# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1745 data_global #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Chen, Xiao-Ming School of Chemistry and Chemical Engineering Zhongshan University Guangzhou, 510275 P. R. China ; _publ_contact_author_phone '86-20-84113986' _publ_contact_author_fax '86 20 84112245' _publ_contact_author_email cescxm@zsu.edu.cn _publ_requested_joiurnal 'Chem. Commun.' _publ_requested_coeditor_name ? _publ_contact_letter ; Dear Sir/Madam: Please consider this CIF as supplmentary data for a manuscript submitted to Chem. Commun. Xiao-Ming Chen ; #================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Hydrothermal synthesis and crystal structures of two bimetallic chain-like and cluster complexes [{Co(phen)2}2V6O17]n and [{Cu(phen)2}4V10O29].6H2O ; loop_ _publ_author_name _publ_author_address 'Zhang, Xian-Ming' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; 'Tong, Ming-Liang' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; 'Chen, Xiao-Ming' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; #============================================================ data_complex_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H32 Co2 N8 O17 V6' _chemical_formula_weight 1416.32 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 TRICLINIC _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.216(7) _cell_length_b 11.372(6) _cell_length_c 11.788(7) _cell_angle_alpha 82.76(1) _cell_angle_beta 72.70(1) _cell_angle_gamma 75.57(1) _cell_volume 1264(1) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 28 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.860 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 1.780 _exptl_absorpt_correction_type semi-emprical _exptl_absorpt_correction_T_min 0.761 _exptl_absorpt_correction_T_max 0.795 _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 'Siemens R3m' _diffrn_measurement_method '\W scan' _diffrn_standards_number 2 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% none _diffrn_reflns_number 5452 _diffrn_reflns_av_R_equivalents 0.0541 _diffrn_reflns_av_sigmaI/netI 0.0749 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 26.91 _reflns_number_total 4973 _reflns_number_gt 3279 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V.5.0 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.1130P)^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 0.0040(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4973 _refine_ls_number_parameters 368 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1100 _refine_ls_R_factor_gt 0.0671 _refine_ls_wR_factor_ref 0.1916 _refine_ls_wR_factor_gt 0.1664 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.134 _refine_ls_shift/su_mean 0.027 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.35007(9) 0.24069(7) 0.78432(8) 0.0281(3) Uani 1 d . . . V1 V 0.33187(11) 0.15283(10) 0.49470(10) 0.0301(3) Uani 1 d . . . V2 V 0.17857(12) -0.00918(10) 0.91102(10) 0.0320(3) Uani 1 d . . . V3 V 0.31722(11) -0.11350(10) 0.62897(10) 0.0300(3) Uani 1 d . . . O1 O 0.3460(5) 0.1933(5) 0.6200(4) 0.0444(13) Uani 1 d . . . O2 O 0.2234(5) 0.1244(4) 0.8761(5) 0.0446(13) Uani 1 d . . . O3 O 0.5019(5) 0.1371(5) 0.3792(4) 0.0412(12) Uani 1 d . . . O4 O 0.2147(5) 0.2567(4) 0.4491(5) 0.0443(12) Uani 1 d . . . O5 O 0.2839(6) -0.0935(6) 0.9824(6) 0.0643(17) Uani 1 d . . . O6 O 0.0000 0.0000 1.0000 0.0454(18) Uani 1 d S . . O7 O 0.2767(5) 0.0089(4) 0.5242(4) 0.0412(12) Uani 1 d . . . O8 O 0.2093(6) -0.0831(5) 0.7737(4) 0.0502(14) Uani 1 d . . . O9 O 0.2875(6) -0.2343(4) 0.5931(5) 0.0470(13) Uani 1 d . . . C1 C 0.1010(8) 0.4326(8) 0.7181(7) 0.050(2) Uani 1 d . . . H1A H 0.1067 0.3754 0.6625 0.080 Uiso 1 d R . . C2 C 0.0117(9) 0.5465(10) 0.7157(9) 0.070(3) Uani 1 d . . . H2A H -0.0459 0.5670 0.6618 0.080 Uiso 1 d R . . C3 C 0.0065(9) 0.6299(8) 0.7938(10) 0.073(3) Uani 1 d . . . H3A H -0.0513 0.7104 0.7917 0.080 Uiso 1 d R . . C4 C 0.0861(8) 0.5978(6) 0.8771(8) 0.052(2) Uani 1 d . . . C5 C 0.1737(7) 0.4780(6) 0.8716(6) 0.0332(15) Uani 1 d . . . C6 C 0.0882(12) 0.6758(8) 0.9655(10) 0.078(4) Uani 1 d . . . H6A H 0.0298 0.7565 0.9702 0.080 Uiso 