# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Li-Min Zheng' 'Deng-Ke Cao' 'Yan Duan' 'Yi-Zhi Li' 'Peng-Fei Wang' _publ_contact_author_name 'Li-Min Zheng' _publ_contact_author_email LMZHENG@NETRA.NJU.EDU.CN _publ_section_title ; Metal carboxylate-phosphonates containing flexible N-donor co-ligands ; # Attachment '1.cif' data_a _database_code_depnum_ccdc_archive 'CCDC 765762' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H12 N2 O5 P Zn' _chemical_formula_weight 384.60 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)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.656(2) _cell_length_b 5.5714(10) _cell_length_c 21.744(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.859(4) _cell_angle_gamma 90.00 _cell_volume 1408.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 1178 _cell_measurement_theta_min 2.4755 _cell_measurement_theta_max 21.529 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.813 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 1.885 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7042 _exptl_absorpt_correction_T_max 0.9116 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7195 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_av_sigmaI/netI 0.0924 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2757 _reflns_number_gt 1827 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0075P)^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 2757 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0667 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.0691 _refine_ls_wR_factor_gt 0.0664 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _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 0.00330(5) 0.35546(8) 0.32828(2) 0.02299(15) Uani 1 1 d . . . P1 P 0.13507(10) 0.8556(2) 0.30692(5) 0.0222(3) Uani 1 1 d . . . O1 O 0.1174(2) 0.8744(5) 0.23687(11) 0.0311(8) Uani 1 1 d . . . O2 O 0.1188(3) 0.6026(4) 0.33015(12) 0.0297(8) Uani 1 1 d . . . O3 O 0.0657(3) 1.0364(5) 0.33951(12) 0.0291(8) Uani 1 1 d . . . O5 O 0.7157(3) 0.9539(6) 0.3578(2) 0.0856(15) Uani 1 1 d . . . O4 O 0.6702(3) 1.2877(6) 0.30946(18) 0.0572(11) Uani 1 1 d . . . H4 H 0.7403 1.2988 0.3090 0.086 Uiso 1 1 calc R . . N1 N -0.0796(3) 0.3821(6) 0.40595(14) 0.0250(9) Uani 1 1 d . . . N2 N -0.1810(3) 0.5101(6) 0.48099(17) 0.0315(10) Uani 1 1 d . . . C1 C 0.2836(4) 0.9288(7) 0.32255(17) 0.0214(11) Uani 1 1 d . . . C2 C 0.3259(4) 1.1469(8) 0.30199(17) 0.0292(11) Uani 1 1 d . . . H2 H 0.2744 1.2600 0.2849 0.035 Uiso 1 1 calc R . . C3 C 0.4405(4) 1.1987(7) 0.30633(18) 0.0299(12) Uani 1 1 d . . . H3 H 0.4659 1.3454 0.2920 0.036 Uiso 1 1 calc R . . C4 C 0.5201(4) 1.0332(7) 0.33211(19) 0.0252(11) Uani 1 1 d . . . C5 C 0.4790(4) 0.8210(8) 0.35473(18) 0.0313(12) Uani 1 1 d . . . H5 H 0.5302 0.7111 0.3735 0.038 Uiso 1 1 calc R . . C6 C 0.3639(4) 0.7699(7) 0.34996(18) 0.0279(12) Uani 1 1 d . . . H6 H 0.3386 0.6251 0.3655 0.033 Uiso 1 1 calc R . . C8 C -0.1498(4) 0.5489(8) 0.4237(2) 0.0319(12) Uani 1 1 d . . . H8 H -0.1748 0.6784 0.3993 0.038 Uiso 1 1 calc R . . C9 C -0.0665(4) 0.2267(8) 0.4546(2) 0.0358(13) Uani 1 1 d . . . H9 H -0.0214 0.0887 0.4556 0.043 Uiso 1 1 calc R . . C10 C -0.1286(4) 0.3032(8) 0.5012(2) 0.0391(14) Uani 1 1 d . . . H10 H -0.1345 0.2296 0.5392 0.047 Uiso 1 1 calc R . . C11 C -0.2614(4) 0.6526(9) 0.5139(2) 0.0413(13) Uani 1 1 d . . . H11A H -0.2578 0.8175 0.4998 0.050 Uiso 1 1 calc R . . H11B H -0.2372 0.6508 0.5574 0.050 Uiso 1 1 calc R . . C12 C -0.3838(4) 0.5689(8) 0.50602(19) 0.0298(12) Uani 1 1 d . . . C13 C -0.4182(4) 0.3577(8) 0.47651(19) 0.0368(12) Uani 1 1 d . . . H13 H -0.3632 0.2599 0.4602 0.044 Uiso 1 1 calc R . . C14 C -0.4693(4) 0.7098(7) 0.52909(19) 0.0336(13) Uani 1 1 d . . . H14 H -0.4492 0.8534 0.5488 0.040 Uiso 1 1 calc R . . C7 C 0.6437(5) 1.0818(9) 0.3347(2) 0.0348(13) 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 0.0236(3) 0.0225(3) 0.0232(3) -0.0001(3) 0.0035(2) -0.0002(3) P1 0.0216(7) 0.0194(6) 0.0258(6) 0.0001(6) 0.0026(5) 0.0000(6) O1 0.028(2) 0.0436(19) 0.0214(16) 0.0019(15) -0.0023(14) 0.0023(17) O2 0.028(2) 0.0189(17) 0.0426(18) 0.0041(14) 0.0026(15) -0.0037(15) O3 0.032(2) 0.0219(16) 0.0347(18) 0.0021(14) 0.0095(16) 0.0063(15) O5 0.031(3) 0.056(3) 0.166(4) 0.046(3) -0.020(3) -0.002(2) O4 0.033(2) 0.072(3) 0.068(2) 0.029(2) 0.007(2) -0.010(2) N1 0.024(2) 0.028(2) 0.024(2) 0.0030(18) 0.0058(17) 0.0040(19) N2 0.029(3) 0.037(2) 0.030(2) -0.0043(19) 0.009(2) -0.001(2) C1 0.025(3) 0.020(3) 0.019(2) -0.0031(19) 0.002(2) -0.003(2) C2 0.029(3) 0.024(3) 0.035(3) 0.001(2) -0.001(2) 0.002(3) C3 0.032(3) 0.026(3) 0.032(3) 0.003(2) 0.005(2) -0.007(2) C4 0.023(3) 0.028(3) 0.024(3) -0.003(2) 0.000(2) 0.000(2) C5 0.032(3) 0.027(3) 0.034(3) 0.000(2) -0.007(2) 0.004(2) C6 0.032(3) 0.021(3) 0.031(3) 0.003(2) 0.003(2) -0.004(2) C8 0.031(3) 0.036(3) 0.029(3) 0.002(2) 0.003(2) 0.002(2) C9 0.039(4) 0.032(3) 0.037(3) 0.006(2) 0.009(3) 0.011(2) C10 0.048(4) 0.039(3) 0.031(3) 0.009(2) 0.009(3) 0.007(3) C11 0.040(4) 0.043(3) 0.043(3) -0.011(3) 0.017(3) 0.001(3) C12 0.035(3) 0.032(3) 0.023(3) -0.001(2) 0.008(2) 0.001(2) C13 0.038(3) 0.035(3) 0.040(3) -0.008(3) 0.014(3) 0.008(3) C14 0.036(4) 0.029(3) 0.037(3) -0.008(2) 0.011(3) -0.002(2) C7 0.033(4) 0.036(3) 0.035(3) -0.001(2) -0.001(3) -0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O2 1.924(3) . ? Zn1 O3 1.930(3) 1_545 ? Zn1 O1 1.931(3) 2_545 ? Zn1 N1 2.007(3) . ? P1 O3 1.500(3) . ? P1 O2 1.513(3) . ? P1 O1 1.527(3) . ? P1 C1 1.788(5) . ? O1 Zn1 1.931(3) 2 ? O3 Zn1 1.930(3) 1_565 ? O5 C7 1.186(5) . ? O4 C7 1.317(5) . ? O4 H4 0.8200 . ? N1 C8 1.312(5) . ? N1 C9 1.368(5) . ? N2 C8 1.339(5) . ? N2 C10 1.363(5) . ? N2 C11 1.453(5) . ? C1 C6 1.393(5) . ? C1 C2 1.396(5) . ? C2 C3 1.364(6) . ? C2 H2 0.9300 . ? C3 C4 1.398(6) . ? C3 H3 0.9300 . ? C4 C5 1.379(5) . ? C4 C7 1.463(6) . ? C5 C6 1.368(6) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 H8 0.9300 . ? C9 C10 1.353(6) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.499(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.386(5) . ? C12 C14 1.389(6) . ? C13 C14 1.362(6) 3_466 ? C13 H13 0.9300 . ? C14 C13 1.362(6) 3_466 ? C14 H14 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 O2 Zn1 O3 113.54(13) . 1_545 ? O2 Zn1 O1 116.77(12) . 2_545 ? O3 Zn1 O1 113.14(12) 1_545 2_545 ? O2 Zn1 N1 107.77(13) . . ? O3 Zn1 N1 99.23(13) 1_545 . ? O1 Zn1 N1 104.17(13) 2_545 . ? O3 P1 O2 112.59(16) . . ? O3 P1 O1 112.61(17) . . ? O2 P1 O1 112.68(17) . . ? O3 P1 C1 107.62(18) . . ? O2 P1 C1 106.90(18) . . ? O1 P1 C1 103.74(17) . . ? P1 O1 Zn1 140.40(19) . 2 ? P1 O2 Zn1 139.72(18) . . ? P1 O3 Zn1 140.34(17) . 1_565 ? C7 O4 H4 109.5 . . ? C8 N1 C9 105.1(4) . . ? C8 N1 Zn1 130.1(3) . . ? C9 N1 Zn1 124.7(3) . . ? C8 N2 C10 107.0(4) . . ? C8 N2 C11 126.5(4) . . ? C10 N2 C11 126.4(4) . . ? C6 C1 C2 116.6(4) . . ? C6 C1 P1 123.4(3) . . ? C2 C1 P1 119.7(3) . . ? C3 C2 C1 121.8(4) . . ? C3 C2 H2 119.1 . . ? C1 C2 H2 119.1 . . ? C2 C3 C4 120.6(4) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C5 C4 C3 118.2(4) . . ? C5 C4 C7 120.6(4) . . ? C3 C4 C7 121.2(4) . . ? C6 C5 C4 120.9(4) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C1 121.9(4) . . ? C5 C6 H6 119.1 . . ? C1 C6 H6 119.1 . . ? N1 C8 N2 111.9(4) . . ? N1 C8 H8 124.1 . . ? N2 C8 H8 124.1 . . ? C10 C9 N1 110.0(4) . . ? C10 C9 H9 125.0 . . ? N1 C9 H9 125.0 . . ? C9 C10 N2 106.0(4) . . ? C9 C10 H10 127.0 . . ? N2 C10 H10 127.0 . . ? N2 C11 C12 114.5(4) . . ? N2 C11 H11A 108.6 . . ? C12 C11 H11A 108.6 . . ? N2 C11 H11B 108.6 . . ? C12 C11 H11B 108.6 . . ? H11A C11 H11B 107.6 . . ? C13 C12 C14 117.0(5) . . ? C13 C12 C11 124.1(5) . . ? C14 C12 C11 118.9(4) . . ? C14 C13 C12 121.5(4) 3_466 . ? C14 C13 H13 119.2 3_466 . ? C12 C13 H13 119.2 . . ? C13 C14 C12 121.4(4) 3_466 . ? C13 C14 H14 119.3 3_466 . ? C12 C14 H14 119.3 . . ? O5 C7 O4 121.3(5) . . ? O5 C7 C4 124.9(5) . . ? O4 C7 C4 113.8(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.600 _refine_diff_density_min -0.637 _refine_diff_density_rms 0.087 # Attachment '2.cif' data_90528a _database_code_depnum_ccdc_archive 'CCDC 765763' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H82 N16 O25 P4 Zn6' _chemical_formula_weight 2231.76 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 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4078(11) _cell_length_b 14.294(2) _cell_length_c 16.0271(13) _cell_angle_alpha 86.884(2) _cell_angle_beta 80.178(3) _cell_angle_gamma 73.201(2) _cell_volume 2249.1(4) _cell_formula_units_Z 1 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 1813 _cell_measurement_theta_min 2.351 _cell_measurement_theta_max 22.0735 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.648 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1138 _exptl_absorpt_coefficient_mu 1.731 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6428 _exptl_absorpt_correction_T_max 0.7233 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12215 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_av_sigmaI/netI 0.0571 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8628 _reflns_number_gt 6451 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0766P)^2^+0.0146P] 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 8628 _refine_ls_number_parameters 613 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0713 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1314 _refine_ls_wR_factor_gt 0.1246 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4923(4) 0.8775(3) 0.4608(3) 0.0332(9) Uani 1 1 d . . . H1 H 0.5031 0.8746 0.4021 0.040 Uiso 1 1 calc R . . C2 C 0.4052(5) 0.8881(3) 0.5906(3) 0.0388(10) Uani 1 1 d . . . H2 H 0.3424 0.8939 0.6402 0.047 Uiso 1 1 calc R . . C3 C 0.5378(5) 0.8778(4) 0.5861(3) 0.0439(11) Uani 1 1 d . . . H3 H 0.5832 0.8759 0.6316 0.053 Uiso 1 1 calc R . . C4 C 0.7390(5) 0.8449(4) 0.4660(3) 0.0412(10) Uani 1 1 d . . . H4A H 0.7888 0.8644 0.5047 0.049 Uiso 1 1 calc R . . H4B H 0.7493 0.8817 0.4139 0.049 Uiso 1 1 calc R . . C5 C 0.7999(5) 0.7396(3) 0.4476(3) 0.0369(9) Uani 1 1 d . . . C6 C 0.9247(5) 0.7116(3) 0.3972(3) 0.0394(10) Uani 1 1 d . . . H6 H 0.9680 0.7581 0.3747 0.047 Uiso 1 1 calc R . . C7 C 0.9856(5) 0.6137(4) 0.3801(3) 0.0456(11) Uani 1 1 d . . . H7 H 1.0715 0.5940 0.3474 0.055 Uiso 1 1 calc R . . C8 C 0.9207(5) 0.5454(4) 0.4109(3) 0.0477(12) Uani 1 1 d . . . H8 H 0.9611 0.4800 0.3968 0.057 Uiso 1 1 calc R . . C9 C 0.7978(5) 0.5722(3) 0.4620(3) 0.0389(10) Uani 1 1 d . . . C10 C 0.7370(5) 0.6689(3) 0.4782(3) 0.0420(11) Uani 1 1 d . . . H10 H 0.6508 0.6878 0.5108 0.050 Uiso 1 1 calc R . . C11 C 0.7250(5) 0.4965(3) 0.4968(3) 0.0398(10) Uani 1 1 d . . . H11A H 0.7880 0.4424 0.5210 0.048 Uiso 1 1 calc R . . H11B H 0.6510 0.5257 0.5416 0.048 Uiso 1 1 calc R . . C12 C 0.6996(5) 0.3672(3) 0.4020(3) 0.0405(11) Uani 1 1 d . . . H12 H 0.7555 0.3107 0.4225 0.049 Uiso 1 1 calc R . . C13 C 0.6299(5) 0.3746(3) 0.3369(3) 0.0374(10) Uani 1 1 d . . . H13 H 0.6308 0.3223 0.3045 0.045 Uiso 1 1 calc R . . C14 C 0.5857(5) 0.5182(4) 0.3822(3) 0.0439(11) Uani 1 1 d . . . H14 H 0.5508 0.5856 0.3885 0.053 Uiso 1 1 calc R . . C15 C 0.0201(5) 1.0660(3) 0.0894(3) 0.0425(11) Uani 1 1 d . . . H15A H -0.0718 1.0917 0.1105 0.051 Uiso 1 1 calc R . . C16 C 0.2220(5) 0.9712(4) 0.0699(3) 0.0462(12) Uani 1 1 d . . . H16A H 0.2987 0.9191 0.0739 0.055 Uiso 1 1 calc R . . C17 C 0.2170(5) 1.0503(4) 0.0167(3) 0.0479(12) Uani 1 1 d . . . H17A H 0.2891 1.0612 -0.0217 0.057 Uiso 1 1 calc R . . C18 C 0.0364(6) 1.2040(4) -0.0072(4) 0.0488(12) Uani 1 1 d . . . H18A H -0.0563 1.2116 -0.0153 0.059 Uiso 1 1 calc R . . H18B H 0.0902 1.2067 -0.0626 0.059 Uiso 1 1 calc R . . C19 C 0.0383(5) 1.2872(3) 0.0448(3) 0.0378(10) Uani 1 1 d . . . C20 C -0.0488(5) 1.3098(4) 0.1205(3) 0.0460(12) Uani 1 1 d . . . H20A H -0.1097 1.2736 0.1386 0.055 Uiso 1 1 calc R . . C21 C -0.0469(5) 1.3850(3) 0.1694(3) 0.0426(11) Uani 1 1 d . . . H21A H -0.1046 1.3981 0.2211 0.051 Uiso 1 1 calc R . . C22 C 0.0399(5) 1.4415(4) 0.1427(3) 0.0425(11) Uani 1 1 d . . . H22A H 0.0396 1.4930 0.1758 0.051 Uiso 1 1 calc R . . C23 C 0.1267(5) 1.4214(4) 0.0670(3) 0.0404(10) Uani 1 1 d . . . C24 C 0.1262(6) 1.3448(4) 0.0169(3) 0.0485(12) Uani 1 1 d . . . H24A H 0.1840 1.3319 -0.0348 0.058 Uiso 1 1 calc R . . C25 C 0.2166(6) 1.4880(3) 0.0404(3) 0.0481(13) Uani 1 1 d . . . H25A H 0.1633 1.5467 0.0169 0.058 Uiso 1 1 d R . . H25B H 0.2435 1.5060 0.0902 0.058 Uiso 1 1 d R . . C26 C 0.4433(6) 1.3684(4) -0.0127(3) 0.0479(12) Uani 1 1 d . . . H26A H 0.4507 1.3248 0.0326 0.058 Uiso 1 1 calc R . . C27 C 0.5334(5) 1.3647(4) -0.0824(3) 0.0493(13) Uani 1 1 d . . . H27A H 0.6151 1.3157 -0.0943 0.059 Uiso 1 1 calc R . . C28 C 0.3721(5) 1.4897(3) -0.0936(3) 0.0422(11) Uani 1 1 d . . . H28A H 0.3175 1.5468 -0.1141 0.051 Uiso 1 1 calc R . . C29 C -0.1096(5) 0.8304(3) 0.6813(3) 0.0363(10) Uani 1 1 d . . . C30 C -0.1979(5) 0.8460(3) 0.7562(3) 0.0369(10) Uani 1 1 d . . . H30 H -0.2073 0.9005 0.7884 0.044 Uiso 1 1 calc R . . C31 C -0.2734(5) 0.7818(3) 0.7848(3) 0.0340(9) Uani 1 1 d . . . H31 H -0.3345 0.7944 0.8352 0.041 Uiso 1 1 calc R . . C32 C -0.2585(4) 0.7002(3) 0.7393(3) 0.0333(9) Uani 1 1 d . . . C33 C -0.1680(4) 0.6822(3) 0.6649(3) 0.0347(9) Uani 1 1 d . . . H33 H -0.1567 0.6267 0.6335 0.042 Uiso 1 1 calc R . . C34 C -0.0943(4) 0.7466(3) 0.6373(3) 0.0325(9) Uani 1 1 d . . . H34 H -0.0320 0.7333 0.5874 0.039 Uiso 1 1 calc R . . C35 C -0.3442(4) 0.6322(3) 0.7675(3) 0.0326(9) Uani 1 1 d . . . C36 C 0.4326(4) 0.8043(3) 0.2669(3) 0.0345(9) Uani 1 1 d . . . C37 C 0.5639(5) 0.7440(4) 0.2586(3) 0.0455(11) Uani 1 1 d . . . H37 H 0.5787 0.6769 0.2650 0.055 Uiso 1 1 calc R . . C38 C 0.6752(5) 0.7820(3) 0.2406(3) 0.0383(10) Uani 1 1 d . . . H38 H 0.7627 0.7399 0.2370 0.046 Uiso 1 1 calc R . . C39 C 0.6575(5) 0.8817(4) 0.2281(3) 0.0393(10) Uani 1 1 d . . . C40 C 0.5246(5) 0.9423(3) 0.2325(3) 0.0419(11) Uani 1 1 d . . . H40 H 0.5098 1.0087 0.2211 0.050 Uiso 1 1 calc R . . C41 C 0.4150(5) 0.9047(3) 0.2535(3) 0.0412(11) Uani 1 1 d . . . H41 H 0.3273 0.9470 0.2589 0.049 Uiso 1 1 calc R . . C42 C 0.7738(5) 0.9261(3) 0.2148(3) 0.0347(9) Uani 1 1 d . . . N1 N 0.3765(4) 0.8887(3) 0.5102(2) 0.0370(8) Uani 1 1 d . . . N2 N 0.5941(4) 0.8705(3) 0.5034(2) 0.0360(8) Uani 1 1 d . . . N3 N 0.5588(4) 0.4682(3) 0.3253(3) 0.0389(8) Uani 1 1 d . . . N4 N 0.6708(4) 0.4598(3) 0.4310(3) 0.0395(9) Uani 1 1 d . . . N5 N 0.0970(4) 0.9815(3) 0.1154(2) 0.0359(8) Uani 1 1 d . . . N6 N 0.0885(4) 1.1094(3) 0.0302(2) 0.0372(8) Uani 1 1 d . . . N7 N 0.3386(4) 1.4481(3) -0.0207(2) 0.0423(9) Uani 1 1 d . . . N8 N 0.4918(4) 1.4406(3) -0.1336(2) 0.0334(8) Uani 1 1 d . . . O1 O -0.0051(3) 0.9802(2) 0.6939(2) 0.0421(7) Uani 1 1 d . . . O2 O -0.1344(3) 0.9802(2) 0.57732(19) 0.0356(7) Uani 1 1 d . . . O3 O 0.0962(3) 0.8645(2) 0.5760(2) 0.0382(7) Uani 1 1 d . . . O4 O -0.2943(3) 0.5464(2) 0.7358(2) 0.0433(8) Uani 1 1 d . . . O5 O -0.4536(3) 0.6581(2) 0.8142(2) 0.0433(8) Uani 1 1 d . . . O6 O 0.2316(3) 0.7940(2) 0.3920(2) 0.0382(7) Uani 1 1 d . . . O7 O 0.3307(3) 0.6524(2) 0.2982(2) 0.0387(7) Uani 1 1 d . . . O8 O 0.1876(3) 0.8045(2) 0.2423(2) 0.0401(7) Uani 1 1 d . . . O9 O 0.7573(3) 1.0113(2) 0.1962(2) 0.0394(7) Uani 1 1 d . . . O10 O 0.8886(3) 0.8654(2) 0.22558(19) 0.0321(6) Uani 1 1 d . . . O1W O 0.0850(4) 0.6678(2) 0.1682(2) 0.0444(8) Uani 1 1 d . . . H1X H 0.1441 0.6947 0.1431 0.053 Uiso 1 1 d R . . H1Y H 0.0727 0.6942 0.2163 0.053 Uiso 1 1 d R . . O2W O 0.3257(4) 0.8094(2) 0.8805(2) 0.0502(9) Uani 1 1 d . . . H2X H 0.3996 0.8011 0.8459 0.060 Uiso 1 1 d R . . H2Y H 0.3414 0.7508 0.8986 0.060 Uiso 1 1 d R . . O3W O 0.5369(6) 0.8728(4) 0.9969(4) 0.0388(14) Uani 0.50 1 d P . . H3X H 0.5462 0.8242 1.0305 0.047 Uiso 0.50 1 d PR . . H3Y H 0.5301 0.8552 0.9484 0.047 Uiso 0.50 1 d PR . . P1 P -0.03180(11) 0.92173(8) 0.62936(7) 0.0295(2) Uani 1 1 d . . . P2 P 0.28586(11) 0.76139(8) 0.30234(7) 0.0302(2) Uani 1 1 d . . . Zn1 Zn 0.19887(5) 0.89535(3) 0.47238(3) 0.03057(13) Uani 1 1 d . . . Zn2 Zn 0.42342(5) 0.52913(3) 0.24754(3) 0.02897(13) Uani 1 1 d . . . Zn3 Zn 0.04065(5) 0.91887(3) 0.22506(3) 0.02758(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.036(2) 0.038(2) 0.0265(19) -0.0022(17) -0.0091(18) -0.0095(18) C2 0.037(2) 0.039(2) 0.039(2) -0.0019(19) -0.011(2) -0.0047(19) C3 0.040(3) 0.056(3) 0.033(2) -0.008(2) -0.012(2) -0.005(2) C4 0.034(2) 0.052(3) 0.043(3) -0.001(2) -0.015(2) -0.016(2) C5 0.039(2) 0.043(2) 0.034(2) -0.0052(18) -0.0160(19) -0.0117(19) C6 0.031(2) 0.041(2) 0.052(3) 0.006(2) -0.003(2) -0.0221(19) C7 0.030(2) 0.058(3) 0.040(3) -0.005(2) 0.003(2) -0.003(2) C8 0.045(3) 0.052(3) 0.044(3) -0.009(2) -0.010(2) -0.007(2) C9 0.033(2) 0.043(2) 0.042(2) -0.005(2) -0.011(2) -0.0081(19) C10 0.038(3) 0.046(3) 0.039(2) -0.001(2) -0.017(2) -0.001(2) C11 0.050(3) 0.035(2) 0.040(2) 0.0074(19) -0.025(2) -0.011(2) C12 0.050(3) 0.030(2) 0.048(3) 0.0013(19) -0.023(2) -0.014(2) C13 0.043(3) 0.032(2) 0.045(2) 0.0080(18) -0.017(2) -0.0200(19) C14 0.038(3) 0.040(3) 0.050(3) 0.005(2) -0.017(2) 0.000(2) C15 0.038(3) 0.036(2) 0.051(3) 0.003(2) -0.002(2) -0.010(2) C16 0.038(3) 0.041(2) 0.054(3) -0.007(2) 0.006(2) -0.009(2) C17 0.046(3) 0.042(3) 0.049(3) -0.004(2) 0.011(2) -0.012(2) C18 0.044(3) 0.045(3) 0.058(3) 0.010(2) -0.014(2) -0.010(2) C19 0.040(2) 0.037(2) 0.040(2) 0.0118(19) -0.011(2) -0.0158(19) C20 0.043(3) 0.050(3) 0.044(3) 0.015(2) 0.001(2) -0.020(2) C21 0.038(3) 0.043(3) 0.043(2) 0.008(2) 0.004(2) -0.014(2) C22 0.047(3) 0.041(2) 0.034(2) 0.0051(19) 0.001(2) -0.008(2) C23 0.039(3) 0.046(3) 0.031(2) 0.0142(19) 0.0013(19) -0.010(2) C24 0.055(3) 0.050(3) 0.035(2) 0.009(2) 0.006(2) -0.016(2) C25 0.059(3) 0.035(2) 0.042(3) -0.008(2) 0.016(2) -0.011(2) C26 