# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_b
_database_code_depnum_ccdc_archive 'CCDC 1450544'
_audit_update_record             
;
2016-05-31 deposited with the CCDC.
2016-06-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17 H29 Cl4 N3 Si2 Zr'
_chemical_formula_weight         564.63

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'
Si Si 0.0817 0.0704 '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'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.139(2)
_cell_length_b                   12.050(2)
_cell_length_c                   12.659(3)
_cell_angle_alpha                118.34(3)
_cell_angle_beta                 110.25(3)
_cell_angle_gamma                91.62(3)
_cell_volume                     1241.9(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    0.7810
_cell_measurement_theta_min      3.3505
_cell_measurement_theta_max      27.0675

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             576
_exptl_absorpt_coefficient_mu    0.978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8284
_exptl_absorpt_correction_T_max  0.8671
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5135
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0612
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         25.05
_reflns_number_total             4291
_reflns_number_gt                3596
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       APEX2
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0579P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4291
_refine_ls_number_parameters     252
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0545
_refine_ls_wR_factor_ref         0.1181
_refine_ls_wR_factor_gt          0.1120
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.73706(5) 0.92792(4) 1.20570(4) 0.02021(15) Uani 1 1 d . . .
Cl2 Cl 0.76780(14) 0.76135(11) 1.26307(12) 0.0310(3) Uani 1 1 d . . .
Si2 Si 0.72043(15) 0.41855(12) 0.78481(13) 0.0264(3) Uani 1 1 d . . .
Si1 Si 0.63179(14) 0.68280(12) 0.85785(12) 0.0227(3) Uani 1 1 d . . .
Cl4 Cl 0.75045(14) 1.08217(11) 1.13487(12) 0.0316(3) Uani 1 1 d . . .
Cl1 Cl 0.78863(16) 1.09818(12) 1.42605(12) 0.0398(4) Uani 1 1 d . . .
Cl3 Cl 0.48127(14) 0.86951(13) 1.11315(14) 0.0398(3) Uani 1 1 d . . .
N1 N 0.9830(4) 0.9558(3) 1.2529(3) 0.0212(9) Uani 1 1 d . . .
C4 C 1.0213(5) 0.9004(4) 1.1498(4) 0.0205(10) Uani 1 1 d . . .
C5 C 1.0888(5) 1.0267(4) 1.3743(5) 0.0263(11) Uani 1 1 d . . .
H5 H 1.0635 1.0646 1.4456 0.032 Uiso 1 1 calc R . .
C2 C 1.1638(5) 0.9199(4) 1.1674(5) 0.0245(11) Uani 1 1 d . . .
H2 H 1.1879 0.8835 1.0953 0.029 Uiso 1 1 calc R . .
C1 C 1.2703(5) 0.9940(4) 1.2931(5) 0.0278(11) Uani 1 1 d . . .
H1 H 1.3668 1.0086 1.3063 0.033 Uiso 1 1 calc R . .
C3 C 1.2333(5) 1.0457(4) 1.3980(5) 0.0292(12) Uani 1 1 d . . .
H3 H 1.3040 1.0927 1.4835 0.035 Uiso 1 1 calc R . .
N2 N 0.7704(4) 0.7926(3) 1.0207(3) 0.0206(9) Uani 1 1 d . . .
C6 C 0.8980(5) 0.8117(4) 1.0204(4) 0.0192(10) Uani 1 1 d . . .
C8 C 0.8482(5) 0.6338(4) 0.7940(4) 0.0227(11) Uani 1 1 d . . .
C7 C 0.9273(5) 0.7499(4) 0.9043(4) 0.0221(10) Uani 1 1 d . . .
H7 H 1.0057 0.7922 0.9047 0.026 Uiso 1 1 calc R . .
C9 C 0.8851(6) 0.5814(4) 0.6730(5) 0.0278(11) Uani 1 1 d . . .
C12 C 0.7803(6) 0.4532(5) 0.5554(5) 0.0408(14) Uani 1 1 d . . .
H12A H 0.7910 0.3864 0.5765 0.061 Uiso 1 1 calc R . .
H12B H 0.8015 0.4295 0.4802 0.061 Uiso 1 1 calc R . .
H12C H 0.6828 0.4637 0.5360 0.061 Uiso 1 1 calc R . .
C11 C 1.0405(6) 0.5671(5) 0.7067(5) 0.0359(13) Uani 1 1 d . . .
H11A H 1.0531 0.5047 0.7339 0.054 Uiso 1 1 calc R . .
H11B H 1.1048 0.6493 0.7769 0.054 Uiso 1 1 calc R . .
