# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email zhxchen@fudan.edu.cn loop_ _publ_author_name 'Zhenxia Chen' 'Haiyang Yang' 'Mingli Deng' 'Yun Ling' 'Linhong Weng' 'Yaming Zhou' data_a01002b _database_code_depnum_ccdc_archive 'CCDC 850191' #TrackingRef 'a01002b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H15 N2 O6 P Zn' _chemical_formula_sum 'C17 H15 N2 O6 P Zn' _chemical_formula_weight 439.65 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 P2(1) _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.939(8) _cell_length_b 6.873(6) _cell_length_c 12.286(10) _cell_angle_alpha 90.00 _cell_angle_beta 93.407(11) _cell_angle_gamma 90.00 _cell_volume 837.8(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 798 _cell_measurement_theta_min 3.398 _cell_measurement_theta_max 26.713 _exptl_crystal_description sheet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.743 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 448 _exptl_absorpt_coefficient_mu 1.602 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7952 _exptl_absorpt_correction_T_max 0.9242 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _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 3448 _diffrn_reflns_av_R_equivalents 0.0579 _diffrn_reflns_av_sigmaI/netI 0.0527 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2560 _reflns_number_gt 2331 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.1923P)^2^+1.7005P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(7) _refine_ls_number_reflns 2560 _refine_ls_number_parameters 251 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0982 _refine_ls_R_factor_gt 0.0927 _refine_ls_wR_factor_ref 0.2536 _refine_ls_wR_factor_gt 0.2414 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.115 _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 Zn1 Zn 0.32556(11) 0.14093(17) 0.74874(8) 0.0242(4) Uani 1 1 d . . . P1 P 0.3707(3) 0.2960(5) 0.4980(2) 0.0210(6) Uani 1 1 d . . . O1 O 0.4804(8) 0.2471(13) 0.4238(7) 0.031(2) Uani 1 1 d . . . O2 O 0.3339(8) 0.5168(13) 0.4959(7) 0.034(2) Uani 1 1 d . . . H2A H 0.3976 0.5799 0.5227 0.051 Uiso 1 1 calc R . . O3 O 0.4015(9) 0.2204(14) 0.6101(7) 0.037(2) Uani 1 1 d . . . O4 O -0.2197(9) 0.0134(15) 0.2390(7) 0.039(2) Uani 1 1 d . . . O5 O -0.1349(9) -0.2694(13) 0.2890(8) 0.034(2) Uani 1 1 d . . . O6 O 0.3451(9) -0.1433(14) 0.7208(8) 0.034(2) Uani 1 1 d D . . H6A H 0.277(11) -0.213(19) 0.735(12) 0.051 Uiso 1 1 d D . . H6B H 0.379(13) -0.20(2) 0.667(9) 0.051 Uiso 1 1 d D . . N1 N 0.5220(9) 0.1607(19) 0.8301(7) 0.027(2) Uani 1 1 d . . . N2 N 0.2877(10) 0.135(2) 0.9211(7) 0.036(2) Uani 1 1 d . . . C1 C 0.6350(14) 0.174(3) 0.7760(11) 0.049(4) Uani 1 1 d . . . H1 H 0.6302 0.1983 0.7014 0.059 Uiso 1 1 calc R . . C2 C 0.7592(13) 0.149(5) 0.8325(12) 0.077(6) Uani 1 1 d . . . H2 H 0.8380 0.1475 0.7953 0.092 Uiso 1 1 calc R . . C3 C 0.7644(14) 0.128(4) 0.9463(12) 0.060(4) Uani 1 1 d . . . H3 H 0.8470 0.1182 0.9857 0.072 Uiso 1 1 calc R . . C4 C 0.6481(14) 0.121(3) 0.9983(10) 0.046(4) Uani 1 1 d . . . H4 H 0.6495 0.1007 1.0732 0.055 Uiso 1 1 calc R . . C5 C 0.5289(12) 0.144(2) 0.9388(8) 0.031(2) Uani 1 1 d . . . C6 C 0.3974(11) 0.130(2) 0.9896(8) 0.028(2) Uani 1 1 d . . . C7 C 0.3862(15) 0.137(3) 1.1032(9) 0.049(4) Uani 1 1 d . . . H7 H 0.4621 0.1496 1.1506 0.058 Uiso 1 1 calc R . . C8 C 0.2572(17) 0.123(4) 1.1427(12) 0.065(5) Uani 1 1 d . . . H8 H 0.2466 0.1113 1.2171 0.077 Uiso 1 1 calc R . . C9 C 0.1460(19) 0.128(6) 1.0700(13) 0.092(8) Uani 1 1 d . . . H9 H 0.0597 0.1386 1.0948 0.110 Uiso 1 1 calc R . . C10 C 0.1653(13) 0.117(3) 0.9601(11) 0.056(5) Uani 1 1 d . . . H10 H 0.0912 0.0974 0.9115 0.067 Uiso 1 1 calc R . . C11 C 0.2145(12) 0.188(2) 0.4387(10) 0.031(3) Uani 1 1 d . . . C12 C 0.1156(14) 0.297(3) 0.3892(12) 0.041(3) Uani 1 1 d . . . H12 H 0.1237 0.4317 0.3900 0.049 Uiso 1 1 calc R . . C13 C 0.0045(14) 0.2146(19) 0.3384(11) 0.029(3) Uani 1 1 d . . . H13 H -0.0602 0.2932 0.3027 0.035 Uiso 1 1 calc R . . C14 C -0.0133(11) 0.012(2) 0.3393(10) 0.026(3) Uani 1 1 d . . . C15 C 0.0910(13) -0.097(2) 0.3941(10) 0.034(3) Uani 1 1 d . . . H15 H 0.0857 -0.2317 0.3948 0.041 Uiso 1 1 calc R . . C16 C 0.2024(14) -0.004(2) 0.4476(11) 0.039(3) Uani 1 1 d . . . H16 H 0.2666 -0.0754 0.4885 0.047 Uiso 1 1 calc R . . C17 C -0.1301(13) -0.086(2) 0.2849(9) 0.030(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 Zn1 0.0336(7) 0.0184(7) 0.0200(6) 0.0009(6) -0.0040(4) -0.0002(6) P1 0.0210(13) 0.0158(14) 0.0259(15) 0.0017(11) 0.0003(10) -0.0019(11) O1 0.029(4) 0.037(6) 0.029(4) 0.011(4) 0.007(3) 0.003(4) O2 0.035(4) 0.018(5) 0.048(5) -0.010(4) -0.009(4) -0.003(4) O3 0.046(5) 0.042(6) 0.024(4) -0.004(4) 0.004(4) -0.005(4) O4 0.036(4) 0.035(6) 0.044(5) 0.001(4) -0.008(4) -0.006(4) O5 0.035(5) 0.023(5) 0.042(5) -0.008(4) -0.004(4) -0.011(4) O6 0.030(5) 0.023(5) 0.049(5) -0.003(4) 0.010(4) -0.002(3) N1 0.029(4) 0.029(6) 0.024(4) -0.004(5) -0.002(3) 0.001(5) N2 0.041(5) 0.045(6) 0.021(4) -0.014(6) -0.007(4) 0.003(7) C1 0.044(7) 0.070(13) 0.032(6) -0.010(8) -0.012(5) 0.000(8) C2 0.018(6) 0.16(2) 0.053(9) -0.002(15) 0.001(5) 0.006(12) C3 0.041(7) 0.085(14) 0.051(8) 0.007(12) -0.017(6) 0.003(10) C4 0.058(8) 0.043(10) 0.035(6) 0.009(8) -0.023(6) -0.014(8) C5 0.049(6) 0.015(5) 0.027(5) 0.000(6) -0.010(4) -0.011(7) C6 0.041(6) 0.019(6) 0.024(5) -0.006(6) -0.001(4) 0.008(6) C7 0.075(9) 0.049(9) 0.020(5) 0.010(8) -0.014(5) 0.028(10) C8 0.074(10) 0.086(15) 0.033(7) -0.010(10) 0.003(6) 0.028(11) C9 0.065(10) 0.17(3) 0.041(8) 0.036(16) 0.015(7) -0.001(18) C10 0.033(7) 0.091(15) 0.042(7) -0.010(9) -0.003(5) 0.013(9) C11 0.021(5) 0.049(11) 0.023(5) -0.006(6) -0.001(4) 0.003(5) C12 0.040(7) 0.038(9) 0.046(8) 0.012(7) 0.006(6) 0.000(6) C13 0.040(7) 0.021(6) 0.025(6) 0.004(5) -0.009(5) 0.006(5) C14 0.018(5) 0.032(7) 0.027(6) -0.004(5) 0.003(4) -0.005(5) C15 0.037(7) 0.028(8) 0.035(7) -0.003(6) -0.024(5) 0.007(6) C16 0.044(7) 0.039(8) 0.033(7) 0.007(7) -0.010(6) 0.002(7) C17 0.039(7) 0.029(7) 0.022(6) -0.002(5) -0.003(5) -0.004(6) _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 O3 1.981(9) . ? Zn1 O6 1.995(10) . ? Zn1 O5 2.020(9) 2_556 ? Zn1 N1 2.144(9) . ? Zn1 N2 2.173(9) . ? P1 O3 1.486(9) . ? P1 O1 1.501(9) . ? P1 O2 1.561(9) . ? P1 C11 1.832(12) . ? O2 H2A 0.8200 . ? O4 C17 1.233(16) . ? O5 C17 1.261(16) . ? O5 Zn1 2.020(9) 2_546 ? O6 H6A 0.86(2) . ? O6 H6B 0.85(2) . ? N1 C5 1.338(14) . ? N1 C1 1.342(18) . ? N2 C6 1.338(14) . ? N2 C10 1.339(17) . ? C1 C2 1.390(18) . ? C1 H1 0.9300 . ? C2 C3 1.40(2) . ? C2 H2 0.9300 . ? C3 C4 1.35(2) . ? C3 H3 0.9300 . ? C4 C5 1.363(17) . ? C4 H4 0.9300 . ? C5 C6 1.485(15) . ? C6 C7 1.407(16) . ? C7 C8 1.40(2) . ? C7 H7 0.9300 . ? C8 C9 1.38(2) . ? C8 H8 0.9300 . ? C9 C10 1.38(2) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C16 1.33(2) . ? C11 C12 1.35(2) . ? C12 C13 1.36(2) . ? C12 H12 0.9300 . ? C13 C14 1.40(2) . ? C13 H13 0.9300 . ? C14 C15 1.416(17) . ? C14 C17 1.470(16) . ? C15 C16 1.407(19) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? 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 O3 Zn1 O6 94.4(4) . . ? O3 Zn1 O5 96.8(4) . 2_556 ? O6 Zn1 O5 111.0(4) . 2_556 ? O3 Zn1 N1 90.1(4) . . ? O6 Zn1 N1 92.7(4) . . ? O5 Zn1 N1 154.6(4) 2_556 . ? O3 Zn1 N2 160.1(4) . . ? O6 Zn1 N2 100.0(5) . . ? O5 Zn1 N2 90.9(4) 2_556 . ? N1 Zn1 N2 75.7(3) . . ? O3 P1 O1 111.6(5) . . ? O3 P1 O2 113.0(5) . . ? O1 P1 O2 112.7(5) . . ? O3 P1 C11 110.5(6) . . ? O1 P1 C11 107.2(6) . . ? O2 P1 C11 101.2(6) . . ? P1 O2 H2A 109.5 . . ? P1 O3 Zn1 145.6(6) . . ? C17 O5 Zn1 109.4(8) . 2_546 ? Zn1 O6 H6A 115(10) . . ? Zn1 O6 H6B 128(10) . . ? H6A O6 H6B 105(3) . . ? C5 N1 C1 120.4(10) . . ? C5 N1 Zn1 116.8(7) . . ? C1 N1 Zn1 122.6(7) . . ? C6 N2 C10 119.8(10) . . ? C6 N2 Zn1 115.6(7) . . ? C10 N2 Zn1 124.3(8) . . ? N1 C1 C2 119.3(12) . . ? N1 C1 H1 120.4 . . ? C2 C1 H1 120.4 . . ? C1 C2 C3 119.3(13) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C4 C3 C2 119.4(12) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C3 C4 C5 118.8(12) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 122.5(11) . . ? N1 C5 C6 115.5(9) . . ? C4 C5 C6 121.7(10) . . ? N2 C6 C7 120.9(11) . . ? N2 C6 C5 116.0(9) . . ? C7 C6 C5 122.6(11) . . ? C8 C7 C6 118.0(12) . . ? C8 C7 H7 121.0 . . ? C6 C7 H7 121.0 . . ? C9 C8 C7 119.3(13) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C10 C9 C8 118.7(15) . . ? C10 C9 H9 120.6 . . ? C8 C9 H9 120.6 . . ? N2 C10 C9 121.9(13) . . ? N2 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? C16 C11 C12 121.2(14) . . ? C16 C11 P1 116.6(10) . . ? C12 C11 P1 122.2(12) . . ? C11 C12 C13 121.8(15) . . ? C11 C12 H12 119.1 . . ? C13 C12 H12 119.1 . . ? C12 C13 C14 120.6(13) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C13 C14 C15 116.0(11) . . ? C13 C14 C17 123.4(13) . . ? C15 C14 C17 120.5(13) . . ? C16 C15 C14 121.0(13) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C11 C16 C15 119.0(13) . . ? C11 C16 H16 120.5 . . ? C15 C16 H16 120.5 . . ? O4 C17 O5 123.0(12) . . ? O4 C17 C14 118.8(13) . . ? O5 C17 C14 118.2(12) . . ? _chemical_absolute_configuration unk _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 3.141 _refine_diff_density_min -1.202 _refine_diff_density_rms 0.255 # Attachment 'a01112a.cif' data_a01112a _database_code_depnum_ccdc_archive 'CCDC 850192' #TrackingRef 'a01112a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H25 N2 O15 P3 Zn2' _chemical_formula_sum 'C31 H25 N2 O15 P3 Zn2' _chemical_formula_weight 889.18 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 Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.488(3) _cell_length_b 11.944(4) _cell_length_c 