data_KM205 _audit_creation_method SHELXL-2014/7 _shelx_SHELXL_version_number 2014/7 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'Bi3 Sn, 9(H3 N), 5(K)' _chemical_formula_sum 'Bi3 H27 K5 N9 Sn' _chemical_formula_weight 1094.43 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' H H 0.0000 0.0000 '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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 33 _space_group_name_H-M_alt 'P n a 21' _space_group_name_Hall 'P 2c -2n' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 38.5023(8) _cell_length_b 9.7164(2) _cell_length_c 6.8765(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2572.52(11) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 20583 _cell_measurement_theta_min 2.9711 _cell_measurement_theta_max 32.8515 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_density_diffrn 2.826 _exptl_crystal_F_000 1936 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_absorpt_coefficient_mu 22.228 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.07622 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.34d Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Xcalibur 3' _diffrn_measurement_method '\w and \p scans' _diffrn_detector_area_resol_mean 16.0238 _diffrn_reflns_number 38474 _diffrn_reflns_av_unetI/netI 0.0362 _diffrn_reflns_av_R_equivalents 0.0733 _diffrn_reflns_limit_h_min -47 _diffrn_reflns_limit_h_max 47 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.979 _diffrn_reflns_theta_max 25.997 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 5048 _reflns_number_gt 4840 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.840 _reflns_Friedel_fraction_max 1.000 _reflns_Friedel_fraction_full 1.000 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.34d ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.34d ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.34d ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2012)' _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+112.7327P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_extinction_coef 0.00019(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details ; Flack x determined using 1978 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.014(5) _chemical_absolute_configuration ? _refine_ls_number_reflns 5048 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0479 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1052 _refine_ls_wR_factor_gt 0.1046 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.128 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Bi1 Bi 0.09145(2) 0.29690(9) 0.2676(3) 0.0150(2) Uani 1 1 d . . . . . Bi2 Bi 0.09729(2) 0.68391(9) 0.7280(3) 0.0146(2) Uani 1 1 d . . . . . Bi3 Bi 0.20545(2) 0.46068(9) 0.4983(3) 0.0183(2) Uani 1 1 d . . . . . Sn1 Sn 0.13149(3) 0.47991(15) 0.5000 0.0126(3) Uani 1 1 d . . . . . K1 K 0.05447(13) 0.3360(5) 0.7651(9) 0.0206(11) Uani 1 1 d . . . . . K2 K 0.16361(12) 0.4835(6) -0.0022(13) 0.0264(11) Uani 1 1 d . . . . . K3 K 0.17460(16) 0.1312(6) 0.3234(9) 0.0263(13) Uani 1 1 d . . . . . K4 K 0.18722(16) 0.8077(6) 0.6582(10) 0.0276(13) Uani 1 1 d . . . . . K5 K 0.05941(13) 0.6511(5) 0.2238(9) 0.0202(11) Uani 1 1 d . . . . . N1 N 0.0558(6) 0.052(3) 0.891(4) 0.034(6) Uani 1 1 d . . . . . H1A H 0.0346 0.0125 0.8689 0.052 Uiso 1 1 d R U . . . H1B H 0.0607 0.0478 1.0202 0.052 Uiso 1 1 d R U . . . H1C H 0.0723 0.0049 0.8232 0.052 Uiso 1 1 d R U . . . N2 N 0.2095(7) 0.195(3) -0.047(6) 0.069(12) Uani 1 1 d . . . . . H2A H 0.2080 0.2387 -0.1639 0.104 Uiso 1 1 d R U . . . H2B H 0.2011 0.1079 -0.0590 0.104 Uiso 1 1 d R U . . . H2C H 0.2320 0.1920 -0.0082 0.104 Uiso 1 1 d R U . . . N3 N 0.2366(5) 0.014(2) 0.504(5) 0.032(5) Uani 1 1 d . . . . . H3A H 0.2469 -0.0372 0.5981 0.048 Uiso 1 1 d R U . . . H3B H 0.2397 0.1053 0.5305 0.048 Uiso 1 1 d R U . . . H3C H 0.2464 -0.0057 0.3866 0.048 Uiso 1 1 d R U . . . N4 N 0.1304(6) -0.101(2) 0.231(4) 0.030(5) Uani 1 1 d . . . . . H4A H 0.1077 -0.0739 0.2350 0.044 Uiso 1 1 d R U . . . H4B H 0.1339 -0.1691 0.3198 0.044 Uiso 1 1 d R U . . . H4C H 0.1356 -0.1324 0.1102 0.044 Uiso 1 1 d R U . . . N5 N 0.1409(6) 0.055(3) 0.702(4) 0.033(6) Uani 1 1 d . . . . . H5A H 0.1287 0.1193 0.6345 0.050 Uiso 1 1 d R U . . . H5B H 0.1567 0.0980 0.7803 0.050 Uiso 1 1 d R U . . . H5C H 0.1261 0.0047 0.7770 0.050 Uiso 1 1 d R U . . . N6 N 0.2032(6) 0.777(3) 1.077(4) 0.031(6) Uani 1 1 d . . . . . H6A H 0.2113 0.7171 1.1688 0.047 Uiso 1 1 d R U . . . H6B H 0.1885 0.8381 1.1337 0.047 Uiso 1 1 d R U . . . H6C H 0.2213 0.8223 1.0223 0.047 Uiso 1 1 d R U . . . N7 N -0.0029(5) 0.251(2) 0.481(4) 0.028(5) Uani 1 1 d . . . . . H7A H -0.0209 0.1907 0.4757 0.041 Uiso 1 1 d R U . . . H7B H 0.0174 0.2058 0.4590 0.041 Uiso 1 1 d R U . . . H7C H -0.0059 0.3176 0.3896 0.041 Uiso 1 1 d R U . . . N8 N 0.0385(6) 0.922(3) 0.367(3) 0.031(6) Uani 1 1 d . . . . . H8A H 0.0559 0.9835 0.3458 0.047 Uiso 1 1 d R U . . . H8B H 0.0340 0.9170 0.4966 0.047 Uiso 1 1 d R U . . . H8C H 0.0191 0.9502 0.3028 0.047 Uiso 1 1 d R U . . . N9 N 0.0028(5) 0.592(2) 0.518(3) 0.019(4) Uani 1 1 d . . . . . H9A H -0.0165 0.6215 0.5817 0.028 Uiso 1 1 d R U . . . H9B H 0.0221 0.6213 0.5830 0.028 Uiso 1 1 d R U . . . H9C H 0.0028 0.4989 0.5113 0.028 Uiso 1 1 d R U . . . 