Hydrothermal crystal growth and Vernier structures of the metal benzenedicarboxylates MIL-47 and MIL-53 containing guest molecules of benzenecarboxylic acid
Wang, Xiqu; Jacobson, Allan J.; Journal of Solid State Chemistry 236 (2016) 230–235; doi:10.1016/j.jssc.2015.08.014

data_1561581
_publ_section_title
;
 Hydrothermal crystal growth and Vernier structures of the metal
 benzenedicarboxylates MIL-47 and MIL-53 containing guest molecules of
 benzenecarboxylic acid
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              230
_journal_page_last               235
_journal_paper_doi               10.1016/j.jssc.2015.08.014
_journal_volume                  236
_journal_year                    2016
_chemical_formula_sum            'C13.65 H8.24 Ga O7.82'
_chemical_formula_weight         367.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 89.9990(10)
_cell_angle_gamma                90
_cell_formula_units_Z            68
_cell_length_a                   114.562(5)
_cell_length_b                   12.1503(5)
_cell_length_c                   17.4275(7)
_cell_measurement_temperature    296(2)
_cell_volume                     24258.4(18)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  'Bruker ApexII DUO'
_diffrn_measurement_method       'narrow frame'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.1021
_diffrn_reflns_Laue_measured_fraction_full 0.917
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_limit_h_max       133
_diffrn_reflns_limit_h_min       -136
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            223922
_diffrn_reflns_point_group_measured_fraction_full 0.919
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_theta_full        66.694
_diffrn_reflns_theta_max         66.694
_diffrn_reflns_theta_min         0.771
_exptl_absorpt_coefficient_mu    3.028
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5902
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_description       prism
_exptl_crystal_F_000             12492
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         4.492
_refine_diff_density_min         -1.357
_refine_diff_density_rms         0.240
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.56(11)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3049
_refine_ls_number_reflns         73866
_refine_ls_number_restraints     8430
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.2135
_refine_ls_R_factor_gt           0.1473
_refine_ls_shift/su_max          1.064
_refine_ls_shift/su_mean         0.084
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0190P)^2^+360.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3661
_refine_ls_wR_factor_ref         0.3981
_reflns_Friedel_coverage         0.904
_reflns_Friedel_fraction_full    0.920
_reflns_Friedel_fraction_max     0.920
_reflns_number_gt                25802
_reflns_number_total             73866
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2016-236-230.cif
_cod_data_source_block           Ga(bdc)
_cod_original_cell_volume        24258.5(17)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1561581
_shelx_shelxl_version_number     2014/7
_exptl_absorpt_special_details   SADABS