# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_author_address ;Department Chemie, Technische Universitaet Muenchen, D-85747 Garching Germany ; _publ_contact_author_address ;Department Chemie, Technische Universitaet Muenchen, D-85747 Garching Germany ; _publ_contact_author_email thomas.faessler@lrz.tum.de _publ_contact_author_fax '(+49) 89-289-13186' _publ_contact_author_phone '(+49) 89-289-13131' _publ_contact_author_name 'Thomas F. Faessler' loop_ _publ_author_name 'Markus Waibel' 'Thomas Henneberger' 'Thomas F. Faessler' data_1_edit _database_code_depnum_ccdc_archive 'CCDC 876865' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C0 H33 Ge3.30 K6 N11 O0 Si4.70 Zn' _chemical_formula_weight 858.69 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' O O 0.0106 0.0060 '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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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 ? _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0694(5) _cell_length_b 11.4274(5) _cell_length_c 15.8894(8) _cell_angle_alpha 77.468(4) _cell_angle_beta 81.547(4) _cell_angle_gamma 87.070(4) _cell_volume 1589.76(14) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.794 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 851 _exptl_absorpt_coefficient_mu 4.802 _exptl_absorpt_correction_T_min 0.91942 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14506 _diffrn_reflns_av_R_equivalents 0.0593 _diffrn_reflns_av_sigmaI/netI 0.1587 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.20 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7193 _reflns_number_gt 3788 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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. The positions and the ADP of the particular Si and Ge atoms were set to be equal. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0280P)^2^+0.0000P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7193 _refine_ls_number_parameters 255 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0895 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.0863 _refine_ls_wR_factor_gt 0.0785 _refine_ls_goodness_of_fit_ref 0.790 _refine_ls_restrained_S_all 0.790 _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 K1 K 0.58105(15) 0.45658(11) 0.40563(9) 0.0273(3) Uani 1 1 d . . . K2 K 0.62906(14) 0.36622(11) 0.08712(8) 0.0223(3) Uani 1 1 d . . . K3 K 1.14332(15) 0.35265(12) 0.12995(9) 0.0270(3) Uani 1 1 d . . . K4 K 0.36284(15) 0.86605(12) 0.11148(10) 0.0342(4) Uani 1 1 d . . . K5 K 0.98362(14) 0.75995(11) 0.25585(8) 0.0230(3) Uani 1 1 d . . . K6 K 1.11314(15) 0.09832(11) 0.54971(9) 0.0261(3) Uani 1 1 d . . . Si1 Si 0.81404(9) 0.21377(7) 0.43284(5) 0.0207(3) Uani 0.379(4) 1 d P . . Si2 Si 1.03994(9) 0.17344(7) 0.32473(5) 0.0193(3) Uani 0.396(4) 1 d P . . Si3 Si 0.97445(13) 0.37730(10) 0.34496(8) 0.0184(4) Uani 0.785(4) 1 d P . . Si4 Si 0.80320(12) 0.25785(9) 0.27546(7) 0.0188(4) Uani 0.728(4) 1 d P . . Si5 Si 0.64200(11) 0.65576(9) 0.20082(7) 0.0171(4) Uani 0.683(4) 1 d P . . Si6 Si 0.86820(13) 0.62170(11) 0.08301(8) 0.0179(5) Uani 0.824(4) 1 d P . . Si7 Si 0.61344(10) 0.66121(8) 0.04850(6) 0.0178(3) Uani 0.539(4) 1 d P . . Si8 Si 0.76047(9) 0.82169(7) 0.08714(5) 0.0206(3) Uani 0.369(4) 1 d P . . Ge1 Ge 0.81404(9) 0.21377(7) 0.43284(5) 0.0207(3) Uani 0.621(4) 1 d P . . Ge2 Ge 1.03994(9) 0.17344(7) 0.32473(5) 0.0193(3) Uani 0.604(4) 1 d P . . Ge3 Ge 0.97445(13) 0.37730(10) 0.34496(8) 0.0184(4) Uani 0.215(4) 1 d P . . Ge4 Ge 0.80320(12) 0.25785(9) 0.27546(7) 0.0188(4) Uani 0.272(4) 1 d P . . Ge5 Ge 0.64200(11) 0.65576(9) 0.20082(7) 0.0171(4) Uani 0.317(4) 1 d P . . Ge6 Ge 0.86820(13) 0.62170(11) 0.08301(8) 0.0179(5) Uani 0.176(4) 1 d P . . Ge7 Ge 0.61344(10) 0.66121(8) 0.04850(6) 0.0178(3) Uani 0.461(4) 1 d P . . Ge8 Ge 0.76047(9) 0.82169(7) 0.08714(5) 0.0206(3) Uani 0.631(4) 1 d P . . Zn1 Zn 0.82982(7) 0.48303(5) 0.22658(4) 0.01647(18) Uani 1 1 d . . . N1 N 1.0986(5) 0.3485(4) 0.5585(3) 0.0201(11) Uani 1 1 d . . . H1A H 1.0787 0.3550 0.6152 0.030 Uiso 1 1 calc R . . H1B H 1.0250 0.3864 0.5289 0.030 Uiso 1 1 calc R . . H1C H 1.1874 0.3829 0.5342 0.030 Uiso 1 1 calc R . . N2 N 0.4551(5) 0.2891(4) 0.5614(3) 0.0249(12) Uani 1 1 d . . . H2A H 0.4095 0.3305 0.6012 0.037 Uiso 1 1 calc R . . H2B H 0.5292 0.2414 0.5842 0.037 Uiso 1 1 calc R . . H2C H 0.3873 0.2430 0.5476 0.037 Uiso 1 1 calc R . . N3 N 0.2861(5) 0.5566(4) 0.3988(3) 0.0296(13) Uani 1 1 d . . . H3A H 0.2218 0.4975 0.3999 0.044 Uiso 1 1 calc R . . H3B H 0.2848 0.6132 0.3488 0.044 Uiso 1 1 calc R . . H3C H 0.2579 0.5908 0.4455 0.044 Uiso 1 1 calc R . . N4 N 1.3944(6) 0.1005(5) 0.4364(3) 0.0359(14) Uani 1 1 d . . . H4A H 1.3799 0.1320 0.3804 0.054 Uiso 1 1 calc R . . H4B H 1.4314 0.0243 0.4405 0.054 Uiso 1 1 calc R . . H4C H 1.4602 0.1460 0.4526 0.054 Uiso 1 1 calc R . . N5 N 1.2170(5) 0.6302(4) 0.1713(3) 0.0279(13) Uani 1 1 d . . . H5A H 1.3043 0.6694 0.1642 0.042 Uiso 1 1 calc R . . H5B H 1.1945 0.6248 0.1183 0.042 Uiso 1 1 calc R . . H5C H 1.2263 0.5553 0.2044 0.042 Uiso 1 1 calc R . . N6 N 0.0856(5) 0.9912(4) 0.1303(3) 0.0261(12) Uani 1 1 d . . . H6A H 0.0788 1.0253 0.1775 0.039 Uiso 1 1 calc R . . H6B H 0.0099 0.9390 0.1378 0.039 Uiso 1 1 calc R . . H6C H 0.0793 1.0493 0.0817 0.039 Uiso 1 1 calc R . . N7 N 0.4046(5) 0.3573(4) 0.2403(3) 0.0274(12) Uani 1 1 d . . . H7A H 0.3165 0.3334 0.2292 0.041 Uiso 1 1 calc R . . H7B H 0.3923 0.4314 0.2529 0.041 Uiso 1 1 calc R . . H7C H 0.4351 0.3043 0.2863 0.041 