Synthesis and Characterization of Octa- and Hexanuclear Polyoxomolybdate Wheels: Role of the Inorganic Template and of the Counterion
Anne Dolbecq; Laurent Lisnard; Pierre Mialane; Jérôme Marrot; Marc Bénard; Marie-Madeleine Rohmer; Francis Sécheresse; Inorganic Chemistry 45 (2006) 5898–5910; doi:10.1021/ic060410+

data_4327298
_publ_section_title
;
 Synthesis and Characterization of Octa- and Hexanuclear Polyoxomolybdate
 Wheels: Role of the Inorganic Template and of the Counterion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5898
_journal_page_last               5910
_journal_paper_doi               10.1021/ic060410+
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C4 H108 Mo8 N12 O72 P8 S2'
_chemical_formula_weight         2556.39
_chemical_name_systematic
; 
 ? 
;
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
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_cell_angle_beta                 88.179(3)
_cell_angle_gamma                79.074(3)
_cell_formula_units_Z            2
_cell_length_a                   14.4390(10)
_cell_length_b                   16.3333(9)
_cell_length_c                   16.6096(11)
_cell_measurement_reflns_used    9243
_cell_measurement_temperature    373(2)
_cell_measurement_theta_max      25.40
_cell_measurement_theta_min      2.16
_cell_volume                     3816.6(4)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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      373(2)
_diffrn_detector_area_resol_mean 512x512
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0541
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            176737
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.24
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.626
_exptl_absorpt_correction_T_max  0.9617
_exptl_absorpt_correction_T_min  0.5459
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, V2.10)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.225
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             4192
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.670
_refine_diff_density_min         -1.349
_refine_diff_density_rms         0.284
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     962
_refine_ls_number_reflns         17414
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0528
_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^)+(0.1010P)^2^+16.2725P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1564
_refine_ls_wR_factor_ref         0.1751
_reflns_number_gt                13269
_reflns_number_total             17414
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0604102Bsi20060310_054443_2.cif
_cod_data_source_block           2a
_cod_original_cell_volume        3816.7(4)
_cod_database_code               4327298