#------------------------------------------------------------------------------
#$Date: 2016-03-21 06:19:05 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178503 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/50/4065011.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_4065011
loop_
_publ_author_name
'Albahily, Khalid'
'Gambarotta, Sandro'
'Duchateau, Robbert'
_publ_section_title
;
 Ethylene Oligomerization Promoted by a Silylated-SNS Chromium System
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4655
_journal_paper_doi               10.1021/om200505a
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C18 H39 Cl3 Cr N S2 Si2'
_chemical_formula_weight         548.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.510(6)
_cell_length_b                   24.278(9)
_cell_length_c                   13.791(5)
_cell_measurement_reflns_used    404
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      21.61
_cell_measurement_theta_min      2.98
_cell_volume                     5528(4)
_computing_cell_refinement       'SMART, Bruker (2000)'
_computing_data_collection       'SMART, Bruker (2000)'
_computing_data_reduction        'XPREP, Bruker (2000)'
_computing_molecular_graphics    'SHELXTL, Bruker (2000)'
_computing_publication_material  'SHELXTL, Bruker (2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  '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  0.0569
_diffrn_reflns_av_sigmaI/netI    0.0553
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5939
_diffrn_reflns_theta_full        22.00
_diffrn_reflns_theta_max         22.00
_diffrn_reflns_theta_min         3.36
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    0.948
_exptl_absorpt_correction_T_max  0.9112
_exptl_absorpt_correction_T_min  0.8709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2312
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         1642
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0747P)²+9.9908P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1252
_reflns_number_gt                1400
_reflns_number_total             1642
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200505a_si_001.cif
_cod_data_source_block           sg2818a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      Fdd2
_cod_database_code               4065011
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
N1 N 0.0218(7) 0.4948(5) 0.2150(9) 0.043(3) Uiso 0.50 1 d P -1
H102 H 0.0743 0.4770 0.2166 0.052 Uiso 0.50 1 d PR -1
Cr1 Cr 0.0000 0.5000 0.05862(12) 0.0409(5) Uani 1 2 d S .
Cl1 Cl -0.13516(13) 0.52569(9) 0.0702(3) 0.0868(9) Uani 1 1 d . .
Cl2 Cl 0.0000 0.5000 -0.1059(2) 0.0838(13) Uani 1 2 d S .
S1 S 0.03163(12) 0.59773(7) 0.06853(16) 0.0517(6) Uani 1 1 d . .
Si1 Si 0.04318(14) 0.55839(8) 0.27074(15) 0.0491(6) Uani 1 1 d . .
C1 C 0.0986(5) 0.5971(3) 0.1700(6) 0.051(2) Uani 1 1 d . .
H1A H 0.1112 0.6348 0.1905 0.061 Uiso 1 1 calc R .
H1B H 0.1493 0.5784 0.1534 0.061 Uiso 1 1 calc R .
C2 C 0.0877(7) 0.6236(4) -0.0347(8) 0.075(3) Uani 1 1 d . .
H2 H 0.0561 0.6126 -0.0926 0.090 Uiso 1 1 calc R .
C3 C 0.0887(7) 0.6854(4) -0.0352(9) 0.093(3) Uani 1 1 d . .
H3A H 0.1190 0.6989 0.0211 0.111 Uiso 1 1 calc R .
H3B H 0.0331 0.6993 -0.0305 0.111 Uiso 1 1 calc R .
C4 C 0.1279(9) 0.7069(5) -0.1281(10) 0.121(5) Uani 1 1 d . .
H4A H 0.0942 0.6970 -0.1840 0.145 Uiso 1 1 calc R .
H4B H 0.1316 0.7472 -0.1254 0.145 Uiso 1 1 calc R .
C5 C 0.2114(9) 0.6828(6) -0.1404(9) 0.128(6) Uani 1 1 d . .
H5A H 0.2345 0.6959 -0.2016 0.154 Uiso 1 1 calc R .
H5B H 0.2462 0.6958 -0.0876 0.154 Uiso 1 1 calc R .
