Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_zincphosphonate(2) _database_code_depnum_ccdc_archive 'CCDC 228183' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H46 O8 P2 Zn4' _chemical_formula_weight 737.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 9.933(2) _cell_length_b 11.311(2) _cell_length_c 13.865(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.59(3) _cell_angle_gamma 90.00 _cell_volume 1550.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 10 _cell_measurement_theta_max 12.5 _exptl_crystal_description blocks _exptl_crystal_colour none _exptl_crystal_size_max 1.00 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.60 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.581 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 3.197 _exptl_absorpt_correction_type 'azimuthal scans' _exptl_absorpt_correction_T_min 0.1423 _exptl_absorpt_correction_T_max 0.2500 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE AED2' _diffrn_measurement_method 'profile fit' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '90 min' _diffrn_standards_decay_% none _diffrn_reflns_number 3640 _diffrn_reflns_av_R_equivalents 0.1860 _diffrn_reflns_av_sigmaI/netI 0.0651 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.60 _diffrn_reflns_theta_max 25.03 _reflns_number_total 2728 _reflns_number_gt 2369 _reflns_threshold_expression >2sigma(I) _computing_data_collection DIF4 _computing_cell_refinement DIF4 _computing_data_reduction REDU4 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0744P)^2^+1.2743P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2728 _refine_ls_number_parameters 159 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0586 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1318 _refine_ls_wR_factor_gt 0.1256 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.113 _refine_ls_shift/su_max 0.005 _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 0.19839(6) 0.86883(4) 0.49400(4) 0.0256(2) Uani 1 1 d . . . P1 P -0.11070(12) 0.86830(9) 0.51912(8) 0.0209(3) Uani 1 1 d . . . O1 O 0.1972(3) 1.0310(3) 0.4479(2) 0.0247(7) Uani 1 1 d . . . C1 C 0.2853(6) 0.7280(4) 0.4499(4) 0.0371(12) Uani 1 1 d . . . H1B H 0.2176 0.6776 0.4139 0.056 Uiso 1 1 calc R . . H1C H 0.3279 0.6844 0.5059 0.056 Uiso 1 1 calc R . . H1D H 0.3544 0.7506 0.4075 0.056 Uiso 1 1 calc R . . Zn2 Zn 0.07971(6) 1.00244(4) 0.67427(4) 0.0261(2) Uani 1 1 d . . . O2 O 0.1038(3) 1.1368(2) 0.5897(2) 0.0248(7) Uani 1 1 d . . . C2 C 0.0400(7) 0.9968(4) 0.8087(4) 0.0434(14) Uani 1 1 d . . . H2B H -0.0332 1.0523 0.8184 0.065 Uiso 1 1 calc R . . H2C H 0.1211 1.0186 0.8509 0.065 Uiso 1 1 calc R . . H2D H 0.0121 0.9166 0.8245 0.065 Uiso 1 1 calc R . . O3 O 0.2894(3) 0.9261(3) 0.6506(2) 0.0286(8) Uani 1 1 d . . . C3 C -0.1814(5) 0.7305(4) 0.5576(3) 0.0261(10) Uani 1 1 d . . . O4 O 0.0348(3) 0.8784(2) 0.5704(2) 0.0249(7) Uani 1 1 d . . . C4 C -0.0941(6) 0.6275(4) 0.5249(4) 0.0362(13) Uani 1 1 d . . . H4A H -0.1313 0.5522 0.5451 0.054 Uiso 1 1 calc R . . H4B H -0.0010 0.6362 0.5547 0.054 Uiso 1 1 calc R . . H4C H -0.0946 0.6288 0.4542 0.054 Uiso 1 1 calc R . . C5 C -0.1786(5) 0.7306(4) 0.6681(3) 0.0299(11) Uani 1 1 d . . . H5A H -0.2222 0.6586 0.6892 0.045 Uiso 1 1 calc R . . H5B H -0.2273 0.8000 0.6888 0.045 Uiso 1 1 calc R . . H5C H -0.0846 0.7331 0.6970 0.045 Uiso 1 1 calc R . . C6 C -0.3249(5) 0.7190(4) 0.5109(4) 0.0346(12) Uani 1 1 d . . . H6A H -0.3651 0.6461 0.5333 0.052 Uiso 1 1 calc R . . H6B H -0.3243 0.7164 0.4403 0.052 Uiso 1 1 calc R . . H6C H -0.3782 0.7870 0.5289 0.052 Uiso 1 1 calc R . . C11 C 0.3225(5) 0.8249(4) 0.7154(4) 0.0331(11) Uani 1 1 d . . . H11A H 0.2865 0.7505 0.6855 0.040 Uiso 1 1 calc R . . H11B H 0.2845 0.8361 0.7782 0.040 Uiso 1 1 calc R . . C12 C 0.4733(5) 0.8227(4) 0.7289(4) 0.0396(13) Uani 1 1 d . . . H12A H 0.5106 0.7763 0.6770 0.048 Uiso 1 1 calc R . . H12B H 0.5063 0.7886 0.7926 0.048 Uiso 1 1 calc R . . C13 C 0.5114(6) 0.9514(5) 0.7232(5) 0.0499(16) Uani 1 1 d . . . H13A H 0.5108 0.9900 0.7872 0.060 Uiso 1 1 calc R . . H13B H 0.6025 0.9602 0.7007 0.060 Uiso 1 1 calc R . . C14 C 0.4071(6) 1.0032(4) 0.6525(5) 0.0453(16) Uani 1 1 d . . . H14A H 0.3838 1.0841 0.6726 0.054 Uiso 1 1 calc R . . H14B H 0.4403 1.0073 0.5875 0.054 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 0.0240(4) 0.0209(3) 0.0320(3) 0.00007(19) 0.0035(3) 0.00541(19) P1 0.0180(6) 0.0183(5) 0.0264(6) 0.0009(4) 0.0023(5) 0.0006(4) O1 0.0221(18) 0.0233(14) 0.0295(16) 0.0039(12) 0.0065(14) 0.0037(12) C1 0.033(3) 0.038(3) 0.041(3) -0.007(2) 0.007(2) 0.009(2) Zn2 0.0302(4) 0.0239(3) 0.0246(3) 0.00166(18) 0.0041(3) 0.0018(2) O2 0.0258(18) 0.0212(14) 0.0285(17) 0.0028(11) 0.0085(15) 0.0002(12) C2 0.065(4) 0.033(3) 0.033(3) 0.004(2) 0.009(3) 0.008(2) O3 0.0214(18) 0.0269(16) 0.0360(18) 0.0075(13) -0.0050(15) 0.0002(13) C3 0.025(3) 0.023(2) 0.031(2) 0.0036(17) 0.005(2) -0.0015(18) O4 0.0250(19) 0.0213(15) 0.0280(16) 0.0007(11) 0.0005(15) 0.0024(12) C4 0.050(4) 0.019(2) 0.042(3) 0.0027(19) 0.014(3) 0.000(2) C5 0.029(3) 0.027(2) 0.033(2) 0.0043(18) 0.002(2) -0.0008(18) C6 0.032(3) 0.037(3) 0.035(3) 0.002(2) 0.002(2) -0.014(2) C11 0.030(3) 0.034(2) 0.035(3) 0.010(2) -0.001(2) 0.001(2) C12 0.026(3) 0.037(3) 0.054(3) 0.008(2) -0.002(3) 0.006(2) C13 0.036(3) 0.036(3) 0.075(4) -0.002(3) -0.013(3) -0.004(2) C14 0.034(3) 0.037(3) 0.061(4) 0.014(2) -0.012(3) -0.011(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 C1 1.940(5) . ? Zn1 O1 1.943(3) . ? Zn1 O4 2.028(4) . ? Zn1 O3 2.360(3) . ? P1 O2 1.518(3) 3_576 ? P1 O1 1.523(3) 3_576 ? P1 O4 1.551(3) . ? P1 C3 1.811(4) . ? O1 P1 1.523(3) 3_576 ? Zn2 C2 1.943(6) . ? Zn2 O2 1.949(3) . ? Zn2 O4 2.029(3) . ? Zn2 O3 2.308(3) . ? O2 P1 1.518(3) 3_576 ? O3 C14 1.457(6) . ? O3 C11 1.471(5) . ? C3 C6 1.512(7) . ? C3 C5 1.529(6) . ? C3 C4 1.547(7) . ? C11 C12 1.492(7) . ? C12 C13 1.509(7) . ? C13 C14 1.476(7) . ? 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 C1 Zn1 O1 131.3(2) . . ? C1 Zn1 O4 127.8(2) . . ? O1 Zn1 O4 98.17(13) . . ? C1 Zn1 O3 111.92(17) . . ? O1 Zn1 O3 91.91(12) . . ? O4 Zn1 O3 76.06(12) . . ? O2 P1 O1 114.11(17) 3_576 3_576 ? O2 P1 O4 109.2(2) 3_576 . ? O1 P1 O4 109.54(17) 3_576 . ? O2 P1 C3 108.45(19) 3_576 . ? O1 P1 C3 108.0(2) 3_576 . ? O4 P1 C3 107.39(19) . . ? P1 O1 Zn1 126.3(2) 3_576 . ? C2 Zn2 O2 130.63(17) . . ? C2 Zn2 O4 127.35(19) . . ? O2 Zn2 O4 98.26(13) . . ? C2 Zn2 O3 113.2(2) . . ? O2 Zn2 O3 92.35(13) . . ? O4 Zn2 O3 77.26(12) . . ? P1 O2 Zn2 126.07(17) 3_576 . ? C14 O3 C11 108.8(3) . . ? C14 O3 Zn2 120.5(3) . . ? C11 O3 Zn2 110.8(3) . . ? C14 O3 Zn1 114.6(3) . . ? C11 O3 Zn1 113.0(3) . . ? Zn2 O3 Zn1 87.90(11) . . ? C6 C3 C5 110.7(4) . . ? C6 C3 C4 110.0(4) . . ? C5 C3 C4 109.8(4) . . ? C6 