Fully conjugated tetraborylethylene: selenium mediated C-C double bond formation from diborylcarbenoid.
Shibutani, Yuki; Kusumoto, Shuhei; Nozaki, Kyoko; Chemical science 15 (2024) 17912–17917; doi:10.1039/d4sc05928j

data_1572732
_publ_section_title
;
 Fully conjugated tetraborylethylene: selenium mediated C-C double bond
 formation from diborylcarbenoid.
;
_journal_issue                   43
_journal_name_full               'Chemical science'
_journal_page_first              17912
_journal_page_last               17917
_journal_paper_doi               10.1039/d4sc05928j
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C31 H32 B2 N2'
_chemical_formula_sum            'C31 H32 B2 N2'
_chemical_formula_weight         454.20
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-11
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-09-03 deposited with the CCDC.	2024-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.9465(4)
_cell_length_b                   14.8115(4)
_cell_length_c                   22.4995(7)
_cell_measurement_reflns_used    14945
_cell_measurement_temperature    93
_cell_measurement_theta_max      29.8400
_cell_measurement_theta_min      3.1350
_cell_volume                     5314.2(3)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      93
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.908
_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    -89.00  67.00   0.50   12.83    --    0.80  46.00-150.00  312
  2  \w     45.00  76.00   0.50   12.83    --    0.80   9.00 -60.00   62
  3  \w    -84.00 -58.00   0.50   12.83    --    0.80  28.00  90.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0333407000
_diffrn_orient_matrix_UB_12      0.0283812000
_diffrn_orient_matrix_UB_13      -0.0092313000
_diffrn_orient_matrix_UB_21      0.0120511000
_diffrn_orient_matrix_UB_22      0.0061675000
_diffrn_orient_matrix_UB_23      0.0300791000
_diffrn_orient_matrix_UB_31      0.0268559000
_diffrn_orient_matrix_UB_32      -0.0380772000
_diffrn_orient_matrix_UB_33      -0.0020356000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.908
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            42031
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.588
_diffrn_reflns_theta_min         2.555
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_coefficient_mu    0.065
_exptl_crystal_density_diffrn    1.135
_exptl_crystal_description       plate
_exptl_crystal_F_000             1936
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         6786
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0735P)^2^+2.3055P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1264
_refine_ls_wR_factor_ref         0.1326
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5901
_reflns_number_total             6786
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc05928j3.cif
_cod_data_source_block           b2ccb2_auto
_cod_depositor_comments
'Adding full bibliography for 1572732--1572735.cif.'
_cod_original_cell_volume        5314.2(2)
_cod_database_code               1572732
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         C60H60B4N4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C4(H4), C15(H15), C13(H13), C27(H27), C31(H31), C21(H21), C30(H30),
 C28(H28), C29(H29), C25(H25), C22(H22), C23(H23), C24(H24)
2.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              46289
_shelx_hkl_checksum              70212
_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 1.691
_oxdiff_exptl_absorpt_empirical_full_min 0.745