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 Bi1 0.0151(4) 0.0131(4) 0.0169(5) -0.0020(4) -0.0019(3) -0.0011(3) Bi2 0.0147(4) 0.0132(4) 0.0158(5) -0.0019(4) 0.0004(3) 0.0014(3) Bi3 0.0128(4) 0.0202(5) 0.0218(4) -0.0017(5) 0.0000(4) 0.0011(3) Sn1 0.0130(6) 0.0118(8) 0.0130(6) -0.0012(7) -0.0009(8) 0.0008(6) K1 0.022(2) 0.022(3) 0.018(3) 0.002(3) 0.003(2) -0.0022(19) K2 0.024(2) 0.041(3) 0.015(2) 0.002(3) -0.001(3) -0.003(2) K3 0.034(3) 0.017(3) 0.028(3) 0.000(2) -0.002(2) 0.007(2) K4 0.029(3) 0.012(3) 0.042(3) -0.001(2) 0.005(2) -0.001(2) K5 0.021(2) 0.020(3) 0.019(3) -0.002(2) -0.002(2) 0.0049(19) N1 0.033(13) 0.021(14) 0.050(16) -0.017(12) -0.007(11) 0.004(11) N2 0.031(15) 0.05(2) 0.12(4) 0.02(2) 0.021(18) 0.015(14) N3 0.046(13) 0.027(12) 0.023(10) 0.000(11) 0.008(14) -0.006(10) N4 0.033(11) 0.022(12) 0.034(13) -0.004(11) -0.006(11) 0.004(9) N5 0.031(12) 0.032(14) 0.037(14) 0.005(11) 0.004(11) 0.007(10) N6 0.024(12) 0.025(14) 0.044(15) -0.015(11) -0.003(10) 0.001(10) N7 0.029(11) 0.023(12) 0.031(12) 0.002(11) 0.009(11) -0.002(9) N8 0.029(12) 0.030(15) 0.035(13) -0.004(11) -0.005(10) 0.013(11) N9 0.019(9) 0.017(10) 0.020(10) -0.005(10) 0.002(9) -0.003(8) _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 Bi1 Sn1 2.8445(19) . ? Bi1 K3 3.604(6) . ? Bi1 K5 3.668(5) . ? Bi1 K1 3.724(6) . ? Bi1 K1 3.757(6) 1_554 ? Bi1 K2 3.801(6) . ? Bi2 Sn1 2.8497(19) . ? Bi2 K4 3.697(6) . ? Bi2 K2 3.709(6) 1_556 ? Bi2 K5 3.722(6) 1_556 ? Bi2 K1 3.770(5) . ? Bi2 K5 3.775(6) . ? Bi3 Sn1 2.8537(15) . ? Bi3 K4 3.615(6) . ? Bi3 K3 3.620(6) . ? Bi3 K2 3.800(8) 1_556 ? Bi3 K2 3.807(8) . ? Sn1 K2 3.640(8) 1_556 ? Sn1 K2 3.668(9) . ? Sn1 K1 3.751(5) . ? Sn1 K5 3.752(5) . ? Sn1 K3 3.963(6) . ? Sn1 K4 3.992(6) . ? K1 N9 2.89(2) 2_565 ? K1 N1 2.90(3) . ? K1 N7 3.06(2) . ? K1 Bi1 3.757(6) 1_556 ? K1 K5 4.396(7) 2_565 ? K1 K5 4.400(7) 1_556 ? K1 K2 4.719(7) 1_556 ? K1 K5 4.823(7) . ? K1 H7B 2.8408 . ? K1 H9C 3.0841 . ? K2 N6 3.27(2) 1_554 ? K2 N2 3.33(3) . ? K2 Sn1 3.640(8) 1_554 ? K2 Bi2 3.709(6) 1_554 ? K2 Bi3 3.800(8) 1_554 ? K2 K4 4.025(9) 1_554 ? K2 K3 4.112(9) . ? K2 K5 4.600(8) . ? K2 K1 4.719(7) 1_554 ? K3 N4 2.90(2) . ? K3 N3 2.92(3) . ? K3 N2 2.95(4) . ? K3 N5 3.00(3) . ? K3 K4 3.926(8) 1_545 ? K3 H2B 2.8302 . ? K3 H3B 2.8944 . ? K3 H5A 2.7781 . ? K4 N6 2.96(3) . ? K4 N3 2.96(2) 1_565 ? K4 N5 3.01(2) 1_565 ? K4 K3 3.926(8) 1_565 ? K4 K2 4.025(9) 1_556 ? K4 H6C 2.8312 . ? K5 N7 2.90(2) 2_564 ? K5 N8 2.92(2) . ? K5 N9 3.03(2) . ? K5 Bi2 3.722(6) 1_554 ? K5 K1 4.396(7) 2_564 ? K5 K1 4.400(7) 1_554 ? K5 H9B 2.8728 . