Partial Halogenation of Cyclic and Branched Perhydropentasilanes
Harald Stueger; Thomas Mitterfellner; Roland Fischer; Christoph Walkner; Matthias Patz; Stephan Wieber; Inorganic Chemistry 51 (2012) 6173–6179; doi:10.1021/ic300214y

data_4329336
_publ_section_title
;
 Partial Halogenation of Cyclic and Branched Perhydropentasilanes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6173
_journal_page_last               6179
_journal_paper_doi               10.1021/ic300214y
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C9 H11 Cl9 Si5'
_chemical_formula_sum            'C9 H11 Cl9 Si5'
_chemical_formula_weight         578.68
_chemical_melting_point          330
_chemical_name_common            Nonachloromesitylcyclopentasilane?
_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
_audit_update_record
;
2012-01-18 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 92.067(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8326(8)
_cell_length_b                   22.1445(15)
_cell_length_c                   8.6689(6)
_cell_measurement_reflns_used    9838
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.29
_cell_measurement_theta_min      2.99
_cell_volume                     2270.0(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0661
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            42455
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    1.368
_exptl_absorpt_correction_T_max  0.645
_exptl_absorpt_correction_T_min  0.515
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (multi-scan)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_description       Block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.082
_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     211
_refine_ls_number_reflns         5473
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0282
_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^)+(0.0444P)^2^+1.0866P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0815
_reflns_number_gt                4950
_reflns_number_total             5473
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300214y_si_001_2.cif
_cod_data_source_block           si5cl9mes
_cod_database_code               4329336