Synthesis of an iron-based metal–organic framework with octahedral cages for the selective capture of sulfur hexafluoride
Wang, Hao; Shi, Le; Cao, Honghao; Xiong, Zhangyi; Ma, Si; Pan, Jun; Chen, Zhijie; CrystEngComm 26 (2024) 1912–1916; doi:10.1039/D4CE00041B

data_7248218
_publ_section_title
;
 Synthesis of an iron-based metal--organic framework with octahedral cages
 for the selective capture of sulfur hexafluoride
;
_journal_issue                   13
_journal_name_full               CrystEngComm
_journal_page_first              1912
_journal_page_last               1916
_journal_paper_doi               10.1039/D4CE00041B
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C57 H37 Fe3 N4 O16'
_chemical_formula_sum            'C81 H93 Fe3 N12 O24'
_chemical_formula_weight         1786.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-01-14
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-01-14 deposited with the CCDC.	2024-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.0780(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.238(2)
_cell_length_b                   16.0211(9)
_cell_length_c                   33.7881(17)
_cell_measurement_reflns_used    9206
_cell_measurement_temperature    173
_cell_measurement_theta_max      26.28
_cell_measurement_theta_min      2.19
_cell_volume                     18530.5(18)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0676
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            113259
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         1.190
_exptl_absorpt_coefficient_mu    0.539
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1368 before and 0.0707 after correction.
The Ratio of minimum to maximum transmission is 0.6276.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_description       prism
_exptl_crystal_F_000             7464
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.956
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.087
_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     724
_refine_ls_number_reflns         16737
_refine_ls_number_restraints     138
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_gt           0.0673
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1332P)^2^+34.3190P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1948
_refine_ls_wR_factor_ref         0.2118
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12964
_reflns_number_total             16737
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00041b2.cif
_cod_data_source_block           Fe-cage-MOF
_cod_depositor_comments          'Adding full bibliography for 7248218.cif.'
_cod_original_cell_volume        18530.6(18)
_cod_database_code               7248218
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.900
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
C32 \\sim C37 \\sim C36 \\sim C35 \\sim C34 \\sim C33: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C37) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C39)
\\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C40) \\sim Ueq,
Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C44)
\\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C49) \\sim Ueq,
Uanis(N4) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C41)
\\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C36) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
3.a Rotating group:
 O9(H9A,H9B)
3.b Aromatic/amide H refined with riding coordinates:
 C29(H29), C17(H17), C6(H6), C4(H4), C15(H15), C18(H18), C3(H3), C22(H22),
 C14(H14), C25(H25), C21(H21), C24(H24), C10(H10), C7(H7), C9(H9), C54(H54),
 C53(H53), C33(H33), C34(H34), C52(H52), C51(H51), C39(H39), C40(H40), C47(H47),
  C37(H37), C48(H48), C43(H43), C36(H36), C42(H42)
3.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C30(H30A,H30B,H30C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 2786 electrons were 
found in a volume of 10232\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
8[C3H7NO] per Asymmetric Unit 
which account for 2560 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              51076
_shelx_fab_checksum              50211
_olex2_submission_special_instructions 'No special instructions were received'