Uiso 1 1 calc R . . N8 N 1.2599(6) 0.0597(4) 0.7038(3) 0.0270(12) Uani 1 1 d . . . H8A H 1.3605 0.0594 0.6879 0.040 Uiso 1 1 calc R . . H8B H 1.2323 -0.0120 0.7390 0.040 Uiso 1 1 calc R . . H8C H 1.2331 0.1196 0.7328 0.040 Uiso 1 1 calc R . . N9 N 0.8079(5) 0.1666(4) 0.0433(3) 0.0328(13) Uani 1 1 d . . . H9A H 0.8525 0.1290 0.0898 0.049 Uiso 1 1 calc R . . H9B H 0.8789 0.1937 -0.0027 0.049 Uiso 1 1 calc R . . H9C H 0.7488 0.1142 0.0288 0.049 Uiso 1 1 calc R . . N10 N 1.2255(6) 0.8668(4) 0.3222(3) 0.0363(15) Uani 1 1 d . . . H10A H 1.2279 0.8314 0.3791 0.054 Uiso 1 1 calc R . . H10B H 1.2075 0.9469 0.3173 0.054 Uiso 1 1 calc R . . H10C H 1.3148 0.8546 0.2905 0.054 Uiso 1 1 calc R . . N11 N 0.4343(6) 1.0813(4) 0.1558(4) 0.0430(15) Uani 1 1 d . . . H11A H 0.4469 1.1406 0.1070 0.065 Uiso 1 1 calc R . . H11B H 0.5200 1.0700 0.1802 0.065 Uiso 1 1 calc R . . H11C H 0.3589 1.1024 0.1945 0.065 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 K1 0.0274(8) 0.0229(7) 0.0261(8) -0.0007(6) 0.0058(6) 0.0046(6) K2 0.0241(8) 0.0198(7) 0.0262(8) -0.0069(6) -0.0106(6) 0.0000(5) K3 0.0267(8) 0.0317(8) 0.0204(8) -0.0030(6) 0.0008(6) -0.0034(6) K4 0.0222(8) 0.0240(8) 0.0592(11) -0.0156(7) -0.0058(7) 0.0020(6) K5 0.0213(7) 0.0248(7) 0.0242(8) -0.0068(6) -0.0047(6) -0.0010(5) K6 0.0300(8) 0.0178(7) 0.0336(9) -0.0063(6) -0.0121(7) -0.0044(6) Si1 0.0197(5) 0.0197(5) 0.0199(5) -0.0006(4) 0.0003(4) 0.0020(3) Si2 0.0182(5) 0.0169(5) 0.0216(6) -0.0021(4) -0.0029(4) 0.0029(3) Si3 0.0175(7) 0.0139(7) 0.0247(8) -0.0024(5) -0.0080(6) -0.0021(5) Si4 0.0214(7) 0.0139(7) 0.0222(8) -0.0018(5) -0.0091(5) -0.0025(5) Si5 0.0172(6) 0.0152(6) 0.0180(7) -0.0011(5) -0.0032(5) 0.0007(4) Si6 0.0153(7) 0.0193(8) 0.0180(8) -0.0003(5) -0.0044(6) 0.0005(5) Si7 0.0157(6) 0.0198(6) 0.0206(6) -0.0077(4) -0.0062(4) 0.0010(4) Si8 0.0224(5) 0.0146(5) 0.0249(6) -0.0006(4) -0.0073(4) -0.0050(3) Ge1 0.0197(5) 0.0197(5) 0.0199(5) -0.0006(4) 0.0003(4) 0.0020(3) Ge2 0.0182(5) 0.0169(5) 0.0216(6) -0.0021(4) -0.0029(4) 0.0029(3) Ge3 0.0175(7) 0.0139(7) 0.0247(8) -0.0024(5) -0.0080(6) -0.0021(5) Ge4 0.0214(7) 0.0139(7) 0.0222(8) -0.0018(5) -0.0091(5) -0.0025(5) Ge5 0.0172(6) 0.0152(6) 0.0180(7) -0.0011(5) -0.0032(5) 0.0007(4) Ge6 0.0153(7) 0.0193(8) 0.0180(8) -0.0003(5) -0.0044(6) 0.0005(5) Ge7 0.0157(6) 0.0198(6) 0.0206(6) -0.0077(4) -0.0062(4) 0.0010(4) Ge8 0.0224(5) 0.0146(5) 0.0249(6) -0.0006(4) -0.0073(4) -0.0050(3) Zn1 0.0164(4) 0.0131(4) 0.0196(4) -0.0010(3) -0.0050(3) -0.0005(3) N1 0.020(3) 0.027(3) 0.012(3) 0.000(2) -0.003(2) -0.001(2) N2 0.019(3) 0.019(3) 0.041(3) -0.013(2) -0.008(2) 0.002(2) N3 0.027(3) 0.024(3) 0.041(4) -0.010(3) -0.010(3) -0.004(2) N4 0.038(4) 0.033(3) 0.042(4) -0.015(3) -0.014(3) 0.001(3) N5 0.032(3) 0.017(3) 0.038(3) -0.006(2) -0.015(3) -0.004(2) N6 0.027(3) 0.023(3) 0.028(3) -0.001(2) -0.005(2) -0.002(2) N7 0.028(3) 0.031(3) 0.025(3) -0.006(2) -0.007(2) -0.006(2) N8 0.034(3) 0.018(3) 0.027(3) 0.001(2) -0.004(3) -0.004(2) N9 0.024(3) 0.029(3) 0.044(4) -0.001(3) -0.011(3) -0.002(2) N10 0.065(4) 0.023(3) 0.023(3) -0.003(2) -0.015(3) 0.001(3) N11 0.037(4) 0.029(3) 0.059(4) 0.000(3) -0.005(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 K1 N3 2.862(5) . ? K1 N2 2.903(5) . ? K1 N2 3.056(4) 2_666 ? K1 Zn1 3.3294(15) . ? K1 Si1 3.3911(15) . ? K1 K1 3.462(3) 2_666 ? K1 N3 3.466(5) 2_666 ? K1 Si5 3.5301(17) . ? K1 Si3 3.6765(18) . ? K2 N9 2.881(5) . ? K2 N7 2.921(5) . ? K2 Si7 3.2922(15) . ? K2 Ge7 3.3670(15) 2_665 ? K2 Si7 3.3670(15) 2_665 ? K2 Si4 3.5447(17) . ? K2 Zn1 3.5673(14) . ? K2 Si6 3.7087(17) . ? K2 K3 4.3631(19) 1_455 ? K3 N7 3.157(5) 1_655 ? K3 Ge6 3.3492(18) 2_765 ? K3 Si6 3.3492(18) 2_765 ? K3 Si2 3.3534(16) . ? K3 Ge7 3.3543(16) 2_765 ? K3 Si7 3.3543(16) 2_765 ? K3 Zn1 3.4551(14) . ? K3 Si3 3.5962(18) . ? K3 Si4 3.6322(18) . ? K4 N11 2.831(5) . ? K4 N6 2.838(5) . ? K4 N5 2.966(5) 1_455 ? K4 N9 3.188(5) 2_665 ? K4 Si7 3.3838(16) . ? K4 N10 3.398(5) 1_455 ? K4 Si8 3.5916(16) . ? K4 Si5 3.6269(17) . ? K4 K5 3.932(2) 1_455 ? K5 N5 2.862(5) . ? K5 N1 2.942(5) 2_766 ? K5 N10 2.988(5) . ? K5 N8 3.038(5) 2_766 ? K5 N6 3.039(5) 1_655 ? K5 Si8 3.5225(15) . ? K5 Si5 3.6615(17) . ? K5 Zn1 3.6683(14) . ? K5 Si6 3.7457(18) . ? K6 N1 2.888(4) . ? K6 N4 2.896(5) . ? K6 N8 2.896(5) . ? K6 Ge2 3.5341(16) 2_756 ? K6 Si2 3.5341(16) 2_756 ? K6 Si1 3.5495(16) . ? K6 Ge1 3.5519(14) 2_756 ? K6 Si1 3.5519(14) 2_756 ? K6 Si2 3.6420(16) . ? K6 K5 3.7641(18) 2_766 ? Si1 Si4 2.4571(14) . ? Si1 Si3 2.4712(15) . ? Si1 Si2 2.5637(11) . ? Si1 K6 3.5519(14) 2_756 ? Si2 Si3 2.4517(13) . ? Si2 Si4 2.4714(13) . ? Si2 K6 3.5340(16) 2_756 ? Si3 Zn1 2.5091(13) . ? Si3 Si4 2.6211(16) . ? Si4 Zn1 2.5345(12) . ? Si5 Si7 2.4588(14) . ? Si5 Si8 2.4827(13) . ? Si5 Zn1 2.5448(11) . ? Si5 Si6 2.6401(16) . ? Si6 Si8 2.4494(14) . ? Si6 Si7 2.4497(15) . ? Si6 Zn1 2.4679(14) . ? Si6 K3 3.3492(18) 2_765 ? Si7 Si8 2.5489(12) . ? Si7 K3 3.3543(16) 2_765 ? Si7 K2 3.3670(15) 2_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 K1 N2 86.55(14) . . ? N3 K1 N2 65.81(13) . 2_666 ? N2 K1 N2 109.02(11) . 2_666 ? N3 K1 Zn1 121.09(11) . . ? N2 K1 Zn1 143.72(9) . . ? N2 K1 Zn1 104.06(10) 2_666 . ? N3 K1 Si1 149.91(11) . . ? N2 K1 Si1 72.57(9) . . ? N2 K1 Si1 141.14(10) 2_666 . ? Zn1 K1 Si1 72.41(3) . . ? N3 K1 K1 65.66(11) . 2_666 ? N2 K1 K1 56.57(9) . 2_666 ? N2 K1 K1 52.45(10) 2_666 2_666 ? Zn1 K1 K1 152.93(7) . 2_666 ? Si1 K1 K1 115.87(6) . 2_666 ? N3 K1 N3 114.47(10) . 2_666 ? N2 K1 N3 59.95(12) . 2_666 ? N2 K1 N3 74.31(12) 2_666 2_666 ? Zn1 K1 N3 117.58(9) . 