#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/18/2231869.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_2231869
loop_
_publ_author_name
'Yagoubi, Said'
'El Ammari, Lahcen'
'Assani, Abderrazzak'
'Saadi, Mohamed'
_publ_section_title
;
 Thorium divanadate dihydrate, Th(V₂O₇)(H₂O)₂
;
_journal_coeditor_code           FJ2454
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i60
_journal_paper_doi               10.1107/S1600536811039584
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'Th (V2 O7) (H2 O)2'
_chemical_formula_structural     'Th (V2 O7) (H2 O)2'
_chemical_formula_sum            'H4 O9 Th V2'
_chemical_formula_weight         481.95
_chemical_name_common            'Thorium divanadate dihydrate'
_chemical_name_systematic
;
Thorium divanadate dihydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.849(2)
_cell_angle_beta                 74.831(2)
_cell_angle_gamma                85.934(2)
_cell_formula_units_Z            2
_cell_length_a                   7.0432(4)
_cell_length_b                   7.3702(4)
_cell_length_c                   7.7204(4)
_cell_measurement_reflns_used    3576
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      36.00
_cell_measurement_theta_min      2.83
_cell_volume                     378.08(4)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics
'ORTEP-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker X8 APEXII diffractometer'
_diffrn_measurement_method       'φ and 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  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0245
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15216
_diffrn_reflns_theta_full        36.00
_diffrn_reflns_theta_max         36.00
_diffrn_reflns_theta_min         2.83
_exptl_absorpt_coefficient_mu    22.056
_exptl_absorpt_correction_T_max  0.110
_exptl_absorpt_correction_T_min  0.052
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    4.233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.601
_refine_diff_density_min         -1.256
_refine_ls_extinction_coef       0.0083(3)
_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   1.153
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         3576
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0148
_refine_ls_R_factor_gt           0.0142
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0019P)²+0.3878P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0324
_refine_ls_wR_factor_ref         0.0326
_reflns_number_gt                3506
_reflns_number_total             3576
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            fj2454.cif
_cod_data_source_block           I
_cod_database_code               2231869
_cod_database_fobs_code          2231869
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_symmetry_multiplicity
Th Th1 0.358260(9) 0.244262(9) 1.084559(8) 0.00611(3) Uani d . 1 1
V V1 0.79469(5) 0.33646(5) 0.25516(4) 0.00702(6) Uani d . 1 1
V V2 0.72488(5) 0.29521(5) 0.70555(4) 0.00705(6) Uani d . 1 1
O O7 0.6164(2) 0.4536(2) 0.8411(2) 0.0112(3) Uani d . 1 1
O O1 0.6561(2) 0.2001(2) 0.1850(2) 0.0122(3) Uani d . 1 1
O O6 0.6084(3) 0.0958(2) 0.8397(2) 0.0137(3) Uani d . 1 1
O O3 1.0237(2) 0.2469(2) 0.2411(2) 0.0153(3) Uani d . 1 1
O O2 0.7983(3) 0.5430(2) 0.1207(2) 0.0162(3) Uani d . 1 1
O O4 0.6682(3) 0.3462(2) 0.4897(2) 0.0151(3) Uani d . 1 1
O O5 0.9622(3) 0.2782(3) 0.6782(2) 0.0191(3) Uani d . 1 1
