Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'R. C. Finn' 'J. Zubieta' _publ_contact_author_name 'Prof Jon Zubieta' _publ_contact_author_address ; ? ; _publ_contact_author_email 'jazubiet@syr.edu' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Hydrothermal synthesis and structural characterisaiton of organically templated zinc vanadium phosphates: [Zn(2,2'-bipyridine)(VO2)(PO4)], [Zn(2,2':6',2''-terpyridine)(VO2)(PO4)], and [Zn(1,10-phenanthroline)(ZnVO)(PO4)2] ; data_compound(1) _database_code_CSD 175194 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H16 N4 O12 P2 V2 Zn2' _chemical_formula_weight 798.93 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' 'V' 'V' 0.3005 0.5294 '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 P21/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 7.7860(3) _cell_length_b 17.2896(7) _cell_length_c 9.7897(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.7440(10) _cell_angle_gamma 90.00 _cell_volume 1274.46(9) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.082 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 2.770 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 8421 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 28.28 _reflns_number_total 3059 _reflns_number_gt 2639 _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^)+(0.0311P)^2^+0.8781P] 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 3059 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0340 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0645 _refine_ls_wR_factor_gt 0.0622 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 0.47409(3) 0.551086(14) 0.71934(3) 0.01030(8) Uani 1 1 d . . . V2 V 0.11637(5) 0.62185(2) 0.49462(4) 0.00976(9) Uani 1 1 d . . . P3 P 0.23732(7) 0.45841(3) 0.47200(6) 0.00895(12) Uani 1 1 d . . . O1 O 0.2916(2) 0.47356(9) 0.63094(16) 0.0130(3) Uani 1 1 d . . . O3 O 0.2872(2) 0.64257(9) 0.62754(17) 0.0138(3) Uani 1 1 d . . . C4 C 0.8446(3) 0.46326(13) 1.0884(2) 0.0147(4) Uani 1 1 d . . . H4 H 0.9073 0.4863 1.1720 0.018 Uiso 1 1 calc R . . O2 O 0.6164(2) 0.57323(9) 0.58697(17) 0.0140(3) Uani 1 1 d . . . O4 O 0.1640(2) 0.53710(8) 0.39492(17) 0.0128(3) Uani 1 1 d . . . O5 O -0.0779(2) 0.59896(9) 0.56382(17) 0.0157(3) Uani 1 1 d . . . O6 O 0.0776(2) 0.69493(9) 0.38964(18) 0.0192(4) Uani 1 1 d . . . N2 N 0.5703(2) 0.62240(10) 0.8921(2) 0.0121(4) Uani 1 1 d . . . N1 N 0.6337(2) 0.47398(10) 0.86394(19) 0.0113(4) Uani 1 1 d . . . C1 C 0.6556(3) 0.39857(13) 0.8406(2) 0.0146(5) Uani 1 1 d . . . H1 H 0.5909 0.3767 0.7564 0.018 Uiso 1 1 calc R . . C2 C 0.7707(3) 0.35220(13) 0.9372(3) 0.0168(5) Uani 1 1 d . . . H2 H 0.7845 0.3002 0.9180 0.020 Uiso 1 1 calc R . . C3 C 0.8654(3) 0.38500(13) 1.0637(3) 0.0172(5) Uani 1 1 d . . . H3 H 0.9420 0.3548 1.1313 0.021 Uiso 1 1 calc R . . C5 C 0.7276(3) 0.50631(12) 0.9848(2) 0.0115(4) Uani 1 1 d . . . C6 C 0.6947(3) 0.59071(12) 0.9992(2) 0.0115(4) Uani 1 1 d . . . C7 C 0.7865(3) 0.63443(13) 1.1129(2) 0.0154(5) Uani 1 1 d . . . H7 H 0.8733 0.6118 1.1850 0.018 Uiso 1 1 calc R . . C8 C 0.7467(3) 0.71275(13) 1.1177(3) 0.0180(5) Uani 1 1 d . . . H8 H 0.8069 0.7431 1.1932 0.022 Uiso 1 1 calc R . . C9 C 0.6172(3) 0.74484(13) 1.0097(3) 0.0186(5) Uani 1 1 d . . . H9 H 0.5873 0.7968 1.0116 0.022 Uiso 1 1 calc R . . C10 C 0.5326(3) 0.69785(13) 0.8981(3) 0.0163(5) Uani 1 1 d . . . H10 H 0.4463 0.7195 0.8245 0.020 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 0.01002(13) 0.01063(12) 0.00905(13) -0.00032(9) 0.00025(9) -0.00045(9) V2 0.00902(18) 0.00877(17) 0.01007(18) -0.00046(13) -0.00018(13) 0.00003(13) P3 0.0073(3) 0.0093(2) 0.0099(3) -0.0006(2) 0.0016(2) -0.0001(2) O1 0.0141(8) 0.0133(7) 0.0108(8) 0.0000(6) 0.0017(6) -0.0036(6) O3 0.0111(8) 0.0141(7) 0.0144(8) -0.0024(6) -0.0001(6) 0.0015(6) C4 