Supplementary Material for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'R.C. Finn' 'J. Sims' 'C. J. O'Connor' 'J. Zubieta' _publ_contact_author_name 'J. Zubieta' _publ_contact_author_address ; Center for Science and Technology 1-014 Syracuse University Syracuse, NY 13244, USA ; _publ_section_title ; Solid state chemistry of oxovanadates ; data_compound_1 _database_code_CSD 171061 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H24 Cu3 N6 O18 V6' _chemical_formula_weight 1252.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cu' 'Cu' 0.3201 1.2651 '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' 'O' 'O' 0.0106 0.0060 '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' '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.973(2) _cell_length_b 10.5682(13) _cell_length_c 19.633(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.565(2) _cell_angle_gamma 90.00 _cell_volume 3924.0(8) _cell_formula_units_Z 4 _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 2.121 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2460 _exptl_absorpt_coefficient_mu 3.038 _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 12467 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0685 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 28.29 _reflns_number_total 4704 _reflns_number_gt 3366 _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^)+(0.0412P)^2^+123.4356P] 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 4704 _refine_ls_number_parameters 286 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1016 _refine_ls_R_factor_gt 0.0689 _refine_ls_wR_factor_ref 0.1705 _refine_ls_wR_factor_gt 0.1600 _refine_ls_goodness_of_fit_ref 1.176 _refine_ls_restrained_S_all 1.176 _refine_ls_shift/su_max 1.446 _refine_ls_shift/su_mean 0.005 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 Cu1 Cu 0.04636(5) 0.05815(8) 0.06743(5) 0.0093(2) Uani 1 1 d . . . Cu2 Cu 0.0000 0.18667(12) 0.2500 0.0101(3) Uani 1 2 d S . . V3 V -0.03622(7) -0.19819(11) 0.10443(6) 0.0083(3) Uani 1 1 d . . . V4 V 0.10921(7) -0.05376(12) 0.26237(7) 0.0102(3) Uani 1 1 d . . . V5 V 0.13043(7) -0.19844(11) 0.11639(6) 0.0087(3) Uani 1 1 d . . . O1 O -0.0291(3) -0.0695(5) 0.0532(3) 0.0096(10) Uani 1 1 d . . . O2 O 0.1211(3) -0.0677(5) 0.0678(3) 0.0111(11) Uani 1 1 d . . . O3 O -0.0544(3) -0.1495(5) 0.1884(3) 0.0155(12) Uani 1 1 d . . . O4 O -0.0984(3) -0.2890(5) 0.0709(3) 0.0121(11) Uani 1 1 d . . . O5 O 