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_4312406
_publ_section_title
;
 Novel Mixed-Valence Heteropolyoxometalates: A Molybdenum Diphosphonate
 Anion [MoV7MoVIO16(O3PPhPO3H)4]3- and Its One- and Two-Dimensional
 Assemblies
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_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            'C33 H33 Mo8 N6 O40 P8'
_chemical_formula_weight         2168.93
_chemical_name_common            (ImH2)3(1)
_chemical_name_systematic
; 
(C3N2H5)4[Mo8O16(O3P-C6H4-PO3H)4] 
;
_space_group_IT_number           41
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'A 2 -2ab'
_symmetry_space_group_name_H-M   'A b a 2'
_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                   16.675(4)
_cell_length_b                   17.2380(10)
_cell_length_c                   24.881(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      8
_cell_volume                     7151.9(19)
_computing_cell_refinement       CAD4_(Enraf-Nonius,_1977
_computing_data_collection       CAD4_(Enraf-Nonius,_1977
_computing_data_reduction        SDS_Package_(Enraf-Nonius,_1985
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  Enraf-Nonius_CAD4
_diffrn_measurement_method       omega-2theta
_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  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0552
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            6432
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.36
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.627
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.547
_exptl_absorpt_correction_type   semiempirical
_exptl_absorpt_process_details   psi-scans
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.014
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4196
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.212
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.152
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(6)
_refine_ls_extinction_coef       0.00010(4)
_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   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         6265
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0792P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1237
_reflns_number_gt                5401
_reflns_number_total             6265
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034505csi20030819_103535_1.cif
_cod_data_source_block           (ImH2)3(1)
_cod_depositor_comments
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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               4312406