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_7063710
_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         'C54 H62 B N5 O2'
_chemical_formula_sum            'C54 H62 B N5 O2'
_chemical_formula_weight         823.89
_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
_atom_sites_solution_primary     dual
_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                104.236(2)
_cell_angle_beta                 109.150(2)
_cell_angle_gamma                95.3780(18)
_cell_formula_units_Z            4
_cell_length_a                   14.8209(3)
_cell_length_b                   16.0372(4)
_cell_length_c                   20.9525(5)
_cell_measurement_reflns_used    26700
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      75.1700
_cell_measurement_theta_min      3.8990
_cell_volume                     4476.6(2)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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   -103.00 -17.00   0.50    1.00    --  -38.50 148.00 100.00  172
  2  \w    -86.00  -5.00   0.50    1.00    --  -38.50 124.00 -63.00  162
  3  \w     39.00 114.00   0.50    1.00    --   48.56-148.00  53.00  150
  4  \w     27.00  97.00   0.50    1.00    --   48.56-124.00-142.00  140
  5  \w     39.00 129.00   0.50    4.05    --  102.00-148.00  53.00  180
  6  \w     39.00 112.00   0.50    4.05    --  102.00-124.00-142.00  146
  7  \w     84.00 165.00   0.50    4.05    --  102.00 148.00 100.00  162
  8  \w     98.00 165.00   0.50    4.05    --  102.00 124.00 -63.00  134
  9  \w   -102.00 -21.00   0.50    1.00    --  -38.50 -70.00-102.40  162
 10  \w    -44.00  31.00   0.50    1.00    --  -38.50  19.00-120.00  150
 11  \w   -101.00 -25.00   0.50    1.00    --  -38.50 -62.00  89.82  152
 12  \w     45.00 115.00   0.50    1.00    --   48.56  38.00-150.00  140
 13  \w     37.00 112.00   0.50    1.00    --   48.56  57.00-120.00  150
 14  \w     45.00 115.00   0.50    1.00    --   48.56  38.00 -60.00  140
 15  \w     97.00 165.00   0.50    4.05    --  102.00 125.00-120.00  136
 16  \w    139.00 166.00   0.50    4.05    --  102.00  45.00-180.00   54
 17  \w     45.00 112.00   0.50    4.05    --  102.00 -61.00   0.00  134
 18  \w     34.00 106.00   0.50    4.05    --  102.00 -94.00-150.00  144
 19  \w     42.00 111.00   0.50    4.05    --  102.00-125.00 120.00  138
 20  \w    116.00 171.00   0.50    4.05    --  102.00  15.00   0.00  110
 21  \w     46.00  95.00   0.50    4.05    --  102.00 -15.00   0.00   98
 22  \w    100.00 166.00   0.50    4.05    --  102.00  41.00 -37.55  132
 23  \w     41.00 112.00   0.50    4.05    --  102.00 -61.00 -90.00  142
 24  \w    111.00 136.00   0.50    4.05    --  102.00  45.00-180.00   50
 25  \w     40.00 105.00   0.50    4.05    --  102.00-125.00 -30.00  130
 26  \w     34.00  69.00   0.50    4.05    --  102.00 -94.00   0.00   70
 27  \w     78.00 105.00   0.50    4.05    --  102.00 -94.00   0.00   54
 28  \w     43.00  85.00   0.50    4.05    --  102.00 -45.00-180.00   84
 29  \w    113.00 148.00   0.50    4.05    --  102.00  45.00  30.00   70
 30  \w    103.00 170.00   0.50    4.05    --  102.00  30.00 -90.00  134
 31  \w     59.00 106.00   0.50    4.05    --  102.00 -94.00  90.00   94
 32  \w     39.00  88.00   0.50    4.05    --  102.00 -45.00 -30.00   98
 33  \w     95.00 122.00   0.50    4.05    --  102.00 -88.00 106.06   54
 34  \w     74.00 106.00   0.50    4.05    --  102.00 -94.00 -90.00   64
 35  \w     36.00 103.00   0.50    4.05    --  102.00 -94.00-180.00  134