2_666 ? Si1 K1 N3 73.81(8) . 2_666 ? K1 K1 N3 48.81(8) 2_666 2_666 ? N3 K1 Si5 80.85(11) . . ? N2 K1 Si5 165.16(10) . . ? N2 K1 Si5 72.87(9) 2_666 . ? Zn1 K1 Si5 43.43(3) . . ? Si1 K1 Si5 115.69(4) . . ? K1 K1 Si5 123.41(6) 2_666 . ? N3 K1 Si5 132.95(9) 2_666 . ? N3 K1 Si3 162.54(12) . . ? N2 K1 Si3 109.99(10) . . ? N2 K1 Si3 111.69(10) 2_666 . ? Zn1 K1 Si3 41.60(3) . . ? Si1 K1 Si3 40.68(3) . . ? K1 K1 Si3 127.80(7) 2_666 . ? N3 K1 Si3 79.89(9) 2_666 . ? Si5 K1 Si3 81.96(4) . . ? N9 K2 N7 125.92(15) . . ? N9 K2 Si7 142.59(11) . . ? N7 K2 Si7 89.83(10) . . ? N9 K2 Ge7 91.75(11) . 2_665 ? N7 K2 Ge7 95.55(10) . 2_665 ? Si7 K2 Ge7 95.65(4) . 2_665 ? N9 K2 Si7 91.75(11) . 2_665 ? N7 K2 Si7 95.55(10) . 2_665 ? Si7 K2 Si7 95.65(4) . 2_665 ? Ge7 K2 Si7 0.00(4) 2_665 2_665 ? N9 K2 Si4 77.14(11) . . ? N7 K2 Si4 71.63(10) . . ? Si7 K2 Si4 109.03(4) . . ? Ge7 K2 Si4 151.75(5) 2_665 . ? Si7 K2 Si4 151.75(5) 2_665 . ? N9 K2 Zn1 105.19(11) . . ? N7 K2 Zn1 78.68(10) . . ? Si7 K2 Zn1 67.90(3) . . ? Ge7 K2 Zn1 162.35(4) 2_665 . ? Si7 K2 Zn1 162.35(4) 2_665 . ? Si4 K2 Zn1 41.75(2) . . ? N9 K2 Si6 110.57(11) . . ? N7 K2 Si6 105.24(10) . . ? Si7 K2 Si6 40.42(3) . . ? Ge7 K2 Si6 129.45(4) 2_665 . ? Si7 K2 Si6 129.45(4) 2_665 . ? Si4 K2 Si6 78.75(4) . . ? Zn1 K2 Si6 39.59(3) . . ? N9 K2 K3 120.96(11) . 1_455 ? N7 K2 K3 46.32(10) . 1_455 ? Si7 K2 K3 90.69(4) . 1_455 ? Ge7 K2 K3 49.40(3) 2_665 1_455 ? Si7 K2 K3 49.40(3) 2_665 1_455 ? Si4 K2 K3 114.96(4) . 1_455 ? Zn1 K2 K3 121.64(4) . 1_455 ? Si6 K2 K3 128.32(4) . 1_455 ? N7 K3 Ge6 133.38(10) 1_655 2_765 ? N7 K3 Si6 133.38(10) 1_655 2_765 ? Ge6 K3 Si6 0.00(6) 2_765 2_765 ? N7 K3 Si2 73.89(9) 1_655 . ? Ge6 K3 Si2 142.07(5) 2_765 . ? Si6 K3 Si2 142.07(5) 2_765 . ? N7 K3 Ge7 91.49(9) 1_655 2_765 ? Ge6 K3 Ge7 42.87(3) 2_765 2_765 ? Si6 K3 Ge7 42.87(3) 2_765 2_765 ? Si2 K3 Ge7 136.77(5) . 2_765 ? N7 K3 Si7 91.49(9) 1_655 2_765 ? Ge6 K3 Si7 42.87(3) 2_765 2_765 ? Si6 K3 Si7 42.87(3) 2_765 2_765 ? Si2 K3 Si7 136.77(5) . 2_765 ? Ge7 K3 Si7 0.00(4) 2_765 2_765 ? N7 K3 Zn1 108.21(9) 1_655 . ? Ge6 K3 Zn1 110.85(4) 2_765 . ? Si6 K3 Zn1 110.85(4) 2_765 . ? Si2 K3 Zn1 72.90(3) . . ? Ge7 K3 Zn1 149.22(5) 2_765 . ? Si7 K3 Zn1 149.22(5) 2_765 . ? N7 K3 Si3 72.86(9) 1_655 . ? Ge6 K3 Si3 151.88(5) 2_765 . ? Si6 K3 Si3 151.88(5) 2_765 . ? Si2 K3 Si3 41.13(3) . . ? Ge7 K3 Si3 164.27(5) 2_765 . ? Si7 K3 Si3 164.27(5) 2_765 . ? Zn1 K3 Si3 41.63(3) . . ? N7 K3 Si4 109.51(9) 1_655 . ? Ge6 K3 Si4 116.45(5) 2_765 . ? Si6 K3 Si4 116.45(5) 2_765 . ? Si2 K3 Si4 41.20(3) . . ? Ge7 K3 Si4 151.08(5) 2_765 . ? Si7 K3 Si4 151.08(5) 2_765 . ? Zn1 K3 Si4 41.81(2) . . ? Si3 K3 Si4 42.52(3) . . ? N11 K4 N6 75.76(15) . . ? N11 K4 N5 146.76(16) . 1_455 ? N6 K4 N5 91.93(14) . 1_455 ? N11 K4 N9 128.56(15) . 2_665 ? N6 K4 N9 73.22(13) . 2_665 ? N5 K4 N9 74.16(13) 1_455 2_665 ? N11 K4 Si7 125.28(12) . . ? N6 K4 Si7 157.74(11) . . ? N5 K4 Si7 73.74(9) 1_455 . ? N9 K4 Si7 86.31(9) 2_665 . ? N11 K4 N10 69.34(15) . 1_455 ? N6 K4 N10 66.79(14) . 1_455 ? N5 K4 N10 77.42(13) 1_455 1_455 ? N9 K4 N10 129.38(14) 2_665 1_455 ? Si7 K4 N10 124.13(10) . 1_455 ? N11 K4 Si8 82.62(12) . . ? N6 K4 Si8 157.71(11) . . ? N5 K4 Si8 109.37(10) 1_455 . ? N9 K4 Si8 118.07(10) 2_665 . ? Si7 K4 Si8 42.74(3) . . ? N10 K4 Si8 110.53(10) 1_455 . ? N11 K4 Si5 102.62(12) . . ? N6 K4 Si5 151.12(11) . . ? N5 K4 Si5 73.58(10) 1_455 . ? N9 K4 Si5 123.87(9) 2_665 . ? Si7 K4 Si5 40.88(3) . . ? N10 K4 Si5 85.45(10) 1_455 . ? Si8 K4 Si5 40.23(3) . . ? N11 K4 K5 106.53(12) . 1_455 ? N6 K4 K5 50.23(10) . 1_455 ? N5 K4 K5 46.46(9) 1_455 1_455 ? N9 K4 K5 83.21(10) 2_665 1_455 ? Si7 K4 K5 119.90(4) . 1_455 ? N10 K4 K5 47.42(9) 1_455 1_455 ? Si8 K4 K5 144.86(5) . 1_455 ? Si5 K4 K5 105.06(4) . 1_455 ? N5 K5 N1 113.12(13) . 2_766 ? N5 K5 N10 86.10(14) . . ? N1 K5 N10 82.74(14) 2_766 . ? N5 K5 N8 164.37(14) . 2_766 ? N1 K5 N8 82.51(12) 2_766 2_766 ? N10 K5 N8 96.67(14) . 2_766 ? N5 K5 N6 89.96(13) . 1_655 ? N1 K5 N6 143.21(13) 2_766 1_655 ? N10 K5 N6 70.16(14) . 1_655 ? N8 K5 N6 76.65(13) 2_766 1_655 ? N5 K5 Si8 97.26(10) . . ? N1 K5 Si8 129.44(10) 2_766 . ? N10 K5 Si8 141.00(11) . . ? N8 K5 Si8 70.96(9) 2_766 . ? N6 K5 Si8 71.00(10) 1_655 . ? N5 K5 Si5 104.04(10) . . ? N1 K5 Si5 91.74(10) 2_766 . ? N10 K5 Si5 169.74(11) . . ? N8 K5 Si5 73.96(10) 2_766 . ? N6 K5 Si5 110.73(10) 1_655 . ? Si8 K5 Si5 40.38(3) . . ? N5 K5 Zn1 71.51(10) . . ? N1 K5 Zn1 82.84(9) 2_766 . ? N10 K5 Zn1 145.84(10) . . ? N8 K5 Zn1 111.90(10) 2_766 . ? N6 K5 Zn1 133.07(10) 1_655 . ? Si8 K5 Zn1 69.28(3) . . ? Si5 K5 Zn1 40.63(2) . . ? N5 K5 Si6 65.64(10) . . ? N1 K5 Si6 120.92(10) 2_766 . ? N10 K5 Si6 148.09(11) . . ? N8 K5 Si6 106.81(10) 2_766 . ? N6 K5 Si6 94.22(10) 1_655 . ? Si8 K5 Si6 39.24(3) . . ? Si5 K5 Si6 41.74(3) . . ? Zn1 K5 Si6 38.87(3) . . ? N1 K6 N4 98.07(14) . . ? N1 K6 N8 85.96(13) . . ? N4 K6 N8 92.25(15) . . ? N1 K6 Ge2 137.47(10) . 2_756 ? N4 K6 Ge2 121.05(11) . 2_756 ? N8 K6 Ge2 77.15(10) . 2_756 ? N1 K6 Si2 137.47(10) . 2_756 ? N4 K6 Si2 121.05(11) . 2_756 ? N8 K6 Si2 77.15(10) . 2_756 ? Ge2 K6 Si2 0.00(3) 2_756 2_756 ? N1 K6 Si1 76.84(10) . . ? N4 K6 Si1 112.16(11) . . ? N8 K6 Si1 151.66(10) . . ? Ge2 K6 Si1 100.53(4) 2_756 . ? Si2 K6 Si1 100.53(4) 2_756 . ? N1 K6 Ge1 168.51(10) . 2_756 ? N4 K6 Ge1 79.04(10) . 2_756 ? N8 K6 Ge1 83.06(9) . 2_756 ? Ge2 K6 Ge1 42.42(2) 2_756 2_756 ? Si2 K6 Ge1 42.42(2) 2_756 2_756 ? Si1 K6 Ge1 114.59(4) . 2_756 ? N1 K6 Si1 168.51(10) . 2_756 ? N4 K6 Si1 79.04(10) . 2_756 ? N8 K6 Si1 83.06(9) . 