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_4129014
_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, C4 H8 O, 2(C24 H20 B)'
_chemical_formula_sum            'C112 H140 B2 N8 O Si4'
_chemical_formula_weight         1748.29
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-06-07
_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                   23.2625(4)
_cell_length_b                   17.5096(8)
_cell_length_c                   24.5181(6)
_cell_measurement_reflns_used    73832
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      64.43
_cell_measurement_theta_min      2.70
_cell_volume                     9986.6(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      150.15
_diffrn_detector_area_resol_mean 13.33
_diffrn_detector_type            Dectris
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34143
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            67280
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        53.597
_diffrn_reflns_theta_max         62.539
_diffrn_reflns_theta_min         3.136
_exptl_absorpt_coefficient_mu    0.616
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.0294
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            'reddish orange'
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_description       block
_exptl_crystal_F_000             3768
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     687
_refine_ls_number_reflns         12014
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0751P)^2^+2.1973P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1232
_refine_ls_wR_factor_ref         0.1321
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9744
_reflns_number_total             12014
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b08018_si_003.cif
_cod_data_source_block           tsxf03b
_cod_database_code               4129014
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.887
_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
 C12-C13B \\sim C12-C13A
 with sigma of 0.02
 C12-C14B \\sim C12-C14A
 with sigma of 0.02
 C12-C15B \\sim C12-C15A
 with sigma of 0.02
 C23-C24B \\sim C23-C24A
 with sigma of 0.02
 C23-C25B \\sim C23-C25A
 with sigma of 0.02
 C23-C26B \\sim C23-C26A
 with sigma of 0.02
 C27-C28B \\sim C27-C28A
 with sigma of 0.02
 C27-C29B \\sim C27-C29A
 with sigma of 0.02
 C27-C30B \\sim C27-C30A
 with sigma of 0.02
3. Others
 Fixed Sof: C13A(0.3) H13D(0.3) H13E(0.3) H13F(0.3) C13B(0.7) H13A(0.7)
 H13B(0.7) H13C(0.7) C14A(0.3) H14D(0.3) H14E(0.3) H14F(0.3) C14B(0.7)
 H14A(0.7) H14B(0.7) H14C(0.7) C15A(0.3) H15D(0.3) H15E(0.3) H15F(0.3)
 C15B(0.7) H15A(0.7) H15B(0.7) H15C(0.7) C24A(0.3) H24D(0.3) H24E(0.3)
 H24F(0.3) C24B(0.7) H24A(0.7) H24B(0.7) H24C(0.7) C25A(0.3) H25D(0.3)
 H25E(0.3) H25F(0.3) C25B(0.7) H25A(0.7) H25B(0.7) H25C(0.7) C26A(0.3)
 H26D(0.3) H26E(0.3) H26F(0.3) C26B(0.7) H26A(0.7) H26B(0.7) H26C(0.7)
 C28A(0.5) H28D(0.5) H28E(0.5) H28F(0.5) C28B(0.5) H28A(0.5) H28B(0.5)
 H28C(0.5) C29A(0.5) H29D(0.5) H29E(0.5) H29F(0.5) C29B(0.5) H29A(0.5)
 H29B(0.5) H29C(0.5) C30A(0.5) H30D(0.5) H30E(0.5) H30F(0.5) C30B(0.5)
 H30A(0.5) H30B(0.5) H30C(0.5) O(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C56(H56A,H56B)
4.b 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)
4.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13A(H13D,H13E,
 H13F), C13B(H13A,H13B,H13C), C14A(H14D,H14E,H14F), C14B(H14A,H14B,H14C),
 C15A(H15D,H15E,H15F), C15B(H15A,H15B,H15C), C24A(H24D,H24E,H24F), C24B(H24A,
 H24B,H24C), C25A(H25D,H25E,H25F), C25B(H25A,H25B,H25C), C26A(H26D,H26E,H26F),
 C26B(H26A,H26B,H26C), C28A(H28D,H28E,H28F), C28B(H28A,H28B,H28C), C29A(H29D,
 H29E,H29F), C29B(H29A,H29B,H29C), C30A(H30D,H30E,H30F), C30B(H30A,H30B,H30C)
;
_shelx_res_checksum              73265
_shelx_hkl_checksum              23651
_olex2_submission_special_instructions 'No special instructions were received'