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_4132261
_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'
_chemical_formula_sum            'C66 H84 O12'
_chemical_formula_weight         1069.33
_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             2017-06-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_cell_angle_alpha                86.472(3)
_cell_angle_beta                 82.616(3)
_cell_angle_gamma                71.064(3)
_cell_formula_units_Z            2
_cell_length_a                   11.0743(4)
_cell_length_b                   12.6665(4)
_cell_length_c                   23.3275(6)
_cell_measurement_reflns_used    3272
_cell_measurement_temperature    298
_cell_measurement_theta_max      21.7255717634
_cell_measurement_theta_min      0.855704124247
_cell_volume                     3068.77(18)
_computing_cell_refinement
'DIALS 2theta refinement, DIALS 1.6.2-g7df89bd4-release'
_computing_data_collection
'DIALS 2theta refinement, DIALS 1.6.2-g7df89bd4-release'
_computing_data_reduction
'DIALS 2theta refinement, DIALS 1.6.2-g7df89bd4-release'
_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      298
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_type            'Dectris Pilatus 2M'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMount'
_diffrn_radiation_collimation    '0.3 x 1.5 Double Pinhole'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.1284
_diffrn_reflns_av_unetI/netI     0.1366
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14607
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        19.535
_diffrn_reflns_theta_max         19.535
_diffrn_reflns_theta_min         1.648
_diffrn_source                   Synchrotron
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.997403905322
_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    1.157
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.017
_exptl_crystal_size_mid          0.013
_exptl_crystal_size_min          0.011
_refine_diff_density_max         0.163
_refine_diff_density_min         -0.185
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.752
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     715
_refine_ls_number_reflns         5846
_refine_ls_number_restraints     594
_refine_ls_restrained_S_all      0.756
_refine_ls_R_factor_all          0.1116
_refine_ls_R_factor_gt           0.0610
_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^)+(0.0300P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1317
_refine_ls_wR_factor_ref         0.1479
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2358
_reflns_number_total             5846
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02621_si_007.cif
_cod_data_source_block           pillar6arene-et_desolvate_298k
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '__diffrn_measurement_device_type' was replaced with
'_diffrn_measurement_device_type'.

Automatic conversion script
Id: cif_correct_tags 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4132261
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C65-C64 = C58-C57 = C59-C57
 1.54 with sigma of 0.01
 O10-C62
 1.415 with sigma of 0.01
 O5-C51
 1.415 with sigma of 0.01
 C65-C64
 1.54 with sigma of 0.01
3. 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
4. Others
 Fixed Sof: H57A(0.5) H57B(0.5) H57C(0.5) H57D(0.5) C59(0.5) H59A(0.5)
 H59B(0.5) H59C(0.5) C58(0.5) H58A(0.5) H58B(0.5) H58C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C21(H21A,H21B), C28(H28A,H28B), C35(H35A,H35B),
 C42(H42A,H42B), C43(H43A,H43B), C45(H45A,H45B), C47(H47A,H47B), C49(H49A,H49B),
  C51(H51A,H51B), C53(H53A,H53B), C55(H55A,H55B), C57(H57A,H57B), C57(H57C,
 H57D), C60(H60A,H60B), C62(H62A,H62B), C64(H64A,H64B), C66(H66A,H66B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C9(H9), C12(H12), C17(H17), C20(H20), C24(H24), C27(H27),
 C31(H31), C34(H34), C37(H37), C40(H40)
5.c Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C50(H50A,H50B,
 H50C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C56(H56A,H56B,H56C), C61(H61A,
 H61B,H61C), C63(H63A,H63B,H63C), C65(H65A,H65B,H65C), C67(H67A,H67B,H67C),
 C59(H59A,H59B,H59C), C58(H58A,H58B,H58C)
;
_thetm01_alert_3_a
;
Problem: ALERT: The value of sine(theta_max)/wavelength is less than 0.550
 Calculated sin(theta_max)/wavelength = 0.4854

Response: Single crystals of this phase were small, disordered and weakly 
diffracting. As a result, a 1.03 ang. resolution limit was applied during 
refinement.
;
_shelx_res_checksum              18565
_shelx_hkl_checksum              99596
_olex2_submission_special_instructions 'No special instructions were received'