2_756 ? Ge2 K6 Si1 42.42(2) 2_756 2_756 ? Si2 K6 Si1 42.42(2) 2_756 2_756 ? Si1 K6 Si1 114.59(4) . 2_756 ? Ge1 K6 Si1 0.00(4) 2_756 2_756 ? N1 K6 Si2 91.07(9) . . ? N4 K6 Si2 71.44(11) . . ? N8 K6 Si2 162.87(11) . . ? Ge2 K6 Si2 115.38(4) 2_756 . ? Si2 K6 Si2 115.38(4) 2_756 . ? Si1 K6 Si2 41.75(2) . . ? Ge1 K6 Si2 98.43(3) 2_756 . ? Si1 K6 Si2 98.43(3) 2_756 . ? N1 K6 K5 50.41(9) . 2_766 ? N4 K6 K5 128.44(10) . 2_766 ? N8 K6 K5 52.31(10) . 2_766 ? Ge2 K6 K5 89.53(4) 2_756 2_766 ? Si2 K6 K5 89.53(4) 2_756 2_766 ? Si1 K6 K5 99.76(4) . 2_766 ? Ge1 K6 K5 123.16(4) 2_756 2_766 ? Si1 K6 K5 123.16(4) 2_756 2_766 ? Si2 K6 K5 134.96(4) . 2_766 ? Si4 Si1 Si3 64.26(4) . . ? Si4 Si1 Si2 58.93(4) . . ? Si3 Si1 Si2 58.25(4) . . ? Si4 Si1 K1 77.18(4) . . ? Si3 Si1 K1 75.88(4) . . ? Si2 Si1 K1 126.02(4) . . ? Si4 Si1 K6 129.98(5) . . ? Si3 Si1 K6 89.73(4) . . ? Si2 Si1 K6 71.06(3) . . ? K1 Si1 K6 139.67(4) . . ? Si4 Si1 K6 95.27(4) . 2_756 ? Si3 Si1 K6 126.14(4) . 2_756 ? Si2 Si1 K6 68.42(3) . 2_756 ? K1 Si1 K6 151.24(4) . 2_756 ? K6 Si1 K6 65.41(4) . 2_756 ? Si3 Si2 Si4 64.33(4) . . ? Si3 Si2 Si1 58.99(4) . . ? Si4 Si2 Si1 58.38(4) . . ? Si3 Si2 K3 74.76(4) . . ? Si4 Si2 K3 75.46(4) . . ? Si1 Si2 K3 124.45(4) . . ? Si3 Si2 K6 127.61(5) . 2_756 ? Si4 Si2 K6 95.45(4) . 2_756 ? Si1 Si2 K6 69.16(3) . 2_756 ? K3 Si2 K6 149.89(4) . 2_756 ? Si3 Si2 K6 87.90(4) . . ? Si4 Si2 K6 125.57(4) . . ? Si1 Si2 K6 67.20(3) . . ? K3 Si2 K6 143.48(4) . . ? K6 Si2 K6 64.62(4) 2_756 . ? Si2 Si3 Si1 62.77(4) . . ? Si2 Si3 Zn1 109.29(5) . . ? Si1 Si3 Zn1 105.71(5) . . ? Si2 Si3 Si4 58.20(4) . . ? Si1 Si3 Si4 57.61(4) . . ? Zn1 Si3 Si4 59.16(4) . . ? Si2 Si3 K3 64.11(4) . . ? Si1 Si3 K3 118.59(5) . . ? Zn1 Si3 K3 66.17(4) . . ? Si4 Si3 K3 69.47(4) . . ? Si2 Si3 K1 119.11(5) . . ? Si1 Si3 K1 63.44(4) . . ? Zn1 Si3 K1 61.77(4) . . ? Si4 Si3 K1 70.14(4) . . ? K3 Si3 K1 125.15(4) . . ? Si1 Si4 Si2 62.69(4) . . ? Si1 Si4 Zn1 105.36(4) . . ? Si2 Si4 Zn1 107.84(5) . . ? Si1 Si4 Si3 58.13(4) . . ? Si2 Si4 Si3 57.47(4) . . ? Zn1 Si4 Si3 58.21(4) . . ? Si1 Si4 K2 154.18(5) . . ? Si2 Si4 K2 143.09(5) . . ? Zn1 Si4 K2 69.60(3) . . ? Si3 Si4 K2 127.13(5) . . ? Si1 Si4 K3 117.76(5) . . ? Si2 Si4 K3 63.34(4) . . ? Zn1 Si4 K3 65.35(4) . . ? Si3 Si4 K3 68.01(4) . . ? K2 Si4 K3 83.97(4) . . ? Si1 Si4 K1 62.73(4) . . ? Si2 Si4 K1 117.00(5) . . ? Zn1 Si4 K1 60.87(3) . . ? Si3 Si4 K1 68.35(4) . . ? K2 Si4 K1 94.43(4) . . ? K3 Si4 K1 122.81(4) . . ? Si7 Si5 Si8 62.10(4) . . ? Si7 Si5 Zn1 100.15(4) . . ? Si8 Si5 Zn1 108.84(4) . . ? Si7 Si5 Si6 57.30(4) . . ? Si8 Si5 Si6 57.03(4) . . ? Zn1 Si5 Si6 56.81(4) . . ? Si7 Si5 K1 138.83(5) . . ? Si8 Si5 K1 157.12(5) . . ? Zn1 Si5 K1 64.08(3) . . ? Si6 Si5 K1 120.89(5) . . ? Si7 Si5 K4 64.25(4) . . ? Si8 Si5 K4 69.12(4) . . ? Zn1 Si5 K4 163.70(5) . . ? Si6 Si5 K4 113.10(5) . . ? K1 Si5 K4 124.01(4) . . ? Si7 Si5 K5 120.72(5) . . ? Si8 Si5 K5 66.80(4) . . ? Zn1 Si5 K5 69.83(3) . . ? Si6 Si5 K5 70.84(4) . . ? K1 Si5 K5 90.67(4) . . ? K4 Si5 K5 121.21(4) . . ? Si8 Si6 Si7 62.70(4) . . ? Si8 Si6 Zn1 112.52(5) . . ? Si7 Si6 Zn1 102.59(5) . . ? Si8 Si6 Si5 58.25(4) . . ? Si7 Si6 Si5 57.63(4) . . ? Zn1 Si6 Si5 59.65(4) . . ? Si8 Si6 K3 94.66(5) . 2_765 ? Si7 Si6 K3 68.68(4) . 2_765 ? Zn1 Si6 K3 144.12(5) . 2_765 ? Si5 Si6 K3 126.13(5) . 2_765 ? Si8 Si6 K2 121.12(5) . . ? Si7 Si6 K2 60.61(4) . . ? Zn1 Si6 K2 67.11(4) . . ? Si5 Si6 K2 78.80(4) . . ? K3 Si6 K2 79.05(4) 2_765 . ? Si8 Si6 K5 65.46(4) . . ? Si7 Si6 K5 118.01(5) . . ? Zn1 Si6 K5 68.87(4) . . ? Si5 Si6 K5 67.42(4) . . ? K3 Si6 K5 146.66(5) 2_765 . ? K2 Si6 K5 133.81(5) . . ? Si8 Si6 K3 156.91(5) . . ? Si7 Si6 K3 138.96(5) . . ? Zn1 Si6 K3 61.39(3) . . ? Si5 Si6 K3 121.03(5) . . ? K3 Si6 K3 101.47(4) 2_765 . ? K2 Si6 K3 78.55(4) . . ? K5 Si6 K3 92.43(4) . . ? Si6 Si7 Si5 65.07(4) . . ? Si6 Si7 Si8 58.64(4) . . ? Si5 Si7 Si8 59.41(4) . . ? Si6 Si7 K2 78.97(4) . . ? Si5 Si7 K2 90.13(4) . . ? Si8 Si7 K2 134.72(4) . . ? Si6 Si7 K3 68.45(4) . 2_765 ? Si5 Si7 K3 133.32(5) . 2_765 ? Si8 Si7 K3 92.68(4) . 2_765 ? K2 Si7 K3 85.23(4) . 2_765 ? Si6 Si7 K2 146.07(5) . 2_665 ? Si5 Si7 K2 144.78(5) . 2_665 ? Si8 Si7 K2 140.04(4) . 2_665 ? K2 Si7 K2 84.35(4) . 2_665 ? K3 Si7 K2 80.95(4) 2_765 2_665 ? Si6 Si7 K4 127.91(5) . . ? Si5 Si7 K4 74.87(4) . . ? Si8 Si7 K4 72.98(4) . . ? K2 Si7 K4 134.40(5) . . ? K3 Si7 K4 135.84(5) 2_765 . ? K2 Si7 K4 84.38(4) 2_665 . ? Si6 Si8 Si5 64.72(4) . . ? Si6 Si8 Si7 58.66(4) . . ? Si5 Si8 Si7 58.49(4) . . ? Si6 Si8 K5 75.31(4) . . ? Si5 Si8 K5 72.83(4) . . ? Si7 Si8 K5 122.87(4) . . ? Si6 Si8 K4 119.78(4) . . ? Si5 Si8 K4 70.65(4) . . ? Si7 Si8 K4 64.28(3) . . ? K5 Si8 K4 126.40(4) . . ? Si6 Zn1 Si3 140.28(5) . . ? Si6 Zn1 Si4 133.90(5) . . ? Si3 Zn1 Si4 62.62(4) . . ? Si6 Zn1 Si5 63.54(4) . . ? Si3 Zn1 Si5 138.58(4) . . ? Si4 Zn1 Si5 133.07(4) . . ? Si6 Zn1 K1 136.02(4) . . ? Si3 Zn1 K1 76.63(4) . . ? Si4 Zn1 K1 77.45(4) . . ? Si5 Zn1 K1 72.49(4) . . ? Si6 Zn1 K3 79.78(4) . . ? Si3 Zn1 K3 72.20(4) . . ? Si4 Zn1 K3 72.83(4) . . ? Si5 Zn1 K3 143.31(4) . . ? K1 Zn1 K3 144.17(4) . . ? Si6 Zn1 K2 73.29(4) . . ? Si3 Zn1 K2 130.52(4) . . ? Si4 Zn1 K2 68.65(4) . . ? Si5 Zn1 K2 82.78(3) . . ? K1 Zn1 K2 101.24(4) . . ? K3 Zn1 K2 86.26(3) . . ? Si6 Zn1 K5 72.26(4) . . ? Si3 Zn1 K5 85.94(4) . . ? Si4 Zn1 K5 148.47(4) . . ? Si5 Zn1 K5 69.54(3) . . ? K1 Zn1 K5 93.83(3) . . ? K3 Zn1 K5 101.07(3) . . ? K2 Zn1 K5 142.77(3) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.986 _refine_diff_density_min -0.793 _refine_diff_density_rms 0.155 # Attachment '- faessler_K6ZnGe3.9Si4.1N11_2.cif' data_2_edit _database_code_depnum_ccdc_archive 'CCDC 876866' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'H33 Ge3.86 K6 N11 Si4.14 Zn' _chemical_formula_weight 883.