H11C H 1.0616 0.5384 0.6308 0.054 Uiso 1 1 calc R . .
C10 C 0.8657(6) 0.6829(5) 0.6307(5) 0.0378(14) Uani 1 1 d . . .
H10A H 0.8899 0.6561 0.5566 0.057 Uiso 1 1 calc R . .
H10B H 0.9281 0.7653 0.7023 0.057 Uiso 1 1 calc R . .
H10C H 0.7671 0.6903 0.6069 0.057 Uiso 1 1 calc R . .
N3 N 0.7259(4) 0.5688(3) 0.7881(3) 0.0192(8) Uani 1 1 d . . .
C14 C 0.5824(6) 0.7790(5) 0.7777(5) 0.0325(12) Uani 1 1 d . . .
H14A H 0.6671 0.8162 0.7773 0.049 Uiso 1 1 calc R . .
H14B H 0.5420 0.8469 0.8252 0.049 Uiso 1 1 calc R . .
H14C H 0.5124 0.7237 0.6889 0.049 Uiso 1 1 calc R . .
C13 C 0.4684(5) 0.6040(5) 0.8519(5) 0.0367(13) Uani 1 1 d . . .
H13A H 0.4284 0.5197 0.7735 0.055 Uiso 1 1 calc R . .
H13B H 0.3983 0.6559 0.8513 0.055 Uiso 1 1 calc R . .
H13C H 0.4935 0.5955 0.9276 0.055 Uiso 1 1 calc R . .
C17 C 0.8981(6) 0.3755(5) 0.8015(5) 0.0367(13) Uani 1 1 d . . .
H17A H 0.9079 0.3444 0.7200 0.055 Uiso 1 1 calc R . .
H17B H 0.9040 0.3090 0.8233 0.055 Uiso 1 1 calc R . .
H17C H 0.9743 0.4508 0.8700 0.055 Uiso 1 1 calc R . .
C16 C 0.5692(6) 0.2874(5) 0.6345(5) 0.0390(14) Uani 1 1 d . . .
H16A H 0.4826 0.3189 0.6209 0.058 Uiso 1 1 calc R . .
H16B H 0.5545 0.2148 0.6450 0.058 Uiso 1 1 calc R . .
H16C H 0.5926 0.2607 0.5599 0.058 Uiso 1 1 calc R . .
C15 C 0.6917(6) 0.4388(5) 0.9305(5) 0.0397(14) Uani 1 1 d . . .
H15A H 0.7398 0.5250 1.0040 0.060 Uiso 1 1 calc R . .
H15B H 0.7304 0.3769 0.9521 0.060 Uiso 1 1 calc R . .
H15C H 0.5901 0.4250 0.9101 0.060 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zr1 0.0248(3) 0.0172(3) 0.0192(3) 0.0076(2) 0.0122(2) 0.00588(19)
Cl2 0.0433(8) 0.0259(7) 0.0309(7) 0.0165(6) 0.0198(6) 0.0092(6)
Si2 0.0301(8) 0.0170(7) 0.0291(8) 0.0091(6) 0.0135(6) 0.0010(6)
Si1 0.0224(8) 0.0201(7) 0.0201(7) 0.0062(6) 0.0093(6) 0.0015(6)
Cl4 0.0381(8) 0.0255(7) 0.0354(7) 0.0182(6) 0.0158(6) 0.0091(6)
Cl1 0.0623(10) 0.0276(7) 0.0263(7) 0.0085(6) 0.0224(7) 0.0144(6)
Cl3 0.0273(8) 0.0398(8) 0.0508(9) 0.0205(7) 0.0184(7) 0.0097(6)
N1 0.026(2) 0.016(2) 0.017(2) 0.0064(17) 0.0072(18) 0.0024(17)
C4 0.028(3) 0.016(2) 0.021(2) 0.013(2) 0.009(2) 0.004(2)
C5 0.037(3) 0.020(3) 0.022(3) 0.012(2) 0.012(2) 0.003(2)
C2 0.027(3) 0.019(2) 0.028(3) 0.011(2) 0.015(2) 0.007(2)
C1 0.024(3) 0.022(3) 0.034(3) 0.014(2) 0.009(2) 0.001(2)
C3 0.025(3) 0.025(3) 0.023(3) 0.011(2) -0.002(2) -0.005(2)
N2 0.022(2) 0.0161(19) 0.022(2) 0.0075(17) 0.0101(18) 0.0037(16)
