Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Soicety of Chemistry 2002 data_1 _database_code_CSD 176756 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Wang, Enbo' 'Chen, Yubiao' 'Hu, Chang-wen' 'Li, Yangguang' 'Lu, ying' 'Luan, Guoyou' 'Qin, Yeyan' 'Yao, Yuangen' 'Yuan, Mei' 'Zhang, Hong' _publ_contact_author_name 'Prof Enbo Wang' _publ_contact_author_address ; Prof Enbo Wang Faculty of Chemistry Institute of Polyoxometalate Chemistry Northeast Normal University, Renmin Changchun Jilin 130024 CHINA ; _publ_contact_author_email 'WANGENBO@PUBLIC.CC.JL.CN' _publ_section_title ; Hydrothermal synthesis and crystal structure of a layered oxovanadium phosphate with a directly coordinate organonitrogen ligand: [V4O7(HPO4)2(2,2กฏ-bipy)2] ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H18 N4 O15 P2 V4' _chemical_formula_weight 820.08 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' 'P' 'P' 0.1023 0.0942 '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' _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 8.3682(17) _cell_length_b 9.2153(18) _cell_length_c 9.5991(19) _cell_angle_alpha 97.04(3) _cell_angle_beta 109.91(3) _cell_angle_gamma 99.01(3) _cell_volume 675.0(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'column' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.364 _exptl_crystal_size_mid 0.301 _exptl_crystal_size_min 0.257 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.018 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 408 _exptl_absorpt_coefficient_mu 1.545 _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 'Rigaku R-AXIS RAPID IP diffractometer' _diffrn_measurement_method 'Oscillation scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5006 _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2863 _reflns_number_gt 2336 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID AUTO' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 2863 _refine_ls_number_parameters 238 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0534 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.1225 _refine_ls_wR_factor_gt 0.1164 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.937 _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 V1 V 0.47245(6) 0.68487(5) 0.98109(6) 0.01974(16) Uani 1 1 d . . . V2 V 0.05808(6) 0.77876(5) 0.87825(5) 0.01977(16) Uani 1 1 d . . . P1 P -0.27831(9) 0.91890(8) 0.88116(8) 0.01868(19) Uani 1 1 d . . . O1 O -0.1352(3) 0.8867(2) 0.8278(3) 0.0263(5) Uani 1 1 d . . . O2 O 0.2236(3) 0.9742(2) 0.9691(2) 0.0260(5) Uani 1 1 d . . . O3 O 0.6100(3) 0.7694(3) 0.8868(3) 0.0319(5) Uani 1 1 d . . . O4 O -0.3989(3) 0.9860(3) 0.7524(3) 0.0339(6) Uani 1 1 