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N1 H1C 0.9100 . ? N2 H2A 0.9100 . ? N2 H2B 0.9100 . ? N2 H2C 0.9100 . ? N3 K4 2.96(2) 1_545 ? N3 H3A 0.9100 . ? N3 H3B 0.9100 . ? N3 H3C 0.9100 . ? N4 H4A 0.9100 . ? N4 H4B 0.9100 . ? N4 H4C 0.9100 . ? N5 K4 3.01(2) 1_545 ? N5 H5A 0.9100 . ? N5 H5B 0.9100 . ? N5 H5C 0.9100 . ? N6 K2 3.27(2) 1_556 ? N6 H6A 0.9100 . ? N6 H6B 0.9100 . ? N6 H6C 0.9100 . ? N7 K5 2.90(2) 2_565 ? N7 H7A 0.9100 . ? N7 H7B 0.9100 . ? N7 H7C 0.9100 . ? N8 H8A 0.9100 . ? N8 H8B 0.9100 . ? N8 H8C 0.9100 . ? N9 K1 2.89(2) 2_564 ? N9 H9A 0.9100 . ? N9 H9B 0.9100 . ? N9 H9C 0.9100 . ? 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 Sn1 Bi1 K3 74.81(10) . . ? Sn1 Bi1 K5 69.02(9) . . ? K3 Bi1 K5 136.60(13) . . ? Sn1 Bi1 K1 68.13(9) . . ? K3 Bi1 K1 106.70(12) . . ? K5 Bi1 K1 81.45(12) . . ? Sn1 Bi1 K1 131.22(9) . 1_554 ? K3 Bi1 K1 118.66(12) . 1_554 ? K5 Bi1 K1 72.67(12) . 1_554 ? K1 Bi1 K1 133.61(14) . 1_554 ? Sn1 Bi1 K2 65.16(13) . . ? K3 Bi1 K2 67.40(13) . . ? K5 Bi1 K2 76.00(12) . . ? K1 Bi1 K2 132.77(15) . . ? K1 Bi1 K2 77.27(14) 1_554 . ? Sn1 Bi2 K4 73.86(10) . . ? Sn1 Bi2 K2 65.91(13) . 1_556 ? K4 Bi2 K2 65.85(13) . 1_556 ? Sn1 Bi2 K5 128.71(9) . 1_556 ? K4 Bi2 K5 120.92(13) . 1_556 ? K2 Bi2 K5 76.49(15) 1_556 1_556 ? Sn1 Bi2 K1 67.39(9) . . ? K4 Bi2 K1 135.24(12) . . ? K2 Bi2 K1 78.25(12) 1_556 . ? K5 Bi2 K1 71.93(11) 1_556 . ? Sn1 Bi2 K5 67.32(9) . . ? K4 Bi2 K5 105.67(13) . . ? K2 Bi2 K5 132.93(15) 1_556 . ? K5 Bi2 K5 133.06(14) 1_556 . ? K1 Bi2 K5 79.48(11) . . ? Sn1 Bi3 K4 75.17(10) . . ? Sn1 Bi3 K3 74.45(10) . . ? K4 Bi3 K3 149.55(14) . . ? Sn1 Bi3 K2 64.50(10) . 1_556 ? K4 Bi3 K2 65.69(14) . 1_556 ? K3 Bi3 K2 102.29(13) . 1_556 ? Sn1 Bi3 K2 65.02(10) . . ? K4 Bi3 K2 97.96(14) . . ? K3 Bi3 K2 67.19(13) . . ? K2 Bi3 K2 129.37(13) 1_556 . ? Bi1 Sn1 Bi2 119.56(5) . . ? Bi1 Sn1 Bi3 119.84(6) . . ? Bi2 Sn1 Bi3 120.59(6) . . ? Bi1 Sn1 K2 135.93(11) . 1_556 ? Bi2 Sn1 K2 68.46(10) . 1_556 ? Bi3 Sn1 K2 70.46(10) . 1_556 ? Bi1 Sn1 K2 70.11(10) . . ? Bi2 Sn1 K2 131.84(11) . . ? Bi3 Sn1 K2 70.15(9) . . ? K2 Sn1 K2 140.42(15) 1_556 . ? Bi1 Sn1 K1 67.14(9) . . ? Bi2 Sn1 K1 68.08(9) . . ? Bi3 Sn1 K1 140.03(11) . . ? K2 Sn1 K1 79.35(13) 1_556 . ? K2 Sn1 K1 136.68(13) . . ? Bi1 Sn1 K5 65.91(9) . . ? Bi2 Sn1 K5 68.18(9) . . ? Bi3 Sn1 K5 139.91(11) . . ? K2 Sn1 K5 136.32(14) 1_556 . ? K2 Sn1 K5 76.61(13) . . ? K1 Sn1 K5 80.01(11) . . ? Bi1 Sn1 K3 61.35(9) . . ? Bi2 Sn1 K3 163.08(11) . . ? Bi3 Sn1 K3 61.63(10) . . ? K2 Sn1 K3 98.87(13) 1_556 . ? K2 Sn1 K3 65.07(13) . . ? K1 Sn1 K3 99.28(13) . . ? K5 Sn1 K3 122.25(13) . . ? Bi1 Sn1 K4 160.60(11) . . ? Bi2 Sn1 K4 62.84(9) . . ? Bi3 Sn1 K4 61.11(9) . . ? K2 Sn1 K4 63.47(13) 1_556 . ? K2 Sn1 K4 93.88(13) . . ? K1 Sn1 K4 126.16(13) . . ? K5 Sn1 K4 100.48(13) . . ? K3 Sn1 K4 122.71(13) . . ? N9 K1 N1 93.6(7) 2_565 . ? N9 K1 N7 84.1(6) 2_565 . ? N1 K1 N7 86.9(7) . . ? N9 K1 Bi1 150.2(4) 2_565 . ? N1 K1 Bi1 99.8(5) . . ? N7 K1 Bi1 70.3(4) . . ? N9 K1 Sn1 143.6(4) 2_565 . ? N1 K1 Sn1 119.2(5) . . ? N7 K1 Sn1 111.2(5) . . ? Bi1 K1 Sn1 44.73(7) . . ? N9 K1 Bi1 76.1(4) 2_565 1_556 ? N1 K1 Bi1 67.8(5) . 