Supplementary Material (ESI) 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 'Gao, Song' 'Hu, Huai-Ming' 'Jin, Xiang-Lin' 'Kou, Hui-Zhong' 'Liu, Cai-Ming' _publ_contact_author_name 'Prof Song Gao' _publ_contact_author_address ; State Key Laboratory of Rare Earth Materials Chemistry & Applications Peking University Beijing 100871 CHINA ; _publ_contact_author_email 'GAOSONG@PKU.EDU.CN' _publ_section_title ; Hydrothermal syntheses and crystal structures of two-dimensional (2D) layered vanadium oxide complexes: M(bipy)(H20)V206 (M = Ni, Co) and [Ni(bipy)2V6O17] ; data_compound_1 _database_code_CSD 173604 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H10 N2 Ni O7 V2' _chemical_formula_weight 430.79 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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Orthorhombic' _symmetry_space_group_name_H-M 'Pca2(1)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 9.171(2) _cell_length_b 10.514(2) _cell_length_c 14.339(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1382.6(5) _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 'block' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.070 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 2.707 _exptl_absorpt_correction_type 'ABSCOR by T. Higashi' _exptl_absorpt_correction_T_min 0.6211 _exptl_absorpt_correction_T_max 1.2394 _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 'Rigaku RAXIS RAPID IP' _diffrn_measurement_method 'Dscillation' _diffrn_detector_area_resol_mean '100x100 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1646 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0345 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1646 _reflns_number_gt 1580 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; Molecular Structure Corporation(1994) MSC/AFC Diffractometer Control Software MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA ; _computing_cell_refinement ; Molecular Structure Corpration(1994) MSC/AFC Diffractometer Control Software MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA ; _computing_data_reduction 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Interactive Molecular Graphics XP, Version 4.2 for MSDOS (1990), Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. ; _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0146P)^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 97 _refine_ls_extinction_coef 0.0132(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(2) _refine_ls_number_reflns 1646 _refine_ls_number_parameters 204 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0185 _refine_ls_R_factor_gt 0.0171 _refine_ls_wR_factor_ref 0.0372 _refine_ls_wR_factor_gt 0.0369 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.006 _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 Ni1 Ni 0.06115(3) 0.36318(3) 0.56201(3) 0.01387(9) Uani 1 1 d . . . V1 V -0.11376(5) 0.33361(4) 0.78897(4) 0.01359(10) Uani 1 1 d . . . V2 V -0.32815(4) 0.53187(4) 0.90765(3) 0.01273(10) Uani 1 1 d . . . N1 N 0.2196(2) 0.2607(2) 0.63379(18) 0.0184(5) Uani 1 1 d . . . N2 N 0.0030(2) 0.1813(2) 0.52721(18) 0.0184(5) Uani 1 1 d . . . O1 O -0.0615(2) 0.3647(2) 0.68256(18) 0.0282(5) Uani 1 1 d . . . O2 O -0.1591(2) 0.18660(18) 0.7999(2) 0.0346(6) Uani 1 1 d . . . O3 O 0.0302(2) 0.36470(19) 0.87145(18) 0.0242(5) Uani 1 1 d . . . O4 O -0.27321(19) 0.43231(18) 0.81369(17) 0.0229(4) Uani 1 1 d . . . O5 O -0.3857(2) 0.4420(2) 0.99627(16) 