Isolation of a Planar 1,2-Dilithio-disilene and Its Conversion to Si−B Hybrid 2π-Electron System and a Planar Tetraboryldisilene
Tian, Miao; Zhang, Jianying; Guo, Lulu; Cui, Chunming; Chemical Science  (2021) –; doi:10.1039/D1SC05125C

data_1565017
_publ_section_title
;
 Isolation of a Planar 1,2-Dilithio-disilene and Its Conversion to
 Si&#x2212;B Hybrid 2\p-Electron System and a Planar Tetraboryldisilene
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC05125C
_journal_year                    2021
_chemical_formula_moiety         '2(C61 H83 B3 N4 Si2)'
_chemical_formula_sum            'C122.08 H165.06 B6 N8 Si4'
_chemical_formula_weight         1921.82
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2021-06-08 deposited with the CCDC.	2021-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3657(5)
_cell_length_b                   17.4514(5)
_cell_length_c                   39.6637(11)
_cell_measurement_reflns_used    31194
_cell_measurement_temperature    113.15
_cell_measurement_theta_max      29.4180
_cell_measurement_theta_min      1.6930
_cell_volume                     12020.3(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      113.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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   -115.00  65.00   1.00    1.00    --  -25.00  45.00   0.00  180
  2  \w   -115.00  35.00   1.00    1.00    --  -25.00  45.00  90.00  150
  3  \w   -115.00   5.00   1.00    1.00    --  -25.00  45.00 180.00  120
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0279368000
_diffrn_orient_matrix_UB_12      -0.0264316000
_diffrn_orient_matrix_UB_13      -0.0059588000
_diffrn_orient_matrix_UB_21      -0.0273798000
_diffrn_orient_matrix_UB_22      0.0300110000
_diffrn_orient_matrix_UB_23      -0.0011564000
_diffrn_orient_matrix_UB_31      0.0117440000
_diffrn_orient_matrix_UB_32      0.0072168000
_diffrn_orient_matrix_UB_33      -0.0168263000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1232
_diffrn_reflns_av_unetI/netI     0.1156
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            89515
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.150
_diffrn_reflns_theta_max         24.150
_diffrn_reflns_theta_min         1.932
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.062
_exptl_crystal_description       block
_exptl_crystal_F_000             4158
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.205
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 4093 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.09(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1320
_refine_ls_number_reflns         19193
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0668
_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^)+(0.0360P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1348
_reflns_Friedel_coverage         0.837
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                13324
_reflns_number_total             19193
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc05125c2.cif
_cod_data_source_block           r20210508a
_cod_database_code               1565017
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.981
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C59-C60 = C59-C61 = C59-C60A = C59-C61A
 1.54 with sigma of 0.01
 C60-C61 = C60A-C61A
 2.52 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C45) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C60A)
\\sim Ueq, Uanis(C61A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Others
 Sof(H59A)=Sof(C60A)=Sof(H60D)=Sof(H60E)=Sof(H60F)=Sof(C61A)=Sof(H61D)=
 Sof(H61E)=Sof(H61F)=1-FVAR(1)
 Sof(H59)=Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(H60C)=Sof(C61)=Sof(H61A)=Sof(H61B)=
 Sof(H61C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C18(H18), C21(H21), C30(H30), C33(H33), C44(H44), C47(H47), C56(H56),
 C59(H59), C59(H59A), C79(H79), C82(H82), C91(H91), C94(H94), C105(H105),
 C108(H108), C117(H117), C120(H120)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C10(H10), C11(H11), C14(H14), C15(H15), C16(H16), C26(H26),
 C27(H27), C28(H28), C36(H36), C37(H37), C40(H40), C41(H41), C42(H42), C52(H52),
  C53(H53), C54(H54), C64(H64), C66(H66), C71(H71), C72(H72), C75(H75),
 C76(H76), C77(H77), C87(H87), C88(H88), C89(H89), C97(H97), C98(H98),
 C101(H101), C102(H102), C103(H103), C113(H113), C114(H114), C115(H115)
5.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C19(H19A,H19B,H19C),
 C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C45(H45A,
 H45B,H45C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C),
 C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C60(H60A,H60B,H60C), C61(H61A,H61B,
 H61C), C60A(H60D,H60E,H60F), C61A(H61D,H61E,H61F), C68(H68A,H68B,H68C),
 C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C80(H80A,H80B,H80C), C81(H81A,H81B,
 H81C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C92(H92A,H92B,H92C), C93(H93A,
 H93B,H93C), C95(H95A,H95B,H95C), C96(H96A,H96B,H96C), C106(H10A,H10B,H10C),
 C107(H10D,H10E,H10F), C109(H10G,H10H,H10I), C110(H11A,H11B,H11C), C118(H11D,
 H11E,H11F), C119(H11G,H11H,H11I), C121(H12A,H12B,H12C), C122(H12D,H12E,H12F)
;
_shelx_res_checksum              6006
_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 1.726
_oxdiff_exptl_absorpt_empirical_full_min 0.457