17.641(5) _cell_angle_alpha 102.156(4) _cell_angle_beta 94.261(4) _cell_angle_gamma 90.904(4) _cell_volume 1742.7(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 968 _cell_measurement_theta_min 2.407 _cell_measurement_theta_max 27.114 _exptl_crystal_description sheet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.695 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 900 _exptl_absorpt_coefficient_mu 1.589 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7417 _exptl_absorpt_correction_T_max 0.9248 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _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 7220 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0382 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5989 _reflns_number_gt 4888 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0890P)^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 5989 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0538 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1255 _refine_ls_wR_factor_gt 0.1172 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 0.28376(4) 0.25369(3) 0.38869(2) 0.02638(14) Uani 1 1 d . . . Zn2 Zn 0.80655(4) 0.01463(3) 0.44749(2) 0.02515(13) Uani 1 1 d . . . P1 P 0.35516(10) 0.23080(8) 0.57194(5) 0.0263(2) Uani 1 1 d . . . P2 P 0.62700(10) 0.17982(7) 0.35775(5) 0.0243(2) Uani 1 1 d . . . P3 P 1.11792(10) 0.00543(7) 0.37852(5) 0.0231(2) Uani 1 1 d . . . O1 O 0.2389(3) 0.1454(2) 0.58938(14) 0.0396(6) Uani 1 1 d . . . O2 O 0.5201(3) 0.1758(3) 0.56351(15) 0.0512(8) Uani 1 1 d . . . H2B H 0.5395 0.1628 0.5177 0.077 Uiso 1 1 calc R . . O3 O 0.3087(3) 0.2864(2) 0.50604(13) 0.0393(6) Uani 1 1 d . . . O4 O 0.3896(6) 0.5789(4) 0.9283(2) 0.1023(16) Uani 1 1 d . . . H4B H 0.4112 0.6329 0.9651 0.154 Uiso 1 1 calc R . . O5 O 0.5501(5) 0.6777(3) 0.87182(18) 0.0781(12) Uani 1 1 d . . . O6 O 0.5064(3) 0.2701(2) 0.36354(14) 0.0303(5) Uani 1 1 d . . . O7 O 0.7918(3) 0.2390(2) 0.35224(14) 0.0339(6) Uani 1 1 d . . . H7B H 0.8628 0.1965 0.3607 0.051 Uiso 1 1 calc R . . O8 O 0.6366(3) 0.11697(19) 0.42415(12) 0.0271(5) Uani 1 1 d . . . O9 O 0.5957(5) -0.1567(3) -0.00262(18) 0.0789(12) Uani 1 1 d . . . H9B H 0.5766 -0.2113 -0.0392 0.118 Uiso 1 1 calc R . . O10 O 0.4387(6) -0.2601(3) 0.0542(2) 0.0979(15) Uani 1 1 d . . . O11 O 0.9606(3) 0.0678(2) 0.38375(13) 0.0299(5) Uani 1 1 d . . . O12 O 1.2526(3) 0.0855(2) 0.37189(14) 0.0317(6) Uani 1 1 d . . . O13 O 1.1420(3) -0.0593(2) 0.44311(13) 0.0315(6) Uani 1 1 d . . . O14 O 0.9419(5) -0.3648(3) 0.03263(19) 0.0790(12) Uani 1 1 d . . . N1 N 0.1787(3) 0.4146(3) 0.39626(17) 0.0333(7) Uani 1 1 d . . . N2 N 0.1701(4) 0.2475(3) 0.27200(18) 0.0372(7) Uani 1 1 d . . . C1 C 0.1956(5) 0.4986(3) 0.4605(2) 0.0427(9) Uani 1 1 d . . . H1A H 0.2538 0.4854 0.5044 0.051 Uiso 1 1 calc R . . C2 C 0.1292(5) 0.6042(4) 0.4634(3) 0.0513(11) Uani 1 1 d . . . H2A H 0.1445 0.6616 0.5082 0.062 Uiso 1 1 calc R . . C3 C 0.0405(5) 0.6233(4) 0.3995(3) 0.0543(12) Uani 1 1 d . . . H3A H -0.0057 0.6936 0.4005 0.065 Uiso 1 1 calc R . . C4 C 0.0209(5) 0.5374(4) 0.3341(3) 0.0506(11) Uani 1 1 d . . . H4A H -0.0405 0.5485 0.2905 0.061 Uiso 1 1 calc R . . C5 C 0.0935(4) 0.4333(3) 0.3333(2) 0.0357(8) Uani 1 1 d . . . C6 C 0.0866(4) 0.3379(4) 0.2637(2) 0.0386(9) Uani 1 1 d . . . C7 C 0.0054(6) 0.3425(5) 0.1933(3) 0.0646(14) Uani 1 1 d . . . H7A H -0.0544 0.4055 0.1882 0.078 Uiso 1 1 calc R . . C8 C 0.0151(7) 0.2519(5) 0.1311(3) 0.0748(16) Uani 1 1 d . . . H8A H -0.0371 0.2540 0.0832 0.090 Uiso 1 1 calc R . . C9 C 0.1002(7) 0.1601(5) 0.1394(3) 0.0658(14) Uani 1 1 d . . . H9A H 0.1072 0.0984 0.0978 0.079 Uiso 1 1 calc R . . C10 C 0.1766(5) 0.1601(4) 0.2113(2) 0.0500(11) Uani 1 1 d . . . H10A H 0.2346 0.0969 0.2176 0.060 Uiso 1 1 calc R . . C11 C 0.4613(6) 0.5936(4) 0.8702(2) 0.0498(11) Uani 1 1 d . . . C12 C 0.4348(5) 0.5050(3) 0.7978(2) 0.0393(9) Uani 1 1 d . . . C13 C 0.4917(5) 0.5231(3) 0.7299(2) 0.0462(10) Uani 1 1 d . . . H13A H 0.5465 0.5912 0.7299 0.055 Uiso 1 1 calc R . . C14 C 0.4677(5) 0.4409(3) 0.6620(2) 0.0420(10) Uani 1 1 d . . . H14A H 0.5071 0.4540 0.6167 0.050 Uiso 1 1 calc R . . C15 C 0.3860(4) 0.3393(3) 0.66033(19) 0.0287(8) Uani 1 1 d . . . C16 C 0.3249(4) 0.3214(3) 0.7287(2) 0.0353(8) Uani 1 1 d . . . H16A H 0.2673 0.2544 0.7282 0.042 Uiso 1 1 calc R . . C17 C 0.3503(5) 0.4032(3) 0.7966(2) 0.0407(9) Uani 1 1 d . . . H17A H 0.3109 0.3906 0.8420 0.049 Uiso 1 1 calc R . . C18 C 0.5951(4) 0.0761(3) 0.2676(2) 0.0290(8) Uani 1 1 d . . . C19 C 0.6445(5) 0.1005(4) 0.1990(2) 0.0439(10) Uani 1 1 d . . . H19A H 0.6923 0.1713 0.1997 0.053 Uiso 1 1 calc R . . C20 C 0.6227(6) 0.0199(4) 0.1301(2) 0.0496(11) Uani 1 1 d . . . H20A H 0.6588 0.0360 0.0850 0.059 Uiso 1 1 calc R . . C21 C 0.5480(5) -0.0839(4) 0.1279(2) 0.0426(10) Uani 1 1 d . . . C22 C 0.4962(5) -0.1088(3) 0.1958(2) 0.0418(9) Uani 1 1 d . . . H22A H 0.4448 -0.1787 0.1943 0.050 Uiso 1 1 calc R . . C23 C 0.5212(4) -0.0298(3) 0.2655(2) 0.0348(8) Uani 1 1 d . . . H23A H 0.4886 -0.0472 0.3109 0.042 Uiso 1 1 calc R . . C24 C 0.5244(6) -0.1725(4) 0.0554(2) 0.0560(12) Uani 1 1 d . . . C25 C 1.0963(4) -0.1062(3) 0.29095(19) 0.0273(7) Uani 1 1 d . . . C26 C 0.9906(5) -0.0967(3) 0.2284(2) 0.0384(9) Uani 1 1 d . . . H26A H 0.9306 -0.0317 0.2313 0.046 Uiso 1 1 calc R . . C27 C 0.9741(5) -0.1831(3) 0.1622(2) 0.0424(10) Uani 1 1 d . . . H27A H 0.9035 -0.1757 0.1207 0.051 Uiso 1 1 calc R . . C28 C 1.0620(5) -0.2806(3) 0.1574(2) 0.0380(9) Uani 1 1 d . . . C29 C 1.1682(5) -0.2909(3) 0.2193(2) 0.0371(9) Uani 1 1 d . . . H29A H 1.2285 -0.3558 0.2161 0.045 Uiso 1 1 calc R . . C30 C 1.1841(4) -0.2045(3) 0.2855(2) 0.0322(8) Uani 1 1 d . . . H30A H 1.2543 -0.2123 0.3270 0.039 Uiso 1 1 calc R . . C31 C 1.0394(6) -0.3744(4) 0.0874(2) 0.0488(11) Uani 1 1 d . . . O15 O 1.1217(5) -0.4633(3) 0.08739(19) 0.0814(12) Uani 1 1 d . . . H15A H 1.0949 -0.5124 0.0484 0.122 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 0.0288(2) 0.0269(2) 0.0237(2) 0.00593(16) 0.00132(16) 0.00277(16) Zn2 0.0286(2) 0.0251(2) 0.0217(2) 0.00483(16) 0.00149(16) 0.00262(16) P1 0.0318(5) 0.0260(5) 0.0200(4) 0.0024(3) 0.0022(4) 0.0035(4) P2 0.0267(4) 0.0237(5) 0.0228(4) 0.0053(3) 0.0030(3) 0.0011(3) P3 0.0252(4) 0.0243(5) 0.0189(4) 0.0022(3) 0.0027(3) 0.0011(3) O1 0.0540(16) 0.0290(14) 0.0334(14) 0.0001(11) 0.0091(12) -0.0084(12) O2 0.0455(16) 0.081(2) 0.0264(14) 0.0079(14) 0.0048(12) 0.0298(15) O3 0.0577(17) 0.0382(15) 0.0211(12) 0.0043(11) 0.0005(11) 0.0104(13) O4 0.153(4) 0.095(3) 0.042(2) -0.0306(19) 0.037(2) -0.054(3) O5 0.130(3) 0.054(2) 0.0422(19) -0.0063(15) 0.0080(19) -0.036(2) O6 0.0292(12) 0.0284(13) 0.0355(13) 0.0112(11) 0.0048(10) 0.0023(10) O7 0.0306(13) 0.0351(14) 0.0373(14) 0.0096(11) 0.0059(11) -0.0018(11) O8 0.0286(12) 0.0318(13) 0.0224(11) 0.0087(10) 0.0029(9) 0.0056(10) O9 0.132(3) 0.065(2) 0.0309(17) -0.0107(15) 0.0171(19) -0.016(2) O10 0.142(4) 0.080(3) 0.055(2) -0.0273(19) 0.030(2) -0.053(3) O11 0.0278(12) 0.0333(14) 0.0297(13) 0.0073(10) 0.0068(10) 0.0061(10) O12 0.0300(13) 0.0295(13) 0.0340(13) 0.0016(10) 0.0070(10) -0.0021(10) O13 0.0423(14) 0.0318(14) 0.0192(12) 0.0028(10) 0.0008(10) 0.0028(11) O14 0.132(3) 0.052(2) 0.0394(19) -0.0108(15) -0.026(2) 0.009(2) N1 0.0369(17) 0.0309(17) 0.0340(17) 0.0108(13) 0.0042(13) 0.0041(13) N2 0.0397(17) 0.0357(18) 0.0363(17) 0.0100(14) -0.0024(14) 0.0009(14) C1 0.052(2) 0.039(2) 0.037(2) 0.0054(17) 0.0051(18) 0.0034(18) C2 0.059(3) 0.036(2) 0.059(3) 0.005(2) 0.016(2) 0.005(2) C3 0.058(3) 0.038(2) 0.074(3) 0.023(2) 0.019(2) 0.020(2) C4 0.047(2) 0.053(3) 0.060(3) 0.029(2) 0.001(2) 0.014(2) C5 0.0319(19) 0.037(2) 0.044(2) 0.0200(17) 0.0055(16) 0.0022(16) C6 0.036(2) 0.049(2) 0.035(2) 0.0208(18) -0.0019(16) 0.0004(18) C7 0.083(4) 0.067(3) 0.048(3) 0.027(2) -0.015(3) 0.011(3) C8 0.109(5) 0.078(4) 0.039(3) 0.028(3) -0.021(3) -0.014(3) C9 0.091(4) 0.071(4) 0.032(2) 0.007(2) -0.003(2) -0.010(3) C10 0.061(3) 0.051(3) 0.034(2) 0.0033(19) 0.000(2) 0.003(2) C11 0.071(3) 0.042(3) 0.032(2) -0.0014(18) 0.006(2) -0.007(2) C12 0.054(2) 0.032(2) 0.0288(19) -0.0010(16) 0.0006(17) 0.0001(18) C13 0.068(3) 0.033(2) 0.036(2) 0.0043(17) 0.0056(19) -0.021(2) C14 0.059(3) 0.040(2) 0.0260(19) 0.0061(16) 0.0077(18) -0.0147(19) C15 0.0335(18) 0.0292(19) 0.0225(17) 0.0043(14) -0.0004(14) 0.0027(15) C16 0.049(2) 0.029(2) 0.0274(18) 0.0045(15) 0.0080(16) -0.0067(16) C17 0.058(2) 0.040(2) 0.0251(19) 0.0058(16) 0.0099(17) -0.0003(19) C18 0.0325(18) 0.0287(19) 0.0253(17) 0.0043(14) 0.0018(14) 0.0041(15) C19 0.066(3) 0.037(2) 0.029(2) 0.0073(16) 0.0063(18) -0.0066(19) C20 0.080(3) 0.046(3) 0.025(2) 0.0089(17) 0.0121(19) -0.006(2) C21 0.053(2) 0.041(2) 0.030(2) 0.0002(17) 0.0003(18) 0.0037(19) C22 0.049(2) 0.035(2) 0.038(2) -0.0015(17) 0.0063(18) -0.0054(18) C23 0.040(2) 0.034(2) 0.0303(19) 0.0030(15) 0.0080(16) -0.0003(16) C24 0.073(3) 0.056(3) 0.032(2) -0.006(2) 0.005(2) 0.001(2) C25 0.0317(18) 0.0282(19) 0.0218(16) 0.0044(14) 0.0043(14) -0.0041(14) C26 0.045(2) 0.037(2) 0.0311(19) 0.0022(16) -0.0026(17) 0.0065(17) C27 0.054(2) 0.043(2) 0.0275(19) 0.0041(17) -0.0080(17) 0.0004(19) C28 0.055(2) 0.032(2) 0.0249(18) 0.0013(15) 0.0048(17) -0.0066(18) C29 0.050(2) 0.027(2) 0.033(2) 0.0024(15) 0.0036(17) 0.0031(16) C30 0.039(2) 0.030(2) 0.0252(18) 0.0015(14) -0.0006(15) 0.0020(15) C31 0.075(3) 0.037(2) 0.030(2) -0.0009(17) 0.001(2) -0.004(2) O15 0.137(4) 0.045(2) 0.049(2) -0.0134(16) -0.019(2) 0.019(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 O12 1.979(2) 1_455 ? Zn1 O6 1.989(2) . ? Zn1 O3 2.019(2) . ? Zn1 N1 2.114(3) . ? Zn1 N2 2.194(3) . ? Zn2 O13 1.906(2) 2_756 ? Zn2 O1 1.908(3) 2_656 ? Zn2 O11 1.967(2) . ? Zn2 O8 1.981(2) . ? P1 