A Stable Aromatic Tetrasilacyclobutadiene Dication.
Sun, Xiaofei; Simler, Thomas; Yadav, Ravi; Köppe, Ralf; Roesky, Peter W.; Journal of the American Chemical Society 141 (2019) 14987–14990; doi:10.1021/jacs.9b08018

data_4129012
_publ_contact_author
;
      Prof. Dr. Peter W. Roesky
      Karlsruher Institut fuer Technologie (KIT), CS
      Institut fuer Anorganische Chemie (AOC)
      Lehrstuhl fuer Anorganische Funktionsmaterialien
      Engesserstr. 15, Geb. 30.45
      76131 Karlsruhe 
      Bundesrepublik Deutschland

;
_publ_section_title
;
 A Stable Aromatic Tetrasilacyclobutadiene Dication.
;
_journal_issue                   38
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14987
_journal_page_last               14990
_journal_paper_doi               10.1021/jacs.9b08018
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C60 H92 N8 Si4, 2(C24 H20 B), 2(C2 H3 N)'
_chemical_formula_sum            'C112 H138 B2 N10 Si4'
_chemical_formula_weight         1758.30
_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             2019-05-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.3425(6)
_cell_length_b                   17.6797(4)
_cell_length_c                   24.6828(8)
_cell_measurement_reflns_used    12994
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.60
_cell_volume                     10186.3(5)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
PLATON (A.L.Spek, 2009)
;
_computing_data_collection       'X-Area Pilatus3_SV 1.31.150.0 (STOE, 2018)'
_computing_data_reduction
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
PLATON (A.L.Spek, 2009)
;
_computing_molecular_graphics    'Diamond 4, Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.84, Darmstadt 2018
MS Word (Microsoft)
Olex2 (Dolomanov et al., 2009)
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CMOS pixel detector'
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'Dectris Pilatus 100k'
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'single reflection optic'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_unetI/netI     0.0734
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            24699
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.100
_diffrn_reflns_theta_min         2.598
_diffrn_source                   'Mo LFF Sealed Tube'
_diffrn_source_type              'Xenocs Genix3D microfocus'
_exptl_absorpt_coefficient_mu    0.111
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'STOE XRED & LANA'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_description       prism
_exptl_crystal_F_000             3784
_exptl_crystal_size_max          0.378
_exptl_crystal_size_mid          0.277
_exptl_crystal_size_min          0.171
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     678
_refine_ls_number_reflns         9838
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1466
_refine_ls_R_factor_gt           0.0851
_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^)+(0.1043P)^2^+10.3750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2033
_refine_ls_wR_factor_ref         0.2381
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5802
_reflns_number_total             9838
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b08018_si_002.cif
_cod_data_source_block           tsxf05
_cod_database_code               4129012
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.959
_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. Restrained distances
 C55-N5
 1.137 with sigma of 0.01
 C55-C56
 1.456 with sigma of 0.01
 C56-N5
 2.593 with sigma of 0.02
 C57-N6
 1.137 with sigma of 0.01
 C57-C58
 1.456 with sigma of 0.01
 C58-N6
 2.593 with sigma of 0.02
 C27-C28B \\sim C27-C28A
 with sigma of 0.02
 C27-C30B \\sim C27-C30A
 with sigma of 0.02
 C27-C29B \\sim C27-C29A
 with sigma of 0.02
 C23-C24B \\sim C23-C24A
 with sigma of 0.02
 C23-C26B \\sim C23-C26A
 with sigma of 0.02
 C23-C25B \\sim C23-C25A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C28B \\sim C29B \\sim C30B \\sim C28A \\sim C29A \\sim C30A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C24B(0.7) H24A(0.7) H24B(0.7) H24C(0.7) C25B(0.7) H25A(0.7)
 H25B(0.7) H25C(0.7) C26B(0.7) H26A(0.7) H26B(0.7) H26C(0.7) C28B(0.6)
 H28A(0.6) H28B(0.6) H28C(0.6) C29B(0.6) H29B(0.6) H29C(0.6) H29A(0.6)
 C30B(0.6) H30A(0.6) H30B(0.6) H30C(0.6) C24A(0.3) H24D(0.3) H24E(0.3)
 H24F(0.3) C25A(0.3) H25D(0.3) H25E(0.3) H25F(0.3) C26A(0.3) H26D(0.3)
 H26E(0.3) H26F(0.3) C28A(0.4) H28D(0.4) H28E(0.4) H28F(0.4) C29A(0.4)
 H29D(0.4) H29E(0.4) H29F(0.4) C30A(0.4) H30D(0.4) H30E(0.4) H30F(0.4) N6(0.5)
 C57(0.5) C58(0.5) H58A(0.5) H58B(0.5) H58C(0.5) N5(0.5) C55(0.5) C56(0.5)
 H56A(0.5) H56B(0.5) H56C(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C18(H18), C19(H19), C20(H20),
 C21(H21), C22(H22), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38),
  C39(H39), C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46),
 C47(H47), C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54)
5.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C24B(H24A,H24B,H24C),
 C25B(H25A,H25B,H25C), C26B(H26A,H26B,H26C), C28B(H28A,H28B,H28C), C29B(H29B,
 H29C,H29A), C30B(H30A,H30B,H30C), C24A(H24D,H24E,H24F), C25A(H25D,H25E,H25F),
 C26A(H26D,H26E,H26F), C28A(H28D,H28E,H28F), C29A(H29D,H29E,H29F), C30A(H30D,
 H30E,H30F), C58(H58A,H58B,H58C), C56(H56A,H56B,H56C)
;
_shelx_res_checksum              3390
_shelx_hkl_checksum              53223
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'