# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name _publ_author_address P.Roesky ; Institut f\"ur Anorganische Chemie KIT Engesserstra\&se 15 76131 Karlsruhe Bundesrepublik Deutschland ; T.Panda ; Institut f\"ur Anorganische Chemie KIT Engesserstra\&se 15 76131 Karlsruhe Bundesrepublik Deutschland ; S.Marks '' _publ_contact_author_name 'Roesky, Peter' _publ_contact_author_email roesky@kit.edu _publ_section_title ; Bis(phosphinimino)methanides as Non-Innocnet Ligand in Zinc Chemistry - Synthesis and Structures ; _publ_contact_author ; Prof. Dr. Peter Roesky Institut f\"ur Anorganische Chemie KIT Engesserstra\&se 15 76131 Karlsruhe Bundesrepublik Deutschland ; _publ_contact_author_fax +49/(0)7216084854 _publ_contact_author_phone +49/(0)7216086117 _publ_contact_letter ; ; _publ_requested_coeditor_name ? # Attachment '- deposit.CIF' data_1 _database_code_depnum_ccdc_archive 'CCDC 770404' #TrackingRef '- deposit.CIF' _audit_creation_date 05-01-06 _audit_creation_method 'STOE X-RED' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C31 H40 Cl2 N2 P2 Si2 Zn), 3(C7 H8)' _chemical_formula_sum 'C83 H104 Cl4 N4 P4 Si4 Zn2' _chemical_formula_weight 1666.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.585(3) _cell_length_b 16.613(3) _cell_length_c 21.407(4) _cell_angle_alpha 84.54(3) _cell_angle_beta 82.55(3) _cell_angle_gamma 76.71(3) _cell_volume 4309.3(15) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 24279 _cell_measurement_theta_min 3.31 _cell_measurement_theta_max 29.50 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.195 _exptl_crystal_size_mid 0.146 _exptl_crystal_size_min 0.070 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.284 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1748 _exptl_absorpt_coefficient_mu 0.854 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8173 _exptl_absorpt_correction_T_max 0.9256 _exptl_absorpt_process_details 'STOE X-RED & X-SHAPE' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'STOE IPDS 2T' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42069 _diffrn_reflns_av_R_equivalents 0.0636 _diffrn_reflns_av_sigmaI/netI 0.0917 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 29.25 _reflns_number_total 22790 _reflns_number_gt 14703 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e' _computing_publication_material 'X-STEP32, Microsoft Word' _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^)+(0.0343P)^2^+1.9477P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 22790 _refine_ls_number_parameters 919 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1084 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.1075 _refine_ls_wR_factor_gt 0.0946 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.77875(3) 0.21860(2) 0.556654(16) 0.02165(8) Uani 1 1 d . . . Zn2 Zn 0.71862(3) 0.26515(2) 0.052512(15) 0.02040(8) Uani 1 1 d . . . Cl1 Cl 0.82301(8) 0.13834(6) 0.64355(4) 0.0387(2) Uani 1 1 d . . . Cl2 Cl 0.71396(7) 0.35362(5) 0.58315(4) 0.03173(18) Uani 1 1 d . . . Cl3 Cl 0.61975(8) 0.31613(6) 0.14026(4) 0.03501(19) Uani 1 1 d . . . Cl4 Cl 0.86581(7) 0.16529(5) 0.08116(4) 0.03082(17) Uani 1 1 d . . . P1 P 0.64007(6) 0.23346(5) 0.44544(3) 0.01794(15) Uani 1 1 d . . . P2 P 0.87817(6) 0.26750(5) 0.42203(3) 0.01738(14) Uani 1 1 d . . . P3 P 0.84193(6) 0.32159(5) -0.07343(3) 0.01864(15) Uani 1 1 d . . . P4 P 0.70143(6) 0.18730(5) -0.06976(3) 0.01745(14) Uani 1 1 d . . . Si1 Si 0.56731(8) 0.13501(6) 0.55915(4) 0.02820(19) Uani 1 1 d . . . Si2 Si 1.04005(7) 0.18808(6) 0.51105(4) 0.02517(18) Uani 1 1 d . . . Si3 Si 0.78399(8) 0.44422(6) 0.02385(4) 0.02684(19) Uani 1 1 d . . . Si4 Si 0.52222(7) 0.17496(6) 0.03322(4) 0.02347(18) Uani 1 1 d . . . N1 N 0.6579(2) 0.18853(16) 0.51347(11) 0.0212(5) Uani 1 1 d . . . N2 N 0.9080(2) 0.21735(15) 0.48670(11) 0.0199(5) Uani 1 1 d . . . N3 N 0.7765(2) 0.35317(15) -0.00866(11) 0.0206(5) Uani 1 1 d . . . N4 N 0.6387(2) 0.20968(15) -0.00249(11) 0.0186(5) Uani 1 1 d . . . C1 C 0.7305(2) 0.30552(18) 0.42461(13) 0.0188(5) Uani 1 1 d . . . H1A H 0.7151 0.3326 0.3825 0.023 Uiso 1 1 calc R . . H1B H 0.7087 0.3493 0.4550 0.023 Uiso 1 1 calc R . . C2 C 0.5066(2) 0.30229(19) 0.44038(13) 0.0215(6) Uani 1 1 d . . . C3 C 0.4760(3) 0.3669(2) 0.48084(15) 0.0282(7) Uani 1 1 d . . . H3 H 0.5231 0.3721 0.5108 0.034 Uiso 1 1 calc R . . C4 C 0.3767(3) 0.4233(2) 0.47714(17) 0.0374(8) Uani 1 1 d . . . H4 H 0.3560 0.4672 0.5047 0.045 Uiso 1 1 calc R . . C5 C 0.3073(3) 0.4162(2) 0.43351(17) 0.0382(8) Uani 1 1 d . . . H5 H 0.2402 0.4560 0.4305 0.046 Uiso 1 1 calc R . . C6 C 0.3361(3) 0.3512(2) 0.39457(16) 0.0330(8) Uani 1 1 d . . . H6 H 0.2875 0.3452 0.3657 0.040 Uiso 1 1 calc R . . C7 C 0.4359(3) 0.2944(2) 0.39742(15) 0.0272(7) Uani 1 1 d . . . H7 H 0.4559 0.2502 0.3701 0.033 Uiso 1 1 calc R . . C8 C 0.6625(2) 0.16378(19) 0.38280(13) 0.0208(6) Uani 1 1 d . . . C9 C 0.6842(3) 0.0786(2) 0.39713(15) 0.0278(7) Uani 1 1 d . . . H9 H 0.6876 0.0572 0.4397 0.033 Uiso 1 1 calc R . . C10 C 0.7008(3) 0.0249(2) 0.34912(17) 0.0366(8) Uani 1 1 d . . . H10 H 0.7144 -0.0332 0.3591 0.044 Uiso 1 1 calc R . . C11 C 0.6977(3) 0.0554(2) 0.28703(17) 0.0380(9) Uani 1 1 d . . . H11 H 0.7092 0.0181 0.2545 0.046 Uiso 1 1 calc R . . C12 C 0.6782(3) 0.1395(2) 0.27190(15) 0.0345(8) Uani 1 1 d . . . H12 H 0.6773 0.1602 0.2290 0.041 Uiso 1 1 calc R . . C13 C 0.6597(3) 0.1943(2) 0.31937(14) 0.0259(6) Uani 1 1 d . . . H13 H 0.6451 0.2524 0.3089 0.031 Uiso 1 1 calc R . . C14 C 0.9173(2) 0.20993(19) 0.35214(13) 0.0205(6) Uani 1 1 d . . . C15 C 0.8929(3) 0.2492(2) 0.29324(14) 0.0252(6) Uani 1 1 d . . . H15 H 0.8624 0.3071 0.2896 0.030 Uiso 1 1 calc R . . C16 C 0.9130(3) 0.2038(2) 0.24028(15) 0.0312(7) Uani 1 1 d . . . H16 H 0.8964 0.2305 0.2004 0.037 Uiso 1 1 calc R . . C17 C 0.9572(3) 0.1199(2) 0.24554(16) 0.0351(8) Uani 1 1 d . . . H17 H 0.9711 0.0889 0.2091 0.042 Uiso 1 1 calc R . . C18 C 0.9814(3) 0.0803(2) 0.30368(16) 0.0336(8) Uani 1 1 d . . . H18 H 1.0121 0.0224 0.3070 0.040 Uiso 1 1 calc R . . C19 C 0.9607(3) 0.1253(2) 0.35698(14) 0.0254(6) Uani 1 1 d . . . H19 H 0.9763 0.0980 0.3969 0.031 Uiso 1 1 calc R . . C20 C 0.9307(2) 0.36112(19) 0.40576(14) 0.0219(6) Uani 1 1 d . . . C21 C 1.0116(3) 0.3699(2) 0.35588(15) 0.0279(7) Uani 1 1 d . . . H21 H 1.0381 0.3271 0.3277 0.033 Uiso 1 1 calc R . . C22 C 1.0535(3) 0.4411(2) 0.34727(17) 0.0347(8) Uani 1 1 d . . . H22 H 1.1088 0.4466 0.3135 0.042 Uiso 1 1 calc R . . C23 C 1.0145(3) 0.5039(2) 0.38786(18) 0.0379(8) Uani 1 1 d . . . H23 H 1.0427 0.5528 0.3817 0.046 Uiso 1 1 calc R . . C24 C 0.9349(3) 0.4959(2) 0.43734(17) 0.0338(8) Uani 1 1 d . . . H24 H 0.9086 0.5393 0.4651 0.041 Uiso 1 1 calc R . . C25 C 0.8928(3) 0.4247(2) 0.44685(15) 0.0279(7) Uani 1 1 d . . . H25 H 0.8384 0.4193 0.4812 0.033 Uiso 1 1 calc R . . C26 C 0.4507(3) 0.1260(3) 0.51635(18) 0.0425(9) Uani 1 1 d . . . H26A H 0.4011 0.1806 0.5115 0.064 Uiso 1 1 calc R . . H26B H 0.4105 0.0871 0.5405 0.064 Uiso 1 1 calc R . . H26C H 0.4794 0.1057 0.4746 0.064 Uiso 1 1 calc R . . C27 C 0.6429(4) 0.0282(3) 0.5818(2) 0.0491(10) Uani 1 1 d . . . H27A H 0.6710 -0.0018 0.5437 0.074 Uiso 1 1 calc R . . H27B H 0.5930 -0.0010 0.6090 0.074 Uiso 1 1 calc R . . H27C H 0.7044 0.0312 0.6046 0.074 Uiso 1 1 calc R . . C28 C 0.5080(4) 0.1904(3) 0.63117(19) 0.0572(13) Uani 1 1 d . . . H28A H 0.5658 0.1875 0.6584 0.086 Uiso 1 1 calc R . . H28B H 0.4505 0.1644 0.6540 0.086 Uiso 1 1 calc R . . H28C H 0.4762 0.2485 0.6192 0.086 Uiso 1 1 calc R . . C29 C 1.0465(4) 0.2536(3) 0.5758(2) 0.0490(10) Uani 1 1 d . . . H29A H 1.0348 0.3119 0.5597 0.073 Uiso 1 1 calc R . . H29B H 1.1187 0.2364 0.5913 0.073 Uiso 1 1 calc R . . H29C H 0.9892 0.2471 0.6104 0.073 Uiso 1 1 calc R . . C30 C 1.0692(3) 0.0765(2) 0.53805(19) 0.0420(9) Uani 1 1 d . . . H30A H 1.0060 0.0642 0.5659 0.063 Uiso 1 1 calc R . . H30B H 1.1341 0.0635 0.5611 0.063 Uiso 1 1 calc R . . H30C H 1.0830 0.0430 0.5014 0.063 Uiso 1 1 calc R . . C31 C 1.1492(3) 0.2034(3) 0.44648(19) 0.0456(10) Uani 1 1 d . . . H31A H 1.1399 0.1771 0.4091 0.068 Uiso 1 1 calc R . . H31B H 1.2215 0.1782 0.4603 0.068 Uiso 1 1 calc R . . H31C H 1.1437 0.2628 0.4361 0.068 Uiso 1 1 calc R . . C32 C 0.8352(2) 0.21514(18) -0.07997(13) 0.0194(6) Uani 1 1 d . . . H32A H 0.8799 0.1804 -0.0485 0.023 Uiso 1 1 calc R . . H32B H 0.8714 0.1990 -0.1222 0.023 Uiso 1 1 calc R . . C33 C 0.9883(3) 0.31652(19) -0.07900(14) 0.0231(6) Uani 1 1 d . . . C34 C 1.0450(3) 0.2700(2) -0.03107(15) 0.0278(7) Uani 1 1 d . . . H34 H 1.0064 0.2429 0.0025 0.033 Uiso 1 1 calc R . . C35 C 1.1566(3) 0.2630(2) -0.03192(17) 0.0337(8) Uani 1 1 d . . . H35 H 1.1946 0.2308 0.0008 0.040 Uiso 1 1 calc R . . C36 C 1.2129(3) 0.3027(2) -0.08030(18) 0.0352(8) Uani 1 1 d . . . H36 H 1.2898 0.2974 -0.0810 0.042 Uiso 1 1 calc R . . C37 C 1.1585(3) 0.3498(2) -0.12710(18) 0.0382(8) Uani 1 1 d . . . H37 H 1.1978 0.3775 -0.1599 0.046 Uiso 1 1 calc R . . C38 C 1.0462(3) 0.3575(2) -0.12726(16) 0.0311(7) Uani 1 1 d . . . H38 H 1.0089 0.3904 -0.1599 0.037 Uiso 1 1 calc R . . C39 C 0.7924(3) 0.3785(2) -0.14388(14) 0.0275(7) Uani 1 1 d . . . C40 C 0.6982(3) 0.4409(2) -0.13921(18) 0.0369(8) Uani 1 1 d . . . H40 H 0.6620 0.4558 -0.0988 0.044 Uiso 1 1 calc R . . C41 C 0.6562(4) 0.4819(3) -0.1936(2) 0.0572(13) Uani 1 1 d . . . H41 H 0.5913 0.5246 -0.1904 0.069 Uiso 1 1 calc R . . C42 C 0.7089(5) 0.4605(4) -0.2518(2) 0.0702(17) Uani 1 1 d . . . H42 H 0.6813 0.4896 -0.2888 0.084 Uiso 1 1 calc R . . C43 C 0.8014(5) 0.3973(3) -0.25749(18) 0.0577(14) Uani 1 1 d . . . H43 H 0.8358 0.3821 -0.2982 0.069 Uiso 1 1 calc R . . C44 C 0.8445(3) 0.3558(3) -0.20378(16) 0.0398(9) Uani 1 1 d . . . H44 H 0.9087 0.3125 -0.2075 0.048 Uiso 1 1 calc R . . C45 C 0.6308(2) 0.23827(19) -0.13488(13) 0.0204(6) Uani 1 1 d . . . C46 C 0.5303(3) 0.2947(2) -0.12302(14) 0.0241(6) Uani 1 1 d . . . H46 H 0.4993 0.3042 -0.0808 0.029 Uiso 1 1 calc R . . C47 C 0.4759(3) 0.3366(2) -0.17293(17) 0.0344(8) Uani 1 1 d . . . H47 H 0.4074 0.3746 -0.1648 0.041 Uiso 1 1 calc R . . C48 C 0.5212(3) 0.3232(3) -0.23450(17) 0.0396(9) Uani 1 1 d . . . H48 H 0.4829 0.3511 -0.2686 0.047 Uiso 1 1 calc R . . C49 C 0.6214(3) 0.2696(3) -0.24664(15) 0.0371(8) Uani 1 1 d . . . H49 H 0.6532 0.2621 -0.2890 0.044 Uiso 1 1 calc R . . C50 C 0.6763(3) 0.2264(2) -0.19734(15) 0.0299(7) Uani 1 1 d . . . H50 H 0.7449 0.1888 -0.2060 0.036 Uiso 1 1 calc R . . C51 C 0.7412(3) 0.07767(19) -0.08178(14) 0.0240(6) Uani 1 1 d . . . C52 C 0.7084(3) 0.0414(2) -0.13022(17) 0.0367(8) Uani 1 1 d . . . H52 H 0.6591 0.0738 -0.1577 0.044 Uiso 1 1 calc R . . C53 C 0.7492(4) -0.0434(3) -0.1377(2) 0.0476(11) Uani 1 1 d . . . H53 H 0.7271 -0.0686 -0.1704 0.057 Uiso 1 1 calc R . . C54 C 0.8202(4) -0.0899(2) -0.0986(2) 0.0495(11) Uani 1 1 d . . . H54 H 0.8500 -0.1467 -0.1055 0.059 Uiso 1 1 calc R . . C55 C 0.8495(3) -0.0554(2) -0.0487(2) 0.0440(9) Uani 1 1 d . . . H55 H 0.8963 -0.0889 -0.0204 0.053 Uiso 1 1 calc R . . C56 C 0.8100(3) 0.0284(2) -0.04036(17) 0.0332(7) Uani 1 1 d . . . H56 H 0.8300 0.0522 -0.0062 0.040 Uiso 1 1 calc R . . C57 C 0.6427(4) 0.5046(3) 0.0470(2) 0.0477(10) Uani 1 1 d . . . H57A H 0.6044 0.5218 0.0093 0.072 Uiso 1 1 calc R . . H57B H 0.6468 0.5537 0.0677 0.072 Uiso 1 1 calc R . . H57C H 0.6025 0.4700 0.0763 0.072 Uiso 1 1 calc R . . C58 C 0.8632(3) 0.4149(3) 0.09298(17) 0.0406(9) Uani 1 1 d . . . H58A H 0.8289 0.3773 0.1228 0.061 Uiso 1 1 calc R . . H58B H 0.8637 0.4649 0.1138 0.061 Uiso 1 1 calc R . . H58C H 0.9388 0.3871 0.0789 0.061 Uiso 1 1 calc R . . C59 C 0.8545(4) 0.5128(2) -0.03351(18) 0.0419(9) Uani 1 1 d . . . H59A H 0.9298 0.4831 -0.0464 0.063 Uiso 1 1 calc R . . H59B H 0.8562 0.5630 -0.0134 0.063 Uiso 1 1 calc R . . H59C H 0.8144 0.5280 -0.0707 0.063 Uiso 1 1 calc R . . C60 C 0.4671(3) 0.1171(2) -0.02180(16) 0.0322(7) Uani 1 1 d . . . H60A H 0.4506 0.1525 -0.0602 0.048 Uiso 1 1 calc R . . H60B H 0.3999 0.1017 -0.0010 0.048 Uiso 1 1 calc R . . H60C H 0.5221 0.0669 -0.0329 0.048 Uiso 1 1 calc R . . C61 C 0.4113(3) 0.2661(2) 0.05589(16) 0.0352(8) Uani 1 1 d . . . H61A H 0.4405 0.3021 0.0798 0.053 Uiso 1 1 calc R . . H61B H 0.3508 0.2470 0.0821 0.053 Uiso 1 1 calc R . . H61C H 0.3843 0.2972 0.0177 0.053 Uiso 1 1 calc R . . C62 C 0.5602(3) 0.1049(3) 0.10367(17) 0.0417(9) Uani 1 1 d . . . H62A H 0.6117 0.0542 0.0901 0.063 Uiso 1 1 calc R . . H62B H 0.4940 0.0907 0.1270 0.063 Uiso 1 1 calc R . . H62C H 0.5949 0.1329 0.1310 0.063 Uiso 1 1 calc R . . C63 C 1.1291(5) 0.3367(4) 0.1867(2) 0.0748(16) Uani 1 1 d . . . H63A H 1.1386 0.3249 0.1420 0.112 Uiso 1 1 calc R . . H63B H 1.1351 0.3938 0.1902 0.112 Uiso 1 1 calc R . . H63C H 1.0565 0.3296 0.2059 0.112 Uiso 1 1 calc R . . C64 C 1.2150(4) 0.2788(3) 0.21973(17) 0.0437(10) Uani 1 1 d . . . C65 C 1.3211(4) 0.2942(3) 0.21670(18) 0.0518(11) Uani 1 1 d . . . H65 H 1.3369 0.3436 0.1954 0.062 Uiso 1 1 calc R . . C66 C 1.4010(4) 0.2379(3) 0.24436(19) 0.0537(12) Uani 1 1 d . . . H66 H 1.4728 0.2483 0.2409 0.064 Uiso 1 1 calc R . . C67 C 1.3814(4) 0.1659(3) 0.27741(19) 0.0495(11) Uani 1 1 d . . . H67 H 1.4384 0.1277 0.2965 0.059 Uiso 1 1 calc R . . C68 C 1.2782(3) 0.1513(3) 0.28180(18) 0.0427(9) Uani 1 1 d . . . H68 H 1.2623 0.1028 0.3046 0.051 Uiso 1 1 calc R . . C69 C 1.1964(3) 0.2078(3) 0.25268(19) 0.0413(9) Uani 1 1 d . . . H69 H 1.1252 0.1965 0.2558 0.050 Uiso 1 1 calc R . . C70 C 1.3253(5) 0.1540(4) -0.1989(3) 0.0818(19) Uani 1 1 d . . . H70A H 1.3467 0.1472 -0.1559 0.123 Uiso 1 1 calc R . . H70B H 1.3223 0.2114 -0.2157 0.123 Uiso 1 1 calc R . . H70C H 1.3795 0.1163 -0.2258 0.123 Uiso 1 1 calc R . . C71 C 1.2137(4) 0.1343(3) -0.19757(19) 0.0460(10) Uani 1 1 d . . . C72 C 1.1751(4) 0.0858(3) -0.1489(2) 0.0565(12) Uani 1 1 d . . . H72 H 1.2168 0.0675 -0.1143 0.068 Uiso 1 1 calc R . . C73 C 1.0768(5) 0.0631(3) -0.1490(2) 0.0623(14) Uani 1 1 d . . . H73 H 1.0518 0.0289 -0.1148 0.075 Uiso 1 1 calc R . . C74 C 1.0152(4) 0.0894(3) -0.1978(3) 0.0644(14) Uani 1 1 d . . . H74 H 0.9478 0.0729 -0.1980 0.077 Uiso 1 1 calc R . . C75 C 1.0506(5) 0.1398(3) -0.2469(2) 0.0642(14) Uani 1 1 d . . . H75 H 1.0076 0.1591 -0.2809 0.077 Uiso 1 1 calc R . . C76 C 1.1495(5) 0.1618(3) -0.2463(2) 0.0582(12) Uani 1 1 d . . . H76 H 1.1741 0.1968 -0.2801 0.070 Uiso 1 1 calc R . . C77 C 0.7598(10) 0.6174(7) 