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_4126633
_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         'I2, C66 H84 O12'
_chemical_formula_sum            'C66 H84 I2 O12'
_chemical_formula_weight         1323.13
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-05-09
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha                106.470(2)
_cell_angle_beta                 103.657(2)
_cell_angle_gamma                110.715(2)
_cell_formula_units_Z            1
_cell_length_a                   10.4135(5)
_cell_length_b                   13.1885(6)
_cell_length_c                   13.7554(7)
_cell_measurement_reflns_used    9993
_cell_measurement_temperature    173
_cell_measurement_theta_max      66.63
_cell_measurement_theta_min      3.92
_cell_volume                     1570.83(14)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      173.0
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16006
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        66.625
_diffrn_reflns_theta_max         66.625
_diffrn_reflns_theta_min         3.614
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.342
_exptl_absorpt_correction_T_max  0.3182
_exptl_absorpt_correction_T_min  0.1841
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0995 before and 0.0396 after correction. The Ratio of minimum to maximum transmission is 0.5786. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       block
_exptl_crystal_F_000             682
_refine_diff_density_max         0.970
_refine_diff_density_min         -1.198
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         5496
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0220P)^2^+2.1442P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0779
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5164
_reflns_number_total             5496
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b09850_si_002.cif
_cod_data_source_block           170503zd_pt_red_0m
_cod_original_cell_volume        1570.83(13)
_cod_database_code               4126633
_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.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C9(H9A,H9B), C12(H12A,H12B), C17(H17A,H17B), C20(H20A,H20B),
 C23(H23A,H23B), C28(H28A,H28B), C31(H31A,H31B), C32(H32A,H32B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C14(H14), C19(H19), C25(H25), C30(H30)
2.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C13(H13A,H13B,H13C), C18(H18A,H18B,H18C), C24(H24A,H24B,
 H24C), C29(H29A,H29B,H29C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              77295
_shelx_hkl_checksum              77453
_olex2_submission_special_instructions 'No special instructions were received'