Reticular Access to Highly Porous acs-MOFs with Rigid Trigonal Prismatic Linkers for Water Sorption.
Chen, Zhijie; Li, Penghao; Zhang, Xuan; Li, Peng; Wasson, Megan C.; Islamoglu, Timur; Stoddart, J. Fraser; Farha, Omar K.; Journal of the American Chemical Society 141 (2019) 2900–2905; doi:10.1021/jacs.8b13710

data_4128438
_publ_section_title
;
 Reticular Access to Highly Porous acs-MOFs with Rigid Trigonal Prismatic
 Linkers for Water Sorption.
;
_journal_issue                   7
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2900
_journal_page_last               2905
_journal_paper_doi               10.1021/jacs.8b13710
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C62 H32 Cr3 O16'
_chemical_formula_sum            'C62 H32 Cr3 O16'
_chemical_formula_weight         1188.87
_space_group_crystal_system      hexagonal
_space_group_IT_number           187
_space_group_name_Hall           'P -6 2'
_space_group_name_H-M_alt        'P -6 m 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   19.503(2)
_cell_length_b                   19.503(2)
_cell_length_c                   11.1225(17)
_cell_measurement_reflns_used    2125
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      45.36
_cell_measurement_theta_min      2.62
_cell_volume                     3663.8(8)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9757
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        53.389
_diffrn_reflns_theta_max         53.389
_diffrn_reflns_theta_min         2.616
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.030
_exptl_absorpt_correction_T_max  0.7510
_exptl_absorpt_correction_T_min  0.4824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1373 before and 0.0545 after correction. The Ratio of minimum to maximum transmission is 0.6423. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    0.539
_exptl_crystal_description       block
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.145
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.030
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.373(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.939
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         1660
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0812P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1152
_refine_ls_wR_factor_ref         0.1246
_reflns_Friedel_coverage         0.885
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1163
_reflns_number_total             1660
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b13710_si_003.cif
_cod_data_source_block           2
_cod_original_cell_volume        3663.8(9)
_cod_database_code               4128438
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.923
_shelx_estimated_absorpt_t_min   0.823
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.627(18)
 0.373(18)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Rigid bond restraints
 C6, C7, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C6 \\sim C7 \\sim C8: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08
5.a Riding coordinates:
 C9(H9), C4(H4), C3(H3)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7)
;
_shelx_res_checksum              52651
_shelx_hkl_checksum              73280
_shelx_fab_checksum              68352
_olex2_submission_special_instructions 'No special instructions were received'