Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_sad _database_code_CSD 177805 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Feng, Shouhua' 'Chen, Xiaobo' 'Dai, Zhimin' 'Fu, Wensheng' 'Hua, Jia' 'Li, Guanghua' 'Shi, Zhan' 'Zhang, Dong' _publ_contact_author_name 'Prof Shouhua Feng' _publ_contact_author_address ; Department of Chemistry, Jilin University State Key Laboratory of Inorganic Synthesis and Preparative Chemistry Jiefang road 119# Changchun Jilin 130023 CHINA ; #==================================================================== _publ_contact_author_phone '86-431-5671974' _publ_contact_author_fax '86-431-5671974' _publ_contact_author_email 'shfeng@mail.jlu.edu.cn' _publ_requested_coeditor_name ? #========================================================================== # 2. TITLE AND AUTHOR LIST _publ_section_title ; First coordination complex-linked vanadium selenite, [Cu(phen)]2V2Se2O11: hydrothermal synthesis and crystal structure ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H16 Cu2 N4 O11 Se2 V2' _chemical_formula_weight 923.29 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' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinc _symmetry_space_group_name_H-M P2/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 11.1059(3) _cell_length_b 9.8725(3) _cell_length_c 13.0827(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.191(2) _cell_angle_gamma 90.00 _cell_volume 1407.15(7) _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 blue _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.179 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 4.790 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.297881 _exptl_absorpt_correction_T_max 0.693214 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6659 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0244 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 23.24 _reflns_number_total 2016 _reflns_number_gt 1880 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXP-97' _computing_publication_material 'SHELXTL' _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^)+(0.0516P)^2^+1.3105P] 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 2016 _refine_ls_number_parameters 236 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0313 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0775 _refine_ls_wR_factor_gt 0.0763 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 Se Se 0.09580(3) 0.02462(4) 0.67732(3) 0.02495(16) Uani 1 1 d . . . Cu Cu 0.19193(4) -0.15930(4) 0.87058(3) 0.02327(16) Uani 1 1 d . . . V V 0.32073(5) -0.13024(6) 1.13853(4) 0.02215(19) Uani 1 1 d . . . O1 O 0.1357(2) 0.0217(2) 0.8082(2) 0.0287(6) Uani 1 1 d . . . O2 O 0.1386(2) -0.1292(3) 0.6442(2) 0.0343(6) Uani 1 1 d . . . O3 O -0.0607(2) -0.0060(3) 0.6567(2) 0.0344(7) Uani 1 1 d . . . O4 O 0.2183(2) -0.0957(3) 1.03327(19) 