#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:42:55 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179859 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/55/7015599.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_paper_doi               10.1039/c0dt01765e
_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/[σ²(Fo²)+(0.0750P)²+0.0248P] where P=(Fo²+2Fc²)/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)
_cod_data_source_file            c0dt01765e.txt
_cod_data_source_block           shelxl
_cod_original_sg_symbol_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