0.0214(5) Uani 1 1 d . . . O6 O -0.1875(2) 0.61538(19) 0.94629(17) 0.0208(4) Uani 1 1 d . . . O1W O 0.1344(2) 0.5416(2) 0.60994(17) 0.0241(5) Uani 1 1 d . . . H1WA H 0.2097 0.5610 0.5826 0.036 Uiso 1 1 calc R . . C1 C 0.3276(3) 0.3069(3) 0.6859(3) 0.0253(7) Uani 1 1 d . . . H1A H 0.3473 0.3935 0.6831 0.030 Uiso 1 1 calc R . . C2 C 0.4114(4) 0.2322(3) 0.7439(3) 0.0331(8) Uani 1 1 d . . . H2B H 0.4868 0.2672 0.7789 0.040 Uiso 1 1 calc R . . C3 C 0.3804(3) 0.1038(4) 0.7486(3) 0.0351(8) Uani 1 1 d . . . H3B H 0.4326 0.0510 0.7885 0.042 Uiso 1 1 calc R . . C4 C 0.2709(3) 0.0550(3) 0.6933(3) 0.0318(7) Uani 1 1 d . . . H4A H 0.2495 -0.0314 0.6953 0.038 Uiso 1 1 calc R . . C5 C 0.1939(3) 0.1332(3) 0.6356(2) 0.0208(6) Uani 1 1 d . . . C6 C 0.0811(3) 0.0885(3) 0.5692(3) 0.0206(6) Uani 1 1 d . . . C7 C 0.0607(3) -0.0382(3) 0.5466(3) 0.0300(9) Uani 1 1 d . . . H7A H 0.1155 -0.1009 0.5761 0.036 Uiso 1 1 calc R . . C8 C -0.0419(3) -0.0712(3) 0.4798(3) 0.0337(8) Uani 1 1 d . . . H8A H -0.0564 -0.1558 0.4634 0.040 Uiso 1 1 calc R . . C9 C -0.1213(3) 0.0233(3) 0.4384(3) 0.0322(8) Uani 1 1 d . . . H9A H -0.1914 0.0033 0.3939 0.039 Uiso 1 1 calc R . . C10 C -0.0970(3) 0.1487(3) 0.4630(2) 0.0253(7) Uani 1 1 d . . . H10A H -0.1514 0.2122 0.4343 0.030 Uiso 1 1 calc R . . H1WB H 0.142(3) 0.552(3) 0.674(3) 0.027(10) Uiso 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 Ni1 0.01312(14) 0.01631(16) 0.01217(16) 0.00122(18) 0.00070(15) 0.00071(12) V1 0.01485(19) 0.01479(19) 0.0111(2) -0.0009(2) 0.00056(18) -0.00115(17) V2 0.01201(18) 0.0153(2) 0.0108(2) -0.00023(19) -0.00065(19) -0.00037(17) N1 0.0192(11) 0.0176(10) 0.0184(12) 0.0009(11) 0.0006(10) 0.0002(9) N2 0.0193(10) 0.0201(11) 0.0159(11) 0.0003(11) 0.0017(10) -0.0024(10) O1 0.0245(11) 0.0444(14) 0.0157(11) 0.0039(11) 0.0056(10) 0.0074(10) O2 0.0445(12) 0.0179(10) 0.0413(15) -0.0027(12) -0.0071(13) -0.0090(9) O3 0.0226(10) 0.0241(11) 0.0259(12) 0.0010(10) -0.0081(9) -0.0048(8) O4 0.0189(9) 0.0302(9) 0.0195(10) -0.0096(10) -0.0005(9) 0.0038(9) O5 0.0186(9) 0.0263(11) 0.0192(11) 0.0029(9) 0.0032(9) -0.0041(8) O6 0.0204(9) 0.0246(10) 0.0176(10) 0.0009(9) -0.0031(9) -0.0035(8) O1W 0.0218(10) 0.0254(11) 0.0251(13) -0.0034(10) 0.0028(9) -0.0031(9) C1 0.0248(14) 0.0262(15) 0.0249(16) -0.0024(15) -0.0044(14) 0.0005(12) C2 0.0274(15) 0.0422(19) 0.0296(19) -0.0008(17) -0.0107(15) -0.0002(14) C3 0.0321(16) 0.0399(18) 0.033(2) 0.0159(18) -0.0073(16) 0.0087(16) C4 0.0307(16) 0.0287(14) 0.0361(19) 0.0122(16) -0.0012(16) 0.0023(14) C5 0.0186(12) 0.0222(14) 0.0214(15) 0.0051(13) 0.0016(13) 0.0002(10) C6 0.0190(12) 0.0200(12) 0.0226(15) 0.0038(17) 0.0048(14) -0.0002(10) C7 0.0285(14) 0.0232(15) 0.038(2) -0.0001(15) 0.0075(15) 0.0020(12) C8 0.0380(18) 0.0268(17) 0.036(2) -0.0102(16) 0.0106(15) -0.0100(15) C9 0.0285(17) 0.0414(19) 0.0268(18) -0.0110(17) -0.0003(14) -0.0127(15) C10 0.0231(14) 0.0311(16) 0.0217(17) -0.0011(14) -0.0035(13) -0.0022(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 Ni1 O6 2.036(2) 2_564 ? Ni1 O5 2.041(2) 4_454 ? Ni1 N2 2.047(2) . ? Ni1 O1 2.062(2) . ? Ni1 N1 2.081(2) . ? Ni1 O1W 2.108(2) . ? V1 O2 1.608(2) . ? V1 O1 1.632(3) . ? V1 O3 1.802(2) . ? V1 O4 1.8279(19) . ? V2 O6 1.6560(19) . ? V2 O5 1.669(2) . ? V2 O3 1.772(2) 3_465 ? V2 O4 1.779(2) . ? N1 C1 1.333(4) . ? N1 C5 1.361(3) . ? N2 C10 1.344(4) . ? N2 C6 1.352(4) . ? O3 V2 1.772(2) 3_565 ? O5 Ni1 2.041(2) 4_455 ? O6 Ni1 2.036(2) 2_565 ? C1 C2 1.378(5) . ? C2 C3 1.381(5) . ? C3 C4 1.378(5) . ? C4 C5 1.364(4) . ? C5 C6 1.482(5) . ? C6 C7 1.384(4) . ? C7 C8 1.388(5) . ? C8 C9 1.367(5) . ? C9 C10 1.383(4) . ? 