O3 1.487(3) . ? P1 O1 1.502(3) . ? P1 O2 1.560(3) . ? P1 C15 1.805(3) . ? P2 O6 1.492(2) . ? P2 O8 1.517(2) . ? P2 O7 1.576(2) . ? P2 C18 1.798(3) . ? P3 O12 1.506(2) . ? P3 O13 1.510(3) . ? P3 O11 1.539(2) . ? P3 C25 1.811(3) . ? O1 Zn2 1.908(3) 2_656 ? O2 H2B 0.8200 . ? O4 C11 1.270(5) . ? O4 H4B 0.8200 . ? O5 C11 1.241(5) . ? O7 H7B 0.8200 . ? O9 C24 1.273(6) . ? O9 H9B 0.8200 . ? O10 C24 1.260(6) . ? O12 Zn1 1.979(2) 1_655 ? O13 Zn2 1.906(2) 2_756 ? O14 C31 1.251(5) . ? N1 C5 1.340(5) . ? N1 C1 1.343(5) . ? N2 C6 1.328(5) . ? N2 C10 1.335(5) . ? C1 C2 1.382(6) . ? C1 H1A 0.9300 . ? C2 C3 1.370(6) . ? C2 H2A 0.9300 . ? C3 C4 1.371(6) . ? C3 H3A 0.9300 . ? C4 C5 1.395(5) . ? C4 H4A 0.9300 . ? C5 C6 1.487(5) . ? C6 C7 1.386(6) . ? C7 C8 1.378(7) . ? C7 H7A 0.9300 . ? C8 C9 1.351(8) . ? C8 H8A 0.9300 . ? C9 C10 1.380(6) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.478(5) . ? C12 C13 1.381(5) . ? C12 C17 1.398(6) . ? C13 C14 1.379(5) . ? C13 H13A 0.9300 . ? C14 C15 1.382(5) . ? C14 H14A 0.9300 . ? C15 C16 1.403(5) . ? C16 C17 1.377(5) . ? C16 H16A 0.9300 . ? C17 H17A 0.9300 . ? C18 C23 1.394(5) . ? C18 C19 1.395(5) . ? C19 C20 1.380(5) . ? C19 H19A 0.9300 . ? C20 C21 1.376(6) . ? C20 H20A 0.9300 . ? C21 C22 1.393(6) . ? C21 C24 1.477(5) . ? C22 C23 1.383(5) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C25 C30 1.391(5) . ? C25 C26 1.394(5) . ? C26 C27 1.383(5) . ? C26 H26A 0.9300 . ? C27 C28 1.384(6) . ? C27 H27A 0.9300 . ? C28 C29 1.391(5) . ? C28 C31 1.480(5) . ? C29 C30 1.383(5) . ? C29 H29A 0.9300 . ? C30 H30A 0.9300 . ? C31 O15 1.279(5) . ? O15 H15A 0.8200 . ? 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 O12 Zn1 O6 102.39(9) 1_455 . ? O12 Zn1 O3 97.18(10) 1_455 . ? O6 Zn1 O3 101.31(10) . . ? O12 Zn1 N1 147.46(11) 1_455 . ? O6 Zn1 N1 107.93(11) . . ? O3 Zn1 N1 88.35(11) . . ? O12 Zn1 N2 89.41(11) 1_455 . ? O6 Zn1 N2 97.69(11) . . ? O3 Zn1 N2 158.00(11) . . ? N1 Zn1 N2 75.25(12) . . ? O13 Zn2 O1 114.38(11) 2_756 2_656 ? O13 Zn2 O11 114.55(10) 2_756 . ? O1 Zn2 O11 109.91(10) 2_656 . ? O13 Zn2 O8 105.33(10) 2_756 . ? O1 Zn2 O8 115.51(11) 2_656 . ? O11 Zn2 O8 95.80(10) . . ? O3 P1 O1 116.90(16) . . ? O3 P1 O2 111.70(16) . . ? O1 P1 O2 109.37(17) . . ? O3 P1 C15 109.22(16) . . ? O1 P1 C15 105.34(15) . . ? O2 P1 C15 103.26(15) . . ? O6 P2 O8 114.80(13) . . ? O6 P2 O7 107.40(14) . . ? O8 P2 O7 110.19(13) . . ? O6 P2 C18 111.16(15) . . ? O8 P2 C18 108.57(15) . . ? O7 P2 C18 104.19(15) . . ? O12 P3 O13 115.30(14) . . ? O12 P3 O11 111.22(14) . . ? O13 P3 O11 110.53(14) . . ? O12 P3 C25 108.58(14) . . ? O13 P3 C25 103.90(15) . . ? O11 P3 C25 106.69(15) . . ? P1 O1 Zn2 135.41(16) . 2_656 ? P1 O2 H2B 109.5 . . ? P1 O3 Zn1 141.38(16) . . ? C11 O4 H4B 109.5 . . ? P2 O6 Zn1 126.10(14) . . ? P2 O7 H7B 109.5 . . ? P2 O8 Zn2 126.22(13) . . ? C24 O9 H9B 109.5 . . ? P3 O11 Zn2 116.17(14) . . ? P3 O12 Zn1 135.22(15) . 1_655 ? P3 O13 Zn2 133.98(15) . 2_756 ? C5 N1 C1 119.0(3) . . ? C5 N1 Zn1 117.9(2) . . ? C1 N1 Zn1 123.0(3) . . ? C6 N2 C10 119.3(4) . . ? C6 N2 Zn1 115.8(3) . . ? C10 N2 Zn1 124.9(3) . . ? N1 C1 C2 122.0(4) . . ? N1 C1 H1A 119.0 . . ? C2 C1 H1A 119.0 . . ? C3 C2 C1 119.2(4) . . ? C3 C2 H2A 120.4 . . ? C1 C2 H2A 120.4 . . ? C2 C3 C4 119.1(4) . . ? C2 C3 H3A 120.4 . . ? C4 C3 H3A 120.4 . . ? C3 C4 C5 119.5(4) . . ? C3 C4 H4A 120.2 . . ? C5 C4 H4A 120.2 . . ? N1 C5 C4 121.1(4) . . ? N1 C5 C6 115.6(3) . . ? C4 C5 C6 123.3(4) . . ? N2 C6 C7 121.2(4) . . ? N2 C6 C5 115.2(3) . . ? C7 C6 C5 123.5(4) . . ? C8 C7 C6 118.6(5) . . ? C8 C7 H7A 120.7 . . ? C6 C7 H7A 120.7 . . ? C9 C8 C7 120.2(4) . . ? C9 C8 H8A 119.9 . . ? C7 C8 H8A 119.9 . . ? C8 C9 C10 118.3(5) . . ? C8 C9 H9A 120.9 . . ? C10 C9 H9A 120.9 . . ? N2 C10 C9 122.4(5) . . ? N2 C10 H10A 118.8 . . ? C9 C10 H10A 118.8 . . ? O5 C11 O4 123.3(4) . . ? O5 C11 C12 119.5(4) . . ? O4 C11 C12 117.2(4) . . ? C13 C12 C17 119.2(3) . . ? C13 C12 C11 120.0(4) . . ? C17 C12 C11 120.8(4) . . ? C14 C13 C12 120.4(4) . . ? C14 C13 H13A 119.8 . . ? C12 C13 H13A 119.8 . . ? C13 C14 C15 120.9(3) . . ? C13 C14 H14A 119.5 . . ? C15 C14 H14A 119.5 . . ? C14 C15 C16 119.0(3) . . ? C14 C15 P1 121.2(3) . . ? C16 C15 P1 119.8(3) . . ? C17 C16 C15 120.0(3) . . ? C17 C16 H16A 120.0 . . ? C15 C16 H16A 120.0 . . ? C16 C17 C12 120.5(3) . . ? C16 C17 H17A 119.8 . . ? C12 C17 H17A 119.8 . . ? C23 C18 C19 119.2(3) . . ? C23 C18 P2 120.4(3) . . ? C19 C18 P2 120.3(3) . . ? C20 C19 C18 120.3(4) . . ? C20 C19 H19A 119.9 . . ? C18 C19 H19A 119.9 . . ? C21 C20 C19 120.5(4) . . ? C21 C20 H20A 119.8 . . ? C19 C20 H20A 119.8 . . ? C20 C21 C22 119.8(3) . . ? C20 C21 C24 121.9(4) . . ? C22 C21 C24 118.3(4) . . ? C23 C22 C21 120.1(4) . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C22 C23 C18 120.1(3) . . ? C22 C23 H23A 120.0 . . ? C18 C23 H23A 120.0 . . ? O10 C24 O9 123.4(4) . . ? O10 C24 C21 119.2(4) . . ? O9 C24 C21 117.3(4) . . ? C30 C25 C26 118.7(3) . . ? C30 C25 P3 120.1(3) . . ? C26 C25 P3 121.2(3) . . ? C27 C26 C25 120.6(4) . . ? C27 C26 H26A 119.7 . . ? C25 C26 H26A 119.7 . . ? C26 C27 C28 120.3(4) . . ? C26 C27 H27A 119.9 . . ? C28 C27 H27A 119.9 . . ? C27 C28 C29 119.6(3) . . ? C27 C28 C31 119.9(4) . . ? C29 C28 C31 120.5(4) . . ? C30 C29 C28 120.0(3) . . ? C30 C29 H29A 120.0 . . ? C28 C29 H29A 120.0 . . ? C29 C30 C25 120.8(3) . . ? C29 C30 H30A 119.6 . . ? C25 C30 H30A 119.6 . . ? O14 C31 O15 123.4(4) . . ? O14 C31 C28 119.8(4) . . ? O15 C31 C28 116.8(4) . . ? C31 O15 H15A 109.5 . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.875 _refine_diff_density_min -0.918 _refine_diff_density_rms 0.138 # Attachment 'a01117c.cif' data_a01117c _database_code_depnum_ccdc_archive 'CCDC 850193' #TrackingRef 'a01117c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H18 N2 O11 P2 Zn3, (H2 O)' _chemical_formula_sum 'C24 H18 N2 O12 P2 Zn3' _chemical_formula_weight 784.45 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 Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.299(3) _cell_length_b 14.826(4) _cell_length_c 19.221(6) _cell_angle_alpha 88.308(4) _cell_angle_beta 86.341(5) _cell_angle_gamma 74.338(4) _cell_volume 2819.9(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 802 _cell_measurement_theta_min 2.350 _cell_measurement_theta_max 25.957 _exptl_crystal_description column _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.848 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 2.712 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7367 _exptl_absorpt_correction_T_max 0.8763 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _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 11692 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_sigmaI/netI 0.0852 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9726 _reflns_number_gt 6578 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0519P)^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 9726 _refine_ls_number_parameters 775 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0722 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1215 _refine_ls_wR_factor_gt 0.1023 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.944 _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 -0.39958(7) 0.42265(5) 0.57046(3) 0.02017(17) Uani 1 1 d . . . Zn2 Zn 0.17807(7) 0.24573(5) 0.48816(4) 0.02708(19) Uani 1 1 d . . . Zn3 Zn 0.11170(7) 0.43895(4) 0.57020(3) 0.02140(17) Uani 1 1 d . . . Zn4 Zn -0.31380(7) 0.92989(5) 0.93303(3) 0.02120(17) Uani 1 1 d . . . Zn5 Zn 0.19512(7) 0.93553(5) 0.92815(3) 0.02122(17) Uani 1 1 d . . . Zn6 Zn 0.18580(8) 0.74424(5) 1.01141(4) 0.02787(19) Uani 1 1 d . . . P1 P -0.20143(15) 0.55524(10) 0.58410(8) 0.0184(3) Uani 1 1 d . . . P2 P 0.31256(15) 0.55812(10) 0.58083(8) 0.0190(3) Uani 1 1 d . . . P3 P 0.39708(16) 0.05361(11) 0.91235(8) 0.0207(3) Uani 1 1 d . . . P4 P -0.10486(15) 1.05613(10) 0.91777(8) 0.0188(3) Uani 1 1 d . . . O1 O -0.3326(4) 0.5303(3) 0.5858(2) 0.0277(10) Uani 1 1 d . . . O2 O -0.1833(4) 0.6191(3) 0.5209(2) 0.0243(10) Uani 1 1 d . . . O3 O -0.0802(4) 0.4705(3) 0.5852(2) 0.0239(9) Uani 1 1 d . . . O4 O -0.0253(4) 0.2873(3) 0.4890(2) 0.0343(11) Uani 1 1 d . . . O5 O 0.1965(5) 0.2163(3) 0.5911(2) 0.0424(13) Uani 1 1 d . . . O6 O 0.1805(4) 0.3497(3) 0.6438(2) 0.0384(12) Uani 1 1 d . . . O7 O 0.3186(4) 0.1145(3) 0.9714(2) 0.0295(10) Uani 1 1 d . . . O8 O 0.5472(4) 0.0413(3) 0.9121(2) 0.0298(10) Uani 1 1 d . . . O9 O 0.3650(4) -0.0404(3) 0.9105(2) 0.0257(10) Uani 1 1 d . . . O10 O 0.1673(4) 0.5525(3) 0.5730(2) 0.0207(9) Uani 1 1 d . . . O11 O 0.3540(4) 0.6189(3) 0.5245(2) 0.0240(9) Uani 1 1 d . . . O12 O 0.4050(4) 0.4619(3) 0.5870(2) 0.0229(9) Uani 1 1 d . . . O13 O 0.2237(5) 0.7047(3) 0.9129(2) 0.0455(13) Uani 1 1 d . . . O14 O 0.1981(5) 0.8432(3) 0.8579(2) 0.0463(13) Uani 1 1 d . . . O15 O -0.0222(4) 0.7757(3) 1.0066(2) 0.0353(11) Uani 1 1 d . . . O16 O 0.0451(4) 1.0439(3) 0.9209(2) 0.0224(9) Uani 1 1 d . . . O17 O -0.1831(4) 1.1213(2) 0.97701(19) 0.0213(9) Uani 1 1 d . . . O18 O -0.1428(4) 0.9651(3) 0.9199(2) 0.0245(9) Uani 1 1 d . . . O19 O -0.3502(5) 1.3297(3) 0.6443(2) 0.0449(13) Uani 1 1 d . . . O20 O -0.1676(5) 1.2367(4) 0.5930(2) 0.0484(13) Uani 1 1 d . . . O21 O -0.3098(5) 0.8376(3) 0.8634(2) 0.0393(12) Uani 1 1 d . . . O22 O -0.1136(5) 0.7400(4) 0.8876(2) 0.0543(15) Uani 1 1 d . . . N1 N 0.1928(6) 0.1515(4) 0.4071(3) 0.0365(14) Uani 1 1 d . . . N2 N 0.3868(5) 0.1875(4) 0.4704(3) 0.0367(14) Uani 1 1 d . . . N3 N 0.1886(7) 0.6533(4) 1.0947(3) 0.0451(16) Uani 1 1 d . . . N4 N 0.3979(5) 0.6916(4) 1.0261(3) 0.0364(14) Uani 1 1 d . . . C1 C -0.2054(6) 0.6233(4) 0.6602(3) 0.0201(13) Uani 1 1 d . . . C2 C -0.3266(6) 0.6758(4) 