1 d R . . C7 C 0.1715(12) 0.6381(9) 1.0380(10) 0.077(3) Uani 1 d . . . H7A H 0.1690 0.6920 1.0955 0.080 Uiso 1 d R . . C8 C 0.2629(10) 0.5177(8) 1.0348(7) 0.055(2) Uani 1 d . . . C9 C 0.2641(7) 0.4387(6) 0.9526(6) 0.0365(16) Uani 1 d . . . C10 C 0.3498(12) 0.4738(10) 1.1092(7) 0.070(3) Uani 1 d . . . H10A H 0.3512 0.5243 1.1680 0.080 Uiso 1 d R . . C11 C 0.4345(12) 0.3580(11) 1.0977(8) 0.069(3) Uani 1 d . . . H11A H 0.4930 0.3264 1.1499 0.080 Uiso 1 d R . . C12 C 0.4336(8) 0.2867(7) 1.0104(7) 0.0459(19) Uani 1 d . . . H12A H 0.4970 0.2084 0.9992 0.080 Uiso 1 d R . . C13 C 0.4709(7) 0.4751(6) 0.6557(6) 0.0331(15) Uani 1 d . . . H13A H 0.3745 0.5181 0.6690 0.080 Uiso 1 d R . . C14 C 0.5767(8) 0.5378(6) 0.6004(6) 0.0388(17) Uani 1 d . . . H14A H 0.5526 0.6227 0.5773 0.080 Uiso 1 d R . . C15 C 0.7160(7) 0.4773(6) 0.5789(6) 0.0365(16) Uani 1 d . . . H15A H 0.7893 0.5200 0.5417 0.080 Uiso 1 d R . . C16 C 0.7496(7) 0.3526(6) 0.6129(6) 0.0345(15) Uani 1 d . . . C17 C 0.6368(7) 0.2950(6) 0.6713(5) 0.0290(14) Uani 1 d . . . C18 C 0.8926(8) 0.2809(7) 0.5928(7) 0.0443(18) Uani 1 d . . . H18A H 0.9698 0.3189 0.5549 0.080 Uiso 1 d R . . C19 C 0.9178(7) 0.1602(7) 0.6291(7) 0.049(2) Uani 1 d . . . H19A H 1.0128 0.1132 0.6127 0.080 Uiso 1 d R . . C20 C 0.8045(7) 0.1011(6) 0.6905(7) 0.0381(16) Uani 1 d . . . C21 C 0.6645(6) 0.1678(6) 0.7111(6) 0.0285(14) Uani 1 d . . . C22 C 0.8286(9) -0.0239(7) 0.7315(8) 0.055(2) Uani 1 d . . . H22A H 0.9225 -0.0719 0.7220 0.080 Uiso 1 d R . . C23 C 0.7141(8) -0.0729(7) 0.7874(8) 0.051(2) Uani 1 d . . . H23A H 0.7273 -0.1576 0.8130 0.080 Uiso 1 d R . . C24 C 0.5777(7) 0.0003(6) 0.8043(7) 0.0409(17) Uani 1 d . . . H24A H 0.4992 -0.0355 0.8441 0.080 Uiso 1 d R . . N1 N 0.1815(6) 0.3978(5) 0.7925(5) 0.0357(13) Uani 1 d . . . N2 N 0.3478(6) 0.3239(5) 0.9392(5) 0.0341(13) Uani 1 d . . . N3 N 0.4988(6) 0.3547(5) 0.6914(4) 0.0285(12) Uani 1 d . . . N4 N 0.5519(5) 0.1179(5) 0.7680(5) 0.0307(12) Uani 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 0.0257(5) 0.0265(5) 0.0311(5) -0.0028(4) -0.0045(4) -0.0077(4) V1 0.0278(6) 0.0305(6) 0.0307(6) -0.0036(5) -0.0040(5) -0.0080(5) V2 0.0279(6) 0.0306(6) 0.0334(6) -0.0047(5) 0.0024(5) -0.0106(5) V3 0.0289(6) 0.0295(6) 0.0290(6) -0.0064(5) 0.0006(5) -0.0102(5) O1 0.047(3) 0.052(3) 0.035(3) -0.011(2) -0.002(2) -0.021(3) O2 0.037(3) 0.038(3) 0.053(3) -0.008(2) 0.006(2) -0.017(2) O3 0.029(2) 0.056(3) 0.030(3) 0.002(2) 0.000(2) -0.007(2) O4 0.035(3) 0.043(3) 0.054(3) 0.005(2) -0.012(2) -0.012(2) O5 0.052(4) 0.068(4) 0.073(4) 0.014(3) -0.026(3) -0.014(3) O6 0.039(4) 0.045(4) 0.047(4) -0.010(3) 0.004(3) -0.017(3) O7 0.041(3) 0.038(3) 0.049(3) 0.004(2) -0.018(2) -0.012(2) O8 0.051(3) 0.054(3) 0.038(3) -0.015(2) 0.010(2) -0.019(3) O9 0.060(3) 0.035(3) 0.051(3) -0.007(2) -0.016(3) -0.018(3) C1 0.040(4) 0.059(5) 0.049(5) 0.015(4) -0.017(4) -0.010(4) C2 0.038(5) 0.082(7) 0.074(7) 0.032(6) -0.016(5) -0.005(5) C3 0.033(4) 0.049(5) 0.095(8) 0.033(5) 0.008(5) 0.015(4) C4 0.038(4) 0.027(4) 0.067(5) -0.002(4) 0.015(4) 0.000(3) C5 0.029(3) 0.029(3) 0.033(4) -0.006(3) 0.006(3) -0.008(3) C6 0.067(7) 0.036(5) 0.095(8) -0.021(5) 0.036(6) -0.009(5) C7 0.084(8) 0.058(6) 0.077(7) -0.034(5) 0.026(6) -0.038(6) C8 0.067(6) 0.052(5) 0.039(4) -0.016(4) 0.009(4) -0.025(4) C9 0.036(4) 0.034(4) 0.038(4) -0.004(3) 0.002(3) -0.018(3) C10 0.099(8) 0.092(8) 0.034(5) -0.022(5) 0.000(5) -0.060(7) C11 0.084(7) 0.105(8) 0.039(5) 0.011(5) -0.028(5) -0.055(7) C12 0.050(5) 0.055(5) 0.040(4) 0.016(4) -0.019(4) -0.025(4) C13 0.037(4) 0.025(3) 0.033(4) 0.002(3) -0.005(3) -0.005(3) C14 0.046(4) 0.032(4) 0.038(4) 0.004(3) -0.007(3) -0.018(3) C15 0.038(4) 0.035(4) 0.038(4) -0.005(3) -0.005(3) -0.016(3) C16 0.031(3) 0.043(4) 0.032(4) -0.007(3) -0.005(3) -0.015(3) C17 0.028(3) 0.033(3) 0.027(3) -0.006(3) -0.007(3) -0.009(3) C18 0.031(4) 0.040(4) 0.060(5) -0.003(4) -0.007(4) -0.012(3) C19 0.020(3) 0.056(5) 0.064(5) 0.001(4) -0.007(3) -0.005(3) C20 0.026(3) 0.038(4) 0.047(4) 0.000(3) -0.010(3) -0.003(3) C21 0.026(3) 0.031(3) 0.030(3) -0.002(3) -0.005(3) -0.013(3) C22 0.041(4) 0.038(4) 0.080(6) 0.008(4) -0.016(4) -0.004(4) C23 0.038(4) 0.030(4) 0.077(6) 