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 O6 Ni1 O5 91.55(9) 2_564 4_454 ? O6 Ni1 N2 93.04(9) 2_564 . ? O5 Ni1 N2 93.52(9) 4_454 . ? O6 Ni1 O1 172.96(9) 2_564 . ? O5 Ni1 O1 87.37(9) 4_454 . ? N2 Ni1 O1 93.97(9) . . ? O6 Ni1 N1 93.61(9) 2_564 . ? O5 Ni1 N1 171.57(9) 4_454 . ? N2 Ni1 N1 79.56(9) . . ? O1 Ni1 N1 88.30(9) . . ? O6 Ni1 O1W 89.19(9) 2_564 . ? O5 Ni1 O1W 92.30(9) 4_454 . ? N2 Ni1 O1W 173.71(10) . . ? O1 Ni1 O1W 83.90(9) . . ? N1 Ni1 O1W 94.43(9) . . ? O2 V1 O1 111.06(14) . . ? O2 V1 O3 107.42(12) . . ? O1 V1 O3 111.24(11) . . ? O2 V1 O4 108.67(10) . . ? O1 V1 O4 107.62(11) . . ? O3 V1 O4 110.83(10) . . ? O6 V2 O5 106.97(11) . . ? O6 V2 O3 110.11(10) . 3_465 ? O5 V2 O3 109.77(11) . 3_465 ? O6 V2 O4 110.16(10) . . ? O5 V2 O4 109.46(10) . . ? O3 V2 O4 110.30(11) 3_465 . ? C1 N1 C5 118.5(3) . . ? C1 N1 Ni1 127.42(19) . . ? C5 N1 Ni1 113.47(19) . . ? C10 N2 C6 118.9(3) . . ? C10 N2 Ni1 125.7(2) . . ? C6 N2 Ni1 115.3(2) . . ? V1 O1 Ni1 160.40(13) . . ? V2 O3 V1 147.20(14) 3_565 . ? V2 O4 V1 135.03(13) . . ? V2 O5 Ni1 146.21(13) . 4_455 ? V2 O6 Ni1 140.77(13) . 2_565 ? N1 C1 C2 123.1(3) . . ? C1 C2 C3 118.1(3) . . ? C4 C3 C2 119.1(3) . . ? C5 C4 C3 120.1(3) . . ? N1 C5 C4 121.1(3) . . ? N1 C5 C6 114.9(3) . . ? C4 C5 C6 124.0(3) . . ? N2 C6 C7 121.2(3) . . ? N2 C6 C5 115.3(2) . . ? C7 C6 C5 123.4(3) . . ? C6 C7 C8 119.6(3) . . ? C9 C8 C7 118.6(3) . . ? C8 C9 C10 119.8(3) . . ? N2 C10 C9 121.9(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.380 _refine_diff_density_min -0.311 _refine_diff_density_rms 0.060 data_compound_2 _database_code_CSD 173605 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H32 N8 Ni2 O17 V6' _chemical_formula_weight 1319.80 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' 'Ni' 'Ni' 0.3393 1.1124 '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 15.503(3) _cell_length_b 14.748(3) _cell_length_c 10.467(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.01(3) _cell_angle_gamma 90.00 _cell_volume 2391.7(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.833 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1316 _exptl_absorpt_coefficient_mu 1.968 _exptl_absorpt_correction_type 'ABSCOR by T. Higashi' _exptl_absorpt_correction_T_min 0.8812 _exptl_absorpt_correction_T_max 1.1705 _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 Rigaku RAXIS RAPID IP _diffrn_measurement_method Dscillation _diffrn_detector_area_resol_mean '100x100 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5473 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0435 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5473 _reflns_number_gt 3859 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; Molecular Structure Corporation(1994) MSC/AFC Diffractometer Control Software MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA ; _computing_cell_refinement ; Molecular Structure Corporation(1994) MSC/AFC Diffractometer Control Software MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA ; _computing_data_reduction ; Molecular Structure Corporation(1994) MSC/AFC Diffractometer Control Software MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Interactive Molecular Graphics XP, Virsion 4.2 for MSDOS (1990), Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. ; _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0350P)^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 