#------------------------------------------------------------------------------
#$Date: 2016-03-21 06:19:05 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178503 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/50/4065015.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_4065015
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            'C14 H34 Cl Cr N S2 Si2'
_chemical_formula_weight         424.17
_chemical_name_systematic
;

 ?

;
_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                96.8850(10)
_cell_angle_beta                 103.7370(10)
_cell_angle_gamma                108.1910(10)
_cell_formula_units_Z            2
_cell_length_a                   9.4189(8)
_cell_length_b                   10.2886(9)
_cell_length_c                   12.5226(11)
_cell_measurement_reflns_used    6463
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.73
_cell_measurement_theta_min      2.38
_cell_volume                     1094.88(16)
_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      200(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_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  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9299
_diffrn_reflns_theta_full        24.73
_diffrn_reflns_theta_max         24.73
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    0.940
_exptl_absorpt_correction_T_max  0.9545
_exptl_absorpt_correction_T_min  0.9119
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3600
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0608P)²+0.3765P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1069
_reflns_number_gt                2881
_reflns_number_total             3600
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200505a_si_001.cif
_cod_data_source_block           sg3919
_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 

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_cell_volume        1094.87(16)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4065015
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cr1 Cr 0.61583(6) 0.63977(5) 0.62040(4) 0.02759(16) Uani 1 1 d .
Cl1 Cl 0.42167(10) 0.61179(8) 0.44609(6) 0.0346(2) Uani 1 1 d .
N1 N 0.7692(3) 0.6643(3) 0.7720(2) 0.0283(6) Uani 1 1 d .
S1 S 0.86946(9) 0.76948(8) 0.56454(6) 0.0318(2) Uani 1 1 d .
S2 S 0.48060(9) 0.76373(8) 0.72377(6) 0.0295(2) Uani 1 1 d .
Si1 Si 0.95583(11) 0.67927(11) 0.77998(8) 0.0389(3) Uani 1 1 d .
Si2 Si 0.68964(10) 0.63950(9) 0.87967(7) 0.0294(2) Uani 1 1 d .
C1 C 0.9733(4) 0.6670(4) 0.6318(3) 0.0389(8) Uani 1 1 d .
H1A H 1.0845 0.7041 0.6336 0.047 Uiso 1 1 calc R
H1B H 0.9272 0.5684 0.5903 0.047 Uiso 1 1 calc R
C2 C 0.5308(4) 0.7200(4) 0.8604(3) 0.0373(8) Uani 1 1 d .
H2A H 0.4360 0.6534 0.8708 0.045 Uiso 1 1 calc R
H2B H 0.5666 0.8059 0.9194 0.045 Uiso 1 1 calc R
C3 C 1.1036(5) 0.8522(6) 0.8644(4) 0.0767(16) Uani 1 1 d .
H3A H 1.0987 0.8635 0.9421 0.115 Uiso 1 1 calc R
H3B H 1.0809 0.9280 0.8316 0.115 Uiso 1 1 calc R
H3C H 1.2085 0.8555 0.8635 0.115 Uiso 1 1 calc R
C4 C 1.0147(6) 0.5389(6) 0.8380(4) 0.0789(16) Uani 1 1 d .
H4A H 1.0068 0.5428 0.9149 0.118 Uiso 1 1 calc R
H4B H 1.1227 0.5528 0.8387 0.118 Uiso 1 1 calc R
H4C H 0.9455 0.4474 0.7909 0.118 Uiso 1 1 calc R
C5 C 0.5987(5) 0.4492(4) 0.8802(3) 0.0446(9) Uani 1 1 d .
H5A H 0.6791 0.4063 0.8898 0.067 Uiso 1 1 calc R
H5B H 0.5175 0.4019 0.8087 0.067 Uiso 1 1 calc R
H5C H 0.5520 0.4400 0.9423 0.067 Uiso 1 1 calc R
C6 C 0.8261(4) 0.7255(4) 1.0237(3) 0.0443(9) Uani 1 1 d .
H6A H 0.9107 0.6877 1.0381 0.066 Uiso 1 1 calc R
H6B H 0.7690 0.7072 1.0795 0.066 Uiso 1 1 calc R
H6C H 0.8702 0.8266 1.0290 0.066 Uiso 1 1 calc R
C7 C 0.8701(4) 0.7406(3) 0.4164(3) 0.0345(8) Uani 1 1 d .
C8 C 0.7806(4) 0.5874(4) 0.3584(3) 0.0395(8) Uani 1 1 d .
