#------------------------------------------------------------------------------
#$Date: 2016-02-17 15:55:00 +0200 (Wed, 17 Feb 2016) $
#$Revision: 176621 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/03/2020332.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_2020332
loop_
_publ_author_name
'Black, Cameron'
'Lightfoot, Philip'
_publ_section_title
;
 V₂O₂F₄(H₂O)₂·H₂O: a new V⁴⁺ layer structure related
 to VOF₃
;
_journal_coeditor_code           FN3211
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              80
_journal_page_last               83
_journal_paper_doi               10.1107/S2053229615024122
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          'V2 O2 F4 (H2 O)2, H2 O'
_chemical_formula_sum            'F4 H6 O5 V2'
_chemical_formula_weight         263.93
_chemical_name_systematic
;
Diaquatetra-μ-fluorido-dioxidodivanadium(IV) monohydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 103.24(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.453(8)
_cell_length_b                   4.8879(19)
_cell_length_c                   9.663(5)
_cell_measurement_reflns_used    1673
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.9
_cell_measurement_theta_min      3.5
_cell_volume                     664.5(6)
_computing_cell_refinement
;
CrystalClear (Rigaku, 2004)
;
_computing_data_collection
;
CrystalClear (Rigaku, 2004)
;
_computing_data_reduction
;
CrystalClear (Rigaku, 2004)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2009)
;
_computing_publication_material
;
WinGX (Farrugia, 2012) and PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku SCXmini'
_diffrn_measurement_method       dtprofit.ref
_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  0.1149
_diffrn_reflns_av_sigmaI/netI    0.0822
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3138
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.34
_diffrn_reflns_theta_min         2.90
_diffrn_standards_interval_count 1
_diffrn_standards_interval_time  2
_diffrn_standards_number         1080
_exptl_absorpt_coefficient_mu    2.873
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.742
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(REQAB; Rigaku, 1998)
;
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    2.638
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.674
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     63
_refine_ls_number_reflns         750
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0095P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0629
_refine_ls_wR_factor_ref         0.0707
_reflns_number_gt                585
_reflns_number_total             750
_reflns_threshold_expression     >2σ(I)
_iucr_refine_instructions_details
;
TITL CB721
CELL  0.71073    14.453 4.8879   9.663  90.000    103.24 90.000
ZERR    4.00     0.008  0.0019  0.005   0.000     0.02   0.000
LATT    7
SYMM   -X,+Y,1/2-Z
SFAC  V  O  F  H
UNIT  8  20 16 24
rem OMIT        4.00    180.00
acta 50
L.S. 4
BOND
FMAP 2
PLAN 10
WGHT    0.009500
FVAR       0.16050
MOLE   1
V1    1    0.185007    0.196555    0.619175    11.00000    0.00964    0.00655 =
         0.00852    0.00015    0.00222    0.00041
F1    3    0.197654    0.451243    0.466501    11.00000    0.01586    0.00865 =
         0.01000    0.00123    0.00418    0.00181
F2    3    0.210712   -0.116860    0.746719    11.00000    0.01495    0.00921 =
         0.01192    0.00387    0.00039    0.00094
O1    2    0.107021   -0.067995    0.477643    11.00000    0.01660    0.00841 =
         0.01318   -0.00188    0.00012    0.00098
O2    2    0.097839    0.339239    0.665650    11.00000    0.01367    0.01140 =
         0.01571   -0.00090    0.00352    0.00221
O3    2    0.000000    0.197249    0.250000    10.50000    0.01503    0.01079 =
         0.01527    0.00000    0.00322    0.00000
H1    4    0.126597   -0.200961    0.467273    11.00000    0.02653
H2    4    0.070040   -0.001261    0.402631    11.00000    0.03574
H3    4    0.033228    0.292025    0.229821    11.00000    0.03685
HKLF 4
REM  CB721
REM R1 =  0.0348 for    585 Fo > 4sig(Fo)  and  0.0577 for all    750 data
REM     63 parameters refined using      0 restraints
END
WGHT      0.0052      0.0000
REM Highest difference peak  0.558,  deepest hole -0.674,  1-sigma level  0.146
Q1    1   0.1199  0.2895  0.6140  11.00000  0.05    0.56
Q2    1   0.2392 -0.1834  0.8351  11.00000  0.05    0.48
Q3    1   0.0536 -0.0455  0.5811  11.00000  0.05    0.47
Q4    1   0.1518  0.2503  0.5212  11.00000  0.05    0.47
Q5    1   0.1492  0.0478  0.4946  11.00000  0.05    0.46
Q6    1   0.1179  0.0846  0.6108  11.00000  0.05    0.46
Q7    1  -0.0161  0.1658  0.4427  11.00000  0.05    0.46
Q8    1   0.0756  0.0880  0.7083  11.00000  0.05    0.45
Q9    1   0.1937  0.3438  0.4375  11.00000  0.05    0.45
Q10   1   0.0000  0.3540  0.7500  10.50000  0.05    0.41
;
_cod_data_source_file            fn3211sup1.cif
_cod_data_source_block           I
_cod_depositor_comments
;Adding full bibliography for 2020332.cif.

