A New Organic-Inorganic Hybrid Layered Molybdenum(V) Cobalt Phosphate Constructed from [H24(Mo16O32)Co16(PO4)24(OH)4(C5H4N)2(H2O)6]4- Wheels and 4,4'-Bipyridine Linkers
Kai Yu; Bai-Bin Zhou; Yang Yu; Zhan-Hua Su; Guo-Yu Yang; Inorganic Chemistry 50 (2011) 1862–1867; doi:10.1021/ic1022664

data_4324531
_publ_section_title
;
 A New Organic-Inorganic Hybrid Layered Molybdenum(V) Cobalt Phosphate
 Constructed from [H24(Mo16O32)Co16(PO4)24(OH)4(C5H4N)2(H2O)6]4- Wheels
 and 4,4'-Bipyridine Linkers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1862
_journal_page_last               1867
_journal_paper_doi               10.1021/ic1022664
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C50 H96 Co17 Mo16 N10 Na2 O148 P24'
_chemical_formula_sum            'C50 H96 Co17 Mo16 N10 Na2 O148 P24'
_chemical_formula_weight         6531.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 93.791(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.6825(15)
_cell_length_b                   39.503(4)
_cell_length_c                   17.2763(17)
_cell_measurement_reflns_used    6757
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      22.76
_cell_measurement_theta_min      2.58
_cell_volume                     10679.3(18)
_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 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.1399
_diffrn_reflns_av_sigmaI/netI    0.1680
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            91862
_diffrn_reflns_theta_full        28.42
_diffrn_reflns_theta_max         28.42
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    2.470
_exptl_absorpt_correction_T_max  0.464
_exptl_absorpt_correction_T_min  0.363
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.031
_exptl_crystal_density_meas      2.031
_exptl_crystal_description       block
_exptl_crystal_F_000             6326.0
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.181
_refine_diff_density_min         -1.181
_refine_diff_density_rms         0.396
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1222
_refine_ls_number_reflns         26437
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0587
_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^)+(0.1774P)^2^+504.4958P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1435
_refine_ls_wR_factor_ref         0.1618
_reflns_number_gt                12865
_reflns_number_total             26853
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1022664_si_002.cif
_cod_data_source_block           yuk23_2_0m
_cod_original_cell_volume        10679.4(18)
_cod_database_code               4324531