Novel Mixed-Valence Heteropolyoxometalates: A Molybdenum Diphosphonate Anion [MoV7MoVIO16(O3PPhPO3H)4]3- and Its One- and Two-Dimensional Assemblies
Nathalie Calin; Slavi C. Sevov; Inorganic Chemistry 42 (2003) 7304–7308; doi:10.1021/ic034505c

data_4312407
_publ_section_title
;
 Novel Mixed-Valence Heteropolyoxometalates: A Molybdenum Diphosphonate
 Anion [MoV7MoVIO16(O3PPhPO3H)4]3- and Its One- and Two-Dimensional
 Assemblies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7304
_journal_page_last               7308
_journal_paper_doi               10.1021/ic034505c
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C50 H50 Mo10 N4 O56 P10'
_chemical_formula_weight         2881.11
_chemical_name_common            (PyH)4(2)
_chemical_name_systematic
; 
 (C5NH6)4[{Mo8O16(O3P-C6H4-PO3)2(O3P-C6H4-PO3H)2}
 {Mo2O4(OH)(HO3P-C6H4-PO3H)}].5H2O 
;
_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                 118.7087(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.8506(9)
_cell_length_b                   22.8656(10)
_cell_length_c                   21.1403(9)
_cell_measurement_temperature    100(2)
_cell_volume                     8839.9(7)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0477
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            94028
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    1.656
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7981
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.139
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5484
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.05
_refine_diff_density_max         4.602
_refine_diff_density_min         -6.939
_refine_diff_density_rms         0.252
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1029
_refine_ls_number_reflns         21960
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0726
_refine_ls_shift/su_max          0.230
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0825P)^2^+179.3759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1863
_refine_ls_wR_factor_ref         0.1980
_reflns_number_gt                17961
_reflns_number_total             21960
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034505csi20030819_103535_2.cif
_cod_data_source_block           (PyH)4(2)
_cod_depositor_comments
;
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 
;
_cod_database_code               4312407