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_4132257
_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         'C66 H84 O12, (C8 H10)'
_chemical_formula_sum            'C74 H94 O12'
_chemical_formula_weight         1175.49
_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             2017-06-28
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_cell_angle_alpha                93.34(17)
_cell_angle_beta                 94.55(18)
_cell_angle_gamma                102.22(16)
_cell_formula_units_Z            1
_cell_length_a                   11.10(2)
_cell_length_b                   12.196(19)
_cell_length_c                   14.06(3)
_cell_measurement_reflns_used    578
_cell_measurement_temperature    298
_cell_measurement_theta_max      21.4271944659
_cell_measurement_theta_min      2.07450477191
_cell_volume                     1849(6)
_computing_cell_refinement
'DIALS 2theta refinement, DIALS 1.6.2-g7df89bd4-release'
_computing_data_collection       'GDA, I19, DLS, RAL'
_computing_data_reduction
;
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
DIALS 1.6.2-g7df89bd4-release
pointless (Evans, P., 2006)
XIA2 0.5.328-gd3a94be2-dials-1.6-hotfix-5d8177 (Winter, G., 2010)
;
_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      298
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_type            'Dectris Pilatus 2M'
_diffrn_measured_fraction_theta_full 0.739
_diffrn_measured_fraction_theta_max 0.739
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       '\f rotation with 0.2 degree frames'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_collimation    synchrotron
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.1184
_diffrn_reflns_Laue_measured_fraction_full 0.739
_diffrn_reflns_Laue_measured_fraction_max 0.739
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4027
_diffrn_reflns_point_group_measured_fraction_full 0.739
_diffrn_reflns_point_group_measured_fraction_max 0.739
_diffrn_reflns_theta_full        22.502
_diffrn_reflns_theta_max         22.502
_diffrn_reflns_theta_min         1.412
_diffrn_source                   Synchrotron
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  1.0
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CCP4 7.0.040: AIMLESS, version 0.5.32 : 29/03/17
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.055
_exptl_crystal_description       block
_exptl_crystal_F_000             634
_exptl_crystal_size_max          0.019
_exptl_crystal_size_mid          0.014
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         3943
_refine_ls_number_restraints     308
_refine_ls_restrained_S_all      4.598
_refine_ls_R_factor_all          0.3027
_refine_ls_R_factor_gt           0.1173
_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^)+(0.0010P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1553
_refine_ls_wR_factor_ref         0.1781
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1247
_reflns_number_total             3943
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02621_si_005.cif
_cod_data_source_block           pillar-6-arene_m-xylene_p-1_298k
_cod_database_code               4132257
_shelx_shelxl_version_number     2014/7
_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
 C40-C37
 1.49 with sigma of 0.01
 C39-C41
 1.49 with sigma of 0.01
 C36-C40 \\sim C40-C38
 with sigma of 0.02
 C38-C41 \\sim C41-C40
 with sigma of 0.02
3. Restrained planarity
 C36, C37, C38, C39, C35, C40, C41, C38, C37, C36, C37, C39, C38, C36, C35,
 C39, C40, C39, C41, C35, C40, C35
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uiso(C40) = Uiso(C37) = Uiso(C38) = Uiso(C36) = Uiso(C39) = Uiso(C35) =
Uiso(C41) = Uiso(C34) = Uiso(C38) = Uiso(C37) = Uiso(C40) = Uiso(C37) =
Uiso(C36) = Uiso(C37) = Uiso(C39) = Uiso(C38) = Uiso(C36) = Uiso(C35) =
Uiso(C39) = Uiso(C41) = Uiso(C39) = Uiso(C34) = Uiso(C35) = Uiso(C34)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C37(0.5) H37(0.5) C38(0.5) H38(0.5) C39(0.5) C40(0.5) H40(0.5)
 C35(0.5) C36(0.5) H36(0.5) C41(0.5) H41A(0.5) H41B(0.5) H41C(0.5) C34(0.5)
 H34A(0.5) H34B(0.5) H34C(0.5)
 Fixed X: H41A(0.83829) H41B(0.73568) H41C(0.81972)
 Fixed Y: H41A(0.38063) H41B(0.2853) H41C(0.3742)
 Fixed Z: H41A(0.939719) H41B(0.973109) H41C(1.04875)
7.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C14(H14A,H14B), C7(H7A,H7B), C24(H24A,H24B), C28(H28A,H28B),
 C26(H26A,H26B), C30(H30A,H30B), C32(H32A,H32B), C22(H22A,H22B)
7.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C9(H9), C20(H20), C12(H12), C1(H1), C17(H17), C37(H37), C38(H38),
 C40(H40), C36(H36)
7.c Fitted hexagon refined as free rotating group:
 C37(C38,C39,C40,C35,C36)
7.d Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C25(H25A,H25B,H25C), C33(H33A,H33B,H33C), C29(H29A,H29B,
 H29C), C31(H31A,H31B,H31C), C23(H23A,H23B,H23C), C34(H34A,H34B,H34C)
;
_plat029_alert_3_a
;
Problem: ALERT: _diffrn_measured_fraction_theta_full value Low .  0.739 Note

Response: Due to severe radiation damage the full data collection could not be 
completed. The final data completeness is ~ 74%. 
;
_thetm01_alert_3_b
;
Problem: The value of sine(theta_max)/wavelength is less than 0.575
            Calculated sin(theta_max)/wavelength =    0.5555
Response: Single crystals of this phase were very small and weakly 
diffracting. A suitable resolution limit of 0.9 ang. was applied during 
refinement. 
;
_plat026_alert_3_b
;
Problem: ALERT: Ratio Observed / Unique Reflections (too) Low ..         32 %

Response: Due to severe radiation damage the full data collection could not be 
completed. The final data completeness is ~ 74% and the number of unique 
reflections is low. 
;
_plat340_alert_3_b
;
Problem: ALERT: Low Bond Precision on  C-C Bonds ...............    0.01503 Ang.  

Response: Due to the poor resolition and quality of the X-ray data. 
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_shelx_res_checksum              86340
_shelx_hkl_checksum              49333
_olex2_submission_special_instructions 'No special instructions were received'