0.6916(3) 0.0298(15) Uani 1 1 d . . . H2 H -0.4071 0.6782 0.6713 0.036 Uiso 1 1 calc R . . C3 C -0.3301(6) 0.7247(4) 0.7524(3) 0.0324(16) Uani 1 1 d . . . H3 H -0.4118 0.7609 0.7719 0.039 Uiso 1 1 calc R . . C4 C -0.2108(7) 0.7190(4) 0.7837(3) 0.0284(15) Uani 1 1 d . . . C5 C -0.0923(6) 0.6682(5) 0.7535(3) 0.0369(17) Uani 1 1 d . . . H5 H -0.0125 0.6642 0.7750 0.044 Uiso 1 1 calc R . . C6 C -0.0872(6) 0.6220(5) 0.6910(3) 0.0332(16) Uani 1 1 d . . . H6 H -0.0042 0.5902 0.6700 0.040 Uiso 1 1 calc R . . C7 C -0.2120(7) 0.7700(5) 0.8508(3) 0.0329(16) Uani 1 1 d . . . C8 C 0.3004(6) 0.6175(4) 0.6630(3) 0.0238(14) Uani 1 1 d . . . C9 C 0.2901(7) 0.7109(4) 0.6668(3) 0.0321(16) Uani 1 1 d . . . H9 H 0.2997 0.7448 0.6262 0.038 Uiso 1 1 calc R . . C10 C 0.2654(7) 0.7558(5) 0.7306(3) 0.0392(18) Uani 1 1 d . . . H10 H 0.2582 0.8196 0.7323 0.047 Uiso 1 1 calc R . . C11 C 0.2515(6) 0.7067(4) 0.7912(3) 0.0258(14) Uani 1 1 d . . . C12 C 0.2642(7) 0.6132(4) 0.7877(3) 0.0341(16) Uani 1 1 d . . . H12 H 0.2542 0.5795 0.8283 0.041 Uiso 1 1 calc R . . C13 C 0.2923(7) 0.5667(4) 0.7237(3) 0.0336(16) Uani 1 1 d . . . H13 H 0.3054 0.5023 0.7222 0.040 Uiso 1 1 calc R . . C14 C 0.2228(7) 0.7554(5) 0.8596(3) 0.0356(17) Uani 1 1 d . . . C15 C 0.3425(6) 0.1147(4) 0.8320(3) 0.0219(13) Uani 1 1 d . . . C16 C 0.3192(6) 0.0680(4) 0.7752(3) 0.0291(15) Uani 1 1 d . . . H16 H 0.3312 0.0036 0.7786 0.035 Uiso 1 1 calc R . . C17 C 0.2785(6) 0.1137(4) 0.7137(3) 0.0292(15) Uani 1 1 d . . . H17 H 0.2671 0.0797 0.6757 0.035 Uiso 1 1 calc R . . C18 C 0.2543(6) 0.2109(5) 0.7081(3) 0.0290(15) Uani 1 1 d . . . C19 C 0.2761(7) 0.2601(5) 0.7651(3) 0.0407(18) Uani 1 1 d . . . H19 H 0.2607 0.3248 0.7625 0.049 Uiso 1 1 calc R . . C20 C 0.3206(8) 0.2117(5) 0.8253(3) 0.045(2) Uani 1 1 d . . . H20 H 0.3367 0.2448 0.8627 0.055 Uiso 1 1 calc R . . C21 C 0.2054(6) 0.2626(5) 0.6427(3) 0.0324(16) Uani 1 1 d . . . C22 C -0.1520(6) 1.1195(4) 0.8381(3) 0.0207(13) Uani 1 1 d . . . C23 C -0.0483(7) 1.1172(5) 0.7860(3) 0.0391(18) Uani 1 1 d . . . H23 H 0.0407 1.0853 0.7938 0.047 Uiso 1 1 calc R . . C24 C -0.0811(7) 1.1630(5) 0.7237(3) 0.0436(19) Uani 1 1 d . . . H24 H -0.0134 1.1609 0.6888 0.052 Uiso 1 1 calc R . . C25 C -0.2142(6) 1.2127(4) 0.7116(3) 0.0258(14) Uani 1 1 d . . . C26 C -0.3131(6) 1.2128(4) 0.7631(3) 0.0295(15) Uani 1 1 d . . . H26 H -0.4020 1.2455 0.7560 0.035 Uiso 1 1 calc R . . C27 C -0.2822(6) 1.1650(4) 0.8254(3) 0.0266(14) Uani 1 1 d . . . H27 H -0.3510 1.1639 0.8589 0.032 Uiso 1 1 calc R . . C28 C -0.2418(6) 1.2616(5) 0.6435(3) 0.0315(15) Uani 1 1 d . . . C29 C 0.0876(9) 0.1471(6) 0.3708(4) 0.067(3) Uani 1 1 d . . . H29 H 0.0020 0.1851 0.3833 0.080 Uiso 1 1 calc R . . C30 C 0.1048(10) 0.0864(7) 0.3146(5) 0.077(3) Uani 1 1 d . . . H30 H 0.0301 0.0807 0.2921 0.093 Uiso 1 1 calc R . . C31 C 0.2250(12) 0.0382(6) 0.2938(5) 0.079(3) Uani 1 1 d . . . H31 H 0.2366 0.0017 0.2542 0.095 Uiso 1 1 calc R . . C32 C 0.3385(10) 0.0402(6) 0.3304(5) 0.069(3) Uani 1 1 d . . . H32 H 0.4251 0.0038 0.3178 0.083 Uiso 1 1 calc R . . C33 C 0.3113(8) 0.1012(5) 0.3873(4) 0.0400(18) Uani 1 1 d . . . C34 C 0.4256(8) 0.1138(5) 0.4280(4) 0.0448(19) Uani 1 1 d . . . C35 C 0.5529(9) 0.0594(6) 0.4228(5) 0.076(3) Uani 1 1 d . . . H35 H 0.5767 0.0072 0.3942 0.091 Uiso 1 1 calc R . . C36 C 0.6474(9) 0.0827(7) 0.4608(6) 0.080(3) Uani 1 1 d . . . H36 H 0.7359 0.0451 0.4578 0.096 Uiso 1 1 calc R . . C37 C 0.6171(8) 0.1565(6) 0.5014(5) 0.064(3) Uani 1 1 d . . . H37 H 0.6824 0.1727 0.5258 0.077 Uiso 1 1 calc R . . C38 C 0.4815(9) 0.2093(6) 0.5061(4) 0.061(2) Uani 1 1 d . . . H38 H 0.4565 0.2611 0.5349 0.073 Uiso 1 1 calc R . . C39 C 0.0779(9) 0.6503(6) 1.1353(4) 0.060(2) Uani 1 1 d . . . H39 H -0.0070 0.6814 1.1204 0.072 Uiso 1 1 calc R . . C40 C 0.0869(12) 0.6024(7) 1.1986(5) 0.092(3) Uani 1 1 d . . . H40 H 0.0117 0.6060 1.2290 0.110 Uiso 1 1 calc R . . C41 C 0.2198(13) 0.5468(8) 1.2145(6) 0.107(4) Uani 1 1 d . . . H41 H 0.2315 0.5051 1.2522 0.129 Uiso 1 1 calc R . . C42 C 0.3224(10) 0.5558(6) 1.1755(6) 0.083(3) Uani 1 1 d . . . H42 H 0.4086 0.5266 1.1895 0.099 Uiso 1 1 calc R . . C43 C 0.3104(7) 0.6057(5) 1.1149(4) 0.0420(19) Uani 1 1 d . . . C44 C 0.4235(8) 0.6193(5) 1.0708(4) 0.050(2) Uani 1 1 d . . . C45 C 0.5599(9) 0.5593(6) 1.0728(6) 0.088(4) Uani 1 1 d . . . H45 H 0.5803 0.5041 1.0990 0.105 Uiso 1 1 calc R . . C46 C 0.6543(9) 0.5880(8) 1.0347(7) 0.107(4) Uani 1 1 d . . . H46 H 0.7435 0.5538 1.0393 0.129 Uiso 1 1 calc R . . C47 C 0.6335(9) 0.6609(7) 0.9904(6) 0.084(3) Uani 1 1 d . . . H47 H 0.7028 0.6766 0.9636 0.101 Uiso 1 1 calc R . . C48 C 0.5009(9) 0.7104(6) 0.9883(4) 0.061(2) Uani 1 1 d . . . H48 H 0.4809 0.7616 0.9578 0.073 Uiso 1 1 calc R . . O23 O 0.9769(11) 0.4514(6) 0.0697(5) 0.176(4) Uani 1 1 d . . . O24 O 0.9833(10) 0.9369(6) 0.4449(5) 0.170(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 Zn1 0.0187(4) 0.0222(4) 0.0177(4) -0.0007(3) -0.0017(3) -0.0020(3) Zn2 0.0316(5) 0.0239(4) 0.0228(4) -0.0030(3) -0.0038(3) -0.0015(3) Zn3 0.0252(4) 0.0189(4) 0.0176(4) -0.0005(3) -0.0022(3) -0.0015(3) Zn4 0.0227(4) 0.0219(4) 0.0181(4) -0.0031(3) -0.0035(3) -0.0036(3) Zn5 0.0242(4) 0.0205(4) 0.0185(4) -0.0026(3) -0.0013(3) -0.0050(3) Zn6 0.0374(5) 0.0244(4) 0.0194(4) -0.0005(3) -0.0041(3) -0.0037(3) P1 0.0182(9) 0.0196(8) 0.0176(8) -0.0060(6) -0.0004(6) -0.0048(6) P2 0.0171(8) 0.0217(8) 0.0172(8) -0.0055(6) -0.0005(6) -0.0034(7) P3 0.0178(9) 0.0238(8) 0.0178(8) 0.0025(6) -0.0020(6) -0.0012(7) P4 0.0184(9) 0.0214(8) 0.0161(8) 0.0003(6) -0.0031(6) -0.0042(7) O1 0.019(2) 0.028(2) 0.037(3) -0.012(2) 0.0021(19) -0.0086(19) O2 0.033(3) 0.016(2) 0.021(2) -0.0024(17) 0.0017(19) -0.0022(18) O3 0.017(2) 0.021(2) 0.031(2) -0.0056(18) -0.0011(18) 0.0002(18) O4 0.026(3) 0.033(3) 0.042(3) 0.005(2) 0.002(2) -0.006(2) O5 0.061(3) 0.052(3) 0.018(2) 0.012(2) -0.015(2) -0.020(3) O6 0.038(3) 0.038(3) 0.032(3) 0.012(2) -0.005(2) 0.001(2) O7 0.036(3) 0.030(2) 0.019(2) 0.0025(18) -0.0004(19) -0.003(2) O8 0.023(2) 0.032(2) 0.036(3) 0.009(2) -0.007(2) -0.010(2) O9 0.020(2) 0.023(2) 0.031(2) 0.0018(18) 0.0011(19) -0.0003(18) O10 0.013(2) 0.022(2) 0.027(2) -0.0056(17) -0.0023(17) -0.0032(17) O11 0.026(2) 0.025(2) 0.019(2) -0.0048(17) -0.0010(18) -0.0048(19) O12 0.018(2) 0.021(2) 0.028(2) -0.0015(18) 0.0003(18) -0.0024(18) O13 0.064(4) 0.049(3) 0.019(3) -0.012(2) -0.002(2) -0.005(3) O14 0.064(4) 0.038(3) 0.037(3) -0.021(2) 0.002(3) -0.013(3) O15 0.033(3) 0.034(3) 0.038(3) -0.004(2) -0.014(2) -0.006(2) O16 0.011(2) 0.026(2) 0.029(2) 0.0015(18) -0.0052(18) -0.0024(17) O17 0.027(2) 0.017(2) 0.016(2) -0.0019(16) 0.0010(18) -0.0001(18) O18 0.022(2) 0.020(2) 0.032(2) -0.0021(18) -0.0015(19) -0.0052(18) O19 0.051(3) 0.047(3) 0.030(3) 0.020(2) -0.008(2) -0.003(3) O20 0.039(3) 0.066(4) 0.030(3) 0.017(3) 0.002(2) 0.000(3) O21 0.038(3) 0.043(3) 0.034(3) -0.025(2) -0.002(2) -0.003(2) O22 0.062(4) 0.063(4) 0.038(3) -0.019(3) -0.023(3) -0.010(3) N1 0.036(4) 0.030(3) 0.042(4) -0.012(3) 0.000(3) -0.007(3) N2 0.027(3) 0.034(3) 0.045(4) -0.011(3) -0.003(3) -0.001(3) N3 0.072(5) 0.034(3) 0.036(4) 0.017(3) -0.016(3) -0.025(3) N4 0.032(4) 0.032(3) 0.039(4) 0.005(3) 0.001(3) 0.000(3) C1 0.023(3) 0.020(3) 0.017(3) -0.003(2) -0.002(3) -0.006(3) C2 0.023(4) 0.040(4) 0.026(4) -0.007(3) -0.009(3) -0.005(3) C3 0.023(4) 0.033(4) 0.035(4) -0.016(3) -0.005(3) 0.005(3) C4 0.037(4) 0.032(4) 0.020(3) -0.008(3) -0.003(3) -0.015(3) C5 0.019(4) 0.054(5) 0.037(4) -0.019(3) -0.007(3) -0.006(3) C6 0.018(4) 0.044(4) 0.037(4) -0.025(3) 0.008(3) -0.007(3) C7 0.039(4) 0.037(4) 0.027(4) -0.015(3) 0.000(3) -0.016(3) C8 0.022(3) 0.031(4) 0.020(3) -0.003(3) -0.006(3) -0.007(3) C9 0.044(4) 0.026(4) 0.026(4) -0.005(3) 0.001(3) -0.010(3) C10 0.059(5) 0.027(4) 0.036(4) -0.011(3) 0.001(4) -0.017(4) C11 0.017(3) 0.030(4) 0.028(4) -0.013(3) 0.004(3) -0.003(3) C12 0.047(5) 0.036(4) 0.018(3) 0.003(3) -0.007(3) -0.007(3) C13 0.051(5) 0.026(4) 0.021(3) -0.002(3) -0.005(3) -0.005(3) C14 0.027(4) 0.054(5) 0.027(4) -0.013(3) -0.005(3) -0.010(3) C15 0.012(3) 0.033(4) 0.017(3) 0.005(3) 0.000(2) -0.002(3) C16 0.024(4) 0.028(4) 0.027(4) 0.001(3) -0.001(3) 0.008(3) C17 0.028(4) 0.034(4) 0.021(3) -0.003(3) 0.001(3) 0.001(3) C18 0.028(4) 0.042(4) 0.021(3) 0.009(3) -0.003(3) -0.015(3) C19 0.059(5) 0.028(4) 0.036(4) 0.014(3) -0.015(4) -0.013(4) C20 0.086(6) 0.038(4) 0.026(4) 0.010(3) -0.027(4) -0.035(4) C21 0.022(4) 0.046(5) 0.029(4) 0.011(3) -0.004(3) -0.010(3) C22 0.021(3) 0.020(3) 0.021(3) 0.000(2) -0.005(3) -0.003(3) C23 0.026(4) 0.066(5) 0.023(4) 0.014(3) -0.006(3) -0.009(4) C24 0.037(4) 0.076(6) 0.021(4) 0.018(4) -0.002(3) -0.024(4) C25 0.019(4) 0.023(3) 0.031(4) 0.003(3) -0.005(3) 0.003(3) C26 0.024(4) 0.037(4) 0.025(4) 0.009(3) -0.009(3) -0.003(3) C27 0.019(3) 0.036(4) 0.023(3) -0.003(3) 0.003(3) -0.005(3) C28 0.022(4) 0.040(4) 0.029(4) 0.008(3) 0.000(3) -0.004(3) C29 0.079(7) 0.067(6) 0.064(6) -0.016(5) -0.024(5) -0.029(5) C30 0.053(6) 0.089(7) 0.093(8) -0.051(6) -0.008(6) -0.020(5) C31 0.117(10) 0.065(7) 0.066(7) -0.036(5) -0.002(6) -0.042(6) C32 0.092(8) 0.055(6) 0.065(6) -0.029(5) 0.017(5) -0.029(5) C33 0.049(5) 0.029(4) 0.042(4) -0.014(3) 0.009(4) -0.011(4) C34 0.051(5) 0.034(4) 0.051(5) -0.002(4) -0.001(4) -0.015(4) C35 0.037(5) 0.057(6) 0.117(9) -0.045(6) 0.017(5) 0.013(4) C36 0.024(5) 0.079(7) 0.124(10) 0.004(7) 0.003(5) 0.006(5) C37 0.024(5) 0.071(6) 0.090(7) -0.015(5) -0.010(5) 0.005(4) C38 0.070(7) 0.055(6) 0.058(6) -0.009(4) -0.008(5) -0.017(5) C39 0.055(6) 0.063(6) 0.059(6) 0.021(5) 0.004(5) -0.013(5) C40 0.110(9) 0.088(8) 0.076(7) 0.033(6) 0.027(6) -0.033(7) C41 0.119(11) 0.107(9) 0.096(9) 0.073(8) -0.016(8) -0.038(8) C42 0.072(7) 0.071(7) 