0.010(4) -0.012(4) -0.003(3) C24 0.035(4) 0.029(4) 0.055(5) 0.002(3) -0.006(3) -0.010(3) N1 0.031(3) 0.037(3) 0.036(3) 0.006(3) -0.009(3) -0.007(3) N2 0.038(3) 0.034(3) 0.028(3) 0.003(2) -0.007(3) -0.010(3) N3 0.030(3) 0.027(3) 0.026(3) -0.001(2) -0.003(2) -0.010(2) N4 0.025(3) 0.028(3) 0.038(3) -0.001(2) -0.006(2) -0.008(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O2 2.062(5) . ? Co1 O1 2.089(5) . ? Co1 N1 2.139(6) . ? Co1 N2 2.151(6) . ? Co1 N4 2.153(5) . ? Co1 N3 2.196(5) . ? V1 O4 1.623(5) . ? V1 O1 1.658(5) . ? V1 O7 1.822(5) . ? V1 O3 1.845(5) . ? V2 O5 1.614(6) . ? V2 O2 1.663(5) . ? V2 O6 1.7982(15) . ? V2 O8 1.826(5) . ? V3 O9 1.608(5) . ? V3 O8 1.757(5) . ? V3 O3 1.774(5) 2_656 ? V3 O7 1.794(5) . ? O3 V3 1.774(5) 2_656 ? O6 V2 1.7982(15) 2_557 ? C1 N1 1.335(9) . ? C1 C2 1.388(11) . ? C2 C3 1.384(14) . ? C3 C4 1.413(14) . ? C4 C5 1.429(9) . ? C4 C6 1.459(14) . ? C5 N1 1.357(9) . ? C5 C9 1.475(10) . ? C6 C7 1.341(15) . ? C7 C8 1.450(13) . ? C8 C10 1.393(14) . ? C8 C9 1.397(10) . ? C9 N2 1.370(9) . ? C10 C11 1.381(14) . ? C11 C12 1.391(12) . ? C12 N2 1.348(9) . ? C13 N3 1.365(8) . ? C13 C14 1.396(9) . ? C14 C15 1.380(10) . ? C15 C16 1.409(9) . ? C16 C17 1.422(9) . ? C16 C18 1.450(10) . ? C17 N3 1.368(8) . ? C17 C21 1.448(9) . ? C18 C19 1.368(10) . ? C19 C20 1.443(10) . ? C20 C21 1.406(9) . ? C20 C22 1.428(10) . ? C21 N4 1.366(8) . ? C22 C23 1.374(11) . ? C23 C24 1.404(10) . ? C24 N4 1.336(8) . ? 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 Co1 O1 92.1(2) . . ? O2 Co1 N1 95.2(2) . . ? O1 Co1 N1 94.1(2) . . ? O2 Co1 N2 95.6(2) . . ? O1 Co1 N2 169.2(2) . . ? N1 Co1 N2 77.7(2) . . ? O2 Co1 N4 98.8(2) . . ? O1 Co1 N4 90.7(2) . . ? N1 Co1 N4 165.0(2) . . ? N2 Co1 N4 95.6(2) . . ? O2 Co1 N3 175.4(2) . . ? O1 Co1 N3 89.50(19) . . ? N1 Co1 N3 88.9(2) . . ? N2 Co1 N3 83.4(2) . . ? N4 Co1 N3 76.9(2) . . ? O4 V1 O1 109.0(3) . . ? O4 V1 O7 109.7(2) . . ? O1 V1 O7 108.6(2) . . ? O4 V1 O3 109.1(2) . . ? O1 V1 O3 110.2(2) . . ? O7 V1 O3 110.2(2) . . ? O5 V2 O2 107.7(3) . . ? O5 V2 O6 109.2(2) . . ? O2 V2 O6 114.22(18) . . ? O5 V2 O8 106.8(3) . . ? O2 V2 O8 108.6(2) . . ? O6 V2 O8 110.02(18) . . ? O9 V3 O8 107.3(3) . . ? O9 V3 O3 109.6(3) . 2_656 ? O8 V3 O3 111.8(3) . 2_656 ? O9 V3 O7 108.7(3) . . ? O8 V3 O7 111.3(2) . . ? O3 V3 O7 108.2(2) 2_656 . ? V1 O1 Co1 175.8(3) . . ? V2 O2 Co1 155.0(3) . . ? V3 O3 V1 138.2(3) 2_656 . ? V2 O6 V2 180.0 2_557 . ? V3 O7 V1 128.2(3) . . ? V3 O8 V2 147.4(3) . . ? N1 C1 C2 123.9(9) . . ? C3 C2 C1 118.5(9) . . ? C2 C3 C4 120.6(8) . . ? C3 C4 C5 115.9(8) . . ? C3 C4 C6 126.2(9) . . ? C5 C4 C6 117.9(9) . . ? N1 C5 C4 123.2(7) . . ? N1 C5 C9 117.3(6) . . ? C4 C5 C9 119.4(7) . . ? C7 C6 C4 121.6(9) . . ? C6 C7 C8 122.3(9) . . ? C10 C8 C9 116.9(8) . . ? C10 C8 C7 124.5(9) . . ? C9 C8 C7 118.6(9) . . ? N2 C9 C8 124.1(7) . . ? N2 C9 C5 115.7(6) . . ? C8 C9 C5 120.2(7) . . ? C11 C10 C8 120.0(8) . . ? C10 C11 C12 119.5(9) . . ? N2 C12 C11 122.5(8) . . ? N3 C13 C14 122.7(6) . . ? C15 C14 C13 119.7(6) . . ? C14 C15 C16 119.5(6) . . ? C15 C16 C17 117.8(6) . . ? C15 C16 C18 123.5(6) . . ? C17 C16 C18 118.6(6) . . ? N3 C17 C16 122.6(6) . . ? N3 C17 C21 116.8(5) . . ? C16 C17 C21 120.5(6) . . ? C19 C18 C16 120.5(7) . . ? C18 C19 C20 121.5(7) . . ? C21 C20 C22 118.0(6) . . ? C21 C20 C19 119.5(6) . . ? C22 C20 C19 122.5(7) . . ? N4 C21 C20 122.8(6) . . ? N4 C21 C17 117.9(6) . . ? C20 C21 C17 119.3(6) . . ? C23 C22 C20 118.4(7) . . ? C22 C23 C24 119.8(7) . . ? N4 C24 C23 123.2(6) . . ? C1 N1 C5 117.9(6) . . ? C1 N1 Co1 127.4(5) . . ? C5 N1 Co1 113.8(4) . . ? C12 N2 C9 116.9(6) . . ? C12 N2 Co1 128.3(5) . . ? C9 N2 Co1 113.8(5) . . ? C13 N3 C17 117.5(5) . . ? C13 N3 Co1 128.7(4) . . ? C17 N3 Co1 113.7(4) . . ? C24 N4 C21 117.8(6) . . ? C24 N4 Co1 127.6(5) . . ? C21 N4 Co1 114.6(4) . . ? _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 26.91 _diffrn_measured_fraction_theta_full 0.911 _refine_diff_density_max 1.063 _refine_diff_density_min -1.187 _refine_diff_density_rms 0.140 #===========================================END data_complex_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H76 Cu4 N16 O35 V10' _chemical_formula_weight 2777.29 