A two-dimensional metal-organic framework assembled from scandium-based cages for the selective capture of sulfur hexafluoride.
Wang, Hao; Shi, Le; Xiong, Zhangyi; Ma, Si; Cao, Honghao; Cai, Shijia; Qiao, Zhiwei; Pan, Jun; Chen, Zhijie; Chemical communications (Cambridge, England) 60 (2024) 2397–2400; doi:10.1039/d3cc05087d

data_7132662
_publ_section_title
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 A two-dimensional metal-organic framework assembled from scandium-based
 cages for the selective capture of sulfur hexafluoride.
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_journal_issue                   17
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2397
_journal_page_last               2400
_journal_paper_doi               10.1039/d3cc05087d
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C60 H42 N5 O16 Sc3'
_chemical_formula_sum            'C84 H98 N13 O24 Sc3'
_chemical_formula_weight         1808.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-01-12
_audit_creation_method
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Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
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_audit_update_record
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2024-01-13 deposited with the CCDC.	2024-01-30 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 101.579(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.847(2)
_cell_length_b                   16.418(3)
_cell_length_c                   34.089(5)
_cell_measurement_reflns_used    7457
_cell_measurement_temperature    170.00
_cell_measurement_theta_max      39.475
_cell_measurement_theta_min      2.302
_cell_volume                     8689(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Apex3 v2017.3-0 (Bruker, 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      170.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0901
_diffrn_reflns_av_unetI/netI     0.0908
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            39396
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        37.569
_diffrn_reflns_theta_max         37.569
_diffrn_reflns_theta_min         2.302
_exptl_absorpt_coefficient_mu    1.771
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.5849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1003 before and 0.0782 after correction.
The Ratio of minimum to maximum transmission is 0.7786.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_description       block
_exptl_crystal_F_000             3792
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.0020(2)
_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   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     761
_refine_ls_number_reflns         6801
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.1084
_refine_ls_R_factor_gt           0.0863
_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^)+(0.1805P)^2^+4.4063P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2510
_refine_ls_wR_factor_ref         0.2754
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4690
_reflns_number_total             6801
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05087d2.cif
_cod_data_source_block           Sc-cage-MOF
_cod_depositor_comments          'Adding full bibliography for 7132662.cif.'
_cod_database_code               7132662
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.829
_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
2. Restrained distances
 N3-C34
 1.45 with sigma of 0.01
 N3-C33 \\sim N3-C34
 with sigma of 0.02
 N3-C34 \\sim N3-C33
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O5 \\sim N3 \\sim C32 \\sim C34 \\sim C33: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
O5 \\sim C32 \\sim N3 \\sim C34 \\sim C33 \\sim C54 \\sim C55: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C43) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4.a Riding coordinates:
 C33(H33A,H33B,H33C)
4.b Aromatic/amide H refined with riding coordinates:
 C38(H38), C50(H50), C37(H37), C40(H40), C57(H57), C41(H41), C27(H27), C3(H3),
 C47(H47), C51(H51), C58(H58), C7(H7), C54(H54), C55(H55), C22(H22), C46(H46),
 C6(H6), C4(H4), C21(H21), C25(H25), C24(H24), C43(H43), C9(H9), C10(H10),
 C44(H44), C14(H14), C13(H13), C32(H32), C18(H18), C17(H17)
4.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C29(H29A,H29B,H29C), C34(H34A,H34B,H34C)
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_smtbx_masks_special_details
;
A solvent mask was calculated and 1176 electrons were 
found in a volume of 3991\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 8[C3H7NO] per Asymmetric Unit 
which account for 1280 electrons per unit cell.
;
_shelx_res_checksum              55637
_shelx_hkl_checksum              51128
_shelx_fab_checksum              42177
_olex2_submission_special_instructions 'No special instructions were received'