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_4327303
_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 H104 Mo8 N10 Na2 O74 P8 S2'
_chemical_formula_weight         2602.36
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.2890(10)
_cell_angle_beta                 95.5330(10)
_cell_angle_gamma                96.2130(10)
_cell_formula_units_Z            1
_cell_length_a                   9.6783(2)
_cell_length_b                   14.2098(2)
_cell_length_c                   14.3744(2)
_cell_measurement_temperature    273(2)
_cell_volume                     1945.55(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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      273(2)
_diffrn_measured_fraction_theta_full 0.857
_diffrn_measured_fraction_theta_max 0.857
_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  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0764
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13460
_diffrn_reflns_theta_full        29.89
_diffrn_reflns_theta_max         29.89
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    1.608
_exptl_absorpt_correction_T_max  0.9097
_exptl_absorpt_correction_T_min  0.7606
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    2.221
_exptl_crystal_density_meas      0
_exptl_crystal_F_000             1300
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.959
_refine_diff_density_min         -1.688
_refine_diff_density_rms         0.242
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         9627
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.1127
_refine_ls_R_factor_gt           0.0755
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0862P)^2^+19.4751P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1902
_refine_ls_wR_factor_ref         0.2153
_reflns_number_gt                6858
_reflns_number_total             9627
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0604102Bsi20060310_054443_7.cif
_cod_data_source_block           2d
_cod_database_code               4327303