0.3313(5) 0.088(3) Uiso 0.60 1 d P A 1 H77A H 0.8390 0.6015 0.3183 0.132 Uiso 0.60 1 calc PR A 1 H77B H 0.7472 0.6258 0.3766 0.132 Uiso 0.60 1 calc PR A 1 H77C H 0.7285 0.6690 0.3076 0.132 Uiso 0.60 1 calc PR A 1 C78 C 0.7076(7) 0.5520(5) 0.3184(4) 0.0407(17) Uiso 0.60 1 d P A 1 C79 C 0.7535(7) 0.5017(5) 0.2689(4) 0.038(2) Uiso 0.60 1 d P A 1 H79 H 0.8221 0.5051 0.2456 0.046 Uiso 0.60 1 calc PR A 1 C80 C 0.6927(7) 0.4455(4) 0.2554(3) 0.0329(16) Uiso 0.60 1 d P A 1 H80 H 0.7213 0.4105 0.2217 0.039 Uiso 0.60 1 calc PR A 1 C81 C 0.5902(6) 0.4385(5) 0.2899(4) 0.0407(15) Uiso 0.60 1 d P A 1 H81 H 0.5498 0.4011 0.2790 0.049 Uiso 0.60 1 calc PR A 1 C82 C 0.5521(6) 0.4879(5) 0.3393(3) 0.0362(14) Uiso 0.60 1 d P A 1 H82 H 0.4850 0.4836 0.3641 0.043 Uiso 0.60 1 calc PR A 1 C83 C 0.6099(7) 0.5442(5) 0.3539(3) 0.0348(14) Uiso 0.60 1 d P A 1 H83 H 0.5822 0.5776 0.3886 0.042 Uiso 0.60 1 calc PR A 1 C77B C 0.8184(10) 0.6108(8) 0.3005(6) 0.053(3) Uiso 0.40 1 d P B 2 H77D H 0.7889 0.6611 0.2748 0.079 Uiso 0.40 1 calc PR B 2 H77E H 0.8927 0.5857 0.2820 0.079 Uiso 0.40 1 calc PR B 2 H77F H 0.8210 0.6250 0.3436 0.079 Uiso 0.40 1 calc PR B 2 C78B C 0.7455(10) 0.5501(7) 0.3020(5) 0.038(2) Uiso 0.40 1 d P B 2 C79B C 0.7382(10) 0.4872(7) 0.2621(5) 0.032(3) Uiso 0.40 1 d P B 2 H79B H 0.7957 0.4744 0.2288 0.038 Uiso 0.40 1 calc PR B 2 C80B C 0.6579(12) 0.4445(8) 0.2670(6) 0.045(3) Uiso 0.40 1 d P B 2 H80B H 0.6575 0.4048 0.2380 0.054 Uiso 0.40 1 calc PR B 2 C81B C 0.5799(10) 0.4610(8) 0.3145(6) 0.047(3) Uiso 0.40 1 d P B 2 H81B H 0.5220 0.4322 0.3190 0.057 Uiso 0.40 1 calc PR B 2 C82B C 0.5780(10) 0.5162(8) 0.3565(5) 0.038(2) Uiso 0.40 1 d P B 2 H82B H 0.5213 0.5239 0.3907 0.046 Uiso 0.40 1 calc PR B 2 C83B C 0.6579(11) 0.5618(7) 0.3505(5) 0.042(2) Uiso 0.40 1 d P B 2 H83B H 0.6536 0.6022 0.3799 0.051 Uiso 0.40 1 calc PR B 2 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 0.02294(19) 0.02435(19) 0.01755(16) -0.00024(13) -0.00493(13) -0.00397(15) Zn2 0.02387(19) 0.02293(18) 0.01597(15) -0.00086(13) -0.00235(13) -0.00847(15) Cl1 0.0398(5) 0.0472(5) 0.0257(4) 0.0113(4) -0.0099(3) -0.0046(4) Cl2 0.0399(5) 0.0284(4) 0.0258(4) -0.0078(3) -0.0027(3) -0.0033(4) Cl3 0.0422(5) 0.0431(5) 0.0231(4) -0.0104(3) 0.0076(3) -0.0192(4) Cl4 0.0324(4) 0.0323(4) 0.0279(4) 0.0056(3) -0.0124(3) -0.0054(3) P1 0.0181(4) 0.0180(4) 0.0176(3) -0.0008(3) -0.0037(3) -0.0027(3) P2 0.0169(4) 0.0167(4) 0.0184(3) -0.0007(3) -0.0034(3) -0.0030(3) P3 0.0190(4) 0.0190(4) 0.0178(3) 0.0005(3) -0.0016(3) -0.0049(3) P4 0.0177(4) 0.0177(4) 0.0167(3) -0.0024(3) -0.0032(3) -0.0022(3) Si1 0.0320(5) 0.0316(5) 0.0235(4) 0.0027(4) -0.0031(3) -0.0140(4) Si2 0.0219(4) 0.0260(5) 0.0286(4) 0.0022(3) -0.0107(3) -0.0045(4) Si3 0.0337(5) 0.0197(4) 0.0283(4) -0.0057(3) 0.0021(4) -0.0098(4) Si4 0.0231(4) 0.0279(5) 0.0208(4) 0.0001(3) -0.0024(3) -0.0093(4) N1 0.0224(13) 0.0215(13) 0.0205(11) 0.0014(10) -0.0061(10) -0.0051(10) N2 0.0196(12) 0.0204(12) 0.0189(11) 0.0002(9) -0.0054(9) -0.0016(10) N3 0.0209(13) 0.0185(12) 0.0222(12) -0.0017(9) 0.0005(9) -0.0054(10) N4 0.0212(13) 0.0178(12) 0.0173(11) -0.0029(9) -0.0013(9) -0.0050(10) C1 0.0190(14) 0.0161(13) 0.0206(13) -0.0015(10) -0.0047(11) -0.0011(11) C2 0.0185(14) 0.0228(15) 0.0213(13) 0.0030(11) -0.0022(11) -0.0027(12) C3 0.0242(16) 0.0323(18) 0.0253(15) -0.0042(13) -0.0023(12) 0.0004(14) C4 0.0290(19) 0.038(2) 0.0372(18) -0.0080(16) -0.0020(15) 0.0090(16) C5 0.0205(17) 0.043(2) 0.042(2) 0.0055(16) -0.0041(14) 0.0076(15) C6 0.0209(16) 0.042(2) 0.0348(17) 0.0029(15) -0.0074(13) -0.0043(15) C7 0.0204(15) 0.0296(17) 0.0317(16) -0.0018(13) -0.0039(12) -0.0053(13) C8 0.0208(15) 0.0205(15) 0.0225(14) -0.0032(11) -0.0044(11) -0.0053(12) C9 0.0308(18) 0.0228(16) 0.0306(16) -0.0047(13) -0.0057(13) -0.0048(14) C10 0.045(2) 0.0255(18) 0.0406(19) -0.0111(15) -0.0030(16) -0.0069(16) C11 0.036(2) 0.043(2) 0.0385(19) -0.0190(16) -0.0026(15) -0.0103(17) C12 0.038(2) 0.047(2) 0.0221(15) -0.0076(14) -0.0026(13) -0.0150(17) C13 0.0243(16) 0.0289(17) 0.0254(15) -0.0033(12) -0.0052(12) -0.0059(13) C14 0.0202(14) 0.0224(15) 0.0196(13) -0.0027(11) 0.0000(11) -0.0071(12) C15 0.0227(16) 0.0280(17) 0.0236(14) 0.0004(12) -0.0023(12) -0.0041(13) C16 0.0292(18) 0.045(2) 0.0198(14) -0.0049(14) -0.0021(12) -0.0095(16) C17 0.0355(19) 0.043(2) 0.0289(16) -0.0167(15) 0.0055(14) -0.0116(17) C18 0.039(2) 0.0262(18) 0.0350(18) -0.0109(14) 0.0044(15) -0.0071(15) C19 0.0266(16) 0.0248(16) 0.0246(14) -0.0029(12) -0.0003(12) -0.0059(13) C20 0.0210(15) 0.0190(15) 0.0256(14) -0.0003(11) -0.0051(11) -0.0035(12) C21 0.0245(16) 0.0254(17) 0.0335(16) -0.0018(13) -0.0001(13) -0.0067(13) C22 0.0311(19) 0.0348(19) 0.0401(19) 0.0033(15) 0.0002(15) -0.0157(16) C23 0.040(2) 0.0233(17) 0.054(2) 0.0023(16) -0.0093(17) -0.0142(16) C24 0.040(2) 0.0216(17) 0.0423(19) -0.0057(14) -0.0059(15) -0.0104(15) C25 0.0299(17) 0.0223(16) 0.0319(16) -0.0043(13) -0.0038(13) -0.0052(14) C26 0.039(2) 0.054(3) 0.043(2) 0.0066(18) -0.0080(16) -0.030(2) C27 0.064(3) 0.037(2) 0.050(2) 0.0169(18) -0.017(2) -0.019(2) C28 0.062(3) 0.078(3) 0.038(2) -0.015(2) 0.016(2) -0.035(3) C29 0.057(3) 0.050(3) 0.049(2) -0.0097(19) -0.024(2) -0.016(2) C30 0.038(2) 0.0298(19) 0.053(2) 0.0104(17) -0.0109(17) 0.0013(16) C31 0.0213(18) 0.062(3) 0.051(2) 0.008(2) -0.0062(16) -0.0075(18) C32 0.0180(14) 0.0186(14) 0.0198(13) -0.0007(11) 0.0000(11) -0.0014(11) C33 0.0214(15) 0.0196(15) 0.0283(15) -0.0028(12) 0.0001(12) -0.0055(12) C34 0.0259(17) 0.0279(17) 0.0309(16) 0.0040(13) -0.0033(13) -0.0107(14) C35 0.0265(17) 0.0348(19) 0.0411(19) 0.0030(15) -0.0099(14) -0.0080(15) C36 0.0227(17) 0.035(2) 0.050(2) -0.0029(16) -0.0033(15) -0.0106(15) C37 0.0299(19) 0.042(2) 0.044(2) 0.0035(17) 0.0048(15) -0.0166(17) C38 0.0262(17) 0.0354(19) 0.0316(16) 0.0062(14) -0.0021(13) -0.0103(15) C39 0.0325(18) 0.0287(17) 0.0244(15) 0.0075(12) -0.0087(13) -0.0135(14) C40 0.037(2) 0.0312(19) 0.046(2) 0.0135(15) -0.0168(16) -0.0135(16) C41 0.051(3) 0.047(3) 0.080(3) 0.034(2) -0.041(2) -0.022(2) C42 0.080(4) 0.093(4) 0.058(3) 0.051(3) -0.046(3) -0.060(3) C43 0.082(4) 0.083(4) 0.0271(19) 0.018(2) -0.020(2) -0.058(3) C44 0.046(2) 0.052(2) 0.0285(17) 0.0035(16) -0.0064(15) -0.0267(19) C45 0.0244(15) 0.0210(15) 0.0180(13) -0.0026(11) -0.0047(11) -0.0078(12) C46 0.0212(15) 0.0262(16) 0.0232(14) 0.0029(12) -0.0038(11) -0.0030(13) C47 0.0265(18) 0.0347(19) 0.0407(19) 0.0099(15) -0.0112(14) -0.0052(15) C48 0.042(2) 0.048(2) 0.0325(18) 0.0150(16) -0.0177(15) -0.0176(18) C49 0.043(2) 0.053(2) 0.0181(15) -0.0020(15) -0.0031(14) -0.0177(19) C50 0.0275(17) 0.040(2) 0.0230(15) -0.0079(13) -0.0017(12) -0.0069(15) C51 0.0238(16) 0.0173(14) 0.0297(15) -0.0059(12) 0.0040(12) -0.0043(12) C52 0.040(2) 0.0308(19) 0.042(2) -0.0125(15) -0.0026(16) -0.0096(16) C53 0.066(3) 0.031(2) 0.048(2) -0.0169(18) 0.009(2) -0.018(2) C54 0.063(3) 0.0157(17) 0.062(3) -0.0085(17) 0.022(2) -0.0078(18) C55 0.040(2) 0.0220(18) 0.064(3) 0.0038(17) 0.0015(19) -0.0010(16) C56 0.0355(19) 0.0214(16) 0.0422(19) 0.0013(14) -0.0055(15) -0.0060(14) C57 0.048(2) 0.032(2) 0.057(2) -0.0128(18) 0.0098(19) -0.0019(18) C58 0.053(2) 0.045(2) 0.0332(18) -0.0082(16) -0.0053(16) -0.027(2) C59 0.062(3) 0.0270(19) 0.043(2) -0.0020(15) 0.0009(18) -0.0249(19) C60 0.0303(18) 0.0342(19) 0.0367(18) -0.0025(14) -0.0030(14) -0.0169(15) C61 0.0263(18) 0.050(2) 0.0292(17) -0.0127(15) 0.0011(13) -0.0056(16) C62 0.046(2) 0.048(2) 0.0326(18) 0.0140(16) -0.0051(16) -0.0189(19) C63 0.068(4) 0.079(4) 0.062(3) 0.015(3) 0.005(3) 0.001(3) C64 0.051(2) 0.052(3) 0.0250(17) -0.0034(16) 0.0070(16) -0.011(2) C65 0.067(3) 0.064(3) 0.0308(19) -0.0028(19) 0.0073(19) -0.036(3) C66 0.050(3) 0.087(4) 0.035(2) 0.000(2) -0.0041(18) -0.038(3) C67 0.041(2) 0.068(3) 0.037(2) -0.005(2) -0.0035(17) -0.008(2) C68 0.041(2) 0.047(2) 0.038(2) -0.0092(17) 0.0021(16) -0.0079(19) C69 0.0268(19) 0.047(2) 0.049(2) -0.0039(18) 0.0031(16) -0.0115(17) C70 0.067(4) 0.102(5) 0.083(4) -0.044(4) 0.004(3) -0.024(3) C71 0.053(3) 0.041(2) 0.044(2) -0.0177(18) -0.0009(18) -0.007(2) C72 0.063(3) 0.053(3) 0.043(2) -0.007(2) -0.001(2) 0.008(2) C73 0.076(4) 0.043(3) 0.055(3) -0.006(2) 0.022(3) -0.002(2) C74 0.055(3) 0.049(3) 0.088(4) -0.037(3) 0.013(3) -0.006(2) C75 0.076(4) 0.053(3) 0.063(3) -0.017(2) -0.028(3) 0.004(3) C76 0.082(4) 0.048(3) 0.045(2) -0.003(2) -0.006(2) -0.017(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N1 2.055(3) . ? Zn1 N2 2.061(3) . ? Zn1 Cl1 2.2370(11) . ? Zn1 Cl2 2.3019(11) . ? Zn2 N4 2.046(2) . ? Zn2 N3 2.064(3) . ? Zn2 Cl3 2.2375(11) . ? Zn2 Cl4 2.2909(12) . ? P1 N1 1.590(3) . ? P1 C8 1.807(3) . ? P1 C2 1.812(3) . ? P1 C1 1.822(3) . ? P2 N2 1.588(3) . ? P2 C14 1.806(3) . ? P2 C20 1.813(3) . ? P2 C1 1.816(3) . ? P3 N3 1.587(2) . ? P3 C39 1.805(3) . ? P3 C32 1.809(3) . ? P3 C33 1.813(3) . ? P4 N4 1.583(2) . ? P4 C45 1.789(3) . ? P4 C51 1.809(3) . ? P4 C32 1.827(3) . ? Si1 N1 1.748(3) . ? Si1 C28 1.854(4) . ? Si1 C27 1.863(4) . ? Si1 C26 1.868(4) . ? Si2 N2 1.753(3) . ? Si2 C30 1.855(4) . ? Si2 C31 1.861(4) . ? Si2 C29 1.863(4) . ? Si3 N3 1.751(3) . ? Si3 C58 1.855(4) . ? Si3 C57 1.860(4) . ? Si3 C59 1.873(4) . ? Si4 N4 1.755(3) . ? Si4 C62 1.859(4) . ? Si4 C61 1.862(4) . ? Si4 C60 1.877(3) . ? C2 C7 1.393(4) . ? C2 C3 1.397(4) . ? C3 C4 1.385(5) . ? C4 C5 1.389(5) . ? C5 C6 1.381(5) . ? C6 C7 1.391(5) . ? C8 C9 1.390(4) . ? C8 C13 1.406(4) . ? C9 C10 1.389(4) . ? C10 C11 1.378(5) . ? C11 C12 1.377(6) . ? C12 C13 1.390(4) . ? C14 C19 1.385(4) . ? C14 C15 1.401(4) . ? C15 C16 1.385(4) . ? C16 C17 1.376(5) . ? C17 C18 1.387(5) . ? C18 C19 1.387(4) . ? C20 C25 1.397(4) . ? C20 C21 1.398(4) . ? C21 C22 1.388(5) . ? C22 C23 1.383(5) . ? C23 C24 1.380(5) . ? C24 C25 1.391(5) . ? C33 C34 1.394(5) . ? C33 C38 1.400(4) . ? C34 C35 1.380(5) . ? C35 C36 1.380(5) . ? C36 C37 1.366(5) . ? C37 C38 1.390(5) . ? C39 C40 1.383(5) . ? C39 C44 1.406(5) . ? C40 C41 1.394(5) . ? C41 C42 1.372(7) . ? C42 C43 1.377(8) . ? C43 C44 1.390(6) . ? C45 C50 1.398(4) . ? C45 C46 1.400(4) . ? C46 C47 1.387(5) . ? C47 C48 1.384(5) . ? C48 C49 1.376(6) . ? C49 C50 1.386(5) . ? C51 C56 1.393(5) . ? C51 C52 1.398(5) . ? C52 C53 1.401(5) . ? C53 C54 1.361(7) . ? C54 C55 1.385(6) . ? C55 C56 1.386(5) . ? C63 C64 1.478(7) . ? C64 C69 1.368(6) . ? C64 C65 1.409(6) . ? C65 C66 1.361(7) . ? C66 C67 1.386(7) . ? C67 C68 1.365(6) . ? C68 C69 1.393(6) . ? C70 C71 1.511(7) . ? C71 C72 1.363(6) . ? C71 C76 1.381(7) . ? C72 C73 1.373(7) . ? C73 C74 1.361(8) . ? C74 C75 1.373(8) . ? C75 C76 1.377(7) . ? C77 C78 1.457(13) . ? C78 C83 1.384(11) . ? C78 C79 1.394(11) . ? C79 C80 1.407(11) . ? C80 C81 1.424(10) . ? C81 C82 1.370(9) . ? C82 C83 1.388(10) . ? C77B C78B 1.507(16) . ? C78B C83B 1.405(15) . ? C78B C79B 1.438(15) . ? C79B C80B 1.351(17) . ? C80B C81B 1.320(19) . ? C81B C82B 1.339(17) . ? C82B C83B 1.379(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zn1 N2 104.86(10) . . ? N1 Zn1 Cl1 114.47(8) . . ? N2 Zn1 Cl1 114.10(8) . . ? N1 Zn1 Cl2 106.38(8) . . ? N2 Zn1 Cl2 107.45(8) . . ? Cl1 Zn1 Cl2 109.09(4) . . ? N4 Zn2 N3 103.97(10) . . ? N4 Zn2 Cl3 115.73(7) . . ? N3 Zn2 Cl3 113.74(7) . . ? N4 Zn2 Cl4 106.04(8) . . ? N3 Zn2 Cl4 108.50(8) . . ? Cl3 Zn2 Cl4 108.40(4) . . ? N1 P1 C8 114.34(14) . . ? N1 P1 C2 114.49(14) . . ? C8 P1 C2 107.36(14) . . ? N1 P1 C1 110.67(13) . . ? C8 P1 C1 107.86(13) . . ? C2 P1 C1 101.14(14) . . ? N2 P2 C14 116.01(14) . . ? N2 P2 C20 114.36(14) . . ? C14 P2 C20 106.87(14) . . ? N2 P2 C1 110.07(14) . . ? C14 P2 C1 105.08(14) . . ? C20 P2 C1 103.32(14) . . ? N3 P3 C39 115.58(15) . . ? N3 P3 C32 109.69(13) . . ? C39 P3 C32 106.06(15) . . ? N3 P3 C33 113.81(14) . . ? C39 P3 C33 107.53(15) . . ? C32 P3 C33 103.20(14) . . ? N4 P4 C45 114.55(14) . . ? N4 P4 C51 114.96(14) . . ? C45 P4 C51 107.99(14) . . ? N4 P4 C32 110.63(13) . . ? C45 P4 C32 106.44(14) . . ? C51 P4 C32 101.13(14) . . ? N1 Si1 C28 109.55(17) . . ? N1 Si1 C27 109.41(17) . . ? C28 Si1 C27 109.7(2) . . ? N1 Si1 C26 112.69(15) . . ? C28 Si1 C26 107.6(2) . . ? C27 Si1 C26 107.9(2) . . ? N2 Si2 C30 109.67(16) . . ? N2 Si2 C31 112.59(15) . . ? C30 Si2 C31 107.4(2) . . ? N2 Si2 C29 108.34(17) . . ? C30 Si2 C29 111.1(2) . . ? C31 Si2 C29 107.8(2) . . ? N3 Si3 C58 108.16(16) . . ? N3 Si3 C57 109.39(17) . . ? C58 Si3 C57 111.3(2) . . ? N3 Si3 C59 112.39(14) . . ? C58 Si3 C59 108.41(18) . . ? C57 Si3 C59 107.2(2) . . ? N4 Si4 C62 108.68(16) . . ? N4 Si4 C61 109.14(15) . . ? C62 Si4 C61 110.93(18) . . ? N4 Si4 C60 112.03(13) . . ? C62 Si4 C60 108.82(18) . . ? C61 Si4 C60 107.25(16) . . ? P1 N1 Si1 125.22(16) . . ? P1 N1 Zn1 115.30(14) . . ? Si1 N1 Zn1 118.08(13) . . ? P2 N2 Si2 125.28(16) . . ? P2 N2 Zn1 115.76(14) . . ? Si2 N2 Zn1 116.25(12) . . ? P3 N3 Si3 124.71(15) . . ? P3 N3 Zn2 116.06(14) . . ? Si3 N3 Zn2 116.50(12) . . ? P4 N4 Si4 125.63(15) . . ? P4 N4 Zn2 115.57(13) . . ? Si4 N4 Zn2 117.74(12) . . ? P2 C1 P1 119.61(16) . . ? C7 C2 C3 119.6(3) . . ? C7 C2 P1 123.0(2) . . ? C3 C2 P1 117.4(2) . . ? C4 C3 C2 119.7(3) . . ? C3 C4 C5 120.6(3) . . ? C6 C5 C4 119.7(3) . . ? C5 C6 C7 120.3(3) . . ? C6 C7 C2 120.0(3) . . ? C9 C8 C13 119.2(3) . . ? C9 C8 P1 119.8(2) . . ? C13 C8 P1 121.0(2) . . ? C10 C9 C8 120.0(3) . . ? C11 C10 C9 120.5(3) . . ? C12 C11 C10 120.3(3) . . ? C11 C12 C13 120.1(3) . . ? C12 C13 C8 120.0(3) . . ? C19 C14 C15 119.4(3) . . ? C19 C14 P2 120.5(2) . . ? C15 C14 P2 119.7(2) . . ? C16 C15 C14 120.2(3) . . ? C17 C16 C15 119.9(3) . . ? C16 C17 C18 120.4(3) . . ? C19 C18 C17 120.0(3) . . ? C14 C19 C18 120.1(3) . . ? C25 C20 C21 119.2(3) . . ? C25 C20 P2 118.3(2) . . ? C21 C20 P2 122.4(2) . . ? C22 C21 C20 120.3(3) . . ? C23 C22 C21 120.0(3) . . ? C24 C23 C22 120.2(3) . . ? C23 C24 C25 120.4(3) . . ? C24 C25 C20 119.8(3) . . ? P3 C32 P4 119.37(16) . . ? C34 C33 C38 118.8(3) . . ? C34 C33 P3 117.1(2) . . ? C38 C33 P3 124.1(3) . . ? C35 C34 C33 120.6(3) . . ? C34 C35 C36 120.0(3) . . ? C37 C36 C35 120.3(3) . . ? C36 C37 C38 120.6(3) . . ? C37 C38 C33 119.6(3) . . ? C40 C39 C44 119.7(3) . . ? C40 C39 P3 119.9(3) . . ? C44 C39 P3 120.2(3) . . ? C39 C40 C41 120.1(4) . . ? C42 C41 C40 119.8(5) . . ? C41 C42 C43 120.9(4) . . ? C42 C43 C44 120.1(4) . . ? C43 C44 C39 119.4(4) . . ? C50 C45 C46 119.2(3) . . ? C50 C45 P4 121.5(2) . . ? C46 C45 P4 119.2(2) . . ? C47 C46 C45 120.0(3) . . ? C48 C47 C46 120.1(3) . . ? C49 C48 C47 120.3(3) . . ? C48 C49 C50 120.3(3) . . ? C49 C50 C45 120.0(3) . . ? C56 C51 C52 119.5(3) . . ? C56 C51 P4 116.8(2) . . ? C52 C51 P4 123.7(3) . . ? C51 C52 C53 119.2(4) . . ? C54 C53 C52 120.5(4) . . ? C53 C54 C55 120.7(4) . . ? C54 C55 C56 119.6(4) . . ? C55 C56 C51 120.3(4) . . ? C69 C64 C65 117.4(4) . . ? C69 C64 C63 122.0(4) . . ? C65 C64 C63 120.6(4) . . ? C66 C65 C64 119.8(4) . . ? C65 C66 C67 122.3(4) . . ? C68 C67 C66 118.3(4) . . ? C67 C68 C69 119.8(4) . . ? C64 C69 C68 122.3(4) . . ? C72 C71 C76 117.9(5) . . ? C72 C71 C70 120.5(5) . . ? C76 C71 C70 121.5(5) . . ? C71 C72 C73 121.2(5) . . ? C74 C73 C72 120.3(5) . . ? C73 C74 C75 119.9(5) . . ? C74 C75 C76 119.1(5) . . ? C75 C76 C71 121.5(5) . . ? C83 C78 C79 121.6(7) . . ? C83 C78 C77 118.8(9) . . ? C79 C78 C77 119.6(9) . . ? C78 C79 C80 116.3(7) . . ? C79 C80 C81 123.0(7) . . ? C82 C81 C80 117.4(7) . . ? C81 C82 C83 121.1(6) . . ? C78 C83 C82 120.6(6) . . ? C83B C78B C79B 111.4(10) . . ? C83B C78B C77B 113.3(10) . . ? C79B C78B C77B 135.0(11) . . ? C80B C79B C78B 126.7(11) . . ? C81B C80B C79B 116.3(12) . . ? C80B C81B C82B 123.5(13) . . ? C81B C82B C83B 120.4(10) . . ? C82B C83B C78B 121.6(10) . . ? 