H8A H 0.7822 0.5739 0.2799 0.059 Uiso 1 1 calc R
H8B H 0.6722 0.5615 0.3608 0.059 Uiso 1 1 calc R
H8C H 0.8298 0.5283 0.3972 0.059 Uiso 1 1 calc R
C9 C 0.7874(5) 0.8336(4) 0.3630(3) 0.0481(10) Uani 1 1 d .
H9A H 0.7834 0.8236 0.2834 0.072 Uiso 1 1 calc R
H9B H 0.8450 0.9314 0.4019 0.072 Uiso 1 1 calc R
H9C H 0.6809 0.8053 0.3696 0.072 Uiso 1 1 calc R
C10 C 1.0392(5) 0.7845(4) 0.4110(3) 0.0547(11) Uani 1 1 d .
H10A H 1.0393 0.7691 0.3322 0.082 Uiso 1 1 calc R
H10B H 1.0921 0.7286 0.4511 0.082 Uiso 1 1 calc R
H10C H 1.0941 0.8839 0.4461 0.082 Uiso 1 1 calc R
C11 C 0.5823(4) 0.9561(3) 0.7493(3) 0.0348(8) Uani 1 1 d .
C12 C 0.7560(4) 0.9986(4) 0.8019(3) 0.0465(9) Uani 1 1 d .
H12A H 0.8050 1.1004 0.8140 0.070 Uiso 1 1 calc R
H12B H 0.8001 0.9532 0.7518 0.070 Uiso 1 1 calc R
H12C H 0.7757 0.9698 0.8742 0.070 Uiso 1 1 calc R
C13 C 0.5087(5) 1.0282(4) 0.8220(4) 0.0541(11) Uani 1 1 d .
H13A H 0.5613 1.1298 0.8362 0.081 Uiso 1 1 calc R
H13B H 0.5197 0.9975 0.8937 0.081 Uiso 1 1 calc R
H13C H 0.3976 1.0037 0.7829 0.081 Uiso 1 1 calc R
C14 C 0.5487(5) 0.9886(4) 0.6323(3) 0.0514(10) Uani 1 1 d .
H14A H 0.5986 1.0892 0.6377 0.077 Uiso 1 1 calc R
H14B H 0.4356 0.9610 0.5992 0.077 Uiso 1 1 calc R
H14C H 0.5902 0.9366 0.5847 0.077 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'
Si Si 0.0817 0.0704 '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'
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
N1 Cr1 Cl1 176.44(8) . .
N1 Cr1 Cl1 95.53(8) . 2_666
Cl1 Cr1 Cl1 85.75(3) . 2_666
N1 Cr1 S2 87.03(7) . .
Cl1 Cr1 S2 89.71(3) . .
Cl1 Cr1 S2 134.64(3) 2_666 .
N1 Cr1 S1 84.10(8) . .
Cl1 Cr1 S1 98.92(3) . .
Cl1 Cr1 S1 101.36(3) 2_666 .
S2 Cr1 S1 123.90(3) . .
Cr1 Cl1 Cr1 94.25(3) . 2_666
Si1 N1 Si2 124.08(15) . .
Si1 N1 Cr1 119.62(13) . .
Si2 N1 Cr1 115.41(14) . .
C1 S1 C7 106.18(15) . .
C1 S1 Cr1 92.17(12) . .
C7 S1 Cr1 120.24(11) . .
C2 S2 C11 104.80(16) . .
C2 S2 Cr1 100.76(11) . .
C11 S2 Cr1 109.62(11) . .
N1 Si1 C4 113.9(2) . .
N1 Si1 C3 113.51(18) . .
C4 Si1 C3 107.6(3) . .
N1 Si1 C1 107.25(14) . .
C4 Si1 C1 107.68(18) . .
C3 Si1 C1 106.49(19) . .
N1 Si2 C6 115.62(15) . .
N1 Si2 C5 112.40(15) . .
C6 Si2 C5 106.75(17) . .
N1 Si2 C2 107.12(14) . .
C6 Si2 C2 106.04(16) . .
C5 Si2 C2 108.57(17) . .
S1 C1 Si1 107.06(17) . .
S2 C2 Si2 113.43(16) . .
C8 C7 C9 110.3(3) . .
C8 C7 C10 110.4(3) . .
C9 C7 C10 111.1(3) . .
C8 C7 S1 110.6(2) . .
C9 C7 S1 104.8(2) . .
C10 C7 S1 109.6(2) . .
C12 C11 C13 111.6(3) . .
C12 C11 C14 110.3(3) . .
C13 C11 C14 110.1(3) . .
C12 C11 S2 112.1(2) . .
C13 C11 S2 108.6(2) . .
C14 C11 S2 103.8(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 N1 2.027(3) .
Cr1 Cl1 2.4118(9) .
