# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Li-Min Zheng.' 'Song-Song Bao.' 'Jian Huang.' 'Yi-Zhi Li.' 'Xun-Gao Liu.' _publ_contact_author_name 'Li-Min Zheng' _publ_contact_author_email LMZHENG@NETRA.NJU.EDU.CN _publ_section_title ; Homochiral Zinc Phosphonates with Layered and Open Framework Structures Using Polycarboxylate as Second Linkers ; # Attachment 'Zn_R-2.cif' data_sad _database_code_depnum_ccdc_archive 'CCDC 741077' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H32 N2 O16 P2 Zn3, H2 O' _chemical_formula_sum 'C28 H34 N2 O17 P2 Zn3' _chemical_formula_weight 928.62 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' 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 'C2 ' _symmetry_space_group_name_Hall 'C 2y ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 31.1328(16) _cell_length_b 7.6264(9) _cell_length_c 17.631(2) _cell_angle_alpha 90.00 _cell_angle_beta 124.494(3) _cell_angle_gamma 90.00 _cell_volume 3450.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 1887 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 23.31 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.788 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 2.242 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.535 _exptl_absorpt_correction_T_max 0.637 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9356 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0488 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 25.98 _reflns_number_total 6256 _reflns_number_gt 5569 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.07P)^2^+1.99P] 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(4) _chemical_absolute_configuration unk _refine_ls_number_reflns 6256 _refine_ls_number_parameters 447 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1159 _refine_ls_wR_factor_gt 0.1139 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2651(2) 0.3947(9) 0.6873(4) 0.0326(13) Uani 1 1 d . . . H1A H 0.2629 0.4610 0.6382 0.039 Uiso 1 1 calc R . . H1B H 0.2992 0.3399 0.7234 0.039 Uiso 1 1 calc R . . C2 C 0.2179(2) 0.1599(8) 0.5650(4) 0.0319(13) Uani 1 1 d . . . H2A H 0.2053 0.2431 0.5159 0.038 Uiso 1 1 d R . . C3 C 0.1764(3) 0.0217(10) 0.5332(5) 0.0416(16) Uani 1 1 d . . . H3A H 0.1714 -0.0391 0.4811 0.062 Uiso 1 1 calc R . . H3B H 0.1443 0.0765 0.5161 0.062 Uiso 1 1 calc R . . H3C H 0.1870 -0.0601 0.5822 0.062 Uiso 1 1 calc R . . C4 C 0.26932(14) 0.0916(6) 0.5892(3) 0.0308(13) Uani 1 1 d G . . C5 C 0.29845(16) -0.0220(6) 0.6631(3) 0.0430(17) Uani 1 1 d G . . H5 H 0.2866 -0.0528 0.6993 0.052 Uiso 1 1 calc R . . C6 C 0.34522(16) -0.0894(6) 0.6828(3) 0.0471(18) Uani 1 1 d G . . H6 H 0.3647 -0.1654 0.7323 0.057 Uiso 1 1 calc R . . C7 C 0.36286(13) -0.0434(6) 0.6286(3) 0.0431(17) Uani 1 1 d G . . H7 H 0.3941 -0.0885 0.6418 0.052 Uiso 1 1 calc R . . C8 C 0.33373(16) 0.0702(6) 0.5547(3) 0.0501(19) Uani 1 1 d G . . H8 H 0.3455 0.1010 0.5185 0.060 Uiso 1 1 calc R . . C9 C 0.28696(16) 0.1376(6) 0.5350(3) 0.0446(16) Uani 1 1 d G . . H9 H 0.2675 0.2136 0.4855 0.054 Uiso 1 1 calc R . . C10 C 0.1084(2) 0.1221(10) 0.8456(4) 0.0376(14) Uani 1 1 d . . . H10A H 0.1050 0.0539 0.7960 0.045 Uiso 1 1 calc R . . H10B H 0.0920 0.0576 0.8701 0.045 Uiso 1 1 calc R . . C11 C 0.0269(2) 0.2865(10) 0.7276(5) 0.0411(16) Uani 1 1 d . . . H11A H 0.0276 0.2378 0.6781 0.049 Uiso 1 1 d R . . C12 C 0.0056(2) 0.4700(9) 0.6969(5) 0.0379(15) Uani 1 1 d . . . H12A H -0.0295 0.4641 0.6430 0.057 Uiso 1 1 calc R . . H12B H 0.0269 0.5338 0.6829 0.057 Uiso 1 1 calc R . . H12C H 0.0058 0.5287 0.7453 0.057 Uiso 1 1 calc R . . C13 C -0.00699(15) 0.1652(5) 0.7402(3) 0.0320(14) Uani 1 1 d G . . C14 C -0.02422(19) 0.0078(6) 0.6921(3) 0.0479(18) Uani 1 1 d G . . H14 H -0.0143 -0.0238 0.6531 0.057 Uiso 1 1 calc R . . C15 C -0.05625(19) -0.1023(5) 0.7022(3) 0.056(2) Uani 1 1 d G . . H15 H -0.0678 -0.2075 0.6700 0.067 Uiso 1 1 calc R . . C16 C -0.07104(16) -0.0550(6) 0.7604(3) 0.0487(19) Uani 1 1 d G . . H16 H -0.0925 -0.1287 0.7672 0.058 Uiso 1 1 calc R . . C17 C -0.05381(16) 0.1023(6) 0.8086(3) 0.0421(16) Uani 1 1 d G . . H17 H -0.0637 0.1339 0.8475 0.050 Uiso 1 1 calc R . . C18 C -0.02179(15) 0.2124(5) 0.7985(3) 0.0372(14) Uani 1 1 d G . . H18 H -0.0103 0.3177 0.8307 0.045 Uiso 1 1 calc R . . C19 C 0.0948(3) 0.9436(9) 0.6235(5) 0.0390(16) Uani 1 1 d . . . C20 C 0.0474(2) 1.0447(9) 0.5565(4) 0.0319(13) Uani 1 1 d . . . C21 C 0.0469(2) 1.2263(9) 0.5542(4) 0.0305(13) Uani 1 1 d . . . C22 C 0.0954(2) 1.3384(9) 0.6049(4) 0.0312(13) Uani 1 1 d . . . C23 C 0.0000 1.3217(13) 0.5000 0.036(2) Uani 1 2 d S . . H23A H 0.0000 1.4437 0.5000 0.044 Uiso 1 2 calc SR . . C24 C 0.0000 0.9542(12) 0.5000 0.040(2) Uani 1 2 d S . . H24A H 0.0000 0.8322 0.5000 0.048 Uiso 1 2 calc SR . . C25 C 0.0855(2) -0.0959(8) 1.0179(4) 0.0330(14) Uani 1 1 d . . . C26 C 0.0413(2) -0.1974(9) 1.0080(4) 0.0350(15) Uani 1 1 d . . . C27 C 0.0407(2) -0.3799(10) 1.0064(4) 0.0327(13) Uani 1 1 d . . . C28 C 0.0808(2) -0.4916(9) 1.0058(5) 0.0373(15) Uani 1 1 d . . . C29 C 0.0000 -0.4698(12) 1.0000 0.0332(19) Uani 1 2 d S . . H29A H 0.0000 -0.5918 1.0000 0.040 Uiso 1 2 calc SR . . C30 C 0.0000 -0.1148(12) 1.0000 0.0322(19) Uani 1 2 d S . . H30A H 0.0000 0.0072 1.0000 0.039 Uiso 1 2 calc SR . . N1 N 0.22422(19) 0.2559(6) 0.6462(3) 0.0302(11) Uani 1 1 d . . . H1C H 0.1935 0.3053 0.6279 0.036 Uiso 1 1 calc R . . H1D H 0.2320 0.1770 0.6902 0.036 Uiso 1 1 calc R . . N2 N 0.0824(2) 0.2943(7) 0.8099(3) 0.0330(12) Uani 1 1 d . . . H2B H 0.1009 0.3582 0.7951 0.040 Uiso 1 1 calc R . . H2C H 0.0831 0.3511 0.8554 0.040 Uiso 1 1 calc R . . O1 O 0.25339(17) 0.4293(6) 0.8232(3) 0.0349(10) Uani 1 1 d . . . O2 O 0.20779(15) 0.6419(6) 0.6962(3) 0.0353(10) Uani 1 1 d . . . O3 O 0.30447(17) 0.6616(6) 0.7999(3) 0.0413(12) Uani 1 1 d . . . O4 O 0.19842(16) 0.2742(6) 0.8963(3) 0.0330(10) Uani 1 1 d . . . O5 O 0.18003(14) 0.2421(6) 1.0155(3) 0.0323(10) Uani 1 1 d . . . O6 O 0.20017(14) -0.0261(6) 0.9566(3) 0.0283(9) Uani 1 1 d . . . O7 O 0.09214(18) 0.7796(6) 0.6086(3) 0.0422(11) Uani 1 1 d . . . O8 O 0.13292(19) 1.0208(7) 0.6846(3) 0.0557(15) Uani 1 1 d . . . O9 O 0.12006(16) 1.3570(6) 0.5705(3) 0.0355(10) Uani 1 1 d . . . O10 O 0.10555(16) 1.4163(6) 0.6771(3) 0.0345(10) Uani 1 1 d . . . O11 O 0.08154(16) 0.0698(6) 1.0199(3) 0.0336(10) Uani 1 1 d . . . O12 O 0.12274(18) -0.1687(7) 1.0282(3) 0.0460(12) Uani 1 1 d . . . O13 O 0.07640(16) -0.5179(6) 0.9338(3) 0.0389(11) Uani 1 1 d . . . O14 O 0.11293(17) -0.5676(6) 1.0811(3) 0.0358(10) Uani 1 1 d . . . O1W O 0.31338(16) 0.1163(6) 0.9909(3) 0.0358(10) Uani 1 1 d . . . H1WA H 0.3457 0.1336 0.9970 0.043 Uiso 1 1 d R . . H1WB H 0.2959 0.0154 0.9531 0.043 Uiso 1 1 d R . . O2W O 0.16679(18) 0.6800(6) 0.8268(3) 0.0406(11) Uani 1 1 d . . . H2WA H 0.1779 0.5740 0.8624 0.049 Uiso 1 1 d R . . H2WB H 0.1946 0.7641 0.8558 0.049 Uiso 1 1 d R . . O3W O 0.23966(17) 1.0204(6) 0.7839(3) 0.0375(10) Uani 1 1 d . . . H3WA H 0.2673 0.9618 0.8035 0.045 Uiso 1 1 d R . . H3WB H 0.2139 0.9509 0.7612 0.045 Uiso 1 1 d R . . P1 P 0.25828(5) 0.5427(2) 0.75961(10) 0.0274(3) Uani 1 1 d . . . P2 P 0.17698(6) 0.1545(2) 0.93559(11) 0.0308(3) Uani 1 1 d . . . Zn1 Zn 0.26875(3) 0.32663(9) 0.93253(4) 0.02831(16) Uani 1 1 d . . . Zn2 Zn 0.14784(2) 0.62634(9) 0.69838(5) 0.02937(17) Uani 1 1 d . . . Zn3 Zn 0.14264(3) 0.21382(9) 1.07307(5) 0.03263(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.035(3) 0.032(3) 0.035(3) 0.001(2) 0.022(3) -0.002(3) C2 0.033(3) 0.028(3) 0.028(3) 0.000(2) 0.014(2) 0.006(2) C3 0.040(4) 0.032(4) 0.050(4) -0.013(3) 0.024(3) -0.005(3) C4 0.033(3) 0.025(3) 0.019(2) 0.003(2) 0.006(2) 0.010(2) C5 0.051(4) 0.035(4) 0.039(4) 0.018(3) 0.023(3) 0.022(3) C6 0.037(4) 0.038(4) 0.047(4) 0.018(3) 0.012(3) 0.015(3) C7 0.027(3) 0.045(4) 0.038(4) -0.014(3) 0.007(3) -0.004(3) C8 0.050(4) 0.041(4) 0.034(4) -0.017(3) 0.009(3) -0.010(3) C9 0.052(4) 0.030(3) 0.047(4) 0.011(3) 0.025(3) -0.001(3) C10 0.036(3) 0.047(4) 0.020(3) 0.004(3) 0.010(2) 0.015(3) C11 0.030(3) 0.048(4) 0.039(4) 0.006(3) 0.016(3) 0.000(3) C12 0.028(3) 0.043(4) 0.044(4) 0.005(3) 0.021(3) 0.005(3) C13 0.024(3) 0.030(3) 0.036(3) 0.003(2) 0.013(3) 0.002(2) C14 0.058(5) 0.040(4) 0.036(4) -0.008(3) 0.021(4) -0.008(3) C15 0.056(5) 0.044(4) 0.043(4) -0.010(3) 0.014(4) -0.020(4) C16 0.030(3) 0.050(5) 0.050(4) 0.016(3) 0.013(3) 0.004(3) C17 0.030(3) 0.053(5) 0.028(3) 0.019(3) 0.008(3) 0.011(3) C18 0.033(3) 0.039(3) 0.029(3) 0.010(3) 0.011(3) 0.009(3) C19 0.036(3) 0.024(3) 0.037(4) 0.005(3) 0.009(3) 0.000(3) C20 0.026(3) 0.032(3) 0.031(3) 0.003(3) 0.012(3) -0.002(2) C21 0.020(3) 0.032(3) 0.022(3) 0.010(3) 0.001(2) 0.001(2) C22 0.028(3) 0.034(3) 0.019(2) 0.007(3) 0.005(2) -0.004(3) C23 0.027(4) 0.030(4) 0.025(4) 0.000 -0.002(3) 0.000 C24 0.039(5) 0.019(4) 0.031(5) 0.000 0.002(4) 0.000 C25 0.034(3) 0.020(3) 0.032(3) 0.004(2) 0.011(3) 0.001(2) C26 0.025(3) 0.044(4) 0.024(3) 0.002(3) 0.007(2) 0.001(3) C27 0.027(3) 0.042(4) 0.025(3) 0.006(3) 0.012(2) -0.001(3) C28 0.021(3) 0.035(4) 0.039(4) -0.002(3) 0.007(3) 0.002(3) C29 0.032(4) 0.024(5) 0.038(5) 0.000 0.017(4) 0.000 C30 0.029(4) 0.028(5) 0.034(4) 0.000 0.015(4) 0.000 N1 0.024(2) 0.025(3) 0.024(2) -0.0017(18) 0.003(2) 0.0038(19) N2 0.033(3) 0.031(3) 0.025(2) 0.002(2) 0.011(2) -0.002(2) O1 0.044(3) 0.030(2) 0.024(2) -0.0026(17) 0.016(2) -0.009(2) O2 0.0223(19) 0.035(2) 0.038(2) 0.010(2) 0.0106(18) 0.0026(18) O3 0.039(2) 