# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Christoph Marschner' _publ_contact_author_email CHRISTOPH.MARSCHNER@TUGRAZ.AT _publ_section_title ; Synthesis and Structural Diversity of Oligosilanylzinc Compounds ; loop_ _publ_author_name 'Christoph Marschner' 'Judith Baumgartner' 'Walter Gaderbauer' 'Harald Wagner' # Attachment '1a_168j-neu.cif' data_168j _database_code_depnum_ccdc_archive 'CCDC 645719' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H49 Cl N2 Si4 Zn' _chemical_formula_weight 542.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 12.093(2) _cell_length_b 14.700(3) _cell_length_c 35.257(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6267(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 14273 _cell_measurement_theta_min 5.531 _cell_measurement_theta_max 52.492 _exptl_crystal_description blocks _exptl_crystal_colour colorless _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.151 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 1.033 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5669 _exptl_absorpt_correction_T_max 0.8047 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'SMART APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34565 _diffrn_reflns_av_R_equivalents 0.0865 _diffrn_reflns_av_sigmaI/netI 0.0552 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 24.71 _reflns_number_total 5225 _reflns_number_gt 3985 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0928P)^2^+8.5845P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5225 _refine_ls_number_parameters 324 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0855 _refine_ls_R_factor_gt 0.0645 _refine_ls_wR_factor_ref 0.1766 _refine_ls_wR_factor_gt 0.1655 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.024 _refine_ls_shift/su_mean 0.002 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 Si2 Si -0.03302(18) 0.39021(13) 0.30975(6) 0.0363(6) Uani 0.606(3) 1 d P A 1 Si3 Si -0.0414(2) 0.64402(14) 0.30262(8) 0.0487(8) Uani 0.606(3) 1 d P A 1 Si4 Si -0.1707(3) 0.5284(6) 0.38382(10) 0.108(2) Uani 0.606(3) 1 d P A 1 C13 C -0.0651(9) 0.2914(6) 0.3405(3) 0.079(4) Uani 0.606(3) 1 d P A 1 H13A H -0.0579 0.2351 0.3258 0.119 Uiso 0.606(3) 1 calc PR A 1 H13B H -0.1409 0.2968 0.3501 0.119 Uiso 0.606(3) 1 calc PR A 1 H13C H -0.0134 0.2900 0.3619 0.119 Uiso 0.606(3) 1 calc PR A 1 C14 C 0.0369(12) 0.6244(14) 0.2578(4) 0.138(3) Uani 0.606(3) 1 d P A 1 H14A H 0.0068 0.5710 0.2447 0.207 Uiso 0.606(3) 1 calc PR A 1 H14B H 0.1151 0.6140 0.2637 0.207 Uiso 0.606(3) 1 calc PR A 1 H14C H 0.0300 0.6779 0.2413 0.207 Uiso 0.606(3) 1 calc PR A 1 C15 C -0.2020(11) 0.6443(8) 0.4038(3) 0.138(3) Uani 0.606(3) 1 d P A 1 H15A H -0.2721 0.6423 0.4177 0.207 Uiso 0.606(3) 1 calc PR A 1 H15B H -0.2078 0.6884 0.3830 0.207 Uiso 0.606(3) 1 calc PR A 1 H15C H -0.1424 0.6627 0.4210 0.207 Uiso 0.606(3) 1 calc PR A 1 C9 C 0.0162(14) 0.7544(8) 0.3170(4) 0.098(7) Uani 0.606(3) 1 d PR A 1 H9A H 0.0878 0.7430 0.3283 0.147 Uiso 0.606(3) 1 d PR A 1 H9B H -0.0318 0.7836 0.3351 0.147 Uiso 0.606(3) 1 d PR A 1 H9C H 0.0262 0.7931 0.2957 0.147 Uiso 0.606(3) 1 d PR A 1 C7 C -0.1399(17) 0.399(2) 0.2711(5) 0.059(3) Uani 0.606(3) 1 d P A 1 H7A H -0.1047 0.4198 0.2477 0.088 Uiso 0.606(3) 1 calc PR A 1 H7B H -0.1974 0.4421 0.2787 0.088 Uiso 0.606(3) 1 calc PR A 1 H7C H -0.1733 0.3389 0.2669 0.088 Uiso 0.606(3) 1 calc PR A 1 C11 C -0.2972(16) 0.4694(11) 0.3626(5) 0.080(5) Uani 0.606(3) 1 d PR A 1 H11A H -0.3126 0.4949 0.3374 0.120 Uiso 0.606(3) 1 calc PR A 1 H11B H -0.3613 0.4791 0.3791 0.120 Uiso 0.606(3) 1 calc PR A 1 H11C H -0.2827 0.4041 0.3603 0.120 Uiso 0.606(3) 1 calc PR A 1 Si5 Si -0.0027(3) 0.4490(2) 0.28897(9) 0.0416(11) Uani 0.394(3) 1 d P A 2 Si6 Si -0.0649(3) 0.6772(2) 0.32956(10) 0.0418(11) Uani 0.394(3) 1 d P A 2 Si7 Si -0.1517(4) 0.4712(4) 0.38370(15) 0.0530(15) Uani 0.394(3) 1 d P A 2 C16 C 0.0629(13) 0.5172(11) 0.2492(3) 0.058(4) Uani 0.394(3) 1 d P A 2 H16A H 0.1428 0.5217 0.2535 0.087 Uiso 0.394(3) 1 calc PR A 2 H16B H 0.0307 0.5784 0.2486 0.087 Uiso 0.394(3) 1 calc PR A 2 H16C H 0.0490 0.4868 0.2249 0.087 Uiso 0.394(3) 1 calc PR A 2 C17 C -0.126(2) 0.7339(14) 0.3749(5) 0.142(14) Uani 0.394(3) 1 d P A 2 H17A H -0.0718 0.7296 0.3956 0.213 Uiso 0.394(3) 1 calc PR A 2 H17B H -0.1939 0.7026 0.3822 0.213 Uiso 0.394(3) 1 calc PR A 2 H17C H -0.1417 0.7980 0.3697 0.213 Uiso 0.394(3) 1 calc PR A 2 C18 C -0.1333(18) 0.3390(15) 0.3818(5) 0.138(3) Uani 0.394(3) 1 d P A 2 H18A H -0.0641 0.3242 0.3688 0.207 Uiso 0.394(3) 1 calc PR A 2 H18B H -0.1956 0.3119 0.3681 0.207 Uiso 0.394(3) 1 calc PR A 2 H18C H -0.1311 0.3148 0.4077 0.207 Uiso 0.394(3) 1 calc PR A 2 C9A C 0.049(3) 0.7531(15) 0.3194(10) 0.25(4) Uani 0.394(3) 1 d PR A 2 H9A1 H 0.0756 0.7332 0.2945 0.372 Uiso 0.394(3) 1 d PR A 2 H9A2 H 0.1070 0.7557 0.3376 0.372 Uiso 0.394(3) 1 d PR A 2 H9A3 H 0.0174 0.8124 0.3166 0.372 Uiso 0.394(3) 1 d PR A 2 C11A C -0.3011(18) 0.5159(13) 0.3638(8) 0.053(6) Uani 0.394(3) 1 d P A 2 H11D H -0.3542 0.5189 0.3847 0.080 Uiso 0.394(3) 1 calc PR A 2 H11E H -0.3284 0.4738 0.3444 0.080 Uiso 0.394(3) 1 calc PR A 2 H11F H -0.2923 0.5766 0.3526 0.080 Uiso 0.394(3) 1 calc PR A 2 C7A C -0.146(3) 0.410(4) 0.2735(10) 0.059(3) Uani 0.394(3) 1 d P A 2 H7A1 H -0.1386 0.3602 0.2550 0.088 Uiso 0.394(3) 1 calc PR A 2 H7A2 H -0.1857 0.4606 0.2619 0.088 Uiso 0.394(3) 1 calc PR A 2 H7A3 H -0.1872 0.3879 0.2956 0.088 Uiso 0.394(3) 1 calc PR A 2 Zn1 Zn 0.15224(4) 0.50647(3) 0.379725(13) 0.0274(2) Uani 1 1 d . A . Cl1 Cl 0.19299(11) 0.36302(7) 0.39971(4) 0.0476(4) Uani 1 1 d . . . Si1 Si -0.01439(10) 0.52695(8) 0.34549(3) 0.0315(3) Uani 1 1 d . . . N1 N 0.1981(4) 0.5818(3) 0.42897(10) 0.0415(9) Uani 1 1 d . . . N4 N 0.3100(3) 0.5510(2) 0.35776(10) 0.0333(8) Uani 1 1 d . . . C1 C 0.1423(5) 0.6711(4) 0.42995(16) 0.0572(15) Uani 1 1 d . A . H1A H 0.1746 0.7085 0.4501 0.086 Uiso 1 1 calc R . . H1B H 0.0633 0.6623 0.4349 0.086 Uiso 1 1 calc R . . H1C H 0.1519 0.7017 0.4055 0.086 Uiso 1 1 calc R . . C2 C 0.1739(7) 0.5347(5) 0.46481(14) 0.076(2) Uani 1 1 d . A . H2A H 0.2066 0.4737 0.4643 0.114 Uiso 1 1 calc R . . H2B H 0.0936 0.5297 0.4680 0.114 Uiso 1 1 calc R . . H2C H 0.2052 0.5693 0.4860 0.114 Uiso 1 1 calc R . . C3 C 0.3179(5) 0.5917(6) 0.42481(16) 0.076(2) Uani 1 1 d . A . H3A H 0.3435 0.6411 0.4418 0.091 Uiso 1 1 calc R . . H3B H 0.3540 0.5347 0.4331 0.091 Uiso 1 1 calc R . . C4 C 0.3524(5) 0.6116(6) 0.38723(18) 0.081(2) Uani 1 1 d . A . H4A H 0.4342 0.6098 0.3864 0.097 Uiso 1 1 calc R . . H4B H 0.3294 0.6745 0.3811 0.097 Uiso 1 1 calc R . . C5 C 0.3829(5) 0.4760(4) 0.3497(2) 0.0639(16) Uani 1 1 d . A . H5A H 0.4541 0.4994 0.3407 0.096 Uiso 1 1 calc R . . H5B H 0.3498 0.4373 0.3302 0.096 Uiso 1 1 calc R . . H5C H 0.3945 0.4403 0.3729 0.096 Uiso 1 1 calc R . . C6 C 0.2979(6) 0.6022(5) 0.3223(2) 0.082(2) Uani 1 1 d . A . H6A H 0.3691 0.6295 0.3154 0.123 Uiso 1 1 calc R . . H6B H 0.2428 0.6504 0.3257 0.123 Uiso 1 1 calc R . . H6C H 0.2738 0.5610 0.3021 0.123 Uiso 1 1 calc R . . C8 C 0.0980(6) 0.3574(5) 0.2905(2) 0.090(3) Uani 1 1 d . . . H8D H 0.0867 0.3274 0.2659 0.135 Uiso 0.606(3) 1 calc PR A 1 H8E H 0.1347 0.3152 0.3079 0.135 Uiso 0.606(3) 1 calc PR A 1 H8F H 0.1442 0.4115 0.2870 0.135 Uiso 0.606(3) 1 calc PR A 1 H8A H 0.0899 0.3022 0.2761 0.135 Uiso 0.394(3) 1 d PR A 2 H8B H 0.1246 0.4049 0.2742 0.135 Uiso 0.394(3) 1 d PR A 2 H8C H 0.1498 0.3477 0.3107 0.135 Uiso 0.394(3) 1 d PR A 2 C12 C -0.1454(7) 0.4831(8) 0.4300(2) 0.138(3) Uani 1 1 d . . . H12A H -0.1243 0.4189 0.4278 0.207 Uiso 1 1 calc R A 1 H12B H -0.2126 0.4883 0.4454 0.207 Uiso 1 1 calc R A 1 H12C H -0.0853 0.5172 0.4421 0.207 Uiso 1 1 calc R A 1 C60 C 0.9762(7) 0.7353(5) 0.5229(2) 0.076(2) Uani 1 1 d . . . H60 H 0.9723 0.6853 0.5399 0.092 Uiso 1 1 calc R . . C61 C 0.9836(12) 0.8758(8) 0.4750(3) 0.139(6) Uani 1 1 d . . . H61 H 0.9836 0.9263 0.4582 0.167 Uiso 1 1 calc R . . C62 C 1.0656(8) 0.8675(7) 0.5019(4) 0.130(4) Uani 1 1 d . . . H62 H 1.1245 0.9101 0.5036 0.156 Uiso 1 1 calc R . . C63 C 0.8991(8) 0.7445(5) 0.4962(2) 0.085(2) Uani 1 1 d . . . H63 H 0.8409 0.7013 0.4945 0.102 Uiso 1 1 calc R . . C64 C 1.0583(7) 0.7944(6) 0.5262(2) 0.091(2) Uani 1 1 d . . . H64 H 1.1124 0.7863 0.5454 0.109 Uiso 1 1 calc R . . C65 C 0.9027(10) 0.8122(8) 0.4725(2) 0.107(3) Uani 1 1 d . . . H65 H 0.8482 0.8171 0.4532 0.129 Uiso 1 1 calc R . . C10 C -0.1862(6) 0.6645(4) 0.29094(19) 0.0720(19) Uani 1 1 d . . . H10A H -0.2205 0.6075 0.2825 0.108 Uiso 1 1 calc R A 1 H10B H -0.1910 0.7097 0.2706 0.108 Uiso 1 1 calc R A 1 H10C H -0.2250 0.6872 0.3134 0.108 Uiso 1 1 calc R A 1 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 Si2 0.0300(12) 0.0250(11) 0.0538(13) 0.0033(9) -0.0114(10) -0.0063(9) Si3 0.0632(17) 0.0254(11) 0.0576(17) 0.0029(10) -0.0301(13) 0.0018(10) Si4 0.0358(19) 0.252(7) 0.0379(17) 0.025(3) 0.0029(13) 0.036(3) C13 0.058(7) 0.042(5) 0.138(10) 0.038(6) -0.057(7) -0.027(5) C14 0.070(4) 0.277(11) 0.068(4) 0.046(5) 0.008(3) 0.012(5) C15 0.070(4) 0.277(11) 0.068(4) 0.046(5) 0.008(3) 0.012(5) C9 0.134(13) 0.027(7) 0.133(12) 0.008(7) -0.119(12) -0.006(7) C7 0.058(4) 0.056(8) 0.062(4) -0.007(4) -0.028(3) -0.006(4) C11 0.041(7) 0.128(15) 0.070(8) 0.015(12) -0.005(6) 0.024(12) Si5 0.046(2) 0.0381(19) 0.0403(19) -0.0089(15) -0.0134(16) 0.0050(16) Si6 0.048(2) 0.0388(19) 0.039(2) 0.0016(16) -0.0196(16) 0.0146(16) Si7 0.032(3) 0.069(3) 0.058(3) 0.044(2) -0.025(2) -0.029(2) C16 0.050(9) 0.089(10) 0.034(7) -0.025(7) 0.007(6) -0.001(8) C17 0.19(3) 0.129(17) 0.106(14) -0.095(13) -0.115(16) 0.150(19) C18 0.070(4) 0.277(11) 0.068(4) 0.046(5) 0.008(3) 0.012(5) C9A 0.30(6) 0.032(14) 0.41(7) 0.08(2) -0.27(5) -0.03(2) C11A 0.012(8) 0.072(13) 0.076(11) 0.032(12) 0.011(7) 0.000(10) C7A 0.058(4) 0.056(8) 0.062(4) -0.007(4) -0.028(3) -0.006(4) Zn1 0.0291(3) 0.0260(3) 0.0272(3) 0.00123(18) -0.00276(19) 0.0038(2) Cl1 0.0495(8) 0.0292(6) 0.0642(8) 0.0150(5) -0.0158(6) -0.0002(5) Si1 0.0307(7) 0.0367(6) 0.0272(6) 0.0019(5) -0.0021(5) 0.0101(5) N1 0.043(2) 0.051(2) 0.0307(19) -0.0081(17) -0.0007(18) 0.000(2) N4 0.032(2) 0.0311(18) 0.0366(19) -0.0048(15) 0.0016(17) -0.0018(16) C1 0.062(4) 0.051(3) 0.059(3) -0.025(3) 0.014(3) -0.007(3) C2 0.114(6) 0.092(4) 0.022(3) 0.001(3) -0.007(3) -0.010(4) C3 0.041(3) 0.138(6) 0.049(3) -0.043(4) -0.012(3) 0.006(4) C4 0.046(4) 0.117(6) 0.079(4) -0.051(4) 0.025(3) -0.039(4) C5 0.042(3) 0.050(3) 0.100(5) 0.000(3) 0.013(3) 0.010(3) C6 0.063(5) 0.089(5) 0.094(5) 0.052(4) 0.029(4) 0.012(4) C8 0.094(6) 0.075(4) 0.101(5) -0.056(4) -0.032(4) 0.037(4) C12 0.070(4) 0.277(11) 0.068(4) 0.046(5) 0.008(3) 0.012(5) C60 0.088(6) 0.063(4) 0.078(5) -0.003(3) 0.037(4) -0.004(4) C61 0.169(13) 0.100(7) 0.149(10) 0.053(7) 0.101(10) 0.065(8) C62 0.069(6) 0.084(6) 0.238(14) 0.004(7) 0.070(8) -0.010(5) C63 0.100(7) 0.082(5) 0.073(5) -0.027(4) 0.019(5) 0.006(5) C64 0.064(5) 0.093(6) 0.116(6) 0.002(5) 0.017(4) 0.022(4) C65 0.142(10) 0.117(7) 0.062(5) -0.009(5) 0.017(5) 0.065(7) C10 0.068(4) 0.062(4) 0.087(4) 0.020(3) -0.038(4) 0.017(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 Si2 C8 1.790(8) . ? Si2 C13 1.854(9) . ? Si2 C7 1.882(19) . ? Si2 Si1 2.383(2) . ? Si3 C10 1.824(7) . ? Si3 C9 1.838(13) . ? Si3 C14 1.866(14) . ? Si3 Si1 2.314(2) . ? Si4 C12 1.785(9) . ? Si4 C15 1.882(13) . ? Si4 C11 1.91(2) . ? Si4 Si1 2.324(4) . ? Si5 C8 1.816(7) . ? Si5 C16 1.898(15) . ? Si5 C7A 1.91(4) . ? Si5 Si1 2.303(3) . ? Si6 C9A 1.81(2) . ? Si6 C17 1.946(18) . ? Si6 C10 2.011(7) . ? Si6 Si1 2.359(3) . ? Si7 C12 1.643(10) . ? Si7 C18 1.96(2) . ? Si7 C11A 2.05(2) . ? Si7 Si1 2.290(5) . ? Zn1 N1 2.133(4) . ? Zn1 N4 2.161(4) . ? Zn1 Cl1 2.2770(12) . ? Zn1 Si1 2.3682(13) . ? N1 C3 1.464(7) . ? N1 C2 1.470(7) . ? N1 C1 1.476(7) . ? N4 C5 1.440(6) . ? N4 C4 1.461(7) . ? N4 C6 1.467(7) . ? C3 C4 1.419(9) . ? C60 C64 1.324(10) . ? C60 C63 1.332(10) . ? C61 C65 1.356(15) . ? C61 C62 1.376(17) . ? C62 C64 1.377(12) . ? C63 C65 1.300(11) . ? 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 C8 Si2 C13 101.3(5) . . ? C8 Si2 C7 110.5(6) . . ? C13 Si2 C7 109.4(11) . . ? C8 Si2 Si1 110.2(2) . . ? C13 Si2 Si1 111.8(4) . . ? C7 Si2 Si1 113.0(10) . . ? C10 Si3 C9 106.3(6) . . ? C10 Si3 C14 108.8(5) . . ? C9 Si3 C14 100.3(7) . . ? C10 Si3 Si1 113.9(2) . . ? C9 Si3 Si1 115.0(5) . . ? C14 Si3 Si1 111.5(6) . . ? C12 Si4 C15 91.8(6) . . ? C12 Si4 C11 109.0(7) . . ? C15 Si4 C11 113.3(7) . . ? C12 Si4 Si1 112.8(3) . . ? C15 Si4 Si1 112.9(5) . . ? C11 Si4 Si1 114.8(6) . . ? C8 Si5 C16 97.6(6) . . ? C8 Si5 C7A 113.1(16) . . ? C16 Si5 C7A 109.2(14) . . ? C8 Si5 Si1 112.7(3) . . ? C16 Si5 Si1 113.7(4) . . ? C7A Si5 Si1 110.0(11) . . ? C9A Si6 C17 100.7(13) . . ? C9A Si6 C10 118.7(13) . . ? C17 Si6 C10 108.7(7) . . ? C9A Si6 Si1 115.3(9) . . ? C17 Si6 Si1 107.6(7) . . ? C10 Si6 Si1 105.2(2) . . ? C12 Si7 C18 97.7(7) . . ? C12 Si7 C11A 110.3(9) . . ? C18 Si7 C11A 114.1(9) . . ? C12 Si7 Si1 120.8(4) . . ? C18 Si7 Si1 104.7(7) . . ? C11A Si7 Si1 108.8(6) . . ? N1 Zn1 N4 84.52(15) . . ? N1 Zn1 Cl1 99.95(11) . . ? N4 Zn1 Cl1 101.56(10) . . ? N1 Zn1 Si1 124.77(12) . . ? N4 Zn1 Si1 122.02(10) . . ? Cl1 Zn1 Si1 117.36(5) . . ? Si7 Si1 Si5 112.04(19) . . ? Si7 Si1 Si3 123.24(15) . . ? Si5 Si1 Si3 79.27(11) . . ? Si7 Si1 Si4 21.8(2) . . ? Si5 Si1 Si4 123.9(2) . . ? Si3 Si1 Si4 104.96(17) . . ? Si7 Si1 Si6 106.72(18) . . ? Si5 Si1 Si6 106.02(13) . . ? Si3 Si1 Si6 27.33(10) . . ? Si4 Si1 Si6 85.4(2) . . ? Si7 Si1 Zn1 105.75(12) . . ? Si5 Si1 Zn1 109.00(10) . . ? Si3 Si1 Zn1 123.22(9) . . ? Si4 Si1 Zn1 113.38(11) . . ? Si6 Si1 Zn1 117.42(10) . . ? Si7 Si1 Si2 86.60(17) . . ? Si5 Si1 Si2 29.36(10) . . ? Si3 Si1 Si2 105.58(9) . . ? Si4 Si1 Si2 103.8(2) . . ? Si6 Si1 Si2 129.74(11) . . ? Zn1 Si1 Si2 104.05(7) . . ? C3 N1 C2 109.3(5) . . ? C3 N1 C1 111.5(5) . . ? C2 N1 C1 107.9(4) . . ? C3 N1 Zn1 103.2(3) . . ? C2 N1 Zn1 113.8(3) . . ? C1 N1 Zn1 111.2(3) . . ? C5 N4 C4 113.0(5) . . ? C5 N4 C6 106.7(5) . . ? C4 N4 C6 109.2(5) . . ? C5 N4 Zn1 112.3(3) . . ? C4 N4 Zn1 103.9(3) . . ? C6 N4 Zn1 111.9(3) . . ? C4 C3 N1 113.9(5) . . ? C3 C4 N4 115.8(5) . . ? Si2 C8 Si5 38.53(19) . . ? Si7 C12 Si4 29.1(3) . . ? C64 C60 C63 121.3(8) . . ? C65 C61 C62 120.2(9) . . ? C64 C62 C61 116.8(9) . . ? C65 C63 C60 120.6(9) . . ? C60 C64 C62 120.4(9) . . ? C63 C65 C61 120.6(10) . . ? Si3 C10 Si6 33.03(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C12 Si7 Si1 Si5 154.3(5) . . . . ? C18 Si7 Si1 Si5 45.8(7) . . . . ? C11A Si7 Si1 Si5 -76.6(8) . . . . ? C12 Si7 Si1 Si3 -114.3(5) . . . . ? C18 Si7 Si1 Si3 137.2(7) . . . . ? C11A Si7 Si1 Si3 14.9(8) . . . . ? C12 Si7 Si1 Si4 -78.2(8) . . . . ? C18 Si7 Si1 Si4 173.2(9) . . . . ? C11A Si7 Si1 Si4 50.9(9) . . . . ? C12 Si7 Si1 Si6 -90.1(6) . . . . ? C18 Si7 Si1 Si6 161.4(7) . . . . ? C11A Si7 Si1 Si6 39.1(8) . . . . ? C12 Si7 Si1 Zn1 35.7(6) . . . . ? C18 Si7 Si1 Zn1 -72.9(7) . . . . ? C11A Si7 Si1 Zn1 164.8(8) . . . . ? C12 Si7 Si1 Si2 139.3(6) . . . . ? C18 Si7 Si1 Si2 30.8(7) . . . . ? C11A Si7 Si1 Si2 -91.5(8) . . . . ? C8 Si5 Si1 Si7 -94.0(4) . . . . ? C16 Si5 Si1 Si7 156.1(6) . . . . ? C7A Si5 Si1 Si7 33.3(17) . . . . ? C8 Si5 Si1 Si3 144.4(4) . . . . ? C16 Si5 Si1 Si3 34.4(6) . . . . ? C7A Si5 Si1 Si3 -88.4(17) . . . . ? C8 Si5 Si1 Si4 -114.7(4) . . . . ? C16 Si5 Si1 Si4 135.3(6) . . . . ? C7A Si5 Si1 Si4 12.5(17) . . . . ? C8 Si5 Si1 Si6 150.0(4) . . . . ? C16 Si5 Si1 Si6 40.1(6) . . . . ? C7A Si5 Si1 Si6 -82.7(17) . . . . ? C8 Si5 Si1 Zn1 22.7(4) . . . . ? C16 Si5 Si1 Zn1 -87.2(6) . . . . ? C7A Si5 Si1 Zn1 150.0(17) . . . . ? C8 Si5 Si1 Si2 -62.2(4) . . . . ? C16 Si5 Si1 Si2 -172.1(6) . . . . ? C7A Si5 Si1 Si2 65.1(17) . . . . ? C10 Si3 Si1 Si7 -18.1(3) . . . . ? C9 Si3 Si1 Si7 105.0(5) . . . . ? C14 Si3 Si1 Si7 -141.7(6) . . . . ? C10 Si3 Si1 Si5 91.4(3) . . . . ? C9 Si3 Si1 Si5 -145.5(5) . . . . ? C14 Si3 Si1 Si5 -32.3(6) . . . . ? C10 Si3 Si1 Si4 -31.1(3) . . . . ? C9 Si3 Si1 Si4 92.0(6) . . . . ? C14 Si3 Si1 Si4 -154.7(6) . . . . ? C10 Si3 Si1 Si6 -76.8(4) . . . . ? C9 Si3 Si1 Si6 46.3(5) . . . . ? C14 Si3 Si1 Si6 159.6(7) . . . . ? C10 Si3 Si1 Zn1 -162.9(3) . . . . ? C9 Si3 Si1 Zn1 -39.8(5) . . . . ? C14 Si3 Si1 Zn1 73.5(6) . . . . ? C10 Si3 Si1 Si2 78.2(3) . . . . ? C9 Si3 Si1 Si2 -158.7(5) . . . . ? C14 Si3 Si1 Si2 -45.4(6) . . . . ? C12 Si4 Si1 Si7 57.1(6) . . . . ? C15 Si4 Si1 Si7 159.5(8) . . . . ? C11 Si4 Si1 Si7 -68.6(9) . . . . ? C12 Si4 Si1 Si5 119.5(5) . . . . ? C15 Si4 Si1 Si5 -138.1(5) . . . . ? C11 Si4 Si1 Si5 -6.2(7) . . . . ? C12 Si4 Si1 Si3 -153.5(5) . . . . ? C15 Si4 Si1 Si3 -51.2(5) . . . . ? C11 Si4 Si1 Si3 80.8(6) . . . . ? C12 Si4 Si1 Si6 -134.3(6) . . . . ? C15 Si4 Si1 Si6 -31.9(5) . . . . ? C11 Si4 Si1 Si6 100.0(6) . . . . ? C12 Si4 Si1 Zn1 -16.4(6) . . . . ? C15 Si4 Si1 Zn1 86.0(5) . . . . ? C11 Si4 Si1 Zn1 -142.0(6) . . . . ? C12 Si4 Si1 Si2 95.9(5) . . . . ? C15 Si4 Si1 Si2 -161.8(5) . . . . ? C11 Si4 Si1 Si2 -29.8(6) . . . . ? C9A Si6 Si1 Si7 152.3(13) . . . . ? C17 Si6 Si1 Si7 40.8(8) . . . . ? C10 Si6 Si1 Si7 -75.0(3) . . . . ? C9A Si6 Si1 Si5 -88.1(13) . . . . ? C17 Si6 Si1 Si5 160.4(8) . . . . ? C10 Si6 Si1 Si5 44.6(3) . . . . ? C9A Si6 Si1 Si3 -76.0(13) . . . . ? C17 Si6 Si1 Si3 172.6(9) . . . . ? C10 Si6 Si1 Si3 56.8(3) . . . . ? C9A Si6 Si1 Si4 147.9(13) . . . . ? C17 Si6 Si1 Si4 36.5(8) . . . . ? C10 Si6 Si1 Si4 -79.3(3) . . . . ? C9A Si6 Si1 Zn1 33.9(13) . . . . ? C17 Si6 Si1 Zn1 -77.5(8) . . . . ? C10 Si6 Si1 Zn1 166.7(2) . . . . ? C9A Si6 Si1 Si2 -108.0(13) . . . . ? C17 Si6 Si1 Si2 140.6(8) . . . . ? C10 Si6 Si1 Si2 24.8(3) . . . . ? N1 Zn1 Si1 Si7 -70.9(2) . . . . ? N4 Zn1 Si1 Si7 -178.1(2) . . . . ? Cl1 Zn1 Si1 Si7 55.73(18) . . . . ? N1 Zn1 Si1 Si5 168.51(17) . . . . ? N4 Zn1 Si1 Si5 61.23(16) . . . . ? Cl1 Zn1 Si1 Si5 -64.91(12) . . . . ? N1 Zn1 Si1 Si3 79.08(17) . . . . ? N4 Zn1 Si1 Si3 -28.19(15) . . . . ? Cl1 Zn1 Si1 Si3 -154.33(10) . . . . ? N1 Zn1 Si1 Si4 -49.2(3) . . . . ? N4 Zn1 Si1 Si4 -156.5(2) . . . . ? Cl1 Zn1 Si1 Si4 77.4(2) . . . . ? N1 Zn1 Si1 Si6 48.02(18) . . . . ? N4 Zn1 Si1 Si6 -59.26(16) . . . . ? Cl1 Zn1 Si1 Si6 174.60(12) . . . . ? N1 Zn1 Si1 Si2 -161.26(14) . . . . ? N4 Zn1 Si1 Si2 91.47(13) . . . . ? Cl1 Zn1 Si1 Si2 -34.67(9) . . . . ? C8 Si2 Si1 Si7 -147.3(3) . . . . ? C13 Si2 Si1 Si7 -35.5(4) . . . . ? C7 Si2 Si1 Si7 88.4(9) . . . . ? C8 Si2 Si1 Si5 61.9(3) . . . . ? C13 Si2 Si1 Si5 173.7(4) . . . . ? C7 Si2 Si1 Si5 -62.3(9) . . . . ? C8 Si2 Si1 Si3 89.1(3) . . . . ? C13 Si2 Si1 Si3 -159.1(4) . . . . ? C7 Si2 Si1 Si3 -35.2(9) . . . . ? C8 Si2 Si1 Si4 -160.8(3) . . . . ? C13 Si2 Si1 Si4 -49.0(4) . . . . ? C7 Si2 Si1 Si4 75.0(9) . . . . ? C8 Si2 Si1 Si6 103.7(3) . . . . ? C13 Si2 Si1 Si6 -144.5(4) . . . . ? C7 Si2 Si1 Si6 -20.5(9) . . . . ? C8 Si2 Si1 Zn1 -42.0(3) . . . . ? C13 Si2 Si1 Zn1 69.9(4) . . . . ? C7 Si2 Si1 Zn1 -166.2(9) . . . . ? N4 Zn1 N1 C3 -18.6(4) . . . . ? Cl1 Zn1 N1 C3 82.2(4) . . . . ? Si1 Zn1 N1 C3 -144.2(4) . . . . ? N4 Zn1 N1 C2 -136.9(4) . . . . ? Cl1 Zn1 N1 C2 -36.1(4) . . . . ? Si1 Zn1 N1 C2 97.5(4) . . . . ? N4 Zn1 N1 C1 101.0(3) . . . . ? Cl1 Zn1 N1 C1 -158.2(3) . . . . ? Si1 Zn1 N1 C1 -24.6(4) . . . . ? N1 Zn1 N4 C5 118.1(4) . . . . ? Cl1 Zn1 N4 C5 19.1(4) . . . . ? Si1 Zn1 N4 C5 -113.9(4) . . . . ? N1 Zn1 N4 C4 -4.3(4) . . . . ? Cl1 Zn1 N4 C4 -103.4(4) . . . . ? Si1 Zn1 N4 C4 123.7(4) . . . . ? N1 Zn1 N4 C6 -122.0(4) . . . . ? Cl1 Zn1 N4 C6 139.0(4) . . . . ? Si1 Zn1 N4 C6 6.0(4) . . . . ? C2 N1 C3 C4 162.7(6) . . . . ? C1 N1 C3 C4 -78.1(7) . . . . ? Zn1 N1 C3 C4 41.3(7) . . . . ? N1 C3 C4 N4 -51.4(9) . . . . ? C5 N4 C4 C3 -92.4(7) . . . . ? C6 N4 C4 C3 149.0(6) . . . . ? Zn1 N4 C4 C3 29.5(7) . . . . ? C13 Si2 C8 Si5 179.8(4) . . . . ? C7 Si2 C8 Si5 63.9(12) . . . . ? Si1 Si2 C8 Si5 -61.7(2) . . . . ? C16 Si5 C8 Si2 -172.4(5) . . . . ? C7A Si5 C8 Si2 -57.7(12) . . . . ? Si1 Si5 C8 Si2 67.9(2) . . . . ? C18 Si7 C12 Si4 -171.3(9) . . . . ? C11A Si7 C12 Si4 -52.0(8) . . . . ? Si1 Si7 C12 Si4 76.4(5) . . . . ? C15 Si4 C12 Si7 -179.0(8) . . . . ? C11 Si4 C12 Si7 65.5(9) . . . . ? Si1 Si4 C12 Si7 -63.2(5) . . . . ? C65 C61 C62 C64 -2.3(14) . . . . ? C64 C60 C63 C65 0.2(11) . . . . ? C63 C60 C64 C62 0.1(11) . . . . ? C61 C62 C64 C60 1.0(13) . . . . ? C60 C63 C65 C61 -1.6(12) . . . . ? C62 C61 C65 C63 2.7(14) . . . . ? C9 Si3 C10 Si6 -53.6(4) . . . . ? C14 Si3 C10 Si6 -160.8(7) . . . . ? Si1 Si3 C10 Si6 74.1(3) . . . . ? C9A Si6 C10 Si3 67.5(9) . . . . ? C17 Si6 C10 Si3 -178.4(9) . . . . ? Si1 Si6 C10 Si3 -63.