0.0341(6) Uani 1 1 d . . . O5 O 0.2500 -0.1335(4) 1.2500 0.0406(10) Uani 1 2 d S . . O6 O 0.3877(3) -0.2714(3) 1.1238(2) 0.0407(7) Uani 1 1 d . . . N1 N 0.2316(3) -0.3608(3) 0.8803(2) 0.0287(7) Uani 1 1 d . . . N2 N 0.0227(3) -0.2291(3) 0.8726(2) 0.0257(7) Uani 1 1 d . . . C1 C 0.3387(4) -0.4229(5) 0.8887(3) 0.0380(10) Uani 1 1 d . . . C2 C 0.3476(5) -0.5651(5) 0.8896(4) 0.0494(13) Uani 1 1 d . . . C3 C 0.2449(5) -0.6435(5) 0.8821(4) 0.0481(12) Uani 1 1 d . . . C4 C 0.1303(4) -0.5803(4) 0.8743(3) 0.0375(10) Uani 1 1 d . . . C5 C 0.1292(4) -0.4383(4) 0.8740(3) 0.0280(8) Uani 1 1 d . . . C6 C 0.0168(4) -0.3667(4) 0.8705(3) 0.0272(9) Uani 1 1 d . . . C7 C -0.0924(4) -0.4389(4) 0.8691(3) 0.0336(9) Uani 1 1 d . . . C8 C -0.1984(4) -0.3618(5) 0.8742(3) 0.0410(11) Uani 1 1 d . . . C9 C -0.1892(4) -0.2248(6) 0.8802(3) 0.0417(11) Uani 1 1 d . . . C10 C -0.0792(4) -0.1606(5) 0.8779(3) 0.0330(9) Uani 1 1 d . . . C11 C 0.0157(5) -0.6504(5) 0.8690(3) 0.0473(13) Uani 1 1 d . . . C12 C -0.0887(5) -0.5833(5) 0.8671(4) 0.0464(12) Uani 1 1 d . . . H1 H 0.409(5) -0.365(5) 0.899(3) 0.039(12) Uiso 1 1 d . . . H2 H 0.422(5) -0.593(5) 0.899(4) 0.048(14) Uiso 1 1 d . . . H3 H 0.251(5) -0.754(6) 0.885(4) 0.071(16) Uiso 1 1 d . . . H8 H -0.279(4) -0.412(5) 0.875(3) 0.036(11) Uiso 1 1 d . . . H9 H -0.244(5) -0.183(5) 0.887(4) 0.042(15) Uiso 1 1 d . . . H10 H -0.070(4) -0.074(5) 0.879(3) 0.039(12) Uiso 1 1 d . . . H11 H 0.018(4) -0.735(6) 0.865(4) 0.052(15) Uiso 1 1 d . . . H12 H -0.156(5) -0.625(5) 0.859(4) 0.041(13) 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 Se 0.0191(2) 0.0251(3) 0.0310(2) 0.00658(14) 0.00581(16) 0.00184(14) Cu 0.0197(3) 0.0243(3) 0.0262(3) 0.00202(17) 0.00542(19) -0.00092(17) V 0.0194(3) 0.0282(4) 0.0199(4) -0.0028(2) 0.0062(3) -0.0024(2) O1 0.0305(14) 0.0247(14) 0.0309(15) -0.0009(11) 0.0055(11) 0.0022(11) O2 0.0204(14) 0.0366(16) 0.0463(16) -0.0141(13) 0.0075(12) 0.0018(12) O3 0.0166(13) 0.0362(16) 0.0498(17) 0.0062(12) 0.0047(12) 0.0042(11) O4 0.0293(14) 0.0470(18) 0.0244(14) -0.0059(12) 0.0014(11) 0.0007(13) O5 0.046(2) 0.052(3) 0.028(2) 0.000 0.0184(18) 0.000 O6 0.0395(16) 0.0403(17) 0.0444(17) -0.0023(13) 0.0135(13) 0.0087(14) N1 0.0331(19) 0.0294(18) 0.0246(17) 0.0005(13) 0.0075(13) 0.0058(15) N2 0.0252(17) 0.0281(18) 0.0237(16) 0.0019(13) 0.0050(13) -0.0009(14) C1 0.037(2) 0.044(3) 0.035(2) 0.0055(19) 0.0126(19) 0.012(2) C2 0.059(3) 0.050(3) 0.044(3) 0.009(2) 0.023(2) 0.033(3) C3 0.076(4) 0.033(3) 0.040(3) 0.0004(19) 0.021(2) 0.013(2) C4 0.063(3) 0.027(2) 0.025(2) -0.0028(17) 0.0157(19) 0.002(2) C5 0.043(2) 0.024(2) 0.0179(18) -0.0013(15) 0.0075(16) -0.0009(18) C6 0.035(2) 0.027(2) 0.0192(18) -0.0005(15) 0.0048(16) -0.0046(17) C7 0.042(2) 0.037(2) 0.0203(19) -0.0022(17) 0.0032(16) -0.015(2) C8 0.029(2) 0.060(3) 0.033(2) 0.006(2) 0.0022(18) -0.016(2) C9 0.026(2) 0.055(3) 0.045(3) 0.010(2) 0.010(2) 