0.0464(3) -0.2819(5) 0.1087(3) 0.0116(11) Uani 1 1 d . . . O6 O 0.1928(3) -0.2856(5) 0.0912(3) 0.0126(11) Uani 1 1 d . . . O7 O 0.1510(3) -0.1546(5) 0.2053(3) 0.0122(11) Uani 1 1 d . . . O8 O 0.0621(3) 0.0607(5) 0.2188(3) 0.0130(11) Uani 1 1 d . . . O9 O 0.1700(3) 0.0133(5) 0.3128(3) 0.0185(12) Uani 1 1 d . . . N1 N -0.0225(3) 0.1986(6) 0.0767(3) 0.0083(12) Uani 1 1 d . . . N2 N 0.1152(3) 0.1987(6) 0.0797(3) 0.0109(13) Uani 1 1 d . . . N3 N 0.0674(3) 0.3280(6) 0.2529(3) 0.0123(13) Uani 1 1 d . . . C1 C -0.0935(4) 0.1872(7) 0.0746(4) 0.0135(16) Uani 1 1 d . . . H1 H -0.1131 0.1065 0.0744 0.016 Uiso 1 1 calc R . . C2 C -0.1376(4) 0.2887(7) 0.0728(4) 0.0137(16) Uani 1 1 d . . . H2 H -0.1863 0.2777 0.0717 0.016 Uiso 1 1 calc R . . C3 C -0.1079(4) 0.4118(7) 0.0725(4) 0.0148(16) Uani 1 1 d . . . H3 H -0.1365 0.4834 0.0703 0.018 Uiso 1 1 calc R . . C4 C -0.0354(4) 0.4219(7) 0.0756(4) 0.0120(15) Uani 1 1 d . . . H4 H -0.0144 0.5014 0.0756 0.014 Uiso 1 1 calc R . . C5 C 0.0063(4) 0.3148(7) 0.0787(4) 0.0121(15) Uani 1 1 d . . . C7 C 0.1263(4) 0.4239(7) 0.0848(4) 0.0131(16) Uani 1 1 d . . . H7 H 0.1048 0.5029 0.0855 0.016 Uiso 1 1 calc R . . C8 C 0.1993(4) 0.4134(7) 0.0879(4) 0.0146(16) Uani 1 1 d . . . H8 H 0.2273 0.4856 0.0914 0.018 Uiso 1 1 calc R . . C9 C 0.2308(4) 0.2935(7) 0.0859(4) 0.0144(16) Uani 1 1 d . . . H9 H 0.2797 0.2837 0.0882 0.017 Uiso 1 1 calc R . . C10 C 0.1857(4) 0.1906(7) 0.0805(4) 0.0136(15) Uani 1 1 d . . . H10 H 0.2056 0.1106 0.0771 0.016 Uiso 1 1 calc R . . C11 C 0.0387(4) 0.4445(7) 0.2519(4) 0.0133(15) Uani 1 1 d . . . C12 C 0.0802(4) 0.5556(8) 0.2545(4) 0.0163(16) Uani 1 1 d . . . H12 H 0.0598 0.6357 0.2534 0.020 Uiso 1 1 calc R . . C13 C 0.1535(5) 0.5388(7) 0.2588(4) 0.0196(18) Uani 1 1 d . . . H13 H 0.1827 0.6096 0.2603 0.024 Uiso 1 1 calc R . . C14 C 0.1836(4) 0.4209(8) 0.2608(4) 0.0148(16) Uani 1 1 d . . . H14 H 0.2325 0.4111 0.2645 0.018 Uiso 1 1 calc R . . C15 C 0.1384(4) 0.3146(7) 0.2571(4) 0.0146(16) Uani 1 1 d . . . H15 H 0.1579 0.2338 0.2575 0.017 Uiso 1 1 calc R . . C6 C 0.0864(4) 0.3159(7) 0.0806(4) 0.012(2) Uani 1.00(3) 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 Cu1 0.0109(4) 0.0034(4) 0.0137(5) -0.0001(4) 0.0024(4) 0.0000(3) Cu2 0.0137(7) 0.0037(6) 0.0133(6) 0.000 0.0040(5) 0.000 V3 0.0113(6) 0.0038(5) 0.0102(6) -0.0005(5) 0.0029(5) -0.0007(5) V4 0.0126(6) 0.0056(5) 0.0126(6) 0.0000(5) 0.0029(5) 0.0016(5) V5 0.0102(6) 0.0047(5) 0.0116(6) -0.0006(5) 0.0029(5) 0.0004(5) O1 