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 monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.726(3) _cell_length_b 14.612(3) _cell_length_c 25.310(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.81(3) _cell_angle_gamma 90.00 _cell_volume 5240.1(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 30 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.760 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2780 _exptl_absorpt_coefficient_mu 1.730 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.745 _exptl_absorpt_correction_T_max 0.917 _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 'Bruker CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37028 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_sigmaI/netI 0.0702 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.93 _diffrn_reflns_theta_max 30.05 _reflns_number_total 15179 _reflns_number_gt 8042 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT+(Bruker,1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V.5.0 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0776P)^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 0.00000(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 15179 _refine_ls_number_parameters 755 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1093 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.1547 _refine_ls_wR_factor_gt 0.1324 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.956 _refine_ls_shift/su_max 0.091 _refine_ls_shift/su_mean 0.002 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.64500(3) 0.70374(3) 0.109646(17) 0.03439(12) Uani 1 d . . . Cu2 Cu 1.37368(3) 0.87057(3) 0.330137(18) 0.04040(13) Uani 1 d . . . V1 V 0.94571(5) 0.74707(9) 0.28479(4) 0.0841(4) Uani 1 d . . . V2 V 1.16612(5) 0.78092(6) 0.26746(3) 0.0521(2) Uani 1 d . . . V3 V 1.05478(5) 0.87767(6) 0.14673(3) 0.0518(2) Uani 1 d . . . V4 V 0.83769(4) 0.82050(5) 0.16094(2) 0.03720(16) Uani 1 d . . . V5 V 1.09751(4) 0.92528(5) 0.02434(3) 0.04173(17) Uani 1 d . . . O1 O 1.0665(2) 0.7716(3) 0.29195(12) 0.0733(10) Uani 1 d U . . O2 O 0.8692(2) 0.8165(2) 0.23314(11) 0.0553(8) Uani 1 d . . . O3 O 0.9170(8) 0.7114(17) 0.3304(5) 0.179(9) Uani 0.50 d PU . . O3' O 0.9260(9) 0.7824(12) 0.3464(4) 0.126(6) Uani 0.50 d PU . . O4 O 0.9185(7) 0.6436(6) 0.2754(6) 0.115(5) Uani 0.50 d PU . . O4' O 0.9487(9) 0.6437(12) 0.2409(9) 0.200(10) Uani 0.50 d PU . . O5 O 1.1352(2) 0.8062(3) 0.19562(12) 0.0819(11) Uani 1 d U . . O6 O 1.2368(2) 0.8610(2) 0.30259(12) 0.0609(8) Uani 1 d . . . O7 O 1.2257(3) 0.6853(3) 0.27570(18) 0.0927(13) Uani 1 d . . . O8 O 0.9411(2) 0.8335(3) 0.13648(13) 0.0717(10) Uani 1 d . . . O9 O 1.0627(3) 0.9772(3) 0.1685(2) 0.1258(19) Uani 1 d . . . O10 O 1.0872(2) 0.86948(19) 0.08688(11) 0.0521(7) Uani 1 d . . . O11 O 0.78133(17) 0.72461(18) 0.13466(11) 0.0449(6) Uani 1 d . . . O12 O 0.7670(2) 0.9054(2) 0.14117(12) 0.0633(8) Uani 1 d . . . O13 O 1.1040(3) 0.8473(3) -0.01897(15) 0.0919(12) Uani 1 d . . . O14 O 1.1953(2) 0.9819(2) 0.03734(18) 0.0885(13) Uani 1 d . . . O15 O 1.0000 1.0000 0.0000 0.0718(14) Uani 1 d S . . N1 N 0.5114(2) 0.7503(2) 0.10394(12) 0.0363(7) Uani 1 d . . . N2 N 0.6348(2) 0.6600(2) 0.18239(12) 0.0380(7) Uani 1 d . . . N3 N 0.6420(2) 0.7379(2) 0.03318(12) 0.0367(7) Uani 1 d . . . N4 N 0.6294(2) 0.5670(2) 0.07189(13) 0.0424(7) Uani 1 d . . . N5 N 1.3835(2) 0.9253(2) 0.25942(12) 0.0410(7) Uani 1 d . . . N6 N 1.5090(2) 0.8315(2) 0.33538(13) 0.0428(7) Uani 1 d . . . N7 N 1.3802(2) 0.9925(2) 0.38068(13) 0.0439(8) Uani 1 d . . . N8 N 1.3736(2) 0.8137(2) 0.40210(15) 0.0472(8) Uani 1 d . . . C1 C 0.4522(3) 0.7995(3) 0.06475(17) 0.0467(9) Uani 1 d . . . H1A H 0.4729 0.8202 0.0339 0.080 Uiso 1 d R . . C2 C 0.3601(3) 0.8199(3) 0.0676(2) 0.0595(12) Uani 1 d . . . H2A H 0.3200 0.8580 0.0400 0.080 Uiso 1 d R . . C3 C 0.3292(3) 0.7875(3) 0.1091(2) 0.0587(12) Uani 1 d . . . H3A H 0.2658 0.8001 0.1101 0.080 Uiso 1 d R . . C4 C 0.3887(3) 0.7343(3) 0.15109(18) 0.0466(10) Uani 1 d . . . C5 C 0.4806(3) 0.7194(2) 0.14675(15) 0.0365(8) Uani 1 d . . . C6 C 0.3629(3) 0.6965(3) 0.1967(2) 0.0592(12) Uani 1 d . . . H6A H 0.3002 0.7059 0.2000 0.080 Uiso 1 d R . . C7 C 0.4246(3) 0.6479(3) 0.2353(2) 0.0600(12) Uani 1 d . . . H7A H 0.4048 0.6225 0.2654 0.080 Uiso 1 d R . . C8 C 0.5198(3) 0.6319(3) 0.23317(17) 0.0467(10) Uani 1 d . . . C9 C 0.5466(2) 0.6693(2) 0.18854(15) 0.0353(8) Uani 1 d . . . C10 C 0.5894(4) 0.5855(3) 0.27259(18) 0.0591(12) Uani 1 d . . . H10A H 0.5745 0.5597 0.3041 0.080 Uiso 1 d R . . C11 C 0.6784(3) 0.5778(3) 0.26679(18) 0.0564(11) Uani 1 d . . . H11A H 0.7263 0.5465 0.2942 0.080 Uiso 1 d R . . C12 C 0.7001(3) 0.6164(3) 0.22132(16) 0.0474(10) Uani 1 d . . . H12A H 0.7628 0.6101 0.2173 0.080 Uiso 1 d R . . C13 C 0.6497(3) 0.8223(3) 0.01554(16) 0.0466(9) Uani 1 d . . . H13A H 0.6566 0.8721 0.0411 0.080 Uiso 1 d R . . C14 C 0.6485(3) 0.8406(3) -0.03906(18) 0.0561(11) Uani 1 d . . . H14A H 0.6539 0.9024 -0.0508 0.080 Uiso 1 d R . . C15 C 0.6396(3) 0.7716(4) -0.07471(18) 0.0608(13) Uani 1 d . . . H15A H 0.6365 0.7842 -0.1124 0.080 Uiso 1 d R . . C16 C 0.6335(3) 0.6809(3) -0.05780(16) 0.0506(11) Uani 1 d . . . C17 C 0.6339(2) 0.6676(3) -0.00238(15) 0.0400(9) Uani 1 d . . . C18 C 0.6279(3) 0.6034(4) -0.09249(19) 0.0669(14) Uani 1 d . . . H18A H 0.6258 0.6123 -0.1304 0.080 Uiso 1 d R . . C19 C 0.6244(3) 0.5177(4) -0.0729(2) 0.0663(14) Uani 1 d . . . H19A H 0.6225 0.4666 -0.0970 0.080 Uiso 1 d R . . C20 C 0.6243(3) 0.5020(3) -0.01736(19) 0.0536(11) Uani 1 d . . . C21 C 0.6288(2) 0.5766(3) 0.01810(15) 0.0407(9) Uani 1 d . . . C22 C 0.6201(3) 0.4160(4) 0.0055(2) 0.0699(14) Uani 1 d . . . H22A H 0.6173 0.3627 -0.0172 0.080 Uiso 1 d R . . C23 C 0.6193(3) 0.4055(3) 0.0591(3) 0.0710(15) Uani 1 d . . . H23A H 0.6161 0.3457 0.0743 0.080 Uiso 1 d R . . C24 C 0.6236(3) 0.4846(3) 0.0912(2) 0.0541(11) Uani 1 d . . . H24A H 0.6218 0.4783 0.1286 0.080 Uiso 1 d R . . C25 C 1.3184(3) 0.9702(3) 0.22209(18) 0.0508(10) Uani 1 d . . . H25A H 1.2567 0.9781 0.2274 0.080 Uiso 1 d R . . C26 C 1.3369(4) 1.0064(3) 0.17508(18) 0.0605(12) Uani 1 d . . . H26A H 1.2883 1.0385 0.1485 0.080 Uiso 1 d R . . C27 C 1.4233(4) 0.9961(3) 0.16652(19) 0.0585(12) Uani 1 d . . . H27A H 1.4361 1.0212 0.1342 0.080 Uiso 1 d R . . C28 C 1.4946(3) 0.9488(3) 0.20540(17) 0.0499(10) Uani 1 d . . . C29 C 1.4710(3) 0.9142(3) 0.25133(16) 0.0399(8) Uani 1 d . . . C30 C 1.5884(4) 0.9330(3) 0.2008(2) 0.0607(12) Uani 1 d . . . H30A H 1.6053 0.9556 0.1692 0.080 Uiso 1 d R . . C31 C 1.6526(3) 0.8870(3) 0.2403(2) 0.0596(12) Uani 1 d . . . H31A H 1.7154 0.8785 0.2368 0.080 Uiso 1 d R . . C32 C 1.6299(3) 0.8504(3) 0.28716(18) 0.0482(10) Uani 1 d . . . C33 C 1.5379(3) 0.8647(3) 0.29234(16) 0.0416(9) Uani 1 d . . . C34 C 1.6918(3) 0.8017(3) 0.3287(2) 0.0638(13) Uani 1 d . . . H34A H 1.7555 0.7915 0.3272 0.080 Uiso 1 d R . . C35 C 1.6623(3) 0.7685(4) 0.3712(2) 0.0686(14) Uani 1 d . . . H35A H 1.7052 0.7346 0.3998 0.080 Uiso 1 d R . . C36 C 1.5705(3) 0.7848(3) 0.37362(18) 0.0532(11) Uani 1 d . . . H36A H 1.5506 0.7607 0.4039 0.080 Uiso 1 d R . . C37 C 1.3819(3) 1.0808(3) 0.3703(2) 0.0655(13) Uani 1 d . . . H37A H 1.3830 1.1003 0.3343 0.080 Uiso 1 d R . . C38 C 1.3801(4) 1.1481(4) 0.4102(4) 0.089(2) Uani 1 d . . . H38A H 1.3818 1.2120 0.4015 0.080 Uiso 1 d R . . C39 C 1.3769(4) 1.1226(5) 0.4601(3) 0.0877(19) Uani 1 d . . . H39A H 1.3755 1.1681 0.4873 0.080 Uiso 1 d R . . C40 C 1.3767(3) 1.0326(4) 0.4737(2) 0.0636(13) Uani 1 d . . . C41 C 1.3777(3) 0.9684(3) 0.43220(16) 0.0439(9) Uani 1 d . . . C42 C 1.3762(4) 0.9988(6) 0.5262(3) 0.098(2) Uani 1 d . . . H42A H 1.3759 1.0410 0.5552 0.080 Uiso 1 d R . . C43 C 1.3775(4) 0.9109(7) 0.5370(2) 0.095(2) Uani 1 d . . . H43A H 1.3790 0.8910 0.5734 0.080 Uiso 1 d R . . C44 C 1.3768(3) 0.8436(4) 0.4974(2) 0.0700(15) Uani 1 d . . . C45 C 1.3770(3) 0.8736(3) 0.44364(16) 0.0462(10) Uani 1 d . . . C46 C 1.3771(4) 0.7495(7) 0.5052(3) 0.106(3) Uani 1 d . . . H46A H 1.3785 0.7272 0.5411 0.080 Uiso 1 d R . . C47 C 1.3740(4) 0.6909(5) 0.4643(4) 0.103(3) Uani 1 d . . . H47A H 1.3748 0.6264 0.4716 0.080 Uiso 1 d R . . C48 C 1.3720(3) 0.7237(3) 0.4117(3) 0.0731(15) Uani 1 d . . . H48A H 1.3684 0.6810 0.3824 0.080 Uiso 1 d R . . O1W O 0.9069(4) 0.6570(4) 0.43103(19) 0.141(2) Uani 1 d . . . O2W O 0.7471(4) 1.0546(3) 0.0696(2) 0.144(2) Uani 1 d . . . O3W O 1.3957(10) 0.9382(7) 0.6676(5) 0.159(6) Uani 0.50 d P . . O4W O 0.4932(9) 0.9910(7) 0.0291(5) 0.146(5) Uani 0.50 d P . . 