Electronic Supplementary Material for CrystEngComm This Journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Edward R.T. Tiekink' _publ_contact_author_address ; Department of Chemistry The University of Texas at San Antonio 6900 North Loop 1604 West San Antonio Texas 78249-0698 UNITED STATES OF AMERICA ; _publ_contact_author_email EDWARD.TIEKINK@UTSA.EDU _publ_section_title ; Supramolecular aggregation in diimine adducts of zinc(II) dithiophosphates: controlling the formation of monomeric, dimeric, polymeric (zig-zag and helical), and 2-D motifs ; loop_ _publ_author_name 'Edward R.T. Tiekink' 'Danlin Chen.' 'Chian Sing Lai.' #============================================================================== # # [Zn(Cy2dtp)2(2-NC5H4C(H)=C(H)C5H4N-2)] # #============================================================================== data_shelxl_1 _database_code_depnum_ccdc_archive 'CCDC 284517' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H54 N2 O4 P2 S4 Zn' _chemical_formula_sum 'C36 H54 N2 O4 P2 S4 Zn' _chemical_formula_weight 834.36 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.7269(8) _cell_length_b 8.6585(7) _cell_length_c 24.853(2) _cell_angle_alpha 90 _cell_angle_beta 100.872(2) _cell_angle_gamma 90 _cell_volume 2055.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 3389 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 23.5 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.348 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 0.917 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.762 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details '(SADABS, Bruker, 2000 & Blessing, 1995)' _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17302 _diffrn_reflns_av_R_equivalents 0.062 _diffrn_reflns_av_sigmaI/netI 0.092 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 0.8 _diffrn_reflns_theta_max 30.1 _reflns_number_total 9963 _reflns_number_gt 7925 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction 'SHELXTL (Bruker, 2000)' _computing_structure_solution 'PATTY in DIRDIF92 (Beurskens et al., 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'Bruker SHEXLTL (Bruker, 2000)' _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^)+(0.0965P)^2^+6.6442P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(3) _refine_ls_number_reflns 9963 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.100 _refine_ls_R_factor_gt 0.078 _refine_ls_wR_factor_ref 0.223 _refine_ls_wR_factor_gt 0.209 _refine_ls_goodness_of_fit_ref 1.08 _refine_ls_restrained_S_all 1.08 _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 Zn Zn 0.09954(8) 0.5000 0.24141(3) 0.02675(19) Uani 1 1 d . . . S1 S -0.11087(17) 0.6402(3) 0.23730(7) 0.0291(4) Uani 1 1 d . . . S2 S 0.0599(2) 0.5310(2) 0.14164(7) 0.0316(4) Uani 1 1 d . . . S3 S 0.12981(19) 0.2460(3) 0.26202(7) 0.0287(4) Uani 1 1 d . . . S4 S -0.0025(2) 0.4272(3) 0.36131(8) 0.0397(5) Uani 1 1 d . . . P1 P -0.08324(17) 0.6757(2) 0.16032(7) 0.0239(3) Uani 1 1 d . . . P2 P 0.09774(18) 0.2504(3) 0.33981(7) 0.0259(4) Uani 1 1 d . . . O1 O -0.2255(5) 0.6729(7) 0.1178(2) 0.0295(11) Uani 1 1 d . . . O2 O -0.0402(5) 0.8494(6) 0.1560(2) 0.0277(11) Uani 1 1 d . . . O3 O 0.0283(6) 0.0875(7) 0.3443(2) 0.0311(11) Uani 1 1 d . . . O4 O 0.2447(5) 0.2224(6) 0.3807(2) 0.0281(11) Uani 1 1 d . . . N1 N 0.2632(6) 0.6515(8) 0.2704(3) 0.0278(12) Uani 1 1 d . . . N2 N 0.4883(7) 0.1841(10) 0.1949(3) 0.0407(17) Uani 1 1 d . . . C1 C -0.3194(7) 0.5364(8) 0.1093(3) 0.0287(15) Uani 1 1 d . . . H1 H -0.3001 0.4682 0.1419 0.034 Uiso 1 1 calc R . . C2 C -0.2934(9) 0.4510(13) 0.0597(4) 0.048(2) Uani 1 1 d . . . H2A H -0.2986 0.5230 0.0290 0.057 Uiso 1 1 calc R . . H2B H -0.1992 0.4059 0.0673 0.057 Uiso 1 1 calc R . . C3 C -0.4019(11) 0.3231(14) 0.0445(5) 0.062(3) Uani 1 1 d . . . H3A H -0.3897 0.2458 0.0738 0.074 Uiso 1 1 calc R . . H3B H -0.3867 0.2720 0.0109 0.074 Uiso 1 1 calc R . . C4 C -0.5479(11) 0.3847(15) 0.0358(4) 0.056(3) Uani 1 1 d . . . H4A H -0.6142 0.2985 0.0288 0.068 Uiso 1 1 calc R . . H4B H -0.5640 0.4516 0.0034 0.068 Uiso 1 1 calc R . . C5 C -0.5752(8) 0.4766(13) 0.0854(4) 0.047(2) Uani 1 1 d . . . H5A H -0.6679 0.5248 0.0764 0.056 Uiso 1 1 calc R . . H5B H -0.5753 0.4059 0.1162 0.056 Uiso 1 1 calc R . . C6 C -0.4667(8) 0.5992(10) 0.1020(4) 0.0369(17) Uani 1 1 d . . . H6A H -0.4806 0.6459 0.1365 0.044 Uiso 1 1 calc R . . H6B H -0.4788 0.6803 0.0740 0.044 Uiso 1 1 calc R . . C7 C 0.0067(8) 0.9071(10) 0.1079(3) 0.0320(16) Uani 1 1 d . . . H7 H 0.0201 0.8183 0.0844 0.038 Uiso 1 1 calc R . . C8 C 0.1426(10) 0.9834(19) 0.1259(4) 0.071(4) Uani 1 1 d . . . H8A H 0.2116 0.9089 0.1443 0.085 Uiso 1 1 calc R . . H8B H 0.1336 1.0666 0.1518 0.085 Uiso 1 1 calc R . . C9 C 0.1915(12) 1.051(2) 0.0742(6) 0.095(6) Uani 1 1 d . . . H9A H 0.2813 1.1038 0.0856 0.113 Uiso 1 1 calc R . . H9B H 0.2059 0.9659 0.0498 0.113 Uiso 1 1 calc R . . C10 C 0.0876(11) 1.1619(13) 0.0434(4) 0.054(2) Uani 1 1 d . . . H10A H 0.0784 1.2515 0.0665 0.065 Uiso 1 1 calc R . . H10B H 0.1205 1.1985 0.0107 0.065 Uiso 1 1 calc R . . C11 C -0.0499(11) 1.0859(13) 0.0270(4) 0.052(2) Uani 1 1 d . . . H11A H -0.0426 1.0050 0.0001 0.063 Uiso 1 1 calc R . . H11B H -0.1184 1.1620 0.0095 0.063 Uiso 1 1 calc R . . C12 C -0.1015(9) 1.0144(16) 0.0756(4) 0.057(3) Uani 1 1 d . . . H12A H -0.1878 0.9565 0.0623 0.069 Uiso 1 1 calc R . . H12B H -0.1234 1.0968 0.0997 0.069 Uiso 1 1 calc R . . C13 C -0.0144(8) 0.0344(9) 0.3943(3) 0.0317(16) Uani 1 1 d . . . H13 H -0.0139 0.1229 0.4195 0.038 Uiso 1 1 calc R . . C14 C 0.0841(9) -0.0869(13) 0.4215(4) 0.047(2) Uani 1 1 d . . . H14A H 0.1778 -0.0426 0.4329 0.057 Uiso 1 1 calc R . . H14B H 0.0902 -0.1709 0.3956 0.057 Uiso 1 1 calc R . . C15 C 0.0331(11) -0.1494(14) 0.4709(4) 0.054(3) Uani 1 1 d . . . H15A H 0.0974 -0.2299 0.4881 0.065 Uiso 1 1 calc R . . H15B H 0.0331 -0.0662 0.4976 0.065 Uiso 1 1 calc R . . C16 C -0.1130(11) -0.2161(13) 0.4557(4) 0.054(3) Uani 1 1 d . . . H16A H -0.1131 -0.3036 0.4307 0.065 Uiso 1 1 calc R . . H16B H -0.1444 -0.2530 0.4886 0.065 Uiso 1 1 calc R . . C17 C -0.2115(11) -0.0904(16) 0.4280(5) 0.060(3) Uani 1 1 d . . . H17A H -0.2155 -0.0063 0.4541 0.072 Uiso 1 1 calc R . . H17B H -0.3060 -0.1330 0.4172 0.072 Uiso 1 1 calc R . . C18 C -0.1631(9) -0.0280(14) 0.3784(4) 0.051(3) Uani 1 1 d . . . H18A H -0.2260 0.0549 0.3620 0.061 Uiso 1 1 calc R . . H18B H -0.1657 -0.1101 0.3511 0.061 Uiso 1 1 calc R . . C19 C 0.3498(7) 0.3445(9) 0.3894(3) 0.0299(15) Uani 1 1 d . . . H19 H 0.3225 0.4284 0.3625 0.036 Uiso 1 1 calc R . . C20 C 0.4869(9) 0.2781(12) 0.3829(4) 0.043(2) Uani 1 1 d . . . H20A H 0.4817 0.2443 0.3449 0.051 Uiso 1 1 calc R . . H20B H 0.5083 0.1877 0.4068 0.051 Uiso 1 1 calc R . . C21 C 0.6044(9) 0.3995(14) 0.3978(4) 0.055(3) Uani 1 1 d . . . H21A H 0.6948 0.3522 0.3957 0.066 Uiso 1 1 calc R . . H21B H 0.5883 0.4845 0.3713 0.066 Uiso 1 1 calc R . . C22 C 0.6089(12) 0.4614(18) 0.4541(5) 0.078(4) Uani 1 1 d . . . H22A H 0.6831 0.5393 0.4622 0.093 Uiso 1 1 calc R . . H22B H 0.6314 0.3775 0.4808 0.093 Uiso 1 1 calc R . . C23 C 0.4672(14) 0.5351(17) 0.4600(5) 0.080(4) Uani 1 1 d . . . H23A H 0.4723 0.5754 0.4971 0.096 Uiso 1 1 calc R . . H23B H 0.4439 0.6204 0.4339 0.096 Uiso 1 1 calc R . . C24 C 0.3537(10) 0.4056(12) 0.4478(4) 0.045(2) Uani 1 1 d . . . H24A H 0.2619 0.4473 0.4510 0.054 Uiso 1 1 calc R . . H24B H 0.3765 0.3215 0.4744 0.054 Uiso 1 1 calc R . . C25 C 0.2320(8) 0.7804(10) 0.2923(3) 0.0345(17) Uani 1 1 d . . . H25 H 0.1389 0.7963 0.2964 0.041 Uiso 1 1 calc R . . C26 C 0.3286(9) 0.8944(11) 0.3097(4) 0.044(2) Uani 1 1 d . . . H26 H 0.3027 0.9855 0.3257 0.053 Uiso 1 1 calc R . . C27 C 0.4638(10) 0.8714(12) 0.3030(5) 0.059(3) Uani 1 1 d . . . H27 H 0.5322 0.9471 0.3146 0.071 Uiso 1 1 calc R . . C28 C 0.4988(8) 0.7381(10) 0.2793(4) 0.0362(17) Uani 1 1 d . . . H28 H 0.5907 0.7238 0.2735 0.043 Uiso 1 1 calc R . . C29 C 0.3992(7) 0.6236(9) 0.2637(3) 0.0309(15) Uani 1 1 d . . . C30 C 0.4288(7) 0.4756(9) 0.2412(3) 0.0302(15) Uani 1 1 d . . . H30 H 0.3544 0.4211 0.2198 0.036 Uiso 1 1 calc R . . C31 C 0.5551(7) 0.4134(9) 0.2491(3) 0.0283(14) Uani 1 1 d . . . H31 H 0.6281 0.4697 0.2706 0.034 Uiso 1 1 calc R . . C32 C 0.5916(7) 0.2653(9) 0.2275(3) 0.0267(14) Uani 1 1 d . . . C33 C 0.5232(9) 0.0484(11) 0.1771(4) 0.048(2) Uani 1 1 d . . . H33 H 0.4517 -0.0121 0.1567 0.057 Uiso 1 1 calc R . . C34 C 0.6553(8) -0.0096(13) 0.1864(4) 0.0433(19) Uani 1 1 d . . . H34 H 0.6750 -0.1031 0.1702 0.052 Uiso 1 1 calc R . . C35 C 0.7617(9) 0.0722(12) 0.2206(4) 0.049(2) Uani 1 1 d . . . H35 H 0.8526 0.0316 0.2303 0.058 Uiso 1 1 calc R . . C36 C 0.7282(8) 0.2128(10) 0.2391(4) 0.0374(19) Uani 1 1 d . . . H36 H 0.7984 0.2745 0.2598 0.045 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.0260(4) 0.0227(4) 0.0302(4) 0.0017(3) 0.0020(3) 0.0041(3) S1 0.0236(7) 0.0346(10) 0.0302(8) 0.0023(7) 0.0079(6) 0.0057(7) S2 0.0391(9) 0.0316(11) 0.0249(7) -0.0009(7) 0.0081(7) 0.0131(8) S3 0.0382(9) 0.0226(8) 0.0268(8) -0.0001(7) 0.0099(7) 0.0023(7) S4 0.0451(11) 0.0389(12) 0.0363(10) -0.0016(9) 0.0110(8) 0.0130(9) P1 0.0214(7) 0.0224(9) 0.0277(8) 0.0005(7) 0.0043(6) 0.0020(6) P2 0.0228(8) 0.0250(9) 0.0298(9) 0.0008(7) 0.0043(6) -0.0010(7) O1 0.028(2) 0.029(3) 0.031(2) 0.008(2) 0.0041(19) 0.001(2) O2 0.027(2) 0.026(3) 0.033(3) 0.000(2) 0.012(2) -0.001(2) O3 0.036(3) 0.030(3) 0.027(2) 0.000(2) 0.006(2) -0.011(2) O4 0.026(2) 0.023(3) 0.033(3) 0.003(2) -0.0006(19) -0.0056(19) N1 0.022(3) 0.025(3) 0.035(3) 0.003(2) 0.004(2) 0.006(2) N2 0.026(3) 0.046(4) 0.048(4) -0.015(3) 0.001(3) 0.006(3) C1 0.027(3) 0.022(4) 0.034(3) 0.000(3) -0.001(3) -0.001(3) C2 0.037(4) 0.057(7) 0.047(5) -0.018(4) 0.004(4) -0.006(4) C3 0.054(6) 0.048(6) 0.080(8) -0.025(6) 0.006(5) -0.010(5) C4 0.055(6) 0.074(8) 0.036(5) -0.012(4) -0.002(4) -0.032(5) C5 0.030(4) 0.055(7) 0.055(5) -0.004(5) 0.008(3) -0.011(4) C6 0.032(4) 0.032(4) 0.045(4) -0.005(3) 0.005(3) -0.005(3) C7 0.033(4) 0.038(5) 0.025(3) 0.001(3) 0.007(3) -0.001(3) C8 0.048(5) 0.113(11) 0.046(5) 0.032(7) -0.005(4) -0.037(7) C9 0.044(6) 0.145(16) 0.095(9) 0.079(10) 0.014(6) -0.013(7) C10 0.074(7) 0.044(6) 0.048(5) 0.016(4) 0.023(5) -0.006(5) C11 0.056(5) 0.051(6) 0.047(5) 0.018(4) 0.001(4) 0.006(5) C12 0.038(4) 0.072(8) 0.063(6) 0.039(6) 0.012(4) 0.007(5) C13 0.036(4) 0.033(4) 0.027(3) 0.006(3) 0.009(3) -0.007(3) C14 0.038(4) 0.061(7) 0.042(5) 0.022(5) 0.005(4) 0.003(4) C15 0.059(6) 0.066(7) 0.036(5) 0.021(4) 0.003(4) -0.013(5) C16 0.056(6) 0.050(6) 0.058(6) 0.017(5) 0.017(5) -0.009(5) C17 0.045(5) 0.079(9) 0.059(6) 0.016(6) 0.016(5) -0.007(5) C18 0.031(4) 0.061(7) 0.059(5) 0.017(5) 0.004(4) -0.011(4) C19 0.030(3) 0.027(4) 0.030(4) 0.003(3) 0.000(3) -0.007(3) C20 0.035(4) 0.042(5) 0.052(5) -0.003(4) 0.011(4) -0.004(4) C21 0.033(4) 0.067(7) 0.064(6) 0.005(5) 0.005(4) -0.022(4) C22 0.058(6) 0.100(12) 0.070(7) -0.001(7) -0.003(5) -0.046(7) C23 0.094(9) 0.084(11) 0.058(6) -0.032(7) 0.007(6) -0.048(8) C24 0.047(5) 0.050(6) 0.038(4) -0.016(4) 0.006(4) -0.011(4) C25 0.031(4) 0.034(5) 0.038(4) -0.003(3) 0.006(3) 0.014(3) C26 0.040(4) 0.033(5) 0.058(5) -0.019(4) 0.005(4) 0.004(4) C27 0.035(4) 0.030(5) 0.109(10) -0.017(5) 0.005(5) -0.008(4) C28 0.030(4) 0.030(4) 0.049(5) -0.008(4) 0.010(3) -0.005(3) C29 0.025(3) 0.024(4) 0.044(4) -0.003(3) 0.008(3) -0.002(3) C30 0.024(3) 0.020(4) 0.048(4) -0.005(3) 0.011(3) -0.005(3) C31 0.027(3) 0.023(4) 0.036(4) 0.000(3) 0.006(3) -0.003(3) C32 0.027(3) 0.020(3) 0.036(3) 0.003(3) 0.014(3) 0.003(3) C33 0.035(4) 0.034(5) 0.072(6) -0.025(4) 0.001(4) -0.001(3) C34 0.039(4) 0.036(5) 0.055(5) -0.014(4) 0.009(3) 0.011(4) C35 0.024(4) 0.049(6) 0.070(6) -0.015(5) 0.003(4) 0.011(4) C36 0.030(4) 0.036(5) 0.046(5) -0.013(3) 0.007(3) 0.005(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 Zn N1 2.084(6) . ? Zn S3 2.265(2) . ? Zn S1 2.3652(19) . ? Zn S2 2.4513(19) . ? Zn P1 2.8610(19) . ? Zn S4 3.373(2) . ? S1 P1 2.005(2) . ? S2 P1 1.992(2) . ? S3 P2 2.016(2) . ? S4 P2 1.944(3) . ? P1 O2 1.571(6) . ? P1 O1 1.575(5) . ? P2 O3 1.577(6) . ? P2 