0.012(3) 0.005(2) 0.012(3) -0.001(2) 0.003(2) 0.001(2) O2 0.013(3) 0.003(2) 0.018(3) 0.000(2) 0.005(2) -0.001(2) O3 0.027(3) 0.009(2) 0.013(3) -0.002(2) 0.008(2) -0.002(2) O4 0.014(3) 0.006(2) 0.016(3) -0.002(2) 0.000(2) -0.003(2) O5 0.012(3) 0.004(2) 0.019(3) 0.002(2) 0.003(2) 0.000(2) O6 0.015(3) 0.008(2) 0.015(3) -0.002(2) 0.002(2) 0.002(2) O7 0.019(3) 0.005(2) 0.014(3) -0.002(2) 0.003(2) 0.000(2) O8 0.015(3) 0.007(2) 0.018(3) 0.004(2) 0.005(2) 0.005(2) O9 0.017(3) 0.017(3) 0.020(3) -0.003(2) -0.005(2) 0.004(2) N1 0.010(3) 0.007(3) 0.009(3) 0.001(2) 0.004(2) -0.001(2) N2 0.016(3) 0.008(3) 0.009(3) -0.002(2) 0.003(3) 0.002(3) N3 0.016(3) 0.010(3) 0.011(3) 0.000(2) 0.002(3) -0.002(2) C1 0.023(4) 0.007(3) 0.011(4) -0.002(3) 0.005(3) 0.002(3) C2 0.018(4) 0.008(3) 0.016(4) -0.002(3) 0.004(3) -0.003(3) C3 0.017(4) 0.009(4) 0.019(4) 0.000(3) 0.005(3) 0.001(3) C4 0.020(4) 0.008(3) 0.009(3) 0.001(3) 0.004(3) 0.000(3) C5 0.018(4) 0.014(4) 0.005(3) 0.000(3) 0.006(3) -0.005(3) C7 0.022(4) 0.005(3) 0.013(4) 0.004(3) 0.005(3) 0.003(3) C8 0.013(4) 0.008(3) 0.022(4) -0.004(3) 0.000(3) -0.006(3) C9 0.008(4) 0.008(3) 0.027(4) 0.002(3) 0.000(3) 0.007(3) C10 0.013(4) 0.010(3) 0.017(4) 0.002(3) 0.001(3) 0.004(3) C11 0.014(4) 0.015(4) 0.011(3) -0.002(3) 0.004(3) -0.010(3) C12 0.021(4) 0.012(4) 0.016(4) -0.001(3) 0.000(3) -0.001(3) C13 0.023(4) 0.009(4) 0.027(5) 0.003(3) 0.002(4) -0.007(3) C14 0.004(3) 0.019(4) 0.021(4) -0.006(3) -0.002(3) -0.006(3) C15 0.017(4) 0.009(3) 0.018(4) -0.002(3) 0.006(3) 0.002(3) C6 0.016(4) 0.008(4) 0.012(4) 0.004(3) 0.000(3) 0.009(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 Cu1 O2 1.943(5) . ? Cu1 O1 1.971(5) . ? Cu1 N2 1.980(7) . ? Cu1 N1 1.995(6) . ? Cu1 O1 2.368(5) 5 ? Cu2 O8 1.911(5) . ? Cu2 O8 1.911(5) 2 ? Cu2 N3 1.965(6) . ? Cu2 N3 1.965(6) 2 ? V3 O4 1.620(5) . ? V3 O1 1.703(5) . ? V3 O3 1.787(5) . ? V3 O5 1.796(5) . ? V4 O9 1.622(6) . ? V4 O8 1.694(5) . ? V4 O7 1.777(5) . ? V4 O3 1.788(6) 2 ? V5 O6 1.608(5) . ? V5 O2 1.681(5) . ? V5 O5 1.819(5) . ? V5 O7 1.819(5) . ? O1 Cu1 2.368(5) 5 ? O3 V4 1.788(6) 2 ? N1 C5 1.344(9) . ? N1 C1 1.349(10) . ? N2 C10 1.339(10) . ? N2 C6 1.355(9) . ? N3 C11 1.346(10) . ? N3 C15 1.350(10) . ? C1 C2 1.359(11) . ? C2 C3 1.417(10) . ? C3 C4 1.376(11) . ? C4 C5 1.379(11) . ? C5 C6 1.516(11) . ? C7 C6 1.368(11) . ? C7 C8 1.387(11) . ? C8 C9 1.403(10) . ? C9 C10 1.382(11) . ? C11 C12 1.412(11) . ? C11 C11 1.465(15) 2 ? C12 C13 1.399(12) . ? C13 C14 1.370(11) . ? C14 C15 1.411(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cu1 O1 93.0(2) . . ? O2 Cu1 N2 92.2(2) . . ? O1 Cu1 N2 174.6(2) . . ? O2 Cu1 N1 172.5(2) . . ? O1 Cu1 N1 92.8(2) . . ? N2 Cu1 N1 82.0(3) . . ? O2 Cu1 O1 94.7(2) . 