# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Ejfler, Jolanta' 'Jiao, Haijun' 'Sobota, Piotr' 'Szafert, Slawomir' _publ_contact_author_name 'Prof Piotr Sobota' _publ_contact_author_address ; Faculty of Chemistry University of Wroclaw 14 F. Joliot-Curie 50-383 Wroclaw POLAND ; _publ_contact_author_email 'PLAS@WCHUWR.CHEM.UNI.WROC.PL' _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Syntheses of novel hexacoordinate germanium(IV) complexes. Crystal structures and properties of [GeCl4(TMEDA)] and [GeCl2(N3)2(TMEDA)] ; _publ_contact_letter ; submitted to New Journal of Chemistry B110770b ; data_1 _database_code_CSD 171326 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C6 H16 Cl4 Ge N2' _chemical_formula_sum 'C6 H16 Cl4 Ge N2' _chemical_formula_weight 330.60 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 orthorombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 14.633(2) _cell_length_b 7.328(3) _cell_length_c 11.7250(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1257.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 9 _cell_measurement_theta_max 11 _exptl_crystal_description needles _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.747 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 3.248 _exptl_absorpt_correction_type COSABS99 _exptl_absorpt_correction_T_min 0.542 _exptl_absorpt_correction_T_max 0.861 _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 'KUMA KM4' _diffrn_measurement_method 'omega-2theta' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% no _diffrn_reflns_number 1672 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.0759 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 28.06 _reflns_number_total 1603 _reflns_number_gt 718 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KUMA KM4 software' _computing_cell_refinement 'KUMA KM4 software' _computing_data_reduction 'KUMA KM4 software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ 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 w=1/[\s^2^(Fo^2^)+(0.0457P)^2^+4.2083P] where P=(Fo^2^+2Fc^2^)/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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(4) _refine_ls_number_reflns 1603 _refine_ls_number_parameters 122 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1642 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1418 _refine_ls_wR_factor_gt 0.1026 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.033 _refine_ls_shift/su_mean 0.001 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ge Ge 0.13581(7) 0.17821(13) 1.00000(13) 0.0468(3) Uani 1 d . . . Cl1 Cl 0.2349(2) 0.4108(4) 1.0166(5) 0.0825(13) Uani 1 d . . . Cl2 Cl 0.0282(4) 0.3039(7) 1.1102(5) 0.107(2) Uani 1 d . . . Cl3 Cl 0.1960(4) 0.0476(7) 1.1569(4) 0.0970(16) Uani 1 d . . . Cl4 Cl 0.0732(3) 0.3156(6) 0.8474(4) 0.0930(16) Uani 1 d . . . N1 N 0.2328(11) 0.0392(17) 0.8933(13) 0.082(5) Uani 1 d . . . N2 N 0.0506(8) -0.0576(15) 0.9718(10) 0.069(4) Uani 1 d . . . C1 C 0.2601(16) 0.130(3) 0.7925(17) 0.142(10) Uani 1 d . . . H1 H 0.2879 0.2445 0.8118 0.213 Uiso 1 calc R . . H11 H 0.2076 0.1513 0.7452 0.213 Uiso 1 calc R . . H12 H 0.3033 0.0558 0.7519 0.213 Uiso 1 calc R . . C2 C 0.3151(14) -0.016(3) 0.953(2) 0.190(15) Uani 1 d . . . H2 H 0.3553 -0.0771 0.9009 0.285 Uiso 1 calc R . . H21 H 0.2994 -0.0963 1.0143 0.285 Uiso 1 calc R . . H22 H 0.3451 0.0905 0.9830 0.285 Uiso 1 calc R . . C3 C 0.1815(18) -0.133(3) 0.861(2) 0.187(15) Uani 1 d . . . H3 H 0.1773 -0.1332 0.7785 0.225 Uiso 1 calc R . . H31 H 0.2211 -0.2343 0.8814 0.225 Uiso 1 calc R . . C4 C 0.1028(14) -0.174(2) 0.898(3) 0.153(12) Uani 1 d . . . H4 H 0.1088 -0.2900 0.9364 0.184 Uiso 1 calc R . . H41 H 0.0651 -0.1956 0.8309 0.184 Uiso 1 calc R . . C5 C -0.0362(11) -0.023(3) 0.916(2) 0.119(8) Uani 1 d . . . H5 H -0.0264 0.0541 0.8504 0.179 Uiso 1 calc R . . H51 H -0.0768 0.0374 0.9679 0.179 Uiso 1 calc R . . H52 H -0.0627 -0.1361 0.8917 0.179 Uiso 1 calc R . . C6 C 0.034(2) -0.169(3) 1.0742(19) 0.163(12) Uani 1 d . . . H6 H -0.0019 -0.2731 1.0544 0.244 Uiso 1 calc R . . H61 H 0.0023 -0.0969 1.1300 0.244 Uiso 1 calc R . . H62 H 0.0917 -0.2081 1.1052 0.244 Uiso 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 Ge 0.0573(6) 0.0319(4) 0.0512(5) -0.0026(9) -0.0017(9) 0.0024(5) Cl1 0.079(2) 0.0416(14) 0.127(4) -0.003(3) -0.006(3) -0.0130(14) Cl2 0.111(4) 0.081(3) 0.129(5) -0.029(3) 0.056(3) 0.006(3) Cl3 0.141(4) 0.069(3) 0.080(3) 0.017(2) -0.047(3) -0.013(3) Cl4 0.132(4) 0.055(2) 0.092(3) 0.011(2) -0.042(3) 0.004(3) N1 0.105(12) 0.047(7) 0.094(11) -0.006(7) 0.052(9) -0.001(7) N2 0.069(7) 0.051(6) 0.087(11) -0.010(6) -0.016(6) -0.014(6) C1 0.19(2) 0.104(14) 0.135(19) -0.001(14) 0.109(18) -0.021(15) C2 0.126(18) 0.19(2) 0.25(4) -0.01(2) 0.04(2) 0.122(18) C3 0.23(3) 0.092(14) 0.24(3) -0.107(17) 0.18(3) -0.066(17) C4 0.124(16) 0.051(9) 0.29(3) -0.084(16) 0.05(2) -0.016(11) C5 0.066(11) 0.083(12) 0.21(2) -0.001(14) -0.055(13) -0.025(10) C6 0.23(3) 0.15(2) 0.104(16) 0.034(16) -0.04(2) -0.12(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 Ge N1 2.148(12) . ? Ge N2 2.156(10) . ? Ge Cl2 2.236(4) . ? Ge Cl1 2.247(3) . ? Ge Cl4 2.248(4) . ? Ge Cl3 2.253(5) . ? N1 C1 1.41(2) . ? N1 C2 1.45(3) . ? N1 C3 1.52(2) . ? N2 C4 1.44(2) . ? N2 C5 1.453(18) . ? N2 C6 1.47(2) . ? C3 C4 1.26(2) . ? 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 Ge N2 85.0(5) . . ? N1 Ge Cl2 175.6(4) . . ? N2 Ge Cl2 90.7(4) . . ? N1 Ge Cl1 89.1(4) . . ? N2 Ge Cl1 174.0(3) . . ? Cl2 Ge Cl1 95.28(18) . . ? N1 Ge Cl4 91.0(5) . . ? N2 Ge Cl4 90.1(3) . . ? Cl2 Ge Cl4 89.3(2) . . ? Cl1 Ge Cl4 89.56(18) . . ? N1 Ge Cl3 90.9(5) . . ? N2 Ge Cl3 90.6(3) . . ? Cl2 Ge Cl3 88.8(2) . . ? Cl1 Ge Cl3 90.0(2) . . ? Cl4 Ge Cl3 178.0(2) . . ? C1 N1 C2 107.4(17) . . ? C1 N1 C3 108.8(17) . . ? C2 N1 C3 107.5(17) . . ? C1 N1 Ge 116.8(12) . . ? C2 N1 Ge 113.5(13) . . ? C3 N1 Ge 102.3(10) . . ? C4 N2 C5 107.2(16) . . ? C4 N2 C6 104.7(17) . . ? C5 N2 C6 109.0(15) . . ? C4 N2 Ge 105.1(10) . . ? C5 N2 Ge 115.7(10) . . ? C6 N2 Ge 114.3(10) . . ? C4 C3 N1 124.2(16) . . ? C3 C4 N2 123.4(15) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.06 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.646 _refine_diff_density_min -1.052 _refine_diff_density_rms 0.141 data_2 _database_code_CSD 171327 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C6 H16 Cl2 Ge N8' _chemical_formula_sum 'C6 H16 Cl2 Ge N8' _chemical_formula_weight 343.76 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 monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 8.570(2) _cell_length_b 13.350(3) _cell_length_c 12.227(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.63(3) _cell_angle_gamma 90.00 _cell_volume 1325.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 9 _cell_measurement_theta_max 11 _exptl_crystal_description needles _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.722 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 2.707 _exptl_absorpt_correction_type no _exptl_absorpt_correction_T_min no _exptl_absorpt_correction_T_max no _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 'KUMA KM4' _diffrn_measurement_method 'omega-2theta' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% no _diffrn_reflns_number 2511 _diffrn_reflns_av_R_equivalents 0.0972 _diffrn_reflns_av_sigmaI/netI 