 Adding full bibliography for 2020332.cif.
;
_cod_original_sg_symbol_Hall     -C2yc
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               2020332
_cod_database_fobs_code          2020332
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_type_symbol
_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_symmetry_multiplicity
V V1 0.18501(4) 0.19656(10) 0.61917(6) 0.00822(18) Uani d . 1 1
F F1 0.19765(13) 0.4512(4) 0.4665(2) 0.0113(4) Uani d . 1 1
F F2 0.21071(14) -0.1169(4) 0.7467(2) 0.0125(4) Uani d . 1 1
O O1 0.10702(19) -0.0680(5) 0.4776(3) 0.0133(6) Uani d . 1 1
O O2 0.09784(17) 0.3392(4) 0.6657(3) 0.0136(5) Uani d . 1 1
O O3 0.0000 0.1972(8) 0.2500 0.0137(8) Uani d S 1 2
H H1 0.127(3) -0.201(9) 0.467(5) 0.027(14) Uiso d . 1 1
H H2 0.070(3) -0.001(10) 0.403(5) 0.036(14) Uiso d . 1 1
H H3 0.033(3) 0.292(8) 0.230(6) 0.037(16) Uiso d . 1 1
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
V1 0.0096(3) 0.0066(3) 0.0085(3) 0.0004(2) 0.0022(2) 0.0001(2)
F1 0.0159(11) 0.0086(9) 0.0100(10) 0.0018(7) 0.0042(9) 0.0012(8)
F2 0.0149(10) 0.0092(9) 0.0119(12) 0.0009(7) 0.0004(9) 0.0039(8)
O1 0.0166(14) 0.0084(13) 0.0132(15) 0.0010(11) 0.0001(11) -0.0019(12)
O2 0.0137(11) 0.0114(12) 0.0157(15) 0.0022(9) 0.0035(11) -0.0009(10)
O3 0.0150(18) 0.0108(17) 0.015(2) 0.000 0.0032(16) 0.000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
V V 0.3005 0.5294 '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'
H H 0.0000 0.0000 '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_1
_geom_angle_site_symmetry_3
_geom_angle
O2 V1 F2 . . 102.39(11)
O2 V1 F1 . . 98.60(11)
F2 V1 F1 . . 159.00(9)
O2 V1 F2 . 4_556 98.46(11)
F2 V1 F2 . 4_556 86.65(5)
F1 V1 F2 . 4_556 90.68(9)
O2 V1 O1 . . 96.67(13)
F2 V1 O1 . . 85.48(11)
F1 V1 O1 . . 91.75(11)
F2 V1 O1 4_556 . 164.14(10)
O2 V1 F1 . 7_556 171.78(11)
F2 V1 F1 . 7_556 85.83(8)
F1 V1 F1 . 7_556 73.18(8)
F2 V1 F1 4_556 7_556 81.86(9)
O1 V1 F1 . 7_556 83.84(10)
V1 F1 V1 . 7_556 106.82(8)
V1 F2 V1 . 4_546 141.81(11)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
V1 O2 . 1.592(2)
V1 F2 . 1.948(2)
V1 F1 . 1.971(2)
V1 F2 4_556 1.972(2)
V1 O1 . 2.027(3)
V1 F1 7_556 2.174(2)
F1 V1 7_556 2.174(2)
F2 V1 4_546 1.972(2)