5 ? O1 Cu1 O1 81.5(2) . 5 ? N2 Cu1 O1 96.9(2) . 5 ? N1 Cu1 O1 90.8(2) . 5 ? O8 Cu2 O8 91.7(3) . 2 ? O8 Cu2 N3 97.0(2) . . ? O8 Cu2 N3 159.6(2) 2 . ? O8 Cu2 N3 159.6(2) . 2 ? O8 Cu2 N3 97.0(2) 2 2 ? N3 Cu2 N3 81.0(4) . 2 ? O4 V3 O1 108.8(3) . . ? O4 V3 O3 111.0(3) . . ? O1 V3 O3 110.2(2) . . ? O4 V3 O5 109.4(3) . . ? O1 V3 O5 108.1(2) . . ? O3 V3 O5 109.3(3) . . ? O9 V4 O8 108.5(3) . . ? O9 V4 O7 108.3(3) . . ? O8 V4 O7 110.7(3) . . ? O9 V4 O3 109.5(3) . 2 ? O8 V4 O3 111.8(3) . 2 ? O7 V4 O3 108.0(2) . 2 ? O6 V5 O2 110.1(3) . . ? O6 V5 O5 111.0(3) . . ? O2 V5 O5 107.4(2) . . ? O6 V5 O7 109.6(3) . . ? O2 V5 O7 109.9(2) . . ? O5 V5 O7 108.8(2) . . ? V3 O1 Cu1 123.6(3) . . ? V3 O1 Cu1 128.3(3) . 5 ? Cu1 O1 Cu1 98.5(2) . 5 ? V5 O2 Cu1 127.5(3) . . ? V3 O3 V4 145.6(4) . 2 ? V3 O5 V5 121.4(3) . . ? V4 O7 V5 133.3(3) . . ? V4 O8 Cu2 130.5(3) . . ? C5 N1 C1 119.0(7) . . ? C5 N1 Cu1 114.5(5) . . ? C1 N1 Cu1 126.2(5) . . ? C10 N2 C6 117.6(7) . . ? C10 N2 Cu1 127.0(5) . . ? C6 N2 Cu1 115.1(5) . . ? C11 N3 C15 119.8(6) . . ? C11 N3 Cu2 115.7(5) . . ? C15 N3 Cu2 124.5(5) . . ? N1 C1 C2 122.8(7) . . ? C1 C2 C3 118.7(7) . . ? C4 C3 C2 117.9(7) . . ? C3 C4 C5 120.4(7) . . ? N1 C5 C4 121.2(7) . . ? N1 C5 C6 114.3(7) . . ? C4 C5 C6 124.4(7) . . ? C6 C7 C8 118.8(7) . . ? C7 C8 C9 119.8(7) . . ? C10 C9 C8 116.7(7) . . ? N2 C10 C9 124.2(7) . . ? N3 C11 C12 122.4(7) . . ? N3 C11 C11 113.8(4) . 2 ? C12 C11 C11 123.7(5) . 2 ? C13 C12 C11 116.4(7) . . ? C14 C13 C12 121.9(7) . . ? C13 C14 C15 118.2(7) . . ? N3 C15 C14 121.2(7) . . ? N2 C6 C7 122.8(7) . . ? N2 C6 C5 113.4(7) . . ? C7 C6 C5 123.8(7) . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 1.667 _refine_diff_density_min -0.997 _refine_diff_density_rms 0.219 #===END data_compound_2 _database_code_CSD 171062 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H11 Cu N3 O6 V2' _chemical_formula_weight 494.69 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' 'V' 'V' 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 9.3222(7) _cell_length_b 21.2995(16) _cell_length_c 8.3524(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.787(2) _cell_angle_gamma 90.00 _cell_volume 1656.