C3 P1 108.9(3) . . ? C5 C3 P1 109.0(3) . . ? C4 C3 P1 108.5(3) . . ? P1 O4 Zn1 120.96(18) . . ? P1 O4 Zn2 120.47(19) . . ? Zn1 O4 Zn2 106.00(15) . . ? O3 C11 C12 104.6(4) . . ? C11 C12 C13 103.4(4) . . ? C14 C13 C12 104.7(4) . . ? O3 C14 C13 106.5(4) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.198 _refine_diff_density_min -0.649 _refine_diff_density_rms 0.140 data_zincphosphonate3 _database_code_depnum_ccdc_archive 'CCDC 228184' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H80 O16 P4 Zn6' _chemical_formula_weight 1285.10 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' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.512(3) _cell_length_b 13.218(3) _cell_length_c 16.542(3) _cell_angle_alpha 89.39(3) _cell_angle_beta 85.99(3) _cell_angle_gamma 78.10(3) _cell_volume 2670.7(9) _cell_formula_units_Z 2 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.598 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 2.830 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.462 _exptl_absorpt_correction_T_max 0.568 _exptl_absorpt_process_details XPREP _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22491 _diffrn_reflns_av_R_equivalents 0.0981 _diffrn_reflns_av_sigmaI/netI 0.1142 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 24.84 _reflns_number_total 9031 _reflns_number_gt 5839 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0228P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9031 _refine_ls_number_parameters 575 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.0833 _refine_ls_wR_factor_gt 0.0796 _refine_ls_goodness_of_fit_ref 0.783 _refine_ls_restrained_S_all 0.783 _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 0.57293(5) 0.32632(4) 0.37570(3) 0.02201(14) Uani 1 1 d . . . Zn2 Zn 0.77390(5) 0.48573(4) 0.23884(3) 0.02243(14) Uani 1 1 d . . . Zn3 Zn 0.83442(5) 0.07707(4) 0.33196(3) 0.02451(14) Uani 1 1 d . . . Zn4 Zn 0.57307(5) 0.32805(4) 0.12279(3) 0.02142(14) Uani 1 1 d . . . Zn5 Zn 0.83109(5) 0.08146(4) 0.14278(3) 0.02474(14) Uani 1 1 d . . . Zn6 Zn 0.97214(5) 0.21106(4) 0.22871(3) 0.02465(14) Uani 1 1 d . . . P7 P 0.51386(11) 0.51130(10) 0.25127(7) 0.0221(3) Uani 1 1 d . . . P8 P 0.60045(11) 0.13650(9) 0.24859(7) 0.0215(3) Uani 1 1 d . . . P9 P 0.82517(11) 0.32329(10) 0.38158(7) 0.0220(3) Uani 1 1 d . . . P10 P 0.82511(11) 0.32868(9) 0.09211(7) 0.0215(3) Uani 1 1 d . . . O13 O 0.8623(3) 0.2258(2) 0.32799(19) 0.0245(8) Uani 1 1 d . . . O12 O 0.8598(3) 0.2285(2) 0.14197(18) 0.0232(8) Uani 1 1 d . . . O11 O 0.8403(3) 0.4171(2) 0.33159(19) 0.0272(8) Uani 1 1 d . . . O10 O 0.8429(3) 0.4202(3) 0.14042(19) 0.0286(8) Uani 1 1 d . . . O9 O 0.9442(3) 0.0597(2) 0.23108(19) 0.0248(8) Uani 1 1 d . . . O8 O 0.5740(3) 0.1975(3) 0.17187(19) 0.0291(8) Uani 1 1 d . . . O60 O 0.4754(3) 0.3180(3) 0.0318(2) 0.0284(8) Uani 1 1 d . . . O7 O 0.7249(3) 0.0881(2) 0.24442(19) 0.0226(8) Uani 1 1 d . . . O6 O 0.5688(3) 0.1984(3) 0.32603(19) 0.0309(9) Uani 1 1 d . . . O5 O 0.7089(3) 0.3304(3) 0.41873(19) 0.0310(9) Uani 1 1 d . . . O50 O 0.4728(3) 0.3175(3) 0.4765(2) 0.0292(8) Uani 1 1 d . . . O40 O 0.8381(3) 0.6155(3) 0.2432(2) 0.0330(9) Uani 1 1 d . . . O4 O 0.5026(3) 0.4521(3) 0.3286(2) 0.0316(9) Uani 1 1 d . . . O3 O 0.7093(3) 0.3401(3) 0.06711(19) 0.0273(8) Uani 1 1 d . . . O2 O 0.6211(3) 0.5485(3) 0.2442(2) 0.0303(8) Uani 1 1 d . . . O1 O 0.4998(3) 