0.053(3) 0.044(3) 0.044(3) 0.008(2) -0.014(2) -0.006(2) C27 0.040(3) 0.043(3) 0.050(3) 0.003(2) 0.004(2) 0.006(2) C28 0.043(3) 0.039(2) 0.044(3) 0.014(2) 0.000(2) -0.017(2) C29 0.033(2) 0.027(2) 0.046(3) 0.0086(18) -0.011(2) -0.0040(17) C30 0.034(2) 0.033(2) 0.042(2) -0.0014(18) -0.006(2) -0.0093(18) C31 0.042(2) 0.030(2) 0.0254(19) 0.0051(16) 0.0014(18) -0.0074(18) C32 0.029(2) 0.038(2) 0.033(2) 0.0063(17) -0.0071(18) -0.0084(18) C33 0.035(2) 0.038(2) 0.035(2) -0.0119(18) -0.0058(19) -0.0138(18) C34 0.026(2) 0.034(2) 0.034(2) -0.0037(17) 0.0000(17) -0.0040(16) C35 0.026(2) 0.033(2) 0.037(2) 0.0009(17) -0.0065(18) -0.0071(17) C36 0.028(2) 0.046(2) 0.029(2) -0.0038(17) -0.0045(17) -0.0110(18) C37 0.044(3) 0.035(2) 0.053(3) -0.006(2) 0.000(2) -0.009(2) C38 0.029(2) 0.035(2) 0.048(3) -0.0074(19) -0.0061(19) -0.0044(17) C39 0.041(3) 0.045(2) 0.035(2) 0.0003(19) -0.0078(19) -0.016(2) C40 0.039(3) 0.033(2) 0.051(3) 0.007(2) -0.008(2) -0.0070(19) C41 0.039(3) 0.031(2) 0.055(3) 0.000(2) -0.019(2) -0.0061(19) C42 0.039(2) 0.033(2) 0.031(2) 0.0015(17) -0.0045(18) -0.0087(18) N1 0.0289(19) 0.0368(19) 0.041(2) 0.0018(16) -0.0040(16) -0.0047(15) N2 0.036(2) 0.043(2) 0.0333(18) -0.0046(16) -0.0142(16) -0.0130(17) N3 0.0308(19) 0.045(2) 0.043(2) 0.0023(17) -0.0110(17) -0.0122(17) N4 0.047(2) 0.0286(18) 0.049(2) 0.0097(16) -0.0234(19) -0.0120(16) N5 0.037(2) 0.039(2) 0.0374(19) 0.0015(16) -0.0024(16) -0.0207(16) N6 0.044(2) 0.042(2) 0.0341(19) 0.0065(16) -0.0089(16) -0.0257(17) N7 0.041(2) 0.042(2) 0.0345(19) 0.0034(16) 0.0154(17) -0.0091(17) N8 0.0334(19) 0.0341(18) 0.0313(18) -0.0023(14) -0.0052(15) -0.0067(15) O1 0.0467(19) 0.0452(18) 0.0373(17) -0.0041(14) -0.0144(15) -0.0125(15) O2 0.0398(17) 0.0308(15) 0.0397(16) 0.0102(12) -0.0169(14) -0.0115(13) O3 0.0297(16) 0.0297(15) 0.0423(17) 0.0049(13) 0.0050(13) 0.0045(12) O4 0.0424(19) 0.0454(18) 0.0475(19) -0.0012(15) 0.0009(15) -0.0254(15) O5 0.0417(18) 0.0391(17) 0.0475(19) -0.0082(14) 0.0141(15) -0.0201(14) O6 0.0408(18) 0.0340(16) 0.0354(16) 0.0029(13) -0.0012(14) -0.0075(13) O7 0.0285(16) 0.0360(16) 0.0460(18) -0.0119(14) 0.0068(14) -0.0055(13) O8 0.0276(16) 0.0507(18) 0.0496(18) 0.0143(15) -0.0147(14) -0.0207(14) O9 0.0395(18) 0.0369(16) 0.0464(18) 0.0160(14) -0.0099(14) -0.0192(14) O10 0.0279(15) 0.0347(15) 0.0422(17) 0.0040(12) -0.0097(13) -0.0204(13) O1W 0.049(2) 0.0413(18) 0.0493(19) -0.0124(15) -0.0156(16) -0.0167(15) O2W 0.056(2) 0.0402(18) 0.0478(19) 0.0063(15) -0.0071(17) -0.0050(16) O3W 0.039(3) 0.037(3) 0.043(3) 0.011(3) -0.013(3) -0.014(3) P1 0.0311(6) 0.0274(5) 0.0285(5) 0.0012(4) -0.0013(4) -0.0083(4) P2 0.0255(5) 0.0305(5) 0.0346(5) -0.0049(4) -0.0025(4) -0.0084(4) Zn1 0.0302(3) 0.0312(2) 0.0279(2) 0.00289(18) -0.00117(19) -0.00747(19) Zn2 0.0277(3) 0.0318(2) 0.0279(2) -0.00105(18) 0.00045(19) -0.01178(19) Zn3 0.0292(3) 0.0285(2) 0.0340(2) 0.00402(18) -0.00966(19) -0.02044(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.297(6) . ? C1 N2 1.333(5) . ? C1 H1 0.9300 . ? C2 C3 1.335(7) . ? C2 N1 1.369(6) . ? C2 H2 0.9300 . ? C3 N2 1.350(6) . ? C3 H3 0.9300 . ? C4 N2 1.471(6) . ? C4 C5 1.480(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.370(6) . ? C5 C10 1.382(7) . ? C6 C7 1.381(7) . ? C6 H6 0.9300 . ? C7 C8 1.366(8) . ? C7 H7 0.9300 . ? C8 C9 1.359(7) . ? C8 H8 0.9300 . ? C9 C10 1.362(7) . ? C9 C11 1.523(7) . ? C10 H10 0.9300 . ? C11 N4 1.463(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.352(6) . ? C12 N4 1.360(6) . ? C12 H12 0.9300 . ? C13 N3 1.349(6) . ? C13 H13 0.9300 . ? C14 N3 1.302(6) . ? C14 N4 1.353(6) . ? C14 H14 0.9300 . ? C15 N6 1.323(6) . ? C15 N5 1.331(6) . ? C15 H15A 0.9300 . ? C16 N5 1.351(6) . ? C16 C17 1.373(7) . ? C16 H16A 0.9300 . ? C17 N6 1.348(6) . ? C17 H17A 0.9300 . ? C18 N6 1.442(6) . ? C18 C19 1.495(7) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.377(7) . ? C19 C24 1.404(7) . ? C20 C21 1.372(7) . ? C20 H20A 0.9300 . ? C21 C22 1.379(7) . ? C21 H21A 0.9300 . ? C22 C23 1.372(6) . ? C22 H22A 0.9300 . ? C23 C24 1.394(7) . ? C23 C25 1.516(7) . ? C24 H24A 0.9300 . ? C25 N7 1.453(6) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C26 C27 1.323(7) . ? C26 N7 1.347(6) . ? C26 H26A 0.9300 . ? C27 N8 1.338(6) . ? C27 H27A 0.9300 . ? C28 N8 1.314(6) . ? C28 N7 1.321(6) . ? C28 H28A 0.9300 . ? C29 C30 1.368(6) . ? C29 C34 1.377(6) . ? C29 P1 1.821(4) . ? C30 C31 1.384(6) . ? C30 H30 0.9300 . ? C31 C32 1.366(6) . ? C31 H31 0.9300 . ? C32 C33 1.373(6) . ? C32 C35 1.504(6) . ? C33 C34 1.371(6) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 O5 1.220(5) . ? C35 O4 1.282(5) . ? C36 C37 1.377(7) . ? C36 C41 1.402(6) . ? C36 P2 1.800(5) . ? C37 C38 1.397(7) . ? C37 H37 0.9300 . ? C38 C39 1.391(7) . ? C38 H38 0.9300 . ? C39 C40 1.395(7) . ? C39 C42 1.501(6) . ? C40 C41 1.382(7) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 O9 1.208(5) . ? C42 O10 1.290(5) . ? N1 Zn1 2.018(4) . ? N3 Zn2 2.017(4) . ? N5 Zn3 2.004(4) . ? N8 Zn2 1.971(4) 2_675 ? O1 P1 1.474(3) . ? O1 Zn3 1.906(3) 2_576 ? O2 P1 1.499(3) . ? O2 Zn1 1.894(3) 2_576 ? O3 P1 1.495(3) . ? O3 Zn1 1.918(3) . ? O4 Zn2 1.930(3) 2_566 ? O6 P2 1.499(3) . ? O6 Zn1 1.908(3) . ? O7 P2 1.493(3) . ? O7 Zn2 1.897(3) . ? O8 P2 1.503(3) . ? O8 Zn3 1.934(3) . ? O10 Zn3 1.946(3) 1_655 ? O1W H1X 0.8499 . ? O1W H1Y 0.8500 . ? O2W H2X 0.8500 . ? O2W H2Y 0.8501 . ? O3W H3X 0.8500 . ? O3W H3Y 0.8500 . ? Zn1 O2 1.894(3) 2_576 ? Zn2 O4 1.930(3) 2_566 ? Zn2 N8 1.971(4) 2_675 ? Zn3 O1 1.906(3) 2_576 ? Zn3 O10 1.946(3) 1_455 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N2 112.5(4) . . ? N1 C1 H1 123.7 . . ? N2 C1 H1 123.7 . . ? C3 C2 N1 108.9(4) . . ? C3 C2 H2 125.5 . . ? N1 C2 H2 125.5 . . ? C2 C3 N2 107.6(4) . . ? C2 C3 H3 126.2 . . ? N2 C3 H3 126.2 . . ? N2 C4 C5 113.7(4) . . ? N2 C4 H4A 108.8 . . ? C5 C4 H4A 108.8 . . ? N2 C4 H4B 108.8 . . ? C5 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? C6 C5 C10 118.9(4) . . ? C6 C5 C4 117.8(4) . . ? C10 C5 C4 123.3(4) . . ? C5 C6 C7 119.2(4) . . ? C5 C6 H6 120.4 . . ? C7 C6 H6 120.4 . . ? C8 C7 C6 120.6(4) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C9 C8 C7 120.6(5) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C10 118.8(5) . . ? C8 C9 C11 121.0(4) . . ? C10 C9 C11 120.1(5) . . ? C9 C10 C5 121.7(5) . . ? C9 C10 H10 119.1 . . ? C5 C10 H10 119.1 . . ? N4 C11 C9 111.8(4) . . ? N4 C11 H11A 109.3 . . ? C9 C11 H11A 109.3 . . ? N4 C11 H11B 109.3 . . ? C9 C11 H11B 109.3 . . ? H11A C11 H11B 107.9 . . ? C13 C12 N4 105.5(4) . . ? C13 C12 H12 127.3 . . ? N4 C12 H12 127.3 . . ? N3 C13 C12 110.8(4) . . ? N3 C13 H13 124.6 . . ? C12 C13 H13 124.6 . . ? N3 C14 N4 111.4(4) . . ? N3 C14 H14 124.3 . . ? N4 C14 H14 124.3 . . ? N6 C15 N5 112.8(4) . . ? N6 C15 H15A 123.6 . . ? N5 C15 H15A 123.6 . . ? N5 C16 C17 108.7(4) . . ? N5 C16 H16A 125.7 . . ? C17 C16 H16A 125.7 . . ? N6 C17 C16 107.5(4) . . ? N6 C17 H17A 126.3 . . ? C16 C17 H17A 126.3 . . ? N6 C18 C19 113.6(4) . . ? N6 C18 H18A 108.9 . . ? C19 C18 H18A 108.9 . . ? N6 C18 H18B 108.9 . . ? C19 C18 H18B 108.9 . . ? H18A C18 H18B 107.7 . . ? C20 C19 C24 118.7(5) . . ? C20 C19 C18 120.2(4) . . ? C24 C19 C18 121.0(5) . . ? C21 C20 C19 120.9(4) . . ? C21 C20 H20A 119.6 . . ? C19 C20 H20A 119.6 . . ? C20 C21 C22 120.7(5) . . ? C20 C21 H21A 119.7 . . ? C22 C21 H21A 119.7 . . ? C23 C22 C21 119.7(5) . . ? C23 C22 H22A 120.1 . . ? C21 C22 H22A 120.1 . . ? C22 C23 C24 120.2(5) . . ? C22 C23 C25 117.0(4) . . ? C24 C23 C25 122.8(4) . . ? C23 C24 C19 119.8(4) . . ? C23 C24 H24A 120.1 . . ? C19 C24 H24A 120.1 . . ? N7 C25 C23 116.2(4) . . ? N7 C25 H25A 108.2 . . ? C23 C25 H25A 108.2 . . ? N7 C25 H25B 108.2 . . ? C23 C25 H25B 108.2 . . ? H25A C25 H25B 107.4 . . ? C27 C26 N7 106.2(4) . . ? C27 C26 H26A 126.9 . . ? N7 C26 H26A 126.9 . . ? C26 C27 N8 111.2(4) . . ? C26 C27 H27A 124.4 . . ? N8 C27 H27A 124.4 . . ? N8 C28 N7 111.9(4) . . ? N8 C28 H28A 124.0 . . ? N7 C28 H28A 124.0 . . ? C30 C29 C34 117.7(4) . . ? C30 C29 P1 123.5(3) . . ? C34 C29 P1 118.2(3) . . ? C29 C30 C31 121.0(4) . . ? C29 C30 H30 119.5 . . ? C31 C30 H30 119.5 . . ? C32 C31 C30 120.3(4) . . ? C32 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? C31 C32 C33 119.5(4) . . ? C31 C32 C35 120.9(4) . . ? C33 C32 C35 119.5(4) . . ? C34 C33 C32 119.5(4) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C33 C34 C29 122.1(4) . . ? C33 C34 H34 119.0 . . ? C29 C34 H34 119.0 . . ? O5 C35 O4 123.4(4) . . ? O5 C35 C32 122.5(4) . . ? O4 C35 C32 114.0(4) . . ? C37 C36 C41 117.5(4) . . ? C37 C36 P2 123.0(4) . . ? C41 C36 P2 119.2(4) . . ? C36 C37 C38 121.1(4) . . ? C36 C37 H37 119.4 . . ? C38 C37 H37 119.4 . . ? C39 C38 C37 121.2(4) . . ? C39 C38 H38 119.4 . . ? C37 C38 H38 119.4 . . ? C38 C39 C40 117.6(4) . . ? C38 C39 C42 122.8(4) . . ? C40 C39 C42 119.6(4) . . ? C41 C40 C39 120.8(4) . . ? C41 C40 H40 119.6 . . ? C39 C40 H40 119.6 . . ? C40 C41 C36 121.6(4) . . ? C40 C41 H41 119.2 . . ? C36 C41 H41 119.2 . . ? O9 C42 O10 124.8(4) . . ? O9 C42 C39 121.3(4) . . ? O10 C42 C39 113.8(4) . . ? C1 N1 C2 105.1(4) . . ? C1 N1 Zn1 125.4(3) . . ? C2 N1 Zn1 129.3(3) . . ? C1 N2 C3 105.8(4) . . ? C1 N2 C4 125.1(4) . . ? C3 N2 C4 128.5(4) . . ? C14 N3 C13 105.5(4) . . ? C14 N3 Zn2 122.6(3) . . ? C13 N3 Zn2 131.7(3) . . ? C14 N4 C12 106.7(4) . . ? C14 N4 C11 123.5(4) . . ? C12 N4 C11 129.6(4) . . ? C15 N5 C16 105.0(4) . . ? C15 N5 Zn3 121.8(3) . . ? C16 N5 Zn3 130.0(3) . . ? C15 N6 C17 106.1(4) . . ? C15 N6 C18 126.2(4) . . ? C17 N6 C18 127.6(4) . . ? C28 N7 C26 106.5(4) . . ? C28 N7 C25 125.0(4) . . ? C26 N7 C25 128.3(4) . . ? C28 N8 C27 104.1(4) . . ? C28 N8 Zn2 125.8(3) . 