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_4128912
_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         'C5 H8 O, C75 H62 O8, C5 H10 O'
_chemical_formula_sum            'C85 H80 O10'
_chemical_formula_weight         1261.49
_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                 107.4470(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7735(2)
_cell_length_b                   34.9942(6)
_cell_length_c                   15.5970(2)
_cell_measurement_reflns_used    9771
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      54.836
_cell_measurement_theta_min      3.453
_cell_volume                     7171.79(19)
_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      169.96
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.989
_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  0.0432
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            55678
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.910
_diffrn_reflns_theta_min         3.392
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.385
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.6104
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1234 before and 0.0563 after correction. The Ratio of minimum to maximum transmission is 0.8130. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_description       block
_exptl_crystal_F_000             2680
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.402
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     868
_refine_ls_number_reflns         13479
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0746
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1068P)^2^+5.2006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2012
_refine_ls_wR_factor_ref         0.2170
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10524
_reflns_number_total             13479
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            MeP5en-C5.cif
_cod_data_source_block           wmj18195_0m
_cod_database_code               4128912
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.945
_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. Restrained distances
 C84-C82 = C82-C81 = C81-C10 = C85-C10
 1.53 with sigma of 0.02
 O83-C81
 2.2 with sigma of 0.02
 O83-C82
 1.28 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C22(H22A,H22B), C27(H27A,H27B), C36(H36A,H36B), C45(H45A,
 H45B), C10(H10A,H10B), C81(H81B,H81A)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C8(H8), C12(H12), C17(H17), C21(H21), C25(H25), C31(H31),
 C35(H35), C40(H40), C44(H44), C47(H47), C53(H53), C56(H56), C57(H57), C58(H58),
  C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C69(H69), C72(H72),
 C73(H73), C74(H74), C75(H75), C76(H76), C77(H77), C78(H78), C79(H79)
3.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C0AA(H0AA,H0AB,H0AC), C16(H16A,H16B,H16C),
 C20(H20A,H20B,H20C), C30(H30A,H30B,H30C), C34(H34A,H34B,H34C), C39(H39A,H39B,
 H39C), C43(H43A,H43B,H43C), C80(H80A,H80B,H80C), C84(H84A,H84B,H84C), C85(H85A,
 H85B,H85C)
;
_shelx_res_checksum              75547
_shelx_hkl_checksum              88940
_shelx_fab_checksum              35692
_olex2_submission_special_instructions 'No special instructions were received'