#------------------------------------------------------------------------------ #$Date: 2011-06-21 23:24:15 +0300 (Tue, 21 Jun 2011) $ #$Revision: 21201 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/7015599.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7015599 loop_ _publ_author_name 'Aidoudi, Farida H.' 'Byrne, Peter J.' 'Allan, Pheobe K.' 'Teat, Simon J.' 'Lightfoot, Philip' 'Morris, Russell E.' _publ_section_title ; Ionic liquids and deep eutectic mixtures as new solvents for the synthesis of vanadium fluorides and oxyfluorides. ; _journal_issue 16 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 4324 _journal_page_last 4331 _journal_volume 40 _journal_year 2011 _chemical_formula_moiety 'F3 H4 O2 V' _chemical_formula_sum 'F3 H4 O2 V' _chemical_formula_weight 143.97 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 107.822(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 5.5473(5) _cell_length_b 9.9914(9) _cell_length_c 7.2050(6) _cell_measurement_reflns_used 14039 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 33.6 _cell_measurement_theta_min 3.3 _cell_volume 380.18(6) _computing_cell_refinement 'SAINT (Bruker, 2006)' _computing_data_collection 'APEXII (Bruker, 2006)' _computing_data_reduction 'SAINT (Bruker, 2006)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean none _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.982 _diffrn_measurement_device_type 'Bruker AXS APEXII' _diffrn_measurement_method 'omega scans' _diffrn_radiation_monochromator 'Si (111) Crystal' _diffrn_radiation_source '11.3.1 ALS. LBNL.CA' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.77490 _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 5181 _diffrn_reflns_theta_full 30.49 _diffrn_reflns_theta_max 30.49 _diffrn_reflns_theta_min 3.60 _diffrn_standards_decay_% none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_number none _exptl_absorpt_coefficient_mu 3.230 _exptl_absorpt_correction_T_max 0.7383 _exptl_absorpt_correction_T_min 0.5789 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_crystal_colour brown _exptl_crystal_density_diffrn 2.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 280 _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.817 _refine_diff_density_min -0.839 _refine_diff_density_rms 0.238 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 74 _refine_ls_number_reflns 1143 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.103 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0372 _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^)+(0.0750P)^2^+0.0248P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1181 _refine_ls_wR_factor_ref 0.1220 _reflns_number_gt 985 _reflns_number_total 1143 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file c0dt01765e.txt _[local]_cod_data_source_block shelxl _[local]_cod_cif_authors_sg_H-M 'P 21/c' _cod_database_code 7015599 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 V2 V 0.5000 0.0000 1.0000 0.0047(2) Uani 1 2 d S . . V1 V 