# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_cd212139 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H61 N3 O Si2 Zn' _chemical_formula_weight 661.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 17.997(2) _cell_length_b 18.266(2) _cell_length_c 14.8576(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4884.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1821 _cell_measurement_theta_min 4.526 _cell_measurement_theta_max 51.205 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.312 _exptl_crystal_size_mid 0.203 _exptl_crystal_size_min 0.075 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.899 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 0.574 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.29661 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9603 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1357 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9603 _reflns_number_gt 3900 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0863P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(2) _chemical_absolute_configuration ad _refine_ls_number_reflns 9603 _refine_ls_number_parameters 407 _refine_ls_number_restraints 62 _refine_ls_R_factor_all 0.1528 _refine_ls_R_factor_gt 0.0653 _refine_ls_wR_factor_ref 0.1742 _refine_ls_wR_factor_gt 0.1456 _refine_ls_goodness_of_fit_ref 0.808 _refine_ls_restrained_S_all 0.813 _refine_ls_shift/su_max 0.029 _refine_ls_shift/su_mean 0.001 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.017 0.466 -0.500 1777 249 ' ' _platon_squeeze_details ; ; 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 0.16981(4) 0.14658(4) 0.06885(5) 0.0700(2) Uani 1 1 d . . . Si1 Si 0.21119(12) 0.06757(11) -0.12078(13) 0.0837(6) Uani 1 1 d . . . Si2 Si 0.06634(11) 0.14456(13) -0.08881(12) 0.0843(6) Uani 1 1 d . . . N1 N 0.1804(3) 0.0695(3) 0.1723(3) 0.0716(13) Uani 1 1 d U . . N2 N 0.2696(3) 0.1914(3) 0.1210(4) 0.0785(15) Uani 1 1 d . . . N3 N 0.1516(3) 0.1121(2) -0.0507(3) 0.0703(14) Uani 1 1 d . . . O1 O 0.0921(2) 0.2037(2) 0.1244(3) 0.0713(12) Uani 1 1 d . . . C1 C 0.0761(3) 0.2050(4) 0.2100(5) 0.0660(17) Uani 1 1 d . . . C2 C 0.0465(4) 0.2661(4) 0.2535(5) 0.0790(19) Uani 1 1 d . . . C3 C 0.0358(4) 0.2654(4) 0.3457(5) 0.094(2) Uani 1 1 d . . . H3 H 0.0188 0.3078 0.3734 0.112 Uiso 1 1 calc R . . C4 C 0.0491(5) 0.2042(5) 0.3991(5) 0.098(2) Uani 1 1 d D A . C5 C 0.0742(4) 0.1448(5) 0.3561(4) 0.093(2) Uani 1 1 d . . . H5 H 0.0828 0.1030 0.3903 0.111 Uiso 1 1 calc R . . C6 C 0.0884(3) 0.1409(4) 0.2642(4) 0.0729(16) Uani 1 1 d . . . C7 C 0.1094(4) 0.0689(4) 0.2213(4) 0.0762(19) Uani 1 1 d . . . H7A H 0.1120 0.0319 0.2680 0.091 Uiso 1 1 calc R . . H7B H 0.0703 0.0547 0.1799 0.091 Uiso 1 1 calc R . . C8 C 0.2421(4) 0.0913(4) 0.2283(4) 0.082(2) Uani 1 1 d . . . H8A H 0.2641 0.0479 0.2550 0.099 Uiso 1 1 calc R . . H8B H 0.2237 0.1218 0.2768 0.099 Uiso 1 1 calc R . . C9 C 0.3040(4) 0.1345(4) 0.1754(5) 0.092(2) Uani 1 1 d . . . H9 H 0.3301 0.1004 0.1355 0.111 Uiso 1 1 calc R . . C10 C 0.3586(5) 0.1684(5) 0.2372(6) 0.120(3) Uani 1 1 d . . . H10A H 0.4067 0.1733 0.2085 0.144 Uiso 1 1 calc R . . H10B H 0.3640 0.1397 0.2917 0.144 Uiso 1 1 calc R . . C11 C 0.3260(6) 0.2413(6) 0.2571(6) 0.138(3) Uani 1 1 d . . . H11A H 0.3623 0.2797 0.2475 0.166 Uiso 1 1 calc R . . H11B H 0.3088 0.2436 0.3189 0.166 Uiso 1 1 calc R . . C12 C 0.2600(4) 0.2495(4) 0.1909(5) 0.099(2) Uani 1 1 d . . . H12A H 0.2132 0.2431 0.2223 0.118 Uiso 1 1 calc R . . H12B H 0.2605 0.2976 0.1633 0.118 Uiso 1 1 calc R . . C13 C 0.3223(4) 0.2187(4) 0.0567(5) 0.102(2) Uani 1 1 d . . . H13A H 0.3449 0.1777 0.0255 0.122 Uiso 1 1 calc R . . H13B H 0.3613 0.2447 0.0884 0.122 Uiso 1 1 calc R . . C14 C 0.2860(5) 0.2711(4) -0.0139(6) 0.123(3) Uani 1 1 d . . . H14A H 0.2440 0.2474 -0.0409 0.184 Uiso 1 1 calc R . . H14B H 0.3218 0.2830 -0.0596 0.184 Uiso 1 1 calc R . . H14C H 0.2700 0.3152 0.0155 0.184 Uiso 1 1 calc R . . C15 C 0.0315(7) 0.2027(7) 0.5021(6) 0.151(4) Uani 1 1 d DU . . C16 C 0.0386(17) 0.1291(12) 0.5517(19) 0.186(7) Uani 0.50 1 d PDU A 1 H16A H 0.0114 0.1289 0.6073 0.279 Uiso 0.50 1 d PR A 1 H16B H 0.0901 0.1195 0.5636 0.279 Uiso 0.50 1 d PR A 1 H16C H 0.0192 0.0919 0.5126 0.279 Uiso 0.50 1 d PR A 1 C17 C 0.0938(15) 0.2442(15) 0.5483(18) 0.189(8) Uani 0.50 1 d PDU A 1 H17A H 0.0877 0.2957 0.5381 0.283 Uiso 0.50 1 calc PR A 1 H17B H 0.1407 0.2285 0.5242 0.283 Uiso 0.50 1 calc PR A 1 H17C H 0.0925 0.2345 0.6118 0.283 Uiso 0.50 1 calc PR A 1 C18 C -0.0438(12) 0.2242(16) 0.5345(17) 0.189(7) Uani 0.50 1 d PDU A 1 H18A H -0.0805 0.1933 0.5071 0.283 Uiso 0.50 1 calc PR A 1 H18B H -0.0533 0.2743 0.5186 0.283 Uiso 0.50 1 calc PR A 1 H18C H -0.0460 0.2189 0.5987 0.283 Uiso 0.50 1 calc PR A 1 C16' C -0.0025(17) 0.1276(13) 0.5281(16) 0.174(7) Uani 0.50 1 d PDU A 2 H16D H -0.0232 0.1301 0.5876 0.261 Uiso 0.50 1 d PR A 2 H16E H 0.0364 0.0917 0.5268 0.261 Uiso 0.50 1 d PR A 2 H16F H -0.0407 0.1141 0.4861 0.261 Uiso 0.50 1 d PR A 2 C17' C 0.1115(13) 0.1886(16) 0.5503(19) 0.190(8) Uani 0.50 1 d PDU A 2 H17D H 0.1066 0.1952 0.6141 0.285 Uiso 0.50 1 calc PR A 2 H17E H 0.1473 0.2228 0.5271 0.285 Uiso 0.50 1 calc PR A 2 H17F H 0.1278 0.1396 0.5379 0.285 Uiso 0.50 1 calc PR A 2 C18' C 0.0031(17) 0.2765(12) 0.5389(15) 0.183(7) Uani 0.50 1 d PDU A 2 H18D H -0.0469 0.2853 0.5193 0.275 Uiso 0.50 1 d PR A 2 H18E H 0.0348 0.3150 0.5176 0.275 Uiso 0.50 1 d PR A 2 H18F H 0.0045 0.2751 0.6035 0.275 Uiso 0.50 1 d PR A 2 C19 C 0.0239(4) 0.3336(4) 0.1989(5) 0.087(2) Uani 1 1 d . . . C20 C 0.0923(4) 0.3670(4) 0.1517(5) 0.110(2) Uani 1 1 d . . . H20A H 0.1129 0.3320 0.1106 0.165 Uiso 1 1 calc R . . H20B H 0.1289 0.3799 0.1960 0.165 Uiso 1 1 calc R . . H20C H 0.0776 0.4101 0.1192 0.165 Uiso 1 1 calc R . . C21 C -0.0147(6) 0.3925(4) 0.2579(5) 0.121(3) Uani 1 1 d . . . H21A H -0.0315 0.4320 0.2204 0.181 Uiso 1 1 calc R . . H21B H 0.0199 0.4109 0.3015 0.181 Uiso 1 1 calc R . . H21C H -0.0564 0.3711 0.2884 0.181 Uiso 1 1 calc R . . C22 C -0.0329(4) 0.3128(4) 0.1279(5) 0.089(2) Uani 1 1 d . . . H22A H -0.0398 0.3530 0.0872 0.134 Uiso 1 1 calc R . . H22B H -0.0793 0.3013 0.1565 0.134 Uiso 1 1 calc R . . H22C H -0.0155 0.2709 0.0951 0.134 Uiso 1 1 calc R . . C23 C 0.1933(4) -0.0072(4) 0.1300(5) 0.092(2) Uani 1 1 d U . . H23A H 0.1540 -0.0162 0.0868 0.110 Uiso 1 1 calc R . . H23B H 0.2397 -0.0058 0.0968 0.110 Uiso 1 1 calc R . . C24 C 0.1963(3) -0.0714(2) 0.1943(3) 0.0793(19) Uani 1 1 d G . . C25 C 0.1315(2) -0.1071(3) 0.2203(4) 0.091(2) Uani 1 1 d G . . H25 H 0.0858 -0.0914 0.1984 0.109 Uiso 1 1 calc R . . C26 C 0.1351(4) -0.1663(3) 0.2789(4) 0.119(3) Uani 1 1 d G . . H26 H 0.0918 -0.1902 0.2963 0.142 Uiso 1 1 calc R . . C27 C 0.2034(5) -0.1898(2) 0.3116(3) 0.130(3) Uani 1 1 d G . . H27 H 0.2058 -0.2295 0.3508 0.155 Uiso 1 1 calc R . . C28 C 0.2682(4) -0.1541(3) 0.2856(4) 0.147(4) Uani 1 1 d G . . H28 H 0.3139 -0.1699 0.3075 0.177 Uiso 1 1 calc R . . C29 C 0.2646(3) -0.0949(3) 0.2270(4) 0.113(3) Uani 1 1 d G . . H29 H 0.3079 -0.0710 0.2096 0.135 Uiso 1 1 calc R . . C30 C 0.2398(5) 0.1222(5) -0.2197(5) 0.130(3) Uani 1 1 d . . . H30A H 0.1990 0.1259 -0.2611 0.195 Uiso 1 1 calc R . . H30B H 0.2810 0.0988 -0.2489 0.195 Uiso 1 1 calc R . . H30C H 0.2542 0.1704 -0.2005 0.195 Uiso 1 1 calc R . . C31 C 0.1756(6) -0.0228(4) -0.1612(7) 0.151(4) Uani 1 1 d . . . H31A H 0.1657 -0.0539 -0.1105 0.226 Uiso 1 1 calc R . . H31B H 0.2122 -0.0454 -0.1991 0.226 Uiso 1 1 calc R . . H31C H 0.1306 -0.0155 -0.1948 0.226 Uiso 1 1 calc R . . C32 C 0.3026(4) 0.0409(4) -0.0654(6) 0.119(3) Uani 1 1 d . . . H32A H 0.3253 0.0836 -0.0396 0.178 Uiso 1 1 calc R . . H32B H 0.3352 0.0202 -0.1097 0.178 Uiso 1 1 calc R . . H32C H 0.2933 0.0055 -0.0190 0.178 Uiso 1 1 calc R . . C33 C 0.0659(4) 0.2448(4) -0.0988(5) 0.116(3) Uani 1 1 d . . . H33A H 0.0656 0.2662 -0.0398 0.174 Uiso 1 1 calc R . . H33B H 0.0224 0.2601 -0.1312 0.174 Uiso 1 1 calc R . . H33C H 0.1095 0.2604 -0.1306 0.174 Uiso 1 1 calc R . . C34 C -0.0126(4) 0.1156(4) -0.0137(4) 0.091(2) Uani 1 1 d . . . H34A H -0.0154 0.0632 -0.0122 0.137 Uiso 1 1 calc R . . H34B H -0.0584 0.1351 -0.0367 0.137 Uiso 1 1 calc R . . H34C H -0.0044 0.1340 0.0460 0.137 Uiso 1 1 calc R . . C35 C 0.0418(5) 0.1146(5) -0.2045(5) 0.137(3) Uani 1 1 d . . . H35A H 0.0850 0.1171 -0.2422 0.205 Uiso 1 1 calc R . . H35B H 0.0038 0.1460 -0.2282 0.205 Uiso 1 1 calc R . . H35C H 0.0238 0.0651 -0.2028 0.205 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 0.0623(4) 0.0800(4) 0.0677(4) 0.0073(4) 0.0026(4) 0.0032(4) Si1 0.0765(14) 0.0920(14) 0.0826(13) 0.0017(11) 0.0203(11) -0.0044(11) Si2 0.0758(13) 0.1049(14) 0.0723(12) 0.0093(13) -0.0027(9) 0.0004(12) N1 0.049(4) 0.088(3) 0.077(3) 0.004(2) 0.000(3) 0.001(3) N2 0.062(4) 0.086(4) 0.088(4) 0.008(3) 0.014(3) 0.004(3) N3 0.071(4) 0.078(3) 0.062(3) -0.002(2) 0.004(2) 0.001(2) O1 0.076(3) 0.087(3) 0.051(3) 0.003(2) 0.002(2) 0.005(2) C1 0.048(4) 0.067(4) 0.083(5) 0.000(4) -0.007(3) 0.007(3) C2 0.071(5) 0.084(5) 0.082(5) 0.011(4) 0.000(4) -0.005(4) C3 0.096(6) 0.102(6) 0.083(5) -0.011(5) -0.010(4) 0.011(4) C4 0.106(7) 0.113(6) 0.075(5) -0.014(5) 0.001(4) 0.028(5) C5 0.094(5) 0.110(6) 0.074(5) 0.026(5) 0.008(4) -0.003(5) C6 0.061(4) 0.085(4) 0.072(4) 0.001(4) 0.009(3) -0.003(4) C7 0.079(5) 0.087(5) 0.063(4) 0.010(4) -0.004(4) 0.009(4) C8 0.079(6) 0.093(5) 0.075(5) 0.010(4) 0.000(4) 0.012(4) C9 0.060(5) 0.122(6) 0.095(5) 0.004(5) -0.004(4) 0.004(4) C10 0.087(7) 0.131(8) 0.141(8) 0.009(6) -0.020(5) 0.001(5) C11 0.097(7) 0.181(10) 0.136(7) -0.007(7) -0.045(7) -0.010(8) C12 0.074(6) 0.101(6) 0.121(6) 0.009(5) 0.006(5) -0.008(4) C13 0.078(5) 0.103(5) 0.124(6) -0.006(5) 0.008(6) 0.002(5) C14 0.117(7) 0.115(7) 0.136(7) 0.006(6) 0.043(6) -0.019(6) C15 0.179(11) 0.179(9) 0.093(6) -0.002(6) -0.014(6) 0.000(8) C16 0.193(18) 0.224(14) 0.139(13) 0.023(12) -0.027(13) -0.068(14) C17 0.229(16) 0.212(17) 0.126(12) -0.030(15) -0.001(12) -0.024(15) C18 0.182(16) 0.221(16) 0.163(13) -0.033(13) 0.022(13) -0.016(14) C16' 0.190(18) 0.230(14) 0.101(12) -0.002(11) -0.002(12) -0.088(14) C17' 0.220(16) 0.210(16) 0.139(12) -0.023(15) -0.005(12) -0.011(15) C18' 0.193(16) 0.221(16) 0.136(12) -0.041(13) 0.023(12) -0.003(14) C19 0.087(6) 0.082(5) 0.092(5) -0.002(4) -0.002(4) 0.011(4) C20 0.090(6) 0.110(6) 0.129(6) 0.023(5) 0.004(5) -0.010(5) C21 0.155(9) 0.087(5) 0.120(6) -0.012(5) 0.001(6) 0.024(5) C22 0.078(5) 0.092(5) 0.098(5) -0.003(4) -0.011(4) 0.015(4) C23 0.089(6) 0.093(4) 0.093(5) 0.000(3) 0.004(4) 0.014(4) C24 0.080(6) 0.074(4) 0.084(5) 0.015(4) 0.007(4) 0.007(4) C25 0.088(6) 0.081(5) 0.103(6) 0.008(4) 0.012(4) -0.013(4) C26 0.149(10) 0.093(7) 0.114(7) -0.006(5) 0.028(6) -0.016(6) C27 0.137(9) 0.101(6) 0.151(8) 0.015(6) 0.011(8) 0.001(7) C28 0.142(10) 0.122(7) 0.179(9) 0.042(7) -0.043(7) 0.004(7) C29 0.083(6) 0.106(6) 0.148(8) 0.029(5) -0.008(5) 0.007(5) C30 0.124(8) 0.173(9) 0.093(6) 0.018(5) 0.030(5) 0.006(6) C31 0.135(9) 0.133(7) 0.184(9) -0.045(7) 0.036(8) 0.004(7) C32 0.098(7) 0.131(6) 0.128(6) -0.003(6) 0.024(6) 0.006(5) C33 0.092(6) 0.143(7) 0.113(7) 0.025(5) 0.004(5) 0.014(5) C34 0.078(5) 0.111(6) 0.085(5) 0.001(4) 0.005(4) 0.007(4) C35 0.112(8) 0.197(10) 0.101(6) -0.003(6) -0.016(5) -0.005(6) _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 N3 1.913(5) . ? Zn1 O1 1.932(4) . ? Zn1 N1 2.093(5) . ? Zn1 N2 2.120(6) . ? Si1 N3 1.701(5) . ? Si1 C30 1.850(7) . ? Si1 C31 1.870(8) . ? Si1 C32 1.902(8) . ? Si2 N3 1.740(5) . ? Si2 C33 1.837(8) . ? Si2 C35 1.857(8) . ? Si2 C34 1.882(7) . ? N1 C8 1.444(8) . ? N1 C7 1.470(7) . ? N1 C23 1.553(8) . ? N2 C13 1.434(8) . ? N2 C9 1.455(8) . ? N2 C12 1.496(8) . ? O1 C1 1.304(7) . ? C1 C2 1.395(9) . ? C1 C6 1.437(9) . ? C2 C3 1.384(9) . ? C2 C19 1.531(9) . ? C3 C4 1.391(10) . ? C3 H3 0.9300 . ? C4 C5 1.337(9) . ? C4 C15 1.564(11) . ? C5 C6 1.392(8) . ? C5 H5 0.9300 . ? C6 C7 1.509(9) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.575(9) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.481(10) . ? C9 H9 0.9800 . ? C10 C11 1.484(11) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.548(10) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.563(10) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C18 1.490(16) . ? C15 C17 1.518(17) . ? C15 C16 1.539(17) . ? C15 C18' 1.542(16) . ? C15 C16' 1.551(16) . ? C15 C17' 1.629(17) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C16 H16D 1.2328 . ? C16 H16E 0.7772 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C18 H18D 1.1412 . ? C16' H16A 1.2039 . ? C16' H16C 0.7953 . ? C16' H16D 0.9600 . ? C16' H16E 0.9600 . ? C16' H16F 0.9600 . ? C17' H17D 0.9600 . ? C17' H17E 0.9600 . ? C17' H17F 0.9600 . ? C18' H18D 0.9600 . ? C18' H18E 0.9600 . ? C18' H18F 0.9600 . ? C19 C22 1.516(9) . ? C19 C20 1.544(10) . ? C19 C21 1.553(9) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.514(7) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.3900 . ? C24 C29 1.3900 . ? C25 C26 1.3900 . ? C25 H25 0.9300 . ? C26 C27 1.3900 . ? C26 H26 0.9300 . ? C27 C28 1.3900 . ? C27 H27 0.9300 . ? C28 C29 1.3900 . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Zn1 O1 116.80(19) . . ? N3 Zn1 N1 118.43(19) . . ? O1 Zn1 N1 96.62(18) . . ? N3 Zn1 N2 127.7(2) . . ? O1 Zn1 N2 104.4(2) . . ? N1 Zn1 N2 85.1(2) . . ? N3 Si1 C30 113.8(3) . . ? N3 Si1 C31 113.7(4) . . ? C30 Si1 C31 108.4(4) . . ? N3 Si1 C32 113.7(3) . . ? C30 Si1 C32 104.0(4) . . ? C31 Si1 C32 102.1(4) . . ? N3 Si2 C33 111.7(3) . . ? N3 Si2 C35 114.2(4) . . ? C33 Si2 C35 102.6(4) . . ? N3 Si2 C34 112.2(3) . . ? C33 Si2 C34 108.9(3) . . ? C35 Si2 C34 106.6(4) . . ? C8 N1 C7 112.6(5) . . ? C8 N1 C23 111.5(5) . . ? C7 N1 C23 109.0(5) . . ? C8 N1 Zn1 107.9(4) . . ? C7 N1 Zn1 106.9(4) . . ? C23 N1 Zn1 108.9(4) . . ? C13 N2 C9 109.7(6) . . ? C13 N2 C12 106.9(5) . . ? C9 N2 C12 99.8(5) . . ? C13 N2 Zn1 116.8(5) . . ? C9 N2 Zn1 106.7(4) . . ? C12 N2 Zn1 115.5(4) . . ? Si1 N3 Si2 121.3(3) . . ? Si1 N3 Zn1 128.1(3) . . ? Si2 N3 Zn1 109.9(2) . . ? C1 O1 Zn1 125.9(4) . . ? O1 C1 C2 123.3(6) . . ? O1 C1 C6 119.9(6) . . ? C2 C1 C6 116.8(6) . . ? C3 C2 C1 120.3(6) . . ? C3 C2 C19 119.7(7) . . ? C1 C2 C19 120.0(6) . . ? C2 C3 C4 123.2(7) . . ? C2 C3 H3 118.4 . . ? C4 C3 H3 118.4 . . ? C5 C4 C3 116.0(7) . . ? C5 C4 C15 121.4(8) . . ? C3 C4 C15 122.5(8) . . ? C4 C5 C6 124.9(7) . . ? C4 C5 H5 117.6 . . ? C6 C5 H5 117.6 . . ? C5 C6 C1 118.6(7) . . ? C5 C6 C7 120.3(7) . . ? C1 C6 C7 120.8(5) . . ? N1 C7 C6 114.9(5) . . ? N1 C7 H7A 108.5 . . ? C6 C7 H7A 108.5 . . ? N1 C7 H7B 108.5 . . ? C6 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? N1 C8 C9 113.2(5) . . ? N1 C8 H8A 108.9 . . ? C9 C8 H8A 108.9 . . ? N1 C8 H8B 108.9 . . ? C9 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? N2 C9 C10 109.1(7) . . ? N2 C9 C8 109.5(5) . . ? C10 C9 C8 111.7(6) . . ? N2 C9 H9 108.8 . . ? C10 C9 H9 108.8 . . ? C8 C9 H9 108.8 . . ? C9 C10 C11 103.7(7) . . ? C9 C10 H10A 111.0 . . ? C11 C10 H10A 111.0 . . ? C9 C10 H10B 111.0 . . ? C11 C10 H10B 111.0 . . ? H10A C10 H10B 109.0 . . ? C10 C11 C12 105.3(7) . . ? C10 C11 H11A 110.7 . . ? C12 C11 H11A 110.7 . . ? C10 C11 H11B 110.7 . . ? C12 C11 H11B 110.7 . . ? H11A C11 H11B 108.8 . . ? N2 C12 C11 106.5(7) . . ? N2 C12 H12A 110.4 . . ? C11 C12 H12A 110.4 . . ? N2 C12 H12B 110.4 . . ? C11 C12 H12B 110.4 . . ? H12A C12 H12B 108.6 . . ? N2 C13 C14 112.6(6) . . ? N2 C13 H13A 109.1 . . ? C14 C13 H13A 109.1 . . ? N2 C13 H13B 109.1 . . ? C14 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C18 C15 C17 113.2(17) . . ? C18 C15 C16 99(2) . . ? C17 C15 C16 99.1(16) . . ? C18 C15 C18' 49.7(12) . . ? C17 C15 C18' 69.4(15) . . ? C16 C15 C18' 128.4(18) . . ? C18 C15 C16' 78.1(17) . . ? C17 C15 C16' 128.4(17) . . ? C16 C15 C16' 30.8(14) . . ? C18' C15 C16' 123.6(18) . . ? C18 C15 C4 119.8(13) . . ? C17 C15 C4 106.5(14) . . ? C16 C15 C4 117.9(15) . . ? C18' C15 C4 113.6(12) . . ? C16' C15 C4 109.9(13) . . ? C18 C15 C17' 134.7(16) . . ? C17 C15 C17' 39.3(12) . . ? C16 C15 C17' 65.1(14) . . ? C18' C15 C17' 106.0(16) . . ? C16' C15 C17' 95.8(17) . . ? C4 C15 C17' 104.7(13) . . ? C15 C16 H16A 111.9 . . ? C15 C16 H16B 109.1 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 107.4 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C16 H16D 96.8 . . ? H16A C16 H16D 33.8 . . ? H16B C16 H16D 142.6 . . ? H16C C16 H16D 86.8 . . ? C15 C16 H16E 122.3 . . ? H16A C16 H16E 112.4 . . ? H16B C16 H16E 88.6 . . ? H16C C16 H16E 21.8 . . ? H16D C16 H16E 100.0 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? C15 C18 H18D 103.8 . . ? H18A C18 H18D 117.2 . . ? H18B C18 H18D 8.0 . . ? H18C C18 H18D 107.1 . . ? C15 C16' H16A 98.3 . . ? C15 C16' H16C 117.4 . . ? H16A C16' H16C 101.3 . . ? C15 C16' H16D 109.9 . . ? H16A C16' H16D 34.9 . . ? H16C C16' H16D 119.7 . . ? C15 C16' H16E 108.1 . . ? H16A C16' H16E 83.1 . . ? H16C C16' H16E 22.2 . . ? H16D C16' H16E 109.5 . . ? C15 C16' H16F 110.4 . . ? H16A C16' H16F 142.1 . . ? H16C C16' H16F 87.3 . . ? H16D C16' H16F 109.5 . . ? H16E C16' H16F 109.5 . . ? C15 C17' H16B 87.6 . . ? C15 C17' H17D 109.5 . . ? C15 C17' H17E 109.5 . . ? H17D C17' H17E 109.5 . . ? C15 C17' H17F 109.5 . . ? H17D C17' H17F 109.5 . . ? H17E C17' H17F 109.5 . . ? C15 C18' H18D 110.5 . . ? C15 C18' H18E 109.1 . . ? H18D C18' H18E 109.5 . . ? C15 C18' H18F 108.8 . . ? H18D C18' H18F 109.5 . . ? H18E C18' H18F 109.5 . . ? C22 C19 C2 110.3(6) . . ? C22 C19 C20 108.7(6) . . ? C2 C19 C20 110.3(6) . . ? C22 C19 C21 105.4(6) . . ? C2 C19 C21 112.2(6) . . ? C20 C19 C21 109.8(6) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 N1 116.7(5) . . ? C24 C23 H23A 108.1 . . ? N1 C23 H23A 108.1 . . ? C24 C23 H23B 108.1 . . ? N1 C23 H23B 108.1 . . ? H23A C23 H23B 107.3 . . ? C25 C24 C29 120.0 . . ? C25 C24 C23 120.6(5) . . ? C29 C24 C23 119.4(5) . . ? C24 C25 C26 120.0 . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C25 C26 C27 120.0 . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C26 C27 C28 120.0 . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C29 C28 C27 120.0 . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C24 120.0 . . ? C28 C29 H29 120.0 . . ? C24 C29 H29 120.0 . . ? Si1 C30 H30A 109.5 . . ? Si1 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si1 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si1 C31 H31A 109.5 . . ? Si1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si1 C32 H32A 109.5 . . ? Si1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si2 C33 H33A 109.5 . . ? Si2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si2 C34 H34A 109.5 . . ? Si2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si2 C35 H35A 109.5 . . ? Si2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si2 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? 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 N3 Zn1 N1 C8 136.9(4) . . . . ? O1 Zn1 N1 C8 -97.7(4) . . . . ? N2 Zn1 N1 C8 6.3(4) . . . . ? N3 Zn1 N1 C7 -101.7(4) . . . . ? O1 Zn1 N1 C7 23.7(4) . . . . ? N2 Zn1 N1 C7 127.6(4) . . . . ? N3 Zn1 N1 C23 15.8(5) . . . . ? O1 Zn1 N1 C23 141.2(4) . . . . ? N2 Zn1 N1 C23 -114.8(4) . . . . ? N3 Zn1 N2 C13 19.5(6) . . . . ? O1 Zn1 N2 C13 -122.4(5) . . . . ? N1 Zn1 N2 C13 142.0(5) . . . . ? N3 Zn1 N2 C9 -103.6(4) . . . . ? O1 Zn1 N2 C9 114.5(4) . . . . ? N1 Zn1 N2 C9 18.9(4) . . . . ? N3 Zn1 N2 C12 146.6(4) . . . . ? O1 Zn1 N2 C12 4.7(5) . . . . ? N1 Zn1 N2 C12 -90.9(5) . . . . ? C30 Si1 N3 Si2 58.6(5) . . . . ? C31 Si1 N3 Si2 -66.2(5) . . . . ? C32 Si1 N3 Si2 177.5(3) . . . . ? C30 Si1 N3 Zn1 -111.5(4) . . . . ? C31 Si1 N3 Zn1 123.7(5) . . . . ? C32 Si1 N3 Zn1 7.3(5) . . . . ? C33 Si2 N3 Si1 -107.4(4) . . . . ? C35 Si2 N3 Si1 8.5(5) . . . . ? C34 Si2 N3 Si1 130.0(4) . . . . ? C33 Si2 N3 Zn1 64.3(4) . . . . ? C35 Si2 N3 Zn1 -179.8(3) . . . . ? C34 Si2 N3 Zn1 -58.3(3) . . . . ? O1 Zn1 N3 Si1 174.0(3) . . . . ? N1 Zn1 N3 Si1 -71.2(4) . . . . ? N2 Zn1 N3 Si1 36.0(4) . . . . ? O1 Zn1 N3 Si2 3.0(3) . . . . ? N1 Zn1 N3 Si2 117.8(3) . . . . ? N2 Zn1 N3 Si2 -135.0(3) . . . . ? N3 Zn1 O1 C1 147.4(5) . . . . ? N1 Zn1 O1 C1 20.9(5) . . . . ? N2 Zn1 O1 C1 -65.8(5) . . . . ? Zn1 O1 C1 C2 149.8(5) . . . . ? Zn1 O1 C1 C6 -30.7(8) . . . . ? O1 C1 C2 C3 -175.5(6) . . . . ? C6 C1 C2 C3 5.0(10) . . . . ? O1 C1 C2 C19 6.2(10) . . . . ? C6 C1 C2 C19 -173.3(6) . . . . ? C1 C2 C3 C4 -3.8(11) . . . . ? C19 C2 C3 C4 174.5(7) . . . . ? C2 C3 C4 C5 0.6(12) . . . . ? C2 C3 C4 C15 -175.7(8) . . . . ? C3 C4 C5 C6 1.0(12) . . . . ? C15 C4 C5 C6 177.4(8) . . . . ? C4 C5 C6 C1 0.5(11) . . . . ? C4 C5 C6 C7 -174.0(7) . . . . ? O1 C1 C6 C5 177.0(6) . . . . ? C2 C1 C6 C5 -3.4(9) . . . . ? O1 C1 C6 C7 -8.6(9) . . . . ? C2 C1 C6 C7 171.0(6) . . . . ? C8 N1 C7 C6 57.3(7) . . . . ? C23 N1 C7 C6 -178.5(5) . . . . ? Zn1 N1 C7 C6 -61.0(6) . . . . ? C5 C6 C7 N1 -123.6(6) . . . . ? C1 C6 C7 N1 62.1(8) . . . . ? C7 N1 C8 C9 -147.3(6) . . . . ? C23 N1 C8 C9 89.9(7) . . . . ? Zn1 N1 C8 C9 -29.6(7) . . . . ? C13 N2 C9 C10 71.5(8) . . . . ? C12 N2 C9 C10 -40.6(7) . . . . ? Zn1 N2 C9 C10 -161.1(5) . . . . ? C13 N2 C9 C8 -166.0(6) . . . . ? C12 N2 C9 C8 82.0(7) . . . . ? Zn1 N2 C9 C8 -38.5(6) . . . . ? N1 C8 C9 N2 47.7(8) . . . . ? N1 C8 C9 C10 168.8(6) . . . . ? N2 C9 C10 C11 32.4(9) . . . . ? C8 C9 C10 C11 -88.9(8) . . . . ? C9 C10 C11 C12 -9.7(9) . . . . ? C13 N2 C12 C11 -81.7(7) . . . . ? C9 N2 C12 C11 32.6(7) . . . . ? Zn1 N2 C12 C11 146.5(5) . . . . ? C10 C11 C12 N2 -14.5(9) . . . . ? C9 N2 C13 C14 171.0(6) . . . . ? C12 N2 C13 C14 -81.6(7) . . . . ? Zn1 N2 C13 C14 49.5(7) . . . . ? C5 C4 C15 C18 -124.2(17) . . . . ? C3 C4 C15 C18 52.0(19) . . . . ? C5 C4 C15 C17 105.8(16) . . . . ? C3 C4 C15 C17 -78.0(16) . . . . ? C5 C4 C15 C16 -4.2(19) . . . . ? C3 C4 C15 C16 171.9(14) . . . . ? C5 C4 C15 C18' -179.9(15) . . . . ? C3 C4 C15 C18' -3.8(18) . . . . ? C5 C4 C15 C16' -36.8(18) . . . . ? C3 C4 C15 C16' 139.3(15) . . . . ? C5 C4 C15 C17' 65.0(16) . . . . ? C3 C4 C15 C17' -118.8(13) . . . . ? C3 C2 C19 C22 -121.0(7) . . . . ? C1 C2 C19 C22 57.3(9) . . . . ? C3 C2 C19 C20 118.9(7) . . . . ? C1 C2 C19 C20 -62.8(8) . . . . ? C3 C2 C19 C21 -3.9(10) . . . . ? C1 C2 C19 C21 174.4(7) . . . . ? C8 N1 C23 C24 65.8(7) . . . . ? C7 N1 C23 C24 -59.1(7) . . . . ? Zn1 N1 C23 C24 -175.3(4) . . . . ? N1 C23 C24 C25 86.7(6) . . . . ? N1 C23 C24 C29 -93.7(6) . . . . ? C29 C24 C25 C26 0.0 . . . . ? C23 C24 C25 C26 179.6(5) . . . . ? C24 C25 C26 C27 0.0 . . . . ? C25 C26 C27 C28 0.0 . . . . ? C26 C27 C28 C29 0.0 . . . . ? C27 C28 C29 C24 0.0 . . . . ? C25 C24 C29 C28 0.0 . . . . ? C23 C24 C29 C28 -179.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.327 _refine_diff_density_min -0.232 _refine_diff_density_rms 0.067 _database_code_depnum_ccdc_archive 'CCDC 936900' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_cd212576 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H65 N3 O Si2 Zn' _chemical_formula_weight 833.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+1/4' 'y, -x, z+3/4' _cell_length_a 19.5766(7) _cell_length_b 19.5766(7) _cell_length_c 13.6033(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5213.