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_4132260
_publ_section_title
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 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         'C55 H70 O10'
_chemical_formula_sum            'C55 H70 O10'
_chemical_formula_weight         891.11
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-12-17
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.11.10 svn.r3248 for OlexSys, GUI svn.r5133)
;
_cell_angle_alpha                102.503(2)
_cell_angle_beta                 108.766(2)
_cell_angle_gamma                108.108(2)
_cell_formula_units_Z            2
_cell_length_a                   12.6553(9)
_cell_length_b                   14.9068(10)
_cell_length_c                   15.8129(12)
_cell_measurement_reflns_used    8758
_cell_measurement_temperature    240
_cell_measurement_theta_max      29.022
_cell_measurement_theta_min      2.196
_cell_volume                     2513.2(3)
_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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      240
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.985
_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  0.0544
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36490
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        27.650
_diffrn_reflns_theta_max         27.672
_diffrn_reflns_theta_min         1.535
_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    0.080
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1524 before and 0.0873 after correction.
The Ratio of minimum to maximum transmission is 0.6374.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         11582
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0635
_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^)+(0.1078P)^2^+0.4379P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1700
_refine_ls_wR_factor_ref         0.1966
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8177
_reflns_number_total             11582
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02621_si_003.cif
_cod_data_source_block           Pillar[5]arene_P-1_240K_publ
_cod_database_code               4132260
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 O5-C46 \\sim O5-C47
 with sigma of 0.02
 C46-C48 \\sim C47-C48
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 O5, C47, C48, C46
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H48D)=Sof(H48E)=Sof(H48F)=Sof(C46)=Sof(H46A)=Sof(H46B)=1-FVAR(1)
 Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H48A)=Sof(H48B)=Sof(H48C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C21(H21A,H21B), C28(H28A,H28B), C35(H35A,H35B),
 C36(H36A,H36B), C38(H38A,H38B), C40(H40A,H40B), C42(H42A,H42B), C47(H47A,H47B),
  C51(H51A,H51B), C55(H55A,H55B), C44(H44A,H44B), C46(H46A,H46B), C49(H49A,
 H49B), C53(H53A,H53B)
5.b Me refined with riding coordinates:
 C48(H48A,H48B,H48C), C48(H48D,H48E,H48F)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C9(H9), C12(H12), C16(H16), C19(H19), C23(H23), C26(H26),
 C31(H31), C34(H34)
5.d Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C43(H43A,H43B,
 H43C), C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C45(H45A,H45B,H45C), C54(H54A,
 H54B,H54C), C56(H56A,H56B,H56C)
;
_shelx_res_checksum              74397
_shelx_hkl_checksum              49329
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'