0.045(3) 0.026(2) -0.0024(19) 0.0100(19) -0.021(2) O4 0.027(2) 0.043(3) 0.0201(19) 0.0047(16) 0.0076(17) -0.0003(17) O5 0.0211(18) 0.036(3) 0.025(2) 0.0005(18) 0.0043(16) 0.0011(17) O6 0.0191(18) 0.032(2) 0.0257(19) 0.0018(17) 0.0080(17) 0.0044(16) O7 0.033(2) 0.030(3) 0.043(3) 0.0004(19) 0.009(2) 0.0088(18) O8 0.036(3) 0.042(3) 0.038(3) 0.002(2) -0.010(2) 0.005(2) O9 0.038(2) 0.031(3) 0.034(2) -0.0140(18) 0.019(2) -0.0116(19) O10 0.030(2) 0.033(2) 0.025(2) 0.0032(18) 0.0070(18) 0.0004(18) O11 0.028(2) 0.027(2) 0.035(2) -0.0019(18) 0.0114(19) 0.0004(17) O12 0.046(3) 0.026(2) 0.053(3) -0.019(2) 0.020(2) 0.001(2) O13 0.023(2) 0.028(2) 0.047(3) -0.002(2) 0.008(2) 0.0107(18) O14 0.032(2) 0.029(2) 0.034(2) 0.0044(18) 0.011(2) 0.0022(18) O1W 0.030(2) 0.023(2) 0.038(2) 0.0049(19) 0.0094(18) 0.0015(18) O2W 0.045(2) 0.036(3) 0.030(2) -0.0199(18) 0.014(2) -0.018(2) O3W 0.029(2) 0.031(2) 0.041(3) 0.0041(19) 0.013(2) -0.0018(18) P1 0.0212(7) 0.0257(8) 0.0272(7) 0.0031(6) 0.0090(6) -0.0022(6) P2 0.0296(7) 0.0248(8) 0.0310(7) 0.0008(6) 0.0130(6) 0.0023(6) Zn1 0.0325(4) 0.0265(3) 0.0255(3) 0.0049(3) 0.0162(3) -0.0032(3) Zn2 0.0243(3) 0.0253(4) 0.0276(3) 0.0013(3) 0.0081(3) -0.0006(3) Zn3 0.0305(3) 0.0258(4) 0.0310(4) 0.0020(3) 0.0111(3) 0.0002(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 C1 N1 1.490(8) . ? C1 P1 1.803(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C4 1.497(7) . ? C2 C3 1.509(9) . ? C2 N1 1.519(8) . ? C2 H2A 0.9597 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C5 1.3900 . ? C4 C9 1.3900 . ? C5 C6 1.3900 . ? C5 H5 0.9300 . ? C6 C7 1.3900 . ? C6 H6 0.9300 . ? C7 C8 1.3900 . ? C7 H7 0.9300 . ? C8 C9 1.3900 . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 N2 1.484(9) . ? C10 P2 1.816(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.501(8) . ? C11 C12 1.512(10) . ? C11 C13 1.513(7) . ? C11 H11A 0.9596 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C14 C15 1.3900 . ? C14 H14 0.9300 . ? C15 C16 1.3900 . ? C15 H15 0.9300 . ? C16 C17 1.3900 . ? C16 H16 0.9300 . ? C17 C18 1.3900 . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 O8 1.211(8) . ? C19 O7 1.271(8) . ? C19 C20 1.481(9) . ? C20 C21 1.386(9) . ? C20 C24 1.408(7) . ? C21 C23 1.413(8) . ? C21 C22 1.510(8) . ? C22 O9 1.227(7) . ? C22 O10 1.272(8) . ? C23 C21 1.413(8) 2_556 ? C23 H23A 0.9300 . ? C24 C20 1.408(7) 2_556 ? C24 H24A 0.9300 . ? C25 O12 1.203(8) . ? C25 O11 1.273(8) . ? C25 C26 1.501(9) . ? C26 C30 1.365(8) . ? C26 C27 1.392(10) . ? C27 C29 1.387(8) . ? C27 C28 1.517(9) . ? C28 O13 1.213(9) . ? C28 O14 1.263(8) . ? C29 C27 1.387(8) 2_557 ? C29 H29A 0.9300 . ? C30 C26 1.365(8) 2_557 ? C30 H30A 0.9300 . ? N1 H1C 0.9000 . ? N1 H1D 0.9000 . ? N2 H2B 0.9000 . ? N2 H2C 0.9000 . ? O1 P1 1.490(4) . ? O1 Zn1 1.874(4) . ? O2 P1 1.518(4) . ? O2 Zn2 1.892(4) . ? O3 P1 1.496(4) . ? O3 Zn3 1.926(4) 4_557 ? O4 P2 1.512(5) . ? O4 Zn1 1.943(4) . ? O5 P2 1.512(5) . ? O5 Zn3 1.942(4) . ? O6 P2 1.501(4) . ? O6 Zn1 1.969(4) 4_547 ? O7 Zn2 1.941(4) . ? O10 Zn2 1.970(5) 1_565 ? O11 Zn3 1.919(4) . ? O14 Zn3 1.950(5) 1_545 ? O1W Zn1 1.986(4) . ? O1W H1WA 0.9596 . ? O1W H1WB 0.9597 . ? O2W Zn2 2.033(4) . ? O2W H2WA 0.9597 . ? O2W H2WB 0.9597 . ? O3W H3WA 0.8496 . ? O3W H3WB 0.8496 . ? Zn1 O6 1.969(4) 4_557 ? Zn2 O10 1.970(5) 1_545 ? Zn3 O3 1.926(4) 4_547 ? Zn3 O14 1.950(5) 1_565 ? 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 C1 P1 112.2(4) . . ? N1 C1 H1A 109.2 . . ? P1 C1 H1A 109.2 . . ? N1 C1 H1B 109.2 . . ? P1 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? C4 C2 C3 114.6(5) . . ? C4 C2 N1 110.7(4) . . ? C3 C2 N1 108.2(5) . . ? C4 C2 H2A 108.1 . . ? C3 C2 H2A 107.5 . . ? N1 C2 H2A 107.5 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C9 120.0 . . ? C5 C4 C2 120.5(3) . . ? C9 C4 C2 119.4(3) . . ? C4 C5 C6 120.0 . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C7 C6 C5 120.0 . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C8 C7 C6 120.0 . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C9 C8 C7 120.0 . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C4 120.0 . . ? C8 C9 H9 120.0 . . ? C4 C9 H9 120.0 . . ? N2 C10 P2 109.9(5) . . ? N2 C10 H10A 109.7 . . ? P2 C10 H10A 109.7 . . ? N2 C10 H10B 109.7 . . ? P2 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? N2 C11 C12 109.9(6) . . ? N2 C11 C13 113.5(5) . . ? C12 C11 C13 114.6(5) . . ? N2 C11 H11A 106.8 . . ? C12 C11 H11A 105.3 . . ? C13 C11 H11A 106.0 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 120.0 . . ? C14 C13 C11 119.9(4) . . ? C18 C13 C11 120.1(4) . . ? C13 C14 C15 120.0 . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C16 C15 C14 120.0 . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C17 C16 C15 120.0 . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C16 C17 C18 120.0 . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C13 120.0 . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? O8 C19 O7 125.3(6) . . ? O8 C19 C20 119.2(6) . . ? O7 C19 C20 115.4(6) . . ? C21 C20 C24 118.7(6) . . ? C21 C20 C19 122.2(6) . . ? C24 C20 C19 118.7(6) . . ? C20 C21 C23 121.7(6) . . ? C20 C21 C22 123.9(5) . . ? C23 C21 C22 114.4(6) . . ? O9 C22 O10 124.8(6) . . ? O9 C22 C21 117.9(5) . . ? O10 C22 C21 117.1(5) . . ? C21 C23 C21 118.0(9) . 2_556 ? C21 C23 H23A 121.0 . . ? C21 C23 H23A 121.0 2_556 . ? C20 C24 C20 121.3(8) . 2_556 ? C20 C24 H24A 119.4 . . ? C20 C24 H24A 119.4 2_556 . ? O12 C25 O11 123.6(6) . . ? O12 C25 C26 121.5(6) . . ? O11 C25 C26 114.8(6) . . ? C30 C26 C27 117.3(7) . . ? C30 C26 C25 121.4(7) . . ? C27 C26 C25 121.2(6) . . ? C29 C27 C26 119.8(6) . . ? C29 C27 C28 116.1(7) . . ? C26 C27 C28 124.1(6) . . ? O13 C28 O14 125.2(6) . . ? O13 C28 C27 119.6(6) . . ? O14 C28 C27 114.6(6) . . ? C27 C29 C27 120.8(9) . 2_557 ? C27 C29 H29A 119.6 . . ? C27 C29 H29A 119.6 2_557 . ? C26 C30 C26 125.0(9) 2_557 . ? C26 C30 H30A 117.5 2_557 . ? C26 C30 H30A 117.5 . . ? C1 N1 C2 114.8(5) . . ? C1 N1 H1C 108.6 . . ? C2 N1 H1C 108.6 . . ? C1 N1 H1D 108.6 . . ? C2 N1 H1D 108.6 . . ? H1C N1 H1D 107.5 . . ? C10 N2 C11 115.4(5) . . ? C10 N2 H2B 108.4 . . ? C11 N2 H2B 108.4 . . ? C10 N2 H2C 108.4 . . ? C11 N2 H2C 108.4 . . ? H2B N2 H2C 107.5 . . ? P1 O1 Zn1 160.2(3) . . ? P1 O2 Zn2 125.2(3) . . ? P1 O3 Zn3 129.5(3) . 4_557 ? P2 O4 Zn1 132.9(3) . . ? P2 O5 Zn3 134.2(3) . . ? P2 O6 Zn1 131.7(3) . 4_547 ? C19 O7 Zn2 120.0(4) . . ? C22 O10 Zn2 109.3(4) . 1_565 ? C25 O11 Zn3 119.8(4) . . ? C28 O14 Zn3 116.2(5) . 1_545 ? Zn1 O1W H1WA 109.2 . . ? Zn1 O1W H1WB 109.5 . . ? H1WA O1W H1WB 109.5 . . ? Zn2 O2W H2WA 109.2 . . ? Zn2 O2W H2WB 109.4 . . ? H2WA O2W H2WB 109.5 . . ? H3WA O3W H3WB 109.5 . . ? O1 P1 O3 118.3(2) . . ? O1 P1 O2 109.8(3) . . ? O3 P1 O2 111.3(3) . . ? O1 P1 C1 105.8(3) . . ? O3 P1 C1 104.4(3) . . ? O2 P1 C1 106.2(3) . . ? O6 P2 O4 113.1(2) . . ? O6 P2 O5 114.1(2) . . ? O4 P2 O5 110.4(3) . . ? O6 P2 C10 104.7(3) . . ? O4 P2 C10 106.7(3) . . ? O5 P2 C10 107.3(3) . . ? O1 Zn1 O4 99.42(18) . . ? O1 Zn1 O6 118.58(19) . 4_557 ? O4 Zn1 O6 105.82(17) . 4_557 ? O1 Zn1 O1W 124.5(2) . . ? O4 Zn1 O1W 109.37(18) . . ? O6 Zn1 O1W 98.05(18) 4_557 . ? O2 Zn2 O7 112.4(2) . . ? O2 Zn2 O10 127.4(2) . 1_545 ? O7 Zn2 O10 98.18(19) . 1_545 ? O2 Zn2 O2W 110.04(19) . . ? O7 Zn2 O2W 110.4(2) . . ? O10 Zn2 O2W 96.69(18) 1_545 . ? O11 Zn3 O3 114.1(2) . 4_547 ? O11 Zn3 O5 122.00(18) . . ? O3 Zn3 O5 105.08(19) 4_547 . ? O11 Zn3 O14 98.33(19) . 1_565 ? O3 Zn3 O14 102.75(18) 4_547 1_565 ? O5 Zn3 O14 113.1(2) . 1_565 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 C2 C4 C5 -65.0(6) . . . . ? N1 C2 C4 C5 57.7(6) . . . . ? C3 C2 C4 C9 112.7(5) . . . . ? N1 C2 C4 C9 -124.6(4) . . . . ? C9 C4 C5 C6 0.0 . . . . ? C2 C4 C5 C6 177.7(5) . . . . ? C4 C5 C6 C7 0.0 . . . . ? C5 C6 C7 C8 0.0 . . . . ? C6 C7 C8 C9 0.0 . . . . ? C7 C8 C9 C4 0.0 . . . . ? C5 C4 C9 C8 0.0 . . . . ? C2 C4 C9 C8 -177.7(5) . . . . ? N2 C11 C13 C14 -109.2(5) . . . . ? C12 C11 C13 C14 123.4(5) . . . . ? N2 C11 C13 C18 72.1(6) . . . . ? C12 C11 C13 C18 -55.3(7) . . . . ? C18 C13 C14 C15 0.0 . . . . ? C11 C13 C14 C15 -178.7(5) . . . . ? C13 C14 C15 C16 0.0 . . . . ? C14 C15 C16 C17 0.0 . . . . ? C15 C16 C17 C18 0.0 . . . . ? C16 C17 C18 C13 0.0 . . . . ? C14 C13 C18 C17 0.0 . . . . ? C11 C13 C18 C17 178.7(5) . . . . ? O8 C19 C20 C21 7.8(11) . . . . ? O7 C19 C20 C21 -169.2(7) . . . . ? O8 C19 C20 C24 -165.1(7) . . . . ? O7 C19 C20 C24 17.8(10) . . . . ? C24 C20 C21 C23 2.8(9) . . . . ? C19 C20 C21 C23 -170.1(5) . . . . ? C24 C20 C21 C22 -174.5(4) . . . . ? C19 C20 C21 C22 12.6(11) . . . . ? C20 C21 C22 O9 79.7(8) . . . . ? C23 C21 C22 O9 -97.8(7) . . . . ? C20 C21 C22 O10 -105.0(8) . . . . ? C23 C21 C22 O10 77.5(6) . . . . ? C20 C21 C23 C21 -1.5(5) . . . 2_556 ? C22 C21 C23 C21 176.1(6) . . . 2_556 ? C21 C20 C24 C20 -1.4(5) . . . 2_556 ? C19 C20 C24 C20 171.8(7) . . . 2_556 ? O12 C25 C26 C30 177.3(5) . . . . ? O11 C25 C26 C30 1.3(8) . . . . ? O12 C25 C26 C27 -2.9(10) . . . . ? O11 C25 C26 C27 -178.9(6) . . . . ? C30 C26 C27 C29 -2.2(8) . . . . ? C25 C26 C27 C29 178.0(5) . . . . ? C30 C26 C27 C28 174.3(5) . . . . ? C25 C26 C27 C28 -5.6(10) . . . . ? C29 C27 C28 O13 94.4(7) . . . . ? C26 C27 C28 O13 -82.2(9) . . . . ? C29 C27 C28 O14 -77.2(7) . . . . ? C26 C27 C28 O14 106.3(7) . . . . ? C26 C27 C29 C27 1.1(4) . . . 2_557 ? C28 C27 C29 C27 -175.6(6) . . . 2_557 ? C27 C26 C30 C26 1.1(4) . . . 2_557 ? C25 C26 C30 C26 -179.1(6) . . . 