# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Zheng, Li-Min' _publ_contact_author_name 'Zheng, Li-Min' _publ_contact_author_email lmzheng@netra.nju.edu.cn _publ_section_title ; Co3(2-OOCC6H4PO3)2(H2O)3*H2O: A layered metal phosphonate showing reversible dehydration-rehydration behavior and ferrimagnetic ordering ; # Attachment '- Co.cif' data_co _database_code_depnum_ccdc_archive 'CCDC 789612' #TrackingRef '- Co.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H16 Co3 O14 P2' _chemical_formula_weight 647.00 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.782(2) _cell_length_b 7.1452(13) _cell_length_c 24.309(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.926(3) _cell_angle_gamma 90.00 _cell_volume 2009.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 2468 _cell_measurement_theta_min 2.976 _cell_measurement_theta_max 28.1045 _exptl_crystal_description blocky _exptl_crystal_colour purple _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.139 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1292 _exptl_absorpt_coefficient_mu 2.683 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5899 _exptl_absorpt_correction_T_max 0.6160 _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 '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 9433 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0252 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3526 _reflns_number_gt 3125 _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^)+(0.0910P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3526 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1247 _refine_ls_wR_factor_gt 0.1204 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 0.7116(3) 0.2358(6) 0.00003(17) 0.0316(9) Uani 1 1 d . . . C2 C 0.6278(4) 0.2078(6) -0.04713(19) 0.0347(9) Uani 1 1 d . . . H2 H 0.6501 0.1778 -0.0808 0.042 Uiso 1 1 calc R . . C3 C 0.5121(3) 0.2230(6) -0.04569(18) 0.0337(9) Uani 1 1 d . . . H3 H 0.4578 0.2011 -0.0782 0.040 Uiso 1 1 calc R . . C4 C 0.4756(4) 0.2695(6) 0.00222(18) 0.0369(10) Uani 1 1 d . . . H4 H 0.3971 0.2774 0.0031 0.044 Uiso 1 1 calc R . . C5 C 0.5565(3) 0.3043(6) 0.04880(18) 0.0323(9) Uani 1 1 d . . . H5 H 0.5324 0.3378 0.0817 0.039 Uiso 1 1 calc R . . C6 C 0.6741(4) 0.2913(7) 0.04881(19) 0.0373(10) Uani 1 1 d . . . C7 C 0.7545(4) 0.3349(6) 0.10222(17) 0.0307(9) Uani 1 1 d . . . C8 C 1.2397(3) 0.6165(6) 0.17923(17) 0.0296(9) Uani 1 1 d . . . C9 C 1.3287(4) 0.7375(7) 0.19932(18) 0.0364(10) Uani 1 1 d . . . H9 H 1.3117 0.8541 0.2127 0.044 Uiso 1 1 calc R . . C10 C 1.4418(3) 0.6907(6) 0.20016(17) 0.0333(9) Uani 1 1 d . . . H10 H 1.4998 0.7771 0.2129 0.040 Uiso 1 1 calc R . . C11 C 1.4699(4) 0.5199(6) 0.18254(18) 0.0357(10) Uani 1 1 d . . . H11 H 1.5470 0.4888 0.1838 0.043 Uiso 1 1 calc R . . C12 C 1.3824(4) 0.3900(7) 0.16244(18) 0.0345(10) Uani 1 1 d . . . H12 H 1.4011 0.2719 0.1508 0.041 Uiso 1 1 calc R . . C13 C 1.2687(4) 0.4390(6) 0.16017(17) 0.0314(9) Uani 1 1 d . . . C14 C 1.1765(4) 0.3009(6) 