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_1565016
_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         'C67 H95 B3 N4 Si2'
_chemical_formula_sum            'C67 H95 B3 N4 Si2'
_chemical_formula_weight         1045.07
_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
_audit_creation_date             2021-04-30
_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
_cell_angle_beta                 90.338(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0914(5)
_cell_length_b                   24.4943(7)
_cell_length_c                   20.4237(7)
_cell_measurement_reflns_used    22687
_cell_measurement_temperature    113.15
_cell_measurement_theta_max      32.7710
_cell_measurement_theta_min      1.9180
_cell_volume                     7049.3(4)
_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_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0808
_diffrn_reflns_av_unetI/netI     0.0925
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            88278
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.939
_diffrn_reflns_theta_min         1.751
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.48777
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.985
_exptl_crystal_description       block
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     707
_refine_ls_number_reflns         24269
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1276
_refine_ls_R_factor_gt           0.0672
_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^)+(0.0742P)^2^+0.1146P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1511
_refine_ls_wR_factor_ref         0.1780
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13916
_reflns_number_total             24269
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc05125c2.cif
_cod_data_source_block           r20210428e_sq_sq
_cod_database_code               1565016
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.983
_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 Ternary CH refined with riding coordinates:
 C00H(H00H), C00T(H00T), C010(H010), C011(H011), C012(H012), C018(H018),
 C01A(H01G), C01C(H01I), C01D(H01J), C01F(H01L), C01G(H01M)
2.b Aromatic/amide H refined with riding coordinates:
 C008(H008), C00C(H00C), C00J(H00J), C00N(H00N), C00O(H00O), C00P(H00P),
 C00Q(H00Q), C00R(H00R), C00S(H00S), C00V(H00V), C00W(H00W), C014(H014),
 C016(H016), C019(H019), C01B(H01H), C01E(H01K), C01H(H01N), C01K(H01R)
2.c Idealised Me refined as rotating group:
 C00Z(H00A,H00B,H00D), C015(H01A,H01B,H01C), C017(H01D,H01E,H01F), C01J(H01O,
 H01P,H01Q), C01M(H01S,H01T,H01U), C01N(H01V,H01W,H01X), C01O(H01Y,H,HA),
 C01Q(H01Z,HB,HC), C01R(H01,HD,HE), C01S(H1,HF,HG), C01T(H2,HH,HI), C01U(H3,HJ,
 HK), C01V(H4,HL,HM), C01W(H5,HN,HO), C01X(H6,HP,HQ), C01Y(H7,HR,HS), C01Z(H8,
 HT,HU), C020(H02A,H02B,H02C), C021(H02D,H02E,H02F), C022(H02G,H02H,H02I),
 C023(H02J,H02K,H02L), C024(H02M,H02N,H02O)
;
_shelx_res_checksum              83594
_shelx_fab_checksum              69309
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'