Trianglamine-Based Supramolecular Organic Framework with Permanent Intrinsic Porosity and Tunable Selectivity.
Chaix, Arnaud; Mouchaham, Georges; Shkurenko, Aleksander; Hoang, Phuong; Moosa, Basem; Bhatt, Prashant M.; Adil, Karim; Salama, Khaled N.; Eddaoudi, Mohamed; Khashab, Niveen M.; Journal of the American Chemical Society 140 (2018) 14571–14575; doi:10.1021/jacs.8b08770

data_4133180
_publ_section_title
;
 Trianglamine-Based Supramolecular Organic Framework with Permanent
 Intrinsic Porosity and Tunable Selectivity.
;
_journal_issue                   44
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14571
_journal_page_last               14575
_journal_paper_doi               10.1021/jacs.8b08770
_journal_volume                  140
_journal_year                    2018
_chemical_absolute_configuration syn
_chemical_formula_moiety         '(C42 H66 N6), 6(Cl 1-), 16.5(H2 O)'
_chemical_formula_sum            'C42 H99 Cl6 N6 O16.5'
_chemical_formula_weight         1164.97
_space_group_crystal_system      trigonal
_space_group_IT_number           150
_space_group_name_Hall           'P 3 2"'
_space_group_name_H-M_alt        'P 3 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   22.378(2)
_cell_length_b                   22.378(2)
_cell_length_c                   7.1487(7)
_cell_measurement_reflns_used    6561
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      66.64
_cell_measurement_theta_min      4.56
_cell_volume                     3100.3(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection
'Bruker APEX2 v2009.3-0 (Bruker AXS Inc., 2009)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2009'
_computing_publication_material
'PublCIF. Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker X8 PROSPECTOR APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0898
_diffrn_reflns_av_unetI/netI     0.0841
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            9800
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        66.652
_diffrn_reflns_theta_max         66.652
_diffrn_reflns_theta_min         6.041
_diffrn_source                   'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    3.054
_exptl_absorpt_correction_T_max  0.1489
_exptl_absorpt_correction_T_min  0.0381
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1639 before and 0.0949 after correction.
The Ratio of minimum to maximum transmission is 0.2559.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_F_000             1254
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_refine_diff_density_max         1.112
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details
;
 Flack x determined using 1312 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.08(1)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.372
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         3581
_refine_ls_number_restraints     128
_refine_ls_restrained_S_all      1.367
_refine_ls_R_factor_all          0.1180
_refine_ls_R_factor_gt           0.1137
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3002
_refine_ls_wR_factor_ref         0.3072
_reflns_Friedel_coverage         0.822
_reflns_Friedel_fraction_full    0.959
_reflns_Friedel_fraction_max     0.959
_reflns_number_gt                3309
_reflns_number_total             3581
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b08770_si_002.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        3100.3(6)
_cod_original_formula_sum        'C42 H99 Cl6 N6 O16.50'
_cod_database_code               4133180
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.625
_shelx_estimated_absorpt_t_max   0.815
_shelx_res_checksum              61711
_shelx_hkl_checksum              89718