Tetra-coordinated organoboron complexes with triaminoguanidine-salicylidene based ligands: aggregation induced enhanced emission and mechanoresponsive features.
Tharmalingam, Balamurugan; Kishore Kumar, Rajendran; Anitha, Ottoor; Kaminsky, Werner; Malecki, Jan Grzegorz; Murugesapandian, Balasubramanian; Dalton transactions (Cambridge, England : 2003) 54 (2025) 3897–3910; doi:10.1039/d4dt03217a

data_7717894
_publ_section_title
;
 Tetra-coordinated organoboron complexes with
 triaminoguanidine-salicylidene based ligands: aggregation induced
 enhanced emission and mechanoresponsive features.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3897
_journal_page_last               3910
_journal_paper_doi               10.1039/d4dt03217a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C31 H29 B N6 O6, 2(C2 H3 N), H2 O'
_chemical_formula_sum            'C35 H37 B N8 O7'
_chemical_formula_weight         692.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2020-01-22
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2024-07-15 deposited with the CCDC.	2025-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.529(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1862(5)
_cell_length_b                   28.1636(12)
_cell_length_c                   10.6937(5)
_cell_measurement_reflns_used    5228
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.7500
_cell_measurement_theta_min      3.7540
_cell_volume                     3499.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4015
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.870
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -22.00  29.00   1.00   30.99    --   10.22  77.00  30.00   51
  2  \w    -34.00  62.00   1.00   30.99    --  -11.23  38.00-180.00   96
  3  \w    -45.00  16.00   1.00   30.99    --  -11.23  19.00 150.00   61
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0287970000
_diffrn_orient_matrix_UB_12      0.0008524000
_diffrn_orient_matrix_UB_13      -0.0485537000
_diffrn_orient_matrix_UB_21      0.0060497000
_diffrn_orient_matrix_UB_22      0.0249530000
_diffrn_orient_matrix_UB_23      0.0081447000
_diffrn_orient_matrix_UB_31      0.0534860000
_diffrn_orient_matrix_UB_32      -0.0032921000
_diffrn_orient_matrix_UB_33      0.0491344000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.870
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            19478
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.870
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.382
_diffrn_reflns_theta_min         3.357
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70105
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       prism
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.216
_refine_diff_density_min         -0.194
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         8402
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1089
_refine_ls_R_factor_gt           0.0596
_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^)+(0.0499P)^2^+1.2305P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1238
_refine_ls_wR_factor_ref         0.1445
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5094
_reflns_number_total             8402
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03217a2.cif
_cod_data_source_block           tgaop
_cod_depositor_comments
'Adding full bibliography for 7717892--7717896.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7717894
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C35 H36 N8 O7 B1'
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Restrained distances
 H7B-O7
 0.87 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C5(H5B), C6(H6), C7(H7), C10(H10), C14(H14), C15(H15), C16(H16),
 C18(H18), C22(H22), C23(H23), C24(H24), C27(H27), C28(H28), C29(H29), C30(H30),
  C31(H31)
3.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C33(H33A,H33B,
 H33C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              77320
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.240
_oxdiff_exptl_absorpt_empirical_full_min 0.786