0.097(8) 0.047(6) -0.019(6) -0.007(6) C43 0.035(5) 0.033(4) 0.051(5) 0.014(4) -0.011(4) 0.002(3) C44 0.058(6) 0.040(5) 0.055(5) 0.008(4) -0.019(4) -0.015(4) C45 0.044(6) 0.060(6) 0.138(10) 0.037(6) -0.011(6) 0.019(5) C46 0.023(6) 0.101(9) 0.175(13) 0.025(9) 0.002(7) 0.020(6) C47 0.036(6) 0.088(8) 0.107(9) 0.006(7) 0.013(5) 0.016(5) C48 0.064(6) 0.060(6) 0.059(6) 0.009(5) -0.006(5) -0.018(5) O23 0.218(11) 0.121(8) 0.184(11) 0.047(7) -0.031(9) -0.035(7) O24 0.211(10) 0.132(8) 0.125(8) -0.032(6) -0.032(7) 0.033(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 Zn1 O11 1.932(4) 2_566 ? Zn1 O1 1.938(4) . ? Zn1 O19 1.942(4) 1_545 ? Zn1 O12 1.947(4) 1_455 ? Zn2 O4 2.017(4) . ? Zn2 O2 2.022(4) 2_566 ? Zn2 O5 2.023(4) . ? Zn2 N1 2.094(5) . ? Zn2 N2 2.099(5) . ? Zn3 O3 1.909(4) . ? Zn3 O10 1.923(4) . ? Zn3 O6 1.940(4) . ? Zn3 O2 1.982(4) 2_566 ? Zn4 O8 1.922(4) 1_465 ? Zn4 O21 1.933(4) . ? Zn4 O7 1.935(4) 2_567 ? Zn4 O18 1.967(4) . ? Zn5 O9 1.886(4) 1_565 ? Zn5 O16 1.914(4) . ? Zn5 O14 1.944(4) . ? Zn5 O17 1.996(4) 2_577 ? Zn6 O13 1.982(4) . ? Zn6 O17 2.005(4) 2_577 ? Zn6 N3 2.058(5) . ? Zn6 O15 2.073(4) . ? Zn6 N4 2.145(6) . ? P1 O1 1.493(4) . ? P1 O3 1.514(4) . ? P1 O2 1.551(4) . ? P1 C1 1.793(5) . ? P2 O12 1.491(4) . ? P2 O11 1.502(4) . ? P2 O10 1.537(4) . ? P2 C8 1.811(6) . ? P3 O8 1.507(4) . ? P3 O7 1.518(4) . ? P3 O9 1.518(4) . ? P3 C15 1.809(6) . ? P4 O18 1.501(4) . ? P4 O16 1.511(4) . ? P4 O17 1.552(4) . ? P4 C22 1.796(6) . ? O2 Zn3 1.982(4) 2_566 ? O2 Zn2 2.022(4) 2_566 ? O5 C21 1.244(7) . ? O6 C21 1.247(7) . ? O7 Zn4 1.935(4) 2_567 ? O8 Zn4 1.922(4) 1_645 ? O9 Zn5 1.886(4) 1_545 ? O11 Zn1 1.932(4) 2_566 ? O12 Zn1 1.947(4) 1_655 ? O13 C14 1.252(8) . ? O14 C14 1.256(8) . ? O17 Zn5 1.996(4) 2_577 ? O17 Zn6 2.005(4) 2_577 ? O19 C28 1.287(7) . ? O19 Zn1 1.942(4) 1_565 ? O20 C28 1.199(7) . ? O21 C7 1.231(7) . ? O22 C7 1.247(7) . ? N1 C33 1.287(8) . ? N1 C29 1.342(8) . ? N2 C34 1.339(8) . ? N2 C38 1.339(9) . ? N3 C43 1.338(8) . ? N3 C39 1.351(9) . ? N4 C44 1.334(8) . ? N4 C48 1.335(10) . ? C1 C6 1.383(8) . ? C1 C2 1.391(8) . ? C2 C3 1.385(8) . ? C2 H2 0.9300 . ? C3 C4 1.385(8) . ? C3 H3 0.9300 . ? C4 C5 1.354(8) . ? C4 C7 1.511(8) . ? C5 C6 1.392(8) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C9 1.363(8) . ? C8 C13 1.380(8) . ? C9 C10 1.388(8) . ? C9 H9 0.9300 . ? C10 C11 1.376(9) . ? C10 H10 0.9300 . ? C11 C12 1.360(8) . ? C11 C14 1.493(8) . ? C12 C13 1.402(8) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C15 C16 1.377(8) . ? C15 C20 1.397(8) . ? C16 C17 1.377(8) . ? C16 H16 0.9300 . ? C17 C18 1.396(8) . ? C17 H17 0.9300 . ? C18 C19 1.396(9) . ? C18 C21 1.496(8) . ? C19 C20 1.380(8) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C22 C27 1.363(8) . ? C22 C23 1.411(8) . ? C23 C24 1.375(8) . ? C23 H23 0.9300 . ? C24 C25 1.401(8) . ? C24 H24 0.9300 . ? C25 C26 1.374(8) . ? C25 C28 1.483(8) . ? C26 C27 1.383(8) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C29 C30 1.399(11) . ? C29 H29 0.9300 . ? C30 C31 1.296(12) . ? C30 H30 0.9300 . ? C31 C32 1.410(11) . ? C31 H31 0.9300 . ? C32 C33 1.405(9) . ? C32 H32 0.9300 . ? C33 C34 1.508(9) . ? C34 C35 1.341(10) . ? C35 C36 1.374(11) . ? C35 H35 0.9300 . ? C36 C37 1.318(12) . ? C36 H36 0.9300 . ? C37 C38 1.403(10) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C40 1.386(11) . ? C39 H39 0.9300 . ? C40 C41 1.442(13) . ? C40 H40 0.9300 . ? C41 C42 1.291(13) . ? C41 H41 0.9300 . ? C42 C43 1.356(11) . ? C42 H42 0.9300 . ? C43 C44 1.452(10) . ? C44 C45 1.447(11) . ? C45 C46 1.333(13) . ? C45 H45 0.9300 . ? C46 C47 1.335(14) . ? C46 H46 0.9300 . ? C47 C48 1.367(11) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? 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 O11 Zn1 O1 109.86(17) 2_566 . ? O11 Zn1 O19 117.47(19) 2_566 1_545 ? O1 Zn1 O19 110.90(19) . 1_545 ? O11 Zn1 O12 109.71(16) 2_566 1_455 ? O1 Zn1 O12 107.38(16) . 1_455 ? O19 Zn1 O12 100.77(19) 1_545 1_455 ? O4 Zn2 O2 89.79(16) . 2_566 ? O4 Zn2 O5 98.23(19) . . ? O2 Zn2 O5 103.96(17) 2_566 . ? O4 Zn2 N1 92.8(2) . . ? O2 Zn2 N1 127.06(19) 2_566 . ? O5 Zn2 N1 127.8(2) . . ? O4 Zn2 N2 168.9(2) . . ? O2 Zn2 N2 96.02(19) 2_566 . ? O5 Zn2 N2 89.6(2) . . ? N1 Zn2 N2 76.1(2) . . ? O3 Zn3 O10 108.05(16) . . ? O3 Zn3 O6 105.23(18) . . ? O10 Zn3 O6 113.85(18) . . ? O3 Zn3 O2 115.15(16) . 2_566 ? O10 Zn3 O2 106.26(16) . 2_566 ? O6 Zn3 O2 108.53(17) . 2_566 ? O8 Zn4 O21 108.21(18) 1_465 . ? O8 Zn4 O7 115.33(18) 1_465 2_567 ? O21 Zn4 O7 115.13(19) . 2_567 ? O8 Zn4 O18 105.55(16) 1_465 . ? O21 Zn4 O18 107.00(18) . . ? O7 Zn4 O18 104.80(17) 2_567 . ? O9 Zn5 O16 114.05(16) 1_565 . ? O9 Zn5 O14 102.20(19) 1_565 . ? O16 Zn5 O14 112.10(19) . . ? O9 Zn5 O17 110.38(16) 1_565 2_577 ? O16 Zn5 O17 108.45(16) . 2_577 ? O14 Zn5 O17 109.52(19) . 2_577 ? O13 Zn6 O17 112.07(19) . 2_577 ? O13 Zn6 N3 124.2(2) . . ? O17 Zn6 N3 122.60(19) 2_577 . ? O13 Zn6 O15 94.41(19) . . ? O17 Zn6 O15 93.03(16) 2_577 . ? N3 Zn6 O15 93.3(2) . . ? O13 Zn6 N4 88.2(2) . . ? O17 Zn6 N4 94.40(18) 2_577 . ? N3 Zn6 N4 77.7(2) . . ? O15 Zn6 N4 170.5(2) . . ? O1 P1 O3 113.1(2) . . ? O1 P1 O2 112.5(2) . . ? O3 P1 O2 109.3(2) . . ? O1 P1 C1 106.8(3) . . ? O3 P1 C1 108.7(2) . . ? O2 P1 C1 106.0(2) . . ? O12 P2 O11 115.2(2) . . ? O12 P2 O10 110.0(2) . . ? O11 P2 O10 110.9(2) . . ? O12 P2 C8 109.0(2) . . ? O11 P2 C8 107.8(3) . . ? O10 P2 C8 103.1(2) . . ? O8 P3 O7 113.1(2) . . ? O8 P3 O9 111.1(2) . . ? O7 P3 O9 112.3(2) . . ? O8 P3 C15 106.3(3) . . ? O7 P3 C15 106.6(2) . . ? O9 P3 C15 106.8(3) . . ? O18 P4 O16 113.4(2) . . ? O18 P4 O17 110.8(2) . . ? O16 P4 O17 110.1(2) . . ? O18 P4 C22 110.9(2) . . ? O16 P4 C22 105.8(3) . . ? O17 P4 C22 105.5(2) . . ? P1 O1 Zn1 139.2(3) . . ? P1 O2 Zn3 119.2(2) . 2_566 ? P1 O2 Zn2 133.3(2) . 2_566 ? Zn3 O2 Zn2 106.05(18) 2_566 2_566 ? P1 O3 Zn3 139.9(3) . . ? C21 O5 Zn2 134.2(4) . . ? C21 O6 Zn3 128.1(4) . . ? P3 O7 Zn4 122.8(2) . 2_567 ? P3 O8 Zn4 128.2(2) . 1_645 ? P3 O9 Zn5 127.3(2) . 1_545 ? P2 O10 Zn3 125.5(2) . . ? P2 O11 Zn1 122.3(2) . 2_566 ? P2 O12 Zn1 128.1(2) . 1_655 ? C14 O13 Zn6 128.0(4) . . ? C14 O14 Zn5 133.1(5) . . ? P4 O16 Zn5 132.6(2) . . ? P4 O17 Zn5 117.6(2) . 2_577 ? P4 O17 Zn6 125.9(2) . 2_577 ? Zn5 O17 Zn6 107.97(17) 2_577 2_577 ? P4 O18 Zn4 134.7(2) . . ? C28 O19 Zn1 125.3(4) . 1_565 ? C7 O21 Zn4 123.6(4) . . ? C33 N1 C29 118.5(6) . . ? C33 N1 Zn2 117.7(5) . . ? C29 N1 Zn2 123.5(5) . . ? C34 N2 C38 117.9(6) . . ? C34 N2 Zn2 116.7(5) . . ? C38 N2 Zn2 124.6(5) . . ? C43 N3 C39 119.0(7) . . ? C43 N3 Zn6 116.5(5) . . ? C39 N3 Zn6 123.7(5) . . ? C44 N4 C48 118.7(7) . . ? C44 N4 Zn6 111.8(5) . . ? C48 N4 Zn6 128.3(5) . . ? C6 C1 C2 118.0(5) . . ? C6 C1 P1 120.5(4) . . ? C2 C1 P1 121.5(4) . . ? C3 C2 C1 121.5(5) . . ? C3 C2 H2 119.2 . . ? C1 C2 H2 119.2 . . ? C4 C3 C2 119.3(6) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C5 C4 C3 119.6(5) . . ? C5 C4 C7 120.0(6) . . ? C3 C4 C7 120.4(6) . . ? C4 C5 C6 121.5(6) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C1 C6 C5 120.0(6) . . ? C1 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? O21 C7 O22 126.4(6) . . ? O21 C7 C4 116.7(6) . . ? O22 C7 C4 116.9(6) . . ? C9 C8 C13 119.2(6) . . ? C9 C8 P2 122.6(5) . . ? C13 C8 P2 118.0(5) . . ? C8 C9 C10 120.8(6) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? C11 C10 C9 120.5(6) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C12 C11 C10 118.9(6) . . ? C12 C11 C14 120.6(6) . . ? C10 C11 C14 120.5(6) . . ? C11 C12 C13 121.0(6) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C8 C13 C12 119.5(6) . . ? C8 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? O13 C14 O14 126.5(6) . . ? O13 C14 C11 116.6(6) . . ? O14 C14 C11 116.9(6) . . ? C16 C15 C20 117.1(5) . . ? C16 C15 P3 121.6(5) . . ? C20 C15 P3 121.3(5) . . ? C15 C16 C17 122.1(6) . . ? C15 C16 H16 119.0 . . ? C17 C16 H16 119.0 . . ? C16 C17 C18 120.2(6) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C19 C18 C17 118.9(6) . . ? C19 C18 C21 119.8(6) . . ? C17 C18 C21 121.3(6) . . ? C20 C19 C18 119.3(6) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C19 C20 C15 122.4(6) . . ? C19 C20 H20 118.8 . . ? C15 C20 H20 118.8 . . ? O5 C21 O6 125.0(6) . . ? O5 C21 C18 118.3(6) . . ? O6 C21 C18 116.7(6) . . ? C27 C22 C23 119.8(5) . . ? C27 C22 P4 123.0(5) . . ? C23 C22 P4 117.2(4) . . ? C24 C23 C22 118.8(6) . . ? C24 C23 H23 120.6 . . ? C22 C23 H23 120.6 . . ? C23 C24 C25 121.4(6) . . ? C23 C24 H24 119.3 . . ? C25 C24 H24 119.3 . . ? C26 C25 C24 118.3(6) . . ? C26 C25 C28 123.3(5) . . ? C24 C25 C28 118.4(6) . . ? C25 C26 C27 121.0(6) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C22 C27 C26 120.6(6) . . ? C22 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? O20 C28 O19 124.8(6) . . ? O20 C28 C25 120.8(6) . . ? O19 C28 C25 114.4(6) . . ? N1 C29 C30 121.1(8) . . ? N1 C29 H29 119.5 . . ? C30 C29 H29 119.5 . . ? C31 C30 C29 119.8(9) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C30 C31 C32 121.0(8) . . ? C30 C31 H31 119.5 . . ? C32 C31 H31 119.5 . . ? C33 C32 C31 115.1(8) . . ? C33 C32 H32 122.4 . . ? C31 C32 H32 122.4 . . ? N1 C33 C32 124.4(7) . . ? N1 C33 C34 115.6(6) . . ? C32 C33 C34 120.1(7) . . ? N2 C34 C35 122.5(7) . . ? N2 C34 C33 112.4(6) . . ? C35 C34 C33 125.1(7) . . ? C34 C35 C36 118.3(8) . . ? C34 C35 H35 120.9 . . ? C36 C35 H35 120.9 . . ? C37 C36 C35 122.3(8) . . ? C37 C36 H36 118.8 . . ? C35 C36 H36 118.8 . . ? C36 C37 C38 116.8(8) . . ? C36 C37 H37 121.6 . . ? C38 C37 H37 121.6 . . ? N2 C38 C37 122.2(8) . . ? N2 C38 H38 118.9 . . ? C37 C38 H38 118.9 . . ? N3 C39 C40 122.0(8) . . ? N3 C39 H39 119.0 . . ? C40 C39 H39 119.0 . . ? C39 C40 C41 115.9(9) . . ? C39 C40 H40 122.0 . . ? C41 C40 H40 122.0 . . ? C42 C41 C40 118.8(10) . . ? C42 C41 H41 120.6 . . ? C40 C41 H41 120.6 . . ? C41 C42 C43 123.1(10) . . ? C41 C42 H42 118.4 . . ? C43 C42 H42 118.4 . . ? N3 C43 C42 120.4(8) . . ? N3 C43 C44 114.9(7) . . ? C42 C43 C44 124.4(7) . . ? N4 C44 C45 119.2(8) . . ? N4 C44 C43 116.9(7) . . ? C45 C44 C43 123.9(8) . . ? C46 C45 C44 115.9(9) . . ? C46 C45 H45 122.0 . . ? C44 C45 H45 122.0 . . ? C45 C46 C47 126.4(9) . . ? C45 C46 H46 116.8 . . ? C47 C46 H46 116.8 . . ? C46 C47 C48 113.8(10) . . ? C46 C47 H47 123.1 . . ? C48 C47 H47 123.1 . . ? N4 C48 C47 125.6(9) . . ? N4 C48 H48 117.2 . . ? C47 C48 H48 117.2 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.713 _refine_diff_density_min -0.611 _refine_diff_density_rms 0.136 # Attachment 'a10418b.cif' data_a10418b _database_code_depnum_ccdc_archive 'CCDC 850194' #TrackingRef 'a10418b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H8 Cl O11 P2 Zn4' _chemical_formula_sum 'C14 H8 Cl O11 P2 Zn4' _chemical_formula_weight 711.07 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Pn _symmetry_space_group_name_Hall 'P -2yac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 13.097(4) _cell_length_b 5.786(2) _cell_length_c 13.138(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.005(4) _cell_angle_gamma 90.00 _cell_volume 985.