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_7058293
_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         'C6 H3 N3 O7, C42 H40 N6'
_chemical_formula_sum            'C48 H43 N9 O7'
_chemical_formula_weight         857.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-11
_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                 94.034(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.0177(17)
_cell_length_b                   25.274(5)
_cell_length_c                   46.068(10)
_cell_measurement_reflns_used    6556
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      22.205
_cell_measurement_theta_min      3.106
_cell_volume                     9312(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 1K area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_reflns_av_R_equivalents  0.2023
_diffrn_reflns_av_unetI/netI     0.1750
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            55487
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.218
_diffrn_reflns_theta_max         25.218
_diffrn_reflns_theta_min         2.903
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5722
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_description       block
_exptl_crystal_F_000             3600
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetone'
_exptl_crystal_size_max          0.159
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.101
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         8261
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.2645
_refine_ls_R_factor_gt           0.1315
_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^)+(0.0549P)^2^+88.0527P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2509
_refine_ls_wR_factor_ref         0.3036
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3446
_reflns_number_total             8261
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj00166b2.cif
_cod_data_source_block           sk233_0m
_cod_depositor_comments
'Adding full bibliography for 7058287--7058293.cif.'
_cod_database_code               7058293
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.987
_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, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C12(H12A,H12B), C14(H14A,H14B)
2.b Aromatic/amide H refined with riding coordinates:
 C46(H46), C48(H48), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23),
 C24(H24), C27(H27), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34),
  C36(H36), C38(H38), C39(H39), 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)
2.d Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_shelx_res_checksum              67504
_shelx_fab_checksum              68367
_olex2_submission_special_instructions 'No special instructions were received'