0.0125(11) 0.0196(11) 0.0108(11) 0.0002(9) 0.0009(8) -0.0012(9) O2 0.0142(8) 0.0117(7) 0.0177(8) 0.0014(6) 0.0073(7) 0.0010(6) O4 0.0140(8) 0.0110(7) 0.0122(8) -0.0020(6) 0.0010(6) 0.0011(6) O5 0.0116(8) 0.0168(8) 0.0185(9) -0.0049(7) 0.0035(6) -0.0020(6) O6 0.0234(9) 0.0139(8) 0.0158(9) 0.0017(6) -0.0033(7) -0.0003(7) N2 0.0118(9) 0.0126(9) 0.0118(9) -0.0015(7) 0.0027(7) -0.0013(7) N1 0.0116(9) 0.0107(8) 0.0114(9) 0.0002(7) 0.0022(7) -0.0008(7) C1 0.0180(12) 0.0133(10) 0.0130(11) -0.0023(8) 0.0048(9) -0.0015(9) C2 0.0207(12) 0.0115(10) 0.0200(12) 0.0016(9) 0.0082(10) 0.0027(9) C3 0.0136(11) 0.0189(11) 0.0187(12) 0.0058(9) 0.0032(9) 0.0047(9) C5 0.0094(10) 0.0147(10) 0.0115(11) 0.0003(8) 0.0046(8) -0.0015(8) C6 0.0090(10) 0.0147(10) 0.0109(10) -0.0005(8) 0.0028(8) -0.0015(8) C7 0.0139(11) 0.0192(11) 0.0110(11) -0.0007(9) -0.0005(9) -0.0024(9) C8 0.0201(12) 0.0172(11) 0.0153(12) -0.0059(9) 0.0022(9) -0.0054(9) C9 0.0223(13) 0.0118(10) 0.0212(13) -0.0029(9) 0.0044(10) -0.0017(9) C10 0.0165(12) 0.0148(11) 0.0159(12) 0.0011(9) 0.0010(9) 0.0008(9) _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 1.9456(16) . ? Zn1 O1 1.9844(15) . ? Zn1 N2 2.0730(19) . ? Zn1 N1 2.1046(18) . ? Zn1 O3 2.1819(15) . ? V2 O6 1.6081(16) . ? V2 O3 1.6463(16) . ? V2 O4 1.8497(15) . ? V2 O5 1.8505(16) . ? P3 O2 1.5046(16) 3_666 ? P3 O1 1.5275(16) . ? P3 O5 1.5577(16) 3_566 ? P3 O4 1.5896(16) . ? C4 C3 1.391(3) . ? C4 C5 1.393(3) . ? O2 P3 1.5046(16) 3_666 ? O5 P3 1.5577(16) 3_566 ? N2 C10 1.342(3) . ? N2 C6 1.349(3) . ? N1 C1 1.342(3) . ? N1 C5 1.345(3) . ? C1 C2 1.381(3) . ? C2 C3 1.391(3) . ? C5 C6 1.494(3) . ? C6 C7 1.384(3) . ? C7 C8 1.393(3) . ? C8 C9 1.379(3) . ? C9 C10 1.386(3) . ? 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 O1 107.96(7) . . ? O2 Zn1 N2 106.11(7) . . ? O1 Zn1 N2 145.85(7) . . ? O2 Zn1 N1 103.52(7) . . ? O1 Zn1 N1 95.74(7) . . ? N2 Zn1 N1 78.41(7) . . ? O2 Zn1 O3 90.92(6) . . ? O1 Zn1 O3 88.95(6) . . ? N2 Zn1 O3 88.26(7) . . ? N1 Zn1 O3 162.52(7) . . ? O6 V2 O3 108.46(8) . . ? O6 V2 O4 108.39(8) . . ? O3 V2 O4 111.05(7) . . ? O6 V2 O5 111.35(8) . . ? O3 V2 O5 109.18(8) . . ? O4 V2 O5 108.43(7) . . ? O2 P3 O1 114.38(9) 3_666 . ? O2 P3 O5 108.64(9) 3_666 3_566 ? O1 P3 O5 109.68(9) . 3_566 ? O2 P3 O4 110.15(9) 3_666 . ? O1 P3 O4 108.04(9) . . ? O5 P3 O4 105.59(9) 3_566 . ? P3 O1 Zn1 122.82(9) . . ? V2 O3 Zn1 119.20(8) . . ? C3 C4 C5 118.5(2) . . ? P3 O2 Zn1 143.04(10) 3_666 . ? P3 O4 V2 121.56(9) . . ? P3 O5 V2 137.10(10) 3_566 . ? C10 N2 C6 118.9(2) . . ? C10 N2 Zn1 125.19(16) . . ? C6 N2 Zn1 115.56(15) . . ? C1 N1 C5 119.29(19) . . ? C1 N1 Zn1 125.45(15) . . ? C5 N1 Zn1 115.12(14) . . ? N1 C1 C2 122.4(2) . . ? C1 C2 C3 118.5(2) . . ? C4 C3 C2 119.5(2) . . ? N1 C5 C4 121.8(2) . . ? N1 C5 C6 114.89(19) . . ? C4 C5 C6 123.3(2) . . ? N2 C6 C7 121.7(2) . . ? N2 C6 C5 115.45(19) . . ? C7 C6 C5 122.9(2) . . ? C6 C7 C8 119.0(2) . . ? C9 C8 C7 119.4(2) . . ? C8 C9 C10 118.5(2) . . ? N2 C10 C9 122.6(2) . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.439 _refine_diff_density_min -0.445 _refine_diff_density_rms 0.092 #================================END data_compound(2) _database_code_CSD 175195 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H22 N6 O12 P2 V2 Zn2' _chemical_formula_weight 953.