2_557 ? P1 C1 N1 C2 163.5(4) . . . . ? C4 C2 N1 C1 52.3(6) . . . . ? C3 C2 N1 C1 178.6(5) . . . . ? P2 C10 N2 C11 173.1(4) . . . . ? C12 C11 N2 C10 -178.5(5) . . . . ? C13 C11 N2 C10 51.6(8) . . . . ? O8 C19 O7 Zn2 10.5(12) . . . . ? C20 C19 O7 Zn2 -172.6(4) . . . . ? O9 C22 O10 Zn2 20.4(8) . . . 1_565 ? C21 C22 O10 Zn2 -154.5(4) . . . 1_565 ? O12 C25 O11 Zn3 -17.3(9) . . . . ? C26 C25 O11 Zn3 158.6(4) . . . . ? O13 C28 O14 Zn3 -18.6(9) . . . 1_545 ? C27 C28 O14 Zn3 152.4(5) . . . 1_545 ? Zn1 O1 P1 O3 0.1(11) . . . . ? Zn1 O1 P1 O2 -129.2(9) . . . . ? Zn1 O1 P1 C1 116.6(9) . . . . ? Zn3 O3 P1 O1 -7.7(5) 4_557 . . . ? Zn3 O3 P1 O2 120.9(4) 4_557 . . . ? Zn3 O3 P1 C1 -125.0(4) 4_557 . . . ? Zn2 O2 P1 O1 0.7(4) . . . . ? Zn2 O2 P1 O3 -132.3(3) . . . . ? Zn2 O2 P1 C1 114.6(4) . . . . ? N1 C1 P1 O1 50.0(5) . . . . ? N1 C1 P1 O3 175.6(4) . . . . ? N1 C1 P1 O2 -66.7(5) . . . . ? Zn1 O6 P2 O4 130.2(3) 4_547 . . . ? Zn1 O6 P2 O5 2.9(4) 4_547 . . . ? Zn1 O6 P2 C10 -114.1(4) 4_547 . . . ? Zn1 O4 P2 O6 -47.6(4) . . . . ? Zn1 O4 P2 O5 81.6(4) . . . . ? Zn1 O4 P2 C10 -162.2(4) . . . . ? Zn3 O5 P2 O6 -75.1(4) . . . . ? Zn3 O5 P2 O4 156.3(3) . . . . ? Zn3 O5 P2 C10 40.4(5) . . . . ? N2 C10 P2 O6 -172.5(4) . . . . ? N2 C10 P2 O4 -52.4(5) . . . . ? N2 C10 P2 O5 65.9(5) . . . . ? P1 O1 Zn1 O4 151.5(9) . . . . ? P1 O1 Zn1 O6 37.6(10) . . . 4_557 ? P1 O1 Zn1 O1W -87.0(10) . . . . ? P2 O4 Zn1 O1 163.1(4) . . . . ? P2 O4 Zn1 O6 -73.5(4) . . . 4_557 ? P2 O4 Zn1 O1W 31.2(4) . . . . ? P1 O2 Zn2 O7 178.2(3) . . . . ? P1 O2 Zn2 O10 -61.1(4) . . . 1_545 ? P1 O2 Zn2 O2W 54.7(4) . . . . ? C19 O7 Zn2 O2 -75.6(6) . . . . ? C19 O7 Zn2 O10 148.0(6) . . . 1_545 ? C19 O7 Zn2 O2W 47.7(6) . . . . ? C25 O11 Zn3 O3 -59.0(5) . . . 4_547 ? C25 O11 Zn3 O5 69.0(5) . . . . ? C25 O11 Zn3 O14 -167.0(5) . . . 1_565 ? P2 O5 Zn3 O11 -9.3(4) . . . . ? P2 O5 Zn3 O3 122.5(4) . . . 4_547 ? P2 O5 Zn3 O14 -126.2(3) . . . 1_565 ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.433 _refine_diff_density_min -0.535 _refine_diff_density_rms 0.095 # Attachment 'Zn_S-1.cif' data_Zn _database_code_depnum_ccdc_archive 'CCDC 741078' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H60 N4 O20 P4 Zn4, 2(H2 O)' _chemical_formula_sum 'C52 H64 N4 O22 P4 Zn4' _chemical_formula_weight 1482.43 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P2(1)2(1)2 ' _symmetry_space_group_name_Hall 'P 2 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 22.773(3) _cell_length_b 27.901(4) _cell_length_c 9.9919(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6348.7(16) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 4111 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 23.13 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3040 _exptl_absorpt_coefficient_mu 1.670 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.65 _exptl_absorpt_correction_T_max 0.72 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD ' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34419 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0469 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 26.00 _reflns_number_total 12451 _reflns_number_gt 10454 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0477P)^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 0.027(8) _chemical_absolute_configuration unk _refine_ls_number_reflns 12451 _refine_ls_number_parameters 788 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0532 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.0900 _refine_ls_wR_factor_gt 0.0877 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.41639(17) 0.41721(15) -0.0247(4) 0.0360(9) Uani 1 1 d . . . H1A H 0.4544 0.4328 -0.0206 0.043 Uiso 1 1 calc R . . H1B H 0.4199 0.3863 0.0188 0.043 Uiso 1 1 calc R . . C2 C 0.44275(19) 0.38151(14) -0.2508(4) 0.0366(9) Uani 1 1 d . . . H2A H 0.4247 0.3781 -0.3394 0.044 Uiso 1 1 calc R . . C3 C 0.49753(18) 0.40950(15) -0.2670(4) 0.0424(10) Uani 1 1 d . . . H3A H 0.5243 0.3922 -0.3234 0.064 Uiso 1 1 calc R . . H3B H 0.5152 0.4145 -0.1809 0.064 Uiso 1 1 calc R . . H3C H 0.4886 0.4399 -0.3070 0.064 Uiso 1 1 calc R . . C4 C 0.45051(18) 0.33283(15) -0.1944(4) 0.0362(9) Uani 1 1 d . . . C5 C 0.50325(18) 0.31741(15) -0.1395(5) 0.0445(11) Uani 1 1 d . . . H5A H 0.5345 0.3387 -0.1315 0.053 Uiso 1 1 calc R . . C6 C 0.50962(19) 0.27067(16) -0.0967(5) 0.0432(10) Uani 1 1 d . . . H6A H 0.5455 0.2605 -0.0623 0.052 Uiso 1 1 calc R . . C7 C 0.4632(2) 0.23887(17) -0.1044(5) 0.0466(11) Uani 1 1 d . . . H7A H 0.4673 0.2076 -0.0733 0.056 Uiso 1 1 calc R . . C8 C 0.4098(2) 0.25412(17) -0.1596(5) 0.0481(11) Uani 1 1 d . . . H8A H 0.3785 0.2329 -0.1670 0.058 Uiso 1 1 calc R . . C9 C 0.4039(2) 0.30067(17) -0.2030(5) 0.0468(11) Uani 1 1 d . . . H9A H 0.3683 0.3108 -0.2384 0.056 Uiso 1 1 calc R . . C10 C 0.41620(16) 0.53969(13) 0.4824(4) 0.0294(8) Uani 1 1 d . . . H10A H 0.4178 0.5696 0.5316 0.035 Uiso 1 1 calc R . . H10B H 0.4547 0.5249 0.4883 0.035 Uiso 1 1 calc R . . C11 C 0.44950(16) 0.58326(15) 0.2798(4) 0.0331(9) Uani 1 1 d . . . H11A H 0.4873 0.5665 0.2808 0.040 Uiso 1 1 calc R . . C12 C 0.43243(16) 0.59320(14) 0.1322(4) 0.0332(8) Uani 1 1 d . . . H12A H 0.4607 0.6144 0.0927 0.050 Uiso 1 1 calc R . . H12B H 0.3943 0.6078 0.1292 0.050 Uiso 1 1 calc R . . H12C H 0.4317 0.5636 0.0834 0.050 Uiso 1 1 calc R . . C13 C 0.45631(17) 0.62918(14) 0.3538(4) 0.0344(9) Uani 1 1 d . . . C14 C 0.51311(18) 0.64567(15) 0.3761(4) 0.0382(10) Uani 1 1 d . . . H14A H 0.5451 0.6271 0.3503 0.046 Uiso 1 1 calc R . . C15 C 0.5222(2) 0.69013(16) 0.4374(4) 0.0429(10) Uani 1 1 d . . . H15A H 0.5602 0.7014 0.4502 0.051 Uiso 1 1 calc R . . C16 C 0.47466(19) 0.71742(17) 0.4792(5) 0.0461(10) Uani 1 1 d . . . H16A H 0.4808 0.7466 0.5218 0.055 Uiso 1 1 calc R . . C17 C 0.41778(19) 0.70089(15) 0.4571(4) 0.0409(10) Uani 1 1 d . . . H17A H 0.3859 0.7194 0.4836 0.049 Uiso 1 1 calc R . . C18 C 0.40847(18) 0.65683(15) 0.3956(4) 0.0380(9) Uani 1 1 d . . . H18A H 0.3704 0.6457 0.3823 0.046 Uiso 1 1 calc R . . C19 C 0.13744(19) 0.52214(15) 0.8904(4) 0.0368(9) Uani 1 1 d . . . H19A H 0.1088 0.5345 0.8273 0.044 Uiso 1 1 calc R . . H19B H 0.1175 0.5001 0.9501 0.044 Uiso 1 1 calc R . . C20 C 0.12461(18) 0.58181(15) 1.0810(4) 0.0365(9) Uani 1 1 d . . . H20A H 0.1227 0.5580 1.1529 0.044 Uiso 1 1 calc R . . C21 C 0.15518(18) 0.62591(15) 1.1330(4) 0.0410(10) Uani 1 1 d . . . H21A H 0.1316 0.6405 1.2015 0.062 Uiso 1 1 calc R . . H21B H 0.1608 0.6482 1.0611 0.062 Uiso 1 1 calc R . . H21C H 0.1926 0.6171 1.1696 0.062 Uiso 1 1 calc R . . C22 C 0.06482(17) 0.59170(16) 1.0338(4) 0.0382(9) Uani 1 1 d . . . C23 C 0.05348(18) 0.62361(14) 0.9309(4) 0.0367(9) Uani 1 1 d . . . H23A H 0.0845 0.6373 0.8837 0.044 Uiso 1 1 calc R . . C24 C -0.00417(19) 0.63532(16) 0.8976(4) 0.0438(10) Uani 1 1 d . . . H24A H -0.0116 0.6569 0.8286 0.053 Uiso 1 1 calc R . . C25 C -0.0506(2) 0.61478(18) 0.9674(5) 0.0513(12) Uani 1 1 d . . . H25A H -0.0891 0.6225 0.9453 0.062 Uiso 1 1 calc R . . C26 C -0.03906(19) 0.58267(17) 1.0705(4) 0.0459(11) Uani 1 1 d . . . H26A H -0.0701 0.5689 1.1171 0.055 Uiso 1 1 calc R . . C27 C 0.01808(19) 0.57102(17) 1.1047(4) 0.0446(11) Uani 1 1 d . . . H27A H 0.0254 0.5496 1.1742 0.054 Uiso 1 1 calc R . . C28 C 0.13935(16) 0.43715(13) 0.3669(4) 0.0305(8) Uani 1 1 d . . . H28A H 0.1087 0.4588 0.3964 0.037 Uiso 1 1 calc R . . H28B H 0.1228 0.4162 0.2993 0.037 Uiso 1 1 calc R . . C29 C 0.12113(16) 0.36714(14) 0.5220(4) 0.0323(8) Uani 1 1 d . . . H29A H 0.1237 0.3428 0.4516 0.039 Uiso 1 1 calc R . . C30 C 0.14049(18) 0.34443(15) 0.6514(4) 0.0386(9) Uani 1 1 d . . . H30A H 0.1151 0.3180 0.6723 0.058 Uiso 1 1 calc R . . H30B H 0.1387 0.3677 0.7220 0.058 Uiso 1 1 calc R . . H30C H 0.1801 0.3331 0.6423 0.058 Uiso 1 1 calc R . . C31 C 0.05866(16) 0.38385(14) 0.5291(4) 0.0345(9) Uani 1 1 d . . . C32 C 0.01663(17) 0.36155(16) 0.4497(4) 0.0410(10) Uani 1 1 d . . . H32A H 0.0272 0.3360 0.3951 0.049 Uiso 1 1 calc R . . C33 C -0.04109(19) 0.37736(16) 0.4518(5) 0.0453(11) Uani 1 1 d . . . H33A H -0.0692 0.3623 0.3991 0.054 Uiso 1 1 calc R . . C34 C -0.0568(2) 0.41577(17) 0.5329(5) 0.0484(11) Uani 1 1 d . . . H34A H -0.0954 0.4266 0.5341 0.058 Uiso 1 1 calc R . . C35 C -0.01481(18) 0.43793(17) 0.6121(5) 0.0429(10) Uani 1 1 d . . . H35A H -0.0252 0.4637 0.6662 0.051 Uiso 1 1 calc R . . C36 C 0.04283(19) 0.42169(16) 0.6105(5) 0.0436(11) Uani 1 1 d . . . H36A H 0.0708 0.4363 0.6645 0.052 Uiso 1 1 calc R . . C37 C 0.19173(18) 0.33037(14) 0.1216(4) 0.0377(9) Uani 1 1 d . . . C38 C 0.18791(19) 0.27733(15) 0.1087(4) 0.0419(10) Uani 1 1 d . . . C39 C 0.20686(18) 0.25366(14) -0.0063(4) 0.0372(9) Uani 1 1 d . . . H39A H 0.2204 0.2713 -0.0789 0.045 Uiso 1 1 calc R . . C40 C 0.20571(17) 0.20418(14) -0.0137(4) 0.0364(9) Uani 1 1 d . . . H40A H 0.2190 0.1888 -0.0905 0.044 Uiso 1 1 calc R . . C41 C 0.18541(17) 0.17803(14) 0.0904(4) 0.0307(8) Uani 1 1 d . . . C42 C 0.16702(17) 0.20094(13) 0.2062(4) 0.0307(8) Uani 1 1 d . . . H42A H 0.1523 0.1831 0.2774 0.037 Uiso 1 1 calc R . . C43 C 0.17053(18) 0.25022(15) 0.2159(4) 0.0373(9) Uani 1 1 d . . . H43A H 0.1610 0.2652 0.2962 0.045 Uiso 1 1 calc R . . C44 C 0.18488(17) 0.12441(14) 0.0823(4) 0.0345(9) Uani 1 1 d . . . C45 C 0.30439(17) 0.33421(14) 0.4159(4) 0.0332(9) Uani 1 1 d . . . C46 C 0.30332(19) 0.28062(14) 0.4051(4) 0.0353(9) Uani 1 1 d . . . C47 C 0.32653(17) 0.25929(14) 0.2946(4) 