Pore space partition on a sulfonate-rich metal–organic framework for purification of methane from natural gas
Xue, Chaozhuang; Peng, Hui; Hou, Jinle; Qu, Konggang; Chemical Communications 61 (2025) 8244–8247; doi:10.1039/D5CC01014D

data_7134488
_publ_section_title
;
 Pore space partition on a sulfonate-rich metal--organic framework for
 purification of methane from natural gas
;
_journal_issue                   45
_journal_name_full               'Chemical Communications'
_journal_page_first              8244
_journal_page_last               8247
_journal_paper_doi               10.1039/D5CC01014D
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C36 H24.001 Fe3 O34 S6, 45[H2O], 3[C3H7NO]'
_chemical_formula_sum            'C36 H25 Fe3 O34 S6'
_chemical_formula_weight         1361.47
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_Hall           'P 6c'
_space_group_name_H-M_alt        'P 63'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-03-27
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-04-26 deposited with the CCDC.	2025-05-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   19.6053(8)
_cell_length_b                   19.6053(8)
_cell_length_c                   17.9744(11)
_cell_measurement_reflns_used    2998
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      53.231
_cell_measurement_theta_min      2.603
_cell_volume                     5983.2(5)
_computing_cell_refinement       'SAINT V8.41 (?, 2016)'
_computing_data_collection       'APEX6 V2024.9-0 (Bruker, 2024)'
_computing_data_reduction        'SAINT V8.41 (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1160
_diffrn_reflns_av_unetI/netI     0.0964
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            26574
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        64.307
_diffrn_reflns_theta_max         64.307
_diffrn_reflns_theta_min         2.458
_diffrn_source_current           1.1
_diffrn_source_power             0.05500000000000001
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.259
_exptl_absorpt_correction_T_max  0.7525
_exptl_absorpt_correction_T_min  0.6180
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1345 before and 0.0739 after correction.
The Ratio of minimum to maximum transmission is 0.8213.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    0.756
_exptl_crystal_description       block
_exptl_crystal_F_000             1374
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_coef       0.00035(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         5679
_refine_ls_number_restraints     863
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.1195
_refine_ls_R_factor_gt           0.0597
_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^)+(0.1117P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1577
_refine_ls_wR_factor_ref         0.1966
_reflns_Friedel_coverage         0.932
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                3070
_reflns_number_total             5679
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01014d2.cif
_cod_data_source_block           cu_20241220_wq_nsf_np_0m
_cod_depositor_comments
'Adding full bibliography for 7134488--7134489.cif.'
_cod_original_cell_volume        5983.2(6)
_cod_database_code               7134488
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.727
_shelx_estimated_absorpt_t_min   0.629
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5127
 0.03479 0.40738 0.04513
2. Restrained distances
 C7-C12 = C7A-C12A = C2-C1 = C2A-C1A
 1.5 with sigma of 0.01
 O2-C1 = O1-C1 = O4-C12 = O3-C12
 1.25 with sigma of 0.01
 Fe1-O2A \\sim Fe1-O1
 with sigma of 0.02
 Fe1_$1-O4 \\sim Fe1_$1-O3A
 with sigma of 0.02
 S1-O6 \\sim S1-O7 \\sim S1-O5 \\sim S2-O8 \\sim S2-O10 \\sim S2-O9
 with sigma of 0.02
 O4-C7 \\sim O3-C7
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
S1 \\sim S2 \\sim O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7
\\sim O8 \\sim O9 \\sim O10 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim
C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim S1A \\sim S2A
\\sim O1A \\sim O2A \\sim O3A \\sim O4A \\sim O5A \\sim O6A \\sim O7A \\sim O8A
\\sim O9A \\sim O10A \\sim C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A \\sim
C6A \\sim C7A \\sim C8A \\sim C9A \\sim C10A \\sim C11A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(O3) \\sim Ueq, Uanis(O3A) \\sim Ueq, Uanis(O4A) \\sim Ueq, Uanis(O4)
\\sim Ueq, Uanis(C12A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Same fragment restrains
{S1A, S2A, O1A, O2A, O3A, O4A, O5A, O6A, O7A, O8A, O9A, O10A, C1A, C2A, C3A,
C4A, C5A, C6A, C7A, C8A, C9A, C10A, C11A} sigma for 1-2: 0.01, 1-3: 0.02
as in
{S1, S2, O1, O2, O3, O4, O5, O6, O7, O8, O9, O10, C1, C2, C3, C4, C5, C6, C7,
C8, C9, C10, C11}
5. Others
 Sof(S1A)=Sof(S2A)=Sof(O1A)=Sof(O2A)=Sof(O3A)=Sof(O4A)=Sof(O5A)=Sof(O6A)=
 Sof(O7A)=Sof(H7A)=Sof(O8A)=Sof(O9A)=Sof(O10A)=Sof(C1A)=Sof(C2A)=Sof(C3A)=
 Sof(H3A)=Sof(C4A)=Sof(C5A)=Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(C8A)=Sof(H8A)=
 Sof(C9A)=Sof(C10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=1-FVAR(1)
 Sof(H7)=0.66666*FVAR(2)
 Sof(S1)=Sof(S2)=Sof(O1)=Sof(O2)=Sof(O3)=Sof(O4)=Sof(O5)=Sof(O6)=Sof(O7)=
 Sof(O8)=Sof(O9)=Sof(O10)=Sof(H10)=Sof(C1)=Sof(C2)=Sof(C3)=Sof(H3)=Sof(C4)=
 Sof(C5)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(C8)=Sof(H8)=Sof(C9)=Sof(C10)=Sof(C11)=
 Sof(H11)=Sof(C12)=FVAR(1)
 Fixed Sof: H10A(0.6667)
 Fixed Z: O7(0.277749) C5(0.249529) C7(0.162951) C6A(0.192841)
6.a Riding coordinates:
 O12(H12A,H12B), O7(H7), O10(H10), O7A(H7A), O10A(H10A)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C8(H8), C11(H11), C3A(H3A), C6A(H6A), C8A(H8A), C11A(H11A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              67314
_shelx_hkl_checksum              77283
_shelx_fab_checksum              93555
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'