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 C8 P1 N1 Si1 -74.4(2) . . . . ? C2 P1 N1 Si1 50.1(2) . . . . ? C1 P1 N1 Si1 163.57(17) . . . . ? C8 P1 N1 Zn1 119.45(15) . . . . ? C2 P1 N1 Zn1 -116.08(16) . . . . ? C1 P1 N1 Zn1 -2.58(19) . . . . ? C28 Si1 N1 P1 -113.9(2) . . . . ? C27 Si1 N1 P1 125.8(2) . . . . ? C26 Si1 N1 P1 5.8(3) . . . . ? C28 Si1 N1 Zn1 51.9(2) . . . . ? C27 Si1 N1 Zn1 -68.4(2) . . . . ? C26 Si1 N1 Zn1 171.62(18) . . . . ? N2 Zn1 N1 P1 -43.61(17) . . . . ? Cl1 Zn1 N1 P1 -169.41(11) . . . . ? Cl2 Zn1 N1 P1 70.05(15) . . . . ? N2 Zn1 N1 Si1 149.19(14) . . . . ? Cl1 Zn1 N1 Si1 23.39(17) . . . . ? Cl2 Zn1 N1 Si1 -97.15(14) . . . . ? C14 P2 N2 Si2 74.6(2) . . . . ? C20 P2 N2 Si2 -50.6(2) . . . . ? C1 P2 N2 Si2 -166.33(16) . . . . ? C14 P2 N2 Zn1 -124.83(15) . . . . ? C20 P2 N2 Zn1 110.04(16) . . . . ? C1 P2 N2 Zn1 -5.73(18) . . . . ? C30 Si2 N2 P2 -130.9(2) . . . . ? C31 Si2 N2 P2 -11.4(3) . . . . ? C29 Si2 N2 P2 107.7(2) . . . . ? C30 Si2 N2 Zn1 68.6(2) . . . . ? C31 Si2 N2 Zn1 -171.88(18) . . . . ? C29 Si2 N2 Zn1 -52.8(2) . . . . ? N1 Zn1 N2 P2 49.07(17) . . . . ? Cl1 Zn1 N2 P2 175.10(11) . . . . ? Cl2 Zn1 N2 P2 -63.84(15) . . . . ? N1 Zn1 N2 Si2 -148.52(14) . . . . ? Cl1 Zn1 N2 Si2 -22.50(16) . . . . ? Cl2 Zn1 N2 Si2 98.57(13) . . . . ? C39 P3 N3 Si3 -73.3(2) . . . . ? C32 P3 N3 Si3 166.89(17) . . . . ? C33 P3 N3 Si3 51.9(2) . . . . ? C39 P3 N3 Zn2 126.15(16) . . . . ? C32 P3 N3 Zn2 6.35(19) . . . . ? C33 P3 N3 Zn2 -108.68(16) . . . . ? C58 Si3 N3 P3 -107.6(2) . . . . ? C57 Si3 N3 P3 131.0(2) . . . . ? C59 Si3 N3 P3 12.0(3) . . . . ? C58 Si3 N3 Zn2 52.9(2) . . . . ? C57 Si3 N3 Zn2 -68.6(2) . . . . ? C59 Si3 N3 Zn2 172.50(18) . . . . ? N4 Zn2 N3 P3 -50.16(17) . . . . ? Cl3 Zn2 N3 P3 -176.90(11) . . . . ? Cl4 Zn2 N3 P3 62.39(16) . . . . ? N4 Zn2 N3 Si3 147.66(14) . . . . ? Cl3 Zn2 N3 Si3 20.92(17) . . . . ? Cl4 Zn2 N3 Si3 -99.80(14) . . . . ? C45 P4 N4 Si4 73.6(2) . . . . ? C51 P4 N4 Si4 -52.4(2) . . . . ? C32 P4 N4 Si4 -166.16(17) . . . . ? C45 P4 N4 Zn2 -118.56(15) . . . . ? C51 P4 N4 Zn2 115.48(16) . . . . ? C32 P4 N4 Zn2 1.73(19) . . . . ? C62 Si4 N4 P4 113.2(2) . . . . ? C61 Si4 N4 P4 -125.7(2) . . . . ? C60 Si4 N4 P4 -7.1(2) . . . . ? C62 Si4 N4 Zn2 -54.4(2) . . . . ? C61 Si4 N4 Zn2 66.68(18) . . . . ? C60 Si4 N4 Zn2 -174.70(16) . . . . ? N3 Zn2 N4 P4 44.62(17) . . . . ? Cl3 Zn2 N4 P4 170.10(11) . . . . ? Cl4 Zn2 N4 P4 -69.69(15) . . . . ? N3 Zn2 N4 Si4 -146.49(14) . . . . ? Cl3 Zn2 N4 Si4 -21.01(17) . . . . ? Cl4 Zn2 N4 Si4 99.20(14) . . . . ? N2 P2 C1 P1 -53.2(2) . . . . ? C14 P2 C1 P1 72.43(19) . . . . ? C20 P2 C1 P1 -175.69(16) . . . . ? N1 P1 C1 P2 58.6(2) . . . . ? C8 P1 C1 P2 -67.2(2) . . . . ? C2 P1 C1 P2 -179.71(16) . . . . ? N1 P1 C2 C7 -123.8(3) . . . . ? C8 P1 C2 C7 4.3(3) . . . . ? C1 P1 C2 C7 117.2(3) . . . . ? N1 P1 C2 C3 57.7(3) . . . . ? C8 P1 C2 C3 -174.2(2) . . . . ? C1 P1 C2 C3 -61.3(3) . . . . ? C7 C2 C3 C4 -1.1(5) . . . . ? P1 C2 C3 C4 177.4(3) . . . . ? C2 C3 C4 C5 0.0(6) . . . . ? C3 C4 C5 C6 1.7(6) . . . . ? C4 C5 C6 C7 -2.1(6) . . . . ? C5 C6 C7 C2 1.0(5) . . . . ? C3 C2 C7 C6 0.7(5) . . . . ? P1 C2 C7 C6 -177.8(3) . . . . ? N1 P1 C8 C9 5.0(3) . . . . ? C2 P1 C8 C9 -123.2(3) . . . . ? C1 P1 C8 C9 128.6(3) . . . . ? N1 P1 C8 C13 -174.2(2) . . . . ? C2 P1 C8 C13 57.6(3) . . . . ? C1 P1 C8 C13 -50.6(3) . . . . ? C13 C8 C9 C10 -1.1(5) . . . . ? P1 C8 C9 C10 179.6(3) . . . . ? C8 C9 C10 C11 1.0(5) . . . . ? C9 C10 C11 C12 0.0(6) . . . . ? C10 C11 C12 C13 -1.0(6) . . . . ? C11 C12 C13 C8 0.9(5) . . . . ? C9 C8 C13 C12 0.2(5) . . . . ? P1 C8 C13 C12 179.4(3) . . . . ? N2 P2 C14 C19 6.1(3) . . . . ? C20 P2 C14 C19 135.0(3) . . . . ? C1 P2 C14 C19 -115.7(3) . . . . ? N2 P2 C14 C15 179.2(2) . . . . ? C20 P2 C14 C15 -51.9(3) . . . . ? C1 P2 C14 C15 57.4(3) . . . . ? C19 C14 C15 C16 -0.7(5) . . . . ? P2 C14 C15 C16 -173.8(2) . . . . ? C14 C15 C16 C17 0.0(5) . . . . ? C15 C16 C17 C18 0.2(5) . . . . ? C16 C17 C18 C19 0.3(5) . . . . ? C15 C14 C19 C18 1.1(5) . . . . ? P2 C14 C19 C18 174.2(3) . . . . ? C17 C18 C19 C14 -0.9(5) . . . . ? N2 P2 C20 C25 -63.2(3) . . . . ? C14 P2 C20 C25 167.0(3) . . . . ? C1 P2 C20 C25 56.4(3) . . . . ? N2 P2 C20 C21 113.3(3) . . . . ? C14 P2 C20 C21 -16.6(3) . . . . ? C1 P2 C20 C21 -127.1(3) . . . . ? C25 C20 C21 C22 -0.1(5) . . . . ? P2 C20 C21 C22 -176.6(3) . . . . ? C20 C21 C22 C23 -0.5(5) . . . . ? C21 C22 C23 C24 0.6(6) . . . . ? C22 C23 C24 C25 -0.1(6) . . . . ? C23 C24 C25 C20 -0.5(5) . . . . ? C21 C20 C25 C24 0.6(5) . . . . ? P2 C20 C25 C24 177.2(3) . . . . ? N3 P3 C32 P4 52.9(2) . . . . ? C39 P3 C32 P4 -72.6(2) . . . . ? C33 P3 C32 P4 174.53(17) . . . . ? N4 P4 C32 P3 -58.5(2) . . . . ? C45 P4 C32 P3 66.6(2) . . . . ? C51 P4 C32 P3 179.29(17) . . . . ? N3 P3 C33 C34 54.9(3) . . . . ? C39 P3 C33 C34 -175.7(3) . . . . ? C32 P3 C33 C34 -63.9(3) . . . . ? N3 P3 C33 C38 -123.7(3) . . . . ? C39 P3 C33 C38 5.7(3) . . . . ? C32 P3 C33 C38 117.5(3) . . . . ? C38 C33 C34 C35 -1.4(5) . . . . ? P3 C33 C34 C35 179.9(3) . . . . ? C33 C34 C35 C36 0.5(5) . . . . ? C34 C35 C36 C37 0.7(6) . . . . ? C35 C36 C37 C38 -0.9(6) . . . . ? C36 C37 C38 C33 -0.1(6) . . . . ? C34 C33 C38 C37 1.2(5) . . . . ? P3 C33 C38 C37 179.8(3) . . . . ? N3 P3 C39 C40 -4.7(3) . . . . ? C32 P3 C39 C40 117.1(3) . . . . ? C33 P3 C39 C40 -133.0(3) . . . . ? N3 P3 C39 C44 179.9(3) . . . . ? C32 P3 C39 C44 -58.3(3) . . . . ? C33 P3 C39 C44 51.5(3) . . . . ? C44 C39 C40 C41 -1.0(5) . . . . ? P3 C39 C40 C41 -176.5(3) . . . . ? C39 C40 C41 C42 -0.3(6) . . . . ? C40 C41 C42 C43 1.7(7) . . . . ? C41 C42 C43 C44 -1.9(7) . . . . ? C42 C43 C44 C39 0.5(6) . . . . ? C40 C39 C44 C43 0.9(5) . . . . ? P3 C39 C44 C43 176.3(3) . . . . ? N4 P4 C45 C50 178.6(2) . . . . ? C51 P4 C45 C50 -51.9(3) . . . . ? C32 P4 C45 C50 56.0(3) . . . . ? N4 P4 C45 C46 2.1(3) . . . . ? C51 P4 C45 C46 131.6(2) . . . . ? C32 P4 C45 C46 -120.5(2) . . . . ? C50 C45 C46 C47 1.5(5) . . . . ? P4 C45 C46 C47 178.1(3) . . . . ? C45 C46 C47 C48 -0.4(5) . . . . ? C46 C47 C48 C49 -1.4(6) . . . . ? C47 C48 C49 C50 2.2(6) . . . . ? C48 C49 C50 C45 -1.1(5) . . . . ? C46 C45 C50 C49 -0.7(5) . . . . ? P4 C45 C50 C49 -177.3(3) . . . . ? N4 P4 C51 C56 -58.9(3) . . . . ? C45 P4 C51 C56 171.8(2) . . . . ? C32 P4 C51 C56 60.3(3) . . . . ? N4 P4 C51 C52 122.2(3) . . . . ? C45 P4 C51 C52 -7.1(3) . . . . ? C32 P4 C51 C52 -118.6(3) . . . . ? C56 C51 C52 C53 -2.7(5) . . . . ? P4 C51 C52 C53 176.2(3) . . . . ? C51 C52 C53 C54 -0.2(6) . . . . ? C52 C53 C54 C55 3.1(6) . . . . ? C53 C54 C55 C56 -3.0(6) . . . . ? C54 C55 C56 C51 0.1(6) . . . . ? C52 C51 C56 C55 2.8(5) . . . . ? P4 C51 C56 C55 -176.2(3) . . . . ? C69 C64 C65 C66 2.0(6) . . . . ? C63 C64 C65 C66 -176.2(4) . . . . ? C64 C65 C66 C67 -1.8(6) . . . . ? C65 C66 C67 C68 0.4(6) . . . . ? C66 C67 C68 C69 0.8(6) . . . . ? C65 C64 C69 C68 -0.8(6) . . . . ? C63 C64 C69 C68 177.4(4) . . . . ? C67 C68 C69 C64 -0.6(6) . . . . ? C76 C71 C72 C73 1.8(6) . . . . ? C70 C71 C72 C73 -175.9(4) . . . . ? C71 C72 C73 C74 -0.6(7) . . . . ? C72 C73 C74 C75 -0.9(7) . . . . ? C73 C74 C75 C76 1.1(7) . . . . ? C74 C75 C76 C71 0.2(7) . . . . ? C72 C71 C76 C75 -1.6(7) . . . . ? C70 C71 C76 C75 176.1(5) . . . . ? C83 C78 C79 C80 2.8(11) . . . . ? C77 C78 C79 C80 -173.8(8) . . . . ? C78 C79 C80 C81 -0.5(11) . . . . ? C79 C80 C81 C82 -1.7(10) . . . . ? C80 C81 C82 C83 1.8(10) . . . . ? C79 C78 C83 C82 -2.8(11) . . . . ? C77 C78 C83 C82 173.9(8) . . . . ? C81 C82 C83 C78 0.4(10) . . . . ? C83B C78B C79B C80B 1.8(17) . . . . ? C77B C78B C79B C80B -171.4(13) . . . . ? C78B C79B C80B C81B -1.9(19) . . . . ? C79B C80B C81B C82B -0.4(18) . . . . ? C80B C81B C82B C83B 2.5(18) . . . . ? C81B C82B C83B C78B -2.4(16) . . . . ? C79B C78B C83B C82B 0.4(15) . . . . ? C77B C78B C83B C82B 175.2(10) . . . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 29.25 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.453 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.076 #============================================================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 770405' #TrackingRef '- deposit.CIF' _audit_creation_date 09-02-03 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H40 I2 N2 P2 Si2 Zn, 2 (C4 H8 O)' _chemical_formula_sum 'C39 H56 I2 N2 O2 P2 Si2 Zn' _chemical_formula_weight 1022.15 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' P P 0.1023 0.0942 '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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.523(2) _cell_length_b 22.951(5) _cell_length_c 16.995(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.95(3) _cell_angle_gamma 90.00 _cell_volume 4491.9(16) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 6180 _cell_measurement_theta_min 1.49 _cell_measurement_theta_max 26.12 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.266 _exptl_crystal_size_mid 0.123 _exptl_crystal_size_min 0.043 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2056 _exptl_absorpt_coefficient_mu 2.079 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6674 _exptl_absorpt_correction_T_max 0.9021 _exptl_absorpt_process_details 'STOE X-RED & X-SHAPE' _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8149 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0722 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 25.62 _reflns_number_total 8149 _reflns_number_gt 5222 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e' _computing_publication_material 'WinGX32, Microsoft Word' _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^)+(0.0608P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8149 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0827 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1135 _refine_ls_wR_factor_gt 0.1016 _refine_ls_goodness_of_fit_ref 0.899 _refine_ls_restrained_S_all 0.899 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.3267(5) 0.1806(3) 0.2533(4) 0.0350(14) Uani 1 1 d . . . H1A H -0.3969 0.2046 0.2479 0.042 Uiso 1 1 calc R . . H1B H -0.2604 0.2066 0.2462 0.042 Uiso 1 1 calc R . . C2 C -0.3304(5) 0.1770(3) 0.0874(4) 0.0350(14) Uani 1 1 d . . . C3 C -0.2297(6) 0.2105(3) 0.0763(4) 0.0426(16) Uani 1 1 d . . . H3 H -0.1683 0.2095 0.1141 0.051 Uiso 1 1 calc R . . C4 C -0.2212(6) 0.2448(3) 0.0096(4) 0.0496(18) Uani 1 1 d . . . H4 H -0.1540 0.2671 0.0025 0.059 Uiso 1 1 calc R . . C5 C -0.3110(7) 0.2463(3) -0.0465(5) 0.0510(19) Uani 1 1 d . . . H5 H -0.3042 0.2692 -0.0920 0.061 Uiso 1 1 calc R . . C6 C -0.4100(6) 0.2143(4) -0.0358(4) 0.0496(18) Uani 1 1 d . . . H6 H -0.4714 0.2160 -0.0737 0.060 Uiso 1 1 calc R . . C7 C -0.4203(6) 0.1795(3) 0.0308(4) 0.0439(16) Uani 1 1 d . . . H7 H -0.4882 0.1576 0.0375 0.053 Uiso 1 1 calc R . . C8 C -0.4686(6) 0.0936(3) 0.1720(4) 0.0387(15) Uani 1 1 d . . . C9 C -0.4722(7) 0.0336(4) 0.1735(4) 0.0514(19) Uani 1 1 d . . . H9 H -0.4027 0.0121 0.1757 0.062 Uiso 1 1 calc R . . C10 C -0.5785(7) 0.0047(4) 0.1719(5) 0.058(2) Uani 1 1 d . . . H10 H -0.5815 -0.0362 0.1706 0.069 Uiso 1 1 calc R . . C11 C -0.6792(7) 0.0369(5) 0.1724(5) 0.062(2) Uani 1 1 d . . . H11 H -0.7510 0.0175 0.1724 0.074 Uiso 1 1 calc R . . C12 C -0.6772(6) 0.0957(5) 0.1727(5) 0.059(2) Uani 1 1 d . . . H12 H -0.7473 0.1167 0.1733 0.071 Uiso 1 1 calc R . . C13 C -0.5709(6) 0.1257(4) 0.1722(4) 0.0464(17) Uani 1 1 d . . . H13 H -0.5690 0.1666 0.1720 0.056 Uiso 1 1 calc R . . C14 C -0.4520(5) 0.1174(3) 0.3710(4) 0.0357(14) Uani 1 1 d . . . C15 C -0.4503(6) 0.0585(3) 0.3890(4) 0.0447(16) Uani 1 1 d . . . H15 H -0.3790 0.0389 0.3954 0.054 Uiso 1 1 calc R . . C16 C -0.5545(7) 0.0282(4) 0.3977(5) 0.0509(18) Uani 1 1 d . . . H16 H -0.5535 -0.0116 0.4109 0.061 Uiso 1 1 calc R . . C17 C -0.6575(7) 0.0569(4) 0.3868(4) 0.054(2) Uani 1 1 d . . . H17 H -0.7276 0.0363 0.3906 0.064 Uiso 1 1 calc R . . C18 C -0.6608(6) 0.1159(4) 0.3701(4) 0.0517(19) Uani 1 1 d . . . H18 H -0.7324 0.1352 0.3637 0.062 Uiso 1 1 calc R . . C19 C -0.5594(6) 0.1461(3) 0.3629(4) 0.0448(16) Uani 1 1 d . . . H19 H -0.5616 0.1863 0.3526 0.054 Uiso 1 1 calc R . . C20 C -0.3167(5) 0.2201(3) 0.4120(4) 0.0347(14) Uani 1 1 d . . . C21 C -0.2308(5) 0.2617(3) 0.3968(4) 0.0389(15) Uani 1 1 d . . . H21 H -0.1772 0.2547 0.3574 0.047 Uiso 1 1 calc R . . C22 C -0.2247(6) 0.3132(3) 0.4398(4) 0.0464(17) Uani 1 1 d . . . H22 H -0.1681 0.3413 0.4288 0.056 Uiso 1 1 calc R . . C23 C -0.3013(7) 0.3227(3) 0.4981(5) 0.0517(19) Uani 1 1 d . . . H23 H -0.2972 0.3576 0.5270 0.062 Uiso 1 1 calc R . . C24 C -0.3844(7) 0.2820(3) 0.5150(5) 0.0512(18) Uani 1 1 d . . . H24 H -0.4359 0.2891 0.5556 0.061 Uiso 1 1 calc R . . C25 C -0.3928(6) 0.2304(3) 0.4724(4) 0.0432(16) Uani 1 1 d . . . H25 H -0.4495 0.2026 0.4842 0.052 Uiso 1 1 calc R . . C26 C -0.2351(8) 0.1213(5) 0.5452(5) 0.070(3) Uani 1 1 d . . . H26A H -0.3141 0.1067 0.5400 0.105 Uiso 1 1 calc R . . H26B H -0.2360 0.1635 0.5439 0.105 Uiso 1 1 calc R . . H26C H -0.2001 0.1082 0.5949 0.105 Uiso 1 1 calc R . . C27 C -0.0005(7) 