Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_1 _database_code_CSD 163766 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Gao, Song' 'Kou, Hui-Zhong' 'Liu, Cai-Ming' _publ_contact_author_name 'Prof Song Gao' _publ_contact_author_address ; Prof Song Gao 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 synthesis and crystal structure of a novel layered vanadium oxide metal coordination complex [(2,2'-biphen)Co]2V6)17 ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H14 Co N4 O8.50 V3' _chemical_formula_weight 706.14 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 Monoclinic _symmetry_space_group_name_H-M C2/c 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 19.660(4) _cell_length_b 18.430(4) _cell_length_c 13.640(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.20(3) _cell_angle_gamma 90.00 _cell_volume 4811.7(17) _cell_formula_units_Z 8 _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 red' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.950 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2800 _exptl_absorpt_coefficient_mu 1.870 _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 'NONIUS Kappa CCD' _diffrn_measurement_method 'CCD' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6778 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0213 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.64 _diffrn_reflns_theta_max 30.05 _reflns_number_total 6778 _reflns_number_gt 5750 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Kappa CCD' _computing_cell_refinement 'HKL Scalepack' _computing_data_reduction 'HKL Denzo & Maxus' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL (1990)' _computing_publication_material 'Siemens SHELXL-97' _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^)+(0.0551P)^2^+14.6957P] 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 6778 _refine_ls_number_parameters 366 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1125 _refine_ls_wR_factor_gt 0.1046 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.002 _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 0.408061(16) 0.221250(17) 0.88895(2) 0.02575(9) Uani 1 1 d . . . V1 V 0.32767(2) 0.18821(2) 0.64219(3) 0.02735(10) Uani 1 1 d . . . V2 V 0.33529(2) 0.27847(2) 0.43483(3) 0.02947(10) Uani 1 1 d . . . V3 V 0.504488(19) 0.27214(2) 1.13120(3) 0.02387(9) Uani 1 1 d . . . C1 C 0.51763(16) 0.34713(16) 0.8749(2) 0.0409(6) Uani 1 1 d . . . H1A H 0.5493 0.3100 0.8729 0.049 Uiso 1 1 calc R . . C2 C 0.5412(2) 0.41912(18) 0.8744(3) 0.0574(9) Uani 1 1 d . . . H2B H 0.5875 0.4289 0.8739 0.069 Uiso 1 1 calc R . . C3 C 0.4959(2) 0.47352(19) 0.8747(3) 0.0623(10) Uani 1 1 d . . . H3A H 0.5109 0.5214 0.8747 0.075 Uiso 1 1 calc R . . C4 C 0.4266(2) 0.45873(18) 0.8751(2) 0.0571(10) Uani 1 1 d . . . C5 C 0.3733(3) 0.5115(2) 0.8721(3) 0.0775(15) Uani 1 1 d . . . H5B H 0.3848 0.5605 0.8718 0.093 Uiso 1 1 calc R . . C6 C 0.3076(3) 0.4932(2) 0.8699(3) 0.0770(15) Uani 1 1 d . . . H6A H 0.2746 0.5298 0.8674 0.092 Uiso 1 1 calc R . . C7 C 0.2854(2) 0.4186(3) 0.8711(3) 0.0687(13) Uani 1 1 d . . . C8 C 0.2190(3) 0.3939(4) 0.8665(3) 0.0861(18) Uani 1 1 d . . . H8B H 0.1831 0.4275 0.8617 0.103 Uiso 1 1 calc R . . C9 C 0.2035(2) 0.3219(4) 0.8688(3) 0.0805(17) Uani 1 1 d . . . H9B H 0.1578 0.3066 0.8646 0.097 Uiso 1 1 calc R . . C10 C 0.25969(16) 0.2696(3) 0.8780(2) 0.0566(10) Uani 1 1 d . . . C11 C 0.33732(19) 0.36462(19) 0.8778(2) 0.0495(8) Uani 1 1 d . . . C12 C 0.40727(18) 0.38435(16) 0.8776(2) 0.0422(7) Uani 1 1 d . . . C13 C 0.25620(15) 0.1905(3) 0.8808(2) 0.0616(12) Uani 1 1 d . . . C14 C 0.1974(2) 0.1456(4) 0.8767(3) 0.090(2) Uani 1 1 d . . . H14A H 0.1537 0.1666 0.8713 0.108 Uiso 1 1 calc R . . C15 C 0.2037(3) 0.0734(4) 0.8805(3) 0.100(2) Uani 1 1 d . . . H15A H 0.1644 0.0453 0.8802 0.121 Uiso 1 1 calc R . . C16 C 0.2687(3) 0.0385(3) 0.8849(3) 0.0852(18) Uani 1 1 d . . . C17 C 0.2831(5) -0.0375(4) 0.8865(4) 0.118(3) Uani 1 1 d . . . H17A H 0.2476 -0.0701 0.8895 0.142 Uiso 1 1 calc R . . C18 C 0.3467(5) -0.0631(3) 0.8836(4) 0.107(3) Uani 1 1 d . . . H18A H 0.3534 -0.1131 0.8835 0.129 Uiso 1 1 calc R . . C19 C 0.4050(3) -0.01593(19) 0.8806(2) 0.0707(14) Uani 1 1 d . . . C20 C 0.4724(4) -0.0384(2) 0.8762(3) 0.0870(18) Uani 1 1 d . . . H20A H 0.4825 -0.0876 0.8745 0.104 Uiso 1 1 calc R . . C21 C 0.5227(3) 0.0114(2) 0.8744(3) 0.0709(13) Uani 1 1 d . . . H21A H 0.5672 -0.0033 0.8704 0.085 Uiso 1 1 calc R . . C22 C 0.50699(18) 0.08574(18) 0.8785(2) 0.0464(7) Uani 1 1 d . . . H22A H 0.5421 0.1195 0.8781 0.056 Uiso 1 1 calc R . . C23 C 0.39362(19) 0.05905(16) 0.88406(19) 0.0467(8) Uani 1 1 d . . . C24 C 0.32565(19) 0.0857(2) 0.8862(2) 0.0532(9) Uani 1 1 d . . . N1 N 0.45287(12) 0.32931(12) 0.87792(15) 0.0334(5) Uani 1 1 d . . . N2 N 0.32357(12) 0.29312(16) 0.88287(17) 0.0434(6) Uani 1 1 d . . . N3 N 0.31834(12) 0.15787(16) 0.88673(17) 