Reversible Iodine Capture by Non-Porous Pillar[6]arene Crystals.
Jie, Kecheng; Zhou, Yujuan; Li, Errui; Li, Zhengtao; Zhao, Run; Huang, Feihe; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b09850

data_4126632
_publ_section_title
;
 Reversible Iodine Capture by Non-Porous Pillar[6]arene Crystals.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b09850
_journal_year                    2017
_chemical_formula_moiety         'C66 H84 O12'
_chemical_formula_sum            'C66 H84 O12'
_chemical_formula_weight         1069.33
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d'
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
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Olex2 1.2-beta
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_cell_angle_gamma                90
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_cell_length_a                   12.6104(7)
_cell_length_b                   26.6968(13)
_cell_length_c                   45.345(2)
_cell_measurement_reflns_used    4569
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      29.5044
_cell_measurement_theta_min      2.8316
_cell_volume                     15265.7(13)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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_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      293.15
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -14.00   73.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8433   38.0000 -150.0000 87

  2 omega  -65.00   37.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8433  -38.0000   30.0000 102

  3 omega  -75.00   21.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.7183  -77.0000  -90.0000 96
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_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0443332000
_diffrn_orient_matrix_UB_12      -0.0146002000
_diffrn_orient_matrix_UB_13      -0.0043484000
_diffrn_orient_matrix_UB_21      -0.0341938000
_diffrn_orient_matrix_UB_22      -0.0203870000
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_diffrn_orient_matrix_UB_31      -0.0056682000
_diffrn_orient_matrix_UB_32      0.0087776000
_diffrn_orient_matrix_UB_33      -0.0146673000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 0.997
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_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            23927
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.837
_diffrn_source                   'Enhance (Mo) X-ray Source'
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_exptl_absorpt_process_details
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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.
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_exptl_crystal_colour            colourless
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_refine_diff_density_rms         0.042
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         3620
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_gt           0.0730
_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^)+(0.1245P)^2^+17.6051P] where P=(Fo^2^+2Fc^2^)/3'
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_refine_ls_wR_factor_gt          0.2207
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_cod_data_source_block           160705_etp6_sq
_cod_database_code               4126632
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'c10 h10 n2 o8'
_reflns_odcompleteness_completeness 99.76
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_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. Others
 Fixed Sof: H9A(0.5) H9B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C9(H9A,H9B), C10(H10A,H10B), C14(H14A,H14B), C16(H16A,H16B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C12(H12)
3.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              60187
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_olex2_submission_special_instructions 'No special instructions were received'