C6 0.023(3) 0.012(2) 0.020(2) 0.0078(19) 0.006(2) 0.0030(19)
C8 0.031(3) 0.017(2) 0.023(3) 0.010(2) 0.015(2) 0.004(2)
C7 0.021(3) 0.021(2) 0.028(3) 0.012(2) 0.015(2) 0.004(2)
C9 0.040(3) 0.021(3) 0.023(3) 0.007(2) 0.019(2) 0.006(2)
C12 0.054(4) 0.031(3) 0.026(3) 0.002(2) 0.025(3) 0.001(3)
C11 0.041(3) 0.032(3) 0.039(3) 0.014(3) 0.027(3) 0.005(2)
C10 0.059(4) 0.033(3) 0.027(3) 0.013(2) 0.027(3) 0.006(3)
N3 0.024(2) 0.0150(19) 0.018(2) 0.0061(16) 0.0109(18) 0.0013(16)
C14 0.033(3) 0.031(3) 0.025(3) 0.011(2) 0.008(2) 0.011(2)
C13 0.025(3) 0.033(3) 0.038(3) 0.007(3) 0.014(3) 0.000(2)
C17 0.041(3) 0.026(3) 0.050(4) 0.021(3) 0.024(3) 0.014(2)
C16 0.044(4) 0.017(3) 0.042(3) 0.006(2) 0.017(3) -0.003(2)
C15 0.052(4) 0.032(3) 0.042(3) 0.020(3) 0.026(3) 0.004(3)

_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
Zr1 N2 2.283(4) . ?
Zr1 N1 2.328(4) . ?
Zr1 Cl3 2.3675(17) . ?
Zr1 Cl1 2.3999(18) . ?
Zr1 Cl2 2.4323(13) . ?
Zr1 Cl4 2.4350(13) . ?
Si2 N3 1.791(4) . ?
Si2 C17 1.858(5) . ?
Si2 C16 1.860(5) . ?
Si2 C15 1.869(5) . ?
Si1 N3 1.756(4) . ?
Si1 N2 1.810(4) . ?
Si1 C13 1.846(5) . ?
Si1 C14 1.850(5) . ?
N1 C5 1.343(6) . ?
N1 C4 1.355(6) . ?
C4 C2 1.379(6) . ?
C4 C6 1.494(6) . ?
C5 C3 1.378(7) . ?
C2 C1 1.380(7) . ?
C1 C3 1.365(7) . ?
N2 C6 1.309(6) . ?
C6 C7 1.441(6) . ?
C8 C7 1.362(6) . ?
C8 N3 1.407(6) . ?
C8 C9 1.542(6) . ?
C9 C11 1.521(7) . ?
C9 C12 1.537(7) . ?
C9 C10 1.544(7) . ?

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 Zr1 N1 70.25(13) . . ?
N2 Zr1 Cl3 98.00(11) . . ?
N1 Zr1 Cl3 168.24(9) . . ?
N2 Zr1 Cl1 160.33(10) . . ?
N1 Zr1 Cl1 90.33(11) . . ?
Cl3 Zr1 Cl1 101.36(7) . . ?
N2 Zr1 Cl2 87.85(10) . . ?
N1 Zr1 Cl2 85.59(10) . . ?
Cl3 Zr1 Cl2 94.81(6) . . ?
Cl1 Zr1 Cl2 93.92(5) . . ?
N2 Zr1 Cl4 82.86(10) . . ?
N1 Zr1 Cl4 83.33(10) . . ?
Cl3 Zr1 Cl4 94.84(6) . . ?
Cl1 Zr1 Cl4 92.05(5) . . ?
Cl2 Zr1 Cl4 167.43(5) . . ?
N3 Si2 C17 109.7(2) . . ?
N3 Si2 C16 111.5(2) . . ?
C17 Si2 C16 112.1(2) . . ?
N3 Si2 C15 109.3(2) . . ?
C17 Si2 C15 106.3(3) . . ?
C16 Si2 C15 107.8(3) . . ?
N3 Si1 N2 101.42(18) . . ?
N3 Si1 C13 111.3(2) . . ?
N2 Si1 C13 115.7(2) . . ?
N3 Si1 C14 112.0(2) . . ?
N2 Si1 C14 106.2(2) . . ?
C13 Si1 C14 109.9(3) . . ?
C5 N1 C4 118.0(4) . . ?
C5 N1 Zr1 124.6(3) . . ?
C4 N1 Zr1 117.4(3) . . ?
N1 C4 C2 121.5(4) . . ?
N1 C4 C6 114.2(4) . . ?
C2 C4 C6 124.2(4) . . ?
N1 C5 C3 122.9(5) . . ?
