Linear Positional Isomer Sorting in Nonporous Adaptive Crystals of a Pillar[5]arene.
Jie, Kecheng; Zhou, Yujuan; Li, Errui; Zhao, Run; Liu, Ming; Huang, Feihe; Journal of the American Chemical Society  (2018) –; doi:10.1021/jacs.7b13156

data_4127186
_publ_section_title
;
 Linear Positional Isomer Sorting in Nonporous Adaptive Crystals of a
 Pillar[5]arene.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b13156
_journal_year                    2018
_chemical_formula_moiety         'C55 H70 O10, C5 H12'
_chemical_formula_sum            'C60 H82 O10'
_chemical_formula_weight         963.25
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-01-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            8
_cell_length_a                   43.4083(19)
_cell_length_b                   15.7004(7)
_cell_length_c                   16.1394(6)
_cell_measurement_reflns_used    3511
_cell_measurement_temperature    170.1
_cell_measurement_theta_max      67.4633
_cell_measurement_theta_min      3.4099
_cell_volume                     10999.4(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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      170.0
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
;
  1 omega  -34.00   67.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       40.3188  -38.0000  -60.0000 101

  2 omega   20.00   61.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000    0.0000 41

  3 omega   23.00   71.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000 -120.0000 48

  4 omega   33.00   77.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000   90.0000 44

  5 omega   76.00  152.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -15.0000 -150.0000 76

  6 omega   40.00   77.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  -60.0000 37

  7 omega   10.00   36.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -15.0000 -150.0000 26
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0196749000
_diffrn_orient_matrix_UB_12      0.0142451000
_diffrn_orient_matrix_UB_13      0.0783066000
_diffrn_orient_matrix_UB_21      0.0257001000
_diffrn_orient_matrix_UB_22      -0.0558368000
_diffrn_orient_matrix_UB_23      -0.0370685000
_diffrn_orient_matrix_UB_31      0.0145630000
_diffrn_orient_matrix_UB_32      0.0793976000
_diffrn_orient_matrix_UB_33      -0.0400909000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0845
_diffrn_reflns_av_unetI/netI     0.0707
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24462
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.579
_diffrn_reflns_theta_max         67.579
_diffrn_reflns_theta_min         4.058
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.617
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49208
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_description       block
_exptl_crystal_F_000             4176
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         9715
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1147
_refine_ls_R_factor_gt           0.0663
_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^)+(0.0908P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1638
_refine_ls_wR_factor_ref         0.2013
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5709
_reflns_number_total             9715
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b13156_si_005.cif
_cod_data_source_block           170110_etp5_p_chcl3_3rd
_cod_original_cell_volume        10999(1)
_cod_database_code               4127186
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'c10 h10 o10'
_cell_oxdiff_angle_alpha         90.020(5)
_cell_oxdiff_angle_beta          90.065(5)
_cell_oxdiff_angle_gamma         90.013(5)
_cell_oxdiff_length_a            43.409(3)
_cell_oxdiff_length_b            15.7019(9)
_cell_oxdiff_length_c            16.1376(10)
_cell_oxdiff_measurement_reflns_used 3468
_cell_oxdiff_volume              10999(1)
_shelx_estimated_absorpt_t_max   0.790
_shelx_estimated_absorpt_t_min   0.756
_reflns_odcompleteness_completeness 99.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_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.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B), C10(H10A,H10B), C12(H12A,H12B), C19(H19A,H19B),
 C21(H21A,H21B), C23(H23A,H23B), C30(H30A,H30B), C32(H32A,H32B), C34(H34A,H34B),
  C41(H41A,H41B), C43(H43A,H43B), C45(H45A,H45B), C52(H52A,H52B), C54(H54A,
 H54B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C15(H15), C18(H18), C26(H26), C29(H29), C37(H37), C40(H40),
 C48(H48), C51(H51)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C20(H20A,H20B,H20C), C22(H22A,H22B,
 H22C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C42(H42A,H42B,H42C), C44(H44A,
 H44B,H44C), C53(H53A,H53B,H53C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C),
 C60(H60A,H60B,H60C)
;
_shelx_res_checksum              98234
_shelx_hkl_checksum              48290
_olex2_submission_special_instructions 'No special instructions were received'