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4886 _cell_measurement_theta_min 4.653 _cell_measurement_theta_max 37.746 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.312 _exptl_crystal_size_mid 0.158 _exptl_crystal_size_min 0.113 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.062 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1784 _exptl_absorpt_coefficient_mu 0.551 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.11145 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10207 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0714 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10207 _reflns_number_gt 7275 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0640P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.024(11) _chemical_absolute_configuration ad _refine_ls_number_reflns 10207 _refine_ls_number_parameters 532 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.0757 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1203 _refine_ls_wR_factor_gt 0.1118 _refine_ls_goodness_of_fit_ref 0.940 _refine_ls_restrained_S_all 0.941 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 -0.019 578 94 ' ' 2 0.500 1.000 -0.028 578 94 ' ' 3 0.601 0.481 -0.072 25 1 ' ' 4 0.519 0.601 0.178 25 1 ' ' 5 0.283 0.444 0.235 6 0 ' ' 6 0.399 0.519 0.428 25 1 ' ' 7 0.556 0.283 0.485 6 0 ' ' 8 0.481 0.399 0.678 25 1 ' ' 9 0.717 0.556 0.735 6 0 ' ' 10 0.444 0.717 0.985 5 0 ' ' _platon_squeeze_details ; ; 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 0.75268(2) 0.69247(2) 0.15998(3) 0.04810(12) Uani 1 1 d . . . Si1 Si 0.63370(6) 0.78404(6) 0.10825(10) 0.0630(3) Uani 1 1 d . . . Si2 Si 0.66358(8) 0.67697(7) -0.04237(11) 0.0815(4) Uani 1 1 d . . . N1 N 0.74304(15) 0.59525(15) 0.2313(2) 0.0511(8) Uani 1 1 d . . . N2 N 0.85406(17) 0.65828(16) 0.1288(2) 0.0555(8) Uani 1 1 d . . . N3 N 0.68223(16) 0.71616(17) 0.0655(2) 0.0569(8) Uani 1 1 d . . . O1 O 0.76355(12) 0.74809(11) 0.27892(17) 0.0446(6) Uani 1 1 d . . . C1 C 0.77727(16) 0.72428(17) 0.3678(3) 0.0400(8) Uani 1 1 d . . . C2 C 0.80831(16) 0.76643(16) 0.4412(3) 0.0410(8) Uani 1 1 d . . . C3 C 0.82484(18) 0.73620(18) 0.5301(3) 0.0467(8) Uani 1 1 d . . . H3 H 0.8465 0.7632 0.5769 0.056 Uiso 1 1 calc R . . C4 C 0.81163(18) 0.66888(19) 0.5546(3) 0.0505(9) Uani 1 1 d . . . C5 C 0.77840(18) 0.63067(18) 0.4857(3) 0.0503(9) Uani 1 1 d . . . H5 H 0.7677 0.5856 0.5006 0.060 Uiso 1 1 calc R . . C6 C 0.75985(17) 0.65622(17) 0.3945(3) 0.0453(8) Uani 1 1 d . . . C7 C 0.71553(19) 0.61394(18) 0.3307(3) 0.0539(9) Uani 1 1 d . . . H7A H 0.6728 0.6382 0.3212 0.065 Uiso 1 1 calc R . . H7B H 0.7051 0.5720 0.3656 0.065 Uiso 1 1 calc R . . C8 C 0.8127(2) 0.56714(19) 0.2384(3) 0.0591(10) Uani 1 1 d . . . H8A H 0.8101 0.5180 0.2462 0.071 Uiso 1 1 calc R . . H8B H 0.8350 0.5858 0.2961 0.071 Uiso 1 1 calc R . . C9 C 0.8551(2) 0.58356(19) 0.1483(3) 0.0627(10) Uani 1 1 d . . . H9 H 0.8371 0.5588 0.0913 0.075 Uiso 1 1 calc R . . C10 C 0.9305(2) 0.5647(2) 0.1648(4) 0.0818(13) Uani 1 1 d . . . H10A H 0.9522 0.5511 0.1037 0.098 Uiso 1 1 calc R . . H10B H 0.9350 0.5279 0.2121 0.098 Uiso 1 1 calc R . . C11 C 0.9620(2) 0.6316(3) 0.2048(5) 0.0897(16) Uani 1 1 d . . . H11A H 0.9771 0.6256 0.2722 0.108 Uiso 1 1 calc R . . H11B H 1.0007 0.6454 0.1651 0.108 Uiso 1 1 calc R . . C12 C 0.90503(19) 0.6852(2) 0.1992(3) 0.0612(10) Uani 1 1 d . . . H12A H 0.8844 0.6918 0.2634 0.073 Uiso 1 1 calc R . . H12B H 0.9230 0.7285 0.1765 0.073 Uiso 1 1 calc R . . C13 C 0.8302(2) 0.6398(2) 0.6535(4) 0.0732(12) Uani 1 1 d . . . H13A H 0.8113 0.6680 0.7044 0.110 Uiso 1 1 calc R . . H13B H 0.8790 0.6385 0.6600 0.110 Uiso 1 1 calc R . . H13C H 0.8123 0.5943 0.6591 0.110 Uiso 1 1 calc R . . C14 C 0.6944(2) 0.5496(2) 0.1788(3) 0.0699(12) Uani 1 1 d . . . H14A H 0.6565 0.5771 0.1559 0.084 Uiso 1 1 calc R . . H14B H 0.7174 0.5315 0.1213 0.084 Uiso 1 1 calc R . . C15 C 0.6663(2) 0.4911(2) 0.2359(3) 0.0674(11) Uani 1 1 d U . . C16 C 0.6027(3) 0.4975(3) 0.2824(6) 0.113(2) Uani 1 1 d . . . H16 H 0.5772 0.5374 0.2759 0.136 Uiso 1 1 calc R . . C17 C 0.5785(4) 0.4442(4) 0.3375(7) 0.149(3) Uani 1 1 d . . . H17 H 0.5357 0.4476 0.3667 0.179 Uiso 1 1 calc R . . C18 C 0.6152(5) 0.3875(4) 0.3503(6) 0.134(3) Uani 1 1 d . . . H18 H 0.5977 0.3525 0.3891 0.161 Uiso 1 1 calc R . . C19 C 0.6775(4) 0.3800(2) 0.3078(5) 0.1002(18) Uani 1 1 d . . . H19 H 0.7033 0.3408 0.3182 0.120 Uiso 1 1 calc R . . C20 C 0.7010(3) 0.4315(2) 0.2492(4) 0.0772(13) Uani 1 1 d U . . H20 H 0.7426 0.4257 0.2170 0.093 Uiso 1 1 calc R . . C21 C 0.8775(3) 0.6740(3) 0.0284(4) 0.0876(16) Uani 1 1 d . B . H21A H 0.8543 0.6437 -0.0170 0.105 Uiso 1 1 calc R . . H21B H 0.9260 0.6641 0.0243 0.105 Uiso 1 1 calc R . . C22 C 0.8663(3) 0.7456(3) -0.0043(4) 0.1032(16) Uani 1 1 d DU . . H22A H 0.8879 0.7775 0.0405 0.124 Uiso 0.60 1 calc PR A 1 H22B H 0.8179 0.7559 -0.0079 0.124 Uiso 0.60 1 calc PR A 1 H22C H 0.9010 0.7685 0.0315 0.124 Uiso 0.40 1 d PR A 2 H22D H 0.8250 0.7575 0.0315 0.124 Uiso 0.40 1 d PR A 2 C23 C 0.8996(5) 0.7490(4) -0.1073(6) 0.1090(19) Uani 0.75 1 d PDU B 1 H23A H 0.9489 0.7486 -0.1004 0.131 Uiso 0.75 1 calc PR B 1 H23B H 0.8864 0.7091 -0.1450 0.131 Uiso 0.75 1 calc PR B 1 C24 C 0.8778(6) 0.8137(6) -0.1626(9) 0.117(3) Uani 0.60 1 d PDU B 1 H24A H 0.8289 0.8146 -0.1686 0.175 Uiso 0.60 1 calc PR B 1 H24B H 0.8979 0.8138 -0.2269 0.175 Uiso 0.60 1 calc PR B 1 H24C H 0.8928 0.8533 -0.1270 0.175 Uiso 0.60 1 calc PR B 1 C23' C 0.8526(12) 0.7858(13) -0.1024(14) 0.111(2) Uani 0.25 1 d PDU B 2 H23C H 0.8078 0.7742 -0.1277 0.133 Uiso 0.25 1 calc PR B 2 H23D H 0.8535 0.8346 -0.0894 0.133 Uiso 0.25 1 calc PR B 2 C24' C 0.9051(9) 0.7686(11) -0.1758(14) 0.120(3) Uani 0.40 1 d PDU B 2 H24D H 0.9425 0.8001 -0.1704 0.181 Uiso 0.40 1 calc PR B 2 H24E H 0.8857 0.7714 -0.2405 0.181 Uiso 0.40 1 calc PR B 2 H24F H 0.9213 0.7230 -0.1643 0.181 Uiso 0.40 1 calc PR B 2 C25 C 0.82378(16) 0.84226(16) 0.4193(3) 0.0423(7) Uani 1 1 d . . . C26 C 0.8497(2) 0.88011(18) 0.5133(3) 0.0525(9) Uani 1 1 d . . . C27 C 0.8065(2) 0.8869(2) 0.5937(3) 0.0628(11) Uani 1 1 d . . . H27 H 0.7636 0.8664 0.5914 0.075 Uiso 1 1 calc R . . C28 C 0.8243(3) 0.9220(3) 0.6745(4) 0.0872(15) Uani 1 1 d . . . H28 H 0.7934 0.9255 0.7262 0.105 Uiso 1 1 calc R . . C29 C 0.8874(3) 0.9528(3) 0.6828(4) 0.0952(17) Uani 1 1 d . . . H29 H 0.8997 0.9758 0.7400 0.114 Uiso 1 1 calc R . . C30 C 0.9316(3) 0.9490(2) 0.6048(5) 0.0917(16) Uani 1 1 d . . . H30 H 0.9737 0.9710 0.6075 0.110 Uiso 1 1 calc R . . C31 C 0.9130(2) 0.9118(2) 0.5210(3) 0.0616(10) Uani 1 1 d . . . H31 H 0.9438 0.9082 0.4692 0.074 Uiso 1 1 calc R . . C32 C 0.75935(16) 0.88342(16) 0.3929(3) 0.0418(8) Uani 1 1 d . . . C33 C 0.7642(2) 0.95148(19) 0.3696(3) 0.0572(10) Uani 1 1 d . . . H33 H 0.8071 0.9715 0.3639 0.069 Uiso 1 1 calc R . . C34 C 0.7059(2) 0.9913(2) 0.3545(4) 0.0711(12) Uani 1 1 d . . . H34 H 0.7105 1.0369 0.3366 0.085 Uiso 1 1 calc R . . C35 C 0.6422(2) 0.9635(2) 0.3656(4) 0.0730(12) Uani 1 1 d . . . H35 H 0.6034 0.9904 0.3576 0.088 Uiso 1 1 calc R . . C36 C 0.6365(2) 0.8954(2) 0.3888(3) 0.0627(11) Uani 1 1 d . . . H36 H 0.5935 0.8757 0.3957 0.075 Uiso 1 1 calc R . . C37 C 0.69420(18) 0.85658(18) 0.4017(3) 0.0512(9) Uani 1 1 d . . . H37 H 0.6893 0.8105 0.4170 0.061 Uiso 1 1 calc R . . C38 C 0.88009(16) 0.84431(16) 0.3394(3) 0.0393(7) Uani 1 1 d . . . C39 C 0.87530(19) 0.87839(19) 0.2535(3) 0.0528(9) Uani 1 1 d . . . H39 H 0.8344 0.8998 0.2373 0.063 Uiso 1 1 calc R . . C40 C 0.93104(19) 0.8824(2) 0.1870(3) 0.0608(10) Uani 1 1 d . . . H40 H 0.9260 0.9051 0.1275 0.073 Uiso 1 1 calc R . . C41 C 0.9908(2) 0.8535(2) 0.2100(3) 0.0669(11) Uani 1 1 d . . . H41 H 1.0283 0.8582 0.1686 0.080 Uiso 1 1 calc R . . C42 C 0.99612(19) 0.8158(2) 0.2977(3) 0.0602(11) Uani 1 1 d . . . H42 H 1.0370 0.7942 0.3135 0.072 Uiso 1 1 calc R . . C43 C 0.94206(17) 0.81091(18) 0.3591(3) 0.0494(9) Uani 1 1 d . . . H43 H 0.9460 0.7847 0.4158 0.059 Uiso 1 1 calc R . . C44 C 0.5888(2) 0.7607(3) 0.2240(4) 0.0842(14) Uani 1 1 d . . . H44A H 0.5633 0.7193 0.2141 0.126 Uiso 1 1 calc R . . H44B H 0.5582 0.7968 0.2423 0.126 Uiso 1 1 calc R . . H44C H 0.6217 0.7538 0.2754 0.126 Uiso 1 1 calc R . . C45 C 0.6885(2) 0.8604(2) 0.1276(4) 0.0766(13) Uani 1 1 d . . . H45A H 0.7225 0.8503 0.1765 0.115 Uiso 1 1 calc R . . H45B H 0.6608 0.8979 0.1494 0.115 Uiso 1 1 calc R . . H45C H 0.7106 0.8723 0.0670 0.115 Uiso 1 1 calc R . . C46 C 0.5622(3) 0.8141(4) 0.0244(5) 0.125(2) Uani 1 1 d . . . H46A H 0.5802 0.8455 -0.0232 0.188 Uiso 1 1 calc R . . H46B H 0.5277 0.8364 0.0627 0.188 Uiso 1 1 calc R . . H46C H 0.5427 0.7755 -0.0089 0.188 Uiso 1 1 calc R . . C47 C 0.6678(4) 0.7355(4) -0.1490(5) 0.136(3) Uani 1 1 d . . . H47A H 0.6306 0.7673 -0.1458 0.205 Uiso 1 1 calc R . . H47B H 0.6647 0.7096 -0.2087 0.205 Uiso 1 1 calc R . . H47C H 0.7103 0.7599 -0.1478 0.205 Uiso 1 1 calc R . . C48 C 0.7232(3) 0.6082(3) -0.0782(5) 0.110(2) Uani 1 1 d . . . H48A H 0.7655 0.6138 -0.0435 0.165 Uiso 1 1 calc R . . H48B H 0.7314 0.6104 -0.1477 0.165 Uiso 1 1 calc R . . H48C H 0.7036 0.5647 -0.0620 0.165 Uiso 1 1 calc R . . C49 C 0.5787(4) 0.6337(4) -0.0407(7) 0.154(3) Uani 1 1 d . . . H49A H 0.5833 0.5893 -0.0113 0.231 Uiso 1 1 calc R . . H49B H 0.5622 0.6290 -0.1067 0.231 Uiso 1 1 calc R . . H49C H 0.5471 0.6605 -0.0031 0.231 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 0.0559(3) 0.0481(2) 0.0403(2) -0.0011(2) -0.0036(2) -0.0069(2) Si1 0.0531(6) 0.0754(8) 0.0607(7) 0.0036(6) -0.0106(6) 0.0005(6) Si2 0.0967(10) 0.0856(9) 0.0622(8) -0.0100(7) -0.0287(7) -0.0133(8) N1 0.0587(19) 0.0412(16) 0.053(2) -0.0013(14) -0.0023(15) -0.0084(14) N2 0.066(2) 0.0565(19) 0.045(2) -0.0085(14) 0.0097(15) -0.0079(15) N3 0.060(2) 0.0612(19) 0.049(2) 0.0001(16) -0.0102(16) -0.0087(15) O1 0.0572(15) 0.0398(13) 0.0367(14) -0.0012(10) -0.0041(11) 0.0023(10) C1 0.0366(17) 0.0446(19) 0.0387(19) 0.0037(15) 0.0049(14) 0.0037(14) C2 0.0365(18) 0.0435(19) 0.043(2) 0.0006(15) 0.0057(14) 0.0028(14) C3 0.046(2) 0.053(2) 0.041(2) 0.0001(17) -0.0008(16) 0.0001(16) C4 0.052(2) 0.059(2) 0.041(2) 0.0089(18) 0.0033(17) 0.0037(17) C5 0.049(2) 0.047(2) 0.055(2) 0.0125(18) 0.0105(18) 0.0010(16) C6 0.0466(19) 0.0440(19) 0.045(2) 0.0066(16) 0.0075(16) -0.0011(15) C7 0.063(2) 0.042(2) 0.057(3) 0.0031(18) 0.0050(19) -0.0088(17) C8 0.070(3) 0.042(2) 0.065(3) -0.0051(19) 0.000(2) 0.0006(18) C9 0.071(3) 0.057(2) 0.060(3) -0.020(2) 0.003(2) 0.0016(19) C10 0.083(3) 0.077(3) 0.085(3) -0.017(3) 0.014(3) 0.010(2) C11 0.060(3) 0.100(4) 0.110(4) -0.015(3) -0.004(3) 0.006(3) C12 0.056(2) 0.073(3) 0.055(2) -0.016(2) 0.0030(19) -0.005(2) C13 0.083(3) 0.080(3) 0.056(3) 0.024(2) -0.003(3) -0.006(2) C14 0.088(3) 0.057(2) 0.065(3) -0.003(2) -0.007(2) -0.020(2) C15 0.074(3) 0.054(2) 0.074(3) -0.013(2) 0.000(2) -0.0252(18) C16 0.094(4) 0.092(4) 0.154(6) -0.016(4) 0.011(4) -0.035(3) C17 0.121(5) 0.106(5) 0.220(9) -0.034(6) 0.078(6) -0.058(5) C18 0.187(8) 0.100(5) 0.114(5) -0.013(4) 0.047(6) -0.083(5) C19 0.143(5) 0.050(3) 0.108(5) 0.004(3) 0.012(4) -0.028(3) C20 0.095(3) 0.054(2) 0.082(3) -0.015(2) 0.014(3) -0.024(2) C21 0.099(4) 0.107(4) 0.057(3) -0.024(3) 0.020(3) -0.026(3) C22 0.120(4) 0.118(4) 0.072(3) 0.032(3) -0.002(3) -0.018(3) C23 0.125(4) 0.119(4) 0.083(4) 0.033(3) 0.000(4) -0.013(3) C24 0.136(6) 0.113(6) 0.100(5) 0.025(5) 0.009(5) -0.005(5) C23' 0.127(5) 0.121(5) 0.085(4) 0.030(4) 0.003(4) -0.011(4) C24' 0.139(7) 0.131(7) 0.091(6) 0.021(6) 0.002(6) -0.011(6) C25 0.0457(18) 0.0450(18) 0.0364(19) -0.0063(16) -0.0010(16) -0.0012(14) C26 0.065(2) 0.046(2) 0.046(2) -0.0058(17) -0.0088(19) 0.0037(18) C27 0.072(3) 0.071(3) 0.046(3) -0.009(2) 0.000(2) 0.011(2) C28 0.102(4) 0.100(4) 0.059(3) -0.030(3) -0.005(3) 0.021(3) C29 0.130(5) 0.098(4) 0.057(3) -0.028(3) -0.016(3) 0.004(4) C30 0.110(4) 0.074(3) 0.091(4) -0.010(3) -0.036(4) -0.017(3) C31 0.066(3) 0.061(2) 0.057(3) -0.008(2) -0.009(2) -0.009(2) C32 0.0431(18) 0.0404(18) 0.042(2) -0.0061(15) 0.0011(15) 0.0021(14) C33 0.057(2) 0.053(2) 0.062(3) -0.0048(19) 0.0070(19) 0.0025(18) C34 0.088(3) 0.052(2) 0.073(3) 0.003(2) 0.008(3) 0.023(2) C35 0.059(3) 0.072(3) 0.087(3) 0.002(2) 0.005(2) 0.021(2) C36 0.047(2) 0.069(3) 0.072(3) 0.002(2) 0.007(2) 0.0124(19) C37 0.055(2) 0.0480(19) 0.050(2) -0.0005(19) 