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 0.0286(2) 0.0456(3) 0.0285(2) 0.00578(18) 0.00703(16) 0.00026(18) Cu2 0.0314(2) 0.0503(3) 0.0379(3) 0.0032(2) 0.00672(19) -0.0015(2) V1 0.0278(4) 0.1462(10) 0.0705(6) 0.0572(6) 0.0001(4) -0.0107(5) V2 0.0348(4) 0.0929(6) 0.0321(3) -0.0031(3) 0.0151(3) -0.0123(4) V3 0.0406(4) 0.0808(5) 0.0405(4) -0.0185(4) 0.0221(3) -0.0196(4) V4 0.0290(3) 0.0545(4) 0.0287(3) -0.0006(3) 0.0089(2) -0.0042(3) V5 0.0365(4) 0.0487(4) 0.0428(4) 0.0172(3) 0.0156(3) 0.0095(3) O1 0.0311(15) 0.152(3) 0.0392(16) 0.0023(18) 0.0130(12) -0.0202(18) O2 0.0456(16) 0.087(2) 0.0324(14) -0.0012(14) 0.0085(12) 0.0075(15) O3 0.040(5) 0.41(3) 0.085(9) 0.153(13) 0.022(7) -0.010(12) O3' 0.045(5) 0.308(19) 0.028(4) -0.018(7) 0.014(3) 0.025(8) O4 0.066(6) 0.059(5) 0.188(13) 0.068(7) -0.022(7) -0.028(4) O4' 0.074(8) 0.231(17) 0.27(2) 0.196(17) 0.011(9) 0.019(8) O5 0.063(2) 0.150(4) 0.0331(17) 0.0114(19) 0.0129(15) -0.013(2) O6 0.0396(16) 0.096(2) 0.0455(17) -0.0043(16) 0.0086(13) -0.0142(15) O7 0.108(3) 0.079(3) 0.111(3) 0.016(2) 0.063(3) 0.022(2) O8 0.0425(17) 0.129(3) 0.0482(18) -0.0073(19) 0.0198(14) -0.0300(18) O9 0.087(3) 0.123(4) 0.183(5) -0.094(3) 0.064(3) -0.022(3) O10 0.0575(18) 0.0642(19) 0.0436(16) 0.0182(14) 0.0292(14) 0.0138(14) O11 0.0304(13) 0.0565(17) 0.0462(16) 0.0034(13) 0.0076(11) -0.0040(12) O12 0.079(2) 0.0588(19) 0.0501(18) 0.0057(15) 0.0149(16) 0.0149(16) O13 0.116(3) 0.109(3) 0.056(2) -0.017(2) 0.033(2) 0.034(2) O14 0.0433(19) 0.068(2) 0.154(4) 0.039(2) 0.027(2) 0.0002(16) O15 0.050(3) 0.070(3) 0.089(4) 0.031(3) 0.009(2) 0.022(2) N1 0.0336(16) 0.0370(17) 0.0371(17) -0.0002(13) 0.0078(13) 0.0035(13) N2 0.0336(16) 0.0469(18) 0.0333(16) 0.0065(13) 0.0090(13) 0.0006(13) N3 0.0303(15) 0.0480(18) 0.0308(15) 0.0029(14) 0.0068(12) -0.0008(13) N4 0.0372(17) 0.0397(18) 0.048(2) 0.0011(15) 0.0086(14) -0.0019(14) N5 0.0352(17) 0.0481(19) 0.0373(17) 0.0000(14) 0.0059(13) -0.0014(14) N6 0.0354(17) 0.0504(19) 0.0411(18) 0.0024(15) 0.0076(14) 0.0010(14) N7 0.0418(18) 0.0429(19) 0.0437(19) 0.0052(15) 0.0061(14) -0.0007(14) N8 0.0345(17) 0.046(2) 0.061(2) 0.0166(17) 0.0118(15) 0.0008(14) C1 0.038(2) 0.051(2) 0.047(2) -0.0017(19) 0.0045(17) 0.0062(18) C2 0.039(2) 0.056(3) 0.074(3) 0.003(2) -0.001(2) 0.018(2) C3 0.038(2) 0.060(3) 0.078(3) -0.008(2) 0.015(2) 0.011(2) C4 0.034(2) 0.048(2) 0.061(3) -0.013(2) 0.0181(19) -0.0003(17) C5 0.0332(19) 0.035(2) 0.042(2) -0.0064(15) 0.0119(15) -0.0017(15) C6 0.041(2) 0.072(3) 0.076(3) -0.010(3) 0.035(2) -0.001(2) C7 0.059(3) 0.068(3) 0.066(3) -0.003(2) 0.039(3) -0.013(2) C8 0.049(2) 0.048(2) 0.048(2) -0.0027(19) 0.0236(19) -0.0071(19) C9 0.0327(18) 0.0375(19) 0.0378(19) -0.0041(16) 0.0131(15) -0.0034(15) C10 0.073(3) 0.062(3) 0.049(3) 0.015(2) 0.028(2) -0.006(2) C11 0.063(3) 0.061(3) 0.047(2) 0.019(2) 0.017(2) 0.010(2) C12 0.041(2) 0.061(3) 0.039(2) 0.0131(19) 0.0091(17) 0.0065(19) C13 0.045(2) 0.055(3) 0.037(2) 0.0115(18) 0.0063(17) -0.0035(19) C14 0.048(3) 0.073(3) 0.044(2) 0.019(2) 0.0065(19) -0.008(2) C15 0.048(3) 0.098(4) 0.036(2) 0.014(2) 0.0100(19) -0.015(2) C16 0.032(2) 0.082(3) 0.036(2) -0.006(2) 0.0075(16) -0.008(2) C17 0.0260(18) 0.058(2) 0.0333(19) 0.0011(17) 0.0041(14) -0.0057(16) C18 0.055(3) 0.107(4) 0.040(2) -0.016(3) 0.014(2) -0.012(3) C19 0.056(3) 0.088(4) 0.054(3) -0.038(3) 0.012(2) -0.006(3) C20 0.040(2) 0.055(3) 0.063(3) -0.016(2) 0.009(2) -0.0040(19) C21 0.0290(18) 0.051(2) 0.040(2) -0.0093(18) 0.0064(15) 0.0011(16) C22 0.055(3) 0.063(3) 0.083(4) -0.021(3) 0.003(3) -0.003(2) C23 0.054(3) 0.037(3) 0.112(5) 0.001(3) 0.004(3) -0.004(2) C24 0.050(3) 0.045(3) 0.063(3) 0.008(2) 0.007(2) -0.0056(19) C25 0.044(2) 0.053(3) 0.050(2) 0.006(2) 0.0041(19) 0.0040(19) C26 0.071(3) 0.056(3) 0.046(3) 0.008(2) 0.002(2) 0.008(2) C27 0.072(3) 0.058(3) 0.047(3) 0.004(2) 0.020(2) -0.002(2) C28 0.060(3) 0.045(2) 0.047(2) -0.0058(19) 0.019(2) -0.010(2) C29 0.038(2) 0.040(2) 0.042(2) -0.0055(16) 0.0108(16) -0.0065(16) C30 0.064(3) 0.065(3) 0.064(3) -0.008(2) 0.036(3) -0.014(2) C31 0.053(3) 