d . . . H1 H -0.4245 1.0596 0.7898 0.051 Uiso 1 1 calc R . . O5 O 0.2668(3) 0.6831(3) 0.8826(3) 0.0291(5) Uani 1 1 d . . . O6 O 0.5262(3) 0.7872(3) 1.1456(3) 0.0309(5) Uani 1 1 d . . . O7 O 0.5000 0.5000 1.0000 0.0376(8) Uani 1 2 d S . . O8 O 0.0330(3) 0.7120(3) 1.0171(3) 0.0341(6) Uani 1 1 d . . . N1 N -0.1224(3) 0.5954(3) 0.7128(3) 0.0226(5) Uani 1 1 d . . . N2 N 0.0698(3) 0.8112(3) 0.6516(3) 0.0228(5) Uani 1 1 d . . . C1 C -0.1533(4) 0.5907(3) 0.5654(3) 0.0233(6) Uani 1 1 d . . . C2 C -0.2787(5) 0.4779(4) 0.4541(4) 0.0345(8) Uani 1 1 d . . . H2 H -0.290(6) 0.473(5) 0.352(5) 0.044(12) Uiso 1 1 d . . . C3 C -0.3760(5) 0.3693(4) 0.4971(4) 0.0384(9) Uani 1 1 d . . . H3 H -0.462(6) 0.310(5) 0.412(5) 0.042(11) Uiso 1 1 d . . . C4 C -0.3467(5) 0.3751(4) 0.6470(5) 0.0381(8) Uani 1 1 d . . . H4 H -0.415(6) 0.302(5) 0.689(5) 0.056(13) Uiso 1 1 d . . . C5 C -0.2188(5) 0.4883(4) 0.7521(4) 0.0293(7) Uani 1 1 d . . . H5 H -0.198(5) 0.498(5) 0.870(5) 0.042(12) Uiso 1 1 d . . . C6 C -0.0441(4) 0.7105(4) 0.5292(3) 0.0236(6) Uani 1 1 d . . . C7 C -0.0508(5) 0.7226(4) 0.3844(4) 0.0329(8) Uani 1 1 d . . . H6 H -0.131(5) 0.661(4) 0.298(4) 0.030(10) Uiso 1 1 d . . . C8 C 0.0616(5) 0.8371(4) 0.3656(4) 0.0378(8) Uani 1 1 d . . . H7 H 0.055(4) 0.839(4) 0.274(4) 0.015(8) Uiso 1 1 d . . . C9 C 0.1798(5) 0.9364(4) 0.4906(4) 0.0345(8) Uani 1 1 d . . . H8 H 0.247(6) 1.011(5) 0.469(5) 0.048(13) Uiso 1 1 d . . . C10 C 0.1785(4) 0.9211(4) 0.6309(4) 0.0289(7) Uani 1 1 d . . . H9 H 0.244(4) 0.998(4) 0.721(4) 0.020(8) 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 V1 0.0204(3) 0.0184(3) 0.0213(3) 0.00374(19) 0.0080(2) 0.00611(19) V2 0.0202(3) 0.0214(3) 0.0166(3) 0.00072(19) 0.00572(19) 0.0057(2) P1 0.0180(4) 0.0195(4) 0.0189(4) 0.0006(3) 0.0084(3) 0.0035(3) O1 0.0271(11) 0.0280(11) 0.0287(11) 0.0057(9) 0.0142(9) 0.0107(9) O2 0.0247(11) 0.0280(11) 0.0232(11) -0.0020(9) 0.0101(9) 0.0020(9) O3 0.0361(13) 0.0256(12) 0.0342(13) -0.0009(10) 0.0192(11) -0.0018(10) O4 0.0340(13) 0.0410(15) 0.0265(12) 0.0025(10) 0.0079(10) 0.0176(11) O5 0.0259(12) 0.0323(12) 0.0289(12) 0.0030(9) 0.0082(9) 0.0120(9) O6 0.0326(13) 0.0333(13) 0.0257(11) 0.0013(10) 0.0111(10) 0.0065(10) O7 0.0369(19) 0.0240(17) 0.061(2) 0.0164(16) 0.0221(18) 0.0161(14) O8 0.0435(15) 0.0347(13) 0.0247(12) 0.0078(10) 0.0128(11) 0.0075(11) N1 0.0241(13) 0.0213(13) 0.0208(12) 0.0012(10) 0.0076(10) 0.0040(10) N2 0.0234(13) 0.0266(13) 0.0192(12) 0.0026(10) 0.0084(10) 0.0072(10) C1 0.0267(15) 0.0221(15) 0.0199(14) -0.0007(11) 0.0085(12) 0.0054(12) C2 0.0362(19) 0.0364(19) 0.0230(16) -0.0041(14) 0.0075(14) 0.0007(15) C3 0.036(2) 0.0318(19) 0.035(2) -0.0067(15) 0.0077(16) -0.0053(15) C4 0.042(2) 0.0272(18) 