0.0080(19) 0.0042(16) C38 0.0412(18) 0.0370(17) 0.040(2) -0.0045(15) -0.0021(15) -0.0074(14) C39 0.050(2) 0.057(2) 0.051(2) 0.0037(19) -0.0022(18) 0.0023(17) C40 0.055(2) 0.078(3) 0.049(3) 0.013(2) 0.0069(18) -0.004(2) C41 0.053(2) 0.084(3) 0.064(3) -0.002(2) 0.015(2) -0.010(2) C42 0.041(2) 0.074(3) 0.065(3) -0.004(2) -0.008(2) 0.0000(18) C43 0.046(2) 0.051(2) 0.052(2) -0.0037(18) 0.0021(18) 0.0003(16) C44 0.062(3) 0.102(4) 0.088(4) -0.007(3) 0.008(3) -0.016(3) C45 0.090(3) 0.065(3) 0.075(3) 0.009(2) -0.001(2) 0.001(2) C46 0.096(4) 0.150(6) 0.129(6) 0.009(5) -0.050(4) 0.038(4) C47 0.210(8) 0.136(6) 0.064(4) -0.002(4) -0.029(4) 0.039(5) C48 0.178(6) 0.085(3) 0.068(4) -0.026(3) -0.019(4) 0.004(4) C49 0.118(5) 0.176(7) 0.168(8) -0.038(6) -0.040(5) -0.057(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 N3 1.941(3) . ? Zn1 O1 1.962(2) . ? Zn1 N2 2.137(3) . ? Zn1 N1 2.145(3) . ? Si1 N3 1.734(4) . ? Si1 C45 1.859(5) . ? Si1 C44 1.861(5) . ? Si1 C46 1.899(5) . ? Si2 N3 1.696(3) . ? Si2 C48 1.847(6) . ? Si2 C47 1.850(7) . ? Si2 C49 1.865(6) . ? N1 C8 1.474(5) . ? N1 C14 1.488(5) . ? N1 C7 1.500(5) . ? N2 C21 1.473(6) . ? N2 C12 1.480(5) . ? N2 C9 1.487(5) . ? O1 C1 1.324(4) . ? C1 C6 1.422(5) . ? C1 C2 1.431(5) . ? C2 C3 1.384(5) . ? C2 C25 1.544(4) . ? C3 C4 1.384(5) . ? C3 H3 0.9300 . ? C4 C5 1.364(5) . ? C4 C13 1.506(6) . ? C5 C6 1.387(5) . ? C5 H5 0.9300 . ? C6 C7 1.480(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.514(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.540(6) . ? C9 H9 0.9800 . ? C10 C11 1.547(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.532(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.489(6) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C20 1.363(6) . ? C15 C16 1.403(7) . ? C16 C17 1.370(10) . ? C16 H16 0.9300 . ? C17 C18 1.332(10) . ? C17 H17 0.9300 . ? C18 C19 1.358(9) . ? C18 H18 0.9300 . ? C19 C20 1.367(7) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.487(7) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.547(9) . ? C22 C23' 1.573(16) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9499 . ? C22 H22D 0.9712 . ? C23 C24 1.535(11) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C23' C24' 1.471(18) . ? C23' H23C 0.9700 . ? C23' H23D 0.9700 . ? C24' H24D 0.9600 . ? C24' H24E 0.9600 . ? C24' H24F 0.9600 . ? C25 C32 1.539(5) . ? C25 C38 1.548(5) . ? C25 C26 1.562(5) . ? C26 C27 1.389(6) . ? C26 C31 1.391(5) . ? C27 C28 1.343(6) . ? C27 H27 0.9300 . ? C28 C29 1.379(8) . ? C28 H28 0.9300 . ? C29 C30 1.371(8) . ? C29 H29 0.9300 . ? C30 C31 1.401(6) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.373(5) . ? C32 C37 1.385(5) . ? C33 C34 1.396(5) . ? C33 H33 0.9300 . ? C34 C35 1.369(6) . ? C34 H34 0.9300 . ? C35 C36 1.374(6) . ? C35 H35 0.9300 . ? C36 C37 1.374(5) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 C39 1.350(5) . ? C38 C43 1.404(5) . ? C39 C40 1.419(5) . ? C39 H39 0.9300 . ? C40 C41 1.336(6) . ? C40 H40 0.9300 . ? C41 C42 1.406(6) . ? C41 H41 0.9300 . ? C42 C43 1.352(5) . ? C42 H42 0.9300 . ? C43 H43 0.9300 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Zn1 O1 119.37(12) . . ? N3 Zn1 N2 127.10(13) . . ? O1 Zn1 N2 103.70(11) . . ? N3 Zn1 N1 116.68(12) . . ? O1 Zn1 N1 97.41(11) . . ? N2 Zn1 N1 83.89(12) . . ? N3 Si1 C45 110.33(19) . . ? N3 Si1 C44 110.7(2) . . ? C45 Si1 C44 110.5(2) . . ? N3 Si1 C46 116.1(3) . . ? C45 Si1 C46 105.2(3) . . ? C44 Si1 C46 103.7(3) . . ? N3 Si2 C48 115.0(2) . . ? N3 Si2 C47 112.9(2) . . ? C48 Si2 C47 102.5(3) . . ? N3 Si2 C49 112.7(3) . . ? C48 Si2 C49 103.6(3) . . ? C47 Si2 C49 109.3(4) . . ? C8 N1 C14 113.5(3) . . ? C8 N1 C7 111.4(3) . . ? C14 N1 C7 110.4(3) . . ? C8 N1 Zn1 106.2(2) . . ? C14 N1 Zn1 111.9(2) . . ? C7 N1 Zn1 102.9(2) . . ? C21 N2 C12 108.4(3) . . ? C21 N2 C9 111.5(3) . . ? C12 N2 C9 103.0(3) . . ? C21 N2 Zn1 114.1(3) . . ? C12 N2 Zn1 112.7(2) . . ? C9 N2 Zn1 106.6(2) . . ? Si2 N3 Si1 121.3(2) . . ? Si2 N3 Zn1 128.2(2) . . ? Si1 N3 Zn1 110.51(17) . . ? C1 O1 Zn1 125.5(2) . . ? O1 C1 C6 120.9(3) . . ? O1 C1 C2 121.4(3) . . ? C6 C1 C2 117.7(3) . . ? C3 C2 C1 117.5(3) . . ? C3 C2 C25 122.3(3) . . ? C1 C2 C25 120.2(3) . . ? C4 C3 C2 125.0(3) . . ? C4 C3 H3 117.5 . . ? C2 C3 H3 117.5 . . ? C5 C4 C3 116.5(3) . . ? C5 C4 C13 121.4(4) . . ? C3 C4 C13 122.0(4) . . ? C4 C5 C6 122.8(3) . . ? C4 C5 H5 118.6 . . ? C6 C5 H5 118.6 . . ? C5 C6 C1 120.2(3) . . ? C5 C6 C7 118.5(3) . . ? C1 C6 C7 121.0(3) . . ? C6 C7 N1 117.0(3) . . ? C6 C7 H7A 108.0 . . ? N1 C7 H7A 108.0 . . ? C6 C7 H7B 108.0 . . ? N1 C7 H7B 108.0 . . ? H7A C7 H7B 107.3 . . ? N1 C8 C9 112.0(3) . . ? N1 C8 H8A 109.2 . . ? C9 C8 H8A 109.2 . . ? N1 C8 H8B 109.2 . . ? C9 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? N2 C9 C8 110.3(3) . . ? N2 C9 C10 106.0(3) . . ? C8 C9 C10 110.9(4) . . ? N2 C9 H9 109.9 . . ? C8 C9 H9 109.9 . . ? C10 C9 H9 109.9 . . ? C9 C10 C11 103.2(3) . . ? C9 C10 H10A 111.1 . . ? C11 C10 H10A 111.1 . . ? C9 C10 H10B 111.1 . . ? C11 C10 H10B 111.1 . . ? H10A C10 H10B 109.1 . . ? C12 C11 C10 105.8(3) . . ? C12 C11 H11A 110.6 . . ? C10 C11 H11A 110.6 . . ? C12 C11 H11B 110.6 . . ? C10 C11 H11B 110.6 . . ? H11A C11 H11B 108.7 . . ? N2 C12 C11 106.2(3) . . ? N2 C12 H12A 110.5 . . ? C11 C12 H12A 110.5 . . ? N2 C12 H12B 110.5 . . ? C11 C12 H12B 110.5 . . ? H12A C12 H12B 108.7 . . ? C4 C13 H13A 109.5 . . ? C4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 N1 116.7(4) . . ? C15 C14 H14A 108.1 . . ? N1 C14 H14A 108.1 . . ? C15 C14 H14B 108.1 . . ? N1 C14 H14B 108.1 . . ? H14A C14 H14B 107.3 . . ? C20 C15 C16 117.4(5) . . ? C20 C15 C14 122.9(4) . . ? C16 C15 C14 119.7(5) . . ? C17 C16 C15 119.1(6) . . ? C17 C16 H16 120.5 . . ? C15 C16 H16 120.5 . . ? C18 C17 C16 121.3(7) . . ? C18 C17 H17 119.3 . . ? C16 C17 H17 119.3 . . ? C17 C18 C19 121.3(6) . . ? C17 C18 H18 119.4 . . ? C19 C18 H18 119.4 . . ? C18 C19 C20 118.1(6) . . ? C18 C19 H19 120.9 . . ? C20 C19 H19 120.9 . . ? C15 C20 C19 122.8(5) . . ? C15 C20 H20 118.6 . . ? C19 C20 H20 118.6 . . ? N2 C21 C22 115.3(4) . . ? N2 C21 H21A 108.5 . . ? C22 C21 H21A 108.5 . . ? N2 C21 H21B 108.5 . . ? C22 C21 H21B 108.5 . . ? H21A C21 H21B 107.5 . . ? C21 C22 C23 104.4(5) . . ? C21 C22 C23' 138.7(11) . . ? C23 C22 C23' 44.0(8) . . ? C21 C22 H22A 110.9 . . ? C23 C22 H22A 110.9 . . ? C23' C22 H22A 106.4 . . ? C21 C22 H22B 110.9 . . ? C23 C22 H22B 110.9 . . ? C23' C22 H22B 71.7 . . ? H22A C22 H22B 108.9 . . ? C21 C22 H22C 100.7 . . ? C23 C22 H22C 98.2 . . ? C23' C22 H22C 108.6 . . ? H22A C22 H22C 20.1 . . ? H22B C22 H22C 128.9 . . ? C21 C22 H22D 101.5 . . ? C23 C22 H22D 142.6 . . ? C23' C22 H22D 99.4 . . ? H22A C22 H22D 83.8 . . ? H22B C22 H22D 33.3 . . ? H22C C22 H22D 103.0 . . ? C24 C23 C22 111.3(8) . . ? C24 C23 H23A 109.4 . . ? C22 C23 H23A 109.4 . . ? C24 C23 H23B 109.4 . . ? C22 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? C24' C23' C22 110.0(16) . . ? C24' C23' H23C 109.7 . . ? C22 C23' H23C 109.7 . . ? C24' C23' H23D 109.7 . . ? C22 C23' H23D 109.7 . . ? H23C C23' H23D 108.2 . . ? C23' C24' H24D 109.5 . . ? C23' C24' H24E 109.5 . . ? H24D C24' H24E 109.5 . . ? C23' C24' H24F 109.5 . . ? H24D C24' H24F 109.5 . . ? H24E C24' H24F 109.5 . . ? C32 C25 C2 112.8(3) . . ? C32 C25 C38 114.0(3) . . ? C2 C25 C38 107.5(3) . . ? C32 C25 C26 102.0(3) . . ? C2 C25 C26 111.2(3) . . ? C38 C25 C26 109.3(3) . . ? C27 C26 C31 116.2(4) . . ? C27 C26 C25 119.5(3) . . ? C31 C26 C25 124.2(3) . . ? C28 C27 C26 122.3(5) . . ? C28 C27 H27 118.8 . . ? C26 C27 H27 118.8 . . ? C27 C28 C29 121.6(5) . . ? C27 C28 H28 119.2 . . ? C29 C28 H28 119.2 . . ? C30 C29 C28 118.5(5) . . ? C30 C29 H29 120.7 . . ? C28 C29 H29 120.7 . . ? C29 C30 C31 119.6(5) . . ? C29 C30 H30 120.2 . . ? C31 C30 H30 120.2 . . ? C26 C31 C30 121.7(5) . . ? C26 C31 H31 119.2 . . ? C30 C31 H31 119.2 . . ? C33 C32 C37 116.8(3) . . ? C33 C32 C25 120.4(3) . . ? C37 C32 C25 122.4(3) . . ? C32 C33 C34 121.3(4) . . ? C32 C33 H33 119.3 . . ? C34 C33 H33 119.3 . . ? C35 C34 C33 120.4(4) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C34 C35 C36 119.0(4) . . ? C34 C35 H35 120.5 . . ? C36 C35 H35 120.5 . . ? C37 C36 C35 120.0(4) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C36 C37 C32 122.4(3) . . ? C36 C37 H37 118.8 . . ? C32 C37 H37 118.8 . . ? C39 C38 C43 117.1(3) . . ? C39 C38 C25 124.8(3) . . ? C43 C38 C25 118.0(3) . . ? C38 C39 C40 121.7(3) . . ? C38 C39 H39 119.1 . . ? C40 C39 H39 119.1 . . ? C41 C40 C39 120.1(4) . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C40 C41 C42 119.0(4) . . ? C40 C41 H41 120.5 . . ? C42 C41 H41 120.5 . . ? C43 C42 C41 120.2(4) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C42 C43 C38 121.7(4) . . ? C42 C43 H43 119.2 . . ? C38 C43 H43 119.2 . . ? Si1 C44 H44A 109.5 . . ? Si1 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? Si1 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? Si1 C45 H45A 109.5 . . ? Si1 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? Si1 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? Si1 C46 H46A 109.5 . . ? Si1 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? Si1 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? Si2 C47 H47A 109.5 . . ? Si2 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? Si2 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? Si2 C48 H48A 109.5 . . ? Si2 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? Si2 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? Si2 C49 H49A 109.5 . . ? Si2 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? Si2 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? 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 N3 Zn1 N1 C8 140.7(2) . . . . ? O1 Zn1 N1 C8 -91.0(2) . . . . ? N2 Zn1 N1 C8 12.1(2) . . . . ? N3 Zn1 N1 C14 16.4(3) . . . . ? O1 Zn1 N1 C14 144.6(3) . . . . ? N2 Zn1 N1 C14 -112.3(3) . . . . ? N3 Zn1 N1 C7 -102.1(2) . . . . ? O1 Zn1 N1 C7 26.1(2) . . . . ? N2 Zn1 N1 C7 129.2(2) . . . . ? N3 Zn1 N2 C21 19.0(3) . . . . ? O1 Zn1 N2 C21 -125.8(3) . . . . ? N1 Zn1 N2 C21 138.1(3) . . . . ? N3 Zn1 N2 C12 143.3(3) . . . . ? O1 Zn1 N2 C12 -1.5(3) . . . . ? N1 Zn1 N2 C12 -97.7(3) . . . . ? N3 Zn1 N2 C9 -104.5(3) . . . . ? O1 Zn1 N2 C9 110.7(2) . . . . ? N1 Zn1 N2 C9 14.6(2) . . . . ? C48 Si2 N3 Si1 177.5(3) . . . . ? C47 Si2 N3 Si1 60.4(4) . . . . ? C49 Si2 N3 Si1 -64.1(4) . . . . ? C48 Si2 N3 Zn1 -5.9(4) . . . . ? C47 Si2 N3 Zn1 -123.1(3) . . . . ? C49 Si2 N3 Zn1 112.5(4) . . . . ? C45 Si1 N3 Si2 -122.5(2) . . . . ? C44 Si1 N3 Si2 114.8(3) . . . . ? C46 Si1 N3 Si2 -3.0(4) . . . . ? C45 Si1 N3 Zn1 60.4(2) . . . . ? C44 Si1 N3 Zn1 -62.3(2) . . . . ? C46 Si1 N3 Zn1 179.9(3) . . . . ? O1 Zn1 N3 Si2 179.20(18) . . . . ? N2 Zn1 N3 Si2 39.2(3) . . . . ? N1 Zn1 N3 Si2 -64.2(3) . . . . ? O1 Zn1 N3 Si1 -3.9(2) . . . . ? N2 Zn1 N3 Si1 -143.96(15) . . . . ? N1 Zn1 N3 Si1 112.70(17) . . . . ? N3 Zn1 O1 C1 140.6(2) . . . . ? N2 Zn1 O1 C1 -71.2(3) . . . . ? N1 Zn1 O1 C1 14.3(3) . . . . ? Zn1 O1 C1 C6 -24.9(4) . . . . ? Zn1 O1 C1 C2 156.9(2) . . . . ? O1 C1 C2 C3 -176.0(3) . . . . ? C6 C1 C2 C3 5.7(4) . . . . ? O1 C1 C2 C25 2.6(4) . . . . ? C6 C1 C2 C25 -175.7(3) . . . . ? C1 C2 C3 C4 -2.2(5) . . . . ? C25 C2 C3 C4 179.2(3) . . . . ? C2 C3 C4 C5 -1.5(5) . . . . ? C2 C3 C4 C13 -179.1(4) . . . . ? C3 C4 C5 C6 1.6(5) . . . . ? C13 C4 C5 C6 179.2(4) . . . . ? C4 C5 C6 C1 2.1(5) . . . . ? C4 C5 C6 C7 -171.5(3) . . . . ? O1 C1 C6 C5 175.9(3) . . . . ? C2 C1 C6 C5 -5.8(4) . . . . ? O1 C1 C6 C7 -10.7(5) . . . . ? C2 C1 C6 C7 167.6(3) . . . . ? C5 C6 C7 N1 -121.4(4) . . . . ? C1 C6 C7 N1 65.1(4) . . . . ? C8 N1 C7 C6 49.6(4) . . . . ? C14 N1 C7 C6 176.7(3) . . . . ? Zn1 N1 C7 C6 -63.8(3) . . . . ? C14 N1 C8 C9 86.0(4) . . . . ? C7 N1 C8 C9 -148.6(3) . . . . ? Zn1 N1 C8 C9 -37.4(3) . . . . ? C21 