Near-Ideal Xylene Selectivity in Adaptive Molecular Pillar[ n]arene Crystals.
Jie, Kecheng; Liu, Ming; Zhou, Yujuan; Little, Marc A.; Pulido, Angeles; Chong, Samantha Y.; Stephenson, Andrew; Hughes, Ashlea R.; Sakakibara, Fumiyasu; Ogoshi, Tomoki; Blanc, Frédéric; Day, Graeme M.; Huang, Feihe; Cooper, Andrew I.; Journal of the American Chemical Society 140 (2018) 6921–6930; doi:10.1021/jacs.8b02621

data_4132258
_publ_section_title
;
 Near-Ideal Xylene Selectivity in Adaptive Molecular Pillar[ n]arene
 Crystals.
;
_journal_issue                   22
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6921
_journal_page_last               6930
_journal_paper_doi               10.1021/jacs.8b02621
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C66 H84 O12, C8 H10'
_chemical_formula_sum            'C74 H94 O12'
_chemical_formula_weight         1175.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-05-31
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 116.6494(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.6748(18)
_cell_length_b                   12.5778(9)
_cell_length_c                   26.133(3)
_cell_measurement_reflns_used    5671
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.532
_cell_measurement_theta_min      2.822
_cell_volume                     7248.9(11)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_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, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            30291
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         1.839
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.6245
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0895 before and 0.0588 after correction.
The Ratio of minimum to maximum transmission is 0.6729.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.077
_exptl_crystal_description       block
_exptl_crystal_F_000             2536
_exptl_crystal_size_max          0.201
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.062
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         7421
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1188
_refine_ls_R_factor_gt           0.0792
_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^)+(0.1300P)^2^+8.9100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2159
_refine_ls_wR_factor_ref         0.2479
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4848
_reflns_number_total             7421
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02621_si_008.cif
_cod_data_source_block           Pillar-6-Arene-Et_o-Xylene_100K_publ
_cod_original_cell_volume        7248.8(10)
_cod_database_code               4132258
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C34-C34_$1 = C34-C35 = C36-C35 = C36-C36_$1
 1.39 with sigma of 0.015
 C36-C37
 1.49 with sigma of 0.02
 C43-C43_$1 = C44-C43 = C45-C44 = C45-C45_$1
 1.39 with sigma of 0.01
 C42-C43
 1.49 with sigma of 0.01
 C39-C39_$1 = C40-C39 = C41-C40 = C41-C41_$1
 1.39 with sigma of 0.015
 C38_$1-C39_$1
 1.49 with sigma of 0.02
 C34-C36
 2.41 with sigma of 0.02
 C39-C41
 2.41 with sigma of 0.02
3. Restrained planarity
 C34, C34_$1, C35_$1, C35, C36, C36_$1, C37
 with sigma of 0.01
 C42, C43, C43_$1, C44, C42_$1, C44_$1, C45, C45_$1
 with sigma of 0.001
 C38_$1, C38, C39_$1, C39, C40_$1, C40, C41, C41_$1
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C45) = Uanis(C43) = Uanis(C44) = Uanis(C43) = Uanis(C42) = Uanis(C44) =
Uanis(C42) = Uanis(C45)
5. Rigid body (RIGU) restrains
 C36, C34, C34, C35, C35, C36, C37, C37
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C42, C43, C43, C44, C42, C44, C45, C45
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C40, C38, C39, C39, C38, C40, C41, C41
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C36, C34, C35, C37, C38, C39, C40, C41
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
6. Others
 Fixed Sof: C38(0.275) H38A(0.275) H38B(0.275) H38C(0.275) C39(0.275)
 C40(0.275) H40(0.275) C41(0.275) H41(0.275) C34(0.45) H34(0.45) C35(0.45)
 H35(0.45) C36(0.45) C37(0.45) H37A(0.45) H37B(0.45) H37C(0.45) C43(0.275)
 C42(0.275) H42A(0.275) H42B(0.275) H42C(0.275) C44(0.275) H44(0.275)
 C45(0.275) H45(0.275)
7.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B), C15(H15A,H15B), C22(H22A,H22B), C24(H24A,H24B),
 C26(H26A,H26B), C28(H28A,H28B), C30(H30A,H30B), C32(H32A,H32B)
7.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C3(H3), C10(H10), C13(H13), C17(H17), C20(H20), C40(H40), C41(H41),
 C34(H34), C35(H35), C44(H44), C45(H45)
7.c Fitted hexagon refined as free rotating group:
 C6(C5,C4,C3,C2,C7)
7.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C29(H29A,H29B,
 H29C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C38(H38A,H38B,H38C), C37(H37A,
 H37B,H37C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              39087
_shelx_hkl_checksum              51427
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'