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_7063709
_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         'C52 H58 B N5 O2, C4 H6 O, C4 H8 O'
_chemical_formula_sum            'C60 H72 B N5 O4'
_chemical_formula_weight         938.03
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-03-05
_audit_creation_method
;
Olex2 1.5-ac5-021
(compiled 2022.02.15 svn.rf212a0ae for Rigaku Oxford Diffraction, GUI svn.r6439)
;
_audit_update_record
;
2025-03-05 deposited with the CCDC.	2025-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.2570(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4390(3)
_cell_length_b                   16.2615(3)
_cell_length_c                   21.0870(3)
_cell_measurement_reflns_used    46363
_cell_measurement_temperature    100.01(11)
_cell_measurement_theta_max      75.3210
_cell_measurement_theta_min      3.9340
_cell_volume                     5294.08(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      100.01(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 1.000
_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    -50.00  24.00   0.50    0.76    --  -38.50  59.00 -89.00  148
  2  \w   -101.00 -26.00   0.50    0.76    --  -38.50 -59.00 129.00  150
  3  \w     37.00 112.00   0.50    0.76    --   48.81  59.00 -89.00  150
  4  \w    -14.00  61.00   0.50    0.76    --   48.81 -59.00 129.00  150
  5  \w     90.00 165.00   0.50    2.81    --  102.00  59.00 -89.00  150
  6  \w     39.00 114.00   0.50    2.81    --  102.00 -59.00 129.00  150
  7  \w    -42.00  28.00   0.50    0.76    --  -38.50  38.00-150.00  140
  8  \w   -101.00 -27.00   0.50    0.76    --  -38.50 -57.00  30.00  148
  9  \w    -50.00  24.00   0.50    0.76    --  -38.50  57.00 -30.00  148
 10  \w     28.00  98.00   0.50    0.76    --   48.81-125.00  90.00  140
 11  \w    103.00 167.00   0.50    2.81    --  102.00  77.00 120.00  128
 12  \w     34.00 106.00   0.50    2.81    --  102.00 -94.00 -90.00  144
 13  \w     34.00 106.00   0.50    2.81    --  102.00 -94.00 -30.00  144
 14  \w     34.00 110.00   0.50    2.81    --  102.00 -15.00-180.00  152
 15  \w     34.00 106.00   0.50    2.81    --  102.00 -94.00  60.00  144
 16  \w     34.00 106.00   0.50    2.81    --  102.00 -94.00 150.00  144
 17  \w     34.00 105.00   0.50    2.81    --  102.00 -30.00 120.00  142
 18  \w     38.00 107.00   0.50    2.81    --  102.00 -45.00 -90.00  138
 19  \w     39.00 112.00   0.50    2.81    --  102.00-125.00 120.00  146
 20  \w     38.00 125.00   0.50    2.81    --  102.00 -77.00 150.00  174
 21  \w     38.00 107.00   0.50    2.81    --  102.00 -45.00  60.00  138
 22  \w    103.00 167.00   0.50    2.81    --  102.00  77.00-150.00  128
 23  \w     34.00 106.00   0.50    2.81    --  102.00 -94.00  30.00  144
 24  \w     89.00 165.00   0.50    2.81    --  102.00  61.00  30.00  152
 25  \w     98.00 167.00   0.50    2.81    --  102.00  45.00-180.00  138
 26  \w     97.00 165.00   0.50    2.81    --  102.00 125.00-120.00  136
 27  \w     38.00 125.00   0.50    2.81    --  102.00 -77.00 -90.00  174
 28  \w    103.00 167.00   0.50    2.81    --  102.00  77.00 150.00  128
 29  \w     37.00 112.00   0.50    0.76    --   48.81  57.00-150.00  150
 30  \w     37.00 112.00   0.50    0.76    --   48.81  57.00   0.00  150
 31  \w     37.00 112.00   0.50    0.76    --   48.81  57.00 -60.00  150
 32  \w     37.00 112.00   0.50    0.76    --   48.81  57.00  60.00  150
 33  \w     37.00 112.00   0.50    0.76    --   48.81  57.00 150.00  150
 34  \w     37.00 112.00   0.50    0.76    --   48.81  57.00 120.00  150
 35  \w     89.00 136.00   0.50    2.81    --  102.00  61.00 -30.00   94
;
_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  0.0716
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            81069
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.250
_diffrn_reflns_theta_min         3.541
_exptl_absorpt_coefficient_mu    0.571
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68961
_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    1.177
_exptl_crystal_description       block
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.764
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     748
_refine_ls_number_reflns         9683
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0810
_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^)+(0.1017P)^2^+7.2916P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2100
_refine_ls_wR_factor_ref         0.2143
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8772
_reflns_number_total             9683
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj00446b2.cif
_cod_data_source_block           sn-sr-c5-201_auto
_cod_depositor_comments
'Adding full bibliography for 7063704--7063710.cif.'
