############################################################################## ### ### ### Electronic paper (Acta Crystallographica Section E) ### ### ### ############################################################################## # # # This CIF contains the data in a paper accepted for publication in Acta # # Crystallographica Section E. It conforms to the requirements of Notes # # for Authors for Section E, and has been peer reviewed under the auspices # # of the IUCr Commission on Journals. # # # # Full details of the Crystallographic Information File format # # are given in the paper "The Crystallographic Information File (CIF): # # a New Standard Archive File for Crystallography" by S. R. Hall, F. H. # # Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. # # # # The current version of the core CIF dictionary is obtainable from # # ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.1. # # # # Software is freely available for graphical display of the structure(s) in # # this CIF. For information consult the CIF home page http://www.iucr.org/ # # cif/home.html # # # ############################################################################## data_I _audit_creation_method SHELXL-97 _chemical_name_systematic ; poly[bis(2,2'-bipyridine-\k^2^N,N')deca-\m-oxido- dioxidodicopper(II)tetravanadium(V)], ; _chemical_name_common ? _chemical_formula_moiety 'C10 H8 Cu N2 O6 V2' _chemical_formula_sum 'C10 H8 Cu N2 O6 V2' _chemical_formula_iupac '[Cu2 V4 O12 (C10 H8 N2)2]' _chemical_formula_weight 417.60 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.1019(4) _cell_length_b 8.3122(5) _cell_length_c 10.3501(4) _cell_angle_alpha 72.332(3) _cell_angle_beta 84.562(3) _cell_angle_gamma 77.878(3) _cell_volume 648.98(6) _cell_formula_units_Z 2 _cell_measurement_reflns_used 3811 _cell_measurement_theta_min 2.07 _cell_measurement_theta_max 28.25 _cell_measurement_temperature 298(2) _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 2.137 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 410 _exptl_absorpt_coefficient_mu 3.061 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 2002)' _exptl_absorpt_correction_T_min 0.379 _exptl_absorpt_correction_T_max 0.469 _diffrn_ambient_temperature 298(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method '\f and \w' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 4603 _diffrn_reflns_av_R_equivalents 0.0548 _diffrn_reflns_av_sigmaI/netI 0.0577 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 28.25 _diffrn_reflns_theta_full 28.25 _diffrn_measured_fraction_theta_max 0.972 _diffrn_measured_fraction_theta_full 