0.13756(17) 0.0328(9) Uani 1 1 d . . . Co1 Co 0.97409(5) 0.54104(8) 0.06136(2) 0.03291(19) Uani 1 1 d . . . Co3 Co 0.88860(5) 0.37845(8) 0.19446(2) 0.03228(19) Uani 1 1 d . . . Co2 Co 1.04658(5) 0.02149(8) 0.10408(2) 0.03028(18) Uani 1 1 d . . . O1 O 0.9293(3) 0.3521(4) -0.00437(12) 0.0340(7) Uani 1 1 d . . . O2 O 0.8971(2) 0.0660(4) 0.05384(12) 0.0321(6) Uani 1 1 d . . . O3 O 0.8539(2) 0.0489(4) -0.05065(12) 0.0331(7) Uani 1 1 d . . . O4 O 0.8486(2) 0.4258(4) 0.10445(12) 0.0309(6) Uani 1 1 d . . . O5 O 0.7304(2) 0.2757(4) 0.14753(11) 0.0301(6) Uani 1 1 d . . . O7 O 1.0442(2) 0.4863(4) 0.20164(11) 0.0288(6) Uani 1 1 d . . . O6 O 1.0279(2) 0.7356(4) 0.12509(12) 0.0311(6) Uani 1 1 d . . . O8 O 1.0954(2) 0.8271(4) 0.22440(12) 0.0329(6) Uani 1 1 d . . . O9 O 1.1005(2) 0.3371(4) 0.09595(12) 0.0327(7) Uani 1 1 d . . . O10 O 1.1836(3) 0.1392(4) 0.16017(12) 0.0342(7) Uani 1 1 d . . . O2W O 0.8366(2) 0.7108(4) 0.02064(12) 0.0336(6) Uani 1 1 d . . . H2A H 0.8571 0.7686 -0.0064 0.040 Uiso 1 1 d R . . H2B H 0.8191 0.7862 0.0430 0.050 Uiso 1 1 d R . . O3W O 0.8012(2) 0.6228(4) 0.21645(13) 0.0364(7) Uani 1 1 d . . . H3A H 0.8450 0.7178 0.2175 0.044 Uiso 1 1 d R . . H3B H 0.7846 0.6086 0.2487 0.044 Uiso 1 1 d R . . O1W O 0.9490(3) 0.0947(4) 0.17323(12) 0.0328(6) Uani 1 1 d . . . H1A H 0.8888 0.0265 0.1673 0.039 Uiso 1 1 d R . . H1B H 0.9906 0.0541 0.2033 0.039 Uiso 1 1 d R . . O4W O 0.7466(3) 0.8843(4) 0.13290(12) 0.0351(7) Uani 1 1 d . . . H4A H 0.7067 0.9514 0.1075 0.053 Uiso 1 1 d R . . H4B H 0.7018 0.8157 0.1478 0.053 Uiso 1 1 d R . . P1 P 0.85814(9) 0.17437(16) -0.00107(5) 0.0309(3) Uani 1 1 d . . . P2 P 1.09272(9) 0.66816(16) 0.18338(5) 0.0337(3) 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 0.029(2) 0.033(2) 0.033(2) 0.0059(18) 0.0055(16) -0.0038(17) C2 0.026(2) 0.039(2) 0.038(2) 0.0050(19) 0.0022(17) -0.0001(18) C3 0.029(2) 0.039(2) 0.030(2) -0.0003(18) -0.0042(16) 0.0026(17) C4 0.036(2) 0.037(2) 0.037(2) 0.0023(19) 0.0032(18) 0.0005(19) C5 0.028(2) 0.035(2) 0.037(2) -0.0020(18) 0.0142(18) 0.0005(17) C6 0.034(2) 0.038(2) 0.038(2) -0.0010(19) 0.0029(18) 0.0041(19) C7 0.036(2) 0.028(2) 0.029(2) -0.0001(17) 0.0080(17) 0.0073(18) C8 0.027(2) 0.027(2) 0.034(2) 0.0020(17) 0.0047(17) -0.0009(16) C9 0.033(2) 0.041(3) 0.035(2) -0.011(2) 0.0068(18) -0.0083(19) C10 0.026(2) 0.040(2) 0.033(2) -0.0046(18) 0.0041(17) -0.0111(17) C11 0.036(2) 0.038(2) 0.031(2) -0.0056(18) 0.0022(18) -0.0021(18) C12 0.032(2) 0.039(3) 0.033(2) 0.0029(18) 0.0072(17) 0.0098(18) C13 0.036(2) 0.028(2) 0.030(2) -0.0002(17) 0.0045(17) 0.0030(17) C14 0.036(2) 0.034(2) 0.029(2) -0.0021(17) 0.0085(18) -0.0011(18) Co1 0.0317(3) 0.0334(4) 0.0332(3) -0.0008(2) 0.0053(3) -0.0007(2) Co3 0.0287(3) 0.0323(3) 0.0356(3) 0.0023(2) 0.0055(2) -0.0022(2) Co2 0.0334(3) 0.0283(3) 0.0285(3) -0.0014(2) 0.0044(2) -0.0007(2) O1 0.0374(16) 0.0365(17) 0.0304(15) -0.0007(13) 0.0119(12) -0.0022(13) O2 0.0292(15) 0.0310(15) 0.0340(16) 0.0084(13) 0.0011(12) 0.0010(12) O3 0.0337(15) 0.0330(16) 