0.0425(6) Uani 1 1 d . . . N4 N 0.44435(13) 0.10940(12) 0.88301(16) 0.0345(5) Uani 1 1 d . . . O1 O 0.38994(9) 0.22343(10) 0.73147(13) 0.0321(4) Uani 1 1 d . . . O2 O 0.32723(12) 0.10187(12) 0.65867(17) 0.0492(5) Uani 1 1 d . . . O3 O 0.34572(10) 0.20595(11) 0.51908(13) 0.0353(4) Uani 1 1 d . . . O4 O 0.33151(14) 0.35090(13) 0.4974(2) 0.0600(6) Uani 1 1 d . . . O5 O 0.25531(10) 0.27023(14) 0.34737(15) 0.0468(5) Uani 1 1 d . . . O6 O 0.40482(11) 0.28105(17) 0.37598(19) 0.0624(8) Uani 1 1 d . . . O7 O 0.46073(10) 0.22021(10) 1.03818(14) 0.0362(4) Uani 1 1 d . . . O8 O 0.5000 0.23262(15) 1.2500 0.0414(6) Uani 1 2 d S . . O9 O 0.46898(12) 0.35118(11) 1.12055(17) 0.0464(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.02209(15) 0.02916(17) 0.02410(16) -0.00124(11) 0.00130(11) 0.00073(11) V1 0.02133(18) 0.0391(2) 0.02032(18) 0.00290(15) 0.00198(14) -0.00543(15) V2 0.01905(18) 0.0407(2) 0.0283(2) 0.00870(16) 0.00467(15) -0.00038(15) V3 0.01925(17) 0.0307(2) 0.02152(17) -0.00295(14) 0.00434(13) 0.00053(13) C1 0.0460(15) 0.0343(13) 0.0371(13) 0.0031(11) -0.0016(11) -0.0084(11) C2 0.072(2) 0.0395(16) 0.0516(18) 0.0069(14) -0.0057(16) -0.0179(16) C3 0.093(3) 0.0374(16) 0.0461(18) 0.0005(13) -0.0051(18) -0.0113(17) C4 0.100(3) 0.0365(15) 0.0284(13) -0.0015(11) 0.0020(15) 0.0222(17) C5 0.129(4) 0.043(2) 0.053(2) -0.0041(16) 0.007(2) 0.042(2) C6 0.120(4) 0.061(2) 0.0458(19) 0.0005(17) 0.010(2) 0.064(3) C7 0.075(3) 0.092(3) 0.0372(16) 0.0038(17) 0.0087(16) 0.059(2) C8 0.078(3) 0.136(5) 0.044(2) 0.009(2) 0.0135(19) 0.067(3) C9 0.0379(17) 0.166(6) 0.0382(18) -0.001(2) 0.0096(14) 0.032(3) C10 0.0313(14) 0.112(3) 0.0258(13) 0.0006(15) 0.0059(11) 0.0158(16) C11 0.066(2) 0.0559(18) 0.0247(12) -0.0010(11) 0.0059(12) 0.0365(16) C12 0.0630(19) 0.0344(13) 0.0250(11) -0.0024(10) 0.0013(12) 0.0177(12) C13 0.0245(13) 0.137(4) 0.0237(12) -0.0033(17) 0.0056(10) -0.0185(17) C14 0.0379(18) 0.189(6) 0.0421(19) -0.004(3) 0.0093(15) -0.051(3) C15 0.070(3) 0.189(7) 0.042(2) -0.004(3) 0.0137(18) -0.091(4) C16 0.099(3) 0.122(4) 0.0323(16) -0.0007(19) 0.0106(18) -0.086(3) C17 0.179(7) 0.117(5) 0.048(2) 0.008(3) 0.006(4) -0.114(5) C18 0.208(7) 0.049(2) 0.050(2) 0.0096(18) 0.000(4) -0.064(4) C19 0.138(4) 0.0323(16) 0.0310(15) 0.0054(12) -0.003(2) -0.019(2) C20 0.182(6) 0.0291(17) 0.0388(18) 0.0033(13) 0.001(3) 0.020(3) C21 0.114(4) 0.052(2) 0.0422(18) 0.0024(15) 0.008(2) 0.040(2) C22 0.0557(18) 0.0424(16) 0.0383(14) 0.0000(12) 