Cr1 Cl1 2.5079(9) 2_666
Cr1 S2 2.5151(9) .
Cr1 S1 2.6466(9) .
Cl1 Cr1 2.5079(9) 2_666
N1 Si1 1.693(3) .
N1 Si2 1.700(3) .
S1 C1 1.801(4) .
S1 C7 1.845(3) .
S2 C2 1.813(3) .
S2 C11 1.860(3) .
Si1 C4 1.866(5) .
Si1 C3 1.878(5) .
Si1 C1 1.894(3) .
Si2 C6 1.869(3) .
Si2 C5 1.878(4) .
Si2 C2 1.906(4) .
C7 C8 1.526(4) .
C7 C9 1.530(5) .
C7 C10 1.535(5) .
C11 C12 1.507(5) .
C11 C13 1.523(5) .
C11 C14 1.525(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 Cr1 Cl1 Cr1 -111.2(13) . 2_666
Cl1 Cr1 Cl1 Cr1 0.0 2_666 2_666
S2 Cr1 Cl1 Cr1 -134.82(3) . 2_666
S1 Cr1 Cl1 Cr1 100.86(3) . 2_666
Cl1 Cr1 N1 Si1 -173.9(11) . .
Cl1 Cr1 N1 Si1 75.18(15) 2_666 .
S2 Cr1 N1 Si1 -150.25(15) . .
S1 Cr1 N1 Si1 -25.71(14) . .
Cl1 Cr1 N1 Si2 16.5(14) . .
Cl1 Cr1 N1 Si2 -94.44(13) 2_666 .
S2 Cr1 N1 Si2 40.13(13) . .
S1 Cr1 N1 Si2 164.66(14) . .
N1 Cr1 S1 C1 43.89(13) . .
Cl1 Cr1 S1 C1 -138.00(11) . .
Cl1 Cr1 S1 C1 -50.58(12) 2_666 .
S2 Cr1 S1 C1 126.29(12) . .
N1 Cr1 S1 C7 154.07(15) . .
Cl1 Cr1 S1 C7 -27.83(14) . .
Cl1 Cr1 S1 C7 59.59(14) 2_666 .
S2 Cr1 S1 C7 -123.54(13) . .
N1 Cr1 S2 C2 -27.50(15) . .
Cl1 Cr1 S2 C2 151.07(13) . .
Cl1 Cr1 S2 C2 67.34(13) 2_666 .
S1 Cr1 S2 C2 -108.36(13) . .
N1 Cr1 S2 C11 82.61(14) . .
Cl1 Cr1 S2 C11 -98.82(12) . .
Cl1 Cr1 S2 C11 177.45(12) 2_666 .
S1 Cr1 S2 C11 1.76(12) . .
Si2 N1 Si1 C4 49.3(3) . .
Cr1 N1 Si1 C4 -119.4(2) . .
Si2 N1 Si1 C3 -74.3(3) . .
Cr1 N1 Si1 C3 117.0(2) . .
Si2 N1 Si1 C1 168.35(18) . .
Cr1 N1 Si1 C1 -0.3(2) . .
Si1 N1 Si2 C6 33.6(2) . .
Cr1 N1 Si2 C6 -157.29(17) . .
Si1 N1 Si2 C5 -89.3(2) . .
Cr1 N1 Si2 C5 79.80(19) . .
Si1 N1 Si2 C2 151.53(19) . .
Cr1 N1 Si2 C2 -39.36(19) . .
C7 S1 C1 Si1 -174.07(16) . .
Cr1 S1 C1 Si1 -51.67(16) . .
N1 Si1 C1 S1 42.3(2) . .
C4 Si1 C1 S1 165.2(2) . .
C3 Si1 C1 S1 -79.6(2) . .
C11 S2 C2 Si2 -101.7(2) . .
Cr1 S2 C2 Si2 12.1(2) . .
N1 Si2 C2 S2 12.4(2) . .
C6 Si2 C2 S2 136.4(2) . .
C5 Si2 C2 S2 -109.2(2) . .
C1 S1 C7 C8 63.5(3) . .
Cr1 S1 C7 C8 -38.9(3) . .
C1 S1 C7 C9 -177.7(2) . .
Cr1 S1 C7 C9 79.9(2) . .
C1 S1 C7 C10 -58.4(3) . .
Cr1 S1 C7 C10 -160.8(2) . .
C2 S2 C11 C12 56.8(3) . .
Cr1 S2 C11 C12 -50.6(3) . .
C2 S2 C11 C13 -67.0(3) . .
Cr1 S2 C11 C13 -174.4(2) . .
C2 S2 C11 C14 175.8(2) . .
Cr1 S2 C11 C14 68.4(2) . .