0.004(2) C10 0.030(2) 0.033(3) 0.037(2) 0.0077(18) 0.0082(17) 0.0033(19) C11 0.082(4) 0.026(3) 0.034(3) -0.0062(19) 0.011(2) -0.011(3) C12 0.061(3) 0.039(3) 0.038(2) -0.005(2) 0.008(2) -0.025(3) _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 Se O2 1.673(3) . ? Se O1 1.684(3) . ? Se O3 1.733(3) . ? Cu O2 1.952(3) 2_556 ? Cu N2 2.007(3) . ? Cu O1 2.013(2) . ? Cu N1 2.036(3) . ? Cu O4 2.184(2) . ? V O6 1.609(3) . ? V O4 1.643(3) . ? V O5 1.7859(5) . ? V O3 1.865(3) 4_656 ? O2 Cu 1.952(2) 2_556 ? O3 V 1.865(3) 4 ? O5 V 1.7859(6) 2_557 ? N1 C1 1.324(5) . ? N1 C5 1.359(5) . ? N2 C10 1.331(5) . ? N2 C6 1.361(5) . ? C1 C2 1.407(7) . ? C1 H1 0.95(5) . ? C2 C3 1.367(8) . ? C2 H2 0.86(5) . ? C3 C4 1.404(7) . ? C3 H3 1.09(6) . ? C4 C5 1.402(6) . ? C4 C11 1.438(7) . ? C5 C6 1.427(5) . ? C6 C7 1.404(6) . ? C7 C8 1.415(6) . ? C7 C12 1.426(7) . ? C8 C9 1.358(7) . ? C8 H8 1.02(4) . ? C9 C10 1.382(6) . ? C9 H9 0.76(5) . ? C10 H10 0.86(5) . ? C11 C12 1.331(8) . ? C11 H11 0.84(6) . ? C12 H12 0.85(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 O2 Se O1 102.51(13) . . ? O2 Se O3 97.35(12) . . ? O1 Se O3 102.33(14) . . ? O2 Cu N2 167.76(12) 2_556 . ? O2 Cu O1 93.11(11) 2_556 . ? N2 Cu O1 95.30(12) . . ? O2 Cu N1 87.36(12) 2_556 . ? N2 Cu N1 81.69(13) . . ? O1 Cu N1 159.90(11) . . ? O2 Cu O4 95.93(11) 2_556 . ? N2 Cu O4 91.96(11) . . ? O1 Cu O4 96.43(10) . . ? N1 Cu O4 103.51(11) . . ? O6 V O4 109.89(14) . . ? O6 V O5 111.69(17) . . ? O4 V O5 110.20(10) . . ? O6 V O3 107.95(14) . 4_656 ? O4 V O3 108.32(14) . 4_656 ? O5 V O3 108.70(14) . 4_656 ? Se O1 Cu 115.26(13) . . ? Se O2 Cu 119.44(15) . 2_556 ? Se O3 V 123.80(16) . 4 ? V O4 Cu 134.22(15) . . ? V O5 V 178.0(3) 2_557 . ? C1 N1 C5 118.2(4) . . ? C1 N1 Cu 129.6(3) . . ? C5 N1 Cu 112.2(3) . . ? C10 N2 C6 118.1(3) . . ? C10 N2 Cu 129.3(3) . . ? C6 N2 Cu 112.6(2) . . ? N1 C1 C2 121.6(5) . . ? N1 C1 H1 115(3) . . ? C2 C1 H1 123(3) . . ? C3 C2 C1 120.5(5) . . ? C3 C2 H2 127(3) . . ? C1 C2 H2 113(3) . . ? C2 C3 C4 119.1(4) . . ? C2 C3 H3 121(3) . . ? C4 C3 H3 120(3) . . ? C5 C4 C3 116.8(4) . . ? C5 C4 C11 118.3(4) . . ? C3 C4 C11 124.8(4) . . ? N1 C5 C4 123.8(4) . . ? N1 C5 C6 116.1(3) . . ? C4 C5 C6 120.1(4) . . ? N2 C6 C7 123.0(4) . . ? N2 C6 C5 117.1(3) . . ? C7 C6 C5 119.8(4) . . ? C6 C7 C8 116.8(4) . . ? C6 C7 C12 118.7(4) . . ? C8 C7 C12 124.5(4) . . ? C9 C8 C7 119.0(4) . . ? C9 C8 H8 122(3) . . ? C7 C8 H8 119(3) . . ? C8 C9 C10 120.9(5) . . ? C8 C9 H9 119(4) . . ? C10 C9 H9 120(4) . . ? N2 C10 C9 122.1(4) . . ? N2 C10 H10 114(3) . . ? C9 C10 H10 124(3) . . ? C12 C11 C4 121.3(4) . . ? C12 C11 H11 122(4) . . ? C4 C11 H11 116(4) . . ? C11 C12 C7 121.7(5) . . ? C11 C12 H12 121(3) . . ? C7 C12 H12 117(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.24 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.641 _refine_diff_density_min -0.735 _refine_diff_density_rms 0.132