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(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 1.984 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 980 _exptl_absorpt_coefficient_mu 2.418 _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 10992 _diffrn_reflns_av_R_equivalents 0.0615 _diffrn_reflns_av_sigmaI/netI 0.0846 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 28.29 _reflns_number_total 4001 _reflns_number_gt 2689 _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^)+(0.0507P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4001 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0858 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1088 _refine_ls_wR_factor_gt 0.0958 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 Cu1 Cu 0.02996(5) 0.37919(2) 0.60516(6) 0.00852(13) Uani 1 1 d . . . V2 V 0.28104(8) 0.32015(3) 0.33807(9) 0.00923(17) Uani 1 1 d . . . V3 V 0.24987(8) 0.17297(3) 0.42987(9) 0.00927(17) Uani 1 1 d . . . O1 O 0.0957(3) 0.33308(14) 0.8243(4) 0.0144(7) Uani 1 1 d . . . O2 O 0.1503(3) 0.33932(13) 0.4607(4) 0.0128(6) Uani 1 1 d . . . O3 O 0.2069(4) 0.32422(14) 0.1375(4) 0.0184(7) Uani 1 1 d . . . O4 O 0.4143(3) 0.36851(14) 0.3617(4) 0.0175(7) Uani 1 1 d . . . O5 O 0.3475(3) 0.24269(13) 0.3772(4) 0.0146(7) Uani 1 1 d . . . O6 O 0.3499(3) 0.11220(13) 0.3961(4) 0.0148(7) Uani 1 1 d . . . N1 N 0.1391(4) 0.46137(16) 0.6406(4) 0.0099(7) Uani 1 1 d . . . N2 N -0.1188(4) 0.42940(15) 0.6963(4) 0.0091(7) Uani 1 1 d . . . N3 N -0.1393(3) 0.31876(16) 0.5813(4) 0.0089(7) Uani 1 1 d . . . C1 C 0.2740(5) 0.4721(2) 0.6055(5) 0.0119(9) Uani 1 1 d . . . H1 H 0.3259 0.4407 0.5571 0.014 Uiso 1 1 calc R . . C2 C 0.3393(5) 0.5294(2) 0.6398(5) 0.0144(9) Uani 1 1 d . . . H2 H 0.4341 0.5363 0.6146 0.017 Uiso 1 1 calc R . . C3 C 0.2628(5) 0.5760(2) 0.7114(5) 0.0152(9) Uani 1 1 d . . . H3 H 0.3053 0.6148 0.7339 0.018 Uiso 1 1 calc R . . C4 C 0.1220(5) 0.56495(19) 0.7498(5) 0.0133(9) Uani 1 1 d . . . H4 H 0.0683 0.5958 0.7979 0.016 Uiso 1 1 calc R . . C5 C 0.0639(5) 0.50633(19) 0.7144(5) 0.0115(9) Uani 1 1 d . . . C6 C -0.0841(5) 0.4874(2) 0.7522(5) 0.0138(9) Uani 1 1 d . . . C7 C -0.1833(5) 0.5221(2) 0.8321(5) 0.0140(9) Uani 1 1 d . . . H7 H -0.1608 0.5621 0.8701 0.017 Uiso 1 1 calc R . . C8 C -0.3179(5) 0.4960(2) 0.8548(5) 0.0183(10) Uani 1 1 d . . . H8 H -0.3857 0.5185 0.9094 0.022 Uiso 1 1 calc R . . C9 C -0.3513(5) 0.4361(2) 0.7957(5) 0.0153(10) Uani 1 1 d . . . H9 H -0.4412 0.4186 0.8091 0.018 Uiso 1 