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.070 _refine_diff_density_min -0.772 _refine_diff_density_rms 0.086 # Attachment '6a_292j_ohne.cif' data_292j _database_code_depnum_ccdc_archive 'CCDC 645720' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H84 Cl K O9 Si8 Zn' _chemical_formula_weight 1001.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.580(4) _cell_length_b 9.934(2) _cell_length_c 32.951(7) _cell_angle_alpha 90.00 _cell_angle_beta 92.20(3) _cell_angle_gamma 90.00 _cell_volume 5750(2) _cell_formula_units_Z 4 _cell_measurement_temperature 233(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.157 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2152 _exptl_absorpt_coefficient_mu 0.752 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7633 _exptl_absorpt_correction_T_max 0.8766 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 233(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44485 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0569 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 26.40 _reflns_number_total 11733 _reflns_number_gt 7890 _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 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0920P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11733 _refine_ls_number_parameters 612 _refine_ls_number_restraints 84 _refine_ls_R_factor_all 0.0825 _refine_ls_R_factor_gt 0.0551 _refine_ls_wR_factor_ref 0.1565 _refine_ls_wR_factor_gt 0.1464 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.033 _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 Si2 Si 0.35073(9) 0.64617(17) 0.77329(4) 0.0439(5) Uani 0.627(3) 1 d PU A 1 C85 C 0.3993(16) 0.683(2) 0.7240(8) 0.071(4) Uani 0.627(3) 1 d PU A 1 H85A H 0.4350 0.6109 0.7186 0.107 Uiso 0.627(3) 1 calc PR A 1 H85B H 0.4263 0.7674 0.7264 0.107 Uiso 0.627(3) 1 calc PR A 1 H85C H 0.3613 0.6879 0.7020 0.107 Uiso 0.627(3) 1 calc PR A 1 C13 C 0.3134(4) 0.4687(5) 0.7680(2) 0.0733(19) Uani 0.627(3) 1 d P A 1 H13A H 0.2801 0.4624 0.7439 0.110 Uiso 0.627(3) 1 calc PR A 1 H13B H 0.2853 0.4455 0.7917 0.110 Uiso 0.627(3) 1 calc PR A 1 H13C H 0.3558 0.4070 0.7655 0.110 Uiso 0.627(3) 1 calc PR A 1 Si5 Si 0.15252(19) 0.6811(4) 0.75866(9) 0.0739(8) Uani 0.627(3) 1 d PU A 1 C17 C 0.1640(11) 0.4915(11) 0.7698(4) 0.225(9) Uani 0.627(3) 1 d PU A 1 H17A H 0.1456 0.4718 0.7965 0.337 Uiso 0.627(3) 1 calc PR A 1 H17B H 0.2174 0.4671 0.7689 0.337 Uiso 0.627(3) 1 calc PR A 1 H17C H 0.1350 0.4403 0.7495 0.337 Uiso 0.627(3) 1 calc PR A 1 C18 C 0.0617(6) 0.715(2) 0.7779(4) 0.234(9) Uani 0.627(3) 1 d PU A 1 H18A H 0.0259 0.6466 0.7684 0.352 Uiso 0.627(3) 1 calc PR A 1 H18B H 0.0443 0.8026 0.7685 0.352 Uiso 0.627(3) 1 calc PR A 1 H18C H 0.0652 0.7142 0.8073 0.352 Uiso 0.627(3) 1 calc PR A 1 Si6 Si 0.27918(12) 1.01295(15) 0.77337(5) 0.0503(5) Uani 0.627(3) 1 d PU A 1 C22 C 0.2688(15) 1.044(2) 0.7170(6) 0.100(6) Uani 0.627(3) 1 d PU A 1 H22A H 0.2814 1.1371 0.7112 0.150 Uiso 0.627(3) 1 calc PR A 1 H22B H 0.2167 1.0262 0.7077 0.150 Uiso 0.627(3) 1 calc PR A 1 H22C H 0.3030 0.9851 0.7029 0.150 Uiso 0.627(3) 1 calc PR A 1 C84 C 0.2093(5) 1.1268(8) 0.7980(3) 0.099(3) Uani 0.627(3) 1 d PU A 1 H84A H 0.1781 1.1718 0.7772 0.148 Uiso 0.627(3) 1 calc PR A 1 H84B H 0.2366 1.1934 0.8144 0.148 Uiso 0.627(3) 1 calc PR A 1 H84C H 0.1770 1.0739 0.8151 0.148 Uiso 0.627(3) 1 calc PR A 1 C21 C 0.3763(4) 1.0640(7) 0.7906(2) 0.084(2) Uani 0.627(3) 1 d P A 1 H21A H 0.4133 1.0126 0.7760 0.126 Uiso 0.627(3) 1 calc PR A 1 H21B H 0.3832 1.0469 0.8195 0.126 Uiso 0.627(3) 1 calc PR A 1 H21C H 0.3832 1.1592 0.7854 0.126 Uiso 0.627(3) 1 calc PR A 1 Si9 Si 0.2233(2) 1.0220(3) 0.77483(9) 0.0622(9) Uani 0.373(3) 1 d PU A 2 C86 C 0.272(2) 1.071(4) 0.7255(12) 0.120(14) Uani 0.373(3) 1 d PU A 2 H86A H 0.2798 0.9904 0.7095 0.180 Uiso 0.373(3) 1 calc PR A 2 H86B H 0.3200 1.1135 0.7321 0.180 Uiso 0.373(3) 1 calc PR A 2 H86C H 0.2391 1.1326 0.7101 0.180 Uiso 0.373(3) 1 calc PR A 2 C20 C 0.2567(10) 1.1304(14) 0.8181(6) 0.131(8) Uani 0.373(3) 1 d PU A 2 H20A H 0.2480 1.2242 0.8112 0.196 Uiso 0.373(3) 1 calc PR A 2 H20B H 0.3107 1.1156 0.8236 0.196 Uiso 0.373(3) 1 calc PR A 2 H20C H 0.2289 1.1079 0.8420 0.196 Uiso 0.373(3) 1 calc PR A 2 C80 C 0.1226(8) 1.0500(13) 0.7698(4) 0.107(5) Uani 0.373(3) 1 d P A 2 H80A H 0.1025 1.0658 0.7964 0.161 Uiso 0.373(3) 1 calc PR A 2 H80B H 0.0981 0.9715 0.7576 0.161 Uiso 0.373(3) 1 calc PR A 2 H80C H 0.1126 1.1280 0.7526 0.161 Uiso 0.373(3) 1 calc PR A 2 Si10 Si 0.1375(2) 0.7395(3) 0.75426(13) 0.0387(8) Uani 0.373(3) 1 d PU A 2 C81 C 0.0629(5) 0.8602(10) 0.7618(3) 0.056(3) Uani 0.373(3) 1 d PU A 2 H81A H 0.0772 0.9464 0.7506 0.083 Uiso 0.373(3) 1 calc PR A 2 H81B H 0.0550 0.8700 0.7906 0.083 Uiso 0.373(3) 1 calc PR A 2 H81C H 0.0161 0.8292 0.7482 0.083 Uiso 0.373(3) 1 calc PR A 2 C82 C 0.1033(5) 0.5671(11) 0.7722(4) 0.057(3) Uani 0.373(3) 1 d PU A 2 H82A H 0.1032 0.5658 0.8016 0.086 Uiso 0.373(3) 1 calc PR A 2 H82B H 0.1373 0.4977 0.7629 0.086 Uiso 0.373(3) 1 calc PR A 2 H82C H 0.0522 0.5506 0.7612 0.086 Uiso 0.373(3) 1 calc PR A 2 Si11 Si 0.37457(15) 0.7469(4) 0.77995(8) 0.0561(10) Uani 0.373(3) 1 d PU A 2 C14 C 0.385(3) 0.667(5) 0.7303(14) 0.106(13) Uani 0.373(3) 1 d PU A 2 H14A H 0.3716 0.7313 0.7090 0.159 Uiso 0.373(3) 1 calc PR A 2 H14B H 0.3522 0.5894 0.7279 0.159 Uiso 0.373(3) 1 calc PR A 2 H14C H 0.4377 0.6394 0.7277 0.159 Uiso 0.373(3) 1 calc PR A 2 C83 C 0.4358(6) 0.9076(15) 0.7802(5) 0.110(5) Uani 0.373(3) 1 d P A 2 H83A H 0.4892 0.8832 0.7794 0.165 Uiso 0.373(3) 1 calc PR A 2 H83B H 0.4273 0.9588 0.8047 0.165 Uiso 0.373(3) 1 calc PR A 2 H83C H 0.4219 0.9619 0.7566 0.165 Uiso 0.373(3) 1 calc PR A 2 Zn1 Zn 0.252897(19) 0.73992(3) 0.862614(10) 0.04115(12) Uani 1 1 d . A . Cl1 Cl 0.14162(5) 0.70296(11) 0.89355(3) 0.0673(3) Uani 1 1 d . . . Si1 Si 0.25011(5) 0.79446(9) 0.79163(3) 0.0438(2) Uani 1 1 d . . . Si3 Si 0.43596(6) 0.62746(12) 0.82952(3) 0.0639(3) Uani 1 1 d . . . Si4 Si 0.37461(5) 0.66640(9) 0.89112(3) 0.0453(2) Uani 1 1 d . A . Si7 Si 0.45076(6) 0.80970(12) 0.93099(3) 0.0621(3) Uani 1 1 d . . . Si8 Si 0.36344(6) 0.46349(11) 0.92632(4) 0.0700(3) Uani 1 1 d . . . K1 K 0.14290(4) 0.67261(7) 0.59857(2) 0.04916(19) Uani 1 1 d . A . O1 O 0.25698(13) 0.8715(2) 0.59065(7) 0.0599(6) Uani 1 1 d . . . O2 O 0.11004(13) 0.9613(2) 0.60580(8) 0.0617(6) Uani 1 1 d . . . O3 O -0.00596(14) 0.7645(2) 0.61192(8) 0.0590(6) Uani 1 1 d . . . O4 O 0.03555(13) 0.5037(2) 0.63436(7) 0.0592(6) Uani 1 1 d . . . O5 O 0.18637(14) 0.4111(2) 0.62883(7) 0.0611(6) Uani 1 1 d . . . O6 O 0.29523(13) 0.6196(3) 0.62450(7) 0.0612(6) Uani 1 1 d . . . O7 O 0.19728(14) 0.5235(3) 0.52766(8) 0.0736(7) Uani 1 1 d . . . O8 O 0.10116(16) 0.7525(3) 0.51746(8) 0.0688(7) Uani 1 1 d . . . O9 O -0.09001(15) 0.6850(3) 0.48372(8) 0.0745(7) Uani 1 1 d . . . C1 C 0.2378(2) 1.0094(4) 0.59424(13) 0.0708(11) Uani 1 1 d . . . H1A H 0.2721 1.0641 0.5783 0.085 Uiso 1 1 calc R . . H1B H 0.2436 1.0374 0.6227 0.085 Uiso 1 1 calc R . . C2 C 0.1585(2) 1.0302(4) 0.57947(12) 0.0681(10) Uani 1 1 d . . . H2A H 0.1464 1.1265 0.5792 0.082 Uiso 1 1 calc R . . H2B H 0.1514 0.9953 0.5518 0.082 Uiso 1 1 calc R . . C3 C 0.0317(2) 0.9877(4) 0.59645(14) 0.0712(11) Uani 1 1 d . . . H3A H 0.0201 0.9683 0.5677 0.085 Uiso 1 1 calc R . . H3B H 0.0207 1.0830 0.6013 0.085 Uiso 1 1 calc R . . C4 C -0.0160(2) 0.9028(4) 0.62209(14) 0.0710(11) Uani 1 1 d . . . H4A H -0.0015 0.9172 0.6508 0.085 Uiso 1 1 calc R . . H4B H -0.0696 0.9279 0.6178 0.085 Uiso 1 1 calc R . . C5 C -0.0555(2) 0.6786(4) 0.63237(13) 0.0688(11) Uani 1 1 d . . . H5A H -0.1085 0.7017 0.6251 0.083 Uiso 1 1 calc R . . H5B H -0.0475 0.6891 0.6618 0.083 Uiso 1 1 calc R . . C6 C -0.0399(2) 0.5364(4) 0.62048(13) 0.0663(10) Uani 1 1 d . . . H6A H -0.0764 0.4757 0.6328 0.080 Uiso 1 1 calc R . . H6B H -0.0449 0.5267 0.5909 0.080 Uiso 1 1 calc R . . C7 C 0.0541(2) 0.3659(4) 0.62866(12) 0.0664(10) Uani 1 1 d . . . H7A H 0.0564 0.3455 0.5996 0.080 Uiso 1 1 calc R . . H7B H 0.0153 0.3081 0.6403 0.080 Uiso 1 1 calc R . . C8 C 0.1297(2) 0.3416(4) 0.64946(12) 0.0677(10) Uani 1 1 d . . . H8A H 0.1288 0.3729 0.6776 0.081 Uiso 1 1 calc R . . H8B H 0.1409 0.2450 0.6497 0.081 Uiso 1 1 calc R . . C9 C 0.2604(2) 0.4047(4) 0.64883(13) 0.0764(12) Uani 1 1 d . . . H9A H 0.2770 0.3108 0.6512 0.092 Uiso 1 1 calc R . . H9B H 0.2582 0.4423 0.6763 0.092 Uiso 1 1 calc R . . C10 C 0.3147(2) 0.4814(4) 0.62537(13) 0.0730(11) Uani 1 1 d . . . H10A H 0.3660 0.4705 0.6376 0.088 Uiso 1 1 calc R . . H10B H 0.3148 0.4465 0.5976 0.088 Uiso 1 1 calc R . . C11 C 0.3478(2) 0.6990(5) 0.60261(13) 0.0771(12) Uani 1 1 d . . . H11A H 0.3440 0.6757 0.5737 0.092 Uiso 1 1 calc R . . H11B H 0.3999 0.6805 0.6127 0.092 Uiso 1 1 calc R . . C12 C 0.3302(2) 0.8433(5) 0.60798(14) 0.0765(12) Uani 1 1 d . . . H12A H 0.3316 0.8656 0.6370 0.092 Uiso 1 1 calc R . . H12B H 0.3683 0.8983 0.5948 0.092 Uiso 1 1 calc R . . C15 C 0.4749(8) 0.4595(9) 0.8242(2) 0.310(8) Uani 1 1 d . A . H15A H 0.5028 0.4546 0.7994 0.465 Uiso 1 1 calc R . . H15B H 0.4338 0.3944 0.8230 0.465 Uiso 1 1 calc R . . H15C H 0.5090 0.4398 0.8472 0.465 Uiso 1 1 calc R . . C16 C 0.5225(4) 0.7332(13) 0.8235(2) 0.309(9) Uani 1 1 d . A . H16A H 0.5676 0.6778 0.8273 0.463 Uiso 1 1 calc R . . H16B H 0.5235 0.8047 0.8436 0.463 Uiso 1 1 calc R . . H16C H 0.5214 0.7721 0.7965 0.463 Uiso 1 1 calc R . . C19 C 0.1505(3) 0.7103(6) 0.70067(13) 0.0754(13) Uani 1 1 d . . . C23 C 0.4563(3) 0.9804(5) 0.9075(2) 0.122(2) Uani 1 1 d . A . H23A H 0.4056 1.0182 0.9044 0.183 Uiso 1 1 calc R . . H23B H 0.4786 0.9732 0.8811 0.183 Uiso 1 1 calc R . . H23C H 0.4877 1.0385 0.9249 0.183 Uiso 1 1 calc R . . C24 C 0.4134(3) 0.8333(7) 0.98349(16) 0.130(2) Uani 1 1 d . A . H24A H 0.4501 0.8841 1.0001 0.194 Uiso 1 1 calc R . . H24B H 0.4054 0.7461 0.9958 0.194 Uiso 1 1 calc R . . H24C H 0.3656 0.8820 0.9816 0.194 Uiso 1 1 calc R . . C25 C 0.5511(2) 0.7506(5) 0.93973(14) 0.0854(14) Uani 1 1 d . A . H25A H 0.5755 0.7434 0.9139 0.128 Uiso 1 1 calc R . . H25B H 0.5511 0.6632 0.9529 0.128 Uiso 1 1 calc R . . H25C H 0.5788 0.8145 0.9570 0.128 Uiso 1 1 calc R . . C26 C 0.4559(3) 0.3744(5) 0.93632(15) 0.0914(14) Uani 1 1 d . A . H26A H 0.4899 0.4315 0.9526 0.137 Uiso 1 1 calc R . . H26B H 0.4789 0.3542 0.9107 0.137 Uiso 1 1 calc R . . H26C H 0.4469 0.2913 0.9508 0.137 Uiso 1 1 calc R . . C27 C 0.3210(4) 0.4907(6) 0.9766(2) 0.164(3) Uani 1 1 d . A . H27A H 0.2739 0.5409 0.9730 0.246 Uiso 1 1 calc R . . H27B H 0.3563 0.5410 0.9941 0.246 Uiso 1 1 calc R . . H27C H 0.3106 0.4043 0.9890 0.246 Uiso 1 1 calc R . . C28 C 0.2968(4) 0.3462(6) 0.8975(3) 0.170(4) Uani 1 1 d . A . H28A H 0.2882 0.2666 0.9137 0.256 Uiso 1 1 calc R . . H28B H 0.3191 0.3203 0.8722 0.256 Uiso 1 1 calc R . . H28C H 0.2487 0.3915 0.8917 0.256 Uiso 1 1 calc R . . C29 C 0.2169(2) 0.3860(5) 0.52343(14) 0.0866(13) Uani 1 1 d . . . H29A H 0.2223 0.3459 0.5506 0.104 Uiso 1 1 calc R . . H29B H 0.2666 0.3807 0.5111 0.104 Uiso 1 1 calc R . . C30 C 0.1951(2) 0.5977(5) 0.49101(12) 0.0802(13) Uani 1 1 d . . . H30A H 0.1578 0.5578 0.4717 0.096 Uiso 1 1 calc R . . H30B H 0.2451 0.5953 0.4789 0.096 Uiso 1 1 calc R . . C31 C 0.1734(3) 0.7406(5) 0.49981(13) 0.0840(14) Uani 1 1 d . . . H31A H 0.2123 0.7803 0.5183 0.101 Uiso 1 1 calc R . . H31B H 0.1728 0.7922 0.4744 0.101 Uiso 1 1 calc R . . C32 C 0.0408(2) 0.7061(5) 0.49083(13) 0.0807(13) Uani 1 1 d . . . H32A H 0.0420 0.6076 0.4891 0.097 Uiso 1 1 calc R . . H32B H 0.0468 0.7428 0.4635 0.097 Uiso 1 1 calc R . . C33 C -0.0327(2) 0.7509(4) 0.50691(14) 0.0788(12) Uani 1 1 d . . . H33A H -0.0355 0.7266 0.5356 0.095 Uiso 1 1 calc R . . H33B H -0.0381 0.8487 0.5043 0.095 Uiso 1 1 calc R . . C34 C -0.1617(2) 0.6959(5) 0.50133(14) 0.0833(13) Uani 1 1 d . . . H34A H -0.1780 0.7902 0.5017 0.100 Uiso 1 1 calc R . . H34B H -0.1586 0.6627 0.5293 0.100 Uiso 1 1 calc R . . H92 H 0.193(3) 0.684(4) 0.6920(14) 0.089(16) Uiso 1 1 d . . . H91 H 0.140(3) 0.803(5) 0.6934(14) 0.103(18) Uiso 1 1 d . . . H90 H 0.108(3) 0.655(6) 0.6886(16) 0.127(19) Uiso 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 Si2 0.0487(9) 0.0431(10) 0.0399(8) -0.0004(6) 0.0019(6) -0.0013(7) C85 0.068(10) 0.095(7) 0.052(7) -0.002(5) 0.020(6) 0.005(6) C13 0.102(5) 0.041(3) 0.075(4) -0.004(3) -0.024(4) -0.006(3) Si5 0.077(2) 0.096(2) 0.0487(13) -0.0153(15) 0.0087(12) -0.0344(17) C17 0.47(3) 0.097(9) 0.108(9) -0.002(7) -0.009(14) -0.123(13) C18 0.080(7) 0.52(3) 0.108(9) -0.092(14) 0.008(6) -0.092(13) Si6 0.0504(12) 0.0427(8) 0.0585(10) 0.0038(7) 0.0119(8) 0.0014(7) C22 0.147(13) 0.090(9) 0.062(6) 0.045(7) 0.004(6) -0.023(8) C84 0.091(6) 0.054(4) 0.155(8) -0.007(5) 0.042(6) 0.012(4) C21 0.080(5) 0.066(4) 0.104(5) 0.000(4) -0.010(4) -0.023(4) Si9 0.068(3) 0.0510(17) 0.0675(19) 0.0110(14) -0.0028(16) 0.0018(15) C86 0.098(17) 0.105(19) 0.15(3) 0.032(17) -0.031(16) -0.004(13) C20 0.127(14) 0.055(8) 0.204(19) -0.015(10) -0.080(13) 0.020(9) C80 0.151(13) 0.083(9) 0.087(9) 0.044(7) -0.004(8) 0.071(9) Si10 0.0336(14) 0.0344(17) 0.0473(16) 0.0052(14) -0.0088(11) 0.0063(13) C81 0.026(4) 0.064(6) 0.076(7) -0.019(5) -0.001(4) 0.016(4) C82 0.036(5) 0.048(6) 0.088(7) 0.002(5) -0.007(5) -0.009(4) Si11 0.0412(14) 0.082(3) 0.0457(15) 0.0129(14) 0.0074(11) 0.0022(14) C14 0.076(19) 0.18(3) 0.065(17) -0.005(18) 0.016(14) 0.064(19) C83 0.056(7) 0.130(12) 0.144(12) 0.057(10) 0.012(7) -0.040(7) Zn1 0.0372(2) 0.0430(2) 0.0430(2) 0.00119(15) -0.00227(15) 0.00049(15) Cl1 0.0435(5) 0.1022(7) 0.0568(5) 0.0098(5) 0.0083(4) 0.0008(5) Si1 0.0408(5) 0.0474(5) 0.0430(5) 0.0081(4) -0.0029(4) -0.0029(4) Si3 0.0552(6) 0.0814(7) 0.0544(6) -0.0136(5) -0.0070(5) 0.0233(5) Si4 0.0388(5) 0.0493(5) 0.0471(5) -0.0005(4) -0.0084(4) 0.0029(4) Si7 0.0487(6) 0.0736(7) 0.0631(7) -0.0125(5) -0.0076(5) -0.0058(5) Si8 0.0537(6) 0.0560(6) 0.1003(9) 0.0189(6) 0.0031(6) 0.0072(5) K1 0.0444(4) 0.0512(4) 0.0518(4) 0.0004(3) 0.0021(3) 0.0005(3) O1 0.0502(14) 0.0643(16) 0.0648(15) -0.0054(12) -0.0030(11) -0.0088(12) O2 0.0558(15) 0.0516(14) 0.0776(17) -0.0024(12) 0.0012(12) -0.0027(11) O3 0.0544(14) 0.0493(14) 0.0739(17) -0.0093(11) 0.0123(12) -0.0012(11) O4 0.0590(15) 0.0474(13) 0.0712(16) -0.0076(12) 0.0040(12) -0.0082(11) O5 0.0636(16) 0.0656(16) 0.0536(14) 0.0001(12) -0.0054(12) 0.0020(12) O6 0.0466(14) 0.0744(17) 0.0623(15) -0.0082(13) 0.0000(11) 0.0087(12) O7 0.0616(16) 0.097(2) 0.0619(17) -0.0095(15) -0.0052(13) -0.0058(15) O8 0.0689(17) 0.0803(18) 0.0562(15) 0.0003(13) -0.0116(13) -0.0245(14) O9 0.0607(17) 0.092(2) 0.0699(17) -0.0184(15) -0.0086(13) -0.0074(14) C1 0.075(3) 0.061(2) 0.077(3) -0.006(2) 0.012(2) -0.023(2) C2 0.078(3) 0.050(2) 0.076(3) 0.0047(19) 0.001(2) -0.0084(19) C3 0.065(2) 0.043(2) 0.104(3) -0.005(2) -0.006(2) 0.0059(18) C4 0.064(2) 0.053(2) 0.097(3) -0.020(2) 0.008(2) 0.0100(19) C5 0.047(2) 0.069(3) 0.091(3) -0.004(2) 0.017(2) -0.0017(18) C6 0.052(2) 0.064(2) 0.083(3) 0.003(2) -0.0015(19) -0.0155(18) C7 0.084(3) 0.050(2) 0.066(2) -0.0034(18) 0.010(2) -0.0127(19) C8 0.087(3) 0.051(2) 0.066(2) 0.0003(18) -0.001(2) 0.0027(19) C9 0.082(3) 0.064(3) 0.081(3) -0.005(2) -0.025(2) 0.019(2) C10 0.049(2) 0.085(3) 0.084(3) -0.017(2) -0.012(2) 0.018(2) C11 0.044(2) 0.111(4) 0.076(3) -0.003(3) 0.0067(19) 0.006(2) C12 0.050(2) 0.096(3) 0.084(3) 0.000(2) 0.005(2) -0.015(2) C15 0.66(2) 0.175(8) 0.100(5) 0.008(5) 0.092(9) 0.242(12) C16 0.086(4) 0.72(3) 0.128(6) -0.191(11) 0.051(4) -0.156(9) C19 0.074(3) 0.095(4) 0.056(3) -0.019(2) -0.004(2) -0.004(3) C23 0.118(4) 0.066(3) 0.180(6) -0.002(3) -0.038(4) -0.015(3) C24 0.071(3) 0.225(7) 0.093(4) -0.074(4) 0.005(3) -0.017(4) C25 0.051(2) 0.125(4) 0.079(3) 0.004(3) -0.012(2) -0.008(2) C26 0.085(3) 0.084(3) 0.105(4) 0.029(3) 0.005(3) 0.030(3) C27 0.182(6) 0.129(5) 0.190(7) 0.093(5) 0.123(6) 0.077(5) C28 0.140(6) 0.078(4) 0.287(10) 0.039(5) -0.070(6) -0.049(4) C29 0.059(3) 0.116(4) 0.084(3) -0.015(3) -0.003(2) 0.011(3) C30 0.057(2) 0.131(4) 0.054(2) -0.007(3) 0.0069(18) -0.020(3) C31 0.076(3) 0.116(4) 0.059(3) 0.011(2) -0.013(2) -0.051(3) C32 0.071(3) 0.101(3) 0.069(3) -0.011(2) -0.008(2) -0.026(2) C33 0.081(3) 0.083(3) 0.071(3) -0.010(2) -0.013(2) -0.005(2) C34 0.071(3) 0.096(3) 0.083(3) -0.022(3) 0.004(2) 0.008(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 Si2 C13 1.887(6) . ? Si2 C85 1.90(2) . ? Si2 Si3 2.3449(19) . ? Si2 Si1 2.3971(17) . ? Si5 C18 1.772(12) . ? Si5 C17 1.927(13) . ? Si5 C19 1.932(5) . ? Si5 Si1 2.291(3) . ? Si6 C21 1.849(7) . ? Si6 C84 1.877(7) . ? Si6 C22 1.887(18) . ? Si6 Si1 2.3148(18) . ? Si9 C80 1.794(14) . ? Si9 C20 1.864(17) . ? Si9 C86 1.92(3) . ? Si9 Si1 2.370(3) . ? Si10 C81 1.802(8) . ? Si10 C19 1.813(6) . ? Si10 C82 1.916(11) . ? Si10 Si1 2.355(4) . ? Si11 C14 1.83(5) . ? Si11 C83 1.926(12) . ? Si11 Si3 2.259(3) . ? Si11 Si1 2.285(3) . ? Zn1 Cl1 2.2701(11) . ? Zn1 Si1 2.3995(10) . ? Zn1 Si4 2.4166(11) . ? Si3 C15 1.814(7) . ? Si3 C16 1.865(7) . ? Si3 Si4 2.3669(15) . ? Si4 Si7 2.3258(14) . ? Si4 Si8 2.3377(15) . ? Si7 C23 1.868(5) . ? Si7 C25 1.871(4) . ? Si7 C24 1.889(5) . ? Si8 C27 1.864(6) . ? Si8 C26 1.869(4) . ? Si8 C28 1.884(6) . ? K1 O4 2.818(2) . ? K1 O3 2.822(3) . ? K1 O6 2.829(2) . ? K1 O1 2.834(2) . ? K1 O8 2.857(3) . ? K1 O5 2.876(3) . ? K1 O2 2.937(3) . ? K1 O7 2.956(3) . ? K1 C19 3.383(4) . ? O1 C12 1.415(4) . ? O1 C1 1.417(5) . ? O2 C2 1.415(4) . ? O2 C3 1.423(4) . ? O3 C5 1.409(4) . ? O3 C4 1.426(4) . ? O4 C7 1.422(4) . ? O4 C6 1.424(4) . ? O5 C8 1.408(4) . ? O5 C9 1.437(4) . ? O6 C10 1.414(5) . ? O6 C11 1.431(5) . ? O7 C30 1.414(5) . ? O7 C29 1.418(5) . ? O8 C31 1.422(5) . ? O8 C32 1.427(4) . ? O9 C33 1.403(5) . ? O9 C34 1.412(5) . ? C1 C2 1.474(5) . ? C3 C4 1.478(5) . ? C5 C6 1.494(5) . ? C7 C8 1.492(5) . ? C9 C10 1.465(6) . ? C11 C12 1.478(6) . ? C29 C34 1.486(6) 3_566 ? C30 C31 1.502(6) . ? C32 C33 1.483(6) . ? C34 C29 1.486(6) 3_566 ? 