O4 1.609(5) . ? O1 C1 1.484(9) . ? O2 C7 1.446(9) . ? O3 C13 1.456(8) . ? O4 C19 1.457(8) . ? N1 C25 1.302(10) . ? N1 C29 1.385(9) . ? N2 C32 1.361(10) . ? N2 C33 1.322(11) . ? C1 C6 1.511(10) . ? C1 C2 1.499(11) . ? C1 H1 0.9900 . ? C2 C3 1.528(14) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C3 C4 1.494(16) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 C5 1.531(14) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 C6 1.500(12) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 C8 1.470(12) . ? C7 C12 1.516(12) . ? C7 H7 0.9900 . ? C8 C9 1.566(14) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 C10 1.496(16) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 C11 1.477(15) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 C12 1.523(13) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 C14 1.495(12) . ? C13 C18 1.525(11) . ? C13 H13 0.9900 . ? C14 C15 1.509(12) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 C16 1.514(14) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 C17 1.525(15) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 C18 1.502(13) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 C20 1.489(12) . ? C19 C24 1.539(11) . ? C19 H19 0.9900 . ? C20 C21 1.546(12) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C21 C22 1.491(16) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C22 C23 1.55(2) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 C24 1.562(14) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 C26 1.375(12) . ? C25 H25 0.9400 . ? C26 C27 1.371(13) . ? C26 H26 0.9400 . ? C27 C28 1.368(13) . ? C27 H27 0.9400 . ? C28 C29 1.389(11) . ? C28 H28 0.9400 . ? C29 C30 1.449(11) . ? C30 C31 1.322(10) . ? C30 H30 0.9400 . ? C31 C32 1.460(10) . ? C31 H31 0.9400 . ? C32 C36 1.383(10) . ? C33 C34 1.358(12) . ? C33 H33 0.9400 . ? C34 C35 1.400(13) . ? C34 H34 0.9400 . ? C35 C36 1.363(12) . ? C35 H35 0.9400 . ? C36 H36 0.9400 . ? 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 Zn S3 118.35(17) . . ? N1 Zn S1 106.88(17) . . ? S3 Zn S1 125.64(8) . . ? N1 Zn S2 104.17(18) . . ? S3 Zn S2 108.91(7) . . ? S1 Zn S2 86.01(6) . . ? N1 Zn S4 98.34(18) . . ? S3 Zn S4 70.50(6) . . ? S1 Zn S4 74.79(6) . . ? S2 Zn S4 153.88(7) . . ? O2 P1 O1 100.4(3) . . ? O2 P1 S2 112.3(2) . . ? O1 P1 S2 113.5(2) . . ? O2 P1 S1 107.3(2) . . ? O1 P1 S1 112.2(2) . . ? S2 P1 S1 110.57(11) . . ? O3 P2 O4 99.3(3) . . ? O3 P2 S4 116.2(2) . . ? O4 P2 S4 112.1(2) . . ? O3 P2 S3 101.3(2) . . ? O4 P2 S3 108.9(2) . . ? S4 P2 S3 117.05(13) . . ? C1 O1 P1 123.2(4) . . ? C7 O2 P1 121.1(5) . . ? C13 O3 P2 122.5(5) . . ? C19 O4 P2 119.9(5) . . ? C25 N1 C29 120.2(7) . . ? C25 N1 Zn 117.4(5) . . ? C29 N1 Zn 122.3(5) . . ? C32 N2 C33 116.8(7) . . ? O1 C1 C6 105.9(6) . . ? O1 C1 C2 108.4(6) . . ? C6 C1 C2 112.4(6) . . ? O1 C1 H1 110.0 . . ? C6 C1 H1 110.0 . . ? C2 C1 H1 110.0 . . ? C3 C2 C1 110.2(8) . . ? C3 C2 H2A 109.6 . . ? C1 C2 H2A 109.6 . . ? C3 C2 H2B 109.6 . . ? C1 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? C2 C3 C4 111.8(9) . . ? C2 C3 H3A 109.3 . . ? C4 C3 H3A 109.3 . . ? C2 C3 H3B 109.3 . . ? C4 C3 H3B 109.3 . . ? H3A C3 H3B 107.9 . . ? C3 C4 C5 111.9(8) . . ? C3 C4 H4A 109.2 . . ? C5 C4 H4A 109.2 . . ? C3 C4 H4B 109.2 . . ? C5 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? C6 C5 C4 111.7(7) . . ? C6 C5 H5A 109.3 . . ? C4 C5 H5A 109.3 . . ? C6 C5 H5B 109.3 . . ? C4 C5 H5B 109.3 . . ? H5A C5 H5B 107.9 . . ? C5 C6 C1 112.4(7) . . ? C5 C6 H6A 109.1 . . ? C1 C6 H6A 109.1 . . ? C5 C6 H6B 109.1 . . ? C1 C6 H6B 109.1 . . ? H6A C6 H6B 107.9 . . ? O2 C7 C8 108.0(6) . . ? O2 C7 C12 110.8(6) . . ? C8 C7 C12 112.4(9) . . ? O2 C7 H7 108.5 . . ? C8 C7 H7 108.5 . . ? C12 C7 H7 108.5 . . ? C7 C8 C9 108.2(8) . . ? C7 C8 H8A 110.0 . . ? C9 C8 H8A 110.0 . . ? C7 C8 H8B 110.0 . . ? C9 C8 H8B 110.0 . . ? H8A C8 H8B 108.4 . . ? C10 C9 C8 112.3(11) . . ? C10 C9 H9A 109.1 . . ? C8 C9 H9A 109.1 . . ? C10 C9 H9B 109.1 . . ? C8 C9 H9B 109.1 . . ? H9A C9 H9B 107.9 . . ? C11 C10 C9 110.1(10) . . ? C11 C10 H10A 109.6 . . ? C9 C10 H10A 109.6 . . ? C11 C10 H10B 109.6 . . ? C9 C10 H10B 109.6 . . ? H10A C10 H10B 108.2 . . ? C10 C11 C12 112.4(8) . . ? C10 C11 H11A 109.1 . . ? C12 C11 H11A 109.1 . . ? C10 C11 H11B 109.1 . . ? C12 C11 H11B 109.1 . . ? H11A C11 H11B 107.9 . . ? C11 C12 C7 111.7(7) . . ? C11 C12 H12A 109.3 . . ? C7 C12 H12A 109.3 . . ? C11 C12 H12B 109.3 . . ? C7 C12 H12B 109.3 . . ? H12A C12 H12B 107.9 . . ? O3 C13 C14 110.3(6) . . ? O3 C13 C18 107.5(6) . . ? C14 C13 C18 111.3(8) . . ? O3 C13 H13 109.2 . . ? C14 C13 H13 109.2 . . ? C18 C13 H13 109.2 . . ? C13 C14 C15 109.8(8) . . ? C13 C14 H14A 109.7 . . ? C15 C14 H14A 109.7 . . ? C13 C14 H14B 109.7 . . ? C15 C14 H14B 109.7 . . ? H14A C14 H14B 108.2 . . ? C16 C15 C14 111.8(8) . . ? C16 C15 H15A 109.3 . . ? C14 C15 H15A 109.3 . . ? C16 C15 H15B 109.3 . . ? C14 C15 H15B 109.3 . . ? H15A C15 H15B 107.9 . . ? C17 C16 C15 108.7(9) . . ? C17 C16 H16A 109.9 . . ? C15 C16 H16A 109.9 . . ? C17 C16 H16B 109.9 . . ? C15 C16 H16B 109.9 . . ? H16A C16 H16B 108.3 . . ? C16 C17 C18 111.1(9) . . ? C16 C17 H17A 109.4 . . ? C18 C17 H17A 109.4 . . ? C16 C17 H17B 109.4 . . ? C18 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? C17 C18 C13 110.1(8) . . ? C17 C18 H18A 109.6 . . ? C13 C18 H18A 109.6 . . ? C17 C18 H18B 109.6 . . ? C13 C18 H18B 109.6 . . ? H18A C18 H18B 108.1 . . ? O4 C19 C20 108.7(7) . . ? O4 C19 C24 106.3(6) . . ? C20 C19 C24 111.8(7) . . ? O4 C19 H19 110.0 . . ? C20 C19 H19 110.0 . . ? C24 C19 H19 110.0 . . ? C19 C20 C21 110.4(8) . . ? C19 C20 H20A 109.6 . . ? C21 C20 H20A 109.6 . . ? C19 C20 H20B 109.6 . . ? C21 C20 H20B 109.6 . . ? H20A C20 H20B 108.1 . . ? C22 C21 C20 111.0(8) . . ? C22 C21 H21A 109.4 . . ? C20 C21 H21A 109.4 . . ? C22 C21 H21B 109.4 . . ? C20 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? C21 C22 C23 111.5(9) . . ? C21 C22 H22A 109.3 . . ? C23 C22 H22A 109.3 . . ? C21 C22 H22B 109.3 . . ? C23 C22 H22B 109.3 . . ? H22A C22 H22B 108.0 . . ? C24 C23 C22 107.2(11) . . ? C24 C23 H23A 110.3 . . ? C22 C23 H23A 110.3 . . ? C24 C23 H23B 110.3 . . ? C22 C23 H23B 110.3 . . ? H23A C23 H23B 108.5 . . ? C23 C24 C19 108.7(8) . . ? C23 C24 H24A 110.0 . . ? C19 C24 H24A 110.0 . . ? C23 C24 H24B 110.0 . . ? C19 C24 H24B 110.0 . . ? H24A C24 H24B 108.3 . . ? N1 C25 C26 123.1(7) . . ? N1 C25 H25 118.4 . . ? C26 C25 H25 118.4 . . ? C25 C26 C27 118.2(8) . . ? C25 C26 H26 120.9 . . ? C27 C26 H26 120.9 . . ? C26 C27 C28 119.8(9) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C29 C28 C27 120.3(8) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 N1 118.3(7) . . ? C28 C29 C30 124.0(7) . . ? N1 C29 C30 117.7(7) . . ? C31 C30 C29 123.3(7) . . ? C31 C30 H30 118.3 . . ? C29 C30 H30 118.3 . . ? C30 C31 C32 125.9(7) . . ? C30 C31 H31 117.0 . . ? C32 C31 H31 117.0 . . ? N2 C32 C36 121.8(7) . . ? N2 C32 C31 118.0(6) . . ? C36 C32 C31 120.2(7) . . ? N2 C33 C34 124.5(8) . . ? N2 C33 H33 117.8 . . ? C34 C33 H33 117.8 . . ? C33 C34 C35 118.9(9) . . ? C33 C34 H34 120.5 . . ? C35 C34 H34 120.5 . . ? C36 C35 C34 117.4(8) . . ? C36 C35 H35 121.3 . . ? C34 C35 H35 121.3 . . ? C32 C36 C35 120.3(8) . . ? C32 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 30.1 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.24 # # located 0.81 \%A from the Zn atom # _refine_diff_density_min -0.73 _refine_diff_density_rms 0.159 # Attachment 'B513393A 2.cif' #============================================================================== # # {[Zn(iPr2dtp)2]2(2-NC5H4C(H)=C(H)C5H4N-2)0.5}2 # #============================================================================== data_shelxl_2 _database_code_depnum_ccdc_archive 'CCDC 284518' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H66 N2 O8 P4 S8 Zn2' _chemical_formula_sum 'C36 H66 N2 O8 P4 S8 Zn2' _chemical_formula_weight 1166.01 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.8735(8) _cell_length_b 17.7046(15) _cell_length_c 20.0325(19) _cell_angle_alpha 90 _cell_angle_beta 90.638(2) _cell_angle_gamma 90 _cell_volume 2792.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 867 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 22.9 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.387 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 1.316 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.803 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details '(SADABS, Bruker, 2000 & Blessing, 1995)' _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 23156 _diffrn_reflns_av_R_equivalents 0.045 _diffrn_reflns_av_sigmaI/netI 0.057 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 30.0 _reflns_number_total 8112 _reflns_number_gt 5566 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction 'SHELXTL (Bruker, 2000)' _computing_structure_solution 'PATTY in DIRDIF92 (Beurskens et al., 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHEXLTL (Bruker, 2000)' _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^)+(0.0510P)^2^] 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 8112 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.079 _refine_ls_R_factor_gt 0.047 _refine_ls_wR_factor_ref 0.113 _refine_ls_wR_factor_gt 0.100 _refine_ls_goodness_of_fit_ref 1.01 _refine_ls_restrained_S_all 1.01 _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 Zn Zn 0.15215(4) 0.148172(16) 0.374610(19) 0.04521(11) Uani 1 1 d . . . S1 S 0.34562(9) 0.24230(3) 0.34965(3) 0.03732(16) Uani 1 1 d . . . S2 S 0.17408(8) 0.21101(4) 0.49645(3) 0.03708(15) Uani 1 1 d . . . S3 S -0.13752(8) 0.14415(3) 0.35205(3) 0.03419(15) Uani 1 1 d . . . S4 S 0.14132(9) 0.08814(4) 0.24133(4) 0.04432(17) Uani 1 1 d . . . P1 P 0.29054(8) 0.28548(3) 0.43986(3) 0.03012(14) Uani 1 1 d . . . P2 P -0.08187(8) 0.06862(4) 0.28019(3) 0.03330(15) Uani 1 1 d . . . O1 O 0.1739(2) 0.35744(8) 0.43381(9) 0.0344(4) Uani 1 1 d . . . O2 O 0.4553(2) 0.32159(9) 0.47255(9) 0.0379(4) Uani 1 1 d . . . O3 O -0.2323(2) 0.06520(9) 0.22726(8) 0.0382(4) Uani 1 1 d . . . O4 O -0.0976(2) -0.01190(9) 0.31396(8) 0.0378(4) Uani 1 1 d . . . N1 N 0.2701(3) 0.05073(10) 0.40512(10) 0.0312(4) Uani 1 1 d . . . C1 C 0.2199(3) 0.41995(13) 0.38894(13) 0.0374(6) Uani 1 1 d . . . H1 H 0.3312 0.4091 0.3685 0.045 Uiso 1 1 calc R . . C2 C 0.2339(5) 0.49036(15) 0.43096(16) 0.0568(8) Uani 1 1 d . . . H2A H 0.3241 0.4841 0.4639 0.085 Uiso 1 1 calc R . . H2B H 0.1272 0.4991 0.4535 0.085 Uiso 1 1 calc R . . H2C H 0.2593 0.5332 0.4026 0.085 Uiso 1 1 calc R . . C3 C 0.0861(4) 0.42387(16) 0.33531(15) 0.0521(8) Uani 1 1 d . . . H3A H 0.0860 0.3772 0.3099 0.078 Uiso 1 1 calc R . . H3B H 0.1099 0.4659 0.3058 0.078 Uiso 1 1 calc R . . H3C H -0.0242 0.4310 0.3555 0.078 Uiso 1 1 calc R . . C4 C 0.6167(3) 0.28151(15) 0.47997(16) 0.0463(7) Uani 1 1 d . . . H4 H 0.6046 0.2296 0.4621 0.056 Uiso 1 1 calc R . . C5 C 0.6572(5) 0.27800(18) 0.55320(18) 0.0748(11) Uani 1 1 d . . . H5A H 0.5719 0.2479 0.5755 0.112 Uiso 1 1 calc R . . H5B H 0.6578 0.3287 0.5716 0.112 Uiso 1 1 calc R . . H5C H 0.7680 0.2551 0.5599 0.112 Uiso 1 1 calc R . . C6 C 0.7443(4) 0.3238(2) 0.4399(2) 0.0741(11) Uani 1 1 d . . . H6A H 0.7111 0.3227 0.3931 0.111 Uiso 1 1 calc R . . H6B H 0.8550 0.3005 0.4454 0.111 Uiso 1 1 calc R . . H6C H 0.7496 0.3758 0.4551 0.111 Uiso 1 1 calc R . . C7 C -0.2545(4) 0.12387(15) 0.17634(14) 0.0448(7) Uani 1 1 d . . . H7 H -0.1686 0.1640 0.1832 0.054 Uiso 1 1 calc R . . C8 C -0.2290(5) 0.0872(2) 0.11015(15) 0.0704(10) Uani 1 1 d . . . H8A H -0.1134 0.0686 0.1074 0.106 Uiso 1 1 calc R . . H8B H -0.2493 0.1238 0.0749 0.106 Uiso 1 1 calc R . . H8C H -0.3076 0.0454 0.1051 0.106 Uiso 1 1 calc R . . C9 C -0.4297(4) 0.15625(18) 0.18438(19) 0.0679(10) Uani 1 1 d . . . H9A H -0.4383 0.1798 0.2279 0.102 Uiso 1 1 calc R . . H9B H -0.5131 0.1161 0.1805 0.102 Uiso 1 1 calc R . . H9C H -0.4507 0.1937 0.1499 0.102 Uiso 1 1 calc R . . C10 C -0.0527(4) -0.08103(14) 0.27655(14) 0.0446(7) Uani 1 1 d . . . H10 H -0.0203 -0.0675 0.2305 0.054 Uiso 1 1 calc R . . C11 C 0.0925(4) -0.11790(17) 