587(5) 0.4725(4) 0.0206(12) Uani 1 1 d . . . . .
H13 H 1.1605 0.5901 0.5346 0.025 Uiso 1 1 calc R U . . .
C27 C 0.4464(5) 0.8445(5) 0.1914(5) 0.0233(13) Uani 1 1 d . . . . .
H27A H 0.4825 0.9161 0.2444 0.035 Uiso 1 1 calc R U . . .
H27B H 0.3745 0.8231 0.1773 0.035 Uiso 1 1 calc R U . . .
H27C H 0.4586 0.8380 0.1311 0.035 Uiso 1 1 calc R U . . .
C9 C 1.0314(5) 0.8695(4) 0.5207(4) 0.0212(13) Uani 1 1 d . . . . .
H9A H 1.0899 0.9156 0.5843 0.025 Uiso 1 1 calc R U . . .
H9B H 0.9704 0.8750 0.5320 0.025 Uiso 1 1 calc R U . . .
C33 C 0.9147(5) 0.8196(4) 0.7228(4) 0.0190(12) Uani 1 1 d . . . . .
C14 C 1.0764(5) 0.4551(5) 0.4033(5) 0.0259(14) Uani 1 1 d . . . . .
H14 H 1.1110 0.4164 0.4172 0.031 Uiso 1 1 calc R U . . .
C36 C 0.2632(5) 0.0912(5) 0.8312(5) 0.0231(13) Uani 1 1 d . . . . .
C37 C 0.2358(5) 0.6781(6) 0.2912(5) 0.0329(17) Uani 1 1 d . . . . .
C23 C 0.5761(5) 0.8735(5) 0.6432(4) 0.0237(13) Uani 1 1 d . . . . .
H23A H 0.6204 0.9429 0.6611 0.036 Uiso 1 1 calc R U . . .
H23B H 0.6047 0.8546 0.6922 0.036 Uiso 1 1 calc R U . . .
H23C H 0.5101 0.8716 0.6426 0.036 Uiso 1 1 calc R U . . .
C38 C 0.1074(5) 0.1574(5) 0.0135(5) 0.0302(15) Uani 1 1 d . . . . .
H38A H 0.0474 0.1635 0.0251 0.045 Uiso 1 1 calc R U . . .
H38B H 0.1194 0.1045 0.0276 0.045 Uiso 1 1 calc R U . . .
H38C H 0.0974 0.1382 -0.0562 0.045 Uiso 1 1 calc R U . . .
C39 C 0.1940(6) 0.2561(6) 0.0791(5) 0.0400(19) Uani 1 1 d . . . . .
O10 O 0.3219(8) 0.7460(7) 0.4782(5) 0.093(3) Uani 1 1 d . . . . .
F14 F 0.1787(7) 0.9468(6) 0.9808(8) 0.117(3) Uani 1 1 d . . . . .
N9 N 0.2616(7) 0.3352(7) 0.1303(6) 0.078(3) Uani 1 1 d . . . . .
C35 C 0.2258(8) 0.8840(7) 0.9631(8) 0.051(2) Uani 1 1 d . . . . .
O15 O 0.3836(6) 0.8564(5) 0.4125(8) 0.110(4) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 Ge1 2.5362(8) . ?
Ag1 Ge2 2.5376(8) . ?
Ge1 N2 2.014(5) . ?
Ge1 N3 2.063(4) . ?
Ge1 N4 2.078(4) . ?
Ge1 N1 2.130(4) . ?
Ge2 N6 2.027(5) . ?
Ge2 N7 2.035(4) . ?
Ge2 N8 2.060(4) . ?
Ge2 N5 2.103(4) . ?
S1 O4 1.431(4) . ?
S1 O5 1.448(4) . ?
S1 O6 1.445(4) . ?
S1 C34 1.821(6) . ?
S2 O3 1.434(5) . ?
S2 O1 1.441(4) . ?
S2 O2 1.441(4) . ?
S2 C33 1.827(6) . ?
S3 O9 1.435(5) . ?
S3 O8 1.436(4) . ?
S3 O7 1.435(4) . ?
S3 C36 1.825(7) . ?
S5 O13 1.429(5) . ?
S5 O12 1.430(5) . ?
S5 O14 1.434(5) . ?
S5 C35 1.815(8) . ?
S4 O15 1.369(7) . ?
S4 O11 1.409(5) . ?
