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_7063704
_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 H66 B N5 O2'
_chemical_formula_sum            'C48 H66 B N5 O2'
_chemical_formula_weight         755.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-08-22
_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                 90.964(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5760(10)
_cell_length_b                   13.9580(9)
_cell_length_c                   18.4436(10)
_cell_measurement_reflns_used    8467
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.2940
_cell_measurement_theta_min      3.6600
_cell_volume                     4266.7(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.52a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.52a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.52a (Rigaku OD, 2022)'
_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      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -23.00  32.00   0.50   59.79    --    3.51 -88.00-155.00  110
  2  \w    -27.00  12.00   0.50   59.79    --   -4.14 -88.00-155.00   78
  3  \w     -9.00  17.00   0.50   59.79    --   -4.14  77.00 -30.00   52
  4  \w    -12.00  31.00   0.50   59.79    --   -4.14 -99.00  60.00   86
  5  \w     35.00  60.00   0.50   59.79    --   -4.14  37.00  60.00   50
  6  \w    -27.00  15.00   0.50   59.79    --   -4.14  77.00  90.00   84
  7  \w     -7.00  54.00   0.50   59.79    --   -4.14  37.00   0.00  122
  8  \w    -16.00  15.00   0.50   59.79    --   -4.14  77.00  60.00   62
;
_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      0.0226897000
_diffrn_orient_matrix_UB_12      -0.0428311000
_diffrn_orient_matrix_UB_13      0.0045084000
_diffrn_orient_matrix_UB_21      0.0138749000
_diffrn_orient_matrix_UB_22      0.0162214000
_diffrn_orient_matrix_UB_23      0.0344314000
_diffrn_orient_matrix_UB_31      -0.0334684000
_diffrn_orient_matrix_UB_32      -0.0221739000
_diffrn_orient_matrix_UB_33      0.0165236000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0972
_diffrn_reflns_av_unetI/netI     0.0731
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            36520
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         3.278
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.52a (Rigaku Oxford Diffraction, 2022)
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    1.177
_exptl_crystal_description       block
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         7777
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0480P)^2^+1.4740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1183
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5101
_reflns_number_total             7777
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj00446b2.cif
_cod_data_source_block           sn_rks_lh_bpin_auto
_cod_depositor_comments
'Adding full bibliography for 7063704--7063710.cif.'
_cod_database_code               7063704
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O S Br B'
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.986
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C44(H44A,H44B), C15(H15A,H15B), C13(H13A,H13B), C23(H23A,
 H23B), C55(H55A,H55B), C53(H53A,H53B), C42(H42A,H42B)
1.b Aromatic/amide H refined with riding coordinates:
 N4(H4), N5(H5), C11(H11), C21(H21), C19(H19), C40(H40), C10(H10), C20(H20),
 C51(H51), C9(H9), C38(H38), C39(H39), C49(H49), C50(H50)
1.c Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C32(H32A,H32B,H32C), C26(H26A,H26B,H26C), C33(H33A,H33B,
 H33C), C31(H31A,H31B,H31C), C24(H24A,H24B,H24C), C43(H43A,H43B,H43C), C54(H54A,
 H54B,H54C), C45(H45A,H45B,H45C), C14(H14A,H14B,H14C), C56(H56A,H56B,H56C),
 C16(H16A,H16B,H16C)
;
_shelx_res_checksum              43908
_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 1.933
_oxdiff_exptl_absorpt_empirical_full_min 0.467