0.057(3) 0.079(3) -0.013(2) 0.034(3) -0.007(2) C32 0.039(2) 0.049(2) 0.059(3) -0.010(2) 0.0175(19) -0.0040(18) C33 0.036(2) 0.041(2) 0.047(2) -0.0084(17) 0.0103(17) -0.0044(16) C34 0.034(2) 0.073(3) 0.081(4) -0.009(3) 0.011(2) 0.006(2) C35 0.047(3) 0.074(3) 0.074(3) 0.004(3) -0.001(2) 0.012(2) C36 0.040(2) 0.063(3) 0.051(3) 0.004(2) 0.0038(19) 0.004(2) C37 0.057(3) 0.042(3) 0.090(4) 0.013(2) 0.007(3) 0.003(2) C38 0.065(4) 0.042(3) 0.153(7) -0.009(4) 0.019(4) -0.003(2) C39 0.058(3) 0.082(5) 0.119(6) -0.045(4) 0.017(4) -0.004(3) C40 0.035(2) 0.094(4) 0.061(3) -0.025(3) 0.012(2) -0.004(2) C41 0.0297(19) 0.060(3) 0.040(2) -0.0049(19) 0.0048(15) -0.0050(17) C42 0.058(4) 0.179(8) 0.056(4) -0.049(4) 0.016(3) -0.017(4) C43 0.052(3) 0.203(8) 0.032(3) -0.007(4) 0.014(2) -0.019(4) C44 0.032(2) 0.120(5) 0.054(3) 0.031(3) 0.0046(19) -0.009(2) C45 0.0269(19) 0.073(3) 0.035(2) 0.013(2) 0.0036(15) -0.0043(18) C46 0.042(3) 0.174(8) 0.092(5) 0.089(5) 0.001(3) -0.010(4) C47 0.060(4) 0.094(5) 0.148(7) 0.086(5) 0.019(4) 0.003(3) C48 0.048(3) 0.054(3) 0.117(5) 0.024(3) 0.021(3) 0.000(2) O1W 0.114(4) 0.221(6) 0.083(3) 0.027(3) 0.016(3) -0.060(4) O2W 0.178(5) 0.123(4) 0.186(5) 0.075(4) 0.143(5) 0.076(4) O3W 0.269(14) 0.133(8) 0.123(8) -0.073(7) 0.132(10) -0.130(9) O4W 0.132(9) 0.075(6) 0.229(17) -0.005(8) 0.046(10) -0.017(5) _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 O11 1.957(3) . ? Cu1 N3 1.988(3) . ? Cu1 N2 1.993(3) . ? Cu1 N1 2.050(3) . ? Cu1 N4 2.200(3) . ? Cu2 O6 1.951(3) . ? Cu2 N5 2.001(3) . ? Cu2 N8 2.003(3) . ? Cu2 N6 2.042(3) . ? Cu2 N7 2.181(3) . ? V1 O3 1.432(8) . ? V1 O4 1.565(9) . ? V1 O3' 1.739(9) . ? V1 O1 1.774(3) . ? V1 O2 1.790(3) . ? V1 O4' 1.88(2) . ? V2 O7 1.633(4) . ? V2 O6 1.655(3) . ? V2 O1 1.747(3) . ? V2 O5 1.789(3) . ? V3 O9 1.549(4) . ? V3 O10 1.712(3) . ? V3 O8 1.746(3) . ? V3 O5 1.795(4) . ? V4 O12 1.610(3) . ? V4 O11 1.671(3) . ? V4 O2 1.760(3) . ? V4 O8 1.803(3) . ? V5 O13 1.602(3) . ? V5 O14 1.614(3) . ? V5 O15 1.7753(7) . ? V5 O10 1.823(3) . ? O3 O3' 1.11(3) . ? O3 O4 1.71(2) . ? O4 O4' 1.08(2) . ? O15 V5 1.7753(7) 3_775 ? N1 C1 1.337(5) . ? N1 C5 1.361(4) . ? N2 C12 1.336(5) . ? N2 C9 1.357(4) . ? N3 C13 1.327(5) . ? N3 C17 1.350(5) . ? N4 C24 1.311(5) . ? N4 C21 1.366(5) . ? N5 C25 1.323(5) . ? N5 C29 1.368(5) . ? N6 C36 1.321(5) . ? N6 C33 1.362(5) . ? N7 C37 1.317(5) . ? N7 C41 1.361(5) . ? N8 C48 1.339(5) . ? N8 C45 1.359(5) . ? C1 C2 1.410(5) . ? C2 C3 1.340(6) . ? C3 C4 1.412(6) . ? C4 C5 1.403(5) . ? C4 C6 1.422(6) . ? C5 C9 1.428(5) . ? C6 C7 1.341(7) . ? C7 C8 1.438(6) . ? C8 C10 1.396(6) . ? C8 C9 1.405(5) . ? C10 C11 1.362(6) . ? C11 C12 1.395(5) . ? C13 C14 1.403(5) . ? C14 C15 1.336(7) . ? C15 C16 1.404(6) . ? C16 C17 1.414(5) . ? C16 C18 1.421(7) . ? C17 C21 1.437(5) . ? C18 C19 1.352(7) . ? C19 C20 1.426(7) . ? C20 C22 1.392(7) . ? C20 C21 1.403(5) . ? C22 C23 1.369(7) . ? C23 C24 1.405(7) . ? C25 C26 1.395(6) . ? C26 C27 1.356(6) . ? C27 C28 1.409(6) . ? C28 C29 1.396(5) . ? C28 C30 1.436(6) . ? C29 C33 1.419(5) . ? C30 C31 1.352(7) . ? C31 C32 1.422(6) . ? C32 C34 1.387(6) . ? C32 C33 1.412(5) . ? C34 C35 1.353(7) . ? C35 C36 1.391(6) . ? C37 C38 1.414(8) . ? C38 C39 1.332(9) . ? C39 C40 1.359(8) . ? C40 C41 1.411(6) . ? C40 C42 1.420(8) . ? C41 C45 1.415(6) . ? C42 C43 1.312(9) . ? C43 C44 1.403(9) . ? C44 C46 1.389(10) . ? C44 C45 1.429(6) . ? C46 C47 1.335(10) . ? C47 C48 1.406(9) . ? O4W O4W 1.56(2) 3_675 ? 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 Cu1 N3 91.40(12) . . ? O11 Cu1 N2 94.58(12) . . ? N3 Cu1 N2 173.18(12) . . ? O11 Cu1 N1 148.36(12) . . ? N3 Cu1 N1 94.68(12) . . ? N2 Cu1 N1 81.92(12) . . ? O11 Cu1 N4 104.97(11) . . ? N3 Cu1 N4 80.41(13) . . ? N2 Cu1 N4 94.86(13) . . ? N1 Cu1 N4 106.66(12) . . ? O6 Cu2 N5 91.63(13) . . ? O6 Cu2 N8 92.21(13) . . ? N5 Cu2 N8 175.95(13) . . ? O6 Cu2 N6 153.97(13) . . ? N5 Cu2 N6 82.12(13) . . ? N8 Cu2 N6 93.86(13) . . ? O6 Cu2 N7 98.29(13) . . ? N5 Cu2 N7 101.29(12) . . ? N8 Cu2 N7 79.43(13) . . ? N6 Cu2 N7 107.70(13) . . ? O3 V1 O4 69.5(9) . . ? O3 V1 O3' 39.4(10) . . ? O4 V1 O3' 108.9(8) . . ? O3 V1 O1 119.9(5) . . ? O4 V1 O1 114.7(5) . . ? O3' V1 O1 