0.0341(9) Uani 1 1 d . . . H47A H 0.3414 0.2778 0.2250 0.041 Uiso 1 1 calc R . . C48 C 0.32776(17) 0.20976(14) 0.2869(5) 0.0391(10) Uani 1 1 d . . . H48A H 0.3457 0.1951 0.2140 0.047 Uiso 1 1 calc R . . C49 C 0.30346(17) 0.18257(14) 0.3826(4) 0.0350(9) Uani 1 1 d . . . C50 C 0.27945(17) 0.20398(14) 0.4962(4) 0.0334(8) Uani 1 1 d . . . H50A H 0.2630 0.1856 0.5642 0.040 Uiso 1 1 calc R . . C51 C 0.28087(18) 0.25241(14) 0.5044(4) 0.0381(9) Uani 1 1 d . . . H51A H 0.2659 0.2671 0.5808 0.046 Uiso 1 1 calc R . . C52 C 0.30265(17) 0.12850(14) 0.3706(5) 0.0389(9) Uani 1 1 d . . . N1 N 0.40038(14) 0.41012(11) -0.1628(3) 0.0306(7) Uani 1 1 d . . . H1C H 0.3955 0.4392 -0.2004 0.037 Uiso 1 1 calc R . . H1D H 0.3653 0.3953 -0.1647 0.037 Uiso 1 1 calc R . . N2 N 0.40388(13) 0.55071(11) 0.3393(3) 0.0304(7) Uani 1 1 d . . . H2B H 0.3684 0.5647 0.3328 0.037 Uiso 1 1 calc R . . H2C H 0.4028 0.5232 0.2924 0.037 Uiso 1 1 calc R . . N3 N 0.16221(14) 0.56211(12) 0.9684(3) 0.0353(7) Uani 1 1 d . . . H3D H 0.1702 0.5863 0.9116 0.042 Uiso 1 1 calc R . . H3E H 0.1966 0.5523 1.0037 0.042 Uiso 1 1 calc R . . N4 N 0.15997(13) 0.40771(11) 0.4834(3) 0.0316(7) Uani 1 1 d . . . H4A H 0.1957 0.3959 0.4638 0.038 Uiso 1 1 calc R . . H4B H 0.1641 0.4272 0.5546 0.038 Uiso 1 1 calc R . . O1 O 0.30621(11) 0.42689(10) 0.0428(3) 0.0322(6) Uani 1 1 d . . . O2 O 0.38278(11) 0.45507(10) 0.2093(3) 0.0346(6) Uani 1 1 d . . . O3 O 0.36581(11) 0.50262(9) 0.0024(3) 0.0331(6) Uani 1 1 d . . . O4 O 0.37084(12) 0.45132(10) 0.5074(3) 0.0346(6) Uani 1 1 d . . . O5 O 0.30658(11) 0.52433(9) 0.5314(3) 0.0312(6) Uani 1 1 d . . . O6 O 0.38081(12) 0.50111(10) 0.7099(3) 0.0349(6) Uani 1 1 d . . . O7 O 0.18098(11) 0.49106(9) 0.6483(3) 0.0326(6) Uani 1 1 d . . . O8 O 0.19435(13) 0.43881(9) 0.8494(3) 0.0374(6) Uani 1 1 d . . . O9 O 0.25120(11) 0.51679(9) 0.8309(3) 0.0327(6) Uani 1 1 d . . . O10 O 0.18816(12) 0.47088(9) 0.1447(3) 0.0342(6) Uani 1 1 d . . . O11 O 0.19421(13) 0.52182(9) 0.3522(3) 0.0354(6) Uani 1 1 d . . . O12 O 0.25317(11) 0.44582(9) 0.3336(3) 0.0318(6) Uani 1 1 d . . . O13 O 0.18318(12) 0.34912(10) 0.2292(3) 0.0393(7) Uani 1 1 d . . . O14 O 0.20635(12) 0.35259(11) 0.0167(3) 0.0409(7) Uani 1 1 d . . . O15 O 0.15493(13) 0.10142(10) 0.1751(3) 0.0421(7) Uani 1 1 d . . . O16 O 0.21502(12) 0.10355(11) -0.0034(3) 0.0394(7) Uani 1 1 d . . . O17 O 0.27153(12) 0.35482(10) 0.4995(3) 0.0358(6) Uani 1 1 d . . . O18 O 0.33831(12) 0.35587(10) 0.3387(3) 0.0374(6) Uani 1 1 d . . . O19 O 0.28600(13) 0.10376(10) 0.4707(3) 0.0403(7) Uani 1 1 d . . . O20 O 0.32234(12) 0.10978(10) 0.2663(3) 0.0393(7) Uani 1 1 d . . . O1W O 0.29373(12) 0.37147(11) 0.7614(3) 0.0418(7) Uani 1 1 d . . . H1WA H 0.2663 0.3851 0.8048 0.050 Uiso 1 1 d R . . H1WB H 0.2885 0.3758 0.6781 0.050 Uiso 1 1 d R . . O2W O 0.2982(2) 0.5887(2) 0.2728(5) 0.0476(13) Uani 0.60 1 d P . . H2WA H 0.2709 0.5713 0.3047 0.057 Uiso 0.60 1 d PR . . H2WC H 0.2950 0.5898 0.1881 0.057 Uiso 0.60 1 d PR . . O3W O 0.4600(3) 0.2200(2) 0.2709(7) 0.0352(15) Uani 0.40 1 d P . . H3WD H 0.4544 0.2464 0.2305 0.042 Uiso 0.40 1 d PR . . H3WB H 0.4729 0.2252 0.3493 0.042 Uiso 0.40 1 d PR . . P1 P 0.36307(5) 0.45326(4) 0.06467(10) 0.0294(2) Uani 1 1 d . . . P2 P 0.36336(4) 0.50055(4) 0.56341(10) 0.0295(2) Uani 1 1 d . . . P3 P 0.19598(5) 0.48976(4) 0.79841(10) 0.0303(2) Uani 1 1 d . . . P4 P 0.19922(4) 0.47157(3) 0.29414(10) 0.0275(2) Uani 1 1 d . . . Zn1 Zn 0.332983(19) 0.425278(15) 0.35009(5) 0.02927(10) Uani 1 1 d . . . Zn2 Zn 0.222774(19) 0.536323(16) 0.53241(5) 0.02994(10) Uani 1 1 d . . . Zn3 Zn 0.331825(19) 0.533325(16) 0.85030(5) 0.03007(10) Uani 1 1 d . . . Zn4 Zn 0.222551(19) 0.420900(16) 0.03013(5) 0.02970(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0322(19) 0.044(2) 0.032(2) 0.0024(18) -0.0075(18) 0.0121(17) C2 0.051(2) 0.032(2) 0.0261(19) -0.0002(16) -0.0125(18) 0.0138(18) C3 0.045(2) 0.040(2) 0.042(2) -0.0121(19) -0.017(2) 0.0153(18) C4 0.043(2) 0.034(2) 0.032(2) 0.0072(17) -0.0020(17) 0.0062(17) C5 0.037(2) 0.034(2) 0.063(3) -0.004(2) -0.009(2) 0.0107(18) C6 0.040(2) 0.042(2) 0.047(3) -0.004(2) 0.000(2) 0.0147(19) C7 0.051(3) 0.043(3) 0.046(3) -0.018(2) -0.003(2) 0.006(2) C8 0.046(2) 0.047(3) 0.052(3) -0.016(2) -0.001(2) 0.001(2) C9 0.046(2) 0.046(3) 0.049(3) -0.008(2) -0.002(2) -0.002(2) C10 0.0320(18) 0.0279(19) 0.028(2) -0.0011(15) 0.0068(16) 0.0001(15) C11 0.0250(17) 0.046(2) 0.029(2) -0.0090(17) 0.0003(15) -0.0083(16) C12 0.0281(17) 0.038(2) 0.033(2) -0.0072(17) -0.0015(16) -0.0150(16) C13 0.037(2) 0.035(2) 0.031(2) -0.0006(17) -0.0030(17) -0.0130(17) C14 0.042(2) 0.034(2) 0.039(2) 0.0033(18) -0.0164(18) -0.0172(18) C15 0.048(2) 0.041(2) 0.040(2) 0.0041(19) 0.008(2) -0.020(2) C16 0.045(2) 0.050(3) 0.044(3) 0.010(2) -0.006(2) -0.009(2) C17 0.046(2) 0.036(2) 0.040(2) 0.0058(18) -0.006(2) 0.0047(18) C18 0.042(2) 0.039(2) 0.033(2) 0.0000(18) 0.0045(18) -0.0103(18) C19 0.041(2) 0.040(2) 0.030(2) 0.0032(17) 0.0022(18) 0.0137(18) C20 0.043(2) 0.040(2) 0.027(2) 0.0007(17) -0.0021(17) 0.0178(18) C21 0.042(2) 0.038(2) 0.043(2) 0.0075(19) 0.0088(19) 0.0091(18) C22 0.0323(19) 0.041(2) 0.041(2) 0.002(2) 0.0000(18) -0.0030(17) C23 0.038(2) 0.032(2) 0.040(2) 0.0052(17) 0.0057(18) 0.0096(17) C24 0.047(2) 0.046(2) 0.038(2) 0.012(2) 0.008(2) 0.017(2) C25 0.039(2) 0.060(3) 0.055(3) 0.020(2) 0.008(2) 0.014(2) C26 0.043(2) 0.056(3) 0.039(2) 0.021(2) -0.0107(19) -0.020(2) C27 0.044(2) 0.051(3) 0.038(2) 0.017(2) -0.0069(19) -0.015(2) C28 0.0309(18) 0.0228(17) 0.038(2) -0.0031(16) -0.0029(17) 0.0002(15) C29 0.0330(18) 0.038(2) 0.0260(18) -0.0033(16) 0.0013(16) -0.0097(16) C30 0.040(2) 0.034(2) 0.041(2) -0.0031(18) -0.0100(19) 0.0019(17) C31 0.0260(18) 0.0281(19) 0.050(2) -0.0124(18) -0.0104(18) -0.0104(15) C32 0.030(2) 0.048(2) 0.046(2) -0.019(2) -0.0077(18) -0.0189(17) C33 0.038(2) 0.046(3) 0.052(3) -0.012(2) 0.0081(19) -0.0139(19) C34 0.044(2) 0.053(3) 0.049(3) -0.021(2) -0.019(2) -0.007(2) C35 0.037(2) 0.048(2) 0.044(3) -0.014(2) -0.0153(19) 0.0038(19) C36 0.038(2) 0.049(3) 0.043(3) -0.015(2) -0.0113(19) 0.0125(19) C37 0.042(2) 0.0291(19) 0.042(2) 0.0037(17) 0.0104(19) -0.0035(17) C38 0.048(2) 0.038(2) 0.040(2) 0.0009(18) 0.007(2) 0.0009(19) C39 0.049(2) 0.0283(19) 0.034(2) -0.0081(16) -0.0150(18) -0.0017(17) C40 0.043(2) 0.030(2) 0.036(2) 0.0014(16) -0.0020(17) 0.0035(17) C41 0.035(2) 0.0277(19) 0.029(2) -0.0026(16) 0.0059(16) 0.0012(16) C42 0.0277(18) 0.032(2) 0.033(2) -0.0061(16) -0.0008(16) 0.0014(16) C43 0.036(2) 0.034(2) 0.042(2) 0.0084(18) -0.0071(19) 0.0030(17) C44 0.0309(19) 0.0275(19) 0.045(2) -0.0069(18) 0.0033(18) 0.0018(16) C45 0.0325(19) 0.0279(19) 0.039(2) 0.0007(17) 0.0033(18) 0.0037(16) C46 0.045(2) 0.0243(19) 0.036(2) 0.0036(16) -0.0084(19) 0.0109(17) C47 0.0298(19) 0.030(2) 0.043(2) -0.0037(17) -0.0091(17) 0.0028(16) C48 0.031(2) 0.0232(18) 0.064(3) 0.0112(19) -0.011(2) -0.0096(16) C49 0.0315(18) 0.032(2) 0.041(2) -0.0009(17) 0.0027(17) 0.0012(16) C50 0.0324(18) 0.032(2) 0.036(2) -0.0066(16) 0.0016(17) -0.0009(16) C51 0.046(2) 0.030(2) 0.039(2) 0.0061(16) -0.0130(19) -0.0093(18) C52 0.0297(19) 0.033(2) 0.054(3) 0.003(2) -0.0006(19) -0.0035(17) N1 0.0347(16) 0.0222(15) 0.0351(18) 0.0035(14) -0.0067(14) 0.0025(13) N2 0.0235(15) 0.0323(17) 0.0355(18) -0.0042(15) -0.0012(14) -0.0054(13) N3 0.0306(16) 0.0366(18) 0.0386(18) 0.0065(15) 0.0013(15) 0.0123(14) N4 0.0304(15) 0.0258(15) 0.0386(18) -0.0014(14) -0.0090(14) -0.0029(13) O1 0.0315(13) 0.0350(14) 0.0300(14) 0.0021(12) 0.0005(12) 0.0031(11) O2 0.0266(13) 0.0418(16) 0.0355(15) -0.0009(13) -0.0023(12) -0.0072(12) O3 0.0354(14) 0.0295(14) 0.0344(15) 0.0002(12) 0.0021(12) -0.0026(12) O4 0.0448(16) 0.0303(15) 0.0288(14) -0.0012(11) 0.0020(12) 0.0022(12) O5 0.0334(13) 0.0287(13) 0.0316(14) -0.0001(11) -0.0046(12) 0.0031(11) O6 0.0381(14) 0.0330(15) 0.0337(15) 0.0018(12) 0.0028(12) 0.0049(12) O7 0.0333(14) 0.0343(14) 0.0302(14) 0.0006(12) -0.0014(12) 0.0001(11) O8 0.0468(16) 0.0315(14) 0.0338(15) -0.0016(12) -0.0015(14) 0.0066(12) O9 0.0337(14) 0.0309(14) 0.0336(15) 0.0109(12) -0.0012(12) 0.0004(11) O10 0.0403(15) 0.0299(14) 0.0323(14) 0.0039(11) -0.0018(13) 0.0018(11) O11 0.0551(17) 0.0236(13) 0.0274(14) 0.0021(11) 0.0018(14) 0.0090(12) O12 0.0317(13) 0.0293(14) 0.0344(15) 0.0015(12) -0.0047(12) 0.0013(11) O13 0.0458(16) 0.0334(15) 0.0388(16) 0.0035(13) -0.0161(13) -0.0021(13) O14 0.0450(16) 0.0396(16) 0.0382(17) -0.0017(13) 0.0051(14) -0.0111(13) O15 0.0419(16) 0.0348(16) 0.0495(19) -0.0041(14) 0.0011(14) -0.0062(13) O16 0.0397(15) 0.0426(16) 0.0360(16) 0.0004(13) 0.0065(13) 0.0096(13) O17 0.0436(15) 0.0323(15) 0.0316(14) 0.0007(11) 0.0031(13) 0.0032(12) O18 0.0416(15) 0.0306(14) 0.0399(16) 0.0002(13) 0.0021(14) -0.0014(13) O19 0.0428(16) 0.0274(14) 0.0507(18) -0.0019(13) -0.0011(15) -0.0040(12) O20 0.0431(16) 0.0276(14) 0.0471(17) 0.0073(13) -0.0068(14) 0.0009(12) O1W 0.0439(16) 0.0448(17) 0.0368(16) 0.0162(13) 0.0018(13) 0.0113(13) O2W 0.044(3) 0.059(3) 0.041(3) -0.012(3) 0.000(2) -0.008(2) O3W 0.041(4) 0.034(4) 0.030(4) -0.001(3) -0.007(3) 0.005(3) P1 0.0321(5) 0.0280(5) 0.0283(5) 0.0007(4) -0.0017(4) 0.0007(4) P2 0.0316(5) 0.0263(5) 0.0305(5) -0.0020(4) 0.0016(4) 0.0000(4) P3 0.0323(5) 0.0323(5) 0.0262(5) 0.0024(4) -0.0017(4) 0.0018(4) P4 0.0292(5) 0.0240(5) 0.0294(5) -0.0018(4) -0.0020(4) 0.0030(4) Zn1 0.0309(2) 0.0298(2) 0.0272(2) 0.00059(18) -0.0008(2) 0.00124(18) Zn2 0.0274(2) 0.0322(2) 