#------------------------------------------------------------------------------ #$Date: 2016-02-19 14:29:56 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176759 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/33/2003325.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2003325 loop_ _publ_author_name 'Marcos, M. D.' 'Amor\'os, P.' 'Beltr\'an-Porter, A.' 'Ram\'irez de Arellano, M. C.' _publ_contact_author ; M. Dolores Marcos University Chemical Laboratory Cambridge CB2 1EW, U.K. ; _publ_section_title ; Hydrothermal Synthesis and Structure of Nickel(II) Metavanadate Monohydrate, NiV~2~O~6~.H~2~O ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 552 _journal_page_last 555 _journal_paper_doi 10.1107/S0108270194006797 _journal_volume 51 _journal_year 1995 _chemical_compound_source ' Hydrothermal synthesis from NiCl~2~.6H~2~O and NaVO~3~.' _chemical_formula_moiety NiV~2~O~6~.H~2~O _chemical_formula_sum 'H4 Ni2 O14 V4' _chemical_formula_weight 549.21 _chemical_melting_point 'non measured' _chemical_name_common 'Nickel(II) Metavanadate Monohydrate' _chemical_name_systematic ; Nickel(II) divanadium(V)hexaoxide monohydrate ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _audit_creation_method SHELXL _cell_angle_alpha 80.97(3) _cell_angle_beta 81.11(3) _cell_angle_gamma 76.43(3) _cell_formula_units_Z 1 _cell_length_a 5.833(2) _cell_length_b 6.593(3) _cell_length_c 7.730(3) _cell_measurement_reflns_used 30 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25 _cell_measurement_theta_min 20 _cell_volume 283.2(2) _computing_cell_refinement 'Siemens P3 software' _computing_data_collection 'Siemens P3 software' _computing_data_reduction XDISK _computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material SHELXL92 _computing_structure_refinement 'SHELXL92 (Sheldrick, 1992)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measurement_device 'Siemens R3m/V' _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min 1 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 980 _diffrn_reflns_theta_max 23.52 _diffrn_reflns_theta_min 2.69 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 100 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 6.495 _exptl_absorpt_correction_T_max 0.120 _exptl_absorpt_correction_T_min 0.062 _exptl_absorpt_correction_type 'Semi empirical' _exptl_crystal_colour Yellow _exptl_crystal_density_diffrn 3.220 _exptl_crystal_description Plate _exptl_crystal_F_000 264 _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _refine_diff_density_max 1.237 _refine_diff_density_min -1.298 _refine_ls_extinction_coef n/a _refine_ls_extinction_method n/a _refine_ls_goodness_of_fit_all 1.088 _refine_ls_goodness_of_fit_obs 1.108 _refine_ls_hydrogen_treatment n/a _refine_ls_matrix_type full _refine_ls_number_parameters 92 _refine_ls_number_reflns 851 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.088 _refine_ls_restrained_S_obs 1.108 _refine_ls_R_factor_all 0.0575 _refine_ls_R_factor_obs 0.0487 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme ; calc w = 1/[\s^2^(Fo^2^) + (0.0943P)^2^ + 1.5608P] where P=(Fo^2^ + 2Fc^2^)/3 ; _refine_ls_wR_factor_all 0.1359 _refine_ls_wR_factor_obs 0.1284 _reflns_number_observed 744 _reflns_number_total 851 _reflns_observed_criterion >2sigma(I) _cod_data_source_file br1075.cif _cod_data_source_block br1075 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2003325 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 Ni 0.0096(6) -0.0036(4) 0.0001(4) 0.0051(6) -0.0007(4) 0.0113(7) V1 0.0057(8) -0.0037(6) -0.0003(6) 0.0044(8) 0.0003(6) 0.0115(8) V2 0.0052(7) -0.0036(6) -0.0001(6) 0.0077(8) -0.0009(6) 0.0121(8) O1 0.012(3) 0.000(3) -0.003(3) 0.025(4) -0.001(3) 0.030(4) O2 0.017(3) -0.006(3) 0.006(3) 0.017(3) -0.004(3) 0.011(3) O3 0.022(3) -0.006(3) -0.003(3) 0.009(3) 0.002(3) 0.021(3) O4 0.012(3) -0.006(3) -0.003(3) 0.015(3) 0.003(3) 0.017(3) O5 0.013(3) -0.010(3) -0.003(3) 0.011(3) 0.002(2) 0.018(3) O6 0.010(3) -0.004(3) 0.002(3) 0.017(3) 0.006(3) 0.022(4) O7 0.013(3) -0.004(2) 0.000(2) 0.010(3) 0.002(2) 0.008(3) loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_type_symbol Ni 1 0.4242(2) 0.6411(2) 0.65246(14) 0.0085(4) Uani d Ni V1 1 0.3937(2) 1.1484(2) 0.7692(2) 0.0070(5) Uani d V V2 1 0.1964(2) 0.6737(2) 1.0909(2) 0.0081(5) Uani d V O1 1 0.0886(11) 0.7597(10) 0.5627(9) 0.023(2) Uani d O O2 1 0.2550(11) 0.5847(10) 0.8965(8) 0.0152(14) Uani d O O3 1 0.4581(11) 0.9269(9) 0.6845(9) 0.0174(14) Uani d O O4 1 0.2490(10) 0.4793(9) 1.2568(8) 0.0148(14) Uani d O O5 1 0.6146(10) 1.1539(9) 0.9039(8) 0.0130(13) Uani d O O6 1 -0.1014(10) 0.8181(10) 1.1231(8) 0.0173(14) Uani d O O7 1 0.4162(10) 1.3437(9) 0.5982(7) 0.0105(13) Uani d O loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag O O 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0106 0.006 V V 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.3005 0.529 Ni Ni 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.3393 1.1 H H 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0000 0.000 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 O3 Ni O2 . . 94.5(3) yes O3 Ni O7 . 2_676 94.0(3) yes O2 Ni O7 . 2_676 171.4(2) yes O3 Ni O4 . 2_667 88.2(3) yes O2 Ni O4 . 2_667 91.0(3) yes O7 Ni O4 2_676 2_667 90.1(2) yes O3 Ni O7 . 1_545 174.2(3) yes O2 Ni O7 . 1_545 90.9(2) yes O7 Ni O7 2_676 1_545 80.6(2) yes O4 Ni O7 2_667 1_545 89.8(2) yes O3 Ni O1 . . 92.5(3) yes O2 Ni O1 . . 88.2(3) yes O7 Ni O1 2_676 . 90.5(3) yes O4 Ni O1 2_667 . 179.0(2) yes O7 Ni O1 1_545 . 89.5(2) yes O3 V1 O7 . . 107.0(3) yes O3 V1 O6 . 2_577 108.2(3) yes O7 V1 O6 . 2_577 110.7(3) yes O3 V1 O5 . . 110.1(3) yes O7 V1 O5 . . 105.4(3) yes O6 V1 O5 2_577 . 115.2(3) yes O2 V2 O4 . . 111.9(3) yes O2 V2 O5 . 2_677 108.7(3) yes O4 V2 O5 . 2_677 107.2(3) yes O2 V2 O6 . . 110.7(3) yes O4 V2 O6 . . 110.4(3) yes O5 V2 O6 2_677 . 107.8(3) yes V2 O2 Ni . . 141.4(4) no V1 O3 Ni . . 156.8(4) no V2 O4 Ni . 2_667 124.9(3) no V2 O5 V1 2_677 . 134.8(4) no V1 O6 V2 2_577 . 151.9(4) no V1 O7 Ni . 2_676 135.6(3) no V1 O7 Ni . 1_565 119.1(3) no Ni O7 Ni 2_676 1_565 99.4(2) no 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 Ni O3 . 1.997(6) yes Ni O2 . 2.012(6) yes Ni O7 2_676 2.014(6) yes Ni O4 2_667 2.070(6) yes Ni O7 1_545 2.081(6) yes Ni O1 . 2.111(6) yes V1 O3 . 1.633(6) yes V1 O7 . 1.707(6) yes V1 O6 2_577 1.759(6) yes V1 O5 . 1.787(6) yes V2 O2 . 1.656(6) yes V2 O4 . 1.674(6) yes V2 O5 2_677 1.768(6) yes V2 O6 . 1.775(6) yes O4 Ni 2_667 2.070(6) no O5 V2 2_677 1.768(5) no O6 V1 2_577 1.759(6) no O7 Ni 2_676 2.014(6) no O7 Ni 1_565 2.081(6) no