Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_V6O14 _journal_coden_Cambridge 186 loop_ _publ_author_name 'Lin, Bi-Zhou' 'Liu, Shi-Xiong' _publ_contact_author_name 'Dr Bi-Zhou Lin' _publ_contact_author_address ; Institute of Material Physical Chemistry Huaqiao University Quanzhou 362011 Peolpe's Republic of China ; _publ_contact_author_email bzlin@qhu.edu.cn _publ_contact_author_fax '86 595 2686969' _publ_contact_author_phone '86 595 2691567' _publ_requested_journal 'J. Chem. Soc. Dalton Trans.' _publ_section_title ; Hydrothermal synthesis, structure and characterization of a novel layered vanadium oxide with metal coordination complexes: [Ni(en)2][V6O14] ; ############################################################################ data_(I) _database_code_CSD 178356 _audit_creation_method SHELXL-97 _publ_requested_category FM _chemical_name_systematic ; [bis-ethylenediamine nickel(II)] hexavanadate(V) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Ni C4 H16 N4 V6 O14 ' _chemical_formula_sum 'C4 H16 N4 Ni O14 V6' _chemical_formula_weight 708.56 _chemical_compound_source 'synthesis' 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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C mca' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' '-x+1/2, y+1, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' 'x+1/2, -y, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 16.597(3) _cell_length_b 6.6200(10) _cell_length_c 17.117(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1880.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 15 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 3.905 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.1957 _exptl_absorpt_correction_T_max 0.8287 _exptl_absorpt_process_details '(North, phillips & Mathews, 1968)' _exptl_special_details ; crystal coated in epoxy glue ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'RIGAKU--AFC5R' _diffrn_measurement_method \w--2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.6 _diffrn_reflns_number 1060 _diffrn_reflns_av_R_equivalents 0.0462 _diffrn_reflns_av_sigmaI/netI 0.1017 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 25.97 _reflns_number_total 956 _reflns_number_gt 650 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; RIGAKU/AFC (Molecuar Structure Corporation, 1987a) ; _computing_cell_refinement ; RIGAKU/AFC (Molecuar Structure Corporation, 1987a) ; _computing_data_reduction ; TEXRAY (Molecuar Structure Corporation, 1987b) ; _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1990)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+51.3841P] 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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00002(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 956 _refine_ls_number_parameters 74 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1009 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.1484 _refine_ls_wR_factor_gt 0.1309 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 Ni1 Ni 0.5000 0.0000 0.5000 0.0144(5) Uani 1 4 d S . . V1 V 0.5000 0.1367(3) 0.29010(10) 0.0094(4) Uani 1 2 d S . . V2 V 0.35139(12) 0.4160(2) 0.28739(9) 0.0297(5) Uani 1 1 d . . . O1 O 0.5000 0.0664(12) 0.3797(4) 0.0201(18) Uani 1 2 d S . . O2 O 0.3847(3) 0.1532(9) 0.2620(3) 0.0239(14) Uani 1 1 d . . . O3 O 0.5000 0.4243(15) 0.2793(6) 0.066(4) Uani 1 2 d S . . O4 O 0.3475(4) 0.4442(9) 0.3788(3) 0.0292(15) Uani 1 1 d . . . O5 O 0.2500 0.4026(17) 0.2500 0.074(4) Uani 1 2 d S . . N1 N 0.5827(6) -0.2207(15) 0.4808(5) 0.050(3) Uani 1 1 d . . . H1 H 0.5821 -0.2992 0.4270 0.050 Uiso 1 1 d R . . H2 H 0.5943 -0.3226 0.5209 0.050 Uiso 1 1 d R . . C1 C 0.6539(9) -0.086(2) 0.4718(8) 0.092(6) Uani 1 1 d . . . H3 H 0.6481 -0.0360 0.4326 0.080 Uiso 1 1 d R . . H4 H 0.6869 -0.2004 0.4560 0.050 Uiso 1 1 d R . . 