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_1567977
_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 H8 Cl Cu2 N3'
_chemical_formula_sum            'C6 H8 Cl Cu2 N3'
_chemical_formula_weight         284.70
_chemical_name_systematic        SNNU-313-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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-09-24
_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                   16.0496(6)
_cell_length_b                   16.0496(6)
_cell_length_c                   20.1900(17)
_cell_measurement_reflns_used    2388
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      26.264
_cell_measurement_theta_min      2.609
_cell_volume                     5200.7(5)
_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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      153.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_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           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0702
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16977
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.496
_diffrn_reflns_theta_min         5.513
_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    5.613
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.4885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1281 before and 0.0925 after correction.
The Ratio of minimum to maximum transmission is 0.6487.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2239
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   0.7531
_exptl_transmission_factor_min   0.4885
_refine_diff_density_max         1.996
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         2387
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0838
_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^)+(0.1813P)^2^+3.7476P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2407
_refine_ls_wR_factor_ref         0.2468
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2148
_reflns_number_total             2387
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nr04187a2.cif
_cod_data_source_block           SNNU-313-Cl
_cod_original_cell_volume        5200.7(6)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               1567977
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C6-C1
 1.54 with sigma of 0.02
 C6'-C1
 1.54 with sigma of 0.02
 C6'-C1 \\sim C6-C1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1.7A
4. Others
 Fixed Sof: C6'(0.7) H6'A(0.7) H6'B(0.7) H6'C(0.7) C6(0.3) H6A(0.3) H6B(0.3)
 H6C(0.3)
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B)
5.b Me refined with riding coordinates:
 C5(H5A,H5B,H5C), C6'(H6'A,H6'B,H6'C), C6(H6A,H6B,H6C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 140 electrons were 
found in a volume of 1796\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.344[C2H6O] per Unit Cell 
which account for 143 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              81422
_shelx_fab_checksum              71988
_olex2_submission_original_sample_id SNNU-313-Cl
_olex2_submission_special_instructions 'No special instructions were received'