0.0927 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 25.06 _reflns_number_total 1174 _reflns_number_gt 1000 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KUMA KM4 software' _computing_cell_refinement 'KUMA KM4 software' _computing_data_reduction 'KUMA KM4 software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ 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 w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+3.5439P] where P=(Fo^2^+2Fc^2^)/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 1174 _refine_ls_number_parameters 78 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0485 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.1066 _refine_ls_wR_factor_gt 0.1020 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.033 _refine_ls_shift/su_mean 0.004 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ge Ge 0.0000 0.34890(4) 0.7500 0.0210(2) Uani 1 d S . . Cl1 Cl 0.19718(13) 0.23287(7) 0.82975(8) 0.0337(3) Uani 1 d . . . N1 N 0.1665(4) 0.4682(2) 0.8245(3) 0.0251(7) Uani 1 d . . . N2 N 0.0685(4) 0.3575(2) 0.6132(3) 0.0266(7) Uani 1 d . . . N3 N 0.0808(4) 0.2786(2) 0.5671(3) 0.0262(7) Uani 1 d . . . N4 N 0.0957(4) 0.2073(3) 0.5215(3) 0.0376(8) Uani 1 d . . . C1 C 0.2451(5) 0.4581(3) 0.9521(3) 0.0345(10) Uani 1 d . . . H1 H 0.3075 0.3971 0.9688 0.041 Uiso 1 d R . . H11 H 0.1614 0.4568 0.9888 0.041 Uiso 1 d R . . H12 H 0.3170 0.5141 0.9807 0.041 Uiso 1 d R . . C2 C 0.3051(5) 0.4786(4) 0.7769(4) 0.0443(12) Uani 1 d . . . H2 H 0.3677 0.4177 0.7896 0.053 Uiso 1 d R . . H21 H 0.3747 0.5330 0.8149 0.053 Uiso 1 d R . . H22 H 0.2623 0.4920 0.6956 0.053 Uiso 1 d R . . C3 C 0.0637(6) 0.5608(3) 0.8065(4) 0.0447(12) Uani 1 d . . . H3 H 0.0122 0.5654 0.8664 0.054 Uiso 1 d R . . H31 H 0.1338 0.6190 0.8128 0.054 Uiso 1 d 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 Ge 0.0306(3) 0.0143(3) 0.0198(3) 0.000 0.0104(2) 0.000 Cl1 0.0480(6) 0.0239(5) 0.0292(6) 0.0040(4) 0.0122(5) 0.0096(4) N1 0.0267(16) 0.0230(16) 0.0235(15) 0.0050(13) 0.0050(13) -0.0006(14) N2 0.0444(19) 0.0199(16) 0.0216(15) 0.0029(13) 0.0190(15) 0.0061(14) N3 0.0307(17) 0.0268(17) 0.0231(16) 0.0032(14) 0.0114(14) 0.0076(15) N4 0.044(2) 0.0301(19) 0.041(2) -0.0055(17) 0.0171(17) 0.0071(17) C1 0.039(2) 0.033(2) 0.030(2) -0.0046(18) 0.0083(18) -0.010(2) C2 0.036(2) 0.063(3) 0.036(2) -0.002(2) 0.0141(18) -0.018(2) C3 0.041(2) 0.020(2) 0.063(3) 0.005(2) 0.003(2) -0.0033(19) _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 Ge N2 1.945(3) . ? Ge N2 1.945(3) 2_556 ? Ge N1 2.138(3) . ? Ge N1 2.138(3) 2_556 ? Ge Cl1 2.2700(11) 2_556 ? Ge Cl1 2.2700(11) . ? N1 C2 1.486(5) . ? N1 C3 1.493(5) . ? N1 C1 1.496(5) . ? N2 N3 1.215(4) . ? N3 N4 1.132(5) . ? C3 C3 1.463(9) 2_556 ? 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 Ge N2 173.20(17) . 2_556 ? N2 Ge N1 88.76(13) . . ? N2 Ge N1 86.18(13) 2_556 . ? N2 Ge N1 86.18(12) . 2_556 ? N2 Ge N1 88.76(13) 2_556 2_556 ? N1 Ge N1 83.69(17) . 2_556 ? N2 Ge Cl1 93.37(11) . 2_556 ? N2 Ge Cl1 91.27(10) 2_556 2_556 ? N1 Ge Cl1 174.35(9) . 2_556 ? N1 Ge Cl1 91.24(9) 2_556 2_556 ? N2 Ge Cl1 91.27(10) . . ? N2 Ge Cl1 93.37(11) 2_556 . ? N1 Ge Cl1 91.24(9) . . ? N1 Ge Cl1 174.35(9) 2_556 . ? Cl1 Ge Cl1 93.94(6) 2_556 . ? C2 N1 C3 111.9(4) . . ? C2 N1 C1 105.5(3) . . ? C3 N1 C1 106.0(3) . . ? C2 N1 Ge 114.3(3) . . ? C3 N1 Ge 105.8(2) . . ? C1 N1 Ge 113.2(2) . . ? N3 N2 Ge 116.3(2) . . ? N4 N3 N2 177.0(4) . . ? C3 C3 N1 111.5(3) 2_556 . ? _diffrn_measured_fraction_theta_max 0.476 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.476 _refine_diff_density_max 1.067 _refine_diff_density_min -0.426 _refine_diff_density_rms 0.106