1 calc R . . C10 C -0.2479(5) 0.40367(19) 0.7169(5) 0.0111(9) Uani 1 1 d . . . C11 C -0.2600(4) 0.33924(19) 0.6503(5) 0.0104(9) Uani 1 1 d . . . C12 C -0.3777(5) 0.3004(2) 0.6641(5) 0.0122(9) Uani 1 1 d . . . H12 H -0.4603 0.3153 0.7093 0.015 Uiso 1 1 calc R . . C13 C -0.3711(5) 0.2390(2) 0.6097(5) 0.0181(10) Uani 1 1 d . . . H13 H -0.4485 0.2119 0.6191 0.022 Uiso 1 1 calc R . . C14 C -0.2463(5) 0.2188(2) 0.5408(5) 0.0153(10) Uani 1 1 d . . . H14 H -0.2397 0.1778 0.5030 0.018 Uiso 1 1 calc R . . C15 C -0.1319(5) 0.25980(19) 0.5287(5) 0.0120(9) Uani 1 1 d . . . H15 H -0.0485 0.2460 0.4831 0.014 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 Cu1 0.0100(3) 0.0050(2) 0.0108(3) -0.0008(2) 0.00279(19) -0.0005(2) V2 0.0120(4) 0.0054(3) 0.0106(4) 0.0000(3) 0.0039(3) -0.0004(3) V3 0.0124(4) 0.0052(3) 0.0102(4) 0.0000(3) 0.0010(3) 0.0006(3) O1 0.0147(16) 0.0121(16) 0.0163(16) 0.0032(13) 0.0006(13) -0.0003(12) O2 0.0111(15) 0.0111(15) 0.0166(16) -0.0042(13) 0.0056(13) 0.0022(12) O3 0.0323(19) 0.0119(16) 0.0110(16) 0.0013(13) 0.0009(14) 0.0005(14) O4 0.0140(16) 0.0115(16) 0.0274(19) -0.0019(14) 0.0048(14) -0.0043(13) O5 0.0137(15) 0.0097(15) 0.0206(17) -0.0006(13) 0.0032(13) 0.0010(12) O6 0.0169(16) 0.0074(15) 0.0201(17) 0.0015(13) 0.0019(13) 0.0032(12) N1 0.0148(19) 0.0073(17) 0.0076(17) 0.0024(14) 0.0013(15) 0.0009(14) N2 0.0112(18) 0.0051(17) 0.0113(18) 0.0016(14) 0.0029(15) 0.0009(14) N3 0.0063(17) 0.0103(18) 0.0099(18) 0.0015(14) -0.0016(14) -0.0005(14) C1 0.019(2) 0.009(2) 0.008(2) 0.0036(16) 0.0014(18) 0.0025(18) C2 0.016(2) 0.013(2) 0.014(2) 0.0029(18) -0.0028(18) -0.0013(18) C3 0.022(2) 0.006(2) 0.018(2) -0.0018(18) -0.0004(19) -0.0016(18) C4 0.022(2) 0.005(2) 0.013(2) -0.0013(17) 0.0038(19) 0.0035(18) C5 0.017(2) 0.008(2) 0.010(2) 0.0030(16) 0.0001(18) 0.0033(17) C6 0.022(2) 0.011(2) 0.008(2) 0.0011(18) 0.0027(18) 0.0023(18) C7 0.021(2) 0.007(2) 0.014(2) 0.0003(18) 0.0022(19) 0.0038(18) C8 0.021(2) 0.018(2) 0.016(2) -0.0007(19) 0.006(2) 0.0098(19) C9 0.016(2) 0.013(2) 0.017(2) 0.0033(19) 0.0065(19) 0.0020(18) C10 0.013(2) 0.010(2) 0.009(2) 0.0030(17) 0.0002(17) 0.0036(17) C11 0.013(2) 0.009(2) 0.010(2) 0.0015(17) 0.0034(17) 0.0007(16) C12 0.012(2) 0.013(2) 0.011(2) 0.0036(17) 0.0002(17) -0.0007(17) C13 0.016(2) 0.020(3) 0.018(2) 0.004(2) -0.0032(19) -0.0092(19) C14 0.022(2) 0.011(2) 0.012(2) -0.0023(18) -0.0025(19) -0.0050(19) C15 0.014(2) 0.011(2) 