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 686 _cell_measurement_theta_min 2.367 _cell_measurement_theta_max 27.439 _exptl_crystal_description sheet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 694 _exptl_absorpt_coefficient_mu 5.165 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5761 _exptl_absorpt_correction_T_max 0.8200 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _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 4231 _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_sigmaI/netI 0.0635 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3354 _reflns_number_gt 3038 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0310P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(5) _refine_ls_number_reflns 3354 _refine_ls_number_parameters 292 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0764 _refine_ls_wR_factor_gt 0.0747 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.998 _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 0.73744(6) -0.19814(14) 0.88171(6) 0.0130(2) Uani 1 1 d . . . Zn2 Zn 0.59297(7) 0.16662(13) 0.75849(6) 0.0137(2) Uani 1 1 d . . . Zn3 Zn 0.40491(6) 0.42106(14) 0.60441(6) 0.0131(2) Uani 1 1 d . . . Zn4 Zn 0.43331(6) 0.91059(14) 0.52133(6) 0.0134(2) Uani 1 1 d . . . P1 P 0.70443(16) 0.3211(3) 0.98064(16) 0.0106(5) Uani 1 1 d . . . P2 P 0.62985(15) 0.6590(3) 0.65905(16) 0.0120(5) Uani 1 1 d . . . O1 O 0.6864(5) 0.1256(9) 0.9012(4) 0.0131(12) Uani 1 1 d . . . O2 O 0.8200(4) 0.3303(9) 1.0234(4) 0.0130(13) Uani 1 1 d . . . O3 O 0.6662(4) 0.5476(8) 0.9341(4) 0.0134(12) Uani 1 1 d . . . O4 O 0.3679(4) 0.2435(11) 1.3232(5) 0.0262(14) Uani 1 1 d . . . O5 O 0.4762(5) -0.0379(9) 1.3880(5) 0.0254(14) Uani 1 1 d . . . O6 O 0.5147(4) 0.6646(8) 0.6080(4) 0.0113(12) Uani 1 1 d . . . O7 O 0.6590(4) 0.4355(9) 0.7098(4) 0.0150(12) Uani 1 1 d . . . O8 O 0.6510(4) 0.8570(9) 0.7375(4) 0.0154(13) Uani 1 1 d . . . O9 O 0.8598(5) 0.5893(10) 0.2376(5) 0.0306(16) Uani 1 1 d . . . O10 O 0.9680(5) 0.8426(10) 0.3235(5) 0.0292(16) Uani 1 1 d . . . O12 O 0.5112(4) 0.1598(7) 0.6095(4) 0.065(4) Uani 0.2(3) 1 d P . . Cl1 Cl 0.5112(4) 0.1598(7) 0.6095(4) 0.065(4) Uani 0.68(16) 1 d P . . O13 O 0.3260(4) 0.1633(8) 0.5292(3) 0.038(5) Uani 0.8(3) 1 d P . . Cl2 Cl 0.3260(4) 0.1633(8) 0.5292(3) 0.038(5) Uani 0.32(16) 1 d P . . C1 C 0.6317(6) 0.2629(13) 1.0853(6) 0.0136(16) Uani 1 1 d . . . C2 C 0.6488(7) 0.0664(14) 1.1456(7) 0.032(2) Uani 1 1 d . . . H2A H 0.6992 -0.0383 1.1324 0.038 Uiso 1 1 calc R . . C3 C 0.5919(7) 0.0228(15) 1.2252(7) 0.033(2) Uani 1 1 d . . . H3A H 0.6054 -0.1076 1.2663 0.040 Uiso 1 1 calc R . . C4 C 0.5147(6) 0.1764(13) 1.2428(6) 0.0183(18) Uani 1 1 d . . . C5 C 0.4968(6) 0.3687(14) 1.1825(7) 0.030(2) Uani 1 1 d . . . H5A H 0.4442 0.4699 1.1935 0.036 Uiso 1 1 calc R . . C6 C 0.5555(6) 0.4147(14) 1.1055(7) 0.030(2) Uani 1 1 d . . . H6A H 0.5437 0.5491 1.0668 0.037 Uiso 1 1 calc R . . C7 C 0.4478(6) 0.1216(15) 1.3246(6) 0.0212(18) Uani 1 1 d . . . C8 C 0.7040(6) 0.6962(12) 0.5570(6) 0.0145(17) Uani 1 1 d . . . C9 C 0.7739(6) 0.8733(14) 0.5522(6) 0.0259(19) Uani 1 1 d . . . H9A H 0.7816 0.9864 0.6030 0.031 Uiso 1 1 calc R . . C10 C 0.8324(6) 0.8841(15) 0.4723(7) 0.030(2) Uani 1 1 d . . . H10A H 0.8782 1.0059 0.4692 0.036 Uiso 1 1 calc R . . C11 C 0.8234(6) 0.7164(14) 0.3978(6) 0.0190(17) Uani 1 1 d . . . C12 C 0.7519(7) 0.5404(14) 0.4011(7) 0.032(2) Uani 1 1 d . . . H12A H 0.7427 0.4297 0.3493 0.038 Uiso 1 1 calc R . . C13 C 0.6950(7) 0.5301(14) 0.4809(7) 0.032(2) Uani 1 1 d . . . H13A H 0.6491 0.4083 0.4838 0.038 Uiso 1 1 calc R . . C14 C 0.8889(6) 0.7219(14) 0.3124(6) 0.0211(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 Zn1 0.0130(5) 0.0131(4) 0.0126(5) 0.0010(3) 0.0015(4) 0.0001(3) Zn2 0.0135(4) 0.0129(4) 0.0147(5) 0.0008(3) 0.0016(4) 0.0016(3) Zn3 0.0147(5) 0.0109(5) 0.0135(5) 0.0011(3) 0.0007(4) -0.0003(3) Zn4 0.0138(5) 0.0126(5) 0.0136(5) 0.0014(3) 0.0017(4) -0.0007(3) P1 0.0111(11) 0.0087(10) 0.0120(11) -0.0009(7) 0.0012(9) -0.0018(7) P2 0.0118(12) 0.0132(11) 0.0113(12) 0.0001(7) 0.0030(9) -0.0012(8) O1 0.020(3) 0.012(3) 0.007(3) 0.001(2) 0.003(3) 0.003(2) O2 0.011(3) 0.006(3) 0.021(3) -0.001(2) 0.000(3) 0.005(2) O3 0.010(3) 0.012(3) 0.017(3) 0.001(2) 0.002(2) -0.001(2) O4 0.014(3) 0.039(4) 0.027(4) 0.003(3) 0.012(3) 0.000(3) O5 0.035(4) 0.026(3) 0.017(3) 0.009(2) 0.013(3) 0.006(3) O6 0.010(3) 0.009(3) 0.013(3) 0.002(2) -0.004(2) -0.002(2) O7 0.014(3) 0.014(3) 0.015(3) 0.002(2) -0.004(2) 0.001(2) O8 0.013(3) 0.018(3) 0.015(3) 0.000(2) 0.000(2) 0.000(2) O9 0.032(4) 0.044(4) 0.019(4) -0.010(3) 0.013(3) -0.014(3) O10 0.021(3) 0.042(4) 0.026(4) -0.008(3) 0.011(3) -0.008(3) O12 0.063(5) 0.060(5) 0.071(5) -0.004(2) 0.002(3) 0.006(2) Cl1 0.063(5) 0.060(5) 0.071(5) -0.004(2) 0.002(3) 0.006(2) O13 0.037(6) 0.037(6) 0.037(6) -0.0024(19) -0.001(2) 0.0037(19) Cl2 0.037(6) 0.037(6) 0.037(6) -0.0024(19) -0.001(2) 0.0037(19) C1 0.014(4) 0.015(4) 0.011(4) 0.004(3) 0.000(3) -0.002(3) C2 0.033(5) 0.031(5) 0.035(6) 0.010(4) 0.022(4) 0.020(4) C3 0.046(6) 0.027(5) 0.032(6) 0.016(4) 0.024(5) 0.017(4) C4 0.013(4) 0.027(5) 0.015(4) -0.001(3) 0.003(3) 0.001(3) C5 0.029(5) 0.028(5) 0.038(6) 0.006(4) 0.019(4) 0.015(4) C6 0.035(5) 0.026(5) 0.035(5) 0.019(4) 0.021(4) 0.017(4) C7 0.019(4) 0.032(5) 0.013(4) -0.005(3) 0.003(3) -0.007(4) C8 0.019(4) 0.015(4) 0.009(4) 0.000(3) 0.000(3) 0.003(3) C9 0.034(5) 0.031(5) 0.015(4) -0.012(3) 0.010(4) -0.011(4) C10 0.021(4) 0.032(5) 0.039(6) -0.006(4) 0.014(4) -0.019(4) C11 0.017(4) 0.027(4) 0.013(4) -0.005(3) 0.003(3) 0.000(3) C12 0.035(5) 0.038(5) 0.027(6) -0.014(4) 0.017(4) -0.009(4) C13 0.039(5) 0.028(5) 0.031(6) -0.010(4) 0.018(4) -0.026(4) C14 0.020(4) 0.028(5) 0.016(4) 0.000(4) 0.003(3) 0.002(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 O3 1.920(5) 1_545 ? Zn1 O4 1.986(5) 2_554 ? Zn1 O1 2.017(6) . ? Zn1 O8 2.092(6) 1_545 ? Zn1 Cl2 2.124(5) 2 ? Zn1 O13 2.124(5) 2 ? Zn1 Zn2 3.1308(12) . ? Zn2 O7 1.932(5) . ? Zn2 O10 1.950(6) 2_465 ? Zn2 O8 1.980(5) 1_545 ? Zn2 O12 2.096(5) . ? Zn2 O1 2.105(6) . ? Zn3 O9 1.925(6) 2_465 ? Zn3 O13 1.996(5) . ? Zn3 O6 2.009(5) . ? Zn3 O2 2.027(6) 2_464 ? Zn3 O12 2.050(5) . ? Zn3 Zn4 3.0766(14) . ? Zn4 O5 1.936(6) 1_564 ? Zn4 O6 2.030(5) . ? Zn4 Cl1 2.033(5) 1_565 ? Zn4 O12 2.033(5) 1_565 ? Zn4 O2 2.038(5) 2_464 ? Zn4 Cl2 2.041(5) 1_565 ? Zn4 O13 2.041(5) 1_565 ? P1 O3 1.502(5) . ? P1 O1 1.535(6) . ? P1 O2 1.541(6) . ? P1 C1 1.810(8) . ? P2 O7 1.481(6) . ? P2 O8 1.540(6) . ? P2 O6 1.563(6) . ? P2 C8 1.775(8) . ? O2 Zn3 2.027(6) 2_565 ? O2 Zn4 2.038(5) 2_565 ? O3 Zn1 1.920(5) 1_565 ? O4 C7 1.260(10) . ? O4 Zn1 1.986(5) 2_455 ? O5 C7 1.264(10) . ? O5 Zn4 1.936(6) 1_546 ? O8 Zn2 1.980(5) 1_565 ? O8 Zn1 2.092(6) 1_565 ? O9 C14 1.264(10) . ? O9 Zn3 1.925(6) 2_564 ? O10 C14 1.241(9) . ? O10 Zn2 1.950(6) 2_564 ? O12 Zn4 2.033(5) 1_545 ? O13 Zn4 2.041(5) 1_545 ? O13 Zn1 2.124(5) 2_454 ? C1 C6 1.382(10) . ? C1 C2 1.386(10) . ? C2 C3 1.389(11) . ? C2 H2A 0.9300 . ? C3 C4 1.390(11) . ? C3 H3A 0.9300 . ? C4 C5 1.367(11) . ? C4 C7 1.512(11) . ? C5 C6 1.379(11) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C8 C13 1.381(11) . ? C8 C9 1.381(10) . ? C9 C10 1.385(11) . ? C9 H9A 0.9300 . ? C10 C11 1.372(11) . ? C10 H10A 0.9300 . ? C11 C12 1.388(11) . ? C11 C14 1.504(11) . ? C12 C13 1.370(11) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? 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 O3 Zn1 O4 121.6(2) 1_545 2_554 ? O3 Zn1 O1 118.7(2) 1_545 . ? O4 Zn1 O1 119.3(2) 2_554 . ? O3 Zn1 O8 102.3(2) 1_545 1_545 ? O4 Zn1 O8 93.2(2) 2_554 1_545 ? O1 Zn1 O8 80.0(2) . 1_545 ? O3 Zn1 Cl2 88.7(2) 1_545 2 ? O4 Zn1 Cl2 88.6(2) 2_554 2 ? O1 Zn1 Cl2 86.8(2) . 2 ? O8 Zn1 Cl2 165.78(18) 1_545 2 ? O3 Zn1 O13 88.7(2) 1_545 2 ? O4 Zn1 O13 88.6(2) 2_554 2 ? O1 Zn1 O13 86.8(2) . 2 ? O8 Zn1 O13 165.78(18) 1_545 2 ? Cl2 Zn1 O13 0.00(14) 2 2 ? O3 Zn1 Zn2 114.40(16) 1_545 . ? O4 Zn1 Zn2 112.31(19) 2_554 . ? O1 Zn1 Zn2 41.62(17) . . ? O8 Zn1 Zn2 38.46(15) 1_545 . ? Cl2 Zn1 Zn2 128.42(13) 2 . ? O13 Zn1 Zn2 128.42(13) 2 . ? O7 Zn2 O10 127.5(2) . 2_465 ? O7 Zn2 O8 119.0(2) . 