Synthesis of a Pentasilapropellane. Exploring the Nature of a Stretched Silicon-Silicon Bond in a Nonclassical Molecule
Dominik Nied; Ralf Köppe; Wim Klopper; Hansgeorg Schnöckel; Frank Breher; Journal of the American Chemical Society 132 (2010) 10264–10265; doi:10.1021/ja104810u

data_4102783
_publ_contact_author_address
;
Institute of Inorganic Chemistry
Karlsruhe Institute of Technology (KIT)
Engesserstr. 15
76131 Karlsruhe
Germany
;
_publ_contact_author_email       breher@kit.edu
_publ_contact_author_fax         '(+49) 721 608 70 21'
_publ_contact_author_name        'Prof. Dr. Frank Breher'
_publ_section_title
;
 Synthesis of a Pentasilapropellane. Exploring the Nature of a Stretched
 Silicon-Silicon Bond in a Nonclassical Molecule
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10264
_journal_page_last               10265
_journal_paper_doi               10.1021/ja104810u
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C54 H66 Si5'
_chemical_formula_sum            'C54 H66 Si5'
_chemical_formula_weight         855.52
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'form.cif (version 2.0)'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   8.5116(17)
_cell_length_b                   26.887(5)
_cell_length_c                   41.174(8)
_cell_measurement_reflns_used    65162
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      3.85
_cell_volume                     9423(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'STOE Stadi with CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0930
_diffrn_reflns_av_sigmaI/netI    0.0519
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            65162
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         3.85
_exptl_absorpt_coefficient_mu    0.188
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rod-like crystal'
_exptl_crystal_F_000             3680
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.380
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         9610
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.380
_refine_ls_R_factor_all          0.1069
_refine_ls_R_factor_gt           0.0980
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+14.4762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1776
_refine_ls_wR_factor_ref         0.1813
_reflns_number_gt                9023
_reflns_number_total             9610
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja104810u_si_002.cif
_cod_data_source_block           Si5Mes6
_cod_database_code               4102783