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_4312408
_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            'C45 H42 Mo10 N3 O53 P10'
_chemical_formula_weight         2747.97
_chemical_name_common            (PyH)3(3)
_chemical_name_systematic
; 
 (C5NH6)3[{Mo8O16(O3P-C6H4-PO3)4}{Mo2O2(OH)2(HO3P-C6H4-PO3H)}].3H2O
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                   19.0574(15)
_cell_length_b                   20.4023(16)
_cell_length_c                   20.6598(16)
_cell_measurement_temperature    100(2)
_cell_volume                     8032.8(11)
_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 0.965
_diffrn_measured_fraction_theta_max 0.965
_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  0.0782
_diffrn_reflns_av_sigmaI/netI    0.0661
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            86047
_diffrn_reflns_theta_full        28.67
_diffrn_reflns_theta_max         28.67
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    1.813
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.911211
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             5236
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.099
_refine_diff_density_min         -0.897
_refine_diff_density_rms         0.187
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.62(3)
_refine_ls_extinction_coef       0.000010(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   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1090
_refine_ls_number_reflns         19816
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0511
_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^)+(0.0503P)^2^+32.1447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1208
_reflns_number_gt                17191
_reflns_number_total             19816
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034505csi20030819_103535_3.cif
_cod_data_source_block           (PyH)3(3)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_database_code               4312408