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 C13 Si2 C85 105.3(7) . . ? C13 Si2 Si3 102.0(2) . . ? C85 Si2 Si3 113.3(9) . . ? C13 Si2 Si1 109.9(2) . . ? C85 Si2 Si1 117.3(9) . . ? Si3 Si2 Si1 107.75(7) . . ? C18 Si5 C17 102.0(8) . . ? C18 Si5 C19 110.0(5) . . ? C17 Si5 C19 109.4(4) . . ? C18 Si5 Si1 113.9(4) . . ? C17 Si5 Si1 108.6(5) . . ? C19 Si5 Si1 112.4(2) . . ? C21 Si6 C84 108.3(4) . . ? C21 Si6 C22 108.1(8) . . ? C84 Si6 C22 106.7(9) . . ? C21 Si6 Si1 112.8(2) . . ? C84 Si6 Si1 107.3(3) . . ? C22 Si6 Si1 113.3(8) . . ? C80 Si9 C20 105.2(8) . . ? C80 Si9 C86 110.3(13) . . ? C20 Si9 C86 111.4(16) . . ? C80 Si9 Si1 110.9(4) . . ? C20 Si9 Si1 108.6(5) . . ? C86 Si9 Si1 110.3(14) . . ? C81 Si10 C19 111.1(4) . . ? C81 Si10 C82 108.3(5) . . ? C19 Si10 C82 102.1(5) . . ? C81 Si10 Si1 112.1(4) . . ? C19 Si10 Si1 114.3(3) . . ? C82 Si10 Si1 108.2(4) . . ? C14 Si11 C83 106.5(14) . . ? C14 Si11 Si3 110.9(17) . . ? C83 Si11 Si3 100.4(4) . . ? C14 Si11 Si1 111.8(16) . . ? C83 Si11 Si1 111.5(5) . . ? Si3 Si11 Si1 114.88(11) . . ? Cl1 Zn1 Si1 119.24(4) . . ? Cl1 Zn1 Si4 122.82(4) . . ? Si1 Zn1 Si4 115.58(4) . . ? Si11 Si1 Si5 121.51(14) . . ? Si11 Si1 Si6 85.86(10) . . ? Si5 Si1 Si6 120.43(12) . . ? Si11 Si1 Si10 130.92(14) . . ? Si5 Si1 Si10 16.06(8) . . ? Si6 Si1 Si10 105.71(11) . . ? Si11 Si1 Si9 109.94(13) . . ? Si5 Si1 Si9 102.67(14) . . ? Si6 Si1 Si9 24.36(8) . . ? Si10 Si1 Si9 86.73(13) . . ? Si11 Si1 Si2 27.13(9) . . ? Si5 Si1 Si2 97.16(11) . . ? Si6 Si1 Si2 109.77(7) . . ? Si10 Si1 Si2 109.84(11) . . ? Si9 Si1 Si2 132.01(11) . . ? Si11 Si1 Zn1 97.68(8) . . ? Si5 Si1 Zn1 109.76(8) . . ? Si6 Si1 Zn1 117.95(6) . . ? Si10 Si1 Zn1 116.27(11) . . ? Si9 Si1 Zn1 116.07(9) . . ? Si2 Si1 Zn1 96.86(5) . . ? C15 Si3 C16 101.2(6) . . ? C15 Si3 Si11 125.7(3) . . ? C16 Si3 Si11 89.8(4) . . ? C15 Si3 Si2 103.2(4) . . ? C16 Si3 Si2 111.8(3) . . ? Si11 Si3 Si2 27.66(9) . . ? C15 Si3 Si4 114.8(3) . . ? C16 Si3 Si4 113.5(2) . . ? Si11 Si3 Si4 108.26(8) . . ? Si2 Si3 Si4 111.48(6) . . ? Si7 Si4 Si8 107.76(6) . . ? Si7 Si4 Si3 108.24(5) . . ? Si8 Si4 Si3 109.53(6) . . ? Si7 Si4 Zn1 121.09(5) . . ? Si8 Si4 Zn1 111.32(5) . . ? Si3 Si4 Zn1 98.16(5) . . ? C23 Si7 C25 106.5(2) . . ? C23 Si7 C24 107.0(3) . . ? C25 Si7 C24 104.9(2) . . ? C23 Si7 Si4 111.10(18) . . ? C25 Si7 Si4 114.43(16) . . ? C24 Si7 Si4 112.37(18) . . ? C27 Si8 C26 106.7(3) . . ? C27 Si8 C28 106.0(4) . . ? C26 Si8 C28 108.4(3) . . ? C27 Si8 Si4 111.12(19) . . ? C26 Si8 Si4 113.99(16) . . ? C28 Si8 Si4 110.2(2) . . ? O4 K1 O3 59.17(7) . . ? O4 K1 O6 113.84(8) . . ? O3 K1 O6 152.37(8) . . ? O4 K1 O1 160.28(7) . . ? O3 K1 O1 116.90(7) . . ? O6 K1 O1 59.52(8) . . ? O4 K1 O8 113.89(8) . . ? O3 K1 O8 81.34(9) . . ? O6 K1 O8 122.71(8) . . ? O1 K1 O8 82.96(7) . . ? O4 K1 O5 59.35(7) . . ? O3 K1 O5 118.29(7) . . ? O6 K1 O5 59.41(7) . . ? O1 K1 O5 118.83(7) . . ? O8 K1 O5 129.10(8) . . ? O4 K1 O2 114.24(7) . . ? O3 K1 O2 58.99(7) . . ? O6 K1 O2 110.14(7) . . ? O1 K1 O2 57.92(7) . . ? O8 K1 O2 76.13(7) . . ? O5 K1 O2 154.77(7) . . ? O4 K1 O7 105.94(8) . . ? O3 K1 O7 127.97(8) . . ? O6 K1 O7 79.29(7) . . ? O1 K1 O7 91.43(8) . . ? O8 K1 O7 58.60(8) . . ? O5 K1 O7 74.44(8) . . ? O2 K1 O7 128.60(8) . . ? O4 K1 C19 69.57(11) . . ? O3 K1 C19 79.07(12) . . ? O6 K1 C19 73.72(11) . . ? O1 K1 C19 90.78(11) . . ? O8 K1 C19 153.98(12) . . ? O5 K1 C19 75.84(12) . . ? O2 K1 C19 79.14(12) . . ? O7 K1 C19 147.15(12) . . ? C12 O1 C1 111.9(3) . . ? C12 O1 K1 117.4(2) . . ? C1 O1 K1 119.7(2) . . ? C2 O2 C3 112.2(3) . . ? C2 O2 K1 107.3(2) . . ? C3 O2 K1 110.73(19) . . ? C5 O3 C4 112.8(3) . . ? C5 O3 K1 118.1(2) . . ? C4 O3 K1 118.1(2) . . ? C7 O4 C6 113.1(3) . . ? C7 O4 K1 111.0(2) . . ? C6 O4 K1 111.1(2) . . ? C8 O5 C9 113.7(3) . . ? C8 O5 K1 115.3(2) . . ? C9 O5 K1 115.0(2) . . ? C10 O6 C11 112.6(3) . . ? C10 O6 K1 114.3(2) . . ? C11 O6 K1 111.5(2) . . ? C30 O7 C29 114.6(3) . . ? C30 O7 K1 114.5(3) . . ? C29 O7 K1 130.4(3) . . ? C31 O8 C32 112.1(3) . . ? C31 O8 K1 99.1(2) . . ? C32 O8 K1 130.1(2) . . ? C33 O9 C34 112.0(3) . . ? O1 C1 C2 109.4(3) . . ? O2 C2 C1 108.3(3) . . ? O2 C3 C4 109.6(3) . . ? O3 C4 C3 109.7(3) . . ? O3 C5 C6 109.0(3) . . ? O4 C6 C5 108.0(3) . . ? O4 C7 C8 107.4(3) . . ? O5 C8 C7 109.5(3) . . ? O5 C9 C10 109.4(3) . . ? O6 C10 C9 110.7(3) . . ? O6 C11 C12 109.4(3) . . ? O1 C12 C11 109.6(3) . . ? Si10 C19 Si5 19.73(11) . . ? Si10 C19 K1 170.1(3) . . ? Si5 C19 K1 165.0(3) . . ? O7 C29 C34 115.2(4) . 3_566 ? O7 C30 C31 109.1(3) . . ? O8 C31 C30 113.3(3) . . ? O8 C32 C33 108.7(3) . . ? O9 C33 C32 106.4(3) . . ? O9 C34 C29 107.9(3) . 3_566 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C14 Si11 Si1 Si5 23.0(16) . . . . ? C83 Si11 Si1 Si5 142.2(5) . . . . ? Si3 Si11 Si1 Si5 -104.45(16) . . . . ? C14 Si11 Si1 Si6 -100.4(16) . . . . ? C83 Si11 Si1 Si6 18.7(5) . . . . ? Si3 Si11 Si1 Si6 132.10(16) . . . . ? C14 Si11 Si1 Si10 6.8(16) . . . . ? C83 Si11 Si1 Si10 126.0(5) . . . . ? Si3 Si11 Si1 Si10 -120.64(16) . . . . ? C14 Si11 Si1 Si9 -96.7(16) . . . . ? C83 Si11 Si1 Si9 22.4(5) . . . . ? Si3 Si11 Si1 Si9 135.81(16) . . . . ? C14 Si11 Si1 Si2 51.9(16) . . . . ? C83 Si11 Si1 Si2 171.0(5) . . . . ? Si3 Si11 Si1 Si2 -75.62(19) . . . . ? C14 Si11 Si1 Zn1 141.9(16) . . . . ? C83 Si11 Si1 Zn1 -99.0(5) . . . . ? Si3 Si11 Si1 Zn1 14.43(17) . . . . ? C18 Si5 Si1 Si11 170.6(7) . . . . ? C17 Si5 Si1 Si11 57.8(5) . . . . ? C19 Si5 Si1 Si11 -63.4(3) . . . . ? C18 Si5 Si1 Si6 -84.2(7) . . . . ? C17 Si5 Si1 Si6 163.0(5) . . . . ? C19 Si5 Si1 Si6 41.8(3) . . . . ? C18 Si5 Si1 Si10 -59.0(9) . . . . ? C17 Si5 Si1 Si10 -171.9(8) . . . . ? C19 Si5 Si1 Si10 66.9(6) . . . . ? C18 Si5 Si1 Si9 -66.2(7) . . . . ? C17 Si5 Si1 Si9 -179.0(5) . . . . ? C19 Si5 Si1 Si9 59.8(3) . . . . ? C18 Si5 Si1 Si2 157.8(7) . . . . ? C17 Si5 Si1 Si2 45.0(5) . . . . ? C19 Si5 Si1 Si2 -76.2(3) . . . . ? C18 Si5 Si1 Zn1 57.9(7) . . . . ? C17 Si5 Si1 Zn1 -55.0(5) . . . . ? C19 Si5 Si1 Zn1 -176.2(2) . . . . ? C21 Si6 Si1 Si11 -36.2(3) . . . . ? C84 Si6 Si1 Si11 -155.4(4) . . . . ? C22 Si6 Si1 Si11 87.1(9) . . . . ? C21 Si6 Si1 Si5 -160.6(3) . . . . ? C84 Si6 Si1 Si5 80.2(4) . . . . ? C22 Si6 Si1 Si5 -37.3(9) . . . . ? C21 Si6 Si1 Si10 -167.6(3) . . . . ? C84 Si6 Si1 Si10 73.2(4) . . . . ? C22 Si6 Si1 Si10 -44.3(9) . . . . ? C21 Si6 Si1 Si9 152.3(4) . . . . ? C84 Si6 Si1 Si9 33.1(4) . . . . ? C22 Si6 Si1 Si9 -84.4(9) . . . . ? C21 Si6 Si1 Si2 -49.2(3) . . . . ? C84 Si6 Si1 Si2 -168.4(4) . . . . ? C22 Si6 Si1 Si2 74.1(9) . . . . ? C21 Si6 Si1 Zn1 60.3(3) . . . . ? C84 Si6 Si1 Zn1 -58.9(4) . . . . ? C22 Si6 Si1 Zn1 -176.4(9) . . . . ? C81 Si10 Si1 Si11 -152.6(4) . . . . ? C19 Si10 Si1 Si11 -25.0(3) . . . . ? C82 Si10 Si1 Si11 88.1(5) . . . . ? C81 Si10 Si1 Si5 148.1(8) . . . . ? C19 Si10 Si1 Si5 -84.3(6) . . . . ? C82 Si10 Si1 Si5 28.8(6) . . . . ? C81 Si10 Si1 Si6 -54.3(4) . . . . ? C19 Si10 Si1 Si6 73.3(3) . . . . ? C82 Si10 Si1 Si6 -173.6(4) . . . . ? C81 Si10 Si1 Si9 -38.9(4) . . . . ? C19 Si10 Si1 Si9 88.7(3) . . . . ? C82 Si10 Si1 Si9 -158.2(4) . . . . ? C81 Si10 Si1 Si2 -172.6(4) . . . . ? C19 Si10 Si1 Si2 -45.1(3) . . . . ? C82 Si10 Si1 Si2 68.0(4) . . . . ? C81 Si10 Si1 Zn1 78.7(4) . . . . ? C19 Si10 Si1 Zn1 -153.7(2) . . . . ? C82 Si10 Si1 Zn1 -40.6(4) . . . . ? C80 Si9 Si1 Si11 163.6(5) . . . . ? C20 Si9 Si1 Si11 -81.2(7) . . . . ? C86 Si9 Si1 Si11 41.1(14) . . . . ? C80 Si9 Si1 Si5 33.0(5) . . . . ? C20 Si9 Si1 Si5 148.1(7) . . . . ? C86 Si9 Si1 Si5 -89.6(14) . . . . ? C80 Si9 Si1 Si6 172.6(6) . . . . ? C20 Si9 Si1 Si6 -72.2(7) . . . . ? C86 Si9 Si1 Si6 50.1(14) . . . . ? C80 Si9 Si1 Si10 31.0(5) . . . . ? C20 Si9 Si1 Si10 146.2(7) . . . . ? C86 Si9 Si1 Si10 -91.5(14) . . . . ? C80 Si9 Si1 Si2 145.0(5) . . . . ? C20 Si9 Si1 Si2 -99.9(7) . . . . ? C86 Si9 Si1 Si2 22.4(14) . . . . ? C80 Si9 Si1 Zn1 -86.7(5) . . . . ? C20 Si9 Si1 Zn1 28.4(7) . . . . ? C86 Si9 Si1 Zn1 150.7(14) . . . . ? C13 Si2 Si1 Si11 173.2(3) . . . . ? C85 Si2 Si1 Si11 -66.6(8) . . . . ? Si3 Si2 Si1 Si11 62.75(16) . . . . ? C13 Si2 Si1 Si5 -31.3(2) . . . . ? C85 Si2 Si1 Si5 89.0(8) . . . . ? Si3 Si2 Si1 Si5 -141.72(10) . . . . ? C13 Si2 Si1 Si6 -157.3(2) . . . . ? C85 Si2 Si1 Si6 -37.0(8) . . . . ? Si3 Si2 Si1 Si6 92.30(9) . . . . ? C13 Si2 Si1 Si10 -41.5(2) . . . . ? C85 Si2 Si1 Si10 78.8(8) . . . . ? Si3 Si2 Si1 Si10 -151.88(12) . . . . ? C13 Si2 Si1 Si9 -145.5(2) . . . . ? C85 Si2 Si1 Si9 -25.3(8) . . . . ? Si3 Si2 Si1 Si9 104.03(13) . . . . ? C13 Si2 Si1 Zn1 79.7(2) . . . . ? C85 Si2 Si1 Zn1 -160.0(8) . . . . ? Si3 Si2 Si1 Zn1 -30.72(8) . . . . ? Cl1 Zn1 Si1 Si11 -162.32(10) . . . . ? Si4 Zn1 Si1 Si11 0.73(11) . . . . ? Cl1 Zn1 Si1 Si5 -34.81(11) . . . . ? Si4 Zn1 Si1 Si5 128.24(11) . . . . ? Cl1 Zn1 Si1 Si6 108.30(8) . . . . ? Si4 Zn1 Si1 Si6 -88.64(7) . . . . ? Cl1 Zn1 Si1 Si10 -18.84(11) . . . . ? Si4 Zn1 Si1 Si10 144.21(10) . . . . ? Cl1 Zn1 Si1 Si9 80.99(12) . . . . ? Si4 Zn1 Si1 Si9 -115.96(12) . . . . ? Cl1 Zn1 Si1 Si2 -134.98(6) . . . . ? Si4 Zn1 Si1 Si2 28.07(6) . . . . ? C14 Si11 Si3 C15 -11.5(16) . . . . ? C83 Si11 Si3 C15 -123.8(7) . . . . ? Si1 Si11 Si3 C15 116.5(6) . . . . ? C14 Si11 Si3 C16 92.3(15) . . . . ? C83 Si11 Si3 C16 -20.0(5) . . . . ? Si1 Si11 Si3 C16 -139.8(3) . . . . ? C14 Si11 Si3 Si2 -51.3(15) . . . . ? C83 Si11 Si3 Si2 -163.6(5) . . . . ? Si1 Si11 Si3 Si2 76.61(18) . . . . ? C14 Si11 Si3 Si4 -152.9(15) . . . . ? C83 Si11 Si3 Si4 94.8(5) . . . . ? Si1 Si11 Si3 Si4 -25.00(19) . . . . ? C13 Si2 Si3 C15 34.5(5) . . . . ? C85 Si2 Si3 C15 -78.2(9) . . . . ? Si1 Si2 Si3 C15 150.2(4) . . . . ? C13 Si2 Si3 C16 142.5(4) . . . . ? C85 Si2 Si3 C16 29.8(9) . . . . ? Si1 Si2 Si3 C16 -101.8(3) . . . . ? C13 Si2 Si3 Si11 -177.8(3) . . . . ? C85 Si2 Si3 Si11 69.5(8) . . . . ? Si1 Si2 Si3 Si11 -62.06(16) . . . . ? C13 Si2 Si3 Si4 -89.2(2) . . . . ? C85 Si2 Si3 Si4 158.0(8) . . . . ? Si1 Si2 Si3 Si4 26.47(9) . . . . ? C15 Si3 Si4 Si7 108.6(5) . . . . ? C16 Si3 Si4 Si7 -7.2(4) . . . . ? Si11 Si3 Si4 Si7 -105.26(11) . . . . ? Si2 Si3 Si4 Si7 -134.51(7) . . . . ? C15 Si3 Si4 Si8 -8.6(5) . . . . ? C16 Si3 Si4 Si8 -124.5(4) . . . . ? Si11 Si3 Si4 Si8 137.50(11) . . . . ? Si2 Si3 Si4 Si8 108.25(7) . . . . ? C15 Si3 Si4 Zn1 -124.8(5) . . . . ? C16 Si3 Si4 Zn1 119.4(4) . . . . ? Si11 Si3 Si4 Zn1 21.36(11) . . . . ? Si2 Si3 Si4 Zn1 -7.89(7) . . . . ? Cl1 Zn1 Si4 Si7 -94.21(7) . . . . ? Si1 Zn1 Si4 Si7 103.41(6) . . . . ? Cl1 Zn1 Si4 Si8 33.94(7) . . . . ? Si1 Zn1 Si4 Si8 -128.44(5) . . . . ? Cl1 Zn1 Si4 Si3 148.68(5) . . . . ? Si1 Zn1 Si4 Si3 -13.70(5) . . . . ? Si8 Si4 Si7 C23 -175.1(2) . . . . ? Si3 Si4 Si7 C23 66.6(2) . . . . ? Zn1 Si4 Si7 C23 -45.3(2) . . . . ? Si8 Si4 Si7 C25 64.26(18) . . . . ? Si3 Si4 Si7 C25 -54.12(18) . . . . ? Zn1 Si4 Si7 C25 -166.03(17) . . . . ? Si8 Si4 Si7 C24 -55.2(3) . . . . ? Si3 Si4 Si7 C24 -173.6(2) . . . . ? Zn1 Si4 Si7 C24 74.5(3) . . . . ? Si7 Si4 Si8 C27 58.9(3) . . . . ? Si3 Si4 Si8 C27 176.4(3) . . . . ? Zn1 Si4 Si8 C27 -76.1(3) . . . . ? Si7 Si4 Si8 C26 -61.8(2) . . . . ? Si3 Si4 Si8 C26 55.8(2) . . . . ? Zn1 Si4 Si8 C26 163.25(19) . . . . ? Si7 Si4 Si8 C28 176.1(3) . . . . ? Si3 Si4 Si8 C28 -66.4(3) . . . . ? Zn1 Si4 Si8 C28 41.1(3) . . . . ? O4 K1 O1 C12 69.1(3) . . . . ? O3 K1 O1 C12 142.4(2) . . . . ? O6 K1 O1 C12 -6.3(2) . . . . ? O8 K1 O1 C12 -141.1(3) . . . . ? O5 K1 O1 C12 -10.0(3) . . . . ? O2 K1 O1 C12 140.9(3) . . . . ? O7 K1 O1 C12 -83.0(3) . . . . ? C19 K1 O1 C12 64.2(3) . . . . ? O4 K1 O1 C1 -72.1(4) . . . . ? O3 K1 O1 C1 1.2(3) . . . . ? O6 K1 O1 C1 -147.5(3) . . . . ? O8 K1 O1 C1 77.7(3) . . . . ? O5 K1 O1 C1 -151.2(2) . . . . ? O2 K1 O1 C1 -0.3(2) . . . . ? O7 K1 O1 C1 135.9(3) . . . . ? C19 K1 O1 C1 -76.9(3) . . . . ? O4 K1 O2 C2 -167.8(2) . . . . ? O3 K1 O2 C2 -145.7(2) . . . . ? O6 K1 O2 C2 62.6(2) . . . . ? O1 K1 O2 C2 32.8(2) . . . . ? O8 K1 O2 C2 -57.5(2) . . . . ? O5 K1 O2 C2 123.1(2) . . . . ? O7 K1 O2 C2 -29.7(2) . . . . ? C19 K1 O2 C2 130.6(2) . . . . ? O4 K1 O2 C3 -45.0(3) . . . . ? O3 K1 O2 C3 -22.9(2) . . . . ? O6 K1 O2 C3 -174.6(2) . . . . ? O1 K1 O2 C3 155.6(3) . . . . ? O8 K1 O2 C3 65.2(2) . . . . ? O5 K1 O2 C3 -114.2(3) . . . . ? O7 K1 O2 C3 93.1(2) . . . . ? C19 K1 O2 C3 -106.6(3) . . . . ? O4 K1 O3 C5 4.1(2) . . . . ? O6 K1 O3 C5 -78.7(3) . . . . ? O1 K1 O3 C5 -153.7(2) . . . . ? O8 K1 O3 C5 128.7(3) . . . . ? O5 K1 O3 C5 -1.2(3) . . . . ? O2 K1 O3 C5 -152.3(3) . . . . ? O7 K1 O3 C5 90.7(3) . . . . ? C19 K1 O3 C5 -68.5(3) . . . . ? O4 K1 O3 C4 145.8(3) . . . . ? O6 K1 O3 C4 63.0(3) . . . . ? O1 K1 O3 C4 -12.1(3) . . . . ? O8 K1 O3 C4 -89.6(3) . . . . ? O5 K1 O3 C4 140.4(3) . . . . ? O2 K1 O3 C4 -10.6(3) . . . . ? O7 K1 O3 C4 -127.6(3) . . . . ? C19 K1 O3 C4 73.2(3) . . . . ? O3 K1 O4 C7 156.3(2) . . . . ? O6 K1 O4 C7 -53.9(2) . . . . ? O1 K1 O4 C7 -119.7(3) . . . . ? O8 K1 O4 C7 93.4(2) . . . . ? O5 K1 O4 C7 -29.2(2) . . . . ? O2 K1 O4 C7 178.4(2) . . . . ? O7 K1 O4 C7 31.2(2) . . . . ? C19 K1 O4 C7 -114.5(3) . . . . ? O3 K1 O4 C6 29.5(2) . . . . ? O6 K1 O4 C6 179.3(2) . . . . ? O1 K1 O4 C6 113.6(3) . . . . ? O8 K1 O4 C6 -33.4(2) . . . . ? O5 K1 O4 C6 -156.0(2) . . . . ? O2 K1 O4 C6 51.6(2) . . . . ? O7 K1 O4 C6 -95.6(2) . . . . ? C19 K1 O4 C6 118.8(2) . . . . ? O4 K1 O5 C8 -5.8(2) . . . . ? O3 K1 O5 C8 -0.4(2) . . . . ? O6 K1 O5 C8 147.8(2) . . . . ? O1 K1 O5 C8 151.5(2) . . . . ? O8 K1 O5 C8 -103.0(2) . . . . ? O2 K1 O5 C8 76.3(3) . . . . ? O7 K1 O5 C8 -125.6(2) . . . . ? C19 K1 O5 C8 68.6(2) . . . . ? O4 K1 O5 C9 -141.1(3) . . . . ? O3 K1 O5 C9 -135.7(2) . . . . ? O6 K1 O5 C9 12.6(2) . . . . ? O1 K1 O5 C9 16.3(3) . . . . ? O8 K1 O5 C9 121.8(2) . . . . ? O2 K1 O5 C9 -59.0(3) . . . . ? O7 K1 O5 C9 99.2(2) . . . . ? C19 K1 O5 C9 -66.7(3) . . . . ? O4 K1 O6 C10 45.2(3) . . . . ? O3 K1 O6 C10 113.8(3) . . . . ? O1 K1 O6 C10 -155.8(3) . . . . ? O8 K1 O6 C10 -98.9(3) . . . . ? O5 K1 O6 C10 20.5(2) . . . . ? O2 K1 O6 C10 175.0(2) . . . . ? O7 K1 O6 C10 -57.7(2) . . . . ? C19 K1 O6 C10 103.4(3) . . . . ? O4 K1 O6 C11 174.4(2) . . . . ? O3 K1 O6 C11 -116.9(3) . . . . ? O1 K1 O6 C11 -26.5(2) . . . . ? O8 K1 O6 C11 30.3(3) . . . . ? O5 K1 O6 C11 149.7(3) . . . . ? O2 K1 O6 C11 -55.8(2) . . . . ? O7 K1 O6 C11 71.6(2) . . . . ? C19 K1 O6 C11 -127.4(3) . . . . ? O4 K1 O7 C30 129.6(2) . . . . ? O3 K1 O7 C30 66.5(2) . . . . ? O6 K1 O7 C30 -118.5(2) . . . . ? O1 K1 O7 C30 -59.9(2) . . . . ? O8 K1 O7 C30 21.0(2) . . . . ? O5 K1 O7 C30 -179.5(2) . . . . ? O2 K1 O7 C30 -11.2(3) . . . . ? C19 K1 O7 C30 -153.5(3) . . . . ? O4 K1 O7 C29 -42.3(3) . . . . ? O3 K1 O7 C29 -105.4(3) . . . . ? O6 K1 O7 C29 69.6(3) . . . . ? O1 K1 O7 C29 128.2(3) . . . . ? O8 K1 O7 C29 -150.9(3) . . . . ? O5 K1 O7 C29 8.6(3) . . . . ? O2 K1 O7 C29 176.9(3) . . . . ? C19 K1 O7 C29 34.6(4) . . . . ? O4 K1 O8 C31 -139.0(2) . . . . ? O3 K1 O8 C31 170.4(2) . . . . ? O6 K1 O8 C31 5.1(3) . . . . ? O1 K1 O8 C31 51.7(2) . . . . ? O5 K1 O8 C31 -70.0(2) . . . . ? O2 K1 O8 C31 110.4(2) . . . . ? O7 K1 O8 C31 -44.3(2) . . . . ? C19 K1 O8 C31 128.9(3) . . . . ? O4 K1 O8 C32 -9.7(4) . . . . ? O3 K1 O8 C32 -60.3(3) . . . . ? O6 K1 O8 C32 134.4(3) . . . . ? O1 K1 O8 C32 -179.0(3) . . . . ? O5 K1 O8 C32 59.3(4) . . . . ? O2 K1 O8 C32 -120.4(3) . . . . ? O7 K1 O8 C32 85.0(3) . . . . ? C19 K1 O8 C32 -101.8(4) . . . . ? C12 O1 C1 C2 -174.4(3) . . . . ? K1 O1 C1 C2 -31.2(4) . . . . ? C3 O2 C2 C1 173.6(3) . . . . ? K1 O2 C2 C1 -64.5(3) . . . . ? O1 C1 C2 O2 65.6(4) . . . . ? C2 O2 C3 C4 174.3(3) . . . . ? K1 O2 C3 C4 54.4(3) . . . . ? C5 O3 C4 C3 -174.1(3) . . . . ? K1 O3 C4 C3 42.3(4) . . . . ? O2 C3 C4 O3 -65.5(4) . . . . ? C4 O3 C5 C6 -178.9(3) . . . . ? K1 O3 C5 C6 -35.3(4) . . . . ? C7 O4 C6 C5 173.6(3) . . . . ? K1 O4 C6 C5 -60.8(3) . . . . ? O3 C5 C6 O4 64.1(4) . . . . ? C6 O4 C7 C8 -172.3(3) . . . . ? K1 O4 C7 C8 62.0(3) . . . . ? C9 O5 C8 C7 174.3(3) . . . . ? K1 O5 C8 C7 38.4(3) . . . . ? O4 C7 C8 O5 -67.9(4) . . . . ? C8 O5 C9 C10 -179.2(3) . . . . ? K1 O5 C9 C10 -43.2(4) . . . . ? C11 O6 C10 C9 178.7(3) . . . . ? K1 O6 C10 C9 -52.6(4) . . . . ? O5 C9 C10 O6 64.3(4) . . . . ? C10 O6 C11 C12 -172.0(3) . . . . ? K1 O6 C11 C12 57.9(4) . . . . ? C1 O1 C12 C11 -178.8(3) . . . . ? K1 O1 C12 C11 37.2(4) . . . . ? O6 C11 C12 O1 -63.8(4) . . . . ? C81 Si10 C19 Si5 -156.6(9) . . . . ? C82 Si10 C19 Si5 -41.4(6) . . . . ? Si1 Si10 C19 Si5 75.3(6) . . . . ? C81 Si10 C19 K1 -25(2) . . . . ? C82 Si10 C19 K1 90.1(18) . . . . ? Si1 Si10 C19 K1 -153.3(17) . . . . ? C18 Si5 C19 Si10 49.6(9) . . . . ? C17 Si5 C19 Si10 160.9(9) . . . . ? Si1 Si5 C19 Si10 -78.4(6) . . . . ? C18 Si5 C19 K1 -100.6(13) . . . . ? C17 Si5 C19 K1 10.7(13) . . . . ? Si1 Si5 C19 K1 131.4(10) . . . . ? O4 K1 C19 Si10 -60.3(18) . . . . ? O3 K1 C19 Si10 0.6(18) . . . . ? O6 K1 C19 Si10 175.7(18) . . . . ? O1 K1 C19 Si10 117.9(18) . . . . ? O8 K1 C19 Si10 42(2) . . . . ? O5 K1 C19 Si10 -122.5(18) . . . . ? O2 K1 C19 Si10 60.8(18) . . . . ? O7 K1 C19 Si10 -148.3(17) . . . . ? O4 K1 C19 Si5 42.6(11) . . . . ? O3 K1 C19 Si5 103.6(11) . . . . ? O6 K1 C19 Si5 -81.3(11) . . . . ? O1 K1 C19 Si5 -139.1(11) . . . . ? O8 K1 C19 Si5 145.4(10) . . . . ? O5 K1 C19 Si5 -19.5(11) . . . . ? O2 K1 C19 Si5 163.8(11) . . . . ? O7 K1 C19 Si5 -45.3(12) . . . . ? C30 O7 C29 C34 -64.3(5) . . . 3_566 ? K1 O7 C29 C34 107.6(4) . . . 3_566 ? C29 O7 C30 C31 179.8(3) . . . . ? K1 O7 C30 C31 6.6(4) . . . . ? C32 O8 C31 C30 -63.1(5) . . . . ? K1 O8 C31 C30 77.1(3) . . . . ? O7 C30 C31 O8 -59.6(4) . . . . ? C31 O8 C32 C33 -166.7(4) . . . . ? K1 O8 C32 C33 68.9(5) . . . . ? C34 O9 C33 C32 167.2(4) . . . . ? O8 C32 C33 O9 -170.6(3) . . . . ? C33 O9 C34 C29 -175.4(4) . . . 3_566 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.906 _refine_diff_density_min -0.763 _refine_diff_density_rms 0.070 # Attachment '8a_317j_ohne.cif' data_317j _database_code_depnum_ccdc_archive 'CCDC 645721' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H123 Cl K O12 Si14 Zn2' _chemical_formula_weight 1527.04 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' 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' O O 0.0106 0.0060 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.652(3) _cell_length_b 16.971(3) _cell_length_c 21.022(4) _cell_angle_alpha 98.67(3) _cell_angle_beta 105.65(3) _cell_angle_gamma 100.28(3) _cell_volume 4181.3(14) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blocks _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.213 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1634 _exptl_absorpt_coefficient_mu 0.901 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7738 _exptl_absorpt_correction_T_max 0.8474 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33510 _diffrn_reflns_av_R_equivalents 0.1056 _diffrn_reflns_av_sigmaI/netI 0.2277 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 26.33 _reflns_number_total 16748 _reflns_number_gt 7856 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16748 _refine_ls_number_parameters 747 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1713 _refine_ls_R_factor_gt 0.0712 _refine_ls_wR_factor_ref 0.1679 _refine_ls_wR_factor_gt 0.1373 _refine_ls_goodness_of_fit_ref 0.931 _refine_ls_restrained_S_all 0.932 _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 Zn1 Zn 0.65957(6) 0.27377(4) 0.79398(4) 0.0283(2) Uani 1 1 d . . . Zn2 Zn 0.58259(6) 0.19027(4) 0.64269(4) 0.02736(19) Uani 1 1 d . . . Cl1 Cl 0.51085(14) 0.15050(10) 0.73418(8) 0.0423(4) Uani 1 1 d . . . K1 K 0.13896(11) 0.80290(8) 0.78432(7) 0.0306(3) Uani 1 1 d . . . O1 O -0.0364(4) 0.8021(3) 0.6586(2) 0.0392(11) Uani 1 1 d . . . O2 O -0.0919(3) 0.7081(3) 0.7494(2) 0.0392(11) Uani 1 1 d . . . O3 O 0.0289(3) 0.7800(3) 0.8885(2) 0.0346(11) Uani 1 1 d . . . O4 O 0.1215(3) 0.9393(2) 0.8846(2) 0.0331(11) Uani 1 1 d . . . O5 O 0.2924(3) 0.9581(3) 0.8259(2) 0.0372(11) Uani 1 1 d . . . O6 O 0.1773(3) 0.9017(3) 0.6862(2) 0.0363(11) Uani 1 1 d . . . O7 O 0.1774(4) 0.6850(3) 0.6838(2) 0.0442(12) Uani 1 1 d . . . O8 O 0.1477(4) 0.6426(3) 0.8026(3) 0.0526(14) Uani 1 1 d . . . O9 O 0.3192(4) 0.7743(3) 0.8947(2) 0.0507(14) Uani 1 1 d . . . O10 O 0.5507(4) 0.8645(3) 0.9744(2) 0.0586(15) Uani 1 1 d . . . O11 O 0.6555(4) 0.7858(3) 0.8676(2) 0.0487(13) Uani 1 1 d . . . O12 O 0.4087(4) 0.7643(3) 0.7308(2) 0.0454(12) Uani 1 1 d . . . Si1 Si 0.49562(14) 0.30350(10) 0.62466(8) 0.0272(4) Uani 1 1 d . . . Si2 Si 0.32544(15) 0.27749(11) 0.65191(9) 0.0322(5) Uani 1 1 d . . . Si3 Si 0.37310(15) 0.32585(11) 0.76983(9) 0.0334(5) Uani 1 1 d . . . Si4 Si 0.56639(15) 0.38298(11) 0.80311(9) 0.0294(4) Uani 1 1 d . . . Si5 Si 0.59071(15) 0.42425(11) 0.70571(9) 0.0293(4) Uani 1 1 d . . . Si6 Si 0.47170(15) 0.32891(11) 0.51645(9) 0.0310(4) Uani 1 1 d . . . Si7 Si 0.63294(17) 0.48640(11) 0.89964(9) 0.0369(5) Uani 1 1 d . . . Si8 Si 0.71658(14) 0.10926(10) 0.63523(8) 0.0250(4) Uani 1 1 d . . . Si9 Si 0.70756(15) 0.01403(10) 