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'V' 'V' 0.3005 0.5294 '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 10.4536(2) _cell_length_b 11.8867(2) _cell_length_c 13.99810(10) _cell_angle_alpha 93.0340(10) _cell_angle_beta 93.7660(10) _cell_angle_gamma 105.4680(10) _cell_volume 1668.27(4) _cell_formula_units_Z 2 _cell_measurement_temperature 89(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.897 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 2.135 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 10526 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.0783 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 28.14 _reflns_number_total 7245 _reflns_number_gt 5479 _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^)+(0.0366P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0019(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7245 _refine_ls_number_parameters 488 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.0966 _refine_ls_wR_factor_gt 0.0896 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.966 _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 0.31926(4) 0.43330(3) 1.07927(3) 0.00836(10) Uani 1 1 d . . . Zn2 Zn 0.15900(4) 0.00644(4) 0.40495(3) 0.00949(10) Uani 1 1 d . . . V1 V 0.24311(6) 0.40474(5) 0.63661(4) 0.01022(14) Uani 1 1 d . . . V2 V 0.28113(6) 0.14980(5) 0.83750(4) 0.01042(14) Uani 1 1 d . . . P1 P 0.38821(9) 0.42314(8) 0.85606(6) 0.01074(19) Uani 1 1 d . . . P2 P 0.14281(9) 0.12313(8) 0.62113(6) 0.00949(19) Uani 1 1 d . . . O1 O -0.0059(2) -0.0954(2) 0.34116(18) 0.0191(6) Uani 1 1 d . . . O2 O 0.1567(2) 0.0334(2) 0.54362(16) 0.0127(5) Uani 1 1 d . . . O3 O 0.1808(3) 0.2486(2) 0.58587(18) 0.0288(7) Uani 1 1 d . . . O4 O 0.3746(3) 0.4702(2) 0.58541(18) 0.0215(6) Uani 1 1 d . . . O5 O 0.1315(3) 0.4739(3) 0.61479(19) 0.0248(7) Uani 1 1 d . . . O6 O 0.2816(2) 0.4101(2) 0.76948(17) 0.0143(5) Uani 1 1 d . . . O7 O 0.4027(2) 0.2967(2) 0.86976(17) 0.0141(5) Uani 1 1 d . . . O8 O 0.3474(3) 0.0496(2) 0.87548(18) 0.0205(6) Uani 1 1 d . . . O9 O 0.1419(3) 0.1392(2) 0.88649(17) 0.0149(6) Uani 1 1 d . . . O10 O 0.2497(2) 0.1248(2) 0.70562(16) 0.0142(5) Uani 1 1 d . . . O11 O 0.3367(2) 0.4707(2) 0.94487(16) 0.0119(5) Uani 1 1 d . . . O12 O 0.4784(2) 0.4997(2) 1.16840(16) 0.0145(5) Uani 1 1 d . . . N1 N 0.3371(4) 0.2572(3) 1.0845(2) 0.0184(7) Uani 1 1 d . . . N2 N 0.1262(3) 0.3321(3) 1.0982(2) 0.0120(6) Uani 1 1 d . . . N3 N 0.2117(3) 0.5598(3) 1.1207(2) 0.0123(6) Uani 1 1 d . . . N4 N 0.1504(3) 0.1752(3) 0.3597(2) 0.0127(6) Uani 1 1 d . . . N5 N 0.3500(3) 0.0802(3) 0.36378(19) 0.0102(6) Uani 1 1 d . . . N6 N 0.2584(3) -0.1334(3) 0.4141(2) 0.0111(6) Uani 1 1 d . . . C1 C 0.4531(5) 0.2280(4) 1.0821(3) 0.0282(11) Uani 1 1 d . . . H1 H 0.5310 0.2861 1.0756 0.034 Uiso 1 1 calc R . . C2 C 0.4593(7) 0.1132(5) 1.0889(3) 0.0446(16) Uani 1 1 d . . . H2 H 0.5402 0.0948 1.0871 0.054 Uiso 1 1 calc R . . C3 C 0.3436(8) 0.0271(5) 1.0985(3) 0.056(2) Uani 1 1 d . . . H3 H 0.3458 -0.0503 1.1019 0.067 Uiso 1 1 calc R . . C4 C 0.2248(6) 0.0558(4) 1.1029(3) 0.0418(14) Uani 1 1 d . . . H4 H 0.1468 -0.0011 1.1116 0.050 Uiso 1 1 calc R . . C5 C 0.2237(5) 0.1720(3) 1.0942(2) 0.0218(9) Uani 1 1 d . . . C6 C 0.1017(4) 0.2149(3) 1.0948(2) 0.0209(9) Uani 1 1 d . . . C7 C -0.0290(5) 0.1439(4) 1.0948(3) 0.0370(13) Uani 1 1 d . . . H7 H -0.0469 0.0629 1.0939 0.044 Uiso 1 1 calc R . . C8 C -0.1311(5) 0.1985(5) 1.0961(3) 0.0463(15) Uani 1 1 d . . . H8 H -0.2189 0.1531 1.0935 0.056 Uiso 1 1 calc R . . C9 C -0.1047(4) 0.3188(5) 1.1012(3) 0.0331(12) Uani 1 1 d . . . H9 H -0.1734 0.3548 1.1028 0.040 Uiso 1 1 calc R . . C10 C 0.0288(4) 0.3856(4) 1.1039(2) 0.0174(8) Uani 1 1 d . . . C11 C 0.0779(4) 0.5149(4) 1.1218(2) 0.0164(8) Uani 1 1 d . . . C12 C -0.0045(5) 0.5854(4) 1.1469(3) 0.0303(11) Uani 1 1 d . . . H12 H -0.0964 0.5544 1.1431 0.036 Uiso 1 1 calc R . . C13 C 0.0532(5) 0.7026(5) 1.1775(3) 0.0359(13) Uani 1 1 d . . . H13 H 0.0003 0.7505 1.1956 0.043 Uiso 1 1 calc R . . C14 C 0.1901(5) 0.7469(4) 1.1808(3) 0.0278(10) Uani 1 1 d . . . H14 H 0.2312 0.8238 1.2035 0.033 Uiso 1 1 calc R . . C15 C 0.2647(4) 0.6733(3) 1.1491(3) 0.0200(9) Uani 1 1 d . . . H15 H 0.3561 0.7045 1.1476 0.024 Uiso 1 1 calc R . . C16 C 0.0440(4) 0.2187(3) 0.3632(2) 0.0163(8) Uani 1 1 d . . . H16 