2_675 ? C27 N8 Zn2 129.9(3) . 2_675 ? P1 O1 Zn3 158.2(2) . 2_576 ? P1 O2 Zn1 143.5(2) . 2_576 ? P1 O3 Zn1 132.07(18) . . ? C35 O4 Zn2 112.7(3) . 2_566 ? P2 O6 Zn1 146.1(2) . . ? P2 O7 Zn2 155.5(2) . . ? P2 O8 Zn3 141.9(2) . . ? C42 O10 Zn3 117.2(3) . 1_655 ? H1X O1W H1Y 97.4 . . ? H2X O2W H2Y 96.5 . . ? H3X O3W H3Y 109.5 . . ? O1 P1 O3 112.2(2) . . ? O1 P1 O2 113.18(18) . . ? O3 P1 O2 112.40(18) . . ? O1 P1 C29 109.5(2) . . ? O3 P1 C29 104.97(19) . . ? O2 P1 C29 103.85(19) . . ? O7 P2 O6 110.17(18) . . ? O7 P2 O8 111.28(19) . . ? O6 P2 O8 113.29(19) . . ? O7 P2 C36 107.92(19) . . ? O6 P2 C36 107.79(19) . . ? O8 P2 C36 106.11(19) . . ? O2 Zn1 O6 110.81(13) 2_576 . ? O2 Zn1 O3 118.23(13) 2_576 . ? O6 Zn1 O3 109.59(13) . . ? O2 Zn1 N1 108.02(14) 2_576 . ? O6 Zn1 N1 108.33(15) . . ? O3 Zn1 N1 101.06(15) . . ? O7 Zn2 O4 106.22(14) . 2_566 ? O7 Zn2 N8 105.11(14) . 2_675 ? O4 Zn2 N8 121.91(15) 2_566 2_675 ? O7 Zn2 N3 102.85(15) . . ? O4 Zn2 N3 105.33(15) 2_566 . ? N8 Zn2 N3 113.60(15) 2_675 . ? O1 Zn3 O8 114.43(14) 2_576 . ? O1 Zn3 O10 113.68(14) 2_576 1_455 ? O8 Zn3 O10 102.94(12) . 1_455 ? O1 Zn3 N5 103.51(14) 2_576 . ? O8 Zn3 N5 107.99(15) . . ? O10 Zn3 N5 114.51(14) 1_455 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 N2 -0.8(6) . . . . ? N2 C4 C5 C6 166.7(4) . . . . ? N2 C4 C5 C10 -13.0(6) . . . . ? C10 C5 C6 C7 -1.5(7) . . . . ? C4 C5 C6 C7 178.7(4) . . . . ? C5 C6 C7 C8 1.9(8) . . . . ? C6 C7 C8 C9 -2.9(8) . . . . ? C7 C8 C9 C10 3.5(7) . . . . ? C7 C8 C9 C11 -179.8(5) . . . . ? C8 C9 C10 C5 -3.2(7) . . . . ? C11 C9 C10 C5 -179.9(4) . . . . ? C6 C5 C10 C9 2.2(7) . . . . ? C4 C5 C10 C9 -178.0(4) . . . . ? C8 C9 C11 N4 -72.2(6) . . . . ? C10 C9 C11 N4 104.4(5) . . . . ? N4 C12 C13 N3 -0.4(6) . . . . ? N5 C16 C17 N6 0.3(6) . . . . ? N6 C18 C19 C20 -69.7(6) . . . . ? N6 C18 C19 C24 111.6(5) . . . . ? C24 C19 C20 C21 -2.2(7) . . . . ? C18 C19 C20 C21 179.1(5) . . . . ? C19 C20 C21 C22 1.8(8) . . . . ? C20 C21 C22 C23 -1.0(8) . . . . ? C21 C22 C23 C24 0.6(7) . . . . ? C21 C22 C23 C25 178.4(5) . . . . ? C22 C23 C24 C19 -1.1(8) . . . . ? C25 C23 C24 C19 -178.7(5) . . . . ? C20 C19 C24 C23 1.9(7) . . . . ? C18 C19 C24 C23 -179.4(4) . . . . ? C22 C23 C25 N7 158.4(5) . . . . ? C24 C23 C25 N7 -23.9(8) . . . . ? N7 C26 C27 N8 1.7(7) . . . . ? C34 C29 C30 C31 -2.7(7) . . . . ? P1 C29 C30 C31 167.8(4) . . . . ? C29 C30 C31 C32 1.5(7) . . . . ? C30 C31 C32 C33 0.0(7) . . . . ? C30 C31 C32 C35 -177.2(4) . . . . ? C31 C32 C33 C34 -0.2(7) . . . . ? C35 C32 C33 C34 177.1(4) . . . . ? C32 C33 C34 C29 -1.1(7) . . . . ? C30 C29 C34 C33 2.6(7) . . . . ? P1 C29 C34 C33 -168.5(4) . . . . ? C31 C32 C35 O5 22.4(6) . . . . ? C33 C32 C35 O5 -154.9(4) . . . . ? C31 C32 C35 O4 -160.0(4) . . . . ? C33 C32 C35 O4 22.7(6) . . . . ? C41 C36 C37 C38 2.4(7) . . . . ? P2 C36 C37 C38 -172.3(4) . . . . ? C36 C37 C38 C39 -1.9(8) . . . . ? C37 C38 C39 C40 -1.2(7) . . . . ? C37 C38 C39 C42 175.6(4) . . . . ? C38 C39 C40 C41 3.8(7) . . . . ? C42 C39 C40 C41 -173.1(4) . . . . ? C39 C40 C41 C36 -3.4(8) . . . . ? C37 C36 C41 C40 0.2(7) . . . . ? P2 C36 C41 C40 175.1(4) . . . . ? C38 C39 C42 O9 173.0(4) . . . . ? C40 C39 C42 O9 -10.3(7) . . . . ? C38 C39 C42 O10 -7.5(6) . . . . ? C40 C39 C42 O10 169.3(4) . . . . ? N2 C1 N1 C2 -0.6(5) . . . . ? N2 C1 N1 Zn1 -176.7(3) . . . . ? C3 C2 N1 C1 0.8(5) . . . . ? C3 C2 N1 Zn1 176.7(3) . . . . ? N1 C1 N2 C3 0.1(5) . . . . ? N1 C1 N2 C4 171.7(4) . . . . ? C2 C3 N2 C1 0.4(5) . . . . ? C2 C3 N2 C4 -170.8(4) . . . . ? C5 C4 N2 C1 -76.3(6) . . . . ? C5 C4 N2 C3 93.3(5) . . . . ? N4 C14 N3 C13 -0.7(6) . . . . ? N4 C14 N3 Zn2 174.8(3) . . . . ? C12 C13 N3 C14 0.7(6) . . . . ? C12 C13 N3 Zn2 -174.3(3) . . . . ? N3 C14 N4 C12 0.5(6) . . . . ? N3 C14 N4 C11 176.2(4) . . . . ? C13 C12 N4 C14 -0.1(6) . . . . ? C13 C12 N4 C11 -175.4(5) . . . . ? C9 C11 N4 C14 -55.3(6) . . . . ? C9 C11 N4 C12 119.3(5) . . . . ? N6 C15 N5 C16 0.2(6) . . . . ? N6 C15 N5 Zn3 161.7(3) . . . . ? C17 C16 N5 C15 -0.3(6) . . . . ? C17 C16 N5 Zn3 -159.8(4) . . . . ? N5 C15 N6 C17 0.1(6) . . . . ? N5 C15 N6 C18 -176.2(4) . . . . ? C16 C17 N6 C15 -0.2(6) . . . . ? C16 C17 N6 C18 176.0(5) . . . . ? C19 C18 N6 C15 82.5(6) . . . . ? C19 C18 N6 C17 -93.0(6) . . . . ? N8 C28 N7 C26 0.8(6) . . . . ? N8 C28 N7 C25 175.9(5) . . . . ? C27 C26 N7 C28 -1.5(6) . . . . ? C27 C26 N7 C25 -176.4(5) . . . . ? C23 C25 N7 C28 125.5(6) . . . . ? C23 C25 N7 C26 -60.4(8) . . . . ? N7 C28 N8 C27 0.2(6) . . . . ? N7 C28 N8 Zn2 175.7(3) . . . 2_675 ? C26 C27 N8 C28 -1.2(6) . . . . ? C26 C27 N8 Zn2 -176.4(4) . . . 2_675 ? O5 C35 O4 Zn2 10.6(6) . . . 2_566 ? C32 C35 O4 Zn2 -167.0(3) . . . 2_566 ? O9 C42 O10 Zn3 7.7(6) . . . 1_655 ? C39 C42 O10 Zn3 -171.9(3) . . . 1_655 ? Zn3 O1 P1 O3 159.3(6) 2_576 . . . ? Zn3 O1 P1 O2 30.7(7) 2_576 . . . ? Zn3 O1 P1 C29 -84.6(6) 2_576 . . . ? Zn1 O3 P1 O1 -89.5(3) . . . . ? Zn1 O3 P1 O2 39.4(3) . . . . ? Zn1 O3 P1 C29 151.7(3) . . . . ? Zn1 O2 P1 O1 35.2(4) 2_576 . . . ? Zn1 O2 P1 O3 -93.2(4) 2_576 . . . ? Zn1 O2 P1 C29 153.9(3) 2_576 . . . ? C30 C29 P1 O1 34.7(4) . . . . ? C34 C29 P1 O1 -154.9(3) . . . . ? C30 C29 P1 O3 155.4(4) . . . . ? C34 C29 P1 O3 -34.2(4) . . . . ? C30 C29 P1 O2 -86.5(4) . . . . ? C34 C29 P1 O2 84.0(4) . . . . ? Zn2 O7 P2 O6 -164.2(5) . . . . ? Zn2 O7 P2 O8 69.3(5) . . . . ? Zn2 O7 P2 C36 -46.8(6) . . . . ? Zn1 O6 P2 O7 154.5(3) . . . . ? Zn1 O6 P2 O8 -80.1(4) . . . . ? Zn1 O6 P2 C36 37.0(4) . . . . ? Zn3 O8 P2 O7 154.3(3) . . . . ? Zn3 O8 P2 O6 29.5(4) . . . . ? Zn3 O8 P2 C36 -88.6(3) . . . . ? C37 C36 P2 O7 -14.2(5) . . . . ? C41 C36 P2 O7 171.2(4) . . . . ? C37 C36 P2 O6 104.8(4) . . . . ? C41 C36 P2 O6 -69.9(4) . . . . ? C37 C36 P2 O8 -133.6(4) . . . . ? C41 C36 P2 O8 51.8(4) . . . . ? P2 O6 Zn1 O2 40.6(4) . . . 2_576 ? P2 O6 Zn1 O3 172.8(4) . . . . ? P2 O6 Zn1 N1 -77.8(4) . . . . ? P1 O3 Zn1 O2 -0.3(3) . . . 2_576 ? P1 O3 Zn1 O6 -128.6(3) . . . . ? P1 O3 Zn1 N1 117.3(3) . . . . ? C1 N1 Zn1 O2 -75.2(4) . . . 2_576 ? C2 N1 Zn1 O2 109.6(4) . . . 2_576 ? C1 N1 Zn1 O6 44.9(4) . . . . ? C2 N1 Zn1 O6 -130.3(4) . . . . ? C1 N1 Zn1 O3 160.0(4) . . . . ? C2 N1 Zn1 O3 -15.1(4) . . . . ? P2 O7 Zn2 O4 -132.8(5) . . . 2_566 ? P2 O7 Zn2 N8 -2.3(6) . . . 2_675 ? P2 O7 Zn2 N3 116.8(5) . . . . ? C14 N3 Zn2 O7 -13.2(4) . . . . ? C13 N3 Zn2 O7 161.0(4) . . . . ? C14 N3 Zn2 O4 -124.3(4) . . . 2_566 ? C13 N3 Zn2 O4 50.0(5) . . . 2_566 ? C14 N3 Zn2 N8 99.8(4) . . . 2_675 ? C13 N3 Zn2 N8 -85.9(4) . . . 2_675 ? P2 O8 Zn3 O1 4.3(4) . . . 2_576 ? P2 O8 Zn3 O10 -119.6(3) . . . 1_455 ? P2 O8 Zn3 N5 119.0(3) . . . . ? C15 N5 Zn3 O1 -53.5(4) . . . 2_576 ? C16 N5 Zn3 O1 103.0(4) . . . 2_576 ? C15 N5 Zn3 O8 -175.2(3) . . . . ? C16 N5 Zn3 O8 -18.7(4) . . . . ? C15 N5 Zn3 O10 70.8(4) . . . 1_455 ? C16 N5 Zn3 O10 -132.7(4) . . . 1_455 ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.443 _refine_diff_density_min -0.962 _refine_diff_density_rms 0.089 # Attachment '3.