[Mo5VMo7VIO30(BPO4)2(O3P-Ph)6]5-: A Phenyl-Substituted Molybdenum(V/VI) Boro-Phosphate Polyoxometalate
Capucine Sassoye; Kieran Norton; Slavi C. Sevov; Inorganic Chemistry 42 (2003) 1652–1655; doi:10.1021/ic020635u

data_4313254
_publ_section_title
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 [Mo5VMo7VIO30(BPO4)2(O3P-Ph)6]5-: A Phenyl-Substituted Molybdenum(V/VI)
 Boro-Phosphate Polyoxometalate
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1652
_journal_page_last               1655
_journal_paper_doi               10.1021/ic020635u
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C51 H55 B2 Mo12 N10 O57 P8'
_chemical_formula_weight         3140.71
_chemical_name_systematic
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(ImH2)5[Mo12O30(BPO4)2(O3P-Ph)6]*H2O 
;
_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_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                 101.293(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.120(3)
_cell_length_b                   13.0426(16)
_cell_length_c                   32.632(4)
_cell_measurement_temperature    293(2)
_cell_volume                     9232(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL-V5.1'
_computing_molecular_graphics    'Bruker SHELXTL-V5.1'
_computing_publication_material  'Bruker SHELXTL-V5.1'
_computing_structure_refinement  'Bruker SHELXTL-V5.1'
_computing_structure_solution    'Bruker SHELXTL-V5.1'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.2330
_diffrn_reflns_av_sigmaI/netI    0.3457
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            123155
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    1.818
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9465
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            dark-blue
_exptl_crystal_density_diffrn    2.260
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle-like
_exptl_crystal_F_000             6084
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.425
_refine_diff_density_min         -1.701
_refine_diff_density_rms         0.375
_refine_ls_extinction_coef       0.00118(3)
_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   0.648
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1252
_refine_ls_number_reflns         21212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.648
_refine_ls_R_factor_all          0.1798
_refine_ls_R_factor_gt           0.0450
_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^)+(0.0761P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1052
_refine_ls_wR_factor_ref         0.1765
_reflns_number_gt                6221
_reflns_number_total             21212
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020635u.cif
_cod_data_source_block           mobphpo
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
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_cod_original_cell_volume        9231.9(19)
_cod_database_code               4313254