Synthesis of Cyclic and Bicyclic Polysilanes of Variable Ring Sizes
Zirngast, Michaela; Baumgartner, Judith; Marschner, Christoph; Organometallics 27 (2008) 6472–; doi:10.1021/om800842p

data_4072401
_publ_section_title
;
 Synthesis of Cyclic and Bicyclic Polysilanes of Variable Ring Sizes
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              6472
_journal_paper_doi               10.1021/om800842p
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C24 H72 Si12'
_chemical_formula_weight         697.89
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.36(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.842(5)
_cell_length_b                   16.013(3)
_cell_length_c                   26.748(5)
_cell_measurement_temperature    100(2)
_cell_volume                     9230(4)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w 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  0.1053
_diffrn_reflns_av_sigmaI/netI    0.0921
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            60613
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         0.94
_exptl_absorpt_coefficient_mu    0.350
_exptl_absorpt_correction_T_max  0.9145
_exptl_absorpt_correction_T_min  0.8726
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.004
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             3072
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.502
_refine_diff_density_min         -1.584
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         14482
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      2.202
_refine_ls_R_factor_all          0.1871
_refine_ls_R_factor_gt           0.1487
_refine_ls_shift/su_max          4.477
_refine_ls_shift/su_mean         0.019
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+107.8498P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2850
_refine_ls_wR_factor_ref         0.3076
_reflns_number_gt                10564
_reflns_number_total             14482
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800842p_si_001.cif
_cod_data_source_block           4_486j
_cod_original_cell_volume        9230(3)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4072401