C4 C2 C1 119.2(4) . . ?
C3 C1 C2 119.7(5) . . ?
C1 C3 C5 118.5(5) . . ?
C6 N2 Si1 112.7(3) . . ?
C6 N2 Zr1 118.6(3) . . ?
Si1 N2 Zr1 127.09(19) . . ?
N2 C6 C7 124.2(4) . . ?
N2 C6 C4 117.4(4) . . ?
C7 C6 C4 118.4(4) . . ?
C7 C8 N3 119.3(4) . . ?
C7 C8 C9 119.8(4) . . ?
N3 C8 C9 120.7(4) . . ?
C8 C7 C6 124.7(4) . . ?
C11 C9 C12 110.6(4) . . ?
C11 C9 C8 111.4(4) . . ?
C12 C9 C8 112.7(4) . . ?
C11 C9 C10 109.3(4) . . ?
C12 C9 C10 106.7(4) . . ?
C8 C9 C10 105.9(4) . . ?
C8 N3 Si1 108.9(3) . . ?
C8 N3 Si2 121.8(3) . . ?
Si1 N3 Si2 123.3(2) . . ?

_diffrn_measured_fraction_theta_max 0.975
_diffrn_reflns_theta_full        25.05
_diffrn_measured_fraction_theta_full 0.975
_refine_diff_density_max         1.064
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.107
####################################################################### 
# 
# 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_hs0350p
_database_code_depnum_ccdc_archive 'CCDC 1450545'
_audit_update_record             
;
2016-05-31 deposited with the CCDC.
2016-06-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C13 H33 Cl N4 Si2 Sn'
_chemical_formula_weight         455.75

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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   11.7137(17)
_cell_length_b                   15.426(2)
_cell_length_c                   11.7657(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.121(2)
_cell_angle_gamma                90.00
_cell_volume                     2125.6(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    4254
_cell_measurement_theta_min      2.183
_cell_measurement_theta_max      16.470

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             936
_exptl_absorpt_coefficient_mu    1.441
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7615
_exptl_absorpt_correction_T_max  0.7615
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      183(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'oil sealed '
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        4.41
_diffrn_reflns_number            8605
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0450
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.18
_diffrn_reflns_theta_max         25.01
_reflns_number_total             3697
_reflns_number_gt                3209
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       SMART
_computing_cell_refinement       SAINT
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1000P)²+9.7463P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3697
_refine_ls_number_parameters     200
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0517
_refine_ls_wR_factor_ref         0.1745
_refine_ls_wR_factor_gt          0.1577
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.40374(4) 0.07754(3) 0.36817(4) 0.0361(2) Uani 1 1 d . . .
Cl1 Cl 0.36942(16) 0.23006(13) 0.42188(17) 0.0480(5) Uani 1 1 d . . .
Si1 Si 0.17722(17) -0.01318(13) 0.25279(17) 0.0385(5) Uani 1 1 d . . .
Si2 Si 0.63765(18) 0.04091(16) 0.21472(19) 0.0483(5) Uani 1 1 d . . .
N1 N 0.5185(5) 0.1069(4) 0.2326(5) 0.0380(13) Uani 1 1 d . . .
N2 N 0.2656(5) 0.0772(3) 0.2404(5) 0.0305(12) Uani 1 1 d . . .
N3 N 0.5641(5) 0.2126(4) 0.0987(5) 0.0414(14) Uani 1 1 d . . .
N4 N 0.1687(5) 0.1616(4) 0.1056(5) 0.0401(13) Uani 1 1 d . . .
C1 C 0.4821(6) 0.1664(4) 0.1544(5) 0.0335(14) Uani 1 1 d . . .
C2 C 0.3671(6) 0.1806(5) 0.1226(6) 0.0368(15) Uani 1 1 d . . .
H2 H 0.3549 0.2247 0.0697 0.044 Uiso 1 1 calc R . .
C3 C 0.2688(5) 0.1384(4) 0.1586(6) 0.0347(14) Uani 1 1 d . . .
C4 C 0.0661(6) 0.1774(6) 0.1716(7) 0.0489(19) Uani 1 1 d . . .
H4A H 0.0718 0.1465 0.2423 0.073 Uiso 1 1 calc R . .
H4B H 0.0002 0.1578 0.1293 0.073 Uiso 1 1 calc R . .
H4C H 0.0592 0.2384 0.1865 0.073 Uiso 1 1 calc R . .
C5 C 0.1671(7) 0.2070(6) -0.0030(7) 0.0512(19) Uani 1 1 d . . .