5473 _refine_ls_number_parameters 331 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0276 _refine_ls_wR_factor_ref 0.0692 _refine_ls_wR_factor_gt 0.0613 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 Ni1 Ni 0.233168(17) 0.020928(19) 0.70081(3) 0.02456(8) Uani 1 1 d . . . V1 V 0.31298(2) -0.19855(3) 0.81429(3) 0.02293(9) Uani 1 1 d . . . V2 V 0.25046(2) -0.14324(3) 1.10418(3) 0.02698(10) Uani 1 1 d . . . V3 V 0.08534(2) -0.05783(3) 0.92480(4) 0.02545(10) Uani 1 1 d . . . N1 N 0.15101(11) -0.03180(13) 0.56144(18) 0.0272(4) Uani 1 1 d . . . N2 N 0.17767(12) 0.13840(13) 0.62506(19) 0.0311(4) Uani 1 1 d . . . N3 N 0.33473(12) 0.03804(14) 0.57154(18) 0.0320(5) Uani 1 1 d . . . N4 N 0.32605(12) 0.08354(13) 0.81563(18) 0.0299(4) Uani 1 1 d . . . O1 O 0.41313(10) -0.21090(13) 0.78375(17) 0.0428(5) Uani 1 1 d . . . O2 O 0.27749(11) -0.10231(12) 0.75782(17) 0.0426(4) Uani 1 1 d . . . O3 O 0.24997(12) -0.28954(12) 0.74155(16) 0.0417(4) Uani 1 1 d . . . O4 O 0.30480(12) -0.20035(15) 0.98611(16) 0.0498(5) Uani 1 1 d . . . O5 O 0.29799(19) -0.05121(16) 1.1371(2) 0.0847(9) Uani 1 1 d . . . O6 O 0.14598(12) -0.12104(15) 1.04692(18) 0.0561(6) Uani 1 1 d . . . O7 O 0.14681(10) 0.01425(11) 0.84842(16) 0.0343(4) Uani 1 1 d . . . O8 O 0.04686(13) -0.13070(13) 0.82338(19) 0.0506(5) Uani 1 1 d . . . O9 O 0.0000 0.0000 1.0000 0.0551(8) Uani 1 2 d S . . C1 C 0.14092(14) -0.12001(17) 0.5353(2) 0.0335(6) Uani 1 1 d . . . H1B H 0.1634 -0.1623 0.5934 0.040 Uiso 1 1 calc R . . C2 C 0.09830(15) -0.15079(19) 0.4254(2) 0.0389(6) Uani 1 1 d . . . H2A H 0.0921 -0.2126 0.4098 0.047 Uiso 1 1 calc R . . C3 C 0.06556(16) -0.0886(2) 0.3402(2) 0.0454(7) Uani 1 1 d . . . H3B H 0.0378 -0.1075 0.2647 0.054 Uiso 1 1 calc R . . C4 C 0.07402(16) 0.0027(2) 0.3671(2) 0.0416(6) Uani 1 1 d . . . H4A H 0.0509 0.0457 0.3107 0.050 Uiso 1 1 calc R . . C5 C 0.11702(14) 0.02954(17) 0.4785(2) 0.0303(5) Uani 1 1 d . . . C6 C 0.12879(14) 0.12512(16) 0.5167(2) 0.0312(5) Uani 1 1 d . . . C7 C 0.09231(17) 0.19717(19) 0.4497(3) 0.0439(7) Uani 1 1 d . . . H7A H 0.0594 0.1871 0.3750 0.053 Uiso 1 1 calc R . . C8 C 0.1053(2) 0.2841(2) 0.4950(3) 0.0532(8) Uani 1 1 d . . . H8B H 0.0816 0.3333 0.4509 0.064 Uiso 1 1 calc R . . C9 C 0.1536(2) 0.29702(19) 0.6056(3) 0.0535(8) Uani 1 1 d . . . H9B H 0.1625 0.3551 0.6382 0.064 Uiso 1 1 calc R . . C10 C 0.18866(17) 0.22280(17) 0.6675(3) 0.0415(6) Uani 1 1 d . . . H10A H 0.2215 0.2320 0.7424 0.050 Uiso 1 1 calc R . . C11 C 0.33426(16) 0.0173(2) 0.4475(2) 0.0403(6) Uani 1 1 d . . . H11A H 0.2900 -0.0192 0.4142 0.048 Uiso 1 1 calc R . . C12 C 0.39618(18) 0.0473(2) 0.3666(3) 0.0521(8) Uani 1 1 d . . . H12A H 0.3936 0.0314 0.2805 0.063 Uiso 1 1 calc R . . C13 C 0.46202(19) 0.1012(2) 0.4150(3) 0.0550(8) Uani 1 1 d . . . H13A H 0.5040 0.1235 0.3620 0.066 Uiso 1 1 calc R . . C14 C 0.46452(17) 0.1214(2) 0.5432(3) 0.0487(7) Uani 1 1 d . . . H14A H 0.5085 0.1575 0.5782 0.058 Uiso 1 1 calc R . . C15 C 0.40097(15) 0.08740(17) 0.6200(2) 0.0346(5) Uani 1 1 d . . . C16 C 0.40069(15) 0.10330(17) 0.7594(2) 0.0338(5) Uani 1 1 d . . . C17 C 0.47261(17) 0.1328(2) 0.8292(3) 0.0507(7) Uani 1 1 d . . . H17A H 0.5244 0.1433 0.7894 0.061 Uiso 1 1 calc R . . C18 C 0.4662(2) 0.1466(2) 0.9589(3) 0.0598(9) Uani 1 1 d . . . H18A H 0.5133 0.1678 1.0075 0.072 Uiso 1 1 calc R . . C19 C 0.3898(2) 0.1286(2) 1.0152(3) 0.0539(8) Uani 1 1 d . . . H19A H 0.3841 0.1380 1.1024 