Porous Organic Cages for Sulfur Hexafluoride Separation.
Hasell, Tom; Miklitz, Marcin; Stephenson, Andrew; Little, Marc A.; Chong, Samantha Y.; Clowes, Rob; Chen, Linjiang; Holden, Daniel; Tribello, Gareth A.; Jelfs, Kim E.; Cooper, Andrew I.; Journal of the American Chemical Society 138 (2016) 1653–1659; doi:10.1021/jacs.5b11797

data_4129911
_publ_section_title
;
 Porous Organic Cages for Sulfur Hexafluoride Separation.
;
_journal_issue                   5
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1653
_journal_page_last               1659
_journal_paper_doi               10.1021/jacs.5b11797
_journal_volume                  138
_journal_year                    2016
_chemical_absolute_configuration CC3-S
_chemical_formula_moiety         '2.5(F6 S), 2(C72 H84 N12), 3(H2 O)'
_chemical_formula_sum            'C144 H174 F15.01 N24 O3 S2.5'
_chemical_formula_weight         2654.40
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-07-23
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                60.384(3)
_cell_angle_beta                 60.308(3)
_cell_angle_gamma                60.168(3)
_cell_formula_units_Z            1
_cell_length_a                   17.385(5)
_cell_length_b                   17.425(6)
_cell_length_c                   17.479(6)
_cell_measurement_reflns_used    9854
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.468
_cell_measurement_theta_min      2.249
_cell_volume                     3768(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 0.0350
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device       'CrystalLogic Kappa (4 circle)'
_diffrn_measurement_device_type  'Kappa Rigaku Saturn724+'
_diffrn_measurement_method       'omega rotation'
_diffrn_radiation_collimation    '0.3 x 1.5 Double Pinhole'
_diffrn_radiation_monochromator  Synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            52288
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         25.503
_diffrn_reflns_theta_min         1.376
_diffrn_source                   Synchrotron
_diffrn_source_target            Cu
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_T_max  0.9705
_exptl_absorpt_correction_T_min  0.8444
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0746 before and 0.0525 after correction. The Ratio of minimum to maximum transmission is 0.8701. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_description       prism
_exptl_crystal_F_000             1405
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.801
_refine_diff_density_min         -0.923
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Flack x determined using 8363 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.14(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1786
_refine_ls_number_reflns         28131
_refine_ls_number_restraints     363
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1091
_refine_ls_R_factor_gt           0.0894
_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^)+(0.1733P)^2^+1.1104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2378
_refine_ls_wR_factor_ref         0.2549
_reflns_Friedel_coverage         0.980
_reflns_Friedel_fraction_full    0.981
_reflns_Friedel_fraction_max     0.959
_reflns_number_gt                22028
_reflns_number_total             28131
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b11797_si_002.cif
_cod_data_source_block           CC3_SF6
_cod_original_formula_sum        'C144 H174 F15.01 N24 O3 S2.50'
_cod_database_code               4129911
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.773(2) 0.227(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 S6-F35 = S6-F31 = S6-F34 = S6-F33 = S6-F32 = S6-F36
 1.54 with sigma of 0.02