H5A H 0.1799 0.2678 0.0097 0.077 Uiso 1 1 calc R . .
H5B H 0.0942 0.1989 -0.0402 0.077 Uiso 1 1 calc R . .
H5C H 0.2261 0.1843 -0.0501 0.077 Uiso 1 1 calc R . .
C6 C 0.5412(7) 0.2548(6) -0.0098(6) 0.0504(19) Uani 1 1 d . . .
H6A H 0.4993 0.2161 -0.0590 0.076 Uiso 1 1 calc R . .
H6B H 0.6122 0.2699 -0.0442 0.076 Uiso 1 1 calc R . .
H6C H 0.4972 0.3064 0.0021 0.076 Uiso 1 1 calc R . .
C7 C 0.6541(7) 0.2553(6) 0.1662(8) 0.060(2) Uani 1 1 d . . .
H7A H 0.6403 0.3166 0.1678 0.090 Uiso 1 1 calc R . .
H7B H 0.7268 0.2443 0.1328 0.090 Uiso 1 1 calc R . .
H7C H 0.6543 0.2329 0.2424 0.090 Uiso 1 1 calc R . .
C8 C 0.6822(11) 0.0351(8) 0.0659(10) 0.089(4) Uani 1 1 d . . .
H8A H 0.6160 0.0295 0.0171 0.134 Uiso 1 1 calc R . .
H8B H 0.7310 -0.0142 0.0562 0.134 Uiso 1 1 calc R . .
H8C H 0.7229 0.0870 0.0469 0.134 Uiso 1 1 calc R . .
C9 C 0.7579(10) 0.0730(8) 0.3145(14) 0.100(5) Uani 1 1 d . . .
H9A H 0.7880 0.1281 0.2918 0.149 Uiso 1 1 calc R . .
H9B H 0.8172 0.0301 0.3122 0.149 Uiso 1 1 calc R . .
H9C H 0.7299 0.0772 0.3905 0.149 Uiso 1 1 calc R . .
C10 C 0.5978(9) -0.0707(6) 0.2574(10) 0.071(3) Uani 1 1 d . . .
H10A H 0.5805 -0.0715 0.3368 0.107 Uiso 1 1 calc R . .
H10B H 0.6602 -0.1094 0.2436 0.107 Uiso 1 1 calc R . .
H10C H 0.5319 -0.0891 0.2139 0.107 Uiso 1 1 calc R . .
C11 C 0.2731(8) -0.1095(5) 0.2636(8) 0.056(2) Uani 1 1 d . . .
H11A H 0.3228 -0.1105 0.1997 0.084 Uiso 1 1 calc R . .
H11B H 0.2279 -0.1614 0.2640 0.084 Uiso 1 1 calc R . .
H11C H 0.3179 -0.1061 0.3327 0.084 Uiso 1 1 calc R . .
C12 C 0.0982(8) -0.0042(7) 0.3872(8) 0.067(3) Uani 1 1 d . . .
H12A H 0.1514 -0.0037 0.4503 0.100 Uiso 1 1 calc R . .
H12B H 0.0476 -0.0527 0.3941 0.100 Uiso 1 1 calc R . .
H12C H 0.0548 0.0486 0.3868 0.100 Uiso 1 1 calc R . .
C13 C 0.0739(7) -0.0324(6) 0.1350(8) 0.055(2) Uani 1 1 d . . .
H13A H 0.0038 -0.0028 0.1503 0.082 Uiso 1 1 calc R . .
H13B H 0.0595 -0.0935 0.1281 0.082 Uiso 1 1 calc R . .