0.0000 0.0000 0.5000 0.0049(2) Uani 1 2 d S . . F1 F 0.25746(11) -0.03440(14) 0.74626(8) 0.0095(3) Uani 1 1 d . . . F2 F -0.1294(2) 0.14169(9) 0.61632(14) 0.0087(2) Uani 1 1 d . . . O1 O 0.3585(2) -0.15775(11) 1.11328(17) 0.0089(3) Uani 1 1 d . . . F3 F 0.27542(19) 0.12032(9) 1.06632(13) 0.0084(2) Uani 1 1 d . . . O2 O 0.2310(3) 0.13293(11) 0.42372(17) 0.0094(3) Uani 1 1 d . . . H3 H 0.242(3) 0.134(2) 0.309(3) 0.029(5) Uiso 1 1 d . . . H1 H 0.291(4) -0.146(2) 1.198(3) 0.036(6) Uiso 1 1 d . . . H2 H 0.271(3) -0.224(2) 1.029(3) 0.029(6) Uiso 1 1 d . . . H4 H 0.248(3) 0.217(2) 0.473(2) 0.028(5) 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 V2 0.0047(3) 0.0052(3) 0.0037(3) -0.00023(8) 0.0006(2) 0.00036(8) V1 0.0051(3) 0.0051(3) 0.0041(3) -0.00045(8) 0.0010(2) 0.00016(8) F1 0.0087(5) 0.0117(6) 0.0055(5) -0.0003(2) -0.0017(4) 0.0002(2) F2 0.0111(5) 0.0075(4) 0.0087(5) -0.0007(3) 0.0049(4) 0.0018(3) O1 0.0115(6) 0.0079(5) 0.0094(5) -0.0014(4) 0.0062(4) -0.0026(4) F3 0.0094(5) 0.0079(4) 0.0087(4) 0.0002(3) 0.0043(3) 0.0026(3) O2 0.0131(6) 0.0079(5) 0.0087(5) -0.0015(3) 0.0057(4) -0.0031(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O -0.0041 0.0074 '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' F F -0.0053 0.0125 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.2324 0.6267 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F3 V2 F3 180.00(5) 3_657 . ? F3 V2 F1 91.73(4) 3_657 3_657 ? F3 V2 F1 88.27(4) . 3_657 ? F3 V2 F1 88.27(4) 3_657 . ? F3 V2 F1 91.73(4) . . ? F1 V2 F1 180.0 3_657 . ? F3 V2 O1 91.50(4) 3_657 3_657 ? F3 V2 O1 88.50(4) . 3_657 ? F1 V2 O1 89.96(4) 3_657 3_657 ? F1 V2 O1 90.04(4) . 3_657 ? F3 V2 O1 88.50(4) 3_657 . ? F3 V2 O1 91.50(4) . . ? F1 V2 O1 90.04(4) 3_657 . ? F1 V2 O1 89.96(4) . . ? O1 V2 O1 180.0 3_657 . ? F2 V1 F2 180.0 3_556 . ? F2 V1 F1 89.98(4) 3_556 . ? F2 V1 F1 90.02(4) . . ? F2 V1 F1 90.02(4) 3_556 3_556 ? F2 V1 F1 89.98(4) . 3_556 ? F1 V1 F1 180.0 . 3_556 ? F2 V1 O2 90.75(4) 3_556 . ? F2 V1 O2 89.25(4) . . ? F1 V1 O2 90.83(4) . . ? F1 V1 O2 89.17(4) 3_556 . ? F2 V1 O2 89.25(4) 3_556 3_556 ? F2 V1 O2 90.75(4) . 3_556 ? F1 V1 O2 89.17(4) . 3_556 ? F1 V1 O2 90.83(4) 3_556 3_556 ? O2 V1 O2 180.00(5) . 3_556 ? V1 F1 V2 159.31(8) . . ? V2 O1 H1 120.8(16) . . ? V2 O1 H2 118.7(9) . . ? H1 O1 H2 108.6(16) . . ? V1 O2 H3 120.8(13) . . ? V1 O2 H4 120.0(10) . . ? H3 O2 H4 109.9(17) . . ? 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 V2 F3 1.8947(9) 3_657 ? V2 F3 1.8947(9) . ? V2 F1 1.9403(6) 3_657 ? V2 F1 1.9403(6) . ? V2 O1 2.0393(11) 3_657 ? V2 O1 2.0393(11) . ? V1 F2 1.8947(9) 3_556 ? V1 F2 1.8947(9) . ? V1 F1 1.9378(6) . ? V1 F1 1.9378(6) 3_556 ? V1 O2 2.0347(11) . ? V1 O2 2.0347(11) 3_556 ? O1 H1 0.82(2) . ? O1 H2 0.93(2) . ? O2 H3 0.85(2) . ? O2 H4 0.90(2) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 F2 0.82(2) 1.82(2) 2.6369(17) 173(2) 3_557 O1 H2 F2 0.93(2) 1.74(2) 2.6610(17) 174.6(16) 2_546 O2 H4 F3 0.90(2) 1.75(2) 2.6532(17) 178.8(16) 4_565 O2 H3 F3 0.85(2) 1.82(2) 2.6637(17) 175(2) 1_554