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 765764' #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H24 N4 O11 P2 Zn3' _chemical_formula_weight 850.56 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 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.251(8) _cell_length_b 12.455(11) _cell_length_c 12.852(11) _cell_angle_alpha 72.734(14) _cell_angle_beta 77.094(14) _cell_angle_gamma 83.361(17) _cell_volume 1525(2) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 3506 _cell_measurement_theta_min 2.382 _cell_measurement_theta_max 28.0795 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.852 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 2.514 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5192 _exptl_absorpt_correction_T_max 0.5837 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8230 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0612 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5837 _reflns_number_gt 4242 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+1.2200P] 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 5837 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0667 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1043 _refine_ls_wR_factor_gt 0.1015 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6540(5) 0.8699(4) -0.3551(4) 0.0369(11) Uani 1 1 d . . . C2 C 0.5531(5) 0.8750(4) -0.4125(4) 0.0361(11) Uani 1 1 d . . . H2 H 0.5758 0.8815 -0.4883 0.043 Uiso 1 1 calc R . . C3 C 0.4221(4) 0.8706(4) -0.3616(4) 0.0302(9) Uani 1 1 d . . . H3 H 0.3570 0.8758 -0.4032 0.036 Uiso 1 1 calc R . . C4 C 0.3834(4) 0.8585(4) -0.2480(4) 0.0297(9) Uani 1 1 d . . . C5 C 0.4842(5) 0.8537(4) -0.1893(4) 0.0364(11) Uani 1 1 d . . . H5 H 0.4614 0.8466 -0.1134 0.044 Uiso 1 1 calc R . . C6 C 0.6172(5) 0.8592(4) -0.2419(4) 0.0333(10) Uani 1 1 d . . . H6 H 0.6828 0.8557 -0.2011 0.040 Uiso 1 1 calc R . . C7 C 0.2416(5) 0.8507(4) -0.1923(3) 0.0287(9) Uani 1 1 d . . . C8 C 0.6616(5) 0.8323(4) 0.2484(4) 0.0317(10) Uani 1 1 d . . . C9 C 0.5169(5) 0.8503(4) 0.2340(4) 0.0327(10) Uani 1 1 d . . . C10 C 0.4918(5) 0.8740(4) 0.1289(4) 0.0322(10) Uani 1 1 d . . . H10 H 0.5623 0.8762 0.0686 0.039 Uiso 1 1 calc R . . C11 C 0.3607(4) 0.8947(4) 0.1130(4) 0.0327(10) Uani 1 1 d . . . H11 H 0.3445 0.9112 0.0414 0.039 Uiso 1 1 calc R . . C12 C 0.2531(5) 0.8914(4) 0.2010(4) 0.0338(10) Uani 1 1 d . . . C13 C 0.2821(5) 0.8671(4) 0.3054(4) 0.0358(10) Uani 1 1 d . . . H13 H 0.2125 0.8642 0.3665 0.043 Uiso 1 1 calc R . . C14 C 0.4134(4) 0.8470(4) 0.3212(4) 0.0316(10) Uani 1 1 d . . . H14 H 0.4304 0.8311 0.3925 0.038 Uiso 1 1 calc R . . C15 C -0.0870(5) 0.6156(4) 0.0823(4) 0.0317(10) Uani 1 1 d . . . H15 H -0.0553 0.6064 0.1470 0.038 Uiso 1 1 calc R . . C16 C -0.1316(5) 0.6858(4) -0.0802(4) 0.0345(10) Uani 1 1 d . . . H16 H -0.1355 0.7351 -0.1499 0.041 Uiso 1 1 calc R . . C17 C -0.1862(5) 0.5842(4) -0.0375(4) 0.0328(10) Uani 1 1 d . . . H17 H -0.2347 0.5511 -0.0718 0.039 Uiso 1 1 calc R . . C18 C -0.1905(5) 0.4281(4) 0.1398(4) 0.0334(10) Uani 1 1 d . . . H18A H -0.1159 0.3949 0.1757 0.040 Uiso 1 1 calc R . . H18B H -0.2028 0.3806 0.0953 0.040 Uiso 1 1 calc R . . C19 C -0.3146(5) 0.4283(4) 0.2277(4) 0.0354(10) Uani 1 1 d . . . C20 C -0.4361(5) 0.4559(4) 0.1947(4) 0.0380(11) Uani 1 1 d . . . H20 H -0.4373 0.4781 0.1191 0.046 Uiso 1 1 calc R . . C21 C -0.5565(5) 0.4516(4) 0.2701(4) 0.0349(11) Uani 1 1 d . . . H21 H -0.6375 0.4695 0.2462 0.042 Uiso 1 1 calc R . . C22 C -0.5532(5) 0.4208(4) 0.3793(4) 0.0351(11) Uani 1 1 d . . . H22 H -0.6334 0.4191 0.4307 0.042 Uiso 1 1 calc R . . C23 C -0.4352(5) 0.3918(4) 0.4172(4) 0.0375(11) Uani 1 1 d . . . H23 H -0.4362 0.3701 0.4932 0.045 Uiso 1 1 calc R . . C24 C -0.3129(5) 0.3949(4) 0.3409(4) 0.0350(11) Uani 1 1 d . . . C25 C -0.1882(5) 0.3608(4) 0.3842(4) 0.0359(11) Uani 1 1 d . . . H25A H -0.1335 0.3102 0.3454 0.043 Uiso 1 1 calc R . . H25B H -0.2101 0.3206 0.4625 0.043 Uiso 1 1 calc R . . C26 C -0.1677(5) 0.5640(4) 0.3674(4) 0.0343(10) Uani 1 1 d . . . H26 H -0.2589 0.5833 0.3727 0.041 Uiso 1 1 calc R . . C27 C 0.0220(5) 0.4647(4) 0.3609(4) 0.0369(11) Uani 1 1 d . . . H27 H 0.0864 0.4057 0.3608 0.044 Uiso 1 1 calc R . . C28 C 0.0430(5) 0.5721(4) 0.3524(4) 0.0396(11) Uani 1 1 d . . . H28 H 0.1263 0.5995 0.3449 0.047 Uiso 1 1 calc R . . N1 N -0.0694(4) 0.7039(3) -0.0030(3) 0.0307(8) Uani 1 1 d . . . N2 N -0.1561(4) 0.5396(3) 0.0659(3) 0.0338(9) Uani 1 1 d . . . N3 N -0.0748(4) 0.6346(3) 0.3563(3) 0.0349(9) Uani 1 1 d . . . N4 N -0.1109(4) 0.4596(3) 0.3698(3) 0.0361(9) Uani 1 1 d . . . O1 O 0.8378(3) 0.9957(3) -0.5092(3) 0.0378(8) Uani 1 1 d . . . O2 O 0.9088(3) 0.8640(3) -0.3381(3) 0.0341(7) Uani 1 1 d . . . O3 O 0.8605(3) 0.7850(3) -0.4834(2) 0.0317(7) Uani 1 1 d . . . O4 O 0.1545(3) 0.8457(3) -0.2470(3) 0.0331(7) Uani 1 1 d . . . O5 O 0.2116(3) 0.8419(3) -0.0905(3) 0.0330(7) Uani 1 1 d . . . O6 O 0.0826(3) 1.0338(3) 0.0942(3) 0.0393(8) Uani 1 1 d . . . O7 O 0.0579(3) 0.8258(3) 0.1309(2) 0.0313(7) Uani 1 1 d . . . O8 O -0.0082(3) 0.9144(3) 0.2859(3) 0.0331(7) Uani 1 1 d . . . O9 O 0.6802(3) 0.8133(3) 0.3465(3) 0.0348(7) Uani 1 1 d . . . O10 O 0.7526(3) 0.8338(3) 0.1715(3) 0.0355(7) Uani 1 1 d . . . O1W O 0.2896(3) 0.6399(3) 0.0883(3) 0.0348(7) Uani 1 1 d . . . H1WA H 0.2479 0.6937 0.1122 0.042 Uiso 1 1 d R . . H1WB H 0.3177 0.6675 0.0189 0.042 Uiso 1 1 d R . . P1 P 0.82616(13) 0.87856(10) -0.42633(10) 0.0332(3) Uani 1 1 d . . . P2 P 0.08752(13) 0.91907(11) 0.17334(10) 0.0338(3) Uani 1 1 d . . . Zn1 Zn 0.01838(5) 0.84296(4) -0.01373(4) 0.03051(14) Uani 1 1 d . . . Zn2 Zn -0.05215(5) 1.04717(4) 0.34703(4) 0.03103(14) Uani 1 1 d . . . Zn3 Zn -0.13472(5) 0.79112(4) 0.36259(4) 0.03106(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.027(2) 0.040(3) 0.039(3) -0.006(2) -0.0023(19) -0.004(2) C2 0.036(3) 0.034(3) 0.036(3) -0.009(2) -0.003(2) -0.003(2) C3 0.024(2) 0.035(2) 0.033(2) -0.0079(19) -0.0106(18) -0.0025(18) C4 0.027(2) 0.027(2) 0.031(2) -0.0033(18) 0.0002(17) -0.0053(17) C5 0.040(3) 0.034(3) 0.033(2) -0.011(2) -0.001(2) -0.004(2) C6 0.029(2) 0.038(3) 0.032(2) -0.008(2) -0.0031(18) -0.0061(19) C7 0.035(2) 0.027(2) 0.021(2) -0.0020(17) -0.0023(18) -0.0057(18) C8 0.031(2) 0.035(2) 0.029(2) -0.0119(19) -0.0044(19) 0.0013(19) C9 0.031(2) 0.038(3) 0.032(2) -0.010(2) -0.0152(19) 0.0023(19) C10 0.028(2) 0.035(3) 0.037(3) -0.016(2) -0.0084(19) 0.0093(18) C11 0.028(2) 0.040(3) 0.031(2) -0.013(2) -0.0046(18) 0.0027(19) C12 0.038(3) 0.032(2) 0.034(2) -0.012(2) -0.011(2) 0.0030(19) C13 0.040(3) 0.037(3) 0.031(2) -0.010(2) -0.009(2) 0.005(2) C14 0.027(2) 0.030(2) 0.038(2) -0.009(2) -0.0122(19) 0.0076(18) C15 0.034(2) 0.028(2) 0.035(2) -0.0071(19) -0.0102(19) -0.0079(19) C16 0.037(3) 0.041(3) 0.030(2) -0.010(2) -0.0115(19) -0.011(2) C17 0.030(2) 0.034(2) 0.039(3) -0.013(2) -0.0101(19) -0.0116(19) C18 0.034(3) 0.034(2) 0.030(2) -0.007(2) 0.0015(19) -0.012(2) C19 0.036(3) 0.033(2) 0.041(3) -0.014(2) -0.004(2) -0.013(2) C20 0.041(3) 0.032(2) 0.038(3) -0.009(2) 0.004(2) -0.013(2) C21 0.038(3) 0.030(2) 0.032(2) -0.0049(19) 0.003(2) -0.0150(19) C22 0.033(3) 0.028(2) 0.038(3) -0.012(2) 0.016(2) -0.0147(19) C23 0.040(3) 0.037(3) 0.037(3) -0.018(2) 0.005(2) -0.015(2) C24 0.034(3) 0.039(3) 0.035(2) -0.017(2) 0.0056(19) -0.019(2) C25 0.034(3) 0.034(3) 0.042(3) -0.008(2) -0.011(2) -0.013(2) C26 0.040(3) 0.029(2) 0.034(2) -0.0097(19) -0.005(2) -0.0015(19) C27 0.038(3) 0.029(2) 0.046(3) -0.016(2) -0.013(2) 0.010(2) C28 0.031(3) 0.042(3) 0.046(3) -0.012(2) -0.014(2) 0.004(2) N1 0.0231(19) 0.035(2) 0.030(2) -0.0011(16) -0.0060(15) -0.0050(16) N2 0.036(2) 0.033(2) 0.028(2) -0.0044(16) -0.0015(16) -0.0086(17) N3 0.039(2) 0.032(2) 0.034(2) -0.0081(17) -0.0127(17) 0.0032(17) N4 0.035(2) 0.039(2) 0.037(2) -0.0102(18) -0.0126(17) -0.0064(17) O1 0.0348(18) 0.0384(19) 0.0318(17) -0.0033(15) 0.0017(14) -0.0025(14) O2 0.0305(17) 0.0345(18) 0.0365(18) -0.0068(14) -0.0033(13) -0.0129(13) O3 0.0299(16) 0.0379(18) 0.0246(15) -0.0092(14) 0.0008(12) -0.0019(13) O4 0.0309(17) 0.0355(18) 0.0306(16) -0.0042(13) -0.0083(13) -0.0015(13) O5 0.0289(16) 0.0394(18) 0.0331(17) -0.0160(14) -0.0026(13) -0.0024(14) O6 0.0315(18) 0.041(2) 0.0363(18) -0.0025(15) -0.0015(14) 0.0018(15) O7 0.0305(17) 0.0307(16) 0.0320(17) -0.0099(13) -0.0046(13) 0.0002(13) O8 0.0335(17) 0.0295(17) 0.0339(17) -0.0077(13) -0.0021(14) -0.0044(13) O9 0.0327(17) 0.0347(18) 0.0382(18) -0.0108(14) -0.0140(14) 0.0079(14) O10 0.0318(17) 0.0386(19) 0.0366(18) -0.0109(15) -0.0118(14) 0.0060(14) O1W 0.0460(19) 0.0303(17) 0.0348(18) -0.0152(14) -0.0160(15) 0.0033(14) P1 0.0333(6) 0.0310(6) 0.0316(6) -0.0048(5) -0.0026(5) -0.0049(5) P2 0.0350(7) 0.0314(6) 0.0313(6) -0.0059(5) -0.0034(5) -0.0009(5) Zn1 0.0318(3) 0.0294(3) 0.0281(3) -0.0046(2) -0.0057(2) -0.0023(2) Zn2 0.0287(3) 0.0281(3) 0.0323(3) -0.0042(2) -0.0026(2) -0.0038(2) Zn3 0.0313(3) 0.0298(3) 0.0317(3) -0.0083(2) -0.0059(2) -0.0017(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 C1 C2 1.385(7) . ? C1 C6 1.389(7) . ? C1 P1 1.797(5) . ? C2 C3 1.355(6) . ? C2 H2 0.9300 . ? C3 C4 1.391(6) . ? C3 H3 0.9300 . ? C4 C5 1.395(7) . ? C4 C7 1.471(6) . ? C5 C6 1.379(7) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 O5 1.249(5) . ? C7 O4 1.270(5) . ? C8 O10 1.195(5) . ? C8 O9 1.265(5) . ? C8 C9 1.518(6) . ? C9 C14 1.355(7) . ? C9 C10 1.371(6) . ? C10 C11 1.389(6) . ? C10 H10 0.9300 . ? C11 C12 1.387(6) . ? C11 H11 0.9300 . ? C12 C13 1.378(7) . ? C12 P2 1.785(5) . ? C13 C14 1.389(7) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 N1 1.299(6) . ? C15 N2 1.336(6) . ? C15 H15 0.9300 . ? C16 C17 1.353(6) . ? C16 N1 1.374(6) . ? C16 H16 0.9300 . ? C17 N2 1.370(6) . ? C17 H17 0.9300 . ? C18 N2 1.461(6) . ? C18 C19 1.502(6) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.378(7) . ? C19 C24 1.393(7) . ? C20 C21 1.384(7) . ? C20 H20 0.9300 . ? C21 C22 1.347(7) . ? C21 H21 0.9300 . ? C22 C23 1.375(7) . ? C22 H22 0.9300 . ? C23 C24 1.405(6) . ? C23 H23 0.9300 . ? C24 C25 