The syntheses, structures and characterizations of a series of frameworks constructed from polyoxometalates, metals and organic units
Wang, Yan; Wang, La-Mei; Li, Zhi-Fang; Hu, Yang-Yang; Li, Guang-Hua; Xiao, Li-Na; Wang, Tie-gang; Zheng, Da-Fang; Cui, Xiao-Bing; Xu, Ji-Qing; CrystEngComm 15 (2013) 285–; doi:10.1039/c2ce26477c

data_7209063
_publ_section_title
;
 The syntheses, structures and characterizations of a series of frameworks
 constructed from polyoxometalates, metals and organic units
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              285
_journal_paper_doi               10.1039/c2ce26477c
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C50 H48 Br2 N10 Ni2 O43 Si W12'
_chemical_formula_weight         3988.51
_chemical_name_systematic
;
?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 104.651(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.2049(9)
_cell_length_b                   14.9418(7)
_cell_length_c                   20.5766(12)
_cell_measurement_temperature    293(2)
_cell_volume                     3927.9(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0648
_diffrn_reflns_av_sigmaI/netI    0.1374
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28474
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.02
_exptl_absorpt_coefficient_mu    19.087
_exptl_absorpt_correction_T_max  0.1246
_exptl_absorpt_correction_T_min  0.0625
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
Higashi, T. (1995). Program for Absorption Correction.
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_density_diffrn    3.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3580
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.19
_refine_diff_density_max         7.564
_refine_diff_density_min         -4.120
_refine_diff_density_rms         0.510
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.50(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1082
_refine_ls_number_reflns         18944
_refine_ls_number_restraints     344
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1266
_refine_ls_R_factor_gt           0.0772
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1044P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1844
_refine_ls_wR_factor_ref         0.2161
_reflns_number_gt                12665
_reflns_number_total             18944
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce26477c.txt
_cod_data_source_block           k_3
_cod_original_sg_symbol_H-M      p2(1)
_cod_database_code               7209063