Alkyl Chain Length-Selective Vapor-Induced Fluorochromism of Pillar[5]arene-Based Nonporous Adaptive Crystals.
Li, Qi; Zhu, Huangtianzhi; Huang, Feihe; Journal of the American Chemical Society 141 (2019) 13290–13294; doi:10.1021/jacs.9b05054

data_4128913
_publ_section_title
;
 Alkyl Chain Length-Selective Vapor-Induced Fluorochromism of
 Pillar[5]arene-Based Nonporous Adaptive Crystals.
;
_journal_issue                   34
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13290
_journal_page_last               13294
_journal_paper_doi               10.1021/jacs.9b05054
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         '2(C6 H12 O), C75 H62 O8'
_chemical_formula_sum            'C87 H86 O10'
_chemical_formula_weight         1291.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.8810(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9839(3)
_cell_length_b                   35.7918(7)
_cell_length_c                   15.4191(3)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      54.79
_cell_measurement_theta_min      3.099
_cell_volume                     7302.1(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      169.98
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            46176
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.964
_diffrn_reflns_theta_min         3.400
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.385
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.6538
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0939 before and 0.0532 after correction. The Ratio of minimum to maximum transmission is 0.8708. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_description       block
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.581
_refine_diff_density_min         -0.987
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     886
_refine_ls_number_reflns         13771
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.1533
_refine_ls_R_factor_gt           0.0984
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1605P)^2^+7.7607P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2711
_refine_ls_wR_factor_ref         0.3177
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7951
_reflns_number_total             13771
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            MeP5en-C6.cif
_cod_data_source_block           wmj18196_0m
_cod_database_code               4128913
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.963
_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. Uiso/Uaniso restraints and constraints
C84 \\sim C86 \\sim C85 \\sim C83 \\sim C82 \\sim C87 \\sim O10: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C14(H14A,H14B), C23(H23A,H23B),
 C28(H28A,H28B), C37(H37A,H37B), C46(H46A,H46B), C83(H83A,H83B), C84(H84A,H84B),
  C85(H85A,H85B)
3.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C13(H13), C18(H18), C22(H22), C26(H26), C32(H32), C36(H36), C41(H41),
 C45(H45), C48(H48), C54(H54), C57(H57), C58(H58), C59(H59), C60(H60), C61(H61),
  C62(H62), C63(H63), C64(H64), C70(H70), C73(H73), C74(H74), C75(H75),
 C76(H76), C77(H77), C78(H78), C79(H79), C80(H80)
3.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C11(H11A,H11B,H11C), C17(H17A,H17B,H17C),
 C21(H21A,H21B,H21C), C31(H31A,H31B,H31C), C35(H35A,H35B,H35C), C40(H40A,H40B,
 H40C), C44(H44A,H44B,H44C), C81(H81A,H81B,H81C), C86(H86A,H86B,H86C), C87(H87A,
 H87B,H87C)
;
_shelx_res_checksum              5383
_shelx_hkl_checksum              82875
_shelx_fab_checksum              70234
_olex2_submission_special_instructions 'No special instructions were received'