0.70456(8) 0.0281(4) Uani 1 1 d . . . Si10 Si 0.78048(15) 0.09276(11) 0.81640(9) 0.0321(5) Uani 1 1 d . . . Si11 Si 0.83068(14) 0.22856(11) 0.80512(9) 0.0296(4) Uani 1 1 d . . . Si12 Si 0.88046(14) 0.20244(11) 0.70575(9) 0.0332(5) Uani 1 1 d . . . Si13 Si 0.74067(14) 0.06361(11) 0.53036(9) 0.0292(4) Uani 1 1 d . . . Si14 Si 0.97515(15) 0.31241(12) 0.89635(9) 0.0357(5) Uani 1 1 d . . . C1 C 0.2455(5) 0.1680(4) 0.6222(3) 0.0461(19) Uani 1 1 d . . . H1A H 0.2297 0.1518 0.5732 0.069 Uiso 1 1 calc R . . H1B H 0.1742 0.1618 0.6331 0.069 Uiso 1 1 calc R . . H1C H 0.2906 0.1331 0.6447 0.069 Uiso 1 1 calc R . . C2 C 0.2228(5) 0.3368(5) 0.6106(3) 0.052(2) Uani 1 1 d . . . H2A H 0.1606 0.3332 0.6304 0.078 Uiso 1 1 calc R . . H2B H 0.1928 0.3136 0.5620 0.078 Uiso 1 1 calc R . . H2C H 0.2617 0.3943 0.6181 0.078 Uiso 1 1 calc R . . C3 C 0.3412(5) 0.2446(4) 0.8193(3) 0.0449(19) Uani 1 1 d . . . H3A H 0.2631 0.2132 0.7985 0.067 Uiso 1 1 calc R . . H3B H 0.3515 0.2710 0.8660 0.067 Uiso 1 1 calc R . . H3C H 0.3926 0.2077 0.8189 0.067 Uiso 1 1 calc R . . C4 C 0.2869(6) 0.4031(4) 0.7856(3) 0.050(2) Uani 1 1 d . . . H4A H 0.3000 0.4199 0.8343 0.075 Uiso 1 1 calc R . . H4B H 0.2066 0.3782 0.7632 0.075 Uiso 1 1 calc R . . H4C H 0.3095 0.4511 0.7674 0.075 Uiso 1 1 calc R . . C5 C 0.7454(5) 0.4561(4) 0.7124(3) 0.0401(17) Uani 1 1 d . . . H5A H 0.7832 0.5017 0.7511 0.060 Uiso 1 1 calc R . . H5B H 0.7524 0.4733 0.6709 0.060 Uiso 1 1 calc R . . H5C H 0.7807 0.4097 0.7185 0.060 Uiso 1 1 calc R . . C6 C 0.5287(5) 0.5151(4) 0.6874(3) 0.0390(17) Uani 1 1 d . . . H6A H 0.5433 0.5303 0.6468 0.059 Uiso 1 1 calc R . . H6B H 0.5637 0.5615 0.7258 0.059 Uiso 1 1 calc R . . H6C H 0.4472 0.5005 0.6800 0.059 Uiso 1 1 calc R . . C7 C 0.6145(5) 0.3689(4) 0.5074(3) 0.0379(17) Uani 1 1 d . . . H7A H 0.6537 0.4186 0.5421 0.057 Uiso 1 1 calc R . . H7B H 0.6052 0.3817 0.4626 0.057 Uiso 1 1 calc R . . H7C H 0.6589 0.3272 0.5127 0.057 Uiso 1 1 calc R . . C8 C 0.4030(6) 0.2312(4) 0.4509(3) 0.0437(18) Uani 1 1 d . . . H8A H 0.4532 0.1932 0.4558 0.066 Uiso 1 1 calc R . . H8B H 0.3887 0.2435 0.4057 0.066 Uiso 1 1 calc R . . H8C H 0.3315 0.2061 0.4571 0.066 Uiso 1 1 calc R . . C9 C 0.3847(5) 0.4066(4) 0.4960(3) 0.0372(17) Uani 1 1 d . . . H9A H 0.3811 0.4157 0.4506 0.056 Uiso 1 1 calc R . . H9B H 0.4196 0.4583 0.5290 0.056 Uiso 1 1 calc R . . H9C H 0.3082 0.3861 0.4977 0.056 Uiso 1 1 calc R . . C10 C 0.5611(7) 0.5743(4) 0.8940(4) 0.062(2) Uani 1 1 d . . . H10A H 0.5766 0.6012 0.8583 0.094 Uiso 1 1 calc R . . H10B H 0.5898 0.6138 0.9373 0.094 Uiso 1 1 calc R . . H10C H 0.4796 0.5536 0.8834 0.094 Uiso 1 1 calc R . . C11 C 0.7872(6) 0.5279(4) 0.9173(4) 0.057(2) Uani 1 1 d . . . H11A H 0.8143 0.5738 0.9564 0.085 Uiso 1 1 calc R . . H11B H 0.8007 0.5469 0.8778 0.085 Uiso 1 1 calc R . . H11C H 0.8276 0.4847 0.9269 0.085 Uiso 1 1 calc R . . C12 C 0.6147(6) 0.4454(4) 0.9752(3) 0.051(2) Uani 1 1 d . . . H12A H 0.6421 0.4901 1.0152 0.076 Uiso 1 1 calc R . . H12B H 0.6577 0.4032 0.9824 0.076 Uiso 1 1 calc R . . H12C H 0.5346 0.4216 0.9673 0.076 Uiso 1 1 calc R . . C13 C 0.5610(5) -0.0504(4) 0.6856(3) 0.0382(17) Uani 1 1 d . . . H13A H 0.5615 -0.0882 0.7165 0.057 Uiso 1 1 calc R . . H13B H 0.5353 -0.0816 0.6389 0.057 Uiso 1 1 calc R . . H13C H 0.5098 -0.0148 0.6915 0.057 Uiso 1 1 calc R . . C14 C 0.8011(6) -0.0601(4) 0.6965(3) 0.0464(19) Uani 1 1 d . . . H14A H 0.7777 -0.0910 0.6498 0.070 Uiso 1 1 calc R . . H14B H 0.7944 -0.0981 0.7267 0.070 Uiso 1 1 calc R . . H14C H 0.8797 -0.0295 0.7089 0.070 Uiso 1 1 calc R . . C15 C 0.6802(6) 0.0805(4) 0.8690(3) 0.0463(19) Uani 1 1 d . . . H15A H 0.7178 0.1129 0.9150 0.069 Uiso 1 1 calc R . . H15B H 0.6583 0.0226 0.8706 0.069 Uiso 1 1 calc R . . H15C H 0.6128 0.0996 0.8486 0.069 Uiso 1 1 calc R . . C16 C 0.9021(6) 0.0518(5) 0.8630(3) 0.059(2) Uani 1 1 d . . . H16A H 0.8751 -0.0061 0.8630 0.088 Uiso 1 1 calc R . . H16B H 0.9335 0.0831 0.9097 0.088 Uiso 1 1 calc R . . H16C H 0.9607 0.0571 0.8405 0.088 Uiso 1 1 calc R . . C17 C 0.9146(6) 0.2947(4) 0.6691(3) 0.056(2) Uani 1 1 d . . . H17A H 0.9508 0.2812 0.6344 0.083 Uiso 1 1 calc R . . H17B H 0.9659 0.3398 0.7050 0.083 Uiso 1 1 calc R . . H17C H 0.8449 0.3113 0.6487 0.083 Uiso 1 1 calc R . . C18 C 1.0093(5) 0.1584(5) 0.7235(3) 0.054(2) Uani 1 1 d . . . H18A H 1.0745 0.2007 0.7532 0.081 Uiso 1 1 calc R . . H18B H 1.0237 0.1395 0.6809 0.081 Uiso 1 1 calc R . . H18C H 0.9968 0.1122 0.7456 0.081 Uiso 1 1 calc R . . C19 C 0.7451(6) 0.1503(4) 0.4856(3) 0.0453(19) Uani 1 1 d . . . H19A H 0.7566 0.1326 0.4419 0.068 Uiso 1 1 calc R . . H19B H 0.8073 0.1962 0.5130 0.068 Uiso 1 1 calc R . . H19C H 0.6737 0.1676 0.4784 0.068 Uiso 1 1 calc R . . C20 C 0.6220(5) -0.0223(4) 0.4727(3) 0.0391(17) Uani 1 1 d . . . H20A H 0.6378 -0.0381 0.4300 0.059 Uiso 1 1 calc R . . H20B H 0.5512 -0.0040 0.4638 0.059 Uiso 1 1 calc R . . H20C H 0.6154 -0.0694 0.4943 0.059 Uiso 1 1 calc R . . C21 C 0.8754(5) 0.0275(4) 0.5400(3) 0.0434(18) Uani 1 1 d . . . H21A H 0.9400 0.0737 0.5631 0.065 Uiso 1 1 calc R . . H21B H 0.8799 0.0052 0.4952 0.065 Uiso 1 1 calc R . . H21C H 0.8764 -0.0152 0.5666 0.065 Uiso 1 1 calc R . . C22 C 0.9175(5) 0.3306(4) 0.9703(3) 0.0437(18) Uani 1 1 d . . . H22A H 0.9726 0.3731 1.0069 0.066 Uiso 1 1 calc R . . H22B H 0.9034 0.2797 0.9865 0.066 Uiso 1 1 calc R . . H22C H 0.8468 0.3484 0.9559 0.066 Uiso 1 1 calc R . . C23 C 1.0253(6) 0.4140(4) 0.8753(3) 0.051(2) Uani 1 1 d . . . H23A H 1.0792 0.4511 0.9159 0.077 Uiso 1 1 calc R . . H23B H 0.9607 0.4379 0.8590 0.077 Uiso 1 1 calc R . . H23C H 1.0620 0.4057 0.8401 0.077 Uiso 1 1 calc R . . C24 C 1.1022(5) 0.2677(5) 0.9233(3) 0.057(2) Uani 1 1 d . . . H24A H 1.0804 0.2167 0.9380 0.086 Uiso 1 1 calc R . . H24B H 1.1606 0.3068 0.9608 0.086 Uiso 1 1 calc R . . H24C H 1.1318 0.2562 0.8852 0.086 Uiso 1 1 calc R . . C25 C -0.1091(6) 0.7218(4) 0.6365(3) 0.0455(19) Uani 1 1 d . . . H25A H -0.0640 0.6803 0.6326 0.055 Uiso 1 1 calc R . . H25B H -0.1634 0.7170 0.5915 0.055 Uiso 1 1 calc R . . C26 C -0.1716(5) 0.7071(4) 0.6867(3) 0.0410(18) Uani 1 1 d . . . H26A H -0.2135 0.7504 0.6925 0.049 Uiso 1 1 calc R . . H26B H -0.2265 0.6535 0.6703 0.049 Uiso 1 1 calc R . . C27 C -0.1444(5) 0.7014(4) 0.8009(3) 0.0415(18) Uani 1 1 d . . . H27A H -0.2013 0.6489 0.7885 0.050 Uiso 1 1 calc R . . H27B H -0.1828 0.7468 0.8064 0.050 Uiso 1 1 calc R . . C28 C -0.0541(5) 0.7052(4) 0.8660(3) 0.0422(18) Uani 1 1 d . . . H28A H -0.0903 0.6974 0.9016 0.051 Uiso 1 1 calc R . . H28B H -0.0167 0.6594 0.8595 0.051 Uiso 1 1 calc R . . C29 C -0.0109(5) 0.8465(4) 0.9140(3) 0.0389(17) Uani 1 1 d . . . H29A H -0.0412 0.8338 0.9510 0.047 Uiso 1 1 calc R . . H29B H -0.0725 0.8565 0.8778 0.047 Uiso 1 1 calc R . . C30 C 0.0838(5) 0.9210(4) 0.9399(3) 0.0354(16) Uani 1 1 d . . . H30A H 0.0577 0.9678 0.9597 0.042 Uiso 1 1 calc R . . H30B H 0.1463 0.9109 0.9753 0.042 Uiso 1 1 calc R . . C31 C 0.2074(6) 1.0124(4) 0.9040(3) 0.0448(19) Uani 1 1 d . . . H31A H 0.2717 1.0079 0.9414 0.054 Uiso 1 1 calc R . . H31B H 0.1780 1.0595 0.9197 0.054 Uiso 1 1 calc R . . C32 C 0.2451(6) 1.0247(4) 0.8439(3) 0.0432(18) Uani 1 1 d . . . H32A H 0.1801 1.0266 0.8057 0.052 Uiso 1 1 calc R . . H32B H 0.3020 1.0770 0.8549 0.052 Uiso 1 1 calc R . . C33 C 0.3440(6) 0.9680(4) 0.7741(3) 0.0431(18) Uani 1 1 d . . . H33A H 0.3780 0.9208 0.7655 0.052 Uiso 1 1 calc R . . H33B H 0.4058 1.0180 0.7906 0.052 Uiso 1 1 calc R . . C34 C 0.2639(6) 0.9746(4) 0.7079(3) 0.0413(18) Uani 1 1 d . . . H34A H 0.2315 1.0231 0.7146 0.050 Uiso 1 1 calc R . . H34B H 0.3041 0.9801 0.6739 0.050 Uiso 1 1 calc R . . C35 C 0.0830(5) 0.9107(4) 0.6357(3) 0.0432(19) Uani 1 1 d . . . H35A H 0.1077 0.9324 0.5996 0.052 Uiso 1 1 calc R . . H35B H 0.0452 0.9499 0.6556 0.052 Uiso 1 1 calc R . . C36 C 0.0025(6) 0.8284(4) 0.6067(3) 0.0426(18) Uani 1 1 d . . . H36A H -0.0619 0.8326 0.5692 0.051 Uiso 1 1 calc R . . H36B H 0.0412 0.7886 0.5888 0.051 Uiso 1 1 calc R . . C37 C 0.1732(7) 0.6037(5) 0.6913(4) 0.069(3) Uani 1 1 d . . . H37A H 0.2503 0.5960 0.7103 0.082 Uiso 1 1 calc R . . H37B H 0.1374 0.5655 0.6470 0.082 Uiso 1 1 calc R . . C38 C 0.1059(7) 0.5874(4) 0.7379(5) 0.066(3) Uani 1 1 d . . . H38A H 0.0274 0.5907 0.7161 0.079 Uiso 1 1 calc R . . H38B H 0.1039 0.5309 0.7449 0.079 Uiso 1 1 calc R . . C39 C 0.2498(6) 0.6333(5) 0.8450(5) 0.080(3) Uani 1 1 d . . . H39A H 0.3089 0.6406 0.8222 0.095 Uiso 1 1 calc R . . H39B H 0.2398 0.5775 0.8544 0.095 Uiso 1 1 calc R . . C40 C 0.2852(7) 0.6946(6) 0.9090(4) 0.075(3) Uani 1 1 d . . . H40A H 0.2218 0.6936 0.9283 0.090 Uiso 1 1 calc R . . H40B H 0.3488 0.6822 0.9421 0.090 Uiso 1 1 calc R . . C41 C 0.3498(6) 0.8412(6) 0.9509(4) 0.080(3) Uani 1 1 d . . . H41A H 0.2901 0.8361 0.9733 0.096 Uiso 1 1 calc R . . H41B H 0.3528 0.8927 0.9341 0.096 Uiso 1 1 calc R . . C42 C 0.4634(6) 0.8475(7) 1.0036(4) 0.096(4) Uani 1 1 d . . . H42A H 0.4753 0.8916 1.0432 0.115 Uiso 1 1 calc R . . H42B H 0.4637 0.7953 1.0192 0.115 Uiso 1 1 calc R . . C43 C 0.6188(5) 0.8085(4) 0.9776(3) 0.0425(18) Uani 1 1 d . . . H43A H 0.5714 0.7522 0.9597 0.051 Uiso 1 1 calc R . . H43B H 0.6628 0.8126 1.0252 0.051 Uiso 1 1 calc R . . C44 C 0.6969(5) 0.8261(5) 0.9369(3) 0.0465(19) Uani 1 1 d . . . H44A H 0.7155 0.8859 0.9395 0.056 Uiso 1 1 calc R . . H44B H 0.7679 0.8103 0.9579 0.056 Uiso 1 1 calc R . . C45 C 0.5559(6) 0.8080(4) 0.8316(3) 0.0440(18) Uani 1 1 d . . . H45A H 0.5726 0.8667 0.8297 0.053 Uiso 1 1 calc R . . H45B H 0.4968 0.7980 0.8541 0.053 Uiso 1 1 calc R . . C46 C 0.5177(6) 0.7556(4) 0.7621(3) 0.0444(19) Uani 1 1 d . . . H46A H 0.5692 0.7736 0.7363 0.053 Uiso 1 1 calc R . . H46B H 0.5166 0.6976 0.7644 0.053 Uiso 1 1 calc R . . C47 C 0.3631(6) 0.7148(5) 0.6648(4) 0.058(2) Uani 1 1 d . . . H47A H 0.3750 0.6588 0.6654 0.070 Uiso 1 1 calc R . . H47B H 0.4007 0.7381 0.6340 0.070 Uiso 1 1 calc R . . C48 C 0.2434(6) 0.7122(5) 0.6418(4) 0.055(2) Uani 1 1 d . . . H48A H 0.2345 0.7679 0.6365 0.066 Uiso 1 1 calc R . . H48B H 0.2110 0.6758 0.5965 0.066 Uiso 1 1 calc R . . C101 C 1.0318(13) 0.5216(7) 0.4770(7) 0.073(5) Uiso 0.50 1 d PD A -1 H101 H 1.0763 0.5458 0.4515 0.087 Uiso 0.50 1 d PR A -1 C102 C 1.0493(6) 0.4481(5) 0.4956(4) 0.068(2) Uiso 1 1 d D A -1 H102 H 1.1051 0.4234 0.4827 0.081 Uiso 0.50 1 d PR A -1 H106 H 1.0619 0.3956 0.5031 0.081 Uiso 0.50 1 d PR A -2 C103 C 0.9893(9) 0.4089(7) 0.5323(6) 0.058(4) Uiso 0.50 1 d PD A -1 H103 H 1.0014 0.3564 0.5400 0.069 Uiso 0.50 1 d PR A -1 C104 C 0.9137(9) 0.4394(6) 0.5589(5) 0.026(3) Uiso 0.50 1 d PD A -1 H104 H 0.8805 0.4126 0.5883 0.032 Uiso 0.50 1 d PR A -1 C105 C 0.8889(14) 0.5116(8) 0.5405(8) 0.076(5) Uiso 0.50 1 d PD A -1 H105 H 0.8360 0.5349 0.5581 0.091 Uiso 0.50 1 d PR A -1 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 Zn1 0.0240(4) 0.0271(4) 0.0335(4) 0.0084(3) 0.0073(3) 0.0058(3) Zn2 0.0239(4) 0.0262(4) 0.0339(4) 0.0086(3) 0.0097(3) 0.0074(3) Cl1 0.0397(10) 0.0410(11) 0.0452(11) 0.0094(8) 0.0128(9) 0.0065(8) K1 0.0285(8) 0.0314(8) 0.0313(8) 0.0098(6) 0.0065(7) 0.0064(6) O1 0.035(3) 0.043(3) 0.041(3) 0.008(2) 0.014(2) 0.009(2) O2 0.028(3) 0.039(3) 0.049(3) 0.010(2) 0.004(2) 0.011(2) O3 0.029(3) 0.033(3) 0.047(3) 0.014(2) 0.014(2) 0.008(2) O4 0.033(3) 0.029(3) 0.034(3) 0.002(2) 0.014(2) -0.001(2) O5 0.034(3) 0.037(3) 0.042(3) 0.010(2) 0.017(2) 0.002(2) O6 0.034(3) 0.039(3) 0.039(3) 0.016(2) 0.011(2) 0.011(2) O7 0.044(3) 0.048(3) 0.041(3) 0.008(2) 0.011(2) 0.016(2) O8 0.045(3) 0.052(3) 0.078(4) 0.033(3) 0.030(3) 0.023(3) O9 0.050(3) 0.086(4) 0.034(3) 0.026(3) 0.019(2) 0.039(3) O10 0.053(3) 0.092(4) 0.042(3) 0.013(3) 0.014(3) 0.047(3) O11 0.043(3) 0.058(3) 0.055(3) 0.013(3) 0.022(3) 0.025(3) O12 0.050(3) 0.052(3) 0.026(3) 0.000(2) 0.011(2) 0.001(3) Si1 0.0256(10) 0.0264(10) 0.0299(10) 0.0088(8) 0.0069(8) 0.0067(8) Si2 0.0239(10) 0.0384(11) 0.0343(11) 0.0089(9) 0.0075(8) 0.0082(9) Si3 0.0289(11) 0.0396(12) 0.0357(11) 0.0108(9) 0.0120(9) 0.0123(9) Si4 0.0310(11) 0.0280(10) 0.0290(10) 0.0069(8) 0.0081(8) 0.0075(8) Si5 0.0293(10) 0.0278(10) 0.0301(10) 0.0063(8) 0.0080(8) 0.0062(8) Si6 0.0338(11) 0.0302(11) 0.0276(10) 0.0084(8) 0.0063(9) 0.0066(9) Si7 0.0538(13) 0.0289(11) 0.0285(11) 0.0074(9) 0.0128(10) 0.0094(10) Si8 0.0226(10) 0.0291(10) 0.0234(10) 0.0060(8) 0.0072(8) 0.0053(8) Si9 0.0316(11) 0.0259(10) 0.0263(10) 0.0054(8) 0.0070(8) 0.0080(8) Si10 0.0350(11) 0.0354(11) 0.0258(10) 0.0061(8) 0.0059(9) 0.0132(9) Si11 0.0223(10) 0.0332(11) 0.0292(10) 0.0015(8) 0.0054(8) 0.0046(8) Si12 0.0206(10) 0.0424(12) 0.0316(11) 0.0014(9) 0.0079(8) -0.0002(9) Si13 0.0275(10) 0.0351(11) 0.0284(10) 0.0097(8) 0.0106(8) 0.0097(8) Si14 0.0235(10) 0.0447(12) 0.0317(11) -0.0008(9) 0.0049(9) 0.0021(9) C1 0.030(4) 0.052(5) 0.051(5) 0.012(4) 0.011(4) -0.003(4) C2 0.034(4) 0.079(6) 0.051(5) 0.022(4) 0.017(4) 0.021(4) C3 0.034(4) 0.061(5) 0.046(4) 0.029(4) 0.015(4) 0.008(4) C4 0.040(4) 0.068(5) 0.049(5) 0.015(4) 0.015(4) 0.027(4) C5 0.036(4) 0.034(4) 0.045(4) 0.008(3) 0.010(3) -0.003(3) C6 0.044(4) 0.034(4) 0.040(4) 0.011(3) 0.012(3) 0.011(3) C7 0.039(4) 0.037(4) 0.047(4) 0.020(3) 0.022(4) 0.011(3) C8 0.056(5) 0.040(4) 0.031(4) 0.001(3) 0.009(4) 0.012(4) C9 0.038(4) 0.037(4) 0.038(4) 0.017(3) 0.007(3) 0.009(3) C10 0.103(7) 0.038(5) 0.058(5) 0.012(4) 0.032(5) 0.031(5) C11 0.053(5) 0.049(5) 0.050(5) -0.005(4) 0.009(4) -0.009(4) C12 0.074(6) 0.052(5) 0.039(4) 0.022(4) 0.024(4) 0.029(4) C13 0.044(4) 0.031(4) 0.042(4) 0.010(3) 0.019(4) 0.003(3) C14 0.059(5) 0.042(4) 0.038(4) 0.005(3) 0.010(4) 0.020(4) C15 0.051(5) 0.050(5) 0.038(4) 0.006(4) 0.022(4) 0.000(4) C16 0.069(6) 0.065(6) 0.043(5) 0.012(4) 0.002(4) 0.038(5) C17 0.054(5) 0.051(5) 0.042(5) -0.004(4) 0.017(4) -0.027(4) C18 0.028(4) 0.086(6) 0.042(5) -0.013(4) 0.008(4) 0.023(4) C19 0.054(5) 0.044(5) 0.042(4) 0.018(4) 0.018(4) 0.006(4) C20 0.043(4) 0.042(4) 0.030(4) -0.003(3) 0.015(3) 0.008(3) C21 0.026(4) 0.061(5) 0.048(4) 0.011(4) 0.014(3) 0.019(4) C22 0.032(4) 0.046(5) 0.045(4) 0.002(4) 0.011(3) -0.003(3) C23 0.048(5) 0.059(5) 0.039(4) 0.002(4) 0.017(4) -0.004(4) C24 0.032(4) 0.080(6) 0.048(5) -0.002(4) 0.001(4) 0.012(4) C25 0.042(5) 0.042(5) 0.044(5) 0.007(4) -0.001(4) 0.010(4) C26 0.026(4) 0.035(4) 0.050(5) 0.002(3) -0.002(4) 0.004(3) C27 0.030(4) 0.037(4) 0.054(5) 0.004(4) 0.017(4) -0.001(3) C28 0.032(4) 0.045(5) 0.054(5) 0.020(4) 0.017(4) 0.005(4) C29 0.029(4) 0.052(5) 0.039(4) 0.016(4) 0.013(3) 0.007(4) C30 0.028(4) 0.044(4) 0.032(4) 0.004(3) 0.011(3) 0.004(3) C31 0.045(5) 0.038(4) 0.041(4) 0.002(3) 0.012(4) -0.010(4) C32 0.040(4) 0.035(4) 0.055(5) 0.013(4) 0.021(4) -0.006(4) C33 0.039(4) 0.042(5) 0.051(5) 0.014(4) 0.020(4) 0.001(3) C34 0.045(5) 0.042(5) 0.048(5) 0.018(4) 0.026(4) 0.012(4) C35 0.035(4) 0.068(5) 0.042(4) 0.033(4) 0.015(4) 0.027(4) C36 0.033(4) 0.069(6) 0.029(4) 0.009(4) 0.008(3) 0.023(4) C37 0.070(6) 0.057(6) 0.085(7) 0.011(5) 0.021(5) 0.035(5) C38 0.065(6) 0.024(4) 0.122(8) 0.017(5) 0.047(6) 0.012(4) C39 0.035(5) 0.062(6) 0.163(10) 0.066(7) 0.031(6) 0.029(5) C40 0.044(5) 0.129(9) 0.073(7) 0.075(7) 0.018(5) 0.028(6) C41 0.057(6) 0.159(10) 0.032(5) 0.000(5) 0.012(4) 0.064(6) C42 0.042(5) 0.221(12) 0.028(5) 0.002(6) 0.008(4) 0.060(7) C43 0.032(4) 0.046(5) 0.049(5) 0.009(4) 0.012(4) 0.009(4) C44 0.026(4) 0.069(5) 0.043(5) 0.016(4) 0.007(4) 0.011(4) C45 0.047(5) 0.041(4) 0.045(5) 0.002(4) 0.015(4) 0.018(4) C46 0.054(5) 0.033(4) 0.050(5) 0.014(4) 0.017(4) 0.012(4) C47 0.061(6) 0.073(6) 0.042(5) 0.018(4) 0.022(4) 0.009(5) C48 0.058(6) 0.074(6) 0.040(5) 0.011(4) 0.017(4) 0.028(5) _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 Zn1 Si4 2.3783(19) . ? Zn1 Si11 2.3882(19) . ? Zn1 Cl1 2.454(2) . ? Zn1 Zn2 3.0902(15) . ? Zn2 Si8 2.3871(19) . ? Zn2 Si1 2.4074(19) . ? Zn2 Cl1 2.4686(19) . ? K1 O8 2.821(5) . ? K1 O5 2.835(4) . ? K1 O7 2.887(5) . ? K1 O2 2.910(5) . ? K1 O3 2.931(4) . ? K1 O6 2.932(4) . ? K1 O9 2.950(5) . ? K1 O1 2.953(5) . ? K1 O4 2.969(4) . ? K1 C33 3.538(7) . ? O1 C36 1.410(7) . ? O1 C25 1.432(7) . ? O2 C27 1.422(7) . ? O2 C26 1.423(7) . ? O3 C29 1.407(7) . ? O3 C28 1.420(7) . ? O4 C31 1.420(7) . ? O4 C30 1.424(7) . ? O5 C32 1.419(7) . ? O5 C33 1.429(7) . ? O6 C35 1.416(7) . ? O6 C34 1.420(7) . ? O7 C37 1.406(8) . ? O7 C48 1.439(8) . ? O8 C39 1.408(8) . ? O8 C38 1.434(9) . ? O9 C41 1.424(9) . ? O9 C40 1.446(9) . ? O10 C43 1.389(7) . ? O10 C42 1.409(9) . ? O11 C44 1.423(7) . ? O11 C45 1.430(7) . ? O12 C46 1.403(7) . ? O12 C47 1.415(8) . ? Si1 Si6 2.329(2) . ? Si1 Si5 2.348(3) . ? Si1 Si2 2.358(2) . ? Si2 C1 1.872(7) . ? Si2 C2 1.891(6) . ? Si2 Si3 2.363(3) . ? Si3 C4 1.895(6) . ? Si3 C3 1.898(6) . ? Si3 Si4 2.332(3) . ? Si4 Si7 2.320(3) . ? Si4 Si5 2.340(2) . ? Si5 C6 1.894(6) . ? Si5 C5 1.896(6) . ? Si6 C7 1.883(6) . ? Si6 C8 1.886(6) . ? Si6 C9 1.889(6) . ? Si7 C11 1.866(7) . ? Si7 C12 1.879(6) . ? Si7 C10 1.882(7) . ? Si8 Si12 2.337(3) . ? Si8 Si9 2.342(2) . ? Si8 Si13 2.342(2) . ? Si9 C13 1.881(6) . ? Si9 C14 1.894(6) . ? Si9 Si10 2.368(3) . ? Si10 C16 1.894(6) . ? Si10 C15 1.899(6) . ? Si10 Si11 2.344(3) . ? Si11 Si14 2.324(3) . ? Si11 Si12 2.343(2) . ? Si12 C17 1.881(7) . ? Si12 C18 1.883(6) . ? Si13 C19 1.863(6) . ? Si13 C21 1.883(6) . ? Si13 C20 1.885(6) . ? Si14 C24 1.886(7) . ? Si14 C23 1.887(7) . ? Si14 C22 1.896(6) . ? C25 C26 1.504(9) . ? C27 C28 1.512(8) . ? C29 C30 1.494(8) . ? C31 C32 1.496(8) . ? C33 C34 1.517(8) . ? C35 C36 1.504(9) . ? C37 C38 1.486(10) . ? C39 C40 1.477(11) . ? C41 C42 1.535(9) . ? C43 C44 1.491(8) . ? C45 C46 1.496(8) . ? C47 C48 1.450(9) . ? C101 C102 1.400(8) . ? C102 C103 1.381(8) . ? C103 C104 1.369(9) . ? C104 C105 1.401(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Si4 Zn1 Si11 149.37(7) . . ? Si4 Zn1 Cl1 106.00(7) . . ? Si11 Zn1 Cl1 104.12(7) . . ? Si4 Zn1 Zn2 106.57(6) . . ? Si11 Zn1 Zn2 88.06(6) . . ? Cl1 Zn1 Zn2 51.32(5) . . ? Si8 Zn2 Si1 154.92(7) . . ? Si8 Zn2 Cl1 104.41(6) . . ? Si1 Zn2 Cl1 99.36(6) . . ? Si8 Zn2 Zn1 103.37(5) . . ? Si1 Zn2 Zn1 85.42(5) . . ? Cl1 Zn2 Zn1 50.91(5) . . ? Zn1 Cl1 Zn2 77.77(6) . . ? O8 K1 O5 135.92(15) . . ? O8 K1 O7 58.78(14) . . ? O5 K1 O7 116.21(14) . . ? O8 K1 O2 72.26(13) . . ? O5 K1 O2 148.61(13) . . ? O7 K1 O2 89.04(13) . . ? O8 K1 O3 75.49(13) . . ? O5 K1 O3 108.65(13) . . ? O7 K1 O3 130.88(14) . . ? O2 K1 O3 58.78(12) . . ? O8 K1 O6 136.78(14) . . ? O5 K1 O6 58.78(12) . . ? O7 K1 O6 78.19(13) . . ? O2 K1 O6 113.72(13) . . ? O3 K1 O6 146.06(12) . . ? O8 K1 O9 59.25(16) . . ? O5 K1 O9 78.53(15) . . ? O7 K1 O9 92.88(13) . . ? O2 K1 O9 120.77(14) . . ? O3 K1 O9 76.95(12) . . ? O6 K1 O9 124.58(14) . . ? O8 K1 O1 111.64(15) . . ? O5 K1 O1 108.44(13) . . ? O7 K1 O1 76.26(12) . . ? O2 K1 O1 57.38(13) . . ? O3 K1 O1 108.04(12) . . ? O6 K1 O1 56.39(12) . . ? O9 K1 O1 168.83(13) . . ? O8 K1 O4 126.44(14) . . ? O5 K1 O4 56.71(12) . . ? O7 K1 O4 172.83(13) . . ? O2 K1 O4 97.28(13) . . ? O3 K1 O4 55.99(12) . . ? O6 K1 O4 96.09(12) . . ? O9 K1 O4 86.80(13) . . ? O1 K1 O4 104.30(12) . . ? O8 K1 C33 132.37(15) . . ? O5 K1 C33 22.65(13) . . ? O7 K1 C33 94.89(15) . . ? O2 K1 C33 152.36(15) . . ? O3 K1 C33 131.30(14) . . ? O6 K1 C33 41.42(14) . . ? O9 K1 C33 86.41(16) . . ? O1 K1 C33 97.00(15) . . ? O4 K1 C33 77.94(14) . . ? C36 O1 C25 112.2(5) . . ? C36 O1 K1 116.2(3) . . ? C25 O1 K1 107.5(4) . . ? C27 O2 C26 111.4(5) . . ? C27 O2 K1 119.7(4) . . ? C26 O2 K1 120.2(4) . . ? C29 O3 C28 113.2(5) . . ? C29 O3 K1 116.5(3) . . ? C28 O3 K1 109.2(4) . . ? C31 O4 C30 111.8(4) . . ? C31 O4 K1 117.7(4) . . ? C30 O4 K1 119.1(3) . . ? C32 O5 C33 113.0(5) . . ? C32 O5 K1 114.7(3) . . ? C33 O5 K1 107.5(3) . . ? C35 O6 C34 111.0(5) . . ? C35 O6 K1 118.8(4) . . ? C34 O6 K1 119.5(3) . . ? C37 O7 C48 115.0(6) . . ? C37 O7 K1 120.4(4) . . ? C48 O7 K1 120.0(4) . . ? C39 O8 C38 115.0(6) . . ? C39 O8 K1 116.3(4) . . ? C38 O8 