Exploring tetra-coordinate bis-guanidinate-supported boron complexes: synthesis, characterization, and photophysical properties
Rajput, Sagrika; M. T., Nithya; Dhala, Sasmita; Venkatasubbaiah, Krishnan; Nembenna, Sharanappa; New Journal of Chemistry 49 (2025) 6731–6740; doi:10.1039/D5NJ00446B

data_7063705
_publ_section_title
;
 Exploring tetra-coordinate bis-guanidinate-supported boron complexes:
 synthesis, characterization, and photophysical properties
;
_journal_issue                   16
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              6731
_journal_page_last               6740
_journal_paper_doi               10.1039/D5NJ00446B
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         'C40 H50 B N5 O2'
_chemical_formula_sum            'C40 H50 B N5 O2'
_chemical_formula_weight         643.66
_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
_audit_creation_date             2025-02-24
_audit_creation_method
;
Olex2 1.5-ac5-021
(compiled 2022.02.15 svn.rf212a0ae for Rigaku Oxford Diffraction, GUI svn.r6439)
;
_audit_update_record
;
2025-03-05 deposited with the CCDC.	2025-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                81.404(2)
_cell_angle_beta                 74.068(2)
_cell_angle_gamma                78.624(2)
_cell_formula_units_Z            2
_cell_length_a                   10.9789(4)
_cell_length_b                   11.8113(2)
_cell_length_c                   17.3241(3)
_cell_measurement_reflns_used    30488
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      79.4520
_cell_measurement_theta_min      3.8930
_cell_volume                     2106.92(10)
_computing_cell_refinement       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-021 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-021 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution
'olex2.solve 1.5-ac5-021 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.975
_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    -97.00 -13.00   0.50    0.40    --  -38.50 139.00  -4.00  168
  2  \w    -91.00  -9.00   0.50    0.40    --  -38.50 130.00-179.00  164
  3  \w     31.00 102.00   0.50    0.40    --   48.81-130.00 109.00  142
  4  \w     35.00 108.00   0.50    0.40    --   48.81-139.00 -65.00  146
  5  \w     95.00 174.00   0.50    1.57    --  111.00 130.00-179.00  158
  6  \w     90.00 174.00   0.50    1.57    --  111.00 139.00  -4.00  168
  7  \w     48.00 116.00   0.50    1.57    --  111.00-130.00 109.00  136
  8  \w   -105.00 -35.00   0.50    0.40    --  -38.50 -38.00   0.00  140
  9  \w   -101.00 -27.00   0.50    0.40    --  -38.50 -57.00 -60.00  148
 10  \w   -101.00 -23.00   0.50    0.40    --  -38.50 -64.00 158.71  156
 11  \w   -101.00 -27.00   0.50    0.40    --  -38.50 -57.00  60.00  148
 12  \w     37.00 112.00   0.50    0.40    --   48.81  57.00 -60.00  150
 13  \w     37.00 112.00   0.50    0.40    --   48.81  57.00-150.00  150
 14  \w     47.00 117.00   0.50    1.57    --  111.00 -50.00   0.00  140
 15  \w    108.00 177.00   0.50    1.57    --  111.00  38.00-120.00  138
 16  \w     42.00 106.00   0.50    1.57    --  111.00 -91.00 -90.00  128
 17  \w     42.00 115.00   0.50    1.57    --  111.00 -25.00 -30.00  146
 18  \w    105.00 175.00   0.50    1.57    --  111.00  50.00 -30.00  140
 19  \w     45.00 114.00   0.50    1.57    --  111.00 -38.00  60.00  138
 20  \w     42.00 115.00   0.50    1.57    --  111.00 -25.00-180.00  146
 21  \w     46.00 109.00   0.50    1.57    --  111.00-111.00   0.00  126
 22  \w     47.00 134.00   0.50    1.57    --  111.00 -77.00 -90.00  174
 23  \w    108.00 177.00   0.50    1.57    --  111.00  38.00   0.00  138
 24  \w     46.00 109.00   0.50    1.57    --  111.00-111.00 150.00  126
 25  \w    105.00 175.00   0.50    1.57    --  111.00  50.00-180.00  140
 26  \w    107.00 178.00   0.50    1.57    --  111.00  25.00 -60.00  142
 27  \w     46.00 109.00   0.50    1.57    --  111.00-111.00  30.00  126
 28  \w     46.00 109.00   0.50    1.57    --  111.00-111.00  60.00  126
 29  \w     47.00 117.00   0.50    1.57    --  111.00 -50.00 150.00  140
 30  \w     48.00 125.00   0.50    1.57    --  111.00 -63.00  90.00  154
 31  \w     45.00 114.00   0.50    1.57    --  111.00 -38.00 -90.00  138
 32  \w     48.00 125.00   0.50    1.57    --  111.00 -63.00   0.00  154
 33  \w     46.00 109.00   0.50    1.57    --  111.00-111.00-120.00  126
 34  \w     46.00 109.00   0.50    1.57    --  111.00-111.00-180.00  126
 35  \w     47.00 117.00   0.50    1.57    --  111.00 -50.00-120.00  140
 36  \w     42.00 121.00   0.50    1.57    --  111.00 -12.00  90.00  158
 37  \w     46.00 109.00   0.50    1.57    --  111.00-111.00 -60.00  126
 38  \w     61.00 146.00   0.50    1.57    --  111.00 178.00  30.00  170
 39  \w    107.00 178.00   0.50    1.57    --  111.00  25.00 120.00  142
 40  \w     46.00 109.00   0.50    1.57    --  111.00-111.00 120.00  126
 41  \w     79.00 106.00   0.50    1.57    --  111.00-111.00-150.00   54
 42  \w     84.00 122.00   0.50    1.57    --  111.00-139.00 -65.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0642
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            36860
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.472
_diffrn_reflns_theta_min         3.837
_exptl_absorpt_coefficient_mu    0.488
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46065
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.89a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.015
_exptl_crystal_description       block
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       0.0037(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         9005
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0601
_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^)+(0.0836P)^2^+1.2014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1587
_refine_ls_wR_factor_ref         0.1610
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8560
_reflns_number_total             9005
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj00446b2.cif
_cod_data_source_block           sn-sr-c6-xbpin_auto
_cod_depositor_comments
'Adding full bibliography for 7063704--7063710.cif.'
_cod_database_code               7063705
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.909
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 N5(H5), N4(H4), C00J(H00J), C00O(H00O), C00R(H00R), C00S(H00S), C00Y(H00Y),
 C00Z(H00Z), C010(H010), C011(H011), C012(H012), C013(H013), C017(H017),
 C018(H018)
1.b Idealised Me refined as rotating group:
 C00N(H00A,H00B,H00C), C00T(H00D,H00E,H00F), C00U(H00G,H00H,H00I), C00V(H00K,
 H00L,H00M), C00W(H00N,H00P,H00Q), C00X(H00T,H00U,H00V), C014(H01A,H01B,H01C),
 C015(H01D,H01E,H01F), C016(H01G,H01H,H01I), C019(H01J,H01K,H01L), C01A(H01M,
 H01N,H01O), C01B(H01P,H01Q,H01R)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 105 electrons were 
found in a volume of 510\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[C7H8] per Formula Unit 
which account for 100 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              2082
_shelx_fab_checksum              79138
_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
;