Friedel-Crafts Peralkylation of Benzene with -Chloroalkyltrichlorosilanes: One-Pot Synthesis of Polyfunctionalized Hexakis[-(trichlorosilyl)alkyl]benzenes
Kyung Mi Kim; Jeong Hyun Kim; Do Hyun Moon; Myoung Soo Lah; Il Nam Jung; Bok Ryul Yoo; Organometallics 24 (2005) 226–230; doi:10.1021/om0495933

data_4060030
_publ_section_title
;
 Friedel-Crafts Peralkylation of Benzene with
 -Chloroalkyltrichlorosilanes: One-Pot Synthesis of Polyfunctionalized
 Hexakis[-(trichlorosilyl)alkyl]benzenes
;
_journal_name_full               Organometallics
_journal_page_first              226
_journal_page_last               230
_journal_paper_doi               10.1021/om0495933
_journal_volume                  24
_journal_year                    2005
_chemical_formula_moiety         'C24 H36 Cl18 Si6'
_chemical_formula_sum            'C24 H36 Cl18 Si6'
_chemical_formula_weight         1131.17
_chemical_melting_point          413
_chemical_name_common            Hexakis[3-(trichlorosilyl)propyl]benzene
_chemical_name_systematic
; 
Hexakis[3-(trichlorosilyl)propyl]benzene 
;
_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
_cell_angle_alpha                89.879(8)
_cell_angle_beta                 79.459(8)
_cell_angle_gamma                74.784(7)
_cell_formula_units_Z            2
_cell_length_a                   13.382(6)
_cell_length_b                   13.436(6)
_cell_length_c                   14.294(7)
_cell_measurement_reflns_used    100783
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      57.13
_cell_measurement_theta_min      4.694
_cell_volume                     2435(2)
_computing_cell_refinement       XPREP
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    XSHELL
_computing_publication_material  XSHELL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'SMART 1000 CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0743
_diffrn_reflns_av_sigmaI/netI    0.0675
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            49913
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    1.179
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.22
_refine_diff_density_max         2.157
_refine_diff_density_min         -0.967
_refine_diff_density_rms         0.213
_refine_ls_extinction_coef       0.0000(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         11770
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1773
_refine_ls_R_factor_gt           0.1319
_refine_ls_shift/su_max          2.265
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1678P)^2^+26.8250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3460
_refine_ls_wR_factor_ref         0.3743
_reflns_number_gt                7651
_reflns_number_total             11770
_reflns_threshold_expression     >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4060030