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_7132967
_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 H16 N12 O8 S Zn3'
_chemical_formula_sum            'C18 H16 N12 O8 S Zn3'
_chemical_formula_weight         756.60
_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             2023-08-30
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-10-27 deposited with the CCDC.	2024-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.777(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.143(2)
_cell_length_b                   9.9829(15)
_cell_length_c                   25.111(5)
_cell_measurement_reflns_used    7577
_cell_measurement_temperature    200.00
_cell_measurement_theta_max      24.96
_cell_measurement_theta_min      2.31
_cell_volume                     3520.6(10)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      200.00
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0650
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19080
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.052
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.139
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0958 before and 0.0679 after correction.
The Ratio of minimum to maximum transmission is 0.7661.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       block
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.514
_refine_diff_density_min         -0.986
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6114
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1191
_refine_ls_R_factor_gt           0.0896
_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^)+(0.1469P)^2^+27.9477P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2568
_refine_ls_wR_factor_ref         0.2797
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4049
_reflns_number_total             6114
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00863d3.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7132967--7132968.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7132967
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.939
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
O9 \\sim Zn3 \\sim O6: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Uanis(N5A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N11A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(H8)=Sof(N5A)=Sof(H5AA)=Sof(H5AB)=1-FVAR(1)
 Sof(N5)=Sof(H5A)=Sof(H5B)=Sof(H10)=FVAR(1)
 Sof(H12)=Sof(N11A)=Sof(H11C)=Sof(H11D)=1-FVAR(2)
 Sof(N11)=Sof(H11A)=Sof(H11B)=Sof(H1)=FVAR(2)
4.a Riding coordinates:
 N11(H11A,H11B)
4.b Rotating group:
 O9(H9A,H9B), N5(H5A,H5B), N9(H9C,H9D), N11A(H11C,H11D)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C8(H8), C10(H10), C12(H12), C20(H20), C13(H13), C5(H5),
 C15(H15), C11(H11)
4.d X=CH2 refined with riding coordinates:
 N5A(H5AA,H5AB)
4.e Naphthalene refined as free rotating group:
 C20(C13,C14,C5,C7,C17,C2,C15,C11,C16)
;
_shelx_res_checksum              91519
_shelx_hkl_checksum              55607
_shelx_fab_checksum              61572
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'