The first heteropoly blue-embedded metal‒organic framework: crystal structure, magnetic property and proton conductivity
Li, Chong; Sun, Minghui; Xu, Lin; Wang, Yuchao; Huang, Jiawei; CrystEngComm 18 (2016) 596–; doi:10.1039/C5CE02074C

data_7223529
_publ_section_title
;
 The first heteropoly blue-embedded metal--organic framework: crystal
 structure, magnetic property and proton conductivity
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              596
_journal_paper_doi               10.1039/C5CE02074C
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C92 H168 Cu12 Mo N5 O130 Si W11'
_chemical_formula_weight         5642.14
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_Hall           '-F 4 2 3'
_space_group_name_H-M_alt        'F m -3 m'
_symmetry_space_group_name_Hall  '-F 4 2 3'
_symmetry_space_group_name_H-M   'F m -3 m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-12-11 deposited with the CCDC.
2015-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.232(7)
_cell_length_b                   26.232(7)
_cell_length_c                   26.232(7)
_cell_measurement_reflns_used    2463
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      22.0812
_cell_measurement_theta_min      2.1935
_cell_volume                     18051(8)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  ccd
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0719
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            26304
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.983
_diffrn_reflns_theta_max         24.983
_diffrn_reflns_theta_min         1.345
_exptl_absorpt_coefficient_mu    8.520
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.060
_exptl_crystal_description       block
_exptl_crystal_F_000             10344
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.200
_platon_squeeze_details
;
SQUEEZE was used to mask numerous diffuse solvent water molecules and organic
 cations. The total solvent accessible void as found to contains 2736
 electrons. Based on the calculation results, elemental analysis and TG
 analysis, 3 [Me4N]+ and 24 H2O were directly added in the final molecular
 formula.
;
_refine_diff_density_max         3.049
_refine_diff_density_min         -2.063
_refine_diff_density_rms         0.614
_refine_ls_extinction_coef       0.00018(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         862
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0635
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1581P)^2^+1426.9498P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2109
_refine_ls_wR_factor_ref         0.2330
_reflns_Friedel_coverage         0.000
_reflns_number_gt                768
_reflns_number_total             862
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02074c2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7223529.cif.'
_cod_original_cell_volume        18051(14)
_cod_original_formula_sum        'C92 H168 Cu12 Mo1 N5 O130 Si1 W11'
_cod_database_code               7223529
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.256
_shelx_estimated_absorpt_t_max   0.281
_shelx_res_checksum              34525