0.972 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _reflns_number_total 3114 _reflns_number_gt 2553 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0442 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_gt 0.0793 _refine_ls_wR_factor_ref 0.0836 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.990 _refine_ls_number_reflns 3114 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0438P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.532 _refine_diff_density_min -0.753 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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' _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2002)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu1 0.59216(4) 0.14236(4) 0.28662(3) 0.01368(10) Uani d . 1 . . V V1 0.87679(6) 0.39002(6) 0.34998(5) 0.01604(12) Uani d . 1 . . V V2 0.73879(6) 0.72867(6) 0.47736(5) 0.01495(12) Uani d . 1 . . O O1 0.7741(3) 0.2421(3) 0.3367(2) 0.0249(5) Uani d . 1 . . O O2 0.9198(3) 0.5062(3) 0.1993(2) 0.0359(6) Uani d . 1 . . O O3 0.7425(3) 0.5317(3) 0.4394(2) 0.0259(5) Uani d . 1 . . O O4 0.5705(3) 0.7685(3) 0.5748(2) 0.0270(5) Uani d . 1 . . O O5 0.9278(3) 0.7084(3) 0.5595(2) 0.0285(5) Uani d . 1 . . O O6 0.7286(3) 0.8942(3) 0.3363(2) 0.0247(5) Uani d . 1 . . N N1 0.5900(3) 0.2590(3) 0.0777(2) 0.0191(5) Uani d . 1 . . N N2 0.3794(3) 0.0700(3) 0.2320(2) 0.0202(5) Uani d . 1 . . C C1 0.7065(4) 0.3461(4) 0.0041(3) 0.0242(6) Uani d . 1 . . H H1 0.7903 0.3671 0.0489 0.029 Uiso calc R 1 . . C C2 0.7057(4) 0.4056(4) -0.1364(3) 0.0300(7) Uani d . 1 . . H H2 0.7869 0.4667 -0.1848 0.036 Uiso calc R 1 . . C C3 0.5828(4) 0.3731(4) -0.2037(3) 0.0270(7) Uani d . 1 . . H H3 0.5811 0.4107 -0.2980 0.032 Uiso calc R 1 . . C C4 0.4620(4) 0.2835(4) -0.1289(3) 0.0232(6) Uani d . 1 . . H H4 0.3787 0.2594 -0.1722 0.028 Uiso calc R 1 . . C C5 0.4675(4) 0.2303(4) 0.0120(3) 0.0192(6) Uani d . 1 . . C C6 0.3397(4) 0.1390(4) 0.1003(3) 0.0187(6) Uani d . 1 . . C C7 0.1878(4) 0.1270(4) 0.0534(3) 0.0288(7) Uani d . 1 . . H H7 0.1610 0.1775 -0.0372 0.035 Uiso calc R 1 . . C C8 0.0781(4) 0.0386(4) 0.1448(4) 0.0309(7) Uani d . 1 . . H H8 -0.0237 0.0290 0.1160 0.037 Uiso calc R 1 . . C C9 0.1209(4) -0.0351(4) 0.2786(3) 0.0274(7) Uani d . 1 . . H H9 0.0492 -0.0962 0.3409 0.033 Uiso calc R 1 . . C C10 0.2718(4) -0.0166(4) 0.3187(3) 0.0247(6) Uani d . 