Cobalt(II)/Nickel(II)-Centered Keggin-Type Heteropolymolybdates: Syntheses, Crystal Structures, Magnetic and Electrochemical Properties
Guang-Gang Gao; Lin Xu; Wen-Ju Wang; Xiao-Shu Qu; Hong Liu; Yan-Yan Yang; Inorganic Chemistry 47 (2008) 2325–2333; doi:10.1021/ic700797v

data_4303974
_publ_section_title
;
Cobalt(II)/Nickel(II)-Centered Keggin-Type Heteropolymolybdates: Syntheses,
Crystal Structures, Magnetic and Electrochemical Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2325
_journal_page_last               2333
_journal_paper_doi               10.1021/ic700797v
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety
;
Co Mo12 O40, 6(C3 H5 N2), 10(H2 O) 
;
_chemical_formula_sum            'C18 H50 Co Mo12 N12 O50'
_chemical_formula_weight         2444.85
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           69
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-F 2 2'
_symmetry_space_group_name_H-M   'F m m m'
_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                   13.043(2)
_cell_length_b                   21.364(3)
_cell_length_c                   21.676(3)
_cell_measurement_reflns_used    3762
_cell_measurement_temperature    185(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.80
_cell_volume                     6040.0(15)
_computing_cell_refinement       'SMART (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 1997)'
_diffrn_ambient_temperature      185(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Smart CCD Apex II'
_diffrn_measurement_method       'omega and phi'
_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  0.0828
_diffrn_reflns_av_sigmaI/netI    0.0749
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            7468
_diffrn_reflns_theta_full        26.03
_diffrn_reflns_theta_max         26.03
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    2.788
_exptl_absorpt_correction_T_max  0.740
_exptl_absorpt_correction_T_min  0.570
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2002)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.667
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4612
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.112
_refine_diff_density_max         1.180
_refine_diff_density_min         -1.148
_refine_diff_density_rms         0.129
_refine_ls_extinction_coef       0.00038(7)
_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   0.957
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         1632
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.1114
_refine_ls_R_factor_gt           0.0590
_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^)+(0.1059P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1264
_refine_ls_wR_factor_ref         0.1440
_reflns_number_gt                1020
_reflns_number_total             1632
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700797v-file003.cif
_cod_data_source_block           CoMo12
_cod_database_code               4303974