0.31128(19) 0.0650(9) Uani 1 1 d . . . H11A H 0.1900 -0.0844 0.3109 0.098 Uiso 1 1 calc R . . H11B H 0.1205 -0.1646 0.2886 0.098 Uiso 1 1 calc R . . H11C H 0.0620 -0.1288 0.3571 0.098 Uiso 1 1 calc R . . C12 C -0.2087(5) -0.13110(18) 0.2749(2) 0.0745(11) Uani 1 1 d . . . H12A H -0.3002 -0.1053 0.2514 0.112 Uiso 1 1 calc R . . H12B H -0.2432 -0.1422 0.3201 0.112 Uiso 1 1 calc R . . H12C H -0.1825 -0.1778 0.2519 0.112 Uiso 1 1 calc R . . C13 C 0.2073(3) 0.00123(13) 0.45015(12) 0.0299(5) Uani 1 1 d . . . C14 C 0.3008(3) -0.06227(13) 0.46943(13) 0.0367(6) Uani 1 1 d . . . H14 H 0.2560 -0.0966 0.5004 0.044 Uiso 1 1 calc R . . C15 C 0.4587(3) -0.07435(14) 0.44292(14) 0.0414(6) Uani 1 1 d . . . H15 H 0.5227 -0.1169 0.4556 0.050 Uiso 1 1 calc R . . C16 C 0.5225(3) -0.02332(14) 0.39744(14) 0.0416(6) Uani 1 1 d . . . H16 H 0.6308 -0.0302 0.3791 0.050 Uiso 1 1 calc R . . C17 C 0.4244(3) 0.03763(14) 0.37958(13) 0.0366(6) Uani 1 1 d . . . H17 H 0.4671 0.0718 0.3480 0.044 Uiso 1 1 calc R . . C18 C 0.0390(3) 0.01748(13) 0.47633(13) 0.0363(6) Uani 1 1 d . . . H18 H -0.0196 0.0581 0.4565 0.044 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.03107(17) 0.03151(17) 0.0729(3) 0.01457(15) -0.00779(16) -0.00489(12) S1 0.0411(4) 0.0349(3) 0.0362(4) -0.0026(3) 0.0130(3) -0.0087(3) S2 0.0373(4) 0.0385(3) 0.0357(4) 0.0057(3) 0.0063(3) 0.0002(3) S3 0.0289(3) 0.0364(3) 0.0374(3) -0.0033(3) 0.0030(3) 0.0021(2) S4 0.0349(4) 0.0562(4) 0.0420(4) -0.0041(3) 0.0098(3) -0.0047(3) P1 0.0249(3) 0.0312(3) 0.0343(3) -0.0007(3) 0.0037(2) 0.0004(2) P2 0.0326(3) 0.0369(3) 0.0305(3) -0.0007(3) 0.0025(3) -0.0022(3) O1 0.0291(9) 0.0324(9) 0.0420(10) 0.0079(7) 0.0061(7) 0.0035(7) O2 0.0261(9) 0.0364(9) 0.0510(11) -0.0104(8) -0.0015(8) 0.0029(7) O3 0.0384(10) 0.0417(10) 0.0344(10) 0.0054(8) -0.0035(8) -0.0093(8) O4 0.0479(11) 0.0338(9) 0.0319(9) -0.0028(7) 0.0055(8) 0.0017(8) N1 0.0293(11) 0.0306(10) 0.0337(11) 0.0020(8) 0.0037(8) 0.0006(8) C1 0.0364(14) 0.0344(13) 0.0415(15) 0.0086(11) 0.0061(11) 0.0015(10) C2 0.077(2) 0.0394(16) 0.0543(19) 0.0028(14) 0.0021(17) -0.0083(14) C3 0.0553(19) 0.0480(17) 0.0528(19) 0.0099(13) -0.0061(15) 0.0024(13) C4 0.0281(14) 0.0378(14) 0.073(2) -0.0112(13) -0.0089(13) 0.0071(11) C5 0.079(3) 0.056(2) 0.089(3) -0.0096(18) -0.039(2) 0.0102(17) C6 0.0345(17) 0.077(2) 0.111(3) -0.018(2) 0.0175(19) -0.0078(16) C7 0.0466(17) 0.0458(15) 0.0418(16) 0.0127(12) -0.0076(13) -0.0145(12) C8 0.080(3) 0.098(3) 0.0330(17) 0.0110(17) 0.0063(16) -0.010(2) C9 0.057(2) 0.062(2) 0.085(3) 0.0123(18) -0.0042(19) 0.0094(16) C10 0.0607(19) 0.0385(14) 0.0348(15) -0.0083(11) 0.0058(13) 0.0041(12) C11 0.060(2) 0.0467(17) 0.088(3) -0.0222(17) -0.0127(19) 0.0114(15) C12 0.067(2) 0.059(2) 0.097(3) -0.028(2) -0.024(2) 0.0001(17) C13 0.0301(12) 0.0296(11) 0.0302(13) 0.0017(9) 0.0044(10) 0.0010(9) C14 0.0375(14) 0.0330(13) 0.0397(15) 0.0065(11) 0.0043(11) 0.0015(10) C15 0.0388(15) 0.0360(14) 0.0493(17) 0.0020(12) 0.0031(12) 0.0097(11) C16 0.0328(14) 0.0426(14) 0.0497(17) -0.0014(12) 0.0082(12) 0.0057(11) C17 0.0325(14) 0.0395(13) 0.0379(14) 0.0041(11) 0.0089(11) -0.0036(10) C18 0.0354(14) 0.0312(12) 0.0424(15) 0.0126(10) 0.0079(11) 0.0072(10) _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 Zn N1 2.0494(19) . ? Zn S1 2.3162(7) . ? Zn S3 2.3213(7) . ? Zn S2 2.6862(8) . ? Zn S4 2.8740(8) . ? S1 P1 2.0140(9) . ? S2 P1 1.9717(9) . ? S3 P2 2.0165(9) . ? S4 P2 1.9605(9) . ? P1 O1 1.5745(16) . ? P1 O2 1.5815(17) . ? P2 O3 1.5822(19) . ? P2 O4 1.5835(17) . ? O1 C1 1.474(3) . ? O2 C4 1.462(3) . ? O3 C7 1.465(3) . ? O4 C10 1.480(3) . ? N1 C13 1.355(3) . ? N1 C17 1.343(3) . ? C1 C2 1.508(4) . ? C1 C3 1.498(4) . ? C1 H1 0.9900 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 C5 1.499(4) . ? C4 C6 1.494(4) . ? C4 H4 0.9900 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 C8 1.492(4) . ? C7 C9 1.504(4) . ? C7 H7 0.9900 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 C11 1.483(4) . ? C10 C12 1.514(4) . ? C10 H10 0.9900 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 C14 1.396(3) . ? C13 C18 1.460(3) . ? C14 C15 1.374(4) . ? C14 H14 0.9400 . ? C15 C16 1.382(4) . ? C15 H15 0.9400 . ? C16 C17 1.372(3) . ? C16 H16 0.9400 . ? C17 H17 0.9400 . ? C18 C18 1.293(5) 3_556 ? C18 H18 0.9400 . ? 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 Zn S1 111.91(6) . . ? N1 Zn S3 118.25(6) . . ? S1 Zn S3 128.84(3) . . ? N1 Zn S2 93.06(6) . . ? S1 Zn S2 82.09(2) . . ? S3 Zn S2 104.05(2) . . ? N1 Zn S4 88.53(6) . . ? S1 Zn S4 94.49(2) . . ? S3 Zn S4 77.81(2) . . ? S2 Zn S4 176.57(2) . . ? P1 S1 Zn 86.02(3) . . ? P1 S2 Zn 77.30(3) . . ? P2 S3 Zn 86.47(3) . . ? P2 S4 Zn 73.37(3) . . ? O1 P1 O2 100.37(9) . . ? O1 P1 S2 108.10(7) . . ? O2 P1 S2 114.63(8) . . ? O1 P1 S1 111.67(8) . . ? O2 P1 S1 109.95(7) . . ? S2 P1 S1 111.61(4) . . ? O3 P2 O4 100.97(9) . . ? O3 P2 S4 114.10(8) . . ? O4 P2 S4 113.76(8) . . ? O3 P2 S3 109.68(8) . . ? O4 P2 S3 105.87(7) . . ? S4 P2 S3 111.68(4) . . ? C1 O1 P1 120.49(15) . . ? C4 O2 P1 123.65(15) . . ? C7 O3 P2 121.47(15) . . ? C10 O4 P2 120.53(15) . . ? C13 N1 C17 118.7(2) . . ? C13 N1 Zn 125.12(16) . . ? C17 N1 Zn 116.13(16) . . ? O1 C1 C2 107.3(2) . . ? O1 C1 C3 107.3(2) . . ? C2 C1 C3 114.1(2) . . ? O1 C1 H1 109.4 . . ? C2 C1 H1 109.4 . . ? C3 C1 H1 109.4 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O2 C4 C5 107.1(2) . . ? O2 C4 C6 106.9(2) . . ? C5 C4 C6 114.2(3) . . ? O2 C4 H4 109.5 . . ? C5 C4 H4 109.5 . . ? C6 C4 H4 109.5 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O3 C7 C8 107.1(2) . . ? O3 C7 C9 107.3(2) . . ? C8 C7 C9 113.2(3) . . ? O3 C7 H7 109.7 . . ? C8 C7 H7 109.7 . . ? C9 C7 H7 109.7 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 O4 108.3(2) . . ? C11 C10 C12 111.9(3) . . ? O4 C10 C12 107.3(2) . . ? C11 C10 H10 109.8 . . ? O4 C10 H10 109.8 . . ? C12 C10 H10 109.8 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C14 120.6(2) . . ? N1 C13 C18 116.8(2) . . ? C14 C13 C18 122.5(2) . . ? C13 C14 C15 119.7(2) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C14 C15 C16 119.4(2) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C17 C16 C15 118.6(2) . . ? C17 C16 H16 120.7 . . ? C15 C16 H16 120.7 . . ? C16 C17 N1 123.0(2) . . ? C16 C17 H17 118.5 . . ? N1 C17 H17 118.5 . . ? C18 C18 C13 127.6(3) 3_556 . ? C18 C18 H18 116.2 3_556 . ? C13 C18 H18 116.2 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.0 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.46 _refine_diff_density_min -0.62 _refine_diff_density_rms 0.075 # Attachment 'B513393A 3.cif' #============================================================================== # # {[Zn(iPr2dtp)2]2(pyrazine)0.5]2 # #============================================================================== data_shelxl_3 _database_code_depnum_ccdc_archive 'CCDC 284519' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H30 N O4 P2 S4 Zn' _chemical_formula_sum 'C14 H30 N O4 P2 S4 Zn' _chemical_formula_weight 531.94 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3237(14) _cell_length_b 11.2642(19) _cell_length_c 14.950(4) _cell_angle_alpha 77.797(3) _cell_angle_beta 73.836(3) _cell_angle_gamma 68.317(3) _cell_volume 1241.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 2494 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 26.3 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 554 _exptl_absorpt_coefficient_mu 1.472 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.720 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details '(SADABS, Bruker, 2000 & Blessing, 1995)' _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 11752 _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_av_sigmaI/netI 0.060 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.4 _diffrn_reflns_theta_max 30.1 _reflns_number_total 7146 _reflns_number_gt 4755 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction 'SHELXTL (Bruker, 2000)' _computing_structure_solution 'PATTY in DIRDIF92 (Beurskens et al., 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHEXLTL (Bruker, 2000)' _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^)+(0.1052P)^2^+0.6361P] 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 7146 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.101 _refine_ls_R_factor_gt 0.065 _refine_ls_wR_factor_ref 0.191 _refine_ls_wR_factor_gt 0.165 _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_restrained_S_all 1.02 _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 Zn Zn 0.13582(6) 0.07749(5) 0.18262(3) 0.04009(17) Uani 1 1 d . . . S1 S 0.23333(14) 0.04137(10) 0.32098(8) 0.0379(2) Uani 1 1 d . . . S2 S 0.06716(16) 0.30563(10) 0.18947(8) 0.0427(3) Uani 1 1 d . . . S3 S -0.09534(13) 0.04804(10) 0.15065(8) 0.0374(2) Uani 1 1 d . . . S4 S 0.23177(15) -0.23062(12) 0.18962(11) 0.0528(3) Uani 1 1 d . . . P1 P 0.19068(13) 0.23015(10) 0.29500(7) 0.0318(2) Uani 1 1 d . . . P2 P -0.02061(14) -0.14273(10) 0.19762(8) 0.0357(2) Uani 1 1 d . . . O1 O 0.3737(4) 0.2518(3) 0.2740(2) 0.0396(7) Uani 1 1 d . . . O2 O 0.0895(4) 0.3008(3) 0.3851(2) 0.0396(7) Uani 1 1 d . . . O3 O -0.1121(4) -0.1661(3) 0.3040(2) 0.0546(9) Uani 1 1 d . . . O4 O -0.1077(4) -0.1903(3) 0.1363(3) 0.0497(8) Uani 1 1 d . . . N1 N 0.3550(4) 0.0329(3) 0.0724(2) 0.0333(7) Uani 1 1 d . . . C1 C 0.3896(6) 0.3809(4) 0.2463(4) 0.0461(11) Uani 1 1 d . . . H1 H 0.2699 0.4455 0.2484 0.055 Uiso 1 1 calc R . . C2 C 0.4967(8) 0.3860(6) 0.1478(4) 0.0706(17) Uani 1 1 d . . . H2A H 0.4355 0.3723 0.1064 0.106 Uiso 1 1 calc R . . H2B H 0.6118 0.3194 0.1446 0.106 Uiso 1 1 calc R . . H2C H 0.5123 0.4696 0.1286 0.106 Uiso 1 1 calc R . . C3 C 0.4693(10) 0.4042(7) 0.3141(5) 0.083(2) Uani 1 1 d . . . H3A H 0.3927 0.4011 0.3762 0.124 Uiso 1 1 calc R . . H3B H 0.4836 0.4883 0.2964 0.124 Uiso 1 1 calc R . . H3C H 0.5842 0.3385 0.3147 0.124 Uiso 1 1 calc R . . C4 C -0.0992(6) 0.3217(5) 0.4234(4) 0.0523(12) Uani 1 1 d . . . H4 H -0.1430 0.2891 0.3816 0.063 Uiso 1 1 calc R . . C5 C -0.1222(9) 0.2467(8) 0.5161(6) 0.114(3) Uani 1 1 d . . . H5A H -0.0587 0.1562 0.5104 0.171 Uiso 1 1 calc R . . H5B H -0.2472 0.2596 0.5417 0.171 Uiso 1 1 calc R . . H5C H -0.0757 0.2748 0.5576 0.171 Uiso 1 1 calc R . . C6 C -0.1940(10) 0.4605(7) 0.4227(6) 0.112(3) Uani 1 1 d . . . H6A H -0.1735 0.5029 0.3590 0.168 Uiso 1 1 calc R . . H6B H -0.1511 0.4949 0.4621 0.168 Uiso 1 1 calc R . . H6C H -0.3199 0.4755 0.4464 0.168 Uiso 1 1 calc R . . C7 C -0.2980(6) -0.0983(5) 0.3412(4) 0.0598(14) Uani 1 1 d . . . H7 H -0.3600 -0.0576 0.2892 0.072 Uiso 1 1 calc R . . C8 C -0.3744(8) -0.2001(6) 0.4025(5) 0.080(2) Uani 1 1 d . . . H8A H -0.3673 -0.2619 0.3639 0.120 Uiso 1 1 calc R . . H8B H -0.4973 -0.1590 0.4320 0.120 Uiso 1 1 calc R . . H8C H -0.3071 -0.2440 0.4504 0.120 Uiso 1 1 calc R . . C9 C -0.3067(8) 0.0026(7) 0.3950(4) 0.0739(17) Uani 1 1 d . . . H9A H -0.2580 0.0651 0.3526 0.111 Uiso 1 1 calc R . . H9B H -0.2386 -0.0373 0.4431 0.111 Uiso 1 1 calc R . . H9C H -0.4292 0.0455 0.4243 0.111 Uiso 1 1 calc R . . C10 C -0.0734(6) -0.3262(4) 0.1338(4) 0.0477(11) Uani 1 1 d . . . H10 H -0.0313 -0.3769 0.1905 0.057 Uiso 1 1 calc R . . C11 C -0.2476(9) -0.3392(6) 0.1346(6) 0.085(2) Uani 1 1 d . . . H11A H -0.3318 -0.3131 0.1924 0.127 Uiso 1 1 calc R . . H11B H -0.2301 -0.4281 0.1306 0.127 Uiso 1 1 calc R . . H11C H -0.2931 -0.2848 0.0815 0.127 Uiso 1 1 calc R . . C12 C 0.0678(9) -0.3673(5) 0.0482(4) 0.0628(14) Uani 1 1 d . . . H12A H 0.1760 -0.3567 0.0522 0.094 Uiso 1 1 calc R . . H12B H 0.0290 -0.3148 -0.0072 0.094 Uiso 1 1 calc R . . H12C H 0.0898 -0.4570 0.0441 0.094 Uiso 1 1 calc R . . C13 C 0.3477(5) -0.0143(4) -0.0004(3) 0.0368(9) Uani 1 1 d . . . H13 H 0.2420 -0.0252 -0.0021 0.044 Uiso 1 1 calc R . . C14 C 0.5061(5) 0.0473(4) 0.0735(3) 0.0356(8) Uani 1 1 d . . . H14 H 0.5134 0.0802 0.1244 0.043 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.0297(2) 0.0603(3) 0.0361(3) -0.0166(2) -0.00320(19) -0.0186(2) S1 0.0443(6) 0.0342(5) 0.0379(5) -0.0009(4) -0.0144(4) -0.0141(4) S2 0.0503(6) 0.0374(5) 0.0441(6) 