1 . . H H10 0.3001 -0.0660 0.4091 0.030 Uiso calc R 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu1 0.01353(17) 0.01631(18) 0.01260(17) -0.00306(12) -0.00204(12) -0.00563(13) V1 0.0140(2) 0.0172(2) 0.0183(2) -0.00322(18) -0.00335(18) -0.00613(19) V2 0.0127(2) 0.0155(2) 0.0177(2) -0.00107(17) -0.00215(18) -0.00696(18) O1 0.0202(11) 0.0282(12) 0.0335(12) -0.0079(9) -0.0034(9) -0.0167(10) O2 0.0332(14) 0.0428(14) 0.0249(12) -0.0122(11) -0.0004(10) 0.0031(11) O3 0.0243(12) 0.0225(11) 0.0346(13) -0.0036(9) 0.0016(10) -0.0154(10) O4 0.0201(11) 0.0366(13) 0.0301(12) -0.0050(9) 0.0047(9) -0.0201(10) O5 0.0228(12) 0.0308(12) 0.0346(13) -0.0013(9) -0.0112(10) -0.0128(10) O6 0.0245(11) 0.0204(11) 0.0266(11) -0.0018(9) -0.0051(9) -0.0034(9) N1 0.0195(12) 0.0206(12) 0.0179(12) -0.0040(10) -0.0029(10) -0.0059(10) N2 0.0225(13) 0.0233(13) 0.0178(12) -0.0065(10) -0.0011(10) -0.0088(10) C1 0.0211(15) 0.0252(16) 0.0269(16) -0.0057(12) -0.0012(12) -0.0077(13) C2 0.0264(17) 0.0326(18) 0.0299(17) -0.0117(14) 0.0065(14) -0.0058(14) C3 0.0328(18) 0.0269(16) 0.0177(15) -0.0036(13) -0.0008(13) -0.0027(12) C4 0.0261(16) 0.0256(16) 0.0199(15) -0.0037(12) -0.0050(12) -0.0090(12) C5 0.0181(14) 0.0190(14) 0.0211(14) -0.0013(11) -0.0044(11) -0.0072(11) C6 0.0188(14) 0.0207(14) 0.0188(14) -0.0048(11) -0.0023(11) -0.0078(11) C7 0.0270(17) 0.0350(18) 0.0252(16) -0.0084(14) -0.0101(13) -0.0056(14) C8 0.0204(16) 0.0381(19) 0.0376(19) -0.0095(14) -0.0062(14) -0.0118(15) C9 0.0242(16) 0.0299(17) 0.0318(18) -0.0129(13) 0.0058(13) -0.0110(14) C10 0.0263(17) 0.0295(17) 0.0192(14) -0.0094(13) 0.0023(12) -0.0065(12) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cu1 O1 . 2.012(2) y Cu1 O4 2_666 2.054(2) y Cu1 O6 1_545 2.061(2) y Cu1 N1 . 2.084(2) y Cu1 N2 . 2.117(2) y V1 O2 . 1.615(2) y V1 O1 . 1.667(2) y V1 O5 2_766 1.824(2) y V1 O3 . 1.833(2) y V2 O4 . 1.655(2) y V2 O6 . 1.670(2) y V2 O5 . 1.774(2) y V2 O3 . 1.790(2) y O4 Cu1 2_666 2.054(2) ? O5 V1 2_766 1.824(2) ? O6 Cu1 1_565 2.061(2) ? N1 C1 . 1.346(4) ? N1 C5 . 1.352(4) ? N2 C10 . 1.344(4) ? N2 C6 . 1.350(4) ? C1 C2 . 1.387(4) ? C1 H1 . 0.9300 ? C2 C3 . 1.381(5) ? C2 H2 . 0.9300 ? C3 C4 . 1.388(5) ? C3 H3 . 0.9300 ? C4 C5 . 1.392(4) ? C4 H4 . 0.9300 ? C5 C6 . 1.488(4) ? C6 C7 . 1.397(4) ? C7 C8 . 1.384(5) ? C7 H7 . 0.9300 ? C8 C9 . 1.379(5) ? C8 H8 . 0.9300 ? C9 C10 . 1.379(4) ? C9 H9 . 0.9300 ? C10 H10 . 0.9300 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Cu1 O4 . 2_666 89.62(9) y O1 Cu1 O6 . 1_545 94.53(9) y O4 Cu1 O6 2_666 1_545 121.32(9) y O1 Cu1 N1 . . 100.17(9) y O4 Cu1 N1 2_666 . 124.55(9) y O6 Cu1 N1 1_545 . 112.18(9) y O1 Cu1 N2 . . 172.29(9) y O4 Cu1 N2 2_666 . 85.25(9) y O6 Cu1 N2 1_545 . 93.05(9) y N1 Cu1 N2 . . 78.18(10) y O2 V1 O1 . . 108.65(12) y O2 V1 O5 . 2_766 109.43(12) y O1 V1 O5 . 2_766 111.53(11) y O2 V1 O3 . . 107.98(12) y O1 V1 O3 . . 110.08(11) y O5 V1 O3 2_766 . 