H -0.0375 0.1682 0.3743 0.020 Uiso 1 1 calc R . . C17 C 0.0505(4) 0.3358(3) 0.3508(3) 0.0184(8) Uani 1 1 d . . . H17 H -0.0245 0.3635 0.3542 0.022 Uiso 1 1 calc R . . C18 C 0.1726(4) 0.4096(3) 0.3334(2) 0.0197(9) Uani 1 1 d . . . H18 H 0.1802 0.4879 0.3243 0.024 Uiso 1 1 calc R . . C19 C 0.2833(4) 0.3669(3) 0.3296(2) 0.0175(8) Uani 1 1 d . . . H19 H 0.3654 0.4162 0.3183 0.021 Uiso 1 1 calc R . . C20 C 0.2698(4) 0.2489(3) 0.3430(2) 0.0133(8) Uani 1 1 d . . . C21 C 0.3822(4) 0.1928(3) 0.3409(2) 0.0123(7) Uani 1 1 d . . . C22 C 0.5109(4) 0.2492(3) 0.3187(3) 0.0167(8) Uani 1 1 d . . . H22 H 0.5328 0.3265 0.3025 0.020 Uiso 1 1 calc R . . C23 C 0.6059(4) 0.1855(4) 0.3216(3) 0.0193(8) Uani 1 1 d . . . H23 H 0.6924 0.2206 0.3071 0.023 Uiso 1 1 calc R . . C24 C 0.5713(4) 0.0693(3) 0.3462(2) 0.0158(8) Uani 1 1 d . . . H24 H 0.6342 0.0267 0.3482 0.019 Uiso 1 1 calc R . . C25 C 0.4413(4) 0.0185(3) 0.3676(2) 0.0119(7) Uani 1 1 d . . . C26 C 0.3893(3) -0.1032(3) 0.3974(2) 0.0108(7) Uani 1 1 d . . . C27 C 0.4669(4) -0.1815(3) 0.4079(3) 0.0160(8) Uani 1 1 d . . . H27 H 0.5554 -0.1610 0.3934 0.019 Uiso 1 1 calc R . . C28 C 0.4091(4) -0.2916(3) 0.4406(3) 0.0178(8) Uani 1 1 d . . . H28 H 0.4596 -0.3444 0.4498 0.021 Uiso 1 1 calc R . . C29 C 0.2751(4) -0.3214(3) 0.4593(3) 0.0159(8) Uani 1 1 d . . . H29 H 0.2353 -0.3936 0.4819 0.019 Uiso 1 1 calc R . . C30 C 0.2024(4) -0.2409(3) 0.4434(2) 0.0138(8) Uani 1 1 d . . . H30 H 0.1123 -0.2617 0.4532 0.017 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 0.0078(2) 0.0088(2) 0.0085(2) -0.00038(14) 0.00051(15) 0.00258(16) Zn2 0.0089(2) 0.0118(2) 0.0085(2) -0.00035(15) 0.00034(15) 0.00424(16) V1 0.0125(3) 0.0090(3) 0.0091(3) 0.0001(2) 0.0000(2) 0.0031(2) V2 0.0124(3) 0.0129(3) 0.0073(3) -0.0007(2) -0.0006(2) 0.0062(2) P1 0.0079(5) 0.0154(5) 0.0073(4) -0.0015(3) 0.0003(3) 0.0009(4) P2 0.0107(5) 0.0095(5) 0.0079(4) -0.0012(3) -0.0017(3) 0.0031(4) O1 0.0100(14) 0.0277(16) 0.0179(14) -0.0114(11) -0.0029(11) 0.0057(12) O2 0.0167(14) 0.0134(13) 0.0085(12) -0.0036(9) -0.0011(10) 0.0062(11) O3 0.059(2) 0.0089(14) 0.0125(14) -0.0019(11) -0.0076(14) 0.0011(14) O4 0.0188(15) 0.0266(17) 0.0186(14) 0.0041(11) 0.0069(12) 0.0033(12) O5 0.0278(17) 0.0313(18) 0.0219(15) 0.0013(12) -0.0031(13) 0.0209(14) O6 0.0094(13) 0.0221(15) 0.0097(12) -0.0014(10) -0.0003(10) 0.0021(11) O7 0.0128(13) 0.0137(14) 0.0147(13) -0.0011(10) 0.0009(10) 0.0024(10) O8 0.0257(16) 0.0233(16) 0.0171(14) -0.0011(11) -0.0045(12) 0.0163(13) O9 0.0172(14) 0.0168(14) 0.0124(12) 0.0022(10) 0.0038(11) 0.0068(11) O10 0.0114(13) 0.0236(15) 0.0086(12) -0.0011(10) -0.0018(10) 0.0072(11) O11 0.0144(13) 0.0145(14) 0.0065(11) -0.0008(9) 0.0036(10) 0.0031(10) O12 0.0083(13) 0.0223(15) 0.0098(12) -0.0004(10) -0.0004(10) -0.0008(11) N1 0.037(2) 0.0139(17) 0.0079(15) -0.0011(12) -0.0028(14) 0.0152(15) N2 0.0118(16) 0.0128(16) 0.0082(14) -0.0011(11) 0.0007(12) -0.0018(12) N3 0.0144(16) 0.0151(17) 0.0094(14) -0.0008(12) 0.0005(12) 0.0080(13) N4 0.0164(17) 0.0142(16) 0.0083(14) -0.0005(12) -0.0007(12) 0.0065(13) N5 0.0112(15) 0.0132(16) 0.0071(14) 0.0002(11) 0.0000(12) 0.0053(12) N6 0.0130(16) 0.0120(16) 0.0092(14) -0.0009(11) -0.0002(12) 0.0054(12) C1 0.046(3) 0.038(3) 0.0106(19) -0.0092(17) -0.0086(19) 0.033(2) C2 0.091(5) 0.054(4) 0.011(2) -0.005(2) -0.011(2) 0.063(4) C3 0.147(7) 0.027(3) 0.012(2) 0.000(2) 0.000(3) 0.055(4) C4 0.100(5) 0.014(2) 0.011(2) -0.0007(16) 0.003(2) 0.015(3) C5 0.049(3) 0.011(2) 0.0052(17) 0.0003(14) -0.0005(17) 0.0086(19) C6 0.031(2) 0.019(2) 0.0054(17) 0.0016(14) 0.0008(16) -0.0065(17) C7 0.044(3) 0.031(3) 0.016(2) -0.0033(18) 0.003(2) -0.024(2) C8 0.022(3) 0.069(4) 0.021(2) -0.008(2) 0.002(2) -0.032(3) C9 0.012(2) 0.059(3) 0.017(2) -0.004(2) 0.0010(17) -0.008(2) C10 0.0123(19) 0.032(2) 0.0065(17) 0.0018(15) 