H13C H 0.1047 -0.0110 0.0654 0.082 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sn1 0.0338(3) 0.0454(3) 0.0289(3) 0.00330(18) 0.0000(2) 0.00396(19)
Cl1 0.0448(10) 0.0501(11) 0.0492(10) -0.0130(8) 0.0042(8) -0.0036(8)
Si1 0.0379(10) 0.0383(10) 0.0393(11) 0.0033(8) 0.0035(8) -0.0040(8)
Si2 0.0375(11) 0.0630(14) 0.0445(12) -0.0011(10) 0.0053(9) 0.0148(10)
N1 0.032(3) 0.042(3) 0.040(3) -0.001(3) 0.003(2) 0.007(3)
N2 0.035(3) 0.030(3) 0.026(3) -0.004(2) -0.003(2) 0.008(2)
N3 0.034(3) 0.053(4) 0.037(3) 0.006(3) 0.005(2) -0.006(3)
N4 0.034(3) 0.043(3) 0.043(3) 0.012(3) -0.002(2) 0.004(3)
C1 0.035(3) 0.034(3) 0.032(3) -0.008(3) 0.004(3) -0.001(3)
C2 0.031(3) 0.042(4) 0.037(4) 0.007(3) 0.000(3) -0.002(3)
C3 0.026(3) 0.039(4) 0.039(4) -0.006(3) -0.001(3) 0.005(3)
C4 0.031(4) 0.060(5) 0.056(5) 0.000(4) -0.001(3) 0.011(3)
C5 0.041(4) 0.061(5) 0.051(5) 0.012(4) -0.009(3) 0.010(4)
C6 0.056(5) 0.057(5) 0.039(4) 0.014(4) 0.020(4) -0.006(4)
C7 0.054(5) 0.067(6) 0.059(5) -0.010(4) 0.004(4) -0.024(4)
C8 0.109(9) 0.087(8) 0.074(7) 0.002(6) 0.044(7) 0.045(7)
C9 0.053(6) 0.099(9) 0.145(13) -0.021(8) -0.031(7) 0.018(6)
C10 0.072(6) 0.064(6) 0.079(7) 0.015(5) 0.019(5) 0.028(5)
C11 0.062(5) 0.037(4) 0.069(6) 0.005(4) -0.011(4) 0.005(4)
C12 0.058(5) 0.092(7) 0.051(5) 0.010(5) 0.024(4) -0.009(5)
C13 0.051(5) 0.048(5) 0.066(6) -0.001(4) -0.006(4) -0.002(4)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 N1 2.154(6) . ?
Sn1 N2 2.187(6) . ?
Sn1 Cl1 2.471(2) . ?
Si1 N2 1.744(6) . ?
Si1 C13 1.846(9) . ?
Si1 C12 1.853(8) . ?
Si1 C11 1.865(8) . ?
Si2 N1 1.744(6) . ?
Si2 C8 1.839(10) . ?
Si2 C10 1.856(10) . ?
Si2 C9 1.882(12) . ?
N1 C1 1.362(9) . ?
N2 C3 1.350(9) . ?
N3 C1 1.372(9) . ?
N3 C6 1.454(9) . ?
N3 C7 1.465(10) . ?
N4 C3 1.365(8) . ?
N4 C5 1.457(9) . ?
N4 C4 1.463(10) . ?
C1 C2 1.408(9) . ?
C2 C3 1.396(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Sn1 N2 87.5(2) . . ?
N1 Sn1 Cl1 95.51(17) . . ?
N2 Sn1 Cl1 93.24(14) . . ?
N2 Si1 C13 116.6(3) . . ?
N2 Si1 C12 108.6(4) . . ?
C13 Si1 C12 108.8(4) . . ?
N2 Si1 C11 106.5(3) . . ?
C13 Si1 C11 107.9(4) . . ?
C12 Si1 C11 108.2(5) . . ?
N1 Si2 C8 112.7(4) . . ?
N1 Si2 C10 107.6(4) . . ?
C8 Si2 C10 106.9(5) . . ?
N1 Si2 C9 111.2(4) . . ?
C8 Si2 C9 112.6(7) . . ?
C10 Si2 C9 105.3(6) . . ?
C1 N1 Si2 123.5(5) . . ?
C1 N1 Sn1 116.8(4) . . ?
Si2 N1 Sn1 118.6(3) . . ?
C3 N2 Si1 130.1(5) . . ?
C3 N2 Sn1 117.3(4) . . ?
Si1 N2 Sn1 112.2(3) . . ?
C1 N3 C6 122.3(6) . . ?
C1 N3 C7 118.5(6) . . ?
C6 N3 C7 113.1(6) . . ?
C3 N4 C5 121.5(6) . . ?
C3 N4 C4 120.5(6) . . ?
C5 N4 C4 112.9(6) . . ?
N1 C1 N3 117.4(6) . . ?
N1 C1 C2 124.7(6) . . ?
N3 C1 C2 117.8(6) . . ?
C1 C2 C3 129.6(6) . . ?
N2 C3 N4 118.3(6) . . ?
N2 C3 C2 125.3(6) . . ?
N4 C3 C2 116.5(6) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.580
_refine_diff_density_min         -1.024
_refine_diff_density_rms         0.109
####################################################################### 
# 
# 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_hs0372p
_database_code_depnum_ccdc_archive 'CCDC 1450546'
_audit_update_record             
;
2016-05-31 deposited with the CCDC.