0.065 Uiso 1 1 calc R . . C20 C 0.32136(18) 0.09656(19) 0.9411(2) 0.0405(6) Uani 1 1 d . . . H20A H 0.2698 0.0834 0.9801 0.049 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 Ni1 0.02359(14) 0.02385(16) 0.02618(15) 0.00105(13) 0.00016(11) -0.00181(12) V1 0.02266(17) 0.0263(2) 0.01975(18) -0.00314(16) -0.00041(13) 0.00303(15) V2 0.0338(2) 0.0269(2) 0.02004(19) -0.00003(17) -0.00210(15) -0.00052(17) V3 0.01934(17) 0.0258(2) 0.0314(2) 0.00632(17) 0.00318(14) 0.00495(15) N1 0.0231(9) 0.0278(11) 0.0305(10) 0.0024(9) -0.0019(7) -0.0003(8) N2 0.0339(10) 0.0263(11) 0.0337(11) 0.0031(9) 0.0079(8) 0.0012(9) N3 0.0284(9) 0.0380(12) 0.0298(10) -0.0003(9) 0.0031(8) -0.0036(9) N4 0.0317(10) 0.0285(11) 0.0295(10) 0.0014(9) -0.0005(8) -0.0051(8) O1 0.0280(8) 0.0589(13) 0.0419(10) -0.0033(9) 0.0061(7) 0.0044(8) O2 0.0540(11) 0.0308(10) 0.0417(10) 0.0000(8) -0.0161(8) 0.0083(9) O3 0.0503(10) 0.0444(11) 0.0309(9) -0.0100(8) 0.0069(8) -0.0199(9) O4 0.0534(11) 0.0749(14) 0.0212(9) -0.0043(9) 0.0020(8) 0.0176(11) O5 0.140(2) 0.0523(14) 0.0598(14) 0.0014(12) -0.0232(15) -0.0487(16) O6 0.0421(10) 0.0812(16) 0.0451(11) 0.0270(11) 0.0042(9) 0.0247(11) O7 0.0330(8) 0.0361(10) 0.0345(9) 0.0030(8) 0.0088(7) -0.0035(7) O8 0.0588(11) 0.0363(11) 0.0560(12) 0.0017(10) -0.0093(10) -0.0105(9) O9 0.0379(14) 0.0516(17) 0.078(2) 0.0173(16) 0.0277(14) 0.0207(13) C1 0.0283(11) 0.0314(14) 0.0403(14) 0.0016(11) -0.0035(10) 0.0000(10) C2 0.0341(12) 0.0404(15) 0.0423(15) -0.0112(13) 0.0014(11) -0.0049(11) C3 0.0400(14) 0.063(2) 0.0322(14) -0.0088(14) -0.0045(11) -0.0042(13) C4 0.0377(14) 0.0542(18) 0.0324(13) 0.0091(13) -0.0041(11) 0.0015(12) C5 0.0248(10) 0.0366(14) 0.0296(12) 0.0075(11) 0.0029(9) 0.0010(10) C6 0.0268(11) 0.0328(13) 0.0344(13) 0.0107(11) 0.0086(9) 0.0024(10) C7 0.0414(14) 0.0422(16) 0.0483(16) 0.0180(13) 0.0048(12) 0.0091(12) C8 0.0601(18) 0.0410(18) 0.060(2) 0.0191(15) 0.0181(15) 0.0190(15) C9 0.071(2) 0.0265(15) 0.065(2) 0.0041(14) 0.0280(17) 0.0094(14) C10 0.0509(15) 0.0296(14) 0.0449(16) -0.0001(12) 0.0137(12) -0.0011(12) C11 0.0360(13) 0.0542(17) 0.0307(13) -0.0066(13) 0.0017(10) -0.0026(13) C12 0.0531(16) 0.070(2) 0.0341(14) -0.0010(15) 0.0110(12) -0.0036(16) C13 0.0551(17) 0.065(2) 0.0465(17) 0.0081(16) 0.0207(14) -0.0117(16) C14 0.0413(14) 0.0530(18) 0.0522(17) 0.0009(14) 0.0085(12) -0.0180(14) C15 0.0312(11) 0.0356(14) 0.0371(13) 0.0010(12) 0.0041(10) -0.0048(11) C16 0.0340(12) 0.0306(13) 0.0364(13) 0.0005(11) -0.0018(10) -0.0068(10) C17 0.0375(14) 0.060(2) 0.0537(18) 0.0003(15) -0.0065(12) -0.0178(14) C18 0.0622(19) 0.066(2) 0.0495(18) -0.0013(16) -0.0244(15) -0.0239(17) C19 0.073(2) 0.058(2) 0.0300(14) -0.0017(14) -0.0108(14) -0.0166(17) C20 0.0494(15) 0.0433(16) 0.0287(13) 0.0003(12) 0.0019(11) -0.0094(13) _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 O2 2.0255(17) . ? Ni1 N1 2.0553(19) . ? Ni1 N4 2.0614(19) . ? Ni1 N2 2.079(2) . ? Ni1 O7 2.0820(17) . ? Ni1 N3 2.127(2) . ? V1 O1 1.6065(16) . ? V1 O2 1.6261(17) . ? V1 O4 1.8076(17) . ? V1 O3 1.8117(17) . ? V2 O5 1.577(2) . ? V2 O4 1.7377(18) . ? V2 O6 1.7384(18) . ? V2 O3 1.7467(17) 4_556 ? V3 O8 1.610(2) . ? V3 O7 1.6526(16) . ? V3 O9 1.7805(5) . ? V3 O6 1.8172(18) . ? N1 C1 1.337(3) . ? N1 C5 1.349(3) . ? N2 C10 1.331(3) . ? N2 C6 1.356(3) . ? N3 C11 1.334(3) . ? N3 C15 1.344(3) . ? N4 C20 1.331(3) . ? N4 C16 1.349(3) . ? O3 V2 1.7467(17) 4 ? O9 V3 1.7805(5) 3_557 ? C1 C2 1.384(3) . ? C2 C3 1.365(4) . ? C3 C4 1.380(4) . ? C4 C5 1.380(3) . ? C5 C6 1.475(3) . ? C6 C7 1.383(3) . ? C7 C8 1.379(4) . ? C8 C9 1.370(5) . ? C9 C10 1.374(4) . ? C11 C12 1.376(4) . ? C12 C13 1.376(4) . ? C13 C14 1.374(4) . ? C14 C15 1.387(3) . ? C15 C16 1.477(3) . ? C16 C17 1.382(3) . ? C17 C18 1.380(4) . ? C18 C19 1.367(4) . ? C19 C20 1.376(4) . ? 