S4 O10 1.485(7) . ?
S4 C37 1.787(7) . ?
F2 C33 1.331(7) . ?
F7 C37 1.310(8) . ?
F12 C36 1.325(8) . ?
F3 C33 1.319(7) . ?
F1 C33 1.336(7) . ?
F4 C34 1.325(7) . ?
F10 C36 1.328(7) . ?
F5 C34 1.346(8) . ?
N3 C10 1.272(7) . ?
N3 C9 1.459(7) . ?
N7 C22 1.267(7) . ?
N7 C24 1.460(7) . ?
N8 C17 1.341(7) . ?
N8 C21 1.356(7) . ?
N2 C6 1.262(7) . ?
N2 C8 1.473(7) . ?
N5 C32 1.343(7) . ?
N5 C28 1.360(7) . ?
F11 C36 1.339(8) . ?
F6 C34 1.308(8) . ?
N4 C16 1.348(7) . ?
N4 C12 1.367(7) . ?
N1 C1 1.345(7) . ?
N1 C5 1.351(7) . ?
N6 C26 1.289(7) . ?
N6 C25 1.481(7) . ?
F8 C37 1.260(8) . ?
C28 C29 1.374(8) . ?
C28 C26 1.482(8) . ?
C17 C18 1.383(8) . ?
C17 H17 0.9300 . ?
C10 C12 1.474(8) . ?
C10 C11 1.494(7) . ?
C26 C27 1.488(7) . ?
C19 C18 1.375(8) . ?
C19 C20 1.399(8) . ?
C19 H19 0.9300 . ?
C18 H18 0.9300 . ?
C16 C15 1.394(8) . ?
C16 H16 0.9300 . ?
F13 C35 1.337(11) . ?
F15 C35 1.337(12) . ?
C21 C20 1.371(8) . ?
C21 C22 1.490(7) . ?
C25 C24 1.534(8) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C5 C4 1.371(8) . ?
C5 C6 1.489(7) . ?
C32 C31 1.386(7) . ?
C32 H32 0.9300 . ?
C4 C3 1.390(8) . ?
C4 H4 0.9300 . ?
C1 C2 1.375(8) . ?
C1 H1 0.9300 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C30 C31 1.386(9) . ?
C30 C29 1.393(9) . ?
C30 H30 0.9300 . ?
C6 C7 1.490(7) . ?
C12 C13 1.379(8) . ?
C3 C2 1.374(8) . ?
C3 H3 0.9300 . ?
C2 H2 0.9300 . ?
C22 C23 1.488(8) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.535(8) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C20 H20 0.9300 . ?
C15 C14 1.375(9) . ?
C15 H15 0.9300 . ?
C31 H31 0.9300 . ?
C29 H29 0.9300 . ?
F9 C37 1.406(10) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C13 C14 1.378(9) . ?
C13 H13 0.9300 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C14 H14 0.9300 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C38 C39 1.438(10) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 N9 1.138(10) . ?
F14 C35 1.307(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Ge1 Ag1 Ge2 157.67(3) . . ?
N2 Ge1 N3 73.54(18) . . ?
N2 Ge1 N4 116.86(18) . . ?
N3 Ge1 N4 75.40(18) . . ?
N2 Ge1 N1 76.04(17) . . ?
N3 Ge1 N1 133.32(18) . . ?
N4 Ge1 N1 88.09(17) . . ?
N2 Ge1 Ag1 119.24(13) . . ?
N3 Ge1 Ag1 107.52(13) . . ?
N4 Ge1 Ag1 122.05(13) . . ?
N1 Ge1 Ag1 118.08(12) . . ?
N6 Ge2 N7 74.97(18) . . ?
N6 Ge2 N8 114.49(18) . . ?
N7 Ge2 N8 76.45(18) . . ?
N6 Ge2 N5 76.51(18) . . ?
N7 Ge2 N5 139.79(18) . . ?
N8 Ge2 N5 90.46(17) . . ?
N6 Ge2 Ag1 130.23(13) . . ?
N7 Ge2 Ag1 113.79(12) . . ?
N8 Ge2 Ag1 115.16(12) . . ?
N5 Ge2 Ag1 106.23(13) . . ?
O4 S1 O5 115.1(3) . . ?
O4 S1 O6 116.2(3) . . ?
O5 S1 O6 112.4(3) . . ?