0.4515(3) 0.1767(2) 0.0296(8) Uani 1 1 d . . . C3 C 0.7799(5) 0.7204(4) 0.2269(4) 0.0393(15) Uani 1 1 d . . . H3A H 0.7117 0.7384 0.2625 0.047 Uiso 1 1 calc R . . H3B H 0.7608 0.7270 0.1697 0.047 Uiso 1 1 calc R . . C2 C 0.4020(4) 0.6240(4) 0.2565(3) 0.0264(12) Uani 1 1 d . . . C1 C 0.5237(4) 0.0334(4) 0.2527(3) 0.0256(12) Uani 1 1 d . . . C25 C 0.9130(4) 0.3185(4) -0.0016(3) 0.0244(11) Uani 1 1 d . . . C24 C 0.8304(4) -0.0090(4) 0.0492(3) 0.0315(13) Uani 1 1 d . . . H24A H 0.9004 -0.0130 0.0163 0.038 Uiso 1 1 calc R . . H24B H 0.8295 -0.0793 0.0700 0.038 Uiso 1 1 calc R . . C23 C 0.9145(5) 0.3118(4) 0.4652(3) 0.0291(12) Uani 1 1 d . . . C22 C 1.0416(4) -0.0199(4) 0.2199(3) 0.0320(13) Uani 1 1 d . . . H22A H 1.0891 -0.0010 0.1742 0.038 Uiso 1 1 calc R . . H22B H 1.0211 -0.0856 0.2057 0.038 Uiso 1 1 calc R . . C21 C 1.0333(4) 0.2932(5) 0.0172(3) 0.0352(13) Uani 1 1 d . . . H21A H 1.0795 0.2916 -0.0333 0.053 Uiso 1 1 calc R . . H21B H 1.0497 0.2255 0.0436 0.053 Uiso 1 1 calc R . . H21C H 1.0479 0.3462 0.0534 0.053 Uiso 1 1 calc R . . C20 C 0.7360(5) 0.0208(5) -0.0082(3) 0.0428(15) Uani 1 1 d . . . H20A H 0.7459 -0.0303 -0.0520 0.064 Uiso 1 1 calc R . . H20B H 0.7367 0.0893 -0.0312 0.064 Uiso 1 1 calc R . . H20C H 0.6658 0.0221 0.0224 0.064 Uiso 1 1 calc R . . C19 C 0.8304(4) -0.0107(4) 0.4288(3) 0.0298(12) Uani 1 1 d . . . H19A H 0.8315 -0.0819 0.4104 0.036 Uiso 1 1 calc R . . H19B H 0.8986 -0.0127 0.4563 0.036 Uiso 1 1 calc R . . C18 C 0.5547(5) -0.0351(4) 0.1763(3) 0.0340(13) Uani 1 1 d . . . H18A H 0.5185 -0.0942 0.1811 0.051 Uiso 1 1 calc R . . H18B H 0.6342 -0.0600 0.1707 0.051 Uiso 1 1 calc R . . H18C H 0.5309 0.0055 0.1284 0.051 Uiso 1 1 calc R . . C17 C 0.4379(5) 0.2225(4) 0.4983(3) 0.0394(15) Uani 1 1 d . . . H17A H 0.4857 0.1836 0.5383 0.047 Uiso 1 1 calc R . . H17B H 0.4413 0.1784 0.4498 0.047 Uiso 1 1 calc R . . C16 C 0.4097(5) 0.6887(4) 0.3310(3) 0.0410(15) Uani 1 1 d . . . H16A H 0.3468 0.7469 0.3358 0.062 Uiso 1 1 calc R . . H16B H 0.4775 0.7150 0.3254 0.062 Uiso 1 1 calc R . . H16C H 0.4097 0.6456 0.3796 0.062 Uiso 1 1 calc R . . C15 C 1.1212(5) 0.2391(4) 0.2198(3) 0.0338(13) Uani 1 1 d . . . H15A H 1.1603 0.2047 0.2659 0.041 Uiso 1 1 calc R . . H15B H 1.1592 0.2053 0.1696 0.041 Uiso 1 1 calc R . . C14 C 0.4433(5) 0.2217(4) 0.0125(4) 0.0400(15) Uani 1 1 d . . . H14A H 0.4492 0.1751 0.0599 0.048 Uiso 1 1 calc R . . H14B H 0.4909 0.1861 -0.0333 0.048 Uiso 1 1 calc R . . C13 C 0.5485(5) -0.0327(4) 0.3280(3) 0.0349(13) Uani 1 1 d . . . H13A H 0.5127 -0.0920 0.3267 0.052 Uiso 1 1 calc R . . H13B H 0.5209 0.0089 0.3766 0.052 Uiso 1 1 calc R . . H13C H 0.6278 -0.0575 0.3291 0.052 Uiso 1 1 calc R . . C12 C 0.9411(4) 0.6170(4) 0.2773(3) 0.0321(13) Uani 1 1 d . . . H12A H 1.0033 0.5850 0.2394 0.038 Uiso 1 1 calc R . . H12B H 0.9465 0.5785 0.3291 0.038 Uiso 1 1 calc R . . C11 C 0.2928(5) 0.5891(5) 0.2617(4) 0.0386(14) Uani 1 1 d . . . H11A H 0.2327 0.6498 0.2669 0.058 Uiso 1 1 calc R . . H11B H 0.2889 0.5446 0.3091 0.058 Uiso 1 1 calc R . . H11C H 0.2868 0.5506 0.2125 0.058 Uiso 1 1 calc R . . C10 C 0.8896(5) 0.4223(4) -0.0466(3) 0.0388(15) Uani 1 1 d . . . H10A H 0.9334 0.4160 -0.0985 0.058 Uiso 1 1 calc R . . H10B H 0.9089 0.4761 -0.0135 0.058 Uiso 1 1 calc R . . H10C H 0.8117 0.4408 -0.0565 0.058 Uiso 1 1 calc R . . C9 C 0.8877(5) 0.2332(4) -0.0554(3) 0.0377(14) Uani 1 1 d . . . H9A H 0.9328 0.2290 -0.1066 0.057 Uiso 1 1 calc R . . H9B H 0.8101 0.2496 -0.0666 0.057 Uiso 1 1 calc R . . H9C H 0.9039 0.1667 -0.0274 0.057 Uiso 1 1 calc R . . C8 C 0.4104(5) 0.6904(4) 0.1798(3) 0.0401(15) Uani 1 1 d . . . H8A H 0.3488 0.7499 0.1818 0.060 Uiso 1 1 calc R . . H8B H 0.4083 0.6486 0.1316 0.060 Uiso 1 1 calc R . . H8C H 0.4794 0.7147 0.1775 0.060 Uiso 1 1 calc R . . C7 C 1.1043(5) -0.0353(5) 0.2948(4) 0.0500(17) Uani 1 1 d . . . H7A H 1.1677 -0.0925 0.2860 0.075 Uiso 1 1 calc R . . H7B H 1.0568 -0.0516 0.3406 0.075 Uiso 1 1 calc R . . H7C H 1.1294 0.0281 0.3067 0.075 Uiso 1 1 calc R . . C43 C 0.3180(5) 0.3588(4) -0.0412(4) 0.0441(16) Uani 1 1 d . . . H43A H 0.3425 0.3583 -0.0995 0.053 Uiso 1 1 calc R . . H43B H 0.2415 0.3980 -0.0339 0.053 Uiso 1 1 calc R . . C42 C 0.3911(5) 0.4047(4) 0.0082(4) 0.0454(17) Uani 1 1 d . . . H42A H 0.4242 0.4553 -0.0240 0.055 Uiso 1 1 calc R . . H42B H 0.3496 0.4401 0.0566 0.055 Uiso 1 1 calc R . . C41 C 0.8556(5) 0.7886(4) 0.2436(4) 0.0432(15) Uani 1 1 d . . . H41A H 0.8161 0.8502 0.2748 0.052 Uiso 1 1 calc R . . H41B H 0.8880 0.8121 0.1923 0.052 Uiso 1 1 calc R . . C40 C 0.4010(4) 0.0811(5) 0.2545(4) 0.0387(14) Uani 1 1 d . . . H40A H 0.3594 0.0259 0.2547 0.058 Uiso 1 1 calc R . . H40B H 0.3859 0.1244 0.2066 0.058 Uiso 1 1 calc R . . H40C H 0.3793 0.1235 0.3035 0.058 Uiso 1 1 calc R . . C39 C 0.7325(5) 0.0202(5) 0.4927(3) 0.0456(16) Uani 1 1 d . . . H39A H 0.7403 -0.0295 0.5373 0.068 Uiso 1 1 calc R . . H39B H 0.6640 0.0202 0.4674 0.068 Uiso 1 1 calc R . . H39C H 0.7314 0.0895 0.5136 0.068 Uiso 1 1 calc R . . C38 C 0.3276(5) 0.2505(5) -0.0097(4) 0.0497(17) Uani 1 1 d . . . H38A H 0.2760 0.2484 0.0382 0.060 Uiso 1 1 calc R . . H38B H 0.3131 0.2035 -0.0519 0.060 Uiso 1 1 calc R . . C37 C 0.3906(5) 0.4054(5) 0.5070(4) 0.0449(16) Uani 1 1 d . . . H37A H 0.3579 0.4477 0.4617 0.054 Uiso 1 1 calc R . . H37B H 0.4231 0.4495 0.5421 0.054 Uiso 1 1 calc R . . C36 C 0.8855(6) 0.4119(5) 0.5162(3) 0.0466(17) Uani 1 1 d . . . H36A H 0.9249 0.4020 0.5658 0.070 Uiso 1 1 calc R . . H36B H 0.8065 0.4285 0.5306 0.070 Uiso 1 1 calc R . . H36C H 0.9067 0.4688 0.4848 0.070 Uiso 1 1 calc R . . C35 C 0.8940(6) 0.2231(5) 0.5195(4) 0.0516(18) Uani 1 1 d . . . H35A H 0.9411 0.2168 0.5649 0.077 Uiso 1 1 calc R . . H35B H 0.9107 0.1585 0.4881 0.077 Uiso 1 1 calc R . . H35C H 0.8171 0.2367 0.5403 0.077 Uiso 1 1 calc R . . C34 C 1.1342(6) 0.3521(5) 0.2183(4) 0.0536(18) Uani 1 1 d . . . H34A H 1.2118 0.3544 0.2087 0.080 Uiso 1 1 calc R . . H34B H 1.1060 0.3850 0.2705 0.080 Uiso 1 1 calc R . . H34C H 1.0931 0.3890 0.1749 0.080 Uiso 1 1 calc R . . C33 C 0.9422(6) 0.7278(4) 0.2911(4) 0.0538(19) Uani 1 1 d . . . H33A H 0.9273 0.7453 0.3494 0.065 Uiso 1 1 calc R . . H33B H 1.0144 0.7426 0.2728 0.065 Uiso 1 1 calc R . . C32 C 1.0333(5) 0.2928(7) 0.4354(4) 0.067(2) Uani 1 1 d . . . H32A H 1.0789 0.2822 0.4817 0.100 Uiso 1 1 calc R . . H32B H 1.0475 0.3527 0.4042 0.100 Uiso 1 1 calc R . . H32C H 1.0508 0.2311 0.4007 0.100 Uiso 1 1 calc R . . C31 C 0.3234(6) 0.2526(6) 0.5338(6) 0.078(3) Uani 1 1 d . . . H31A H 0.2711 0.2413 0.4943 0.093 Uiso 1 1 calc R . . H31B H 0.3126 0.2117 0.5831 0.093 Uiso 1 1 calc R . . C30 C 0.3083(6) 0.3606(5) 0.5533(6) 0.080(3) Uani 1 1 d . . . H30A H 0.3151 0.3690 0.6120 0.096 Uiso 1 1 calc R . . H30B H 0.2342 0.3970 0.5403 0.096 