0.041(2) 0.0020(15) 0.0164(17) -0.0025(15) C5 0.0356(18) 0.0238(16) 0.0273(16) 0.0020(13) 0.0125(14) 0.0027(13) C6 0.0228(15) 0.0292(16) 0.0174(14) 0.0017(12) 0.0058(11) 0.0070(12) C7 0.0394(19) 0.0392(19) 0.0196(15) 0.0032(14) 0.0108(14) 0.0083(16) C8 0.053(2) 0.048(2) 0.0240(17) 0.0139(15) 0.0228(16) 0.0166(18) C9 0.0369(19) 0.036(2) 0.038(2) 0.0108(16) 0.0216(16) 0.0071(15) C10 0.0270(16) 0.0303(17) 0.0315(17) 0.0056(14) 0.0136(14) 0.0059(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 V1 O6 1.614(2) . ? V1 O5 1.654(2) . ? V1 O7 1.7773(6) . ? V1 O3 1.830(2) . ? V2 O8 1.596(2) . ? V2 O1 1.982(2) . ? V2 O2 1.983(2) . ? V2 O5 2.066(2) . ? V2 N1 2.138(3) . ? V2 N2 2.264(3) . ? P1 O1 1.509(2) . ? P1 O2 1.520(2) 2_577 ? P1 O3 1.557(2) 1_455 ? P1 O4 1.569(2) . ? O2 P1 1.520(2) 2_577 ? O3 P1 1.557(2) 1_655 ? O7 V1 1.7773(6) 2_667 ? N1 C1 1.343(4) . ? N1 C5 1.347(4) . ? N2 C10 1.333(4) . ? N2 C6 1.357(4) . ? C1 C2 1.395(4) . ? C1 C6 1.472(4) . ? C2 C3 1.382(5) . ? C3 C4 1.368(6) . ? C4 C5 1.382(5) . ? C6 C7 1.391(4) . ? C7 C8 1.372(5) . ? C8 C9 1.376(5) . ? C9 C10 1.375(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 O6 V1 O5 108.44(12) . . ? O6 V1 O7 109.82(9) . . ? O5 V1 O7 110.21(9) . . ? O6 V1 O3 108.33(12) . . ? O5 V1 O3 109.22(12) . . ? O7 V1 O3 110.76(9) . . ? O8 V2 O1 99.84(12) . . ? O8 V2 O2 105.33(12) . . ? O1 V2 O2 88.87(10) . . ? O8 V2 O5 94.73(12) . . ? O1 V2 O5 165.38(10) . . ? O2 V2 O5 88.42(10) . . ? O8 V2 N1 93.92(12) . . ? O1 V2 N1 85.83(10) . . ? O2 V2 N1 160.64(10) . . ? O5 V2 N1 92.04(10) . . ? O8 V2 N2 165.31(11) . . ? O1 V2 N2 85.47(10) . . ? O2 V2 N2 88.36(10) . . ? O5 V2 N2 80.10(10) . . ? N1 V2 N2 72.68(10) . . ? O1 P1 O2 116.86(13) . 2_577 ? O1 P1 O3 109.73(13) . 1_455 ? O2 P1 O3 109.24(13) 2_577 1_455 ? O1 P1 O4 104.69(14) . . ? O2 P1 O4 109.34(13) 2_577 . ? O3 P1 O4 106.43(15) 1_455 . ? P1 O1 V2 139.83(14) . . ? P1 O2 V2 133.74(14) 2_577 . ? P1 O3 V1 143.89(15) 1_655 . ? V1 O5 V2 144.40(13) . . ? V1 O7 V1 180.000(1) . 2_667 ? C1 N1 C5 118.1(3) . . ? C1 N1 V2 120.6(2) . . ? C5 N1 V2 121.0(2) . . ? C10 N2 C6 118.7(3) . . ? C10 N2 V2 124.8(2) . . ? C6 N2 V2 116.5(2) . . ? N1 C1 C2 122.0(3) . . ? N1 C1 C6 115.7(3) . . ? C2 C1 C6 122.3(3) . . ? C3 C2 C1 118.8(3) . . ? C4 C3 C2 119.3(3) . . ? C3 C4 C5 119.2(3) . . ? N1 C5 C4 122.6(3) . . ? N2 C6 C7 121.1(3) . . ? N2 C6 C1 114.2(3) . . ? C7 C6 C1 124.7(3) . . ? C8 C7 C6 119.3(3) . . ? C7 C8 C9 119.2(3) . . ? C10 C9 C8 119.1(3) . . ? N2 C10 C9 122.6(3) . . ? _diffrn_measured_fraction_theta_max 0.923 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.923 _refine_diff_density_max 0.563 _refine_diff_density_min -0.449 _refine_diff_density_rms 0.109