0.0006(4) -0.0225(5) -0.0131(5) S3 0.0295(5) 0.0368(5) 0.0495(6) -0.0045(4) -0.0146(4) -0.0112(4) S4 0.0366(6) 0.0462(6) 0.0753(9) -0.0053(6) -0.0204(6) -0.0088(5) P1 0.0305(5) 0.0331(5) 0.0338(5) -0.0054(4) -0.0076(4) -0.0114(4) P2 0.0351(5) 0.0353(5) 0.0384(6) -0.0080(4) -0.0056(4) -0.0134(4) O1 0.0289(14) 0.0380(15) 0.0504(18) -0.0040(13) -0.0071(12) -0.0112(12) O2 0.0361(15) 0.0448(16) 0.0412(16) -0.0153(13) -0.0041(12) -0.0151(12) O3 0.0396(17) 0.057(2) 0.048(2) -0.0004(16) -0.0012(14) -0.0032(15) O4 0.0513(18) 0.0359(16) 0.074(2) -0.0080(15) -0.0323(17) -0.0142(14) N1 0.0267(15) 0.0446(19) 0.0312(17) -0.0104(14) -0.0053(12) -0.0125(13) C1 0.037(2) 0.039(2) 0.063(3) -0.005(2) -0.011(2) -0.0139(18) C2 0.067(4) 0.060(3) 0.071(4) 0.005(3) 0.005(3) -0.027(3) C3 0.108(5) 0.076(4) 0.095(5) -0.008(4) -0.042(4) -0.052(4) C4 0.034(2) 0.066(3) 0.049(3) -0.015(2) -0.0021(19) -0.009(2) C5 0.059(4) 0.117(7) 0.109(6) 0.031(5) 0.021(4) -0.017(4) C6 0.086(5) 0.068(4) 0.128(7) -0.023(4) 0.025(5) 0.006(4) C7 0.035(2) 0.064(3) 0.061(3) 0.004(3) -0.001(2) -0.008(2) C8 0.048(3) 0.071(4) 0.087(5) 0.009(3) 0.013(3) -0.011(3) C9 0.064(4) 0.083(4) 0.058(4) -0.024(3) 0.007(3) -0.013(3) C10 0.053(3) 0.034(2) 0.064(3) -0.003(2) -0.023(2) -0.0191(19) C11 0.070(4) 0.054(3) 0.153(7) -0.018(4) -0.043(4) -0.030(3) C12 0.090(4) 0.054(3) 0.048(3) -0.011(2) -0.015(3) -0.026(3) C13 0.0290(18) 0.053(2) 0.034(2) -0.0101(18) -0.0076(15) -0.0171(17) C14 0.0320(19) 0.049(2) 0.032(2) -0.0113(17) -0.0056(15) -0.0180(17) _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 Zn N1 2.072(3) . ? Zn S3 2.2563(11) . ? Zn S1 2.3320(12) . ? Zn S2 2.4361(13) . ? Zn S4 3.2463(15) . ? S1 P1 1.9921(15) . ? S2 P1 1.9897(15) . ? S3 P2 2.0286(15) . ? S4 P2 1.9444(16) . ? P1 O1 1.567(3) . ? P1 O2 1.576(3) . ? P2 O3 1.573(3) . ? P2 O4 1.586(3) . ? O1 C1 1.470(5) . ? O2 C4 1.461(5) . ? O3 C7 1.454(5) . ? O4 C10 1.456(5) . ? N1 C14 1.331(5) . ? N1 C13 1.333(5) . ? C1 C3 1.466(8) . ? C1 C2 1.496(7) . ? C1 H1 0.9900 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 C6 1.468(8) . ? C4 C5 1.465(9) . ? C4 H4 0.9900 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 C9 1.497(9) . ? C7 C8 1.525(8) . ? C7 H7 0.9900 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 C11 1.507(7) . ? C10 C12 1.498(7) . ? C10 H10 0.9900 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 C14 1.382(5) 2_655 ? C13 H13 0.9400 . ? C14 C13 1.382(5) 2_655 ? C14 H14 0.9400 . ? 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 Zn S3 110.23(9) . . ? N1 Zn S1 108.67(9) . . ? S3 Zn S1 132.36(5) . . ? N1 Zn S2 104.41(10) . . ? S3 Zn S2 109.16(4) . . ? S1 Zn S2 86.29(4) . . ? N1 Zn S4 77.77(10) . . ? S3 Zn S4 73.22(4) . . ? S1 Zn S4 89.45(4) . . ? S2 Zn S4 175.65(4) . . ? P1 S1 Zn 82.64(5) . . ? P1 S2 Zn 80.04(5) . . ? P2 S3 Zn 94.27(5) . . ? P2 S4 Zn 69.45(5) . . ? O1 P1 O2 101.17(16) . . ? O1 P1 S2 112.52(13) . . ? O2 P1 S2 112.26(13) . . ? O1 P1 S1 108.11(12) . . ? O2 P1 S1 112.48(13) . . ? S2 P1 S1 109.99(6) . . ? O3 P2 O4 108.6(2) . . ? O3 P2 S4 105.66(14) . . ? O4 P2 S4 115.75(14) . . ? O3 P2 S3 110.52(14) . . ? O4 P2 S3 99.78(13) . . ? S4 P2 S3 116.37(7) . . ? C1 O1 P1 121.8(2) . . ? C4 O2 P1 121.0(3) . . ? C7 O3 P2 122.3(3) . . ? C10 O4 P2 122.4(3) . . ? C14 N1 C13 118.7(3) . . ? C14 N1 Zn 121.4(3) . . ? C13 N1 Zn 119.9(3) . . ? O1 C1 C3 108.1(4) . . ? O1 C1 C2 107.9(4) . . ? C3 C1 C2 113.6(5) . . ? O1 C1 H1 109.1 . . ? C3 C1 H1 109.1 . . ? C2 C1 H1 109.1 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O2 C4 C6 108.8(5) . . ? O2 C4 C5 109.1(4) . . ? C6 C4 C5 114.5(6) . . ? O2 C4 H4 108.1 . . ? C6 C4 H4 108.1 . . ? C5 C4 H4 108.1 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O3 C7 C9 107.8(5) . . ? O3 C7 C8 106.1(4) . . ? C9 C7 C8 113.0(5) . . ? O3 C7 H7 109.9 . . ? C9 C7 H7 109.9 . . ? C8 C7 H7 109.9 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O4 C10 C11 106.6(4) . . ? O4 C10 C12 108.3(4) . . ? C11 C10 C12 113.7(5) . . ? O4 C10 H10 109.4 . . ? C11 C10 H10 109.4 . . ? C12 C10 H10 109.4 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C14 120.6(4) . 2_655 ? N1 C13 H13 119.7 . . ? C14 C13 H13 119.7 2_655 . ? N1 C14 C13 120.7(4) . 2_655 ? N1 C14 H14 119.7 . . ? C13 C14 H14 119.7 2_655 . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 30.10 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 2.21 # # 0.87 \%A from S4 # _refine_diff_density_min -0.76 _refine_diff_density_rms 0.133 # Attachment 'revised B513393A 4.CIF' #============================================================================== # # {[Zn(iPr2dtp)2](4-NC5H4S2C5H4N-4)}n # #============================================================================== data_shelxl_8 _database_code_depnum_ccdc_archive 'CCDC 284520' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H36 N2 O4 P2 S6 Zn' _chemical_formula_sum 'C22 H36 N2 O4 P2 S6 Zn' _chemical_formula_weight 712.20 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Ccca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x, -y+1/2, z' 'x+1/2, y+1/2, z' '-x+1, y+1/2, z+1/2' 'x+1, -y+1, z+1/2' '-x+1/2, -y+1, z' '-x, -y, -z' 'x-1/2, -y, -z-1/2' '-x-1/2, y-1/2, -z-1/2' 'x, y-1/2, -z' '-x+1/2, -y+1/2, -z' 'x, -y+1/2, -z-1/2' '-x, y, -z-1/2' 'x+1/2, y, -z' _cell_length_a 21.988(5) _cell_length_b 35.283(7) _cell_length_c 17.564(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 13626(5) _cell_formula_units_Z 16 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4709 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 20.8 _exptl_crystal_description flat _exptl_crystal_colour colourless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5920 _exptl_absorpt_coefficient_mu 1.211 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.090 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details '(SADABS, Bruker, 2000 & Blessing, 1995)' _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 54255 _diffrn_reflns_av_R_equivalents 0.102 _diffrn_reflns_av_sigmaI/netI 0.086 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -48 _diffrn_reflns_limit_k_max 49 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.2 _diffrn_reflns_theta_max 30.0 _reflns_number_total 9885 _reflns_number_gt 4186 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction 'SHELXTL (Bruker, 2000)' _computing_structure_solution 'PATTY in DIRDIF92 (Beurskens et al., 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'Bruker SHEXLTL (Bruker, 2000)' _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^)+(0.2P)^2^] 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 9885 _refine_ls_number_parameters 287 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.212 _refine_ls_R_factor_gt 0.108 _refine_ls_wR_factor_ref 0.390 _refine_ls_wR_factor_gt 0.324 _refine_ls_goodness_of_fit_ref 1.14 _refine_ls_restrained_S_all 1.14 _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 Zn Zn 0.18613(4) 0.59473(2) 0.57656(5) 0.0587(3) Uani 1 1 d . . . S1 S 0.20231(11) 0.65690(7) 0.54661(19) 0.0919(8) Uani 1 1 d . A . S2 S 0.04843(13) 0.66487(8) 0.5698(2) 0.1047(10) Uani 1 1 d . A . S3 S 0.27394(10) 0.55847(7) 0.57691(13) 0.0763(6) Uani 1 1 d . . . S4 S 0.39481(12) 0.55526(8) 0.69269(18) 0.0970(9) Uani 1 1 d . . . S5 S -0.00174(9) 0.48745(6) 0.37585(12) 0.0714(6) Uani 1 1 d . . . S6 S 0.02448(10) 0.43278(6) 0.38502(12) 0.0703(6) Uani 1 1 d . . . P1 P 0.12258(13) 0.68314(8) 0.5276(2) 0.1029(10) Uani 1 1 d . . . P2 P 0.32106(8) 0.58171(7) 0.66322(14) 0.0673(6) Uani 1 1 d . . . O1 O 0.1347(4) 0.7251(2) 0.5216(6) 0.134(3) Uani 1 1 d D A . O3 O 0.2720(3) 0.5909(2) 0.7255(4) 0.112(3) Uani 1 1 d D . . O4 O 0.3364(3) 0.62461(17) 0.6371(4) 0.096(2) Uani 1 1 d D . . N1 N 0.1316(3) 0.56151(17) 0.5065(3) 0.0559(14) Uani 1 1 d . . . N2 N 0.1408(3) 0.41295(19) 0.1774(3) 0.0605(15) Uani 1 1 d . . . C1 C 0.1411(10) 0.7389(7) 0.6010(10) 0.218(9) Uiso 1 1 d D . . H1 H 0.1383 0.7172 0.6366 0.261 Uiso 1 1 calc R A . C2 C 0.0967(12) 0.7693(8) 0.6247(14) 0.270(13) Uiso 1 1 d D A . H2A H 0.0557 0.7592 0.6240 0.405 Uiso 1 1 calc R . . H2B H 0.0994 0.7905 0.5897 0.405 Uiso 1 1 calc R . . H2C H 0.1065 0.7779 0.6758 0.405 Uiso 1 1 calc R . . C3 C 0.2005(11) 0.7593(9) 0.6130(15) 0.278(13) Uiso 1 1 d D A . H3A H 0.2340 0.7422 0.6027 0.417 Uiso 1 1 calc R . . H3B H 0.2029 0.7681 0.6652 0.417 Uiso 1 1 calc R . . H3C H 0.2028 0.7809 0.5787 0.417 Uiso 1 1 calc R . . O2' O 0.1188(5) 0.6772(3) 0.4331(5) 0.145(4) Uani 0.77(2) 1 d P A 1 C4' C 0.068(2) 0.6932(9) 0.388(3) 0.45(5) Uiso 0.77(2) 1 d PD A 1 H4' H 0.0963 0.6995 0.3455 0.545 Uiso 0.77(2) 1 calc PR A 1 C5' C 0.0435(18) 0.7328(8) 0.389(2) 0.31(2) Uiso 0.77(2) 1 d PD A 1 H5'1 H 0.0703 0.7490 0.4181 0.471 Uiso 0.77(2) 1 calc PR A 1 H5'2 H 0.0033 0.7327 0.4115 0.471 Uiso 0.77(2) 1 calc PR A 1 H5'3 H 0.0409 0.7423 0.3369 0.471 Uiso 0.77(2) 1 calc PR A 1 C6' C 0.0426(13) 0.6600(7) 0.3441(17) 0.177(10) Uiso 0.77(2) 1 d PD A 1 H6'1 H 0.0669 0.6376 0.3542 0.265 Uiso 0.77(2) 1 calc PR A 1 H6'2 H 0.0435 0.6656 0.2900 0.265 Uiso 0.77(2) 1 calc PR A 1 H6'3 H 0.0010 0.6555 0.3600 0.265 Uiso 0.77(2) 1 calc PR A 1 O2 O 0.1188(5) 0.6772(3) 0.4331(5) 0.145(4) Uani 0.23(2) 1 d PD A 2 C4 C 0.0685(9) 0.6882(7) 0.3825(13) 0.047(9) Uiso 0.23(2) 1 d PD A 2 H4 H 0.0272 0.6899 0.4047 0.057 Uiso 0.23(2) 1 calc PR A 2 C5 C 0.077(7) 0.663(4) 0.314(5) 0.29(8) Uiso 0.23(2) 1 d PD A 2 H5A H 0.0736 0.6368 0.3295 0.431 Uiso 0.23(2) 1 calc PR A 2 H5B H 0.1173 0.6675 0.2928 0.431 Uiso 0.23(2) 1 calc PR A 2 H5C H 0.0465 0.6689 0.2764 0.431 Uiso 0.23(2) 1 calc PR A 2 C6 C 0.087(2) 0.7177(11) 0.326(2) 0.095(17) Uiso 0.23(2) 1 d PD A 2 H6A H 0.0953 0.7414 0.3517 0.143 Uiso 0.23(2) 1 calc PR A 2 H6B H 0.0542 0.7215 0.2893 0.143 Uiso 0.23(2) 1 calc PR A 2 H6C H 0.1231 0.7094 0.2988 0.143 Uiso 0.23(2) 1 calc PR A 2 C7 C 0.2846(8) 0.6106(4) 0.7992(7) 0.158(6) Uiso 1 1 d D . . H7 H 0.3292 0.6119 0.8066 0.189 Uiso 1 1 calc R . . C8 C 0.2589(9) 0.5813(5) 0.8531(10) 0.171(7) Uiso 1 1 d D . . H8A H 0.2818 0.5580 0.8484 0.257 Uiso 1 1 calc R . . H8B H 0.2166 0.5766 0.8405 0.257 Uiso 1 1 calc R . . H8C H 0.2618 0.5906 0.9050 0.257 Uiso 1 1 calc R . . C9 C 0.2594(8) 0.6505(5) 0.7993(12) 0.193(8) Uiso 1 1 d D . . H9A H 0.2824 0.6660 0.7640 0.290 Uiso 1 1 calc R . . H9B H 0.2624 0.6611 0.8501 0.290 Uiso 1 1 calc R . . H9C H 0.2171 0.6499 0.7837 0.290 Uiso 1 1 calc R . . C10 C 0.3893(6) 0.6341(4) 0.5873(7) 0.131(5) Uiso 1 1 d D . . H10 H 0.4277 0.6212 0.6015 0.157 Uiso 1 1 calc R . . C11 C 0.3753(9) 0.6332(6) 0.5048(8) 0.195(8) Uiso 1 1 d D . . H11A H 0.3536 0.6100 0.4927 0.293 Uiso 1 1 calc R . . H11B H 0.4129 0.6341 0.4759 0.293 Uiso 1 1 calc R . . H11C H 0.3503 0.6549 0.4917 0.293 Uiso 1 1 calc R . . C12 C 0.3866(16) 0.6757(6) 0.6095(16) 0.36(2) Uiso 1 1 d D . . H12A H 0.3970 0.6784 0.6629 0.544 Uiso 1 1 calc R . . H12B H 0.3458 0.6853 0.6009 0.544 Uiso 1 1 calc R . . H12C H 0.4153 0.6899 0.5788 0.544 Uiso 1 1 calc R . . C13 C 0.0840(4) 0.5752(2) 0.4684(5) 0.067(2) Uani 1 1 d . . . H13 H 0.0769 0.6014 0.4691 0.080 Uiso 1 1 calc R . . C14 C 0.0450(4) 0.5525(2) 0.4283(5) 0.071(2) Uani 1 1 d . . . H14 H 0.0119 0.5634 0.4024 0.085 Uiso 1 1 calc R . . C15 C 0.0539(3) 0.5138(2) 0.4256(4) 0.0596(18) Uani 1 1 d . . . C16 C 0.1044(4) 0.4985(2) 0.4636(4) 0.0607(18) Uani 1 1 d . . . H16 H 0.1126 0.4723 0.4628 0.073 Uiso 1 1 calc R . . C17 C 0.1419(4) 0.5238(2) 0.5026(4) 0.0653(19) Uani 1 1 d . . . H17 H 0.1763 0.5140 0.5276 0.078 Uiso 1 1 calc R . . C18 C 0.0713(3) 0.4265(2) 0.3038(4) 0.0572(17) Uani 1 1 d . . . C19 C 0.0822(4) 0.3895(2) 0.2797(5) 0.070(2) Uani 1 1 d . . . H19 H 0.0666 0.3688 0.3073 0.083 Uiso 1 1 calc R . . C20 C 0.1155(4) 0.3837(3) 0.2163(5) 0.070(2) Uani 1 1 d . . . H20 H 0.1213 0.3588 0.1987 0.085 Uiso 1 1 calc R . . C21 C 0.1333(3) 0.4474(2) 0.2019(4) 0.0606(18) Uani 1 1 d . . . H21 H 0.1522 0.4673 0.1753 0.073 Uiso 1 1 calc R . . C22 C 0.0987(3) 0.4561(2) 0.2655(5) 0.0634(19) Uani 1 1 d . . . H22 H 0.0940 0.4813 0.2820 0.076 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.0501(5) 0.0580(6) 