1_556 ? N7 K1 Bi1 146.4(5) . 1_556 ? Bi1 K1 Bi1 133.60(14) . 1_556 ? Sn1 K1 Bi1 100.66(12) . 1_556 ? N9 K1 Bi2 99.1(4) 2_565 . ? N1 K1 Bi2 150.3(5) . . ? N7 K1 Bi2 120.9(5) . . ? Bi1 K1 Bi2 82.07(11) . . ? Sn1 K1 Bi2 44.53(6) . . ? Bi1 K1 Bi2 89.26(12) 1_556 . ? N9 K1 K5 43.2(4) 2_565 2_565 ? N1 K1 K5 93.7(5) . 2_565 ? N7 K1 K5 41.1(4) . 2_565 ? Bi1 K1 K5 108.96(13) . 2_565 ? Sn1 K1 K5 138.28(16) . 2_565 ? Bi1 K1 K5 116.12(13) 1_556 2_565 ? Bi2 K1 K5 113.96(15) . 2_565 ? N9 K1 K5 55.6(4) 2_565 1_556 ? N1 K1 K5 116.7(5) . 1_556 ? N7 K1 K5 132.5(5) . 1_556 ? Bi1 K1 K5 135.46(15) . 1_556 ? Sn1 K1 K5 93.14(13) . 1_556 ? Bi1 K1 K5 52.73(9) 1_556 1_556 ? Bi2 K1 K5 53.53(11) . 1_556 ? K5 K1 K5 93.98(14) 2_565 1_556 ? N9 K1 K2 113.7(4) 2_565 1_556 ? N1 K1 K2 100.0(5) . 1_556 ? N7 K1 K2 160.2(5) . 1_556 ? Bi1 K1 K2 90.12(14) . 1_556 ? Sn1 K1 K2 49.28(12) . 1_556 ? Bi1 K1 K2 51.78(12) 1_556 1_556 ? Bi2 K1 K2 50.30(10) . 1_556 ? K5 K1 K2 154.33(17) 2_565 1_556 ? K5 K1 K2 60.46(13) 1_556 1_556 ? N9 K1 K5 109.9(4) 2_565 . ? N1 K1 K5 146.7(5) . . ? N7 K1 K5 73.0(5) . . ? Bi1 K1 K5 48.77(9) . . ? Sn1 K1 K5 50.00(9) . . ? Bi1 K1 K5 139.38(14) 1_556 . ? Bi2 K1 K5 50.30(10) . . ? K5 K1 K5 88.36(13) 2_565 . ? K5 K1 K5 96.30(13) 1_556 . ? K2 K1 K5 91.93(14) 1_556 . ? N9 K1 H7B 99.7 2_565 . ? N1 K1 H7B 78.8 . . ? N7 K1 H7B 17.2 . . ? Bi1 K1 H7B 57.8 . . ? Sn1 K1 H7B 101.8 . . ? Bi1 K1 H7B 145.8 1_556 . ? Bi2 K1 H7B 124.7 . . ? K5 K1 H7B 57.5 2_565 . ? K5 K1 H7B 149.6 1_556 . ? K2 K1 H7B 146.6 1_556 . ? K5 K1 H7B 74.4 . . ? N9 K1 H9C 74.0 2_565 . ? N1 K1 H9C 132.1 . . ? N7 K1 H9C 46.5 . . ? Bi1 K1 H9C 77.2 . . ? Sn1 K1 H9C 92.5 . . ? Bi1 K1 H9C 144.8 1_556 . ? Bi2 K1 H9C 77.5 . . ? K5 K1 H9C 46.0 2_565 . ? K5 K1 H9C 94.4 1_556 . ? K2 K1 H9C 127.6 1_556 . ? K5 K1 H9C 42.5 . . ? H7B K1 H9C 59.0 . . ? N6 K2 N2 120.1(7) 1_554 . ? N6 K2 Sn1 108.9(5) 1_554 1_554 ? N2 K2 Sn1 94.9(8) . 1_554 ? N6 K2 Sn1 90.5(5) 1_554 . ? N2 K2 Sn1 105.0(7) . . ? Sn1 K2 Sn1 140.42(15) 1_554 . ? N6 K2 Bi2 87.0(5) 1_554 1_554 ? N2 K2 Bi2 139.6(8) . 1_554 ? Sn1 K2 Bi2 45.62(9) 1_554 1_554 ? Sn1 K2 Bi2 104.12(15) . 1_554 ? N6 K2 Bi3 90.2(5) 1_554 1_554 ? N2 K2 Bi3 69.0(7) . 1_554 ? Sn1 K2 Bi3 45.05(11) 1_554 1_554 ? Sn1 K2 Bi3 173.32(18) . 