Transformation of Nonporous Adaptive Pillar[4]arene[1]quinone Crystals into Fluorescent Crystals via Multi-Step Solid-Vapor Postsynthetic Modification for Fluorescence Turn-on Sensing of Ethylenediamine.
Li, Errui; Jie, Kecheng; Fang, Yu; Cai, Peiyu; Huang, Feihe; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c07482

data_4135212
_publ_section_title
;
 Transformation of Nonporous Adaptive Pillar[4]arene[1]quinone Crystals
 into Fluorescent Crystals via Multi-Step Solid-Vapor Postsynthetic
 Modification for Fluorescence Turn-on Sensing of Ethylenediamine.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c07482
_journal_year                    2020
_chemical_formula_moiety         'C51 H60 O10, C2 H3 N'
_chemical_formula_sum            'C53 H63 N O10'
_chemical_formula_weight         874.04
_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     direct
_audit_creation_date             2017-11-03
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Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5381)
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_cell_length_a                   13.4820(6)
_cell_length_b                   17.7729(7)
_cell_length_c                   21.1215(10)
_cell_measurement_reflns_used    4893
_cell_measurement_temperature    170.6
_cell_measurement_theta_max      29.3388
_cell_measurement_theta_min      3.0246
_cell_volume                     5046.3(4)
_computing_cell_refinement
;
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)
;
_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)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      170.6
_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  -53.00   38.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       11.7808  -38.0000   30.0000 91

  2 omega  -15.00   88.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       11.7808   38.0000 -150.0000 103
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0226719000
_diffrn_orient_matrix_UB_12      0.0055754000
_diffrn_orient_matrix_UB_13      0.0288599000
_diffrn_orient_matrix_UB_21      -0.0164801000
_diffrn_orient_matrix_UB_22      0.0360848000
_diffrn_orient_matrix_UB_23      -0.0105768000
_diffrn_orient_matrix_UB_31      -0.0447091000
_diffrn_orient_matrix_UB_32      -0.0161288000
_diffrn_orient_matrix_UB_33      -0.0137443000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_av_unetI/netI     0.0823
_diffrn_reflns_Laue_measured_fraction_full 0.997
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_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21663
_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         25.350
_diffrn_reflns_theta_min         3.031
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.079
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_exptl_absorpt_correction_T_min  0.86522
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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.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.150
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_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.230
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         9217
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0613P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1270
_refine_ls_wR_factor_ref         0.1548
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5688
_reflns_number_total             9217
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           171102_ler_p5q_c6n2
_cod_original_cell_volume        5046.2(4)
_cod_database_code               4135212
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_chemical_oxdiff_formula         'c h n o'
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_shelx_estimated_absorpt_t_min   0.978
_reflns_odcompleteness_completeness 99.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C1(H1A,H1B), C8(H8A,H8B), C15(H15A,H15B), C17(H17A,H17B), C19(H19A,H19B),
 C26(H26A,H26B), C28(H28A,H28B), C30(H30A,H30B), C37(H37A,H37B), C39(H39A,H39B),
  C41(H41A,H41B), C48(H48A,H48B), C50(H50A,H50B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C10(H10), C13(H13), C21(H21), C24(H24), C32(H32), C35(H35),
 C43(H43), C46(H46)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C27(H27A,H27B,H27C), C29(H29A,H29B,
 H29C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C49(H49A,H49B,H49C), C51(H51A,
 H51B,H51C), C53(H53A,H53B,H53C)
;
_shelx_res_checksum              99844
_shelx_hkl_checksum              50957
_olex2_submission_special_instructions 'No special instructions were received'