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_4128914
_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         'C75 H62 O8, 2(C3 O)'
_chemical_formula_sum            'C81 H62 O10'
_chemical_formula_weight         1195.30
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-10-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.7437(4)
_cell_length_b                   31.7874(7)
_cell_length_c                   32.5089(10)
_cell_measurement_reflns_used    9886
_cell_measurement_temperature    170.15
_cell_measurement_theta_max      26.30
_cell_measurement_theta_min      2.40
_cell_volume                     13169.0(6)
_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)'
_diffrn_ambient_temperature      170.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'D8 VENTUNE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            84345
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_min         2.401
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0855 before and 0.0613 after correction.
The Ratio of minimum to maximum transmission is 0.9060.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_description       block
_exptl_crystal_F_000             5024
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.075
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     832
_refine_ls_number_reflns         12049
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.1251
_refine_ls_R_factor_gt           0.0957
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0869P)^2^+33.8099P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2515
_refine_ls_wR_factor_ref         0.2745
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8879
_reflns_number_total             12049
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            MeP5en-C3.cif
_cod_data_source_block           181015_mep5_en_acechcl3_0m_a_pl
_cod_database_code               4128914
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.975
_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
 O7-C35A
 1.51 with sigma of 0.001
 C80-C81
 1.51 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O7 \\sim C35 \\sim C35A: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C77 \\sim C79 \\sim C80 \\sim O10 \\sim C81: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C35) = Uanis(C35A)
4. Others
 Sof(C35A)=Sof(H35D)=Sof(H35E)=Sof(H35F)=1-FVAR(1)
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=FVAR(1)
 Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=1-FVAR(2)
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=FVAR(2)
 Fixed X: O10(-0.11071) C79(0.048141) C80(-0.03442) C81(0.0101)
 Fixed Y: O10(0.41596) C79(0.403529) C80(0.42504) C81(0.466419)
 Fixed Z: O10(0.19274) C79(0.15019) C80(0.18488) C81(0.20996)
5.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C37(H37A,H37B), C1(H1A,H1B), C28(H28A,H28B), C10(H10A,H10B)
5.b Aromatic/amide H refined with riding coordinates:
 C42(H42), C33(H33), C39(H39), C72(H72), C69(H69), C53(H53), C15(H15),
 C56(H56), C59(H59), C57(H57), C64(H64), C73(H73), C12(H12), C75(H75), C6(H6),
 C67(H67), C74(H74), C58(H58), C24(H24), C51(H51), C21(H21), C3(H3), C48(H48),
 C66(H66), C30(H30), C65(H65), C50(H50), C49(H49)
5.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C36(H36A,H36B,H36C), C27(H27A,H27B,H27C), C26(H26A,H26B,
 H26C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C35(H35A,H35B,H35C), C8(H8A,
 H8B,H8C), C35A(H35D,H35E,H35F), C8A(H8AA,H8AB,H8AC)
;
_shelx_res_checksum              39435
_shelx_hkl_checksum              37166
_olex2_submission_special_instructions 'No special instructions were received'