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 0.0244(3) 0.0183(3) 0.0225(3) -0.0013(2) -0.0026(2) -0.0019(2) Zn2 0.0258(3) 0.0162(3) 0.0246(3) -0.0027(2) -0.0036(2) -0.0017(2) Zn3 0.0261(3) 0.0189(3) 0.0277(3) 0.0000(2) -0.0035(3) -0.0020(3) Zn4 0.0237(3) 0.0171(3) 0.0229(3) -0.0012(2) -0.0040(2) -0.0020(2) Zn5 0.0279(3) 0.0177(3) 0.0278(3) -0.0032(2) -0.0030(3) -0.0023(3) Zn6 0.0241(3) 0.0178(3) 0.0315(3) -0.0003(2) -0.0038(3) -0.0024(2) P7 0.0246(7) 0.0162(6) 0.0234(6) -0.0015(5) -0.0026(6) 0.0009(5) P8 0.0239(7) 0.0147(6) 0.0254(6) -0.0011(5) -0.0030(6) -0.0021(5) P9 0.0250(7) 0.0167(6) 0.0236(6) -0.0018(5) -0.0052(6) -0.0012(5) P10 0.0247(7) 0.0157(6) 0.0227(6) 0.0003(5) -0.0005(5) -0.0014(5) O13 0.028(2) 0.0170(17) 0.0307(18) -0.0041(14) -0.0084(16) -0.0076(15) O12 0.0272(19) 0.0176(17) 0.0249(17) 0.0049(13) -0.0016(15) -0.0053(15) O11 0.038(2) 0.0186(18) 0.0272(18) -0.0011(14) -0.0064(16) -0.0086(16) O10 0.038(2) 0.0203(18) 0.0239(17) -0.0012(14) -0.0016(16) 0.0014(16) O9 0.0244(19) 0.0138(17) 0.0354(19) -0.0024(14) -0.0057(16) -0.0009(15) O8 0.033(2) 0.028(2) 0.0262(18) 0.0066(15) -0.0050(16) -0.0053(17) O60 0.032(2) 0.0184(18) 0.0352(19) -0.0023(15) -0.0121(17) -0.0034(16) O7 0.0154(17) 0.0207(18) 0.0324(18) -0.0034(14) -0.0018(15) -0.0049(14) O6 0.033(2) 0.029(2) 0.0273(18) -0.0102(15) 0.0047(16) 0.0002(17) O5 0.031(2) 0.034(2) 0.0243(18) -0.0043(15) -0.0012(16) 0.0012(17) O50 0.034(2) 0.0201(18) 0.0321(18) 0.0001(15) 0.0026(17) -0.0027(16) O40 0.033(2) 0.0179(18) 0.050(2) 0.0014(16) -0.0171(18) -0.0059(16) O4 0.033(2) 0.0256(19) 0.0324(19) 0.0034(15) 0.0018(17) 0.0013(17) O3 0.0236(19) 0.029(2) 0.0290(18) 0.0042(15) -0.0032(15) -0.0051(16) O2 0.025(2) 0.0219(19) 0.043(2) -0.0028(16) -0.0034(17) -0.0039(16) O1 0.030(2) 0.0249(19) 0.0338(19) -0.0081(15) -0.0068(17) -0.0035(16) C3 0.055(4) 0.015(3) 0.050(3) 0.010(2) -0.022(3) -0.007(3) C2 0.026(3) 0.019(3) 0.032(3) -0.001(2) -0.003(2) 0.000(2) C1 0.024(3) 0.022(3) 0.033(3) -0.005(2) -0.005(2) -0.007(2) C25 0.025(3) 0.024(3) 0.023(2) -0.002(2) -0.001(2) -0.003(2) C24 0.028(3) 0.023(3) 0.042(3) -0.008(2) 0.000(3) -0.004(2) C23 0.039(3) 0.023(3) 0.024(3) 0.000(2) -0.008(2) -0.001(2) C22 0.028(3) 0.017(3) 0.047(3) -0.002(2) 0.003(3) 0.004(2) C21 0.021(3) 0.041(3) 0.042(3) -0.002(3) 0.008(2) -0.005(3) C20 0.046(4) 0.048(4) 0.038(3) -0.005(3) -0.010(3) -0.016(3) C19 0.035(3) 0.020(3) 0.037(3) 0.004(2) -0.012(3) -0.009(2) C18 0.043(4) 0.025(3) 0.038(3) -0.008(2) -0.005(3) -0.015(3) C17 0.052(4) 0.026(3) 0.038(3) 0.002(2) 0.016(3) -0.010(3) C16 0.038(4) 0.026(3) 0.055(4) -0.016(3) -0.008(3) 0.004(3) C15 0.031(3) 0.030(3) 0.039(3) 0.002(2) 0.000(3) -0.004(3) C14 0.058(4) 0.019(3) 0.044(3) -0.002(2) -0.025(3) -0.004(3) C13 0.037(3) 0.026(3) 0.047(3) 0.006(2) -0.003(3) -0.020(3) C12 0.022(3) 0.027(3) 0.047(3) -0.002(2) -0.011(3) -0.002(2) C11 0.028(3) 0.034(3) 0.050(3) -0.005(3) 0.000(3) 0.000(3) C10 0.049(4) 0.031(3) 0.033(3) 0.002(2) 0.011(3) -0.004(3) C9 0.039(3) 0.040(3) 0.034(3) -0.015(3) 0.009(3) -0.010(3) C8 0.037(3) 0.025(3) 0.052(3) 0.008(3) 0.000(3) 0.008(3) C7 0.032(3) 0.047(4) 0.065(4) 0.010(3) -0.007(3) 0.009(3) C43 0.040(4) 0.031(3) 0.061(4) -0.004(3) -0.029(3) 0.000(3) C42 0.053(4) 0.024(3) 0.057(4) -0.004(3) -0.035(3) 0.009(3) C41 0.046(4) 0.020(3) 0.062(4) -0.006(3) -0.009(3) -0.002(3) C40 0.025(3) 0.043(4) 0.050(3) 