#------------------------------------------------------------------------------
#$Date: 2016-08-10 04:02:38 +0300 (Wed, 10 Aug 2016) $
#$Revision: 185712 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/18/2241808.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_2241808
loop_
_publ_author_name
'Kobsch, Anaïs'
'Downs, Robert T.'
'Domanik, Kenneth J.'
_publ_section_title
;
 Redetermination of metarossite, CaV⁵⁺₂O₆·2H₂O
;
_journal_coeditor_code           WM5311
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1280
_journal_page_last               1284
_journal_paper_doi               10.1107/S2056989016012433
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          'Ca V2 O6, 2H2 O'
_chemical_formula_moiety         'Ca V2 O6, 2H2 O'
_chemical_formula_sum            'Ca H4 O8 V2'
_chemical_formula_weight         273.99
_chemical_name_systematic        'Calcium vanadium (V) oxide dihydrate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                93.166(4)
_cell_angle_beta                 96.548(4)
_cell_angle_gamma                105.883(4)
_cell_formula_units_Z            2
_cell_length_a                   6.2059(4)
_cell_length_b                   7.0635(4)
_cell_length_c                   7.7516(5)
_cell_measurement_reflns_used    1255
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.8325
_cell_measurement_theta_min      2.656
_cell_volume                     323.36(4)
_computing_cell_refinement
;
SAINT (Bruker, 2004)
;
_computing_data_collection
;
APEX2 (Bruker, 2004)
;
_computing_data_reduction
;
SAINT (Bruker, 2004)
;
_computing_molecular_graphics
;
XtalDraw (Downs & Hall-Wallace, 2003)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5576
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.498
_diffrn_reflns_theta_min         2.656
_exptl_absorpt_coefficient_mu    3.682
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2004)
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    2.814
_exptl_crystal_description       Platy
_exptl_crystal_F_000             268
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.581
_refine_ls_extinction_coef       0.005(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         2075
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0318P)²+0.0696P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0760
_reflns_number_gt                1508
_reflns_number_total             2075
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            wm5311sup1.cif
_cod_data_source_block           I
_cod_database_code               2241808
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.783
_shelx_estimated_absorpt_t_max   0.809
loop_
_space_group_symop_operation_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_occupancy
Ca Ca 0.76199(10) 0.46286(9) 0.14933(8) 0.01285(14) Uani d 1
V V1 0.44824(9) 0.10219(7) 0.33438(6) 0.01068(13) Uani d 1
V V2 0.37329(8) 0.58264(7) 0.34629(6) 0.01004(13) Uani d 1
O O1 0.4051(4) 0.8480(3) 0.4170(3) 0.0137(4) Uani d 1
O O2 0.5250(3) 0.3869(3) 0.3867(3) 0.0106(4) Uani d 1
O OW3 0.8519(5) 0.7632(4) 0.3671(4) 0.0236(6) Uani d 1
O O4 0.1030(3) 0.4726(3) 0.3330(3) 0.0157(5) Uani d 1
O O5 0.1896(4) 0.0684(3) 0.2322(3) 0.0207(5) Uani d 1
O O6 0.6214(4) 0.1115(3) 0.1910(3) 0.0232(5) Uani d 1
O O7 0.4308(4) 0.5998(3) 0.1408(3) 0.0155(5) Uani d 1
O OW8 0.0045(4) 0.7225(3) 0.0059(3) 0.0164(5) Uani d 1
H H1 0.937(8) 0.747(6) 0.444(6) 0.040 Uiso d 1
H H2 0.900(8) 0.856(7) 0.332(6) 0.040 Uiso d 1
H H3 0.078(8) 0.808(7) 0.066(6) 0.040 Uiso d 1
H H4 -0.069(7) 0.766(6) -0.073(6) 0.040 Uiso d 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Ca Ca 0.2262 0.3064 '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'
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
O7 Ca O4 2_665 1_655 145.60(8)
O7 Ca OW8 2_665 1_655 79.03(8)
O4 Ca OW8 1_655 1_655 84.88(8)
O7 Ca O6 2_665 . 89.84(8)
O4 Ca O6 1_655 . 88.49(8)
OW8 Ca O6 1_655 . 148.85(8)
O7 Ca O2 2_665 . 116.63(7)
O4 Ca O2 1_655 . 93.49(7)
OW8 Ca O2 1_655 . 145.90(8)
O6 Ca O2 . . 64.79(7)
O7 Ca O7 2_665 . 72.07(8)
O4 Ca O7 1_655 . 140.72(7)
OW8 Ca O7 1_655 . 97.51(8)
O6 Ca O7 . . 106.65(8)
O2 Ca O7 . . 63.17(7)
O7 Ca OW3 2_665 . 131.12(9)
O4 Ca OW3 1_655 . 72.51(9)
OW8 Ca OW3 1_655 . 76.53(8)
O6 Ca OW3 . . 129.97(8)
O2 Ca OW3 . . 70.58(8)
O7 Ca OW3 . . 70.05(8)
O7 Ca OW8 2_665 2_665 77.53(7)
O4 Ca OW8 1_655 2_665 69.34(7)
OW8 Ca OW8 1_655 2_665 77.39(8)
O6 Ca OW8 . 2_665 71.80(7)
O2 Ca OW8 . 2_665 133.65(7)
O7 Ca OW8 . 2_665 149.58(7)
OW3 Ca OW8 . 2_665 135.12(8)
O6 V1 O5 . . 109.11(13)
O6 V1 O1 . 1_545 105.21(11)
O5 V1 O1 . 1_545 97.89(11)
O6 V1 O2 . . 94.99(10)
O5 V1 O2 . . 97.89(10)
O1 V1 O2 1_545 . 148.57(9)
O6 V1 O1 . 2_666 114.83(11)
O5 V1 O1 . 2_666 135.88(11)
O1 V1 O1 1_545 2_666 74.72(9)
O2 V1 O1 . 2_666 75.01(8)
O4 V2 O7 . . 106.24(11)
O4 V2 O1 . . 105.17(10)
O7 V2 O1 . . 100.84(10)
O4 V2 O2 . . 106.81(10)
O7 V2 O2 . . 93.48(10)
O1 V2 O2 . . 139.47(9)
O4 V2 O2 . 2_666 102.14(10)
O7 V2 O2 . 2_666 151.38(10)
O1 V2 O2 . 2_666 74.79(8)
O2 V2 O2 . 2_666 74.69(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Ca O7 2_665 2.381(2)
Ca O4 1_655 2.394(2)
Ca OW8 1_655 2.441(2)
Ca O6 . 2.448(2)
Ca O2 . 2.476(2)
Ca O7 . 2.496(2)
Ca OW3 . 2.530(3)
Ca OW8 2_665 2.554(2)
V1 O6 . 1.623(2)
V1 O5 . 1.655(2)
V1 O1 1_545 1.899(2)
V1 O2 . 1.943(2)
V1 O1 2_666 2.004(2)
V1 V1 2_656 3.1033(10)
V1 V2 2_666 3.1187(7)
V2 O4 . 1.633(2)
V2 O7 . 1.675(2)
V2 O1 . 1.874(2)
V2 O2 . 1.895(2)
V2 O2 2_666 2.075(2)
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
OW3 H1 O4 2_666 0.78(5) 2.37(5) 2.965(4) 133(4)
OW3 H2 O5 1_665 0.72(4) 2.25(5) 2.900(3) 150(5)
OW8 H3 O5 1_565 0.75(4) 2.09(5) 2.810(3) 162(5)
OW8 H4 O5 2_565 0.84(4) 1.97(5) 2.794(3) 166(4)

_cod_database_fobs_code 2241808
