#------------------------------------------------------------------------------
#$Date: 2016-02-14 15:26:36 +0100 (dom 14 de feb de 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/76/2017690.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_2017690
loop_
_publ_author_name
'Harrison, William T. A.'
_publ_section_title
;
 [VO(SeO₃)(H₂O)₂]·0.5H₂O
;
_journal_coeditor_code           SQ3246
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              i61
_journal_page_last               i63
_journal_paper_doi               10.1107/S0108270110016707
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[V O (Se O3) (H2 O)2], 0.5H2 O'
_chemical_formula_moiety         'H4 O6 Se V, 0.5(H2 O)'
_chemical_formula_sum            'H5 O6.5 Se V'
_chemical_formula_weight         238.9
_chemical_name_systematic
;
poly[[diaquaoxido[μ₃-trioxidoseleato(2-)]vanadium(IV)] hemihydrate]
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 116.443(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.7819(13)
_cell_length_b                   6.2881(4)
_cell_length_c                   10.5581(4)
_cell_measurement_reflns_used    1307
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     1116.48(12)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997) and SORTAV
(Blessing, 1995)
;
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       ω
_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  0.0352
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6097
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         3.46
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    8.258
_exptl_absorpt_correction_T_max  0.558
_exptl_absorpt_correction_T_min  0.289
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2003)'
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    2.843
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.586
_refine_ls_extinction_coef       0.00084(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         1276
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0209P)²+3.7270P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0518
_refine_ls_wR_factor_ref         0.0541
_reflns_number_gt                1133
_reflns_number_total             1276
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sq3246.cif
_cod_data_source_block           I
_cod_original_cell_volume        1116.48(11)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'H5 O6.5 Se1 V1'
_cod_database_code               2017690
_cod_database_fobs_code          2017690
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_disorder_assembly
_atom_site_disorder_group
V V1 0.13707(3) 0.20376(7) 0.10551(5) 0.00758(13) Uani d . 1 . .
Se Se1 0.301049(15) 0.21533(4) 0.38827(3) 0.00773(11) Uani d . 1 . .
O O1 0.35664(11) -0.0024(3) 0.4528(2) 0.0137(4) Uani d . 1 . .
O O2 0.25565(11) 0.1678(3) 0.20962(19) 0.0098(4) Uani d . 1 . .
O O3 0.37527(10) 0.3863(3) 0.40497(19) 0.0107(4) Uani d . 1 . .
O O4 0.02336(12) 0.2178(3) -0.0511(2) 0.0133(4) Uani d . 1 . .
H H1 0.0149 0.3160 -0.1073 0.016 Uiso d R 1 . .
H H2 -0.0208 0.1901 -0.0588 0.016 Uiso d R 1 . .
O O5 0.12003(12) 0.2360(3) 0.2411(2) 0.0128(4) Uani d . 1 . .
O O6 0.16168(11) 0.1385(3) -0.07887(19) 0.0131(4) Uani d . 1 . .
H H3 0.1346 0.0576 -0.1430 0.016 Uiso d R 1 . .
H H4 0.1819 0.2161 -0.1166 0.016 Uiso d R 1 . .
O O7 0.0000 0.4909(4) 0.2500 0.0128(6) Uani d S 1 . .
H H5 0.0378 0.4115 0.2702 0.015 Uiso d R 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 0.0074(2) 0.0066(3) 0.0087(3) 0.00051(16) 0.00358(18) 0.00006(16)
Se1 0.00737(16) 0.00703(17) 0.00867(17) -0.00025(10) 0.00345(11) -0.00030(10)
O1 0.0144(10) 0.0069(10) 0.0133(10) 0.0018(8) 0.0005(8) -0.0010(8)
O2 0.0087(10) 0.0123(10) 0.0082(10) -0.0007(7) 0.0036(8) -0.0009(7)
O3 0.0075(9) 0.0075(10) 0.0165(10) -0.0015(7) 0.0048(8) -0.0004(7)
O4 0.0067(10) 0.0144(11) 0.0169(11) -0.0002(7) 0.0036(8) 0.0057(8)
O5 0.0122(10) 0.0145(11) 0.0125(10) 0.0013(8) 0.0061(8) 0.0006(8)
O6 0.0162(10) 0.0139(10) 0.0124(10) -0.0072(8) 0.0092(8) -0.0044(8)
O7 0.0087(14) 0.0131(15) 0.0150(14) 0.000 0.0038(11) 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'
Se Se -0.0929 2.2259 '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'
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
O5 V1 O1 . 4 102.87(9) ?
O5 V1 O3 . 4_545 96.34(9) ?
O1 V1 O3 4 4_545 159.77(8) ?
O5 V1 O2 . . 97.95(9) ?
O1 V1 O2 4 . 94.04(8) ?
O3 V1 O2 4_545 . 89.48(8) ?
O5 V1 O4 . . 99.44(9) ?
O1 V1 O4 4 . 83.84(8) ?
O3 V1 O4 4_545 . 86.85(8) ?
O2 V1 O4 . . 162.52(8) ?
O5 V1 O6 . . 176.58(9) ?
O1 V1 O6 4 . 80.51(8) ?
O3 V1 O6 4_545 . 80.36(7) ?
O2 V1 O6 . . 81.19(7) ?
O4 V1 O6 . . 81.35(8) ?
O1 Se1 O3 . . 98.08(9) ?
O1 Se1 O2 . . 102.70(9) ?
O3 Se1 O2 . . 101.92(9) ?
Se1 O1 V1 . 4_545 139.04(11) ?
Se1 O2 V1 . . 117.97(10) ?
Se1 O3 V1 . 4 123.50(10) ?
V1 O4 H1 . . 114.4 ?
V1 O4 H2 . . 136.3 ?
H1 O4 H2 . . 103.2 ?
V1 O6 H3 . . 122.9 ?
V1 O6 H4 . . 129.3 ?
H3 O6 H4 . . 102.7 ?
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
V1 O5 . 1.613(2) y
V1 O1 4 1.9677(19) y
V1 O3 4_545 2.007(2) y
V1 O2 . 2.0098(19) y
V1 O4 . 2.039(2) y
V1 O6 . 2.2300(18) y
Se1 O1 . 1.6718(19) y
Se1 O3 . 1.7060(18) y
Se1 O2 . 1.7151(18) y
O1 V1 4_545 1.9677(19) ?
O3 V1 4 2.007(2) ?
O4 H1 . 0.8212 ?
O4 H2 . 0.8145 ?
O6 H3 . 0.8179 ?
O6 H4 . 0.8223 ?
O7 H5 . 0.8147 ?
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
O4 H1 O7 5_565 0.82 1.86 2.671(3) 171
O4 H2 O3 8_455 0.81 1.88 2.689(3) 174
O6 H3 O5 6 0.82 2.16 2.906(3) 151
O6 H4 O2 7 0.82 1.97 2.777(3) 165
O7 H5 O5 . 0.81 2.03 2.801(3) 158
