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#$Date: 2016-03-22 12:11:15 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178939 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/68/4116845.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4116845
loop_
_publ_author_name
'Karl Hensen'
'Thorsten Stumpf'
'Michael Bolte'
'Christian Näther'
'Holger Fleischer'
_publ_contact_author
;
      Dr. Michael Bolte
      Institut für Organische Chemie
      J.-W.-Goethe-Universität
      Marie-Curie-Str. 11
      60439 Frankfurt/Main
      Germany
;
_publ_contact_author_email       bolte@chemie.uni-frankfurt.de
_publ_contact_author_fax         '49 69 798 29128'
_publ_contact_author_phone       '49 69 798 29136'
_publ_section_title
;
 Experimental Investigations and ab Initio Studies on Hexacoordinated
 Complexes of Dichlorosilane
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10402
_journal_page_last               10408
_journal_paper_doi               10.1021/ja981016g
_journal_volume                  120
_journal_year                    1998
_chemical_formula_sum            'C24 H26 Cl14 N4 Si'
_chemical_formula_weight         894.88
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 99.767(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.5080(10)
_cell_length_b                   14.8330(10)
_cell_length_c                   12.5080(10)
_cell_measurement_temperature    130(2)
_cell_volume                     1921.3(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_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  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2470
_diffrn_reflns_theta_max         26.49
_diffrn_reflns_theta_min         2.40
_exptl_absorpt_coefficient_mu    1.059
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_F_000             900
_refine_diff_density_max         0.841
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.061
_refine_ls_goodness_of_fit_obs   1.117
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         2065
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_restrained_S_obs      1.117
_refine_ls_R_factor_all          0.0897
_refine_ls_R_factor_obs          0.0641
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0487P)²+10.9459P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1609
_refine_ls_wR_factor_obs         0.1446
_reflns_number_observed          1530
_reflns_number_total             2065
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja981016g_1.cif
_cod_data_source_block           bock327
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+10.9459P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+10.9459P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'C 1 2/c 1'
_cod_database_code               4116845
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Si1 Si 0.5000 0.5000 0.5000 0.0245(4) Uani 1 d S
N1 N 0.3728(4) 0.5000 0.3657(4) 0.0261(9) Uani 1 d S
C1 C 0.2441(5) 0.5000 0.3692(4) 0.0290(11) Uani 1 d S
H1 H 0.2170(5) 0.5000 0.4380(4) 0.035 Uiso 1 calc SR
C2 C 0.1522(6) 0.5000 0.2777(5) 0.0360(13) Uani 1 d S
H2 H 0.0630(6) 0.5000 0.2828(5) 0.043 Uiso 1 calc SR
C3 C 0.1916(6) 0.5000 0.1773(5) 0.0393(14) Uani 1 d S
H3 H 0.1298(6) 0.5000 0.1123(5) 0.047 Uiso 1 calc SR
C4 C 0.3221(6) 0.5000 0.1733(5) 0.0418(14) Uani 1 d S
H4 H 0.3511(6) 0.5000 0.1053(5) 0.050 Uiso 1 calc SR
C5 C 0.4102(6) 0.5000 0.2684(5) 0.0336(12) Uani 1 d S
H5 H 0.4998(6) 0.5000 0.2649(5) 0.040 Uiso 1 calc SR
N2 N 0.5000 0.6328(3) 0.5000 0.0319(10) Uani 1 d S
C6 C 0.4201(5) 0.6783(3) 0.5537(4) 0.0467(11) Uani 1 d .
H6 H 0.3631(5) 0.6461(3) 0.5912(4) 0.056 Uiso 1 calc R
C7 C 0.4199(6) 0.7710(3) 0.5552(5) 0.063(2) Uani 1 d .
H7 H 0.3639(6) 0.8023(3) 0.5946(5) 0.076 Uiso 1 calc R
C8 C 0.5000 0.8185(5) 0.5000 0.070(3) Uani 1 d S
H8 H 0.5000 0.8825(5) 0.5000 0.083 Uiso 1 calc SR
Cl1 Cl 0.16359(14) 0.5000 0.63944(11) 0.0329(3) Uani 1 d S
C9 C 0.2212(4) 0.3410(3) 0.8294(4) 0.0431(10) Uani 1 d .