1_545 ? O10 Zn2 O8 113.5(2) 2_465 1_545 ? O7 Zn2 O12 84.3(2) . . ? O10 Zn2 O12 93.3(2) 2_465 . ? O8 Zn2 O12 90.5(2) 1_545 . ? O7 Zn2 O1 98.8(3) . . ? O10 Zn2 O1 91.5(3) 2_465 . ? O8 Zn2 O1 80.5(2) 1_545 . ? O12 Zn2 O1 170.9(2) . . ? O7 Zn2 Zn1 116.60(17) . . ? O10 Zn2 Zn1 103.82(18) 2_465 . ? O8 Zn2 Zn1 41.08(17) 1_545 . ? O12 Zn2 Zn1 131.55(13) . . ? O1 Zn2 Zn1 39.54(15) . . ? O9 Zn3 O13 102.9(2) 2_465 . ? O9 Zn3 O6 108.0(3) 2_465 . ? O13 Zn3 O6 148.8(2) . . ? O9 Zn3 O2 106.5(2) 2_465 2_464 ? O13 Zn3 O2 93.6(2) . 2_464 ? O6 Zn3 O2 81.55(18) . 2_464 ? O9 Zn3 O12 103.9(2) 2_465 . ? O13 Zn3 O12 76.58(15) . . ? O6 Zn3 O12 92.0(2) . . ? O2 Zn3 O12 149.4(2) 2_464 . ? O9 Zn3 Zn4 114.76(18) 2_465 . ? O13 Zn3 Zn4 126.30(14) . . ? O6 Zn3 Zn4 40.65(16) . . ? O2 Zn3 Zn4 40.96(15) 2_464 . ? O12 Zn3 Zn4 125.12(14) . . ? O5 Zn4 O6 114.8(2) 1_564 . ? O5 Zn4 Cl1 102.7(2) 1_564 1_565 ? O6 Zn4 Cl1 89.7(2) . 1_565 ? O5 Zn4 O12 102.7(2) 1_564 1_565 ? O6 Zn4 O12 89.7(2) . 1_565 ? Cl1 Zn4 O12 0.0(3) 1_565 1_565 ? O5 Zn4 O2 114.9(3) 1_564 2_464 ? O6 Zn4 O2 80.77(18) . 2_464 ? Cl1 Zn4 O2 141.8(2) 1_565 2_464 ? O12 Zn4 O2 141.8(2) 1_565 2_464 ? O5 Zn4 Cl2 103.0(2) 1_564 1_565 ? O6 Zn4 Cl2 141.8(2) . 1_565 ? Cl1 Zn4 Cl2 75.98(16) 1_565 1_565 ? O12 Zn4 Cl2 75.98(16) 1_565 1_565 ? O2 Zn4 Cl2 88.9(2) 2_464 1_565 ? O5 Zn4 O13 103.0(2) 1_564 1_565 ? O6 Zn4 O13 141.8(2) . 1_565 ? Cl1 Zn4 O13 75.98(16) 1_565 1_565 ? O12 Zn4 O13 75.98(16) 1_565 1_565 ? O2 Zn4 O13 88.9(2) 2_464 1_565 ? Cl2 Zn4 O13 0.0(3) 1_565 1_565 ? O5 Zn4 Zn3 121.83(17) 1_564 . ? O6 Zn4 Zn3 40.14(16) . . ? Cl1 Zn4 Zn3 121.78(14) 1_565 . ? O12 Zn4 Zn3 121.78(14) 1_565 . ? O2 Zn4 Zn3 40.68(17) 2_464 . ? Cl2 Zn4 Zn3 121.57(13) 1_565 . ? O13 Zn4 Zn3 121.57(13) 1_565 . ? O3 P1 O1 110.8(3) . . ? O3 P1 O2 111.9(3) . . ? O1 P1 O2 108.9(3) . . ? O3 P1 C1 106.9(3) . . ? O1 P1 C1 109.4(3) . . ? O2 P1 C1 108.9(3) . . ? O7 P2 O8 109.7(3) . . ? O7 P2 O6 112.6(3) . . ? O8 P2 O6 110.2(3) . . ? O7 P2 C8 108.2(3) . . ? O8 P2 C8 110.4(3) . . ? O6 P2 C8 105.7(3) . . ? P1 O1 Zn1 138.4(4) . . ? P1 O1 Zn2 122.5(3) . . ? Zn1 O1 Zn2 98.8(2) . . ? P1 O2 Zn3 130.9(3) . 2_565 ? P1 O2 Zn4 130.7(3) . 2_565 ? Zn3 O2 Zn4 98.4(3) 2_565 2_565 ? P1 O3 Zn1 131.6(3) . 1_565 ? C7 O4 Zn1 132.7(6) . 2_455 ? C7 O5 Zn4 127.8(5) . 1_546 ? P2 O6 Zn3 129.8(3) . . ? P2 O6 Zn4 130.9(3) . . ? Zn3 O6 Zn4 99.2(3) . . ? P2 O7 Zn2 138.9(4) . . ? P2 O8 Zn2 136.8(4) . 1_565 ? P2 O8 Zn1 121.1(3) . 1_565 ? Zn2 O8 Zn1 100.5(2) 1_565 1_565 ? C14 O9 Zn3 128.9(6) . 2_564 ? C14 O10 Zn2 132.2(6) . 2_564 ? Zn4 O12 Zn3 102.7(2) 1_545 . ? Zn4 O12 Zn2 134.1(2) 1_545 . ? Zn3 O12 Zn2 105.8(2) . . ? Zn3 O13 Zn4 104.3(2) . 1_545 ? Zn3 O13 Zn1 124.1(2) . 2_454 ? Zn4 O13 Zn1 108.3(2) 1_545 2_454 ? C6 C1 C2 118.4(7) . . ? C6 C1 P1 119.9(6) . . ? C2 C1 P1 121.7(6) . . ? C1 C2 C3 121.2(7) . . ? C1 C2 H2A 119.4 . . ? C3 C2 H2A 119.4 . . ? C2 C3 C4 119.2(7) . . ? C2 C3 H3A 120.4 . . ? C4 C3 H3A 120.4 . . ? C5 C4 C3 119.6(7) . . ? C5 C4 C7 120.9(7) . . ? C3 C4 C7 119.4(7) . . ? C4 C5 C6 120.9(8) . . ? C4 C5 H5A 119.5 . . ? C6 C5 H5A 119.5 . . ? C5 C6 C1 120.6(7) . . ? C5 C6 H6A 119.7 . . ? C1 C6 H6A 119.7 . . ? O4 C7 O5 125.9(8) . . ? O4 C7 C4 115.8(8) . . ? O5 C7 C4 118.4(7) . . ? C13 C8 C9 118.3(8) . . ? C13 C8 P2 117.5(6) . . ? C9 C8 P2 124.1(6) . . ? C8 C9 C10 120.6(7) . . ? C8 C9 H9A 119.7 . . ? C10 C9 H9A 119.7 . . ? C11 C10 C9 120.5(7) . . ? C11 C10 H10A 119.8 . . ? C9 C10 H10A 119.8 . . ? C10 C11 C12 119.2(7) . . ? C10 C11 C14 121.0(7) . . ? C12 C11 C14 119.7(7) . . ? C13 C12 C11 119.8(7) . . ? C13 C12 H12A 120.1 . . ? C11 C12 H12A 120.1 . . ? C12 C13 C8 121.6(8) . . ? C12 C13 H13A 119.2 . . ? C8 C13 H13A 119.2 . . ? O10 C14 O9 126.1(8) . . ? O10 C14 C11 118.5(7) . . ? O9 C14 C11 115.2(7) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.593 _refine_diff_density_min -0.803 _refine_diff_density_rms 0.116 # Attachment 'mo10420a.cif' data_mo10420a _database_code_depnum_ccdc_archive 'CCDC 850195' #TrackingRef 'mo10420a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety C14H8O10P2Zn2,C10H16N2O4Zn,3(H2O) _chemical_formula_sum 'C24 H30 N2 O17 P2 Zn3' _chemical_formula_weight 876.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.7666(15) _cell_length_b 16.462(2) _cell_length_c 17.912(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.098(2) _cell_angle_gamma 90.00 _cell_volume 3174.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4246 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 27.19 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.834 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 _exptl_absorpt_coefficient_mu 2.430 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7591 _exptl_absorpt_correction_T_max 0.8293 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19622 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0527 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 26.01 _reflns_number_total 6216 _reflns_number_gt 4600 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0632P)^2^+4.6693P] 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 6216 _refine_ls_number_parameters 475 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0704 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1277 _refine_ls_wR_factor_gt 0.1110 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.073 _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 0.92149(5) 0.44328(3) 0.08887(3) 0.01577(14) Uani 1 1 d . . . Zn2 Zn 0.61572(5) 0.54334(3) -0.08384(3) 0.01702(14) Uani 1 1 d . . . Zn3 Zn 0.61962(6) 0.22854(4) 0.03568(4) 0.03301(18) Uani 1 1 d . . . P1 P 0.85449(11) 0.43135(7) -0.08550(6) 0.0157(2) Uani 1 1 d . . . P2 P 0.84467(11) 0.04625(7) 0.40947(6) 0.0160(2) Uani 1 1 d . . . O1 O 0.7143(3) 0.44564(18) -0.08472(18) 0.0191(7) Uani 1 1 d . . . O2 O 0.9225(3) 0.5058(2) -0.1119(2) 0.0271(8) Uani 1 1 d . . . O3 O 0.9031(3) 0.3983(2) -0.01119(18) 0.0246(8) Uani 1 1 d . . . O4 O 0.8595(3) 0.1391(2) -0.35379(19) 0.0268(8) Uani 1 1 d . . . O5 O 0.9143(5) 0.0686(2) -0.2547(2) 0.0519(12) Uani 1 1 d . . . O6 O 1.0461(4) 0.2898(3) 0.1308(3) 0.0496(12) Uani 1 1 d . . . O7 O 0.8811(3) 0.3590(2) 0.16323(18) 0.0258(8) Uani 1 1 d . . . O8 O 0.9365(3) -0.02364(19) 0.40301(18) 0.0213(7) Uani 1 1 d . . . O9 O 0.7120(3) 0.0203(2) 0.3970(2) 0.0263(8) Uani 1 1 d . . . O10 O 0.8644(3) 0.09251(19) 0.48342(17) 0.0222(7) Uani 1 1 d . . . C1 C 0.8739(4) 0.3483(3) -0.1502(2) 0.0177(9) Uani 1 1 d . . . C2 C 0.9653(5) 0.2894(3) -0.1369(3) 0.0278(12) Uani 1 1 d . . . H2 H 1.0232 0.2969 -0.0984 0.033 Uiso 1 1 calc R . . C3 C 0.9704(5) 0.2204(3) -0.1804(3) 0.0320(12) Uani 1 1 d . . . H3 H 1.0291 0.1805 -0.1696 0.038 Uiso 1 1 calc R . . C4 C 0.8877(5) 0.2106(3) -0.2404(3) 0.0263(11) Uani 1 1 d . . . C5 C 0.8005(5) 0.2704(3) -0.2561(3) 0.0277(12) Uani 1 1 d . . . H5 H 0.7472 0.2655 -0.2973 0.033 Uiso 1 1 calc R . . C6 C 0.7934(5) 0.3381(3) -0.2095(3) 0.0251(11) Uani 1 1 d . . . H6 H 0.7325 0.3771 -0.2188 0.030 Uiso 1 1 calc R . . C7 C 0.8889(5) 0.1330(3) -0.2844(3) 0.0280(11) Uani 1 1 d . . . C8 C 0.8756(4) 0.1200(3) 0.3372(3) 0.0188(10) Uani 1 1 d . . . C9 C 0.9569(5) 0.1033(3) 0.2802(3) 0.0249(11) Uani 1 1 d . . . H9 H 0.9961 0.0530 0.2785 0.030 Uiso 1 1 calc R . . C10 C 0.9805(5) 0.1603(3) 0.2261(3) 0.0290(12) Uani 1 1 d . . . H10 H 1.0359 0.1482 0.1885 0.035 Uiso 1 1 calc R . . C11 C 0.9226(5) 0.2356(3) 0.2269(3) 0.0234(10) Uani 1 1 d . . . C12 C 0.8385(5) 0.2512(3) 0.2819(3) 0.0277(11) Uani 1 1 d . . . H12 H 0.7954 0.3002 0.2815 0.033 Uiso 1 1 calc R . . C13 C 0.8171(5) 0.1951(3) 0.3380(3) 0.0284(12) Uani 1 1 d . . . H13 H 0.7633 0.2079 0.3763 0.034 Uiso 1 1 calc R . . C14 C 0.9539(5) 0.2982(3) 0.1687(3) 0.0251(11) Uani 1 1 d . . . N1 N 0.6232(5) 0.1328(3) -0.0454(3) 0.0420(12) Uani 1 1 d . . . N2 N 0.6381(5) 0.1253(3) 0.1028(3) 0.0385(12) Uani 1 1 d . . . C15 C 0.6161(7) 0.1428(5) -0.1187(4) 0.0572(19) Uani 1 1 d . . . H15 H 0.5975 0.1942 -0.1372 0.069 Uiso 1 1 calc R . . C16 C 0.6352(8) 0.0801(6) -0.1697(5) 0.078(3) Uani 1 1 d . . . H16 H 0.6316 0.0887 -0.2210 0.093 Uiso 1 1 calc R . . C17 C 0.6601(9) 0.0035(7) -0.1389(8) 0.110(4) Uani 1 1 d . . . H17 H 0.6718 -0.0407 -0.1702 0.132 Uiso 1 1 calc R . . C18 C 0.6673(9) -0.0068(5) -0.0639(6) 0.082(3) Uani 1 1 d . . . H18 H 0.6844 -0.0580 -0.0443 0.099 Uiso 1 1 calc R . . C19 C 0.6492(6) 0.0593(4) -0.0156(4) 0.0516(18) Uani 1 1 d . . . C20 C 0.6550(6) 0.0547(4) 0.0663(4) 0.0478(17) Uani 1 1 d . . . C21 C 0.6693(9) -0.0161(5) 0.1088(6) 0.080(3) Uani 1 1 d . . . H21 H 0.6803 -0.0657 0.0851 0.096 Uiso 1 1 calc R . . C22 C 0.6672(9) -0.0126(6) 0.1851(6) 0.090(3) Uani 1 1 d . . . H22 H 0.6825 -0.0593 0.2130 0.108 Uiso 1 1 calc R . . C23 C 0.6430(8) 0.0579(5) 0.2200(5) 0.072(3) Uani 1 1 d . . . H23 H 0.6341 0.0602 0.2715 0.086 Uiso 1 1 calc R . . C24 C 0.6323(6) 0.1256(4) 0.1766(4) 0.0516(18) Uani 1 1 d . . . H24 H 0.6201 0.1752 0.2002 0.062 Uiso 1 1 calc R . . O11 O 0.8120(4) 0.2424(3) 0.0227(3) 0.0428(10) Uani 1 1 d D . . H11A H 0.867(4) 0.206(2) 0.026(4) 0.064 Uiso 1 1 d D . . H11B H 0.845(5) 0.2884(17) 0.026(4) 0.064 Uiso 1 1 d D . . O12 O 0.6384(4) 0.3150(2) 0.1247(2) 0.0362(9) Uani 1 1 d D . . H12A H 0.713(3) 0.322(3) 0.140(4) 0.054 Uiso 1 1 d D . . H12B H 0.615(5) 0.3649(18) 0.114(4) 0.054 Uiso 1 1 d D . . O13 O 0.5766(4) 0.3151(2) -0.0391(3) 0.0382(10) Uani 1 1 d D . . H13A H 0.510(3) 0.335(3) -0.025(4) 0.057 Uiso 1 1 d D . . H13B H 0.619(5) 0.352(3) -0.059(4) 0.057 Uiso 1 1 d D . . O14 O 0.4233(4) 0.2256(3) 0.0631(3) 0.0448(10) Uani 1 1 d D . . H14A H 0.353(3) 0.204(4) 0.066(4) 0.067 Uiso 1 1 d D . . H14B H 0.420(6) 0.268(3) 0.091(3) 0.067 Uiso 1 1 d D . . O15 O -0.0035(8) 0.1240(4) 0.0164(4) 0.101(2) Uani 1 1 d D . . H15A H 0.000(12) 0.104(7) -0.027(2) 0.152 Uiso 1 1 d D . . H15B H 0.040(10) 0.093(6) 0.044(5) 0.152 Uiso 1 1 d D . . O16 O 0.1888(6) 0.2717(5) 0.0080(3) 0.0818(18) Uani 1 1 d D . . H16A