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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' H H 0.0000 0.0000 '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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.5430(3) _cell_length_b 12.2351(4) _cell_length_c 13.8927(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.145(3) _cell_angle_gamma 90.00 _cell_volume 1579.60(8) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.858 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 871 _exptl_absorpt_coefficient_mu 5.334 _exptl_absorpt_correction_T_min 0.91719 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12970 _diffrn_reflns_av_R_equivalents 0.0551 _diffrn_reflns_av_sigmaI/netI 0.1068 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.30 _diffrn_reflns_theta_max 26.25 _reflns_number_total 5149 _reflns_number_gt 3248 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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. The positions and the ADP of the particular Si and Ge atoms were set to be equal. The positions of the hydrogen atoms connected to N1 to N11 could not be determined. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment . _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 0.55(3) _refine_ls_number_reflns 5149 _refine_ls_number_parameters 246 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0657 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0792 _refine_ls_wR_factor_gt 0.0746 _refine_ls_goodness_of_fit_ref 0.824 _refine_ls_restrained_S_all 0.824 _refine_ls_shift/su_max 0.002 _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 K1 K 0.97051(17) 0.4832(3) 0.43486(11) 0.0281(4) Uani 1 1 d . . . K2 K 0.2901(3) 0.2475(2) 0.3938(2) 0.0261(7) Uani 1 1 d . . . K3 K 1.1728(2) 0.4988(3) 0.88164(12) 0.0288(6) Uani 1 1 d . . . K4 K 0.2886(3) 0.7141(2) 0.3961(2) 0.0263(7) Uani 1 1 d . . . K5 K 0.4313(3) 0.6918(2) 0.12186(17) 0.0403(6) Uani 1 1 d . . . K6 K 0.5038(2) 0.21447(18) 0.15677(15) 0.0295(5) Uani 1 1 d . . . Ge1 Ge 0.8216(2) 0.59015(11) 0.81142(13) 0.0227(7) Uani 0.695(9) 1 d P . . Ge2 Ge 0.8120(2) 0.38207(11) 0.81523(13) 0.0233(7) Uani 0.671(9) 1 d P . . Ge3 Ge 0.61949(13) 0.4876(2) 0.70602(9) 0.0220(5) Uani 0.364(5) 1 d P . . Ge4 Ge 0.88379(15) 0.4805(2) 0.67808(9) 0.0201(5) Uani 0.282(5) 1 d P . . Ge5 Ge 0.6036(3) 0.37423(17) 0.38047(18) 0.0205(10) Uani 0.292(8) 1 d P . . Ge6 Ge 0.5987(3) 0.58849(16) 0.37639(18) 0.0146(10) Uani 0.249(8) 1 d P . . Ge7 Ge 0.66373(11) 0.47993(18) 0.24497(7) 0.0201(4) Uani 0.618(5) 1 d P . . Ge8 Ge 0.40569(10) 0.47658(16) 0.27150(6) 0.0184(4) Uani 0.681(5) 1 d P . . Si1 Si 0.8216(2) 0.59015(11) 0.81142(13) 0.0227(7) Uani 0.305(9) 1 d P . . Si2 Si 0.8120(2) 0.38207(11) 0.81523(13) 0.0233(7) Uani 0.329(9) 1 d P . . Si3 Si 0.61949(13) 0.4876(2) 0.70602(9) 0.0220(5) Uani 0.636(5) 1 d P . . Si4 Si 0.88379(15) 0.4805(2) 0.67808(9) 0.0201(5) Uani 0.718(5) 1 d P . . Si5 Si 0.6036(3) 0.37423(17) 0.38047(18) 0.0205(10) Uani 0.708(8) 1 d P . . Si6 Si 0.5987(3) 0.58849(16) 0.37639(18) 0.0146(10) Uani 0.751(8) 1 d P . . Si7 Si 0.66373(11) 0.47993(18) 0.24497(7) 0.0201(4) Uani 0.382(5) 1 d P . . Si8 Si 0.40569(10) 0.47658(16) 0.27150(6) 0.0184(4) Uani 0.319(5) 1 d P . . Zn1 Zn 0.66776(8) 0.48346(15) 0.53584(5) 0.0179(2) Uani 1 1 d . . . N1 N 1.4778(7) 0.4773(10) 0.9517(5) 0.0399(18) Uani 1 1 d . . . N2 N 1.2782(7) 0.5011(7) 0.5092(5) 0.025(2) Uani 1 1 d . . . N3 N 0.2656(12) 0.7972(8) -0.0562(8) 0.033(3) Uani 1 1 d . . . N4 N 0.6952(11) 0.6725(8) 0.0471(8) 0.029(3) Uani 1 1 d . . . N5 N 1.1088(12) 0.6121(8) 1.0519(9) 0.037(3) Uani 1 1 d . . . N6 N 1.1390(12) 0.3520(8) 1.0421(8) 0.038(3) Uani 1 1 d . . . N7 N 0.0022(11) 0.6475(8) 0.2829(7) 0.035(3) Uani 1 1 d . . . N8 N 0.0386(10) 0.3612(7) 0.2682(7) 0.030(2) Uani 1 1 d . . . N9 N 0.7849(10) 0.1495(7) 0.2822(6) 0.038(3) Uani 1 1 d . . . N10 N 1.2855(10) 0.3436(7) 0.7496(6) 0.036(2) Uani 1 1 d . . . N11 N 1.0670(9) 0.2670(7) 0.5174(6) 0.040(2) Uani 1 1 d . . . 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 K1 0.0251(9) 0.0354(10) 0.0249(9) -0.0039(19) 0.0079(7) 0.003(2) K2 0.0353(18) 0.0194(16) 0.0259(17) 0.0005(13) 0.0120(14) -0.0047(15) K3 0.0272(10) 0.0402(18) 0.0192(9) 0.0060(12) 0.0056(7) 0.0041(13) K4 0.0267(17) 0.0238(16) 0.0281(18) -0.0013(14) 0.0055(14) 0.0037(15) K5 0.0485(16) 0.0438(16) 0.0336(14) 0.0219(12) 0.0198(12) 0.0195(13) K6 0.0324(13) 0.0312(14) 0.0259(12) -0.0040(10) 0.0088(10) -0.0077(11) Ge1 0.0300(12) 0.0197(11) 0.0185(11) -0.0037(8) 0.0057(9) 0.0013(8) Ge2 0.0339(13) 0.0183(10) 0.0170(11) 0.0041(8) 0.0045(9) -0.0029(8) Ge3 0.0212(8) 0.0313(10) 0.0144(7) -0.0047(14) 0.0059(5) -0.0013(14) Ge4 0.0212(9) 0.0247(10) 0.0140(8) 0.0008(15) 0.0032(6) 0.0011(16) Ge5 0.0265(18) 0.0193(16) 0.0147(15) -0.0020(11) 0.0027(12) -0.0027(12) Ge6 0.0227(17) 0.0087(14) 0.0124(15) -0.0007(11) 0.0043(12) 0.0004(11) Ge7 0.0236(6) 0.0235(7) 0.0150(5) 0.0006(11) 0.0078(4) 0.0006(11) Ge8 0.0184(6) 0.0204(7) 0.0154(5) 0.0006(9) 0.0022(4) -0.0010(10) Si1 0.0300(12) 0.0197(11) 0.0185(11) -0.0037(8) 0.0057(9) 0.0013(8) Si2 0.0339(13) 0.0183(10) 0.0170(11) 0.0041(8) 0.0045(9) -0.0029(8) Si3 0.0212(8) 0.0313(10) 0.0144(7) -0.0047(14) 0.0059(5) -0.0013(14) Si4 0.0212(9) 0.0247(10) 0.0140(8) 0.0008(15) 