Synthesis and Characterization of Cs5P[Mo4O14(OH)]2.2H2O: A New Molybdophosphate Cluster with Face-Sharing MoO6Octahedra
Eddy Dumas; Slavi C. Sevov; Inorganic Chemistry 41 (2002) 144–146; doi:10.1021/ic010900w

data_4317406
_publ_section_title
;
 Synthesis and Characterization of Cs5P[Mo4O14(OH)]2.2H2O: A New
 Molybdophosphate Cluster with Face-Sharing MoO6Octahedra
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              144
_journal_page_last               146
_journal_paper_doi               10.1021/ic010900w
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         Cs5PMo8032H6
_chemical_formula_sum            'Cs5 H6 Mo8 O32 P'
_chemical_formula_weight         1981.08
_chemical_melting_point          ?
_chemical_name_common            Cs5PMo8032H6
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8151(6)
_cell_length_b                   23.1028(16)
_cell_length_c                   16.0683(11)
_cell_measurement_reflns_used    577
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      56.497
_cell_measurement_theta_min      4.343
_cell_volume                     3272.4(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega 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  0.0246
_diffrn_reflns_av_sigmaI/netI    0.0142
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17957
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.47
_exptl_absorpt_coefficient_mu    8.600
_exptl_absorpt_correction_T_max  0.6264
_exptl_absorpt_correction_T_min  0.4251
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.021
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             3552
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.958
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       0.000177(11)
_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   1.146
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         2235
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0208
_refine_ls_R_factor_gt           0.0191
_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^)+(0.0228P)^2^+7.7391P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0472
_refine_ls_wR_factor_ref         0.0480
_reflns_number_gt                2113
_reflns_number_total             2235
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010900w.cif
_cod_data_source_block           Cs5PMo8032H6
_cod_depositor_comments
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The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_formula_sum        'H6 Cs5 Mo8 O32 P'
_cod_database_code               4317406