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 Ni1 N1 93.72(7) . . ? O2 Ni1 N4 90.42(8) . . ? N1 Ni1 N4 170.43(8) . . ? O2 Ni1 N2 172.58(7) . . ? N1 Ni1 N2 78.86(8) . . ? N4 Ni1 N2 96.91(8) . . ? O2 Ni1 O7 87.66(7) . . ? N1 Ni1 O7 96.33(7) . . ? N4 Ni1 O7 92.45(7) . . ? N2 Ni1 O7 93.10(7) . . ? O2 Ni1 N3 92.45(8) . . ? N1 Ni1 N3 92.72(7) . . ? N4 Ni1 N3 78.47(8) . . ? N2 Ni1 N3 87.95(8) . . ? O7 Ni1 N3 170.92(7) . . ? O1 V1 O2 110.10(10) . . ? O1 V1 O4 107.35(9) . . ? O2 V1 O4 109.87(9) . . ? O1 V1 O3 110.06(9) . . ? O2 V1 O3 108.86(9) . . ? O4 V1 O3 110.59(9) . . ? O5 V2 O4 109.77(13) . . ? O5 V2 O6 109.63(13) . . ? O4 V2 O6 108.37(10) . . ? O5 V2 O3 108.91(11) . 4_556 ? O4 V2 O3 109.06(9) . 4_556 ? O6 V2 O3 111.09(9) . 4_556 ? O8 V3 O7 108.48(10) . . ? O8 V3 O9 110.33(8) . . ? O7 V3 O9 110.84(6) . . ? O8 V3 O6 106.97(11) . . ? O7 V3 O6 112.17(9) . . ? O9 V3 O6 107.99(7) . . ? C1 N1 C5 118.7(2) . . ? C1 N1 Ni1 125.32(16) . . ? C5 N1 Ni1 114.95(15) . . ? C10 N2 C6 118.4(2) . . ? C10 N2 Ni1 127.28(18) . . ? C6 N2 Ni1 114.23(16) . . ? C11 N3 C15 118.0(2) . . ? C11 N3 Ni1 127.82(17) . . ? C15 N3 Ni1 113.39(16) . . ? C20 N4 C16 118.5(2) . . ? C20 N4 Ni1 125.33(17) . . ? C16 N4 Ni1 115.76(16) . . ? V1 O2 Ni1 175.81(11) . . ? V2 O3 V1 138.46(10) 4 . ? V2 O4 V1 138.87(12) . . ? V2 O6 V3 142.37(12) . . ? V3 O7 Ni1 141.83(10) . . ? V3 O9 V3 180.00(2) 3_557 . ? N1 C1 C2 122.6(2) . . ? C3 C2 C1 118.6(3) . . ? C2 C3 C4 119.5(2) . . ? C5 C4 C3 119.4(2) . . ? N1 C5 C4 121.2(2) . . ? N1 C5 C6 115.1(2) . . ? C4 C5 C6 123.7(2) . . ? N2 C6 C7 121.3(2) . . ? N2 C6 C5 115.2(2) . . ? C7 C6 C5 123.5(2) . . ? C8 C7 C6 119.2(3) . . ? C9 C8 C7 119.3(3) . . ? C8 C9 C10 118.9(3) . . ? N2 C10 C9 122.9(3) . . ? N3 C11 C12 123.1(3) . . ? C11 C12 C13 118.9(3) . . ? C14 C13 C12 118.7(3) . . ? C13 C14 C15 119.5(3) . . ? N3 C15 C14 121.7(2) . . ? N3 C15 C16 115.5(2) . . ? C14 C15 C16 122.8(2) . . ? N4 C16 C17 121.7(2) . . ? N4 C16 C15 115.4(2) . . ? C17 C16 C15 122.8(2) . . ? C18 C17 C16 118.8(3) . . ? C19 C18 C17 119.3(3) . . ? C18 C19 C20 119.0(3) . . ? N4 C20 C19 122.6(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.810 _refine_diff_density_min -1.265 _refine_diff_density_rms 0.105 data_compound_3 _database_code_CSD 173606 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H10 Co N2 O7 V2' _chemical_formula_weight 431.01 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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 9.212(2) _cell_length_b 10.543(2) _cell_length_c 14.388(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1397.4(5) _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 Rod _exptl_crystal_colour 'black brown' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.049 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 2.518 _exptl_absorpt_correction_type 'ABSCOR by T. Higashi' _exptl_absorpt_correction_T_min 0.6416 _exptl_absorpt_correction_T_max 1.1985 _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 Rigaku RAXIS RAPID IP _diffrn_measurement_method Oscillation _diffrn_detector_area_resol_mean '100x100 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1663 