Hydrothermal Synthesis, Thermal, and Magnetic Data on New Alkaline Vanadium Phosphate My(VO)9+x(PO4)4x(HPO4)12-4x with M = Cs+ (y = 5.29, x = 1) and M = NH4+, Rb+ (y ~ 5, x ~ 1)
E. Le Fur; B. de Villars; J. Tortelier; Y. Pivan; Inorganic Chemistry 40 (2001) 272–276; doi:10.1021/ic000464y

data_4319144
_publ_contact_author
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      Jean Yves Pivan
      Laboratoire de Physicochimie
      Ecole Nationale Superieure de Chimie
      Campus de Beaulieu
      Avenue du General Leclerc
      35000 Rennes 
      France
    Identification number IC000464Y

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_publ_contact_author_email       jean-yves.pivan@ensc-rennes.fr
_publ_section_title
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 Hydrothermal Synthesis, Thermal, and Magnetic Data on New Alkaline
 Vanadium Phosphate My(VO)9+x(PO4)4x(HPO4)12-4x with M = Cs+ (y = 5.29, x
 = 1) and M = NH4+, Rb+ (y ~ 5, x ~ 1)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              272
_journal_page_last               276
_journal_paper_doi               10.1021/ic000464y
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'Cs5.29 O58 P12 V10'
_chemical_formula_weight         2511.80
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.0000(8)
_cell_angle_beta                 109.742(5)
_cell_angle_gamma                90.000(2)
_cell_formula_units_Z            4
_cell_length_a                   21.195(5)
_cell_length_b                   12.2051(8)
_cell_length_c                   20.6230(4)
_cell_measurement_reflns_used    17143
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      60
_cell_measurement_theta_min      2
_cell_volume                     5021.3(12)
_computing_cell_refinement       'DENZO (Otwinowski, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'SCALEPACK (Otwinowski, 1997)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Kappa CCD'
_diffrn_measurement_method       'w-f scans'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0609
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            4430
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    6.077
_exptl_absorpt_correction_T_max  0.873
_exptl_absorpt_correction_T_min  0.751
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            brownish
_exptl_crystal_density_diffrn    3.323
_exptl_crystal_description       plates
_exptl_crystal_F_000             4659
_exptl_crystal_size_max          0.04
_refine_diff_density_max         1.506
_refine_diff_density_min         -1.164
_refine_diff_density_rms         0.184
_refine_ls_extinction_coef       0.00015(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_all   1.093
_refine_ls_goodness_of_fit_obs   1.170
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         4130
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.083
_refine_ls_restrained_S_obs      1.167
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_obs          0.0537
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0191P)^2^+141.2619P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1194
_refine_ls_wR_factor_obs         0.1085
_reflns_number_observed          3267
_reflns_number_total             4430
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000464y.cif
_cod_data_source_block           cs
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0191P)^2^+141.2619P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0191P)^2^+141.2619P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5021.4(12)
_cod_database_code               4319144