Tetraphenylethene-2-Pyrone Conjugate: Aggregation-Induced Emission Study and Explosives Sensor.
Mahendran, Vaithiyanathan; Pasumpon, Kamaraj; Thimmarayaperumal, Solaimalai; Thilagar, Pakkirisamy; Shanmugam, Sivakumar; The Journal of organic chemistry 81 (2016) 3597–3602; doi:10.1021/acs.joc.6b00267

data_4036675
_publ_section_title
;
 Tetraphenylethene-2-Pyrone Conjugate: Aggregation-Induced Emission Study
 and Explosives Sensor.
;
_journal_issue                   9
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              3597
_journal_page_last               3602
_journal_paper_doi               10.1021/acs.joc.6b00267
_journal_volume                  81
_journal_year                    2016
_chemical_formula_moiety         'C33 H23 N O2 S'
_chemical_formula_sum            'C33 H23 N O2 S'
_chemical_formula_weight         497.58
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-10-31
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_cell_angle_alpha                83.904(12)
_cell_angle_beta                 80.980(12)
_cell_angle_gamma                88.585(14)
_cell_formula_units_Z            4
_cell_length_a                   9.225(2)
_cell_length_b                   11.400(3)
_cell_length_c                   27.925(6)
_cell_measurement_reflns_used    6220
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.68
_cell_measurement_theta_min      2.71
_cell_volume                     2883.9(12)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0727
_diffrn_reflns_av_unetI/netI     0.1284
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            35813
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.72
_diffrn_reflns_theta_min         1.48
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.140
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_platon_squeeze_details
;
;
_refine_diff_density_max         0.809
_refine_diff_density_min         -0.953
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     669
_refine_ls_number_reflns         15792
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1661
_refine_ls_R_factor_gt           0.1026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1749P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2656
_refine_ls_wR_factor_ref         0.3067
_reflns_number_gt                8253
_reflns_number_total             15792
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo6b00267_si_002.cif
_cod_data_source_block           m_0m-sr
_cod_depositor_comments
;

2020-04-07
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        2884.0(12)
_cod_original_formula_moiety     '2(C33 H23 N O2 S)'
_cod_original_formula_sum        'C66 H46 N2 O4 S2'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     995.17
_cod_database_code               4036675
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7), C12(H12), C13(H13), C14(H14), C18(H18), C19(H19),
 C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C29(H29),
  C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36),
 C41(H41), C42(H42), C45(H45), C51(H51), C52(H52), C54(H54), C55(H55), C56(H56),
  C57(H57), C58(H58), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64),
 C65(H65), C66(H66)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C47(H47A,H47B,H47C)
;