0.000(3) -0.004(3) -0.012(3) C39 0.053(4) 0.052(4) 0.036(3) -0.002(3) 0.001(3) -0.023(3) C38 0.048(4) 0.040(4) 0.068(4) 0.005(3) -0.030(4) -0.017(3) C37 0.055(4) 0.028(3) 0.043(3) -0.005(3) 0.017(3) 0.003(3) C36 0.073(5) 0.033(3) 0.038(3) -0.005(3) -0.025(3) -0.013(3) C35 0.080(5) 0.033(3) 0.049(4) 0.009(3) -0.037(4) -0.019(3) C34 0.069(5) 0.048(4) 0.050(4) -0.002(3) -0.011(4) -0.024(4) C33 0.059(4) 0.027(3) 0.083(5) 0.009(3) -0.042(4) -0.015(3) C32 0.036(4) 0.113(7) 0.049(4) -0.020(4) -0.019(3) -0.003(4) C31 0.051(5) 0.054(5) 0.127(7) 0.009(5) 0.024(5) -0.017(4) C30 0.061(5) 0.033(4) 0.135(7) -0.012(4) 0.062(5) -0.008(4) _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 O6 1.899(4) . ? Zn1 O4 1.900(3) . ? Zn1 O5 1.900(4) . ? Zn1 O50 2.031(3) . ? Zn2 O10 1.916(3) . ? Zn2 O2 1.917(3) . ? Zn2 O11 1.925(3) . ? Zn2 O40 2.042(4) . ? Zn3 C19 1.972(5) . ? Zn3 O7 2.046(3) . ? Zn3 O13 2.066(3) . ? Zn3 O9 2.069(3) . ? Zn3 Zn6 3.1313(13) . ? Zn3 Zn5 3.1323(10) . ? Zn4 O1 1.897(3) . ? Zn4 O8 1.898(3) . ? Zn4 O3 1.915(4) . ? Zn4 O60 2.026(3) . ? Zn5 C24 1.968(5) . ? Zn5 O12 2.048(3) . ? Zn5 O7 2.059(3) . ? Zn5 O9 2.081(3) . ? Zn5 Zn6 3.1176(12) . ? Zn6 C15 1.970(6) . ? Zn6 O13 2.050(3) . ? Zn6 O12 2.057(3) . ? Zn6 O9 2.100(3) . ? P7 O4 1.506(4) . ? P7 O1 1.511(4) . ? P7 O2 1.518(4) . ? P7 C2 1.820(5) . ? P8 O6 1.512(3) . ? P8 O8 1.515(3) . ? P8 O7 1.554(3) . ? P8 C1 1.820(5) . ? P9 O11 1.520(4) . ? P9 O5 1.524(4) . ? P9 O13 1.544(3) . ? P9 C23 1.824(5) . ? P10 O3 1.512(4) . ? P10 O10 1.520(4) . ? P10 O12 1.553(3) . ? P10 C25 1.826(5) . ? O9 C22 1.439(5) . ? O60 C14 1.456(6) . ? O60 C42 1.460(6) . ? O50 C17 1.447(6) . ? O50 C37 1.452(6) . ? O40 C12 1.448(6) . ? O40 C3 1.459(6) . ? C3 C41 1.477(8) . ? C2 C11 1.525(8) . ? C2 C16 1.527(7) . ? C2 C8 1.544(7) . ? C1 C13 1.527(7) . ? C1 C40 1.533(7) . ? C1 C18 1.542(7) . ? C25 C21 1.526(7) . ? C25 C10 1.537(7) . ? C25 C9 1.541(7) . ? C24 C20 1.552(8) . ? C23 C32 1.504(8) . ? C23 C35 1.522(8) . ? C23 C36 1.542(7) . ? C22 C7 1.503(8) . ? C19 C39 1.550(8) . ? C17 C31 1.486(9) . ? C15 C34 1.535(8) . ? C14 C38 1.490(8) . ? C12 C33 1.488(8) . ? C43 C42 1.489(8) . ? C43 C38 1.503(8) . ? C41 C33 1.477(8) . ? C37 C30 1.459(9) . ? C31 C30 1.439(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Zn1 O4 119.62(16) . . ? O6 Zn1 O5 114.02(15) . . ? O4 Zn1 O5 114.79(17) . . ? O6 Zn1 O50 99.46(15) . . ? O4 Zn1 O50 101.98(14) . . ? O5 Zn1 O50 103.01(15) . . ? O10 Zn2 O2 119.62(15) . . ? O10 Zn2 O11 110.72(14) . . ? O2 Zn2 O11 120.88(15) . . ? O10 Zn2 O40 102.76(16) . . ? O2 Zn2 O40 99.52(15) . . ? O11 Zn2 O40 97.56(15) . . ? C19 Zn3 O7 123.43(19) . . ? C19 Zn3 O13 126.67(18) . . ? O7 Zn3 O13 99.54(13) . . ? C19 Zn3 O9 130.07(17) . . ? O7 Zn3 O9 81.45(13) . . ? O13 Zn3 O9 81.98(13) . . ? C19 Zn3 Zn6 145.00(17) . . ? O7 Zn3 Zn6 91.05(10) . . ? O13 Zn3 Zn6 40.28(9) . . ? O9 Zn3 Zn6 41.70(9) . . ? C19 Zn3 Zn5 144.42(16) . . ? O7 Zn3 Zn5 40.43(9) . . ? O13 Zn3 Zn5 88.67(9) . . ? O9 Zn3 Zn5 41.14(9) . . ? Zn6 Zn3 Zn5 59.70(3) . . ? O1 Zn4 O8 120.48(15) . . ? O1 Zn4 O3 113.19(16) . . ? O8 Zn4 O3 114.26(15) . . ? O1 Zn4 O60 102.52(14) . . ? O8 Zn4 O60 99.22(15) . . ? O3 Zn4 O60 103.53(14) . . ? C24 Zn5 O12 127.78(19) . . ? C24 Zn5 O7 123.7(2) . . ? O12 Zn5 O7 100.59(13) . . ? C24 Zn5 O9 126.68(17) . . ? O12 Zn5 O9 82.72(13) . . ? O7 Zn5 O9 80.84(13) . . ? C24 Zn5 Zn6 