O O8 0.2995(3) 0.1801(3) 1.4332(2) 0.0250(4) Uani d . 1 1
H H8A 0.3836 0.1644 1.4984 0.030 Uiso d R 1 1
H H8B 0.1908 0.2063 1.5061 0.030 Uiso d R 1 1
O O9 0.1870(4) 0.1056(3) 0.9082(4) 0.0366(6) Uani d . 1 1
H H9A 0.2211 0.0097 0.8594 0.044 Uiso d R 1 1
H H9B 0.1036 0.1642 0.8519 0.044 Uiso d R 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
Th1 0.00668(4) 0.00456(3) 0.00738(3) 0.00008(2) -0.00182(2) -0.00181(2)
V1 0.00677(13) 0.00767(13) 0.00671(12) -0.00029(10) -0.00215(10) -0.00106(10)
V2 0.00842(13) 0.00610(13) 0.00644(12) 0.00028(10) -0.00092(10) -0.00219(10)
O7 0.0146(7) 0.0082(6) 0.0112(6) 0.0006(5) -0.0021(5) -0.0050(5)
O1 0.0109(6) 0.0117(7) 0.0160(6) 0.0013(5) -0.0050(5) -0.0054(5)
O6 0.0204(8) 0.0070(6) 0.0129(6) -0.0018(6) -0.0026(6) -0.0016(5)
O3 0.0097(6) 0.0200(8) 0.0139(6) 0.0018(6) -0.0020(5) -0.0006(6)
O2 0.0186(8) 0.0122(7) 0.0176(7) -0.0045(6) -0.0092(6) 0.0049(6)
O4 0.0159(7) 0.0211(8) 0.0084(6) 0.0043(6) -0.0033(5) -0.0046(5)
O5 0.0100(7) 0.0303(10) 0.0163(7) 0.0025(7) -0.0016(6) -0.0063(7)
O8 0.0151(8) 0.0467(13) 0.0123(7) 0.0038(8) -0.0024(6) -0.0066(7)
O9 0.0460(13) 0.0252(10) 0.0645(15) 0.0236(10) -0.0464(13) -0.0327(11)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 '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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Th Th -7.2400 8.8979 '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
O3 Th1 O1 1_456 1_556 133.04(5)
O3 Th1 O2 1_456 2_666 74.96(6)
O1 Th1 O2 1_556 2_666 141.47(6)
O3 Th1 O7 1_456 2_667 87.85(6)
O1 Th1 O7 1_556 2_667 79.21(5)
O2 Th1 O7 2_666 2_667 75.88(6)
O3 Th1 O9 1_456 . 74.46(8)
O1 Th1 O9 1_556 . 139.27(6)
O2 Th1 O9 2_666 . 63.63(7)
O7 Th1 O9 2_667 . 138.65(6)
O3 Th1 O6 1_456 2_657 93.95(6)
O1 Th1 O6 1_556 2_657 77.24(6)
O2 Th1 O6 2_666 2_657 134.16(6)
O7 Th1 O6 2_667 2_657 149.25(5)
O9 Th1 O6 . 2_657 70.53(6)
O3 Th1 O8 1_456 . 66.51(6)
O1 Th1 O8 1_556 . 66.54(6)
O2 Th1 O8 2_666 . 131.90(7)
O7 Th1 O8 2_667 . 75.03(6)
O9 Th1 O8 . . 126.93(8)
O6 Th1 O8 2_657 . 77.61(6)
O3 Th1 O7 1_456 . 140.50(5)
O1 Th1 O7 1_556 . 73.42(5)
O2 Th1 O7 2_666 . 69.92(5)
O7 Th1 O7 2_667 . 66.76(6)
O9 Th1 O7 . . 104.44(8)
O6 Th1 O7 2_657 . 123.52(5)
O8 Th1 O7 . . 128.58(6)
O3 Th1 O6 1_456 . 142.46(6)
O1 Th1 O6 1_556 . 74.59(5)
O2 Th1 O6 2_666 . 97.58(6)
O7 Th1 O6 2_667 . 126.68(5)
O9 Th1 O6 . . 69.48(7)
O6 Th1 O6 2_657 . 64.61(6)
O8 Th1 O6 . . 130.52(6)
O7 Th1 O6 . . 61.59(5)
O2 V1 O3 . . 111.26(9)
O2 V1 O1 . . 106.38(8)
O3 V1 O1 . . 110.92(8)
O2 V1 O4 . . 110.99(9)
O3 V1 O4 . . 111.03(8)
O1 V1 O4 . . 106.04(8)
O5 V2 O6 . . 111.61(9)
O5 V2 O7 . . 112.45(9)
O6 V2 O7 . . 99.47(8)
O5 V2 O4 . . 110.14(8)
O6 V2 O4 . . 110.71(8)
O7 V2 O4 . . 112.08(8)
V2 O4 V1 . . 136.90(10)
H8A O8 H8B . . 104.5
H9A O9 H9B . . 104.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Th1 O3 1_456 2.3508(16)
Th1 O1 1_556 2.3988(15)
Th1 O2 2_666 2.4104(15)
Th1 O7 2_667 2.4430(16)
Th1 O9 . 2.4440(19)
Th1 O6 2_657 2.4598(16)
Th1 O8 . 2.5593(17)
Th1 O7 . 2.5706(16)
Th1 O6 . 2.5937(17)
V1 O2 . 1.6498(16)
V1 O3 . 1.6845(16)
V1 O1 . 1.7037(16)
V1 O4 . 1.8109(16)
V2 O5 . 1.6285(17)
V2 O6 . 1.7296(16)
V2 O7 . 1.7351(16)
V2 O4 . 1.7722(15)
O8 H8A . 0.8599
O8 H8B . 0.8599
O9 H9A . 0.8600
O9 H9B . 0.8600
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
O8 H8A O4 1_556 0.86 2.47 3.114(3) 133
O8 H8B O5 1_456 0.86 1.92 2.779(3) 175
O9 H9A O1 2_656 0.86 1.77 2.594(3) 160
O9 H9B O5 1_455 0.86 1.90 2.741(3) 166
