#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/58/2015810.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_2015810
loop_
_publ_author_name
'Magnussen, Magnus '
'Brock-Nannestad, Theis'
'Bendix, Jesper'
_publ_section_title
;
 Pentaaquaoxovanadium(IV) bis(trifluoromethanesulfonate)
;
_journal_coeditor_code           IZ3014
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m51
_journal_page_last               m53
_journal_paper_doi               10.1107/S010827010605219X
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[V O (H2 O)5] (C F3 S O3)2'
_chemical_formula_moiety         'H10 O6 V, 2(C F3 O3 S)'
_chemical_formula_sum            'C2 H10 F6 O12 S2 V'
_chemical_formula_weight         455.16
_chemical_name_common            Vanadyltriflate
_chemical_name_systematic
;
Pentaaquaoxovanadium(IV) trifluoromethanesulfonate
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 102.684(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.688(2)
_cell_length_b                   7.7579(17)
_cell_length_c                   10.219(4)
_cell_measurement_reflns_used    11327
_cell_measurement_temperature    122.0(10)
_cell_measurement_theta_max      25.98
_cell_measurement_theta_min      2.04
_cell_volume                     749.3(4)
_computing_cell_refinement       'DIRAX (Duisenberg, 1992)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'EvalCCD (Duisenberg, 1998)'
_computing_molecular_graphics
;
ORTEPII (Johnson, 1976) and Mercury (Macrae et al.,
2006)
;
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      122.0(10)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       'ω and φ'
_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  0.1412
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            18866
_diffrn_reflns_theta_full        25.98
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    1.066
_exptl_absorpt_correction_T_max  0.843
_exptl_absorpt_correction_T_min  0.747
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    2.017
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             454
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.558
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         1588
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0379
_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)+(0.0498P)²+0.7459P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1039
_reflns_number_gt                1429
_reflns_number_total             1588
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            iz3014.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               2015810
_cod_database_fobs_code          2015810
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
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_disorder_group
V V 0.17902(5) 0.2500 0.05125(6) 0.0193(2) Uani d S 1 .
O O1 0.0193(2) 0.2500 -0.0267(3) 0.0294(6) Uani d S 1 .
O O2 0.4049(2) 0.2500 0.1391(3) 0.0244(5) Uani d S 1 .
H H2 0.4602 0.3407 0.1490 0.029 Uiso d R 1 .
O O3 0.17120(15) 0.4314(2) 0.19209(18) 0.0257(4) Uani d . 1 .
H H3A 0.1910 0.5443 0.1871 0.031 Uiso d R 1 .
H H3B 0.1126 0.4263 0.2399 0.031 Uiso d R 1 .
O O4 0.24447(15) 0.0615(2) -0.05857(17) 0.0259(4) Uani d . 1 .
H H4A 0.1860 0.0290 -0.1326 0.031 Uiso d R 1 .
H H4B 0.3325 0.0635 -0.0728 0.031 Uiso d R 1 .
C C1 0.5576(5) 0.7500 0.3632(5) 0.0636(16) Uani d SD 1 .
F F11 0.5170(19) 0.849(3) 0.4427(13) 0.098(5) Uani d PDU 0.43(3) .
F F12 0.6941(3) 0.7500 0.3650(4) 0.0823(11) Uani d SD 1 .
F F11A 0.5340(12) 0.914(3) 0.4100(17) 0.095(4) Uani d PU 0.57(3) 1
S S1 0.45741(8) 0.7500 0.19089(10) 0.0230(2) Uani d S 1 .
O O11 0.50218(17) 0.5942(2) 0.1362(2) 0.0339(5) Uani d . 1 .
O O12 0.3103(2) 0.7500 0.1998(3) 0.0295(6) Uani d S 1 .
C C2 -0.1222(4) 0.2500 0.4869(4) 0.0281(8) Uani d SD 1 .
F F21 -0.18113(17) 0.3884(2) 0.52622(16) 0.0421(4) Uani d D 1 .
F F22 0.0143(2) 0.2500 0.5438(2) 0.0415(6) Uani d SD 1 .
S S2 -0.14717(7) 0.2500 0.30406(8) 0.0188(2) Uani d S 1 .
O O21 -0.07609(15) 0.4061(2) 0.27632(17) 0.0249(4) Uani d . 1 .
O O22 -0.2970(2) 0.2500 0.2535(3) 0.0273(6) Uani d S 1 .