0.1229(4) 0.4764(5) 0.056(2) Uani 1 1 d . . . H27A H -0.0027 0.1650 0.4714 0.083 Uiso 1 1 calc R . . H27B H 0.0489 0.1068 0.4367 0.083 Uiso 1 1 calc R . . H27C H 0.0304 0.1125 0.5283 0.083 Uiso 1 1 calc R . . C28 C -0.1540(6) 0.0129(3) 0.4716(4) 0.0494(18) Uani 1 1 d . . . H28A H -0.2336 -0.0004 0.4645 0.074 Uiso 1 1 calc R . . H28B H -0.1241 0.0015 0.5233 0.074 Uiso 1 1 calc R . . H28C H -0.1069 -0.0045 0.4316 0.074 Uiso 1 1 calc R . . C29 C -0.1794(7) -0.0336(3) 0.1249(5) 0.0538(19) Uani 1 1 d . . . H29A H -0.2587 -0.0440 0.1364 0.081 Uiso 1 1 calc R . . H29B H -0.1293 -0.0412 0.1708 0.081 Uiso 1 1 calc R . . H29C H -0.1538 -0.0567 0.0809 0.081 Uiso 1 1 calc R . . C30 C -0.0225(7) 0.0680(3) 0.0760(5) 0.0492(18) Uani 1 1 d . . . H30A H 0.0280 0.0638 0.1225 0.074 Uiso 1 1 calc R . . H30B H -0.0233 0.1085 0.0594 0.074 Uiso 1 1 calc R . . H30C H 0.0061 0.0438 0.0341 0.074 Uiso 1 1 calc R . . C31 C -0.2648(8) 0.0536(4) 0.0070(4) 0.058(2) Uani 1 1 d . . . H31A H -0.3440 0.0422 0.0169 0.087 Uiso 1 1 calc R . . H31B H -0.2345 0.0292 -0.0341 0.087 Uiso 1 1 calc R . . H31C H -0.2635 0.0940 -0.0097 0.087 Uiso 1 1 calc R . . C32 C -0.0034(10) 0.3581(5) 0.1720(7) 0.088(3) Uani 1 1 d . . . H32A H 0.0542 0.3893 0.1789 0.106 Uiso 1 1 calc R . . H32B H 0.0364 0.3208 0.1803 0.106 Uiso 1 1 calc R . . C33 C -0.0960(15) 0.3650(6) 0.2313(9) 0.119(5) Uani 1 1 d . . . H33A H -0.1097 0.3287 0.2599 0.143 Uiso 1 1 calc R . . H33B H -0.0776 0.3963 0.2690 0.143 Uiso 1 1 calc R . . C34 C -0.1965(17) 0.3806(14) 0.1771(13) 0.215(13) Uani 1 1 d . . . H34A H -0.2561 0.3502 0.1796 0.258 Uiso 1 1 calc R . . H34B H -0.2308 0.4173 0.1944 0.258 Uiso 1 1 calc R . . C35 C -0.1614(12) 0.3865(6) 0.0982(9) 0.105(4) Uani 1 1 d . . . H35A H -0.2172 0.3673 0.0619 0.126 Uiso 1 1 calc R . . H35B H -0.1566 0.4278 0.0838 0.126 Uiso 1 1 calc R . . C36 C -0.6677(8) 0.2835(5) 0.2415(7) 0.080(3) Uani 1 1 d . . . H36A H -0.7116 0.2506 0.2621 0.096 Uiso 1 1 calc R . . H36B H -0.6832 0.2859 0.1846 0.096 Uiso 1 1 calc R . . C37 C -0.7042(7) 0.3408(5) 0.2818(6) 0.071(3) Uani 1 1 d . . . H37A H -0.7211 0.3715 0.2430 0.086 Uiso 1 1 calc R . . H37B H -0.7725 0.3349 0.3138 0.086 Uiso 1 1 calc R . . C38 C -0.5979(9) 0.3557(5) 0.3329(6) 0.075(3) Uani 1 1 d . . . H38A H -0.5886 0.3980 0.3384 0.090 Uiso 1 1 calc R . . H38B H -0.6025 0.3383 0.3854 0.090 Uiso 1 1 calc R . . C39 C -0.5011(8) 0.3299(4) 0.2887(7) 0.074(3) Uani 1 1 d . . . H39A H -0.4788 0.3557 0.2458 0.089 Uiso 1 1 calc R . . H39B H -0.4330 0.3231 0.3236 0.089 Uiso 1 1 calc R . . N1 N -0.2201(4) 0.0874(2) 0.1775(3) 0.0369(12) Uani 1 1 d . . . N2 N -0.2050(4) 0.1143(2) 0.3689(3) 0.0353(12) Uani 1 1 d . . . O1 O -0.0528(7) 0.3603(4) 0.0944(5) 0.100(2) Uani 1 1 d . . . O2 O -0.5465(5) 0.2756(3) 0.2580(5) 0.0772(19) Uani 1 1 d . . . Si1 Si -0.17280(17) 0.04491(9) 0.09934(11) 0.0405(4) Uani 1 1 d . . . Si2 Si -0.14925(16) 0.09325(9) 0.46256(11) 0.0398(4) Uani 1 1 d . . . P1 P -0.32978(13) 0.12990(7) 0.17269(9) 0.0334(3) Uani 1 1 d . . . P2 P -0.31726(13) 0.15392(7) 0.35486(9) 0.0321(3) Uani 1 1 d . . . Zn1 Zn -0.10843(6) 0.09631(3) 0.27404(4) 0.03359(17) Uani 1 1 d . . . I1 I 0.01996(4) 0.19126(2) 0.25200(3) 0.03989(12) Uani 1 1 d . . . I2 I 0.03215(4) 0.00885(2) 0.29086(3) 0.04603(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.020(3) 0.037(4) 0.047(4) 0.006(3) -0.005(3) 0.000(2) C2 0.030(3) 0.040(4) 0.035(3) -0.001(3) -0.001(3) 0.000(3) C3 0.030(3) 0.060(4) 0.037(3) 0.004(3) -0.007(3) 0.002(3) C4 0.032(3) 0.063(5) 0.053(4) 0.014(4) 0.002(3) -0.004(3) C5 0.047(4) 0.057(5) 0.049(4) 0.019(4) -0.003(3) 0.004(4) C6 0.039(4) 0.067(5) 0.043(4) 0.015(4) -0.005(3) 0.002(3) C7 0.029(3) 0.055(5) 0.047(4) 0.007(3) -0.004(3) -0.002(3) C8 0.032(3) 0.052(4) 0.031(3) -0.001(3) -0.003(3) -0.003(3) C9 0.045(4) 0.061(5) 0.048(4) 0.002(4) -0.006(3) -0.013(3) C10 0.050(4) 0.068(5) 0.055(4) 0.000(4) 0.000(4) -0.024(4) C11 0.045(4) 0.093(7) 0.048(4) -0.009(4) 0.006(4) -0.024(4) C12 0.030(3) 0.104(7) 0.043(4) -0.013(4) -0.002(3) -0.010(4) C13 0.039(4) 0.061(5) 0.040(4) -0.003(3) 0.002(3) -0.002(3) C14 0.032(3) 0.044(4) 0.030(3) 0.001(3) 0.000(3) 0.001(3) C15 0.042(4) 0.054(4) 0.039(4) 0.001(3) 0.000(3) -0.002(3) C16 0.049(4) 0.053(5) 0.051(4) 0.002(3) 0.000(3) -0.016(3) C17 0.042(4) 0.076(6) 0.042(4) 0.002(4) -0.001(3) -0.017(4) C18 0.027(3) 0.080(6) 0.048(4) -0.001(4) 0.007(3) -0.008(3) C19 0.038(4) 0.052(4) 0.045(4) 0.004(3) 0.004(3) 0.001(3) C20 0.027(3) 0.046(4) 0.031(3) -0.003(3) -0.003(2) 0.006(3) C21 0.029(3) 0.044(4) 0.044(4) -0.001(3) 0.002(3) 0.000(3) C22 0.033(3) 0.045(4) 0.061(4) -0.011(3) -0.002(3) -0.004(3) C23 0.054(4) 0.049(4) 0.052(4) -0.020(3) -0.009(4) 0.011(3) C24 0.048(4) 0.058(5) 0.047(4) -0.015(4) -0.001(3) 0.006(4) C25 0.041(4) 0.050(4) 0.039(4) -0.005(3) 0.005(3) 0.004(3) C26 0.071(6) 0.098(7) 0.041(4) 0.008(4) -0.005(4) 0.034(5) C27 0.054(4) 0.051(5) 0.060(5) 0.005(4) -0.022(4) -0.005(3) C28 0.038(3) 0.061(5) 0.049(4) 0.018(4) -0.001(3) 0.005(3) C29 0.054(5) 0.050(5) 0.057(5) -0.011(4) 0.004(4) -0.003(4) C30 0.049(4) 0.050(4) 0.049(4) -0.005(3) 0.012(3) 0.006(3) C31 0.073(6) 0.061(5) 0.040(4) -0.011(4) -0.004(4) 0.005(4) C32 0.082(7) 0.092(8) 0.091(8) 0.022(6) -0.001(6) 0.008(6) C33 0.161(15) 0.091(9) 0.107(10) 0.027(8) 0.030(10) 0.005(9) C34 0.094(12) 0.40(4) 0.152(18) -0.01(2) 0.037(13) 0.068(17) C35 0.088(8) 0.102(9) 0.124(11) -0.035(8) -0.014(8) 0.024(7) C36 0.052(5) 0.098(8) 0.089(7) 0.004(6) -0.018(5) 0.002(5) C37 0.042(4) 0.094(7) 0.079(6) 0.027(5) 0.016(4) 0.011(4) C38 0.071(6) 0.069(6) 0.084(7) 0.012(5) -0.004(5) -0.002(5) C39 0.052(5) 0.058(6) 0.112(8) 0.012(5) -0.013(5) -0.004(4) N1 0.028(3) 0.044(3) 0.038(3) 0.004(2) -0.005(2) 0.000(2) N2 0.031(3) 0.035(3) 0.040(3) -0.001(2) -0.003(2) 0.008(2) O1 0.068(5) 0.141(7) 0.090(5) -0.004(5) 0.001(4) 0.019(5) O2 0.049(3) 0.061(4) 0.121(6) 0.012(4) -0.006(4) 0.007(3) Si1 0.0396(10) 0.0452(11) 0.0366(10) -0.0055(8) -0.0005(8) -0.0001(8) Si2 0.0357(9) 0.0494(11) 0.0339(9) 0.0030(8) -0.0022(8) 0.0070(8) P1 0.0266(7) 0.0420(9) 0.0314(8) -0.0015(7) -0.0030(6) -0.0012(6) P2 0.0258(7) 0.0390(9) 0.0315(8) -0.0001(7) -0.0005(6) 0.0018(6) Zn1 0.0263(3) 0.0409(4) 0.0334(4) -0.0008(3) -0.0015(3) 0.0013(3) I1 0.0313(2) 0.0454(2) 0.0427(2) 0.0004(2) -0.00158(17) -0.00583(18) I2 0.0377(2) 0.0512(3) 0.0490(3) 0.0012(2) -0.00081(19) 0.0121(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 C1 P1 1.796(7) . ? C1 P2 1.832(7) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C2 C7 1.390(8) . ? C2 C3 1.410(10) . ? C2 P1 1.808(7) . ? C3 C4 1.386(10) . ? C3 H3 0.9400 . ? C4 C5 1.384(10) . ? C4 H4 0.9400 . ? C5 C6 1.374(11) . ? C5 H5 0.9400 . ? C6 C7 1.395(10) . ? C6 H6 0.9400 . ? C7 H7 0.9400 . ? C8 C9 1.380(11) . ? C8 C13 1.389(10) . ? C8 P1 1.803(7) . ? C9 C10 1.393(10) . ? C9 H9 0.9400 . ? C10 C11 1.376(13) . ? C10 H10 0.9400 . ? C11 C12 1.350(13) . ? C11 H11 0.9400 . ? C12 C13 1.406(11) . ? C12 H12 0.9400 . ? C13 H13 0.9400 . ? C14 C15 1.385(10) . ? C14 C19 1.405(9) . ? C14 P2 1.794(7) . ? C15 C16 1.400(10) . ? C15 H15 0.9400 . ? C16 C17 1.366(12) . ? C16 H16 0.9400 . ? C17 C18 1.383(12) . ? C17 H17 0.9400 . ? C18 C19 1.366(10) . ? C18 H18 0.9400 . ? C19 H19 0.9400 . ? C20 C25 1.392(9) . ? C20 C21 1.405(9) . ? C20 P2 1.804(7) . ? C21 C22 1.390(10) . ? C21 H21 0.9400 . ? C22 C23 1.367(11) . ? C22 H22 0.9400 . ? C23 C24 1.375(12) . ? C23 H23 0.9400 . ? C24 C25 1.389(10) . ? C24 H24 0.9400 . ? C25 H25 0.9400 . ? C26 Si2 1.861(9) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 Si2 1.852(8) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 Si2 1.851(8) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C29 Si1 1.856(8) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C30 Si1 1.867(8) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? C31 Si1 1.875(8) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 O1 1.419(13) . ? C32 C33 1.502(19) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C33 C34 1.50(2) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C34 C35 1.42(2) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C35 O1 1.393(14) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C36 O2 1.426(10) . ? C36 C37 1.549(15) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C37 C38 1.517(13) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C38 C39 1.490(15) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C39 O2 1.442(11) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? N1 P1 1.596(5) . ? N1 Si1 1.750(6) . ? N1 Zn1 2.061(5) . ? N2 P2 1.592(5) . ? N2 Si2 1.763(5) . ? N2 Zn1 2.033(6) . ? Zn1 I2 2.5891(9) . ? Zn1 I1 2.6675(10) . ? 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 P1 C1 P2 120.1(3) . . ? P1 C1 H1A 107.3 . . ? P2 C1 H1A 107.3 . . ? P1 C1 H1B 107.3 . . ? P2 C1 H1B 107.3 . . ? H1A C1 H1B 106.9 . . ? C7 C2 C3 118.8(6) . . ? C7 C2 P1 124.2(5) . . ? C3 C2 P1 116.9(4) . . ? C4 C3 C2 120.1(6) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C5 C4 C3 120.4(7) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C6 C5 C4 120.0(7) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C7 120.5(6) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C2 C7 C6 120.2(6) . . ? C2 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C9 C8 C13 120.2(7) . . ? C9 C8 P1 119.2(5) . . ? C13 C8 P1 120.5(6) . . ? C8 C9 C10 120.1(8) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C11 C10 C9 119.0(8) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? C12 C11 C10 121.6(7) . . ? C12 C11 H11 119.2 . . ? C10 C11 H11 119.2 . . ? C11 C12 C13 120.3(8) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C8 C13 C12 118.7(8) . . ? C8 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C15 C14 C19 119.0(6) . . ? C15 C14 P2 119.0(5) . . ? C19 C14 P2 122.0(5) . . ? C14 C15 C16 120.2(7) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C17 C16 C15 119.3(8) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C18 121.2(7) . . ? C16 C17 H17 119.4 . . ? C18 C17 H17 119.4 . . ? C19 C18 C17 119.8(7) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C14 120.4(7) . . ? C18 C19 H19 119.8 . . ? C14 C19 H19 119.8 . . ? C25 C20 C21 119.1(6) . . ? C25 C20 P2 123.3(5) . . ? C21 C20 P2 117.5(5) . . ? C22 C21 C20 120.2(7) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C23 C22 C21 119.6(7) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C22 C23 C24 121.0(7) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C23 C24 C25 120.4(7) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C24 C25 C20 119.6(7) . . ? C24 C25 H25 120.2 . . ? C20 C25 H25 120.2 . . ? 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 . . ? Si2 C28 H28A 109.5 . . ? Si2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si1 C29 H29A 109.5 . . ? Si1 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si1 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? 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 . . ? O1 C32 C33 110.4(10) . . ? O1 C32 H32A 109.6 . . ? C33 C32 H32A 109.6 . . ? O1 C32 H32B 109.6 . . ? C33 C32 H32B 109.6 . . ? H32A C32 H32B 108.1 . . ? C34 C33 C32 99.4(12) . . ? C34 C33 H33A 111.9 . . ? C32 C33 H33A 111.9 . . ? C34 C33 H33B 111.9 . . ? C32 C33 H33B 111.9 . . ? H33A C33 H33B 109.6 . . ? C35 C34 C33 111.4(15) . . ? C35 C34 H34A 109.4 . . ? C33 C34 H34A 109.4 . . ? C35 C34 H34B 109.4 . . ? C33 C34 H34B 109.4 . . ? H34A C34 H34B 108.0 . . ? O1 C35 C34 106.7(13) . . ? O1 C35 H35A 110.4 . . ? C34 C35 H35A 110.4 . . ? O1 C35 H35B 110.4 . . ? C34 C35 H35B 110.4 . . ? H35A C35 H35B 108.6 . . ? O2 C36 C37 107.5(8) . . ? O2 C36 H36A 110.2 . . ? C37 C36 H36A 110.2 . . ? O2 C36 H36B 110.2 . . ? C37 C36 H36B 110.2 . . ? H36A C36 H36B 108.5 . . ? C38 C37 C36 102.6(7) . . ? C38 C37 H37A 111.2 . . ? C36 C37 H37A 111.2 . . ? C38 C37 H37B 111.2 . . ? C36 C37 H37B 111.2 . . ? H37A C37 H37B 109.2 . . ? C39 C38 C37 103.0(8) . . ? C39 C38 H38A 111.2 . . ? C37 C38 H38A 111.2 . . ? C39 C38 H38B 111.2 . . ? C37 C38 H38B 111.2 . . ? H38A C38 H38B 109.1 . . ? O2 C39 C38 104.9(8) . . ? O2 C39 H39A 110.8 . . ? C38 C39 H39A 110.8 . . ? O2 C39 H39B 110.8 . . ? C38 C39 H39B 110.8 . . ? H39A C39 H39B 108.8 . . ? P1 N1 Si1 124.6(3) . . ? P1 N1 Zn1 116.9(3) . . ? Si1 N1 Zn1 117.2(3) . . ? P2 N2 Si2 124.2(3) . . ? P2 N2 Zn1 117.4(3) . . ? Si2 N2 Zn1 117.9(3) . . ? C35 O1 C32 107.8(10) . . ? C36 O2 C39 107.6(7) . . ? N1 Si1 C29 110.3(3) . . ? N1 Si1 C30 108.5(3) . . ? C29 Si1 C30 111.8(4) . . ? N1 Si1 C31 113.2(3) . . ? C29 Si1 C31 105.8(4) . . ? C30 Si1 C31 107.1(4) . . ? N2 Si2 C28 109.7(3) . . ? N2 Si2 C27 108.7(3) . . ? C28 Si2 C27 112.7(3) . . ? N2 Si2 C26 113.6(3) . . ? C28 Si2 C26 105.3(4) . . ? C27 Si2 C26 106.9(4) . . ? N1 P1 C1 111.2(3) . . ? N1 P1 C8 114.8(3) . . ? C1 P1 C8 107.4(3) . . ? N1 P1 C2 112.8(3) . . ? C1 P1 C2 102.9(3) . . ? C8 P1 C2 107.0(3) . . ? N2 P2 C14 114.4(3) . . ? N2 P2 C20 114.3(3) . . ? C14 P2 C20 107.4(3) . . ? N2 P2 C1 110.7(3) . . ? C14 P2 C1 106.1(3) . . ? C20 P2 C1 103.0(3) . . ? N2 Zn1 N1 107.9(2) . . ? N2 Zn1 I2 115.30(14) . . ? N1 Zn1 I2 112.48(16) . . ? N2 Zn1 I1 105.47(15) . . ? N1 Zn1 I1 107.67(16) . . ? I2 Zn1 I1 107.52(3) . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 25.62 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 0.562 _refine_diff_density_min -0.970 _refine_diff_density_rms 0.108 #============================================================================== data_3 _database_code_depnum_ccdc_archive 'CCDC 770406' #TrackingRef '- deposit.CIF' _audit_creation_date 09-02-04 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H44 N2 P2 Si2 Zn' _chemical_formula_sum 'C37 H44 N2 P2 Si2 Zn' _chemical_formula_weight 700.