0.0010(14) 0.0026(16) C11 0.015(2) 0.030(2) 0.0084(17) 0.0015(15) -0.0007(15) 0.0145(17) C12 0.025(2) 0.059(3) 0.017(2) 0.002(2) 0.0018(18) 0.029(2) C13 0.056(3) 0.054(3) 0.016(2) -0.003(2) 0.000(2) 0.049(3) C14 0.050(3) 0.021(2) 0.019(2) -0.0046(17) -0.007(2) 0.027(2) C15 0.028(2) 0.017(2) 0.0170(19) 0.0007(15) -0.0011(17) 0.0113(17) C16 0.022(2) 0.020(2) 0.0098(17) -0.0006(14) 0.0015(15) 0.0113(17) C17 0.025(2) 0.020(2) 0.0149(19) 0.0009(15) -0.0012(16) 0.0155(18) C18 0.038(3) 0.013(2) 0.0095(18) -0.0039(14) -0.0034(17) 0.0123(18) C19 0.028(2) 0.013(2) 0.0097(17) 0.0013(14) 0.0003(16) 0.0024(16) C20 0.019(2) 0.017(2) 0.0047(16) 0.0003(14) 0.0009(14) 0.0070(16) C21 0.0159(19) 0.0157(19) 0.0052(16) -0.0017(13) -0.0005(14) 0.0049(15) C22 0.019(2) 0.017(2) 0.0134(18) -0.0018(15) 0.0015(15) 0.0034(16) C23 0.012(2) 0.027(2) 0.0152(19) -0.0025(16) 0.0046(15) 0.0003(16) C24 0.0122(19) 0.024(2) 0.0128(18) -0.0011(15) 0.0013(15) 0.0077(16) C25 0.0135(19) 0.018(2) 0.0053(16) 0.0007(13) 0.0010(14) 0.0073(15) C26 0.0102(18) 0.0160(19) 0.0062(16) -0.0004(13) -0.0014(13) 0.0042(14) C27 0.0137(19) 0.024(2) 0.0139(18) 0.0006(15) 0.0020(15) 0.0115(16) C28 0.026(2) 0.016(2) 0.0143(18) -0.0001(15) -0.0012(16) 0.0123(17) C29 0.025(2) 0.0103(19) 0.0138(18) 0.0013(14) 0.0013(16) 0.0076(16) C30 0.0143(19) 0.017(2) 0.0101(17) -0.0013(14) 0.0015(14) 0.0051(15) _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 1.965(2) . ? Zn1 O12 1.967(2) . ? Zn1 N2 2.097(3) . ? Zn1 N1 2.155(3) . ? Zn1 N3 2.182(3) . ? Zn2 O1 1.950(3) . ? Zn2 O2 1.953(2) . ? Zn2 N5 2.088(3) . ? Zn2 N4 2.158(3) . ? Zn2 N6 2.187(3) . ? V1 O5 1.619(3) . ? V1 O4 1.621(3) . ? V1 O6 1.871(2) . ? V1 O3 1.878(3) . ? V2 O8 1.624(2) . ? V2 O9 1.627(2) . ? V2 O10 1.848(2) . ? V2 O7 1.877(3) . ? P1 O12 1.522(3) 2_667 ? P1 O11 1.527(2) . ? P1 O6 1.564(3) . ? P1 O7 1.571(3) . ? P2 O1 1.517(3) 2_556 ? P2 O2 1.522(2) . ? P2 O3 1.554(3) . ? P2 O10 1.569(3) . ? O1 P2 1.517(3) 2_556 ? O12 P1 1.522(2) 2_667 ? N1 C1 1.350(5) . ? N1 C5 1.357(5) . ? N2 C10 1.342(5) . ? N2 C6 1.345(5) . ? N3 C15 1.342(5) . ? N3 C11 1.359(5) . ? N4 C16 1.348(5) . ? N4 C20 1.363(5) . ? N5 C25 1.350(4) . ? N5 C21 1.352(4) . ? N6 C30 1.354(4) . ? N6 C26 1.359(4) . ? C1 C2 1.391(6) . ? C2 C3 1.380(8) . ? C3 C4 1.376(8) . ? C4 C5 1.397(6) . ? C5 C6 1.495(6) . ? C6 C7 1.401(6) . ? C7 C8 1.390(7) . ? C8 C9 1.378(7) . ? C9 C10 1.406(5) . ? C10 C11 1.487(6) . ? C11 C12 1.399(5) . ? C12 C13 1.395(7) . ? C13 C14 1.384(7) . ? C14 C15 1.392(5) . ? C16 C17 1.397(5) . ? C17 C18 1.387(6) . ? C18 C19 1.384(5) . ? C19 C20 1.396(5) . ? C20 C21 1.498(5) . ? C21 C22 1.398(5) . ? C22 C23 1.399(5) . ? C23 C24 1.399(5) . ? C24 C25 1.392(5) . ? C25 C26 1.495(5) . ? C26 C27 1.396(5) . ? C27 C28 1.403(5) . ? C28 C29 1.397(5) . ? C29 C30 1.388(5) . ? 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 O12 115.90(10) . . ? O11 Zn1 N2 111.08(11) . . ? O12 Zn1 N2 132.97(10) . . ? O11 Zn1 N1 105.67(10) . . ? O12 Zn1 N1 93.36(12) . . ? N2 Zn1 N1 75.44(13) . . ? O11 Zn1 N3 97.75(10) . . ? O12 Zn1 N3 96.50(11) . . ? N2 Zn1 N3 75.13(12) . . ? N1 Zn1 N3 147.40(12) . . ? O1 Zn2 O2 114.54(11) . . ? O1 Zn2 N5 135.11(11) . . ? O2 Zn2 N5 109.88(11) . . ? O1 Zn2 N4 101.48(12) . . ? O2 Zn2 N4 100.23(10) . . ? N5 Zn2 N4 76.30(11) . . ? O1 Zn2 N6 94.27(11) . . ? O2 Zn2 N6 94.98(10) . . ? N5 Zn2 N6 75.39(11) . . ? N4 Zn2 N6 151.04(11) . . ? O5 V1 O4 107.48(14) . . ? O5 V1 O6 108.93(12) . . ? O4 V1 O6 110.46(13) . . ? O5 V1 O3 110.18(15) . . ? O4 V1 O3 109.64(14) . . ? O6 V1 O3 110.11(11) . . ? O8 V2 O9 109.11(13) . . ? O8 V2 O10 107.80(12) . . ? O9 V2 O10 110.25(12) . . ? O8 V2 O7 108.40(13) . . ? O9 V2 O7 111.40(12) . . ? O10 V2 O7 109.79(11) . . ? O12 P1 O11 113.12(14) 2_667 . ? O12 P1 O6 109.87(13) 2_667 . ? O11 P1 O6 108.41(14) . . ? O12 