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_2017525
_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 V2 O3 (P O4) (H P O4)'
_chemical_formula_moiety         'Cs2 O11 P2 V2'
_chemical_formula_sum            'Cs2 O11 P2 V2'
_chemical_formula_weight         605.64
_chemical_name_systematic
;
Dicaesium divanadium trioxide phosphate hydrogenphosphate
;
_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
_cell_angle_alpha                90.000
_cell_angle_beta                 99.0920(10)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   8.9180(2)
_cell_length_b                   16.9479(4)
_cell_length_c                   7.21990(10)
_cell_measurement_reflns_used    19026
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      34.97
_cell_measurement_theta_min      2.91
_cell_volume                     1077.52(4)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            18070
_diffrn_reflns_theta_full        36.90
_diffrn_reflns_theta_max         36.90
_diffrn_reflns_theta_min         3.59
_exptl_absorpt_coefficient_mu    8.738
_exptl_absorpt_correction_T_max  0.277
_exptl_absorpt_correction_T_min  0.251
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2002)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.733
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.147
_refine_diff_density_max         1.697
_refine_diff_density_min         -2.533
_refine_ls_extinction_coef       8.74
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         5051
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0328
_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/[\s^2^(Fo^2^)+(0.0137P)^2^+2.8067P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0526
_refine_ls_wR_factor_ref         0.0548
_reflns_number_gt                4170
_reflns_number_total             5051
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sq3221.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2017525
_cod_database_fobs_code          2017525