1_554 ? Bi2 K2 Bi3 82.55(17) 1_554 1_554 ? N6 K2 Bi1 132.3(5) 1_554 . ? N2 K2 Bi1 91.8(6) . . ? Sn1 K2 Bi1 101.90(14) 1_554 . ? Sn1 K2 Bi1 44.72(9) . . ? Bi2 K2 Bi1 89.51(10) 1_554 . ? Bi3 K2 Bi1 136.3(2) 1_554 . ? N6 K2 Bi3 72.7(5) 1_554 . ? N2 K2 Bi3 79.1(8) . . ? Sn1 K2 Bi3 173.49(19) 1_554 . ? Sn1 K2 Bi3 44.84(10) . . ? Bi2 K2 Bi3 140.7(2) 1_554 . ? Bi3 K2 Bi3 129.38(13) 1_554 . ? Bi1 K2 Bi3 80.80(16) . . ? N6 K2 K4 46.5(5) 1_554 1_554 ? N2 K2 K4 119.0(6) . 1_554 ? Sn1 K2 K4 62.53(16) 1_554 1_554 ? Sn1 K2 K4 129.0(2) . 1_554 ? Bi2 K2 K4 56.94(13) 1_554 1_554 ? Bi3 K2 K4 54.94(14) 1_554 1_554 ? Bi1 K2 K4 145.25(17) . 1_554 ? Bi3 K2 K4 118.34(18) . 1_554 ? N6 K2 K3 125.8(5) 1_554 . ? N2 K2 K3 45.1(7) . . ? Sn1 K2 K3 122.62(19) 1_554 . ? Sn1 K2 K3 60.93(15) . . ? Bi2 K2 K3 141.29(17) 1_554 . ? Bi3 K2 K3 113.57(17) 1_554 . ? Bi1 K2 K3 54.01(13) . . ? Bi3 K2 K3 54.23(13) . . ? K4 K2 K3 160.74(18) 1_554 . ? N6 K2 K5 92.4(4) 1_554 . ? N2 K2 K5 142.4(6) . . ? Sn1 K2 K5 91.42(13) 1_554 . ? Sn1 K2 K5 52.51(11) . . ? Bi2 K2 K5 51.88(10) 1_554 . ? Bi3 K2 K5 134.08(19) 1_554 . ? Bi1 K2 K5 50.69(10) . . ? Bi3 K2 K5 94.83(18) . . ? K4 K2 K5 96.67(16) 1_554 . ? K3 K2 K5 101.56(18) . . ? N6 K2 K1 137.3(5) 1_554 1_554 ? N2 K2 K1 100.7(6) . 1_554 ? Sn1 K2 K1 51.36(10) 1_554 1_554 ? Sn1 K2 K1 90.93(13) . 1_554 ? Bi2 K2 K1 51.45(10) 1_554 1_554 ? Bi3 K2 K1 93.05(17) 1_554 1_554 ? Bi1 K2 K1 50.94(9) . 1_554 ? Bi3 K2 K1 131.73(18) . 1_554 ? K4 K2 K1 104.01(19) 1_554 1_554 ? K3 K2 K1 91.34(15) . 1_554 ? K5 K2 K1 56.33(10) . 1_554 ? N4 K3 N3 105.7(6) . . ? N4 K3 N2 104.1(9) . . ? N3 K3 N2 94.4(9) . . ? N4 K3 N5 75.2(7) . . ? N3 K3 N5 83.6(8) . . ? N2 K3 N5 177.5(8) . . ? N4 K3 Bi1 78.6(4) . . ? N3 K3 Bi1 160.9(7) . . ? N2 K3 Bi1 102.6(6) . . ? N5 K3 Bi1 79.5(5) . . ? N4 K3 Bi3 162.6(5) . . ? N3 K3 Bi3 86.2(5) . . ? N2 K3 Bi3 87.2(7) . . ? N5 K3 Bi3 94.1(5) . . ? Bi1 K3 Bi3 86.09(13) . . ? N4 K3 K4 65.0(5) . 1_545 ? N3 K3 K4 48.6(5) . 1_545 ? N2 K3 K4 128.3(6) . 1_545 ? N5 K3 K4 49.3(5) . 1_545 ? Bi1 K3 K4 122.00(18) . 1_545 ? Bi3 K3 K4 118.20(17) . 1_545 ? N4 K3 Sn1 119.1(5) . . ? N3 K3 Sn1 123.0(6) . . ? N2 K3 Sn1 106.0(6) . . ? N5 K3 Sn1 76.3(5) . . ? Bi1 K3 Sn1 43.84(7) . . ? Bi3 K3 Sn1 43.92(7) . . ? K4 K3 Sn1 123.82(17) 1_545 . ? N4 K3 K2 117.9(5) . . ? N3 K3 K2 129.7(5) . . ? N2 K3 K2 53.2(6) . . ? N5 K3 K2 129.3(5) . . ? Bi1 K3 K2 58.59(11) . . ? Bi3 K3 K2 58.57(14) . . ? K4 K3 K2 176.8(2) 1_545 . ? Sn1 K3 K2 54.00(13) . . ? N4 K3 H2B 86.9 . . ? N3 K3 H2B 93.9 . . ? N2 K3 H2B 18.0 . . ? N5 K3 H2B 160.4 . . ? Bi1 K3 H2B 104.9 . . ? Bi3 K3 H2B 105.2 . . ? K4 K3 H2B 115.8 1_545 . ? Sn1 K3 H2B 120.3 . . ? K2 K3 H2B 