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 27.47 _reflns_number_total 1663 _reflns_number_gt 1590 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; Molecular Structure Corporation(1994) MSC/AFC Diffractometer Control Software MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. ; _computing_cell_refinement ; Molecular Structure Corporation(1994) MSC/AFC Diffractometer Control Software MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. ; _computing_data_reduction ; Molecular Structure Corporation(1994) MSC/AFC Diffractometer Control Software MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Interactive Molecular Graphics XP, Virsion 4.2 for MSDOS(1990), Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. ; _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0142P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.07(2) _refine_ls_number_reflns 1663 _refine_ls_number_parameters 203 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0185 _refine_ls_R_factor_gt 0.0167 _refine_ls_wR_factor_ref 0.0349 _refine_ls_wR_factor_gt 0.0347 _refine_ls_goodness_of_fit_ref 0.927 _refine_ls_restrained_S_all 0.926 _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 Co1 Co 0.05969(3) 0.13961(3) 0.73892(3) 0.01685(8) Uani 1 1 d . . . V1 V -0.11405(5) 0.16508(4) 0.96740(3) 0.01630(9) Uani 1 1 d . . . V2 V 0.17157(4) 0.03076(4) 1.08464(3) 0.01494(9) Uani 1 1 d . . . N1 N 0.0057(2) 0.3273(2) 0.70540(16) 0.0222(5) Uani 1 1 d . . . N2 N 0.2208(2) 0.2452(2) 0.81156(16) 0.0218(5) Uani 1 1 d . . . O1 O -0.0620(2) 0.1390(2) 0.86051(16) 0.0352(5) Uani 1 1 d . . . O2 O -0.1613(2) 0.31066(18) 0.98115(18) 0.0392(5) Uani 1 1 d . . . O3 O -0.2710(2) 0.06467(17) 0.98976(15) 0.0268(4) Uani 1 1 d . . . O4 O 0.0283(2) 0.13166(18) 1.04903(15) 0.0275(5) Uani 1 1 d . . . O5 O 0.1164(2) -0.0620(2) 1.17214(14) 0.0243(4) Uani 1 1 d . . . O6 O 0.30896(19) 0.11519(17) 1.12458(14) 0.0237(4) Uani 1 1 d . . . O1W O 0.1344(3) -0.0434(2) 0.78786(15) 0.0294(5) Uani 1 1 d . . . H1WA H 0.2087 -0.0632 0.7600 0.044 Uiso 1 1 calc R . . H1WB H 0.138(3) -0.055(3) 0.844(2) 0.025(8) Uiso 1 1 d . . . C1 C -0.0942(3) 0.3623(3) 0.6423(2) 0.0301(7) Uani 1 1 d . . . H1A H -0.1498 0.2998 0.6138 0.036 Uiso 1 1 calc R . . C2 C -0.1173(3) 0.4867(3) 0.6183(2) 0.0373(8) Uani 1 1 d . . . H2A H -0.1866 0.5075 0.5738 0.045 Uiso 1 1 calc R . . C3 C -0.0372(4) 0.5800(3) 0.6604(3) 0.0408(8) Uani 1 1 d . . . H3B H -0.0510 0.6647 0.6447 0.049 Uiso 1 1 calc R . . C4 C 0.0651(3) 0.5458(3) 0.7268(3) 0.0333(8) Uani 1 1 d . . . H4A H 0.1199 0.6075 0.7568 0.040 Uiso 1 1 calc R . . C5 C 0.0845(3) 0.4183(3) 0.7477(2) 0.0234(6) Uani 1 1 d . . . C6 C 0.1956(3) 0.3723(3) 0.81342(19) 0.0228(6) Uani 1 1 d . . . C7 C 0.2725(3) 0.4503(3) 0.8720(2) 0.0357(7) Uani 1 1 d . . . H7A H 0.2513 0.5364 0.8746 0.043 Uiso 1 1 calc R . . C8 C 0.3815(3) 0.4001(3) 0.9273(2) 0.0393(8) Uani 1 1 d . . . H8B H 0.4343 0.4522 0.9671 0.047 Uiso 1 1 calc R . . C9 C 0.4104(3) 0.2726(4) 0.9225(2) 0.0386(8) Uani 1 1 d . . . H9B H 0.4846 0.2371 0.9578 0.046 Uiso 1 1 calc R . . C10 C 0.3273(3) 0.1982(3) 0.8644(2) 0.0315(7) Uani 1 1 d . . . H10A H 0.3461 0.1116 0.8619 0.038 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 Co1 0.01622(16) 0.02070(16) 0.01364(14) -0.00134(17) 0.00127(15) -0.00126(13) V1 0.0176(2) 0.01876(19) 0.01250(18) 0.00098(18) 0.00055(17) 0.00091(17) V2 0.01407(18) 0.01859(19) 0.01215(17) -0.00029(17) -0.00059(19) -0.00044(17) N1 0.0208(12) 0.0261(11) 0.0199(10) -0.0004(10) 