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_7134489
_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         'C58 H30 Fe3 N9 O31 S6, 19.5[H2O], 6[C3H7NO]'
_chemical_formula_sum            'C58 H30 Fe3 N9 O31 S6'
_chemical_formula_weight         1708.82
_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             2025-03-25
_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                   19.2686(13)
_cell_length_b                   19.2686(13)
_cell_length_c                   18.143(2)
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.46
_cell_measurement_theta_min      2.18
_cell_volume                     5833.6(9)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2019)'
_computing_data_collection       'APEX4 V2022.10-1 (Bruker, 2022)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2019)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       SSRF
_diffrn_measurement_device_type
'Shanghai Synchrotron Radiation Facility, beam line station'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'nylon loop'
_diffrn_radiation_type           'synchrotron radiation'
_diffrn_radiation_wavelength     0.68887
_diffrn_reflns_av_R_equivalents  0.0719
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            60999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.414
_diffrn_reflns_theta_max         24.556
_diffrn_reflns_theta_min         1.088
_exptl_absorpt_coefficient_mu    0.492
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.4987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1213 before and 0.0563 after correction.
The Ratio of minimum to maximum transmission is 0.6693.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.973
_exptl_crystal_description       block
_exptl_crystal_F_000             1726
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.585
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.285
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         7143
_refine_ls_number_restraints     1055
_refine_ls_restrained_S_all      1.370
_refine_ls_R_factor_all          0.1198
_refine_ls_R_factor_gt           0.0985
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2699
_refine_ls_wR_factor_ref         0.2970
_reflns_Friedel_coverage         0.934
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                5779
_reflns_number_total             7143
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01014d2.cif
_cod_data_source_block           fe_ndc(so3h)_tph
_cod_depositor_comments
'Adding full bibliography for 7134488--7134489.cif.'
_cod_original_cell_volume        5833.7(10)
_cod_database_code               7134489
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.971
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.25(11)
 0.22(6) 0.28(7) 0.25(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
3. Restrained distances
 O1-C1 = O1A-C1A = O2A-C1A = O2-C1
 1.25 with sigma of 0.01
 S1A-O6A \\sim S1A-O5A \\sim S1A-O7A \\sim S1-O5 \\sim S1-O7 \\sim S1-O6 \\sim
S2-O8 \\sim S2-O10 \\sim S2-O9
 \\sim S2A-O8A \\sim S2A-O10A \\sim S2A-O9A
 with sigma of 0.01
 O10-C9 \\sim O8-C9 \\sim O9-C9 \\sim O8A-C9A \\sim O10A-C9A \\sim O9A-C9A
\\sim O6A-C4A \\sim O5A-C4A ~
 O5-C4 \\sim O7A-C4A \\sim O6-C4 \\sim O7-C4
 with sigma of 0.02
 O3A-C7A \\sim O4A-C7A
 with sigma of 0.02
 O1A-C2A \\sim O2A-C2A
 with sigma of 0.02
 S1-C4 \\sim S1A-C4A \\sim S2-C9 \\sim S2A-C9A
 with sigma of 0.02
4. Restrained planarity
 C1A, C11A, C2A, C3A, C4A, C5A, C10A, C9A, C8A, C7A, C6A, C12A, S1A, S2A
 with sigma of 0.01
 O3A, O4A, C7A, C12A
 with sigma of 0.01
 O1A, O2A, C1A, C2A
 with sigma of 0.01
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Uanis(C13) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C16)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C18) \\sim Ueq,
Uanis(N2) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C20)
\\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.015
Uanis(O3) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O1A) \\sim Ueq, Uanis(C1) \\sim
Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
6. Same fragment restrains
{S1A, S2A, O1A, O2A, O3A, O4A, O5A, O6A, O7A, O8A, O9A, O10A, C1A, C11A, C2A,
C3A, C4A, C5A, C10A, C9A, C8A, C7A, C6A, C12A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{S1, S2, O1, O2, O3, O4, O5, O6, O7, O8, O9, O10, C1, C11, C2, C3, C4, C5, C10,
C9, C8, C7, C6, C12}
7. Others
 Fixed Sof: S1(0.666667) S2(0.666667) O1(0.666667) O2(0.666667) O3(0.666667)
 O4(0.666667) O5(0.666667) O6(0.666667) O7(0.666667) H7(0.666667) O8(0.666667)
 O9(0.666667) O10(0.666667) H10(0.666667) C1(0.666667) C11(0.666667)
 H11(0.666667) C2(0.666667) C3(0.666667) H3(0.666667) C4(0.666667) C5(0.666667)
 C10(0.666667) C9(0.666667) C8(0.666667) H8(0.666667) C7(0.666667) C6(0.666667)
 H6(0.666667) C12(0.666667) S1A(0.333333) S2A(0.333333) O1A(0.333333)
 O2A(0.333333) O3A(0.333333) O4A(0.333333) O5A(0.333333) O6A(0.333333)
 H6A(0.333333) O7A(0.333333) O8A(0.333333) O9A(0.333333) O10A(0.333333)
 H10A(0.333333) C1A(0.333333) C11A(0.333333) H11A(0.333333) C2A(0.333333)
 C3A(0.333333) H3A(0.333333) C4A(0.333333) C5A(0.333333) C10A(0.333333)
 C9A(0.333333) C8A(0.333333) H8A(0.333333) C7A(0.333333) C6A(0.333333)
 H6AA(0.333333) C12A(0.333333)
8.a Riding coordinates:
 O7(H7), O10(H10), O6A(H6A), O10A(H10A)
8.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C17(H17), C16(H16), C14(H14), C11(H11), C3(H3), C8(H8), C6(H6),
 C11A(H11A), C3A(H3A), C8A(H8A), C6A(H6AA)
8.c Fitted hexagon refined as free rotating group:
 C13(N1,C17,C16,C15,C14)
8.d Naphthalene refined as free rotating group:
 C11(C2,C3,C4,C5,C10,C9,C8,C7,C6), C11A(C2A,C3A,C4A,C5A,C10A,C9A,C8A,C7A,C6A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              58652
_shelx_hkl_checksum              1023
_shelx_fab_checksum              40029
_olex2_submission_special_instructions 'No special instructions were received'