66.3 . . ? N4 K3 H3B 123.3 . . ? N3 K3 H3B 18.0 . . ? N2 K3 H3B 92.8 . . ? N5 K3 H3B 85.7 . . ? Bi1 K3 H3B 149.4 . . ? Bi3 K3 H3B 68.3 . . ? K4 K3 H3B 62.3 1_545 . ? Sn1 K3 H3B 106.7 . . ? K2 K3 H3B 115.5 . . ? H2B K3 H3B 97.9 . . ? N4 K3 H5A 76.2 . . ? N3 K3 H5A 100.2 . . ? N2 K3 H5A 164.8 . . ? N5 K3 H5A 17.6 . . ? Bi1 K3 H5A 62.3 . . ? Bi3 K3 H5A 89.4 . . ? K4 K3 H5A 66.0 1_545 . ? Sn1 K3 H5A 62.2 . . ? K2 K3 H5A 112.9 . . ? H2B K3 H5A 160.4 . . ? H3B K3 H5A 99.7 . . ? N6 K4 N3 106.6(8) . 1_565 ? N6 K4 N5 96.1(7) . 1_565 ? N3 K4 N5 82.8(7) 1_565 1_565 ? N6 K4 Bi3 99.2(5) . . ? N3 K4 Bi3 113.5(5) 1_565 . ? N5 K4 Bi3 153.0(5) 1_565 . ? N6 K4 Bi2 92.0(5) . . ? N3 K4 Bi2 150.3(5) 1_565 . ? N5 K4 Bi2 72.0(5) 1_565 . ? Bi3 K4 Bi2 85.29(13) . . ? N6 K4 K3 132.7(5) . 1_565 ? N3 K4 K3 47.7(5) 1_565 1_565 ? N5 K4 K3 49.2(5) 1_565 1_565 ? Bi3 K4 K3 126.33(19) . 1_565 ? Bi2 K4 K3 102.75(17) . 1_565 ? N6 K4 Sn1 107.2(5) . . ? N3 K4 Sn1 142.0(7) 1_565 . ? N5 K4 Sn1 110.3(5) 1_565 . ? Bi3 K4 Sn1 43.72(7) . . ? Bi2 K4 Sn1 43.30(7) . . ? K3 K4 Sn1 114.37(18) 1_565 . ? N6 K4 K2 53.3(5) . 1_556 ? N3 K4 K2 152.0(6) 1_565 1_556 ? N5 K4 K2 115.6(5) 1_565 1_556 ? Bi3 K4 K2 59.37(14) . 1_556 ? Bi2 K4 K2 57.21(11) . 1_556 ? K3 K4 K2 159.8(2) 1_565 1_556 ? Sn1 K4 K2 54.00(13) . 1_556 ? N6 K4 H6C 17.9 . . ? N3 K4 H6C 89.2 1_565 . ? N5 K4 H6C 98.4 1_565 . ? Bi3 K4 H6C 103.0 . . ? Bi2 K4 H6C 109.6 . . ? K3 K4 H6C 122.4 1_565 . ? Sn1 K4 H6C 122.0 . . ? K2 K4 H6C 68.3 1_556 . ? N7 K5 N8 72.1(7) 2_564 . ? N7 K5 N9 84.6(6) 2_564 . ? N8 K5 N9 75.3(7) . . ? N7 K5 Bi1 127.4(5) 2_564 . ? N8 K5 Bi1 155.5(5) . . ? N9 K5 Bi1 90.6(4) . . ? N7 K5 Bi2 74.9(5) 2_564 1_554 ? N8 K5 Bi2 109.8(5) . 1_554 ? N9 K5 Bi2 155.5(4) . 1_554 ? Bi1 K5 Bi2 91.37(12) . 1_554 ? N7 K5 Sn1 172.3(5) 2_564 . ? N8 K5 Sn1 115.6(5) . . ? N9 K5 Sn1 96.4(4) . . ? Bi1 K5 Sn1 45.07(7) . . ? Bi2 K5 Sn1 102.24(12) 1_554 . ? N7 K5 Bi2 142.2(5) 2_564 . ? N8 K5 Bi2 73.8(5) . . ? N9 K5 Bi2 71.4(4) . . ? Bi1 K5 Bi2 82.76(11) . . ? Bi2 K5 Bi2 133.06(14) 1_554 . ? Sn1 K5 Bi2 44.50(7) . . ? N7 K5 K1 43.9(5) 2_564 2_564 ? N8 K5 K1 71.2(5) . 2_564 ? N9 K5 K1 40.9(4) . 2_564 ? Bi1 K5 K1 110.92(15) . 2_564 ? Bi2 K5 K1 116.59(13) 1_554 2_564 ? Sn1 K5 K1 135.88(16) . 2_564 ? Bi2 K5 K1 108.88(13) . 2_564 ? N7 K5 K1 77.5(5) 2_564 1_554 ? N8 K5 K1 148.9(5) . 1_554 ? N9 K5 K1 108.5(4) . 1_554 ? Bi1 K5 K1 54.60(11) . 1_554 ? Bi2 K5 K1 54.54(9) 1_554 1_554 ? Sn1 K5 K1 94.96(13) . 1_554 ? Bi2 K5 K1 137.22(15) . 