0.0032(6) 0.0011(16) Si5 0.0265(18) 0.0193(16) 0.0147(15) -0.0020(11) 0.0027(12) -0.0027(12) Si6 0.0227(17) 0.0087(14) 0.0124(15) -0.0007(11) 0.0043(12) 0.0004(11) Si7 0.0236(6) 0.0235(7) 0.0150(5) 0.0006(11) 0.0078(4) 0.0006(11) Si8 0.0184(6) 0.0204(7) 0.0154(5) 0.0006(9) 0.0022(4) -0.0010(10) Zn1 0.0236(5) 0.0189(5) 0.0114(4) -0.0005(8) 0.0045(3) -0.0002(9) N1 0.039(4) 0.028(4) 0.049(4) 0.007(7) 0.003(3) 0.007(7) N2 0.022(4) 0.020(6) 0.031(4) 0.007(4) 0.002(3) 0.001(4) N3 0.034(7) 0.036(6) 0.031(6) 0.011(5) 0.009(5) 0.012(5) N4 0.022(5) 0.044(6) 0.024(5) 0.011(5) 0.011(4) 0.006(4) N5 0.055(8) 0.025(6) 0.030(6) -0.007(5) 0.007(6) 0.001(5) N6 0.048(7) 0.039(6) 0.027(6) 0.000(5) 0.011(5) 0.018(5) N7 0.046(7) 0.038(6) 0.022(5) -0.001(4) 0.009(4) -0.002(5) N8 0.030(5) 0.028(6) 0.033(5) -0.005(4) 0.011(4) 0.014(4) N9 0.053(7) 0.037(6) 0.020(5) -0.009(4) 0.004(5) 0.009(5) N10 0.051(7) 0.031(5) 0.028(5) -0.009(4) 0.010(5) -0.001(5) N11 0.053(6) 0.038(5) 0.033(5) 0.011(4) 0.020(4) 0.008(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 K1 N2 2.891(7) . ? K1 N11 2.946(9) . ? K1 N8 2.949(9) 1_655 ? K1 N7 2.981(10) 1_655 ? K1 Ge7 3.4668(19) . ? K1 Zn1 3.4870(17) . ? K1 Ge4 3.6573(19) . ? K1 Ge5 3.661(3) . ? K1 Ge6 3.688(3) . ? K2 N8 2.973(9) . ? K2 N11 3.034(9) 1_455 ? K2 Zn1 3.373(3) 2_646 ? K2 Si1 3.404(3) 2_646 ? K2 Ge1 3.404(3) 2_646 ? K2 Ge5 3.411(4) . ? K2 Ge8 3.579(3) . ? K2 Si3 3.650(4) 2_646 ? K2 Ge3 3.650(4) 2_646 ? K2 Si6 3.684(4) 2_646 ? K3 N1 2.863(7) . ? K3 N5 2.924(12) . ? K3 N6 2.938(12) . ? K3 N10 3.004(9) . ? K3 N9 3.027(9) 2_756 ? K3 Ge1 3.457(3) . ? K3 Ge4 3.480(2) . ? K3 Ge2 3.648(3) . ? K3 K6 4.185(3) 2_756 ? K4 N7 2.942(10) . ? K4 N2 3.057(9) 1_455 ? K4 Ge6 3.400(4) . ? K4 Zn1 3.428(3) 2_656 ? K4 Si2 3.533(3) 2_656 ? K4 Ge2 3.533(3) 2_656 ? K4 Si5 3.617(4) 2_656 ? K4 Ge5 3.617(4) 2_656 ? K4 Ge8 3.683(3) . ? K4 Si4 3.690(4) 2_656 ? K5 N3 2.916(11) . ? K5 N4 2.943(10) . ? K5 N5 3.164(12) 1_454 ? K5 Ge8 3.398(3) . ? K5 N10 3.427(10) 2_756 ? K5 Si2 3.535(3) 2_656 ? K5 Ge2 3.535(3) 2_656 ? K5 Ge7 3.583(3) . ? K5 Ge6 3.753(3) . ? K6 N9 2.956(9) . ? K6 N3 3.036(11) 2_645 ? K6 N4 3.074(10) 2_645 ? K6 N1 3.293(12) 2_746 ? K6 Si1 3.574(3) 2_646 ? K6 Ge1 3.574(3) 2_646 ? K6 Ge5 3.611(3) . ? K6 Ge7 3.678(3) . ? K6 Si3 3.707(3) 2_646 ? K6 Ge3 3.707(3) 2_646 ? Ge1 Ge4 2.467(3) . ? Ge1 Ge3 2.481(3) . ? Ge1 Ge2 2.5485(14) . ? Ge1 K2 3.404(3) 2_656 ? Ge1 K6 3.574(3) 2_656 ? Ge2 Ge3 2.465(3) . ? Ge2 Ge4 2.478(2) . ? Ge2 K4 3.533(3) 2_646 ? Ge2 K5 3.535(3) 2_646 ? Ge3 Zn1 2.5099(13) . ? Ge3 Ge4 2.6392(19) . ? Ge3 K2 3.650(4) 2_656 ? Ge3 K6 3.707(3) 2_656 ? Ge3 K4 3.814(4) 2_646 ? Ge4 Zn1 2.5107(15) . ? Ge4 K4 3.690(4) 2_646 ? Ge4 K2 3.698(4) 2_656 ? Ge5 Ge7 2.457(3) . ? Ge5 Ge8 2.475(3) . ? Ge5 Zn1 2.494(3) . ? Ge5 Ge6 2.6223(19) . ? Ge5 K4 3.617(4) 2_646 ? Ge6 Ge7 2.449(3) . ? Ge6 Ge8 2.484(3) . ? Ge6 Zn1 2.516(3) . ? Ge6 K2 3.683(4) 2_656 ? Ge7 Ge8 2.5718(14) . ? Zn1 K2 3.373(3) 2_656 ? Zn1 K4 3.428(3) 2_646 ? N1 K6 3.293(12) 2_756 ? N2 K4 3.057(9) 1_655 ? N3 K6 3.036(11) 2_655 ? N4 K6 3.074(10) 2_655 ? N5 K5 3.164(12) 1_656 ? N7 K1 2.981(10) 1_455 ? N8 K1 2.949(9) 1_455 ? N9 K3 3.027(9) 2_746 ? N10 K5 3.427(9) 2_746 ? N11 K2 3.034(9) 1_655 ? 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 K1 N11 74.1(2) . . ? N2 K1 N8 86.1(2) . 1_655 ? N11 K1 N8 75.3(2) . 1_655 ? N2 K1 N7 86.8(2) . 1_655 ? N11 K1 N7 143.9(2) . 1_655 ? N8 K1 N7 73.1(3) 1_655 1_655 ? N2 K1 Ge7 152.39(14) . . ? N11 K1 Ge7 114.89(19) . . ? N8 K1 Ge7 72.26(19) 1_655 . ? N7 K1 Ge7 70.9(2) 1_655 . ? N2 K1 Zn1 136.32(14) . . ? N11 K1 Zn1 93.36(17) . . ? N8 K1 Zn1 131.8(2) 1_655 . ? N7 K1 Zn1 120.74(19) 1_655 . ? Ge7 K1 Zn1 70.89(4) . . ? N2 K1 Ge4 95.47(13) . . ? N11 K1 Ge4 75.44(16) . . ? N8 K1 Ge4 149.0(2) 1_655 . ? N7 K1 Ge4 137.9(2) 1_655 . ? Ge7 K1 Ge4 111.94(5) . . ? Zn1 K1 Ge4 41.06(3) . . ? N2 K1 Ge5 161.3(2) . . ? N11 K1 Ge5 87.31(19) . . ? N8 K1 Ge5 91.4(2) 1_655 . ? N7 K1 Ge5 110.2(2) 1_655 . ? Ge7 K1 Ge5 40.21(5) . . ? Zn1 K1 Ge5 40.74(5) . . ? Ge4 K1 Ge5 77.33(6) . . ? N2 K1 Ge6 154.2(2) . . ? N11 K1 Ge6 126.83(18) . . ? N8 K1 Ge6 112.12(19) 1_655 . ? N7 K1 Ge6 81.7(2) 1_655 . ? Ge7 K1 Ge6 39.89(5) . . ? Zn1 K1 Ge6 40.93(5) . . ? Ge4 K1 Ge6 78.35(6) . . ? Ge5 K1 Ge6 41.81(3) . . ? N8 K2 N11 73.6(2) . 1_455 ? N8 K2 Zn1 130.19(19) . 2_646 ? N11 K2 Zn1 87.93(17) 1_455 2_646 ? N8 K2 Si1 73.49(18) . 2_646 ? N11 K2 Si1 113.08(18) 1_455 2_646 ? Zn1 K2 Si1 72.24(6) 2_646 2_646 ? N8 K2 Ge1 73.49(18) . 2_646 ? N11 K2 Ge1 113.08(18) 1_455 2_646 ? Zn1 K2 Ge1 72.24(6) 2_646 2_646 ? Si1 K2 Ge1 0.00(7) 2_646 2_646 ? N8 K2 Ge5 110.90(19) . . ? N11 K2 Ge5 137.05(19) 1_455 . ? Zn1 K2 Ge5 113.76(9) 2_646 . ? Si1 K2 Ge5 108.86(9) 2_646 . ? Ge1 K2 Ge5 108.86(9) 2_646 . ? N8 K2 Ge8 69.51(18) . . ? N11 K2 Ge8 122.60(17) 1_455 . ? Zn1 K2 Ge8 149.15(10) 2_646 . ? Si1 K2 Ge8 96.73(8) 2_646 . ? Ge1 K2 Ge8 96.73(8) 2_646 . ? Ge5 K2 Ge8 41.39(5) . . ? N8 K2 Si3 114.44(19) . 2_646 ? N11 K2 Si3 122.71(17) 1_455 2_646 ? Zn1 K2 Si3 41.64(4) 2_646 2_646 ? Si1 K2 Si3 40.99(5) 2_646 2_646 ? Ge1 K2 Si3 40.99(5) 2_646 2_646 ? Ge5 K2 Si3 95.14(8) . 2_646 ? Ge8 K2 Si3 112.16(9) . 2_646 ? N8 K2 Ge3 114.44(19) . 2_646 ? N11 K2 Ge3 122.71(17) 1_455 2_646 ? Zn1 K2 Ge3 41.64(4) 2_646 2_646 ? Si1 K2 Ge3 40.99(5) 2_646 2_646 ? Ge1 K2 Ge3 40.99(5) 2_646 2_646 ? Ge5 K2 Ge3 95.14(8) . 2_646 ? Ge8 K2 Ge3 112.16(9) . 2_646 ? Si3 K2 Ge3 0.00(7) 2_646 2_646 ? N8 K2 Si6 142.27(19) . 