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 Ni1 0.0145(10) 0.0139(10) 0.0147(10) 0.0019(9) 0.000 0.000 V1 0.0100(9) 0.0077(8) 0.0105(9) 0.0004(7) 0.000 0.000 V2 0.0533(11) 0.0159(8) 0.0199(8) 0.0006(6) 0.0005(8) -0.0009(7) O1 0.021(4) 0.021(4) 0.018(4) 0.006(4) 0.000 0.000 O2 0.018(3) 0.030(3) 0.024(3) -0.006(3) -0.005(3) 0.005(3) O3 0.151(13) 0.012(5) 0.034(6) 0.003(4) 0.000 0.000 O4 0.033(3) 0.032(4) 0.022(3) 0.000(3) 0.002(3) 0.003(3) O5 0.078(9) 0.035(6) 0.108(10) 0.000 -0.052(9) 0.000 N1 0.075(7) 0.048(6) 0.027(5) 0.005(4) 0.012(4) -0.005(5) C1 0.093(11) 0.095(13) 0.088(13) 0.045(9) 0.040(9) 0.058(10) _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 Ni1 N1 2.032(10) 4_556 ? Ni1 N1 2.032(10) 12_655 ? Ni1 N1 2.032(10) 9_656 ? Ni1 N1 2.032(10) . ? Ni1 O1 2.105(8) 9_656 ? Ni1 O1 2.105(8) 9_656 ? Ni1 O1 2.105(8) . ? V1 O1 1.603(8) . ? V1 O3 1.841(10) 10_556 ? V1 O3 1.912(10) . ? V1 O2 1.976(5) 12_655 ? V1 O2 1.976(5) . ? V1 V2 3.083(2) 12_655 ? V1 V2 3.083(2) . ? V2 O4 1.576(6) . ? V2 O5 1.803(2) . ? V2 O2 1.867(6) 10_566 ? V2 O2 1.877(6) . ? V2 O3 2.471(2) . ? O2 V2 1.867(6) 10_556 ? O3 V1 1.841(10) 10_566 ? O5 V2 1.803(2) 7_545 ? N1 C1 1.486(17) . ? N1 H1 1.0570 . ? N1 H2 0.9823 . ? C1 C1 1.50(3) 4_556 ? C1 H3 0.7567 . ? C1 H4 0.9710 . ? 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 N1 Ni1 N1 180.00 4_556 12_655 ? N1 Ni1 N1 85.0(5) 4_556 9_656 ? N1 Ni1 N1 95.0(5) 12_655 9_656 ? N1 Ni1 N1 95.0(5) 4_556 . ? N1 Ni1 N1 85.00 12_655 . ? N1 Ni1 N1 180.0(5) 9_656 . ? N1 Ni1 O1 89.5(3) 4_556 9_656 ? N1 Ni1 O1 90.5(3) 12_655 9_656 ? N1 Ni1 O1 89.5(3) 9_656 9_656 ? N1 Ni1 O1 90.5(3) . 9_656 ? N1 Ni1 O1 90.5(3) 4_556 . ? N1 Ni1 O1 89.5(3) 12_655 . ? N1 Ni1 O1 90.5(3) 9_656 . ? N1 Ni1 O1 89.5(3) . . ? O1 Ni1 O1 180.000(1) 9_656 . ? O1 V1 O3 113.3(4) . 10_556 ? O1 V1 O3 112.4(4) . . ? O3 V1 O3 134.3(2) 10_556 . ? O1 V1 O2 104.44(18) . 12_655 ? O3 V1 O2 83.39(18) 10_556 12_655 ? O3 V1 O2 85.5(2) . 12_655 ? O1 V1 O2 104.44(18) . . ? O3 V1 O2 83.39(19) 10_556 . ? O3 V1 O2 85.5(2) . . ? O2 V1 O2 151.0(4) 12_655 . ? O4 V2 O5 108.6(3) . . ? O4 V2 O2 111.2(3) . 10_566 ? O5 V2 O2 99.1(4) . 10_566 ? O4 V2 O2 110.6(3) . . ? O5 V2 O2 98.5(4) . . ? O2 V2 O2 126.0(2) 10_566 . ? O4 V2 O3 95.4(3) . . ? O5 V2 O3 155.9(3) . . ? O2 V2 O3 70.1(3) 10_566 . ? O2 V2 O3 73.3(3) . . ? V1 O1 Ni1 175.2(5) . . ? V2 O2 V2 142.9(3) 10_556 . ? V2 O2 V1 110.5(3) 10_556 . ? V2 O2 V1 106.3(3) . . ? V1 O3 V1 145.3(6) 10_566 . ? V1 O3 V2 93.0(2) 10_566 . ? V1 O3 V2 88.4(2) . . ? V2 O5 V2 174.4(7) . 7_545 ? C1 N1 Ni1 97.1(7) . . ? C1 N1 H1 102.3 . . ? Ni1 N1 H1 119.2 . . ? C1 N1 H2 109.1 . . ? Ni1 N1 H2 120.8 . . ? H1 N1 H2 105.9 . . ? N1 C1 C1 113.0(9) . 4_556 ? N1 C1 H3 104.8 . . ? C1 C1 H3 103.6 4_556 . ? N1 C1 H4 90.7 . . ? C1 C1 H4 140.8 4_556 . ? H3 C1 H4 99.5 . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 O3 O2 O3 64.7(3) . 10_556 . . ? O1 O3 O2 O3 -64.7(3) . . . 10_556 ? O1 O3 O2 O3 -64.7(3) . 10_556 12_655 . ? O1 O3 O2 O3 64.7(3) . . 12_655 10_556 ? O3 O1 O2 O3 -95.41(19) 10_556 . . . ? O3 O1 O2 O3 95.41(19) 10_556 . 12_655 . ? O2 O1 O3 O2 115.7(4) . . 10_556 12_655 ? O2 O1 O3 O2 -111.8(4) . . . 12_655 ? O2 O3 O3 O2 -165.9(4) . . 10_556 12_655 ? O4 O2 O5 O2 66.4(2) . . . 10_566 ? O4 O2 O5 O2 -66.5(2) . 10_566 . . ? O4 O2 O3 O2 -61.3(2) . . . 10_566 ? O4 O2 O3 O2 60.3(2) . 10_566 . . ? O2 O4 O5 O2 85.40(17) 10_566 . . . ? O2 O4 O3 O2 96.2(3) . . . 10_566 ? O5 O4 O2 O3 119.5(3) . . . . ? O5 O4 O2 O3 -121.8(3) . . 10_566 . ? O5 O2 O2 O3 -164.9(3) . 10_566 . . ? loop_ _geom_hbond_atom_label_D _geom_hbond_atom_label_H _geom_hbond_atom_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O4 1.057 2.221 3.051(11) 134.0(2) 12_645 N1 H2 O4 0.982 2.128 3.052(10) 155.9(5) 9_656 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.936 _refine_diff_density_min -0.819 _refine_diff_density_rms 0.096 ############################################################################