1_554 ? K1 K5 K1 91.33(13) 2_564 1_554 ? N7 K5 K2 125.2(5) 2_564 . ? N8 K5 K2 132.3(5) . . ? N9 K5 K2 141.9(4) . . ? Bi1 K5 K2 53.31(10) . . ? Bi2 K5 K2 51.62(12) 1_554 . ? Sn1 K5 K2 50.88(12) . . ? Bi2 K5 K2 90.19(14) . . ? K1 K5 K2 154.41(17) 2_564 . ? K1 K5 K2 63.21(13) 1_554 . ? N7 K5 K1 128.5(5) 2_564 . ? N8 K5 K1 107.5(5) . . ? N9 K5 K1 48.4(4) . . ? Bi1 K5 K1 49.78(10) . . ? Bi2 K5 K1 140.97(14) 1_554 . ? Sn1 K5 K1 49.99(9) . . ? Bi2 K5 K1 50.22(9) . . ? K1 K5 K1 85.93(13) 2_564 . ? K1 K5 K1 96.31(13) 1_554 . ? K2 K5 K1 94.04(14) . . ? N7 K5 H9B 98.7 2_564 . ? N8 K5 H9B 70.3 . . ? N9 K5 H9B 17.5 . . ? Bi1 K5 H9B 90.2 . . ? Bi2 K5 H9B 172.9 1_554 . ? Sn1 K5 H9B 83.7 . . ? Bi2 K5 H9B 54.0 . . ? K1 K5 H9B 56.5 2_564 . ? K1 K5 H9B 121.6 1_554 . ? K2 K5 H9B 133.8 . . ? K1 K5 H9B 41.7 . . ? K1 N1 H1A 109.4 . . ? K1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? K1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? K3 N2 K2 81.7(8) . . ? K3 N2 H2A 146.5 . . ? K2 N2 H2A 69.9 . . ? K3 N2 H2B 73.8 . . ? K2 N2 H2B 127.3 . . ? H2A N2 H2B 109.5 . . ? K3 N2 H2C 100.0 . . ? K2 N2 H2C 120.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? K3 N3 K4 83.7(6) . 1_545 ? K3 N3 H3A 150.7 . . ? K4 N3 H3A 69.5 1_545 . ? K3 N3 H3B 79.4 . . ? K4 N3 H3B 132.0 1_545 . ? H3A N3 H3B 109.5 . . ? K3 N3 H3C 92.6 . . ? K4 N3 H3C 115.9 1_545 . ? H3A N3 H3C 109.5 . . ? H3B N3 H3C 109.5 . . ? K3 N4 H4A 109.5 . . ? K3 N4 H4B 109.5 . . ? H4A N4 H4B 109.5 . . ? K3 N4 H4C 109.4 . . ? H4A N4 H4C 109.5 . . ? H4B N4 H4C 109.5 . . ? K3 N5 K4 81.5(6) . 1_545 ? K3 N5 H5A 67.0 . . ? K4 N5 H5A 143.3 1_545 . ? K3 N5 H5B 96.3 . . ? K4 N5 H5B 91.7 1_545 . ? H5A N5 H5B 109.5 . . ? K3 N5 H5C 153.1 . . ? K4 N5 H5C 89.9 1_545 . ? H5A N5 H5C 109.5 . . ? H5B N5 H5C 109.5 . . ? K4 N6 K2 80.2(6) . 1_556 ? K4 N6 H6A 144.1 . . ? K2 N6 H6A 74.0 1_556 . ? K4 N6 H6B 102.7 . . ? K2 N6 H6B 110.7 1_556 . ? H6A N6 H6B 109.5 . . ? K4 N6 H6C 72.9 . . ? K2 N6 H6C 135.5 1_556 . ? H6A N6 H6C 109.5 . . ? H6B N6 H6C 109.5 . . ? K5 N7 K1 95.0(7) 2_565 . ? K5 N7 H7A 70.5 2_565 . ? K1 N7 H7A 138.7 . . ? K5 N7 H7B 154.1 2_565 . ? K1 N7 H7B 67.6 . . ? H7A N7 H7B 109.5 . . ? K5 N7 H7C 94.2 2_565 . ? K1 N7 H7C 110.0 . . ? H7A N7 H7C 109.5 . . ? H7B N7 H7C 109.5 . . ? K5 N8 H8A 109.5 . . ? K5 N8 H8B 109.5 . . ? H8A N8 H8B 109.5 . . ? K5 N8 H8C 109.5 . . ? H8A N8 H8C 109.5 . . ? H8B N8 H8C 109.5 . . ? K1 N9 K5 95.9(7) 2_564 . ? K1 N9 H9A 65.8 2_564 . ? K5 N9 H9A 148.6 . . ? K1 N9 H9B 147.4 2_564 . ? K5 N9 H9B 71.6 . . ? H9A N9 H9B 109.5 . . ? K1 N9 H9C 102.1 2_564 . ? K5 N9 H9C 98.9 . . ? H9A N9 H9C 109.5 . . ? H9B N9 H9C 109.5 . . ? #============================================================================== # END of CIF #==============================================================================