0.0342(16) -0.0143(12) 0.0107(12) -0.0056(12) O4 0.0265(14) 0.0324(16) 0.0316(15) -0.0032(12) -0.0007(12) -0.0016(12) O5 0.0286(14) 0.0315(15) 0.0321(14) 0.0033(12) 0.0107(11) -0.0095(12) O7 0.0281(14) 0.0301(15) 0.0291(14) 0.0023(12) 0.0075(11) -0.0041(11) O6 0.0291(14) 0.0327(16) 0.0325(15) -0.0039(13) 0.0088(12) -0.0011(12) O8 0.0287(14) 0.0352(15) 0.0342(15) -0.0021(13) 0.0043(12) -0.0052(12) O9 0.0323(15) 0.0353(16) 0.0267(14) -0.0025(12) -0.0038(12) 0.0074(12) O10 0.0386(16) 0.0301(16) 0.0312(15) 0.0023(13) -0.0001(12) -0.0037(12) O2W 0.0370(16) 0.0355(16) 0.0277(14) 0.0065(12) 0.0045(12) 0.0063(13) O3W 0.0371(16) 0.0345(17) 0.0376(16) 0.0040(13) 0.0067(13) 0.0224(13) O1W 0.0372(16) 0.0278(15) 0.0318(15) 0.0027(12) 0.0020(12) 0.0038(12) O4W 0.0374(16) 0.0294(16) 0.0329(15) 0.0213(13) -0.0074(12) -0.0095(12) P1 0.0309(5) 0.0323(6) 0.0291(6) -0.0017(4) 0.0048(4) -0.0007(4) P2 0.0324(6) 0.0334(6) 0.0349(6) 0.0005(5) 0.0052(5) -0.0004(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 C1 C2 1.378(6) . ? C1 C6 1.399(6) . ? C1 P1 1.787(4) . ? C2 C3 1.375(6) . ? C2 H2 0.9300 . ? C3 C4 1.357(6) . ? C3 H3 0.9300 . ? C4 C5 1.358(6) . ? C4 H4 0.9300 . ? C5 C6 1.389(6) . ? C5 H5 0.9300 . ? C6 C7 1.488(6) . ? C7 O5 1.262(5) . ? C7 O4 1.277(5) . ? C7 Co3 2.505(4) . ? C8 C9 1.375(6) . ? C8 C13 1.414(6) . ? C8 P2 1.792(4) . ? C9 C10 1.370(6) . ? C9 H9 0.9300 . ? C10 C11 1.355(6) . ? C10 H10 0.9300 . ? C11 C12 1.405(6) . ? C11 H11 0.9300 . ? C12 C13 1.375(6) . ? C12 H12 0.9300 . ? C13 C14 1.493(6) . ? C14 O9 1.244(5) . ? C14 O10 1.276(5) . ? Co1 O1 2.082(3) . ? Co1 O6 2.088(3) . ? Co1 O1 2.097(3) 3_765 ? Co1 O2W 2.113(3) . ? Co1 O4 2.133(3) . ? Co1 O9 2.139(3) . ? Co3 O7 1.965(3) . ? Co3 O8 1.980(3) 2_745 ? Co3 O5 2.123(3) . ? Co3 O3W 2.145(3) . ? Co3 O4 2.176(3) . ? Co3 O1W 2.241(3) . ? Co2 O2 1.969(3) . ? Co2 O3 1.973(3) 3_755 ? Co2 O10 2.083(3) . ? Co2 O6 2.127(3) 1_545 ? Co2 O1W 2.270(3) . ? Co2 O9 2.361(3) . ? O1 P1 1.532(3) . ? O1 Co1 2.097(3) 3_765 ? O2 P1 1.536(3) . ? O3 P1 1.495(3) . ? O3 Co2 1.973(3) 3_755 ? O7 P2 1.519(3) . ? O6 P2 1.553(3) . ? O6 Co2 2.127(3) 1_565 ? O8 P2 1.508(3) . ? O8 Co3 1.980(3) 2_755 ? O2W H2A 0.8501 . ? O2W H2B 0.8200 . ? O3W H3A 0.8501 . ? O3W H3B 0.8500 . ? O1W H1A 0.8500 . ? O1W H1B 0.8500 . ? O4W H4A 0.8500 . ? O4W H4B 0.8500 . ? 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 C2 C1 C6 117.1(4) . . ? C2 C1 P1 119.6(3) . . ? C6 C1 P1 122.9(3) . . ? C3 C2 C1 121.7(4) . . ? C3 C2 H2 119.2 . . ? C1 C2 H2 119.2 . . ? C4 C3 C2 121.2(4) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C3 C4 C5 118.3(4) . . ? C3 C4 H4 120.9 . . ? C5 C4 H4 120.9 . . ? C4 C5 C6 122.1(4) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C5 C6 C1 119.6(4) . . ? C5 C6 C7 117.2(4) . . ? C1 C6 C7 123.2(4) . . ? O5 C7 O4 118.1(4) . . ? O5 C7 C6 118.7(4) . . ? O4 C7 C6 123.2(4) . . ? O5 C7 Co3 57.9(2) . . ? O4 C7 Co3 60.3(2) . . ? C6 C7 Co3 174.9(3) . . ? C9 C8 C13 117.7(4) . . ? C9 C8 P2 122.0(3) . . ? C13 C8 P2 119.9(3) . . ? C10 C9 