K1 109.1(4) . . ? C41 O9 C40 115.0(6) . . ? C41 O9 K1 109.0(4) . . ? C40 O9 K1 110.1(4) . . ? C43 O10 C42 114.5(6) . . ? C44 O11 C45 112.8(5) . . ? C46 O12 C47 111.3(5) . . ? Si6 Si1 Si5 109.99(9) . . ? Si6 Si1 Si2 113.20(10) . . ? Si5 Si1 Si2 99.32(9) . . ? Si6 Si1 Zn2 112.99(9) . . ? Si5 Si1 Zn2 113.03(8) . . ? Si2 Si1 Zn2 107.57(8) . . ? C1 Si2 C2 104.2(3) . . ? C1 Si2 Si1 113.5(2) . . ? C2 Si2 Si1 112.3(2) . . ? C1 Si2 Si3 113.8(2) . . ? C2 Si2 Si3 106.7(2) . . ? Si1 Si2 Si3 106.29(10) . . ? C4 Si3 C3 106.0(3) . . ? C4 Si3 Si4 113.3(2) . . ? C3 Si3 Si4 110.4(2) . . ? C4 Si3 Si2 108.2(2) . . ? C3 Si3 Si2 115.0(2) . . ? Si4 Si3 Si2 104.11(10) . . ? Si7 Si4 Si3 115.04(10) . . ? Si7 Si4 Si5 114.42(10) . . ? Si3 Si4 Si5 102.26(9) . . ? Si7 Si4 Zn1 119.58(9) . . ? Si3 Si4 Zn1 107.68(9) . . ? Si5 Si4 Zn1 94.87(8) . . ? C6 Si5 C5 105.9(3) . . ? C6 Si5 Si4 113.4(2) . . ? C5 Si5 Si4 111.7(2) . . ? C6 Si5 Si1 112.8(2) . . ? C5 Si5 Si1 113.0(2) . . ? Si4 Si5 Si1 100.17(9) . . ? C7 Si6 C8 107.6(3) . . ? C7 Si6 C9 107.5(3) . . ? C8 Si6 C9 108.0(3) . . ? C7 Si6 Si1 108.8(2) . . ? C8 Si6 Si1 110.5(2) . . ? C9 Si6 Si1 114.2(2) . . ? C11 Si7 C12 107.0(3) . . ? C11 Si7 C10 108.1(4) . . ? C12 Si7 C10 107.3(3) . . ? C11 Si7 Si4 109.5(2) . . ? C12 Si7 Si4 110.7(2) . . ? C10 Si7 Si4 113.9(3) . . ? Si12 Si8 Si9 97.96(9) . . ? Si12 Si8 Si13 109.76(9) . . ? Si9 Si8 Si13 116.86(9) . . ? Si12 Si8 Zn2 99.21(8) . . ? Si9 Si8 Zn2 109.36(8) . . ? Si13 Si8 Zn2 119.85(9) . . ? C13 Si9 C14 106.3(3) . . ? C13 Si9 Si8 112.7(2) . . ? C14 Si9 Si8 113.0(2) . . ? C13 Si9 Si10 113.0(2) . . ? C14 Si9 Si10 106.7(2) . . ? Si8 Si9 Si10 105.09(9) . . ? C16 Si10 C15 102.8(3) . . ? C16 Si10 Si11 114.6(3) . . ? C15 Si10 Si11 112.0(2) . . ? C16 Si10 Si9 107.8(2) . . ? C15 Si10 Si9 114.5(2) . . ? Si11 Si10 Si9 105.29(9) . . ? Si14 Si11 Si12 114.07(10) . . ? Si14 Si11 Si10 114.35(10) . . ? Si12 Si11 Si10 98.10(9) . . ? Si14 Si11 Zn1 110.58(9) . . ? Si12 Si11 Zn1 115.70(9) . . ? Si10 Si11 Zn1 103.03(8) . . ? C17 Si12 C18 106.9(3) . . ? C17 Si12 Si8 111.6(2) . . ? C18 Si12 Si8 113.9(2) . . ? C17 Si12 Si11 115.0(2) . . ? C18 Si12 Si11 109.0(2) . . ? Si8 Si12 Si11 100.43(9) . . ? C19 Si13 C21 109.0(3) . . ? C19 Si13 C20 106.2(3) . . ? C21 Si13 C20 107.4(3) . . ? C19 Si13 Si8 108.3(2) . . ? C21 Si13 Si8 111.8(2) . . ? C20 Si13 Si8 114.0(2) . . ? C24 Si14 C23 107.2(3) . . ? C24 Si14 C22 108.3(3) . . ? C23 Si14 C22 109.0(3) . . ? C24 Si14 Si11 113.8(2) . . ? C23 Si14 Si11 110.4(2) . . ? C22 Si14 Si11 108.0(2) . . ? O1 C25 C26 109.1(5) . . ? O2 C26 C25 108.5(5) . . ? O2 C27 C28 108.2(5) . . ? O3 C28 C27 113.5(5) . . ? O3 C29 C30 109.2(5) . . ? O4 C30 C29 108.1(5) . . ? O4 C31 C32 108.1(5) . . ? O5 C32 C31 107.8(5) . . ? O5 C33 C34 114.3(5) . . ? O5 C33 K1 49.8(3) . . ? C34 C33 K1 89.4(4) . . ? O6 C34 C33 106.7(5) . . ? O6 C35 C36 108.6(5) . . ? O1 C36 C35 108.3(5) . . ? O7 C37 C38 107.6(6) . . ? O8 C38 C37 114.4(6) . . ? O8 C39 C40 109.7(7) . . ? O9 C40 C39 108.0(6) . . ? O9 C41 C42 114.5(7) . . ? O10 C42 C41 109.2(6) . . ? O10 C43 C44 109.4(6) . . ? O11 C44 C43 115.6(6) . . ? O11 C45 C46 106.2(5) . . ? O12 C46 C45 106.8(5) . . ? O12 C47 C48 108.1(6) . . ? O7 C48 C47 117.1(6) . . ? C103 C102 C101 122.5(9) . . ? C104 C103 C102 124.8(9) . . ? C103 C104 C105 115.7(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Si4 Zn1 Zn2 Si8 164.68(6) . . . . ? Si11 Zn1 Zn2 Si8 12.03(6) . . . . ? Cl1 Zn1 Zn2 Si8 -97.84(7) . . . . ? Si4 Zn1 Zn2 Si1 8.49(7) . . . . ? Si11 Zn1 Zn2 Si1 -144.16(7) . . . . ? Cl1 Zn1 Zn2 Si1 105.97(7) . . . . ? Si4 Zn1 Zn2 Cl1 -97.48(7) . . . . ? Si11 Zn1 Zn2 Cl1 109.87(7) . . . . ? Si4 Zn1 Cl1 Zn2 98.66(6) . . . . ? Si11 Zn1 Cl1 Zn2 -75.75(7) . . . . ? Si8 Zn2 Cl1 Zn1 95.68(6) . . . . ? Si1 Zn2 Cl1 Zn1 -76.23(6) . . . . ? O8 K1 O1 C36 -111.1(4) . . . . ? O5 K1 O1 C36 50.2(4) . . . . ? O7 K1 O1 C36 -63.2(4) . . . . ? O2 K1 O1 C36 -161.0(4) . . . . ? O3 K1 O1 C36 167.8(4) . . . . ? O6 K1 O1 C36 21.6(4) . . . . ? O9 K1 O1 C36 -77.1(8) . . . . ? O4 K1 O1 C36 109.4(4) . . . . ? C33 K1 O1 C36 30.1(4) . . . . ? O8 K1 O1 C25 15.5(4) . . . . ? O5 K1 O1 C25 176.8(4) . . . . ? O7 K1 O1 C25 63.3(4) . . . . ? O2 K1 O1 C25 -34.5(4) . . . . ? O3 K1 O1 C25 -65.6(4) . . . . ? O6 K1 O1 C25 148.1(4) . . . . ? O9 K1 O1 C25 49.4(9) . . . . ? O4 K1 O1 C25 -124.0(4) . . . . ? C33 K1 O1 C25 156.7(4) . . . . ? O8 K1 O2 C27 86.3(4) . . . . ? O5 K1 O2 C27 -71.2(5) . . . . ? O7 K1 O2 C27 143.7(4) . . . . ? O3 K1 O2 C27 2.9(4) . . . . ? O6 K1 O2 C27 -139.6(4) . . . . ? O9 K1 O2 C27 50.9(4) . . . . ? O1 K1 O2 C27 -142.0(4) . . . . ? O4 K1 O2 C27 -39.7(4) . . . . ? C33 K1 O2 C27 -117.6(5) . . . . ? O8 K1 O2 C26 -128.8(4) . . . . ? O5 K1 O2 C26 73.7(5) . . . . ? O7 K1 O2 C26 -71.4(4) . . . . ? O3 K1 O2 C26 147.8(4) . . . . ? O6 K1 O2 C26 5.3(4) . . . . ? O9 K1 O2 C26 -164.2(4) . . . . ? O1 K1 O2 C26 2.9(4) . . . . ? O4 K1 O2 C26 105.2(4) . . . . ? C33 K1 O2 C26 27.3(6) . . . . ? O8 K1 O3 C29 180.0(4) . . . . ? O5 K1 O3 C29 45.9(4) . . . . ? O7 K1 O3 C29 -158.8(4) . . . . ? O2 K1 O3 C29 -102.2(4) . . . . ? O6 K1 O3 C29 -15.5(5) . . . . ? O9 K1 O3 C29 118.8(4) . . . . ? O1 K1 O3 C29 -71.6(4) . . . . ? O4 K1 O3 C29 23.8(4) . . . . ? C33 K1 O3 C29 45.6(4) . . . . ? O8 K1 O3 C28 -50.2(4) . . . . ? O5 K1 O3 C28 175.7(3) . . . . ? O7 K1 O3 C28 -28.9(4) . . . . ? O2 K1 O3 C28 27.7(3) . . . . ? O6 K1 O3 C28 114.3(4) . . . . ? O9 K1 O3 C28 -111.3(4) . . . . ? O1 K1 O3 C28 58.3(4) . . . . ? O4 K1 O3 C28 153.7(4) . . . . ? C33 K1 O3 C28 175.5(3) . . . . ? O8 K1 O4 C31 122.2(4) . . . . ? O5 K1 O4 C31 -3.5(4) . . . . ? O7 K1 O4 C31 -12.8(12) . . . . ? O2 K1 O4 C31 -164.5(4) . . . . ? O3 K1 O4 C31 151.2(4) . . . . ? O6 K1 O4 C31 -49.6(4) . . . . ? O9 K1 O4 C31 74.8(4) . . . . ? O1 K1 O4 C31 -106.4(4) . . . . ? C33 K1 O4 C31 -12.2(4) . . . . ? O8 K1 O4 C30 -18.4(4) . . . . ? O5 K1 O4 C30 -144.1(4) . . . . ? O7 K1 O4 C30 -153.4(10) . . . . ? O2 K1 O4 C30 54.9(4) . . . . ? O3 K1 O4 C30 10.7(4) . . . . ? O6 K1 O4 C30 169.8(4) . . . . ? O9 K1 O4 C30 -65.7(4) . . . . ? O1 K1 O4 C30 113.0(4) . . . . ? C33 K1 O4 C30 -152.7(4) . . . . ? O8 K1 O5 C32 -141.1(4) . . . . ? O7 K1 O5 C32 147.7(4) . . . . ? O2 K1 O5 C32 7.3(5) . . . . ? O3 K1 O5 C32 -52.9(4) . . . . ? O6 K1 O5 C32 92.1(4) . . . . ? O9 K1 O5 C32 -124.7(4) . . . . ? O1 K1 O5 C32 64.3(4) . . . . ? O4 K1 O5 C32 -31.0(4) . . . . ? C33 K1 O5 C32 126.6(6) . . . . ? O8 K1 O5 C33 92.3(4) . . . . ? O7 K1 O5 C33 21.1(4) . . . . ? O2 K1 O5 C33 -119.3(4) . . . . ? O3 K1 O5 C33 -179.5(4) . . . . ? O6 K1 O5 C33 -34.5(4) . . . . ? O9 K1 O5 C33 108.7(4) . . . . ? O1 K1 O5 C33 -62.3(4) . . . . ? O4 K1 O5 C33 -157.6(4) . . . . ? O8 K1 O6 C35 100.2(4) . . . . ? O5 K1 O6 C35 -134.2(4) . . . . ? O7 K1 O6 C35 94.9(4) . . . . ? O2 K1 O6 C35 11.3(4) . . . . ? O3 K1 O6 C35 -57.5(5) . . . . ? O9 K1 O6 C35 -179.7(4) . . . . ? O1 K1 O6 C35 13.7(4) . . . . ? O4 K1 O6 C35 -89.4(4) . . . . ? C33 K1 O6 C35 -153.4(5) . . . . ? O8 K1 O6 C34 -118.5(4) . . . . ? O5 K1 O6 C34 7.1(4) . . . . ? O7 K1 O6 C34 -123.8(4) . . . . ? O2 K1 O6 C34 152.6(4) . . . . ? O3 K1 O6 C34 83.7(5) . . . . ? O9 K1 O6 C34 -38.5(4) . . . . ? O1 K1 O6 C34 155.0(4) . . . . ? O4 K1 O6 C34 51.8(4) . . . . ? C33 K1 O6 C34 -12.1(4) . . . . ? O8 K1 O7 C37 4.7(5) . . . . ? O5 K1 O7 C37 134.4(5) . . . . ? O2 K1 O7 C37 -65.0(5) . . . . ? O3 K1 O7 C37 -19.4(5) . . . . ? O6 K1 O7 C37 -179.5(5) . . . . ? O9 K1 O7 C37 55.8(5) . . . . ? O1 K1 O7 C37 -121.6(5) . . . . ? O4 K1 O7 C37 143.0(10) . . . . ? C33 K1 O7 C37 142.4(5) . . . . ? O8 K1 O7 C48 -150.1(5) . . . . ? O5 K1 O7 C48 -20.5(5) . . . . ? O2 K1 O7 C48 140.1(4) . . . . ? O3 K1 O7 C48 -174.3(4) . . . . ? O6 K1 O7 C48 25.6(4) . . . . ? O9 K1 O7 C48 -99.1(4) . . . . ? O1 K1 O7 C48 83.6(4) . . . . ? O4 K1 O7 C48 -11.9(13) . . . . ? C33 K1 O7 C48 -12.5(4) . . . . ? O5 K1 O8 C39 3.7(6) . . . . ? O7 K1 O8 C39 100.4(6) . . . . ? O2 K1 O8 C39 -159.6(6) . . . . ? O3 K1 O8 C39 -98.3(6) . . . . ? O6 K1 O8 C39 94.3(6) . . . . ? O9 K1 O8 C39 -15.0(5) . . . . ? O1 K1 O8 C39 157.7(5) . . . . ? O4 K1 O8 C39 -73.7(6) . . . . ? C33 K1 O8 C39 35.1(6) . . . . ? O5 K1 O8 C38 -128.3(4) . . . . ? O7 K1 O8 C38 -31.6(4) . . . . ? O2 K1 O8 C38 68.3(4) . . . . ? O3 K1 O8 C38 129.7(4) . . . . ? O6 K1 O8 C38 -37.7(5) . . . . ? O9 K1 O8 C38 -147.0(4) . . . . ? O1 K1 O8 C38 25.7(4) . . . . ? O4 K1 O8 C38 154.3(4) . . . . ? C33 K1 O8 C38 -96.9(4) . . . . ? O8 K1 O9 C41 -147.4(5) . . . . ? O5 K1 O9 C41 45.7(5) . . . . ? O7 K1 O9 C41 161.9(5) . . . . ? O2 K1 O9 C41 -107.5(5) . . . . ? O3 K1 O9 C41 -66.7(5) . . . . ? O6 K1 O9 C41 84.3(5) . . . . ? O1 K1 O9 C41 175.4(7) . . . . ? O4 K1 O9 C41 -10.9(5) . . . . ? C33 K1 O9 C41 67.2(5) . . . . ? O8 K1 O9 C40 -20.4(5) . . . . ? O5 K1 O9 C40 172.8(5) . . . . ? O7 K1 O9 C40 -71.1(5) . . . . ? O2 K1 O9 C40 19.5(5) . . . . ? O3 K1 O9 C40 60.3(5) . . . . ? O6 K1 O9 C40 -148.7(5) . . . . ? O1 K1 O9 C40 -57.5(9) . . . . ? O4 K1 O9 C40 116.1(5) . . . . ? C33 K1 O9 C40 -165.8(5) . . . . ? Si8 Zn2 Si1 Si6 43.30(19) . . . . ? Cl1 Zn2 Si1 Si6 -155.45(9) . . . . ? Zn1 Zn2 Si1 Si6 155.41(8) . . . . ? Si8 Zn2 Si1 Si5 -82.42(17) . . . . ? Cl1 Zn2 Si1 Si5 78.83(9) . . . . ? Zn1 Zn2 Si1 Si5 29.70(8) . . . . ? Si8 Zn2 Si1 Si2 168.98(13) . . . . ? Cl1 Zn2 Si1 Si2 -29.78(9) . . . . ? Zn1 Zn2 Si1 Si2 -78.91(8) . . . . ? Si6 Si1 Si2 C1 85.0(3) . . . . ? Si5 Si1 Si2 C1 -158.4(2) . . . . ? Zn2 Si1 Si2 C1 -40.5(3) . . . . ? Si6 Si1 Si2 C2 -32.8(3) . . . . ? Si5 Si1 Si2 C2 83.8(3) . . . . ? Zn2 Si1 Si2 C2 -158.4(3) . . . . ? Si6 Si1 Si2 Si3 -149.15(10) . . . . ? Si5 Si1 Si2 Si3 -32.59(11) . . . . ? Zn2 Si1 Si2 Si3 85.30(10) . . . . ? C1 Si2 Si3 C4 -110.8(3) . . . . ? C2 Si2 Si3 C4 3.6(3) . . . . ? Si1 Si2 Si3 C4 123.6(3) . . . . ? C1 Si2 Si3 C3 7.5(3) . . . . ? C2 Si2 Si3 C3 121.9(3) . . . . ? Si1 Si2 Si3 C3 -118.1(2) . . . . ? C1 Si2 Si3 Si4 128.4(2) . . . . ? C2 Si2 Si3 Si4 -117.2(2) . . . . ? Si1 Si2 Si3 Si4 2.79(12) . . . . ? C4 Si3 Si4 Si7 35.8(3) . . . . ? C3 Si3 Si4 Si7 -82.9(3) . . . . ? Si2 Si3 Si4 Si7 153.18(10) . . . . ? C4 Si3 Si4 Si5 -88.8(2) . . . . ? C3 Si3 Si4 Si5 152.5(2) . . . . ? Si2 Si3 Si4 Si5 28.53(11) . . . . ? C4 Si3 Si4 Zn1 171.9(2) . . . . ? C3 Si3 Si4 Zn1 53.2(3) . . . . ? Si2 Si3 Si4 Zn1 -70.70(10) . . . . ? Si11 Zn1 Si4 Si7 -46.91(18) . . . . ? Cl1 Zn1 Si4 Si7 143.78(10) . . . . ? Zn2 Zn1 Si4 Si7 -162.59(8) . . . . ? Si11 Zn1 Si4 Si3 179.32(11) . . . . ? Cl1 Zn1 Si4 Si3 10.01(10) . . . . ? Zn2 Zn1 Si4 Si3 63.64(9) . . . . ? Si11 Zn1 Si4 Si5 74.79(15) . . . . ? Cl1 Zn1 Si4 Si5 -94.52(8) . . . . ? Zn2 Zn1 Si4 Si5 -40.89(8) . . . . ? Si7 Si4 Si5 C6 -54.3(3) . . . . ? Si3 Si4 Si5 C6 70.8(2) . . . . ? Zn1 Si4 Si5 C6 -179.9(2) . . . . ? Si7 Si4 Si5 C5 65.3(2) . . . . ? Si3 Si4 Si5 C5 -169.6(2) . . . . ? Zn1 Si4 Si5 C5 -60.3(2) . . . . ? Si7 Si4 Si5 Si1 -174.72(10) . . . . ? Si3 Si4 Si5 Si1 -49.66(10) . . . . ? Zn1 Si4 Si5 Si1 59.63(9) . . . . ? Si6 Si1 Si5 C6 48.2(2) . . . . ? Si2 Si1 Si5 C6 -70.8(2) . . . . ? Zn2 Si1 Si5 C6 175.5(2) . . . . ? Si6 Si1 Si5 C5 -72.0(2) . . . . ? Si2 Si1 Si5 C5 169.0(2) . . . . ? Zn2 Si1 Si5 C5 55.3(2) . . . . ? Si6 Si1 Si5 Si4 169.00(9) . . . . ? Si2 Si1 Si5 Si4 50.02(10) . . . . ? Zn2 Si1 Si5 Si4 -63.69(10) . . . . ? Si5 Si1 Si6 C7 58.8(2) . . . . ? Si2 Si1 Si6 C7 168.9(2) . . . . ? Zn2 Si1 Si6 C7 -68.5(2) . . . . ? Si5 Si1 Si6 C8 176.7(2) . . . . ? Si2 Si1 Si6 C8 -73.2(3) . . . . ? Zn2 Si1 Si6 C8 49.4(3) . . . . ? Si5 Si1 Si6 C9 -61.3(2) . . . . ? Si2 Si1 Si6 C9 48.8(2) . . . . ? Zn2 Si1 Si6 C9 171.4(2) . . . . ? Si3 Si4 Si7 C11 -177.9(3) . . . . ? Si5 Si4 Si7 C11 -59.9(3) . . . . ? Zn1 Si4 Si7 C11 51.6(3) . . . . ? Si3 Si4 Si7 C12 64.4(3) . . . . ? Si5 Si4 Si7 C12 -177.6(2) . . . . ? Zn1 Si4 Si7 C12 -66.2(3) . . . . ? Si3 Si4 Si7 C10 -56.7(3) . . . . ? Si5 Si4 Si7 C10 61.3(3) . . . . ? Zn1 Si4 Si7 C10 172.7(3) . . . . ? Si1 Zn2 Si8 Si12 66.90(17) . . . . ? Cl1 Zn2 Si8 Si12 -93.98(8) . . . . ? Zn1 Zn2 Si8 Si12 -41.43(8) . . . . ? Si1 Zn2 Si8 Si9 168.77(13) . . . . ? Cl1 Zn2 Si8 Si9 7.88(9) . . . . ? Zn1 Zn2 Si8 Si9 60.44(8) . . . . ? Si1 Zn2 Si8 Si13 -52.3(2) . . . . ? Cl1 Zn2 Si8 Si13 146.81(9) . . . . ? Zn1 Zn2 Si8 Si13 -160.64(8) . . . . ? Si12 Si8 Si9 C13 157.0(2) . . . . ? Si13 Si8 Si9 C13 -86.0(2) . . . . ? Zn2 Si8 Si9 C13 54.3(2) . . . . ? Si12 Si8 Si9 C14 -82.5(2) . . . . ? Si13 Si8 Si9 C14 34.5(3) . . . . ? Zn2 Si8 Si9 C14 174.8(2) . . . . ? Si12 Si8 Si9 Si10 33.49(10) . . . . ? Si13 Si8 Si9 Si10 150.46(9) . . . . ? Zn2 Si8 Si9 Si10 -69.24(10) . . . . ? C13 Si9 Si10 C16 112.9(3) . . . . ? C14 Si9 Si10 C16 -3.6(4) . . . . ? Si8 Si9 Si10 C16 -123.8(3) . . . . ? C13 Si9 Si10 C15 -0.9(3) . . . . ? C14 Si9 Si10 C15 -117.4(3) . . . . ? Si8 Si9 Si10 C15 122.4(3) . . . . ? C13 Si9 Si10 Si11 -124.4(2) . . . . ? C14 Si9 Si10 Si11 119.1(2) . . . . ? Si8 Si9 Si10 Si11 -1.10(11) . . . . ? C16 Si10 Si11 Si14 -34.5(3) . . . . ? C15 Si10 Si11 Si14 82.1(3) . . . . ? Si9 Si10 Si11 Si14 -152.78(10) . . . . ? C16 Si10 Si11 Si12 86.6(3) . . . . ? C15 Si10 Si11 Si12 -156.8(2) . . . . ? Si9 Si10 Si11 Si12 -31.68(10) . . . . ? C16 Si10 Si11 Zn1 -154.5(2) . . . . ? C15 Si10 Si11 Zn1 -37.9(2) . . . . ? Si9 Si10 Si11 Zn1 87.17(10) . . . . ? Si4 Zn1 Si11 Si14 35.15(17) . . . . ? Cl1 Zn1 Si11 Si14 -155.44(9) . . . . ? Zn2 Zn1 Si11 Si14 155.35(9) . . . . ? Si4 Zn1 Si11 Si12 -96.46(15) . . . . ? Cl1 Zn1 Si11 Si12 72.95(11) . . . . ? Zn2 Zn1 Si11 Si12 23.74(9) . . . . ? Si4 Zn1 Si11 Si10 157.76(11) . . . . ? Cl1 Zn1 Si11 Si10 -32.83(9) . . . . ? Zn2 Zn1 Si11 Si10 -82.04(8) . . . . ? Si9 Si8 Si12 C17 -177.1(3) . . . . ? Si13 Si8 Si12 C17 60.6(3) . . . . ? Zn2 Si8 Si12 C17 -65.8(3) . . . . ? Si9 Si8 Si12 C18 61.7(3) . . . . ? Si13 Si8 Si12 C18 -60.7(3) . . . . ? Zn2 Si8 Si12 C18 172.9(3) . . . . ? Si9 Si8 Si12 Si11 -54.68(10) . . . . ? Si13 Si8 Si12 Si11 -177.03(9) . . . . ? Zn2 Si8 Si12 Si11 56.53(10) . . . . ? Si14 Si11 Si12 C17 -64.8(3) . . . . ? Si10 Si11 Si12 C17 173.9(3) . . . . ? Zn1 Si11 Si12 C17 65.2(3) . . . . ? Si14 Si11 Si12 C18 55.3(3) . . . . ? Si10 Si11 Si12 C18 -66.0(3) . . . . ? Zn1 Si11 Si12 C18 -174.8(3) . . . . ? Si14 Si11 Si12 Si8 175.27(10) . . . . ? Si10 Si11 Si12 Si8 53.96(10) . . . . ? Zn1 Si11 Si12 Si8 -54.78(12) . . . . ? Si12 Si8 Si13 C19 -69.7(3) . . . . ? Si9 Si8 Si13 C19 180.0(2) . . . . ? Zn2 Si8 Si13 C19 44.0(3) . . . . ? Si12 Si8 Si13 C21 50.3(3) . . . . ? Si9 Si8 Si13 C21 -60.0(3) . . . . ? Zn2 Si8 Si13 C21 164.0(2) . . . . ? Si12 Si8 Si13 C20 172.3(2) . . . . ? Si9 Si8 Si13 C20 62.0(3) . . . . ? Zn2 Si8 Si13 C20 -74.0(3) . . . . ? Si12 Si11 Si14 C24 -62.3(3) . . . . ? Si10 Si11 Si14 C24 49.5(3) . . . . ? Zn1 Si11 Si14 C24 165.2(3) . . . . ? Si12 Si11 Si14 C23 58.3(3) . . . . ? Si10 Si11 Si14 C23 170.1(2) . . . . ? Zn1 Si11 Si14 C23 -74.2(3) . . . . ? Si12 Si11 Si14 C22 177.4(2) . . . . ? Si10 Si11 Si14 C22 -70.8(3) . . . . ? Zn1 Si11 Si14 C22 44.9(3) . . . . ? C36 O1 C25 C26 -164.7(5) . . . . ? K1 O1 C25 C26 66.5(5) . . . . ? C27 O2 C26 C25 175.1(5) . . . . ? K1 O2 C26 C25 27.6(6) . . . . ? O1 C25 C26 O2 -64.0(7) . . . . ? C26 O2 C27 C28 -178.5(5) . . . . ? K1 O2 C27 C28 -30.8(6) . . . . ? C29 O3 C28 C27 72.3(7) . . . . ? K1 O3 C28 C27 -59.3(6) . . . . ? O2 C27 C28 O3 61.7(7) . . . . ? C28 O3 C29 C30 176.8(5) . . . . ? K1 O3 C29 C30 -55.3(6) . . . . ? C31 O4 C30 C29 176.5(5) . . . . ? K1 O4 C30 C29 -40.7(6) . . . . ? O3 C29 C30 O4 62.1(6) . . . . ? C30 O4 C31 C32 177.6(5) . . . . ? K1 O4 C31 C32 34.3(7) . . . . ? C33 O5 C32 C31 -172.8(5) . . . . ? K1 O5 C32 C31 63.5(6) . . . . ? O4 C31 C32 O5 -63.1(7) . . . . ? C32 O5 C33 C34 -60.9(7) . . . . ? K1 O5 C33 C34 66.7(6) . . . . ? C32 O5 C33 K1 -127.6(5) . . . . ? O8 K1 C33 O5 -109.8(4) . . . . ? O7 K1 C33 O5 -161.0(4) . . . . ? O2 K1 C33 O5 101.6(4) . . . . ? O3 K1 C33 O5 0.7(4) . . . . ? O6 K1 C33 O5 133.0(5) . . . . ? O9 K1 C33 O5 -68.5(4) . . . . ? O1 K1 C33 O5 122.2(4) . . . . ? O4 K1 C33 O5 19.0(3) . . . . ? O8 K1 C33 C34 127.1(4) . . . . ? O5 K1 C33 C34 -123.1(6) . . . . ? O7 K1 C33 C34 75.8(4) . . . . ? O2 K1 C33 C34 -21.5(6) . . . . ? O3 K1 C33 C34 -122.5(4) . . . . ? O6 K1 C33 C34 9.9(3) . . . . ? O9 K1 C33 C34 168.4(4) . . . . ? O1 K1 C33 C34 -0.9(4) . . . . ? O4 K1 C33 C34 -104.1(4) . . . . ? C35 O6 C34 C33 163.9(5) . . . . ? K1 O6 C34 C33 19.8(6) . . . . ? O5 C33 C34 O6 -58.7(7) . . . . ? K1 C33 C34 O6 -14.2(4) . . . . ? C34 O6 C35 C36 171.0(5) . . . . ? K1 O6 C35 C36 -44.7(6) . . . . ? C25 O1 C36 C35 -176.8(5) . . . . ? K1 O1 C36 C35 -52.6(6) . . . . ? O6 C35 C36 O1 63.4(6) . . . . ? C48 O7 C37 C38 177.8(6) . . . . ? K1 O7 C37 C38 21.8(8) . . . . ? C39 O8 C38 C37 -70.2(8) . . . . ? K1 O8 C38 C37 62.5(7) . . . . ? O7 C37 C38 O8 -56.8(9) . . . . ? C38 O8 C39 C40 178.7(6) . . . . ? K1 O8 C39 C40 49.5(8) . . . . ? C41 O9 C40 C39 176.5(6) . . . . ? K1 O9 C40 C39 53.0(7) . . . . ? O8 C39 C40 O9 -70.0(8) . . . . ? C40 O9 C41 C42 72.6(9) . . . . ? K1 O9 C41 C42 -163.3(6) . . . . ? C43 O10 C42 C41 -123.9(8) . . . . ? O9 C41 C42 O10 65.3(11) . . . . ? C42 O10 C43 C44 172.1(6) . . . . ? C45 O11 C44 C43 61.3(8) . . . . ? O10 C43 C44 O11 -89.3(7) . . . . ? C44 O11 C45 C46 -175.1(5) . . . . ? C47 O12 C46 C45 -178.2(6) . . . . ? O11 C45 C46 O12 168.1(5) . . . . ? C46 O12 C47 C48 167.1(6) . . . . ? C37 O7 C48 C47 -63.2(9) . . . . ? K1 O7 C48 C47 93.0(7) . . . . ? O12 C47 C48 O7 -55.6(9) . . . . ? C101 C102 C103 C104 -5.2(15) . . . . ? C102 C103 C104 C105 6.9(18) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.33 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.778 _refine_diff_density_min -0.671 _refine_diff_density_rms 0.101 # Attachment '2a_346j_ohne.cif' data_346j _database_code_depnum_ccdc_archive 'CCDC 645722' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H180 Si28 Zn2' _chemical_formula_weight 1819.30 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' Si Si 0.0817 0.0704 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 38.527(8) _cell_length_b 15.157(3) _cell_length_c 19.744(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.62(3) _cell_angle_gamma 90.00 _cell_volume 11525(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blocks _exptl_crystal_colour colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.049 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3968 _exptl_absorpt_coefficient_mu 0.736 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7673 _exptl_absorpt_correction_T_max 0.8549 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 77997 _diffrn_reflns_av_R_equivalents 0.0625 _diffrn_reflns_av_sigmaI/netI 0.0556 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 24.50 _reflns_number_total 19158 _reflns_number_gt 16910 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+23.4198P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19158 _refine_ls_number_parameters 871 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0888 _refine_ls_R_factor_gt 0.0752 _refine_ls_wR_factor_ref 0.1495 _refine_ls_wR_factor_gt 0.1440 _refine_ls_goodness_of_fit_ref 1.286 _refine_ls_restrained_S_all 1.286 _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 Zn1 Zn 0.364940(14) 0.95614(4) 0.14309(3) 0.01270(14) Uani 1 1 d . . . Zn2 Zn 0.128246(14) 0.39664(4) 0.37511(3) 0.01217(13) Uani 1 1 d . . . Si1 Si 0.38042(3) 0.82657(9) 0.08029(7) 0.0137(3) Uani 1 1 d . . . Si2 Si 0.33645(4) 0.72262(10) 0.10334(8) 0.0211(3) Uani 1 1 d . . . Si3 Si 0.36637(4) 0.87481(9) -0.03135(7) 0.0197(3) Uani 1 1 d . . . Si4 Si 0.43784(3) 0.77139(9) 0.09969(7) 0.0143(3) Uani 1 1 d . . . Si5 Si 0.44440(4) 0.68174(9) 0.19700(7) 0.0200(3) Uani 1 1 d . . . Si6 Si 0.46047(4) 0.68354(10) 0.01251(7) 0.0214(3) Uani 1 1 d . . . Si7 Si 0.47606(4) 0.89089(10) 0.11861(8) 0.0225(3) Uani 1 