O4 S1 C34 103.8(3) . . ?
O5 S1 C34 103.5(3) . . ?
O6 S1 C34 103.7(3) . . ?
O3 S2 O1 114.1(3) . . ?
O3 S2 O2 115.6(3) . . ?
O1 S2 O2 114.5(3) . . ?
O3 S2 C33 103.0(3) . . ?
O1 S2 C33 102.9(3) . . ?
O2 S2 C33 104.6(3) . . ?
O9 S3 O8 113.9(3) . . ?
O9 S3 O7 116.3(3) . . ?
O8 S3 O7 114.8(3) . . ?
O9 S3 C36 102.5(3) . . ?
O8 S3 C36 103.5(3) . . ?
O7 S3 C36 103.4(3) . . ?
O13 S5 O12 114.2(4) . . ?
O13 S5 O14 116.0(4) . . ?
O12 S5 O14 114.9(3) . . ?
O13 S5 C35 102.3(4) . . ?
O12 S5 C35 104.0(4) . . ?
O14 S5 C35 103.0(4) . . ?
O15 S4 O11 120.7(4) . . ?
O15 S4 O10 111.4(7) . . ?
O11 S4 O10 109.9(4) . . ?
O15 S4 C37 107.0(4) . . ?
O11 S4 C37 105.8(3) . . ?
O10 S4 C37 99.8(4) . . ?
C10 N3 C9 128.5(5) . . ?
C10 N3 Ge1 120.9(4) . . ?
C9 N3 Ge1 109.1(4) . . ?
C22 N7 C24 129.6(5) . . ?
C22 N7 Ge2 120.3(4) . . ?
C24 N7 Ge2 109.9(3) . . ?
C17 N8 C21 119.1(5) . . ?
C17 N8 Ge2 125.6(4) . . ?
C21 N8 Ge2 114.4(3) . . ?
C6 N2 C8 121.9(5) . . ?
C6 N2 Ge1 121.7(4) . . ?
C8 N2 Ge1 116.4(4) . . ?
C32 N5 C28 119.9(5) . . ?
C32 N5 Ge2 123.5(3) . . ?
C28 N5 Ge2 114.9(3) . . ?
C16 N4 C12 117.9(5) . . ?
C16 N4 Ge1 125.6(4) . . ?
C12 N4 Ge1 116.3(4) . . ?
C1 N1 C5 118.2(5) . . ?
C1 N1 Ge1 127.0(4) . . ?
C5 N1 Ge1 114.1(3) . . ?
C26 N6 C25 122.3(5) . . ?
C26 N6 Ge2 120.4(4) . . ?
C25 N6 Ge2 117.2(3) . . ?
N5 C28 C29 121.7(5) . . ?
N5 C28 C26 113.5(5) . . ?
C29 C28 C26 124.7(5) . . ?
N8 C17 C18 122.0(5) . . ?
N8 C17 H17 119.0 . . ?
C18 C17 H17 119.0 . . ?
N3 C10 C12 113.4(5) . . ?
N3 C10 C11 126.8(6) . . ?
C12 C10 C11 119.7(5) . . ?
N6 C26 C28 114.1(5) . . ?
N6 C26 C27 125.6(5) . . ?
C28 C26 C27 120.3(5) . . ?
C18 C19 C20 119.0(5) . . ?
C18 C19 H19 120.5 . . ?
C20 C19 H19 120.5 . . ?
C17 C18 C19 119.1(5) . . ?
C17 C18 H18 120.4 . . ?
C19 C18 H18 120.4 . . ?
N4 C16 C15 121.9(5) . . ?
N4 C16 H16 119.0 . . ?
C15 C16 H16 119.0 . . ?
N8 C21 C20 121.7(5) . . ?
N8 C21 C22 113.9(5) . . ?
C20 C21 C22 124.2(5) . . ?
N6 C25 C24 107.2(4) . . ?
N6 C25 H25A 110.3 . . ?
C24 C25 H25A 110.3 . . ?
N6 C25 H25B 110.3 . . ?
C24 C25 H25B 110.3 . . ?
H25A C25 H25B 108.5 . . ?
N1 C5 C4 123.1(5) . . ?
N1 C5 C6 113.9(5) . . ?
C4 C5 C6 123.0(5) . . ?
N5 C32 C31 120.8(5) . . ?
N5 C32 H32 119.6 . . ?