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.286(2) _cell_length_b 16.726(3) _cell_length_c 22.270(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.73(3) _cell_angle_gamma 90.00 _cell_volume 3751.1(13) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plates _exptl_crystal_colour colourless _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.333 _exptl_crystal_size_min 0.300 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.240 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 0.831 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'STOE X-RED & X-SHAPE' _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30061 _diffrn_reflns_av_R_equivalents 0.0616 _diffrn_reflns_av_sigmaI/netI 0.0374 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 27.93 _reflns_number_total 8939 _reflns_number_gt 7913 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e' _computing_publication_material 'WinGX32, Microsoft Word' _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^)+(0.0467P)^2^+0.9406P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8939 _refine_ls_number_parameters 573 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0387 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0918 _refine_ls_wR_factor_gt 0.0890 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.24164(15) 0.36356(9) 0.22141(7) 0.0290(3) Uani 1 1 d . . . C2 C 0.02788(19) 0.15218(11) 0.21708(10) 0.0493(5) Uani 1 1 d . . . C3 C 0.0267(2) 0.10176(13) 0.26720(15) 0.0665(7) Uani 1 1 d . . . C4 C 0.0384(3) 0.01874(15) 0.2634(2) 0.0988(13) Uani 1 1 d . . . C5 C 0.0500(3) -0.01612(19) 0.2101(3) 0.1190(19) Uani 1 1 d . . . C6 C 0.0516(3) 0.0302(2) 0.1597(3) 0.1071(16) Uani 1 1 d . . . C7 C 0.0414(3) 0.11412(18) 0.16328(15) 0.0744(9) Uani 1 1 d . . . C8 C -0.21067(15) 0.38223(9) 0.34881(7) 0.0297(3) Uani 1 1 d . . . C9 C -0.28495(18) 0.31303(10) 0.35223(8) 0.0384(3) Uani 1 1 d . . . C10 C -0.3470(2) 0.30071(12) 0.40113(9) 0.0464(4) Uani 1 1 d . . . C11 C -0.3351(2) 0.35705(12) 0.44744(9) 0.0487(4) Uani 1 1 d . . . C12 C -0.2611(2) 0.42569(12) 0.44487(8) 0.0458(4) Uani 1 1 d . . . C13 C -0.19837(18) 0.43794(10) 0.39612(8) 0.0364(3) Uani 1 1 d . . . C14 C -0.07659(15) 0.49611(9) 0.28210(7) 0.0294(3) Uani 1 1 d . . . C15 C 0.04735(17) 0.51490(10) 0.26985(8) 0.0375(3) Uani 1 1 d . . . C16 C 0.0812(2) 0.59375(12) 0.26068(10) 0.0481(4) Uani 1 1 d . . . C17 C -0.0093(2) 0.65411(11) 0.26352(10) 0.0479(4) Uani 1 1 d . . . C18 C -0.1327(2) 0.63647(10) 0.27556(8) 0.0405(4) Uani 1 1 d . . . C19 C -0.16703(17) 0.55793(9) 0.28485(7) 0.0332(3) Uani 1 1 d . . . C20 C -0.27009(16) 0.44790(9) 0.10055(7) 0.0325(3) Uani 1 1 d . . . C21 C -0.2731(2) 0.52235(10) 0.12760(9) 0.0443(4) Uani 1 1 d . . . C22 C -0.3052(2) 0.59022(12) 0.09182(11) 0.0549(5) Uani 1 1 d . . . C23 C -0.3372(2) 0.58381(13) 0.02861(11) 0.0550(5) Uani 1 1 d . . . C24 C -0.3370(2) 0.51010(14) 0.00128(9) 0.0529(5) Uani 1 1 d . . . C25 C -0.30378(19) 0.44198(12) 0.03671(8) 0.0423(4) Uani 1 1 d . . . C26 C -0.32095(16) 0.28202(9) 0.10925(7) 0.0315(3) Uani 1 1 d . . . C27 C -0.45779(18) 0.28550(11) 0.10276(9) 0.0429(4) Uani 1 1 d . . . C28 C -0.5365(2) 0.22149(14) 0.07774(11) 0.0565(5) Uani 1 1 d . . . C29 C -0.4786(3) 0.15427(13) 0.05876(10) 0.0582(6) Uani 1 1 d . . . C30 C -0.3433(2) 0.15039(11) 0.06426(9) 0.0502(5) Uani 1 1 d . . . C31 C -0.2637(2) 0.21406(10) 0.08919(8) 0.0386(4) Uani 1 1 d . . . C32 C 0.0518(3) 0.48511(15) 0.09497(14) 0.0639(6) Uani 1 1 d . . . C33 C 0.0196(4) 0.3254(2) 0.02978(14) 0.0722(8) Uani 1 1 d . . . C34 C 0.2168(2) 0.3446(2) 0.15134(18) 0.0798(9) Uani 1 1 d . . . C35 C 0.1755(2) 0.41425(13) 0.40609(10) 0.0494(4) Uani 1 1 d . . . C36 C 0.0705(3) 0.24826(14) 0.41511(11) 0.0569(6) Uani 1 1 d . . . C37 C 0.2744(2) 0.27761(18) 0.33679(15) 0.0643(6) Uani 1 1 d . . . N1 N 0.00609(13) 0.33627(8) 0.29583(6) 0.0312(3) Uani 1 1 d . . . N2 N -0.06035(13) 0.34296(8) 0.15030(6) 0.0338(3) Uani 1 1 d . . . H1 H -0.327(2) 0.3616(12) 0.2253(10) 0.040(5) Uiso 1 1 d . . . H3 H 0.007(3) 0.127(2) 0.3085(17) 0.109(12) Uiso 1 1 d . . . H4 H 0.044(4) -0.022(3) 0.306(2) 0.152(16) Uiso 1 1 d . . . H5 H 0.059(4) -0.076(3) 0.209(2) 0.150(16) Uiso 1 1 d . . . H6 H 0.054(4) 0.014(2) 0.1252(18) 0.113(13) Uiso 1 1 d . . . H7 H 0.057(2) 0.1438(14) 0.1322(12) 0.050(7) Uiso 1 1 d . . . H9 H -0.286(2) 0.2720(14) 0.3223(11) 0.054(6) Uiso 1 1 d . . . H10 H -0.394(2) 0.2527(14) 0.4049(11) 0.053(6) Uiso 1 1 d . . . H11 H -0.379(2) 0.3497(14) 0.4801(11) 0.054(6) Uiso 1 1 d . . . H12 H -0.252(2) 0.4684(15) 0.4764(11) 0.060(7) Uiso 1 1 d . . . H13 H -0.147(2) 0.4850(13) 0.3948(10) 0.044(5) Uiso 1 1 d . . . H15 H 0.106(2) 0.4737(13) 0.2662(10) 0.042(5) Uiso 1 1 d . . . H16 H 0.165(2) 0.6036(14) 0.2513(11) 0.057(6) Uiso 1 1 d . . . H17 H 0.014(2) 0.7079(16) 0.2596(12) 0.063(7) Uiso 1 1 d . . . H18 H -0.198(2) 0.6766(13) 0.2778(10) 0.048(6) Uiso 1 1 d . . . H19 H -0.252(2) 0.5463(11) 0.2925(9) 0.036(5) Uiso 1 1 d . . . H21 H -0.252(2) 0.5276(13) 0.1702(11) 0.048(6) Uiso 1 1 d . . . H22 H -0.303(3) 0.6392(15) 0.1120(12) 0.064(7) Uiso 1 1 d . . . H23 H -0.356(3) 0.6309(16) 0.0070(12) 0.065(7) Uiso 1 1 d . . . H24 H -0.362(2) 0.5062(15) -0.0444(12) 0.059(7) Uiso 1 1 d . . . H25 H -0.304(2) 0.3934(14) 0.0202(10) 0.046(6) Uiso 1 1 d . . . H27 H -0.500(2) 0.3295(14) 0.1145(10) 0.047(6) Uiso 1 1 d . . . H28 H -0.629(3) 0.2271(15) 0.0751(13) 0.067(8) Uiso 1 1 d . . . H29 H -0.536(3) 0.1121(17) 0.0400(13) 0.078(8) Uiso 1 1 d . . . H30 H -0.301(3) 0.1035(16) 0.0503(12) 0.067(7) Uiso 1 1 d . . . H31 H -0.169(2) 0.2084(13) 0.0942(10) 0.042(5) Uiso 1 1 d . . . H32A H 0.058(4) 0.510(2) 0.1330(19) 0.120(13) Uiso 1 1 d . . . H32B H 0.125(3) 0.5002(18) 0.0799(14) 0.085(9) Uiso 1 1 d . . . H32C H -0.029(4) 0.507(2) 0.0649(17) 0.105(12) Uiso 1 1 d . . . H33A H 0.084(3) 0.340(2) 0.0112(16) 0.095(10) Uiso 1 1 d . . . H33B H 0.024(4) 0.275(2) 0.0355(16) 0.093(11) Uiso 1 1 d . . . H33C H -0.069(4) 0.338(2) 0.0072(18) 0.116(14) Uiso 1 1 d . . . H34A H 0.234(4) 0.375(2) 0.1903(19) 0.114(13) Uiso 1 1 d . . . H34B H 0.227(3) 0.286(2) 0.1620(16) 0.092(10) Uiso 1 1 d . . . H34C H 0.282(4) 0.358(2) 0.1323(19) 0.124(14) Uiso 1 1 d . . . H35A H 0.201(2) 0.4570(15) 0.3821(12) 0.061(7) Uiso 1 1 d . . . H35B H 0.248(3) 0.3977(16) 0.4361(13) 0.068(8) Uiso 1 1 d . . . H35C H 0.104(3) 0.4384(17) 0.4193(13) 0.078(9) Uiso 1 1 d . . . H36A H -0.008(4) 0.2703(19) 0.4327(15) 0.094(11) Uiso 1 1 d . . . H36B H 0.142(3) 0.2398(18) 0.4482(16) 0.088(10) Uiso 1 1 d . . . H36C H 0.054(4) 0.200(2) 0.3966(17) 0.108(12) Uiso 1 1 d . . . H37A H 0.254(3) 0.2265(19) 0.3125(15) 0.088(10) Uiso 1 1 d . . . H37B H 0.311(3) 0.313(2) 0.3146(17) 0.100(12) Uiso 1 1 d . . . H37C H 0.339(4) 0.263(2) 0.370(2) 0.121(13) Uiso 1 1 d . . . Si1 Si 0.12623(5) 0.32066(3) 0.36144(2) 0.03674(11) Uani 1 1 d . . . Si2 Si 0.05019(5) 0.37468(3) 0.10677(3) 0.04553(13) Uani 1 1 d . . . P1 P -0.12517(4) 0.39163(2) 0.285263(17) 0.02616(8) Uani 1 1 d . . . P2 P -0.21455(4) 0.36095(2) 0.147885(17) 0.02730(8) Uani 1 1 d . . . Zn1 Zn -0.003688(19) 0.267623(11) 0.222318(9) 0.03515(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0282(7) 0.0296(7) 0.0294(7) -0.0019(5) 0.0061(6) -0.0013(5) C2 0.0395(9) 0.0348(8) 0.0667(12) -0.0150(8) -0.0053(8) 0.0101(7) C3 0.0544(12) 0.0349(10) 0.104(2) 0.0031(11) 0.0014(13) 0.0049(9) C4 0.0659(16) 0.0358(12) 0.185(4) 0.0079(18) 0.003(2) 0.0053(11) C5 0.0591(16) 0.0424(14) 0.235(6) -0.042(2) -0.020(2) 0.0154(12) C6 0.0592(16) 0.089(2) 0.155(4) -0.083(3) -0.0215(19) 0.0294(16) C7 0.0591(14) 0.0695(16) 0.085(2) -0.0380(16) -0.0069(13) 0.0260(12) C8 0.0322(7) 0.0283(7) 0.0280(7) 0.0003(6) 0.0052(6) 0.0012(6) C9 0.0442(9) 0.0334(8) 0.0380(8) 0.0018(7) 0.0096(7) -0.0048(7) C10 0.0479(10) 0.0455(10) 0.0477(10) 0.0096(8) 0.0144(8) -0.0081(8) C11 0.0534(11) 0.0546(11) 0.0437(10) 0.0119(9) 0.0234(9) 0.0046(9) C12 0.0636(12) 0.0435(9) 0.0335(8) -0.0004(7) 0.0177(8) 0.0049(8) C13 0.0463(9) 0.0326(7) 0.0313(8) -0.0018(6) 0.0106(7) -0.0012(7) C14 0.0356(7) 0.0254(6) 0.0264(6) -0.0005(5) 0.0045(6) -0.0028(5) C15 0.0376(8) 0.0339(8) 0.0417(9) 0.0023(7) 0.0097(7) -0.0027(7) C16 0.0468(10) 0.0430(9) 0.0557(11) 0.0062(8) 0.0134(9) -0.0131(8) C17 0.0648(12) 0.0293(8) 0.0488(10) 0.0026(7) 0.0101(9) -0.0111(8) C18 0.0584(11) 0.0275(7) 0.0357(8) -0.0020(6) 0.0097(8) 0.0033(7) C19 0.0405(8) 0.0283(7) 0.0309(7) -0.0017(6) 0.0074(6) 0.0007(6) C20 0.0355(7) 0.0302(7) 0.0316(7) 0.0027(6) 0.0062(6) 0.0009(6) C21 0.0572(11) 0.0319(8) 0.0407(9) 0.0011(7) 0.0027(8) 0.0054(7) C22 0.0666(13) 0.0323(9) 0.0626(13) 0.0053(9) 0.0057(10) 0.0038(8) C23 0.0545(12) 0.0467(10) 0.0617(13) 0.0247(10) 0.0069(10) 0.0022(9) C24 0.0569(11) 0.0616(12) 0.0389(9) 0.0171(9) 0.0067(9) -0.0004(9) C25 0.0500(10) 0.0432(9) 0.0333(8) 0.0022(7) 0.0077(7) 0.0007(8) C26 0.0389(8) 0.0283(7) 0.0250(7) -0.0001(5) 0.0015(6) -0.0013(6) C27 0.0390(9) 0.0405(9) 0.0455(10) -0.0025(8) -0.0002(7) -0.0029(7) C28 0.0485(11) 0.0586(12) 0.0551(12) 0.0023(10) -0.0065(9) -0.0162(9) C29 0.0815(15) 0.0421(10) 0.0423(10) -0.0035(8) -0.0081(10) -0.0235(10) C30 0.0830(15) 0.0308(8) 0.0345(9) -0.0045(7) 0.0063(9) -0.0044(9) C31 0.0544(10) 0.0307(7) 0.0291(7) -0.0010(6) 0.0045(7) 0.0023(7) C32 0.0749(16) 0.0593(13) 0.0675(15) -0.0010(12) 0.0380(14) -0.0183(12) C33 0.094(2) 0.0770(18) 0.0584(15) -0.0194(13) 0.0452(16) -0.0109(16) C34 0.0372(11) 0.104(2) 0.103(2) -0.001(2) 0.0253(13) 0.0012(13) C35 0.0540(11) 0.0473(10) 0.0411(10) -0.0013(8) -0.0039(9) -0.0111(9) C36 0.0756(16) 0.0441(10) 0.0434(11) 0.0099(9) -0.0057(11) -0.0098(10) C37 0.0376(10) 0.0736(16) 0.0760(17) -0.0072(14) -0.0018(11) 0.0121(10) N1 0.0326(6) 0.0288(6) 0.0314(6) -0.0024(5) 0.0043(5) 0.0028(5) N2 0.0338(6) 0.0369(7) 0.0314(6) -0.0007(5) 0.0086(5) 0.0025(5) Si1 0.0355(2) 0.0346(2) 0.0361(2) 0.00131(18) -0.00225(18) -0.00046(17) Si2 0.0438(3) 0.0527(3) 0.0459(3) -0.0075(2) 0.0225(2) -0.0050(2) P1 0.02917(17) 0.02293(16) 0.02636(17) -0.00176(13) 0.00562(14) -0.00016(13) P2 0.03067(18) 0.02493(16) 0.02587(17) -0.00131(13) 0.00477(14) 0.00076(13) Zn1 0.03682(11) 0.02928(10) 0.03745(11) -0.00540(7) 0.00308(8) 0.00754(7) _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 C1 P2 1.7164(16) . ? C1 P1 1.7277(16) . ? C2 C7 1.388(3) . ? C2 C3 1.401(4) . ? C2 Zn1 1.9653(18) . ? C3 C4 1.398(3) . ? C4 C5 1.349(7) . ? C5 C6 1.366(7) . ? C6 C7 1.411(5) . ? C8 C13 1.393(2) . ? C8 C9 1.398(2) . ? C8 P1 1.8184(16) . ? C9 C10 1.385(3) . ? C10 C11 1.384(3) . ? C11 C12 1.385(3) . ? C12 C13 1.386(2) . ? C14 C15 1.393(2) . ? C14 C19 1.400(2) . ? C14 P1 1.8229(15) . ? C15 C16 1.390(2) . ? C16 C17 1.383(3) . ? C17 C18 1.381(3) . ? C18 C19 1.387(2) . ? C20 C21 1.386(2) . ? C20 C25 1.397(2) . ? C20 P2 1.8188(16) . ? C21 C22 1.388(3) . ? C22 C23 1.383(3) . ? C23 C24 1.375(3) . ? C24 C25 1.388(3) . ? C26 C27 1.387(2) . ? C26 C31 1.394(2) . ? C26 P2 1.8161(16) . ? C27 C28 1.388(3) . ? C28 C29 1.378(4) . ? C29 C30 1.374(4) . ? C30 C31 1.388(3) . ? C32 Si2 1.866(3) . ? C33 Si2 1.871(3) . ? C34 Si2 1.866(3) . ? C35 Si1 1.868(2) . ? C36 Si1 1.871(2) . ? C37 Si1 1.867(3) . ? N1 P1 1.6144(13) . ? N1 Si1 1.7308(15) . ? N1 Zn1 1.9853(13) . ? N2 P2 1.6044(14) . ? N2 Si2 1.7211(15) . ? N2 Zn1 2.0298(14) . ? P1 Zn1 2.9224(6) . ? P2 Zn1 2.9028(8) . ? 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 P2 C1 P1 124.90(9) . . ? C7 C2 C3 115.5(2) . . ? C7 C2 Zn1 123.3(2) . . ? C3 C2 Zn1 121.06(17) . . ? C4 C3 C2 122.3(3) . . ? C5 C4 C3 120.5(4) . . ? C4 C5 C6 119.7(3) . . ? C5 C6 C7 120.3(4) . . ? C2 C7 C6 121.7(4) . . ? C13 C8 C9 118.64(15) . . ? C13 C8 P1 123.16(12) . . ? C9 C8 P1 118.06(12) . . ? C10 C9 C8 120.70(17) . . ? C11 C10 C9 119.97(17) . . ? C10 C11 C12 119.97(17) . . ? C11 C12 C13 120.14(17) . . ? C12 C13 C8 120.56(16) . . ? C15 C14 C19 118.98(14) . . ? C15 C14 P1 119.53(12) . . ? C19 C14 P1 121.09(12) . . ? C16 C15 C14 120.63(17) . . ? C17 C16 C15 119.66(18) . . ? C18 C17 C16 120.42(16) . . ? C17 C18 C19 120.23(17) . . ? C18 C19 C14 120.07(16) . . ? C21 C20 C25 118.90(16) . . ? C21 C20 P2 119.90(13) . . ? C25 C20 P2 121.13(13) . . ? C20 C21 C22 120.59(18) . . ? C23 C22 C21 120.04(19) . . ? C24 C23 C22 119.91(18) . . ? C23 C24 C25 120.43(19) . . ? C24 C25 C20 120.12(18) . . ? C27 C26 C31 119.10(16) . . ? C27 C26 P2 121.34(13) . . ? C31 C26 P2 119.43(13) . . ? C26 C27 C28 120.40(19) . . ? C29 C28 C27 119.9(2) . . ? C30 C29 C28 120.29(18) . . ? C29 C30 C31 120.22(19) . . ? C30 C31 C26 120.05(19) . . ? P1 N1 Si1 129.93(8) . . ? P1 N1 Zn1 108.11(7) . . ? Si1 N1 Zn1 121.10(7) . . ? P2 N2 Si2 133.24(9) . . ? P2 N2 Zn1 105.42(7) . . ? Si2 N2 Zn1 121.33(8) . . ? N1 Si1 C37 107.19(11) . . ? N1 Si1 C35 113.12(9) . . ? C37 Si1 C35 109.29(12) . . ? N1 Si1 C36 112.22(9) . . ? C37 Si1 C36 108.22(14) . . ? C35 Si1 C36 106.69(11) . . ? N2 Si2 C32 114.21(9) . . ? N2 Si2 C34 104.94(12) . . ? C32 Si2 C34 107.94(16) . . ? N2 Si2 C33 111.89(11) . . ? C32 Si2 C33 108.19(15) . . ? C34 Si2 C33 109.51(17) . . ? N1 P1 C1 112.55(7) . . ? N1 P1 C8 111.07(7) . . ? C1 P1 C8 104.65(7) . . ? N1 P1 C14 109.13(7) . . ? C1 P1 C14 112.23(7) . . ? C8 P1 C14 107.02(7) . . ? N1 P1 Zn1 40.22(5) . . ? C1 P1 Zn1 72.84(5) . . ? C8 P1 Zn1 129.31(5) . . ? C14 P1 Zn1 120.97(5) . . ? N2 P2 C1 108.90(8) . . ? N2 P2 C26 112.08(8) . . ? C1 P2 C26 105.75(7) . . ? N2 P2 C20 111.18(8) . . ? C1 P2 C20 116.09(7) . . ? C26 P2 C20 102.63(8) . . ? N2 P2 Zn1 42.38(5) . . ? C1 P2 Zn1 73.52(6) . . ? C26 P2 Zn1 100.83(6) . . ? C20 P2 Zn1 150.60(5) . . ? C2 Zn1 N1 129.48(8) . . ? C2 Zn1 N2 125.97(8) . . ? N1 Zn1 N2 104.52(6) . . ? C2 Zn1 P2 127.42(6) . . ? N1 Zn1 P2 93.82(4) . . ? N2 Zn1 P2 32.19(4) . . ? C2 Zn1 P1 144.85(7) . . ? N1 Zn1 P1 31.67(4) . . ? N2 Zn1 P1 81.74(4) . . ? P2 Zn1 P1 63.229(18) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.93 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.354 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.048 #============================================================================== data_4 _database_code_depnum_ccdc_archive 'CCDC 770407' #TrackingRef '- deposit.CIF' _audit_creation_date 09-08-12 _audit_creation_method 'STOE X-RED' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H58 N4 P2 Si2 Zn' _chemical_formula_sum 'C52 H58 N4 P2 Si2 Zn' _chemical_formula_weight 922.