1 d . . . Si8 Si 0.34297(3) 1.07396(9) 0.21112(7) 0.0127(3) Uani 1 1 d . . . Si9 Si 0.37559(4) 1.04493(10) 0.31189(7) 0.0194(3) Uani 1 1 d . . . Si10 Si 0.28684(4) 1.02302(9) 0.23758(7) 0.0181(3) Uani 1 1 d . . . Si11 Si 0.34543(3) 1.22097(9) 0.16963(7) 0.0133(3) Uani 1 1 d . . . Si12 Si 0.39537(4) 1.23777(10) 0.10502(7) 0.0190(3) Uani 1 1 d . . . Si13 Si 0.29860(4) 1.25646(9) 0.09481(7) 0.0163(3) Uani 1 1 d . . . Si14 Si 0.34635(4) 1.32875(10) 0.25625(7) 0.0230(3) Uani 1 1 d . . . Si15 Si 0.12241(3) 0.23870(9) 0.37023(6) 0.0121(3) Uani 1 1 d . . . Si16 Si 0.14349(3) 0.17418(9) 0.27027(7) 0.0140(3) Uani 1 1 d . . . Si17 Si 0.16240(3) 0.19132(9) 0.45630(7) 0.0150(3) Uani 1 1 d . . . Si18 Si 0.06388(3) 0.19502(9) 0.38474(6) 0.0124(3) Uani 1 1 d . . . Si19 Si 0.04941(4) 0.04667(9) 0.35906(7) 0.0175(3) Uani 1 1 d . . . Si20 Si 0.04892(4) 0.21472(9) 0.49889(7) 0.0160(3) Uani 1 1 d . . . Si21 Si 0.02610(4) 0.29005(9) 0.32296(7) 0.0163(3) Uani 1 1 d . . . Si22 Si 0.13896(3) 0.55164(9) 0.39158(7) 0.0145(3) Uani 1 1 d . . . Si23 Si 0.17709(4) 0.55746(10) 0.48767(7) 0.0198(3) Uani 1 1 d . . . Si24 Si 0.08929(4) 0.62968(9) 0.42653(7) 0.0190(3) Uani 1 1 d . . . Si25 Si 0.16355(4) 0.61083(9) 0.29201(7) 0.0147(3) Uani 1 1 d . . . Si26 Si 0.13305(4) 0.55308(10) 0.19674(7) 0.0205(3) Uani 1 1 d . . . Si27 Si 0.22125(4) 0.56207(10) 0.27872(7) 0.0207(3) Uani 1 1 d . . . Si28 Si 0.16441(4) 0.76578(9) 0.28052(7) 0.0206(3) Uani 1 1 d . . . C1 C 0.33467(15) 0.6911(4) 0.1953(3) 0.0293(14) Uani 1 1 d . . . H1A H 0.3133 0.6578 0.2029 0.044 Uiso 1 1 calc R . . H1B H 0.3349 0.7445 0.2232 0.044 Uiso 1 1 calc R . . H1C H 0.3548 0.6544 0.2076 0.044 Uiso 1 1 calc R . . C2 C 0.34035(16) 0.6163(4) 0.0550(3) 0.0326(14) Uani 1 1 d . . . H2A H 0.3621 0.5867 0.0687 0.049 Uiso 1 1 calc R . . H2B H 0.3404 0.6289 0.0064 0.049 Uiso 1 1 calc R . . H2C H 0.3206 0.5780 0.0649 0.049 Uiso 1 1 calc R . . C3 C 0.29277(14) 0.7712(4) 0.0793(3) 0.0332(14) Uani 1 1 d . . . H3A H 0.2744 0.7293 0.0905 0.050 Uiso 1 1 calc R . . H3B H 0.2917 0.7833 0.0305 0.050 Uiso 1 1 calc R . . H3C H 0.2895 0.8263 0.1043 0.050 Uiso 1 1 calc R . . C4 C 0.35373(16) 0.7819(4) -0.0900(3) 0.0304(14) Uani 1 1 d . . . H4A H 0.3474 0.8058 -0.1348 0.046 Uiso 1 1 calc R . . H4B H 0.3338 0.7504 -0.0719 0.046 Uiso 1 1 calc R . . H4C H 0.3733 0.7412 -0.0939 0.046 Uiso 1 1 calc R . . C5 C 0.40123(16) 0.9399(4) -0.0727(3) 0.0321(14) Uani 1 1 d . . . H5A H 0.3940 0.9536 -0.1195 0.048 Uiso 1 1 calc R . . H5B H 0.4227 0.9053 -0.0727 0.048 Uiso 1 1 calc R . . H5C H 0.4052 0.9950 -0.0477 0.048 Uiso 1 1 calc R . . C6 C 0.32818(15) 0.9517(4) -0.0271(3) 0.0300(14) Uani 1 1 d . . . H6A H 0.3345 1.0029 0.0010 0.045 Uiso 1 1 calc R . . H6B H 0.3086 0.9207 -0.0071 0.045 Uiso 1 1 calc R . . H6C H 0.3215 0.9714 -0.0729 0.045 Uiso 1 1 calc R . . C7 C 0.42143(16) 0.7242(4) 0.2716(3) 0.0320(14) Uani 1 1 d . . . H7A H 0.4205 0.6780 0.3062 0.048 Uiso 1 1 calc R . . H7B H 0.3978 0.7414 0.2578 0.048 Uiso 1 1 calc R . . H7C H 0.4339 0.7756 0.2901 0.048 Uiso 1 1 calc R . . C8 C 0.49128(14) 0.6750(4) 0.2242(3) 0.0340(15) Uani 1 1 d . . . H8A H 0.5004 0.7347 0.2316 0.051 Uiso 1 1 calc R . . H8B H 0.5044 0.6457 0.1889 0.051 Uiso 1 1 calc R . . H8C H 0.4935 0.6412 0.2665 0.051 Uiso 1 1 calc R . . C9 C 0.42911(16) 0.5654(4) 0.1798(3) 0.0314(14) Uani 1 1 d . . . H9A H 0.4300 0.5315 0.2221 0.047 Uiso 1 1 calc R . . H9B H 0.4442 0.5376 0.1469 0.047 Uiso 1 1 calc R . . H9C H 0.4052 0.5667 0.1616 0.047 Uiso 1 1 calc R . . C10 C 0.50207(15) 0.6280(4) 0.0412(3) 0.0308(14) Uani 1 1 d . . . H10A H 0.4974 0.5871 0.0783 0.046 Uiso 1 1 calc R . . H10B H 0.5188 0.6727 0.0571 0.046 Uiso 1 1 calc R . . H10C H 0.5117 0.5954 0.0033 0.046 Uiso 1 1 calc R . . C11 C 0.42980(16) 0.5934(4) -0.0147(3) 0.0345(15) Uani 1 1 d . . . H11A H 0.4076 0.6193 -0.0296 0.052 Uiso 1 1 calc R . . H11B H 0.4261 0.5535 0.0234 0.052 Uiso 1 1 calc R . . H11C H 0.4397 0.5604 -0.0522 0.052 Uiso 1 1 calc R . . C12 C 0.47078(17) 0.7513(4) -0.0641(3) 0.0400(16) Uani 1 1 d . . . H12A H 0.4832 0.7148 -0.0964 0.060 Uiso 1 1 calc R . . H12B H 0.4854 0.8015 -0.0503 0.060 Uiso 1 1 calc R . . H12C H 0.4492 0.7730 -0.0855 0.060 Uiso 1 1 calc R . . C13 C 0.52238(14) 0.8609(4) 0.1025(3) 0.0340(15) Uani 1 1 d . . . H13A H 0.5245 0.8427 0.0552 0.051 Uiso 1 1 calc R . . H13B H 0.5296 0.8123 0.1325 0.051 Uiso 1 1 calc R . . H13C H 0.5373 0.9122 0.1115 0.051 Uiso 1 1 calc R . . C14 C 0.47380(18) 0.9302(4) 0.2086(3) 0.0468(18) Uani 1 1 d . . . H14A H 0.4880 0.9834 0.2146 0.070 Uiso 1 1 calc R . . H14B H 0.4825 0.8839 0.2393 0.070 Uiso 1 1 calc R . . H14C H 0.4497 0.9438 0.2189 0.070 Uiso 1 1 calc R . . C15 C 0.46411(15) 0.9862(4) 0.0624(3) 0.0355(15) Uani 1 1 d . . . H15A H 0.4803 1.0351 0.0712 0.053 Uiso 1 1 calc R . . H15B H 0.4404 1.0053 0.0716 0.053 Uiso 1 1 calc R . . H15C H 0.4654 0.9681 0.0149 0.053 Uiso 1 1 calc R . . C16 C 0.38335(16) 0.9229(4) 0.3102(3) 0.0331(14) Uani 1 1 d . . . H16A H 0.3978 0.9059 0.3498 0.050 Uiso 1 1 calc R . . H16B H 0.3953 0.9072 0.2687 0.050 Uiso 1 1 calc R . . H16C H 0.3611 0.8919 0.3113 0.050 Uiso 1 1 calc R . . C17 C 0.35395(19) 1.0718(5) 0.3920(3) 0.055(2) Uani 1 1 d . . . H17A H 0.3317 1.0405 0.3935 0.082 Uiso 1 1 calc R . . H17B H 0.3499 1.1355 0.3943 0.082 Uiso 1 1 calc R . . H17C H 0.3688 1.0535 0.4306 0.082 Uiso 1 1 calc R . . C18 C 0.41997(15) 1.0967(4) 0.3174(3) 0.0368(15) Uani 1 1 d . . . H18A H 0.4178 1.1609 0.3129 0.055 Uiso 1 1 calc R . . H18B H 0.4341 1.0737 0.2809 0.055 Uiso 1 1 calc R . . H18C H 0.4311 1.0824 0.3613 0.055 Uiso 1 1 calc R . . C19 C 0.28897(15) 0.9087(4) 0.2738(3) 0.0348(15) Uani 1 1 d . . . H19A H 0.3017 0.9099 0.3175 0.052 Uiso 1 1 calc R . . H19B H 0.3010 0.8697 0.2426 0.052 Uiso 1 1 calc R . . H19C H 0.2654 0.8867 0.2803 0.052 Uiso 1 1 calc R . . C20 C 0.25678(15) 1.0154(4) 0.1614(3) 0.0313(14) Uani 1 1 d . . . H20A H 0.2352 0.9863 0.1740 0.047 Uiso 1 1 calc R . . H20B H 0.2679 0.9810 0.1260 0.047 Uiso 1 1 calc R . . H20C H 0.2516 1.0748 0.1444 0.047 Uiso 1 1 calc R . . C21 C 0.26480(15) 1.0928(4) 0.3017(3) 0.0334(14) Uani 1 1 d . . . H21A H 0.2422 1.0669 0.3117 0.050 Uiso 1 1 calc R . . H21B H 0.2614 1.1525 0.2835 0.050 Uiso 1 1 calc R . . H21C H 0.2792 1.0956 0.3433 0.050 Uiso 1 1 calc R . . C22 C 0.38992(14) 1.1773(4) 0.0223(3) 0.0310(14) Uani 1 1 d . . . H22A H 0.3708 1.2036 -0.0044 0.047 Uiso 1 1 calc R . . H22B H 0.3848 1.1151 0.0312 0.047 Uiso 1 1 calc R . . H22C H 0.4114 1.1816 -0.0029 0.047 Uiso 1 1 calc R . . C23 C 0.43482(14) 1.1929(4) 0.1504(3) 0.0359(15) Uani 1 1 d . . . H23A H 0.4548 1.1971 0.1210 0.054 Uiso 1 1 calc R . . H23B H 0.4309 1.1310 0.1623 0.054 Uiso 1 1 calc R . . H23C H 0.4394 1.2272 0.1918 0.054 Uiso 1 1 calc R . . C24 C 0.40429(16) 1.3563(4) 0.0860(3) 0.0374(15) Uani 1 1 d . . . H24A H 0.4092 1.3881 0.1285 0.056 Uiso 1 1 calc R . . H24B H 0.3839 1.3825 0.0629 0.056 Uiso 1 1 calc R . . H24C H 0.4244 1.3606 0.0568 0.056 Uiso 1 1 calc R . . C25 C 0.30736(14) 1.3595(4) 0.0466(3) 0.0293(14) Uani 1 1 d . . . H25A H 0.3274 1.3504 0.0180 0.044 Uiso 1 1 calc R . . H25B H 0.3123 1.4079 0.0784 0.044 Uiso 1 1 calc R . . H25C H 0.2870 1.3744 0.0180 0.044 Uiso 1 1 calc R . . C26 C 0.25798(13) 1.2772(4) 0.1421(3) 0.0264(13) Uani 1 1 d . . . H26A H 0.2387 1.2888 0.1098 0.040 Uiso 1 1 calc R . . H26B H 0.2614 1.3284 0.1719 0.040 Uiso 1 1 calc R . . H26C H 0.2526 1.2253 0.1694 0.040 Uiso 1 1 calc R . . C27 C 0.29080(14) 1.1678(4) 0.0304(3) 0.0240(12) Uani 1 1 d . . . H27A H 0.2879 1.1111 0.0534 0.036 Uiso 1 1 calc R . . H27B H 0.3107 1.1644 0.0006 0.036 Uiso 1 1 calc R . . H27C H 0.2697 1.1815 0.0034 0.036 Uiso 1 1 calc R . . C28 C 0.33384(16) 1.4397(3) 0.2209(3) 0.0325(14) Uani 1 1 d . . . H28A H 0.3343 1.4835 0.2575 0.049 Uiso 1 1 calc R . . H28B H 0.3104 1.4366 0.2006 0.049 Uiso 1 1 calc R . . H28C H 0.3503 1.4570 0.1863 0.049 Uiso 1 1 calc R . . C29 C 0.31473(19) 1.3036(4) 0.3242(3) 0.0454(18) Uani 1 1 d . . . H29A H 0.3153 1.3512 0.3578 0.068 Uiso 1 1 calc R . . H29B H 0.3211 1.2478 0.3462 0.068 Uiso 1 1 calc R . . H29C H 0.2913 1.2987 0.3039 0.068 Uiso 1 1 calc R . . C30 C 0.39069(17) 1.3415(4) 0.2971(4) 0.0470(19) Uani 1 1 d . . . H30A H 0.4077 1.3528 0.2621 0.070 Uiso 1 1 calc R . . H30B H 0.3970 1.2873 0.3215 0.070 Uiso 1 1 calc R . . H30C H 0.3906 1.3911 0.3289 0.070 Uiso 1 1 calc R . . C31 C 0.11204(14) 0.1824(4) 0.1966(2) 0.0238(12) Uani 1 1 d . . . H31A H 0.1091 0.2445 0.1838 0.036 Uiso 1 1 calc R . . H31B H 0.0896 0.1578 0.2092 0.036 Uiso 1 1 calc R . . H31C H 0.1210 0.1493 0.1582 0.036 Uiso 1 1 calc R . . C32 C 0.15301(14) 0.0539(3) 0.2843(3) 0.0226(12) Uani 1 1 d . . . H32A H 0.1323 0.0245 0.3010 0.034 Uiso 1 1 calc R . . H32B H 0.1721 0.0477 0.3177 0.034 Uiso 1 1 calc R . . H32C H 0.1596 0.0269 0.2414 0.034 Uiso 1 1 calc R . . C33 C 0.18506(13) 0.2233(3) 0.2415(3) 0.0219(12) Uani 1 1 d . . . H33A H 0.1957 0.1838 0.2087 0.033 Uiso 1 1 calc R . . H33B H 0.2010 0.2314 0.2806 0.033 Uiso 1 1 calc R . . H33C H 0.1803 0.2806 0.2201 0.033 Uiso 1 1 calc R . . C34 C 0.16047(14) 0.0706(3) 0.4775(3) 0.0235(12) Uani 1 1 d . . . H34A H 0.1764 0.0581 0.5158 0.035 Uiso 1 1 calc R . . H34B H 0.1672 0.0359 0.4381 0.035 Uiso 1 1 calc R . . H34C H 0.1368 0.0549 0.4895 0.035 Uiso 1 1 calc R . . C35 C 0.20778(12) 0.2124(4) 0.4277(3) 0.0223(12) Uani 1 1 d . . . H35A H 0.2242 0.2041 0.4659 0.033 Uiso 1 1 calc R . . H35B H 0.2095 0.2731 0.4109 0.033 Uiso 1 1 calc R . . H35C H 0.2133 0.1711 0.3913 0.033 Uiso 1 1 calc R . . C36 C 0.15770(13) 0.2553(4) 0.5372(2) 0.0214(12) Uani 1 1 d . . . H36A H 0.1345 0.2457 0.5547 0.032 Uiso 1 1 calc R . . H36B H 0.1610 0.3183 0.5282 0.032 Uiso 1 1 calc R . . H36C H 0.1752 0.2353 0.5707 0.032 Uiso 1 1 calc R . . C37 C 0.00486(14) 0.0234(4) 0.3904(3) 0.0249(13) Uani 1 1 d . . . H37A H -0.0017 -0.0373 0.3788 0.037 Uiso 1 1 calc R . . H37B H -0.0118 0.0645 0.3691 0.037 Uiso 1 1 calc R . . H37C H 0.0048 0.0308 0.4397 0.037 Uiso 1 1 calc R . . C38 C 0.07875(14) -0.0359(3) 0.4022(3) 0.0245(12) Uani 1 1 d . . . H38A H 0.0772 -0.0297 0.4514 0.037 Uiso 1 1 calc R . . H38B H 0.1027 -0.0255 0.3890 0.037 Uiso 1 1 calc R . . H38C H 0.0717 -0.0956 0.3887 0.037 Uiso 1 1 calc R . . C39 C 0.04765(16) 0.0213(4) 0.2654(3) 0.0308(14) Uani 1 1 d . . . H39A H 0.0376 -0.0374 0.2581 0.046 Uiso 1 1 calc R . . H39B H 0.0712 0.0226 0.2479 0.046 Uiso 1 1 calc R . . H39C H 0.0333 0.0654 0.2417 0.046 Uiso 1 1 calc R . . C40 C 0.06852(13) 0.1258(3) 0.5535(2) 0.0201(12) Uani 1 1 d . . . H40A H 0.0935 0.1218 0.5455 0.030 Uiso 1 1 calc R . . H40B H 0.0574 0.0693 0.5423 0.030 Uiso 1 1 calc R . . H40C H 0.0649 0.1398 0.6013 0.030 Uiso 1 1 calc R . . C41 C 0.06363(15) 0.3253(3) 0.5311(3) 0.0270(13) Uani 1 1 d . . . H41A H 0.0590 0.3300 0.5795 0.040 Uiso 1 1 calc R . . H41B H 0.0510 0.3719 0.5063 0.040 Uiso 1 1 calc R . . H41C H 0.0886 0.3319 0.5242 0.040 Uiso 1 1 calc R . . C42 C 0.00089(13) 0.2114(4) 0.5115(3) 0.0268(13) Uani 1 1 d . . . H42A H -0.0088 0.1577 0.4908 0.040 Uiso 1 1 calc R . . H42B H -0.0100 0.2632 0.4901 0.040 Uiso 1 1 calc R . . H42C H -0.0036 0.2115 0.5601 0.040 Uiso 1 1 calc R . . C43 C 0.02590(16) 0.4014(4) 0.3637(3) 0.0333(14) Uani 1 1 d . . . H43A H 0.0498 0.4230 0.3691 0.050 Uiso 1 1 calc R . . H43B H 0.0154 0.3972 0.4082 0.050 Uiso 1 1 calc R . . H43C H 0.0124 0.4425 0.3351 0.050 Uiso 1 1 calc R . . C44 C 0.03764(17) 0.3066(4) 0.2329(3) 0.0381(16) Uani 1 1 d . . . H44A H 0.0215 0.3489 0.2115 0.057 Uiso 1 1 calc R . . H44B H 0.0361 0.2501 0.2088 0.057 Uiso 1 1 calc R . . H44C H 0.0614 0.3294 0.2309 0.057 Uiso 1 1 calc R . . C45 C -0.01976(15) 0.2490(4) 0.3212(3) 0.0360(15) Uani 1 1 d . . . H45A H -0.0349 0.2929 0.2991 0.054 Uiso 1 1 calc R . . H45B H -0.0272 0.2392 0.3677 0.054 Uiso 1 1 calc R . . H45C H -0.0212 0.1934 0.2959 0.054 Uiso 1 1 calc R . . C46 C 0.15254(15) 0.5284(4) 0.5664(3) 0.0285(13) Uani 1 1 d . . . H46A H 0.1691 0.5192 0.6044 0.043 Uiso 1 1 calc R . . H46B H 0.1391 0.4744 0.5583 0.043 Uiso 1 1 calc R . . H46C H 0.1368 0.5768 0.5773 0.043 Uiso 1 1 calc R . . C47 C 0.19747(15) 0.6682(4) 0.5034(3) 0.0293(13) Uani 1 1 d . . . H47A H 0.2133 0.6647 0.5430 0.044 Uiso 1 1 calc R . . H47B H 0.1793 0.7117 0.5119 0.044 Uiso 1 1 calc R . . H47C H 0.2104 0.6860 0.4636 0.044 Uiso 1 1 calc R . . C48 C 0.21367(15) 0.4759(4) 0.4825(3) 0.0296(14) Uani 1 1 d . . . H48A H 0.2293 0.4939 0.4467 0.044 Uiso 1 1 calc R . . H48B H 0.2042 0.4173 0.4720 0.044 Uiso 1 1 calc R . . H48C H 0.2265 0.4740 0.5260 0.044 Uiso 1 1 calc R . . C49 C 0.05691(14) 0.6538(4) 0.3562(3) 0.0285(13) Uani 1 1 d . . . H49A H 0.0382 0.6904 0.3736 0.043 Uiso 1 1 calc R . . H49B H 0.0472 0.5983 0.3386 0.043 Uiso 1 1 calc R . . H49C H 0.0684 0.6853 0.3198 0.043 Uiso 1 1 calc R . . C50 C 0.06555(15) 0.5672(4) 0.4929(3) 0.0306(14) Uani 1 1 d . . . H50A H 0.0821 0.5465 0.5280 0.046 Uiso 1 1 calc R . . H50B H 0.0537 0.5165 0.4721 0.046 Uiso 1 1 calc R . . H50C H 0.0484 0.6060 0.5135 0.046 Uiso 1 1 calc R . . C51 C 0.10226(14) 0.7366(3) 0.4671(3) 0.0258(13) Uani 1 1 d . . . H51A H 0.0815 0.7672 0.4825 0.039 Uiso 1 1 calc R . . H51B H 0.1140 0.7735 0.4340 0.039 Uiso 1 1 calc R . . H51C H 0.1180 0.7251 0.5059 0.039 Uiso 1 1 calc R . . C52 C 0.08466(14) 0.5481(4) 0.2082(3) 0.0380(16) Uani 1 1 d . . . H52A H 0.0755 0.6081 0.2119 0.057 Uiso 1 1 calc R . . H52B H 0.0798 0.5150 0.2495 0.057 Uiso 1 1 calc R . . H52C H 0.0736 0.5186 0.1690 0.057 Uiso 1 1 calc R . . C53 C 0.14685(14) 0.4359(3) 0.1832(3) 0.0232(12) Uani 1 1 d . . . H53A H 0.1334 0.4106 0.1451 0.035 Uiso 1 1 calc R . . H53B H 0.1427 0.4015 0.2243 0.035 Uiso 1 1 calc R . . H53C H 0.1716 0.4343 0.1733 0.035 Uiso 1 1 calc R . . C54 C 0.14070(19) 0.6167(4) 0.1181(3) 0.0407(17) Uani 1 1 d . . . H54A H 0.1656 0.6178 0.1095 0.061 Uiso 1 1 calc R . . H54B H 0.1323 0.6772 0.1235 0.061 Uiso 1 1 calc R . . H54C H 0.1283 0.5887 0.0799 0.061 Uiso 1 1 calc R . . C55 C 0.22592(14) 0.4422(4) 0.3016(3) 0.0300(14) Uani 1 1 d . . . H55A H 0.2502 0.4295 0.3137 0.045 Uiso 1 1 calc R . . H55B H 0.2186 0.4058 0.2628 0.045 Uiso 1 1 calc R . . H55C H 0.2114 0.4289 0.3402 0.045 Uiso 1 1 calc R . . C56 C 0.23434(15) 0.5737(4) 0.1877(3) 0.0342(15) Uani 1 1 d . . . H56A H 0.2585 0.5545 0.1835 0.051 Uiso 1 1 calc R . . H56B H 0.2322 0.6356 0.1738 0.051 Uiso 1 1 calc R . . H56C H 0.2192 0.5371 0.1587 0.051 Uiso 1 1 calc R . . C57 C 0.25355(14) 0.6281(4) 0.3316(3) 0.0319(14) Uani 1 1 d . . . H57A H 0.2484 0.6215 0.3797 0.048 Uiso 1 1 calc R . . H57B H 0.2520 0.6905 0.3189 0.048 Uiso 1 1 calc R . . H57C H 0.2771 0.6065 0.3238 0.048 Uiso 1 1 calc R . . C58 C 0.19274(16) 0.7972(4) 0.2085(3) 0.0345(15) Uani 1 1 d . . . H58A H 0.1849 0.7661 0.1674 0.052 Uiso 1 1 calc R . . H58B H 0.2168 0.7808 0.2197 0.052 Uiso 1 1 calc R . . H58C H 0.1913 0.8610 0.2010 0.052 Uiso 1 1 calc R . . C59 C 0.18299(16) 0.8238(4) 0.3574(3) 0.0308(14) Uani 1 1 d . . . H59A H 0.1818 0.8878 0.3503 0.046 Uiso 1 1 calc R . . H59B H 0.2073 0.8062 0.3648 0.046 Uiso 1 1 calc R . . H59C H 0.1696 0.8078 0.3970 0.046 Uiso 1 1 calc R . . C60 C 0.11991(15) 0.8092(4) 0.2599(3) 0.0317(14) Uani 1 1 d . . . H60A H 0.1215 0.8710 0.2457 0.048 Uiso 1 1 calc R . . H60B H 0.1056 0.8051 0.3001 0.048 Uiso 1 1 calc R . . H60C H 0.1093 0.7742 0.2231 0.048 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 Zn1 0.0137(3) 0.0128(3) 0.0116(3) -0.0016(2) 0.0004(2) 0.0003(2) Zn2 0.0138(3) 0.0107(3) 0.0119(3) -0.0003(2) -0.0006(2) 0.0004(2) Si1 0.0156(7) 0.0129(7) 0.0127(7) -0.0023(5) 0.0002(5) -0.0003(6) Si2 0.0173(8) 0.0187(8) 0.0272(8) 0.0010(6) 0.0003(6) -0.0024(6) Si3 0.0271(8) 0.0179(8) 0.0139(7) -0.0027(6) -0.0017(6) 0.0058(6) Si4 0.0155(7) 0.0140(7) 0.0136(7) -0.0006(6) -0.0003(5) 0.0003(6) Si5 0.0228(8) 0.0183(8) 0.0186(8) 0.0019(6) -0.0052(6) 0.0017(6) Si6 0.0222(8) 0.0236(8) 0.0183(8) -0.0042(6) -0.0011(6) 0.0070(6) Si7 0.0191(8) 0.0178(8) 0.0307(9) -0.0020(7) 0.0022(6) -0.0037(6) Si8 0.0140(7) 0.0129(7) 0.0113(7) -0.0009(5) 0.0002(5) 0.0002(5) Si9 0.0228(8) 0.0210(8) 0.0141(7) 0.0002(6) -0.0043(6) 0.0036(6) Si10 0.0150(7) 0.0188(8) 0.0205(8) 0.0041(6) 0.0012(6) -0.0011(6) Si11 0.0140(7) 0.0122(7) 0.0137(7) 0.0005(5) -0.0006(5) 0.0005(5) Si12 0.0144(7) 0.0224(8) 0.0203(8) -0.0013(6) 0.0028(6) -0.0018(6) Si13 0.0146(7) 0.0177(7) 0.0168(7) 0.0040(6) 0.0017(6) 0.0003(6) Si14 0.0329(9) 0.0148(8) 0.0212(8) -0.0035(6) -0.0026(7) 0.0039(7) Si15 0.0125(7) 0.0129(7) 0.0109(7) 0.0000(5) -0.0005(5) 0.0000(5) Si16 0.0155(7) 0.0147(7) 0.0117(7) 0.0012(6) 0.0023(5) -0.0008(6) Si17 0.0155(7) 0.0168(7) 0.0125(7) 0.0001(6) -0.0011(6) 0.0005(6) Si18 0.0124(7) 0.0134(7) 0.0114(7) 0.0012(5) -0.0006(5) -0.0009(5) Si19 0.0199(8) 0.0159(7) 0.0167(7) 0.0011(6) -0.0019(6) -0.0053(6) Si20 0.0174(7) 0.0193(8) 0.0113(7) 0.0016(6) -0.0003(6) 0.0027(6) Si21 0.0176(7) 0.0157(7) 0.0153(7) 0.0035(6) -0.0047(6) 0.0003(6) Si22 0.0167(7) 0.0116(7) 0.0151(7) -0.0011(6) -0.0032(6) 0.0014(6) Si23 0.0260(8) 0.0188(8) 0.0143(7) -0.0010(6) -0.0067(6) 0.0019(6) Si24 0.0212(8) 0.0139(7) 0.0218(8) -0.0019(6) 0.0009(6) 0.0030(6) Si25 0.0168(7) 0.0116(7) 0.0153(7) 0.0002(6) -0.0031(6) 0.0004(6) Si26 0.0256(8) 0.0187(8) 0.0167(7) -0.0040(6) -0.0087(6) 0.0068(6) Si27 0.0172(8) 0.0215(8) 0.0232(8) 0.0010(6) 0.0001(6) 0.0014(6) Si28 0.0272(8) 0.0111(7) 0.0234(8) 0.0019(6) -0.0039(6) -0.0016(6) C1 0.026(3) 0.024(3) 0.038(4) 0.008(3) 0.005(3) -0.001(2) C2 0.036(4) 0.018(3) 0.044(4) -0.004(3) 0.002(3) -0.004(3) C3 0.016(3) 0.035(4) 0.048(4) 0.008(3) -0.003(3) 0.000(3) C4 0.045(4) 0.028(3) 0.018(3) -0.005(2) -0.001(3) 0.005(3) C5 0.050(4) 0.026(3) 0.022(3) 0.000(2) 0.012(3) 0.003(3) C6 0.031(3) 0.029(3) 0.030(3) 0.001(3) -0.009(3) 0.014(3) C7 0.048(4) 0.031(3) 0.017(3) 0.003(3) 0.001(3) 0.001(3) C8 0.025(3) 0.038(4) 0.039(4) 0.003(3) -0.012(3) 0.003(3) C9 0.044(4) 0.020(3) 0.030(3) 0.007(3) -0.004(3) -0.001(3) C10 0.029(3) 0.028(3) 0.035(3) -0.005(3) -0.002(3) 0.011(3) C11 0.042(4) 0.036(4) 0.025(3) -0.014(3) -0.008(3) 0.008(3) C12 0.052(4) 0.046(4) 0.023(3) -0.007(3) 0.009(3) 0.013(3) C13 0.018(3) 0.037(4) 0.047(4) 0.007(3) 0.000(3) -0.003(3) C14 0.056(5) 0.038(4) 0.046(4) -0.022(3) 0.008(3) -0.017(3) C15 0.025(3) 0.022(3) 0.060(4) 0.013(3) 0.006(3) 0.001(3) C16 0.037(4) 0.023(3) 0.038(4) 0.013(3) -0.009(3) 0.003(3) C17 0.058(5) 0.091(6) 0.015(3) 0.003(3) -0.001(3) 0.031(4) C18 0.033(4) 0.032(4) 0.043(4) 0.003(3) -0.022(3) -0.005(3) C19 0.032(3) 0.028(3) 0.045(4) 0.013(3) 0.004(3) -0.006(3) C20 0.027(3) 0.033(3) 0.033(3) 0.011(3) -0.007(3) -0.012(3) C21 0.027(3) 0.043(4) 0.030(3) -0.003(3) 0.008(3) 0.010(3) C22 0.022(3) 0.048(4) 0.023(3) -0.010(3) 0.006(2) 0.000(3) C23 0.018(3) 0.051(4) 0.038(4) -0.001(3) -0.001(3) 0.002(3) C24 0.042(4) 0.024(3) 0.048(4) -0.003(3) 0.013(3) -0.009(3) C25 0.025(3) 0.030(3) 0.033(3) 0.014(3) -0.002(3) 0.000(3) C26 0.020(3) 0.029(3) 0.030(3) 0.002(3) 0.003(2) 0.005(2) C27 0.023(3) 0.031(3) 0.017(3) -0.006(2) -0.007(2) 0.002(2) C28 0.045(4) 0.015(3) 0.037(4) -0.004(3) 0.000(3) 0.003(3) C29 0.073(5) 0.036(4) 0.028(4) -0.005(3) 0.019(3) 0.010(4) C30 0.052(4) 0.030(4) 0.058(5) -0.024(3) -0.028(4) 0.010(3) C31 0.027(3) 0.030(3) 0.014(3) -0.003(2) 0.001(2) -0.003(2) C32 0.034(3) 0.013(3) 0.022(3) 0.000(2) 0.008(2) 0.000(2) C33 0.019(3) 0.023(3) 0.024(3) 0.004(2) 0.004(2) 0.001(2) C34 0.032(3) 0.024(3) 0.014(3) 0.003(2) -0.006(2) 0.005(2) C35 0.014(3) 0.033(3) 0.020(3) -0.005(2) -0.001(2) 0.004(2) C36 0.021(3) 0.031(3) 0.012(3) -0.001(2) -0.004(2) 0.003(2) C37 0.029(3) 0.019(3) 0.026(3) 0.006(2) -0.001(2) -0.007(2) C38 0.031(3) 0.020(3) 0.022(3) -0.002(2) 0.002(2) -0.001(2) C39 0.040(4) 0.031(3) 0.021(3) -0.005(3) -0.005(3) -0.017(3) C40 0.022(3) 0.024(3) 0.014(3) 0.004(2) -0.003(2) 0.002(2) C41 0.039(3) 