0.0302(2) 0.00036(19) 0.00036(19) 0.00375(18) Zn3 0.0298(2) 0.0325(2) 0.0280(2) 0.00019(18) 0.0021(2) -0.00261(18) Zn4 0.0281(2) 0.0309(2) 0.0302(2) 0.00089(18) -0.0014(2) -0.00251(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.441(4) . ? C1 P1 1.812(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.481(6) . ? C2 C4 1.481(5) . ? C2 N1 1.530(4) . ? C2 H2A 0.9800 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C5 1.389(6) . ? C4 C9 1.392(6) . ? C5 C6 1.380(6) . ? C5 H5A 0.9300 . ? C6 C7 1.383(6) . ? C6 H6A 0.9300 . ? C7 C8 1.400(6) . ? C7 H7A 0.9300 . ? C8 C9 1.375(7) . ? C8 H8A 0.9300 . ? C9 H9A 0.9300 . ? C10 N2 1.489(4) . ? C10 P2 1.815(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C13 1.487(5) . ? C11 N2 1.503(4) . ? C11 C12 1.550(5) . ? C11 H11A 0.9800 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.391(5) . ? C13 C18 1.399(6) . ? C14 C15 1.399(6) . ? C14 H14A 0.9300 . ? C15 C16 1.387(7) . ? C15 H15A 0.9300 . ? C16 C17 1.393(6) . ? C16 H16A 0.9300 . ? C17 C18 1.391(6) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 N3 1.473(4) . ? C19 P3 1.854(4) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C22 1.467(5) . ? C20 C21 1.506(6) . ? C20 N3 1.517(4) . ? C20 H20A 0.9800 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.384(6) . ? C22 C27 1.403(6) . ? C23 C24 1.393(6) . ? C23 H23A 0.9300 . ? C24 C25 1.391(6) . ? C24 H24A 0.9300 . ? C25 C26 1.390(6) . ? C25 H25A 0.9300 . ? C26 C27 1.384(6) . ? C26 H26A 0.9300 . ? C27 H27A 0.9300 . ? C28 N4 1.500(4) . ? C28 P4 1.819(4) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 N4 1.488(4) . ? C29 C31 1.499(5) . ? C29 C30 1.505(6) . ? C29 H29A 0.9800 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C36 1.381(6) . ? C31 C32 1.390(5) . ? C32 C33 1.387(6) . ? C32 H32A 0.9300 . ? C33 C34 1.391(6) . ? C33 H33A 0.9300 . ? C34 C35 1.387(6) . ? C34 H34A 0.9300 . ? C35 C36 1.389(6) . ? C35 H35A 0.9300 . ? C36 H36A 0.9300 . ? C37 O13 1.212(4) . ? C37 O14 1.262(4) . ? C37 C38 1.488(6) . ? C38 C43 1.370(4) . ? C38 C39 1.394(6) . ? C39 C40 1.383(5) . ? C39 H39A 0.9300 . ? C40 C41 1.351(4) . ? C40 H40A 0.9300 . ? C41 C42 1.387(5) . ? C41 C44 1.498(5) . ? C42 C43 1.381(5) . ? C42 H42A 0.9300 . ? C43 H43A 0.9300 . ? C44 O16 1.242(5) . ? C44 O15 1.317(5) . ? C45 O18 1.248(5) . ? C45 O17 1.260(5) . ? C45 C46 1.499(5) . ? C46 C47 1.361(6) . ? C46 C51 1.366(6) . ? C47 C48 1.385(6) . ? C47 H47A 0.9300 . ? C48 C49 1.340(6) . ? C48 H48A 0.9300 . ? C49 C50 1.395(6) . ? C49 C52 1.514(5) . ? C50 C51 1.354(6) . ? C50 H50A 0.9300 . ? C51 H51A 0.9300 . ? C52 O20 1.249(5) . ? C52 O19 1.273(5) . ? N1 H1C 0.9000 . ? N1 H1D 0.9000 . ? N2 H2B 0.9000 . ? N2 H2C 0.9000 . ? N3 H3D 0.9000 . ? N3 H3E 0.9000 . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? O1 P1 1.505(3) . ? O1 Zn4 1.917(3) . ? O2 P1 1.514(3) . ? O2 Zn1 1.989(3) . ? O3 P1 1.512(3) . ? O3 Zn3 1.908(3) 1_554 ? O4 P2 1.493(3) . ? O4 Zn1 1.934(3) . ? O5 P2 1.488(3) . ? O5 Zn2 1.938(3) . ? O6 P2 1.517(3) . ? O6 Zn3 2.005(3) . ? O7 P3 1.538(3) . ? O7 Zn2 1.960(3) . ? O8 P3 1.511(3) . ? O8 Zn4 1.980(3) 1_556 ? O9 P3 1.502(3) . ? O9 Zn3 1.903(3) . ? O10 P4 1.515(3) . ? O10 Zn4 1.967(3) . ? O11 P4 1.522(3) . ? O11 Zn2 1.957(3) . ? O12 P4 1.477(3) . ? O12 Zn1 1.913(3) . ? O14 Zn4 1.946(3) . ? O15 Zn3 1.940(3) 4_546 ? O18 Zn1 1.944(3) . ? O19 Zn2 1.892(3) 4_546 ? O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? O2W H2WA 0.8500 . ? O2W H2WC 0.8500 . ? O3W H3WD 0.8500 . ? O3W H3WB 0.8500 . ? Zn2 O19 1.892(3) 4_556 ? Zn3 O3 1.908(3) 1_556 ? Zn3 O15 1.940(3) 4_556 ? Zn4 O8 1.980(3) 1_554 ? 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 C1 P1 112.2(2) . . ? N1 C1 H1A 109.2 . . ? P1 C1 H1A 109.2 . . ? N1 C1 H1B 109.2 . . ? P1 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? C3 C2 C4 115.1(4) . . ? C3 C2 N1 108.6(3) . . ? C4 C2 N1 109.6(3) . . ? C3 C2 H2A 107.8 . . ? C4 C2 H2A 107.8 . . ? N1 C2 H2A 107.8 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C9 118.9(4) . . ? C5 C4 C2 122.5(4) . . ? C9 C4 C2 118.5(4) . . ? C6 C5 C4 120.4(4) . . ? C6 C5 H5A 119.8 . . ? C4 C5 H5A 119.8 . . ? C5 C6 C7 120.6(4) . . ? C5 C6 H6A 119.7 . . ? C7 C6 H6A 119.7 . . ? C6 C7 C8 119.4(4) . . ? C6 C7 H7A 120.3 . . ? C8 C7 H7A 120.3 . . ? C9 C8 C7 119.7(4) . . ? C9 C8 H8A 120.1 . . ? C7 C8 H8A 120.1 . . ? C8 C9 C4 121.0(4) . . ? C8 C9 H9A 119.5 . . ? C4 C9 H9A 119.5 . . ? N2 C10 P2 115.3(2) . . ? N2 C10 H10A 108.4 . . ? P2 C10 H10A 108.4 . . ? N2 C10 H10B 108.4 . . ? P2 C10 H10B 108.4 . . ? H10A C10 H10B 107.5 . . ? C13 C11 N2 113.3(3) . . ? C13 C11 C12 110.2(3) . . ? N2 C11 C12 108.1(3) . . ? C13 C11 H11A 108.4 . . ? N2 C11 H11A 108.4 . . ? C12 C11 H11A 108.4 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 119.6(4) . . ? C14 C13 C11 117.5(4) . . ? C18 C13 C11 122.8(3) . . ? C13 C14 C15 120.1(4) . . ? C13 C14 H14A 120.0 . . ? C15 C14 H14A 120.0 . . ? C16 C15 C14 120.2(4) . . ? C16 C15 H15A 119.9 . . ? C14 C15 H15A 119.9 . . ? C15 C16 C17 119.7(4) . . ? C15 C16 H16A 120.1 . . ? C17 C16 H16A 120.1 . . ? C18 C17 C16 120.3(4) . . ? C18 C17 H17A 119.8 . . ? C16 C17 H17A 119.8 . . ? C17 C18 C13 120.1(4) . . ? C17 C18 H18A 120.0 . . ? C13 C18 H18A 120.0 . . ? N3 C19 P3 110.8(3) . . ? N3 C19 H19A 109.5 . . ? P3 C19 H19A 109.5 . . ? N3 C19 H19B 109.5 . . ? P3 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? C22 C20 C21 112.7(3) . . ? C22 C20 N3 110.7(3) . . ? C21 C20 N3 106.9(3) . . ? C22 C20 H20A 108.8 . . ? C21 C20 H20A 108.8 . . ? N3 C20 H20A 108.8 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C27 119.9(4) . . ? C23 C22 C20 122.2(4) . . ? C27 C22 C20 117.7(4) . . ? C22 C23 C24 120.3(4) . . ? C22 C23 H23A 119.9 . . ? C24 C23 H23A 119.9 . . ? C25 C24 C23 120.0(4) . . ? C25 C24 H24A 120.0 . . ? C23 C24 H24A 120.0 . . ? C26 C25 C24 119.6(4) . . ? C26 C25 H25A 120.2 . . ? C24 C25 H25A 120.2 . . ? C27 C26 C25 120.8(4) . . ? C27 C26 H26A 119.6 . . ? C25 C26 H26A 119.6 . . ? C26 C27 C22 119.5(4) . . ? C26 C27 H27A 120.3 . . ? C22 C27 H27A 120.3 . . ? N4 C28 P4 111.4(2) . . ? N4 C28 H28A 109.4 . . ? P4 C28 H28A 109.4 . . ? N4 C28 H28B 109.4 . . ? P4 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? N4 C29 C31 109.9(3) . . ? N4 C29 C30 111.7(3) . . ? C31 C29 C30 111.6(3) . . ? N4 C29 H29A 107.8 . . ? C31 C29 H29A 107.8 . . ? C30 C29 H29A 107.8 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C36 C31 C32 119.9(4) . . ? C36 C31 C29 120.9(3) . . ? C32 C31 C29 119.2(4) . . ? C33 C32 C31 120.1(4) . . ? C33 C32 H32A 119.9 . . ? C31 C32 H32A 119.9 . . ? C32 C33 C34 119.9(4) . . ? C32 C33 H33A 120.1 . . ? C34 C33 H33A 120.1 . . ? C35 C34 C33 119.9(4) . . ? C35 C34 H34A 120.1 . . ? C33 C34 H34A 120.1 . . ? C34 C35 C36 120.0(4) . . ? C34 C35 H35A 120.0 . . ? C36 C35 H35A 120.0 . . ? C31 C36 C35 120.2(4) . . ? C31 C36 H36A 119.9 . . ? C35 C36 H36A 119.9 . . ? O13 C37 O14 124.5(3) . . ? O13 C37 C38 119.8(3) . . ? O14 C37 C38 115.6(3) . . ? C43 C38 C39 118.2(4) . . ? C43 C38 C37 119.9(4) . . ? C39 C38 C37 121.6(4) . . ? C40 C39 C38 120.7(4) . . ? C40 C39 H39A 119.6 . . ? C38 C39 H39A 119.6 . . ? C41 C40 C39 120.3(4) . . ? C41 C40 H40A 119.8 . . ? C39 C40 H40A 119.8 . . ? C40 C41 C42 119.8(3) . . ? C40 C41 C44 120.0(3) . . ? C42 C41 C44 120.2(4) . . ? C43 C42 C41 120.0(4) . . ? C43 C42 H42A 120.0 . . ? C41 C42 H42A 120.0 . . ? C38 C43 C42 120.8(4) . . ? C38 C43 H43A 119.6 . . ? C42 C43 H43A 119.6 . . ? O16 C44 O15 122.9(4) . . ? O16 C44 C41 120.0(4) . . ? O15 C44 C41 116.9(3) . . ? O18 C45 O17 123.8(4) . . ? O18 C45 C46 116.6(4) . . ? O17 C45 C46 119.5(4) . . ? C47 C46 C51 118.9(4) . . ? C47 C46 C45 119.2(4) . . ? C51 C46 C45 121.9(4) . . ? C46 C47 C48 119.3(4) . . ? C46 C47 H47A 120.3 . . ? C48 C47 H47A 120.3 . . ? C49 C48 C47 121.1(5) . . ? C49 C48 H48A 119.4 . . ? C47 C48 H48A 119.4 . . ? C48 C49 C50 120.0(4) . . ? C48 C49 C52 120.9(4) . . ? C50 C49 C52 119.1(4) . . ? C51 C50 C49 117.9(4) . . ? C51 C50 H50A 121.1 . . ? C49 C50 H50A 121.1 . . ? C50 C51 C46 122.7(4) . . ? C50 C51 H51A 118.7 . . ? C46 C51 H51A 118.7 . . ? O20 C52 O19 122.4(4) . . ? O20 C52 C49 118.6(4) . . ? O19 C52 C49 118.8(4) . . ? C1 N1 C2 117.5(2) . . ? C1 N1 H1C 107.9 . . ? C2 N1 H1C 107.9 . . ? C1 N1 H1D 107.9 . . ? C2 N1 H1D 107.9 . . ? H1C N1 H1D 107.2 . . ? C10 N2 C11 112.0(2) . . ? C10 N2 H2B 109.2 . . ? C11 N2 H2B 109.2 . . ? C10 N2 H2C 109.2 . . ? C11 N2 H2C 109.2 . . ? H2B N2 H2C 107.9 . . ? C19 N3 C20 116.8(2) . . ? C19 N3 H3D 108.1 . . ? C20 N3 H3D 108.1 . . ? C19 N3 H3E 108.1 . . ? C20 N3 H3E 108.1 . . ? H3D N3 H3E 107.3 . . ? C29 N4 C28 115.6(2) . . ? C29 N4 H4A 108.4 . . ? C28 N4 H4A 108.4 . . ? C29 N4 H4B 108.4 . . ? C28 N4 H4B 108.4 . . ? H4A N4 H4B 107.4 . . ? P1 O1 Zn4 155.13(18) . . ? P1 O2 Zn1 119.48(15) . . ? P1 O3 Zn3 136.02(17) . 1_554 ? P2 O4 Zn1 126.83(17) . . ? P2 O5 Zn2 158.72(18) . . ? P2 O6 Zn3 122.27(17) . . ? P3 O7 Zn2 118.90(16) . . ? P3 O8 Zn4 122.49(17) . 1_556 ? P3 O9 Zn3 162.11(19) . . ? P4 O10 Zn4 121.10(16) . . ? P4 O11 Zn2 121.11(16) . . ? P4 O12 Zn1 163.60(19) . . ? C37 O14 Zn4 118.30(19) . . ? C44 O15 Zn3 107.7(2) . 4_546 ? C45 O18 Zn1 114.0(3) . . ? C52 O19 Zn2 123.9(3) . 