Friedel−Crafts Alkylation of Polychlorobenzenes with (1,2-Dichloroethyl)trichlorosilane
Han, Joon Soo; Lim, Weon Cheol; Yoo, Bok Ryul; Jin, Jung-Il; Jung, Il Nam; Organometallics 21 (2002) 3803–; doi:10.1021/om020296c

data_4076924
_publ_section_title
;
 Friedel&#x2212;Crafts Alkylation of Polychlorobenzenes with
 (1,2-Dichloroethyl)trichlorosilane
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              3803
_journal_paper_doi               10.1021/om020296c
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C16 H6 Cl14 Si2'
_chemical_formula_weight         750.69
_chemical_melting_point          484(1)
_chemical_name_common
;1,2-trans-2,3-trans-4,5,6,7-Tetrachloro-1-(2,3,4,5-tetrachlorophenyl)
-2-trichlorosilyl-3-(trichlorosilylmethyl)indane 
;
_chemical_name_systematic
; 
1,2-trans-2,3-trans-4,5,6,7-Tetrachloro-1-(2,3,4,5-tetrachlorophenyl)
-2-trichlorosilyl-3-(trichlorosilylmethyl)indane 
;
_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                81.684(5)
_cell_angle_beta                 84.035(5)
_cell_angle_gamma                76.512(5)
_cell_formula_units_Z            2
_cell_length_a                   8.751(2)
_cell_length_b                   12.110(3)
_cell_length_c                   13.516(4)
_cell_measurement_reflns_used    4274
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      1.53
_cell_volume                     1374.5(6)
_computing_cell_refinement       'SMART v5.060'
_computing_data_collection       'SMART v5.060'
_computing_data_reduction        'SAINT v6.02'
_computing_molecular_graphics    'XSHELL v4.01'
_computing_publication_material  'XSHELL v4.01'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.827
_diffrn_measured_fraction_theta_max 0.827
_diffrn_measurement_device_type  'Bruker SMART CCD-1000'
_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  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0609
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10698
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    1.499
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.571886
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   (SADABS;Blessing,1995)
_exptl_crystal_colour            transparency
_exptl_crystal_density_diffrn    1.814
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       0.0000(6)
_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   0.962
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         5650
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          4.472
_refine_ls_shift/su_mean         0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0647P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1217
_reflns_number_gt                3646
_reflns_number_total             5650
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om020296c.cif
_cod_data_source_block           compound4
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1374.5(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4076924