Topology meets MOF chemistry for pore-aperture fine tuning: ftw-MOF platform for energy-efficient separations via adsorption kinetics or molecular sieving
Xue, Dong-Xu; Cadiau, Amandine; Weseliński, Łukasz J.; Jiang, Hao; Bhatt, Prashant M.; Shkurenko, Aleksander; Wojtas, Lukasz; Zhijie, Chen; Belmabkhout, Youssef; Adil, Karim; Eddaoudi, Mohamed; Chemical Communications  (2018) –; doi:10.1039/C8CC03841D

data_7121807
_publ_section_title
;
 Topology meets MOF chemistry for pore-aperture fine tuning: ftw-MOF
 platform for energy-efficient separations via adsorption kinetics or
 molecular sieving
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC03841D
_journal_year                    2018
_chemical_formula_moiety
'2(C2 H8 N),(Tb6 (O H)8 (C16 H6 N2 O8)3 (C3 H7 N O)1.5 (H2 O)1.5), 1.75(H2 O)'
_chemical_formula_sum            'C56.5 H59 N9.5 O36.75 Tb6'
_chemical_formula_weight         2412.59
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c'
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-04-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2018-05-13 deposited with the CCDC.
2018-06-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   18.232(1)
_cell_length_b                   18.232(1)
_cell_length_c                   45.607(3)
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      69.92
_cell_measurement_theta_min      3.40
_cell_volume                     13129.0(13)
_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    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker X8 PROSPECTOR APEX2 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5090
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.260
_diffrn_reflns_theta_min         3.404
_diffrn_source                   'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    24.043
_exptl_absorpt_correction_T_max  0.753288
_exptl_absorpt_correction_T_min  0.621737
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0663 before and 0.0408 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.0727 before and 0.0411 after correction.
 The Ratio of minimum to maximum transmission is 0.83.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 32025 reflections, Rint = 0.0490
 (18318 with I > 3sig(I), Rint = 0.0421)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.831
_exptl_crystal_description       rod
_exptl_crystal_F_000             6891
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.957
_refine_diff_density_min         -0.973
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2744
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+280.1767P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1187
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2425
_reflns_number_total             2744
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc03841d2.cif
_cod_data_source_block           kme_726b
_cod_original_cell_volume        13130(2)
_cod_original_formula_sum        'C56.50 H59 N9.50 O36.75 Tb6'
_cod_database_code               7121807
_shelx_estimated_absorpt_t_max   0.795
_shelx_estimated_absorpt_t_min   0.326
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O9-C16
 1.23 with sigma of 0.02
 N10-C16
 1.32 with sigma of 0.02
 N10-C18 = N10-C17
 1.45 with sigma of 0.02
 N11-C20 = N11-C19
 1.47 with sigma of 0.02
 N10-O9
 2.26 with sigma of 0.04
 C16-C17
 2.41 with sigma of 0.04
 C16-C18
 2.41 with sigma of 0.04
 C18-C17
 2.47 with sigma of 0.04
 C19-C20
 2.48 with sigma of 0.04
3. Restrained planarity
 O9, C16, N10, C17, C18
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
O9 \\sim C16 \\sim N10 \\sim C17 \\sim C18: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C21 \\sim N12: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
N12 \\sim C21: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
5. Others
 Fixed Sof: O9(0.5) C19(0.25) H19A(0.25) H19B(0.25) H19C(0.25) N11(0.25)
 H11A(0.25) H11B(0.25) N10(0.25) C16(0.25) H16(0.25) C18(0.25) H18A(0.25)
 H18B(0.25) H18C(0.25) C17(0.25) H17A(0.25) H17B(0.25) H17C(0.25) C21(0.166)
 H21A(0.166) H21B(0.166) H21C(0.166) O12(0.25) C20(0.25) H20A(0.25) H20B(0.25)
 H20C(0.25) O14(0.04167) N12(0.083) H12A(0.083) H12B(0.083)
6.a Riding coordinates:
 C19(H19A,H19B,H19C), C18(H18A,H18B,H18C), C17(H17A,H17B,H17C)
6.b Ternary CH refined with riding coordinates:
 O3(H3), O4(H4)
6.c Secondary CH2 refined with riding coordinates:
 N11(H11A,H11B), N12(H12A,H12B)
6.d Aromatic/amide H refined with riding coordinates:
 C15(H15), C11(H11), C10(H10), C16(H16)
6.e Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C20(H20A,H20B,H20C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'