4_546 ? H1WA O1W H1WB 109.5 . . ? H2WA O2W H2WC 109.5 . . ? H3WD O3W H3WB 109.8 . . ? O1 P1 O3 114.89(15) . . ? O1 P1 O2 114.20(15) . . ? O3 P1 O2 110.49(16) . . ? O1 P1 C1 103.50(14) . . ? O3 P1 C1 105.96(14) . . ? O2 P1 C1 106.86(12) . . ? O5 P2 O4 115.38(16) . . ? O5 P2 O6 115.49(16) . . ? O4 P2 O6 109.97(16) . . ? O5 P2 C10 102.24(12) . . ? O4 P2 C10 108.09(12) . . ? O6 P2 C10 104.52(12) . . ? O9 P3 O8 114.85(16) . . ? O9 P3 O7 112.62(16) . . ? O8 P3 O7 110.22(16) . . ? O9 P3 C19 104.50(14) . . ? O8 P3 C19 105.87(13) . . ? O7 P3 C19 108.18(13) . . ? O12 P4 O10 113.28(17) . . ? O12 P4 O11 114.14(17) . . ? O10 P4 O11 112.04(15) . . ? O12 P4 C28 105.07(12) . . ? O10 P4 C28 105.23(13) . . ? O11 P4 C28 106.12(12) . . ? O12 Zn1 O4 112.41(12) . . ? O12 Zn1 O18 110.66(12) . . ? O4 Zn1 O18 113.21(12) . . ? O12 Zn1 O2 110.82(11) . . ? O4 Zn1 O2 99.41(11) . . ? O18 Zn1 O2 109.84(12) . . ? O19 Zn2 O5 106.00(12) 4_556 . ? O19 Zn2 O11 98.94(12) 4_556 . ? O5 Zn2 O11 106.69(12) . . ? O19 Zn2 O7 126.80(13) 4_556 . ? O5 Zn2 O7 111.71(11) . . ? O11 Zn2 O7 104.42(12) . . ? O9 Zn3 O3 111.32(11) . 1_556 ? O9 Zn3 O15 111.96(12) . 4_556 ? O3 Zn3 O15 118.72(12) 1_556 4_556 ? O9 Zn3 O6 110.90(12) . . ? O3 Zn3 O6 97.48(11) 1_556 . ? O15 Zn3 O6 105.13(12) 4_556 . ? O1 Zn4 O14 106.16(12) . . ? O1 Zn4 O10 107.20(12) . . ? O14 Zn4 O10 131.22(12) . . ? O1 Zn4 O8 111.13(12) . 1_554 ? O14 Zn4 O8 97.06(12) . 1_554 ? O10 Zn4 O8 102.85(11) . 1_554 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 C2 C4 C5 10.6(6) . . . . ? N1 C2 C4 C5 -112.2(4) . . . . ? C3 C2 C4 C9 -166.2(4) . . . . ? N1 C2 C4 C9 71.0(5) . . . . ? C9 C4 C5 C6 1.3(7) . . . . ? C2 C4 C5 C6 -175.5(4) . . . . ? C4 C5 C6 C7 -1.8(7) . . . . ? C5 C6 C7 C8 1.7(7) . . . . ? C6 C7 C8 C9 -1.3(7) . . . . ? C7 C8 C9 C4 0.9(7) . . . . ? C5 C4 C9 C8 -0.9(7) . . . . ? C2 C4 C9 C8 176.0(4) . . . . ? N2 C11 C13 C14 137.1(3) . . . . ? C12 C11 C13 C14 -101.6(4) . . . . ? N2 C11 C13 C18 -45.7(5) . . . . ? C12 C11 C13 C18 75.6(5) . . . . ? C18 C13 C14 C15 -1.4(6) . . . . ? C11 C13 C14 C15 175.9(4) . . . . ? C13 C14 C15 C16 1.6(6) . . . . ? C14 C15 C16 C17 -1.5(7) . . . . ? C15 C16 C17 C18 1.2(6) . . . . ? C16 C17 C18 C13 -1.0(6) . . . . ? C14 C13 C18 C17 1.1(6) . . . . ? C11 C13 C18 C17 -176.0(4) . . . . ? C21 C20 C22 C23 60.1(5) . . . . ? N3 C20 C22 C23 -59.6(5) . . . . ? C21 C20 C22 C27 -114.1(5) . . . . ? N3 C20 C22 C27 126.2(4) . . . . ? C27 C22 C23 C24 0.1(7) . . . . ? C20 C22 C23 C24 -174.0(4) . . . . ? C22 C23 C24 C25 -0.3(7) . . . . ? C23 C24 C25 C26 0.2(8) . . . . ? C24 C25 C26 C27 0.2(8) . . . . ? C25 C26 C27 C22 -0.4(8) . . . . ? C23 C22 C27 C26 0.2(7) . . . . ? C20 C22 C27 C26 174.6(4) . . . . ? N4 C29 C31 C36 -56.3(5) . . . . ? C30 C29 C31 C36 68.1(5) . . . . ? N4 C29 C31 C32 122.1(4) . . . . ? C30 C29 C31 C32 -113.5(4) . . . . ? C36 C31 C32 C33 0.3(7) . . . . ? C29 C31 C32 C33 -178.1(4) . . . . ? C31 C32 C33 C34 0.4(7) . . . . ? C32 C33 C34 C35 -0.4(8) . . . . ? C33 C34 C35 C36 -0.2(8) . . . . ? C32 C31 C36 C35 -0.9(7) . . . . ? C29 C31 C36 C35 177.5(4) . . . . ? C34 C35 C36 C31 0.8(8) . . . . ? O13 C37 C38 C43 4.8(6) . . . . ? O14 C37 C38 C43 -177.9(3) . . . . ? O13 C37 C38 C39 -169.1(4) . . . . ? O14 C37 C38 C39 8.2(6) . . . . ? C43 C38 C39 C40 2.7(6) . . . . ? C37 C38 C39 C40 176.7(4) . . . . ? C38 C39 C40 C41 0.9(6) . . . . ? C39 C40 C41 C42 -1.6(4) . . . . ? C39 C40 C41 C44 -179.4(3) . . . . ? C40 C41 C42 C43 -1.2(6) . . . . ? C44 C41 C42 C43 176.5(4) . . . . ? C39 C38 C43 C42 -5.5(5) . . . . ? C37 C38 C43 C42 -179.6(3) . . . . ? C41 C42 C43 C38 4.9(6) . . . . ? C40 C41 C44 O16 17.0(6) . . . . ? C42 C41 C44 O16 -160.7(4) . . . . ? C40 C41 C44 O15 -167.8(3) . . . . ? C42 C41 C44 O15 14.5(6) . . . . ? O18 C45 C46 C47 -16.2(6) . . . . ? O17 C45 C46 C47 163.2(4) . . . . ? O18 C45 C46 C51 162.3(4) . . . . ? O17 C45 C46 C51 -18.3(6) . . . . ? C51 C46 C47 C48 -1.2(6) . . . . ? C45 C46 C47 C48 177.4(4) . . . . ? C46 C47 C48 C49 3.9(6) . . . . ? C47 C48 C49 C50 -3.8(6) . . . . ? C47 C48 C49 C52 177.3(4) . . . . ? C48 C49 C50 C51 1.0(6) . . . . ? C52 C49 C50 C51 179.9(4) . . . . ? C49 C50 C51 C46 1.7(6) . . . . ? C47 C46 C51 C50 -1.6(6) . . . . ? C45 C46 C51 C50 179.9(4) . . . . ? C48 C49 C52 O20 -3.7(6) . . . . ? C50 C49 C52 O20 177.4(4) . . . . ? C48 C49 C52 O19 171.2(4) . . . . ? C50 C49 C52 O19 -7.6(6) . . . . ? P1 C1 N1 C2 178.2(2) . . . . ? C3 C2 N1 C1 -67.0(4) . . . . ? C4 C2 N1 C1 59.5(4) . . . . ? P2 C10 N2 C11 180.0(2) . . . . ? C13 C11 N2 C10 -56.7(4) . . . . ? C12 C11 N2 C10 -179.2(3) . . . . ? P3 C19 N3 C20 -161.2(2) . . . . ? C22 C20 N3 C19 -49.5(4) . . . . ? C21 C20 N3 C19 -172.6(3) . . . . ? C31 C29 N4 C28 -47.0(4) . . . . ? C30 C29 N4 C28 -171.5(3) . . . . ? P4 C28 N4 C29 -160.9(2) . . . . ? O13 C37 O14 Zn4 5.2(5) . . . . ? C38 C37 O14 Zn4 -172.0(3) . . . . ? O16 C44 O15 Zn3 0.4(5) . . . 4_546 ? C41 C44 O15 Zn3 -174.7(3) . . . 4_546 ? O17 C45 O18 Zn1 -3.6(5) . . . . ? C46 C45 O18 Zn1 175.8(3) . . . . ? O20 C52 O19 Zn2 -10.0(6) . . . 4_546 ? C49 C52 O19 Zn2 175.3(3) . . . 4_546 ? Zn4 O1 P1 O3 -40.9(5) . . . . ? Zn4 O1 P1 O2 88.3(4) . . . . ? Zn4 O1 P1 C1 -155.9(4) . . . . ? Zn3 O3 P1 O1 -29.6(3) 1_554 . . . ? Zn3 O3 P1 O2 -160.6(2) 1_554 . . . ? Zn3 O3 P1 C1 84.0(2) 1_554 . . . ? Zn1 O2 P1 O1 -1.5(2) . . . . ? Zn1 O2 P1 O3 129.88(18) . . . . ? Zn1 O2 P1 C1 -115.28(15) . . . . ? N1 C1 P1 O1 55.3(3) . . . . ? N1 C1 P1 O3 -65.9(3) . . . . ? N1 C1 P1 O2 176.2(2) . . . . ? Zn2 O5 P2 O4 67.3(5) . . . . ? Zn2 O5 P2 O6 -62.8(5) . . . . ? Zn2 O5 P2 C10 -175.6(5) . . . . ? Zn1 O4 P2 O5 25.7(3) . . . . ? Zn1 O4 P2 O6 158.51(19) . . . . ? Zn1 O4 P2 C10 -87.96(19) . . . . ? Zn3 O6 P2 O5 -1.7(3) . . . . ? Zn3 O6 P2 O4 -134.39(19) . . . . ? Zn3 O6 P2 C10 109.80(17) . . . . ? N2 C10 P2 O5 -51.3(2) . . . . ? N2 C10 P2 O4 70.9(2) . . . . ? N2 C10 P2 O6 -172.01(18) . . . . ? Zn3 O9 P3 O8 49.1(7) . . . . ? Zn3 O9 P3 O7 -78.2(6) . . . . ? Zn3 O9 P3 C19 164.6(6) . . . . ? Zn4 O8 P3 O9 42.2(3) 1_556 . . . ? Zn4 O8 P3 O7 170.64(17) 1_556 . . . ? Zn4 O8 P3 C19 -72.59(19) 1_556 . . . ? Zn2 O7 P3 O9 -12.7(2) . . . . ? Zn2 O7 P3 O8 -142.37(17) . . . . ? Zn2 O7 P3 C19 102.31(15) . . . . ? N3 C19 P3 O9 -1.9(2) . . . . ? N3 C19 P3 O8 119.7(2) . . . . ? N3 C19 P3 O7 -122.1(2) . . . . ? Zn1 O12 P4 O10 57.4(7) . . . . ? Zn1 O12 P4 O11 -72.4(7) . . . . ? Zn1 O12 P4 C28 171.7(6) . . . . ? Zn4 O10 P4 O12 22.8(2) . . . . ? Zn4 O10 P4 O11 153.66(17) . . . . ? Zn4 O10 P4 C28 -91.46(17) . . . . ? Zn2 O11 P4 O12 -35.9(3) . . . . ? Zn2 O11 P4 O10 -166.37(17) . . . . ? Zn2 O11 P4 C28 79.29(19) . . . . ? N4 C28 P4 O12 22.8(2) . . . . ? N4 C28 P4 O10 142.67(18) . . . . ? N4 C28 P4 O11 -98.4(2) . . . . ? P4 O12 Zn1 O4 98.6(7) . . . . ? P4 O12 Zn1 O18 -133.7(7) . . . . ? P4 O12 Zn1 O2 -11.6(7) . . . . ? P2 O4 Zn1 O12 -38.4(2) . . . . ? P2 O4 Zn1 O18 -164.67(19) . . . . ? P2 O4 Zn1 O2 78.9(2) . . . . ? C45 O18 Zn1 O12 -51.4(3) . . . . ? C45 O18 Zn1 O4 75.8(3) . . . . ? C45 O18 Zn1 O2 -174.0(3) . . . . ? P1 O2 Zn1 O12 -49.4(2) . . . . ? P1 O2 Zn1 O4 -167.90(19) . . . . ? P1 O2 Zn1 O18 73.1(2) . . . . ? P2 O5 Zn2 O19 143.9(5) . . . 4_556 ? P2 O5 Zn2 O11 -111.4(5) . . . . ? P2 O5 Zn2 O7 2.1(5) . . . . ? P4 O11 Zn2 O19 171.9(2) . . . 4_556 ? P4 O11 Zn2 O5 62.1(2) . . . . ? P4 O11 Zn2 O7 -56.3(2) . . . . ? P3 O7 Zn2 O19 -71.1(2) . . . 4_556 ? P3 O7 Zn2 O5 60.8(2) . . . . ? P3 O7 Zn2 O11 175.74(16) . . . . ? P3 O9 Zn3 O3 -77.9(6) . . . 1_556 ? P3 O9 Zn3 O15 146.6(6) . . . 4_556 ? P3 O9 Zn3 O6 29.5(6) . . . . ? P2 O6 Zn3 O9 46.5(2) . . . . ? P2 O6 Zn3 O3 162.7(2) . . . 1_556 ? P2 O6 Zn3 O15 -74.7(2) . . . 4_556 ? P1 O1 Zn4 O14 -171.3(4) . . . . ? P1 O1 Zn4 O10 -27.4(5) . . . . ? P1 O1 Zn4 O8 84.3(4) . . . 1_554 ? C37 O14 Zn4 O1 98.0(2) . . . . ? C37 O14 Zn4 O10 -33.5(3) . . . . ? C37 O14 Zn4 O8 -147.5(2) . . . 1_554 ? P4 O10 Zn4 O1 -62.0(2) . . . . ? P4 O10 Zn4 O14 69.2(2) . . . . ? P4 O10 Zn4 O8 -179.23(18) . . . 1_554 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.317 _refine_diff_density_min -0.541 _refine_diff_density_rms 0.065 # Attachment 'Zn_S-2.cif' data_70314cm _database_code_depnum_ccdc_archive 'CCDC 741079' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H32 N2 O16 P2 Zn3, H2 O' _chemical_formula_sum 'C28 H34 N2 O17 P2 Zn3' _chemical_formula_weight 928.62 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' 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 'C2 ' _symmetry_space_group_name_Hall 'C 2y ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 31.147(4) _cell_length_b 7.6286(8) _cell_length_c 17.6399(19) _cell_angle_alpha 90.00 _cell_angle_beta 124.4960(10) _cell_angle_gamma 90.00 _cell_volume 3454.