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_7063706
_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         'C44 H58 B N5 O2'
_chemical_formula_sum            'C44 H58 B N5 O2'
_chemical_formula_weight         699.76
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-08-05
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.6239(2)
_cell_length_b                   17.4050(3)
_cell_length_c                   29.4625(4)
_cell_measurement_reflns_used    14064
_cell_measurement_temperature    99.99(13)
_cell_measurement_theta_max      74.7890
_cell_measurement_theta_min      4.0660
_cell_volume                     8011.9(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
'olex2.solve 1.5-ac5-021 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.974
_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    -66.00 -29.00   0.50    3.47    --  -38.50 109.00 -63.00   74
  2  \w     42.00  68.00   0.50    3.47    --   49.06-109.00-159.00   52
  3  \w     60.00 105.00   0.50   14.58    --  102.00-109.00-159.00   90
  4  \w    117.00 157.00   0.50   14.58    --  102.00 109.00 -63.00   80
  5  \w    -34.00  23.00   0.50    3.47    --  -38.50  38.00-150.00  114
  6  \w   -105.00 -35.00   0.50    3.47    --  -38.50 -38.00  30.00  140
  7  \w    -99.00 -28.00   0.50    3.47    --  -38.50 -57.00 120.00  142
  8  \w     40.00  65.00   0.50    3.47    --   49.06  57.00 -60.00   50
  9  \w     89.00 115.00   0.50   14.58    --  102.00  61.00-150.00   52
 10  \w     99.00 167.00   0.50   14.58    --  102.00  45.00 120.00  136
 11  \w    119.00 163.00   0.50   14.58    --  102.00  61.00-150.00   88
 12  \w     40.00 111.00   0.50   14.58    --  102.00-125.00 120.00  142
 13  \w    114.00 162.00   0.50   14.58    --  102.00 125.00 -30.00   96
 14  \w    115.00 157.00   0.50   14.58    --  102.00  77.00-180.00   84
 15  \w     56.00  83.00   0.50   14.58    --  102.00 -30.00-150.00   54
 16  \w     39.00  64.00   0.50   14.58    --  102.00 -45.00 -30.00   50
;
_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      0.0203841000
_diffrn_orient_matrix_UB_12      0.0806874000
_diffrn_orient_matrix_UB_13      -0.0186024000
_diffrn_orient_matrix_UB_21      0.0143458000
_diffrn_orient_matrix_UB_22      -0.0343204000
_diffrn_orient_matrix_UB_23      -0.0475843000
_diffrn_orient_matrix_UB_31      -0.0953993000
_diffrn_orient_matrix_UB_32      0.0120182000
_diffrn_orient_matrix_UB_33      -0.0111572000
_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  0.0416
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            35328
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.373
_diffrn_reflns_theta_min         4.088
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.550
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71655
_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    1.160
_exptl_crystal_description       block
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.000087(19)
_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   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         8077
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0495
_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^)+(0.0510P)^2^+4.2688P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1183
_refine_ls_wR_factor_ref         0.1243
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6771
_reflns_number_total             8077
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj00446b2.cif
_cod_data_source_block           sn-sr-mesbpin_auto
_cod_depositor_comments
'Adding full bibliography for 7063704--7063710.cif.'
_cod_database_code               7063706
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N B O'
_shelx_estimated_absorpt_t_max   0.912
_shelx_estimated_absorpt_t_min   0.898
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 N4(H4), N5(H5), C48(H48), C38(H38), C46(H46), C11(H11), C36(H36), C9(H9),
 C20(H20), C18(H18)
1.b Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C23(H23A,H23B,H23C), C41(H41A,H41B,
 H41C), C14(H14A,H14B,H14C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C13(H13A,
 H13B,H13C), C42(H42A,H42B,H42C), C22(H22A,H22B,H22C), C40(H40A,H40B,H40C),
 C15(H15A,H15B,H15C), C52(H52A,H52B,H52C), C24(H24A,H24B,H24C), C32(H32A,H32B,
 H32C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              44330
_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 1.536
_oxdiff_exptl_absorpt_empirical_full_min 0.570