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_4132262
_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         'C55 H70 O10, C8 H10'
_chemical_formula_sum            'C63 H80 O10'
_chemical_formula_weight         997.27
_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   mixed
_audit_creation_date             2015-12-14
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.11.10 svn.r3248 for OlexSys, GUI svn.r5133)
;
_cell_angle_alpha                82.538(2)
_cell_angle_beta                 89.865(2)
_cell_angle_gamma                89.331(2)
_cell_formula_units_Z            4
_cell_length_a                   12.6961(10)
_cell_length_b                   20.7685(18)
_cell_length_c                   21.3724(18)
_cell_measurement_reflns_used    9858
_cell_measurement_temperature    150
_cell_measurement_theta_max      32.416
_cell_measurement_theta_min      2.273
_cell_volume                     5587.3(8)
_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      150.0
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0526
_diffrn_reflns_av_unetI/netI     0.0671
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            95265
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        29.000
_diffrn_reflns_theta_max         29.130
_diffrn_reflns_theta_min         1.466
_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    0.079
_exptl_absorpt_correction_T_max  0.9282
_exptl_absorpt_correction_T_min  0.7166
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1221 before and 0.0723 after correction.
The Ratio of minimum to maximum transmission is 0.7720.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_description       plate
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.377
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1902
_refine_ls_number_reflns         30091
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+1.7749P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1198
_refine_ls_wR_factor_ref         0.1311
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22927
_reflns_number_total             30091
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02621_si_002.cif
_cod_data_source_block           pillar_5_arene_pxylene
_cod_database_code               4132262
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  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. Others
 Sof(H46D)=Sof(H46E)=Sof(H46F)=Sof(C45)=Sof(H45A)=Sof(H45B)=1-FVAR(1)
 Sof(H46A)=Sof(H46B)=Sof(H46C)=Sof(C44)=Sof(H44A)=Sof(H44B)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C45(H45A,H45B)
3.b Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C46(H46D,H46E,H46F), C57(H57A,H57B,H57C), C64(H64A,H64B,
 H64C), C120(H12A,H12B,H12C), C127(H12D,H12E,H12F)
;
_shelx_res_checksum              20027
_shelx_hkl_checksum              7396
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'