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 1892 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 23.29 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.786 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 2.239 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.539 _exptl_absorpt_correction_T_max 0.637 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9406 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6394 _reflns_number_gt 5465 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.07P)^2^+1.99P] 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 0.031(15) _chemical_absolute_configuration unk _refine_ls_number_reflns 6394 _refine_ls_number_parameters 447 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0605 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1212 _refine_ls_wR_factor_gt 0.1191 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7355(3) 0.6061(9) 0.3136(4) 0.0376(15) Uani 1 1 d . . . H1A H 0.7014 0.6604 0.2779 0.045 Uiso 1 1 calc R . . H1B H 0.7381 0.5403 0.3630 0.045 Uiso 1 1 calc R . . C2 C 0.7821(3) 0.8387(9) 0.4338(4) 0.0378(14) Uani 1 1 d . . . H2A H 0.7947 0.7556 0.4829 0.045 Uiso 1 1 d R . . C3 C 0.8240(3) 0.9791(10) 0.4649(5) 0.0444(17) Uani 1 1 d . . . H3A H 0.8292 1.0405 0.5170 0.067 Uiso 1 1 calc R . . H3B H 0.8130 1.0604 0.4156 0.067 Uiso 1 1 calc R . . H3C H 0.8560 0.9246 0.4817 0.067 Uiso 1 1 calc R . . C4 C 0.73093(14) 0.9084(5) 0.4107(3) 0.0325(13) Uani 1 1 d G . . C5 C 0.70184(18) 1.0230(6) 0.3373(3) 0.0512(19) Uani 1 1 d G . . H5 H 0.7135 1.0542 0.3009 0.061 Uiso 1 1 calc R . . C6 C 0.65531(17) 1.0910(6) 0.3183(3) 0.0489(18) Uani 1 1 d G . . H6 H 0.6359 1.1677 0.2692 0.059 Uiso 1 1 calc R . . C7 C 0.63787(14) 1.0444(6) 0.3727(3) 0.0463(18) Uani 1 1 d G . . H7 H 0.6067 1.0899 0.3600 0.056 Uiso 1 1 calc R . . C8 C 0.66695(16) 0.9298(7) 0.4461(3) 0.0424(16) Uani 1 1 d G . . H8 H 0.6553 0.8986 0.4824 0.051 Uiso 1 1 calc R . . C9 C 0.71348(16) 0.8618(6) 0.4650(3) 0.0467(16) Uani 1 1 d G . . H9 H 0.7329 0.7851 0.5141 0.056 Uiso 1 1 calc R . . C10 C 0.8907(2) 0.8728(10) 0.1551(4) 0.0364(14) Uani 1 1 d . . . H10A H 0.9075 0.9404 0.1323 0.044 Uiso 1 1 calc R . . H10B H 0.8936 0.9383 0.2049 0.044 Uiso 1 1 calc R . . C11 C 0.9737(2) 0.7155(8) 0.2751(4) 0.0320(14) Uani 1 1 d . . . H11A H 0.9730 0.7642 0.3246 0.038 Uiso 1 1 d R . . C12 C 0.9941(3) 0.5310(9) 0.3023(5) 0.0465(17) Uani 1 1 d . . . H12A H 1.0292 0.5338 0.3562 0.070 Uiso 1 1 calc R . . H12B H 0.9936 0.4759 0.2529 0.070 Uiso 1 1 calc R . . H12C H 0.9726 0.4659 0.3152 0.070 Uiso 1 1 calc R . . C13 C 1.00675(14) 0.8330(5) 0.2595(3) 0.0312(13) Uani 1 1 d G . . C14 C 1.02418(18) 0.9895(6) 0.3083(3) 0.0471(18) Uani 1 1 d G . . H14 H 1.0142 1.0207 0.3472 0.056 Uiso 1 1 calc R . . C15 C 1.05657(19) 1.0993(5) 0.2991(3) 0.060(2) Uani 1 1 d G . . H15 H 1.0682 1.2040 0.3317 0.072 Uiso 1 1 calc R . . C16 C 1.07153(17) 1.0526(6) 0.2411(4) 0.055(2) Uani 1 1 d G . . H16 H 1.0932 1.1261 0.2349 0.066 Uiso 1 1 calc R . . C17 C 1.05410(17) 0.8961(7) 0.1923(3) 0.0446(17) Uani 1 1 d G . . H17 H 1.0641 0.8648 0.1535 0.054 Uiso 1 1 calc R . . C18 C 1.02171(16) 0.7862(5) 0.2015(3) 0.0380(14) Uani 1 1 d G . . H18 H 1.0101 0.6815 0.1689 0.046 Uiso 1 1 calc R . . C19 C 0.9050(3) 0.0573(9) 0.3769(4) 0.0386(15) Uani 1 1 d . . . C20 C 0.9534(2) -0.0434(9) 0.4435(4) 0.0325(13) Uani 1 1 d . . . C21 C 0.9529(2) -0.2243(9) 0.4452(4) 0.0321(12) Uani 1 1 d . . . C22 C 0.9048(2) -0.3363(10) 0.3944(4) 0.0377(14) Uani 1 1 d . . . C23 C 1.0000 -0.3194(13) 0.5000 0.0337(18) Uani 1 2 d S . . H23A H 1.0000 -0.4413 0.5000 0.040 Uiso 1 2 calc SR . . C24 C 1.0000 0.0420(13) 0.5000 0.037(2) Uani 1 2 d S . . H24A H 1.0000 0.1639 0.5000 0.044 Uiso 1 2 calc SR . . C25 C 0.9144(3) 1.0974(9) -0.0189(4) 0.0352(14) Uani 1 1 d . . . C26 C 0.9590(2) 1.2009(8) -0.0076(4) 0.0332(13) Uani 1 1 d . . . C27 C 0.9596(2) 1.3813(9) -0.0058(4) 0.0359(14) Uani 1 1 d . . . C28 C 0.9192(3) 1.4931(9) -0.0071(5) 0.0375(15) Uani 1 1 d . . . C29 C 1.0000 1.4690(12) 0.0000 0.0304(18) Uani 1 2 d S . . H29A H 1.0000 1.5909 0.0000 0.037 Uiso 1 2 calc SR . . C30 C 1.0000 1.1162(13) 0.0000 0.038(2) Uani 1 2 d S . . H30A H 1.0000 0.9943 0.0000 0.046 Uiso 1 2 calc SR . . N1 N 0.7757(2) 0.7439(7) 0.3534(4) 0.0348(12) Uani 1 1 d . . . H1C H 0.7676 0.8227 0.3092 0.042 Uiso 1 1 calc R . . H1D H 0.8064 0.6952 0.3714 0.042 Uiso 1 1 calc R . . N2 N 0.91782(19) 0.7045(7) 0.1906(3) 0.0327(12) Uani 1 1 d . . . H2B H 0.9180 0.6501 0.1455 0.039 Uiso 1 1 calc R . . H2C H 0.8994 0.6371 0.2045 0.039 Uiso 1 1 calc R . . O1 O 0.74607(18) 0.5711(7) 0.1764(3) 0.0433(11) Uani 1 1 d . . . O2 O 0.79246(16) 0.3578(6) 0.3038(3) 0.0394(10) Uani 1 1 d . . . O3 O 0.69558(16) 0.3388(6) 0.2002(3) 0.0362(10) Uani 1 1 d . . . O4 O 0.80184(17) 0.7269(6) 0.1033(3) 0.0401(11) Uani 1 1 d . . . O5 O 0.82008(16) 0.7578(6) -0.0161(3) 0.0367(10) Uani 1 1 d . . . O6 O 0.79988(17) 1.0282(6) 0.0437(3) 0.0412(11) Uani 1 1 d . . . O7 O 0.90740(17) 0.2202(6) 0.3900(3) 0.0430(12) Uani 1 1 d . . . O8 O 0.86715(18) -0.0209(7) 0.3142(3) 0.0474(13) Uani 1 1 d . . . O9 O 0.87977(18) -0.3562(7) 0.4291(3) 0.0466(12) Uani 1 1 d . . . O10 O 0.89433(18) -0.4175(6) 0.3221(3) 0.0413(11) Uani 1 1 d . . . O11 O 0.91825(18) 0.9308(6) -0.0206(3) 0.0417(11) Uani 1 1 d . . . O12 O 0.87730(17) 1.1685(7) -0.0265(3) 0.0413(10) Uani 1 1 d . . . O13 O 0.9234(2) 1.5135(7) 0.0673(4) 0.0512(13) Uani 1 1 d . . . O14 O 0.88629(17) 1.5655(6) -0.0823(3) 0.0371(10) Uani 1 1 d . . . O1W O 0.68599(17) 0.8823(7) 0.0083(3) 0.0421(11) Uani 1 1 d . . . H1WA H 0.6536 0.8649 0.0022 0.063 Uiso 1 1 d R . . H1WB H 0.7034 0.9831 0.0461 0.063 Uiso 1 1 d R . . O2W O 0.83297(17) 0.3231(6) 0.1720(3) 0.0415(12) Uani 1 1 d . . . H2WA H 0.8219 0.4291 0.1364 0.062 Uiso 1 1 d R . . H2WB H 0.8052 0.2390 0.1430 0.062 Uiso 1 1 d R . . O3W O 0.76014(18) -0.0178(7) 0.2151(4) 0.0468(12) Uani 1 1 d . . . H3WA H 0.7325 0.0408 0.1955 0.070 Uiso 1 1 d R . . H3WB H 0.7859 0.0517 0.2377 0.070 Uiso 1 1 d R . . P1 P 0.74190(6) 0.4570(2) 0.24070(11) 0.0306(3) Uani 1 1 d . . . P2 P 0.82292(6) 0.8459(2) 0.06407(11) 0.0321(3) Uani 1 1 d . . . Zn1 Zn 0.73125(3) 0.67335(10) 0.06752(5) 0.03481(18) Uani 1 1 d . . . Zn2 Zn 0.85222(3) 0.37354(9) 0.30132(5) 0.03149(17) Uani 1 1 d . . . Zn3 Zn 0.85738(3) 0.78589(10) -0.07297(5) 0.03548(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.035(3) 0.031(3) 0.031(3) -0.004(2) 0.010(3) 0.000(3) C2 0.039(3) 0.031(4) 0.031(3) -0.004(2) 0.012(3) 0.005(3) C3 0.040(4) 0.044(4) 0.036(3) -0.011(3) 0.013(3) -0.003(3) C4 0.040(3) 0.017(3) 0.031(3) -0.003(2) 0.015(3) 0.002(2) C5 0.055(5) 0.037(4) 0.056(5) 0.021(3) 0.029(4) 0.018(4) C6 0.044(4) 0.043(4) 0.042(4) 0.013(3) 0.014(3) 0.013(3) C7 0.044(4) 0.049(5) 0.029(3) -0.014(3) 0.011(3) -0.001(3) C8 0.046(4) 0.044(4) 0.033(3) -0.011(3) 0.019(3) -0.009(3) C9 0.045(4) 0.037(4) 0.054(4) 0.008(3) 0.025(3) -0.005(3) C10 0.029(3) 0.036(3) 0.031(3) 0.004(3) 0.009(2) 0.002(3) C11 0.025(3) 0.037(4) 0.030(3) 0.003(2) 0.013(2) 0.006(2) C12 0.041(4) 0.038(4) 0.044(4) 0.015(3) 0.014(3) 0.006(3) C13 0.020(3) 0.034(3) 0.026(3) 0.007(2) 0.006(2) 0.006(2) C14 0.034(3) 0.048(4) 0.041(4) -0.009(3) 0.011(3) -0.009(3) C15 0.054(5) 0.051(5) 0.054(5) -0.007(4) 0.018(4) -0.020(4) C16 0.047(4) 0.049(5) 0.053(5) 0.021(4) 0.019(4) -0.002(4) C17 0.029(3) 0.053(5) 0.046(4) 0.018(3) 0.018(3) 0.008(3) C18 0.034(3) 0.043(4) 0.035(3) 0.011(3) 0.018(3) 0.006(3) C19 0.038(4) 0.034(4) 0.027(3) 0.008(3) 0.008(3) 0.005(3) C20 0.028(3) 0.032(3) 0.035(3) 0.002(3) 0.016(3) 0.003(3) C21 0.033(3) 0.031(3) 0.025(3) 0.003(3) 0.012(2) 0.002(3) C22 0.033(3) 0.033(3) 0.029(3) 0.008(3) 0.007(3) 0.001(3) C23 0.032(4) 0.027(4) 0.030(4) 0.000 0.011(4) 0.000 C24 0.032(5) 0.034(5) 0.036(5) 0.000 0.014(4) 0.000 C25 0.035(3) 0.033(3) 0.032(3) -0.005(3) 0.016(3) -0.004(3) C26 0.034(3) 0.031(4) 0.028(3) -0.003(2) 0.013(3) -0.002(3) C27 0.024(3) 0.032(3) 0.036(3) 0.004(3) 0.007(2) 0.001(3) C28 0.030(3) 0.031(4) 0.043(4) -0.001(3) 0.016(3) -0.001(3) C29 0.036(4) 0.031(5) 0.023(4) 0.000 0.017(4) 0.000 C30 0.027(4) 0.032(5) 0.040(5) 0.000 0.010(4) 0.000 N1 0.035(3) 0.033(3) 0.030(3) -0.003(2) 0.015(2) 0.000(2) N2 0.026(2) 0.032(3) 0.030(3) 0.000(2) 0.010(2) -0.001(2) O1 0.045(3) 0.041(3) 0.037(3) 0.007(2) 0.019(2) -0.008(2) O2 0.032(2) 0.030(2) 0.050(3) 0.008(2) 0.019(2) 0.003(2) O3 0.034(2) 0.043(3) 0.026(2) -0.0081(18) 0.0137(17) -0.015(2) O4 0.031(2) 0.045(3) 0.032(2) 0.0121(19) 0.0110(19) -0.0002(19) O5 0.034(2) 0.035(3) 0.032(2) 0.0005(19) 0.0127(18) 0.000(2) O6 0.035(2) 0.031(2) 0.042(3) 0.0057(19) 0.012(2) 0.0074(19) O7 0.031(2) 0.036(3) 0.042(3) 0.0012(19) 0.009(2) 0.0079(19) O8 0.035(3) 0.038(3) 0.043(3) -0.005(2) 0.006(2) 0.011(2) O9 0.038(3) 0.044(3) 0.049(3) -0.003(2) 0.019(2) -0.007(2) O10 0.032(2) 0.034(2) 0.043(3) -0.004(2) 0.012(2) -0.005(2) O11 0.033(2) 0.032(3) 0.046(3) 0.000(2) 0.014(2) -0.0024(19) O12 0.037(2) 0.037(2) 0.044(3) -0.016(2) 0.019(2) -0.007(2) O13 0.047(3) 0.053(3) 0.042(3) 0.002(2) 0.018(2) 0.010(3) O14 0.029(2) 0.038(3) 0.041(2) -0.003(2) 0.018(2) 0.0086(19) O1W 0.036(2) 0.032(3) 0.042(2) 0.002(2) 0.012(2) 0.003(2) O2W 0.037(2) 0.039(3) 0.033(2) -0.0157(19) 0.0102(19) -0.006(2) O3W 0.033(2) 0.040(3) 0.052(3) 0.003(2) 0.015(2) -0.005(2) P1 0.0289(8) 0.0265(8) 0.0306(8) 0.0003(6) 0.0133(6) -0.0035(6) P2 0.0275(7) 0.0271(8) 0.0345(8) 0.0027(6) 0.0133(6) 0.0015(6) Zn1 0.0363(4) 0.0287(4) 0.0360(4) 0.0053(3) 0.0183(3) -0.0017(3) Zn2 0.0268(3) 0.0282(4) 0.0290(3) 0.0003(3) 0.0095(3) -0.0008(3) Zn3 0.0340(4) 0.0287(4) 0.0333(4) 0.0011(3) 0.0128(3) 0.0002(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 C1 N1 1.472(8) . ? C1 P1 1.810(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N1 1.501(8) . ? C2 C4 1.501(7) . ? C2 C3 1.529(10) . ? C2 H2A 0.9601 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C5 1.3900 . ? C4 C9 1.3900 . ? C5 C6 1.3900 . ? C5 H5 0.9300 . ? C6 C7 1.3900 . ? C6 H6 0.9300 . ? C7 C8 1.3900 . ? C7 H7 0.9300 . ? C8 C9 1.3900 . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 N2 1.468(8) . ? C10 P2 1.800(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C13 1.504(7) . ? C11 C12 1.507(9) . ? C11 N2 1.522(7) . ? C11 H11A 0.9601 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C14 C15 1.3900 . ? C14 H14 0.9300 . ? C15 C16 1.3900 . ? C15 H15 0.9300 . ? C16 C17 1.3900 . ? C16 H16 0.9300 . ? C17 C18 1.3900 . