Microporous chromium-organic framework fabricated via solvent-assisted metal metathesis for C2H2/CO2 Separation
Lu, Ting-ting; Fan, Ying-yi; Wang, Xiao-ning; Wang, Qiang; Li, Bao; Dalton Transactions  (2022) –; doi:10.1039/D2DT01546C

data_7710676
_publ_section_title
;
 Microporous chromium-organic framework fabricated via solvent-assisted
 metal metathesis for C2H2/CO2 Separation
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01546C
_journal_year                    2022
_chemical_formula_moiety         'C66 H40 Fe3 N3 O20 S2'
_chemical_formula_sum            'C66 H40 Fe3 N3 O20 S2'
_chemical_formula_weight         1426.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-10
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-04-08 deposited with the CCDC.	2022-07-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 122.1830(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   34.4082(10)
_cell_length_b                   26.2769(9)
_cell_length_c                   18.7449(6)
_cell_measurement_reflns_used    9964
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      2.28
_cell_volume                     14344.0(8)
_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  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  synchrotron
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_type           'Synchrotron radiation X-rays'
_diffrn_radiation_wavelength     0.77488
_diffrn_reflns_av_R_equivalents  0.0642
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_number            11343
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        26.498
_diffrn_reflns_theta_max         26.498
_diffrn_reflns_theta_min         1.455
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.460
_exptl_absorpt_correction_T_max  0.745551
_exptl_absorpt_correction_T_min  0.416595
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1018 before and 0.0648 after correction.
 The Ratio of minimum to maximum transmission is 0.56.

Final HKLF 4 output contains 61361 reflections, Rint = 0.0642
 (24658 with I > 3sig(I), Rint = 0.0492)
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    0.661
_exptl_crystal_description       block
_exptl_crystal_F_000             2908
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.788
_refine_diff_density_min         -0.871
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.193
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         11343
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.204
_refine_ls_R_factor_all          0.1021
_refine_ls_R_factor_gt           0.0875
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2841
_refine_ls_wR_factor_ref         0.2970
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8151
_reflns_number_total             11343
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01546c2.cif
_cod_data_source_block           1
_cod_database_code               7710676
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.951
_shelx_estimated_absorpt_t_min   0.934
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Restrained distances
 N2-C25
 1.3 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C37) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C35) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C31) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C17) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C15) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C19) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Sof(H13)=Sof(C33)=Sof(H33)=Sof(C17)=Sof(C35)=Sof(H35)=Sof(C9)=Sof(H9)=
 Sof(C37)=Sof(H37)=Sof(C19)=1-FVAR(1)
 Sof(H3)=Sof(C27)=Sof(H27)=Sof(C7)=Sof(H7)=Sof(C29)=Sof(C15)=Sof(H15)=Sof(C31)=
 Sof(H31)=Sof(C2)=FVAR(1)
 Fixed Sof: H2A(0.5) H2B(0.5)
5.a Rotating group:
 N1(H1A,H1B)
5.b Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B)
5.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C16(H16), C24(H24), C30(H30), C32(H32), C34(H34), C36(H36),
 C38(H38), C39(H39), C5(H5), C21(H21), C23(H23), C3(H3), C13(H13), C27(H27),
 C7(H7), C15(H15), C31(H31), C33(H33), C35(H35), C9(H9), C37(H37)
5.d Fitted hexagon refined as free rotating group:
 C21(C11,C23,C3,C25,C13), C27(C7,C29,C15,C31,C2)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              52744
_shelx_fab_checksum              41588
_olex2_submission_special_instructions 'No special instructions were received'