0.0681(6) -0.0057(4) -0.0003(4) -0.0057(4) S1 0.0687(14) 0.0577(13) 0.149(2) 0.0044(13) 0.0100(15) -0.0091(10) S2 0.0678(15) 0.0889(18) 0.157(3) 0.0095(17) -0.0026(16) 0.0139(13) S3 0.0595(12) 0.0795(14) 0.0899(15) -0.0277(11) 0.0011(10) 0.0053(10) S4 0.0716(15) 0.0835(17) 0.136(2) 0.0114(15) -0.0164(15) 0.0159(12) S5 0.0560(11) 0.0814(14) 0.0767(13) -0.0163(11) -0.0016(9) -0.0105(10) S6 0.0643(12) 0.0725(13) 0.0740(13) -0.0030(10) 0.0082(10) -0.0147(10) P1 0.0822(18) 0.0715(16) 0.155(3) 0.0360(17) -0.0207(17) 0.0002(13) P2 0.0386(10) 0.0789(14) 0.0845(15) -0.0104(11) 0.0026(9) 0.0014(9) O1 0.127(7) 0.080(5) 0.195(9) 0.017(5) 0.006(6) 0.002(5) O3 0.064(4) 0.197(8) 0.075(4) -0.033(4) -0.008(3) 0.003(4) O4 0.071(4) 0.067(4) 0.150(6) -0.008(4) -0.005(4) 0.004(3) N1 0.053(3) 0.058(4) 0.057(3) -0.001(3) -0.006(3) -0.007(3) N2 0.045(3) 0.070(4) 0.067(4) 0.014(3) -0.001(3) -0.001(3) O2' 0.135(8) 0.170(10) 0.131(7) 0.030(6) -0.025(6) 0.005(7) O2 0.135(8) 0.170(10) 0.131(7) 0.030(6) -0.025(6) 0.005(7) C13 0.062(5) 0.063(5) 0.075(5) -0.003(4) -0.008(4) -0.003(4) C14 0.051(4) 0.078(6) 0.083(6) -0.012(4) -0.009(4) 0.011(4) C15 0.049(4) 0.075(5) 0.055(4) -0.006(3) 0.004(3) -0.009(3) C16 0.069(5) 0.059(4) 0.055(4) -0.008(3) 0.001(3) -0.007(4) C17 0.059(4) 0.066(5) 0.071(5) -0.001(4) -0.010(4) -0.007(4) C18 0.044(4) 0.072(5) 0.056(4) 0.006(4) -0.002(3) -0.004(3) C19 0.077(5) 0.057(5) 0.075(5) 0.006(4) -0.006(4) -0.005(4) C20 0.060(5) 0.074(5) 0.077(5) 0.005(4) 0.006(4) -0.004(4) C21 0.045(4) 0.071(5) 0.065(5) 0.012(4) 0.004(3) 0.008(3) C22 0.053(4) 0.065(5) 0.072(5) -0.003(4) 0.003(3) 0.002(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 Zn N2 2.051(6) 7_455 ? Zn N1 2.080(6) . ? Zn S1 2.284(3) . ? Zn S3 2.316(2) . ? Zn S2 3.912(3) . ? Zn S4 5.211(3) . ? S1 P1 2.011(4) . ? S2 P1 1.904(4) . ? S3 P2 2.011(3) . ? S4 P2 1.941(3) . ? S5 C15 1.769(7) . ? S5 S6 2.020(3) . ? S6 C18 1.774(7) . ? P1 O1 1.508(8) . ? P1 O2 1.674(10) . ? P1 O2' 1.674(10) . ? P2 O3 1.570(7) . ? P2 O4 1.617(7) . ? O1 C1 1.483(9) . ? O3 C7 1.495(9) . ? O4 C10 1.493(9) . ? N1 C13 1.333(9) . ? N1 C17 1.352(10) . ? N2 C21 1.300(10) . ? N2 C20 1.356(10) . ? N2 Zn 2.051(6) 7_454 ? C1 C2 1.510(10) . ? C1 C3 1.506(10) . ? C1 H1 0.9900 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? O2' C4' 1.478(10) . ? C4' C5' 1.501(10) . ? C4' C6' 1.509(10) . ? C4' H4' 0.9900 . ? C5' H5'1 0.9700 . ? C5' H5'2 0.9700 . ? C5' H5'3 0.9700 . ? C6' H6'1 0.9700 . ? C6' H6'2 0.9700 . ? C6' H6'3 0.9700 . ? O2 C4 1.472(10) . ? C4 C5 1.502(10) . ? C4 C6 1.501(10) . ? C4 H4 0.9900 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 C8 1.511(9) . ? C7 C9 1.513(9) . ? C7 H7 0.9900 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 C11 1.482(9) . ? C10 C12 1.519(10) . ? C10 H10 0.9900 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 C14 1.366(11) . ? C13 H13 0.9400 . ? C14 C15 1.381(11) . ? C14 H14 0.9400 . ? C15 C16 1.404(11) . ? C16 C17 1.395(10) . ? C16 H16 0.9400 . ? C17 H17 0.9400 . ? C18 C19 1.394(11) . ? C18 C22 1.380(10) . ? C19 C20 1.347(12) . ? C19 H19 0.9400 . ? C20 H20 0.9400 . ? C21 C22 1.386(11) . ? C21 H21 0.9400 . ? C22 H22 0.9400 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Zn N1 99.0(2) 7_455 . ? N2 Zn S1 113.7(2) 7_455 . ? N1 Zn S1 119.66(19) . . ? N2 Zn S3 109.29(19) 7_455 . ? N1 Zn S3 99.82(18) . . ? S1 Zn S3 113.66(10) . . ? N2 Zn S2 74.53(19) 7_455 . ? N1 Zn S2 83.84(18) . . ? S1 Zn S2 60.39(8) . . ? S3 Zn S2 174.05(8) . . ? N2 Zn S4 93.15(18) 7_455 . ? N1 Zn S4 126.04(17) . . ? S1 Zn S4 102.10(8) . . ? S3 Zn S4 28.03(6) . . ? S2 Zn S4 149.59(6) . . ? P1 S1 Zn 110.17(13) . . ? P1 S2 Zn 64.10(11) . . ? P2 S3 Zn 101.90(11) . . ? P2 S4 Zn 14.45(9) . . ? C15 S5 S6 105.4(3) . . ? C18 S6 S5 102.8(3) . . ? O1 P1 O2 93.6(6) . . ? O1 P1 O2' 93.6(6) . . ? O1 P1 S2 120.7(4) . . ? O2 P1 S2 107.5(4) . . ? O2' P1 S2 107.5(4) . . ? O1 P1 S1 108.1(4) . . ? O2 P1 S1 98.6(4) . . ? O2' P1 S1 98.6(4) . . ? S2 P1 S1 121.74(18) . . ? O3 P2 O4 98.5(4) . . ? O3 P2 S4 119.2(3) . . ? O4 P2 S4 110.6(3) . . ? O3 P2 S3 104.8(3) . . ? O4 P2 S3 106.0(3) . . ? S4 P2 S3 115.80(16) . . ? P1 O1 C1 105.9(12) . . ? C7 O3 P2 124.9(8) . . ? C10 O4 P2 122.6(7) . . ? C13 N1 C17 117.5(6) . . ? C13 N1 Zn 123.1(5) . . ? C17 N1 Zn 119.3(5) . . ? C21 N2 C20 119.5(7) . . ? C21 N2 Zn 118.1(5) . 7_454 ? C20 N2 Zn 122.3(6) . 7_454 ? C2 C1 O1 115.6(18) . . ? C2 C1 C3 100(2) . . ? O1 C1 C3 111.8(19) . . ? C2 C1 H1 109.6 . . ? O1 C1 H1 109.6 . . ? C3 C1 H1 109.6 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C4' O2' P1 122(3) . . ? C5' C4' O2' 129(2) . . ? C5' C4' C6' 126(2) . . ? O2' C4' C6' 105.0(19) . . ? C5' C4' H4' 91.4 . . ? O2' C4' H4' 91.4 . . ? C6' C4' H4' 91.4 . . ? C4' C5' H5'1 109.5 . . ? C4' C5' H5'2 109.5 . . ? H5'1 C5' H5'2 109.5 . . ? C4' C5' H5'3 109.5 . . ? H5'1 C5' H5'3 109.5 . . ? H5'2 C5' H5'3 109.5 . . ? C4' C6' H6'1 109.5 . . ? C4' C6' H6'2 109.5 . . ? H6'1 C6' H6'2 109.5 . . ? C4' C6' H6'3 109.5 . . ? H6'1 C6' H6'3 109.5 . . ? H6'2 C6' H6'3 109.5 . . ? C4 O2 P1 127.0(13) . . ? C5 C4 C6 81(6) . . ? C5 C4 O2 103(6) . . ? C6 C4 O2 113(2) . . ? C5 C4 H4 117.9 . . ? C6 C4 H4 117.9 . . ? O2 C4 H4 117.9 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 O3 99.0(11) . . ? C8 C7 C9 119.9(15) . . ? O3 C7 C9 111.4(13) . . ? C8 C7 H7 108.7 . . ? O3 C7 H7 108.7 . . ? C9 C7 H7 108.7 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 O4 114.0(12) . . ? C11 C10 C12 105.3(9) . . ? O4 C10 C12 92.1(16) . . ? C11 C10 H10 114.4 . . ? O4 C10 H10 114.4 . . ? C12 C10 H10 114.4 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C14 122.7(7) . . ? N1 C13 H13 118.6 . . ? C14 C13 H13 118.6 . . ? C15 C14 C13 120.4(7) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 118.6(7) . . ? C14 C15 S5 116.0(6) . . ? C16 C15 S5 125.4(6) . . ? C15 C16 C17 116.9(7) . . ? C15 C16 H16 121.5 . . ? C17 C16 H16 121.5 . . ? N1 C17 C16 123.8(7) . . ? N1 C17 H17 118.1 . . ? C16 C17 H17 118.1 . . ? C19 C18 C22 119.1(7) . . ? C19 C18 S6 117.5(6) . . ? C22 C18 S6 123.4(6) . . ? C20 C19 C18 119.0(8) . . ? C20 C19 H19 120.5 . . ? C18 C19 H19 120.5 . . ? N2 C20 C19 121.6(8) . . ? N2 C20 H20 119.2 . . ? C19 C20 H20 119.2 . . ? N2 C21 C22 122.9(7) . . ? N2 C21 H21 118.6 . . ? C22 C21 H21 118.6 . . ? C21 C22 C18 117.7(8) . . ? C21 C22 H22 121.2 . . ? C18 C22 H22 121.2 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.0 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.41 # # 1.04 A from S5 # _refine_diff_density_min -0.64 _refine_diff_density_rms 0.210 # Attachment 'B513393A 5.cif' #============================================================================== # # {[Zn(iPr2dtp)2](4-NC5H4(CH2)3C5H4N-4)}n # #============================================================================== data_shelxl_4 _database_code_depnum_ccdc_archive 'CCDC 284521' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H42 N2 O4 P2 S4 Zn' _chemical_formula_sum 'C25 H42 N2 O4 P2 S4 Zn' _chemical_formula_weight 690.16 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.5675(6) _cell_length_b 23.9914(7) _cell_length_c 16.1405(5) _cell_angle_alpha 90 _cell_angle_beta 103.262(1) _cell_angle_gamma 90 _cell_volume 6998.2(4) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 9464 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 25.2 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.310 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2896 _exptl_absorpt_coefficient_mu 1.062 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.627 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details '(SADABS, Bruker, 2000 & Blessing, 1995)' _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 59094 _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_av_sigmaI/netI 0.058 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.1 _diffrn_reflns_theta_max 30.1 _reflns_number_total 20496 _reflns_number_gt 11846 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction 'SHELXTL (Bruker, 2000)' _computing_structure_solution 'PATTY in DIRDIF92 (Beurskens et al., 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'Bruker SHEXLTL (Bruker, 2000)' _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^)+(0.1013P)^2^+6.1193P] 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 20496 _refine_ls_number_parameters 683 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.124 _refine_ls_R_factor_gt 0.074 _refine_ls_wR_factor_ref 0.223 _refine_ls_wR_factor_gt 0.192 _refine_ls_goodness_of_fit_ref 1.06 _refine_ls_restrained_S_all 1.06 _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 0.58280(3) 0.629092(19) 0.75813(3) 0.04655(13) Uani 1 1 d . . . Zn2 Zn -0.06248(2) 0.63339(2) 0.20502(3) 0.04539(13) Uani 1 1 d . . . S1 S 0.66781(8) 0.57900(5) 0.85714(8) 0.0672(4) Uani 1 1 d . . . S2 S 0.65198(7) 0.49197(5) 0.68650(7) 0.0607(3) Uani 1 1 d . . . S3 S 0.54147(9) 0.68585(8) 0.85276(11) 0.0980(6) Uani 1 1 d . . . S4 S 0.41827(11) 0.72299(9) 0.67486(14) 0.1143(7) Uani 1 1 d . . . S5 S -0.15616(8) 0.57529(7) 0.13529(8) 0.0755(4) Uani 1 1 d . . . S6 S -0.18849(8) 0.57687(9) 0.33404(8) 0.0918(5) Uani 1 1 d . . . S7 S -0.01365(6) 0.66110(4) 0.09152(6) 0.0485(2) Uani 1 1 d . . . S8 S 0.09997(7) 0.73766(6) 0.24318(8) 0.0679(3) Uani 1 1 d . . . P1 P 0.69380(6) 0.50731(4) 0.80601(7) 0.0471(2) Uani 1 1 d . . . P2 P 0.47083(9) 0.74174(6) 0.78720(13) 0.0868(5) Uani 1 1 d . . . P3 P -0.21469(7) 0.54842(5) 0.21914(8) 0.0559(3) Uani 1 1 d . A . P4 P 0.03287(6) 0.73526(5) 0.13209(7) 0.0463(2) Uani 1 1 d . . . O1 O 0.78035(18) 0.50530(16) 0.8214(2) 0.0717(10) Uani 1 1 d . . . O2 O 0.6727(3) 0.46311(14) 0.8688(2) 0.0851(12) Uani 1 1 d . . . O3 O 0.5171(5) 0.7960(2) 0.7828(7) 0.225(5) Uani 1 1 d . . . O4 O 0.4250(2) 0.76322(19) 0.8533(3) 0.1055(15) Uani 1 1 d . . . O5 O -0.29829(17) 0.56179(15) 0.1805(2) 0.0665(8) Uani 1 1 d . . . O6 O -0.2220(3) 0.48194(17) 0.2089(3) 0.1026(14) Uani 1 1 d . . . O7 O 0.06819(17) 0.75841(13) 0.05815(19) 0.0567(7) Uani 1 1 d . . . O8 O -0.03574(16) 0.77599(12) 0.12168(19) 0.0541(7) Uani 1 1 d . . . N1 N 0.02114(17) 0.59374(14) 0.29040(19) 0.0445(7) Uani 1 1 d . . . N2 N 0.49883(17) 0.58482(13) 0.68564(19) 0.0406(7) Uani 1 1 d . . . N3 N -0.10181(18) 0.69382(15) 0.27015(19) 0.0485(8) Uani 1 1 d . . . N4 N -0.36760(18) 0.66508(14) 0.6694(2) 0.0504(8) Uani 1 1 d . . . C1 C 0.8326(3) 0.5219(2) 0.9001(3) 0.0678(13) Uani 1 1 d . . . H1 H 0.8061 0.5433 0.9364 0.081 Uiso 1 1 calc R . . C2 C 0.8887(4) 0.5583(3) 0.8747(4) 0.0955(19) Uani 1 1 d . . . H2A H 0.8647 0.5915 0.8467 0.143 Uiso 1 1 calc R . . H2B H 0.9122 0.5383 0.8358 0.143 Uiso 1 1 calc R . . H2C H 0.9258 0.5691 0.9249 0.143 Uiso 1 1 calc R . . C3 C 0.8654(4) 0.4708(3) 0.9460(4) 0.109(2) Uani 1 1 d . . . H3A H 0.8269 0.4491 0.9623 0.164 Uiso 1 1 calc R . . H3B H 0.9023 0.4813 0.9965 0.164 Uiso 1 1 calc R . . H3C H 0.8886 0.4486 0.9090 0.164 Uiso 1 1 calc R . . C4 C 0.6443(3) 0.4074(2) 0.8465(3) 0.0693(13) Uani 1 1 d . . . H4 H 0.6181 0.4063 0.7857 0.083 Uiso 1 1 calc R . . C5 C 0.7048(5) 0.3675(3) 0.8620(7) 0.156(4) Uani 1 1 d . . . H5A H 0.7385 0.3763 0.8260 0.233 Uiso 1 1 calc R . . H5B H 0.6852 0.3302 0.8491 0.233 Uiso 1 1 calc R . . H5C H 0.7310 0.3693 0.9213 0.233 Uiso 1 1 calc R . . C6 C 0.5924(6) 0.3948(4) 0.8996(6) 0.148(4) Uani 1 1 d . . . H6A H 0.5514 0.4209 0.8869 0.222 Uiso 1 1 calc R . . H6B H 0.6175 0.3979 0.9591 0.222 Uiso 1 1 calc R . . H6C H 0.5738 0.3571 0.8880 0.222 Uiso 1 1 calc R . . C7 C 0.5454(5) 0.8354(4) 0.8260(5) 0.129(3) Uani 1 1 d . . . H7 H 0.5776 0.8134 0.8719 0.155 Uiso 1 1 calc R . . C8 C 0.6079(6) 0.8588(4) 0.7863(8) 0.187(5) Uani 1 1 d . . . H8A H 0.6253 0.8297 0.7541 0.281 Uiso 1 1 calc R . . H8B H 0.6485 0.8717 0.8313 0.281 Uiso 1 1 calc R . . H8C H 0.5888 0.8896 0.7488 0.281 Uiso 1 1 calc R . . C9 C 0.5202(4) 0.8740(3) 0.8794(6) 0.116(3) Uani 1 1 d . . . H9A H 0.4820 0.8568 0.9029 0.174 Uiso 1 1 calc R . . H9B H 0.5000 0.9066 0.8464 0.174 Uiso 1 1 calc R . . H9C H 0.5611 0.8852 0.9253 0.174 Uiso 1 1 calc R . . C10 C 0.3506(5) 