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_7063707
_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         'C48 H58 B N5 O2'
_chemical_formula_sum            'C48 H58 B N5 O2'
_chemical_formula_weight         747.80
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-08-06
_audit_creation_method
;
Olex2 1.5-ac5-021
(compiled 2022.02.15 svn.rf212a0ae for Rigaku Oxford Diffraction, GUI svn.r6439)
;
_audit_update_record
;
2024-10-03 deposited with the CCDC.	2025-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.435(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4681(3)
_cell_length_b                   16.5069(4)
_cell_length_c                   17.7735(4)
_cell_measurement_reflns_used    20851
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      77.8110
_cell_measurement_theta_min      3.6040
_cell_volume                     4128.57(16)
_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      100.00(11)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 1.000
_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   -104.00 -35.00   0.50    2.79    --  -38.50 -39.00-129.00  138
  2  \w    -42.00  28.00   0.50    2.79    --  -38.50  39.00  24.00  140
  3  \w    -17.00  53.00   0.50    2.79    --   49.06 -39.00-129.00  140
  4  \w     46.00 115.00   0.50    2.79    --   49.06  39.00  24.00  138
  5  \w     42.00 111.00   0.50    9.81    --  107.46 -39.00-129.00  138
  6  \w    104.00 173.00   0.50    9.81    --  107.46  39.00  24.00  138
  7  \w   -108.00 -33.00   0.50    2.79    --  -38.50 -19.00 -90.00  150
  8  \w    -14.00  61.00   0.50    2.79    --   49.06 -57.00  60.00  150
  9  \w     28.00  98.00   0.50    2.79    --   49.06-125.00 120.00  140
 10  \w     43.00 112.00   0.50    9.81    --  107.46 -45.00  30.00  138
 11  \w     45.00 113.00   0.50    9.81    --  107.46-125.00   0.00  136
 12  \w     39.00 107.00   0.50    9.81    --  107.46 -94.00  30.00  136
 13  \w    103.00 172.00   0.50    9.81    --  107.46  77.00 120.00  138
 14  \w     45.00 121.00   0.50    9.81    --  107.46 -61.00-180.00  152
 15  \w     39.00 107.00   0.50    9.81    --  107.46 -94.00 150.00  136
 16  \w     58.00 113.00   0.50    9.81    --  107.46-125.00  90.00  110
 17  \w    105.00 175.00   0.50    9.81    --  107.46  15.00  90.00  140
 18  \w    117.00 157.00   0.50    9.81    --  107.46  77.00 -60.00   80
 19  \w    104.00 141.00   0.50    9.81    --  107.46  77.00  90.00   74
 20  \w     44.00  71.00   0.50    9.81    --  107.46 -77.00  30.00   54
 21  \w     83.00 111.00   0.50    9.81    --  107.46 -77.00  30.00   56
 22  \w     53.00  89.00   0.50    9.81    --  107.46 -61.00   0.00   72
;
_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  0.0393
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33423
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.228
_diffrn_reflns_theta_min         3.560
_exptl_absorpt_coefficient_mu    0.568
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64659
_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    1.203
_exptl_crystal_description       block
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         8637
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0521
_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^)+(0.0870P)^2^+1.1910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1385
_refine_ls_wR_factor_ref         0.1448
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7407
_reflns_number_total             8637
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj00446b2.cif
_cod_data_source_block           sr-c3-211_auto
_cod_depositor_comments
'Adding full bibliography for 7063704--7063710.cif.'
_cod_database_code               7063707
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.910
_shelx_estimated_absorpt_t_min   0.895
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C31(H31a,H31b), C21(H21a,H21b), C33(H33a,H33b), C23(H23a,H23b), C55(H55a,
 H55b), C53(H53a,H53b), C42(H42a,H42b), C44(H44a,H44b)
2.b Aromatic/amide H refined with riding coordinates:
 N5(H5), N4(H4), C51(H51), C4(H4a), C49(H49), C7(H7), C50(H50), C28(H28),
 C29(H29), C40(H40), C27(H27), C6(H6), C19(H19), C18(H18), C38(H38), C17(H17),
 C5(H5a), C39(H39)
2.c Idealised Me refined as rotating group:
 C56(H56a,H56b,H56c), C22(H22a,H22b,H22c), C32(H32a,H32b,H32c), C24(H24a,H24b,
 H24c), C45(H45a,H45b,H45c), C34(H34a,H34b,H34c), C54(H54a,H54b,H54c), C43(H43a,
 H43b,H43c)
;
_shelx_res_checksum              97081
_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
;