C8 121.7(4) . . ? C10 C9 H9 119.1 . . ? C8 C9 H9 119.1 . . ? C11 C10 C9 120.7(4) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C10 C11 C12 119.8(4) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C13 C12 C11 119.4(4) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 C8 120.6(4) . . ? C12 C13 C14 118.8(4) . . ? C8 C13 C14 120.6(4) . . ? O9 C14 O10 121.1(4) . . ? O9 C14 C13 121.6(4) . . ? O10 C14 C13 117.2(4) . . ? O1 Co1 O6 176.41(11) . . ? O1 Co1 O1 79.61(13) . 3_765 ? O6 Co1 O1 96.95(11) . 3_765 ? O1 Co1 O2W 87.26(12) . . ? O6 Co1 O2W 93.64(12) . . ? O1 Co1 O2W 86.88(12) 3_765 . ? O1 Co1 O4 91.60(11) . . ? O6 Co1 O4 91.94(11) . . ? O1 Co1 O4 168.22(11) 3_765 . ? O2W Co1 O4 84.85(11) . . ? O1 Co1 O9 85.20(11) . . ? O6 Co1 O9 94.07(11) . . ? O1 Co1 O9 94.75(12) 3_765 . ? O2W Co1 O9 171.86(12) . . ? O4 Co1 O9 92.30(12) . . ? O7 Co3 O8 94.18(11) . 2_745 ? O7 Co3 O5 153.16(11) . . ? O8 Co3 O5 112.30(11) 2_745 . ? O7 Co3 O3W 98.17(12) . . ? O8 Co3 O3W 82.08(12) 2_745 . ? O5 Co3 O3W 90.08(12) . . ? O7 Co3 O4 92.81(11) . . ? O8 Co3 O4 172.92(11) 2_745 . ? O5 Co3 O4 60.84(10) . . ? O3W Co3 O4 95.80(11) . . ? O7 Co3 O1W 92.51(12) . . ? O8 Co3 O1W 95.02(11) 2_745 . ? O5 Co3 O1W 81.26(11) . . ? O3W Co3 O1W 169.09(12) . . ? O4 Co3 O1W 85.81(11) . . ? O7 Co3 C7 123.19(13) . . ? O8 Co3 C7 142.52(13) 2_745 . ? O5 Co3 C7 30.22(12) . . ? O3W Co3 C7 94.20(12) . . ? O4 Co3 C7 30.64(13) . . ? O1W Co3 C7 81.68(12) . . ? O2 Co2 O3 101.90(12) . 3_755 ? O2 Co2 O10 146.29(12) . . ? O3 Co2 O10 92.88(12) 3_755 . ? O2 Co2 O6 100.54(12) . 1_545 ? O3 Co2 O6 90.84(12) 3_755 1_545 ? O10 Co2 O6 109.46(11) . 1_545 ? O2 Co2 O1W 84.44(12) . . ? O3 Co2 O1W 173.63(12) 3_755 . ? O10 Co2 O1W 81.99(12) . . ? O6 Co2 O1W 87.34(10) 1_545 . ? O2 Co2 O9 90.99(11) . . ? O3 Co2 O9 89.16(11) 3_755 . ? O10 Co2 O9 58.78(10) . . ? O6 Co2 O9 168.22(10) 1_545 . ? O1W Co2 O9 91.38(10) . . ? P1 O1 Co1 123.99(17) . . ? P1 O1 Co1 135.03(18) . 3_765 ? Co1 O1 Co1 100.39(13) . 3_765 ? P1 O2 Co2 134.84(18) . . ? P1 O3 Co2 138.60(18) . 3_755 ? C7 O4 Co1 148.5(3) . . ? C7 O4 Co3 89.1(2) . . ? Co1 O4 Co3 121.05(12) . . ? C7 O5 Co3 91.9(2) . . ? P2 O7 Co3 134.89(18) . . ? P2 O6 Co1 119.85(17) . . ? P2 O6 Co2 117.49(16) . 1_565 ? Co1 O6 Co2 119.46(13) . 1_565 ? P2 O8 Co3 141.7(2) . 2_755 ? C14 O9 Co1 143.2(3) . . ? C14 O9 Co2 84.1(3) . . ? Co1 O9 Co2 120.33(13) . . ? C14 O10 Co2 96.0(2) . . ? Co1 O2W H2A 109.7 . . ? Co1 O2W H2B 109.5 . . ? H2A O2W H2B 109.8 . . ? Co3 O3W H3A 109.9 . . ? Co3 O3W H3B 109.8 . . ? H3A O3W H3B 108.2 . . ? Co3 O1W Co2 127.34(13) . . ? Co3 O1W H1A 105.4 . . ? Co2 O1W H1A 105.4 . . ? Co3 O1W H1B 105.5 . . ? Co2 O1W H1B 105.5 . . ? H1A O1W H1B 106.1 . . ? H4A O4W H4B 109.5 . . ? O3 P1 O1 112.94(17) . . ? O3 P1 O2 110.91(19) . . ? O1 P1 O2 112.77(17) . . ? O3 P1 C1 105.93(19) . . ? O1 P1 C1 109.69(19) . . ? O2 P1 C1 103.98(18) . . ? O8 P2 O7 114.37(17) . . ? O8 P2 O6 108.34(17) . . ? O7 P2 O6 112.62(16) . . ? O8 P2 C8 107.04(18) . . ? O7 P2 C8 105.18(18) . . ? O6 P2 C8 109.01(18) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.347 _refine_diff_density_min -0.757 _refine_diff_density_rms 0.084 # Attachment '- zn.cif' data_zn _database_code_depnum_ccdc_archive 'CCDC 789613' #TrackingRef '- zn.