0.7500(5) 0.8503(6) 0.152(4) Uani 1 1 d . . . H10 H 0.3249 0.7419 0.7907 0.182 Uiso 1 1 calc R . . C11 C 0.3396(11) 0.7059(6) 0.9017(14) 0.359(15) Uani 1 1 d . . . H11A H 0.3561 0.6715 0.8803 0.539 Uiso 1 1 calc R . . H11B H 0.2875 0.7030 0.9014 0.539 Uiso 1 1 calc R . . H11C H 0.3678 0.7122 0.9595 0.539 Uiso 1 1 calc R . . C12 C 0.3189(7) 0.8073(7) 0.8796(9) 0.247(8) Uani 1 1 d . . . H12A H 0.3284 0.8375 0.8436 0.371 Uiso 1 1 calc R . . H12B H 0.3432 0.8152 0.9383 0.371 Uiso 1 1 calc R . . H12C H 0.2660 0.8039 0.8746 0.371 Uiso 1 1 calc R . . C13 C -0.3367(3) 0.5528(3) 0.0910(3) 0.0778(15) Uani 1 1 d . . . H13 H -0.3005 0.5439 0.0565 0.093 Uiso 1 1 calc R . . C14 C -0.3894(4) 0.5052(4) 0.0884(5) 0.130(3) Uani 1 1 d . . . H14A H -0.3618 0.4714 0.1072 0.195 Uiso 1 1 calc R . . H14B H -0.4182 0.5003 0.0306 0.195 Uiso 1 1 calc R . . H14C H -0.4223 0.5132 0.1256 0.195 Uiso 1 1 calc R . . C15 C -0.3757(4) 0.6060(4) 0.0611(5) 0.122(3) Uani 1 1 d . . . H15A H -0.3395 0.6351 0.0608 0.183 Uiso 1 1 calc R . . H15B H -0.4070 0.6164 0.0991 0.183 Uiso 1 1 calc R . . H15C H -0.4059 0.6010 0.0040 0.183 Uiso 1 1 calc R . . C16 C -0.1714(6) 0.4395(5) 0.2329(6) 0.079(3) Uiso 0.636(13) 1 d P A 1 H16 H -0.1245 0.4547 0.2675 0.094 Uiso 0.636(13) 1 calc PR A 1 C17 C -0.2021(11) 0.3988(8) 0.2825(12) 0.173(8) Uiso 0.636(13) 1 d P A 1 H17A H -0.2137 0.4169 0.3315 0.260 Uiso 0.636(13) 1 calc PR A 1 H17B H -0.1661 0.3694 0.3015 0.260 Uiso 0.636(13) 1 calc PR A 1 H17C H -0.2468 0.3828 0.2473 0.260 Uiso 0.636(13) 1 calc PR A 1 C18 C -0.1574(9) 0.4077(6) 0.1651(9) 0.123(5) Uiso 0.636(13) 1 d P A 1 H18A H -0.1366 0.4315 0.1278 0.185 Uiso 0.636(13) 1 calc PR A 1 H18B H -0.2033 0.3915 0.1332 0.185 Uiso 0.636(13) 1 calc PR A 1 H18C H -0.1226 0.3782 0.1874 0.185 Uiso 0.636(13) 1 calc PR A 1 C16' C -0.1383(14) 0.4626(10) 0.2457(14) 0.106(7) Uiso 0.364(13) 1 d P A 2 H16' H -0.1073 0.4965 0.2587 0.127 Uiso 0.364(13) 1 calc PR A 2 C17' C -0.1419(15) 0.4327(11) 0.3364(16) 0.136(10) Uiso 0.364(13) 1 d P A 2 H17D H -0.1626 0.4586 0.3709 0.204 Uiso 0.364(13) 1 calc PR A 2 H17E H -0.0924 0.4222 0.3666 0.204 Uiso 0.364(13) 1 calc PR A 2 H17F H -0.1728 0.3998 0.3253 0.204 Uiso 0.364(13) 1 calc PR A 2 C18' C -0.1080(16) 0.4284(11) 0.1897(16) 0.128(9) Uiso 0.364(13) 1 d P A 2 H18D H -0.1079 0.4489 0.1379 0.192 Uiso 0.364(13) 1 calc PR A 2 H18E H -0.1379 0.3950 0.1758 0.192 Uiso 0.364(13) 1 calc PR A 2 H18F H -0.0578 0.4180 0.2173 0.192 Uiso 0.364(13) 1 calc PR A 2 C19 C 0.1421(3) 0.7426(3) 0.0493(4) 0.091(2) Uani 1 1 d . . . H19 H 0.1702 0.7250 0.1024 0.109 Uiso 1 1 calc R . . C20 C 0.1352(4) 0.7037(3) -0.0224(4) 0.101(2) Uani 1 1 d . . . H20A H 0.1128 0.6692 -0.0093 0.151 Uiso 1 1 calc R . . H20B H 0.1839 0.6959 -0.0320 0.151 Uiso 1 1 calc R . . H20C H 0.1045 0.7202 -0.0732 0.151 Uiso 1 1 calc R . . C21 C 0.1787(7) 0.7950(6) 0.0328(10) 0.265(10) Uani 1 1 d . . . H21A H 0.1846 0.8193 0.0818 0.397 Uiso 1 1 calc R . . H21B H 0.1486 0.8134 -0.0167 0.397 Uiso 1 1 calc R . . H21C H 0.2270 0.7865 0.0223 0.397 Uiso 1 1 calc R . . C22 C -0.0230(3) 0.83557(19) 0.1393(3) 0.0652(12) Uani 1 1 d . . . H22 H 0.0303 0.8427 0.1628 0.078 Uiso 1 1 calc R . . C23 C -0.0669(4) 0.8515(3) 0.2034(4) 0.095(2) Uani 1 1 d . . . H23A H -0.0474 0.8320 0.2564 0.143 Uiso 1 1 calc R . . H23B H -0.1183 0.8413 0.1818 0.143 Uiso 1 1 calc R . . H23C H -0.0632 0.8914 0.2132 0.143 Uiso 1 1 calc R . . C24 C -0.0489(5) 0.8657(2) 0.0566(4) 0.103(2) Uani 1 1 d . . . H24A H -0.0183 0.8553 0.0178 0.155 Uiso 1 1 calc R . . H24B H -0.0453 0.9056 0.0665 0.155 Uiso 1 1 calc R . . H24C H -0.1000 0.8559 0.0318 0.155 Uiso 1 1 calc R . . C25 C 0.0869(2) 0.5886(2) 0.2725(3) 0.0593(11) Uani 1 1 d . . . H25 H 0.0955 0.6072 0.2244 0.071 Uiso 1 1 calc R . . C26 C 0.1433(2) 0.5573(2) 0.3209(3) 0.0576(11) Uani 1 1 d . . . H26 H 0.1894 0.5553 0.3062 0.069 Uiso 1 1 calc R . . C27 C 0.1320(2) 0.52883(16) 0.3914(3) 0.0463(9) Uani 1 1 d . . . C28 C 0.0645(2) 0.5361(2) 0.4115(3) 0.0575(11) Uani 1 1 d . . . H28 H 0.0554 0.5193 0.4607 0.069 Uiso 1 1 calc R . . C29 C 0.0101(2) 0.56789(19) 0.3602(3) 0.0550(10) Uani 1 1 d . . . H29 H -0.0360 0.5715 0.3746 0.066 Uiso 1 1 calc R . . C30 C 0.1920(2) 0.49310(17) 0.4429(3) 0.0532(10) Uani 1 1 d . . . H30A H 0.2105 0.4680 0.4045 0.064 Uiso 1 1 calc R . . H30B H 0.1711 0.4701 0.4816 0.064 Uiso 1 1 calc R . . C31 C 0.2569(2) 0.52658(16) 0.4949(3) 0.0465(9) Uani 1 1 d . . . H31A H 0.2755 0.5521 0.4571 0.056 Uiso 1 1 calc R . . H31B H 0.2399 0.5490 0.5374 0.056 Uiso 1 1 calc R . . C32 C 0.3190(2) 0.48856(16) 0.5392(3) 0.0471(9) Uani 1 1 d . . . H32A H 0.3003 0.4628 0.5764 0.056 Uiso 1 1 calc R . . H32B H 0.3363 0.4664 0.4965 0.056 Uiso 1 1 calc R . . C33 C 0.3829(2) 0.52137(15) 0.5912(2) 0.0412(8) Uani 1 1 d . . . C34 C 0.4348(2) 0.5455(2) 0.5546(3) 0.0580(11) Uani 1 1 d . . . H34 H 0.4317 0.5409 0.4960 0.070 Uiso 1 1 calc R . . C35 C 0.4915(3) 0.5764(2) 0.6032(3) 0.0597(12) Uani 1 1 d . . . H35 H 0.5266 0.5923 0.5765 0.072 Uiso 1 1 calc R . . C36 C 0.3909(2) 0.52993(19) 0.6770(3) 0.0562(11) Uani 1 1 d . . . H36 H 0.3569 0.5139 0.7051 0.067 Uiso 1 1 calc R . . C37 C 0.4482(2) 0.56162(19) 0.7220(3) 0.0546(10) Uani 1 1 d . . . H37 H 0.4520 0.5673 0.7805 0.066 Uiso 1 1 calc R . . C38 C -0.0609(2) 0.71535(18) 0.3422(3) 0.0506(9) Uani 1 1 d . . . H38 H -0.0107 0.7054 0.3593 0.061 Uiso 1 1 calc R . . C39 C -0.0898(2) 0.75147(19) 0.3921(3) 0.0540(10) Uani 1 1 d . . . H39 H -0.0595 0.7653 0.4427 0.065 Uiso 1 1 calc R . . C40 C -0.1632(2) 0.76764(17) 0.3685(3) 0.0490(9) Uani 1 1 d . . . C41 C -0.2037(3) 0.7463(2) 0.2925(3) 0.0649(13) Uani 1 1 d . . . H41 H -0.2534 0.7570 0.2727 0.078 Uiso 1 1 calc R . . C42 C -0.1726(3) 0.7099(2) 0.2458(3) 0.0636(13) Uani 1 1 d . . . H42 H -0.2018 0.6957 0.1948 0.076 Uiso 1 1 calc R . . C43 C -0.1961(3) 0.80541(18) 0.4239(3) 0.0595(11) Uani 1 1 d . . . H43A H -0.2397 0.8240 0.3889 0.071 Uiso 1 1 calc R . . H43B H -0.1600 0.8343 0.4478 0.071 Uiso 1 1 calc R . . C44 C -0.2191(3) 0.77430(18) 0.4973(3) 0.0526(10) Uani 1 1 d . . . H44A H -0.1752 0.7568 0.5333 0.063 Uiso 1 1 calc R . . H44B H -0.2384 0.8013 0.5323 0.063 Uiso 1 1 calc R . . C45 C -0.2771(3) 0.7300(2) 0.4670(3) 0.0639(12) Uani 1 1 d . . . H45A H -0.3174 0.7459 0.4234 0.077 Uiso 1 1 calc R . . H45B H -0.2551 0.6995 0.4408 0.077 Uiso 1 1 calc R . . C46 C -0.3080(2) 0.70709(19) 0.5383(3) 0.0535(10) Uani 1 1 d . . . C47 C -0.3674(3) 0.7322(2) 0.5616(3) 0.0616(11) Uani 1 1 d . . . H47 H -0.3884 0.7647 0.5333 0.074 Uiso 1 1 calc R . . C48 C -0.3959(3) 0.71020(18) 0.6254(3) 0.0558(10) Uani 1 1 d . . . H48 H -0.4372 0.7276 0.6388 0.067 Uiso 1 1 calc R . . C49 C -0.3100(3) 0.6408(2) 0.6483(4) 0.0667(13) Uani 1 1 d . . . H49 H -0.2894 0.6090 0.6787 0.080 Uiso 1 1 calc R . . C50 C -0.2795(3) 0.6601(2) 0.5842(4) 0.0672(13) Uani 1 1 d . . . H50 H -0.2390 0.6413 0.5712 0.081 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0443(3) 0.0455(3) 0.0475(3) -0.00434(19) 0.00579(19) -0.01038(19) Zn2 0.0422(3) 0.0604(3) 0.0342(2) 0.00086(19) 0.01016(17) 0.0091(2) S1 0.0787(8) 0.0604(7) 0.0517(6) -0.0153(5) -0.0076(6) 0.0167(6) S2 0.0757(8) 0.0607(6) 0.0412(5) -0.0065(5) 0.0042(5) 0.0007(6) S3 0.0819(10) 0.1103(12) 0.0860(10) -0.0563(9) -0.0135(8) 0.0277(9) S4 0.1050(14) 0.1246(15) 0.1170(14) 0.0399(12) 0.0329(11) 0.0594(12) S5 0.0680(8) 0.1179(11) 0.0457(6) -0.0127(6) 0.0237(5) -0.0354(8) S6 0.0564(8) 0.1789(17) 0.0432(6) 0.0042(8) 0.0178(5) -0.0176(9) S7 0.0613(6) 0.0491(5) 0.0383(5) 0.0013(4) 0.0180(4) 0.0025(4) S8 0.0602(7) 0.0870(9) 0.0526(6) -0.0074(6) 0.0047(5) -0.0022(6) P1 0.0568(6) 0.0425(5) 0.0399(5) -0.0029(4) 0.0069(4) -0.0007(4) P2 0.0836(10) 0.0518(7) 0.1491(16) 0.0005(8) 0.0764(11) 0.0041(7) P3 0.0514(6) 0.0655(7) 0.0549(6) 0.0131(5) 0.0207(5) 0.0055(5) P4 0.0441(6) 0.0531(6) 0.0450(5) -0.0011(4) 0.0170(4) 0.0032(4) O1 0.057(2) 0.102(3) 0.0541(19) -0.0271(17) 0.0095(15) 0.0085(18) O2 0.149(4) 0.0548(19) 0.0471(18) 0.0004(14) 0.014(2) -0.033(2) O3 0.243(8) 0.089(3) 0.437(13) -0.109(6) 0.269(9) -0.088(4) O4 0.079(3) 0.095(3) 0.164(5) -0.018(3) 0.073(3) -0.006(2) O5 0.0522(18) 0.095(2) 0.0534(18) -0.0019(17) 0.0139(14) -0.0014(17) O6 0.128(4) 0.074(3) 0.120(4) 0.031(2) 0.057(3) 0.031(2) O7 0.0549(18) 0.0644(18) 0.0577(18) 0.0028(14) 0.0273(14) -0.0028(14) O8 0.0512(17) 0.0504(16) 0.0657(18) 0.0007(13) 0.0239(14) 0.0071(13) N1 0.0418(17) 0.0540(18) 0.0382(16) 0.0004(14) 0.0100(13) 0.0079(14) N2 0.0390(16) 0.0437(16) 0.0389(16) -0.0005(13) 0.0085(12) -0.0048(13) N3 0.0442(18) 0.068(2) 0.0334(16) 0.0012(14) 0.0100(13) 0.0119(16) N4 0.0408(18) 0.0494(18) 0.059(2) 0.0041(16) 0.0084(15) -0.0099(15) C1 0.050(3) 0.089(4) 0.060(3) -0.025(3) 0.005(2) 0.006(2) C2 0.081(4) 0.102(5) 0.105(5) -0.031(4) 0.022(3) -0.009(4) C3 0.111(5) 0.110(5) 0.083(4) -0.001(4) -0.023(4) 0.001(4) C4 0.078(4) 0.057(3) 0.072(3) 0.004(2) 0.013(3) -0.014(2) C5 0.125(7) 0.065(4) 0.252(13) -0.020(5) -0.006(7) 0.009(4) C6 0.184(10) 0.122(7) 0.164(9) -0.033(6) 0.092(8) -0.058(7) C7 0.140(7) 0.144(7) 0.122(6) -0.058(5) 0.071(5) -0.085(6) C8 0.212(11) 0.161(9) 0.228(12) -0.062(8) 0.132(10) -0.115(8) C9 0.110(6) 0.089(5) 0.153(8) -0.025(5) 0.038(5) 0.000(4) C10 0.119(7) 0.223(11) 0.140(8) -0.034(7) 0.083(6) -0.058(7) C11 0.49(3) 0.189(14) 0.56(3) 0.056(18) 0.45(3) -0.001(16) C12 0.191(13) 0.33(2) 0.273(16) 0.055(14) 0.160(12) 0.127(13) C13 0.062(3) 0.119(5) 0.050(3) 0.005(3) 0.008(2) 0.001(3) C14 0.107(6) 0.176(8) 0.092(5) -0.023(5) -0.007(4) -0.043(6) C15 0.110(6) 0.146(7) 0.107(6) 0.028(5) 0.016(4) 0.037(5) C19 0.050(3) 0.163(6) 0.067(3) -0.008(4) 0.028(2) 0.001(3) C20 0.114(5) 0.115(5) 0.091(4) 0.010(4) 0.060(4) 0.039(4) C21 0.200(12) 0.261(14) 0.42(2) -0.196(15) 0.240(14) -0.155(11) C22 0.073(3) 0.051(2) 0.080(3) -0.008(2) 0.033(3) 0.003(2) C23 0.121(6) 0.079(4) 0.101(5) -0.016(3) 0.055(4) 0.020(4) C24 0.161(7) 0.059(3) 0.101(5) 0.011(3) 0.053(5) 0.024(4) C25 0.056(3) 0.079(3) 0.047(2) 0.016(2) 0.0210(19) 0.020(2) C26 0.047(2) 0.078(3) 0.051(2) 0.010(2) 0.0167(18) 0.016(2) C27 0.042(2) 0.045(2) 0.046(2) 0.0021(16) -0.0016(16) -0.0019(16) C28 0.048(2) 0.073(3) 0.051(2) 0.018(2) 0.0124(18) -0.004(2) C29 0.040(2) 0.074(3) 0.053(2) 0.012(2) 0.0150(17) 0.0017(19) C30 0.043(2) 0.049(2) 0.058(2) 0.0079(18) -0.0066(18) -0.0028(17) C31 0.041(2) 0.046(2) 0.048(2) 0.0012(16) 0.0001(16) -0.0015(16) C32 0.041(2) 0.048(2) 0.046(2) 0.0024(16) -0.0026(16) -0.0071(16) C33 0.0393(19) 0.0420(19) 0.0402(19) 0.0017(15) 0.0046(14) -0.0030(15) C34 0.058(3) 0.080(3) 0.035(2) -0.0062(19) 0.0089(17) -0.023(2) C35 0.059(3) 0.080(3) 0.044(2) -0.005(2) 0.0191(19) -0.031(2) C36 0.054(3) 0.071(3) 0.046(2) -0.001(2) 0.0169(18) -0.024(2) C37 0.061(3) 0.068(3) 0.037(2) -0.0043(18) 0.0157(18) -0.021(2) C38 0.042(2) 0.066(3) 0.045(2) -0.0035(19) 0.0116(16) 0.0073(18) C39 0.056(3) 0.064(3) 0.045(2) -0.0051(19) 0.0175(18) 0.000(2) C40 0.059(3) 0.051(2) 0.042(2) 0.0077(17) 0.0234(18) 0.0078(18) C41 0.050(3) 0.088(3) 0.056(3) 0.011(2) 0.011(2) 0.031(2) C42 0.056(3) 0.094(3) 0.038(2) -0.004(2) 0.0039(18) 0.025(2) C43 0.074(3) 0.048(2) 0.066(3) 0.008(2) 0.037(2) 0.019(2) C44 0.063(3) 0.051(2) 0.051(2) -0.0067(18) 0.0276(19) 0.0020(19) C45 0.064(3) 0.079(3) 0.051(2) -0.011(2) 0.018(2) -0.001(2) C46 0.052(2) 0.060(3) 0.051(2) -0.0058(19) 0.0171(18) -0.007(2) C47 0.071(3) 0.060(3) 0.057(3) 0.009(2) 0.020(2) 0.011(2) C48 0.054(3) 0.056(2) 0.058(3) 0.005(2) 0.0154(19) 0.006(2) C49 0.055(3) 0.054(3) 0.095(4) 0.016(2) 0.025(3) 0.002(2) C50 0.058(3) 0.056(3) 0.095(4) 0.005(3) 0.031(3) 0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N2 2.022(3) . ? Zn1 N4 2.061(3) 1_655 ? Zn1 S3 2.3052(15) . ? Zn1 S1 2.3092(12) . ? Zn1 S4 3.7854(16) . ? Zn1 S2 3.8066(13) . ? Zn2 N3 2.023(3) . ? Zn2 N1 2.057(3) . ? Zn2 S5 2.3101(13) . ? Zn2 S7 2.3199(11) . ? Zn2 S6 3.7262(14) . ? Zn2 S8 3.8579(15) . ? S1 P1 2.0136(15) . ? S2 P1 1.9420(14) . ? S3 P2 2.000(2) . ? S4 P2 1.905(3) . ? S5 P3 2.0257(16) . ? S6 P3 1.9307(19) . ? S7 P4 2.0200(15) . ? S8 P4 1.9354(16) . ? P1 O1 1.570(4) . ? P1 O2 1.578(3) . ? P2 