104.8(4) . . ? O3 V1 O2 122.0(6) . . ? O4 V1 O2 110.7(4) . . ? O3' V1 O2 105.1(5) . . ? O1 V1 O2 111.97(15) . . ? O3 V1 O4' 104.1(10) . . ? O4 V1 O4' 35.1(5) . . ? O3' V1 O4' 143.4(7) . . ? O1 V1 O4' 92.2(4) . . ? O2 V1 O4' 97.7(4) . . ? O7 V2 O6 107.4(2) . . ? O7 V2 O1 111.20(19) . . ? O6 V2 O1 109.30(16) . . ? O7 V2 O5 106.6(2) . . ? O6 V2 O5 110.40(17) . . ? O1 V2 O5 111.76(15) . . ? O9 V3 O10 111.6(2) . . ? O9 V3 O8 112.1(2) . . ? O10 V3 O8 109.28(15) . . ? O9 V3 O5 109.2(3) . . ? O10 V3 O5 106.17(14) . . ? O8 V3 O5 108.24(17) . . ? O12 V4 O11 108.26(15) . . ? O12 V4 O2 108.29(15) . . ? O11 V4 O2 110.32(14) . . ? O12 V4 O8 110.33(18) . . ? O11 V4 O8 109.03(15) . . ? O2 V4 O8 110.59(14) . . ? O13 V5 O14 106.7(2) . . ? O13 V5 O15 113.18(15) . . ? O14 V5 O15 110.35(12) . . ? O13 V5 O10 108.09(18) . . ? O14 V5 O10 109.42(18) . . ? O15 V5 O10 109.01(9) . . ? V2 O1 V1 153.5(2) . . ? V4 O2 V1 135.46(18) . . ? O3' O3 V1 85.4(13) . . ? O3' O3 O4 144.1(12) . . ? V1 O3 O4 58.9(6) . . ? O3 O3' V1 55.1(6) . . ? O4' O4 V1 88.7(12) . . ? O4' O4 O3 138.9(15) . . ? V1 O4 O3 51.6(5) . . ? O4 O4' V1 56.2(13) . . ? V2 O5 V3 139.3(2) . . ? V2 O6 Cu2 132.82(19) . . ? V3 O8 V4 148.5(2) . . ? V3 O10 V5 147.79(17) . . ? V4 O11 Cu1 127.86(15) . . ? V5 O15 V5 180.0 3_775 . ? C1 N1 C5 118.5(3) . . ? C1 N1 Cu1 130.5(3) . . ? C5 N1 Cu1 110.8(2) . . ? C12 N2 C9 118.9(3) . . ? C12 N2 Cu1 127.9(3) . . ? C9 N2 Cu1 112.9(2) . . ? C13 N3 C17 118.9(3) . . ? C13 N3 Cu1 125.5(3) . . ? C17 N3 Cu1 115.6(2) . . ? C24 N4 C21 118.9(4) . . ? C24 N4 Cu1 133.0(3) . . ? C21 N4 Cu1 108.1(2) . . ? C25 N5 C29 118.8(3) . . ? C25 N5 Cu2 128.5(3) . . ? C29 N5 Cu2 112.8(2) . . ? C36 N6 C33 118.0(3) . . ? C36 N6 Cu2 130.9(3) . . ? C33 N6 Cu2 111.1(2) . . ? C37 N7 C41 116.8(4) . . ? C37 N7 Cu2 133.1(3) . . ? C41 N7 Cu2 110.0(3) . . ? C48 N8 C45 119.4(4) . . ? C48 N8 Cu2 125.3(4) . . ? C45 N8 Cu2 115.3(3) . . ? N1 C1 C2 121.2(4) . . ? C3 C2 C1 120.1(4) . . ? C2 C3 C4 120.8(4) . . ? C5 C4 C3 116.1(4) . . ? C5 C4 C6 118.7(4) . . ? C3 C4 C6 125.2(4) . . ? N1 C5 C4 123.2(3) . . ? N1 C5 C9 116.9(3) . . ? C4 C5 C9 119.9(3) . . ? C7 C6 C4 121.3(4) . . ? C6 C7 C8 122.2(4) . . ? C10 C8 C9 116.8(4) . . ? C10 C8 C7 125.9(4) . . ? C9 C8 C7 117.2(4) . . ? N2 C9 C8 122.7(3) . . ? N2 C9 C5 116.5(3) . . ? C8 C9 C5 120.7(3) . . ? C11 C10 C8 120.2(4) . . ? C10 C11 C12 120.0(4) . . ? N2 C12 C11 121.3(4) . . ? N3 C13 C14 122.0(4) . . ? C15 C14 C13 119.6(4) . . ? C14 C15 C16 120.7(4) . . ? C15 C16 C17 116.6(4) . . ? C15 C16 C18 124.2(4) . . ? C17 C16 C18 119.2(4) . . ? N3 C17 C16 122.2(4) . . ? N3 C17 C21 117.9(3) . . ? C16 C17 C21 119.9(4) . . ? C19 C18 C16 120.8(4) . . ? C18 C19 C20 121.4(4) . . ? C22 C20 C21 115.9(4) . . ? C22 C20 C19 124.6(5) . . ? C21 C20 C19 119.6(4) . . ? N4 C21 C20 123.0(4) . . ? N4 C21 C17 117.9(3) . . ? C20 C21 C17 119.1(4) . . ? C23 C22 C20 121.7(5) . . ? C22 C23 C24 118.0(5) . . ? N4 C24 C23 122.5(5) . . ? N5 C25 C26 121.7(4) . . ? C27 C26 C25 120.3(4) . . ? C26 C27 C28 119.7(4) . . ? C29 C28 C27 116.9(4) . . ? C29 C28 C30 118.2(4) . . ? C27 C28 C30 124.9(4) . . ? N5 C29 C28 122.7(4) . . ? N5 C29 C33 116.5(3) . . ? C28 C29 C33 120.9(4) . . ? C31 C30 C28 121.0(4) . . ? C30 C31 C32 121.8(4) . . ? C34 C32 C33 117.0(4) . . ? C34 C32 C31 124.8(4) . . ? C33 C32 C31 118.1(4) . . ? N6 C33 C32 122.6(4) . . ? N6 C33 C29 117.4(3) . . ? C32 C33 C29 120.0(4) . . ? C35 C34 C32 119.9(4) . . ? C34 C35 C36 120.1(5) . . ? N6 C36 C35 122.4(4) . . ? N7 C37 C38 122.3(5) . . ? C39 C38 C37 119.7(5) . . ? C38 C39 C40 120.9(6) . . ? C39 C40 C41 117.1(5) . . ? C39 C40 C42 125.0(6) . . ? C41 C40 C42 117.9(6) . . ? N7 C41 C40 123.3(4) . . ? N7 C41 C45 117.0(4) . . ? C40 C41 C45 119.8(4) . . ? C43 C42 C40 122.1(6) . . ? C42 C43 C44 122.7(6) . . ? C46 C44 C43 126.3(6) . . ? C46 C44 C45 116.1(6) . . ? C43 C44 C45 117.6(6) . . ? N8 C45 C41 118.2(3) . . ? N8 C45 C44 121.9(4) . . ? C41 C45 C44 119.8(4) . . ? C47 C46 C44 121.7(6) . . ? C46 C47 C48 120.2(6) . . ? N8 C48 C47 120.6(6) . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 1.873 _refine_diff_density_min -1.489 _refine_diff_density_rms 0.091 #_eof #End of Crystallographic Information File