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_4327302
_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            'C6 H82 Li14 Mo8 O86 P12'
_chemical_formula_weight         2767.04
_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                101.2000(10)
_cell_angle_beta                 107.4770(10)
_cell_angle_gamma                108.0670(10)
_cell_formula_units_Z            1
_cell_length_a                   11.85910(10)
_cell_length_b                   11.98120(10)
_cell_length_c                   16.0452(2)
_cell_measurement_temperature    293(2)
_cell_volume                     1960.79(4)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.867
_diffrn_measured_fraction_theta_max 0.867
_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  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13706
_diffrn_reflns_theta_full        29.67
_diffrn_reflns_theta_max         29.67
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    1.602
_exptl_absorpt_correction_T_max  0.7400
_exptl_absorpt_correction_T_min  0.4466
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.310
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1364
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.581
_refine_diff_density_min         -1.313
_refine_diff_density_rms         0.179
_refine_ls_extinction_coef       0.0015(3)
_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   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         9767
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0602P)^2^+13.0206P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1359
_refine_ls_wR_factor_ref         0.1440
_reflns_number_gt                8310
_reflns_number_total             9767
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0604102Bsi20060310_054443_6.cif
_cod_data_source_block           4c
_cod_original_cell_volume        1960.72(3)
_cod_database_code               4327302