N2 C9 C8 -163.8(4) . . . . ? C12 N2 C9 C8 80.1(4) . . . . ? Zn1 N2 C9 C8 -38.7(4) . . . . ? C21 N2 C9 C10 76.1(5) . . . . ? C12 N2 C9 C10 -40.0(4) . . . . ? Zn1 N2 C9 C10 -158.8(3) . . . . ? N1 C8 C9 N2 53.2(4) . . . . ? N1 C8 C9 C10 170.3(3) . . . . ? N2 C9 C10 C11 27.7(5) . . . . ? C8 C9 C10 C11 -92.0(4) . . . . ? C9 C10 C11 C12 -5.2(5) . . . . ? C21 N2 C12 C11 -82.0(5) . . . . ? C9 N2 C12 C11 36.3(4) . . . . ? Zn1 N2 C12 C11 150.7(3) . . . . ? C10 C11 C12 N2 -19.0(5) . . . . ? C8 N1 C14 C15 78.9(5) . . . . ? C7 N1 C14 C15 -47.0(5) . . . . ? Zn1 N1 C14 C15 -160.9(3) . . . . ? N1 C14 C15 C20 -81.4(6) . . . . ? N1 C14 C15 C16 95.6(6) . . . . ? C20 C15 C16 C17 -0.5(9) . . . . ? C14 C15 C16 C17 -177.7(6) . . . . ? C15 C16 C17 C18 2.2(12) . . . . ? C16 C17 C18 C19 -1.1(13) . . . . ? C17 C18 C19 C20 -1.6(11) . . . . ? C16 C15 C20 C19 -2.3(7) . . . . ? C14 C15 C20 C19 174.8(5) . . . . ? C18 C19 C20 C15 3.4(8) . . . . ? C12 N2 C21 C22 -78.1(5) . . . . ? C9 N2 C21 C22 169.2(4) . . . . ? Zn1 N2 C21 C22 48.4(5) . . . . ? N2 C21 C22 C23 176.2(5) . . . . ? N2 C21 C22 C23' -150.1(14) . . . . ? C21 C22 C23 C24 166.1(7) . . . . ? C23' C22 C23 C24 17.9(16) . . . . ? C21 C22 C23' C24' -53(3) . . . . ? C23 C22 C23' C24' -2.2(12) . . . . ? C3 C2 C25 C32 -121.9(3) . . . . ? C1 C2 C25 C32 59.5(4) . . . . ? C3 C2 C25 C38 111.6(3) . . . . ? C1 C2 C25 C38 -66.9(3) . . . . ? C3 C2 C25 C26 -8.0(4) . . . . ? C1 C2 C25 C26 173.5(3) . . . . ? C32 C25 C26 C27 56.7(4) . . . . ? C2 C25 C26 C27 -63.9(4) . . . . ? C38 C25 C26 C27 177.6(3) . . . . ? C32 C25 C26 C31 -119.4(4) . . . . ? C2 C25 C26 C31 120.0(4) . . . . ? C38 C25 C26 C31 1.5(5) . . . . ? C31 C26 C27 C28 0.1(6) . . . . ? C25 C26 C27 C28 -176.4(4) . . . . ? C26 C27 C28 C29 -0.8(8) . . . . ? C27 C28 C29 C30 2.1(8) . . . . ? C28 C29 C30 C31 -2.6(8) . . . . ? C27 C26 C31 C30 -0.7(6) . . . . ? C25 C26 C31 C30 175.5(4) . . . . ? C29 C30 C31 C26 2.0(7) . . . . ? C2 C25 C32 C33 -178.9(3) . . . . ? C38 C25 C32 C33 -56.0(4) . . . . ? C26 C25 C32 C33 61.7(4) . . . . ? C2 C25 C32 C37 8.4(5) . . . . ? C38 C25 C32 C37 131.3(3) . . . . ? C26 C25 C32 C37 -111.0(4) . . . . ? C37 C32 C33 C34 -0.8(6) . . . . ? C25 C32 C33 C34 -173.9(4) . . . . ? C32 C33 C34 C35 2.1(7) . . . . ? C33 C34 C35 C36 -2.1(7) . . . . ? C34 C35 C36 C37 0.9(7) . . . . ? C35 C36 C37 C32 0.4(6) . . . . ? C33 C32 C37 C36 -0.4(6) . . . . ? C25 C32 C37 C36 172.6(4) . . . . ? C32 C25 C38 C39 0.0(5) . . . . ? C2 C25 C38 C39 125.8(3) . . . . ? C26 C25 C38 C39 -113.4(4) . . . . ? C32 C25 C38 C43 177.0(3) . . . . ? C2 C25 C38 C43 -57.2(4) . . . . ? C26 C25 C38 C43 63.6(4) . . . . ? C43 C38 C39 C40 -2.1(5) . . . . ? C25 C38 C39 C40 175.0(3) . . . . ? C38 C39 C40 C41 -1.8(6) . . . . ? C39 C40 C41 C42 3.8(6) . . . . ? C40 C41 C42 C43 -2.1(6) . . . . ? C41 C42 C43 C38 -1.9(6) . . . . ? C39 C38 C43 C42 3.8(5) . . . . ? C25 C38 C43 C42 -173.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.405 _refine_diff_density_min -0.183 _refine_diff_density_rms 0.049 _database_code_depnum_ccdc_archive 'CCDC 936901' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_cd212599 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H43 Cl2 N3 O Si2 Zn' _chemical_formula_weight 618.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 26.943(3) _cell_length_b 13.5555(12) _cell_length_c 17.9722(16) _cell_angle_alpha 90.00 _cell_angle_beta 100.167(2) _cell_angle_gamma 90.00 _cell_volume 6460.8(10) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5493 _cell_measurement_theta_min 4.590 _cell_measurement_theta_max 43.173 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.276 _exptl_crystal_size_mid 0.211 _exptl_crystal_size_min 0.143 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.271 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2608 _exptl_absorpt_coefficient_mu 1.023 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.55095 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36037 _diffrn_reflns_av_R_equivalents 0.0739 _diffrn_reflns_av_sigmaI/netI 0.0786 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 0.77 _diffrn_reflns_theta_max 25.50 _reflns_number_total 11995 _reflns_number_gt 8031 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^+153.0902P] 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 SHELXL _refine_ls_extinction_coef ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11995 _refine_ls_number_parameters 774 _refine_ls_number_restraints 132 _refine_ls_R_factor_all 0.1882 _refine_ls_R_factor_gt 0.1523 _refine_ls_wR_factor_ref 0.3425 _refine_ls_wR_factor_gt 0.3275 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_restrained_S_all 1.135 _refine_ls_shift/su_max 0.018 _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 0.38341(6) 0.57017(11) 0.30854(8) 0.0451(4) Uani 1 1 d . B . Zn2 Zn 0.11342(6) 0.09338(13) 0.36976(9) 0.0521(5) Uani 1 1 d . D . Si1 Si 0.3626(2) 0.8036(3) 0.2921(3) 0.0743(14) Uani 1 1 d . B . Si2 Si 0.33596(16) 0.6863(4) 0.4201(2) 0.0589(11) Uani 1 1 d . B . Si3 Si 0.13175(17) 0.3276(4) 0.3647(3) 0.0663(12) Uani 1 1 d . D . Si4 Si 0.17374(19) 0.2039(5) 0.4995(3) 0.0807(16) Uani 1 1 d . D . Cl1 Cl 0.18697(17) -0.1984(5) 0.4838(3) 0.0985(18) Uani 1 1 d . D . Cl2 Cl 0.0063(2) -0.3726(3) 0.4587(3) 0.0915(15) Uani 1 1 d . D . Cl3 Cl 0.49626(18) 0.1092(3) 0.4483(3) 0.0815(13) Uani 1 1 d . B . Cl4 Cl 0.31427(16) 0.2776(4) 0.3879(3) 0.0879(15) Uani 1 1 d . B . N1 N 0.4620(4) 0.5402(8) 0.3159(6) 0.046(3) Uani 1 1 d . B . N2 N 0.3739(5) 0.5027(9) 0.2013(7) 0.057(3) Uani 1 1 d D . . N3 N 0.3596(4) 0.6962(8) 0.3385(6) 0.050(3) Uani 1 1 d . . . N4 N 0.0352(4) 0.0563(9) 0.3387(6) 0.051(3) Uani 1 1 d . D . N5 N 0.1221(4) 0.0289(8) 0.2663(6) 0.051(3) Uani 1 1 d D . . N6 N 0.1404(4) 0.2152(9) 0.4112(7) 0.058(3) Uani 1 1 d . . . O1 O 0.3706(4) 0.4592(8) 0.3702(6) 0.067(3) Uani 1 1 d . . . O2 O 0.1279(4) -0.0187(9) 0.4379(6) 0.075(3) Uani 1 1 d . . . C1 C 0.3997(5) 0.3824(10) 0.3852(7) 0.045(3) Uani 1 1 d . B . C2 C 0.3799(6) 0.2876(14) 0.3972(8) 0.068(5) Uani 1 1 d . . . C3 C 0.4084(5) 0.2076(10) 0.4175(8) 0.050(3) Uani 1 1 d . B . H3 H 0.3932 0.1488 0.4277 0.060 Uiso 1 1 calc R . . C4 C 0.4580(6) 0.2115(10) 0.4229(7) 0.054(4) Uani 1 1 d . . . C5 C 0.4812(5) 0.3003(11) 0.4080(7) 0.050(3) Uani 1 1 d . B . H5 H 0.5159 0.3027 0.4095 0.060 Uiso 1 1 calc R . . C6 C 0.4523(5) 0.3844(9) 0.3911(7) 0.045(3) Uani 1 1 d . . . C7 C 0.4799(5) 0.4814(11) 0.3845(8) 0.053(3) Uani 1 1 d . B . H7A H 0.4771 0.5216 0.4282 0.063 Uiso 1 1 calc R . . H7B H 0.5153 0.4670 0.3865 0.063 Uiso 1 1 calc R . . C8 C 0.4673(5) 0.4876(11) 0.2457(8) 0.057(3) Uani 1 1 d DU . . H8A H 0.4692 0.4175 0.2567 0.068 Uiso 0.50 1 calc PR A 1 H8B H 0.4992 0.5068 0.2321 0.068 Uiso 0.50 1 calc PR A 1 H8C H 0.4934 0.4391 0.2573 0.068 Uiso 0.50 1 d PR A 2 H8D H 0.4763 0.5340 0.2100 0.068 Uiso 0.50 1 d PR A 2 C9 C 0.4253(9) 0.504(2) 0.1759(12) 0.055(4) Uani 0.50 1 d PDU B 1 H9 H 0.4300 0.5708 0.1575 0.066 Uiso 0.50 1 calc PR B 1 C10 C 0.4236(12) 0.434(2) 0.1079(16) 0.057(4) Uani 0.50 1 d PDU B 1 H10A H 0.4554 0.4003 0.1093 0.068 Uiso 0.50 1 calc PR B 1 H10B H 0.4149 0.4694 0.0603 0.068 Uiso 0.50 1 calc PR B 1 C11 C 0.3815(11) 0.363(2) 0.1205(15) 0.057(4) Uani 0.50 1 d PDU B 1 H11A H 0.3953 0.2973 0.1315 0.069 Uiso 0.50 1 calc PR B 1 H11B H 0.3559 0.3593 0.0753 0.069 Uiso 0.50 1 calc PR B 1 C12 C 0.3578(12) 0.401(2) 0.1883(16) 0.058(5) Uani 0.50 1 d PDU B 1 H12A H 0.3213 0.3975 0.1763 0.070 Uiso 0.50 1 calc PR B 1 H12B H 0.3693 0.3617 0.2330 0.070 Uiso 0.50 1 calc PR B 1 C13 C 0.3387(10) 0.557(2) 0.1432(15) 0.070(7) Uani 0.50 1 d PDU B 1 H13A H 0.3355 0.5235 0.0950 0.084 Uiso 0.50 1 calc PR B 1 H13B H 0.3515 0.6231 0.1373 0.084 Uiso 0.50 1 calc PR B 1 C14 C 0.2865(11) 0.564(3) 0.167(2) 0.076(8) Uani 0.50 1 d PDU B 1 H14A H 0.2837 0.5128 0.2034 0.114 Uiso 0.50 1 calc PR B 1 H14B H 0.2605 0.5558 0.1239 0.114 Uiso 0.50 1 calc PR B 1 H14C H 0.2830 0.6270 0.1900 0.114 Uiso 0.50 1 calc PR B 1 C9' C 0.4206(8) 0.4354(18) 0.2118(11) 0.044(4) Uani 0.50 1 d PDU B 2 H9' H 0.4153 0.3782 0.2429 0.053 Uiso 0.50 1 calc PR B 2 C10' C 0.4257(11) 0.401(2) 0.1314(11) 0.046(4) Uani 0.50 1 d PDU B 2 H10C H 0.4152 0.3332 0.1229 0.055 Uiso 0.50 1 calc PR B 2 H10D H 0.4601 0.4083 0.1230 0.055 Uiso 0.50 1 calc PR B 2 C11' C 0.3897(11) 0.4720(17) 0.0801(12) 0.049(4) Uani 0.50 1 d PDU B 2 H11C H 0.4069 0.5033 0.0433 0.059 Uiso 0.50 1 calc PR B 2 H11D H 0.3606 0.4366 0.0535 0.059 Uiso 0.50 1 calc PR B 2 C12' C 0.3735(12) 0.5493(19) 0.1337(14) 0.050(4) Uani 0.50 1 d PDU B 2 H12C H 0.3968 0.6044 0.1400 0.059 Uiso 0.50 1 calc PR B 2 H12D H 0.3400 0.5738 0.1137 0.059 Uiso 0.50 1 calc PR B 2 C13' C 0.3337(10) 0.430(2) 0.206(2) 0.097(11) Uani 0.50 1 d PDU B 2 H13C H 0.3437 0.3899 0.2510 0.116 Uiso 0.50 1 calc PR B 2 H13D H 0.3304 0.3864 0.1626 0.116 Uiso 0.50 1 calc PR B 2 C14' C 0.2823(13) 0.477(4) 0.209(2) 0.101(11) Uani 0.50 1 d PDU B 2 H14D H 0.2801 0.4929 0.2603 0.151 Uiso 0.50 1 calc PR B 2 H14E H 0.2559 0.4321 0.1888 0.151 Uiso 0.50 1 calc PR B 2 H14F H 0.2788 0.5366 0.1792 0.151 Uiso 0.50 1 calc PR B 2 C15 C 0.4915(5) 0.6322(13) 0.3226(8) 0.064(4) Uani 1 1 d . . . H15A H 0.4826 0.6691 0.3646 0.077 Uiso 1 1 calc R B . H15B H 0.4800 0.6705 0.2773 0.077 Uiso 1 1 calc R . . C16 C 0.5484(5) 0.6293(11) 0.3339(8) 0.057(4) Uani 1 1 d . B . C17 C 0.5775(6) 0.6194(13) 0.4056(8) 0.066(4) Uani 1 1 d . . . H17 H 0.5615 0.6150 0.4473 0.079 Uiso 1 1 calc R B . C18 C 0.6287(7) 0.6161(19) 0.4164(10) 0.099(7) Uani 1 1 d . B . H18 H 0.6474 0.6138 0.4651 0.119 Uiso 1 1 calc R . . C19 C 0.6534(7) 0.6161(18) 0.3529(11) 0.098(7) Uani 1 1 d . . . H19 H 0.6881 0.6077 0.3583 0.118 Uiso 1 1 calc R B . C20 C 0.6245(7) 0.6289(17) 0.2844(10) 0.090(6) Uani 1 1 d . B . H20 H 0.6401 0.6349 0.2424 0.108 Uiso 1 1 calc R . . C21 C 0.5725(6) 0.6333(14) 0.2742(9) 0.072(5) Uani 1 1 d . . . H21 H 0.5539 0.6392 0.2256 0.086 Uiso 1 1 calc R B . C22 C 0.3966(9) 0.7971(12) 0.2134(11) 0.106(8) Uani 1 1 d . . . H22A H 0.4226 0.7480 0.2238 0.160 Uiso 1 1 calc R B . H22B H 0.4116 0.8601 0.2067 0.160 Uiso 1 1 calc R . . H22C H 0.3737 0.7798 0.1681 0.160 Uiso 1 1 calc R . . C23 C 0.3000(10) 0.848(2) 0.2502(18) 0.173(13) Uani 1 1 d . . . H23A H 0.2879 0.8111 0.2049 0.259 Uiso 1 1 calc R B . H23B H 0.3017 0.9164 0.2383 0.259 Uiso 1 1 calc R . . H23C H 0.2774 0.8385 0.2855 0.259 Uiso 1 1 calc R . . C24 C 0.3962(12) 0.9057(17) 0.3524(13) 0.164(14) Uani 1 1 d . . . H24A H 0.3792 0.9183 0.3941 0.246 Uiso 1 1 calc R B . H24B H 0.3960 0.9645 0.3225 0.246 Uiso 1 1 calc R . . H24C H 0.4304 0.8863 0.3711 0.246 Uiso 1 1 calc R . . C25 C 0.3155(9) 0.8059(17) 0.4584(13) 0.124(10) Uani 1 1 d . . . H25A H 0.3447 0.8443 0.4788 0.186 Uiso 1 1 calc R B . H25B H 0.2964 0.7923 0.4976 0.186 Uiso 1 1 calc R . . H25C H 0.2950 0.8420 0.4185 0.186 Uiso 1 1 calc R . . C26 C 0.2815(6) 0.6025(14) 0.4100(11) 0.084(5) Uani 1 1 d . . . H26A H 0.2566 0.6231 0.3679 0.126 Uiso 1 1 calc R B . H26B H 0.2673 0.6042 0.4553 0.126 Uiso 1 1 calc R . . H26C H 0.2922 0.5366 0.4015 0.126 Uiso 1 1 calc R . . C27 C 0.3853(8) 0.646(2) 0.4980(10) 0.141(12) Uani 1 1 d . . . H27A H 0.3908 0.5762 0.4937 0.212 Uiso 1 1 calc R B . H27B H 0.3748 0.6593 0.5454 0.212 Uiso 1 1 calc R . . H27C H 0.4160 0.6806 0.4958 0.212 Uiso 1 1 calc R . . C28 C 0.1001(5) -0.0938(11) 0.4403(8) 0.052(3) Uani 1 1 d . D . C29 C 0.1217(6) -0.1875(13) 0.4630(8) 0.059(4) Uani 1 1 d . . . C30 C 0.0944(6) -0.2720(13) 0.4693(8) 0.065(4) Uani 1 1 d . D . H30 H 0.1112 -0.3300 0.4859 0.078 Uiso 1 1 calc R . . C31 C 0.0425(6) -0.2718(12) 0.4512(8) 0.064(4) Uani 1 1 d . . . C32 C 0.0189(5) -0.1829(10) 0.4266(8) 0.051(3) Uani 1 1 d . D . H32 H -0.0160 -0.1810 0.4131 0.061 Uiso 1 1 calc R . . C33 C 0.0471(5) -0.0951(10) 0.4218(7) 0.046(3) Uani 1 1 d . . . C34 C 0.0193(6) -0.0009(11) 0.4016(8) 0.056(4) Uani 1 1 d . D . H34A H 0.0235 0.0407 0.4462 0.067 Uiso 1 1 calc R . . H34B H -0.0164 -0.0158 0.3877 0.067 Uiso 1 1 calc R . . C36 C 0.0306(5) -0.0007(11) 0.2676(8) 0.055(3) Uani 1 1 d DU . . H36A H -0.0026 0.0111 0.2380 0.066 Uiso 0.50 1 calc PR C 1 H36B H 0.0329 -0.0703 0.2800 0.066 Uiso 0.50 1 calc PR C 1 H36C H 0.0191 0.0421 0.2254 0.066 Uiso 0.50 1 d PR C 2 H36D H 0.0061 -0.0518 0.2687 0.066 Uiso 0.50 1 d PR C 2 C37 C 0.0703(9) 0.023(2) 0.2182(13) 0.055(4) Uani 0.50 1 d PDU D 1 H37 H 0.0623 0.0882 0.1950 0.066 Uiso 0.50 1 calc PR D 1 C38 C 0.0731(12) -0.051(2) 0.1547(16) 0.056(4) Uani 0.50 1 d PDU D 1 H38A H 0.0765 -0.0168 0.1085 0.067 Uiso 0.50 1 calc PR D 1 H38B H 0.0427 -0.0908 0.1451 0.067 Uiso 0.50 1 calc PR D 1 C39 C 0.1195(10) -0.117(2) 0.1809(14) 0.059(4) Uani 0.50 1 d PDU D 1 H39A H 0.1098 -0.1860 0.1830 0.071 Uiso 0.50 1 calc PR D 1 H39B H 0.1438 -0.1110 0.1473 0.071 Uiso 0.50 1 calc PR D 1 C40 C 0.1413(12) -0.078(2) 0.2604(14) 0.059(5) Uani 0.50 1 d PDU D 1 H40A H 0.1779 -0.0789 0.2684 0.070 Uiso 0.50 1 calc PR D 1 H40B H 0.1304 -0.1193 0.2986 0.070 Uiso 0.50 1 calc PR D 1 C41 C 0.1525(10) 0.086(2) 0.2231(17) 0.068(7) Uani 0.50 1 d PDU D 1 H41A H 0.1364 0.1499 0.2110 0.082 Uiso 0.50 1 calc PR D 1 H41B H 0.1537 0.0527 0.1759 0.082 Uiso 0.50 1 calc PR D 1 C42 C 0.2068(11) 0.104(3) 0.265(2) 0.073(8) Uani 0.50 1 d PDU D 1 H42A H 0.2064 0.1165 0.3174 0.110 Uiso 0.50 1 calc PR D 1 H42B H 0.2210 0.1594 0.2431 0.110 Uiso 0.50 1 calc PR D 1 H42C H 0.2268 0.0462 0.2603 0.110 Uiso 0.50 1 calc PR D 1 C37' C 0.0802(9) -0.044(2) 0.2574(14) 0.066(6) Uani 0.50 1 d PDU D 2 H37' H 0.0891 -0.0997 0.2916 0.080 Uiso 0.50 1 calc PR D 2 C38' C 0.0705(14) -0.079(2) 0.1742(14) 0.067(5) Uani 0.50 1 d PDU D 2 H38C H 0.0826 -0.1455 0.1702 0.081 Uiso 0.50 1 calc PR D 2 H38D H 0.0349 -0.0760 0.1529 0.081 Uiso 0.50 1 calc PR D 2 C39' C 0.1005(13) -0.006(2) 0.1342(15) 0.069(5) Uani 0.50 1 d PDU D 2 H39C H 0.0800 0.0206 0.0886 0.083 Uiso 0.50 1 calc PR D 2 H39D H 0.1304 -0.0362 0.1213 0.083 Uiso 0.50 1 calc PR D 2 C40' C 0.1146(15) 0.076(2) 0.1948(15) 0.070(6) Uani 0.50 1 d PDU D 2 H40C H 0.1451 0.1098 0.1874 0.084 Uiso 0.50 1 calc PR D 2 H40D H 0.0876 0.1242 0.1913 0.084 Uiso 0.50 1 calc PR D 2 C41' C 0.1679(10) -0.028(3) 0.291(2) 0.127(16) Uani 0.50 1 d PDU D 2 H41C H 0.1714 -0.0770 0.2531 0.152 Uiso 0.50 1 calc PR D 2 H41D H 0.1654 -0.0619 0.3376 0.152 Uiso 0.50 1 calc PR D 2 C42' C 0.2156(13) 0.039(4) 0.304(2) 0.130(16) Uani 0.50 1 d PDU D 2 H42D H 0.2285 0.0452 0.2579 0.194 Uiso 0.50 1 calc PR D 2 H42E H 0.2409 0.0104 0.3423 0.194 Uiso 0.50 1 calc PR D 2 H42F H 0.2068 0.1034 0.3204 0.194 Uiso 0.50 1 calc PR D 2 C43 C 0.0051(5) 0.1491(12) 0.3276(9) 0.063(4) Uani 1 1 d . . . H43A H 0.0170 0.1872 0.2885 0.076 Uiso 1 1 calc R D . H43B H 0.0127 0.1870 0.3740 0.076 Uiso 1 1 calc R . . C44 C -0.0514(5) 0.1404(11) 0.3066(8) 0.053(4) Uani 1 1 d . D . C45 C -0.0817(6) 0.1260(14) 0.3585(9) 0.070(5) Uani 1 1 d . . . H45 H -0.0669 0.1202 0.4091 0.084 Uiso 1 1 calc R D . C46 C -0.1340(6) 0.1194(15) 0.3390(10) 0.080(5) Uani 1 1 d . D . H46 H -0.1535 0.1114 0.3764 0.095 Uiso 1 1 calc R . . C47 C -0.1563(6) 0.1247(17) 0.2662(10) 0.089(6) Uani 1 1 d . . . H47 H -0.1909 0.1156 0.2525 0.106 Uiso 1 1 calc R D . C48 C -0.1268(7) 0.1443(17) 0.2109(9) 0.090(6) Uani 1 1 d . D . H48 H -0.1419 0.1549 0.1609 0.108 Uiso 1 1 calc R . . C49 C -0.0750(6) 0.1476(12) 0.2315(8) 0.058(4) Uani 1 1 d . . . H49 H -0.0554 0.1548 0.1941 0.070 Uiso 1 1 calc R D . C50 C 0.0904(7) 0.3230(13) 0.2694(11) 0.095(6) Uani 1 1 d . . . H50A H 0.1052 0.2797 0.2370 0.142 Uiso 1 1 calc R D . H50B H 0.0873 0.3880 0.2479 0.142 Uiso 1 1 calc R . . H50C H 0.0577 0.2989 0.2744 0.142 Uiso 1 1 calc R . . C51 C 0.1908(7) 0.3746(16) 0.3450(16) 0.137(11) Uani 1 1 d . . . H51A H 0.2112 0.3973 0.3911 0.206 Uiso 1 1 calc R D . H51B H 0.1844 0.4285 0.3100 0.206 Uiso 1 1 calc R . . H51C H 0.2083 0.3231 0.3235 0.206 Uiso 1 1 calc R . . C52 C 0.0967(11) 0.4165(19) 0.4152(15) 0.155(12) Uani 1 1 d . . . H52A H 0.0675 0.3845 0.4281 0.232 Uiso 1 1 calc R D . H52B H 0.0862 0.4719 0.3830 0.232 Uiso 1 1 calc R . . H52C H 0.1181 0.4387 0.4605 0.232 Uiso 1 1 calc R . . C53 C 0.2252(6) 0.1103(18) 0.5043(11) 0.107(8) Uani 1 1 d . . . H53A H 0.2259 0.0696 0.5482 0.161 Uiso 1 1 calc R D . H53B H 0.2571 0.1434 0.5075 0.161 Uiso 1 1 calc R . . H53C H 0.2192 0.0699 0.4598 0.161 Uiso 1 1 calc R . . C54 C 0.2048(10) 0.324(2) 0.5409(15) 0.180(15) Uani 1 1 d . . . H54A H 0.1893 0.3794 0.5120 0.270 Uiso 1 1 calc R D . H54B H 0.2401 0.3229 0.5387 0.270 Uiso 1 1 calc R . . H54C H 0.2004 0.3310 0.5925 0.270 Uiso 1 1 calc R . . C55 C 0.1306(9) 0.163(2) 0.5654(12) 0.141(11) Uani 1 1 d . . . H55A H 0.1128 0.2187 0.5803 0.211 Uiso 1 1 calc R D . H55B H 0.1501 0.1327 0.6094 0.211 Uiso 1 1 calc R . . H55C H 0.1067 0.1157 0.5401 0.211 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 0.0529(9) 0.0398(8) 0.0430(8) 0.0076(7) 0.0094(7) 0.0065(7) Zn2 0.0495(10) 0.0552(11) 0.0502(9) 0.0031(8) 0.0050(7) -0.0094(8) Si1 0.109(4) 0.043(2) 0.076(3) 0.003(2) 0.029(3) 0.005(3) Si2 0.054(2) 0.073(3) 0.050(2) -0.019(2) 0.0098(19) -0.012(2) Si3 0.050(2) 0.056(3) 0.091(3) -0.018(2) 0.009(2) 0.004(2) Si4 0.065(3) 0.119(5) 0.055(3) -0.013(3) 0.002(2) -0.017(3) Cl1 0.057(3) 0.138(5) 0.099(4) 0.034(3) 0.011(2) 0.028(3) Cl2 0.105(4) 0.054(3) 0.109(4) 0.008(2) 0.001(3) -0.008(3) Cl3 0.092(3) 0.054(2) 0.098(3) 0.010(2) 0.015(3) 0.028(2) Cl4 0.055(2) 0.091(3) 0.122(4) 0.033(3) 0.027(2) 0.002(2) N1 0.042(6) 0.055(7) 0.043(6) 0.004(5) 0.011(5) -0.004(5) N2 0.056(8) 0.048(7) 0.065(8) -0.006(6) 0.007(6) -0.002(6) N3 0.063(7) 0.032(6) 0.058(7) -0.006(5) 0.017(6) -0.001(5) N4 0.052(7) 0.055(7) 0.045(6) 0.003(5) 0.002(5) -0.004(6) N5 0.059(7) 0.036(6) 0.056(7) 0.002(5) 0.008(6) 0.001(5) N6 0.054(7) 0.053(7) 0.060(8) -0.007(6) -0.005(6) 0.010(6) O1 0.056(6) 0.061(7) 0.090(8) 0.034(6) 0.033(6) 0.021(5) O2 0.053(6) 0.084(8) 0.080(8) 0.040(6) -0.010(5) -0.024(6) C1 0.051(8) 0.046(8) 0.042(7) 0.015(6) 0.013(6) 0.003(6) C2 0.050(9) 0.105(14) 0.052(9) 0.023(9) 0.016(7) 0.005(9) C3 0.058(9) 0.039(8) 0.053(8) 0.008(6) 0.012(7) 0.011(7) C4 0.081(11) 0.041(8) 0.042(8) 0.013(6) 0.017(7) 0.018(7) C5 0.050(8) 0.064(9) 0.036(7) 0.004(6) 0.005(6) 0.013(7) C6 0.054(8) 0.038(7) 0.041(7) 0.016(6) 0.006(6) 0.010(6) C7 0.054(9) 0.051(9) 0.052(8) 0.009(7) 0.006(7) 0.009(7) C8 0.063(8) 0.056(7) 0.055(7) 0.003(6) 0.021(6) 0.007(6) C9 0.064(8) 0.052(8) 0.055(7) -0.002(6) 0.024(6) 0.007(7) C10 0.067(9) 0.052(8) 0.056(8) -0.005(7) 0.022(7) 0.008(7) C11 0.069(9) 0.050(8) 0.058(9) -0.008(7) 0.022(8) 0.006(8) C12 0.069(10) 0.049(9) 0.059(10) -0.008(8) 0.021(9) 0.005(9) C13 0.081(18) 0.041(14) 0.082(18) -0.007(13) 0.000(15) 0.015(14) C14 0.083(18) 0.052(14) 0.085(18) -0.007(14) -0.006(15) 0.013(14) C9' 0.060(10) 0.040(9) 0.036(9) -0.005(8) 0.020(8) 0.006(8) C10' 0.064(10) 0.042(8) 0.037(8) -0.004(7) 0.021(7) 0.004(8) C11' 0.066(10) 0.044(9) 0.040(8) -0.004(7) 0.017(7) 0.003(8) C12' 0.067(11) 0.043(9) 0.040(9) -0.003(8) 0.015(8) 0.001(9) C13' 0.074(19) 0.16(3) 0.065(17) 0.00(2) 0.041(15) 0.01(2) C14' 0.075(19) 0.16(3) 0.073(18) 0.00(2) 0.039(15) 0.01(2) C15 0.052(9) 0.093(13) 0.048(8) 0.008(8) 0.013(7) 0.006(9) C16 0.054(9) 0.063(10) 0.052(8) 0.022(7) 0.005(7) 0.003(7) C17 0.073(11) 0.080(12) 0.046(8) 0.001(8) 0.012(8) -0.011(9) C18 0.058(11) 0.18(2) 0.056(11) 0.013(13) -0.006(8) 0.005(13) C19 0.061(11) 0.15(2) 0.084(14) 0.014(14) 0.003(10) -0.022(12) C20 0.083(13) 0.134(19) 0.059(11) 0.003(11) 0.025(10) -0.030(13) C21 0.064(11) 0.099(14) 0.054(9) 0.006(9) 0.016(8) -0.032(10) C22 0.20(2) 0.033(9) 0.102(15) 0.024(9) 0.072(16) 0.032(12) C23 0.16(3) 0.15(3) 0.21(3) 0.06(3) 0.01(2) 0.04(2) C24 0.31(4) 0.088(17) 0.107(18) -0.016(14) 0.06(2) -0.11(2) C25 0.14(2) 0.111(18) 0.14(2) -0.066(16) 0.101(17) -0.041(16) C26 0.075(12) 0.077(13) 0.103(14) -0.015(11) 0.027(10) -0.015(10) C27 0.116(18) 0.26(4) 0.039(10) -0.016(16) -0.001(10) 0.02(2) C28 0.049(8) 0.053(9) 0.050(8) 0.014(7) 0.000(6) 0.005(7) C29 0.050(9) 0.070(11) 0.056(9) -0.002(8) 0.001(7) 0.004(8) C30 0.074(11) 0.078(12) 0.039(8) 0.007(8) -0.002(7) 0.020(9) C31 0.078(11) 0.063(10) 0.051(9) -0.005(8) 0.013(8) -0.008(9) C32 0.049(8) 0.050(8) 0.052(8) 0.002(7) 0.003(6) -0.003(7) C33 0.044(7) 0.050(8) 0.043(7) 0.013(6) 0.008(6) -0.013(6) C34 0.059(9) 0.056(9) 0.051(8) 0.011(7) 0.007(7) 0.003(7) C36 0.062(8) 0.046(7) 0.052(7) 0.000(6) -0.004(6) -0.006(6) C37 0.064(8) 0.044(7) 0.052(7) -0.001(6) -0.002(6) -0.002(6) C38 0.067(9) 0.042(8) 0.055(8) -0.003(7) -0.001(7) -0.002(7) C39 0.071(9) 0.042(8) 0.059(9) -0.005(7) -0.002(8) 0.000(8) C40 0.071(10) 0.038(9) 0.061(10) -0.003(8) -0.005(9) 0.002(9) C41 0.074(17) 0.054(15) 0.082(19) 0.012(14) 0.033(15) -0.002(14) C42 0.078(17) 0.058(15) 0.089(19) 0.008(14) 0.028(15) -0.003(14) C37' 0.099(14) 0.058(12) 0.043(10) -0.016(9) 0.017(10) 0.000(11) C38' 0.100(14) 0.061(11) 0.043(10) -0.015(9) 0.017(9) 0.001(11) C39' 0.099(14) 0.065(11) 0.045(10) -0.014(9) 0.017(9) 0.002(11) C40' 0.099(14) 0.067(12) 0.046(10) -0.012(9) 0.018(10) 0.002(11) C41' 0.057(17) 0.24(5) 0.08(2) -0.08(3) 0.007(16) 0.02(2) C42' 0.057(17) 0.24(5) 0.09(2) -0.08(3) 0.009(16) 0.02(2) C43 0.061(10) 0.063(10) 0.060(9) 0.014(8) -0.001(7) -0.018(8) C44 0.041(8) 0.053(9) 0.061(9) 0.015(7) -0.002(6) 0.002(6) C45 0.061(10) 0.094(13) 0.055(9) 0.024(9) 0.010(8) 0.011(9) C46 0.057(10) 0.106(15) 0.083(12) 0.014(11) 0.030(9) 0.010(10) C47 0.054(10) 0.143(19) 0.062(11) 0.032(12) -0.009(8) -0.010(11) C48 0.068(12) 0.15(2) 0.047(10) 0.000(11) -0.003(8) 0.016(12) C49 0.055(9) 0.064(10) 0.056(9) 0.014(7) 0.013(7) 0.003(8) C50 0.107(16) 0.051(10) 0.119(16) 0.035(11) 0.002(12) -0.002(10) C51 0.068(13) 0.084(16) 0.25(3) 0.068(19) 0.009(16) -0.009(12) C52 0.19(3) 0.12(2) 0.16(2) -0.050(19) 0.05(2) 0.06(2) C53 0.055(11) 0.16(2) 0.092(14) 0.019(15) -0.017(10) -0.006(13) C54 0.14(2) 0.25(4) 0.15(2) -0.13(3) 0.004(18) -0.09(2) C55 0.110(18) 0.22(3) 0.092(16) 0.011(19) 0.028(14) -0.05(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 Zn1 O1 1.934(10) . ? Zn1 N3 1.935(11) . ? Zn1 N2 2.108(12) . ? Zn1 N1 2.138(11) . ? Zn2 N6 1.902(12) . ? Zn2 O2 1.947(10) . ? Zn2 N5 2.105(11) . ? Zn2 N4 2.142(11) . ? Si1 N3 1.687(12) . ? Si1 C22 1.819(18) . ? Si1 C23 1.82(3) . ? Si1 C24 1.89(2) . ? Si2 N3 1.703(12) . ? Si2 C27 1.84(2) . ? Si2 C26 1.838(17) . ? Si2 C25 1.88(2) . ? Si3 N6 1.734(13) . ? Si3 C51 1.81(2) . ? Si3 C52 1.86(2) . ? Si3 C50 1.872(19) . ? Si4 N6 1.687(12) . ? Si4 C53 1.87(2) . ? Si4 C55 1.89(2) . ? Si4 C54 1.92(2) . ? Cl1 C29 1.738(15) . ? Cl2 C31 1.698(17) . ? Cl3 C4 1.740(14) . ? Cl4 C2 1.752(15) . ? N1 C15 1.472(19) . ? N1 C7 1.475(16) . ? N1 C8 1.477(16) . ? N2 C12' 1.37(3) . ? N2 C12 1.45(3) . ? N2 C13' 1.479(19) . ? N2 C13 1.480(17) . ? N2 C9 1.53(3) . ? N2 C9' 1.54(3) . ? N4 C36 1.479(17) . ? N4 C43 1.491(19) . ? N4 C34 1.495(17) . ? N5 C40' 1.42(3) . ? N5 C41 1.452(17) . ? N5 C41' 1.455(19) . ? N5 C37' 1.48(3) . ? N5 C37 1.51(3) . ? N5 C40 1.55(3) . ? O1 C1 1.303(16) . ? O2 C28 1.269(17) . ? C1 C6 1.401(18) . ? C1 C2 1.42(2) . ? C2 C3 1.34(2) . ? C3 C4 1.32(2) . ? C3 H3 0.9300 . ? C4 C5 1.41(2) . ? C5 C6 1.384(18) . ? C5 H5 0.9300 . ? C6 C7 1.526(19) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9' 1.479(17) . ? C8 C9 1.549(17) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9593 . ? C8 H8D 0.9607 . ? C9 C10 1.538(18) . ? C9 H9 0.9800 . ? C10 C11 1.539(19) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.560(18) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.545(19) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C9' C10' 1.546(17) . ? C9' H9' 0.9800 . ? C10' C11' 1.547(18) . ? C10' H10C 0.9700 . ? C10' H10D 0.9700 . ? C11' C12' 1.537(18) . ? C11' H11C 0.9700 . ? C11' H11D 0.9700 . ? C12' H12C 0.9700 . ? C12' H12D 0.9700 . ? C13' C14' 1.537(19) . ? C13' H13C 0.9700 . ? C13' H13D 0.9700 . ? C14' H14D 0.9600 . ? C14' H14E 0.9600 . ? C14' H14F 0.9600 . ? C15 C16 1.509(19) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C21 1.351(19) . ? C16 C17 1.391(19) . ? C17 C18 1.36(2) . ? C17 H17 0.9300 . ? C18 C19 1.42(2) . ? C18 H18 0.9300 . ? C19 C20 1.35(2) . ? C19 H19 0.9300 . ? C20 C21 1.38(2) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C33 1.406(18) . ? C28 C29 1.43(2) . ? C29 C30 1.38(2) . ? C30 C31 1.38(2) . ? C30 H30 0.9300 . ? C31 C32 1.40(2) . ? C32 C33 1.423(18) . ? C32 H32 0.9300 . ? C33 C34 1.494(19) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C36 C37' 1.499(18) . ? C36 C37 1.540(17) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C36 H36C 0.9609 . ? C36 H36D 0.9599 . ? C37 C38 1.535(18) . ? C37 H37 0.9800 . ? C38 C39 1.544(19) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.539(18) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.539(19) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C37' C38' 1.547(18) . ? C37' H37' 0.9800 . ? C38' C39' 1.535(19) . ? C38' H38C 0.9700 . ? C38' H38D 0.9700 . ? C39' C40' 1.552(18) . ? C39' H39C 0.9700 . ? C39' H39D 0.9700 . ? C40' H40C 0.9700 . ? C40' H40D 0.9700 . ? C41' C42' 1.56(2) . ? C41' H41C 0.9700 . ? C41' H41D 0.9700 . ? C42' H42D 0.9600 . ? C42' H42E 0.9600 . ? C42' H42F 0.9600 . ? C43 C44 1.508(19) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.36(2) . ? C44 C49 1.390(19) . ? C45 C46 1.39(2) . ? C45 H45 0.9300 . ? C46 C47 1.34(2) . ? C46 H46 0.9300 . ? C47 C48 1.40(2) . ? C47 H47 0.9300 . ? C48 C49 1.38(2) . ? C48 H48 0.9300 . ? C49 H49 0.9300 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? 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 O1 Zn1 N3 115.2(5) . . ? O1 Zn1 N2 100.4(5) . . ? N3 Zn1 N2 130.2(5) . . ? O1 Zn1 N1 95.3(4) . . ? N3 Zn1 N1 121.6(5) . . ? N2 Zn1 N1 86.1(4) . . ? N6 Zn2 O2 114.3(5) . . ? N6 Zn2 N5 127.7(5) . . ? O2 Zn2 N5 101.0(5) . . ? N6 Zn2 N4 126.6(5) . . ? O2 Zn2 N4 93.4(4) . . ? N5 Zn2 N4 86.0(4) . . ? N3 Si1 C22 114.7(7) . . ? N3 Si1 C23 111.4(11) . . ? C22 Si1 C23 104.6(13) . . ? N3 Si1 C24 114.2(9) . . ? C22 Si1 C24 103.0(11) . . ? C23 Si1 C24 108.2(15) . . ? N3 Si2 C27 110.5(8) . . ? N3 Si2 C26 112.1(7) . . ? C27 Si2 C26 110.4(12) . . ? N3 Si2 C25 115.2(8) . . ? C27 Si2 C25 101.4(12) . . ? C26 Si2 C25 106.7(9) . . ? N6 Si3 C51 110.8(8) . . ? N6 Si3 C52 111.8(10) . . ? C51 Si3 C52 114.1(13) . . ? N6 Si3 C50 114.8(7) . . ? C51 Si3 C50 103.6(11) . . ? C52 Si3 C50 101.3(11) . . ? N6 Si4 C53 111.9(8) . . ? N6 Si4 C55 109.5(9) . . ? C53 Si4 C55 107.8(12) . . ? N6 Si4 C54 114.1(11) . . ? C53 Si4 C54 106.8(11) . . ? C55 Si4 C54 106.4(12) . . ? C15 N1 C7 107.3(11) . . ? C15 N1 C8 110.3(10) . . ? C7 N1 C8 112.7(11) . . ? C15 N1 Zn1 111.1(9) . . ? C7 N1 Zn1 109.1(8) . . ? C8 N1 Zn1 106.4(8) . . ? C12' N2 C12 109.9(18) . . ? C12' N2 C13' 118(2) . . ? C12 N2 C13' 34.4(14) . . ? C12' N2 C13 40.5(15) . . ? C12 N2 C13 103(2) . . ? C13' N2 C13 89(2) . . ? C12' N2 C9 66.2(16) . . ? C12 N2 C9 102.9(17) . . ? C13' N2 C9 137.3(18) . . ? C13 N2 C9 106.6(17) . . ? C12' N2 C9' 105.2(16) . . ? C12 N2 C9' 70.8(16) . . ? C13' N2 C9' 100.8(17) . . ? C13 N2 C9' 142.5(17) . . ? C9 N2 C9' 44.1(13) . . ? C12' N2 Zn1 126.3(12) . . ? C12 N2 Zn1 123.0(13) . . ? C13' N2 Zn1 102.0(15) . . ? C13 N2 Zn1 112.8(14) . . ? C9 N2 Zn1 107.3(10) . . ? C9' N2 Zn1 100.4(9) . . ? Si1 N3 Si2 123.5(7) . . ? Si1 N3 Zn1 125.2(6) . . ? Si2 N3 Zn1 111.3(6) . . ? C36 N4 C43 111.4(11) . . ? C36 N4 C34 113.1(11) . . ? C43 N4 C34 108.4(11) . . ? C36 N4 Zn2 106.0(8) . . ? C43 N4 Zn2 108.8(8) . . ? C34 N4 Zn2 109.0(8) . . ? C40' N5 C41 43.7(17) . . ? C40' N5 C41' 120(2) . . ? C41 N5 C41' 85(2) . . ? C40' N5 C37' 102.5(19) . . ? C41 N5 C37' 142.1(18) . . ? C41' N5 C37' 106(2) . . ? C40' N5 C37 62.2(18) . . ? C41 N5 C37 105.9(16) . . ? C41' N5 C37 143(2) . . ? C37' N5 C37 45.3(14) . . ? C40' N5 C40 110.9(17) . . ? C41 N5 C40 104(2) . . ? C41' N5 C40 41.6(17) . . ? C37' N5 C40 68.2(16) . . ? C37 N5 C40 101.6(16) . . ? C40' N5 Zn2 126.4(13) . . ? C41 N5 Zn2 114.2(15) . . ? C41' N5 Zn2 99.8(16) . . ? C37' N5 Zn2 99.7(10) . . ? C37 N5 Zn2 106.9(10) . . ? C40 N5 Zn2 122.6(12) . . ? Si4 N6 Si3 122.5(8) . . ? Si4 N6 Zn2 113.1(7) . . ? Si3 N6 Zn2 124.4(6) . . ? C1 O1 Zn1 125.4(8) . . ? C28 O2 Zn2 126.4(9) . . ? O1 C1 C6 124.3(12) . . ? O1 C1 C2 121.7(13) . . ? C6 C1 C2 114.0(12) . . ? C3 C2 C1 124.0(14) . . ? C3 C2 Cl4 118.9(14) . . ? C1 C2 Cl4 117.0(12) . . ? C4 C3 C2 120.7(14) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 119.9(13) . . ? C3 C4 Cl3 122.2(12) . . ? C5 C4 Cl3 117.9(12) . . ? C6 C5 C4 119.6(13) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C5 C6 C1 121.6(13) . . ? C5 C6 C7 117.6(12) . . ? C1 C6 C7 120.6(11) . . ? N1 C7 C6 116.1(11) . . ? N1 C7 H7A 108.3 . . ? C6 C7 H7A 108.3 . . ? N1 C7 H7B 108.3 . . ? C6 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? N1 C8 C9' 112.3(12) . . ? N1 C8 C9 117.2(13) . . ? C9' C8 C9 44.6(14) . . ? N1 C8 H8A 108.0 . . ? C9' C8 H8A 68.0 . . ? C9 C8 H8A 108.0 . . ? N1 C8 H8B 108.0 . . ? C9' C8 H8B 138.8 . . ? C9 C8 H8B 108.0 . . ? H8A C8 H8B 107.3 . . ? N1 C8 H8C 108.9 . . ? C9' C8 H8C 107.5 . . ? C9 C8 H8C 132.6 . . ? H8A C8 H8C 43.5 . . ? H8B C8 H8C 65.7 . . ? N1 C8 H8D 109.2 . . ? C9' C8 H8D 109.6 . . ? C9 C8 H8D 66.4 . . ? H8A C8 H8D 140.1 . . ? H8B C8 H8D 46.7 . . ? H8C C8 H8D 109.3 . . ? N2 C9 C10 109.1(19) . . ? N2 C9 C8 109.0(16) . . ? C10 C9 C8 118(2) . . ? N2 C9 H8D 135.3 . . ? C10 C9 H8D 113.5 . . ? C8 C9 H8D 37.1 . . ? N2 C9 H9 106.7 . . ? C10 C9 H9 106.7 . . ? C8 C9 H9 106.7 . . ? H8D C9 H9 73.5 . . ? C9 C10 C11 101(2) . . ? C9 C10 H10A 111.6 . . ? C11 C10 H10A 111.6 . . ? C9 C10 H10B 111.6 . . ? C11 C10 H10B 111.6 . . ? H10A C10 H10B 109.4 . . ? C10 C11 C12 109(2) . . ? C10 C11 H11A 110.0 . . ? C12 C11 H11A 110.0 . . ? C10 C11 H11B 110.0 . . ? C12 C11 H11B 110.0 . . ? H11A C11 H11B 108.4 . . ? N2 C12 C11 107(2) . . ? N2 C12 H12A 110.4 . . ? C11 C12 H12A 110.4 . . ? N2 C12 H12B 110.4 . . ? C11 C12 H12B 110.4 . . ? H12A C12 H12B 108.6 . . ? N2 C13 C14 109(2) . . ? N2 C13 H13A 109.8 . . ? C14 C13 H13A 109.8 . . ? N2 C13 H13B 109.8 . . ? C14 C13 H13B 109.8 . . ? H13A C13 H13B 108.2 . . ? C8 C9' N2 112.6(16) . . ? C8 C9' C10' 108.6(18) . . ? N2 C9' C10' 105.5(17) . . ? C8 C9' H9' 110.0 . . ? N2 C9' H9' 110.0 . . ? C10' C9' H9' 110.0 . . ? C9' C10' C11' 102.9(18) . . ? C9' C10' H10C 111.2 . . ? C11' C10' H10C 111.2 . . ? C9' C10' H10D 111.2 . . ? C11' C10' H10D 111.2 . . ? H10C C10' H10D 109.1 . . ? C12' C11' C10' 105.4(19) . . ? C12' C11' H11C 110.7 . . ? C10' C11' H11C 110.7 . . ? C12' C11' H11D 110.7 . . ? C10' C11' H11D 110.7 . . ? H11C C11' H11D 108.8 . . ? N2 C12' C11' 106(2) . . ? N2 C12' H12C 110.4 . . ? C11' C12' H12C 110.4 . . ? N2 C12' H12D 110.4 . . ? C11' C12' H12D 110.4 . . ? H12C C12' H12D 108.6 . . ? N2 C13' C14' 113(3) . . ? N2 C13' H13C 108.9 . . ? C14' C13' H13C 108.9 . . ? N2 C13' H13D 108.9 . . ? C14' C13' H13D 108.9 . . ? H13C C13' H13D 107.7 . . ? C13' C14' H14D 109.5 . . ? C13' C14' H14E 109.5 . . ? H14D C14' H14E 109.5 . . ? C13' C14' H14F 109.5 . . ? H14D C14' H14F 109.5 . . ? H14E C14' H14F 109.5 . . ? N1 C15 C16 120.6(14) . . ? N1 C15 H15A 107.2 . . ? C16 C15 H15A 107.2 . . ? N1 C15 H15B 107.2 . . ? C16 C15 H15B 107.2 . . ? H15A C15 H15B 106.8 . . ? C21 C16 C17 117.9(15) . . ? C21 C16 C15 120.8(13) . . ? C17 C16 C15 121.3(13) . . ? C18 C17 C16 121.8(15) . . ? C18 C17 H17 119.1 . . ? C16 C17 H17 119.1 . . ? C17 C18 C19 119.5(16) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C20 C19 C18 117.2(18) . . ? C20 C19 H19 121.4 . . ? C18 C19 H19 121.4 . . ? C19 C20 C21 122.5(17) . . ? C19 C20 H20 118.8 . . ? C21 C20 H20 118.8 . . ? C16 C21 C20 120.8(16) . . ? C16 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? Si1 C22 H22A 109.5 . . ? Si1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si1 C23 H23A 109.5 . . ? Si1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si1 C24 H24A 109.5 . . ? Si1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si2 C25 H25A 109.5 . . ? Si2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si2 C26 H26A 109.5 . . ? Si2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si2 C27 H27A 109.5 . . ? Si2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O2 C28 C33 125.6(13) . . ? O2 C28 C29 120.6(13) . . ? C33 C28 C29 113.7(13) . . ? C30 C29 C28 124.5(14) . . ? C30 C29 Cl1 116.5(13) . . ? C28 C29 Cl1 119.0(12) . . ? C29 C30 C31 120.9(15) . . ? C29 C30 H30 119.6 . . ? C31 C30 H30 119.6 . . ? C30 C31 C32 117.5(15) . . ? C30 C31 Cl2 123.5(14) . . ? C32 C31 Cl2 119.0(13) . . ? C31 C32 C33 121.5(13) . . ? C31 C32 H32 119.3 . . ? C33 C32 H32 119.3 . . ? C28 C33 C32 121.8(13) . . ? C28 C33 C34 119.4(12) . . ? C32 C33 C34 118.6(12) . . ? C33 C34 N4 115.3(12) . . ? C33 C34 H34A 108.4 . . ? N4 C34 H34A 108.4 . . ? C33 C34 H34B 108.4 . . ? N4 C34 H34B 108.4 . . ? H34A C34 H34B 107.5 . . ? N4 C36 C37' 111.6(13) . . ? N4 C36 C37 115.3(13) . . ? C37' C36 C37 44.5(16) . . ? N4 C36 H36A 108.5 . . ? C37' C36 H36A 138.9 . . ? C37 C36 H36A 108.4 . . ? N4 C36 H36B 108.4 . . ? C37' C36 H36B 68.2 . . ? C37 C36 H36B 108.5 . . ? H36A C36 H36B 107.5 . . ? N4 C36 H36C 109.5 . . ? C37' C36 H36C 107.9 . . ? C37 C36 H36C 65.0 . . ? H36A C36 H36C 48.0 . . ? H36B C36 H36C 140.1 . . ? N4 C36 H36D 108.2 . . ? C37' C36 H36D 110.6 . . ? C37 C36 H36D 135.5 . . ? H36A C36 H36D 63.8 . . ? H36B C36 H36D 46.1 . . ? H36C C36 H36D 109.0 . . ? N5 C37 C38 107.3(19) . . ? N5 C37 C36 110.3(16) . . ? C38 C37 C36 115(2) . . ? N5 C37 H36C 138.5 . . ? C38 C37 H36C 111.0 . . ? C36 C37 H36C 37.5 . . ? N5 C37 H37 108.1 . . ? C38 C37 H37 108.1 . . ? C36 C37 H37 108.1 . . ? H36C C37 H37 74.7 . . ? C37 C38 C39 107(2) . . ? C37 C38 H38A 110.2 . . ? C39 C38 H38A 110.2 . . ? C37 C38 H38B 110.2 . . ? C39 C38 H38B 110.2 . . ? H38A C38 H38B 108.5 . . ? C40 C39 C38 104(2) . . ? C40 C39 H39A 111.0 . . ? C38 C39 H39A 111.0 . . ? C40 C39 H39B 111.0 . . ? C38 C39 H39B 111.0 . . ? H39A C39 H39B 109.0 . . ? C39 C40 N5 108(2) . . ? C39 C40 H40A 110.1 . . ? N5 C40 H40A 110.1 . . ? C39 C40 H40B 110.1 . . ? N5 C40 H40B 110.1 . . ? H40A C40 H40B 108.4 . . ? N5 C41 C42 113(2) . . ? N5 C41 H41A 108.9 . . ? C42 C41 H41A 108.9 . . ? N5 C41 H41B 108.9 . . ? C42 C41 H41B 108.9 . . ? H41A C41 H41B 107.7 . . ? N5 C37' C36 114(2) . . ? N5 C37' C38' 108(2) . . ? C36 C37' C38' 104(2) . . ? N5 C37' H37' 110.5 . . ? C36 C37' H37' 110.5 . . ? C38' C37' H37' 110.5 . . ? C39' C38' C37' 104(2) . . ? C39' C38' H38C 110.9 . . ? C37' C38' H38C 110.9 . . ? C39' C38' H38D 110.9 . . ? C37' C38' H38D 110.9 . . ? H38C C38' H38D 109.0 . . ? C38' C39' C40' 102(2) . . ? C38' C39' H39C 111.3 . . ? C40' C39' H39C 111.3 . . ? C38' C39' H39D 111.3 . . ? C40' C39' H39D 111.3 . . ? H39C C39' H39D 109.2 . . ? N5 C40' C39' 107(2) . . ? N5 C40' H40C 110.3 . . ? C39' C40' H40C 110.3 . . ? N5 C40' H40D 110.3 . . ? C39' C40' H40D 110.3 . . ? H40C C40' H40D 108.6 . . ? N5 C41' C42' 112(3) . . ? N5 C41' H41C 109.2 . . ? C42' C41' H41C 109.2 . . ? N5 C41' H41D 109.2 . . ? C42' C41' H41D 109.2 . . ? H41C C41' H41D 107.9 . . ? C41' C42' H42D 109.5 . . ? C41' C42' H42E 109.5 . . ? H42D C42' H42E 109.5 . . ? C41' C42' H42F 109.5 . . ? H42D C42' H42F 109.5 . . ? H42E C42' H42F 109.5 . . ? N4 C43 C44 117.9(12) . . ? N4 C43 H43A 107.8 . . ? C44 C43 H43A 107.8 . . ? N4 C43 H43B 107.8 . . ? C44 C43 H43B 107.8 . . ? H43A C43 H43B 107.2 . . ? C45 C44 C49 116.8(13) . . ? C45 C44 C43 122.8(14) . . ? C49 C44 C43 120.4(13) . . ? C44 C45 C46 122.7(15) . . ? C44 C45 H45 118.7 . . ? C46 C45 H45 118.7 . . ? C47 C46 C45 120.1(16) . . ? C47 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C46 C47 C48 119.2(16) . . ? C46 C47 H47 120.4 . . ? C48 C47 H47 120.4 . . ? C49 C48 C47 119.3(15) . . ? C49 C48 H48 120.3 . . ? C47 C48 H48 120.3 . . ? C48 C49 C44 121.7(14) . . ? C48 C49 H49 119.2 . . ? C44 C49 H49 119.2 . . ? Si3 C50 H50A 109.5 . . ? Si3 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? Si3 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? Si3 C51 H51A 109.5 . . ? Si3 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? Si3 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? Si3 C52 H52A 109.5 . . ? Si3 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? Si3 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? Si4 C53 H53A 109.5 . . ? Si4 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? Si4 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? Si4 C54 H54A 109.5 . . ? Si4 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? Si4 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? Si4 C55 H55A 109.5 . . ? Si4 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? Si4 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? 