Ratiometric Turn-On Fluorophore Displacement Ensembles for Nitroaromatic Explosives Detection
Lee, Ji Yoon; Root, Harrison D.; Ali, Rashid; An, Won; Lynch, Vincent M.; Bähring, Steffen; Kim, In Su; Sessler, Jonathan L.; Park, Jung Su; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c08106

data_4135294
_publ_section_title
;
 Ratiometric Turn-On Fluorophore Displacement Ensembles for Nitroaromatic
 Explosives Detection
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c08106
_journal_year                    2020
_chemical_formula_moiety         'C60 H44 N4 S16, C28 H31 N2 O3, C H Cl3, Cl'
_chemical_formula_sum            'C89 H76 Cl4 N6 O3 S16'
_chemical_formula_weight         1932.31
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-12
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_cell_angle_alpha                69.421(7)
_cell_angle_beta                 75.275(6)
_cell_angle_gamma                72.132(6)
_cell_formula_units_Z            2
_cell_length_a                   13.2198(9)
_cell_length_b                   19.9501(14)
_cell_length_c                   21.0748(14)
_cell_measurement_reflns_used    7436
_cell_measurement_temperature    223
_cell_measurement_theta_max      55.6
_cell_measurement_theta_min      2.27
_cell_volume                     4885.3(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_diffrn_ambient_temperature      223
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker PhotonIII M14'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.2323
_diffrn_reflns_av_unetI/netI     0.1394
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            111323
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        56.354
_diffrn_reflns_theta_max         56.354
_diffrn_reflns_theta_min         2.270
_exptl_absorpt_coefficient_mu    4.687
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS.  G. M. Sheldrick, BrukerAXS, Inc.'
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       needle
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.131
_exptl_crystal_size_mid          0.019
_exptl_crystal_size_min          0.013
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.00072(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1077
_refine_ls_number_reflns         12771
_refine_ls_number_restraints     708
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.1880
_refine_ls_R_factor_gt           0.0726
_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^)+(0.1191P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1776
_refine_ls_wR_factor_ref         0.2447
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5165
_reflns_number_total             12771
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c08106_si_004.cif
_cod_data_source_block           jungsu3
_cod_database_code               4135294
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.579
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C89(H89)
3.b Secondary CH2 refined with riding coordinates:
 C74(H74A,H74B), C78(H78A,H78B), C87(H87A,H87B)
3.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4), C24(H24), C25(H25), C26(H26), C27(H27),
 C34(H34), C35(H35), C36(H36), C37(H37), C44(H44), C45(H45), C46(H46), C47(H47),
  C54(H54), C55(H55), C56(H56), C57(H57), N5(H5), N6(H6), C62(H62), C65(H65),
 C69(H69), C72(H72), C82(H82), C83(H83), C84(H84), C85(H85)
3.d Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C59(H59A,H59B,H59C), C60(H60A,
 H60B,H60C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C77(H77A,H77B,H77C),
 C79(H79A,H79B,H79C), C88(H88A,H88B,H88C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              52930
_shelx_hkl_checksum              9671
_shelx_fab_checksum              28587
_olex2_submission_special_instructions 'No special instructions were received'