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'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
_geom_angle_publ_flag
O1 V O2 . . 174.23(12) y
O1 V O3 . . 99.97(8) y
O1 V O4 . . 96.43(8) y
O3 V O4 . . 163.52(7) y
O1 V O3 . 4_565 99.97(8) ?
O3 V O3 . 4_565 87.98(10) ?
O1 V O4 . 4_565 96.43(8) ?
O3 V O4 . 4_565 87.56(8) ?
O3 V O4 4_565 4_565 163.52(7) ?
O3 V O4 4_565 . 87.56(8) ?
O4 V O4 4_565 . 92.28(10) ?
O3 V O2 . . 84.15(7) y
O3 V O2 4_565 . 84.15(7) ?
O4 V O2 4_565 . 79.62(7) ?
O4 V O2 . . 79.62(7) y
V O2 H2 . . 125.6 ?
V O3 H3A . . 126.4 ?
V O3 H3B . . 121.6 ?
H3A O3 H3B . . 105.2 ?
V O4 H4A . . 117.7 ?
V O4 H4B . . 120.1 ?
H4A O4 H4B . . 108.8 ?
F11 C1 F11 . 4_575 76(2) ?
F11 C1 F12 . . 116.8(10) ?
F11 C1 F12 4_575 . 116.8(10) ?
F11 C1 F11A . 4_575 104(2) ?
F12 C1 F11A . 4_575 103.6(5) ?
F11 C1 F11A 4_575 . 104(2) ?
F12 C1 F11A . . 103.6(5) ?
F11A C1 F11A 4_575 . 131.3(18) ?
F11 C1 S1 . . 117.0(7) ?
F11 C1 S1 4_575 . 117.0(7) ?
F12 C1 S1 . . 109.6(4) ?
F11A C1 S1 4_575 . 103.9(8) ?
F11A C1 S1 . . 103.9(8) ?
C1 F11 F11 . 4_575 51.8(12) ?
O11 S1 O11 4_575 . 114.43(15) ?
O11 S1 O12 4_575 . 114.17(8) ?
O11 S1 O12 . . 114.17(8) ?
O11 S1 C1 4_575 . 103.54(12) ?
O11 S1 C1 . . 103.54(12) ?
O12 S1 C1 . . 105.3(2) ?
F21 C2 F21 4_565 . 108.9(3) ?
F21 C2 F22 4_565 . 108.9(2) ?
F21 C2 F22 . . 108.9(2) ?
F21 C2 S2 4_565 . 110.01(19) ?
F21 C2 S2 . . 110.01(19) ?
F22 C2 S2 . . 110.1(2) ?
O22 S2 O21 . . 114.64(8) ?
O22 S2 O21 . 4_565 114.64(8) ?
O21 S2 O21 . 4_565 113.08(13) ?
O22 S2 C2 . . 105.37(15) ?
O21 S2 C2 . . 103.74(9) ?
O21 S2 C2 4_565 . 103.74(9) ?
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 O1 . 1.577(2) y
V O2 . 2.175(2) y
V O3 . 2.0262(18) y
V O4 . 2.0277(17) y
V O3 4_565 2.0262(18) ?
V O4 4_565 2.0277(17) ?
O2 H2 . 0.8768 ?
O3 H3A . 0.9008 ?
O3 H3B . 0.8276 ?
O4 H4A . 0.8768 ?
O4 H4B . 0.8966 ?
C1 F11 . 1.245(13) ?
C1 F12 . 1.318(5) ?
C1 F11A 4_575 1.394(14) ?
C1 F11A . 1.394(14) ?
C1 S1 . 1.814(5) ?
S1 O11 4_575 1.4381(19) ?
S1 O11 . 1.4382(19) ?
S1 O12 . 1.448(2) ?
C2 F21 4_565 1.319(3) ?
C2 F21 . 1.319(3) ?
C2 F22 . 1.323(4) ?
C2 S2 . 1.830(4) ?
S2 O22 . 1.430(2) ?
S2 O21 . 1.4512(18) ?
S2 O21 4_565 1.4512(17) ?
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
O2 H2 O11 . 0.88 2.02 2.834(2) 154.3
O3 H3A O12 . 0.90 1.96 2.808(2) 156.8
O3 H3B O21 . 0.83 1.95 2.725(2) 155.5
O4 H4B O11 2_645 0.90 1.87 2.752(2) 167.5
O4 H4A O21 2_545 0.88 1.87 2.734(2) 166.1
