Selective adsorptive separation of cyclohexane over benzene using thienothiophene cages
Ding, Yanjun; Alimi, Lukman O.; Moosa, Basem; Maaliki, Carine; Jacquemin, Johan; Huang, Feihe; Khashab, Niveen M.; Chemical Science 12 (2021) 5315–5318; doi:10.1039/D1SC00440A

data_1560720
_publ_section_title
;
 Selective adsorptive separation of cyclohexane over benzene using
 thienothiophene cages
;
_journal_issue                   14
_journal_name_full               'Chemical Science'
_journal_page_first              5315
_journal_page_last               5318
_journal_paper_doi               10.1039/D1SC00440A
_journal_volume                  12
_journal_year                    2021
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C36 H36 N8 S6, C6 H12'
_chemical_formula_sum            'C42 H48 N8 S6'
_chemical_formula_weight         857.24
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-09-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-01-24 deposited with the CCDC.	2021-02-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.1011(9)
_cell_length_b                   14.1412(8)
_cell_length_c                   41.847(3)
_cell_measurement_reflns_used    9708
_cell_measurement_temperature    120.72
_cell_measurement_theta_max      63.71
_cell_measurement_theta_min      4.23
_cell_volume                     8344.6(9)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120.72
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.1155
_diffrn_reflns_av_unetI/netI     0.0869
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            66061
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        62.492
_diffrn_reflns_theta_max         62.492
_diffrn_reflns_theta_min         2.111
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.357
_exptl_absorpt_correction_T_max  0.7524
_exptl_absorpt_correction_T_min  0.5103
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1457 before and 0.0718 after correction.
The Ratio of minimum to maximum transmission is 0.6782.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       Needle
_exptl_crystal_F_000             3616
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.971
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1009
_refine_ls_number_reflns         12999
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0699
_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^)+(0.1030P)^2^+4.9890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1598
_refine_ls_wR_factor_ref         0.1666
_reflns_Friedel_coverage         0.969
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                10880
_reflns_number_total             12999
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc00440a2.cif
_cod_data_source_block           ThT_cage3
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_colour_primary' value 'Colourless' was
changed to 'colourless' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 1560718--1560720.cif.

2022-06-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        8344.5(9)
_cod_original_formula_moiety     '2(C36 H36 N8 S6), 2(C6 H12)'
_cod_original_formula_sum        'C84 H96 N16 S12'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1714.48
_cod_database_code               1560720
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.539
_shelx_estimated_absorpt_t_min   0.500
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C77) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C81)
\\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(C78) \\sim Ueq,
Uanis(C63) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C79)
\\sim Ueq, Uanis(C72) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C20(H20A,H20B), C23(H23A,H23B), C27(H27A,H27B), C32(H32A,
 H32B), C33(H33A,H33B), C36(H36A,H36B), C42(H42A,H42B), C43(H43A,H43B),
 C44(H44A,H44B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C54(H54A,H54B),
  C55(H55A,H55B), C62(H62A,H62B), C63(H63A,H63B), C65(H65A,H65B), C66(H66A,
 H66B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B),
 C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B),
  C77(H77A,H77B), C78(H78A,H78B), C79(H79A,H79B), C80(H80A,H80B), C81(H81A,
 H81B), C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C10(H10), C12(H12), C14(H14),
 C15(H15), C16(H16), C22(H22), C24(H24), C28(H28), C30(H30), C35(H35), C39(H39),
  C40(H40), C41(H41), C49(H49), C56(H56), C58(H58), C59(H59), C64(H64), C67(H67)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              69372
_shelx_hkl_checksum              43363
_shelx_fab_checksum              66058
_olex2_submission_special_instructions 'No special instructions were received'