P1 O7 108.59(14) 2_667 . ? O11 P1 O7 110.59(13) . . ? O6 P1 O7 106.01(14) . . ? O1 P2 O2 113.46(15) 2_556 . ? O1 P2 O3 110.53(17) 2_556 . ? O2 P2 O3 111.12(14) . . ? O1 P2 O10 109.22(14) 2_556 . ? O2 P2 O10 106.78(13) . . ? O3 P2 O10 105.33(15) . . ? P2 O1 Zn2 126.87(15) 2_556 . ? P2 O2 Zn2 142.63(15) . . ? P2 O3 V1 139.40(16) . . ? P1 O6 V1 148.30(16) . . ? P1 O7 V2 130.33(16) . . ? P2 O10 V2 142.02(15) . . ? P1 O11 Zn1 137.29(15) . . ? P1 O12 Zn1 126.79(14) 2_667 . ? C1 N1 C5 118.9(4) . . ? C1 N1 Zn1 124.2(3) . . ? C5 N1 Zn1 116.8(3) . . ? C10 N2 C6 122.1(3) . . ? C10 N2 Zn1 118.7(3) . . ? C6 N2 Zn1 118.9(3) . . ? C15 N3 C11 118.2(3) . . ? C15 N3 Zn1 126.8(3) . . ? C11 N3 Zn1 114.9(2) . . ? C16 N4 C20 118.5(3) . . ? C16 N4 Zn2 125.3(3) . . ? C20 N4 Zn2 115.2(2) . . ? C25 N5 C21 121.4(3) . . ? C25 N5 Zn2 119.9(2) . . ? C21 N5 Zn2 118.5(2) . . ? C30 N6 C26 119.4(3) . . ? C30 N6 Zn2 124.7(2) . . ? C26 N6 Zn2 115.6(2) . . ? N1 C1 C2 121.8(5) . . ? C3 C2 C1 118.9(5) . . ? C4 C3 C2 120.0(4) . . ? C3 C4 C5 118.7(5) . . ? N1 C5 C4 121.6(4) . . ? N1 C5 C6 113.9(3) . . ? C4 C5 C6 124.5(4) . . ? N2 C6 C7 120.4(4) . . ? N2 C6 C5 114.2(3) . . ? C7 C6 C5 125.4(4) . . ? C8 C7 C6 117.8(4) . . ? C9 C8 C7 121.3(4) . . ? C8 C9 C10 118.3(5) . . ? N2 C10 C9 120.0(4) . . ? N2 C10 C11 113.8(3) . . ? C9 C10 C11 126.0(4) . . ? N3 C11 C12 121.5(4) . . ? N3 C11 C10 115.2(3) . . ? C12 C11 C10 123.0(4) . . ? C13 C12 C11 119.1(4) . . ? C14 C13 C12 119.2(4) . . ? C13 C14 C15 118.4(4) . . ? N3 C15 C14 123.4(4) . . ? N4 C16 C17 123.1(4) . . ? C18 C17 C16 117.6(4) . . ? C19 C18 C17 120.3(4) . . ? C18 C19 C20 119.0(4) . . ? N4 C20 C19 121.4(3) . . ? N4 C20 C21 114.6(3) . . ? C19 C20 C21 124.0(3) . . ? N5 C21 C22 121.1(3) . . ? N5 C21 C20 114.3(3) . . ? C22 C21 C20 124.6(3) . . ? C21 C22 C23 117.9(4) . . ? C24 C23 C22 120.3(3) . . ? C25 C24 C23 118.9(3) . . ? N5 C25 C24 120.4(3) . . ? N5 C25 C26 114.1(3) . . ? C24 C25 C26 125.6(3) . . ? N6 C26 C27 121.4(3) . . ? N6 C26 C25 114.8(3) . . ? C27 C26 C25 123.8(3) . . ? C26 C27 C28 118.8(3) . . ? C29 C28 C27 119.4(3) . . ? C30 C29 C28 118.6(3) . . ? N6 C30 C29 122.3(3) . . ? _diffrn_measured_fraction_theta_max 0.889 _diffrn_reflns_theta_full 28.14 _diffrn_measured_fraction_theta_full 0.889 _refine_diff_density_max 0.810 _refine_diff_density_min -0.854 _refine_diff_density_rms 0.124 #========================================END data_compound(3) _database_code_CSD 175196 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H8 N2 O9 P2 V Zn2' _chemical_formula_weight 567.82 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' 'V' 'V' 0.3005 0.5294 '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 7.9657(3) _cell_length_b 9.0824(4) _cell_length_c 11.8322(5) _cell_angle_alpha 81.4210(10) _cell_angle_beta 71.3010(10) _cell_angle_gamma 74.9980(10) _cell_volume 781.16(6) _cell_formula_units_Z 2 _cell_measurement_temperature 88(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.414 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 558 _exptl_absorpt_coefficient_mu 3.895 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 5337 _diffrn_reflns_av_R_equivalents 0.0165 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 28.31 _reflns_number_total 3633 _reflns_number_gt 3346 _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^)+(0.0539P)^2^+1.5137P] 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 3633 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0897 _refine_ls_wR_factor_gt 0.0878 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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 1.06229(4) 0.87913(4) 0.17356(3) 0.00771(10) Uani 1 1 d . . . Zn2 Zn 1.47959(4) 0.74885(4) -0.03138(3) 0.00750(10) Uani 1 1 d . . . V1 V 0.78120(7) 0.63377(6) 0.15032(5) 