Synthesis of dual state emissive β-carboline boron complexes
Dutta, Kartik; Agrawal, Richa; Wadawale, A. P.; Gamre, Sunita; Mula, Soumyaditya; New Journal of Chemistry 47 (2023) 11371–11375; doi:10.1039/D3NJ01607B

data_7062486
_publ_section_title
;
 Synthesis of dual state emissive \b-carboline boron complexes
;
_journal_issue                   24
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              11371
_journal_page_last               11375
_journal_paper_doi               10.1039/D3NJ01607B
_journal_volume                  47
_journal_year                    2023
_chemical_formula_sum            'C30 H22 B N3 O2'
_chemical_formula_weight         467.31
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2023-03-29 deposited with the CCDC.	2023-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.9550(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.0809(2)
_cell_length_b                   9.84330(10)
_cell_length_c                   31.2561(3)
_cell_measurement_reflns_used    44061
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      75.7220
_cell_measurement_theta_min      2.9170
_cell_volume                     4779.92(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_molecular_graphics    'ORTEP-3 for windows'
_computing_publication_material  'WinGX 2021.3'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_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    -12.00  14.00   0.50    0.50    --   48.17 -43.00  22.00   52
  2  \w    -25.00  25.00   0.50    0.50    --   48.17 -19.00  30.00  100
  3  \w     36.00 119.00   0.50    0.50    --   48.17  57.00 -30.00  166
  4  \w     97.00 177.00   0.50    2.06    --  107.75  61.00-150.00  160
  5  \w    140.00 166.00   0.50    2.06    --  107.75  77.00 -90.00   52
  6  \w    124.00 149.00   0.50    2.06    --  107.75  77.00-150.00   50
  7  \w     94.00 125.00   0.50    2.06    --  107.75  61.00-120.00   62
  8  \w     95.00 122.00   0.50    2.06    --  107.75  77.00-150.00   54
  9  \w     93.00 178.00   0.50    2.06    --  107.75  61.00 -90.00  170
 10  \w    133.00 159.00   0.50    2.06    --  107.75  45.00   0.00   52
 11  \w    153.00 178.00   0.50    2.06    --  107.75  45.00  30.00   50
 12  \w    151.00 178.00   0.50    2.06    --  107.75  61.00  90.00   54
 13  \w    139.00 171.00   0.50    2.06    --  107.75  77.00 150.00   64
 14  \w    129.00 168.00   0.50    2.06    --  107.75  61.00  60.00   78
 15  \w    107.00 177.00   0.50    2.06    --  107.75  45.00  90.00  140
 16  \w     97.00 137.00   0.50    2.06    --  107.75  43.00 173.00   80
 17  \w     96.00 122.00   0.50    2.06    --  107.75  61.00  90.00   52
 18  \w     92.00 117.00   0.50    2.06    --  107.75  61.00  60.00   50
 19  \w     87.00 156.00   0.50    2.06    --  107.75  77.00 120.00  138
 20  \w     95.00 147.00   0.50    2.06    --  107.75 125.00 150.00  104
 21  \w     96.00 134.00   0.50    2.06    --  107.75  45.00  30.00   76
 22  \w     85.00 159.00   0.50    2.06    --  107.75  77.00 -60.00  148
 23  \w     89.00 170.00   0.50    2.06    --  107.75  68.00 -39.21  162
 24  \w     93.00 162.00   0.50    2.06    --  107.75  67.00-119.31  138
 25  \w     92.00 148.00   0.50    2.06    --  107.75  74.00-111.39  112
 26  \w     96.00 162.00   0.50    2.06    --  107.75  45.00 -60.00  132
 27  \w     96.00 159.00   0.50    2.06    --  107.75 125.00   0.00  126
 28  \w     87.00 112.00   0.50    2.06    --  107.75  73.00 -70.25   50
 29  \w     84.00 147.00   0.50    2.06    --  107.75  80.00-120.72  126
 30  \w     86.00 112.00   0.50    2.06    --  107.75  77.00 -90.00   52
 31  \w     87.00 147.00   0.50    2.06    --  107.75  77.00 -30.00  120
 32  \w     89.00 132.00   0.50    2.06    --  107.75  77.00 150.00   86
 33  \w     37.00  63.00   0.50    0.50    --   48.17  43.00 173.00   52
 34  \w     36.00  68.00   0.50    2.06    --  107.75 -61.00 150.00   64
 35  \w     57.00  94.00   0.50    2.06    --  107.75 -94.00 150.00   74
 36  \w     77.00 111.00   0.50    2.06    --  107.75-125.00  90.00   68
 37  \w     80.00 106.00   0.50    2.06    --  107.75 -77.00  90.00   52
 38  \w     55.00  81.00   0.50    2.06    --  107.75-125.00 120.00   52
 39  \w     37.00  62.00   0.50    2.06    --  107.75-125.00 150.00   50
 40  \w     36.00  67.00   0.50    2.06    --  107.75-125.00  90.00   62
 41  \w     36.00  74.00   0.50    2.06    --  107.75 -77.00  90.00   76
 42  \w     44.00  71.00   0.50    2.06    --  107.75 -61.00  30.00   54
 43  \w     39.00  79.00   0.50    2.06    --  107.75 -77.00   0.00   80
