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_4329337
_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         'C12 H17 Cl9 Si5'
_chemical_formula_sum            'C12 H17 Cl9 Si5'
_chemical_formula_weight         620.76
_chemical_melting_point          397
_chemical_name_common
(4-t-Butyl-2,6-dimethylphenyl)nonachloro-cyclopentasilane
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                66.4150(10)
_cell_angle_beta                 84.3530(10)
_cell_angle_gamma                84.6660(10)
_cell_formula_units_Z            2
_cell_length_a                   9.2711(3)
_cell_length_b                   11.4701(4)
_cell_length_c                   13.3919(5)
_cell_measurement_reflns_used    9864
_cell_measurement_temperature    102(2)
_cell_measurement_theta_max      33.338
_cell_measurement_theta_min      2.677
_cell_volume                     1296.56(8)
_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      102(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0196
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26211
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    1.203
_exptl_absorpt_correction_T_max  0.5522
_exptl_absorpt_correction_T_min  0.5131
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (multi-scan)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_description       block
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.59
_exptl_crystal_size_min          0.56
_refine_diff_density_max         0.641
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         6869
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0224
_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^)+(0.0218P)^2^+0.6893P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0568
_refine_ls_wR_factor_ref         0.0584
_reflns_number_gt                6411
_reflns_number_total             6869
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300214y_si_001_3.cif
_cod_data_source_block           ja2010_147_0m
_cod_database_code               4329337