O3 1.570(5) . ? P2 O4 1.595(4) . ? P3 O5 1.568(3) . ? P3 O6 1.606(4) . ? P4 O8 1.584(3) . ? P4 O7 1.588(3) . ? O1 C1 1.465(5) . ? O2 C4 1.452(6) . ? O3 C7 1.220(9) . ? O4 C10 1.408(9) . ? O5 C13 1.473(6) . ? O6 C16 1.378(10) . ? O6 C16' 1.60(2) . ? O7 C19 1.462(6) . ? O8 C22 1.466(5) . ? N1 C25 1.324(5) . ? N1 C29 1.343(5) . ? N2 C37 1.339(5) . ? N2 C35 1.322(5) . ? N3 C42 1.339(5) . ? N3 C38 1.338(5) . ? N4 C48 1.335(5) . ? N4 C49 1.329(6) . ? N4 Zn1 2.061(3) 1_455 ? C1 C3 1.490(8) . ? C1 C2 1.488(8) . ? C1 H1 0.9900 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 C5 1.453(9) . ? C4 C6 1.460(9) . ? C4 H4 0.9900 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 C9 1.416(10) . ? C7 C8 1.553(11) . ? C7 H7 0.9900 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 C11 1.389(16) . ? C10 C12 1.609(16) . ? C10 H10 0.9900 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 C15 1.492(9) . ? C13 C14 1.496(9) . ? C13 H13 0.9900 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 C18 1.408(16) . ? C16 C17 1.459(19) . ? C16 H16 0.9900 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C16' C18' 1.43(3) . ? C16' C17' 1.65(3) . ? C16' H16' 0.9900 . ? C17' H17D 0.9700 . ? C17' H17E 0.9700 . ? C17' H17F 0.9700 . ? C18' H18D 0.9700 . ? C18' H18E 0.9700 . ? C18' H18F 0.9700 . ? C19 C21 1.482(13) . ? C19 C20 1.469(9) . ? C19 H19 0.9900 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 C23 1.504(7) . ? C22 C24 1.499(8) . ? C22 H22 0.9900 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 H24C 0.9700 . ? C25 C26 1.378(6) . ? C25 H25 0.9400 . ? C26 C27 1.383(6) . ? C26 H26 0.9400 . ? C27 C28 1.377(6) . ? C27 C30 1.497(5) . ? C28 C29 1.380(6) . ? C28 H28 0.9400 . ? C29 H29 0.9400 . ? C30 C31 1.529(5) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C31 C32 1.514(5) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C32 C33 1.508(5) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C33 C34 1.369(6) . ? C33 C36 1.374(6) . ? C34 C35 1.377(6) . ? C34 H34 0.9400 . ? C35 H35 0.9400 . ? C36 C37 1.371(6) . ? C36 H36 0.9400 . ? C37 H37 0.9400 . ? C38 C39 1.373(6) . ? C38 H38 0.9400 . ? C39 C40 1.384(6) . ? C39 H39 0.9400 . ? C40 C41 1.381(6) . ? C40 C43 1.499(6) . ? C41 C42 1.365(6) . ? C41 H41 0.9400 . ? C42 H42 0.9400 . ? C43 C44 1.541(6) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C44 C45 1.512(6) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C45 C46 1.504(6) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C46 C47 1.383(6) . ? C46 C50 1.386(7) . ? C47 C48 1.367(6) . ? C47 H47 0.9400 . ? C48 H48 0.9400 . ? C49 C50 1.369(7) . ? C49 H49 0.9400 . ? C50 H50 0.9400 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Zn1 N4 103.07(13) . 1_655 ? N2 Zn1 S3 111.34(10) . . ? N4 Zn1 S3 118.85(12) 1_655 . ? N2 Zn1 S1 116.16(10) . . ? N4 Zn1 S1 110.81(10) 1_655 . ? S3 Zn1 S1 97.33(5) . . ? N2 Zn1 S4 69.82(10) . . ? N4 Zn1 S4 87.53(10) 1_655 . ? S3 Zn1 S4 61.28(5) . . ? S1 Zn1 S4 157.41(5) . . ? N2 Zn1 S2 68.87(9) . . ? N4 Zn1 S2 85.14(10) 1_655 . ? S3 Zn1 S2 153.97(6) . . ? S1 Zn1 S2 62.33(3) . . ? S4 Zn1 S2 135.03(4) . . ? N3 Zn2 N1 106.87(12) . . ? N3 Zn2 S5 111.37(11) . . ? N1 Zn2 S5 114.55(11) . . ? N3 Zn2 S7 117.26(10) . . ? N1 Zn2 S7 106.85(10) . . ? S5 Zn2 S7 100.09(4) . . ? N3 Zn2 S6 67.83(11) . . ? N1 Zn2 S6 86.07(10) . . ? S5 Zn2 S6 63.49(4) . . ? S7 Zn2 S6 162.71(4) . . ? N3 Zn2 S8 79.31(10) . . ? N1 Zn2 S8 75.56(10) . . ? S5 Zn2 S8 160.52(4) . . ? S7 Zn2 S8 60.48(3) . . ? S6 Zn2 S8 135.64(3) . . ? P1 S1 Zn1 110.54(6) . . ? P1 S2 Zn1 67.70(5) . . ? P2 S3 Zn1 108.84(9) . . ? P2 S4 Zn1 66.87(6) . . ? P3 S5 Zn2 109.02(6) . . ? P3 S6 Zn2 69.14(5) . . ? P4 S7 Zn2 102.24(5) . . ? P4 S8 Zn2 61.26(5) . . ? O1 P1 O2 105.9(2) . . ? O1 P1 S2 108.23(13) . . ? O2 P1 S2 114.17(14) . . ? O1 P1 S1 107.12(14) . . ? O2 P1 S1 101.09(16) . . ? S2 P1 S1 119.35(7) . . ? O3 P2 O4 98.3(3) . . ? O3 P2 S4 108.6(4) . . ? O4 P2 S4 118.5(2) . . ? O3 P2 S3 106.3(4) . . ? O4 P2 S3 104.4(2) . . ? S4 P2 S3 118.40(10) . . ? O5 P3 O6 96.3(2) . . ? O5 P3 S6 108.54(14) . . ? O6 P3 S6 116.52(19) . . ? O5 P3 S5 107.65(14) . . ? O6 P3 S5 107.04(18) . . ? S6 P3 S5 118.27(8) . . ? O8 P4 O7 99.51(16) . . ? O8 P4 S8 114.28(13) . . ? O7 P4 S8 113.37(13) . . ? O8 P4 S7 103.61(12) . . ? O7 P4 S7 106.50(13) . . ? S8 P4 S7 117.58(7) . . ? C1 O1 P1 125.4(3) . . ? C4 O2 P1 126.1(3) . . ? C7 O3 P2 141.7(8) . . ? C10 O4 P2 125.1(5) . . ? C13 O5 P3 124.9(3) . . ? C16 O6 C16' 30.8(8) . . ? C16 O6 P3 131.9(6) . . ? C16' O6 P3 101.4(10) . . ? C19 O7 P4 122.8(3) . . ? C22 O8 P4 119.4(3) . . ? C25 N1 C29 117.8(3) . . ? C25 N1 Zn2 119.2(3) . . ? C29 N1 Zn2 122.6(3) . . ? C37 N2 C35 117.2(3) . . ? C37 N2 Zn1 119.4(3) . . ? C35 N2 Zn1 123.4(3) . . ? C42 N3 C38 117.8(4) . . ? C42 N3 Zn2 120.1(3) . . ? C38 N3 Zn2 121.9(3) . . ? C48 N4 C49 117.5(4) . . ? C48 N4 Zn1 121.7(3) . 1_455 ? C49 N4 Zn1 120.6(3) . 1_455 ? O1 C1 C3 108.7(4) . . ? O1 C1 C2 106.7(5) . . ? C3 C1 C2 112.8(5) . . ? O1 C1 H1 109.5 . . ? C3 C1 H1 109.5 . . ? C2 C1 H1 109.5 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O2 C4 C5 109.9(5) . . ? O2 C4 C6 107.3(5) . . ? C5 C4 C6 110.5(7) . . ? O2 C4 H4 109.7 . . ? C5 C4 H4 109.7 . . ? C6 C4 H4 109.7 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O3 C7 C9 134.0(8) . . ? O3 C7 C8 108.0(7) . . ? C9 C7 C8 113.4(7) . . ? O3 C7 H7 97.0 . . ? C9 C7 H7 97.0 . . ? C8 C7 H7 97.0 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 O4 115.3(13) . . ? C11 C10 C12 111.3(10) . . ? O4 C10 C12 102.7(8) . . ? C11 C10 H10 109.1 . . ? O4 C10 H10 109.1 . . ? C12 C10 H10 109.1 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O5 C13 C15 106.3(5) . . ? O5 C13 C14 107.8(5) . . ? C15 C13 C14 112.2(6) . . ? O5 C13 H13 110.1 . . ? C15 C13 H13 110.1 . . ? C14 C13 H13 110.1 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O6 C16 C18 114.7(9) . . ? O6 C16 C17 108.9(11) . . ? C18 C16 C17 103.1(12) . . ? O6 C16 H16 110.0 . . ? C18 C16 H16 110.0 . . ? C17 C16 H16 110.0 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C18' C16' O6 114.9(18) . . ? C18' C16' C17' 114(2) . . ? O6 C16' C17' 102.9(17) . . ? C18' C16' H16' 108.1 . . ? O6 C16' H16' 108.1 . . ? C17' C16' H16' 108.1 . . ? C16' C17' H17D 109.5 . . ? C16' C17' H17E 109.5 . . ? H17D C17' H17E 109.5 . . ? C16' C17' H17F 109.5 . . ? H17D C17' H17F 109.5 . . ? H17E C17' H17F 109.5 . . ? C16' C18' H18D 109.5 . . ? C16' C18' H18E 109.5 . . ? H18D C18' H18E 109.5 . . ? C16' C18' H18F 109.5 . . ? H18D C18' H18F 109.5 . . ? H18E C18' H18F 109.5 . . ? O7 C19 C21 106.1(7) . . ? O7 C19 C20 109.2(5) . . ? C21 C19 C20 111.0(7) . . ? O7 C19 H19 110.2 . . ? C21 C19 H19 110.2 . . ? C20 C19 H19 110.2 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O8 C22 C23 107.0(4) . . ? O8 C22 C24 107.0(4) . . ? C23 C22 C24 112.1(5) . . ? O8 C22 H22 110.2 . . ? C23 C22 H22 110.2 . . ? C24 C22 H22 110.2 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N1 C25 C26 123.1(4) . . ? N1 C25 H25 118.5 . . ? C26 C25 H25 118.5 . . ? C25 C26 C27 119.8(4) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C28 C27 C26 116.7(4) . . ? C28 C27 C30 122.9(4) . . ? C26 C27 C30 120.4(4) . . ? C27 C28 C29 120.6(4) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? N1 C29 C28 121.8(4) . . ? N1 C29 H29 119.1 . . ? C28 C29 H29 119.1 . . ? C27 C30 C31 113.3(3) . . ? C27 C30 H30A 108.9 . . ? C31 C30 H30A 108.9 . . ? C27 C30 H30B 108.9 . . ? C31 C30 H30B 108.9 . . ? H30A C30 H30B 107.7 . . ? C32 C31 C30 111.2(3) . . ? C32 C31 H31A 109.4 . . ? C30 C31 H31A 109.4 . . ? C32 C31 H31B 109.4 . . ? C30 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? C33 C32 C31 111.4(3) . . ? C33 C32 H32A 109.3 . . ? C31 C32 H32A 109.3 . . ? C33 C32 H32B 109.3 . . ? C31 C32 H32B 109.3 . . ? H32A C32 H32B 108.0 . . ? C34 C33 C36 116.6(3) . . ? C34 C33 C32 121.4(4) . . ? C36 C33 C32 122.0(4) . . ? C33 C34 C35 120.2(4) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? N2 C35 C34 123.0(4) . . ? N2 C35 H35 118.5 . . ? C34 C35 H35 118.5 . . ? C33 C36 C37 120.6(4) . . ? C33 C36 H36 119.7 . . ? C37 C36 H36 119.7 . . ? N2 C37 C36 122.4(4) . . ? N2 C37 H37 118.8 . . ? C36 C37 H37 118.8 . . ? N3 C38 C39 122.2(4) . . ? N3 C38 H38 118.9 . . ? C39 C38 H38 118.9 . . ? C40 C39 C38 120.5(4) . . ? C40 C39 H39 119.7 . . ? C38 C39 H39 119.7 . . ? C39 C40 C41 116.2(4) . . ? C39 C40 C43 121.0(4) . . ? C41 C40 C43 122.7(4) . . ? C42 C41 C40 120.9(4) . . ? C42 C41 H41 119.5 . . ? C40 C41 H41 119.5 . . ? N3 C42 C41 122.3(4) . . ? N3 C42 H42 118.9 . . ? C41 C42 H42 118.9 . . ? C40 C43 C44 112.9(3) . . ? C40 C43 H43A 109.0 . . ? C44 C43 H43A 109.0 . . ? C40 C43 H43B 109.0 . . ? C44 C43 H43B 109.0 . . ? H43A C43 H43B 107.8 . . ? C45 C44 C43 113.2(4) . . ? C45 C44 H44A 108.9 . . ? C43 C44 H44A 108.9 . . ? C45 C44 H44B 108.9 . . ? C43 C44 H44B 108.9 . . ? H44A C44 H44B 107.8 . . ? C46 C45 C44 112.2(4) . . ? C46 C45 H45A 109.2 . . ? C44 C45 H45A 109.2 . . ? C46 C45 H45B 109.2 . . ? C44 C45 H45B 109.2 . . ? H45A C45 H45B 107.9 . . ? C47 C46 C50 116.1(4) . . ? C47 C46 C45 121.2(4) . . ? C50 C46 C45 122.7(4) . . ? C48 C47 C46 120.5(4) . . ? C48 C47 H47 119.8 . . ? C46 C47 H47 119.8 . . ? N4 C48 C47 122.7(4) . . ? N4 C48 H48 118.6 . . ? C47 C48 H48 118.6 . . ? N4 C49 C50 122.8(4) . . ? N4 C49 H49 118.6 . . ? C50 C49 H49 118.6 . . ? C49 C50 C46 120.4(5) . . ? C49 C50 H50 119.8 . . ? C46 C50 H50 119.8 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.1 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.62 # # 0.73 \%A from S4 # _refine_diff_density_min -1.50 _refine_diff_density_rms 0.098 # Attachment 'B513393A 6.cif' #============================================================================== # # {[Zn(iPr2dtp)2](4-NC5H4N(H)C5H4N-4)}n # #============================================================================== data_shelxl_5 _database_code_depnum_ccdc_archive 'CCDC 284522' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H37 N3 O4 P2 S4 Zn' _chemical_formula_sum 'C22 H37 N3 O4 P2 S4 Zn' _chemical_formula_weight 663.10 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 Pc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 12.1969(7) _cell_length_b 8.3847(5) _cell_length_c 15.5757(10) _cell_angle_alpha 90 _cell_angle_beta 95.676(2) _cell_angle_gamma 90 _cell_volume 1585.08(17) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 2817 _cell_measurement_theta_min 4.5 _cell_measurement_theta_max 24.7 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 692 _exptl_absorpt_coefficient_mu 1.170 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.454 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details '(SADABS, Bruker, 2000 & Blessing, 1995)' _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS SMART CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13069 _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_av_sigmaI/netI 0.058 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.7 _diffrn_reflns_theta_max 30.0 _reflns_number_total 7130 _reflns_number_gt 5816 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_reduction 'SHELXTL (Bruker, 2000)' _computing_structure_solution 'PATTY in DIRDIF92 (Beurskens et al., 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'Bruker SHEXLTL (Bruker, 2000)' _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^)+(0.0719P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.009(12) _refine_ls_number_reflns 7130 _refine_ls_number_parameters 325 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.065 _refine_ls_R_factor_gt 0.051 _refine_ls_wR_factor_ref 0.128 _refine_ls_wR_factor_gt 0.118 _refine_ls_goodness_of_fit_ref 1.01 _refine_ls_restrained_S_all 1.01 _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 Zn Zn -0.00003(4) -0.01952(5) 0.49995(3) 0.02905(12) Uani 1 1 d . . . S1 S 0.11030(10) -0.24067(12) 0.52624(8) 0.0323(2) Uani 1 1 d . . . S2 S 0.31596(11) 0.00445(14) 0.61124(9) 0.0395(3) Uani 1 1 d . . . S3 S -0.17506(11) -0.05344(17) 0.43373(9) 0.0448(3) Uani 1 1 d . . . S4 S -0.14422(12) -0.3338(2) 