 44  \w     87.00 112.00   0.50    2.06    --  107.75-125.00 -30.00   50
 45  \w     37.00  75.00   0.50    2.06    --  107.75-125.00 -30.00   76
 46  \w     40.00  95.00   0.50    2.06    --  107.75 -77.00 -90.00  110
 47  \w     41.00  70.00   0.50    2.06    --  107.75 -61.00 -90.00   58
 48  \w     37.00  86.00   0.50    2.06    --  107.75 -94.00-120.00   98
 49  \w     56.00  85.00   0.50    2.06    --  107.75 -94.00-180.00   58
 50  \w     44.00  71.00   0.50    2.06    --  107.75 -61.00-180.00   54
 51  \w     37.00  62.00   0.50    2.06    --  107.75 -77.00-120.00   50
 52  \w     36.00  78.00   0.50    2.06    --  107.75 -94.00-150.00   84
 53  \w     36.00  62.00   0.50    2.06    --  107.75 -61.00-120.00   52
 54  \w     42.00  70.00   0.50    2.06    --  107.75 -61.00 -60.00   56
 55  \w     35.00  60.00   0.50    2.06    --  107.75 -61.00 -30.00   50
 56  \w     40.00  70.00   0.50    2.06    --  107.75 -61.00  90.00   60
 57  \w     35.00 120.00   0.50    0.50    --   48.17  57.00 -90.00  170
 58  \w    -19.00  26.00   0.50    0.50    --   48.17 -19.00 -90.00   90
 59  \w    -48.00  19.00   0.50    0.50    --  -48.17  43.00 173.00  134
 60  \w   -100.00 -56.00   0.50    0.50    --  -48.17 -57.00 -90.00   88
 61  \w    -91.00 -66.00   0.50    2.06    --  -86.25 -72.00-111.44   50
 62  \w    -93.00 -65.00   0.50    2.06    --  -86.25 -77.00-120.00   56
 63  \w    -88.00 -63.00   0.50    2.06    --  -86.25 -77.00 -84.74   50
 64  \w    -90.00 -65.00   0.50    2.06    --  -86.25 -77.00 -90.00   50
 65  \w    -88.00 -63.00   0.50    2.06    --  -86.25 -77.00 -60.00   50
 66  \w    -92.00 -67.00   0.50    2.06    --  -86.25 -73.00 -74.44   50
 67  \w    -88.00 -63.00   0.50    2.06    --  -86.25 -77.00 -30.00   50
 68  \w    -99.00 -74.00   0.50    2.06    --  -86.25 -51.00 -85.08   50
 69  \w   -119.00 -67.00   0.50    0.50    --  -48.17 -43.00  22.00  104
 70  \w   -130.00 -80.00   0.50    2.06    --  -86.25 -43.00  22.00  100
 71  \w   -110.00 -84.00   0.50    0.50    --  -48.17-125.00 150.00   52
 72  \w   -120.00 -74.00   0.50    0.50    --  -48.17-125.00 120.00   92
 73  \w   -120.00 -92.00   0.50    0.50    --  -48.17-125.00  30.00   56
 74  \w   -115.00 -74.00   0.50    0.50    --  -48.17-125.00 -90.00   82
 75  \w   -148.00-123.00   0.50    2.06    --  -86.25 -77.00 -60.00   50
 76  \w   -152.00-127.00   0.50    2.06    --  -86.25 -77.00 -30.00   50
 77  \w    -48.00 -17.00   0.50    2.06    --  -86.25  45.00 -30.00   62
 78  \w    -44.00 -19.00   0.50    2.06    --  -86.25  43.00 173.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0976269000
_diffrn_orient_matrix_UB_12      -0.0047002000
_diffrn_orient_matrix_UB_13      -0.0353492000
_diffrn_orient_matrix_UB_21      0.0221390000
_diffrn_orient_matrix_UB_22      0.0455725000
_diffrn_orient_matrix_UB_23      -0.0626544000
_diffrn_orient_matrix_UB_31      0.0216974000
_diffrn_orient_matrix_UB_32      -0.0674847000
_diffrn_orient_matrix_UB_33      -0.0399879000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0831
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            60396
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.180
_diffrn_reflns_theta_min         2.927
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.649
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32423
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.57a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       plate
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.248
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         5027
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0645
_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^)+(0.1557P)^2^+2.8001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2004
_refine_ls_wR_factor_ref         0.2299
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4323
_reflns_number_total             5027
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj01607b2.cif
_cod_data_source_block           kd-sm-04d-4
_cod_depositor_comments          'Adding full bibliography for 7062486.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7062486
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.944
_shelx_estimated_absorpt_t_max   0.994
_oxdiff_exptl_absorpt_empirical_full_min 0.517
_oxdiff_exptl_absorpt_empirical_full_max 4.496
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_oxdiff_digest_frames
;
01235f2a352a326b0d01f9d4d4b59d5d8b000314f63
;
_diffrn_oxdiff_digest_hkl
;
012a951c7440592155a81bcd2552f453f23c60
;
_shelx_res_checksum              57645