2016-06-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H14 Cl5 Ge2 N4'
_chemical_formula_weight         476.65

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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.7293(16)
_cell_length_b                   9.6018(18)
_cell_length_c                   10.0436(19)
_cell_angle_alpha                91.651(2)
_cell_angle_beta                 98.999(2)
_cell_angle_gamma                102.452(2)
_cell_volume                     810.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    456(2)
_cell_measurement_reflns_used    9516
_cell_measurement_theta_min      2.929
_cell_measurement_theta_max      28.464

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.954
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             466
_exptl_absorpt_coefficient_mu    4.522
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3440
_exptl_absorpt_correction_T_max  0.4649
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      456(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3339
_diffrn_reflns_av_R_equivalents  0.0166
_diffrn_reflns_av_sigmaI/netI    0.0397
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.06
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2782
_reflns_number_gt                2275
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       APEX2
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0419P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2782
_refine_ls_number_parameters     167
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0335
_refine_ls_wR_factor_ref         0.0831
_refine_ls_wR_factor_gt          0.0808
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.19015(5) 0.31267(5) 0.73616(4) 0.02755(14) Uani 1 1 d . . .
Ge2 Ge -0.19618(5) 0.19196(5) 0.77876(4) 0.03052(14) Uani 1 1 d . . .
Cl1 Cl 0.29867(14) 0.20996(13) 0.89649(11) 0.0425(3) Uani 1 1 d . . .
Cl2 Cl 0.18320(13) 0.18360(12) 0.55788(11) 0.0379(3) Uani 1 1 d . . .
Cl3 Cl -0.27266(17) 0.19320(16) 0.96827(12) 0.0569(4) Uani 1 1 d . . .
Cl4 Cl -0.39466(15) 0.12980(14) 0.62162(12) 0.0519(3) Uani 1 1 d . . .
Cl5 Cl -0.10691(15) -0.00167(13) 0.78357(15) 0.0535(4) Uani 1 1 d . . .
N1 N -0.0150(4) 0.3200(4) 0.7540(3) 0.0306(8) Uani 1 1 d . . .
N2 N 0.2927(4) 0.4914(4) 0.7293(3) 0.0318(9) Uani 1 1 d . . .
H2 H 0.3940 0.5108 0.7316 0.038 Uiso 1 1 calc RD . .
N3 N 0.2989(4) 0.7288(4) 0.7123(4) 0.0300(8) Uani 1 1 d . . .
N4 N -0.2155(4) 0.4345(4) 0.7561(3) 0.0301(8) Uani 1 1 d . . .
C1 C -0.0497(5) 0.4522(5) 0.7421(4) 0.0273(9) Uani 1 1 d . . .
C2 C 0.0456(5) 0.5759(5) 0.7244(4) 0.0301(10) Uani 1 1 d . . .
H2A H 0.0017 0.6558 0.7137 0.036 Uiso 1 1 calc R . .
C3 C 0.2166(5) 0.5938(5) 0.7207(4) 0.0275(9) Uani 1 1 d . . .
C4 C 0.2270(5) 0.8504(5) 0.6889(5) 0.0369(11) Uani 1 1 d . . .
H4A H 0.1373 0.8251 0.6172 0.055 Uiso 1 1 calc R . .
H4B H 0.3036 0.9288 0.6641 0.055 Uiso 1 1 calc R . .
H4C H 0.1923 0.8780 0.7698 0.055 Uiso 1 1 calc R . .
C5 C 0.4715(4) 0.7566(5) 0.7301(4) 0.0372(11) Uani 1 1 d . . .
H5A H 0.5104 0.7060 0.8045 0.056 Uiso 1 1 calc RD . .
H5B H 0.5148 0.8573 0.7484 0.056 Uiso 1 1 calc R . .
H5C H 0.5032 0.7248 0.6493 0.056 Uiso 1 1 calc R . .
C6 C -0.2369(5) 0.5186(5) 0.8749(5) 0.0435(12) Uani 1 1 d . . .
H6A H -0.1727 0.4960 0.9544 0.065 Uiso 1 1 calc R . .
H6B H -0.3468 0.4957 0.8855 0.065 Uiso 1 1 calc R . .
H6C H -0.2052 0.6187 0.8619 0.065 Uiso 1 1 calc R . .
C7 C -0.3121(5) 0.4721(5) 0.6321(5) 0.0414(12) Uani 1 1 d . . .
H7A H -0.2841 0.5734 0.6240 0.062 Uiso 1 1 calc R . .
H7B H -0.4231 0.4435 0.6381 0.062 Uiso 1 1 calc R . .