2_646 ? N11 K2 Si6 69.62(17) 1_455 2_646 ? Zn1 K2 Si6 41.48(5) 2_646 2_646 ? Si1 K2 Si6 113.62(8) 2_646 2_646 ? Ge1 K2 Si6 113.62(8) 2_646 2_646 ? Ge5 K2 Si6 101.76(10) . 2_646 ? Ge8 K2 Si6 140.00(9) . 2_646 ? Si3 K2 Si6 79.78(7) 2_646 2_646 ? Ge3 K2 Si6 79.78(7) 2_646 2_646 ? N1 K3 N5 98.7(3) . . ? N1 K3 N6 88.0(3) . . ? N5 K3 N6 66.21(19) . . ? N1 K3 N10 70.9(3) . . ? N5 K3 N10 164.5(3) . . ? N6 K3 N10 101.1(3) . . ? N1 K3 N9 90.7(3) . 2_756 ? N5 K3 N9 114.1(3) . 2_756 ? N6 K3 N9 178.7(3) . 2_756 ? N10 K3 N9 78.4(2) . 2_756 ? N1 K3 Ge1 166.2(3) . . ? N5 K3 Ge1 73.0(2) . . ? N6 K3 Ge1 98.3(2) . . ? N10 K3 Ge1 119.39(19) . . ? N9 K3 Ge1 82.97(19) 2_756 . ? N1 K3 Ge4 145.78(16) . . ? N5 K3 Ge4 114.5(2) . . ? N6 K3 Ge4 111.9(2) . . ? N10 K3 Ge4 77.91(18) . . ? N9 K3 Ge4 69.19(18) 2_756 . ? Ge1 K3 Ge4 41.66(5) . . ? N1 K3 Ge2 151.4(3) . . ? N5 K3 Ge2 91.8(2) . . ? N6 K3 Ge2 72.1(2) . . ? N10 K3 Ge2 92.66(19) . . ? N9 K3 Ge2 109.15(18) 2_756 . ? Ge1 K3 Ge2 41.94(3) . . ? Ge4 K3 Ge2 40.61(5) . . ? N1 K3 K6 51.6(2) . 2_756 ? N5 K3 K6 95.8(2) . 2_756 ? N6 K3 K6 133.9(2) . 2_756 ? N10 K3 K6 86.79(18) . 2_756 ? N9 K3 K6 44.92(17) 2_756 2_756 ? Ge1 K3 K6 117.14(9) . 2_756 ? Ge4 K3 K6 114.10(7) . 2_756 ? Ge2 K3 K6 153.59(7) . 2_756 ? N7 K4 N2 84.5(2) . 1_455 ? N7 K4 Ge6 123.49(19) . . ? N2 K4 Ge6 77.67(14) 1_455 . ? N7 K4 Zn1 117.0(2) . 2_656 ? N2 K4 Zn1 133.93(17) 1_455 2_656 ? Ge6 K4 Zn1 113.80(9) . 2_656 ? N7 K4 Si2 70.91(19) . 2_656 ? N2 K4 Si2 152.74(16) 1_455 2_656 ? Ge6 K4 Si2 105.86(9) . 2_656 ? Zn1 K4 Si2 70.31(6) 2_656 2_656 ? N7 K4 Ge2 70.91(19) . 2_656 ? N2 K4 Ge2 152.74(16) 1_455 2_656 ? Ge6 K4 Ge2 105.86(9) . 2_656 ? Zn1 K4 Ge2 70.31(6) 2_656 2_656 ? Si2 K4 Ge2 0.00(8) 2_656 2_656 ? N7 K4 Si5 131.1(2) . 2_656 ? N2 K4 Si5 93.23(16) 1_455 2_656 ? Ge6 K4 Si5 103.35(10) . 2_656 ? Zn1 K4 Si5 41.35(5) 2_656 2_656 ? Si2 K4 Si5 111.63(8) 2_656 2_656 ? Ge2 K4 Si5 111.63(8) 2_656 2_656 ? N7 K4 Ge5 131.1(2) . 2_656 ? N2 K4 Ge5 93.23(16) 1_455 2_656 ? Ge6 K4 Ge5 103.35(10) . 2_656 ? Zn1 K4 Ge5 41.35(5) 2_656 2_656 ? Si2 K4 Ge5 111.63(8) 2_656 2_656 ? Ge2 K4 Ge5 111.63(8) 2_656 2_656 ? Si5 K4 Ge5 0.00(9) 2_656 2_656 ? N7 K4 Ge8 82.81(18) . . ? N2 K4 Ge8 67.53(15) 1_455 . ? Ge6 K4 Ge8 40.81(5) . . ? Zn1 K4 Ge8 149.03(10) 2_656 . ? Si2 K4 Ge8 97.06(8) 2_656 . ? Ge2 K4 Ge8 97.06(8) 2_656 . ? Si5 K4 Ge8 140.63(9) 2_656 . ? Ge5 K4 Ge8 140.63(9) 2_656 . ? N7 K4 Si4 78.12(19) . 2_656 ? N2 K4 Si4 146.30(16) 1_455 2_656 ? Ge6 K4 Si4 135.86(10) . 2_656 ? Zn1 K4 Si4 41.10(4) 2_656 2_656 ? Si2 K4 Si4 40.06(4) 2_656 2_656 ? Ge2 K4 Si4 40.06(4) 2_656 2_656 ? Si5 K4 Si4 77.46(7) 2_656 2_656 ? Ge5 K4 Si4 77.46(7) 2_656 2_656 ? Ge8 K4 Si4 136.83(9) . 2_656 ? N3 K5 N4 94.5(3) . . ? N3 K5 N5 64.8(3) . 1_454 ? N4 K5 N5 135.9(3) . 1_454 ? N3 K5 Ge8 139.5(2) . . ? N4 K5 Ge8 109.9(2) . . ? N5 K5 Ge8 75.4(2) 1_454 . ? N3 K5 N10 114.4(3) . 2_756 ? N4 K5 N10 65.9(3) . 2_756 ? N5 K5 N10 157.5(3) 1_454 2_756 ? Ge8 K5 N10 105.02(15) . 2_756 ? N3 K5 Si2 70.0(2) . 2_656 ? N4 K5 Si2 143.4(2) . 2_656 ? N5 K5 Si2 68.3(2) 1_454 2_656 ? Ge8 K5 Si2 102.49(7) . 2_656 ? N10 K5 Si2 89.93(17) 2_756 2_656 ? N3 K5 Ge2 70.0(2) . 2_656 ? N4 K5 Ge2 143.4(2) . 2_656 ? N5 K5 Ge2 68.3(2) 1_454 2_656 ? Ge8 K5 Ge2 102.49(7) . 2_656 ? N10 K5 Ge2 89.93(17) 2_756 2_656 ? Si2 K5 Ge2 0.00(6) 2_656 2_656 ? N3 K5 Ge7 151.9(2) . . ? N4 K5 Ge7 67.9(2) . . ? N5 K5 Ge7 112.1(2) 1_454 . ? Ge8 K5 Ge7 43.13(4) . . ? N10 K5 Ge7 79.30(15) 2_756 . ? Si2 K5 Ge7 136.75(7) 2_656 . ? Ge2 K5 Ge7 136.75(7) 2_656 . ? N3 K5 Ge6 168.7(2) . . ? N4 K5 Ge6 95.2(2) . . ? N5 K5 Ge6 111.2(2) 1_454 . ? Ge8 K5 Ge6 40.26(5) . . ? N10 K5 Ge6 64.88(15) 2_756 . ? Si2 K5 Ge6 98.72(7) 2_656 . ? Ge2 K5 Ge6 98.72(7) 2_656 . ? Ge7 K5 Ge6 38.92(5) . . ? N9 K6 N3 72.9(3) . 2_645 ? N9 K6 N4 141.8(3) . 2_645 ? N3 K6 N4 89.5(3) 2_645 2_645 ? N9 K6 N1 84.1(2) . 2_746 ? N3 K6 N1 87.9(2) 2_645 2_746 ? N4 K6 N1 61.1(2) 2_645 2_746 ? N9 K6 Si1 120.7(2) . 2_646 ? N3 K6 Si1 160.0(2) 2_645 2_646 ? N4 K6 Si1 70.78(19) 2_645 2_646 ? N1 K6 Si1 79.62(13) 2_746 2_646 ? N9 K6 Ge1 120.7(2) . 2_646 ? N3 K6 Ge1 160.0(2) 2_645 2_646 ? N4 K6 Ge1 70.78(19) 2_645 2_646 ? N1 K6 Ge1 79.62(13) 2_746 2_646 ? Si1 K6 Ge1 0.00(5) 2_646 2_646 ? N9 K6 Ge5 67.15(17) . . ? N3 K6 Ge5 98.0(2) 2_645 . ? N4 K6 Ge5 150.5(2) 2_645 . ? N1 K6 Ge5 147.12(16) 2_746 . ? Si1 K6 Ge5 100.97(7) 2_646 . ? Ge1 K6 Ge5 100.97(7) 2_646 . ? N9 K6 Ge7 77.81(18) . . ? N3 K6 Ge7 64.5(2) 2_645 . ? N4 K6 Ge7 125.2(2) 2_645 . ? N1 K6 Ge7 150.39(14) 2_746 . ? Si1 K6 Ge7 129.86(7) 2_646 . ? Ge1 K6 Ge7 129.86(7) 2_646 . ? Ge5 K6 Ge7 39.39(5) . . ? N9 K6 Si3 81.20(19) . 2_646 ? N3 K6 Si3 146.5(2) 2_645 2_646 ? N4 K6 Si3 98.5(2) 2_645 2_646 ? N1 K6 Si3 68.39(15) 2_746 2_646 ? Si1 K6 Si3 39.78(4) 2_646 2_646 ? Ge1 K6 Si3 39.78(4) 2_646 2_646 ? Ge5 K6 Si3 90.87(7) . 2_646 ? Ge7 K6 Si3 130.24(7) . 2_646 ? N9 K6 Ge3 81.20(19) . 2_646 ? N3 K6 Ge3 146.5(2) 2_645 2_646 ? N4 K6 Ge3 98.5(2) 2_645 2_646 ? N1 K6 Ge3 68.39(15) 2_746 2_646 ? Si1 K6 Ge3 39.78(4) 2_646 2_646 ? Ge1 K6 Ge3 39.78(4) 2_646 2_646 ? Ge5 K6 Ge3 90.87(7) . 2_646 ? Ge7 K6 Ge3 130.24(7) . 2_646 ? Si3 K6 Ge3 0.00(7) 2_646 2_646 ? Ge4 Ge1 Ge3 64.48(7) . . ? Ge4 Ge1 Ge2 59.21(9) . . ? Ge3 Ge1 Ge2 58.69(9) . . ? Ge4 Ge1 K2 76.23(8) . 2_656 ? Ge3 Ge1 K2 74.83(8) . 2_656 ? Ge2 Ge1 K2 125.21(10) . 2_656 ? Ge4 Ge1 K3 69.67(7) . . ? Ge3 Ge1 K3 125.24(9) . . ? Ge2 Ge1 K3 73.04(9) . . ? K2 Ge1 K3 121.21(8) 2_656 . ? Ge4 Ge1 K6 133.51(8) . 2_656 ? Ge3 Ge1 K6 72.99(7) . 2_656 ? Ge2 Ge1 K6 112.72(10) . 2_656 ? K2 Ge1 K6 75.36(7) 2_656 2_656 ? K3 Ge1 K6 156.44(7) . 