 36  \w     34.00  84.00   0.50    4.05    --  102.00 -94.00 150.00  100
 37  \w     47.00  97.00   0.50    4.05    --  102.00 -61.00 -60.00  100
 38  \w     43.00 113.00   0.50    4.05    --  102.00 -61.00-180.00  140
 39  \w     99.00 170.00   0.50    4.05    --  102.00  30.00 -60.00  142
 40  \w     94.00 170.00   0.50    4.05    --  102.00  15.00-120.00  152
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0883280000
_diffrn_orient_matrix_UB_12      -0.0727771000
_diffrn_orient_matrix_UB_13      -0.0193224000
_diffrn_orient_matrix_UB_21      -0.0264703000
_diffrn_orient_matrix_UB_22      -0.0063160000
_diffrn_orient_matrix_UB_23      -0.0787656000
_diffrn_orient_matrix_UB_31      0.0637243000
_diffrn_orient_matrix_UB_32      -0.0696791000
_diffrn_orient_matrix_UB_33      -0.0073875000
_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  0.0907
_diffrn_reflns_av_unetI/netI     0.0657
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            63879
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         3.897
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52632
_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    1.222
_exptl_crystal_description       block
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1133
_refine_ls_number_reflns         16306
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.1137
_refine_ls_R_factor_gt           0.0913
_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^)+(0.1177P)^2^+5.8960P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2314
_refine_ls_wR_factor_ref         0.2486
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12406
_reflns_number_total             16306
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj00446b2.cif
_cod_data_source_block           sn-sr-c5-158_auto
_cod_depositor_comments
'Adding full bibliography for 7063704--7063710.cif.'
_cod_original_cell_volume        4476.57(19)
_cod_database_code               7063710
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N B O'
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.894
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B), C101(H10A,H10B), C99(H99A,H99B), C110(H11A,H11B), C89(H89A,
 H89B), C50(H50A,H50B), C37(H37A,H37B), C91(H91A,H91B), C29(H29A,H29B),
 C59(H59A,H59B), C112(H11C,H11D), C123(H12A,H12B), C48(H48A,H48B), C61(H61A,
 H61B), C27(H27A,H27B), C121(H12C,H12D)
1.b Aromatic/amide H refined with riding coordinates:
 N103(H103), N114(H114), N4(H4), N5(H5), C46(H46), C4(H4A), C7(H7), C35(H35),
 C119(H119), C97(H97), C69(H69), C44(H44), C33(H33), C75(H75), C68(H68),
 C74(H74), C95(H95), C108(H108), C72(H72), C10(H10), C45(H45), C6(H6), C67(H67),
  C25(H25), C5(H5A), C57(H57), C66(H66), C12(H12), C11(H11), C96(H96), C87(H87),
  C85(H85), C34(H34), C73(H73), C117(H117), C118(H118), C55(H55), C13(H13),
 C23(H23), C24(H24), C106(H106), C86(H86), C107(H107), C56(H56)
1.c Idealised Me refined as rotating group:
 C92(H92A,H92B,H92C), C90(H90A,H90B,H90C), C40(H40A,H40B,H40C), C111(H11E,H11F,
 H11G), C30(H30A,H30B,H30C), C102(H10C,H10D,H10E), C100(H10F,H10G,H10H),
 C38(H38A,H38B,H38C), C62(H62A,H62B,H62C), C60(H60A,H60B,H60C), C122(H12E,H12F,
 H12G), C124(H12H,H12I,H12J), C51(H51A,H51B,H51C), C49(H49A,H49B,H49C),
 C113(H11H,H11I,H11J), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              49668
_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 2.098
_oxdiff_exptl_absorpt_empirical_full_min 0.392