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H16 O14 P2 Zn3' _chemical_formula_weight 666.32 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)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.764(2) _cell_length_b 7.2014(13) _cell_length_c 24.274(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.887(3) _cell_angle_gamma 90.00 _cell_volume 2019.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2355 _cell_measurement_theta_min 2.955 _cell_measurement_theta_max 27.0265 _exptl_crystal_description blocky _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.192 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 3.769 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.454 _exptl_absorpt_correction_T_max 0.471 _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Bruker Smart Aepex 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 9537 _diffrn_reflns_av_R_equivalents 0.0886 _diffrn_reflns_av_sigmaI/netI 0.0833 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3555 _reflns_number_gt 2865 _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^)+(0.0590P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3555 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0691 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.1283 _refine_ls_wR_factor_gt 0.1217 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7116(5) 0.2365(9) 0.0013(3) 0.0209(15) Uani 1 1 d . . . C2 C 0.6283(6) 0.2026(11) -0.0457(3) 0.0342(18) Uani 1 1 d . . . H2 H 0.6511 0.1662 -0.0787 0.041 Uiso 1 1 calc R . . C3 C 0.5130(7) 0.2209(12) -0.0451(4) 0.047(2) Uani 1 1 d . . . H3 H 0.4592 0.1997 -0.0778 0.056 Uiso 1 1 calc R . . C4 C 0.4752(6) 0.2696(13) 0.0025(3) 0.046(2) Uani 1 1 d . . . H4 H 0.3966 0.2790 0.0030 0.055 Uiso 1 1 calc R . . C5 C 0.5567(6) 0.3046(11) 0.0500(3) 0.0384(19) Uani 1 1 d . . . H5 H 0.5323 0.3379 0.0829 0.046 Uiso 1 1 calc R . . C6 C 0.6731(6) 0.2917(9) 0.0500(3) 0.0244(15) Uani 1 1 d . . . C7 C 0.7558(6) 0.3391(9) 0.1038(3) 0.0244(16) Uani 1 1 d . . . C8 C 1.2403(5) 0.6096(9) 0.1797(2) 0.0183(14) Uani 1 1 d . . . C9 C 1.3298(6) 0.7327(10) 0.1992(3) 0.0290(17) Uani 1 1 d . . . H9 H 1.3127 0.8499 0.2115 0.035 Uiso 1 1 calc R . . C10 C 1.4427(6) 0.6842(11) 0.2006(3) 0.0354(18) Uani 1 1 d . . . H10 H 1.5014 0.7692 0.2134 0.043 Uiso 1 1 calc R . . C11 C 1.4704(6) 0.5102(11) 0.1831(3) 0.0357(19) Uani 1 1 d . . . H11 H 1.5473 0.4773 0.1844 0.043 Uiso 1 1 calc R . . C12 C 1.3818(6) 0.3843(11) 0.1636(3) 0.0296(17) Uani 1 1 d . . . H12 H 1.3996 0.2662 0.1522 0.036 Uiso 1 1 calc R . . C13 C 1.2674(5) 0.4351(9) 0.1610(2) 0.0175(14) Uani 1 1 d . . . C14 C 1.1758(5) 0.2999(9) 0.1366(3) 0.0185(14) Uani 1 1 d . . . Zn1 Zn 0.97346(6) 0.54607(10) 0.06094(3) 0.0179(2) Uani 1 1 d . . . Zn3 Zn 0.88641(7) 