Preparation and Characterization of 6-Molybdocobaltate and 6-Molybdoaluminate Cobalt Salts. Evidence of a New Heteropolymolybdate Structure
Catherine Martin; Carole Lamonier; Michel Fournier; Olivier Mentré; Virginie Harlé; Denis Guillaume; Edmond Payen; Inorganic Chemistry 43 (2004) 4636–4644; doi:10.1021/ic0354365

data_4311317
_publ_contact_author_address
;
   Laboratoire de Catalyse de Lille, UMR C.N.R.S N\% 8010,
Universit\'e des Sciences et Technologies de Lille,
 B\^atiment C3, 59650 Villeneuve d?Ascq, France.
;
_publ_contact_author_email       carole.lamonier@univ-lille1.fr
_publ_contact_author_name        'Carole Lamonier'
_publ_section_title
;
 Preparation and Characterization of 6-Molybdocobaltate and
 6-Molybdoaluminate Cobalt Salts. Evidence of a New Heteropolymolybdate
 Structure
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4636
_journal_page_last               4644
_journal_paper_doi               10.1021/ic0354365
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         '(CoMo6O24H6) (Co, 5H2O) (H2O)6 (H3O)'
_chemical_formula_sum            'Co2 H31 Mo6 O36'
_chemical_formula_weight         1294.70
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2bc 2ac'
_symmetry_space_group_name_H-M   'P c a b'
_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            8
_cell_length_a                   11.139(2)
_cell_length_b                   22.960(4)
_cell_length_c                   24.486(5)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.52
_cell_measurement_theta_min      3.55
_cell_volume                     6262(2)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    Diamond
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.463
_diffrn_measured_fraction_theta_max 0.463
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0350
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            25111
_diffrn_reflns_theta_full        29.52
_diffrn_reflns_theta_max         29.52
_diffrn_reflns_theta_min         3.55
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.475
_exptl_crystal_density_diffrn    2.746
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4952
_refine_diff_density_max         1.783
_refine_diff_density_min         -0.790
_refine_diff_density_rms         0.180
_refine_ls_extinction_coef       0.000000(14)
_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   1.108
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         4045
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          1.130
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0495P)^2^+26.9108P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.0924
_reflns_number_gt                4045
_reflns_number_total             4045
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0354365si20040316_122934_2.cif
_cod_data_source_block           como6m
_cod_original_formula_sum        'H31 O36 Mo6 Co2'
_cod_database_code               4311317