Synthesis and characterization of a novel POM compound containing two different layers stacked alternately
Shi, Shu-Yun; Wang, Yan; Cui, Xiao-Bing; Wang, Guo-Wu; Yang, Guang-Di; Xu, Ji-Qing; Dalton Transactions  (2009) 6099–; doi:10.1039/b906066a

data_7001789
_publ_section_title
;
 Synthesis and characterization of a novel POM compound containing two
 different layers stacked alternately
;
_journal_issue                   31
_journal_name_full               'Dalton Transactions'
_journal_page_first              6099
_journal_paper_doi               10.1039/b906066a
_journal_year                    2009
_chemical_formula_sum            'C5 H41 Mo24 N5 O88.5 Sb4 Si2'
_chemical_formula_weight         4433.17
_chemical_name_systematic
;
?
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 104.37(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.544(4)
_cell_length_b                   20.438(4)
_cell_length_c                   20.551(4)
_cell_measurement_temperature    293(2)
_cell_volume                     8359(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0553
_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       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            33768
_diffrn_reflns_theta_full        26.05
_diffrn_reflns_theta_max         26.05
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    4.889
_exptl_absorpt_correction_T_max  0.2728
_exptl_absorpt_correction_T_min  0.1360
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    3.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             8216
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.36
_refine_diff_density_max         2.326
_refine_diff_density_min         -4.429
_refine_diff_density_rms         0.330
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.52(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1090
_refine_ls_number_reflns         16355
_refine_ls_number_restraints     196
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1675
_refine_ls_wR_factor_ref         0.1775
_reflns_number_gt                12658
_reflns_number_total             16355
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b906066a.txt
_cod_data_source_block           k
_cod_original_sg_symbol_H-M      C2
_cod_original_formula_sum        'C5 H41 Mo24 N5 O88.50 Sb4 Si2'
_cod_database_code               7001789