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 O1 Zn1 N1 C15 -141.4(9) . . . . ? N3 Zn1 N1 C15 -17.4(10) . . . . ? N2 Zn1 N1 C15 118.4(9) . . . . ? O1 Zn1 N1 C7 -23.4(9) . . . . ? N3 Zn1 N1 C7 100.6(9) . . . . ? N2 Zn1 N1 C7 -123.5(9) . . . . ? O1 Zn1 N1 C8 98.5(9) . . . . ? N3 Zn1 N1 C8 -137.5(8) . . . . ? N2 Zn1 N1 C8 -1.6(9) . . . . ? O1 Zn1 N2 C12' 172.9(18) . . . . ? N3 Zn1 N2 C12' 37(2) . . . . ? N1 Zn1 N2 C12' -92.5(19) . . . . ? O1 Zn1 N2 C12 4.4(18) . . . . ? N3 Zn1 N2 C12 -131.8(17) . . . . ? N1 Zn1 N2 C12 99.0(18) . . . . ? O1 Zn1 N2 C13' 34.2(15) . . . . ? N3 Zn1 N2 C13' -102.1(16) . . . . ? N1 Zn1 N2 C13' 128.8(15) . . . . ? O1 Zn1 N2 C13 128.6(15) . . . . ? N3 Zn1 N2 C13 -7.7(17) . . . . ? N1 Zn1 N2 C13 -136.8(16) . . . . ? O1 Zn1 N2 C9 -114.3(12) . . . . ? N3 Zn1 N2 C9 109.4(13) . . . . ? N1 Zn1 N2 C9 -19.7(13) . . . . ? O1 Zn1 N2 C9' -69.4(11) . . . . ? N3 Zn1 N2 C9' 154.4(10) . . . . ? N1 Zn1 N2 C9' 25.3(11) . . . . ? C22 Si1 N3 Si2 172.5(11) . . . . ? C23 Si1 N3 Si2 -68.9(14) . . . . ? C24 Si1 N3 Si2 54.0(15) . . . . ? C22 Si1 N3 Zn1 -5.9(13) . . . . ? C23 Si1 N3 Zn1 112.6(13) . . . . ? C24 Si1 N3 Zn1 -124.5(13) . . . . ? C27 Si2 N3 Si1 -116.7(13) . . . . ? C26 Si2 N3 Si1 119.8(10) . . . . ? C25 Si2 N3 Si1 -2.5(13) . . . . ? C27 Si2 N3 Zn1 62.0(13) . . . . ? C26 Si2 N3 Zn1 -61.6(10) . . . . ? C25 Si2 N3 Zn1 176.2(9) . . . . ? O1 Zn1 N3 Si1 -176.3(7) . . . . ? N2 Zn1 N3 Si1 -45.0(11) . . . . ? N1 Zn1 N3 Si1 69.6(9) . . . . ? O1 Zn1 N3 Si2 5.1(8) . . . . ? N2 Zn1 N3 Si2 136.4(6) . . . . ? N1 Zn1 N3 Si2 -109.0(6) . . . . ? N6 Zn2 N4 C36 140.3(9) . . . . ? O2 Zn2 N4 C36 -95.8(9) . . . . ? N5 Zn2 N4 C36 5.0(9) . . . . ? N6 Zn2 N4 C43 20.4(11) . . . . ? O2 Zn2 N4 C43 144.3(9) . . . . ? N5 Zn2 N4 C43 -114.9(9) . . . . ? N6 Zn2 N4 C34 -97.7(10) . . . . ? O2 Zn2 N4 C34 26.2(10) . . . . ? N5 Zn2 N4 C34 127.0(9) . . . . ? N6 Zn2 N5 C40' -49(2) . . . . ? O2 Zn2 N5 C40' 178(2) . . . . ? N4 Zn2 N5 C40' 85(2) . . . . ? N6 Zn2 N5 C41 0.0(17) . . . . ? O2 Zn2 N5 C41 -132.8(15) . . . . ? N4 Zn2 N5 C41 134.5(15) . . . . ? N6 Zn2 N5 C41' 89.2(19) . . . . ? O2 Zn2 N5 C41' -43.6(19) . . . . ? N4 Zn2 N5 C41' -136.3(18) . . . . ? N6 Zn2 N5 C37' -162.8(12) . . . . ? O2 Zn2 N5 C37' 64.4(13) . . . . ? N4 Zn2 N5 C37' -28.3(12) . . . . ? N6 Zn2 N5 C37 -116.8(12) . . . . ? O2 Zn2 N5 C37 110.4(12) . . . . ? N4 Zn2 N5 C37 17.8(12) . . . . ? N6 Zn2 N5 C40 126.9(16) . . . . ? O2 Zn2 N5 C40 -5.9(17) . . . . ? N4 Zn2 N5 C40 -98.6(16) . . . . ? C53 Si4 N6 Si3 -125.5(10) . . . . ? C55 Si4 N6 Si3 115.1(13) . . . . ? C54 Si4 N6 Si3 -4.0(14) . . . . ? C53 Si4 N6 Zn2 55.2(11) . . . . ? C55 Si4 N6 Zn2 -64.2(13) . . . . ? C54 Si4 N6 Zn2 176.7(10) . . . . ? C51 Si3 N6 Si4 66.4(14) . . . . ? C52 Si3 N6 Si4 -62.0(14) . . . . ? C50 Si3 N6 Si4 -176.7(10) . . . . ? C51 Si3 N6 Zn2 -114.3(12) . . . . ? C52 Si3 N6 Zn2 117.2(12) . . . . ? C50 Si3 N6 Zn2 2.5(12) . . . . ? O2 Zn2 N6 Si4 1.6(9) . . . . ? N5 Zn2 N6 Si4 -126.2(7) . . . . ? N4 Zn2 N6 Si4 116.1(7) . . . . ? O2 Zn2 N6 Si3 -177.7(7) . . . . ? N5 Zn2 N6 Si3 54.5(10) . . . . ? N4 Zn2 N6 Si3 -63.1(10) . . . . ? N3 Zn1 O1 C1 -147.0(12) . . . . ? N2 Zn1 O1 C1 68.7(13) . . . . ? N1 Zn1 O1 C1 -18.3(13) . . . . ? N6 Zn2 O2 C28 148.7(13) . . . . ? N5 Zn2 O2 C28 -70.9(14) . . . . ? N4 Zn2 O2 C28 15.7(14) . . . . ? Zn1 O1 C1 C6 31(2) . . . . ? Zn1 O1 C1 C2 -149.0(11) . . . . ? O1 C1 C2 C3 -175.6(14) . . . . ? C6 C1 C2 C3 4(2) . . . . ? O1 C1 C2 Cl4 2(2) . . . . ? C6 C1 C2 Cl4 -178.0(10) . . . . ? C1 C2 C3 C4 -4(2) . . . . ? Cl4 C2 C3 C4 178.0(11) . . . . ? C2 C3 C4 C5 0(2) . . . . ? C2 C3 C4 Cl3 -179.5(12) . . . . ? C3 C4 C5 C6 3(2) . . . . ? Cl3 C4 C5 C6 -177.1(10) . . . . ? C4 C5 C6 C1 -3(2) . . . . ? C4 C5 C6 C7 173.0(12) . . . . ? O1 C1 C6 C5 179.3(13) . . . . ? C2 C1 C6 C5 -0.6(19) . . . . ? O1 C1 C6 C7 4(2) . . . . ? C2 C1 C6 C7 -176.3(12) . . . . ? C15 N1 C7 C6 177.1(12) . . . . ? C8 N1 C7 C6 -61.3(15) . . . . ? Zn1 N1 C7 C6 56.7(13) . . . . ? C5 C6 C7 N1 130.1(13) . . . . ? C1 C6 C7 N1 -54.1(17) . . . . ? C15 N1 C8 C9' -145.6(15) . . . . ? C7 N1 C8 C9' 94.5(17) . . . . ? Zn1 N1 C8 C9' -25.0(16) . . . . ? C15 N1 C8 C9 -96.4(18) . . . . ? C7 N1 C8 C9 143.6(17) . . . . ? Zn1 N1 C8 C9 24.1(18) . . . . ? C12' N2 C9 C10 -71(2) . . . . ? C12 N2 C9 C10 36(3) . . . . ? C13' N2 C9 C10 35(4) . . . . ? C13 N2 C9 C10 -72(3) . . . . ? C9' N2 C9 C10 79(2) . . . . ? Zn1 N2 C9 C10 166.5(18) . . . . ? C12' N2 C9 C8 159(2) . . . . ? C12 N2 C9 C8 -95(2) . . . . ? C13' N2 C9 C8 -95(3) . . . . ? C13 N2 C9 C8 157.2(19) . . . . ? C9' N2 C9 C8 -51.0(14) . . . . ? Zn1 N2 C9 C8 36(2) . . . . ? N1 C8 C9 N2 -42(2) . . . . ? C9' C8 C9 N2 53.1(18) . . . . ? N1 C8 C9 C10 -167.2(19) . . . . ? C9' C8 C9 C10 -72(2) . . . . ? N2 C9 C10 C11 -25(3) . . . . ? C8 C9 C10 C11 100(3) . . . . ? C9 C10 C11 C12 6(3) . . . . ? C12' N2 C12 C11 39(3) . . . . ? C13' N2 C12 C11 150(5) . . . . ? C13 N2 C12 C11 81(3) . . . . ? C9 N2 C12 C11 -30(3) . . . . ? C9' N2 C12 C11 -61(2) . . . . ? Zn1 N2 C12 C11 -150.7(17) . . . . ? C10 C11 C12 N2 15(3) . . . . ? C12' N2 C13 C14 -179(4) . . . . ? C12 N2 C13 C14 75(3) . . . . ? C13' N2 C13 C14 43(3) . . . . ? C9 N2 C13 C14 -177(2) . . . . ? C9' N2 C13 C14 150(2) . . . . ? Zn1 N2 C13 C14 -59(3) . . . . ? N1 C8 C9' N2 52(2) . . . . ? C9 C8 C9' N2 -54.7(19) . . . . ? N1 C8 C9' C10' 168.4(16) . . . . ? C9 C8 C9' C10' 62(2) . . . . ? C12' N2 C9' C8 85(2) . . . . ? C12 N2 C9' C8 -169(2) . . . . ? C13' N2 C9' C8 -152(2) . . . . ? C13 N2 C9' C8 104(3) . . . . ? C9 N2 C9' C8 56.4(16) . . . . ? Zn1 N2 C9' C8 -47.7(16) . . . . ? C12' N2 C9' C10' -34(2) . . . . ? C12 N2 C9' C10' 73(2) . . . . ? C13' N2 C9' C10' 89(2) . . . . ? C13 N2 C9' C10' -14(4) . . . . ? C9 N2 C9' C10' -62(2) . . . . ? Zn1 N2 C9' C10' -166.0(16) . . . . ? C8 C9' C10' C11' -107(2) . . . . ? N2 C9' C10' C11' 14(3) . . . . ? C9' C10' C11' C12' 8(3) . . . . ? C12 N2 C12' C11' -35(3) . . . . ? C13' N2 C12' C11' -72(3) . . . . ? C13 N2 C12' C11' -122(4) . . . . ? C9 N2 C12' C11' 60(2) . . . . ? C9' N2 C12' C11' 39(2) . . . . ? Zn1 N2 C12' C11' 154.8(15) . . . . ? C10' C11' C12' N2 -30(3) . . . . ? C12' N2 C13' C14' -75(3) . . . . ? C12 N2 C13' C14' -159(5) . . . . ? C13 N2 C13' C14' -45(3) . . . . ? C9 N2 C13' C14' -159(2) . . . . ? C9' N2 C13' C14' 172(3) . . . . ? Zn1 N2 C13' C14' 68(3) . . . . ? C7 N1 C15 C16 56.7(16) . . . . ? C8 N1 C15 C16 -66.4(16) . . . . ? Zn1 N1 C15 C16 175.9(10) . . . . ? N1 C15 C16 C21 92.9(19) . . . . ? N1 C15 C16 C17 -85(2) . . . . ? C21 C16 C17 C18 1(3) . . . . ? C15 C16 C17 C18 179.6(19) . . . . ? C16 C17 C18 C19 -4(3) . . . . ? C17 C18 C19 C20 6(4) . . . . ? C18 C19 C20 C21 -5(4) . . . . ? C17 C16 C21 C20 -1(3) . . . . ? C15 C16 C21 C20 -178.8(18) . . . . ? C19 C20 C21 C16 3(3) . . . . ? Zn2 O2 C28 C33 -30(2) . . . . ? Zn2 O2 C28 C29 149.7(12) . . . . ? O2 C28 C29 C30 178.0(14) . . . . ? C33 C28 C29 C30 -2(2) . . . . ? O2 C28 C29 Cl1 -3(2) . . . . ? C33 C28 C29 Cl1 177.4(10) . . . . ? C28 C29 C30 C31 2(2) . . . . ? Cl1 C29 C30 C31 -177.5(12) . . . . ? C29 C30 C31 C32 0(2) . . . . ? C29 C30 C31 Cl2 -179.1(12) . . . . ? C30 C31 C32 C33 -1(2) . . . . ? Cl2 C31 C32 C33 177.7(11) . . . . ? O2 C28 C33 C32 -179.5(14) . . . . ? C29 C28 C33 C32 1(2) . . . . ? O2 C28 C33 C34 -4(2) . . . . ? C29 C28 C33 C34 176.3(13) . . . . ? C31 C32 C33 C28 1(2) . . . . ? C31 C32 C33 C34 -174.7(13) . . . . ? C28 C33 C34 N4 54.9(18) . . . . ? C32 C33 C34 N4 -129.3(13) . . . . ? C36 N4 C34 C33 57.9(16) . . . . ? C43 N4 C34 C33 -178.1(12) . . . . ? Zn2 N4 C34 C33 -59.8(14) . . . . ? C43 N4 C36 C37' 139.0(18) . . . . ? C34 N4 C36 C37' -98.6(19) . . . . ? Zn2 N4 C36 C37' 20.7(18) . . . . ? C43 N4 C36 C37 90.4(17) . . . . ? C34 N4 C36 C37 -147.2(16) . . . . ? Zn2 N4 C36 C37 -27.9(17) . . . . ? C40' N5 C37 C38 75(2) . . . . ? C41 N5 C37 C38 75(3) . . . . ? C41' N5 C37 C38 -28(4) . . . . ? C37' N5 C37 C38 -75(2) . . . . ? C40 N5 C37 C38 -33(2) . . . . ? Zn2 N5 C37 C38 -162.4(17) . . . . ? C40' N5 C37 C36 -159(2) . . . . ? C41 N5 C37 C36 -159(2) . . . . ? C41' N5 C37 C36 98(3) . . . . ? C37' N5 C37 C36 50.2(15) . . . . ? C40 N5 C37 C36 93(2) . . . . ? Zn2 N5 C37 C36 -36.7(19) . . . . ? N4 C36 C37 N5 45(2) . . . . ? C37' C36 C37 N5 -50(2) . . . . ? N4 C36 C37 C38 166.6(18) . . . . ? C37' C36 C37 C38 71(3) . . . . ? N5 C37 C38 C39 21(3) . . . . ? C36 C37 C38 C39 -102(3) . . . . ? C37 C38 C39 C40 1(3) . . . . ? C38 C39 C40 N5 -22(3) . . . . ? C40' N5 C40 C39 -31(3) . . . . ? C41 N5 C40 C39 -76(3) . . . . ? C41' N5 C40 C39 -142(4) . . . . ? C37' N5 C40 C39 65(2) . . . . ? C37 N5 C40 C39 34(3) . . . . ? Zn2 N5 C40 C39 152.8(17) . . . . ? C40' N5 C41 C42 178(4) . . . . ? C41' N5 C41 C42 -38(3) . . . . ? C37' N5 C41 C42 -148(3) . . . . ? C37 N5 C41 C42 178(3) . . . . ? C40 N5 C41 C42 -76(3) . . . . ? Zn2 N5 C41 C42 60(3) . . . . ? C40' N5 C37' C36 -81(2) . . . . ? C41 N5 C37' C36 -104(3) . . . . ? C41' N5 C37' C36 153(2) . . . . ? C37 N5 C37' C36 -54.2(17) . . . . ? C40 N5 C37' C36 171(2) . . . . ? Zn2 N5 C37' C36 50.0(19) . . . . ? C40' N5 C37' C38' 33(3) . . . . ? C41 N5 C37' C38' 10(4) . . . . ? C41' N5 C37' C38' -93(3) . . . . ? C37 N5 C37' C38' 60(2) . . . . ? C40 N5 C37' C38' -74(2) . . . . ? Zn2 N5 C37' C38' 164(2) . . . . ? N4 C36 C37' N5 -51(2) . . . . ? C37 C36 C37' N5 54(2) . . . . ? N4 C36 C37' C38' -167.7(18) . . . . ? C37 C36 C37' C38' -63(2) . . . . ? N5 C37' C38' C39' -12(3) . . . . ? C36 C37' C38' C39' 109(3) . . . . ? C37' C38' C39' C40' -12(4) . . . . ? C41 N5 C40' C39' 118(4) . . . . ? C41' N5 C40' C39' 75(3) . . . . ? C37' N5 C40' C39' -42(3) . . . . ? C37 N5 C40' C39' -63(2) . . . . ? C40 N5 C40' C39' 30(3) . . . . ? Zn2 N5 C40' C39' -153.9(18) . . . . ? C38' C39' C40' N5 34(4) . . . . ? C40' N5 C41' C42' 66(3) . . . . ? C41 N5 C41' C42' 38(3) . . . . ? C37' N5 C41' C42' -179(3) . . . . ? C37 N5 C41' C42' 148(3) . . . . ? C40 N5 C41' C42' 155(5) . . . . ? Zn2 N5 C41' C42' -76(3) . . . . ? C36 N4 C43 C44 64.4(16) . . . . ? C34 N4 C43 C44 -60.6(16) . . . . ? Zn2 N4 C43 C44 -179.0(10) . . . . ? N4 C43 C44 C45 83(2) . . . . ? N4 C43 C44 C49 -97.2(17) . . . . ? C49 C44 C45 C46 -1(3) . . . . ? C43 C44 C45 C46 179.0(17) . . . . ? C44 C45 C46 C47 2(3) . . . . ? C45 C46 C47 C48 -5(3) . . . . ? C46 C47 C48 C49 7(3) . . . . ? C47 C48 C49 C44 -6(3) . . . . ? C45 C44 C49 C48 3(3) . . . . ? C43 C44 C49 C48 -177.1(17) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.207 _refine_diff_density_min -0.985 _refine_diff_density_rms 0.138 _database_code_depnum_ccdc_archive 'CCDC 936902'