Cl2 Cl 0.3797(2) 0.36107(15) 0.8887(2) 0.1011(7) Uani 1 d .
Cl3 Cl 0.1196(2) 0.35664(15) 0.9239(2) 0.0993(7) Uani 1 d .
Cl4 Cl 0.2049(2) 0.23201(11) 0.7782(2) 0.1040(7) Uani 1 d .
H9 H 0.1934(44) 0.3832(34) 0.7674(38) 0.049(13) Uiso 1 d .
H1SI H 0.4050(46) 0.5000 0.5575(38) 0.014(12) Uiso 1 d S
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 Si1 N1 180.0 5_666 .
N1 Si1 N2 90.0 5_666 .
N1 Si1 N2 90.0 . .
N1 Si1 N2 90.0 5_666 5_666
N1 Si1 N2 90.0 . 5_666
N2 Si1 N2 180.0 . 5_666
C5 N1 C1 118.4(5) . .
C5 N1 Si1 121.0(4) . .
C1 N1 Si1 120.6(4) . .
N1 C1 C2 122.5(5) . .
C1 C2 C3 118.8(5) . .
C4 C3 C2 118.9(6) . .
C5 C4 C3 119.6(6) . .
N1 C5 C4 121.8(5) . .
C6 N2 C6 119.7(5) 2_656 .
C6 N2 Si1 120.2(3) 2_656 .
C6 N2 Si1 120.2(3) . .
N2 C6 C7 120.8(5) . .
C8 C7 C6 120.3(6) . .
C7 C8 C7 118.1(6) . 2_656
Cl2 C9 Cl4 110.2(3) . .
Cl2 C9 Cl3 110.1(3) . .
Cl4 C9 Cl3 110.0(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 N1 1.962(4) 5_666
Si1 N1 1.962(4) .
Si1 N2 1.970(4) .
Si1 N2 1.970(4) 5_666
N1 C5 1.341(7) .
N1 C1 1.361(7) .
C1 C2 1.366(8) .
C2 C3 1.388(8) .
C3 C4 1.381(9) .
C4 C5 1.377(8) .
N2 C6 1.343(5) 2_656
N2 C6 1.343(5) .
C6 C7 1.375(6) .
C7 C8 1.371(7) .
C8 C7 1.371(7) 2_656
C9 Cl2 1.730(5) .
C9 Cl4 1.736(5) .
C9 Cl3 1.738(5) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N1 Si1 N1 C5 -73.5(1000) 5_666 .
N2 Si1 N1 C5 90.0 . .
N2 Si1 N1 C5 -90.0 5_666 .
N1 Si1 N1 C1 106.5(1000) 5_666 .
N2 Si1 N1 C1 -90.0 . .
N2 Si1 N1 C1 90.0 5_666 .
C5 N1 C1 C2 0.000(1) . .
Si1 N1 C1 C2 180.0 . .
N1 C1 C2 C3 0.000(1) . .
C1 C2 C3 C4 0.0 . .
C2 C3 C4 C5 0.0 . .
C1 N1 C5 C4 0.0 . .
Si1 N1 C5 C4 180.0 . .
C3 C4 C5 N1 0.0 . .
N1 Si1 N2 C6 92.4(3) 5_666 2_656
N1 Si1 N2 C6 -87.6(3) . 2_656
N2 Si1 N2 C6 0.0(1000) 5_666 2_656
N1 Si1 N2 C6 -87.6(3) 5_666 .
N1 Si1 N2 C6 92.4(3) . .
N2 Si1 N2 C6 0.0(1000) 5_666 .
C6 N2 C6 C7 -0.6(4) 2_656 .
Si1 N2 C6 C7 179.4(4) . .
N2 C6 C7 C8 1.1(7) . .
C6 C7 C8 C7 -0.5(4) . 2_656