1.475(7) . ? C25 N4 1.484(6) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 N3 1.326(6) . ? C26 N4 1.356(6) . ? C26 H26 0.9300 . ? C27 N4 1.348(6) . ? C27 C28 1.349(7) . ? C27 H27 0.9300 . ? C28 N3 1.359(6) . ? C28 H28 0.9300 . ? N1 Zn1 1.998(4) . ? N3 Zn3 1.995(4) . ? O1 P1 1.529(3) . ? O1 Zn2 1.905(3) 1_654 ? O2 P1 1.519(4) . ? O2 Zn2 1.903(3) 2_675 ? O3 P1 1.522(3) . ? O3 Zn3 1.947(3) 1_654 ? O4 Zn2 1.948(3) 2_575 ? O5 Zn1 2.007(3) . ? O6 P2 1.491(4) . ? O6 Zn1 1.915(3) 2_575 ? O7 P2 1.507(3) . ? O7 Zn1 1.936(3) . ? O8 P2 1.545(3) . ? O8 Zn2 1.999(3) . ? O8 Zn3 2.000(3) . ? O9 Zn3 1.933(3) 1_655 ? O1W H1WA 0.8501 . ? O1W H1WB 0.8500 . ? Zn1 O6 1.915(3) 2_575 ? Zn2 O2 1.903(3) 2_675 ? Zn2 O1 1.905(3) 1_456 ? Zn2 O4 1.948(3) 2_575 ? Zn3 O9 1.933(4) 1_455 ? Zn3 O3 1.947(3) 1_456 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 117.8(4) . . ? C2 C1 P1 120.5(4) . . ? C6 C1 P1 121.7(4) . . ? C3 C2 C1 121.9(5) . . ? C3 C2 H2 119.0 . . ? C1 C2 H2 119.0 . . ? C2 C3 C4 121.1(4) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C3 C4 C5 117.5(4) . . ? C3 C4 C7 121.0(4) . . ? C5 C4 C7 121.5(4) . . ? C6 C5 C4 121.1(4) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C1 120.6(4) . . ? C5 C6 H6 119.7 . . ? C1 C6 H6 119.7 . . ? O5 C7 O4 121.9(4) . . ? O5 C7 C4 118.6(4) . . ? O4 C7 C4 119.3(4) . . ? O10 C8 O9 121.9(4) . . ? O10 C8 C9 121.7(4) . . ? O9 C8 C9 116.4(4) . . ? C14 C9 C10 119.6(4) . . ? C14 C9 C8 121.9(4) . . ? C10 C9 C8 118.5(4) . . ? C9 C10 C11 119.6(4) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C12 C11 C10 121.8(4) . . ? C12 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C13 C12 C11 117.0(5) . . ? C13 C12 P2 124.1(4) . . ? C11 C12 P2 118.9(4) . . ? C12 C13 C14 121.2(5) . . ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? C9 C14 C13 120.8(4) . . ? C9 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? N1 C15 N2 111.8(4) . . ? N1 C15 H15 124.1 . . ? N2 C15 H15 124.1 . . ? C17 C16 N1 108.5(4) . . ? C17 C16 H16 125.8 . . ? N1 C16 H16 125.8 . . ? C16 C17 N2 106.7(4) . . ? C16 C17 H17 126.7 . . ? N2 C17 H17 126.7 . . ? N2 C18 C19 114.1(4) . . ? N2 C18 H18A 108.7 . . ? C19 C18 H18A 108.7 . . ? N2 C18 H18B 108.7 . . ? C19 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? C20 C19 C24 118.9(5) . . ? C20 C19 C18 118.1(4) . . ? C24 C19 C18 122.8(5) . . ? C19 C20 C21 122.2(5) . . ? C19 C20 H20 118.9 . . ? C21 C20 H20 118.9 . . ? C22 C21 C20 118.2(5) . . ? C22 C21 H21 120.9 . . ? C20 C21 H21 120.9 . . ? C21 C22 C23 122.1(4) . . ? C21 C22 H22 118.9 . . ? C23 C22 H22 118.9 . . ? C22 C23 C24 119.8(5) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C19 C24 C23 118.7(5) . . ? C19 C24 C25 122.8(4) . . ? C23 C24 C25 118.5(4) . . ? C24 C25 N4 111.5(4) . . ? C24 C25 H25A 109.3 . . ? N4 C25 H25A 109.3 . . ? C24 C25 H25B 109.3 . . ? N4 C25 H25B 109.3 . . ? H25A C25 H25B 108.0 . . ? N3 C26 N4 110.3(4) . . ? N3 C26 H26 124.8 . . ? N4 C26 H26 124.8 . . ? N4 C27 C28 106.5(4) . . ? N4 C27 H27 126.7 . . ? C28 C27 H27 126.7 . . ? C27 C28 N3 110.2(4) . . ? C27 C28 H28 124.9 . . ? N3 C28 H28 124.9 . . ? C15 N1 C16 106.4(4) . . ? C15 N1 Zn1 126.2(3) . . ? C16 N1 Zn1 127.2(3) . . ? C15 N2 C17 106.7(4) . . ? C15 N2 C18 128.1(4) . . ? C17 N2 C18 125.2(4) . . ? C26 N3 C28 105.5(4) . . ? C26 N3 Zn3 118.1(3) . . ? C28 N3 Zn3 136.1(3) . . ? C27 N4 C26 107.4(4) . . ? C27 N4 C25 128.9(4) . . ? C26 N4 C25 123.7(4) . . ? P1 O1 Zn2 131.1(2) . 1_654 ? P1 O2 Zn2 126.53(19) . 2_675 ? P1 O3 Zn3 129.4(2) . 1_654 ? C7 O4 Zn2 136.4(3) . 2_575 ? C7 O5 Zn1 119.9(3) . . ? P2 O6 Zn1 149.6(2) . 2_575 ? P2 O7 Zn1 126.05(19) . . ? P2 O8 Zn2 122.84(18) . . ? P2 O8 Zn3 122.48(19) . . ? Zn2 O8 Zn3 112.80(16) . . ? C8 O9 Zn3 115.6(3) . 1_655 ? H1WA O1W H1WB 106.4 . . ? O2 P1 O3 111.5(2) . . ? O2 P1 O1 111.59(19) . . ? O3 P1 O1 112.35(19) . . ? O2 P1 C1 106.4(2) . . ? O3 P1 C1 108.5(2) . . ? O1 P1 C1 106.2(2) . . ? O6 P2 O7 114.7(2) . . ? O6 P2 O8 111.12(19) . . ? O7 P2 O8 108.96(18) . . ? O6 P2 C12 107.3(2) . . ? O7 P2 C12 107.8(2) . . ? O8 P2 C12 106.6(2) . . ? O6 Zn1 O7 126.09(14) 2_575 . ? O6 Zn1 N1 105.96(16) 2_575 . ? O7 Zn1 N1 106.87(14) . . ? O6 Zn1 O5 110.93(14) 2_575 . ? O7 Zn1 O5 94.29(14) . . ? N1 Zn1 O5 112.34(15) . . ? O2 Zn2 O1 115.64(15) 2_675 1_456 ? O2 Zn2 O4 100.68(15) 2_675 2_575 ? O1 Zn2 O4 110.11(15) 1_456 2_575 ? O2 Zn2 O8 117.77(14) 2_675 . ? O1 Zn2 O8 106.62(14) 1_456 . ? O4 Zn2 O8 105.27(14) 2_575 . ? O9 Zn3 O3 105.27(13) 1_455 1_456 ? O9 Zn3 N3 106.90(15) 1_455 . ? O3 Zn3 N3 103.52(15) 1_456 . ? O9 Zn3 O8 120.19(14) 1_455 . ? O3 Zn3 O8 99.49(13) 1_456 . ? N3 Zn3 O8 118.84(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.5(7) . . . . ? P1 C1 C2 C3 -178.8(4) . . . . ? C1 C2 C3 C4 -1.3(7) . . . . ? C2 C3 C4 C5 1.4(7) . . . . ? C2 C3 C4 C7 -178.3(4) . . . . ? C3 C4 C5 C6 -0.8(7) . . . . ? C7 C4 C5 C6 178.9(4) . . . . ? C4 C5 C6 C1 0.1(7) . . . . ? C2 C1 C6 C5 0.1(7) . . . . ? P1 C1 C6 C5 179.4(4) . . . . ? C3 C4 C7 O5 -178.8(4) . . . . ? C5 C4 C7 O5 1.5(6) . . . . ? C3 C4 C7 O4 5.8(6) . . . . ? C5 C4 C7 O4 -173.9(4) . . . . ? O10 C8 C9 C14 179.0(5) . . . . ? O9 C8 C9 C14 0.4(7) . . . . ? O10 C8 C9 C10 -3.1(7) . . . . ? O9 C8 C9 C10 178.3(4) . . . . ? C14 C9 C10 C11 0.2(7) . . . . ? C8 C9 C10 C11 -177.8(4) . . . . ? C9 C10 C11 C12 -0.4(7) . . . . ? C10 C11 C12 C13 0.4(7) . . . . ? C10 C11 C12 P2 180.0(4) . . . . ? C11 C12 C13 C14 0.0(7) . . . . ? P2 C12 C13 C14 -179.6(4) . . . . ? C10 C9 C14 C13 0.1(7) . . . . ? C8 C9 C14 C13 178.0(4) . . . . ? C12 C13 C14 C9 -0.2(7) . . . . ? N1 C16 C17 N2 -0.5(5) . . . . ? N2 C18 C19 C20 68.2(6) . . . . ? N2 C18 C19 C24 -116.1(5) . . . . ? C24 C19 C20 C21 0.0(7) . . . . ? C18 C19 C20 C21 175.9(4) . . . . ? C19 C20 C21 C22 1.0(7) . . . . ? C20 C21 C22 C23 -1.3(7) . . . . ? C21 C22 C23 C24 0.7(7) . . . . ? C20 C19 C24 C23 -0.6(7) . . . . ? C18 C19 C24 C23 -176.4(4) . . . . ? C20 C19 C24 C25 178.3(4) . . . . ? C18 C19 C24 C25 2.5(7) . . . . ? C22 C23 C24 C19 0.3(7) . . . . ? C22 C23 C24 C25 -178.6(4) . . . . ? C19 C24 C25 N4 75.6(6) . . . . ? C23 C24 C25 N4 -105.5(5) . . . . ? N4 C27 C28 N3 0.3(6) . . . . ? N2 C15 N1 C16 0.6(5) . . . . ? N2 C15 N1 Zn1 176.2(3) . . . . ? C17 C16 N1 C15 0.0(5) . . . . ? C17 C16 N1 Zn1 -175.6(3) . . . . ? N1 C15 N2 C17 -0.9(5) . . . . ? N1 C15 N2 C18 176.9(4) . . . . ? C16 C17 N2 C15 0.8(5) . . . . ? C16 C17 N2 C18 -177.1(4) . . . . ? C19 C18 N2 C15 84.3(6) . . . . ? C19 C18 N2 C17 -98.2(5) . . . . ? N4 C26 N3 C28 -0.4(5) . . . . ? N4 C26 N3 Zn3 -175.2(3) . . . . ? C27 C28 N3 C26 0.1(6) . . . . ? C27 C28 N3 Zn3 173.5(4) . . . . ? C28 C27 N4 C26 -0.5(6) . . . . ? C28 C27 N4 C25 -178.2(5) . . . . ? N3 C26 N4 C27 0.6(5) . . . . ? N3 C26 N4 C25 178.5(4) . . . . ? C24 C25 N4 C27 -154.2(5) . . . . ? C24 C25 N4 C26 28.4(6) . . . . ? O5 C7 O4 Zn2 100.8(5) . . . 2_575 ? C4 C7 O4 Zn2 -83.9(5) . . . 2_575 ? O4 C7 O5 Zn1 -9.4(6) . . . . ? C4 C7 O5 Zn1 175.3(3) . . . . ? O10 C8 O9 Zn3 1.6(6) . . . 1_655 ? C9 C8 O9 Zn3 -179.8(3) . . . 1_655 ? Zn2 O2 P1 O3 107.8(3) 2_675 . . . ? Zn2 O2 P1 O1 -18.7(3) 2_675 . . . ? Zn2 O2 P1 C1 -134.2(3) 2_675 . . . ? Zn3 O3 P1 O2 -145.4(2) 1_654 . . . ? Zn3 O3 P1 O1 -19.4(3) 1_654 . . . ? Zn3 O3 P1 C1 97.7(3) 1_654 . . . ? Zn2 O1 P1 O2 97.5(3) 1_654 . . . ? Zn2 O1 P1 O3 -28.6(3) 1_654 . . . ? Zn2 O1 P1 C1 -147.0(3) 1_654 . . . ? C2 C1 P1 O2 -177.0(4) . . . . ? C6 C1 P1 O2 3.7(5) . . . . ? C2 C1 P1 O3 -57.0(5) . . . . ? C6 C1 P1 O3 123.7(4) . . . . ? C2 C1 P1 O1 63.9(5) . . . . ? C6 C1 P1 O1 -115.3(4) . . . . ? Zn1 O6 P2 O7 66.7(5) 2_575 . . . ? Zn1 O6 P2 O8 -57.4(5) 2_575 . . . ? Zn1 O6 P2 C12 -173.6(4) 2_575 . . . ? Zn1 O7 P2 O6 1.0(3) . . . . ? Zn1 O7 P2 O8 126.3(2) . . . . ? Zn1 O7 P2 C12 -118.4(2) . . . . ? Zn2 O8 P2 O6 -30.5(3) . . . . ? Zn3 O8 P2 O6 132.8(2) . . . . ? Zn2 O8 P2 O7 -157.8(2) . . . . ? Zn3 O8 P2 O7 5.4(3) . . . . ? Zn2 O8 P2 C12 86.1(3) . . . . ? Zn3 O8 P2 C12 -110.6(2) . . . . ? C13 C12 P2 O6 121.2(4) . . . . ? C11 C12 P2 O6 -58.4(4) . . . . ? C13 C12 P2 O7 -114.8(4) . . . . ? C11 C12 P2 O7 65.6(4) . . . . ? C13 C12 P2 O8 2.0(5) . . . . ? C11 C12 P2 O8 -177.5(4) . . . . ? P2 O7 Zn1 O6 -36.4(3) . . . 2_575 ? P2 O7 Zn1 N1 -161.7(2) . . . . ? P2 O7 Zn1 O5 83.4(2) . . . . ? C15 N1 Zn1 O6 -141.4(4) . . . 2_575 ? C16 N1 Zn1 O6 33.3(4) . . . 2_575 ? C15 N1 Zn1 O7 -4.8(4) . . . . ? C16 N1 Zn1 O7 170.0(4) . . . . ? C15 N1 Zn1 O5 97.3(4) . . . . ? C16 N1 Zn1 O5 -87.9(4) . . . . ? C7 O5 Zn1 O6 -48.9(4) . . . 2_575 ? C7 O5 Zn1 O7 179.7(3) . . . . ? C7 O5 Zn1 N1 69.5(4) . . . . ? P2 O8 Zn2 O2 -44.0(3) . . . 2_675 ? Zn3 O8 Zn2 O2 151.32(15) . . . 2_675 ? P2 O8 Zn2 O1 -175.8(2) . . . 1_456 ? Zn3 O8 Zn2 O1 19.4(2) . . . 1_456 ? P2 O8 Zn2 O4 67.2(2) . . . 2_575 ? Zn3 O8 Zn2 O4 -97.53(18) . . . 2_575 ? C26 N3 Zn3 O9 -14.4(4) . . . 1_455 ? C28 N3 Zn3 O9 172.8(5) . . . 1_455 ? C26 N3 Zn3 O3 96.4(4) . . . 