C6 C 0.2106(10) 0.6224(8) -0.1404(11) 0.137(5) Uani 1 1 d . .
H6A H 0.2664 0.6088 -0.1449 0.164 Uiso 1 1 calc R .
H6B H 0.1811 0.6093 -0.1975 0.164 Uiso 1 1 calc R .
C7 C 0.1709(6) 0.5988(5) -0.0485(8) 0.087(3) Uani 1 1 d . .
H7A H 0.1663 0.5587 -0.0543 0.105 Uiso 1 1 calc R .
H7B H 0.2047 0.6071 0.0080 0.105 Uiso 1 1 calc R .
C8 C -0.0394(6) 0.6010(4) 0.3178(9) 0.086(3) Uani 1 1 d . .
H8A H -0.0761 0.6103 0.2654 0.129 Uiso 1 1 calc R .
H8B H -0.0172 0.6345 0.3455 0.129 Uiso 1 1 calc R .
H8C H -0.0685 0.5807 0.3673 0.129 Uiso 1 1 calc R .
C9 C 0.1145(7) 0.5363(5) 0.3632(8) 0.094(4) Uani 1 1 d . .
H9A H 0.1562 0.5137 0.3337 0.142 Uiso 1 1 calc R .
H9B H 0.0862 0.5150 0.4121 0.142 Uiso 1 1 calc R .
H9C H 0.1392 0.5683 0.3931 0.142 Uiso 1 1 calc R .
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'
S S 0.1246 0.1234 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 '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
Si1 N1 Si1 123.2(7) . 2_565
Si1 N1 Cr1 114.3(6) . .
Si1 N1 Cr1 110.8(6) 2_565 .
N1 Cr1 N1 20.1(6) . 2_565
N1 Cr1 Cl2 170.0(3) . .
N1 Cr1 Cl2 170.0(3) 2_565 .
N1 Cr1 Cl1 76.0(3) . 2_565
N1 Cr1 Cl1 96.1(3) 2_565 2_565
Cl2 Cr1 Cl1 93.94(10) . 2_565
N1 Cr1 Cl1 96.1(3) . .
N1 Cr1 Cl1 76.0(3) 2_565 .
Cl2 Cr1 Cl1 93.94(10) . .
Cl1 Cr1 Cl1 172.12(19) 2_565 .
N1 Cr1 S1 85.6(3) . 2_565
N1 Cr1 S1 88.0(4) 2_565 2_565
Cl2 Cr1 S1 93.22(7) . 2_565
Cl1 Cr1 S1 86.58(7) 2_565 2_565
Cl1 Cr1 S1 92.97(7) . 2_565
N1 Cr1 S1 88.0(4) . .
N1 Cr1 S1 85.6(3) 2_565 .
Cl2 Cr1 S1 93.22(7) . .
Cl1 Cr1 S1 92.98(7) 2_565 .
Cl1 Cr1 S1 86.58(7) . .
S1 Cr1 S1 173.56(13) 2_565 .
C1 S1 C2 107.6(4) . .
C1 S1 Cr1 99.7(2) . .
C2 S1 Cr1 113.8(3) . .
N1 Si1 C9 100.2(5) . .
N1 Si1 C8 120.1(5) . .
C9 Si1 C8 113.7(6) . .
N1 Si1 N1 24.3(7) . 2_565
C9 Si1 N1 117.5(5) . 2_565
C8 Si1 N1 96.3(5) . 2_565
N1 Si1 C1 102.1(5) . .
C9 Si1 C1 110.2(4) . .
C8 Si1 C1 109.7(4) . .
N1 Si1 C1 108.6(5) 2_565 .
S1 C1 Si1 106.1(4) . .
C3 C2 C7 112.8(9) . .
C3 C2 S1 110.8(8) . .
C7 C2 S1 115.3(7) . .
C2 C3 C4 110.5(10) . .
C5 C4 C3 110.4(11) . .
C6 C5 C4 112.4(11) . .
C5 C6 C7 112.1(12) . .
C2 C7 C6 110.1(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 Si1 1.761(13) .