109.09(10) y O4 V2 O6 . . 107.88(11) ? O4 V2 O5 . . 111.20(11) ? O6 V2 O5 . . 108.55(11) ? O4 V2 O3 . . 109.63(11) ? O6 V2 O3 . . 111.29(11) ? O5 V2 O3 . . 108.30(10) ? V1 O1 Cu1 . . 159.01(14) ? V2 O3 V1 . . 139.64(14) ? V2 O4 Cu1 . 2_666 162.64(14) ? V2 O5 V1 . 2_766 160.20(14) ? V2 O6 Cu1 . 1_565 133.16(13) ? C1 N1 C5 . . 118.7(3) ? C1 N1 Cu1 . . 125.5(2) ? C5 N1 Cu1 . . 115.6(2) ? C10 N2 C6 . . 118.8(3) ? C10 N2 Cu1 . . 125.7(2) ? C6 N2 Cu1 . . 114.9(2) ? N1 C1 C2 . . 122.1(3) ? N1 C1 H1 . . 118.9 ? C2 C1 H1 . . 118.9 ? C3 C2 C1 . . 119.2(3) ? C3 C2 H2 . . 120.4 ? C1 C2 H2 . . 120.4 ? C2 C3 C4 . . 119.1(3) ? C2 C3 H3 . . 120.4 ? C4 C3 H3 . . 120.4 ? C3 C4 C5 . . 118.9(3) ? C3 C4 H4 . . 120.6 ? C5 C4 H4 . . 120.6 ? N1 C5 C4 . . 121.9(3) ? N1 C5 C6 . . 115.6(3) ? C4 C5 C6 . . 122.5(3) ? N2 C6 C7 . . 121.6(3) ? N2 C6 C5 . . 114.8(2) ? C7 C6 C5 . . 123.6(3) ? C8 C7 C6 . . 118.6(3) ? C8 C7 H7 . . 120.7 ? C6 C7 H7 . . 120.7 ? C9 C8 C7 . . 119.6(3) ? C9 C8 H8 . . 120.2 ? C7 C8 H8 . . 120.2 ? C8 C9 C10 . . 118.9(3) ? C8 C9 H9 . . 120.6 ? C10 C9 H9 . . 120.6 ? N2 C10 C9 . . 122.5(3) ? N2 C10 H10 . . 118.7 ? C9 C10 H10 . . 118.7 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag O2 V1 O1 Cu1 . . . . -60.3(4) ? O5 V1 O1 Cu1 2_766 . . . 179.0(4) ? O3 V1 O1 Cu1 . . . . 57.8(4) ? O4 Cu1 O1 V1 2_666 . . . -68.8(4) ? O6 Cu1 O1 V1 1_545 . . . 169.8(4) ? N1 Cu1 O1 V1 . . . . 56.3(4) ? O4 V2 O3 V1 . . . . -176.89(19) ? O6 V2 O3 V1 . . . . 63.8(2) ? O5 V2 O3 V1 . . . . -55.4(2) ? O2 V1 O3 V2 . . . . -51.5(2) ? O1 V1 O3 V2 . . . . -169.94(19) ? O5 V1 O3 V2 2_766 . . . 67.4(2) ? O6 V2 O4 Cu1 . . . 2_666 -84.8(5) ? O5 V2 O4 Cu1 . . . 2_666 34.1(5) ? O3 V2 O4 Cu1 . . . 2_666 153.8(4) ? O4 V2 O5 V1 . . . 2_766 104.6(4) ? O6 V2 O5 V1 . . . 2_766 -136.9(4) ? O3 V2 O5 V1 . . . 2_766 -15.9(5) ? O4 V2 O6 Cu1 . . . 1_565 17.23(19) ? O5 V2 O6 Cu1 . . . 1_565 -103.38(17) ? O3 V2 O6 Cu1 . . . 1_565 137.53(15) ? O1 Cu1 N1 C1 . . . . 11.4(3) ? O4 Cu1 N1 C1 2_666 . . . 108.1(2) ? O6 Cu1 N1 C1 1_545 . . . -87.8(3) ? N2 Cu1 N1 C1 . . . . -176.2(3) ? O1 Cu1 N1 C5 . . . . -174.30(19) ? O4 Cu1 N1 C5 2_666 . . . -77.7(2) ? O6 Cu1 N1 C5 1_545 . . . 86.5(2) ? N2 Cu1 N1 C5 . . . . -1.97(19) ? O4 Cu1 N2 C10 2_666 . . . -48.2(3) ? O6 Cu1 N2 C10 1_545 . . . 73.0(3) ? N1 Cu1 N2 C10 . . . . -175.0(3) ? O4 Cu1 N2 C6 2_666 . . . 122.4(2) ? O6 Cu1 N2 C6 1_545 . . . -116.4(2) ? N1 Cu1 N2 C6 . . . . -4.4(2) ? C5 N1 C1 C2 . . . . -0.6(5) ? Cu1 N1 C1 C2 . . . . 173.5(2) ? N1 C1 C2 C3 . . . . -0.8(5) ? C1 C2 C3 C4 . . . . 0.8(5) ? C2 C3 C4 C5 . . . . 0.5(5) ? C1 N1 C5 C4 . . . . 