H7C H -0.2913 0.4235 0.5543 0.062 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ge1 0.0225(3) 0.0212(3) 0.0391(3) 0.00109(19) 0.00435(19) 0.00568(19)
Ge2 0.0251(3) 0.0302(3) 0.0345(3) 0.0025(2) 0.0066(2) 0.0010(2)
Cl1 0.0480(7) 0.0364(7) 0.0424(7) 0.0046(5) -0.0031(5) 0.0156(6)
Cl2 0.0444(7) 0.0311(7) 0.0395(6) -0.0013(5) 0.0054(5) 0.0129(5)
Cl3 0.0717(9) 0.0692(10) 0.0399(7) 0.0187(7) 0.0245(6) 0.0251(8)
Cl4 0.0489(8) 0.0404(8) 0.0510(7) 0.0038(6) -0.0100(6) -0.0104(6)
Cl5 0.0451(8) 0.0285(7) 0.0891(10) 0.0080(6) 0.0204(7) 0.0060(6)
N1 0.0240(19) 0.020(2) 0.050(2) 0.0038(16) 0.0107(17) 0.0059(15)
N2 0.0157(17) 0.027(2) 0.053(2) 0.0051(17) 0.0067(16) 0.0029(16)
N3 0.0251(19) 0.020(2) 0.045(2) 0.0033(16) 0.0048(16) 0.0054(16)
N4 0.0217(18) 0.033(2) 0.035(2) 0.0020(16) 0.0053(15) 0.0057(16)
C1 0.023(2) 0.030(3) 0.029(2) -0.0021(18) 0.0016(17) 0.0086(19)
C2 0.024(2) 0.027(3) 0.040(2) 0.0039(19) 0.0020(19) 0.0072(19)
C3 0.024(2) 0.028(3) 0.031(2) 0.0001(18) 0.0046(18) 0.0047(19)
C4 0.038(3) 0.025(3) 0.050(3) 0.010(2) 0.007(2) 0.010(2)
C5 0.025(2) 0.028(3) 0.054(3) 0.007(2) 0.002(2) 0.001(2)
C6 0.036(3) 0.045(3) 0.051(3) -0.009(2) 0.011(2) 0.010(2)
C7 0.025(2) 0.045(3) 0.053(3) 0.012(2) 0.001(2) 0.009(2)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 N2 1.765(3) . ?
Ge1 N1 1.844(3) . ?
Ge1 Cl1 2.1165(12) . ?
Ge1 Cl2 2.1335(12) . ?
Ge2 N1 1.838(3) . ?
Ge2 Cl3 2.1139(13) . ?
Ge2 Cl4 2.1198(13) . ?
Ge2 Cl5 2.1644(14) . ?
N1 C1 1.371(5) . ?
N2 C3 1.297(5) . ?
N3 C3 1.352(5) . ?
N3 C4 1.450(5) . ?
N3 C5 1.453(5) . ?
N4 C1 1.450(5) . ?
N4 C6 1.481(5) . ?
N4 C7 1.490(5) . ?
C1 C2 1.329(6) . ?
C2 C3 1.472(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ge1 N1 106.03(15) . . ?
N2 Ge1 Cl1 112.23(12) . . ?
N1 Ge1 Cl1 111.77(11) . . ?
N2 Ge1 Cl2 112.81(12) . . ?
N1 Ge1 Cl2 108.78(12) . . ?
Cl1 Ge1 Cl2 105.30(5) . . ?
N1 Ge2 Cl3 119.39(12) . . ?
N1 Ge2 Cl4 121.64(11) . . ?
Cl3 Ge2 Cl4 110.26(6) . . ?
N1 Ge2 Cl5 99.18(11) . . ?
Cl3 Ge2 Cl5 100.64(6) . . ?
Cl4 Ge2 Cl5 99.91(6) . . ?
C1 N1 Ge2 108.3(3) . . ?
C1 N1 Ge1 115.1(3) . . ?
Ge2 N1 Ge1 136.6(2) . . ?
C3 N2 Ge1 120.6(3) . . ?
C3 N3 C4 124.4(3) . . ?
C3 N3 C5 118.8(3) . . ?
C4 N3 C5 116.8(3) . . ?
C1 N4 C6 112.5(3) . . ?
C1 N4 C7 111.6(3) . . ?
C6 N4 C7 109.5(3) . . ?
C2 C1 N1 128.9(4) . . ?
C2 C1 N4 124.6(4) . . ?
N1 C1 N4 106.5(3) . . ?
C1 C2 C3 123.8(4) . . ?
N2 C3 N3 118.8(4) . . ?
N2 C3 C2 124.9(4) . . ?
N3 C3 C2 116.3(4) . . ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.092