0.38749(12) 0.19648(3) 0.0279(2) Uani 1 1 d . . . Zn2 Zn 1.04687(7) 0.01155(10) 0.10376(3) 0.0211(2) Uani 1 1 d . . . O1 O 0.9289(3) 0.3521(6) -0.00324(17) 0.0175(10) Uani 1 1 d . . . O2 O 0.8983(4) 0.0697(6) 0.05541(19) 0.0246(11) Uani 1 1 d . . . O3 O 0.8554(4) 0.0518(6) -0.04948(19) 0.0283(11) Uani 1 1 d . . . O4 O 0.8488(4) 0.4301(6) 0.10460(18) 0.0257(11) Uani 1 1 d . . . O5 O 0.7306(4) 0.2836(7) 0.14885(19) 0.0351(13) Uani 1 1 d . . . O7 O 1.0412(4) 0.4912(6) 0.20205(18) 0.0223(10) Uani 1 1 d . . . O6 O 1.0285(4) 0.7339(5) 0.12517(16) 0.0178(9) Uani 1 1 d . . . O8 O 1.0970(4) 0.8263(6) 0.22437(17) 0.0219(10) Uani 1 1 d . . . O9 O 1.0992(4) 0.3445(6) 0.09524(18) 0.0249(11) Uani 1 1 d . . . O10 O 1.1797(4) 0.1394(6) 0.15728(18) 0.0244(11) Uani 1 1 d . . . O2W O 0.8353(4) 0.7091(6) 0.0197(2) 0.0313(12) Uani 1 1 d . . . H2A H 0.8558 0.7670 -0.0074 0.038 Uiso 1 1 d R . . H2B H 0.8178 0.7846 0.0420 0.047 Uiso 1 1 d R . . O3W O 0.7949(5) 0.6248(8) 0.2179(2) 0.0513(16) Uani 1 1 d . . . H3A H 0.8388 0.7197 0.2189 0.062 Uiso 1 1 d R . . H3B H 0.7783 0.6106 0.2502 0.062 Uiso 1 1 d R . . O1W O 0.9465(4) 0.0955(7) 0.1741(2) 0.0339(12) Uani 1 1 d . . . H1A H 0.8863 0.0273 0.1681 0.041 Uiso 1 1 d R . . H1B H 0.9881 0.0549 0.2041 0.041 Uiso 1 1 d R . . O4W O 0.7454(7) 0.8881(11) 0.1358(3) 0.106(3) Uani 1 1 d . . . H4A H 0.7055 0.9553 0.1104 0.159 Uiso 1 1 d R . . H4B H 0.7006 0.8196 0.1507 0.159 Uiso 1 1 d R . . P1 P 0.85928(15) 0.1756(2) 0.00067(7) 0.0189(4) Uani 1 1 d . . . P2 P 1.09272(14) 0.6673(2) 0.18350(6) 0.0159(4) 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 0.021(4) 0.022(4) 0.021(4) 0.005(3) 0.008(3) -0.006(3) C2 0.037(4) 0.044(5) 0.022(4) -0.006(3) 0.007(3) -0.008(4) C3 0.030(5) 0.067(6) 0.040(5) -0.009(4) -0.006(4) -0.001(4) C4 0.019(4) 0.069(6) 0.048(5) -0.004(5) 0.002(4) 0.000(4) C5 0.031(4) 0.050(5) 0.037(5) -0.004(4) 0.014(4) -0.003(4) C6 0.026(4) 0.023(4) 0.025(4) 0.003(3) 0.006(3) -0.001(3) C7 0.033(4) 0.024(4) 0.019(4) -0.001(3) 0.013(3) 0.009(3) C8 0.022(3) 0.023(4) 0.011(3) 0.004(3) 0.005(3) -0.002(3) C9 0.030(4) 0.025(4) 0.033(4) -0.007(3) 0.010(3) -0.006(3) C10 0.026(4) 0.045(5) 0.036(5) -0.005(4) 0.007(3) -0.010(4) C11 0.023(4) 0.054(5) 0.032(4) -0.003(4) 0.007(3) 0.007(4) C12 0.028(4) 0.036(4) 0.025(4) -0.006(3) 0.005(3) 0.000(3) C13 0.025(4) 0.021(3) 0.008(3) 0.002(3) 0.006(3) 0.002(3) C14 0.023(4) 0.023(4) 0.014(3) -0.005(3) 0.014(3) 0.002(3) Zn1 0.0268(4) 0.0162(4) 0.0120(4) -0.0013(3) 0.0068(3) -0.0007(3) Zn3 0.0319(5) 0.0383(5) 0.0136(4) 0.0066(4) 0.0048(3) -0.0075(4) Zn2 0.0281(4) 0.0191(4) 0.0160(4) -0.0017(3) 0.0040(3) -0.0016(3) O1 0.022(2) 0.017(2) 0.015(2) -0.0036(18) 0.0060(18) -0.0038(19) O2 0.025(3) 0.020(2) 0.028(3) 0.006(2) 0.002(2) 0.002(2) O3 0.030(3) 0.029(3) 0.028(3) -0.016(2) 0.012(2) -0.005(2) O4 0.032(3) 0.027(3) 0.017(2) -0.002(2) 0.000(2) -0.007(2) O5 0.041(3) 0.050(3) 0.017(3) 0.005(2) 0.013(2) -0.003(3) O7 0.027(2) 0.024(2) 0.017(2) 0.0005(19) 0.0071(19) -0.009(2) O6 0.029(2) 0.015(2) 