H 0.181(10) 0.2181(16) 0.002(5) 0.123 Uiso 1 1 d D . . H16B H 0.149(8) 0.279(5) 0.049(3) 0.123 Uiso 1 1 d D . . O17 O 0.5053(8) 0.5222(5) 0.6085(4) 0.117(3) Uani 1 1 d D . . H17A H 0.575(6) 0.516(10) 0.588(6) 0.176 Uiso 1 1 d D . . H17B H 0.522(11) 0.536(8) 0.653(3) 0.176 Uiso 1 1 d 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 Zn1 0.0190(3) 0.0142(3) 0.0141(3) 0.0001(2) 0.0004(2) -0.0011(2) Zn2 0.0233(3) 0.0141(3) 0.0137(3) 0.0010(2) 0.0012(2) 0.0012(2) Zn3 0.0391(4) 0.0254(3) 0.0344(4) 0.0044(3) -0.0022(3) 0.0001(3) P1 0.0180(6) 0.0140(5) 0.0149(6) -0.0028(4) -0.0004(4) 0.0011(5) P2 0.0196(6) 0.0143(5) 0.0140(6) 0.0029(4) -0.0005(4) -0.0028(4) O1 0.0180(16) 0.0175(16) 0.0220(17) -0.0031(13) 0.0028(13) 0.0020(13) O2 0.0219(17) 0.0216(18) 0.037(2) 0.0039(15) -0.0054(15) -0.0081(14) O3 0.033(2) 0.0232(17) 0.0170(17) -0.0035(14) -0.0053(14) 0.0065(15) O4 0.032(2) 0.0235(18) 0.0248(19) -0.0092(15) -0.0014(15) 0.0012(15) O5 0.095(4) 0.028(2) 0.033(2) -0.0037(18) 0.001(2) 0.018(2) O6 0.039(2) 0.052(3) 0.059(3) 0.033(2) 0.019(2) 0.011(2) O7 0.035(2) 0.0216(17) 0.0211(18) 0.0082(14) 0.0033(15) -0.0020(15) O8 0.0216(17) 0.0167(16) 0.0254(18) 0.0034(14) -0.0005(14) 0.0021(13) O9 0.0181(17) 0.0269(18) 0.034(2) 0.0080(16) -0.0009(15) -0.0065(14) O10 0.035(2) 0.0196(16) 0.0117(16) 0.0005(13) 0.0003(14) -0.0032(14) C1 0.017(2) 0.022(2) 0.014(2) -0.0046(18) 0.0018(18) 0.0029(18) C2 0.025(3) 0.032(3) 0.026(3) -0.013(2) -0.012(2) 0.010(2) C3 0.034(3) 0.033(3) 0.028(3) -0.007(2) -0.005(2) 0.017(2) C4 0.031(3) 0.021(2) 0.026(3) -0.007(2) 0.001(2) 0.004(2) C5 0.033(3) 0.029(3) 0.021(3) -0.007(2) -0.009(2) 0.005(2) C6 0.026(3) 0.027(3) 0.022(3) -0.005(2) -0.004(2) 0.008(2) C7 0.035(3) 0.028(3) 0.022(3) -0.007(2) 0.004(2) 0.005(2) C8 0.019(2) 0.018(2) 0.020(2) 0.0031(19) -0.0034(18) -0.0031(18) C9 0.034(3) 0.019(2) 0.022(3) 0.005(2) 0.006(2) 0.005(2) C10 0.032(3) 0.031(3) 0.024(3) 0.008(2) 0.010(2) 0.006(2) C11 0.024(2) 0.021(2) 0.026(3) 0.008(2) 0.002(2) -0.003(2) C12 0.038(3) 0.018(2) 0.028(3) 0.007(2) 0.007(2) 0.008(2) C13 0.034(3) 0.027(3) 0.024(3) 0.004(2) 0.013(2) 0.006(2) C14 0.025(3) 0.030(3) 0.020(3) 0.007(2) -0.002(2) -0.004(2) N1 0.039(3) 0.038(3) 0.048(3) -0.005(2) -0.004(2) -0.008(2) N2 0.046(3) 0.029(3) 0.041(3) 0.011(2) -0.007(2) -0.006(2) C15 0.054(4) 0.075(5) 0.043(4) -0.008(4) 0.002(3) -0.014(4) C16 0.068(6) 0.094(7) 0.073(6) -0.037(5) 0.020(4) -0.011(5) C17 0.087(7) 0.103(8) 0.141(11) -0.088(8) 0.023(7) -0.010(6) C18 0.098(7) 0.047(5) 0.103(8) -0.027(5) 0.012(6) 0.003(5) C19 0.047(4) 0.032(3) 0.077(5) -0.009(3) 0.006(4) -0.002(3) C20 0.040(4) 0.028(3) 0.075(5) 0.011(3) -0.010(3) -0.001(3) C21 0.102(7) 0.037(4) 0.101(7) 0.014(5) -0.001(6) 0.004(4) C22 0.108(8) 0.063(6) 0.099(8) 0.047(6) -0.029(6) -0.004(5) C23 0.085(6) 0.061(5) 0.068(5) 0.032(4) -0.020(5) -0.028(5) C24 0.052(4) 0.053(4) 0.049(4) 0.018(3) -0.020(3) -0.014(3) O11 0.035(2) 0.034(2) 0.060(3) 0.000(2) 0.005(2) -0.0004(18) O12 0.032(2) 0.032(2) 0.044(2) -0.0007(19) -0.0020(18) 0.0015(17) O13 0.030(2) 0.034(2) 0.051(3) 0.009(2) 0.0024(19) 0.0023(17) O14 0.037(2) 0.039(2) 0.059(3) -0.001(2) 0.008(2) -0.0031(19) O15 0.139(6) 0.084(5) 0.079(4) -0.012(4) -0.015(5) 0.057(4) O16 0.060(4) 0.131(6) 0.055(3) -0.008(4) 0.009(3) -0.006(4) O17 0.184(8) 0.090(5) 0.077(5) -0.009(4) -0.023(5) -0.035(6) _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 O2 1.916(3) 3_765 ? Zn1 O9 1.937(3) 2_655 ? Zn1 O3 1.946(3) . ? Zn1 O7 1.978(3) . ? Zn2 O1 1.927(3) . ? Zn2 O4 1.954(3) 2_654 ? Zn2 O8 1.967(3) 4_565 ? Zn2 O10 1.980(3) 2_655 ? Zn3 O13 2.004(4) . ? Zn3 N2 2.089(5) . ? Zn3 O11 2.101(4) . ? Zn3 O12 2.143(4) . ? Zn3 N1 2.143(5) . ? Zn3 O14 2.180(4) . ? P1 O2 1.508(3) . ? P1 O3 1.522(3) . ? P1 O1 1.528(3) . ? P1 C1 1.807(4) . ? P2 O9 1.503(3) . ? P2 O8 1.523(3) . ? P2 O10 1.539(3) . ? P2 C8 1.809(5) . ? O2 Zn1 1.916(3) 3_765 ? O4 C7 1.281(6) . ? O4 Zn2 1.954(3) 2_644 ? O5 C7 1.214(6) . ? O6 C14 1.221(6) . ? O7 C14 1.274(6) . ? O8 Zn2 1.967(3) 4_666 ? O9 Zn1 1.937(3) 2_645 ? O10 Zn2 1.980(3) 2_645 ? C1 C6 1.368(6) . ? C1 C2 1.398(6) . ? C2 C3 1.379(7) . ? C2 H2 0.9300 . ? C3 C4 1.392(7) . ? C3 H3 0.9300 . ? C4 C5 1.386(7) . ? C4 C7 1.502(7) . ? C5 C6 1.396(7) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C9 1.385(7) . ? C8 C13 1.388(7) . ? C9 C10 1.376(7) . ? C9 H9 0.9300 . ? C10 C11 1.387(7) . ? C10 H10 0.9300 . ? C11 C12 1.375(7) . ? C11 C14 1.509(7) . ? C12 C13 1.388(7) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? N1 C15 1.324(8) . ? N1 C19 1.351(8) . ? N2 C24 1.323(8) . ? N2 C20 1.348(8) . ? C15 C16 1.396(11) . ? C15 H15 0.9300 . ? C16 C17 1.400(15) . ? C16 H16 0.9300 . ? C17 C18 1.354(15) . ? C17 H17 0.9300 . ? C18 C19 1.406(10) . ? C18 H18 0.9300 . ? C19 C20 1.469(10) . ? C20 C21 1.398(10) . ? C21 C22 1.368(13) . ? C21 H21 0.9300 . ? C22 C23 1.346(13) . ? C22 H22 0.9300 . ? C23 C24 1.364(9) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? O11 H11A 0.839(19) . ? O11 H11B 0.838(19) . ? O12 H12A 0.86(2) . ? O12 H12B 0.877(19) . ? O13 H13A 0.832(19) . ? O13 H13B 0.842(19) . ? O14 H14A 0.84(2) . ? O14 H14B 0.86(2) . ? O15 H15A 0.85(2) . ? O15 H15B 0.85(2) . ? O16 H16A 0.89(2) . ? O16 H16B 0.86(2) . ? O17 H17A 0.85(2) . ? O17 H17B 0.85(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Zn1 O9 109.58(14) 3_765 2_655 ? O2 Zn1 O3 116.00(15) 3_765 . ? O9 Zn1 O3 107.89(14) 2_655 . ? O2 Zn1 O7 111.45(14) 3_765 . ? O9 Zn1 O7 101.38(15) 2_655 . ? O3 Zn1 O7 109.49(14) . . ? O1 Zn2 O4 125.98(14) . 2_654 ? O1 Zn2 O8 113.63(13) . 4_565 ? O4 Zn2 O8 102.08(14) 2_654 4_565 ? O1 Zn2 O10 107.37(13) . 2_655 ? O4 Zn2 O10 100.13(14) 2_654 2_655 ? O8 Zn2 O10 105.36(14) 4_565 2_655 ? O13 Zn3 N2 168.97(18) . . ? O13 Zn3 O11 93.69(17) . . ? N2 Zn3 O11 93.95(18) . . ? O13 Zn3 O12 92.40(17) . . ? N2 Zn3 O12 96.04(18) . . ? O11 Zn3 O12 86.07(17) . . ? O13 Zn3 N1 94.43(19) . . ? N2 Zn3 N1 77.8(2) . . ? O11 Zn3 N1 88.51(18) . . ? O12 Zn3 N1 171.54(18) . . ? O13 Zn3 O14 87.32(17) . . ? N2 Zn3 O14 86.25(19) . . ? O11 Zn3 O14 171.77(18) . . ? O12 Zn3 O14 85.73(16) . . ? N1 Zn3 O14 99.56(18) . . ? O2 P1 O3 113.8(2) . . ? O2 P1 O1 111.30(18) . . ? O3 P1 O1 111.74(19) . . ? O2 P1 C1 110.5(2) . . ? O3 P1 C1 104.4(2) . . ? O1 P1 C1 104.42(19) . . ? O9 P2 O8 112.94(19) . . ? O9 P2 O10 112.6(2) . . ? O8 P2 O10 111.11(18) . . ? O9 P2 C8 105.7(2) . . ? O8 P2 C8 108.9(2) . . ? O10 P2 C8 105.04(19) . . ? P1 O1 Zn2 132.30(19) . . ? P1 O2 Zn1 135.8(2) . 3_765 ? P1 O3 Zn1 134.2(2) . . ? C7 O4 Zn2 117.2(3) . 2_644 ? C14 O7 Zn1 117.4(3) . . ? P2 O8 Zn2 138.8(2) . 4_666 ? P2 O9 Zn1 150.7(2) . 2_645 ? P2 O10 Zn2 126.17(19) . 2_645 ? C6 C1 C2 118.7(4) . . ? C6 C1 P1 120.7(4) . . ? C2 C1 P1 120.3(3) . . ? C3 C2 C1 120.7(4) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C2 C3 C4 120.0(5) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 119.7(5) . . ? C5 C4 C7 120.7(5) . . ? C3 C4 C7 119.5(5) . . ? C4 C5 C6 119.4(4) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C1 C6 C5 121.4(4) . . ? C1 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? O5 C7 O4 122.9(5) . . ? O5 C7 C4 121.1(5) . . ? O4 C7 C4 116.0(4) . . ? C9 C8 C13 118.5(4) . . ? C9 C8 P2 121.5(4) . . ? C13 C8 P2 120.0(4) . . ? C10 C9 C8 120.8(4) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C9 C10 C11 120.8(5) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C12 C11 C10 118.5(4) . . ? C12 C11 C14 121.7(4) . . ? C10 C11 C14 119.8(5) . . ? C11 C12 C13 121.0(5) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C8 C13 C12 120.3(5) . . ? C8 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? O6 C14 O7 123.5(5) . . ? O6 C14 C11 120.1(5) . . ? O7 C14 C11 116.4(4) . . ? C15 N1 C19 120.7(6) . . ? C15 N1 Zn3 125.4(5) . . ? C19 N1 Zn3 113.5(5) . . ? C24 N2 C20 119.8(6) . . ? C24 N2 Zn3 124.5(4) . . ? C20 N2 Zn3 115.7(4) . . ? N1 C15 C16 123.4(8) . . ? N1 C15 H15 118.3 . . ? C16 C15 H15 118.3 . . ? C15 C16 C17 116.0(9) . . ? C15 C16 H16 122.0 . . ? C17 C16 H16 122.0 . . ? C18 C17 C16 120.7(8) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C17 C18 C19 120.5(9) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? N1 C19 C18 118.8(8) . . ? N1 C19 C20 116.4(6) . . ? C18 C19 C20 124.9(7) . . ? N2 C20 C21 117.9(7) . . ? N2 C20 C19 115.9(5) . . ? C21 C20 C19 126.0(7) . . ? C22 C21 C20 120.3(8) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C23 C22 C21 120.5(8) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 C24 117.0(8) . . ? C22 C23 H23 121.5 . . ? C24 C23 H23 121.5 . . ? N2 C24 C23 124.2(8) . . ? N2 C24 H24 117.9 . . ? C23 C24 H24 117.9 . . ? Zn3 O11 H11A 127(4) . . ? Zn3 O11 H11B 121(4) . . ? H11A O11 H11B 110(3) . . ? Zn3 O12 H12A 114(4) . . ? Zn3 O12 H12B 116(4) . . ? H12A O12 H12B 102(3) . . ? Zn3 O13 H13A 106(4) . . ? Zn3 O13 H13B 133(4) . . ? H13A O13 H13B 109(3) . . ? Zn3 O14 H14A 154(4) . . ? Zn3 O14 H14B 99(4) . . ? H14A O14 H14B 105(3) . . ? H15A O15 H15B 105(3) . . ? H16A O16 H16B 100(3) . . ? H17A O17 H17B 106(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O11 H11A O15 0.839(19) 1.96(2) 2.787(7) 171(8) 1_655 O11 H11B O3 0.838(19) 2.03(3) 2.818(5) 156(7) . O14 H14B O4 0.86(2) 1.94(3) 2.773(6) 162(6) 4_566 O14 H14A O16 0.84(2) 2.32(7) 2.797(8) 117(6) . O13 H13B O1 0.842(19) 1.92(3) 2.744(5) 168(7) . O16 H16B O6 0.86(2) 1.87(3) 2.724(7) 173(10) 1_455 O13 H13A O10 0.832(19) 1.98(3) 2.780(5) 162(6) 4_565 O12 H12A O7 0.86(2) 1.94(2) 2.786(5) 168(5) . O12 H12B O8 0.877(19) 1.94(2) 2.818(5) 177(7) 2_655 O16 H16A O15 0.89(2) 2.53(8) 3.199(11) 132(8) . _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.785 _refine_diff_density_min -1.034 _refine_diff_density_rms 0.127