_cod_database_code               7063709
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.894
_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. Restrained distances
 C50-C01H \\sim C50-C54
 with sigma of 0.02
 C01G-C01H \\sim C52-C54
 with sigma of 0.04
 C49-C01G \\sim C49-C52
 with sigma of 0.04
 C49-C01D \\sim C49-C51
 with sigma of 0.02
 C50-C01K \\sim C50-C53
 with sigma of 0.04
 C01D-C01G \\sim C51-C52
 with sigma of 0.02
 C01D-C01K \\sim C51-C53
 with sigma of 0.04
 C01G-C01K \\sim C52-C53
 with sigma of 0.02
 C01H-C01K \\sim C54-C53
 with sigma of 0.02
 C61-C58 \\sim C62-C57
 with sigma of 0.04
 O3-C58 \\sim O3-C57
 with sigma of 0.04
 O3-C56 \\sim O3-C55
 with sigma of 0.02
 O3-C61 \\sim O3-C62
 with sigma of 0.02
 C56-C58 \\sim C55-C57
 with sigma of 0.02
 O3-C59 \\sim O3-C60
 with sigma of 0.04
 C56-C59 \\sim C55-C60
 with sigma of 0.04
 C61-C59 \\sim C62-C60
 with sigma of 0.02
 C59-C58 \\sim C60-C57
 with sigma of 0.02
3. Rigid bond restraints
 C17, C18, C19, C14, C15, C16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C17, C16, C18, C19, C14, C15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C17, C18, C16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C17, C16, C15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C17, C18, C19
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C60) = Uanis(C59)
5. Rigid body (RIGU) restrains
 C17, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C17, C18, C19
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C17, C16, C15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C51)=Sof(H51)=Sof(C52)=Sof(H52)=Sof(C54)=Sof(H54)=Sof(C53)=Sof(H53)=1-
 FVAR(1)
 Sof(C01D)=Sof(H01D)=Sof(C01G)=Sof(H01G)=Sof(C01H)=Sof(H01H)=Sof(C01K)=
 Sof(H01K)=FVAR(1)
 Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(C60)=Sof(H60A)=
 Sof(H60B)=Sof(C57)=Sof(H57A)=Sof(H57B)=1-FVAR(2)
 Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(C59)=Sof(H59A)=
 Sof(H59B)=Sof(C58)=Sof(H58A)=Sof(H58B)=FVAR(2)
 Fixed Sof: H32(0.5) H32A(0.5) H5A(0.5) H5B(0.5) H63A(0.5) H63B(0.5) H66A(0.5)
 H66B(0.5) C34(0.5) H34A(0.5) H34B(0.5) H34C(0.5) C67(0.5) H67A(0.5) H67B(0.5)
 C65(0.5) H65A(0.5) H65B(0.5) C33(0.5) H33A(0.5) H33B(0.5) H33C(0.5) C7(0.5)
 H7A(0.5) H7B(0.5) H7C(0.5) C6(0.5) H6A(0.5) H6B(0.5) H6C(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C12(H12A,H12B), C63(H63A,H63B), C43(H43A,H43B), C20(H20A,
 H20B), C64(H64A,H64B), C66(H66A,H66B), C41(H41A,H41B), C22(H22A,H22B),
 C67(H67A,H67B), C65(H65A,H65B), C56(H56A,H56B), C61(H61A,H61B), C59(H59A,H59B),
  C58(H58A,H58B), C55(H55A,H55B), C62(H62A,H62B), C60(H60A,H60B), C57(H57A,H57B)
7.b Aromatic/amide H refined with riding coordinates:
 N4(H4), N5(H5), C48(H48), C37(H37), C38(H38), C8(H8), C47(H47), C39(H39),
 C10(H10), C26(H26), C9(H9), C28(H28), C27(H27), C01D(H01D), C01G(H01G),
 C01H(H01H), C01K(H01K), C18(H18), C16(H16), C17(H17), C51(H51), C52(H52),
 C54(H54), C53(H53)
7.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C31(H31A,H31B,H31C), C44(H44A,H44B,H44C), C21(H21A,H21B,
 H21C), C42(H42A,H42B,H42C), C34(H34A,H34B,H34C), C23(H23A,H23B,H23C), C33(H33A,
 H33B,H33C), C7(H7A,H7B,H7C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              99165
_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
;