0.0048(13) 0.0148(13) C23 0.076(2) 0.0364(14) 0.0217(11) 0.0046(10) -0.0013(12) -0.0204(14) C24 0.061(2) 0.074(2) 0.0223(12) 0.0017(13) 0.0047(12) -0.0416(18) N1 0.0443(12) 0.0267(10) 0.0250(9) -0.0003(8) -0.0006(9) 0.0064(9) N2 0.0313(11) 0.0708(17) 0.0268(10) -0.0030(11) 0.0041(9) 0.0196(11) N3 0.0309(11) 0.0720(18) 0.0240(10) 0.0006(10) 0.0052(8) -0.0178(11) N4 0.0441(12) 0.0299(10) 0.0264(10) 0.0015(8) 0.0013(9) -0.0021(9) O1 0.0280(8) 0.0408(10) 0.0243(8) -0.0009(7) -0.0004(6) -0.0026(7) O2 0.0552(13) 0.0427(12) 0.0455(12) 0.0098(9) 0.0027(10) -0.0179(10) O3 0.0419(10) 0.0398(10) 0.0259(8) 0.0042(7) 0.0112(7) 0.0029(8) O4 0.0628(15) 0.0402(12) 0.0698(16) -0.0028(11) 0.0006(13) 0.0022(11) O5 0.0237(9) 0.0873(17) 0.0279(9) 0.0021(10) 0.0028(7) 0.0031(9) O6 0.0246(9) 0.116(2) 0.0496(13) 0.0320(14) 0.0146(9) 0.0071(11) O7 0.0412(10) 0.0384(10) 0.0241(8) -0.0013(7) -0.0028(7) -0.0037(8) O8 0.0612(18) 0.0381(14) 0.0242(12) 0.000 0.0085(12) 0.000 O9 0.0541(12) 0.0338(10) 0.0502(12) 0.0016(9) 0.0098(10) 0.0074(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 Co1 O7 2.0624(19) . ? Co1 O1 2.0959(18) . ? Co1 N3 2.110(2) . ? Co1 N2 2.111(2) . ? Co1 N4 2.189(2) . ? Co1 N1 2.197(2) . ? V1 O2 1.607(2) . ? V1 O1 1.6499(18) . ? V1 O3 1.8233(19) . ? V1 O5 1.837(2) 7_556 ? V2 O4 1.596(3) . ? V2 O6 1.737(2) . ? V2 O3 1.7441(19) . ? V2 O5 1.750(2) . ? V3 O9 1.607(2) . ? V3 O7 1.6636(19) . ? V3 O8 1.7971(13) . ? V3 O6 1.815(2) 2_656 ? C1 N1 1.325(4) . ? C1 C2 1.406(4) . ? C2 C3 1.342(6) . ? C3 C4 1.389(6) . ? C4 C5 1.425(5) . ? C4 C12 1.425(5) . ? C5 C6 1.329(8) . ? C6 C7 1.443(7) . ? C7 C8 1.372(8) . ? C7 C11 1.413(4) . ? C8 C9 1.363(8) . ? C9 C10 1.450(6) . ? C10 N2 1.316(4) . ? C10 C13 1.459(7) . ? C11 N2 1.350(5) . ? C11 C12 1.423(5) . ? C12 N1 1.353(3) . ? C13 N3 1.348(5) . ? C13 C14 1.412(5) . ? C14 C15 1.336(9) . ? C15 C16 1.421(9) . ? C16 C24 1.414(4) . ? C16 C17 1.429(10) . ? C17 C18 1.345(10) . ? C18 C19 1.448(7) . ? C19 C20 1.401(7) . ? C19 C23 1.403(5) . ? C20 C21 1.353(7) . ? C21 C22 1.408(5) . ? C22 N4 1.321(4) . ? C23 N4 1.365(4) . ? C23 C24 1.430(5) . ? C24 N3 1.339(5) . ? O5 V1 1.837(2) 7_556 ? O6 V3 1.815(2) 2_656 ? O8 V3 1.7971(13) 2_657 ? 