A carbon-functionality-appended diborylacetylene available for a component of organic synthesis and OLEDs
Tsukada, Tetsuyoshi; Shoji, Yoshiaki; Takenouchi, Kumiko; Taka, Hideo; Fukushima, Takanori; Chemical Communications  (2022) –; doi:10.1039/D2CC01159J

data_7129898
_publ_section_title
;
 A carbon-functionality-appended diborylacetylene available for a
 component of organic synthesis and OLEDs
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC01159J
_journal_year                    2022
_chemical_formula_moiety         'C32 H16 B2 Co2 O8'
_chemical_formula_sum            'C32 H16 B2 Co2 O8'
_chemical_formula_weight         667.93
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-02-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-02-25 deposited with the CCDC.	2022-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                99.675(3)
_cell_angle_beta                 92.194(3)
_cell_angle_gamma                102.399(3)
_cell_formula_units_Z            2
_cell_length_a                   9.2258(4)
_cell_length_b                   12.6088(4)
_cell_length_c                   12.6939(4)
_cell_measurement_reflns_used    6860
_cell_measurement_temperature    93.15
_cell_measurement_theta_max      76.0350
_cell_measurement_theta_min      3.6010
_cell_volume                     1417.43(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      93.15
_diffrn_detector                 'Rigaku HyPix-6000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.954
_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    -65.00 -15.00   0.50    0.05    --  -46.20  71.00 175.00  100
  2  \w    -12.00  13.00   0.50    0.05    --  -46.20  71.00 175.00   50
  3  \w    -64.00 -38.00   0.50    0.20    -- -102.00  71.00 175.00   52
  4  \w   -108.00 -61.00   0.50    0.20    -- -102.00 109.00 115.69   94
  5  \w   -104.00 -50.00   0.50    0.20    -- -102.00  77.00   0.00  108
  6  \w    -61.00 -29.00   0.50    0.20    -- -102.00 110.00 -37.04   64
  7  \w    -54.00 -29.00   0.50    0.20    -- -102.00 125.00 -30.00   50
  8  \w    -69.00 -44.00   0.50    0.20    -- -102.00  61.00 -60.00   50
  9  \w   -110.00 -82.00   0.50    0.20    -- -102.00 125.00-180.00   56
 10  \w   -112.00 -59.00   0.50    0.20    -- -102.00 125.00-150.00  106
 11  \w   -108.00 -77.00   0.50    0.20    -- -102.00 110.00 -37.04   62
 12  \w   -109.00 -63.00   0.50    0.20    -- -102.00 125.00 -30.00   92
 13  \w   -173.00 -90.00   0.50    0.20    -- -102.00 -45.00 -90.00  166
 14  \w   -117.00 -29.00   0.50    0.05    --  -46.20 -71.00  44.00  176
 15  \w    -27.00  27.00   0.50    0.05    --   46.20 -19.00  60.00  108
 16  \w    -19.00  45.00   0.50    0.05    --   46.20 -71.00  44.00  128
 17  \w     22.00  58.00   0.50    0.05    --   46.20-125.00  60.00   72
 18  \w     41.00  90.00   0.50    0.20    --  104.61 -71.00  44.00   98
 19  \w     54.00  87.00   0.50    0.20    --  104.61 -94.00 120.00   66
 20  \w     55.00 105.00   0.50    0.20    --  104.61 -94.00 150.00  100
 21  \w     81.00 107.00   0.50    0.20    --  104.61-125.00  30.00   52
 22  \w     73.00 107.00   0.50    0.20    --  104.61 -77.00 -60.00   68
 23  \w     93.00 137.00   0.50    0.20    --  104.61  15.00-150.00   88
 24  \w     95.00 155.00   0.50    0.20    --  104.61  45.00-150.00  120
 25  \w     96.00 175.00   0.50    0.20    --  104.61  45.00  90.00  158
 26  \w     94.00 167.00   0.50    0.20    --  104.61  45.00 120.00  146
 27  \w     86.00 168.00   0.50    0.20    --  104.61  71.00 175.00  164
 28  \w     38.00  64.00   0.50    0.20    --  104.61 -77.00 -60.00   52
 29  \w     32.00  57.00   0.50    0.20    --  104.61 -61.00 -90.00   50
 30  \w     33.00  69.00   0.50    0.20    --  104.61 -61.00-150.00   72
 31  \w     44.00  69.00   0.50    0.20    --  104.61 -61.00-180.00   50
 32  \w     20.00  88.00   0.50    0.05    --   46.20-125.00 -90.00  136
 33  \w     33.00  62.00   0.50    0.20    --  104.61-125.00  30.00   58
 34  \w     37.00 100.00   0.50    0.20    --  104.61 -94.00  60.00  126
 35  \w     32.00  73.00   0.50    0.20    --  104.61 -61.00 120.00   82
 36  \w     42.00 111.00   0.50    0.05    --   46.20  71.00 175.00  138
 37  \w   -157.00-106.00   0.50    0.20    -- -102.00 -71.00  44.00  102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-DW'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0604655000
_diffrn_orient_matrix_UB_12      0.1118051000
_diffrn_orient_matrix_UB_13      -0.0341889000
_diffrn_orient_matrix_UB_21      0.1233190000
_diffrn_orient_matrix_UB_22      0.0291603000
_diffrn_orient_matrix_UB_23      0.0922080000
_diffrn_orient_matrix_UB_31      0.1026817000
_diffrn_orient_matrix_UB_32      -0.0531684000
_diffrn_orient_matrix_UB_33      -0.0746772000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0764
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16475
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.459
_diffrn_reflns_theta_min         3.543
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              PhotonJet-DW
_exptl_absorpt_coefficient_mu    9.623
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28234
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.54a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       plate
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.767
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         5686
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0696
_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^)+(0.1222P)^2^+2.3909P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1809
_refine_ls_wR_factor_ref         0.1959
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4795
_reflns_number_total             5686
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc01159j2.cif
_cod_data_source_block           tkd-01-40
_cod_database_code               7129898
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Co2 B2 C32 H16 O8 '
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C19(H19), C17(H17), C7(H7), C13(H13), C10(H10), C5(H5), C25(H25),
 C12(H12), C18(H18), C4(H4), C6(H6), C24(H24), C23(H23), C22(H22), C11(H11)
;
_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 3.142
_oxdiff_exptl_absorpt_empirical_full_min 0.532