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_1561582
_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            'C13.71 H6.86 O7.86 V'
_chemical_formula_weight         348.27
_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-2013
_cell_angle_alpha                90
_cell_angle_beta                 105.9140(8)
_cell_angle_gamma                90
_cell_formula_units_Z            28
_cell_length_a                   23.903(2)
_cell_length_b                   17.1907(15)
_cell_length_c                   25.722(2)
_cell_measurement_temperature    296(2)
_cell_volume                     10164.3(15)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       'narrow frame'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            64053
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.277
_diffrn_reflns_theta_min         1.443
_exptl_absorpt_coefficient_mu    0.721
_exptl_absorpt_correction_T_max  0.737
_exptl_absorpt_correction_T_min  0.614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_description       prism
_exptl_crystal_F_000             4900
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.344(18)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2798
_refine_ls_number_reflns         36260
_refine_ls_number_restraints     3874
_refine_ls_restrained_S_all      0.939
_refine_ls_R_factor_all          0.1481
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          1.103
_refine_ls_shift/su_mean         0.166
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0101P)^2^+9.9518P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0964
_reflns_Friedel_coverage         0.941
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.959
_reflns_number_gt                7411
_reflns_number_total             36260
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2016-236-230.cif
_cod_data_source_block           VObdc
_cod_original_cell_volume        10164.2(16)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1561582