Novel aza-BODIPY-carborane conjugates: synthesis and characterization
Zaitsev, Andrei V.; Smol’yakov, Alexander F.; Kononova, Elena G.; Ol'shevskaya, Valentina A.; New Journal of Chemistry 49 (2025) 9035–9042; doi:10.1039/D5NJ01231G

data_7063798
_publ_section_title
;
 Novel aza-BODIPY-carborane conjugates: synthesis and characterization
;
_journal_issue                   21
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              9035
_journal_page_last               9042
_journal_paper_doi               10.1039/D5NJ01231G
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         'C H2 Cl2, C36 H42 B21 F2 N3 S2'
_chemical_formula_sum            'C37 H44 B21 Cl2 F2 N3 S2'
_chemical_formula_weight         930.78
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-02-17
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-02-17 deposited with the CCDC.	2025-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.5190(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.2330(6)
_cell_length_b                   10.6778(3)
_cell_length_c                   22.9940(7)
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    120
_cell_measurement_theta_max      33.111
_cell_measurement_theta_min      2.30
_cell_volume                     4952.3(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0511
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            69850
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.396
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.256
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9471
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0790 before and 0.0642 after correction.
The Ratio of minimum to maximum transmission is 0.9471.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       prism
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.330
_refine_diff_density_min         -1.357
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         9720
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0635
_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^)+(0.0997P)^2^+8.4599P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1810
_refine_ls_wR_factor_ref         0.1892
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7842
_reflns_number_total             9720
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj01231g2.cif
_cod_data_source_block           a_CCDC3
_cod_depositor_comments
'Adding full bibliography for 7063795--7063798.cif.'
_cod_database_code               7063798
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.932
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
 C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30),
  C32(H32), C33(H33), C34(H34), C35(H35), C36(H36)
2.c Boron cage BH refined with riding coordinates:
 C48(H48), C50(H50), C60(H60), C62(H62), B41(H41), B42(H42), B43(H43),
 B44(H44), B45(H45), B46(H46), B47(H47), B49(H49), B51(H51), B54(H54), B55(H55),
  B56(H56), B57(H57), B58(H58), B59(H59), B61(H61), B63(H63), B64(H64)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              87192
_shelx_fab_checksum              44521
_olex2_submission_special_instructions 'No special instructions were received'