#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2014296.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_2014296 loop_ _publ_author_name 'Mohanu, Antoneta' 'Trombe, Jean-Christian' _publ_section_title ; VF(C~4~O~4~)(H~2~O)~2~: a new layer type of diaquavanadium(III) fluoride squarate ; _journal_coeditor_code AV1268 _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m16 _journal_page_last m18 _journal_volume 62 _journal_year 2006 _chemical_formula_iupac '[V (C4 O4) F (H2 O)2]' _chemical_formula_moiety 'C4 H4 F O6 V' _chemical_formula_sum 'C4 H4 F O6 V' _chemical_formula_weight 218.01 _chemical_name_systematic ; poly[diaqua-\m-fluoro-\m-squarato-vanadium(III)] ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90 _cell_angle_beta 102.019(9) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 3.7790(4) _cell_length_b 11.2070(8) _cell_length_c 7.8410(7) _cell_measurement_reflns_used 1121 _cell_measurement_temperature 295 _cell_measurement_theta_max 31.98 _cell_measurement_theta_min 6.07 _cell_volume 324.80(5) _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_collection 'COLLECT (Nonius 1998)' _computing_data_reduction DENZO-SMN _computing_molecular_graphics 'ORTEPIII (Burnett & Johnson, 1996)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _diffrn_ambient_temperature 295 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device_type 'Nonius KappaCCD area-detector' _diffrn_measurement_method '\y and \w' _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 0.0803 _diffrn_reflns_av_sigmaI/netI 0.0841 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 5487 _diffrn_reflns_theta_full 31.98 _diffrn_reflns_theta_max 31.98 _diffrn_reflns_theta_min 6.07 _exptl_absorpt_coefficient_mu 1.536 _exptl_absorpt_correction_T_max 0.956 _exptl_absorpt_correction_T_min 0.512 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Sortav; Blessing, 1995)' _exptl_crystal_colour brown _exptl_crystal_density_diffrn 2.229 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Platelet _exptl_crystal_F_000 216 _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.419 _refine_diff_density_min -0.492 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 58 _refine_ls_number_reflns 1121 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.945 _refine_ls_R_factor_all 0.0792 _refine_ls_R_factor_gt 0.0351 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0314P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0673 _refine_ls_wR_factor_ref 0.0749 _reflns_number_gt 709 _reflns_number_total 1121 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file av1268.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' 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 2014296 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _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_type_symbol V 0.5000 0.5000 0.5000 0.01408(14) Uani d S 1 V F 1.0000 0.5000 0.5000 0.0295(4) Uani d S 1 F O1 0.3863(4) 0.43415(13) 0.25861(16) 0.0193(3) Uani d . 1 O O2 0.3009(4) 0.32002(14) -0.11716(19) 0.0283(4) Uani d . 1 O C1 0.4523(5) 0.47278(17) 0.1173(3) 0.0145(4) Uani d . 1 C C2 0.4097(5) 0.41845(18) -0.0537(3) 0.0160(4) Uani d . 1 C O3 0.5368(4) 0.33348(12) 0.5817(2) 0.0228(3) Uani d . 1 O H3A 0.6400 0.2814 0.5305 0.027 Uiso d R 1 H H3B 0.4550 0.2992 0.6634 0.027 Uiso d R 1 H 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 V 0.0219(2) 0.0134(2) 0.0077(2) 0.0006(2) 0.00485(16) 0.0002(2) F 0.0211(8) 0.0368(11) 0.0320(10) -0.0004(8) 0.0085(7) -0.0010(9) O1 0.0299(8) 0.0215(8) 0.0081(7) -0.0066(6) 0.0077(6) -0.0017(6) O2 0.0526(10) 0.0199(8) 0.0160(8) -0.0159(7) 0.0158(7) -0.0056(6) C1 0.0159(9) 0.0169(11) 0.0109(9) 0.0000(7) 0.0033(7) -0.0006(7) C2 0.0198(9) 0.0178(11) 0.0112(9) -0.0029(7) 0.0052(7) -0.0007(8) O3 0.0404(8) 0.0153(8) 0.0174(8) 0.0050(6) 0.0167(6) 0.0024(6) 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag F V O3 . 89.84(4) y F V O1 . 91.02(4) y O3 V O1 . 86.83(6) y C1 O1 V . 131.58(13) ? O1 C1 C2 . 131.56(18) y O1 C1 C2 3_665 137.68(19) y C2 C1 C2 3_665 90.76(16) y O2 C2 C1 . 134.85(18) y O2 C2 C1 3_665 135.9(2) y V O3 H3A . 120.4 ? V O3 H3B . 131.0 ? H3A O3 H3B . 108.5 ? 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 V F . 1.8895(2) y V O3 . 1.9687(14) y V O1 . 1.9932(13) y O1 C1 . 1.262(2) y O2 C2 . 1.244(2) y C1 C2 . 1.451(3) y C1 C2 3_665 1.454(3) y O3 H3A . 0.8484 ? O3 H3B . 0.8577 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA O3 H3B O2 1_556 0.86 1.94 2.696(2) 145.9 O3 H3A O2 4_666 0.85 1.82 2.6525(19) 168.8