Crystal structure and catalytic properties of three inorganic‒organic hybrid constructed from heteropolymolybdate and aminopyridine
Deng, Qian; Huang, Yilan; Peng, Zhenshan; Dai, Zengjin; Lin, Minru; Cai, Tiejun; Journal of Solid State Chemistry 200 (2013) 60–69; doi:10.1016/j.jssc.2013.01.003

data_1562702
_publ_section_title
;
 Crystal structure and catalytic properties of three inorganic--organic
 hybrid constructed from heteropolymolybdate and aminopyridine
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              60
_journal_page_last               69
_journal_paper_doi               10.1016/j.jssc.2013.01.003
_journal_volume                  200
_journal_year                    2013
_chemical_formula_sum            'C30 H42 Mo12 N12 O40 Si'
_chemical_formula_weight         2390.13
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   21.584(4)
_cell_length_b                   21.584(4)
_cell_length_c                   10.475(4)
_cell_measurement_reflns_used    4781
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.23
_cell_volume                     4226(2)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.2491
_diffrn_reflns_av_sigmaI/netI    0.1011
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10274
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    2.713
_exptl_absorpt_correction_T_max  0.779
_exptl_absorpt_correction_T_min  0.437
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.817
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3432
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.092
_refine_diff_density_max         1.152
_refine_diff_density_min         -1.318
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         1656
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+190.7104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1689
_refine_ls_wR_factor_ref         0.1756
_reflns_number_gt                1440
_reflns_number_total             1656
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2013-200-60.cif
_cod_data_source_block           hyl10
_cod_original_sg_symbol_H-M      R-3
_cod_original_formula_sum        'C30 H42 Mo12 N12 O40 Si '
_cod_database_code               1562702