0.0000(10) 0.0030(10) N2 0.0205(12) 0.0242(11) 0.0207(11) -0.0008(10) -0.0007(10) -0.0025(9) O1 0.0318(13) 0.0559(15) 0.0180(10) -0.0046(10) 0.0073(10) -0.0118(10) O2 0.0507(13) 0.0215(9) 0.0453(13) 0.0033(11) -0.0084(13) 0.0103(9) O3 0.0241(10) 0.0349(9) 0.0213(8) 0.0092(10) -0.0009(9) -0.0050(9) O4 0.0256(10) 0.0287(11) 0.0283(11) -0.0005(9) -0.0089(9) 0.0056(9) O5 0.0223(10) 0.0297(11) 0.0210(9) 0.0075(9) 0.0028(8) -0.0033(9) O6 0.0212(9) 0.0273(10) 0.0226(8) 0.0021(8) -0.0026(8) -0.0048(8) O1W 0.0281(11) 0.0342(12) 0.0259(11) 0.0060(10) 0.0034(9) 0.0039(9) C1 0.0251(14) 0.0398(18) 0.0255(16) 0.0008(13) -0.0025(13) 0.0030(13) C2 0.0325(18) 0.051(2) 0.0284(15) 0.0139(16) 0.0035(14) 0.0136(16) C3 0.045(2) 0.0347(18) 0.0427(19) 0.0154(16) 0.0168(16) 0.0155(16) C4 0.0334(16) 0.0254(13) 0.041(2) 0.0016(14) 0.0115(15) -0.0006(12) C5 0.0219(13) 0.0246(12) 0.0238(13) -0.0042(13) 0.0064(13) 0.0021(11) C6 0.0208(13) 0.0259(13) 0.0215(12) -0.0043(11) 0.0039(12) -0.0017(11) C7 0.0343(17) 0.0348(15) 0.0379(17) -0.0138(15) 0.0012(15) -0.0040(14) C8 0.0356(18) 0.047(2) 0.0349(17) -0.0128(16) -0.0092(16) -0.0094(17) C9 0.0303(15) 0.056(2) 0.0298(16) 0.0039(16) -0.0117(14) -0.0024(16) C10 0.0296(16) 0.0334(16) 0.0316(15) 0.0033(15) -0.0066(14) -0.0013(13) _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 Co1 O5 2.0555(19) 2_554 ? Co1 O6 2.058(2) 4_554 ? Co1 O1 2.078(2) . ? Co1 N1 2.096(2) . ? Co1 N2 2.129(2) . ? Co1 O1W 2.166(2) . ? V1 O2 1.6075(19) . ? V1 O1 1.634(2) . ? V1 O4 1.795(2) . ? V1 O3 1.8205(19) . ? V2 O6 1.6506(18) . ? V2 O5 1.673(2) . ? V2 O4 1.7709(19) . ? V2 O3 1.777(2) 3 ? N1 C1 1.344(4) . ? N1 C5 1.349(4) . ? N2 C10 1.337(3) . ? N2 C6 1.360(3) . ? O3 V2 1.777(2) 3_455 ? O5 Co1 2.0555(19) 2 ? O6 Co1 2.058(2) 4 ? C1 C2 1.374(4) . ? C2 C3 1.370(5) . ? C3 C4 1.390(5) . ? C4 C5 1.390(4) . ? C5 C6 1.475(4) . ? C6 C7 1.374(4) . ? C7 C8 1.386(5) . ? C8 C9 1.372(5) . ? C9 C10 1.378(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 O5 Co1 O6 92.32(8) 2_554 4_554 ? O5 Co1 O1 88.08(8) 2_554 . ? O6 Co1 O1 171.78(8) 4_554 . ? O5 Co1 N1 94.65(9) 2_554 . ? O6 Co1 N1 94.23(8) 4_554 . ? O1 Co1 N1 93.93(9) . . ? O5 Co1 N2 171.01(8) 2_554 . ? O6 Co1 N2 92.76(8) 4_554 . ? O1 Co1 N2 87.95(8) . . ? N1 Co1 N2 77.58(9) . . ? O5 Co1 O1W 92.75(9) 2_554 . ? O6 Co1 O1W 87.80(8) 4_554 . ? O1 Co1 O1W 83.97(9) . . ? N1 Co1 O1W 172.24(9) . . ? N2 Co1 O1W 94.85(9) . . ? O2 V1 O1 110.84(12) . . ? O2 V1 O4 107.73(11) . . ? O1 V1 O4 111.61(11) . . ? O2 V1 O3 108.58(10) . . ? O1 V1 O3 107.55(10) . . ? O4 V1 O3 110.50(10) . . ? O6 V2 O5 106.62(10) . . ? O6 V2 O4 110.38(9) . . ? O5 V2 O4 110.03(10) . . ? O6 V2 O3 110.15(10) . 3 ? O5 V2 O3 109.74(10) . 3 ? O4 V2 O3 109.87(10) . 3 ? C1 N1 C5 118.6(3) . . ? C1 N1 Co1 125.2(2) . . ? C5 N1 Co1 116.10(19) . . ? C10 N2 C6 118.6(2) . . ? C10 N2 Co1 126.67(19) . . ? C6 N2 Co1 113.96(17) . . ? V1 O1 Co1 161.83(13) . . ? V2 O3 V1 134.56(12) 3_455 . ? V2 O4 V1 148.38(12) . . ? V2 O5 Co1 145.50(12) . 2 ? V2 O6 Co1 142.79(11) . 4 ? N1 C1 C2 122.6(3) . . ? C3 C2 C1 119.4(3) . . ? C2 C3 C4 118.9(3) . . ? C5 C4 C3 119.2(3) . . ? N1 C5 C4 121.4(3) . . ? N1 C5 C6 115.4(2) . . ? C4 C5 C6 123.1(3) . . ? N2 C6 C7 120.9(3) . . ? N2 C6 C5 115.4(2) . . ? C7 C6 C5 123.6(2) . . ? C6 C7 C8 119.9(3) . . ? C9 C8 C7 119.0(3) . . ? C8 C9 C10 118.7(3) . . ? N2 C10 C9 122.8(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.238 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.067