2.0(4) ? Cu1 N1 C5 C4 . . . . -172.6(2) ? C1 N1 C5 C6 . . . . -177.8(3) ? Cu1 N1 C5 C6 . . . . 7.5(3) ? C3 C4 C5 N1 . . . . -2.0(4) ? C3 C4 C5 C6 . . . . 177.9(3) ? C10 N2 C6 C7 . . . . 2.1(4) ? Cu1 N2 C6 C7 . . . . -169.2(2) ? C10 N2 C6 C5 . . . . -179.3(3) ? Cu1 N2 C6 C5 . . . . 9.5(3) ? N1 C5 C6 N2 . . . . -11.3(4) ? C4 C5 C6 N2 . . . . 168.8(3) ? N1 C5 C6 C7 . . . . 167.3(3) ? C4 C5 C6 C7 . . . . -12.5(5) ? N2 C6 C7 C8 . . . . -1.5(5) ? C5 C6 C7 C8 . . . . 180.0(3) ? C6 C7 C8 C9 . . . . 0.0(5) ? C7 C8 C9 C10 . . . . 0.9(5) ? C6 N2 C10 C9 . . . . -1.2(5) ? Cu1 N2 C10 C9 . . . . 169.1(2) ? C8 C9 C10 N2 . . . . -0.3(5) ? data_global _journal_date_recd_electronic 2007-11-23 _journal_date_accepted 2007-12-21 _journal_name_full 'Acta Crystallographica, Section E' _journal_year 2008 _journal_volume 64 _journal_issue 2 _journal_page_first m287 _journal_page_last m288 _journal_paper_category QM _journal_coeditor_code HY2113 _publ_contact_author_name 'Wujiong Xia' _publ_contact_author_address ; Research Academy of Science & Technology Harbin Institute of Technology Harbin, Heilongjiang 150080 and State key Laboratory of Applied Organic Chemistry Lanzhou, Gansu 730000 People's Republic of China ; _publ_contact_author_email xiawj@hit.edu.cn _publ_contact_author_fax '+86-451-86403193' _publ_contact_author_phone '+86-451-86403193' _publ_section_title ;\ Poly[[dodecaoxidotetravanadate(V)-\k^6^O]bis[(2,2'-bipyridine-\ \k^2^N,N')copper(II)]] ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Zhang, Xiao' . ; Research Academy of Science and Technology Harbin Institute of Technology Harbin, Heilongjiang 150080 and State Key Laboratory of Applied Organic Chemistry Lanzhou, Gansu 730000 People's Republic of China ; 'Xia, Wujiong' . ; Research Academy of Science and Technology Harbin Institute of Technology Harbin, Heilongjiang 150080 and State Key Laboratory of Applied Organic Chemistry Lanzhou, Gansu 730000 People's Republic of China ; 'Xu, Xianzhu' . ; Research Academy of Science and Technology Harbin Institute of Technology Harbin, Heilongjiang 150080 and State Key Laboratory of Applied Organic Chemistry Lanzhou, Gansu 730000 People's Republic of China ; 'Yi, ZhiHui' . ; State Key Laboratory of Polymer Physics and Chemistry Changchun Institute of Applied Chemistry Graduate School of the Chinese Academy of Sciences Chinese Academy of Sciences Changchun 130022 People's Republic of China ; 'Yang, Chao' . ; Research Academy of Science and Technology Harbin Institute of Technology Harbin, Heilongjiang 150080 and State Key Laboratory of Applied Organic Chemistry Lanzhou, Gansu 730000 People's Republic of China ;