Rational regulation of acetylene adsorption and separation for ultra-microporous copper-1,2,4-triazolate frameworks by halogen hydrogen bonds
Li, Haipeng; Dou, Zhao-Di; Xiao, Yi; Fan, Guan-Jiang; Pan, Dong-Chen; Hu, Mancheng; Zhai, Quan-Guo; Nanoscale  (2022) –; doi:10.1039/D2NR04187A

data_1567974
_publ_section_title
;
 Rational regulation of acetylene adsorption and separation for
 ultra-microporous copper-1,2,4-triazolate frameworks by halogen hydrogen
 bonds
;
_journal_name_full               Nanoscale
_journal_paper_doi               10.1039/D2NR04187A
_journal_year                    2022
_chemical_formula_moiety         'C6 H10 Br Cu2 N3'
_chemical_formula_sum            'C6 H10 Br Cu2 N3'
_chemical_formula_weight         331.16
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-09-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-10-08 deposited with the CCDC.	2022-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   16.3337(3)
_cell_length_b                   16.3337(3)
_cell_length_c                   20.1543(5)
_cell_measurement_reflns_used    9988
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      26.264
_cell_measurement_theta_min      2.609
_cell_volume                     5376.96(19)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       SMART
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      200.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_unetI/netI     0.0186
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            50187
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.494
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    6.098
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5922
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_description       block
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   0.7454
_exptl_transmission_factor_min   0.5922
_refine_diff_density_max         1.001
_refine_diff_density_min         -0.839
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         2751
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+8.7491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.0891
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2372
_reflns_number_total             2751
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nr04187a2.cif
_cod_data_source_block           SNNU-313-Br
_cod_original_cell_volume        5377.0(2)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               1567974
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.461
_shelx_estimated_absorpt_t_min   0.375
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C6-C5 = C7-C5
 1.54 with sigma of 0.02
 C7-C5 \\sim C6-C5
 with sigma of 0.02
 C3-C2 \\sim C8-C2
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C8) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C6) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C7) = Uanis(C6)
Uanis(C8) = Uanis(C3)
4. Others
 Fixed Sof: H2AA(0.5) H2AB(0.5) H2BC(0.5) H2BD(0.5) H5AA(0.5) H5AB(0.5)
 H5BC(0.5) H5BD(0.5) C3(0.5) H3A(0.5) H3B(0.5) H3C(0.5) C6(0.5) H6A(0.5)
 H6B(0.5) H6C(0.5) C8(0.5) H8A(0.5) H8B(0.5) H8C(0.5) C7(0.5) H7A(0.5) H7B(0.5)
 H7C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2AA,H2AB), C2(H2BC,H2BD), C5(H5AA,H5AB), C5(H5BC,H5BD)
5.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              13756
_shelx_fab_checksum              84528
_olex2_submission_special_instructions 'No special instructions were received'