0.024(3) 0.018(3) -0.003(2) -0.009(2) 0.005(3) C42 0.020(3) 0.037(3) 0.024(3) 0.003(3) 0.008(2) 0.012(3) C43 0.034(3) 0.026(3) 0.040(4) 0.007(3) -0.009(3) 0.003(3) C44 0.045(4) 0.046(4) 0.024(3) 0.009(3) 0.000(3) 0.017(3) C45 0.027(3) 0.034(4) 0.047(4) 0.011(3) -0.008(3) -0.003(3) C46 0.040(4) 0.031(3) 0.015(3) 0.000(2) -0.001(2) -0.003(3) C47 0.032(3) 0.030(3) 0.025(3) -0.004(3) -0.009(3) -0.005(3) C48 0.035(3) 0.032(3) 0.021(3) 0.003(3) -0.015(3) 0.009(3) C49 0.022(3) 0.030(3) 0.033(3) -0.006(3) -0.002(3) 0.011(3) C50 0.032(3) 0.022(3) 0.038(4) 0.005(3) 0.009(3) 0.003(3) C51 0.031(3) 0.016(3) 0.030(3) -0.002(2) -0.002(3) 0.002(2) C52 0.027(3) 0.042(4) 0.044(4) -0.021(3) -0.020(3) 0.010(3) C53 0.029(3) 0.022(3) 0.018(3) -0.007(2) -0.009(2) 0.001(2) C54 0.072(5) 0.027(3) 0.022(3) 0.001(3) -0.016(3) 0.007(3) C55 0.025(3) 0.030(3) 0.035(3) -0.004(3) -0.002(3) 0.009(3) C56 0.032(3) 0.036(4) 0.035(4) 0.002(3) 0.012(3) -0.001(3) C57 0.021(3) 0.036(4) 0.038(4) -0.004(3) -0.004(3) -0.002(3) C58 0.049(4) 0.022(3) 0.033(3) 0.007(3) 0.005(3) -0.010(3) C59 0.040(4) 0.016(3) 0.036(3) -0.002(3) -0.006(3) -0.002(3) C60 0.035(3) 0.017(3) 0.042(4) -0.002(3) -0.009(3) 0.007(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 Zn1 Si8 2.4028(15) . ? Zn1 Si1 2.4066(15) . ? Zn2 Si22 2.4058(15) . ? Zn2 Si15 2.4060(15) . ? Si1 Si2 2.367(2) . ? Si1 Si3 2.370(2) . ? Si1 Si4 2.3857(19) . ? Si2 C1 1.880(6) . ? Si2 C2 1.881(6) . ? Si2 C3 1.886(5) . ? Si3 C5 1.873(6) . ? Si3 C4 1.878(5) . ? Si3 C6 1.880(5) . ? Si4 Si7 2.357(2) . ? Si4 Si5 2.361(2) . ? Si4 Si6 2.362(2) . ? Si5 C7 1.854(6) . ? Si5 C8 1.872(6) . ? Si5 C9 1.887(6) . ? Si6 C11 1.875(6) . ? Si6 C12 1.880(6) . ? Si6 C10 1.883(5) . ? Si7 C15 1.871(6) . ? Si7 C13 1.877(6) . ? Si7 C14 1.879(6) . ? Si8 Si9 2.364(2) . ? Si8 Si10 2.368(2) . ? Si8 Si11 2.3768(19) . ? Si9 C17 1.854(6) . ? Si9 C16 1.874(6) . ? Si9 C18 1.882(6) . ? Si10 C21 1.871(6) . ? Si10 C19 1.876(6) . ? Si10 C20 1.876(6) . ? Si11 Si12 2.352(2) . ? Si11 Si13 2.361(2) . ? Si11 Si14 2.365(2) . ? Si12 C24 1.869(6) . ? Si12 C23 1.870(6) . ? Si12 C22 1.879(5) . ? Si13 C25 1.865(5) . ? Si13 C27 1.869(5) . ? Si13 C26 1.872(5) . ? Si14 C29 1.876(6) . ? Si14 C30 1.878(6) . ? Si14 C28 1.879(6) . ? Si15 Si16 2.3670(19) . ? Si15 Si17 2.373(2) . ? Si15 Si18 2.3750(19) . ? Si16 C33 1.869(5) . ? Si16 C31 1.870(5) . ? Si16 C32 1.878(5) . ? Si17 C34 1.879(5) . ? Si17 C35 1.880(5) . ? Si17 C36 1.881(5) . ? Si18 Si20 2.3608(19) . ? Si18 Si21 2.3624(19) . ? Si18 Si19 2.3682(19) . ? Si19 C37 1.874(5) . ? Si19 C38 1.875(5) . ? Si19 C39 1.887(5) . ? Si20 C40 1.871(5) . ? Si20 C41 1.875(5) . ? Si20 C42 1.875(5) . ? Si21 C44 1.862(6) . ? Si21 C43 1.870(6) . ? Si21 C45 1.873(6) . ? Si22 Si23 2.368(2) . ? Si22 Si24 2.369(2) . ? Si22 Si25 2.382(2) . ? Si23 C47 1.875(6) . ? Si23 C48 1.879(6) . ? Si23 C46 1.895(5) . ? Si24 C51 1.868(5) . ? Si24 C49 1.876(5) . ? Si24 C50 1.876(6) . ? Si25 Si26 2.358(2) . ? Si25 Si28 2.360(2) . ? Si25 Si27 2.364(2) . ? Si26 C54 1.858(6) . ? Si26 C53 1.875(5) . ? Si26 C52 1.886(6) . ? Si27 C55 1.879(6) . ? Si27 C56 1.888(6) . ? Si27 C57 1.888(6) . ? Si28 C60 1.870(6) . ? Si28 C58 1.878(6) . ? Si28 C59 1.878(6) . ? 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 Si8 Zn1 Si1 172.23(5) . . ? Si22 Zn2 Si15 172.96(5) . . ? Si2 Si1 Si3 103.78(7) . . ? Si2 Si1 Si4 113.65(7) . . ? Si3 Si1 Si4 116.35(8) . . ? Si2 Si1 Zn1 104.77(7) . . ? Si3 Si1 Zn1 100.02(6) . . ? Si4 Si1 Zn1 116.45(7) . . ? C1 Si2 C2 106.1(3) . . ? C1 Si2 C3 106.6(3) . . ? C2 Si2 C3 106.9(3) . . ? C1 Si2 Si1 113.63(19) . . ? C2 Si2 Si1 113.9(2) . . ? C3 Si2 Si1 109.26(19) . . ? C5 Si3 C4 107.6(3) . . ? C5 Si3 C6 105.4(3) . . ? C4 Si3 C6 107.6(3) . . ? C5 Si3 Si1 114.9(2) . . ? C4 Si3 Si1 112.98(19) . . ? C6 Si3 Si1 107.92(19) . . ? Si7 Si4 Si5 105.14(8) . . ? Si7 Si4 Si6 107.86(8) . . ? Si5 Si4 Si6 103.60(7) . . ? Si7 Si4 Si1 109.17(7) . . ? Si5 Si4 Si1 114.21(8) . . ? Si6 Si4 Si1 116.12(7) . . ? C7 Si5 C8 105.6(3) . . ? C7 Si5 C9 108.3(3) . . ? C8 Si5 C9 107.1(3) . . ? C7 Si5 Si4 113.82(19) . . ? C8 Si5 Si4 110.2(2) . . ? C9 Si5 Si4 111.47(19) . . ? C11 Si6 C12 108.2(3) . . ? C11 Si6 C10 106.6(3) . . ? C12 Si6 C10 106.8(3) . . ? C11 Si6 Si4 112.1(2) . . ? C12 Si6 Si4 111.6(2) . . ? C10 Si6 Si4 111.16(19) . . ? C15 Si7 C13 107.8(3) . . ? C15 Si7 C14 107.4(3) . . ? C13 Si7 C14 107.8(3) . . ? C15 Si7 Si4 110.9(2) . . ? C13 Si7 Si4 112.3(2) . . ? C14 Si7 Si4 110.4(2) . . ? Si9 Si8 Si10 102.74(7) . . ? Si9 Si8 Si11 116.04(7) . . ? Si10 Si8 Si11 115.30(7) . . ? Si9 Si8 Zn1 98.32(6) . . ? Si10 Si8 Zn1 102.67(6) . . ? Si11 Si8 Zn1 119.07(7) . . ? C17 Si9 C16 107.9(3) . . ? C17 Si9 C18 106.8(3) . . ? C16 Si9 C18 105.5(3) . . ? C17 Si9 Si8 115.9(2) . . ? C16 Si9 Si8 104.49(19) . . ? C18 Si9 Si8 115.6(2) . . ? C21 Si10 C19 106.3(3) . . ? C21 Si10 C20 107.2(3) . . ? C19 Si10 C20 105.5(3) . . ? C21 Si10 Si8 113.6(2) . . ? C19 Si10 Si8 110.8(2) . . ? C20 Si10 Si8 112.97(19) . . ? Si12 Si11 Si13 104.97(7) . . ? Si12 Si11 Si14 108.76(8) . . ? Si13 Si11 Si14 106.89(7) . . ? Si12 Si11 Si8 109.25(7) . . ? Si13 Si11 Si8 113.07(7) . . ? Si14 Si11 Si8 113.47(7) . . ? C24 Si12 C23 107.1(3) . . ? C24 Si12 C22 108.2(3) . . ? C23 Si12 C22 108.0(3) . . ? C24 Si12 Si11 111.7(2) . . ? C23 Si12 Si11 111.5(2) . . ? C22 Si12 Si11 110.19(19) . . ? C25 Si13 C27 106.4(3) . . ? C25 Si13 C26 106.2(3) . . ? C27 Si13 C26 109.9(3) . . ? C25 Si13 Si11 111.36(19) . . ? C27 Si13 Si11 111.56(18) . . ? C26 Si13 Si11 111.18(18) . . ? C29 Si14 C30 108.4(3) . . ? C29 Si14 C28 106.4(3) . . ? C30 Si14 C28 106.7(3) . . ? C29 Si14 Si11 112.3(2) . . ? C30 Si14 Si11 112.1(2) . . ? C28 Si14 Si11 110.59(19) . . ? Si16 Si15 Si17 103.94(7) . . ? Si16 Si15 Si18 109.56(7) . . ? Si17 Si15 Si18 115.39(7) . . ? Si16 Si15 Zn2 114.24(6) . . ? Si17 Si15 Zn2 102.38(6) . . ? Si18 Si15 Zn2 111.13(6) . . ? C33 Si16 C31 106.2(2) . . ? C33 Si16 C32 105.4(2) . . ? C31 Si16 C32 107.4(2) . . ? C33 Si16 Si15 113.95(18) . . ? C31 Si16 Si15 112.99(18) . . ? C32 Si16 Si15 110.38(17) . . ? C34 Si17 C35 106.0(2) . . ? C34 Si17 C36 107.9(2) . . ? C35 Si17 C36 106.3(2) . . ? C34 Si17 Si15 115.16(17) . . ? C35 Si17 Si15 108.89(17) . . ? C36 Si17 Si15 112.07(17) . . ? Si20 Si18 Si21 104.62(7) . . ? Si20 Si18 Si19 105.20(7) . . ? Si21 Si18 Si19 109.29(7) . . ? Si20 Si18 Si15 109.76(7) . . ? Si21 Si18 Si15 109.94(7) . . ? Si19 Si18 Si15 117.22(7) . . ? C37 Si19 C38 105.7(2) . . ? C37 Si19 C39 106.1(3) . . ? C38 Si19 C39 108.2(3) . . ? C37 Si19 Si18 108.68(18) . . ? C38 Si19 Si18 113.66(18) . . ? C39 Si19 Si18 113.90(19) . . ? C40 Si20 C41 109.6(2) . . ? C40 Si20 C42 106.7(2) . . ? C41 Si20 C42 105.6(3) . . ? C40 Si20 Si18 110.71(17) . . ? C41 Si20 Si18 110.91(19) . . ? C42 Si20 Si18 113.04(18) . . ? C44 Si21 C43 107.1(3) . . ? C44 Si21 C45 106.1(3) . . ? C43 Si21 C45 107.0(3) . . ? C44 Si21 Si18 114.5(2) . . ? C43 Si21 Si18 109.78(19) . . ? C45 Si21 Si18 111.98(19) . . ? Si23 Si22 Si24 103.66(7) . . ? Si23 Si22 Si25 113.26(7) . . ? Si24 Si22 Si25 113.32(7) . . ? Si23 Si22 Zn2 104.17(6) . . ? Si24 Si22 Zn2 112.96(7) . . ? Si25 Si22 Zn2 109.08(6) . . ? C47 Si23 C48 106.7(3) . . ? C47 Si23 C46 106.7(3) . . ? C48 Si23 C46 106.5(3) . . ? C47 Si23 Si22 114.43(18) . . ? C48 Si23 Si22 112.40(18) . . ? C46 Si23 Si22 109.63(19) . . ? C51 Si24 C49 108.2(3) . . ? C51 Si24 C50 105.5(3) . . ? C49 Si24 C50 106.7(3) . . ? C51 Si24 Si22 110.44(19) . . ? C49 Si24 Si22 114.06(18) . . ? C50 Si24 Si22 111.43(19) . . ? Si26 Si25 Si28 107.50(7) . . ? Si26 Si25 Si27 104.15(8) . . ? Si28 Si25 Si27 106.55(7) . . ? Si26 Si25 Si22 108.52(7) . . ? Si28 Si25 Si22 117.46(7) . . ? Si27 Si25 Si22 111.78(7) . . ? C54 Si26 C53 108.7(3) . . ? C54 Si26 C52 107.5(3) . . ? C53 Si26 C52 105.3(3) . . ? C54 Si26 Si25 112.7(2) . . ? C53 Si26 Si25 109.15(17) . . ? C52 Si26 Si25 113.06(19) . . ? C55 Si27 C56 107.0(3) . . ? C55 Si27 C57 108.8(3) . . ? C56 Si27 C57 106.7(3) . . ? C55 Si27 Si25 111.06(19) . . ? C56 Si27 Si25 110.7(2) . . ? C57 Si27 Si25 112.34(19) . . ? C60 Si28 C58 107.2(3) . . ? C60 Si28 C59 109.7(3) . . ? C58 Si28 C59 106.0(3) . . ? C60 Si28 Si25 110.84(19) . . ? C58 Si28 Si25 109.58(19) . . ? C59 Si28 Si25 113.24(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Si8 Zn1 Si1 Si2 1.7(4) . . . . ? Si8 Zn1 Si1 Si3 109.0(4) . . . . ? Si8 Zn1 Si1 Si4 -124.8(4) . . . . ? Si3 Si1 Si2 C1 -167.0(2) . . . . ? Si4 Si1 Si2 C1 65.6(2) . . . . ? Zn1 Si1 Si2 C1 -62.6(2) . . . . ? Si3 Si1 Si2 C2 71.3(2) . . . . ? Si4 Si1 Si2 C2 -56.0(2) . . . . ? Zn1 Si1 Si2 C2 175.8(2) . . . . ? Si3 Si1 Si2 C3 -48.1(2) . . . . ? Si4 Si1 Si2 C3 -175.4(2) . . . . ? Zn1 Si1 Si2 C3 56.4(2) . . . . ? Si2 Si1 Si3 C5 -167.5(2) . . . . ? Si4 Si1 Si3 C5 -41.9(2) . . . . ? Zn1 Si1 Si3 C5 84.4(2) . . . . ? Si2 Si1 Si3 C4 -43.6(2) . . . . ? Si4 Si1 Si3 C4 82.1(2) . . . . ? Zn1 Si1 Si3 C4 -151.6(2) . . . . ? Si2 Si1 Si3 C6 75.3(2) . . . . ? Si4 Si1 Si3 C6 -159.1(2) . . . . ? Zn1 Si1 Si3 C6 -32.8(2) . . . . ? Si2 Si1 Si4 Si7 -157.00(8) . . . . ? Si3 Si1 Si4 Si7 82.53(9) . . . . ? Zn1 Si1 Si4 Si7 -35.08(9) . . . . ? Si2 Si1 Si4 Si5 -39.65(10) . . . . ? Si3 Si1 Si4 Si5 -160.13(8) . . . . ? Zn1 Si1 Si4 Si5 82.27(9) . . . . ? Si2 Si1 Si4 Si6 80.85(10) . . . . ? Si3 Si1 Si4 Si6 -39.62(11) . . . . ? Zn1 Si1 Si4 Si6 -157.22(7) . . . . ? Si7 Si4 Si5 C7 77.7(2) . . . . ? Si6 Si4 Si5 C7 -169.2(2) . . . . ? Si1 Si4 Si5 C7 -41.9(2) . . . . ? Si7 Si4 Si5 C8 -40.7(2) . . . . ? Si6 Si4 Si5 C8 72.4(2) . . . . ? Si1 Si4 Si5 C8 -160.3(2) . . . . ? Si7 Si4 Si5 C9 -159.5(2) . . . . ? Si6 Si4 Si5 C9 -46.4(2) . . . . ? Si1 Si4 Si5 C9 80.9(2) . . . . ? Si7 Si4 Si6 C11 -173.2(2) . . . . ? Si5 Si4 Si6 C11 75.7(2) . . . . ? Si1 Si4 Si6 C11 -50.3(2) . . . . ? Si7 Si4 Si6 C12 -51.5(2) . . . . ? Si5 Si4 Si6 C12 -162.6(2) . . . . ? Si1 Si4 Si6 C12 71.3(2) . . . . ? Si7 Si4 Si6 C10 67.6(2) . . . . ? Si5 Si4 Si6 C10 -43.5(2) . . . . ? Si1 Si4 Si6 C10 -169.5(2) . . . . ? Si5 Si4 Si7 C15 -161.0(2) . . . . ? Si6 Si4 Si7 C15 88.9(2) . . . . ? Si1 Si4 Si7 C15 -38.1(2) . . . . ? Si5 Si4 Si7 C13 78.3(2) . . . . ? Si6 Si4 Si7 C13 -31.8(2) . . . . ? Si1 Si4 Si7 C13 -158.8(2) . . . . ? Si5 Si4 Si7 C14 -42.1(3) . . . . ? Si6 Si4 Si7 C14 -152.2(3) . . . . ? Si1 Si4 Si7 C14 80.8(3) . . . . ? Si1 Zn1 Si8 Si9 92.0(4) . . . . ? Si1 Zn1 Si8 Si10 -13.1(4) . . . . ? Si1 Zn1 Si8 Si11 -141.9(4) . . . . ? Si10 Si8 Si9 C17 -42.4(3) . . . . ? Si11 Si8 Si9 C17 84.3(3) . . . . ? Zn1 Si8 Si9 C17 -147.5(3) . . . . ? Si10 Si8 Si9 C16 76.2(2) . . . . ? Si11 Si8 Si9 C16 -157.1(2) . . . . ? Zn1 Si8 Si9 C16 -28.9(2) . . . . ? Si10 Si8 Si9 C18 -168.4(2) . . . . ? Si11 Si8 Si9 C18 -41.7(2) . . . . ? Zn1 Si8 Si9 C18 86.5(2) . . . . ? Si9 Si8 Si10 C21 69.6(2) . . . . ? Si11 Si8 Si10 C21 -57.6(2) . . . . ? Zn1 Si8 Si10 C21 171.3(2) . . . . ? Si9 Si8 Si10 C19 -49.9(2) . . . . ? Si11 Si8 Si10 C19 -177.1(2) . . . . ? Zn1 Si8 Si10 C19 51.8(2) . . . . ? Si9 Si8 Si10 C20 -168.1(2) . . . . ? Si11 Si8 Si10 C20 64.7(2) . . . . ? Zn1 Si8 Si10 C20 -66.4(2) . . . . ? Si9 Si8 Si11 Si12 83.79(9) . . . . ? Si10 Si8 Si11 Si12 -156.04(7) . . . . ? Zn1 Si8 Si11 Si12 -33.34(10) . . . . ? Si9 Si8 Si11 Si13 -159.71(7) . . . . ? Si10 Si8 Si11 Si13 -39.54(10) . . . . ? Zn1 Si8 Si11 Si13 83.16(9) . . . . ? Si9 Si8 Si11 Si14 -37.75(11) . . . . ? Si10 Si8 Si11 Si14 82.42(10) . . . . ? Zn1 Si8 Si11 Si14 -154.88(7) . . . . ? Si13 Si11 Si12 C24 70.6(2) . . . . ? Si14 Si11 Si12 C24 -43.6(2) . . . . ? Si8 Si11 Si12 C24 -167.9(2) . . . . ? Si13 Si11 Si12 C23 -169.6(2) . . . . ? Si14 Si11 Si12 C23 76.3(2) . . . . ? Si8 Si11 Si12 C23 -48.1(2) . . . . ? Si13 Si11 Si12 C22 -49.7(2) . . . . ? Si14 Si11 Si12 C22 -163.8(2) . . . . ? Si8 Si11 Si12 C22 71.8(2) . . . . ? Si12 Si11 Si13 C25 -46.1(2) . . . . ? Si14 Si11 Si13 C25 69.3(2) . . . . ? Si8 Si11 Si13 C25 -165.1(2) . . . . ? Si12 Si11 Si13 C27 72.6(2) . . . . ? Si14 Si11 Si13 C27 -171.9(2) . . . . ? Si8 Si11 Si13 C27 -46.4(2) . . . . ? Si12 Si11 Si13 C26 -164.3(2) . . . . ? Si14 Si11 Si13 C26 -48.9(2) . . . . ? Si8 Si11 Si13 C26 76.6(2) . . . . ? Si12 Si11 Si14 C29 -164.8(2) . . . . ? Si13 Si11 Si14 C29 82.4(3) . . . . ? Si8 Si11 Si14 C29 -42.9(3) . . . . ? Si12 Si11 Si14 C30 -42.4(3) . . . . ? Si13 Si11 Si14 C30 -155.3(3) . . . . ? Si8 Si11 Si14 C30 79.4(3) . . . . ? Si12 Si11 Si14 C28 76.6(2) . . . . ? Si13 Si11 Si14 C28 -36.3(2) . . . . ? Si8 Si11 Si14 C28 -161.6(2) . . . . ? Si22 Zn2 Si15 Si16 -115.0(4) . . . . ? Si22 Zn2 Si15 Si17 -3.3(5) . . . . ? Si22 Zn2 Si15 Si18 120.4(4) . . . . ? Si17 Si15 Si16 C33 -69.9(2) . . . . ? Si18 Si15 Si16 C33 166.21(19) . . . . ? Zn2 Si15 Si16 C33 40.8(2) . . . . ? Si17 Si15 Si16 C31 168.73(19) . . . . ? Si18 Si15 Si16 C31 44.9(2) . . . . ? Zn2 Si15 Si16 C31 -80.5(2) . . . . ? Si17 Si15 Si16 C32 48.5(2) . . . . ? Si18 Si15 Si16 C32 -75.4(2) . . . . ? Zn2 Si15 Si16 C32 159.19(19) . . . . ? Si16 Si15 Si17 C34 -69.9(2) . . . . ? Si18 Si15 Si17 C34 50.1(2) . . . . ? Zn2 Si15 Si17 C34 170.97(19) . . . . ? Si16 Si15 Si17 C35 49.00(19) . . . . ? Si18 Si15 Si17 C35 168.98(19) . . . . ? Zn2 Si15 Si17 C35 -70.18(19) . . . . ? Si16 Si15 Si17 C36 166.27(19) . . . . ? Si18 Si15 Si17 C36 -73.8(2) . . . . ? Zn2 Si15 Si17 C36 47.1(2) . . . . ? Si16 Si15 Si18 Si20 160.10(7) . . . . ? Si17 Si15 Si18 Si20 43.25(10) . . . . ? Zn2 Si15 Si18 Si20 -72.72(8) . . . . ? Si16 Si15 Si18 Si21 -85.35(9) . . . . ? Si17 Si15 Si18 Si21 157.81(7) . . . . ? Zn2 Si15 Si18 Si21 41.84(9) . . . . ? Si16 Si15 Si18 Si19 40.23(10) . . . . ? Si17 Si15 Si18 Si19 -76.62(9) . . . . ? Zn2 Si15 Si18 Si19 167.41(6) . . . . ? Si20 Si18 Si19 C37 46.79(19) . . . . ? Si21 Si18 Si19 C37 -65.06(19) . . . . ? Si15 Si18 Si19 C37 169.05(19) . . . . ? Si20 Si18 Si19 C38 -70.6(2) . . . . ? Si21 Si18 Si19 C38 177.58(19) . . . . ? Si15 Si18 Si19 C38 51.7(2) . . . . ? Si20 Si18 Si19 C39 164.8(2) . . . . ? Si21 Si18 Si19 C39 53.0(2) . . . . ? Si15 Si18 Si19 C39 -72.9(2) . . . . ? Si21 Si18 Si20 C40 166.45(18) . . . . ? Si19 Si18 Si20 C40 51.32(19) . . . . ? Si15 Si18 Si20 C40 -75.64(19) . . . . ? Si21 Si18 Si20 C41 -71.7(2) . . . . ? Si19 Si18 Si20 C41 173.21(19) . . . . ? Si15 Si18 Si20 C41 46.3(2) . . . . ? Si21 Si18 Si20 C42 46.8(2) . . . . ? Si19 Si18 Si20 C42 -68.4(2) . . . . ? Si15 Si18 Si20 C42 164.7(2) . . . . ? Si20 Si18 Si21 C44 168.0(2) . . . . ? Si19 Si18 Si21 C44 -79.7(3) . . . . ? Si15 Si18 Si21 C44 50.2(3) . . . . ? Si20 Si18 Si21 C43 47.6(2) . . . . ? Si19 Si18 Si21 C43 159.8(2) . . . . ? Si15 Si18 Si21 C43 -70.2(2) . . . . ? Si20 Si18 Si21 C45 -71.1(2) . . . . ? Si19 Si18 Si21 C45 41.1(2) . . . . ? Si15 Si18 Si21 C45 171.1(2) . . . . ? Si15 Zn2 Si22 Si23 -2.2(5) . . . . ? Si15 Zn2 Si22 Si24 -114.0(4) . . . . ? Si15 Zn2 Si22 Si25 119.0(4) . . . . ? Si24 Si22 Si23 C47 -73.2(2) . . . . ? Si25 Si22 Si23 C47 50.0(2) . . . . ? Zn2 Si22 Si23 C47 168.4(2) . . . . ? Si24 Si22 Si23 C48 164.9(2) . . . . ? Si25 Si22 Si23 C48 -71.9(2) . . . . ? Zn2 Si22 Si23 C48 46.5(2) . . . . ? Si24 Si22 Si23 C46 46.6(2) . . . . ? Si25 Si22 Si23 C46 169.8(2) . . . . ? Zn2 Si22 Si23 C46 -71.8(2) . . . . ? Si23 Si22 Si24 C51 47.9(2) . . . . ? Si25 Si22 Si24 C51 -75.2(2) . . . . ? Zn2 Si22 Si24 C51 160.05(19) . . . . ? Si23 Si22 Si24 C49 170.0(2) . . . . ? Si25 Si22 Si24 C49 46.8(2) . . . . ? Zn2 Si22 Si24 C49 -77.9(2) . . . . ? Si23 Si22 Si24 C50 -69.0(2) . . . . ? Si25 Si22 Si24 C50 167.8(2) . . . . ? Zn2 Si22 Si24 C50 43.1(2) . . . . ? Si23 Si22 Si25 Si26 158.65(7) . . . . ? Si24 Si22 Si25 Si26 -83.64(9) . . . . ? Zn2 Si22 Si25 Si26 43.14(9) . . . . ? Si23 Si22 Si25 Si28 -79.24(10) . . . . ? Si24 Si22 Si25 Si28 38.47(11) . . . . ? Zn2 Si22 Si25 Si28 165.25(7) . . . . ? Si23 Si22 Si25 Si27 44.35(10) . . . . ? Si24 Si22 Si25 Si27 162.06(7) . . . . ? Zn2 Si22 Si25 Si27 -71.16(8) . . . . ? Si28 Si25 Si26 C54 35.5(2) . . . . ? Si27 Si25 Si26 C54 -77.3(2) . . . . ? Si22 Si25 Si26 C54 163.5(2) . . . . ? Si28 Si25 Si26 C53 156.4(2) . . . . ? Si27 Si25 Si26 C53 43.6(2) . . . . ? Si22 Si25 Si26 C53 -75.6(2) . . . . ? Si28 Si25 Si26 C52 -86.7(2) . . . . ? Si27 Si25 Si26 C52 160.5(2) . . . . ? Si22 Si25 Si26 C52 41.3(2) . . . . ? Si26 Si25 Si27 C55 -76.4(2) . . . . ? Si28 Si25 Si27 C55 170.1(2) . . . . ? Si22 Si25 Si27 C55 40.6(2) . . . . ? Si26 Si25 Si27 C56 42.3(2) . . . . ? Si28 Si25 Si27 C56 -71.1(2) . . . . ? Si22 Si25 Si27 C56 159.3(2) . . . . ? Si26 Si25 Si27 C57 161.5(2) . . . . ? Si28 Si25 Si27 C57 48.0(2) . . . . ? Si22 Si25 Si27 C57 -81.5(2) . . . . ? Si26 Si25 Si28 C60 49.1(2) . . . . ? Si27 Si25 Si28 C60 160.3(2) . . . . ? Si22 Si25 Si28 C60 -73.5(2) . . . . ? Si26 Si25 Si28 C58 -68.9(2) . . . . ? Si27 Si25 Si28 C58 42.2(2) . . . . ? Si22 Si25 Si28 C58 168.4(2) . . . . ? Si26 Si25 Si28 C59 172.9(2) . . . . ? Si27 Si25 Si28 C59 -75.9(2) . . . . ? Si22 Si25 Si28 C59 50.