0.00881(12) Uani 1 1 d . . . P1 P 0.72428(10) 0.92340(8) 0.05259(7) 0.00705(15) Uani 1 1 d . . . P2 P 1.21530(10) 0.53933(8) 0.07373(7) 0.00670(15) Uani 1 1 d . . . O1 O 1.2523(3) 0.6995(2) 0.07608(19) 0.0084(4) Uani 1 1 d . . . O2 O 0.8598(3) 0.8339(2) 0.12397(19) 0.0089(4) Uani 1 1 d . . . O3 O 0.5945(3) 1.0594(2) 0.11663(19) 0.0092(4) Uani 1 1 d . . . O4 O 0.8211(3) 0.9624(2) -0.07598(19) 0.0120(4) Uani 1 1 d . . . O5 O 0.6263(3) 0.7899(2) 0.06316(19) 0.0089(4) Uani 1 1 d . . . O6 O 0.6559(3) 0.6106(3) 0.2844(2) 0.0150(5) Uani 1 1 d . . . O7 O 1.0246(3) 0.5345(2) 0.15776(19) 0.0099(4) Uani 1 1 d . . . O8 O 1.2253(3) 0.5223(2) -0.05611(19) 0.0101(4) Uani 1 1 d . . . O9 O 1.3560(3) 0.4172(2) 0.11852(19) 0.0091(4) Uani 1 1 d . . . N1 N 0.8663(3) 1.0406(3) 0.2917(2) 0.0100(5) Uani 1 1 d . . . N2 N 1.0793(3) 0.7715(3) 0.3389(2) 0.0100(5) Uani 1 1 d . . . C1 C 0.7653(4) 1.1749(4) 0.2654(3) 0.0120(6) Uani 1 1 d . . . H1 H 0.7921 1.2162 0.1866 0.014 Uiso 1 1 calc R . . C2 C 0.6197(4) 1.2561(4) 0.3522(3) 0.0148(6) Uani 1 1 d . . . H2 H 0.5488 1.3479 0.3305 0.018 Uiso 1 1 calc R . . C3 C 0.5827(4) 1.1993(4) 0.4695(3) 0.0154(6) Uani 1 1 d . . . H3 H 0.4860 1.2519 0.5278 0.018 Uiso 1 1 calc R . . C4 C 0.6924(4) 1.0600(4) 0.5013(3) 0.0120(6) Uani 1 1 d . . . C5 C 0.8302(4) 0.9843(3) 0.4082(3) 0.0106(6) Uani 1 1 d . . . C6 C 0.6712(4) 0.9951(4) 0.6220(3) 0.0157(6) Uani 1 1 d . . . H6 H 0.5793 1.0448 0.6843 0.019 Uiso 1 1 calc R . . C7 C 0.7832(4) 0.8624(4) 0.6464(3) 0.0150(6) Uani 1 1 d . . . H7 H 0.7673 0.8225 0.7253 0.018 Uiso 1 1 calc R . . C8 C 0.9255(4) 0.7826(4) 0.5526(3) 0.0125(6) Uani 1 1 d . . . C9 C 0.9483(4) 0.8411(3) 0.4327(3) 0.0099(6) Uani 1 1 d . . . C10 C 1.0497(5) 0.6463(4) 0.5736(3) 0.0150(6) Uani 1 1 d . . . H10 H 1.0402 0.6023 0.6510 0.018 Uiso 1 1 calc R . . C11 C 1.1846(5) 0.5801(4) 0.4776(3) 0.0160(6) Uani 1 1 d . . . H11 H 1.2693 0.4922 0.4901 0.019 Uiso 1 1 calc R . . C12 C 1.1947(4) 0.6447(4) 0.3614(3) 0.0142(6) Uani 1 1 d . . . H12 H 1.2855 0.5971 0.2977 0.017 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 0.00709(17) 0.00786(17) 0.00849(17) -0.00078(12) -0.00292(13) -0.00132(12) Zn2 0.00604(17) 0.00616(17) 0.01024(18) -0.00066(12) -0.00297(12) -0.00049(12) V1 0.0084(2) 0.0077(2) 0.0103(2) -0.00013(18) -0.00303(19) -0.00164(18) P1 0.0065(3) 0.0057(3) 0.0093(3) -0.0011(3) -0.0030(3) -0.0010(3) P2 0.0057(3) 0.0049(3) 0.0095(3) -0.0005(3) -0.0029(3) -0.0004(3) O1 0.0081(9) 0.0046(9) 0.0119(10) -0.0018(7) -0.0018(8) -0.0013(7) O2 0.0074(9) 0.0058(9) 0.0147(10) -0.0002(8) -0.0063(8) 0.0003(7) O3 0.0095(10) 0.0065(9) 0.0095(10) 0.0008(7) -0.0026(8) 0.0006(8) O4 0.0129(10) 0.0103(10) 0.0117(10) 0.0000(8) -0.0018(8) -0.0031(8) O5 0.0089(9) 0.0065(9) 0.0130(10) 0.0013(8) -0.0054(8) -0.0028(8) O6 0.0163(11) 0.0147(11) 0.0128(11) 0.0006(8) -0.0042(9) -0.0023(9) O7 0.0067(9) 0.0093(10) 0.0133(10) 0.0027(8) -0.0031(8) -0.0027(8) O8 0.0133(10) 0.0069(10) 0.0115(10) -0.0014(8) -0.0054(8) -0.0023(8) O9 0.0088(10) 0.0074(9) 0.0104(10) -0.0019(8) -0.0038(8) 0.0013(8) N1 0.0107(12) 0.0097(12) 0.0112(12) -0.0012(9) -0.0047(10) -0.0029(10) N2 0.0097(11) 0.0119(12) 0.0101(12) -0.0012(9) -0.0045(9) -0.0028(10) C1 0.0131(14) 0.0113(14) 0.0139(14) -0.0022(11) -0.0061(12) -0.0035(11) C2 0.0120(14) 0.0121(14) 0.0218(16) -0.0047(12) -0.0068(13) -0.0011(12) C3 0.0078(13) 0.0166(16) 0.0213(16) -0.0085(12) -0.0014(12) -0.0017(12) C4 0.0133(14) 0.0122(14) 0.0127(14) -0.0033(11) -0.0032(12) -0.0062(12) C5 0.0093(13) 0.0119(14) 0.0127(14) -0.0012(11) -0.0034(11) -0.0058(11) C6 0.0135(15) 0.0244(17) 0.0098(14) -0.0047(12) 0.0017(12) -0.0100(13) C7 0.0168(15) 0.0211(16) 0.0090(14) 0.0010(12) -0.0026(12) -0.0103(13) C8 0.0151(14) 0.0137(14) 0.0123(14) 0.0014(11) -0.0056(12) -0.0091(12) C9 0.0106(13) 0.0122(14) 