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_7063708
_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         '3(C44 H44 B N5 O2), 2(C4 H8 O), 2(C4 H6 O)'
_chemical_formula_sum            'C148 H160 B3 N15 O10'
_chemical_formula_weight         2341.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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                90
_cell_angle_beta                 115.055(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.7642(6)
_cell_length_b                   17.1299(3)
_cell_length_c                   21.1867(6)
_cell_measurement_reflns_used    16555
_cell_measurement_temperature    99.99(11)
_cell_measurement_theta_max      77.0560
_cell_measurement_theta_min      3.5990
_cell_volume                     6826.8(3)
_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      99.99(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 0.976
_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    -67.00  30.00   0.50    1.20    --  -38.50  87.00 124.00  194
  2  \w     -9.00  78.00   0.50    1.20    --   48.56 -87.00   6.00  174
  3  \w     39.00 136.00   0.50    5.12    --  106.83 -87.00   6.00  194
  4  \w    102.00 175.00   0.50    5.12    --  106.83  87.00 124.00  146
  5  \w    -50.00  24.00   0.50    1.20    --  -38.50  57.00-120.00  148
  6  \w   -101.00 -27.00   0.50    1.20    --  -38.50 -57.00 -60.00  148
  7  \w    -42.00  28.00   0.50    1.20    --  -38.50  38.00  30.00  140
  8  \w     37.00 112.00   0.50    1.20    --   48.56  57.00-150.00  150
  9  \w     39.00 110.00   0.50    5.12    --  106.83 -30.00  60.00  142
 10  \w     42.00 111.00   0.50    5.12    --  106.83 -45.00-180.00  138
 11  \w    104.00 175.00   0.50    5.12    --  106.83  30.00  90.00  142
 12  \w     63.00 110.00   0.50    5.12    --  106.83 -30.00 -30.00   94
 13  \w     39.00 114.00   0.50    5.12    --  106.83 -15.00-150.00  150
 14  \w     59.00 110.00   0.50    5.12    --  106.83 -45.00   0.00  102
 15  \w    111.00 162.00   0.50    5.12    --  106.83  30.00   0.00  102
 16  \w     43.00 111.00   0.50    5.12    --  106.83 -45.00 -60.00  136
 17  \w     43.00 111.00   0.50    5.12    --  106.83 -45.00 120.00  136
 18  \w     39.00  99.00   0.50    5.12    --  106.83 -94.00 -30.00  120
 19  \w    107.00 175.00   0.50    5.12    --  106.83  15.00  60.00  136
;
_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  0.0413
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            27824
_diffrn_reflns_point_group_measured_fraction_full 0.806
_diffrn_reflns_point_group_measured_fraction_max 0.771
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.678
_diffrn_reflns_theta_min         3.490
_exptl_absorpt_coefficient_mu    0.562
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63246
_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    1.139
_exptl_crystal_description       block
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Flack x determined using 3151 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.32(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     815
_refine_ls_number_reflns         11228
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0664
_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^)+(0.1215P)^2^+5.1446P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1843
_refine_ls_wR_factor_ref         0.1921
_reflns_Friedel_coverage         0.528
_reflns_Friedel_fraction_full    0.598
_reflns_Friedel_fraction_max     0.552
_reflns_number_gt                10232
_reflns_number_total             11228
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj00446b2.cif
_cod_data_source_block           sn-sr-c6-xbnap_auto
_cod_depositor_comments
'Adding full bibliography for 7063704--7063710.cif.'
_cod_original_cell_volume        6826.7(3)
_cod_database_code               7063708
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.911
_shelx_estimated_absorpt_t_min   0.896
_olex2_refinement_description
;
1. Others
 Fixed Sof: H86A(0.5) H86B(0.5) H89A(0.5) H89B(0.5) C35(0.7) H35A(0.7)
 H35B(0.7) C17(0.3) H17A(0.3) H17B(0.3)
2.a Secondary CH2 refined with riding coordinates:
 C84(H84A,H84B), C86(H86A,H86B), C81(H81A,H81B), C82(H82A,H82B), C83(H83A,
 H83B), C88(H88A,H88B), C89(H89A,H89B), C35(H35A,H35B), C17(H17A,H17B)
2.b Aromatic/amide H refined with riding coordinates:
 N5(H5), N4(H4), N6(H6A), C49(H49), C48(H48), C63(H63), C23(H23), C47(H47),
 C21(H21), C11(H11), C4(H4A), C8(H8), C31(H31), C22(H22), C39(H39), C9(H9),
 C7(H7), C29(H29), C6(H6), C30(H30), C40(H40), C38(H38), C76(H76), C74(H74),
 C57(H57), C65(H65), C75(H75), C55(H55), C66(H66), C56(H56)
2.c Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C71(H71A,H71B,H71C), C26(H26A,H26B,H26C), C25(H25A,H25B,
 H25C), C70(H70A,H70B,H70C), C33(H33A,H33B,H33C), C78(H78A,H78B,H78C), C34(H34A,
 H34B,H34C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C51(H51A,H51B,H51C),
 C79(H79A,H79B,H79C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 168 electrons were 
found in a volume of 596\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[C4H8O] per Formula Unit 
which account for 160 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              90307
_shelx_fab_checksum              33147
_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
;