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_1565015
_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         'C64 H82 B3 N5 Si2'
_chemical_formula_sum            'C64 H82 B3 N5 Si2'
_chemical_formula_weight         1009.95
_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     dual
_audit_creation_date             2021-03-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2021-05-02 deposited with the CCDC.	2021-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                90.572(3)
_cell_angle_beta                 92.148(3)
_cell_angle_gamma                114.215(4)
_cell_formula_units_Z            2
_cell_length_a                   13.3902(5)
_cell_length_b                   13.4787(5)
_cell_length_c                   18.5010(5)
_cell_measurement_reflns_used    15543
_cell_measurement_temperature    113.15
_cell_measurement_theta_max      28.2830
_cell_measurement_theta_min      3.6480
_cell_volume                     3042.0(2)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      113.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.849
_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    -73.00 -47.00   0.50   30.00    --    5.00  45.00 177.89   52
  2  \w     67.00  93.00   0.50   30.00    --    5.00  45.00   0.00   52
  3  \w     24.00  74.00   0.50   30.00    --  -13.60  45.00 163.76  100
  4  \w     29.00  55.00   0.50   30.00    --  -13.60  45.00 155.89   52
  5  \w    -96.00 -70.00   0.50   30.00    --  -13.60  45.00  30.00   52
  6  \w    -65.00  27.00   0.50   30.00    --  -13.60  45.00  30.00  184
  7  \w    -85.00 -59.00   0.50   30.00    --  -13.60  45.00  90.00   52
  8  \w    -99.00  72.00   0.50   30.00    --  -13.60  45.00   0.00  342
  9  \w     30.00  71.00   0.50   30.00    --  -13.60  45.00  90.00   82
 10  \w    -99.00  -9.00   0.50   30.00    --  -13.60  45.00 120.00  180
 11  \w   -102.00 -77.00   0.50   30.00    --  -13.60  45.00 155.89   50
 12  \w      5.00  66.00   0.50   30.00    --  -13.60  45.00  60.00  122
 13  \w   -102.00 -46.00   0.50   30.00    --  -13.60  45.00 163.76  112
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0100713000
_diffrn_orient_matrix_UB_12      0.0003537000
_diffrn_orient_matrix_UB_13      0.0379370000
_diffrn_orient_matrix_UB_21      0.0341017000
_diffrn_orient_matrix_UB_22      -0.0278677000
_diffrn_orient_matrix_UB_23      -0.0054519000
_diffrn_orient_matrix_UB_31      0.0460068000
_diffrn_orient_matrix_UB_32      0.0505512000
_diffrn_orient_matrix_UB_33      -0.0020536000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0652
_diffrn_reflns_av_unetI/netI     0.0699
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.849
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            44829
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.849
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.011
_diffrn_reflns_theta_min         3.465
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64692
_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            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.103
_exptl_crystal_description       plate
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.846
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         13746
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.1071
_refine_ls_R_factor_gt           0.0773
_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^)+(0.0939P)^2^+3.3866P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2066
_refine_ls_wR_factor_ref         0.2253
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9833
_reflns_number_total             13746
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc05125c2.cif
_cod_data_source_block           m20210312c
_cod_database_code               1565015
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.980
_reflns_odcompleteness_completeness 98.28
_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
 C1B-C01T \\sim C1A-C01T
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C1A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C1B) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C1A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 C01T
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C01T, C1B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C01T, C1A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C021
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
5. Others
 Sof(HD)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=1-FVAR(1)
 Sof(H1)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C00F(H00F), C00N(H00N), C00P(H00P), C00R(H00R), C014(H014), C015(H015),
 C01J(H01J), C01T(HD), C01T(H1)
6.b Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C00C(H00C), C00D(H00D), C00E(H00E), C00H(H00H), C00J(H00J),
 C00K(H00K), C00O(H00O), C00Q(H00Q), C00S(H00S), C00T(H00T), C00W(H00W),
 C00X(H00X), C00Y(H00Y), C010(H010), C011(H011), C012(H012), C013(H013),
 C016(H016), C018(H018), C019(H019), C01A(H01A), C01E(H01E), C01I(H01I),
 C01U(H2), C01W(H4)
6.c Idealised Me refined as rotating group:
 C01K(H01B,H01C,H01D), C01L(H01F,H01G,H01H), C01M(H01K,H01L,H01M), C01N(H01N,
 H01O,H01P), C01O(H01Q,H01R,H01S), C01P(H01T,H01U,H01V), C01Q(H01W,H01X,H01Y),
 C01R(H01Z,H,HA), C01S(H01,HB,HC), C01V(H3,HE,HF), C01X(H5,HG,HH), C01Y(H6,HI,
 HJ), C01Z(H7,HK,HL), C020(H02A,H02B,H02C), C021(H02D,H02E,H02F), C1B(H1BA,H1BB,
 H1BC), C1A(H1AA,H1AB,H1AC)
;
_shelx_res_checksum              58141
_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 1.534
_oxdiff_exptl_absorpt_empirical_full_min 0.609