0.0102(14) -0.0009(11) -0.0038(11) -0.0070(11) C10 0.0208(16) 0.0154(15) 0.0148(15) 0.0045(12) -0.0116(13) -0.0095(13) C11 0.0199(16) 0.0111(14) 0.0205(16) 0.0027(12) -0.0133(13) -0.0022(12) C12 0.0131(14) 0.0128(15) 0.0188(16) -0.0023(12) -0.0085(12) -0.0012(12) _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 O4 1.943(2) 2_775 ? Zn1 O2 2.034(2) . ? Zn1 N2 2.081(3) . ? Zn1 O1 2.108(2) . ? Zn1 N1 2.138(3) . ? Zn2 O9 1.905(2) 2_865 ? Zn2 O3 1.930(2) 2_775 ? Zn2 O1 1.967(2) . ? Zn2 O5 1.986(2) 1_655 ? V1 O6 1.598(2) . ? V1 O7 1.939(2) . ? V1 O8 1.950(2) 2_765 ? V1 O5 2.018(2) . ? V1 O2 2.022(2) . ? V1 P1 2.6970(9) . ? P1 O4 1.504(2) . ? P1 O3 1.511(2) . ? P1 O2 1.570(2) . ? P1 O5 1.573(2) . ? P2 O9 1.526(2) . ? P2 O7 1.533(2) . ? P2 O8 1.542(2) . ? P2 O1 1.563(2) . ? O3 Zn2 1.930(2) 2_775 ? O4 Zn1 1.943(2) 2_775 ? O5 Zn2 1.986(2) 1_455 ? O8 V1 1.950(2) 2_765 ? O9 Zn2 1.905(2) 2_865 ? N1 C1 1.331(4) . ? N1 C5 1.362(4) . ? N2 C12 1.326(4) . ? N2 C9 1.359(4) . ? C1 C2 1.401(4) . ? C2 C3 1.372(5) . ? C3 C4 1.415(5) . ? C4 C5 1.397(4) . ? C4 C6 1.436(4) . ? C5 C9 1.446(4) . ? C6 C7 1.356(5) . ? C7 C8 1.432(5) . ? C8 C9 1.410(4) . ? C8 C10 1.416(5) . ? C10 C11 1.376(5) . ? C11 C12 1.398(5) . ? 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 O4 Zn1 O2 116.20(9) 2_775 . ? O4 Zn1 N2 130.06(10) 2_775 . ? O2 Zn1 N2 112.84(9) . . ? O4 Zn1 O1 94.32(8) 2_775 . ? O2 Zn1 O1 90.65(8) . . ? N2 Zn1 O1 93.99(9) . . ? O4 Zn1 N1 91.93(9) 2_775 . ? O2 Zn1 N1 89.94(9) . . ? N2 Zn1 N1 79.09(10) . . ? O1 Zn1 N1 172.71(9) . . ? O9 Zn2 O3 119.47(9) 2_865 2_775 ? O9 Zn2 O1 114.21(9) 2_865 . ? O3 Zn2 O1 105.26(9) 2_775 . ? O9 Zn2 O5 101.29(9) 2_865 1_655 ? O3 Zn2 O5 105.95(9) 2_775 1_655 ? O1 Zn2 O5 110.19(9) . 1_655 ? O6 V1 O7 103.76(11) . . ? O6 V1 O8 109.11(11) . 2_765 ? O7 V1 O8 92.77(9) . 2_765 ? O6 V1 O5 106.81(10) . . ? O7 V1 O5 146.97(9) . . ? O8 V1 O5 88.89(9) 2_765 . ? O6 V1 O2 110.82(11) . . ? O7 V1 O2 87.03(9) . . ? O8 V1 O2 138.90(9) 2_765 . ? O5 V1 O2 70.71(8) . . ? O6 V1 P1 114.59(9) . . ? O7 V1 P1 118.15(7) . . ? O8 V1 P1 115.91(7) 2_765 . ? O5 V1 P1 35.42(6) . . ? O2 V1 P1 35.33(6) . . ? O4 P1 O3 113.58(12) . . ? O4 P1 O2 112.21(12) . . ? O3 P1 O2 111.54(12) . . ? O4 P1 O5 110.82(12) . . ? O3 P1 O5 111.34(12) . . ? O2 P1 O5 96.07(11) . . ? O4 P1 V1 121.21(9) . . ? O3 P1 V1 125.20(9) . . ? O2 P1 V1 48.13(8) . . ? O5 P1 V1 48.01(8) . . ? O9 P2 O7 109.27(12) . . ? O9 P2 O8 112.96(12) . . ? O7 P2 O8 110.32(12) . . ? O9 P2 O1 108.60(12) . . ? O7 P2 O1 108.56(12) . . ? O8 P2 O1 106.99(12) . . ? P2 O1 Zn2 118.94(12) . . ? P2 O1 Zn1 124.49(12) . . ? Zn2 O1 Zn1 116.23(10) . . ? P1 O2 V1 96.54(10) . . ? P1 O2 Zn1 136.03(13) . . ? V1 O2 Zn1 127.36(10) . . ? P1 O3 Zn2 121.97(13) . 2_775 ? P1 O4 Zn1 139.68(14) . 2_775 ? P1 O5 Zn2 132.09(13) . 1_455 ? P1 O5 V1 96.57(10) . . ? Zn2 O5 V1 126.89(10) 1_455 . ? P2 O7 V1 133.45(13) . . ? P2 O8 V1 138.40(13) . 2_765 ? P2 O9 Zn2 125.40(13) . 2_865 ? C1 N1 C5 118.3(3) . . ? C1 N1 Zn1 129.0(2) . . ? C5 N1 Zn1 112.2(2) . . ? C12 N2 C9 118.4(3) . . ? C12 N2 Zn1 128.3(2) . . ? C9 N2 Zn1 113.2(2) . . ? N1 C1 C2 122.3(3) . . ? C3 C2 C1 119.5(3) . . ? C2 C3 C4 119.6(3) . . ? C5 C4 C3 116.8(3) . . ? C5 C4 C6 119.2(3) . . ? C3 C4 C6 123.9(3) . . ? N1 C5 C4 123.4(3) . . ? N1 C5 C9 116.1(3) . . ? C4 C5 C9 120.5(3) . . ? C7 C6 C4 120.9(3) . . ? C6 C7 C8 121.0(3) . . ? C9 C8 C10 117.0(3) . . ? C9 C8 C7 119.8(3) . . ? C10 C8 C7 123.2(3) . . ? N2 C9 C8 123.2(3) . . ? N2 C9 C5 118.2(3) . . ? C8 C9 C5 118.6(3) . . ? C11 C10 C8 118.8(3) . . ? C10 C11 C12 120.2(3) . . ? N2 C12 C11 122.3(3) . . ? _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.935 _refine_diff_density_max 0.752 _refine_diff_density_min -1.045 _refine_diff_density_rms 0.139 #===============================================END