2_656 ? Ge3 Ge2 Ge4 64.53(7) . . ? Ge3 Ge2 Ge1 59.28(9) . . ? Ge4 Ge2 Ge1 58.75(9) . . ? Ge3 Ge2 K4 76.69(8) . 2_646 ? Ge4 Ge2 K4 73.40(8) . 2_646 ? Ge1 Ge2 K4 124.62(10) . 2_646 ? Ge3 Ge2 K5 93.30(8) . 2_646 ? Ge4 Ge2 K5 145.27(9) . 2_646 ? Ge1 Ge2 K5 133.75(11) . 2_646 ? K4 Ge2 K5 75.68(7) 2_646 2_646 ? Ge3 Ge2 K3 118.62(8) . . ? Ge4 Ge2 K3 66.05(6) . . ? Ge1 Ge2 K3 65.02(9) . . ? K4 Ge2 K3 120.04(7) 2_646 . ? K5 Ge2 K3 146.18(8) 2_646 . ? Ge2 Ge3 Ge1 62.03(4) . . ? Ge2 Ge3 Zn1 107.36(8) . . ? Ge1 Ge3 Zn1 106.36(8) . . ? Ge2 Ge3 Ge4 57.98(7) . . ? Ge1 Ge3 Ge4 57.51(7) . . ? Zn1 Ge3 Ge4 58.30(4) . . ? Ge2 Ge3 K2 118.87(8) . 2_656 ? Ge1 Ge3 K2 64.18(8) . 2_656 ? Zn1 Ge3 K2 63.26(8) . 2_656 ? Ge4 Ge3 K2 69.93(9) . 2_656 ? Ge2 Ge3 K6 110.80(7) . 2_656 ? Ge1 Ge3 K6 67.23(7) . 2_656 ? Zn1 Ge3 K6 130.34(10) . 2_656 ? Ge4 Ge3 K6 121.75(10) . 2_656 ? K2 Ge3 K6 70.92(7) 2_656 2_656 ? Ge2 Ge3 K4 64.34(8) . 2_646 ? Ge1 Ge3 K4 116.72(8) . 2_646 ? Zn1 Ge3 K4 61.64(8) . 2_646 ? Ge4 Ge3 K4 66.92(9) . 2_646 ? K2 Ge3 K4 121.95(5) 2_656 2_646 ? K6 Ge3 K4 167.14(8) 2_656 2_646 ? Ge1 Ge4 Ge2 62.04(4) . . ? Ge1 Ge4 Zn1 106.76(8) . . ? Ge2 Ge4 Zn1 106.92(8) . . ? Ge1 Ge4 Ge3 58.01(7) . . ? Ge2 Ge4 Ge3 57.49(7) . . ? Zn1 Ge4 Ge3 58.27(4) . . ? Ge1 Ge4 K3 68.67(7) . . ? Ge2 Ge4 K3 73.34(7) . . ? Zn1 Ge4 K3 174.85(12) . . ? Ge3 Ge4 K3 119.07(6) . . ? Ge1 Ge4 K1 146.36(13) . . ? Ge2 Ge4 K1 151.03(13) . . ? Zn1 Ge4 K1 65.83(4) . . ? Ge3 Ge4 K1 124.07(5) . . ? K3 Ge4 K1 116.50(5) . . ? Ge1 Ge4 K4 121.46(8) . 2_646 ? Ge2 Ge4 K4 66.54(8) . 2_646 ? Zn1 Ge4 K4 63.83(8) . 2_646 ? Ge3 Ge4 K4 71.94(9) . 2_646 ? K3 Ge4 K4 120.30(9) . 2_646 ? K1 Ge4 K4 86.01(8) . 2_646 ? Ge1 Ge4 K2 63.39(8) . 2_656 ? Ge2 Ge4 K2 116.82(8) . 2_656 ? Zn1 Ge4 K2 62.41(8) . 2_656 ? Ge3 Ge4 K2 67.98(9) . 2_656 ? K3 Ge4 K2 112.74(9) . 2_656 ? K1 Ge4 K2 85.67(8) . 2_656 ? K4 Ge4 K2 124.11(5) 2_646 2_656 ? Ge7 Ge5 Ge8 62.86(7) . . ? Ge7 Ge5 Zn1 109.08(10) . . ? Ge8 Ge5 Zn1 105.15(10) . . ? Ge7 Ge5 Ge6 57.55(10) . . ? Ge8 Ge5 Ge6 58.23(10) . . ? Zn1 Ge5 Ge6 58.85(9) . . ? Ge7 Ge5 K2 129.88(11) . . ? Ge8 Ge5 K2 72.94(8) . . ? Zn1 Ge5 K2 104.03(9) . . ? Ge6 Ge5 K2 116.35(13) . . ? Ge7 Ge5 K6 71.78(8) . . ? Ge8 Ge5 K6 74.47(8) . . ? Zn1 Ge5 K6 178.83(11) . . ? Ge6 Ge5 K6 121.51(13) . . ? K2 Ge5 K6 74.80(8) . . ? Ge7 Ge5 K4 150.73(11) . 2_646 ? Ge8 Ge5 K4 145.85(11) . 2_646 ? Zn1 Ge5 K4 65.26(8) . 2_646 ? Ge6 Ge5 K4 124.08(13) . 2_646 ? K2 Ge5 K4 77.83(8) . 2_646 ? K6 Ge5 K4 114.42(8) . 2_646 ? Ge7 Ge5 K1 65.63(7) . . ? Ge8 Ge5 K1 120.19(10) . . ? Zn1 Ge5 K1 65.87(7) . . ? Ge6 Ge5 K1 69.64(11) . . ? K2 Ge5 K1 164.48(10) . . ? K6 Ge5 K1 115.29(8) . . ? K4 Ge5 K1 87.03(8) 2_646 . ? Ge7 Ge6 Ge8 62.84(7) . . ? Ge7 Ge6 Zn1 108.62(10) . . ? Ge8 Ge6 Zn1 104.24(10) . . ? Ge7 Ge6 Ge5 57.84(10) . . ? Ge8 Ge6 Ge5 57.91(10) . . ? Zn1 Ge6 Ge5 58.03(9) . . ? Ge7 Ge6 K4 132.68(11) . . ? Ge8 Ge6 K4 75.74(9) . . ? Zn1 Ge6 K4 102.64(9) . . ? Ge5 Ge6 K4 117.50(13) . . ? Ge7 Ge6 K2 149.41(11) . 2_656 ? Ge8 Ge6 K2 145.98(10) . 2_656 ? Zn1 Ge6 K2 62.63(8) . 2_656 ? Ge5 Ge6 K2 120.61(13) . 2_656 ? K4 Ge6 K2 77.05(7) . 2_656 ? Ge7 Ge6 K1 65.19(7) . . ? Ge8 Ge6 K1 118.98(10) . . ? Zn1 Ge6 K1 65.24(7) . . ? Ge5 Ge6 K1 68.56(11) . . ? K4 Ge6 K1 162.10(10) . . ? K2 Ge6 K1 85.44(8) 2_656 . ? Ge7 Ge6 K5 66.80(7) . . ? Ge8 Ge6 K5 62.17(8) . . ? Zn1 Ge6 K5 166.39(11) . . ? Ge5 Ge6 K5 111.03(12) . . ? K4 Ge6 K5 74.45(8) . . ? K2 Ge6 K5 128.01(8) 2_656 . ? K1 Ge6 K5 120.47(8) . . ? Ge6 Ge7 Ge5 64.61(5) . . ? Ge6 Ge7 Ge8 59.23(7) . . ? Ge5 Ge7 Ge8 58.91(7) . . ? Ge6 Ge7 K1 74.92(8) . . ? Ge5 Ge7 K1 74.16(8) . . ? Ge8 Ge7 K1 124.16(4) . . ? Ge6 Ge7 K5 74.28(8) . . ? Ge5 Ge7 K5 121.29(8) . . ? Ge8 Ge7 K5 64.60(6) . . ? K1 Ge7 K5 132.74(9) . . ? Ge6 Ge7 K6 124.81(8) . . ? Ge5 Ge7 K6 68.84(8) . . ? Ge8 Ge7 K6 72.27(7) . . ? K1 Ge7 K6 118.57(8) . . ? K5 Ge7 K6 108.36(7) . . ? Ge5 Ge8 Ge6 63.85(5) . . ? Ge5 Ge8 Ge7 58.23(7) . . ? Ge6 Ge8 Ge7 57.93(7) . . ? Ge5 Ge8 K5 127.97(8) . . ? Ge6 Ge8 K5 77.57(8) . . ? Ge7 Ge8 K5 72.27(6) . . ? Ge5 Ge8 K2 65.67(8) . . ? Ge6 Ge8 K2 114.88(8) . . ? Ge7 Ge8 K2 119.27(8) . . ? K5 Ge8 K2 165.94(7) . . ? Ge5 Ge8 K4 112.50(8) . . ? Ge6 Ge8 K4 63.46(8) . . ? Ge7 Ge8 K4 117.22(8) . . ? K5 Ge8 K4 75.39(7) . . ? K2 Ge8 K4 103.64(4) . . ? Ge5 Ge8 K6 66.56(7) . . ? Ge6 Ge8 K6 119.46(8) . . ? Ge7 Ge8 K6 67.49(6) . . ? K5 Ge8 K6 109.83(6) . . ? K2 Ge8 K6 70.70(7) . . ? K4 Ge8 K6 174.24(7) . . ? Ge5 Zn1 Ge3 139.87(10) . . ? Ge5 Zn1 Ge4 132.03(10) . . ? Ge3 Zn1 Ge4 63.43(4) . . ? Ge5 Zn1 Ge6 63.13(5) . . ? Ge3 Zn1 Ge6 138.73(10) . . ? Ge4 Zn1 Ge6 134.78(10) . . ? Ge5 Zn1 K2 138.93(9) . 2_656 ? Ge3 Zn1 K2 75.09(9) . 2_656 ? Ge4 Zn1 K2 76.32(9) . 2_656 ? Ge6 Zn1 K2 75.89(9) . 2_656 ? Ge5 Zn1 K4 73.39(9) . 2_646 ? Ge3 Zn1 K4 78.25(9) . 2_646 ? Ge4 Zn1 K4 75.07(9) . 2_646 ? Ge6 Zn1 K4 136.48(9) . 2_646 ? K2 Zn1 K4 147.34(4) 2_656 2_646 ? Ge5 Zn1 K1 73.39(8) . . ? Ge3 Zn1 K1 136.50(5) . . ? Ge4 Zn1 K1 73.11(4) . . ? Ge6 Zn1 K1 73.82(7) . . ? K2 Zn1 K1 93.59(8) 2_656 . ? K4 Zn1 K1 92.89(8) 2_646 . ? K3 N1 K6 85.4(3) . 2_756 ? K1 N2 K4 91.7(2) . 1_655 ? K5 N3 K6 86.2(3) . 2_655 ? K5 N4 K6 85.0(3) . 2_655 ? K3 N5 K5 91.5(3) . 1_656 ? K4 N7 K1 92.3(3) . 1_455 ? K1 N8 K2 93.9(3) 1_455 . ? K6 N9 K3 88.8(2) . 2_746 ? K3 N10 K5 111.9(3) . 2_746 ? K1 N11 K2 92.7(2) . 1_655 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.25 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.612 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.124