Two caesium vanadium hydrogenphosphates with tunnelled structures: Cs~2~V~2~O~3~(PO~4~)(HPO~4~) and Cs~2~[(VO)~3~(HPO~4~)~4~(H~2~O)]·H~2~O
Gautier, Romain; Colin, Jean-François; Le Fur, Eric; Acta Crystallographica Section C 66 (2010) i12–i15; doi:10.1107/S010827010905433X

data_2017524
_publ_section_title
;
 Two caesium vanadium hydrogenphosphates with tunnelled structures:
 Cs~2~V~2~O~3~(PO~4~)(HPO~4~) and
 Cs~2~[(VO)~3~(HPO~4~)~4~(H~2~O)]&#x00B7;H~2~O
;
_journal_coeditor_code           SQ3221
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              i12
_journal_page_last               i15
_journal_paper_doi               10.1107/S010827010905433X
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'Cs2 [(V O)3 (H P O4)4 (H 2O)], H2 O'
_chemical_formula_moiety         'Cs2 O21 P4 V3'
_chemical_formula_sum            'Cs2 O21 P4 V3'
_chemical_formula_weight         878.52
_chemical_name_systematic
;
dicaesium tris[oxidovanadate(IV)] hydrogenphosphate dihydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000
_cell_angle_beta                 96.7859(6)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   12.54650(10)
_cell_length_b                   11.91810(10)
_cell_length_c                   12.65310(10)
_cell_measurement_reflns_used    29575
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      42.11
_cell_measurement_theta_min      2.91
_cell_volume                     1878.77(3)
_computing_cell_refinement       'DIRAX/LSQ (Duisenberg, 1998)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'EvalCCD (Duisenberg, 1998)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2005)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  '95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_sigmaI/netI    0.0554
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            40158
_diffrn_reflns_theta_full        42.00
_diffrn_reflns_theta_max         42.00
_diffrn_reflns_theta_min         3.24
_exptl_absorpt_coefficient_mu    5.724
_exptl_absorpt_correction_T_max  0.293
_exptl_absorpt_correction_T_min  0.208
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2002)'
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    3.106
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1628
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.19
_refine_diff_density_max         3.640
_refine_diff_density_min         -3.143
_refine_ls_extinction_coef       0.0059(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         12989
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+3.9230P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0952
_reflns_number_gt                9367
_reflns_number_total             12989
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sq3221.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               2017524
_cod_database_fobs_code          2017524