143.65(17) . . ? O12 Zn5 Zn6 40.69(9) . . ? O7 Zn5 Zn6 91.18(10) . . ? O9 Zn5 Zn6 42.02(9) . . ? C24 Zn5 Zn3 141.62(16) . . ? O12 Zn5 Zn3 89.86(9) . . ? O7 Zn5 Zn3 40.11(9) . . ? O9 Zn5 Zn3 40.86(9) . . ? Zn6 Zn5 Zn3 60.13(3) . . ? C15 Zn6 O13 128.74(19) . . ? C15 Zn6 O12 128.49(19) . . ? O13 Zn6 O12 97.14(13) . . ? C15 Zn6 O9 121.85(18) . . ? O13 Zn6 O9 81.60(13) . . ? O12 Zn6 O9 82.03(13) . . ? C15 Zn6 Zn5 139.63(16) . . ? O13 Zn6 Zn5 89.35(10) . . ? O12 Zn6 Zn5 40.48(9) . . ? O9 Zn6 Zn5 41.56(9) . . ? C15 Zn6 Zn3 139.40(16) . . ? O13 Zn6 Zn3 40.65(9) . . ? O12 Zn6 Zn3 89.72(10) . . ? O9 Zn6 Zn3 40.95(9) . . ? Zn5 Zn6 Zn3 60.17(2) . . ? O4 P7 O1 112.9(2) . . ? O4 P7 O2 111.2(2) . . ? O1 P7 O2 111.3(2) . . ? O4 P7 C2 106.6(2) . . ? O1 P7 C2 106.1(2) . . ? O2 P7 C2 108.3(2) . . ? O6 P8 O8 114.5(2) . . ? O6 P8 O7 109.4(2) . . ? O8 P8 O7 109.1(2) . . ? O6 P8 C1 107.0(2) . . ? O8 P8 C1 107.5(2) . . ? O7 P8 C1 109.1(2) . . ? O11 P9 O5 113.9(2) . . ? O11 P9 O13 108.58(18) . . ? O5 P9 O13 111.1(2) . . ? O11 P9 C23 108.2(2) . . ? O5 P9 C23 107.0(2) . . ? O13 P9 C23 107.9(2) . . ? O3 P10 O10 113.5(2) . . ? O3 P10 O12 111.2(2) . . ? O10 P10 O12 108.85(19) . . ? O3 P10 C25 106.3(2) . . ? O10 P10 C25 108.3(2) . . ? O12 P10 C25 108.5(2) . . ? P9 O13 Zn6 125.7(2) . . ? P9 O13 Zn3 135.1(2) . . ? Zn6 O13 Zn3 99.06(13) . . ? P10 O12 Zn5 136.7(2) . . ? P10 O12 Zn6 124.2(2) . . ? Zn5 O12 Zn6 98.83(13) . . ? P9 O11 Zn2 134.7(2) . . ? P10 O10 Zn2 133.0(2) . . ? C22 O9 Zn3 125.5(3) . . ? C22 O9 Zn5 119.4(3) . . ? Zn3 O9 Zn5 98.00(14) . . ? C22 O9 Zn6 114.6(3) . . ? Zn3 O9 Zn6 97.35(13) . . ? Zn5 O9 Zn6 96.42(13) . . ? P8 O8 Zn4 142.9(2) . . ? C14 O60 C42 109.0(4) . . ? C14 O60 Zn4 122.0(3) . . ? C42 O60 Zn4 122.6(3) . . ? P8 O7 Zn3 129.94(19) . . ? P8 O7 Zn5 125.52(19) . . ? Zn3 O7 Zn5 99.46(14) . . ? P8 O6 Zn1 143.2(2) . . ? P9 O5 Zn1 134.1(2) . . ? C17 O50 C37 109.7(4) . . ? C17 O50 Zn1 121.2(3) . . ? C37 O50 Zn1 122.3(3) . . ? C12 O40 C3 110.6(4) . . ? C12 O40 Zn2 123.2(3) . . ? C3 O40 Zn2 125.4(3) . . ? P7 O4 Zn1 137.9(2) . . ? P10 O3 Zn4 134.2(2) . . ? P7 O2 Zn2 136.5(2) . . ? P7 O1 Zn4 137.1(2) . . ? O40 C3 C41 106.0(5) . . ? C11 C2 C16 109.9(4) . . ? C11 C2 C8 109.5(5) . . ? C16 C2 C8 109.0(5) . . ? C11 C2 P7 109.6(4) . . ? C16 C2 P7 109.5(4) . . ? C8 C2 P7 109.4(3) . . ? C13 C1 C40 109.9(4) . . ? C13 C1 C18 109.5(4) . . ? C40 C1 C18 108.2(5) . . ? C13 C1 P8 110.2(4) . . ? C40 C1 P8 109.1(4) . . ? C18 C1 P8 109.8(4) . . ? C21 C25 C10 109.0(5) . . ? C21 C25 C9 110.0(4) . . ? C10 C25 C9 109.3(4) . . ? C21 C25 P10 110.3(3) . . ? C10 C25 P10 109.1(3) . . ? C9 C25 P10 109.1(4) . . ? C20 C24 Zn5 118.0(4) . . ? C32 C23 C35 109.6(5) . . ? C32 C23 C36 109.5(6) . . ? C35 C23 C36 107.9(4) . . ? C32 C23 P9 111.7(4) . . ? C35 C23 P9 108.9(4) . . ? C36 C23 P9 109.3(4) . . ? O9 C22 C7 111.8(4) . . ? C39 C19 Zn3 117.7(4) . . ? O50 C17 C31 106.6(5) . . ? C34 C15 Zn6 118.4(4) . . ? O60 C14 C38 106.3(4) . . ? O40 C12 C33 106.0(4) . . ? C42 C43 C38 104.4(5) . . ? O60 C42 C43 105.5(4) . . ? C3 C41 C33 107.1(5) . . ? C14 C38 C43 103.4(5) . . ? O50 C37 C30 105.1(5) . . ? C41 C33 C12 106.7(5) . . ? C30 C31 C17 105.2(6) . . ? C31 C30 C37 109.7(6) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 24.84 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.741 _refine_diff_density_min -0.654 _refine_diff_density_rms 0.101