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_1567975
_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         'C8 H14 Br Cu2 N3'
_chemical_formula_sum            'C8 H14 Br Cu2 N3'
_chemical_formula_weight         359.21
_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                   16.5753(17)
_cell_length_b                   16.5753(17)
_cell_length_c                   19.1960(18)
_cell_measurement_reflns_used    2754
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.971
_cell_measurement_theta_min      2.458
_cell_volume                     5273.9(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      298.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 1.000
_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  0.0410
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11570
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.014
_diffrn_reflns_theta_min         1.623
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    6.225
_exptl_absorpt_correction_T_max  0.3165
_exptl_absorpt_correction_T_min  0.1897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2816
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.24
_exptl_transmission_factor_max   0.3165
_exptl_transmission_factor_min   0.1897
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         2328
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0377P)^2^+17.9578P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0984
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1475
_reflns_number_total             2328
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nr04187a2.cif
_cod_data_source_block           SNNU-314-Br
_cod_original_cell_volume        5273.9(12)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               1567975
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.317
_shelx_estimated_absorpt_t_min   0.190
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C4'-C3 = C4-C3
 1.54 with sigma of 0.02
 C5-C4 = C5'-C4'
 1.54 with sigma of 0.02
 C8-C7 = C8'-C7'
 1.54 with sigma of 0.02
 C4'-C3 \\sim C4-C3
 with sigma of 0.02
 C5-C4 \\sim C5'-C4'
 with sigma of 0.02
 C7-C6 \\sim C7'-C6
 with sigma of 0.02
 C8'-C7' \\sim C8-C7
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C8') \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C7') \\sim Ueq, Uanis(C4)
\\sim Ueq, Uanis(C4') \\sim Ueq, Uanis(C5') \\sim Ueq, Uanis(C5) \\sim Ueq,
Uanis(C7) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Sof(H3bc)=Sof(H3bd)=Sof(C4')=Sof(H4'a)=Sof(H4'b)=Sof(C5')=Sof(H5'a)=Sof(H5'b)=
 Sof(H5'c)=1-FVAR(1)
 Sof(H3aa)=Sof(H3ab)=Sof(C4)=Sof(H4a)=Sof(H4b)=Sof(C5)=Sof(H5a)=Sof(H5b)=
 Sof(H5c)=FVAR(1)
 Sof(H6bc)=Sof(H6bd)=Sof(C7')=Sof(H7'a)=Sof(H7'b)=Sof(C8')=Sof(H8'a)=Sof(H8'b)=
 Sof(H8'c)=1-FVAR(2)
 Sof(H6aa)=Sof(H6ab)=Sof(C7)=Sof(H7a)=Sof(H7b)=Sof(C8)=Sof(H8a)=Sof(H8b)=
 Sof(H8c)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C3(H3aa,H3ab), C3(H3bc,H3bd), C4(H4a,H4b), C6(H6aa,H6ab), C6(H6bc,H6bd),
 C7(H7a,H7b), C4'(H4'a,H4'b), C7'(H7'a,H7'b)
5.b Idealised Me refined as rotating group:
 C5(H5a,H5b,H5c), C8(H8a,H8b,H8c), C5'(H5'a,H5'b,H5'c), C8'(H8'a,H8'b,H8'c)
;
_shelx_res_checksum              66938
_olex2_submission_special_instructions 'No special instructions were received'