0.010(2) -0.0018(18) 0.0060(18) 0.0027(19) O8 0.034(3) 0.022(2) 0.011(2) -0.0052(19) 0.0067(19) 0.001(2) O9 0.026(3) 0.027(3) 0.019(3) -0.005(2) -0.002(2) 0.004(2) O10 0.040(3) 0.017(2) 0.016(2) 0.0029(19) 0.004(2) -0.005(2) O2W 0.038(3) 0.022(3) 0.038(3) 0.007(2) 0.016(2) 0.006(2) O3W 0.076(4) 0.047(4) 0.035(3) 0.006(3) 0.018(3) 0.014(3) O1W 0.042(3) 0.032(3) 0.027(3) 0.006(2) 0.004(2) 0.005(2) O4W 0.103(6) 0.076(5) 0.118(7) 0.051(5) -0.031(5) -0.031(5) P1 0.0249(9) 0.0169(9) 0.0166(9) -0.0022(7) 0.0079(7) -0.0030(7) P2 0.0222(9) 0.0168(8) 0.0097(8) 0.0000(6) 0.0053(7) -0.0001(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.378(9) . ? C1 C6 1.402(9) . ? C1 P1 1.795(7) . ? C2 C3 1.366(11) . ? C2 H2 0.9300 . ? C3 C4 1.360(11) . ? C3 H3 0.9300 . ? C4 C5 1.375(10) . ? C4 H4 0.9300 . ? C5 C6 1.372(10) . ? C5 H5 0.9300 . ? C6 C7 1.513(9) . ? C7 O5 1.251(8) . ? C7 O4 1.272(8) . ? C7 Zn3 2.497(7) . ? C8 C9 1.390(9) . ? C8 C13 1.394(9) . ? C8 P2 1.805(6) . ? C9 C10 1.367(10) . ? C9 H9 0.9300 . ? C10 C11 1.381(10) . ? C10 H10 0.9300 . ? C11 C12 1.396(10) . ? C11 H11 0.9300 . ? C12 C13 1.385(9) . ? C12 H12 0.9300 . ? C13 C14 1.489(9) . ? C14 O9 1.257(7) . ? C14 O10 1.257(7) . ? C14 Zn2 2.606(6) . ? Zn1 O1 2.084(4) . ? Zn1 O6 2.073(4) . ? Zn1 O1 2.104(4) 3_765 ? Zn1 O2W 2.099(4) . ? Zn1 O4 2.135(5) . ? Zn1 O9 2.127(4) . ? Zn3 O7 1.949(4) . ? Zn3 O8 1.945(4) 2_745 ? Zn3 O5 2.111(5) . ? Zn3 O3W 2.135(5) . ? Zn3 O4 2.212(4) . ? Zn3 O1W 2.316(5) . ? Zn2 O2 1.958(4) . ? Zn2 O3 1.960(4) 3_755 ? Zn2 O10 2.052(4) . ? Zn2 O6 2.087(4) 1_545 ? Zn2 O1W 2.330(5) . ? Zn2 O9 2.494(5) . ? O1 P1 1.525(4) . ? O1 Zn1 2.104(4) 3_765 ? O2 P1 1.525(5) . ? O3 P1 1.502(4) . ? O3 Zn2 1.960(4) 3_755 ? O7 P2 1.511(4) . ? O6 P2 1.550(4) . ? O6 Zn2 2.087(4) 1_565 ? O8 P2 1.510(4) . ? O8 Zn3 1.945(4) 2_755 ? O2W H2A 0.8506 . ? O2W H2B 0.8220 . ? O3W H3A 0.8539 . ? O3W H3B 0.8488 . ? O1W H1A 0.8514 . ? O1W H1B 0.8500 . ? O4W H4A 0.8515 . ? O4W H4B 0.8512 . ? 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 C2 C1 C6 117.1(6) . . ? C2 C1 P1 119.2(5) . . ? C6 C1 P1 122.9(5) . . ? C3 C2 C1 121.7(7) . . ? C3 C2 H2 119.1 . . ? C1 C2 H2 119.1 . . ? C4 C3 C2 121.3(7) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C3 C4 C5 118.1(7) . . ? C3 C4 H4 121.0 . . ? C5 C4 H4 121.0 . . ? C4 C5 C6 121.7(7) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C5 C6 C1 120.0(6) . . ? C5 C6 C7 117.7(6) . . ? C1 C6 C7 122.3(6) . . ? O5 C7 O4 119.8(6) . . ? O5 C7 C6 117.5(6) . . ? O4 C7 C6 122.7(6) . . ? O5 C7 Zn3 57.6(4) . . ? O4 C7 Zn3 62.2(3) . . ? C6 C7 Zn3 174.3(5) . . ? C9 C8 C13 118.8(6) . . ? C9 C8 P2 120.7(5) . . ? C13 C8 P2 120.4(5) . . ? C10 C9 C8 121.1(7) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C11 C10 C9 120.5(7) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C10 C11 C12 119.3(7) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? C13 C12 C11 120.1(7) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C8 120.2(6) . . ? C12 C13 C14 118.0(6) . . ? C8 C13 C14 121.8(6) . . ? O9 C14 O10 121.3(6) . . ? O9 C14 C13 120.4(6) . . ? O10 C14 C13 118.2(6) . . ? O9 C14 Zn2 70.8(3) . . ? O10 C14 Zn2 50.6(3) . . ? C13 C14 Zn2 168.0(4) . . ? O1 Zn1 O6 176.39(17) . . ? O1 Zn1 O1 80.08(17) . 