1_456 ? C28 N3 Zn3 O3 -76.4(5) . . . 1_456 ? C26 N3 Zn3 O8 -154.5(3) . . . . ? C28 N3 Zn3 O8 32.7(5) . . . . ? P2 O8 Zn3 O9 -97.3(2) . . . 1_455 ? Zn2 O8 Zn3 O9 67.5(2) . . . 1_455 ? P2 O8 Zn3 O3 148.8(2) . . . 1_456 ? Zn2 O8 Zn3 O3 -46.43(18) . . . 1_456 ? P2 O8 Zn3 N3 37.5(3) . . . . ? Zn2 O8 Zn3 N3 -157.69(16) . . . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.426 _refine_diff_density_min -0.724 _refine_diff_density_rms 0.099 # Attachment '4.cif' data_1-new _database_code_depnum_ccdc_archive 'CCDC 765765' #TrackingRef '4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H28 N6 Ni O6 P' _chemical_formula_weight 634.24 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8809(15) _cell_length_b 10.9757(17) _cell_length_c 14.284(2) _cell_angle_alpha 69.836(3) _cell_angle_beta 72.732(3) _cell_angle_gamma 74.874(3) _cell_volume 1366.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1644 _cell_measurement_theta_min 2.514 _cell_measurement_theta_max 23.163 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 658 _exptl_absorpt_coefficient_mu 0.824 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8863 _exptl_absorpt_correction_T_max 0.9221 _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6863 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0862 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4727 _reflns_number_gt 3316 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0268P)^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 4727 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0687 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.0975 _refine_ls_wR_factor_gt 0.0923 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.991 _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 Ni1 Ni 0.72556(5) 0.29485(5) 0.26894(4) 0.03028(16) Uani 1 1 d . . . P1 P 0.86559(11) -0.42944(10) 0.11988(8) 0.0288(3) Uani 1 1 d . . . C1 C 0.8259(4) -0.2729(3) 0.1468(3) 0.0281(9) Uani 1 1 d . . . C2 C 0.8574(4) -0.1587(4) 0.0719(3) 0.0364(10) Uani 1 1 d . . . H2 H 0.8974 -0.1611 0.0047 0.044 Uiso 1 1 calc R . . C3 C 0.7671(4) -0.2641(4) 0.2452(3) 0.0456(12) Uani 1 1 d . . . H3 H 0.7443 -0.3395 0.2976 0.055 Uiso 1 1 calc R . . C4 C 0.7483(4) 0.0955(4) 0.2168(3) 0.0315(9) Uani 1 1 d . . . C5 C 0.7732(4) -0.0329(4) 0.1929(3) 0.0299(9) Uani 1 1 d . . . C6 C 0.8313(4) -0.0404(4) 0.0939(3) 0.0368(10) Uani 1 1 d . . . H6 H 0.8531 0.0351 0.0414 0.044 Uiso 1 1 calc R . . C7 C 0.7407(5) -0.1459(4) 0.2684(3) 0.0482(12) Uani 1 1 d . . . H7 H 0.7009 -0.1433 0.3356 0.058 Uiso 1 1 calc R . . C8 C 0.5175(4) 0.4799(4) 0.1502(3) 0.0384(10) Uani 1 1 d . . . H8 H 0.5908 0.5276 0.1113 0.046 Uiso 1 1 calc R . . C9 C 0.4018(4) 0.3348(4) 0.2599(3) 0.0408(11) Uani 1 1 d . . . H9 H 0.3800 0.2599 0.3131 0.049 Uiso 1 1 calc R . . C10 C 0.3079(5) 0.4213(4) 0.2066(3) 0.0401(11) Uani 1 1 d . . . H10 H 0.2114 0.4182 0.2161 0.048 Uiso 1 1 calc R . . C11 C 0.3270(4) 0.6393(4) 0.0665(3) 0.0437(11) Uani 1 1 d . . . H11A H 0.2320 0.6363 0.0618 0.052 Uiso 1 1 calc R . . H11B H 0.3897 0.6509 -0.0014 0.052 Uiso 1 1 calc R . . C12 C 0.3181(4) 0.7546(4) 0.1038(3) 0.0359(10) Uani 1 1 d . . . C13 C 0.4413(4) 0.8051(4) 0.0876(3) 0.0427(11) Uani 1 1 d . . . H13 H 0.5296 0.7679 0.0534 0.051 Uiso 1 1 calc R . . C14 C 0.4326(4) 0.9092(4) 0.1219(3) 0.0428(11) Uani 1 1 d . . . H14 H 0.5160 0.9410 0.1116 0.051 Uiso 1 1 calc R . . C15 C 0.3033(5) 0.9683(4) 0.1714(3) 0.0405(11) Uani 1 1 d . . . C16 C 0.1824(4) 0.9168(4) 0.1887(3) 0.0436(11) Uani 1 1 d . . . H16 H 0.0942 0.9538 0.2232 0.052 Uiso 1 1 calc R . . C17 C 0.1908(4) 0.8116(4) 0.1555(3) 0.0436(11) Uani 1 1 d . . . H17 H 0.1078 0.7778 0.1684 0.052 Uiso 1 1 calc R . . C18 C 0.0477(5) 1.2069(4) 0.2232(3) 0.0405(11) Uani 1 1 d . . . H18 H 0.0505 1.2472 0.1538 0.049 Uiso 1 1 calc R . . C19 C 0.1146(5) 1.0943(5) 0.3640(4) 0.0662(15) Uani 1 1 d . . . H19 H 0.1694 1.0425 0.4113 0.079 Uiso 1 1 calc R . . C20 C -0.0279(5) 1.1436(5) 0.3848(3) 0.0619(14) Uani 1 1 d . . . H20 H -0.0880 1.1309 0.4499 0.074 Uiso 1 1 calc R . . C21 C 0.3016(5) 1.0901(4) 0.1991(4) 0.0549(13) Uani 1 1 d . . . H21A H 0.3750 1.0710 0.2372 0.066 Uiso 1 1 calc R . . H21B H 0.3254 1.1604 0.1368 0.066 Uiso 1 1 calc R . . C22 C 0.7146(5) 0.3882(4) 0.4423(3) 0.0428(11) Uani 1 1 d . . . H22 H 0.7814 0.4405 0.3982 0.051 Uiso 1 1 calc R . . C23 C 0.5638(5) 0.2607(5) 0.4991(3) 0.0572(14) Uani 1 1 d . . . H23 H 0.5034 0.2060 0.5030 0.069 Uiso 1 1 calc R . . C24 C 0.5759(5) 0.2923(5) 0.5790(3) 0.0640(15) Uani 1 1 d . . . H24 H 0.5269 0.2629 0.6468 0.077 Uiso 1 1 calc R . . C25 C 0.7160(5) 0.4374(5) 0.6010(3) 0.0574(14) Uani 1 1 d . . . H25A H 0.7157 0.3789 0.6697 0.069 Uiso 1 1 calc R . . H25B H 0.6477 0.5175 0.6063 0.069 Uiso 1 1 calc R . . C26 C 0.8628(5) 0.4702(5) 0.5508(3) 0.0482(12) Uani 1 1 d . . . C27 C 0.9832(6) 0.3721(5) 0.5514(3) 0.0586(13) Uani 1 1 d . . . H27 H 0.9732 0.2849 0.5862 0.070 Uiso 1 1 calc R . . C28 C 1.1188(5) 0.4025(5) 0.5006(4) 0.0576(13) Uani 1 1 d . . . H28 H 1.1987 0.3351 0.5016 0.069 Uiso 1 1 calc R . . N1 N 0.5337(3) 0.3717(3) 0.2251(2) 0.0329(8) Uani 1 1 d . . . N2 N 0.3827(4) 0.5142(3) 0.1360(2) 0.0357(8) Uani 1 1 d . . . N3 N -0.0697(4) 1.2140(3) 0.2966(2) 0.0357(8) Uani 1 1 d . . . N4 N 0.1622(4) 1.1350(3) 0.2603(3) 0.0425(9) Uani 1 1 d . . . N5 N 0.6522(3) 0.3202(3) 0.4128(2) 0.0344(8) Uani 1 1 d . . . N6 N 0.6711(4) 0.3735(3) 0.5426(2) 0.0399(9) Uani 1 1 d . . . O1 O 0.7810(3) -0.5201(2) 0.20805(18) 0.0342(7) Uani 1 1 d . . . O2 O 0.8199(3) -0.3982(2) 0.01900(18) 0.0345(7) Uani 1 1 d . . . H2D H 0.8725 -0.4389 -0.0290 0.052 Uiso 1 1 d R . . O3 O 1.0289(3) -0.4737(3) 0.10448(19) 0.0374(7) Uani 1 1 d . . . O4 O 0.7929(3) 0.1927(2) 0.14956(19) 0.0377(7) Uani 1 1 d . . . O5 O 0.6848(3) 0.0999(2) 0.3077(2) 0.0397(7) Uani 1 1 d . . . O1W O 0.3545(8) 0.0600(6) 0.4930(4) 0.228(3) Uani 1 1 d . . . H1WB H 0.4334 0.0696 0.4487 0.273 Uiso 1 1 d R . . H1WA H 0.3401 -0.0181 0.5074 0.342 Uiso 1 1 d 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 Ni1 0.0383(3) 0.0211(3) 0.0353(3) -0.0119(2) -0.0112(2) -0.0034(2) P1 0.0306(6) 0.0234(6) 0.0379(6) -0.0160(5) -0.0078(5) -0.0040(5) C1 0.026(2) 0.023(2) 0.038(2) -0.0123(18) -0.0046(18) -0.0057(17) C2 0.049(3) 0.030(2) 0.033(2) -0.0131(19) -0.007(2) -0.009(2) C3 0.068(3) 0.023(2) 0.039(3) -0.011(2) 0.006(2) -0.015(2) C4 0.036(3) 0.025(2) 0.041(3) -0.014(2) -0.015(2) -0.0021(19) C5 0.033(2) 0.024(2) 0.035(2) -0.0111(19) -0.0079(19) -0.0045(18) C6 0.051(3) 0.023(2) 0.035(2) -0.0040(19) -0.012(2) -0.007(2) C7 0.073(3) 0.032(3) 0.038(3) -0.019(2) 0.007(2) -0.016(2) C8 0.039(3) 0.038(3) 0.041(3) -0.013(2) -0.011(2) -0.009(2) C9 0.047(3) 0.032(3) 0.051(3) -0.012(2) -0.014(2) -0.014(2) C10 0.036(3) 0.037(3) 0.053(3) -0.014(2) -0.014(2) -0.011(2) C11 0.049(3) 0.038(3) 0.049(3) -0.012(2) -0.026(2) -0.001(2) C12 0.041(3) 0.029(2) 0.037(2) -0.0047(19) -0.019(2) -0.001(2) C13 0.037(3) 0.038(3) 0.050(3) -0.014(2) -0.005(2) -0.005(2) C14 0.032(3) 0.039(3) 0.059(3) -0.013(2) -0.012(2) -0.009(2) C15 0.041(3) 0.031(3) 0.049(3) -0.010(2) -0.012(2) -0.006(2) C16 0.030(3) 0.035(3) 0.064(3) -0.018(2) -0.007(2) -0.002(2) C17 0.035(3) 0.034(3) 0.064(3) -0.010(2) -0.020(2) -0.007(2) C18 0.051(3) 0.029(3) 0.042(3) -0.011(2) -0.015(2) -0.001(2) C19 0.057(4) 0.075(4) 0.055(3) -0.004(3) -0.024(3) 0.002(3) C20 0.054(3) 0.078(4) 0.039(3) -0.007(3) -0.011(3) 0.002(3) C21 0.040(3) 0.046(3) 0.085(4) -0.034(3) -0.008(3) -0.005(2) C22 0.054(3) 0.040(3) 0.035(3) -0.012(2) -0.007(2) -0.011(2) C23 0.058(3) 0.070(4) 0.052(3) -0.022(3) 0.003(3) -0.038(3) C24 0.064(4) 0.095(4) 0.037(3) -0.022(3) 0.009(3) -0.041(3) C25 0.063(3) 0.083(4) 0.043(3) -0.036(3) -0.012(3) -0.018(3) C26 0.052(3) 0.063(4) 0.044(3) -0.031(3) -0.015(2) -0.008(3) C27 0.071(4) 0.051(3) 0.058(3) -0.016(3) -0.021(3) -0.010(3) C28 0.056(4) 0.060(4) 0.065(3) -0.030(3) -0.023(3) 0.002(3) N1 0.039(2) 0.026(2) 0.039(2) -0.0126(16) -0.0150(17) -0.0042(16) N2 0.039(2) 0.031(2) 0.044(2) -0.0149(17) -0.0176(18) -0.0027(17) N3 0.042(2) 0.029(2) 0.037(2) -0.0107(16) -0.0131(18) -0.0013(16) N4 0.042(2) 0.036(2) 0.051(2) -0.0155(19) -0.012(2) -0.0049(18) N5 0.039(2) 0.035(2) 0.0345(19) -0.0165(16) -0.0086(17) -0.0062(17) N6 0.043(2) 0.049(2) 0.031(2) -0.0164(17) -0.0037(17) -0.0115(18) O1 0.0437(17) 0.0208(15) 0.0414(16) -0.0101(12) -0.0096(14) -0.0097(13) O2 0.0351(16) 0.0346(17) 0.0376(15) -0.0198(13) -0.0089(13) 0.0010(13) O3 0.0274(16) 0.0441(18) 0.0492(17) -0.0262(14) -0.0140(13) 0.0024(13) O4 0.0523(19) 0.0218(16) 0.0418(16) -0.0079(13) -0.0125(14) -0.0111(14) O5 0.057(2) 0.0250(16) 0.0414(17) -0.0149(13) -0.0126(15) -0.0063(14) O1W 0.371(10) 0.140(6) 0.225(6) 0.004(5) -0.180(7) -0.080(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 Ni1 N1 2.050(3) . ? Ni1 N5 2.057(3) . ? Ni1 O1 2.065(2) 1_565 ? Ni1 N3 2.081(3) 1_645 ? Ni1 