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.711 _refine_diff_density_min -0.411 _refine_diff_density_rms 0.102 # Attachment '3a_355j_ohne.cif' data_355j _database_code_depnum_ccdc_archive 'CCDC 645723' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H102 Si16 Zn' _chemical_formula_weight 1025.97 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' Si Si 0.0817 0.0704 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.261(3) _cell_length_b 9.6806(19) _cell_length_c 41.968(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.33(3) _cell_angle_gamma 90.00 _cell_volume 6499(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blocks _exptl_crystal_colour colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.048 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 0.694 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7883 _exptl_absorpt_correction_T_max 0.8623 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36430 _diffrn_reflns_av_R_equivalents 0.0798 _diffrn_reflns_av_sigmaI/netI 0.0674 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 0.99 _diffrn_reflns_theta_max 22.50 _reflns_number_total 8501 _reflns_number_gt 7714 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0421P)^2^+38.8432P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8501 _refine_ls_number_parameters 494 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1074 _refine_ls_R_factor_gt 0.0958 _refine_ls_wR_factor_ref 0.1895 _refine_ls_wR_factor_gt 0.1843 _refine_ls_goodness_of_fit_ref 1.325 _refine_ls_restrained_S_all 1.325 _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 Zn1 Zn 0.87547(6) 0.86146(9) 0.12596(2) 0.0167(3) Uani 1 1 d . . . Si1 Si 0.76882(13) 0.8999(2) 0.07973(5) 0.0141(5) Uani 1 1 d . . . Si2 Si 0.82748(13) 0.8112(2) 0.03622(5) 0.0164(5) Uani 1 1 d . . . Si3 Si 0.75206(14) 0.7867(2) -0.01724(5) 0.0170(5) Uani 1 1 d . . . Si4 Si 0.83460(15) 0.6449(2) -0.04507(5) 0.0234(6) Uani 1 1 d . . . Si5 Si 0.75404(14) 1.1404(2) 0.08452(5) 0.0197(5) Uani 1 1 d . . . Si6 Si 0.66185(14) 0.7823(2) 0.09964(6) 0.0211(6) Uani 1 1 d . . . Si7 Si 0.62393(15) 0.6745(3) -0.01839(6) 0.0260(6) Uani 1 1 d . . . Si8 Si 0.72492(16) 0.9955(2) -0.04557(6) 0.0255(6) Uani 1 1 d . . . Si9 Si 0.98438(13) 0.8226(2) 0.17137(5) 0.0156(5) Uani 1 1 d . . . Si10 Si 0.91798(13) 0.8185(2) 0.21700(5) 0.0174(5) Uani 1 1 d . . . Si11 Si 0.98742(14) 0.7586(2) 0.26985(5) 0.0168(5) Uani 1 1 d . . . Si12 Si 0.98397(17) 0.5183(2) 0.27872(6) 0.0280(6) Uani 1 1 d . . . Si13 Si 1.03861(15) 0.6236(2) 0.15115(5) 0.0236(6) Uani 1 1 d . . . Si14 Si 1.07281(15) 1.0091(2) 0.16491(6) 0.0250(6) Uani 1 1 d . . . Si15 Si 0.91033(15) 0.8581(2) 0.30687(6) 0.0254(6) Uani 1 1 d . . . Si16 Si 1.12495(15) 0.8381(3) 0.28382(6) 0.0292(6) Uani 1 1 d . . . C1 C 0.8651(6) 0.6311(9) 0.0494(2) 0.030(2) Uani 1 1 d . . . H1A H 0.9047 0.5991 0.0360 0.045 Uiso 1 1 calc R . . H1B H 0.8172 0.5680 0.0469 0.045 Uiso 1 1 calc R . . H1C H 0.8927 0.6331 0.0722 0.045 Uiso 1 1 calc R . . C2 C 0.9220(5) 0.9206(10) 0.0342(2) 0.031(2) Uani 1 1 d . . . H2A H 0.9601 0.9177 0.0551 0.047 Uiso 1 1 calc R . . H2B H 0.9044 1.0162 0.0291 0.047 Uiso 1 1 calc R . . H2C H 0.9506 0.8850 0.0172 0.047 Uiso 1 1 calc R . . C3 C 0.9478(5) 0.6950(10) -0.0378(2) 0.037(2) Uani 1 1 d . . . H3A H 0.9774 0.6391 -0.0517 0.056 Uiso 1 1 calc R . . H3B H 0.9723 0.6790 -0.0151 0.056 Uiso 1 1 calc R . . H3C H 0.9528 0.7930 -0.0430 0.056 Uiso 1 1 calc R . . C4 C 0.7935(6) 0.6596(10) -0.0895(2) 0.038(2) Uani 1 1 d . . . H4A H 0.8010 0.7545 -0.0966 0.056 Uiso 1 1 calc R . . H4B H 0.7339 0.6361 -0.0939 0.056 Uiso 1 1 calc R . . H4C H 0.8240 0.5960 -0.1013 0.056 Uiso 1 1 calc R . . C5 C 0.8288(6) 0.4576(9) -0.0330(2) 0.034(2) Uani 1 1 d . . . H5A H 0.7701 0.4291 -0.0358 0.050 Uiso 1 1 calc R . . H5B H 0.8554 0.4463 -0.0103 0.050 Uiso 1 1 calc R . . H5C H 0.8579 0.4004 -0.0468 0.050 Uiso 1 1 calc R . . C6 C 0.7826(5) 1.1897(9) 0.12858(18) 0.026(2) Uani 1 1 d . . . H6A H 0.7721 1.2885 0.1310 0.039 Uiso 1 1 calc R . . H6B H 0.8419 1.1701 0.1364 0.039 Uiso 1 1 calc R . . H6C H 0.7486 1.1362 0.1412 0.039 Uiso 1 1 calc R . . C7 C 0.8277(5) 1.2387(8) 0.0631(2) 0.027(2) Uani 1 1 d . . . H7A H 0.8114 1.2255 0.0397 0.040 Uiso 1 1 calc R . . H7B H 0.8848 1.2046 0.0702 0.040 Uiso 1 1 calc R . . H7C H 0.8253 1.3372 0.0682 0.040 Uiso 1 1 calc R . . C8 C 0.6445(5) 1.1986(9) 0.0695(2) 0.028(2) Uani 1 1 d . . . H8A H 0.6069 1.1538 0.0822 0.043 Uiso 1 1 calc R . . H8B H 0.6280 1.1735 0.0466 0.043 Uiso 1 1 calc R . . H8C H 0.6411 1.2991 0.0718 0.043 Uiso 1 1 calc R . . C9 C 0.6474(6) 0.8762(10) 0.1378(2) 0.037(2) Uani 1 1 d . . . H9A H 0.6286 0.9709 0.1323 0.055 Uiso 1 1 calc R . . H9B H 0.7006 0.8783 0.1530 0.055 Uiso 1 1 calc R . . H9C H 0.6054 0.8279 0.1477 0.055 Uiso 1 1 calc R . . C10 C 0.6966(6) 0.6005(9) 0.1109(2) 0.035(2) Uani 1 1 d . . . H10A H 0.6504 0.5492 0.1174 0.052 Uiso 1 1 calc R . . H10B H 0.7441 0.6026 0.1289 0.052 Uiso 1 1 calc R . . H10C H 0.7133 0.5550 0.0922 0.052 Uiso 1 1 calc R . . C11 C 0.5549(5) 0.7759(10) 0.0746(2) 0.038(2) Uani 1 1 d . . . H11A H 0.5550 0.7143 0.0561 0.057 Uiso 1 1 calc R . . H11B H 0.5382 0.8690 0.0668 0.057 Uiso 1 1 calc R . . H11C H 0.5154 0.7413 0.0878 0.057 Uiso 1 1 calc R . . C12 C 0.5472(6) 0.8089(10) -0.0094(2) 0.041(3) Uani 1 1 d . . . H12A H 0.5342 0.8726 -0.0277 0.061 Uiso 1 1 calc R . . H12B H 0.5718 0.8605 0.0101 0.061 Uiso 1 1 calc R . . H12C H 0.4958 0.7633 -0.0058 0.061 Uiso 1 1 calc R . . C13 C 0.6352(6) 0.5308(10) 0.0119(2) 0.043(3) Uani 1 1 d . . . H13A H 0.5821 0.4808 0.0100 0.064 Uiso 1 1 calc R . . H13B H 0.6503 0.5690 0.0338 0.064 Uiso 1 1 calc R . . H13C H 0.6791 0.4672 0.0078 0.064 Uiso 1 1 calc R . . C14 C 0.5831(6) 0.5941(11) -0.0592(2) 0.046(3) Uani 1 1 d . . . H14A H 0.6179 0.5146 -0.0625 0.069 Uiso 1 1 calc R . . H14B H 0.5848 0.6624 -0.0763 0.069 Uiso 1 1 calc R . . H14C H 0.5253 0.5635 -0.0599 0.069 Uiso 1 1 calc R . . C15 C 0.6743(6) 1.1239(9) -0.0221(2) 0.035(2) Uani 1 1 d . . . H15A H 0.7064 1.1307 0.0000 0.053 Uiso 1 1 calc R . . H15B H 0.6172 1.0939 -0.0212 0.053 Uiso 1 1 calc R . . H15C H 0.6728 1.2143 -0.0326 0.053 Uiso 1 1 calc R . . C16 C 0.8242(7) 1.0706(10) -0.0548(3) 0.048(3) Uani 1 1 d . . . H16A H 0.8110 1.1482 -0.0698 0.072 Uiso 1 1 calc R . . H16B H 0.8545 0.9996 -0.0647 0.072 Uiso 1 1 calc R . . H16C H 0.8590 1.1032 -0.0347 0.072 Uiso 1 1 calc R . . C17 C 0.6516(7) 0.9690(11) -0.0851(2) 0.049(3) Uani 1 1 d . . . H17A H 0.5977 0.9355 -0.0809 0.073 Uiso 1 1 calc R . . H17B H 0.6755 0.9009 -0.0981 0.073 Uiso 1 1 calc R . . H17C H 0.6435 1.0568 -0.0969 0.073 Uiso 1 1 calc R . . C18 C 0.8725(5) 0.9989(9) 0.2185(2) 0.027(2) Uani 1 1 d . . . H18A H 0.8425 1.0245 0.1970 0.041 Uiso 1 1 calc R . . H18B H 0.9179 1.0650 0.2255 0.041 Uiso 1 1 calc R . . H18C H 0.8338 1.0002 0.2339 0.041 Uiso 1 1 calc R . . C19 C 0.8276(5) 0.6957(10) 0.2066(2) 0.032(2) Uani 1 1 d . . . H19A H 0.7954 0.6946 0.2242 0.047 Uiso 1 1 calc R . . H19B H 0.8488 0.6026 0.2036 0.047 Uiso 1 1 calc R . . H19C H 0.7916 0.7258 0.1865 0.047 Uiso 1 1 calc R . . C20 C 1.0196(9) 0.4170(11) 0.2459(3) 0.074(4) Uani 1 1 d . . . H20A H 1.0107 0.3184 0.2492 0.110 Uiso 1 1 calc R . . H20B H 1.0792 0.4342 0.2464 0.110 Uiso 1 1 calc R . . H20C H 0.9877 0.4454 0.2249 0.110 Uiso 1 1 calc R . . C21 C 0.8749(6) 0.4630(9) 0.2803(2) 0.041(3) Uani 1 1 d . . . H21A H 0.8735 0.3628 0.2835 0.061 Uiso 1 1 calc R . . H21B H 0.8382 0.4874 0.2599 0.061 Uiso 1 1 calc R . . H21C H 0.8556 0.5097 0.2983 0.061 Uiso 1 1 calc R . . C22 C 1.0527(6) 0.4647(9) 0.3171(2) 0.035(2) Uani 1 1 d . . . H22A H 1.0385 0.5183 0.3351 0.053 Uiso 1 1 calc R . . H22B H 1.1112 0.4815 0.3154 0.053 Uiso 1 1 calc R . . H22C H 1.0445 0.3662 0.3208 0.053 Uiso 1 1 calc R . . C23 C 1.0681(6) 0.6726(10) 0.1111(2) 0.036(2) Uani 1 1 d . . . H23A H 1.0847 0.5896 0.1004 0.055 Uiso 1 1 calc R . . H23B H 1.1148 0.7380 0.1148 0.055 Uiso 1 1 calc R . . H23C H 1.0200 0.7155 0.0972 0.055 Uiso 1 1 calc R . . C24 C 0.9567(6) 0.4856(9) 0.1433(2) 0.031(2) Uani 1 1 d . . . H24A H 0.9784 0.4067 0.1327 0.047 Uiso 1 1 calc R . . H24B H 0.9069 0.5222 0.1292 0.047 Uiso 1 1 calc R . . H24C H 0.9420 0.4558 0.1639 0.047 Uiso 1 1 calc R . . C25 C 1.1358(6) 0.5511(10) 0.1767(2) 0.036(2) Uani 1 1 d . . . H25A H 1.1239 0.5248 0.1980 0.054 Uiso 1 1 calc R . . H25B H 1.1801 0.6211 0.1795 0.054 Uiso 1 1 calc R . . H25C H 1.1542 0.4696 0.1660 0.054 Uiso 1 1 calc R . . C26 C 1.0496(6) 1.0633(10) 0.1219(2) 0.042(3) Uani 1 1 d . . . H26A H 1.0864 1.1399 0.1184 0.063 Uiso 1 1 calc R . . H26B H 0.9912 1.0933 0.1163 0.063 Uiso 1 1 calc R . . H26C H 1.0588 0.9853 0.1080 0.063 Uiso 1 1 calc R . . C27 C 1.1858(6) 0.9654(11) 0.1755(3) 0.057(3) Uani 1 1 d . . . H27A H 1.1982 0.8878 0.1622 0.086 Uiso 1 1 calc R . . H27B H 1.1994 0.9397 0.1985 0.086 Uiso 1 1 calc R . . H27C H 1.2192 1.0457 0.1716 0.086 Uiso 1 1 calc R . . C28 C 1.0504(7) 1.1661(9) 0.1880(2) 0.045(3) Uani 1 1 d . . . H28A H 1.0859 1.2426 0.1834 0.067 Uiso 1 1 calc R . . H28B H 1.0621 1.1460 0.2113 0.067 Uiso 1 1 calc R . . H28C H 0.9915 1.1919 0.1815 0.067 Uiso 1 1 calc R . . C29 C 0.9290(7) 1.0477(9) 0.3109(2) 0.050(3) Uani 1 1 d . . . H29A H 0.9142 1.0914 0.2896 0.075 Uiso 1 1 calc R . . H29B H 0.9882 1.0648 0.3196 0.075 Uiso 1 1 calc R . . H29C H 0.8946 1.0867 0.3256 0.075 Uiso 1 1 calc R . . C30 C 0.9427(6) 0.7820(10) 0.34831(19) 0.033(2) Uani 1 1 d . . . H30A H 0.9114 0.8267 0.3634 0.050 Uiso 1 1 calc R . . H30B H 1.0027 0.7968 0.3557 0.050 Uiso 1 1 calc R . . H30C H 0.9308 0.6827 0.3475 0.050 Uiso 1 1 calc R . . C31 C 0.7964(5) 0.8295(10) 0.2942(2) 0.037(2) Uani 1 1 d . . . H31A H 0.7664 0.8746 0.3096 0.056 Uiso 1 1 calc R . . H31B H 0.7847 0.7302 0.2937 0.056 Uiso 1 1 calc R . . H31C H 0.7779 0.8687 0.2725 0.056 Uiso 1 1 calc R . . C32 C 1.1945(6) 0.7396(13) 0.2611(3) 0.062(3) Uani 1 1 d . . . H32A H 1.1733 0.7473 0.2378 0.093 Uiso 1 1 calc R . . H32B H 1.1956 0.6422 0.2676 0.093 Uiso 1 1 calc R . . H32C H 1.2512 0.7776 0.2661 0.093 Uiso 1 1 calc R . . C33 C 1.1328(7) 1.0246(12) 0.2743(3) 0.066(4) Uani 1 1 d . . . H33A H 1.1892 1.0578 0.2831 0.099 Uiso 1 1 calc R . . H33B H 1.0919 1.0767 0.2840 0.099 Uiso 1 1 calc R . . H33C H 1.1213 1.0376 0.2508 0.099 Uiso 1 1 calc R . . C34 C 1.1641(6) 0.8136(11) 0.3284(2) 0.041(3) Uani 1 1 d . . . H34A H 1.2242 0.8330 0.3333 0.061 Uiso 1 1 calc R . . H34B H 1.1540 0.7181 0.3344 0.061 Uiso 1 1 calc R . . H34C H 1.1346 0.8770 0.3407 0.061 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 Zn1 0.0196(5) 0.0157(5) 0.0147(5) 0.0010(4) 0.0028(4) 0.0008(4) Si1 0.0168(12) 0.0104(11) 0.0158(12) 0.0004(9) 0.0047(9) 0.0004(9) Si2 0.0176(12) 0.0157(12) 0.0162(12) -0.0018(9) 0.0035(9) -0.0018(10) Si3 0.0189(13) 0.0178(12) 0.0148(12) -0.0016(10) 0.0045(10) -0.0001(10) Si4 0.0298(14) 0.0211(13) 0.0206(13) -0.0063(11) 0.0084(11) 0.0021(11) Si5 0.0245(13) 0.0150(12) 0.0193(12) 0.0007(10) 0.0032(10) 0.0036(10) Si6 0.0222(13) 0.0187(13) 0.0243(13) 0.0001(10) 0.0094(10) -0.0028(10) Si7 0.0238(14) 0.0299(15) 0.0239(13) 0.0000(11) 0.0028(11) -0.0082(11) Si8 0.0355(15) 0.0221(14) 0.0209(13) 0.0023(11) 0.0099(11) 0.0037(11) Si9 0.0196(12) 0.0121(12) 0.0152(12) -0.0004(9) 0.0038(9) -0.0005(9) Si10 0.0169(12) 0.0191(13) 0.0162(12) 0.0010(10) 0.0026(9) 0.0006(10) Si11 0.0185(13) 0.0170(12) 0.0145(12) -0.0011(9) 0.0019(10) 0.0020(10) Si12 0.0458(16) 0.0188(13) 0.0188(13) 0.0028(10) 0.0047(12) 0.0062(12) Si13 0.0291(14) 0.0215(13) 0.0199(13) 0.0000(10) 0.0039(11) 0.0072(11) Si14 0.0288(14) 0.0218(13) 0.0245(13) -0.0001(11) 0.0048(11) -0.0071(11) Si15 0.0342(15) 0.0239(13) 0.0206(13) 0.0016(11) 0.0117(11) 0.0045(11) Si16 0.0218(14) 0.0427(17) 0.0217(13) 0.0079(12) 0.0000(11) -0.0042(12) C1 0.035(6) 0.025(5) 0.031(5) 0.004(4) 0.009(4) 0.013(4) C2 0.030(5) 0.040(6) 0.022(5) -0.001(4) -0.003(4) -0.009(4) C3 0.029(6) 0.042(6) 0.044(6) -0.013(5) 0.014(5) -0.002(5) C4 0.045(6) 0.040(6) 0.030(5) -0.015(5) 0.013(5) 0.001(5) C5 0.044(6) 0.029(6) 0.032(5) -0.006(4) 0.019(5) -0.003(5) C6 0.038(6) 0.020(5) 0.017(5) -0.006(4) -0.004(4) 0.006(4) C7 0.039(6) 0.014(5) 0.027(5) 0.005(4) 0.008(4) -0.003(4) C8 0.028(5) 0.025(5) 0.032(5) 0.006(4) 0.005(4) 0.013(4) C9 0.039(6) 0.042(6) 0.036(6) 0.003(5) 0.025(5) 0.008(5) C10 0.046(6) 0.021(5) 0.042(6) 0.003(4) 0.021(5) -0.002(4) C11 0.022(5) 0.048(6) 0.046(6) -0.005(5) 0.007(5) -0.004(5) C12 0.032(6) 0.048(6) 0.046(6) -0.001(5) 0.013(5) 0.001(5) C13 0.035(6) 0.043(6) 0.053(7) 0.000(5) 0.014(5) -0.009(5) C14 0.045(7) 0.049(7) 0.043(6) -0.001(5) 0.006(5) -0.012(5) C15 0.041(6) 0.029(5) 0.039(6) 0.004(4) 0.015(5) 0.009(5) C16 0.067(8) 0.030(6) 0.058(7) 0.010(5) 0.038(6) 0.004(5) C17 0.068(8) 0.040(6) 0.040(6) 0.001(5) 0.011(6) 0.011(6) C18 0.029(5) 0.029(5) 0.023(5) 0.003(4) 0.004(4) 0.010(4) C19 0.025(5) 0.044(6) 0.025(5) 0.015(4) 0.002(4) -0.001(4) C20 0.157(13) 0.033(7) 0.036(7) 0.014(5) 0.033(8) 0.023(7) C21 0.058(7) 0.022(5) 0.037(6) 0.010(4) -0.007(5) -0.014(5) C22 0.035(6) 0.029(6) 0.037(6) 0.012(4) -0.004(5) 0.004(4) C23 0.048(6) 0.034(6) 0.032(5) -0.001(4) 0.019(5) 0.012(5) C24 0.041(6) 0.019(5) 0.031(5) -0.002(4) -0.001(4) 0.009(4) C25 0.038(6) 0.033(6) 0.038(6) -0.002(5) 0.011(5) 0.008(5) C26 0.049(7) 0.047(7) 0.032(6) 0.005(5) 0.015(5) -0.021(5) C27 0.031(6) 0.045(7) 0.092(9) 0.003(6) 0.002(6) -0.013(5) C28 0.076(8) 0.016(5) 0.042(6) 0.001(4) 0.010(5) -0.004(5) C29 0.084(9) 0.028(6) 0.044(6) -0.003(5) 0.029(6) 0.014(6) C30 0.046(6) 0.036(6) 0.020(5) 0.001(4) 0.012(4) 0.006(5) C31 0.031(6) 0.054(7) 0.030(5) 0.015(5) 0.014(4) 0.020(5) C32 0.024(6) 0.102(10) 0.060(8) -0.011(7) 0.007(5) 0.010(6) C33 0.042(7) 0.069(8) 0.072(8) 0.036(7) -0.029(6) -0.029(6) C34 0.036(6) 0.051(7) 0.030(5) 0.004(5) -0.007(4) -0.021(5) _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 Zn1 Si9 2.387(2) . ? Zn1 Si1 2.388(2) . ? Si1 Si5 2.352(3) . ? Si1 Si6 2.354(3) . ? Si1 Si2 2.368(3) . ? Si2 C2 1.881(8) . ? Si2 C1 1.897(8) . ? Si2 Si3 2.368(3) . ? Si3 Si7 2.342(3) . ? Si3 Si8 2.347(3) . ? Si3 Si4 2.369(3) . ? Si4 C4 1.871(9) . ? Si4 C3 1.875(9) . ? Si4 C5 1.889(9) . ? Si5 C8 1.867(8) . ? Si5 C7 1.880(8) . ? Si5 C6 1.886(8) . ? Si6 C11 1.864(9) . ? Si6 C10 1.882(9) . ? Si6 C9 1.892(9) . ? Si7 C13 1.871(10) . ? Si7 C12 1.887(9) . ? Si7 C14 1.889(10) . ? Si8 C15 1.866(9) . ? Si8 C16 1.872(10) . ? Si8 C17 1.878(10) . ? Si9 Si13 2.340(3) . ? Si9 Si14 2.353(3) . ? Si9 Si10 2.362(3) . ? Si10 C19 1.880(9) . ? Si10 C18 1.902(8) . ? Si10 Si11 2.373(3) . ? Si11 Si16 2.338(3) . ? Si11 Si12 2.359(3) . ? Si11 Si15 2.369(3) . ? Si12 C22 1.860(8) . ? Si12 C21 1.866(10) . ? Si12 C20 1.866(11) . ? Si13 C24 1.874(9) . ? Si13 C25 1.880(9) . ? Si13 C23 1.891(9) . ? Si14 C26 1.854(9) . ? Si14 C27 1.859(10) . ? Si14 C28 1.874(9) . ? Si15 C31 1.854(9) . ? Si15 C29 1.864(10) . ? Si15 C30 1.875(8) . ? Si16 C33 1.858(11) . ? Si16 C32 1.866(10) . ? Si16 C34 1.880(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Si9 Zn1 Si1 178.69(8) . . ? Si5 Si1 Si6 110.80(12) . . ? Si5 Si1 Si2 119.11(11) . . ? Si6 Si1 Si2 121.58(12) . . ? Si5 Si1 Zn1 98.93(10) . . ? Si6 Si1 Zn1 96.39(10) . . ? Si2 Si1 Zn1 103.62(10) . . ? C2 Si2 C1 107.9(4) . . ? C2 Si2 Si3 107.6(3) . . ? C1 Si2 Si3 105.6(3) . . ? C2 Si2 Si1 106.0(3) . . ? C1 Si2 Si1 105.2(3) . . ? Si3 Si2 Si1 123.72(12) . . ? Si7 Si3 Si8 107.64(12) . . ? Si7 Si3 Si2 111.93(12) . . ? Si8 Si3 Si2 114.34(12) . . ? Si7 Si3 Si4 107.58(12) . . ? Si8 Si3 Si4 108.73(12) . . ? Si2 Si3 Si4 106.39(12) . . ? C4 Si4 C3 107.9(4) . . ? C4 Si4 C5 108.3(4) . . ? C3 Si4 C5 107.4(4) . . ? C4 Si4 Si3 108.3(3) . . ? C3 Si4 Si3 113.4(3) . . ? C5 Si4 Si3 111.4(3) . . ? C8 Si5 C7 109.7(4) . . ? C8 Si5 C6 107.9(4) . . ? C7 Si5 C6 105.9(4) . . ? C8 Si5 Si1 112.1(3) . . ? C7 Si5 Si1 112.1(3) . . ? C6 Si5 Si1 108.9(3) . . ? C11 Si6 C10 108.6(4) . . ? C11 Si6 C9 104.4(4) . . ? C10 Si6 C9 108.3(4) . . ? C11 Si6 Si1 119.3(3) . . ? C10 Si6 Si1 109.5(3) . . ? C9 Si6 Si1 106.2(3) . . ? C13 Si7 C12 111.3(4) . . ? C13 Si7 C14 106.5(5) . . ? C12 Si7 C14 109.2(5) . . ? C13 Si7 Si3 110.6(3) . . ? C12 Si7 Si3 107.1(3) . . ? C14 Si7 Si3 112.1(3) . . ? C15 Si8 C16 109.2(4) . . ? C15 Si8 C17 106.7(4) . . ? C16 Si8 C17 107.7(5) . . ? C15 Si8 Si3 111.5(3) . . ? C16 Si8 Si3 110.4(3) . . ? C17 Si8 Si3 111.2(3) . . ? Si13 Si9 Si14 108.17(12) . . ? Si13 Si9 Si10 122.47(12) . . ? Si14 Si9 Si10 118.95(12) . . ? Si13 Si9 Zn1 96.55(10) . . ? Si14 Si9 Zn1 99.69(10) . . ? Si10 Si9 Zn1 105.57(10) . . ? C19 Si10 C18 107.2(4) . . ? C19 Si10 Si9 105.9(3) . . ? C18 Si10 Si9 104.4(3) . . ? C19 Si10 Si11 106.5(3) . . ? C18 Si10 Si11 108.4(3) . . ? Si9 Si10 Si11 123.50(12) . . ? Si16 Si11 Si12 109.50(13) . . ? Si16 Si11 Si15 107.27(12) . . ? Si12 Si11 Si15 105.49(12) . . ? Si16 Si11 Si10 115.30(12) . . ? Si12 Si11 Si10 111.57(12) . . ? Si15 Si11 Si10 107.13(12) . . ? C22 Si12 C21 108.5(4) . . ? C22 Si12 C20 105.9(5) . . ? C21 Si12 C20 107.4(6) . . ? C22 Si12 Si11 112.6(3) . . ? C21 Si12 Si11 109.8(3) . . ? C20 Si12 Si11 112.5(4) . . ? C24 Si13 C25 109.4(4) . . ? C24 Si13 C23 107.9(4) . . ? C25 Si13 C23 106.3(4) . . ? C24 Si13 Si9 110.4(3) . . ? C25 Si13 Si9 115.7(3) . . ? C23 Si13 Si9 106.8(3) . . ? C26 Si14 C27 108.6(5) . . ? C26 Si14 C28 104.5(5) . . ? C27 Si14 C28 109.6(5) . . ? C26 Si14 Si9 107.9(3) . . ? C27 Si14 Si9 113.3(3) . . ? C28 Si14 Si9 112.5(3) . . ? C31 Si15 C29 108.1(5) . . ? C31 Si15 C30 107.9(4) . . ? C29 Si15 C30 106.8(5) . . ? C31 Si15 Si11 111.7(3) . . ? C29 Si15 Si11 111.3(3) . . ? C30 Si15 Si11 110.8(3) . . ? C33 Si16 C32 108.4(6) . . ? C33 Si16 C34 108.2(5) . . ? C32 Si16 C34 108.4(5) . . ? C33 Si16 Si11 111.4(3) . . ? C32 Si16 Si11 110.1(4) . . ? C34 Si16 Si11 110.3(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Si9 Zn1 Si1 Si5 -103(4) . . . . ? Si9 Zn1 Si1 Si6 145(4) . . . . ? Si9 Zn1 Si1 Si2 20(4) . . . . ? Si5 Si1 Si2 C2 45.3(3) . . . . ? Si6 Si1 Si2 C2 -169.7(3) . . . . ? Zn1 Si1 Si2 C2 -63.3(3) . . . . ? Si5 Si1 Si2 C1 159.5(3) . . . . ? Si6 Si1 Si2 C1 -55.5(3) . . . . ? Zn1 Si1 Si2 C1 50.9(3) . . . . ? Si5 Si1 Si2 Si3 -79.42(17) . . . . ? Si6 Si1 Si2 Si3 65.59(18) . . . . ? Zn1 Si1 Si2 Si3 172.06(11) . . . . ? C2 Si2 Si3 Si7 -173.3(3) . . . . ? C1 Si2 Si3 Si7 71.6(3) . . . . ? Si1 Si2 Si3 Si7 -49.29(18) . . . . ? C2 Si2 Si3 Si8 -50.6(3) . . . . ? C1 Si2 Si3 Si8 -165.7(3) . . . . ? Si1 Si2 Si3 Si8 73.44(17) . . . . ? C2 Si2 Si3 Si4 69.5(3) . . . . ? C1 Si2 Si3 Si4 -45.6(3) . . . . ? Si1 Si2 Si3 Si4 -166.53(12) . . . . ? Si7 Si3 Si4 C4 74.8(3) . . . . ? Si8 Si3 Si4 C4 -41.5(4) . . . . ? Si2 Si3 Si4 C4 -165.1(3) . . . . ? Si7 Si3 Si4 C3 -165.5(4) . . . . ? Si8 Si3 Si4 C3 78.2(4) . . . . ? Si2 Si3 Si4 C3 -45.4(4) . . . . ? Si7 Si3 Si4 C5 -44.2(4) . . . . ? Si8 Si3 Si4 C5 -160.5(3) . . . . ? Si2 Si3 Si4 C5 75.9(3) . . . . ? Si6 Si1 Si5 C8 -47.2(3) . . . . ? Si2 Si1 Si5 C8 101.3(3) . . . . ? Zn1 Si1 Si5 C8 -147.6(3) . . . . ? Si6 Si1 Si5 C7 -171.1(3) . . . . ? Si2 Si1 Si5 C7 -22.6(3) . . . . ? Zn1 Si1 Si5 C7 88.6(3) . . . . ? Si6 Si1 Si5 C6 72.0(3) . . . . ? Si2 Si1 Si5 C6 -139.5(3) . . . . ? Zn1 Si1 Si5 C6 -28.3(3) . . . . ? Si5 Si1 Si6 C11 76.4(4) . . . . ? Si2 Si1 Si6 C11 -71.2(4) . . . . ? Zn1 Si1 Si6 C11 178.5(4) . . . . ? Si5 Si1 Si6 C10 -157.8(3) . . . . ? Si2 Si1 Si6 C10 54.6(4) . . . . ? Zn1 Si1 Si6 C10 -55.7(3) . . . . ? Si5 Si1 Si6 C9 -41.0(3) . . . . ? Si2 Si1 Si6 C9 171.4(3) . . . . ? Zn1 Si1 Si6 C9 61.1(3) . . . . ? Si8 Si3 Si7 C13 -165.8(4) . . . . ? Si2 Si3 Si7 C13 -39.3(4) . . . . ? Si4 Si3 Si7 C13 77.2(4) . . . . ? Si8 Si3 Si7 C12 -44.3(3) . . . . ? Si2 Si3 Si7 C12 82.2(3) . . . . ? Si4 Si3 Si7 C12 -161.3(3) . . . . ? Si8 Si3 Si7 C14 75.5(4) . . . . ? Si2 Si3 Si7 C14 -158.1(4) . . . . ? Si4 Si3 Si7 C14 -41.5(4) . . . . ? Si7 Si3 Si8 C15 72.5(4) . . . . ? Si2 Si3 Si8 C15 -52.5(4) . . . . ? Si4 Si3 Si8 C15 -171.2(3) . . . . ? Si7 Si3 Si8 C16 -165.9(4) . . . . ? Si2 Si3 Si8 C16 69.0(4) . . . . ? Si4 Si3 Si8 C16 -49.7(4) . . . . ? Si7 Si3 Si8 C17 -46.5(4) . . . . ? Si2 Si3 Si8 C17 -171.5(4) . . . . ? Si4 Si3 Si8 C17 69.8(4) . . . . ? Si1 Zn1 Si9 Si13 -51(4) . . . . ? Si1 Zn1 Si9 Si14 59(4) . . . . ? Si1 Zn1 Si9 Si10 -178(100) . . . . ? Si13 Si9 Si10 C19 -58.6(3) . . . . ? Si14 Si9 Si10 C19 160.6(3) . . . . ? Zn1 Si9 Si10 C19 49.9(3) . . . . ? Si13 Si9 Si10 C18 -171.7(3) . . . . ? Si14 Si9 Si10 C18 47.6(3) . . . . ? Zn1 Si9 Si10 C18 -63.1(3) . . . . ? Si13 Si9 Si10 Si11 64.26(19) . . . . ? Si14 Si9 Si10 Si11 -76.50(18) . . . . ? Zn1 Si9 Si10 Si11 172.78(11) . . . . ? C19 Si10 Si11 Si16 160.6(3) . . . . ? C18 Si10 Si11 Si16 -84.3(3) . . . . ? Si9 Si10 Si11 Si16 38.00(19) . . . . ? C19 Si10 Si11 Si12 34.9(3) . . . . ? C18 Si10 Si11 Si12 150.0(3) . . . . ? Si9 Si10 Si11 Si12 -87.71(16) . . . . ? C19 Si10 Si11 Si15 -80.1(3) . . . . ? C18 Si10 Si11 Si15 35.0(3) . . . . ? Si9 Si10 Si11 Si15 157.30(13) . . . . ? Si16 Si11 Si12 C22 41.5(4) . . . . ? Si15 Si11 Si12 C22 -73.7(4) . . . . ? Si10 Si11 Si12 C22 170.3(3) . . . . ? Si16 Si11 Si12 C21 162.4(3) . . . . ? Si15 Si11 Si12 C21 47.2(3) . . . . ? Si10 Si11 Si12 C21 -68.8(3) . . . . ? Si16 Si11 Si12 C20 -78.1(5) . . . . ? Si15 Si11 Si12 C20 166.8(5) . . . . ? Si10 Si11 Si12 C20 50.8(5) . . . . ? Si14 Si9 Si13 C24 -162.1(3) . . . . ? Si10 Si9 Si13 C24 53.5(3) . . . . ? Zn1 Si9 Si13 C24 -59.7(3) . . . . ? Si14 Si9 Si13 C25 72.9(4) . . . . ? Si10 Si9 Si13 C25 -71.5(4) . . . . ? Zn1 Si9 Si13 C25 175.4(3) . . . . ? Si14 Si9 Si13 C23 -45.1(4) . . . . ? Si10 Si9 Si13 C23 170.5(3) . . . . ? Zn1 Si9 Si13 C23 57.4(3) . . . . ? Si13 Si9 Si14 C26 77.7(4) . . . . ? Si10 Si9 Si14 C26 -136.4(4) . . . . ? Zn1 Si9 Si14 C26 -22.5(4) . . . . ? Si13 Si9 Si14 C27 -42.5(4) . . . . ? Si10 Si9 Si14 C27 103.3(4) . . . . ? Zn1 Si9 Si14 C27 -142.7(4) . . . . ? Si13 Si9 Si14 C28 -167.5(4) . . . . ? Si10 Si9 Si14 C28 -21.7(4) . . . . ? Zn1 Si9 Si14 C28 92.3(4) . . . . ? Si16 Si11 Si15 C31 169.6(3) . . . . ? Si12 Si11 Si15 C31 -73.7(3) . . . . ? Si10 Si11 Si15 C31 45.3(3) . . . . ? Si16 Si11 Si15 C29 48.7(4) . . . . ? Si12 Si11 Si15 C29 165.3(4) . . . . ? Si10 Si11 Si15 C29 -75.7(4) . . . . ? Si16 Si11 Si15 C30 -70.0(4) . . . . ? Si12 Si11 Si15 C30 46.7(4) . . . . ? Si10 Si11 Si15 C30 165.7(3) . . . . ? Si12 Si11 Si16 C33 175.6(5) . . . . ? Si15 Si11 Si16 C33 -70.4(5) . . . . ? Si10 Si11 Si16 C33 48.8(5) . . . . ? Si12 Si11 Si16 C32 55.2(4) . . . . ? Si15 Si11 Si16 C32 169.2(4) . . . . ? Si10 Si11 Si16 C32 -71.5(4) . . . . ? Si12 Si11 Si16 C34 -64.3(4) . . . . ? Si15 Si11 Si16 C34 49.7(4) . . . . ? Si10 Si11 Si16 C34 168.9(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.592 _refine_diff_density_min -0.676 _refine_diff_density_rms 0.109