C31 C32 H32 119.6 . . ?
C5 C4 C3 118.1(5) . . ?
C5 C4 H4 120.9 . . ?
C3 C4 H4 120.9 . . ?
N1 C1 C2 121.4(5) . . ?
N1 C1 H1 119.3 . . ?
C2 C1 H1 119.3 . . ?
N7 C24 C25 104.7(4) . . ?
N7 C24 H24A 110.8 . . ?
C25 C24 H24A 110.8 . . ?
N7 C24 H24B 110.8 . . ?
C25 C24 H24B 110.8 . . ?
H24A C24 H24B 108.9 . . ?
C31 C30 C29 119.4(5) . . ?
C31 C30 H30 120.3 . . ?
C29 C30 H30 120.3 . . ?
N2 C6 C7 125.8(5) . . ?
N2 C6 C5 114.1(5) . . ?
C7 C6 C5 120.1(5) . . ?
N4 C12 C13 122.0(5) . . ?
N4 C12 C10 113.7(5) . . ?
C13 C12 C10 124.3(5) . . ?
C2 C3 C4 118.9(5) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
C1 C2 C3 120.2(5) . . ?
C1 C2 H2 119.9 . . ?
C3 C2 H2 119.9 . . ?
N7 C22 C23 126.8(5) . . ?
N7 C22 C21 112.7(5) . . ?
C23 C22 C21 120.5(5) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N2 C8 C9 107.8(4) . . ?
N2 C8 H8A 110.1 . . ?
C9 C8 H8A 110.1 . . ?
N2 C8 H8B 110.1 . . ?
C9 C8 H8B 110.1 . . ?
H8A C8 H8B 108.5 . . ?
C21 C20 C19 119.1(5) . . ?
C21 C20 H20 120.5 . . ?
C19 C20 H20 120.5 . . ?
C14 C15 C16 119.4(6) . . ?
C14 C15 H15 120.3 . . ?
C16 C15 H15 120.3 . . ?
C30 C31 C32 119.5(6) . . ?
C30 C31 H31 120.3 . . ?
C32 C31 H31 120.3 . . ?
C28 C29 C30 118.6(5) . . ?
C28 C29 H29 120.7 . . ?
C30 C29 H29 120.7 . . ?
F6 C34 F4 108.4(6) . . ?
F6 C34 F5 107.1(5) . . ?
F4 C34 F5 107.6(6) . . ?
F6 C34 S1 112.5(5) . . ?
F4 C34 S1 111.6(4) . . ?
F5 C34 S1 109.5(4) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C12 C13 C14 119.5(5) . . ?
C12 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N3 C9 C8 105.5(4) . . ?
N3 C9 H9A 110.6 . . ?
C8 C9 H9A 110.6 . . ?
N3 C9 H9B 110.6 . . ?
C8 C9 H9B 110.6 . . ?
H9A C9 H9B 108.8 . . ?
F3 C33 F2 108.3(5) . . ?
F3 C33 F1 108.2(5) . . ?
F2 C33 F1 106.6(5) . . ?
F3 C33 S2 111.8(4) . . ?
F2 C33 S2 111.1(4) . . ?
F1 C33 S2 110.6(4) . . ?
C15 C14 C13 119.1(6) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
F12 C36 F10 107.8(5) . . ?
F12 C36 F11 107.1(5) . . ?
F10 C36 F11 108.5(5) . . ?
F12 C36 S3 111.0(4) . . ?
F10 C36 S3 111.4(4) . . ?
F11 C36 S3 110.9(5) . . ?
F8 C37 F7 114.8(7) . . ?
F8 C37 F9 98.4(7) . . ?
F7 C37 F9 102.2(6) . . ?
F8 C37 S4 117.4(5) . . ?
F7 C37 S4 115.6(5) . . ?
F9 C37 S4 104.6(6) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C39 C38 H38A 109.5 . . ?
C39 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C39 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N9 C39 C38 178.7(12) . . ?
F14 C35 F15 107.3(9) . . ?
F14 C35 F13 107.2(9) . . ?
F15 C35 F13 108.1(7) . . ?
F14 C35 S5 112.1(7) . . ?
F15 C35 S5 111.0(7) . . ?
F13 C35 S5 110.8(6) . . ?

_refine_diff_density_max         3.065
_refine_diff_density_min         -1.348
_refine_diff_density_rms         0.151