O5 2.132(2) . ? Ni1 O4 2.205(2) . ? P1 O1 1.490(2) . ? P1 O3 1.530(3) . ? P1 O2 1.537(2) . ? P1 C1 1.807(3) . ? C1 C2 1.376(5) . ? C1 C3 1.380(5) . ? C2 C6 1.382(5) . ? C2 H2 0.9300 . ? C3 C7 1.389(5) . ? C3 H3 0.9300 . ? C4 O4 1.242(4) . ? C4 O5 1.275(4) . ? C4 C5 1.505(5) . ? C5 C7 1.373(5) . ? C5 C6 1.381(5) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 N1 1.306(5) . ? C8 N2 1.343(5) . ? C8 H8 0.9300 . ? C9 C10 1.343(5) . ? C9 N1 1.364(4) . ? C9 H9 0.9300 . ? C10 N2 1.359(5) . ? C10 H10 0.9300 . ? C11 N2 1.471(5) . ? C11 C12 1.507(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C17 1.370(5) . ? C12 C13 1.393(5) . ? C13 C14 1.364(5) . ? C13 H13 0.9300 . ? C14 C15 1.379(5) . ? C14 H14 0.9300 . ? C15 C16 1.374(5) . ? C15 C21 1.515(5) . ? C16 C17 1.368(5) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 N3 1.319(4) . ? C18 N4 1.336(5) . ? C18 H18 0.9300 . ? C19 C20 1.352(6) . ? C19 N4 1.361(5) . ? C19 H19 0.9300 . ? C20 N3 1.351(5) . ? C20 H20 0.9300 . ? C21 N4 1.461(5) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 N5 1.313(4) . ? C22 N6 1.333(4) . ? C22 H22 0.9300 . ? C23 C24 1.344(5) . ? C23 N5 1.346(5) . ? C23 H23 0.9300 . ? C24 N6 1.334(5) . ? C24 H24 0.9300 . ? C25 N6 1.471(5) . ? C25 C26 1.491(6) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C28 1.368(6) 2_766 ? C26 C27 1.380(6) . ? C27 C28 1.386(6) . ? C27 H27 0.9300 . ? C28 C26 1.368(6) 2_766 ? C28 H28 0.9300 . ? N3 Ni1 2.081(3) 1_465 ? O1 Ni1 2.065(2) 1_545 ? O2 H2D 0.9043 . ? O1W H1WB 0.8500 . ? O1W H1WA 0.8500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N5 96.25(12) . . ? N1 Ni1 O1 89.58(11) . 1_565 ? N5 Ni1 O1 91.18(11) . 1_565 ? N1 Ni1 N3 173.36(12) . 1_645 ? N5 Ni1 N3 90.39(13) . 1_645 ? O1 Ni1 N3 90.10(11) 1_565 1_645 ? N1 Ni1 O5 90.44(11) . . ? N5 Ni1 O5 98.08(11) . . ? O1 Ni1 O5 170.68(10) 1_565 . ? N3 Ni1 O5 88.81(11) 1_645 . ? N1 Ni1 O4 88.18(11) . . ? N5 Ni1 O4 158.60(11) . . ? O1 Ni1 O4 109.83(9) 1_565 . ? N3 Ni1 O4 85.69(11) 1_645 . ? O5 Ni1 O4 60.86(9) . . ? O1 P1 O3 114.15(16) . . ? O1 P1 O2 113.26(14) . . ? O3 P1 O2 110.46(14) . . ? O1 P1 C1 107.25(15) . . ? O3 P1 C1 106.02(15) . . ? O2 P1 C1 104.96(16) . . ? C2 C1 C3 116.9(3) . . ? C2 C1 P1 122.2(3) . . ? C3 C1 P1 120.9(3) . . ? C1 C2 C6 121.7(4) . . ? C1 C2 H2 119.1 . . ? C6 C2 H2 119.1 . . ? C1 C3 C7 121.9(4) . . ? C1 C3 H3 119.0 . . ? C7 C3 H3 119.0 . . ? O4 C4 O5 121.7(3) . . ? O4 C4 C5 119.9(4) . . ? O5 C4 C5 118.4(3) . . ? C7 C5 C6 118.1(3) . . ? C7 C5 C4 121.2(3) . . ? C6 C5 C4 120.7(3) . . ? C5 C6 C2 120.9(4) . . ? C5 C6 H6 119.5 . . ? C2 C6 H6 119.5 . . ? C5 C7 C3 120.5(4) . . ? C5 C7 H7 119.8 . . ? C3 C7 H7 119.8 . . ? N1 C8 N2 112.1(4) . . ? N1 C8 H8 124.0 . . ? N2 C8 H8 124.0 . . ? C10 C9 N1 110.7(4) . . ? C10 C9 H9 124.6 . . ? N1 C9 H9 124.6 . . ? C9 C10 N2 105.9(4) . . ? C9 C10 H10 127.1 . . ? N2 C10 H10 127.1 . . ? N2 C11 C12 111.2(3) . . ? N2 C11 H11A 109.4 . . ? C12 C11 H11A 109.4 . . ? N2 C11 H11B 109.4 . . ? C12 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? C17 C12 C13 118.0(4) . . ? C17 C12 C11 121.7(4) . . ? C13 C12 C11 120.3(4) . . ? C14 C13 C12 120.0(4) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 121.6(4) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C16 C15 C14 118.2(4) . . ? C16 C15 C21 123.8(4) . . ? C14 C15 C21 118.0(4) . . ? C17 C16 C15 120.4(4) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C12 121.7(4) . . ? C16 C17 H17 119.1 . . ? C12 C17 H17 119.1 . . ? N3 C18 N4 111.9(4) . . ? N3 C18 H18 124.1 . . ? N4 C18 H18 124.1 . . ? C20 C19 N4 106.7(4) . . ? C20 C19 H19 126.7 . . ? N4 C19 H19 126.7 . . ? N3 C20 C19 109.8(4) . . ? N3 C20 H20 125.1 . . ? C19 C20 H20 125.1 . . ? N4 C21 C15 112.5(3) . . ? N4 C21 H21A 109.1 . . ? C15 C21 H21A 109.1 . . ? N4 C21 H21B 109.1 . . ? C15 C21 H21B 109.1 . . ? H21A C21 H21B 107.8 . . ? N5 C22 N6 112.3(4) . . ? N5 C22 H22 123.9 . . ? N6 C22 H22 123.9 . . ? C24 C23 N5 109.9(4) . . ? C24 C23 H23 125.1 . . ? N5 C23 H23 125.1 . . ? N6 C24 C23 107.2(4) . . ? N6 C24 H24 126.4 . . ? C23 C24 H24 126.4 . . ? N6 C25 C26 111.4(3) . . ? N6 C25 H25A 109.3 . . ? C26 C25 H25A 109.3 . . ? N6 C25 H25B 109.3 . . ? C26 C25 H25B 109.3 . . ? H25A C25 H25B 108.0 . . ? C28 C26 C27 118.3(5) 2_766 . ? C28 C26 C25 120.9(5) 2_766 . ? C27 C26 C25 120.7(5) . . ? C26 C27 C28 120.6(5) . . ? C26 C27 H27 119.7 . . ? C28 C27 H27 119.7 . . ? C26 C28 C27 121.2(5) 2_766 . ? C26 C28 H28 119.4 2_766 . ? C27 C28 H28 119.4 . . ? C8 N1 C9 104.6(3) . . ? C8 N1 Ni1 121.9(3) . . ? C9 N1 Ni1 133.5(3) . . ? C8 N2 C10 106.7(4) . . ? C8 N2 C11 124.6(3) . . ? C10 N2 C11 128.1(4) . . ? C18 N3 C20 105.4(4) . . ? C18 N3 Ni1 123.3(3) . 1_465 ? C20 N3 Ni1 130.6(3) . 1_465 ? C18 N4 C19 106.3(4) . . ? C18 N4 C21 125.2(4) . . ? C19 N4 C21 127.6(4) . . ? C22 N5 C23 104.5(3) . . ? C22 N5 Ni1 120.8(3) . . ? C23 N5 Ni1 133.4(3) . . ? C22 N6 C24 106.1(3) . . ? C22 N6 C25 126.8(4) . . ? C24 N6 C25 127.0(3) . . ? P1 O1 Ni1 146.29(15) . 1_545 ? P1 O2 H2D 120.7 . . ? C4 O4 Ni1 87.4(2) . . ? C4 O5 Ni1 89.9(2) . . ? H1WB O1W H1WA 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 P1 C1 C2 -163.9(3) . . . . ? O3 P1 C1 C2 73.8(4) . . . . ? O2 P1 C1 C2 -43.1(4) . . . . ? O1 P1 C1 C3 18.6(4) . . . . ? O3 P1 C1 C3 -103.7(3) . . . . ? O2 P1 C1 C3 139.3(3) . . . . ? C3 C1 C2 C6 -0.1(6) . . . . ? P1 C1 C2 C6 -177.7(3) . . . . ? C2 C1 C3 C7 -0.1(6) . . . . ? P1 C1 C3 C7 177.5(3) . . . . ? O4 C4 C5 C7 172.1(4) . . . . ? O5 C4 C5 C7 -5.9(6) . . . . ? O4 C4 C5 C6 -7.1(6) . . . . ? O5 C4 C5 C6 175.0(4) . . . . ? C7 C5 C6 C2 -0.7(6) . . . . ? C4 C5 C6 C2 178.5(4) . . . . ? C1 C2 C6 C5 0.5(6) . . . . ? C6 C5 C7 C3 0.5(6) . . . . ? C4 C5 C7 C3 -178.7(4) . . . . ? C1 C3 C7 C5 0.0(7) . . . . ? N1 C9 C10 N2 0.6(5) . . . . ? N2 C11 C12 C17 -100.1(4) . . . . ? N2 C11 C12 C13 78.9(5) . . . . ? C17 C12 C13 C14 -0.7(6) . . . . ? C11 C12 C13 C14 -179.8(4) . . . . ? C12 C13 C14 C15 -1.1(7) . . . . ? C13 C14 C15 C16 2.1(6) . . . . ? C13 C14 C15 C21 -175.1(4) . . . . ? C14 C15 C16 C17 -1.3(6) . . . . ? C21 C15 C16 C17 175.7(4) . . . . ? C15 C16 C17 C12 -0.4(7) . . . . ? C13 C12 C17 C16 1.4(6) . . . . ? C11 C12 C17 C16 -179.5(4) . . . . ? N4 C19 C20 N3 -0.1(6) . . . . ? C16 C15 C21 N4 8.9(6) . . . . ? C14 C15 C21 N4 -174.0(4) . . . . ? N5 C23 C24 N6 0.8(6) . . . . ? N6 C25 C26 C28 105.7(5) . . . 2_766 ? N6 C25 C26 C27 -71.4(5) . . . . ? C28 C26 C27 C28 -0.3(7) 2_766 . . . ? C25 C26 C27 C28 176.9(4) . . . . ? C26 C27 C28 C26 0.3(7) . . . 2_766 ? N2 C8 N1 C9 0.5(4) . . . . ? N2 C8 N1 Ni1 -178.5(2) . . . . ? C10 C9 N1 C8 -0.7(4) . . . . ? C10 C9 N1 Ni1 178.1(3) . . . . ? N5 Ni1 N1 C8 115.1(3) . . . . ? O1 Ni1 N1 C8 24.0(3) 1_565 . . . ? N3 Ni1 N1 C8 -63.3(12) 1_645 . . . ? O5 Ni1 N1 C8 -146.7(3) . . . . ? O4 Ni1 N1 C8 -85.9(3) . . . . ? N5 Ni1 N1 C9 -63.5(3) . . . . ? O1 Ni1 N1 C9 -154.6(3) 1_565 . . . ? N3 Ni1 N1 C9 118.1(10) 1_645 . . . ? O5 Ni1 N1 C9 34.7(3) . . . . ? O4 Ni1 N1 C9 95.5(3) . . . . ? N1 C8 N2 C10 -0.1(4) . . . . ? N1 C8 N2 C11 172.0(3) . . . . ? C9 C10 N2 C8 -0.3(4) . . . . ? C9 C10 N2 C11 -172.0(3) . . . . ? C12 C11 N2 C8 -67.2(5) . . . . ? C12 C11 N2 C10 103.2(4) . . . . ? N4 C18 N3 C20 0.2(5) . . . . ? N4 C18 N3 Ni1 -171.3(2) . . . 1_465 ? C19 C20 N3 C18 -0.1(5) . . . . ? C19 C20 N3 Ni1 170.6(3) . . . 1_465 ? N3 C18 N4 C19 -0.3(5) . . . . ? N3 C18 N4 C21 169.2(3) . . . . ? C20 C19 N4 C18 0.2(5) . . . . ? C20 C19 N4 C21 -169.0(4) . . . . ? C15 C21 N4 C18 -80.6(5) . . . . ? C15 C21 N4 C19 86.6(5) . . . . ? N6 C22 N5 C23 0.6(5) . . . . ? N6 C22 N5 Ni1 -168.2(3) . . . . ? C24 C23 N5 C22 -0.8(5) . . . . ? C24 C23 N5 Ni1 165.8(3) . . . . ? N1 Ni1 N5 C22 -123.7(3) . . . . ? O1 Ni1 N5 C22 -34.0(3) 1_565 . . . ? N3 Ni1 N5 C22 56.1(3) 1_645 . . . ? O5 Ni1 N5 C22 144.9(3) . . . . ? O4 Ni1 N5 C22 135.2(3) . . . . ? N1 Ni1 N5 C23 71.3(4) . . . . ? O1 Ni1 N5 C23 161.0(4) 1_565 . . . ? N3 Ni1 N5 C23 -108.8(4) 1_645 . . . ? O5 Ni1 N5 C23 -20.0(4) . . . . ? O4 Ni1 N5 C23 -29.7(6) . . . . ? N5 C22 N6 C24 -0.1(5) . . . . ? N5 C22 N6 C25 -178.5(4) . . . . ? C23 C24 N6 C22 -0.4(5) . . . . ? C23 C24 N6 C25 178.0(4) . . . . ? C26 C25 N6 C22 -27.2(6) . . . . ? C26 C25 N6 C24 154.8(5) . . . . ? O3 P1 O1 Ni1 -65.6(3) . . . 1_545 ? O2 P1 O1 Ni1 62.0(3) . . . 1_545 ? C1 P1 O1 Ni1 177.3(3) . . . 1_545 ? O5 C4 O4 Ni1 4.4(4) . . . . ? C5 C4 O4 Ni1 -173.5(3) . . . . ? N1 Ni1 O4 C4 -94.1(2) . . . . ? N5 Ni1 O4 C4 8.5(4) . . . . ? O1 Ni1 O4 C4 177.0(2) 1_565 . . . ? N3 Ni1 O4 C4 88.5(2) 1_645 . . . ? O5 Ni1 O4 C4 -2.6(2) . . . . ? O4 C4 O5 Ni1 -4.5(4) . . . . ? C5 C4 O5 Ni1 173.4(3) . . . . ? N1 Ni1 O5 C4 90.2(2) . . . . ? N5 Ni1 O5 C4 -173.5(2) . . . . ? O1 Ni1 O5 C4 0.1(8) 1_565 . . . ? N3 Ni1 O5 C4 -83.2(2) 1_645 . . . ? O4 Ni1 O5 C4 2.5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.599 _refine_diff_density_min -0.446 _refine_diff_density_rms 0.067