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_1562701
_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            'C25 H47 Mo12 N11 O46 Si'
_chemical_formula_weight         2417.10
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n :2'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P 42/n :2'
_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                   14.3504(2)
_cell_length_b                   14.3504(2)
_cell_length_c                   29.0183(6)
_cell_measurement_temperature    293(2)
_cell_volume                     5975.85(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0312
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            34675
_diffrn_reflns_theta_full        27.91
_diffrn_reflns_theta_max         27.91
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    2.566
_exptl_absorpt_correction_T_max  0.5663
_exptl_absorpt_correction_T_min  0.4940
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    2.685
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4636
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.348
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         7124
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0545P)^2^+31.9511P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1268
_refine_ls_wR_factor_ref         0.1462
_reflns_number_gt                4823
_reflns_number_total             7124
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2013-200-60.cif
_cod_data_source_block           hyl2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Tetragonal' was changed to
'tetragonal' in accordance with the built-in table derived from the
CIF Core dictionary named 'cif_core.dic' version 2.4.5 last updated
on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8369 2020-08-20 11:38:08Z andrius 

2022-09-18
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C50 H94 Mo24 N22 O92 Si2'
_cod_original_formula_weight         4834.20
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      P42/n
_cod_database_code               1562701