Aggregation induced emission enhancement (AIEE) of tripodal pyrazole derivatives for sensing of nitroaromatics and vapor phase detection of picric acid
Kandel, Shambhu; Sathish, Veerasamy; Mathivathanan, Logesh; Morozov, Alexander N.; Mebel, Alexander M.; Raptis, Raphael G.; New Journal of Chemistry 43 (2019) 7251–; doi:10.1039/C9NJ00166B

data_7058292
_publ_section_title
;
 Aggregation induced emission enhancement (AIEE) of tripodal pyrazole
 derivatives for sensing of nitroaromatics and vapor phase detection of
 picric acid
;
_journal_issue                   19
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              7251
_journal_paper_doi               10.1039/C9NJ00166B
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C42 H39 Cl3 N6'
_chemical_formula_sum            'C42 H39 Cl3 N6'
_chemical_formula_weight         734.14
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-12-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-09 deposited with the CCDC.    2019-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.9640(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1425(5)
_cell_length_b                   16.1254(8)
_cell_length_c                   23.3070(12)
_cell_measurement_reflns_used    9850
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.26
_cell_measurement_theta_min      2.81
_cell_volume                     3729.1(3)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0682
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            65441
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.433
_diffrn_reflns_theta_min         2.963
_exptl_absorpt_coefficient_mu    0.285
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7129
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0674 before and 0.0513 after correction.
The Ratio of minimum to maximum transmission is 0.9564.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_description       Block
_exptl_crystal_F_000             1536
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetone'
_exptl_crystal_size_max          0.254
_exptl_crystal_size_mid          0.217
_exptl_crystal_size_min          0.143
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         7635
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1365
_refine_ls_R_factor_gt           0.0700
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0787P)^2^+2.5726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1591
_refine_ls_wR_factor_ref         0.1893
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4231
_reflns_number_total             7635
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj00166b2.cif
_cod_data_source_block           sk066_a
_cod_depositor_comments
'Adding full bibliography for 7058287--7058293.cif.'
_cod_database_code               7058292
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.931
_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:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C12(H12A,H12B),
 C14(H14A,H14B)
2.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C18(H18), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25),
 C27(H27), C29(H29), C30(H30), C31(H31), C33(H33), C34(H34), C36(H36), C38(H38),
  C40(H40), C41(H41), C42(H42)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              88549
_shelx_fab_checksum              19055
_olex2_submission_special_instructions 'No special instructions were received'