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_4132259
_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           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-01-19
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.11.10 svn.r3248 for OlexSys, GUI svn.r5133)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.752(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.5241(9)
_cell_length_b                   12.9030(11)
_cell_length_c                   22.5069(19)
_cell_measurement_reflns_used    9967
_cell_measurement_temperature    240
_cell_measurement_theta_max      28.78
_cell_measurement_theta_min      2.40
_cell_volume                     3345.1(5)
_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 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0563
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            44537
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.144
_diffrn_reflns_theta_min         1.810
_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    0.078
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.6776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0960 before and 0.0740 after correction.
The Ratio of minimum to maximum transmission is 0.7301.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_description       block
_exptl_crystal_F_000             1268
_exptl_crystal_size_max          0.322
_exptl_crystal_size_mid          0.317
_exptl_crystal_size_min          0.266
_refine_diff_density_max         0.180
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         9003
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.0528
_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^)+(0.0670P)^2^+0.7050P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1329
_refine_ls_wR_factor_ref         0.1563
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6296
_reflns_number_total             9003
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02621_si_009.cif
_cod_data_source_block           pillar_6_arene_p_xylene
_cod_database_code               4132259
_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
 O6-C32 \\sim O6-C32B
 with sigma of 0.02
 C33-C32 \\sim C33B-C32B
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 O6, C32B, C33B, C32, C33
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C33B)=Sof(H33D)=Sof(H33E)=Sof(H33F)=Sof(C32B)=Sof(H32C)=Sof(H32D)=1-FVAR(1)
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C15(H15A,H15B), C1(H1A,H1B), C24(H24A,H24B), C28(H28A,H28B),
 C26(H26A,H26B), C22(H22A,H22B), C30(H30A,H30B), C32(H32A,H32B), C32B(H32C,H32D)
5.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C3(H3), C10(H10), C6(H6), C18(H18), C21(H21), C37(H37), C35(H35)
5.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C29(H29A,H29B,
 H29C), C34(H34A,H34B,H34C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C),
 C33B(H33D,H33E,H33F)
;
_shelx_res_checksum              89110
_shelx_hkl_checksum              59598
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'