0.58921(11) 0.0591(4) Uani 1 1 d . . . P1 P 0.26800(10) -0.16498(13) 0.53143(8) 0.0294(2) Uani 1 1 d . . . P2 P -0.24451(10) -0.21642(15) 0.50815(9) 0.0359(3) Uani 1 1 d . A . O1 O 0.2852(3) -0.1281(4) 0.4333(2) 0.0348(7) Uani 1 1 d . . . O2 O 0.3381(3) -0.3245(4) 0.5462(2) 0.0354(7) Uani 1 1 d . . . O3 O -0.3221(3) -0.3249(4) 0.4440(3) 0.0448(9) Uani 1 1 d . . . O4 O -0.3407(3) -0.1303(4) 0.5522(3) 0.0429(8) Uani 1 1 d . . . N1 N 0.0098(3) 0.1110(4) 0.6121(3) 0.0313(8) Uani 1 1 d . . . N2 N 0.0542(3) 0.8382(4) 0.9228(3) 0.0330(8) Uani 1 1 d . . . N3 N 0.1220(4) 0.3880(4) 0.8251(3) 0.0400(10) Uani 1 1 d . . . H3 H 0.1716 0.3373 0.8587 0.048 Uiso 1 1 calc R . . C1 C 0.3972(4) -0.0935(6) 0.4090(4) 0.0426(12) Uani 1 1 d . . . H1 H 0.4519 -0.1089 0.4597 0.051 Uiso 1 1 calc R . . C2 C 0.3990(7) 0.0772(8) 0.3799(5) 0.070(2) Uani 1 1 d . . . H2A H 0.3847 0.1466 0.4273 0.105 Uiso 1 1 calc R . . H2B H 0.3427 0.0932 0.3322 0.105 Uiso 1 1 calc R . . H2C H 0.4707 0.1019 0.3614 0.105 Uiso 1 1 calc R . . C3 C 0.4189(6) -0.2092(8) 0.3402(5) 0.0624(18) Uani 1 1 d . . . H3A H 0.4168 -0.3169 0.3628 0.094 Uiso 1 1 calc R . . H3B H 0.4909 -0.1885 0.3212 0.094 Uiso 1 1 calc R . . H3C H 0.3629 -0.1976 0.2918 0.094 Uiso 1 1 calc R . . C4 C 0.3946(5) -0.3739(6) 0.6293(4) 0.0498(14) Uani 1 1 d . . . H4 H 0.4303 -0.2800 0.6588 0.060 Uiso 1 1 calc R . . C5 C 0.4798(7) -0.4887(9) 0.6092(6) 0.087(3) Uani 1 1 d . . . H5A H 0.5307 -0.4372 0.5740 0.130 Uiso 1 1 calc R . . H5B H 0.4452 -0.5786 0.5780 0.130 Uiso 1 1 calc R . . H5C H 0.5196 -0.5261 0.6624 0.130 Uiso 1 1 calc R . . C6 C 0.3128(7) -0.4418(11) 0.6837(6) 0.089(3) Uani 1 1 d . . . H6A H 0.2587 -0.3611 0.6939 0.133 Uiso 1 1 calc R . . H6B H 0.3501 -0.4768 0.7383 0.133 Uiso 1 1 calc R . . H6C H 0.2762 -0.5320 0.6542 0.133 Uiso 1 1 calc R . . C7 C -0.2744(7) -0.4507(8) 0.3951(5) 0.073(2) Uani 0.59(2) 1 d P A 1 H7 H -0.2034 -0.4925 0.4223 0.088 Uiso 0.59(2) 1 calc PR A 1 C8 C -0.2720(9) -0.4022(11) 0.3042(6) 0.094(3) Uani 0.59(2) 1 d P A 1 H8A H -0.2117 -0.3283 0.2996 0.141 Uiso 0.59(2) 1 calc PR A 1 H8B H -0.3411 -0.3509 0.2840 0.141 Uiso 0.59(2) 1 calc PR A 1 H8C H -0.2616 -0.4956 0.2691 0.141 Uiso 0.59(2) 1 calc PR A 1 C9 C -0.3749(12) -0.5800(16) 0.3893(9) 0.074(5) Uiso 0.59(2) 1 d P A 1 H9A H -0.3828 -0.6221 0.4463 0.111 Uiso 0.59(2) 1 calc PR A 1 H9B H -0.3587 -0.6665 0.3511 0.111 Uiso 0.59(2) 1 calc PR A 1 H9C H -0.4429 -0.5282 0.3669 0.111 Uiso 0.59(2) 1 calc PR A 1 C7' C -0.2744(7) -0.4507(8) 0.3951(5) 0.073(2) Uani 0.41(2) 1 d P A 2 H7' H -0.1956 -0.4356 0.4156 0.088 Uiso 0.41(2) 1 calc PR A 2 C8' C -0.2720(9) -0.4022(11) 0.3042(6) 0.094(3) Uani 0.41(2) 1 d P A 2 H8'1 H -0.2334 -0.3014 0.3017 0.141 Uiso 0.41(2) 1 calc PR A 2 H8'2 H -0.3468 -0.3904 0.2774 0.141 Uiso 0.41(2) 1 calc PR A 2 H8'3 H -0.2342 -0.4830 0.2736 0.141 Uiso 0.41(2) 1 calc PR A 2 C9' C -0.2879(19) -0.599(2) 0.4226(15) 0.080(7) Uiso 0.41(2) 1 d P A 2 H9'1 H -0.2785 -0.6003 0.4852 0.120 Uiso 0.41(2) 1 calc PR A 2 H9'2 H -0.2338 -0.6679 0.4003 0.120 Uiso 0.41(2) 1 calc PR A 2 H9'3 H -0.3614 -0.6353 0.4025 0.120 Uiso 0.41(2) 1 calc PR A 2 C10 C -0.3114(5) -0.0151(7) 0.6207(4) 0.0500(13) Uani 1 1 d . A . H10 H -0.2306 0.0006 0.6272 0.060 Uiso 1 1 calc R . . C11 C -0.3474(8) -0.0768(11) 0.7034(5) 0.085(2) Uani 1 1 d . . . H11A H -0.3094 -0.1759 0.7186 0.127 Uiso 1 1 calc R A . H11B H -0.4263 -0.0956 0.6965 0.127 Uiso 1 1 calc R . . H11C H -0.3300 0.0010 0.7488 0.127 Uiso 1 1 calc R . . C12 C -0.3669(8) 0.1382(8) 0.5923(6) 0.088(3) Uani 1 1 d . . . H12A H -0.3399 0.1734 0.5389 0.132 Uiso 1 1 calc R A . H12B H -0.3507 0.2187 0.6365 0.132 Uiso 1 1 calc R . . H12C H -0.4459 0.1216 0.5832 0.132 Uiso 1 1 calc R . . C13 C -0.0022(4) 0.2709(6) 0.6103(3) 0.0380(11) Uani 1 1 d . . . H13 H -0.0358 0.3178 0.5596 0.046 Uiso 1 1 calc R . . C14 C 0.0314(4) 0.3684(5) 0.6778(3) 0.0392(12) Uani 1 1 d . . . H14 H 0.0227 0.4795 0.6724 0.047 Uiso 1 1 calc R . . C15 C 0.0784(4) 0.3030(5) 0.7542(3) 0.0301(9) Uani 1 1 d . . . C16 C 0.0886(4) 0.1362(5) 0.7578(3) 0.0334(10) Uani 1 1 d . . . H16 H 0.1184 0.0860 0.8088 0.040 Uiso 1 1 calc R . . C17 C 0.0548(4) 0.0477(5) 0.6866(3) 0.0317(9) Uani 1 1 d . . . H17 H 0.0635 -0.0636 0.6898 0.038 Uiso 1 1 calc R . . C18 C 0.0998(4) 0.5404(5) 0.8513(3) 0.0312(9) Uani 1 1 d . . . C19 C 0.0094(4) 0.6329(6) 0.8181(3) 0.0376(11) Uani 1 1 d . . . H19 H -0.0384 0.5966 0.7711 0.045 Uiso 1 1 calc R . . C20 C -0.0079(4) 0.7786(5) 0.8561(3) 0.0347(10) Uani 1 1 d . . . H20 H -0.0682 0.8398 0.8327 0.042 Uiso 1 1 calc R . . C21 C 0.1447(4) 0.7513(5) 0.9529(3) 0.0347(10) Uani 1 1 d . . . H21 H 0.1927 0.7929 0.9983 0.042 Uiso 1 1 calc R . . C22 C 0.1679(4) 0.6052(5) 0.9191(3) 0.0372(11) Uani 1 1 d . . . H22 H 0.2306 0.5487 0.9421 0.045 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.0375(3) 0.0232(2) 0.0256(2) -0.0012(2) -0.00107(19) 0.0026(2) S1 0.0341(5) 0.0242(5) 0.0381(6) -0.0002(4) 0.0010(4) 0.0025(4) S2 0.0445(7) 0.0366(6) 0.0358(7) -0.0073(5) -0.0046(5) -0.0017(5) S3 0.0412(7) 0.0489(7) 0.0417(7) 0.0178(6) -0.0099(5) -0.0064(6) S4 0.0454(8) 0.0727(10) 0.0585(10) 0.0341(8) 0.0012(7) 0.0160(7) P1 0.0331(6) 0.0278(5) 0.0262(6) -0.0002(4) -0.0018(4) 0.0033(4) P2 0.0336(6) 0.0369(6) 0.0361(7) 0.0069(5) -0.0016(5) 0.0042(5) O1 0.0292(16) 0.0454(18) 0.0293(17) 0.0030(14) 0.0004(13) -0.0003(14) O2 0.0298(16) 0.0346(16) 0.040(2) 0.0011(14) -0.0025(14) 0.0064(13) O3 0.046(2) 0.0374(18) 0.051(2) -0.0065(16) 0.0060(17) -0.0019(16) O4 0.0392(18) 0.0444(18) 0.044(2) -0.0063(17) -0.0012(15) 0.0069(17) N1 0.036(2) 0.0286(17) 0.028(2) -0.0042(15) -0.0004(16) 0.0046(15) N2 0.044(2) 0.0265(17) 0.028(2) -0.0016(15) 0.0012(17) -0.0020(16) N3 0.061(3) 0.0275(17) 0.028(2) -0.0005(15) -0.0141(18) 0.0089(18) C1 0.040(3) 0.050(3) 0.037(3) 0.005(2) 0.003(2) -0.008(2) C2 0.082(5) 0.057(4) 0.074(5) 0.001(3) 0.031(4) -0.021(4) C3 0.064(4) 0.064(4) 0.064(4) -0.008(3) 0.026(3) 0.007(3) C4 0.054(3) 0.039(3) 0.052(4) 0.010(2) -0.015(3) 0.005(2) C5 0.081(5) 0.084(5) 0.092(7) 0.020(4) -0.003(5) 0.045(4) C6 0.081(5) 0.108(6) 0.078(6) 0.053(5) 0.011(4) 0.011(5) C7 0.089(5) 0.058(4) 0.070(5) -0.013(3) -0.005(4) 0.029(4) C8 0.118(7) 0.092(6) 0.073(6) -0.031(5) 0.023(5) -0.009(6) C7' 0.089(5) 0.058(4) 0.070(5) -0.013(3) -0.005(4) 0.029(4) C8' 0.118(7) 0.092(6) 0.073(6) -0.031(5) 0.023(5) -0.009(6) C10 0.050(3) 0.053(3) 0.046(3) -0.010(3) -0.002(3) 0.000(3) C11 0.106(6) 0.102(6) 0.048(4) -0.016(4) 0.018(4) -0.017(5) C12 0.113(7) 0.056(4) 0.092(7) -0.022(4) -0.002(5) 0.023(4) C13 0.049(3) 0.036(2) 0.028(2) -0.0010(19) -0.003(2) 0.019(2) C14 0.060(3) 0.025(2) 0.031(2) -0.0031(18) 0.000(2) 0.016(2) C15 0.040(2) 0.0254(19) 0.025(2) -0.0032(16) 0.0005(18) 0.0054(18) C16 0.052(3) 0.0235(19) 0.024(2) 0.0039(16) 0.0001(19) 0.0057(19) C17 0.045(3) 0.0215(18) 0.029(2) 0.0003(17) 0.0043(19) 0.0025(18) C18 0.038(2) 0.0261(19) 0.029(2) 0.0009(17) 0.0019(18) 0.0022(18) C19 0.048(3) 0.036(2) 0.026(2) -0.0044(19) -0.007(2) 0.000(2) C20 0.045(3) 0.032(2) 0.026(2) 0.0019(18) 0.0005(19) 0.007(2) C21 0.039(2) 0.032(2) 0.033(2) -0.0025(18) -0.0011(19) -0.0046(19) C22 0.050(3) 0.0243(19) 0.035(3) -0.0008(18) -0.008(2) 0.001(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 Zn N1 2.054(4) . ? Zn N2 2.085(4) 2_564 ? Zn S3 2.2950(14) . ? Zn S1 2.3039(12) . ? Zn S4 3.5288(16) . ? Zn S2 4.0715(14) . ? S1 P1 2.0195(17) . ? S2 P1 1.9396(17) . ? S3 P2 2.0305(17) . ? S4 P2 1.9372(19) . ? P1 O2 1.592(3) . ? P1 O1 1.593(3) . ? P2 O3 1.591(4) . ? P2 O4 1.590(4) . ? O1 C1 1.482(6) . ? O2 C4 1.465(6) . ? O3 C7' 1.456(7) . ? O3 C7 1.456(7) . ? O4 C10 1.458(7) . ? N1 C17 1.343(6) . ? N1 C13 1.349(6) . ? N2 C20 1.323(6) . ? N2 C21 1.365(6) . ? N2 Zn 2.085(4) 2_565 ? N3 C18 1.376(6) . ? N3 C15 1.377(6) . ? N3 H3 0.8700 . ? C1 C2 1.502(9) . ? C1 C3 1.488(8) . ? C1 H1 0.9900 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 C5 1.472(9) . ? C4 C6 1.484(9) . ? C4 H4 0.9900 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 C8 1.476(12) . ? C7 C9 1.632(16) . ? C7 H7 0.9900 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C7' C9' 1.33(2) . ? C7' C8' 1.476(12) . ? C7' H7' 0.9900 . ? C8' H8'1 0.9700 . ? C8' H8'2 0.9700 . ? C8' H8'3 0.9700 . ? C9' H9'1 0.9700 . ? C9' H9'2 0.9700 . ? C9' H9'3 0.9700 . ? C10 C12 1.498(9) . ? C10 C11 1.494(10) . ? C10 H10 0.9900 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 C14 1.362(7) . ? C13 H13 0.9400 . ? C14 C15 1.382(7) . ? C14 H14 0.9400 . ? C15 C16 1.405(6) . ? C16 C17 1.363(6) . ? C16 H16 0.9400 . ? C17 H17 0.9400 . ? C18 C22 1.388(7) . ? C18 C19 1.405(7) . ? C19 C20 1.382(6) . ? C19 H19 0.9400 . ? C20 H20 0.9400 . ? C21 C22 1.374(6) . ? C21 H21 0.9400 . ? C22 H22 0.9400 . ? 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 Zn N2 96.09(15) . 2_564 ? N1 Zn S3 114.94(12) . . ? N2 Zn S3 99.53(12) 2_564 . ? N1 Zn S1 107.08(11) . . ? N2 Zn S1 118.43(11) 2_564 . ? S3 Zn S1 118.76(5) . . ? N1 Zn S4 93.00(11) . . ? N2 Zn S4 165.97(12) 2_564 . ? S3 Zn S4 66.85(4) . . ? S1 Zn S4 68.54(4) . . ? N1 Zn S2 68.81(11) . . ? N2 Zn S2 82.43(12) 2_564 . ? S3 Zn S2 175.39(4) . . ? S1 Zn S2 56.80(4) . . ? S4 Zn S2 110.90(3) . . ? P1 S1 Zn 106.94(6) . . ? P1 S2 Zn 58.55(5) . . ? P2 S3 Zn 104.41(7) . . ? P2 S4 Zn 70.80(6) . . ? O2 P1 O1 100.48(18) . . ? O2 P1 S2 113.50(15) . . ? O1 P1 S2 114.37(14) . . ? O2 P1 S1 103.76(14) . . ? O1 P1 S1 103.77(13) . . ? S2 P1 S1 118.78(8) . . ? O3 P2 O4 96.4(2) . . ? O3 P2 S4 114.61(16) . . ? O4 P2 S4 113.25(17) . . ? O3 P2 S3 106.39(16) . . ? O4 P2 S3 107.96(15) . . ? S4 P2 S3 116.21(8) . . ? C1 O1 P1 119.7(3) . . ? C4 O2 P1 124.4(3) . . ? C7' O3 C7 0.0(6) . . ? C7' O3 P2 120.0(4) . . ? C7 O3 P2 120.0(4) . . ? C10 O4 P2 118.6(4) . . ? C17 N1 C13 116.4(4) . . ? C17 N1 Zn 120.6(3) . . ? C13 N1 Zn 121.0(3) . . ? C20 N2 C21 116.6(4) . . ? C20 N2 Zn 122.6(3) . 2_565 ? C21 N2 Zn 118.9(3) . 2_565 ? C18 N3 C15 130.3(4) . . ? C18 N3 H3 114.9 . . ? C15 N3 H3 114.9 . . ? O1 C1 C2 107.7(5) . . ? O1 C1 C3 106.9(4) . . ? C2 C1 C3 113.3(5) . . ? O1 C1 H1 109.6 . . ? C2 C1 H1 109.6 . . ? C3 C1 H1 109.6 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O2 C4 C5 106.1(6) . . ? O2 C4 C6 109.2(5) . . ? C5 C4 C6 113.5(6) . . ? O2 C4 H4 109.3 . . ? C5 C4 H4 109.3 . . ? C6 C4 H4 109.3 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O3 C7 C8 110.5(6) . . ? O3 C7 C9 100.0(7) . . ? C8 C7 C9 102.5(8) . . ? O3 C7 H7 114.2 . . ? C8 C7 H7 114.2 . . ? C9 C7 H7 114.2 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C9' C7' O3 116.0(11) . . ? C9' C7' C8' 125.6(12) . . ? O3 C7' C8' 110.5(6) . . ? C9' C7' H7' 99.4 . . ? O3 C7' H7' 99.4 . . ? C8' C7' H7' 99.4 . . ? C7' C8' H8'1 109.5 . . ? C7' C8' H8'2 109.5 . . ? H8'1 C8' H8'2 109.5 . . ? C7' C8' H8'3 109.5 . . ? H8'1 C8' H8'3 109.5 . . ? H8'2 C8' H8'3 109.5 . . ? C7' C9' H9'1 109.5 . . ? C7' C9' H9'2 109.5 . . ? H9'1 C9' H9'2 109.5 . . ? C7' C9' H9'3 109.5 . . ? H9'1 C9' H9'3 109.5 . . ? H9'2 C9' H9'3 109.5 . . ? O4 C10 C12 106.3(6) . . ? O4 C10 C11 109.3(5) . . ? C12 C10 C11 112.9(6) . . ? O4 C10 H10 109.4 . . ? C12 C10 H10 109.4 . . ? C11 C10 H10 109.4 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C14 123.9(5) . . ? N1 C13 H13 118.1 . . ? C14 C13 H13 118.1 . . ? C13 C14 C15 119.5(4) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C14 C15 N3 125.4(4) . . ? C14 C15 C16 117.2(4) . . ? N3 C15 C16 117.3(4) . . ? C17 C16 C15 119.4(4) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? N1 C17 C16 123.6(4) . . ? N1 C17 H17 118.2 . . ? C16 C17 H17 118.2 . . ? N3 C18 C22 117.9(4) . . ? N3 C18 C19 125.1(4) . . ? C22 C18 C19 116.9(4) . . ? C18 C19 C20 118.5(4) . . ? C18 C19 H19 120.7 . . ? C20 C19 H19 120.7 . . ? N2 C20 C19 124.8(5) . . ? N2 C20 H20 117.6 . . ? C19 C20 H20 117.6 . . ? N2 C21 C22 122.4(5) . . ? N2 C21 H21 118.8 . . ? C22 C21 H21 118.8 . . ? C18 C22 C21 120.6(5) . . ? C18 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.0 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.90 _refine_diff_density_min -0.30 _refine_diff_density_rms 0.083