Pure separation of acetylene based on a sulfonic acid and amino group functionalized Zn-MOF.
Deng, Yu-Xin; Yang, Guo-Ping; Wang, Yao-Yu; Chemical communications (Cambridge, England) 60 (2024) 5046–5049; doi:10.1039/d4cc00863d

data_7132968
_publ_section_title
;
 Pure separation of acetylene based on a sulfonic acid and amino group
 functionalized Zn-MOF.
;
_journal_issue                   38
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5046
_journal_page_last               5049
_journal_paper_doi               10.1039/d4cc00863d
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C18 H14 N12 O7 S Zn3'
_chemical_formula_sum            'C18 H14 N12 O7 S Zn3'
_chemical_formula_weight         738.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-10-27 deposited with the CCDC.	2024-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.909(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0795(7)
_cell_length_b                   9.8510(5)
_cell_length_c                   25.9541(12)
_cell_measurement_reflns_used    9878
_cell_measurement_temperature    210.0
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.25
_cell_volume                     3580.6(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      210.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            46137
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.362
_diffrn_reflns_theta_min         2.213
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.099
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6154
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0861 before and 0.0500 after correction.
The Ratio of minimum to maximum transmission is 0.8258.
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    1.370
_exptl_crystal_description       plate
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.918
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         6528
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0826P)^2^+4.4923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1296
_refine_ls_wR_factor_ref         0.1367
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5236
_reflns_number_total             6528
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00863d3.cif
_cod_data_source_block           1a
_cod_depositor_comments
'Adding full bibliography for 7132967--7132968.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7132968
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.802
_shelx_estimated_absorpt_t_min   0.787
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Rigid bond restraints
 C13
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
3. Others
 Sof(H13)=Sof(N13A)=Sof(H13C)=Sof(H13D)=1-FVAR(1)
 Sof(H11)=Sof(N13)=Sof(H13A)=Sof(H13B)=FVAR(1)
4.a Rotating group:
 N13(H13A,H13B), N13A(H13C,H13D)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C7(H7), C9(H9), C11(H11), C12(H12), C13(H13), C15(H15),
 C18(H18)
4.c X=CH2 refined with riding coordinates:
 N2(H2A,H2B), N10(H10A,H10B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              61451
_shelx_hkl_checksum              60369
_shelx_fab_checksum              2011
_olex2_submission_special_instructions 'No special instructions were received'