0.010(2) -0.0004(17) -0.0001(17) -0.0018(17) _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 Cu1 O2 1.889(3) . ? Cu1 N2 1.937(3) . ? Cu1 N3 2.038(3) . ? Cu1 N1 2.039(3) . ? Cu1 O1 2.140(3) . ? V2 O4 1.619(3) . ? V2 O2 1.680(3) . ? V2 O3 1.783(3) . ? V2 O5 1.787(3) . ? V3 O6 1.628(3) . ? V3 O1 1.654(3) 4_565 ? V3 O3 1.800(3) 4_566 ? V3 O5 1.807(3) . ? O1 V3 1.654(3) 4_566 ? O3 V3 1.800(3) 4_565 ? N1 C1 1.326(5) . ? N1 C5 1.353(5) . ? N2 C10 1.340(5) . ? N2 C6 1.355(5) . ? N3 C15 1.333(5) . ? N3 C11 1.361(5) . ? C1 C2 1.387(6) . ? C2 C3 1.376(6) . ? C3 C4 1.386(6) . ? C4 C5 1.387(6) . ? C5 C6 1.486(6) . ? C6 C7 1.380(6) . ? C7 C8 1.393(6) . ? C8 C9 1.397(6) . ? C9 C10 1.379(6) . ? C10 C11 1.483(6) . ? C11 C12 1.383(6) . ? C12 C13 1.387(6) . ? C13 C14 1.391(6) . ? C14 C15 1.387(6) . ? 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 Cu1 N2 163.44(14) . . ? O2 Cu1 N3 97.73(13) . . ? N2 Cu1 N3 79.71(14) . . ? O2 Cu1 N1 99.85(13) . . ? N2 Cu1 N1 80.25(14) . . ? N3 Cu1 N1 159.16(14) . . ? O2 Cu1 O1 100.71(12) . . ? N2 Cu1 O1 95.62(13) . . ? N3 Cu1 O1 88.98(12) . . ? N1 Cu1 O1 98.62(12) . . ? O4 V2 O2 110.26(15) . . ? O4 V2 O3 110.11(16) . . ? O2 V2 O3 107.55(15) . . ? O4 V2 O5 107.95(15) . . ? O2 V2 O5 111.60(14) . . ? O3 V2 O5 109.38(14) . . ? O6 V3 O1 109.63(15) . 4_565 ? O6 V3 O3 110.45(15) . 4_566 ? O1 V3 O3 106.75(15) 4_565 4_566 ? O6 V3 O5 108.17(14) . . ? O1 V3 O5 111.65(14) 4_565 . ? O3 V3 O5 110.21(14) 4_566 . ? V3 O1 Cu1 134.17(17) 4_566 . ? V2 O2 Cu1 165.87(18) . . ? V2 O3 V3 144.4(2) . 4_565 ? V2 O5 V3 128.99(17) . . ? C1 N1 C5 119.8(4) . . ? C1 N1 Cu1 126.0(3) . . ? C5 N1 Cu1 114.1(3) . . ? C10 N2 C6 122.0(4) . . ? C10 N2 Cu1 119.3(3) . . ? C6 N2 Cu1 118.4(3) . . ? C15 N3 C11 119.9(4) . . ? C15 N3 Cu1 125.1(3) . . ? C11 N3 Cu1 114.1(3) . . ? N1 C1 C2 121.2(4) . . ? C3 C2 C1 119.6(4) . . ? C2 C3 C4 119.6(4) . . ? C3 C4 C5 117.9(4) . . ? N1 C5 C4 121.9(4) . . ? N1 C5 C6 114.3(4) . . ? C4 C5 C6 123.7(4) . . ? N2 C6 C7 120.0(4) . . ? N2 C6 C5 112.5(4) . . ? C7 C6 C5 127.5(4) . . ? C6 C7 C8 118.8(4) . . ? C7 C8 C9 120.1(4) . . ? C10 C9 C8 118.6(4) . . ? N2 C10 C9 120.6(4) . . ? N2 C10 C11 112.5(4) . . ? C9 C10 C11 126.9(4) . . ? N3 C11 C12 121.3(4) . . ? N3 C11 C10 113.9(4) . . ? C12 C11 C10 124.7(4) . . ? C11 C12 C13 119.3(4) . . ? C12 C13 C14 118.6(4) . . ? C15 C14 C13 119.8(4) . . ? N3 C15 C14 121.1(4) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.048 _refine_diff_density_min -0.814 _refine_diff_density_rms 0.147 #===END