3_765 ? O6 Zn1 O1 98.10(16) . 3_765 ? O1 Zn1 O2W 87.44(17) . . ? O6 Zn1 O2W 95.62(17) . . ? O1 Zn1 O2W 87.58(18) 3_765 . ? O1 Zn1 O4 90.55(16) . . ? O6 Zn1 O4 91.63(17) . . ? O1 Zn1 O4 168.32(16) 3_765 . ? O2W Zn1 O4 85.03(18) . . ? O1 Zn1 O9 83.87(16) . . ? O6 Zn1 O9 93.18(16) . . ? O1 Zn1 O9 94.11(17) 3_765 . ? O2W Zn1 O9 170.72(18) . . ? O4 Zn1 O9 91.78(17) . . ? O7 Zn3 O8 95.76(18) . 2_745 ? O7 Zn3 O5 151.29(18) . . ? O8 Zn3 O5 112.05(18) 2_745 . ? O7 Zn3 O3W 100.6(2) . . ? O8 Zn3 O3W 84.36(19) 2_745 . ? O5 Zn3 O3W 89.5(2) . . ? O7 Zn3 O4 91.34(17) . . ? O8 Zn3 O4 172.44(18) 2_745 . ? O5 Zn3 O4 60.60(17) . . ? O3W Zn3 O4 96.92(19) . . ? O7 Zn3 O1W 92.37(19) . . ? O8 Zn3 O1W 92.77(17) 2_745 . ? O5 Zn3 O1W 79.72(19) . . ? O3W Zn3 O1W 166.9(2) . . ? O4 Zn3 O1W 84.31(17) . . ? O7 Zn3 C7 121.6(2) . . ? O8 Zn3 C7 142.0(2) 2_745 . ? O5 Zn3 C7 30.04(19) . . ? O3W Zn3 C7 94.5(2) . . ? O4 Zn3 C7 30.58(18) . . ? O1W Zn3 C7 79.91(19) . . ? O2 Zn2 O3 102.6(2) . 3_755 ? O2 Zn2 O10 140.39(18) . . ? O3 Zn2 O10 93.25(18) 3_755 . ? O2 Zn2 O6 103.40(17) . 1_545 ? O3 Zn2 O6 92.61(18) 3_755 1_545 ? O10 Zn2 O6 111.99(16) . 1_545 ? O2 Zn2 O1W 82.25(18) . . ? O3 Zn2 O1W 174.58(18) 3_755 . ? O10 Zn2 O1W 81.40(18) . . ? O6 Zn2 O1W 88.62(16) 1_545 . ? O2 Zn2 O9 87.19(16) . . ? O3 Zn2 O9 89.00(17) 3_755 . ? O10 Zn2 O9 56.67(15) . . ? O6 Zn2 O9 168.64(15) 1_545 . ? O1W Zn2 O9 88.77(15) . . ? O2 Zn2 C14 114.51(19) . . ? O3 Zn2 C14 90.55(18) 3_755 . ? O10 Zn2 C14 28.25(18) . . ? O6 Zn2 C14 140.24(18) 1_545 . ? O1W Zn2 C14 85.14(18) . . ? O9 Zn2 C14 28.43(16) . . ? P1 O1 Zn1 125.0(2) . . ? P1 O1 Zn1 134.4(2) . 3_765 ? Zn1 O1 Zn1 99.92(17) . 3_765 ? P1 O2 Zn2 135.8(3) . . ? P1 O3 Zn2 138.7(3) . 3_755 ? C7 O4 Zn1 149.7(4) . . ? C7 O4 Zn3 87.2(4) . . ? Zn1 O4 Zn3 122.0(2) . . ? C7 O5 Zn3 92.3(4) . . ? P2 O7 Zn3 136.3(3) . . ? P2 O6 Zn1 120.9(2) . . ? P2 O6 Zn2 117.9(2) . 1_565 ? Zn1 O6 Zn2 118.04(18) . 1_565 ? P2 O8 Zn3 143.7(3) . 2_755 ? C14 O9 Zn1 145.8(4) . . ? C14 O9 Zn2 80.7(4) . . ? Zn1 O9 Zn2 121.61(19) . . ? C14 O10 Zn2 101.2(4) . . ? Zn1 O2W H2A 109.6 . . ? Zn1 O2W H2B 108.8 . . ? H2A O2W H2B 109.3 . . ? Zn3 O3W H3A 108.6 . . ? Zn3 O3W H3B 110.1 . . ? H3A O3W H3B 108.2 . . ? Zn3 O1W Zn2 128.8(2) . . ? Zn3 O1W H1A 106.4 . . ? Zn2 O1W H1A 104.3 . . ? Zn3 O1W H1B 105.2 . . ? Zn2 O1W H1B 104.5 . . ? H1A O1W H1B 105.8 . . ? H4A O4W H4B 109.7 . . ? O3 P1 O2 111.6(3) . . ? O3 P1 O1 112.3(3) . . ? O2 P1 O1 113.2(2) . . ? O3 P1 C1 105.7(3) . . ? O2 P1 C1 104.3(3) . . ? O1 P1 C1 109.2(3) . . ? O8 P2 O7 114.0(2) . . ? O8 P2 O6 108.4(2) . . ? O7 P2 O6 112.2(2) . . ? O8 P2 C8 107.2(3) . . ? O7 P2 C8 105.5(3) . . ? O6 P2 C8 109.4(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.934 _refine_diff_density_min -0.859 _refine_diff_density_rms 0.201