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 'P 21/c' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2ybc' 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 11.032(2) _cell_length_b 19.711(4) _cell_length_c 22.993(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.71(3) _cell_angle_gamma 90.00 _cell_volume 4895.9(17) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 21152 _cell_measurement_theta_min 1.37 _cell_measurement_theta_max 27.21 _exptl_crystal_description plates _exptl_crystal_colour colorless _exptl_crystal_size_max 0.236 _exptl_crystal_size_mid 0.146 _exptl_crystal_size_min 0.093 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.252 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 0.655 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8796 _exptl_absorpt_correction_T_max 0.9423 _exptl_absorpt_process_details 'STOE X-RED & X-SHAPE' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37500 _diffrn_reflns_av_R_equivalents 0.0725 _diffrn_reflns_av_sigmaI/netI 0.0638 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 26.75 _reflns_number_total 10377 _reflns_number_gt 7335 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA, PLATON (A.L.Spek, 2005)' _computing_data_reduction 'STOE X-RED, PLATON (A.L.Spek, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e/3' _computing_publication_material 'X-STEP32, Microsoft Word' _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^)+(0.0476P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10377 _refine_ls_number_parameters 558 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0854 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1043 _refine_ls_wR_factor_gt 0.0945 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4162(2) 0.71372(14) 0.55847(11) 0.0283(5) Uani 1 1 d . . . H1 H 0.4731 0.6894 0.5913 0.034 Uiso 1 1 calc R . . C2 C 0.1100(3) 0.82389(17) 0.39655(13) 0.0375(7) Uani 1 1 d . . . C3 C 0.0049(3) 0.7818(2) 0.37910(15) 0.0478(8) Uani 1 1 d . . . H3 H 0.0041 0.7388 0.3977 0.057 Uiso 1 1 calc R . . C4 C -0.0963(3) 0.8003(3) 0.33640(18) 0.0700(13) Uani 1 1 d . . . H4 H -0.1633 0.7695 0.3251 0.084 Uiso 1 1 calc R . . C5 C -0.1004(4) 0.8623(3) 0.31053(18) 0.0781(15) Uani 1 1 d . . . H5 H -0.1707 0.8752 0.2815 0.094 Uiso 1 1 calc R . . C6 C -0.0031(5) 0.9061(3) 0.32625(18) 0.0742(14) Uani 1 1 d . . . H6 H -0.0059 0.9499 0.3087 0.089 Uiso 1 1 calc R . . C7 C 0.1020(4) 0.8857(2) 0.36904(16) 0.0548(9) Uani 1 1 d . . . H7 H 0.1696 0.9162 0.3790 0.066 Uiso 1 1 calc R . . C8 C 0.3406(2) 0.65840(14) 0.52028(12) 0.0287(6) Uani 1 1 d . . . C9 C 0.1850(2) 0.63958(14) 0.43268(12) 0.0304(6) Uani 1 1 d . . . C10 C 0.1182(3) 0.58635(15) 0.45055(14) 0.0363(7) Uani 1 1 d . . . H10 H 0.1304 0.5750 0.4915 0.044 Uiso 1 1 calc R . . C11 C 0.0334(3) 0.54937(16) 0.40918(15) 0.0418(7) Uani 1 1 d . . . H11 H -0.0116 0.5134 0.4224 0.050 Uiso 1 1 calc R . . C12 C 0.0139(3) 0.56442(16) 0.34898(15) 0.0439(8) Uani 1 1 d . . . C13 C -0.0830(4) 0.5263(2) 0.30439(17) 0.0612(11) Uani 1 1 d . . . H13A H -0.1461 0.5583 0.2845 0.092 Uiso 1 1 calc R . . H13B H -0.1220 0.4918 0.3251 0.092 Uiso 1 1 calc R . . H13C H -0.0434 0.5044 0.2748 0.092 Uiso 1 1 calc R . . C14 C 0.0840(3) 0.61495(18) 0.33119(15) 0.0473(8) Uani 1 1 d . . . H14 H 0.0742 0.6247 0.2900 0.057 Uiso 1 1 calc R . . C15 C 0.1693(3) 0.65235(16) 0.37197(13) 0.0395(7) Uani 1 1 d . . . H15 H 0.2170 0.6867 0.3583 0.047 Uiso 1 1 calc R . . C16 C 0.4452(3) 0.57292(14) 0.58170(13) 0.0366(7) Uani 1 1 d . . . C17 C 0.5592(3) 0.54691(17) 0.57491(15) 0.0438(8) Uani 1 1 d . . . H17 H 0.5792 0.5458 0.5366 0.053 Uiso 1 1 calc R . . C18 C 0.6439(3) 0.52266(18) 0.62375(16) 0.0480(8) Uani 1 1 d . . . H18 H 0.7213 0.5054 0.6183 0.058 Uiso 1 1 calc R . . C19 C 0.6174(3) 0.52316(17) 0.68012(15) 0.0463(8) Uani 1 1 d . . . C20 C 0.7071(4) 0.4932(2) 0.73282(17) 0.0653(11) Uani 1 1 d . . . H20A H 0.6952 0.4440 0.7338 0.098 Uiso 1 1 calc R . . H20B H 0.6917 0.5133 0.7696 0.098 Uiso 1 1 calc R . . H20C H 0.7923 0.5030 0.7291 0.098 Uiso 1 1 calc R . . C21 C 0.5040(3) 0.54868(17) 0.68661(15) 0.0490(8) Uani 1 1 d . . . H21 H 0.4843 0.5498 0.7250 0.059 Uiso 1 1 calc R . . C22 C 0.4181(3) 0.57280(16) 0.63807(14) 0.0446(8) Uani 1 1 d . . . H22 H 0.3404 0.5893 0.6436 0.054 Uiso 1 1 calc R . . C23 C 0.5996(3) 0.69346(15) 0.48283(12) 0.0335(6) Uani 1 1 d . . . C24 C 0.5321(3) 0.65372(16) 0.43711(13) 0.0360(7) Uani 1 1 d . . . H24 H 0.4448 0.6587 0.4263 0.043 Uiso 1 1 calc R . . C25 C 0.5910(3) 0.60752(17) 0.40771(14) 0.0442(8) Uani 1 1 d . . . H25 H 0.5440 0.5799 0.3775 0.053 Uiso 1 1 calc R . . C26 C 0.7180(3) 0.6010(2) 0.42183(16) 0.0570(10) Uani 1 1 d . . . H26 H 0.7584 0.5690 0.4015 0.068 Uiso 1 1 calc R . . C27 C 0.7862(3) 0.6414(2) 0.46578(17) 0.0660(12) Uani 1 1 d . . . H27 H 0.8739 0.6376 0.4749 0.079 Uiso 1 1 calc R . . C28 C 0.7281(3) 0.6873(2) 0.49653(15) 0.0515(9) Uani 1 1 d . . . H28 H 0.7757 0.7146 0.5269 0.062 Uiso 1 1 calc R . . C29 C 0.6345(2) 0.79994(16) 0.57093(12) 0.0345(7) Uani 1 1 d . . . C30 C 0.6550(3) 0.86891(17) 0.56676(15) 0.0421(7) Uani 1 1 d . . . H30 H 0.6063 0.8945 0.5355 0.051 Uiso 1 1 calc R . . C31 C 0.7467(3) 0.9008(2) 0.60816(17) 0.0543(9) Uani 1 1 d . . . H31 H 0.7610 0.9481 0.6050 0.065 Uiso 1 1 calc R . . C32 C 0.8164(3) 0.8641(2) 0.65353(16) 0.0581(10) Uani 1 1 d . . . H32 H 0.8794 0.8861 0.6815 0.070 Uiso 1 1 calc R . . C33 C 0.7962(3) 0.7960(2) 0.65886(15) 0.0533(9) Uani 1 1 d . . . H33 H 0.8444 0.7712 0.6908 0.064 Uiso 1 1 calc R . . C34 C 0.7049(3) 0.76294(19) 0.61758(14) 0.0433(7) Uani 1 1 d . . . H34 H 0.6909 0.7157 0.6212 0.052 Uiso 1 1 calc R . . C35 C 0.4294(3) 0.80396(17) 0.65772(12) 0.0380(7) Uani 1 1 d . . . C36 C 0.4555(3) 0.87277(19) 0.66036(16) 0.0494(9) Uani 1 1 d . . . H36 H 0.4161 0.9023 0.6296 0.059 Uiso 1 1 calc R . . C37 C 0.5406(4) 0.8981(3) 0.7089(2) 0.0742(14) Uani 1 1 d . . . H37 H 0.5597 0.9451 0.7108 0.089 Uiso 1 1 calc R . . C38 C 0.5965(4) 0.8562(4) 0.75342(18) 0.0872(18) Uani 1 1 d . . . H38 H 0.6527 0.8745 0.7866 0.105 Uiso 1 1 calc R . . C39 C 0.5721(3) 0.7881(3) 0.75072(16) 0.0772(15) Uani 1 1 d . . . H39 H 0.6120 0.7593 0.7819 0.093 Uiso 1 1 calc R . . C40 C 0.4895(3) 0.7607(2) 0.70267(14) 0.0529(9) Uani 1 1 d . . . H40 H 0.4741 0.7133 0.7004 0.063 Uiso 1 1 calc R . . C41 C 0.2125(2) 0.71890(15) 0.62663(12) 0.0318(6) Uani 1 1 d . . . C42 C 0.2082(3) 0.72008(18) 0.68718(13) 0.0446(8) Uani 1 1 d . . . H42 H 0.2710 0.7433 0.7143 0.054 Uiso 1 1 calc R . . C43 C 0.1140(3) 0.6880(2) 0.70783(15) 0.0548(9) Uani 1 1 d . . . H43 H 0.1117 0.6897 0.7489 0.066 Uiso 1 1 calc R . . C44 C 0.0230(3) 0.65339(19) 0.66897(16) 0.0495(8) Uani 1 1 d . . . H44 H -0.0410 0.6307 0.6834 0.059 Uiso 1 1 calc R . . C45 C 0.0250(3) 0.65184(17) 0.60925(15) 0.0441(8) Uani 1 1 d . . . H45 H -0.0379 0.6282 0.5826 0.053 Uiso 1 1 calc R . . C46 C 0.1180(3) 0.68438(16) 0.58790(13) 0.0366(7) Uani 1 1 d . . . H46 H 0.1179 0.6834 0.5466 0.044 Uiso 1 1 calc R . . C47 C -0.0197(3) 0.8522(2) 0.52263(16) 0.0509(9) Uani 1 1 d . . . H47A H -0.0246 0.8464 0.4799 0.076 Uiso 1 1 calc R . . H47B H -0.0807 0.8859 0.5292 0.076 Uiso 1 1 calc R . . H47C H -0.0370 0.8088 0.5401 0.076 Uiso 1 1 calc R . . C48 C 0.1754(4) 0.96236(19) 0.5251(2) 0.0684(12) Uani 1 1 d . . . H48A H 0.2586 0.9770 0.5446 0.103 Uiso 1 1 calc R . . H48B H 0.1150 0.9970 0.5306 0.103 Uiso 1 1 calc R . . H48C H 0.1724 0.9559 0.4825 0.103 Uiso 1 1 calc R . . C49 C 0.1349(3) 0.8965(2) 0.63805(16) 0.0595(10) Uani 1 1 d . . . H49A H 0.1104 0.8548 0.6557 0.089 Uiso 1 1 calc R . . H49B H 0.0754 0.9326 0.6412 0.089 Uiso 1 1 calc R . . H49C H 0.2176 0.9102 0.6592 0.089 Uiso 1 1 calc R . . C50 C 0.3978(3) 0.8185(2) 0.33740(15) 0.0564(9) Uani 1 1 d . . . H50A H 0.4191 0.7710 0.3321 0.085 Uiso 1 1 calc R . . H50B H 0.4189 0.8458 0.3052 0.085 Uiso 1 1 calc R . . H50C H 0.3089 0.8223 0.3366 0.085 Uiso 1 1 calc R . . C51 C 0.6543(3) 0.8403(2) 0.40950(18) 0.0631(11) Uani 1 1 d . . . H51A H 0.7035 0.8542 0.4481 0.095 Uiso 1 1 calc R . . H51B H 0.6756 0.8689 0.3782 0.095 Uiso 1 1 calc R . . H51C H 0.6721 0.7928 0.4019 0.095 Uiso 1 1 calc R . . C52 C 0.4531(4) 0.94175(19) 0.41760(19) 0.0639(11) Uani 1 1 d . . . H52A H 0.3733 0.9469 0.4296 0.096 Uiso 1 1 calc R . . H52B H 0.4498 0.9645 0.3794 0.096 Uiso 1 1 calc R . . H52C H 0.5185 0.9622 0.4477 0.096 Uiso 1 1 calc R . . N1 N 0.43908(19) 0.80663(12) 0.46706(10) 0.0307(5) Uani 1 1 d . . . N2 N 0.2496(2) 0.82226(12) 0.54830(10) 0.0304(5) Uani 1 1 d . . . N3 N 0.2609(2) 0.68503(12) 0.47278(9) 0.0292(5) Uani 1 1 d . . . N4 N 0.3580(2) 0.59495(12) 0.53163(11) 0.0380(6) Uani 1 1 d . . . Si1 Si 0.48650(8) 0.84994(5) 0.41010(4) 0.0402(2) Uani 1 1 d . . . Si2 Si 0.13773(7) 0.88129(4) 0.55813(4) 0.03574(19) Uani 1 1 d . . . P1 P 0.51719(6) 0.75827(4) 0.51550(3) 0.02878(16) Uani 1 1 d . . . P2 P 0.31991(6) 0.76975(4) 0.59471(3) 0.02833(16) Uani 1 1 d . . . Zn1 Zn 0.24833(3) 0.788985(17) 0.460252(14) 0.02929(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0264(12) 0.0317(14) 0.0243(12) 0.0048(12) -0.0012(10) 0.0049(11) C2 0.0351(15) 0.0495(18) 0.0263(14) -0.0008(13) 0.0028(12) 0.0164(13) C3 0.0348(15) 0.062(2) 0.0444(18) -0.0067(17) 0.0035(13) 0.0098(15) C4 0.0380(18) 0.110(4) 0.055(2) -0.016(3) -0.0055(16) 0.021(2) C5 0.056(3) 0.126(4) 0.048(2) 0.004(3) -0.0006(19) 0.041(3) C6 0.089(3) 0.089(3) 0.050(2) 0.034(2) 0.028(2) 0.051(3) C7 0.064(2) 0.058(2) 0.0438(19) 0.0144(17) 0.0129(17) 0.0197(18) C8 0.0282(13) 0.0328(15) 0.0237(13) -0.0006(11) 0.0019(10) 0.0035(11) C9 0.0285(13) 0.0300(14) 0.0308(14) -0.0052(12) 0.0015(11) 0.0056(11) C10 0.0351(15) 0.0371(16) 0.0347(16) -0.0022(13) 0.0020(12) 0.0033(12) C11 0.0343(15) 0.0383(17) 0.0503(19) -0.0060(15) 0.0031(14) 0.0002(13) C12 0.0405(17) 0.0389(18) 0.0469(19) -0.0140(15) -0.0039(14) 0.0080(14) C13 0.060(2) 0.056(2) 0.057(2) -0.0176(19) -0.0133(18) -0.0029(18) C14 0.0532(19) 0.050(2) 0.0328(16) -0.0065(15) -0.0053(14) 0.0059(16) C15 0.0407(16) 0.0416(17) 0.0328(15) -0.0003(13) -0.0007(13) 0.0007(13) C16 0.0433(16) 0.0266(15) 0.0349(16) 0.0043(12) -0.0037(13) 0.0035(12) C17 0.0411(17) 0.0462(18) 0.0407(17) 0.0060(15) 0.0006(14) 0.0079(14) C18 0.0378(17) 0.050(2) 0.052(2) 0.0089(16) -0.0008(15) 0.0073(14) C19 0.0502(19) 0.0393(18) 0.0423(18) 0.0064(15) -0.0078(15) 0.0047(15) C20 0.069(2) 0.066(2) 0.051(2) 0.013(2) -0.0127(19) 0.012(2) C21 0.068(2) 0.0426(19) 0.0335(16) 0.0067(15) 0.0040(15) 0.0093(16) C22 0.0528(19) 0.0381(17) 0.0409(18) 0.0053(14) 0.0046(15) 0.0162(14) C23 0.0326(14) 0.0380(16) 0.0287(14) -0.0013(12) 0.0035(11) 0.0050(12) C24 0.0308(14) 0.0445(17) 0.0329(15) -0.0027(13) 0.0066(12) 0.0009(12) C25 0.0492(18) 0.050(2) 0.0335(16) -0.0074(15) 0.0083(14) 0.0037(15) C26 0.052(2) 0.071(3) 0.046(2) -0.0166(18) 0.0042(16) 0.0266(18) C27 0.0376(18) 0.104(3) 0.052(2) -0.026(2) -0.0019(16) 0.0275(19) C28 0.0334(16) 0.073(2) 0.0451(18) -0.0219(18) 0.0000(14) 0.0139(15) C29 0.0246(12) 0.0462(18) 0.0320(14) -0.0068(13) 0.0040(11) 0.0021(12) C30 0.0370(16) 0.0464(19) 0.0435(18) -0.0088(15) 0.0094(13) -0.0057(13) C31 0.0489(19) 0.057(2) 0.060(2) -0.0227(19) 0.0189(17) -0.0155(17) C32 0.0373(18) 0.089(3) 0.048(2) -0.031(2) 0.0068(15) -0.0121(18) C33 0.0326(15) 0.086(3) 0.0382(17) -0.0101(19) -0.0016(13) 0.0055(17) C34 0.0331(15) 0.058(2) 0.0368(16) -0.0056(15) 0.0018(13) 0.0020(14) C35 0.0321(14) 0.059(2) 0.0241(13) -0.0067(13) 0.0072(11) -0.0029(13) C36 0.0411(17) 0.061(2) 0.0477(19) -0.0231(17) 0.0122(15) -0.0094(16) C37 0.059(2) 0.101(4) 0.067(3) -0.051(3) 0.024(2) -0.034(2) C38 0.051(2) 0.176(6) 0.036(2) -0.041(3) 0.0125(18) -0.045(3) C39 0.0397(18) 0.159(5) 0.0298(17) 0.005(2) -0.0011(14) -0.023(3) C40 0.0340(16) 0.087(3) 0.0337(17) 0.0072(18) -0.0018(13) -0.0067(17) C41 0.0299(13) 0.0346(15) 0.0303(14) 0.0044(12) 0.0048(11) 0.0059(11) C42 0.0366(15) 0.066(2) 0.0301(15) 0.0051(15) 0.0038(12) -0.0054(15) C43 0.0497(19) 0.081(3) 0.0354(17) 0.0121(18) 0.0118(15) -0.0009(18) C44 0.0403(17) 0.058(2) 0.051(2) 0.0180(17) 0.0122(15) -0.0025(15) C45 0.0382(16) 0.0436(18) 0.0486(19) 0.0041(15) 0.0044(14) -0.0056(14) C46 0.0365(15) 0.0409(16) 0.0317(15) -0.0004(13) 0.0049(12) 0.0007(12) C47 0.0350(16) 0.069(2) 0.047(2) -0.0116(18) 0.0055(14) 0.0103(16) C48 0.064(2) 0.041(2) 0.104(3) 0.004(2) 0.026(2) 0.0109(18) C49 0.0453(19) 0.080(3) 0.051(2) -0.028(2) 0.0056(16) 0.0122(18) C50 0.054(2) 0.082(3) 0.0344(17) 0.0039(18) 0.0117(15) 0.0041(19) C51 0.045(2) 0.094(3) 0.054(2) 0.009(2) 0.0190(17) -0.004(2) C52 0.074(3) 0.050(2) 0.068(3) 0.018(2) 0.015(2) -0.0024(19) N1 0.0248(11) 0.0359(13) 0.0311(12) 0.0021(10) 0.0046(9) 0.0026(9) N2 0.0323(11) 0.0340(12) 0.0237(11) -0.0018(10) 0.0029(9) 0.0042(10) N3 0.0294(11) 0.0307(12) 0.0240(11) 0.0013(9) -0.0024(9) 0.0036(9) N4 0.0372(13) 0.0336(13) 0.0372(14) 0.0018(11) -0.0065(11) 0.0075(11) Si1 0.0372(4) 0.0507(5) 0.0337(4) 0.0057(4) 0.0099(3) -0.0006(4) Si2 0.0322(4) 0.0349(4) 0.0393(4) -0.0060(4) 0.0054(3) 0.0053(3) P1 0.0237(3) 0.0343(4) 0.0267(3) -0.0026(3) 0.0014(3) 0.0027(3) P2 0.0274(3) 0.0344(4) 0.0217(3) -0.0014(3) 0.0015(3) 0.0020(3) Zn1 0.02763(15) 0.03276(17) 0.02528(15) 0.00284(14) 0.00015(11) 0.00499(13) _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 C1 C8 1.536(4) . ? C1 P2 1.844(3) . ? C1 P1 1.853(3) . ? C1 H1 1.0000 . ? C2 C7 1.367(5) . ? C2 C3 1.416(5) . ? C2 Zn1 2.010(3) . ? C3 C4 1.378(5) . ? C3 H3 0.9500 . ? C4 C5 1.356(7) . ? C4 H4 0.9500 . ? C5 C6 1.369(7) . ? C5 H5 0.9500 . ? C6 C7 1.418(5) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 N4 1.284(4) . ? C8 N3 1.361(3) . ? C9 C15 1.394(4) . ? C9 C10 1.392(4) . ? C9 N3 1.428(3) . ? C10 C11 1.396(4) . ? C10 H10 0.9500 . ? C11 C12 1.389(5) . ? C11 H11 0.9500 . ? C12 C14 1.373(5) . ? C12 C13 1.521(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.397(4) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C22 1.388(5) . ? C16 C17 1.396(4) . ? C16 N4 1.411(3) . ? C17 C18 1.392(4) . ? C17 H17 0.9500 . ? C18 C19 1.385(5) . ? C18 H18 0.9500 . ? C19 C21 1.384(5) . ? C19 C20 1.520(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.393(4) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C28 1.394(4) . ? C23 C24 1.399(4) . ? C23 P1 1.817(3) . ? C24 C25 1.374(4) . ? C24 H24 0.9500 . ? C25 C26 1.378(5) . ? C25 H25 0.9500 . ? C26 C27 1.383(5) . ? C26 H26 0.9500 . ? C27 C28 1.383(5) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.385(4) . ? C29 C34 1.396(4) . ? C29 P1 1.818(3) . ? C30 C31 1.391(4) . ? C30 H30 0.9500 . ? C31 C32 1.370(6) . ? C31 H31 0.9500 . ? C32 C33 1.371(6) . ? C32 H32 0.9500 . ? C33 C34 1.397(4) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C36 1.385(5) . ? C35 C40 1.399(5) . ? C35 P2 1.817(3) . ? C36 C37 1.396(5) . ? C36 H36 0.9500 . ? C37 C38 1.361(7) . ? C37 