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 O7 Co1 O1 160.26(8) . . ? O7 Co1 N3 103.80(9) . . ? O1 Co1 N3 92.87(8) . . ? O7 Co1 N2 104.94(9) . . ? O1 Co1 N2 89.98(8) . . ? N3 Co1 N2 72.49(12) . . ? O7 Co1 N4 86.18(8) . . ? O1 Co1 N4 87.75(8) . . ? N3 Co1 N4 75.91(11) . . ? N2 Co1 N4 148.16(11) . . ? O7 Co1 N1 87.55(8) . . ? O1 Co1 N1 83.65(8) . . ? N3 Co1 N1 147.99(10) . . ? N2 Co1 N1 75.69(10) . . ? N4 Co1 N1 135.40(9) . . ? O2 V1 O1 108.24(10) . . ? O2 V1 O3 108.34(11) . . ? O1 V1 O3 109.97(10) . . ? O2 V1 O5 111.64(12) . 7_556 ? O1 V1 O5 107.52(10) . 7_556 ? O3 V1 O5 111.08(9) . 7_556 ? O4 V2 O6 111.25(15) . . ? O4 V2 O3 107.53(12) . . ? O6 V2 O3 109.82(11) . . ? O4 V2 O5 107.04(13) . . ? O6 V2 O5 111.52(11) . . ? O3 V2 O5 109.56(11) . . ? O9 V3 O7 108.31(11) . . ? O9 V3 O8 109.82(11) . . ? O7 V3 O8 109.34(10) . . ? O9 V3 O6 108.96(13) . 2_656 ? O7 V3 O6 110.74(11) . 2_656 ? O8 V3 O6 109.65(10) . 2_656 ? N1 C1 C2 123.7(3) . . ? C3 C2 C1 119.1(4) . . ? C2 C3 C4 120.3(3) . . ? C3 C4 C5 125.6(4) . . ? C3 C4 C12 117.1(3) . . ? C5 C4 C12 117.3(4) . . ? C6 C5 C4 122.2(4) . . ? C5 C6 C7 122.4(3) . . ? C8 C7 C11 115.8(5) . . ? C8 C7 C6 127.1(4) . . ? C11 C7 C6 117.2(4) . . ? C9 C8 C7 122.6(4) . . ? C8 C9 C10 118.6(4) . . ? N2 C10 C9 119.0(5) . . ? N2 C10 C13 112.2(3) . . ? C9 C10 C13 128.8(4) . . ? N2 C11 C7 122.7(4) . . ? N2 C11 C12 117.0(2) . . ? C7 C11 C12 120.2(4) . . ? N1 C12 C11 116.6(3) . . ? N1 C12 C4 122.7(3) . . ? C11 C12 C4 120.6(3) . . ? N3 C13 C14 117.6(5) . . ? N3 C13 C10 113.6(3) . . ? C14 C13 C10 128.8(4) . . ? C15 C14 C13 121.0(5) . . ? C14 C15 C16 121.8(4) . . ? C24 C16 C15 115.1(5) . . ? C24 C16 C17 116.7(6) . . ? C15 C16 C17 128.2(5) . . ? C18 C17 C16 121.8(4) . . ? C17 C18 C19 122.5(5) . . ? C20 C19 C23 116.9(4) . . ? C20 C19 C18 125.9(5) . . ? C23 C19 C18 117.2(5) . . ? C21 C20 C19 120.1(4) . . ? C20 C21 C22 119.4(4) . . ? N4 C22 C21 122.6(4) . . ? N4 C23 C19 123.1(4) . . ? N4 C23 C24 117.1(3) . . ? C19 C23 C24 119.8(4) . . ? N3 C24 C16 121.7(4) . . ? N3 C24 C23 116.3(2) . . ? C16 C24 C23 122.0(4) . . ? C1 N1 C12 117.1(3) . . ? C1 N1 Co1 129.08(19) . . ? C12 N1 Co1 113.8(2) . . ? C10 N2 C11 121.3(3) . . ? C10 N2 Co1 121.9(3) . . ? C11 N2 Co1 116.7(2) . . ? C24 N3 C13 122.7(3) . . ? C24 N3 Co1 117.4(2) . . ? C13 N3 Co1 119.8(3) . . ? C22 N4 C23 117.9(3) . . ? C22 N4 Co1 128.9(2) . . ? C23 N4 Co1 113.3(2) . . ? V1 O1 Co1 132.28(11) . . ? V2 O3 V1 136.55(12) . . ? V2 O5 V1 125.92(13) . 7_556 ? V2 O6 V3 155.35(15) . 2_656 ? V3 O7 Co1 143.42(11) . . ? V3 O8 V3 132.18(17) 2_657 . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.789 _refine_diff_density_min -0.837 _refine_diff_density_rms 0.088