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 O8 1.222(8) . ? C19 O7 1.258(9) . ? C19 C20 1.494(8) . ? C20 C24 1.374(8) . ? C20 C21 1.380(9) . ? C21 C23 1.416(8) . ? C21 C22 1.503(9) . ? C22 O9 1.242(8) . ? C22 O10 1.283(9) . ? C23 C21 1.416(8) 2_756 ? C23 H23A 0.9300 . ? C24 C20 1.374(8) 2_756 ? C24 H24A 0.9300 . ? C25 O12 1.214(8) . ? C25 O11 1.278(8) . ? C25 C26 1.509(9) . ? C26 C30 1.369(8) . ? C26 C27 1.376(9) . ? C27 C29 1.376(8) . ? C27 C28 1.511(9) . ? C28 O13 1.253(9) . ? C28 O14 1.255(8) . ? C29 C27 1.376(8) 2_755 ? C29 H29A 0.9300 . ? C30 C26 1.369(8) 2_755 ? C30 H30A 0.9300 . ? N1 H1C 0.9000 . ? N1 H1D 0.9000 . ? N2 H2B 0.9000 . ? N2 H2C 0.9000 . ? O1 P1 1.492(5) . ? O1 Zn1 1.873(5) . ? O2 P1 1.519(5) . ? O2 Zn2 1.890(4) . ? O3 P1 1.496(4) . ? O3 Zn3 1.931(4) 4_645 ? O4 P2 1.500(5) . ? O4 Zn1 1.956(5) . ? O5 P2 1.523(5) . ? O5 Zn3 1.929(5) . ? O6 P2 1.512(5) . ? O6 Zn1 1.965(5) 4_655 ? O7 Zn2 1.930(4) . ? O10 Zn2 1.962(5) 1_545 ? O11 Zn3 1.920(5) . ? O14 Zn3 1.958(4) 1_565 ? O1W Zn1 1.988(5) . ? O1W H1WA 0.9600 . ? O1W H1WB 0.9600 . ? O2W Zn2 2.041(4) . ? O2W H2WA 0.9600 . ? O2W H2WB 0.9600 . ? O3W H3WA 0.8499 . ? O3W H3WB 0.8499 . ? Zn1 O6 1.965(5) 4_645 ? Zn2 O10 1.962(5) 1_565 ? Zn3 O3 1.931(4) 4_655 ? Zn3 O14 1.958(5) 1_545 ? 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 C1 P1 112.5(5) . . ? N1 C1 H1A 109.1 . . ? P1 C1 H1A 109.1 . . ? N1 C1 H1B 109.1 . . ? P1 C1 H1B 109.1 . . ? H1A C1 H1B 107.8 . . ? N1 C2 C4 111.2(5) . . ? N1 C2 C3 107.9(6) . . ? C4 C2 C3 114.1(5) . . ? N1 C2 H2A 107.6 . . ? C4 C2 H2A 107.9 . . ? C3 C2 H2A 108.0 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C9 120.0 . . ? C5 C4 C2 120.5(4) . . ? C9 C4 C2 119.5(4) . . ? C4 C5 C6 120.0 . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C7 C6 C5 120.0 . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C8 120.0 . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C7 C8 C9 120.0 . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C8 C9 C4 120.0 . . ? C8 C9 H9 120.0 . . ? C4 C9 H9 120.0 . . ? N2 C10 P2 112.4(5) . . ? N2 C10 H10A 109.1 . . ? P2 C10 H10A 109.1 . . ? N2 C10 H10B 109.1 . . ? P2 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? C13 C11 C12 113.9(5) . . ? C13 C11 N2 112.0(5) . . ? C12 C11 N2 107.6(5) . . ? C13 C11 H11A 107.9 . . ? C12 C11 H11A 107.1 . . ? N2 C11 H11A 108.1 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 120.0 . . ? C14 C13 C11 117.8(4) . . ? C18 C13 C11 122.2(4) . . ? C13 C14 C15 120.0 . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C16 C15 C14 120.0 . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C17 C16 C15 120.0 . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C18 C17 C16 120.0 . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C13 120.0 . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? O8 C19 O7 125.1(6) . . ? O8 C19 C20 119.1(6) . . ? O7 C19 C20 115.8(6) . . ? C24 C20 C21 118.6(6) . . ? C24 C20 C19 120.4(6) . . ? C21 C20 C19 120.9(6) . . ? C20 C21 C23 120.5(6) . . ? C20 C21 C22 125.0(6) . . ? C23 C21 C22 114.4(6) . . ? O9 C22 O10 123.6(7) . . ? O9 C22 C21 117.9(6) . . ? O10 C22 C21 118.2(6) . . ? C21 C23 C21 118.4(9) 2_756 . ? C21 C23 H23A 120.8 2_756 . ? C21 C23 H23A 120.8 . . ? C20 C24 C20 123.4(9) . 2_756 ? C20 C24 H24A 118.3 . . ? C20 C24 H24A 118.3 2_756 . ? O12 C25 O11 122.5(6) . . ? O12 C25 C26 121.9(6) . . ? O11 C25 C26 115.6(6) . . ? C30 C26 C27 118.0(7) . . ? C30 C26 C25 120.2(6) . . ? C27 C26 C25 121.8(6) . . ? C26 C27 C29 119.3(7) . . ? C26 C27 C28 124.3(6) . . ? C29 C27 C28 116.4(7) . . ? O13 C28 O14 126.3(6) . . ? O13 C28 C27 117.6(6) . . ? O14 C28 C27 116.0(6) . . ? C27 C29 C27 121.8(9) . 2_755 ? C27 C29 H29A 119.1 . . ? C27 C29 H29A 119.1 2_755 . ? C26 C30 C26 123.6(9) 2_755 . ? C26 C30 H30A 118.2 2_755 . ? C26 C30 H30A 118.2 . . ? C1 N1 C2 114.7(5) . . ? C1 N1 H1C 108.6 . . ? C2 N1 H1C 108.6 . . ? C1 N1 H1D 108.6 . . ? C2 N1 H1D 108.6 . . ? H1C N1 H1D 107.6 . . ? C10 N2 C11 115.6(5) . . ? C10 N2 H2B 108.4 . . ? C11 N2 H2B 108.4 . . ? C10 N2 H2C 108.4 . . ? C11 N2 H2C 108.4 . . ? H2B N2 H2C 107.5 . . ? P1 O1 Zn1 161.0(3) . . ? P1 O2 Zn2 125.3(3) . . ? P1 O3 Zn3 129.7(3) . 4_645 ? P2 O4 Zn1 133.1(3) . . ? P2 O5 Zn3 134.3(3) . . ? P2 O6 Zn1 130.9(3) . 4_655 ? C19 O7 Zn2 121.2(4) . . ? C22 O10 Zn2 110.2(5) . 1_545 ? C25 O11 Zn3 120.3(4) . . ? C28 O14 Zn3 115.3(4) . 1_565 ? Zn1 O1W H1WA 109.6 . . ? Zn1 O1W H1WB 108.9 . . ? H1WA O1W H1WB 109.5 . . ? Zn2 O2W H2WA 109.9 . . ? Zn2 O2W H2WB 109.0 . . ? H2WA O2W H2WB 109.5 . . ? H3WA O3W H3WB 109.5 . . ? O1 P1 O3 117.7(3) . . ? O1 P1 O2 110.3(3) . . ? O3 P1 O2 111.7(3) . . ? O1 P1 C1 105.4(3) . . ? O3 P1 C1 104.7(3) . . ? O2 P1 C1 106.1(3) . . ? O4 P2 O6 113.1(3) . . ? O4 P2 O5 110.6(3) . . ? O6 P2 O5 114.5(3) . . ? O4 P2 C10 104.9(3) . . ? O6 P2 C10 105.4(3) . . ? O5 P2 C10 107.5(3) . . ? O1 Zn1 O4 100.18(19) . . ? O1 Zn1 O6 119.0(2) . 4_645 ? O4 Zn1 O6 105.6(2) . 4_645 ? O1 Zn1 O1W 124.2(2) . . ? O4 Zn1 O1W 109.6(2) . . ? O6 Zn1 O1W 97.2(2) 4_645 . ? O2 Zn2 O7 112.3(2) . . ? O2 Zn2 O10 127.6(2) . 1_565 ? O7 Zn2 O10 98.4(2) . 1_565 ? O2 Zn2 O2W 110.1(2) . . ? O7 Zn2 O2W 110.8(2) . . ? O10 Zn2 O2W 96.0(2) 1_565 . ? O11 Zn3 O5 122.3(2) . . ? O11 Zn3 O3 113.6(2) . 4_655 ? O5 Zn3 O3 104.95(18) . 4_655 ? O11 Zn3 O14 99.2(2) . 1_545 ? O5 Zn3 O14 112.9(2) . 1_545 ? O3 Zn3 O14 102.27(19) 4_655 1_545 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C4 C5 -57.9(6) . . . . ? C3 C2 C4 C5 64.4(6) . . . . ? N1 C2 C4 C9 124.2(5) . . . . ? C3 C2 C4 C9 -113.5(5) . . . . ? C9 C4 C5 C6 0.0 . . . . ? C2 C4 C5 C6 -178.0(5) . . . . ? C4 C5 C6 C7 0.0 . . . . ? C5 C6 C7 C8 0.0 . . . . ? C6 C7 C8 C9 0.0 . . . . ? C7 C8 C9 C4 0.0 . . . . ? C5 C4 C9 C8 0.0 . . . . ? C2 C4 C9 C8 178.0(5) . . . . ? C12 C11 C13 C14 -125.5(5) . . . . ? N2 C11 C13 C14 112.1(5) . . . . ? C12 C11 C13 C18 51.9(6) . . . . ? N2 C11 C13 C18 -70.5(5) . . . . ? C18 C13 C14 C15 0.0 . . . . ? C11 C13 C14 C15 177.5(4) . . . . ? C13 C14 C15 C16 0.0 . . . . ? C14 C15 C16 C17 0.0 . . . . ? C15 C16 C17 C18 0.0 . . . . ? C16 C17 C18 C13 0.0 . . . . ? C14 C13 C18 C17 0.0 . . . . ? C11 C13 C18 C17 -177.4(4) . . . . ? O8 C19 C20 C24 164.0(6) . . . . ? O7 C19 C20 C24 -15.0(9) . . . . ? O8 C19 C20 C21 -11.5(11) . . . . ? O7 C19 C20 C21 169.5(7) . . . . ? C24 C20 C21 C23 -3.7(9) . . . . ? C19 C20 C21 C23 171.9(5) . . . . ? C24 C20 C21 C22 174.1(5) . . . . ? C19 C20 C21 C22 -10.3(11) . . . . ? C20 C21 C22 O9 -80.6(9) . . . . ? C23 C21 C22 O9 97.4(7) . . . . ? C20 C21 C22 O10 105.2(8) . . . . ? C23 C21 C22 O10 -76.8(7) . . . . ? C20 C21 C23 C21 1.9(5) . . . 2_756 ? C22 C21 C23 C21 -176.2(6) . . . 2_756 ? C21 C20 C24 C20 1.9(5) . . . 2_756 ? C19 C20 C24 C20 -173.7(7) . . . 2_756 ? O12 C25 C26 C30 -179.5(5) . . . . ? O11 C25 C26 C30 0.1(9) . . . . ? O12 C25 C26 C27 -0.4(10) . . . . ? O11 C25 C26 C27 179.2(6) . . . . ? C30 C26 C27 C29 2.4(9) . . . . ? C25 C26 C27 C29 -176.7(5) . . . . ? C30 C26 C27 C28 -175.8(5) . . . . ? C25 C26 C27 C28 5.1(10) . . . . ? C26 C27 C28 O13 80.5(9) . . . . ? C29 C27 C28 O13 -97.8(7) . . . . ? C26 C27 C28 O14 -103.7(8) . . . . ? C29 C27 C28 O14 78.1(7) . . . . ? C26 C27 C29 C27 -1.2(4) . . . 2_755 ? C28 C27 C29 C27 177.1(6) . . . 2_755 ? C27 C26 C30 C26 -1.2(4) . . . 2_755 ? C25 C26 C30 C26 177.9(6) . . . 2_755 ? P1 C1 N1 C2 -163.5(4) . . . . ? C4 C2 N1 C1 -52.9(7) . . . . ? C3 C2 N1 C1 -178.6(5) . . . . ? P2 C10 N2 C11 -173.1(4) . . . . ? C13 C11 N2 C10 -55.5(7) . . . . ? C12 C11 N2 C10 178.6(6) . . . . ? O8 C19 O7 Zn2 -7.4(11) . . . . ? C20 C19 O7 Zn2 171.5(4) . . . . ? O9 C22 O10 Zn2 -19.5(8) . . . 1_545 ? C21 C22 O10 Zn2 154.4(5) . . . 1_545 ? O12 C25 O11 Zn3 19.8(9) . . . . ? C26 C25 O11 Zn3 -159.8(4) . . . . ? O13 C28 O14 Zn3 23.7(9) . . . 1_565 ? C27 C28 O14 Zn3 -151.7(5) . . . 1_565 ? Zn1 O1 P1 O3 -3.2(13) . . . . ? Zn1 O1 P1 O2 126.5(11) . . . . ? Zn1 O1 P1 C1 -119.4(11) . . . . ? Zn3 O3 P1 O1 8.8(5) 4_645 . . . ? Zn3 O3 P1 O2 -120.3(4) 4_645 . . . ? Zn3 O3 P1 C1 125.3(4) 4_645 . . . ? Zn2 O2 P1 O1 -0.5(5) . . . . ? Zn2 O2 P1 O3 132.3(3) . . . . ? Zn2 O2 P1 C1 -114.2(4) . . . . ? N1 C1 P1 O1 -50.1(5) . . . . ? N1 C1 P1 O3 -174.8(4) . . . . ? N1 C1 P1 O2 66.9(5) . . . . ? Zn1 O4 P2 O6 48.1(5) . . . . ? Zn1 O4 P2 O5 -82.0(4) . . . . ? Zn1 O4 P2 C10 162.5(4) . . . . ? Zn1 O6 P2 O4 -130.1(4) 4_655 . . . ? Zn1 O6 P2 O5 -2.1(5) 4_655 . . . ? Zn1 O6 P2 C10 115.9(4) 4_655 . . . ? Zn3 O5 P2 O4 -155.9(3) . . . . ? Zn3 O5 P2 O6 74.8(4) . . . . ? Zn3 O5 P2 C10 -42.0(5) . . . . ? N2 C10 P2 O4 53.7(5) . . . . ? N2 C10 P2 O6 173.4(5) . . . . ? N2 C10 P2 O5 -64.0(5) . . . . ? P1 O1 Zn1 O4 -148.9(11) . . . . ? P1 O1 Zn1 O6 -34.6(12) . . . 4_645 ? P1 O1 Zn1 O1W 88.8(12) . . . . ? P2 O4 Zn1 O1 -162.8(4) . . . . ? P2 O4 Zn1 O6 73.0(5) . . . 4_645 ? P2 O4 Zn1 O1W -30.7(5) . . . . ? P1 O2 Zn2 O7 -178.0(3) . . . . ? P1 O2 Zn2 O10 60.9(5) . . . 1_565 ? P1 O2 Zn2 O2W -54.1(4) . . . . ? C19 O7 Zn2 O2 74.6(6) . . . . ? C19 O7 Zn2 O10 -148.8(6) . . . 1_565 ? C19 O7 Zn2 O2W -49.0(6) . . . . ? C25 O11 Zn3 O5 -68.9(6) . . . . ? C25 O11 Zn3 O3 58.6(6) . . . 4_655 ? C25 O11 Zn3 O14 166.4(5) . . . 1_545 ? P2 O5 Zn3 O11 8.9(5) . . . . ? P2 O5 Zn3 O3 -122.3(4) . . . 4_655 ? P2 O5 Zn3 O14 127.1(4) . . . 1_545 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.395 _refine_diff_density_min -0.465 _refine_diff_density_rms 0.094