H37 0.9500 . ? C38 C39 1.368(8) . ? C38 H38 0.9500 . ? C39 C40 1.391(5) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C46 1.402(4) . ? C41 C42 1.403(4) . ? C41 P2 1.817(3) . ? C42 C43 1.381(5) . ? C42 H42 0.9500 . ? C43 C44 1.381(5) . ? C43 H43 0.9500 . ? C44 C45 1.378(5) . ? C44 H44 0.9500 . ? C45 C46 1.381(4) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 Si2 1.854(3) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 Si2 1.853(4) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 Si2 1.868(4) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 Si1 1.863(4) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 Si1 1.864(4) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 Si1 1.862(4) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? N1 P1 1.582(2) . ? N1 Si1 1.731(2) . ? N1 Zn1 2.107(2) . ? N2 P2 1.574(2) . ? N2 Si2 1.744(2) . ? N2 Zn1 2.126(2) . ? N3 Zn1 2.070(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C8 C1 P2 112.81(18) . . ? C8 C1 P1 110.31(18) . . ? P2 C1 P1 114.89(15) . . ? C8 C1 H1 106.0 . . ? P2 C1 H1 106.0 . . ? P1 C1 H1 106.0 . . ? C7 C2 C3 114.7(3) . . ? C7 C2 Zn1 127.6(3) . . ? C3 C2 Zn1 117.6(2) . . ? C4 C3 C2 123.1(4) . . ? C4 C3 H3 118.4 . . ? C2 C3 H3 118.4 . . ? C5 C4 C3 120.0(4) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.0(4) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C7 119.3(4) . . ? C5 C6 H6 120.3 . . ? C7 C6 H6 120.3 . . ? C2 C7 C6 122.8(4) . . ? C2 C7 H7 118.6 . . ? C6 C7 H7 118.6 . . ? N4 C8 N3 125.8(2) . . ? N4 C8 C1 122.3(2) . . ? N3 C8 C1 111.9(2) . . ? C15 C9 C10 117.8(3) . . ? C15 C9 N3 118.1(3) . . ? C10 C9 N3 124.0(3) . . ? C11 C10 C9 121.0(3) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C12 C11 C10 120.9(3) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C14 C12 C11 118.0(3) . . ? C14 C12 C13 121.2(3) . . ? C11 C12 C13 120.8(3) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 C15 121.8(3) . . ? C12 C14 H14 119.1 . . ? C15 C14 H14 119.1 . . ? C9 C15 C14 120.4(3) . . ? C9 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C22 C16 C17 118.2(3) . . ? C22 C16 N4 121.5(3) . . ? C17 C16 N4 120.1(3) . . ? C18 C17 C16 120.6(3) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C19 C18 C17 121.2(3) . . ? C19 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C21 C19 C18 118.1(3) . . ? C21 C19 C20 120.8(3) . . ? C18 C19 C20 121.1(3) . . ? 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 C22 121.4(3) . . ? C19 C21 H21 119.3 . . ? C22 C21 H21 119.3 . . ? C16 C22 C21 120.6(3) . . ? C16 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C28 C23 C24 118.9(3) . . ? C28 C23 P1 122.6(2) . . ? C24 C23 P1 118.0(2) . . ? C25 C24 C23 120.6(3) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 120.3(3) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C25 C26 C27 119.7(3) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C28 C27 C26 120.7(3) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C23 119.8(3) . . ? C27 C28 H28 120.1 . . ? C23 C28 H28 120.1 . . ? C30 C29 C34 119.5(3) . . ? C30 C29 P1 119.9(2) . . ? C34 C29 P1 120.6(2) . . ? C29 C30 C31 120.2(3) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C32 C31 C30 120.0(4) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C33 120.6(3) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C32 C33 C34 120.3(3) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C29 C34 C33 119.4(3) . . ? C29 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? C36 C35 C40 120.1(3) . . ? C36 C35 P2 119.8(2) . . ? C40 C35 P2 120.1(3) . . ? C35 C36 C37 119.0(4) . . ? C35 C36 H36 120.5 . . ? C37 C36 H36 120.5 . . ? C38 C37 C36 120.9(5) . . ? C38 C37 H37 119.5 . . ? C36 C37 H37 119.5 . . ? C37 C38 C39 120.3(4) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C38 C39 C40 120.5(4) . . ? C38 C39 H39 119.7 . . ? C40 C39 H39 119.7 . . ? C39 C40 C35 119.1(4) . . ? C39 C40 H40 120.5 . . ? C35 C40 H40 120.5 . . ? C46 C41 C42 117.9(3) . . ? C46 C41 P2 118.2(2) . . ? C42 C41 P2 123.2(2) . . ? C43 C42 C41 120.9(3) . . ? C43 C42 H42 119.6 . . ? C41 C42 H42 119.6 . . ? C44 C43 C42 120.2(3) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C43 C44 C45 119.9(3) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C46 C45 C44 120.5(3) . . ? C46 C45 H45 119.8 . . ? C44 C45 H45 119.8 . . ? C45 C46 C41 120.6(3) . . ? C45 C46 H46 119.7 . . ? C41 C46 H46 119.7 . . ? 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 . . ? Si1 C50 H50A 109.5 . . ? Si1 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? Si1 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? Si1 C51 H51A 109.5 . . ? Si1 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? Si1 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? Si1 C52 H52A 109.5 . . ? Si1 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? Si1 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? P1 N1 Si1 128.67(14) . . ? P1 N1 Zn1 110.24(13) . . ? Si1 N1 Zn1 118.41(12) . . ? P2 N2 Si2 127.99(15) . . ? P2 N2 Zn1 110.49(12) . . ? Si2 N2 Zn1 117.47(12) . . ? C8 N3 C9 118.3(2) . . ? C8 N3 Zn1 120.50(18) . . ? C9 N3 Zn1 121.15(16) . . ? C8 N4 C16 121.0(2) . . ? N1 Si1 C50 109.32(15) . . ? N1 Si1 C52 108.25(16) . . ? C50 Si1 C52 109.16(19) . . ? N1 Si1 C51 114.11(15) . . ? C50 Si1 C51 107.52(18) . . ? C52 Si1 C51 108.4(2) . . ? N2 Si2 C48 107.39(16) . . ? N2 Si2 C47 111.13(14) . . ? C48 Si2 C47 110.76(19) . . ? N2 Si2 C49 112.83(14) . . ? C48 Si2 C49 108.4(2) . . ? C47 Si2 C49 106.37(17) . . ? N1 P1 C23 112.30(13) . . ? N1 P1 C29 115.46(14) . . ? C23 P1 C29 105.24(13) . . ? N1 P1 C1 111.12(12) . . ? C23 P1 C1 107.02(14) . . ? C29 P1 C1 105.05(13) . . ? N2 P2 C35 116.94(14) . . ? N2 P2 C41 111.38(13) . . ? C35 P2 C41 105.38(13) . . ? N2 P2 C1 109.71(12) . . ? C35 P2 C1 103.41(13) . . ? C41 P2 C1 109.57(13) . . ? C2 Zn1 N3 117.37(11) . . ? C2 Zn1 N1 126.63(12) . . ? N3 Zn1 N1 96.64(9) . . ? C2 Zn1 N2 116.47(10) . . ? N3 Zn1 N2 100.69(9) . . ? N1 Zn1 N2 93.72(9) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.75 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.299 _refine_diff_density_min -0.438 _refine_diff_density_rms 0.053 #============================================================================== data_5 _database_code_depnum_ccdc_archive 'CCDC 770408' #TrackingRef '- deposit.CIF' _audit_creation_date 09-09-15 _audit_creation_method 'STOE X-RED' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C51 H54 N2 O P2 Si2 Zn, C4 H8 O' _chemical_formula_sum 'C55 H62 N2 O2 P2 Si2 Zn' _chemical_formula_weight 966.56 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' P P 0.1023 0.0942 '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 ' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 10.987(2) _cell_length_b 21.913(4) _cell_length_c 21.031(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.72(3) _cell_angle_gamma 90.00 _cell_volume 5004.9(17) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 41234 _cell_measurement_theta_min 1.35 _cell_measurement_theta_max 27.28 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.748 _exptl_crystal_size_mid 0.384 _exptl_crystal_size_min 0.082 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.283 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2040 _exptl_absorpt_coefficient_mu 0.645 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 'STOE IPDS 2' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49953 _diffrn_reflns_av_R_equivalents 0.1287 _diffrn_reflns_av_sigmaI/netI 0.0720 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 26.76 _reflns_number_total 10625 _reflns_number_gt 8245 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA, PLATON (A.L.Spek, 2005)' _computing_data_reduction 'STOE X-RED, PLATON (A.L.Spek, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e/3' _computing_publication_material 'X-STEP32, Microsoft Word' _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^)+(0.0834P)^2^+1.8342P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10625 _refine_ls_number_parameters 558 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0771 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_ref 0.1661 _refine_ls_wR_factor_gt 0.1547 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.006 _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 C1 C 0.1525(3) 0.24179(13) 0.49323(13) 0.0392(6) Uani 1 1 d . . . H1 H 0.1266 0.2059 0.5165 0.047 Uiso 1 1 calc R . . C2 C 0.2987(3) 0.27545(14) 0.61555(14) 0.0414(6) Uani 1 1 d . . . C3 C 0.2756(3) 0.25763(16) 0.67601(14) 0.0479(7) Uani 1 1 d . . . H3 H 0.1952 0.2599 0.6860 0.057 Uiso 1 1 calc R . . C4 C 0.3705(4) 0.23654(19) 0.72165(17) 0.0599(9) Uani 1 1 d . . . H4 H 0.3541 0.2242 0.7623 0.072 Uiso 1 1 calc R . . C5 C 0.4885(4) 0.23361(19) 0.70770(18) 0.0639(10) Uani 1 1 d . . . H5 H 0.5523 0.2191 0.7388 0.077 Uiso 1 1 calc R . . C6 C 0.5141(3) 0.25195(19) 0.64797(19) 0.0616(9) Uani 1 1 d . . . H6 H 0.5951 0.2504 0.6387 0.074 Uiso 1 1 calc R . . C7 C 0.4195(3) 0.27256(16) 0.60220(16) 0.0495(7) Uani 1 1 d . . . H7 H 0.4364 0.2848 0.5616 0.059 Uiso 1 1 calc R . . C8 C 0.0429(3) 0.31498(14) 0.58618(13) 0.0395(6) Uani 1 1 d . . . C9 C -0.0109(3) 0.37265(16) 0.58380(15) 0.0466(7) Uani 1 1 d . . . H9 H 0.0256 0.4054 0.5648 0.056 Uiso 1 1 calc R . . C10 C -0.1189(3) 0.38168(19) 0.60959(17) 0.0569(9) Uani 1 1 d . . . H10 H -0.1552 0.4206 0.6082 0.068 Uiso 1 1 calc R . . C11 C -0.1725(3) 0.33385(19) 0.63711(17) 0.0573(9) Uani 1 1 d . . . H11 H -0.2447 0.3404 0.6550 0.069 Uiso 1 1 calc R . . C12 C -0.1215(3) 0.27620(18) 0.63874(15) 0.0527(8) Uani 1 1 d . . . H12 H -0.1597 0.2436 0.6570 0.063 Uiso 1 1 calc R . . C13 C -0.0142(3) 0.26664(15) 0.61339(14) 0.0446(7) Uani 1 1 d . . . H13 H 0.0206 0.2274 0.6145 0.053 Uiso 1 1 calc R . . C14 C -0.1157(3) 0.25513(17) 0.45674(14) 0.0484(7) Uani 1 1 d . . . C15 C -0.1875(3) 0.3072(2) 0.45351(16) 0.0591(9) Uani 1 1 d . . . H15 H -0.1571 0.3440 0.4392 0.071 Uiso 1 1 calc R . . C16 C -0.3039(4) 0.3055(3) 0.4711(2) 0.0781(14) Uani 1 1 d . . . H16 H -0.3516 0.3413 0.4693 0.094 Uiso 1 1 calc R . . C17 C -0.3491(4) 0.2525(3) 0.4910(2) 0.0866(16) Uani 1 1 d . . . H17 H -0.4302 0.2510 0.5002 0.104 Uiso 1 1 calc R . . C18 C -0.2764(4) 0.2006(3) 0.4979(2) 0.0784(14) Uani 1 1 d . . . H18 H -0.3072 0.1646 0.5137 0.094 Uiso 1 1 calc R . . C19 C -0.1582(4) 0.2013(2) 0.48153(17) 0.0600(9) Uani 1 1 d . . . H19 H -0.1081 0.1664 0.4871 0.072 Uiso 1 1 calc R . . C20 C 0.0254(3) 0.19389(15) 0.36912(14) 0.0442(7) Uani 1 1 d . . . C21 C -0.0749(3) 0.15562(17) 0.35317(16) 0.0545(8) Uani 1 1 d . . . H21 H -0.1442 0.1594 0.3742 0.065 Uiso 1 1 calc R . . C22 C -0.0725(4) 0.11144(19) 0.30583(18) 0.0654(10) Uani 1 1 d . . . H22 H -0.1405 0.0854 0.2953 0.079 Uiso 1 1 calc R . . C23 C 0.0270(4) 0.10510(17) 0.27434(17) 0.0633(10) Uani 1 1 d . . . H23 H 0.0273 0.0748 0.2427 0.076 Uiso 1 1 calc R . . C24 C 0.1271(4) 0.14346(17) 0.28917(16) 0.0590(9) Uani 1 1 d . . . H24 H 0.1959 0.1392 0.2679 0.071 Uiso 1 1 calc R . . C25 C 0.1256(3) 0.18836(16) 0.33563(15) 0.0496(7) Uani 1 1 d . . . H25 H 0.1926 0.2153 0.3447 0.060 Uiso 1 1 calc R . . C26 C -0.1750(4) 0.3120(2) 0.29343(18) 0.0661(10) Uani 1 1 d . . . H26A H -0.1592 0.2693 0.2859 0.099 Uiso 1 1 calc R . . H26B H -0.2134 0.3308 0.2536 0.099 Uiso 1 1 calc R . . H26C H -0.2296 0.3155 0.3255 0.099 Uiso 1 1 calc R . . C27 C 0.0681(4) 0.34615(19) 0.25693(17) 0.0623(10) Uani 1 1 d . . . H27A H 0.1465 0.3664 0.2698 0.093 Uiso 1 1 calc R . . H27B H 0.0248 0.3656 0.2186 0.093 Uiso 1 1 calc R . . H27C H 0.0823 0.3035 0.2479 0.093 Uiso 1 1 calc R . . C28 C -0.0603(4) 0.43366(19) 0.3405(2) 0.0705(11) Uani 1 1 d . . . H28A H -0.1241 0.4353 0.3677 0.106 Uiso 1 1 calc R . . H28B H -0.0882 0.4549 0.3004 0.106 Uiso 1 1 calc R . . H28C H 0.0137 0.4531 0.3624 0.106 Uiso 1 1 calc R . . C29 C 0.2289(4) 0.49631(17) 0.51737(19) 0.0654(10) Uani 1 1 d . . . H29A H 0.2372 0.4957 0.4721 0.098 Uiso 1 1 calc R . . H29B H 0.2686 0.5325 0.5374 0.098 Uiso 1 1 calc R . . H29C H 0.1423 0.4967 0.5218 0.098 Uiso 1 1 calc R . . C30 C 0.4685(4) 0.42765(19) 0.54780(19) 0.0629(10) Uani 1 1 d . . . H30A H 0.5096 0.3929 0.5702 0.094 Uiso 1 1 calc R . . H30B H 0.5065 0.4651 0.5657 0.094 Uiso 1 1 calc R . . H30C H 0.4757 0.4252 0.5025 0.094 Uiso 1 1 calc R . . C31 C 0.2900(4) 0.42969(18) 0.64501(16) 0.0585(9) Uani 1 1 d . . . H31A H 0.2045 0.4246 0.6505 0.088 Uiso 1 1 calc R . . H31B H 0.3199 0.4687 0.6628 0.088 Uiso 1 1 calc R . . H31C H 0.3389 0.3971 0.6672 0.088 Uiso 1 1 calc R . . C32 C 0.3230(3) 0.40532(15) 0.36878(14) 0.0441(7) Uani 1 1 d . . . C33 C 0.2821(4) 0.46120(16) 0.34197(16) 0.0554(8) Uani 1 1 d . . . H33 H 0.2074 0.4771 0.3514 0.066 Uiso 1 1 calc R . . C34 C 0.3470(4) 0.49437(19) 0.30191(18) 0.0655(10) Uani 1 1 d . . . H34 H 0.3160 0.5320 0.2852 0.079 Uiso 1 1 calc R . . C35 C 0.4556(4) 0.4726(2) 0.28658(18) 0.0669(11) Uani 1 1 d . . . H35 H 0.4989 0.4947 0.2589 0.080 Uiso 1 1 calc R . . C36 C 0.5005(4) 0.4178(2) 0.31247(19) 0.0654(10) Uani 1 1 d . . . H36 H 0.5757 0.4026 0.3030 0.078 Uiso 1 1 calc R . . C37 C 0.4349(3) 0.38475(18) 0.35262(16) 0.0542(8) Uani 1 1 d . . . H37 H 0.4669 0.3473 0.3694 0.065 Uiso 1 1 calc R . . C38 C 0.2710(3) 0.22386(14) 0.46603(13) 0.0411(6) Uani 1 1 d . . . C39 C 0.3175(3) 0.16579(14) 0.47470(14) 0.0422(6) Uani 1 1 d . . . C40 C 0.2665(3) 0.12374(14) 0.52053(15) 0.0444(7) Uani 1 1 d . . . C41 C 0.3202(4) 0.12106(17) 0.58508(17) 0.0565(8) Uani 1 1 d . . . H41 H 0.3907 0.1447 0.5989 0.068 Uiso 1 1 calc R . . C42 C 0.2729(4) 0.08481(19) 0.62933(19) 0.0677(11) Uani 1 1 d . . . H42 H 0.3116 0.0838 0.6723 0.081 Uiso 1 1 calc R . . C43 C 0.1721(5) 0.0511(2) 0.6111(2) 0.0820(13) Uani 1 1 d . . . H43 H 0.1405 0.0261 0.6410 0.098 Uiso 1 1 calc R . . C44 C 0.1156(5) 0.0533(3) 0.5489(3) 0.0922(16) Uani 1 1 d . . . H44 H 0.0432 0.0307 0.5365 0.111 Uiso 1 1 calc R . . C45 C 0.1629(4) 0.0884(2) 0.5031(2) 0.0735(12) Uani 1 1 d . . . H45 H 0.1241 0.0880 0.4601 0.088 Uiso 1 1 calc R . . C46 C 0.4157(3) 0.14153(15) 0.44059(15) 0.0446(7) Uani 1 1 d . . . C47 C 0.4751(3) 0.08671(16) 0.46084(18) 0.0537(8) Uani 1 1 d . . . H47 H 0.4545 0.0669 0.4974 0.064 Uiso 1 1 calc R . . C48 C 0.5634(4) 0.06082(18) 0.4286(2) 0.0621(9) Uani 1 1 d . . . H48 H 0.6015 0.0240 0.4435 0.075 Uiso 1 1 calc R . . C49 C 0.5960(4) 0.08902(18) 0.37416(19) 0.0611(9) Uani 1 1 d . . . H49 H 0.6552 0.0715 0.3518 0.073 Uiso 1 1 calc R . . C50 C 0.5393(4) 0.14304(19) 0.35398(18) 0.0610(9) Uani 1 1 d . . . H50 H 0.5600 0.1624 0.3172 0.073 Uiso 1 1 calc R . . C51 C 0.4519(3) 0.16983(17) 0.38672(16) 0.0521(8) Uani 1 1 d . . . H51 H 0.4167 0.2074 0.3725 0.062 Uiso 1 1 calc R . . C52 C 0.6438(6) 0.0732(3) 0.6520(3) 0.1089(19) Uiso 1 1 d . . . H52A H 0.5807 0.0646 0.6149 0.131 Uiso 1 1 calc R . . H52B H 0.6032 0.0885 0.6872 0.131 Uiso 1 1 calc R . . C53 C 0.7174(6) 0.0155(3) 0.6729(3) 0.1016(17) Uiso 1 1 d . . . H53A H 0.7336 0.0120 0.7198 0.122 Uiso 1 1 calc R . . H53B H 0.6742 -0.0211 0.6548 0.122 Uiso 1 1 calc R . . C54 C 0.8354(7) 0.0255(3) 0.6452(3) 0.119(2) Uiso 1 1 d . . . H54A H 0.9057 0.0287 0.6798 0.143 Uiso 1 1 calc R . . H54B H 0.8500 -0.0085 0.6171 0.143 Uiso 1 1 calc R . . C55 C 0.8189(7) 0.0823(3) 0.6089(3) 0.1121(19) Uiso 1 1 d . . . H55A H 0.8965 0.1050 0.6129 0.135 Uiso 1 1 calc R . . H55B H 0.7908 0.0739 0.5632 0.135 Uiso 1 1 calc R . . N1 N 0.2293(2) 0.36355(11) 0.51954(11) 0.0409(5) Uani 1 1 d . . . N2 N 0.0546(2) 0.32100(12) 0.39328(12) 0.0428(6) Uani 1 1 d . . . O1 O 0.3132(2) 0.26756(10) 0.43259(10) 0.0438(5) Uani 1 1 d . . . O2 O 0.7284(4) 0.1162(2) 0.6357(2) 0.1147(13) Uiso 1 1 d . . . Si1 Si 0.30303(9) 0.42714(4) 0.55740(4) 0.0471(2) Uani 1 1 d . . . Si2 Si -0.02612(9) 0.35174(4) 0.32299(4) 0.0483(2) Uani 1 1 d . . . P1 P 0.18346(7) 0.30476(4) 0.55203(3) 0.03742(17) Uani 1 1 d . . . P2 P 0.02894(7) 0.25786(4) 0.42543(3) 0.04077(18) Uani 1 1 d . . . Zn1 Zn 0.23511(3) 0.351308(16) 0.422491(16) 0.04207(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0398(15) 0.0414(15) 0.0373(14) 0.0003(11) 0.0093(12) -0.0011(12) C2 0.0387(15) 0.0464(16) 0.0395(14) -0.0001(12) 0.0073(12) 0.0004(12) C3 0.0462(18) 0.061(2) 0.0351(14) 0.0020(13) 0.0029(13) 0.0013(14) C4 0.059(2) 0.076(2) 0.0415(16) 0.0073(16) -0.0018(15) 0.0027(18) C5 0.056(2) 0.077(3) 0.0528(19) 0.0045(17) -0.0121(17) 0.0073(19) C6 0.0372(18) 0.078(3) 0.068(2) 0.0024(19) 0.0027(16) 0.0028(17) C7 0.0420(17) 0.0578(19) 0.0499(17) 0.0029(14) 0.0110(14) -0.0011(14) C8 0.0370(15) 0.0495(16) 0.0324(13) -0.0035(11) 0.0063(11) 0.0002(12) C9 0.0452(18) 0.0515(17) 0.0432(15) -0.0012(13) 0.0069(13) 0.0039(14) C10 0.051(2) 0.065(2) 0.0540(19) -0.0077(16) 0.0079(15) 0.0124(17) C11 0.0432(19) 0.081(3) 0.0497(18) -0.0086(17) 0.0148(15) 0.0031(17) C12 0.0478(19) 0.069(2) 0.0434(16) 0.0015(15) 0.0126(14) -0.0079(16) C13 0.0433(17) 0.0511(17) 0.0393(14) -0.0005(12) 0.0066(12) 0.0002(13) C14 0.0358(16) 0.071(2) 0.0383(14) -0.0068(14) 0.0060(12) -0.0049(15) C15 0.0456(19) 0.087(3) 0.0446(17) -0.0118(17) 0.0058(14) 0.0100(18) C16 0.053(2) 0.120(4) 0.061(2) -0.030(2) 0.0073(19) 0.011(2) C17 0.050(2) 0.144(5) 0.069(3) -0.042(3) 0.019(2) -0.011(3) C18 0.068(3) 0.114(4) 0.058(2) -0.022(2) 0.025(2) -0.038(3) C19 0.054(2) 0.082(3) 0.0459(17) -0.0078(17) 0.0118(15) -0.0148(18) C20 0.0454(17) 0.0497(17) 0.0372(14) -0.0005(12) 0.0048(12) -0.0002(13) C21 0.053(2) 0.065(2) 0.0457(17) -0.0068(15) 0.0055(15) -0.0062(16) C22 0.076(3) 0.064(2) 0.054(2) -0.0119(17) 0.0018(19) -0.012(2) C23 0.090(3) 0.053(2) 0.0456(18) -0.0106(15) 0.0065(18) 0.0033(19) C24 0.073(3) 0.063(2) 0.0431(17) -0.0072(15) 0.0154(17) 0.0103(19) C25 0.053(2) 0.0549(19) 0.0410(16) -0.0044(13) 0.0087(14) -0.0009(15) C26 0.054(2) 0.094(3) 0.0466(18) 0.0010(18) -0.0042(16) 0.006(2) C27 0.067(2) 0.077(3) 0.0427(17) -0.0027(16) 0.0075(16) 0.0062(19) C28 0.084(3) 0.067(2) 0.060(2) 0.0037(18) 0.010(2) 0.027(2) C29 0.086(3) 0.050(2) 0.064(2) 0.0005(16) 0.022(2) 0.0015(19) C30 0.058(2) 0.070(2) 0.062(2) -0.0052(18) 0.0116(17) -0.0175(18) C31 0.068(2) 0.065(2) 0.0441(17) -0.0075(15) 0.0117(16) -0.0123(18) C32 0.0466(17) 0.0494(17) 0.0363(14) -0.0011(12) 0.0066(12) -0.0037(13) C33 0.063(2) 0.0538(19) 0.0509(18) 0.0067(14) 0.0141(16) -0.0006(16) C34 0.083(3) 0.060(2) 0.0509(19) 0.0124(16) 0.0022(19) -0.012(2) C35 0.070(3) 0.084(3) 0.0478(19) 0.0070(18) 0.0115(18) -0.027(2) C36 0.049(2) 0.090(3) 0.061(2) -0.001(2) 0.0217(17) -0.0088(19) C37 0.0485(19) 0.065(2) 0.0497(18) 0.0016(15) 0.0089(15) -0.0033(16) C38 0.0393(16) 0.0498(16) 0.0345(13) -0.0006(11) 0.0069(11) 0.0013(13) C39 0.0427(16) 0.0460(16) 0.0387(14) -0.0003(12) 0.0086(12) 0.0009(13) C40 0.0453(17) 0.0420(15) 0.0467(16) 0.0017(12) 0.0099(13) 0.0046(13) C41 0.066(2) 0.054(2) 0.0499(18) 0.0059(15) 0.0083(16) -0.0002(17) C42 0.087(3) 0.065(2) 0.054(2) 0.0155(17) 0.022(2) 0.015(2) C43 0.088(3) 0.082(3) 0.080(3) 0.027(2) 0.028(3) -0.001(3) C44 0.093(4) 0.091(4) 0.094(4) 0.009(3) 0.017(3) -0.040(3) C45 0.076(3) 0.076(3) 0.064(2) 0.007(2) -0.003(2) -0.025(2) C46 0.0419(17) 0.0493(17) 0.0430(15) -0.0014(12) 0.0080(13) 0.0012(13) C47 0.054(2) 0.0485(18) 0.061(2) 0.0034(14) 0.0173(16) 0.0041(15) C48 0.057(2) 0.053(2) 0.080(3) 0.0014(17) 0.0208(19) 0.0111(16) C49 0.055(2) 0.063(2) 0.070(2) -0.0069(17) 0.0242(18) 0.0100(17) C50 0.059(2) 0.075(2) 0.055(2) 0.0031(17) 0.0250(17) 0.0082(18) C51 0.052(2) 0.0576(19) 0.0484(17) 0.0059(14) 0.0140(15) 0.0107(15) N1 0.0442(14) 0.0453(14) 0.0339(11) 0.0012(9) 0.0079(10) -0.0032(11) N2 0.0380(13) 0.0493(14) 0.0407(13) 0.0018(10) 0.0046(10) 0.0023(11) O1 0.0450(12) 0.0461(12) 0.0431(11) 0.0050(8) 0.0154(9) 0.0025(9) Si1 0.0545(5) 0.0470(5) 0.0410(4) -0.0021(3) 0.0111(4) -0.0067(4) Si2 0.0493(5) 0.0589(5) 0.0359(4) 0.0003(3) 0.0042(4) 0.0101(4) P1 0.0374(4) 0.0436(4) 0.0319(3) 0.0011(3) 0.0073(3) 0.0005(3) P2 0.0370(4) 0.0503(4) 0.0352(4) -0.0024(3) 0.0065(3) -0.0002(3) Zn1 0.0449(2) 0.0464(2) 0.03606(18) 0.00374(13) 0.00977(14) 0.00032(15) _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 C1 C38 1.550(4) . ? C1 P2 1.847(3) . ? C1 P1 1.850(3) . ? C1 H1 0.9900 . ? C2 C3 1.390(4) . ? C2 C7 1.399(4) . ? C2 P1 1.813(3) . ? C3 C4 1.385(5) . ? C3 H3 0.9400 . ? C4 C5 1.373(6) . ? C4 H4 0.9400 . ? C5 C6 1.388(6) . ? C5 H5 0.9400 . ? C6 C7 1.382(5) . ? C6 H6 0.9400 . ? C7 H7 0.9400 . ? C8 C9 1.393(4) . ? C8 C13 1.397(4) . ? C8 P1 1.813(3) . ? C9 C10 1.392(5) . ? C9 H9 0.9400 . ? C10 C11 1.372(6) . ? C10 H10 0.9400 . ? C11 C12 1.380(6) . ? C11 H11 0.9400 . ? C12 C13 1.382(5) . ? C12 H12 0.9400 . ? C13 H13 0.9400 . ? C14 C15 1.382(5) . ? C14 C19 1.398(5) . ? C14 P2 1.811(3) . ? C15 C16 1.385(6) . ? C15 H15 0.9400 . ? C16 C17 1.354(8) . ? C16 H16 0.9400 . ? C17 C18 1.384(8) . ? C17 H17 0.9400 . ? C18 C19 1.393(6) . ? C18 H18 0.9400 . ? C19 H19 0.9400 . ? C20 C21 1.385(5) . ? C20 C25 1.400(5) . ? C20 P2 1.832(3) . ? C21 C22 1.392(5) . ? C21 H21 0.9400 . ? C22 C23 1.368(6) . ? C22 H22 0.9400 . ? C23 C24 1.382(6) . ? C23 H23 0.9400 . ? C24 C25 1.388(5) . ? C24 H24 0.9400 . ? C25 H25 0.9400 . ? C26 Si2 1.874(4) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 Si2 1.858(4) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 Si2 1.882(4) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C29 Si1 1.860(4) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C30 Si1 1.859(4) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? C31 Si1 1.870(3) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 C33 1.394(5) . ? C32 C37 1.399(5) . ? C32 Zn1 1.985(3) . ? C33 C34 1.389(5) . ? C33 H33 0.9400 . ? C34 C35 1.368(6) . ? C34 H34 0.9400 . ? C35 C36 1.380(6) . ? C35 H35 0.9400 . ? C36 C37 1.393(5) . ? C36 H36 0.9400 . ? C37 H37 0.9400 . ? C38 O1 1.314(4) . ? C38 C39 1.373(4) . ? C39 C46 1.482(4) . ? C39 C40 1.502(4) . ? C40 C45 1.380(5) . ? C40 C41 1.397(5) . ? C41 C42 1.383(5) . ? C41 H41 0.9400 . ? C42 C43 1.338(7) . ? C42 H42 0.9400 . ? C43 C44 1.361(7) . ? C43 H43 0.9400 . ? C44 C45 1.392(6) . ? C44 H44 0.9400 . ? C45 H45 0.9400 . ? C46 C51 1.401(5) . ? C46 C47 1.402(5) . ? C47 C48 1.386(5) . ? C47 H47 0.9400 . ? C48 C49 1.395(6) . ? C48 H48 0.9400 . ? C49 C50 1.374(5) . ? C49 H49 0.9400 . ? C50 C51 1.393(5) . ? C50 H50 0.9400 . ? C51 H51 0.9400 . ? C52 O2 1.403(7) . ? C52 C53 1.528(8) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C53 C54 1.515(9) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C54 C55 1.457(9) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C55 O2 1.424(7) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? N1 P1 1.576(3) . ? N1 Si1 1.743(3) . ? N1 Zn1 2.069(2) . ? N2 P2 1.584(3) . ? N2 Si2 1.740(3) . ? N2 Zn1 2.093(3) . ? O1 Zn1 2.024(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C38 C1 P2 108.88(19) . . ? C38 C1 P1 110.8(2) . . ? P2 C1 P1 114.40(16) . . ? C38 C1 H1 107.5 . . ? P2 C1 H1 107.5 . . ? P1 C1 H1 107.5 . . ? C3 C2 C7 118.8(3) . . ? C3 C2 P1 124.7(2) . . ? C7 C2 P1 116.5(2) . . ? C2 C3 C4 120.3(3) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 120.2(3) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 120.5(3) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C7 C6 C5 119.4(4) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C6 C7 C2 120.8(3) . . ? C6 C7 H7 119.6 . . ? C2 C7 H7 119.6 . . ? C9 C8 C13 119.2(3) . . ? C9 C8 P1 118.7(2) . . ? C13 C8 P1 122.1(2) . . ? C8 C9 C10 119.8(3) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C11 C10 C9 120.1(3) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.7(3) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C13 C12 C11 119.7(3) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C8 120.4(3) . . ? C12 C13 H13 119.8 . . ? C8 C13 H13 119.8 . . ? C15 C14 C19 119.6(3) . . ? C15 C14 P2 118.7(3) . . ? C19 C14 P2 121.7(3) . . ? C14 C15 C16 120.6(4) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C17 C16 C15 120.1(5) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 120.2(4) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C17 C18 C19 120.7(5) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C18 C19 C14 118.5(4) . . ? C18 C19 H19 120.7 . . ? C14 C19 H19 120.7 . . ? C21 C20 C25 118.9(3) . . ? C21 C20 P2 123.9(3) . . ? C25 C20 P2 116.8(2) . . ? C20 C21 C22 119.6(4) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C23 C22 C21 121.3(4) . . ? C23 C22 H22 119.3 . . ? C21 C22 H22 119.3 . . ? C22 C23 C24 119.7(3) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C23 C24 C25 119.7(4) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C24 C25 C20 120.6(3) . . ? C24 C25 H25 119.7 . . ? C20 C25 H25 119.7 . . ? 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 . . ? Si2 C28 H28A 109.5 . . ? Si2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si1 C29 H29A 109.5 . . ? Si1 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si1 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? 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 . . ? C33 C32 C37 115.2(3) . . ? C33 C32 Zn1 126.8(3) . . ? C37 C32 Zn1 117.9(3) . . ? C34 C33 C32 122.8(4) . . ? C34 C33 H33 118.6 . . ? C32 C33 H33 118.6 . . ? C35 C34 C33 120.5(4) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C34 C35 C36 118.8(4) . . ? C34 C35 H35 120.6 . . ? C36 C35 H35 120.6 . . ? C35 C36 C37 120.3(4) . . ? C35 C36 H36 119.8 . . ? C37 C36 H36 119.8 . . ? C36 C37 C32 122.3(4) . . ? C36 C37 H37 118.8 . . ? C32 C37 H37 118.8 . . ? O1 C38 C39 126.3(3) . . ? O1 C38 C1 113.4(3) . . ? C39 C38 C1 120.2(3) . . ? C38 C39 C46 123.5(3) . . ? C38 C39 C40 119.1(3) . . ? C46 C39 C40 117.4(3) . . ? C45 C40 C41 116.4(3) . . ? C45 C40 C39 123.2(3) . . ? C41 C40 C39 120.4(3) . . ? C42 C41 C40 122.1(4) . . ? C42 C41 H41 118.9 . . ? C40 C41 H41 118.9 . . ? C43 C42 C41 120.2(4) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C42 C43 C44 119.6(4) . . ? C42 C43 H43 120.2 . . ? C44 C43 H43 120.2 . . ? C43 C44 C45 121.3(4) . . ? C43 C44 H44 119.3 . . ? C45 C44 H44 119.3 . . ? C40 C45 C44 120.4(4) . . ? C40 C45 H45 119.8 . . ? C44 C45 H45 119.8 . . ? C51 C46 C47 116.7(3) . . ? C51 C46 C39 123.3(3) . . ? C47 C46 C39 120.0(3) . . ? C48 C47 C46 122.0(3) . . ? C48 C47 H47 119.0 . . ? C46 C47 H47 119.0 . . ? C47 C48 C49 120.4(4) . . ? C47 C48 H48 119.8 . . ? C49 C48 H48 119.8 . . ? C50 C49 C48 118.3(3) . . ? C50 C49 H49 120.8 . . ? C48 C49 H49 120.8 . . ? C49 C50 C51 121.6(3) . . ? C49 C50 H50 119.2 . . ? C51 C50 H50 119.2 . . ? C50 C51 C46 121.0(3) . . ? C50 C51 H51 119.5 . . ? C46 C51 H51 119.5 . . ? O2 C52 C53 106.5(5) . . ? O2 C52 H52A 110.4 . . ? C53 C52 H52A 110.4 . . ? O2 C52 H52B 110.4 . . ? C53 C52 H52B 110.4 . . ? H52A C52 H52B 108.6 . . ? C54 C53 C52 102.5(5) . . ? C54 C53 H53A 111.3 . . ? C52 C53 H53A 111.3 . . ? C54 C53 H53B 111.3 . . ? C52 C53 H53B 111.3 . . ? H53A C53 H53B 109.2 . . ? C55 C54 C53 106.2(6) . . ? C55 C54 H54A 110.5 . . ? C53 C54 H54A 110.5 . . ? C55 C54 H54B 110.5 . . ? C53 C54 H54B 110.5 . . ? H54A C54 H54B 108.7 . . ? O2 C55 C54 106.0(6) . . ? O2 C55 H55A 110.5 . . ? C54 C55 H55A 110.5 . . ? O2 C55 H55B 110.5 . . ? C54 C55 H55B 110.5 . . ? H55A C55 H55B 108.7 . . ? P1 N1 Si1 127.76(15) . . ? P1 N1 Zn1 112.42(13) . . ? Si1 N1 Zn1 118.20(13) . . ? P2 N2 Si2 126.86(16) . . ? P2 N2 Zn1 111.96(13) . . ? Si2 N2 Zn1 117.69(14) . . ? C38 O1 Zn1 122.58(19) . . ? C52 O2 C55 106.0(5) . . ? N1 Si1 C29 107.66(17) . . ? N1 Si1 C30 110.47(16) . . ? C29 Si1 C30 108.3(2) . . ? N1 Si1 C31 111.98(15) . . ? C29 Si1 C31 109.14(18) . . ? C30 Si1 C31 109.20(18) . . ? N2 Si2 C27 109.85(16) . . ? N2 Si2 C26 114.14(16) . . ? C27 Si2 C26 106.20(19) . . ? N2 Si2 C28 107.11(16) . . ? C27 Si2 C28 111.1(2) . . ? C26 Si2 C28 108.5(2) . . ? N1 P1 C8 114.70(14) . . ? N1 P1 C2 112.06(14) . . ? C8 P1 C2 107.08(14) . . ? N1 P1 C1 111.00(13) . . ? C8 P1 C1 105.99(14) . . ? C2 P1 C1 105.40(14) . . ? N2 P2 C14 114.02(16) . . ? N2 P2 C20 112.34(14) . . ? C14 P2 C20 106.02(16) . . ? N2 P2 C1 109.79(14) . . ? C14 P2 C1 107.19(14) . . ? C20 P2 C1 107.11(14) . . ? C32 Zn1 O1 111.42(11) . . ? C32 Zn1 N1 125.07(11) . . ? O1 Zn1 N1 95.18(9) . . ? C32 Zn1 N2 122.90(12) . . ? O1 Zn1 N2 96.37(10) . . ? N1 Zn1 N2 99.26(10) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.76 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.634 _refine_diff_density_min -0.662 _refine_diff_density_rms 0.071 _publ_section_abstract ; ; _publ_section_experimental ; ; _publ_section_comment ; ; _publ_section_references ; ; _publ_section_figure_captions ; ; #END==========================================================================