 S5-F26 = S5-F30 = S5-F27 = S5-F25 = S5-F28 = S5-F29
 1.54 with sigma of 0.02
 S3-F17 = S3-F14 = S3-F15 = S3-F16 = S3-F13 = S3-F18
 1.54 with sigma of 0.02
 S4-F21 = S4-F20 = S4-F24 = S4-F23 = S4-F22 = S4-F19
 1.54 with sigma of 0.02
 F33-F34 \\sim F33-F36 \\sim F33-F31 \\sim F33-F32 \\sim F35-F34 \\sim F35-F36
\\sim F35-F31 \\sim F35-F32
 \\sim F34-F31 \\sim F34-F32 \\sim F36-F31 \\sim F36-F32
 with sigma of 0.02
 F26-F30 \\sim F26-F28 \\sim F26-F29 \\sim F26-F27 \\sim F25-F30 \\sim F25-F28
\\sim F25-F29 \\sim F25-F27
 \\sim F30-F29 \\sim F30-F27 \\sim F28-F29 \\sim F28-F27
 with sigma of 0.02
 F16-F15 \\sim F16-F17 \\sim F16-F14 \\sim F16-F13 \\sim F18-F15 \\sim F18-F17
\\sim F18-F14 \\sim F18-F13
 \\sim F15-F14 \\sim F15-F13 \\sim F17-F14 \\sim F17-F13
 with sigma of 0.02
 F20-F23 \\sim F20-F21 \\sim F20-F24 \\sim F20-F22 \\sim F19-F23 \\sim F19-F21
\\sim F19-F24 \\sim F19-F22
 \\sim F23-F24 \\sim F23-F22 \\sim F21-F24 \\sim F21-F22
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uiso(F34) = Uiso(S6) = Uiso(F31) = Uiso(F35) = Uiso(F32) = Uiso(F33) = Uiso(F36)
Uiso(F26) = Uiso(S5) = Uiso(F30) = Uiso(F29) = Uiso(F28) = Uiso(F27) = Uiso(F25)
Uiso(F16) = Uiso(S3) = Uiso(F13) = Uiso(F17) = Uiso(F18) = Uiso(F15) = Uiso(F14)
Uiso(F22) = Uiso(S4) = Uiso(F21) = Uiso(F23) = Uiso(F24) = Uiso(F19) = Uiso(F20)
5. Rigid body (RIGU) restrains
 C49, C50, C51, C52, C53, C54
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C72, C71, C70, C69, C68, C67
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(S6)=Sof(F34)=Sof(F31)=Sof(F35)=Sof(F32)=Sof(F33)=Sof(F36)=FVAR(1)
 Sof(S5)=Sof(F26)=Sof(F30)=Sof(F29)=Sof(F28)=Sof(F27)=Sof(F25)=FVAR(2)
 Sof(S3)=Sof(F13)=Sof(F17)=Sof(F16)=Sof(F18)=Sof(F15)=Sof(F14)=FVAR(3)
 Sof(S4)=Sof(F21)=Sof(F23)=Sof(F24)=Sof(F19)=Sof(F20)=Sof(F22)=FVAR(4)
 Fixed Sof: O7(0.5) O6(0.5) O5(0.5) O8(0.5) O9(0.5) O4(0.5)
7.a Ternary CH refined with riding coordinates:
 C144(H144), C109(H109), C48(H48), C121(H121), C132(H132), C115(H115),
 C127(H127), C114(H114), C126(H126), C120(H120), C42(H42), C138(H138), C72(H72),
  C43(H43), C54(H54), C37(H37), C139(H139), C67(H67), C55(H55), C59(H59),
 C133(H133), C66(H66), C61(H61), C49(H49)
7.b Secondary CH2 refined with riding coordinates:
 C110(H11A,H11B), C116(H11C,H11D), C125(H12A,H12B), C113(H11E,H11F), C38(H38A,
 H38B), C111(H11G,H11H), C122(H12C,H12D), C123(H12E,H12F), C143(H14A,H14B),
 C47(H47A,H47B), C128(H12G,H12H), C140(H14C,H14D), C142(H14E,H14F), C134(H13A,
 H13B), C130(H13C,H13D), C112(H11I,H11J), C119(H11K,H11L), C131(H13E,H13F),
 C124(H12I,H12J), C135(H13G,H13H), C44(H44A,H44B), C65(H65A,H65B), C41(H41A,
 H41B), C46(H46A,H46B), C117(H11M,H11N), C129(H12K,H12L), C60(H60A,H60B),
 C71(H71A,H71B), C118(H11O,H11P), C58(H58A,H58B), C136(H13I,H13J), C141(H14G,
 H14H), C45(H45A,H45B), C40(H40A,H40B), C137(H13K,H13L), C39(H39A,H39B),
 C56(H56A,H56B), C53(H53A,H53B), C57(H57A,H57B), C50(H50A,H50B), C52(H52A,H52B),
  C64(H64A,H64B), C68(H68A,H68B), C51(H51A,H51B), C62(H62A,H62B), C63(H63A,
 H63B), C70(H70A,H70B), C69(H69A,H69B)
7.c Aromatic/amide H refined with riding coordinates:
 C103(H103), C101(H101), C107(H107), C106(H106), C31(H31), C105(H105),
 C108(H108), C78(H78), C34(H34), C96(H96), C35(H35), C74(H74), C36(H36),
 C83(H83), C9(H9), C29(H29), C33(H33), C22(H22), C76(H76), C80(H80), C85(H85),
 C25(H25), C81(H81), C87(H87), C98(H98), C4(H4), C26(H26), C24(H24), C8(H8),
 C6(H6), C7(H7), C20(H20), C94(H94), C90(H90), C97(H97), C27(H27), C89(H89),
 C2(H2), C79(H79), C88(H88), C92(H92), C99(H99), C16(H16), C11(H11), C15(H15),
 C13(H13), C18(H18), C17(H17)
;
_shelx_res_checksum              40757
_shelx_hkl_checksum              45718
_olex2_submission_special_instructions 'No special instructions were received'