N1 Si1 1.846(13) 2_565
N1 Cr1 2.190(12) .
Cr1 N1 2.190(12) 2_565
Cr1 Cl2 2.269(4) .
Cr1 Cl1 2.323(2) 2_565
Cr1 Cl1 2.323(2) .
Cr1 S1 2.433(2) 2_565
Cr1 S1 2.433(2) .
S1 C1 1.784(9) .
S1 C2 1.810(10) .
Si1 C9 1.817(11) .
Si1 C8 1.830(10) .
Si1 N1 1.847(13) 2_565
Si1 C1 1.912(8) .
C2 C3 1.502(13) .
C2 C7 1.510(15) .
C3 C4 1.527(16) .
C4 C5 1.51(2) .
C5 C6 1.466(19) .
C6 C7 1.537(16) .
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
Si1 N1 Cr1 N1 -78.8(19) . 2_565
Si1 N1 Cr1 N1 65.7(18) 2_565 2_565
Si1 N1 Cr1 Cl2 101.2(19) . .
Si1 N1 Cr1 Cl2 -114.3(18) 2_565 .
Si1 N1 Cr1 Cl1 97.3(6) . 2_565
Si1 N1 Cr1 Cl1 -118.1(5) 2_565 2_565
Si1 N1 Cr1 Cl1 -82.6(5) . .
Si1 N1 Cr1 Cl1 62.0(5) 2_565 .
Si1 N1 Cr1 S1 -175.1(6) . 2_565
Si1 N1 Cr1 S1 -30.6(5) 2_565 2_565
Si1 N1 Cr1 S1 3.8(5) . .
Si1 N1 Cr1 S1 148.3(5) 2_565 .
N1 Cr1 S1 C1 28.1(4) . .
N1 Cr1 S1 C1 48.1(4) 2_565 .
Cl2 Cr1 S1 C1 -141.9(3) . .
Cl1 Cr1 S1 C1 -47.8(3) 2_565 .
Cl1 Cr1 S1 C1 124.3(3) . .
S1 Cr1 S1 C1 38.1(3) 2_565 .
N1 Cr1 S1 C2 142.3(5) . .
N1 Cr1 S1 C2 162.3(5) 2_565 .
Cl2 Cr1 S1 C2 -27.7(4) . .
Cl1 Cr1 S1 C2 66.4(4) 2_565 .
Cl1 Cr1 S1 C2 -121.4(4) . .
S1 Cr1 S1 C2 152.3(4) 2_565 .
Si1 N1 Si1 C9 74.6(7) 2_565 .
Cr1 N1 Si1 C9 -145.8(6) . .
Si1 N1 Si1 C8 -50.6(9) 2_565 .
Cr1 N1 Si1 C8 89.1(7) . .
Si1 N1 Si1 N1 -63.4(10) 2_565 2_565
Cr1 N1 Si1 N1 76.2(9) . 2_565
Si1 N1 Si1 C1 -172.0(6) 2_565 .
Cr1 N1 Si1 C1 -32.4(6) . .
C2 S1 C1 Si1 -170.5(4) . .
Cr1 S1 C1 Si1 -51.6(4) . .
N1 Si1 C1 S1 56.6(5) . .
C9 Si1 C1 S1 162.3(5) . .
C8 Si1 C1 S1 -71.8(6) . .
N1 Si1 C1 S1 32.3(5) 2_565 .
C1 S1 C2 C3 -83.4(8) . .
Cr1 S1 C2 C3 167.1(7) . .
C1 S1 C2 C7 46.2(9) . .
Cr1 S1 C2 C7 -63.3(9) . .
C7 C2 C3 C4 55.4(13) . .
S1 C2 C3 C4 -173.7(9) . .
C2 C3 C4 C5 -55.2(15) . .
C3 C4 C5 C6 56.5(16) . .
C4 C5 C6 C7 -55.8(18) . .
C3 C2 C7 C6 -53.6(14) . .
S1 C2 C7 C6 177.8(10) . .
C5 C6 C7 C2 53.3(17) . .
