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_1567976
_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 Cl Cu2 N3'
_chemical_formula_sum            'C8 H14 Cl Cu2 N3'
_chemical_formula_weight         314.75
_chemical_name_systematic        SNNU-314-Cl
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-09-29
_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                   15.9814(7)
_cell_length_b                   15.9814(7)
_cell_length_c                   20.7345(18)
_cell_measurement_reflns_used    9299
_cell_measurement_temperature    153.02
_cell_measurement_theta_max      68.39
_cell_measurement_theta_min      3.91
_cell_volume                     5295.7(6)
_computing_cell_refinement       'SMART (Bruker, 2000)'
_computing_data_collection       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_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    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      153.02
_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 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0621
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20460
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.394
_diffrn_reflns_theta_min         5.536
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    5.567
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.1844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1728 before and 0.1100 after correction.
The Ratio of minimum to maximum transmission is 0.2449.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_description       prism
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   0.7531
_exptl_transmission_factor_min   0.1844
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         2432
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0652
_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^)+(0.1363P)^2^+15.4066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2007
_refine_ls_wR_factor_ref         0.2028
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2306
_reflns_number_total             2432
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nr04187a2.cif
_cod_data_source_block           SNNU-314-Cl
_cod_original_cell_volume        5295.7(7)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               1567976
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.402
_shelx_estimated_absorpt_t_min   0.402
_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 = C5-C4
 1.54 with sigma of 0.02
3. Rigid bond restraints
 C3, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C9) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: Cl1(0.4) H7AA(0.7) H7AB(0.7) H7BC(0.3) H7BD(0.3) C8(0.7) H8A(0.7)
 H8B(0.7) H8C(0.7) H4BC(0.6) H4BD(0.6) H4AA(0.4) H4AB(0.4) C3(0.6) H3A(0.6)
 H3B(0.6) H3C(0.6) C5(0.4) H5A(0.4) H5B(0.4) H5C(0.4) Cl2(0.6) C9(0.3) H9A(0.3)
 H9B(0.3) H9C(0.3)
6.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7AA,H7AB), C7(H7BC,H7BD), C4(H4BC,H4BD), C4(H4AA,H4AB),
 C10(H10A,H10B)
6.b Me refined with riding coordinates:
 C5(H5A,H5B,H5C)
6.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C3(H3A,H3B,H3C), C9(H9A,H9B,H9C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 216 electrons were 
found in a volume of 1108\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.5[C2H6O] per Formula Unit 
which account for 208 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              20421
_shelx_fab_checksum              89578
_olex2_submission_special_instructions 'No special instructions were received'