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#$Date: 2015-09-05 20:45:30 +0300 (Sat, 05 Sep 2015) $
#$Revision: 154499 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/62/4086228.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_4086228
loop_
_publ_author_name
'Bayram, Melike'
'Bläser, Dieter'
'Wölper, Christoph'
'Schulz, Stephan'
_publ_contact_author
;
         Prof. Dr. Schulz, Stephan
         Fachbereich Chemie der
         Universität Duisburg-Essen
         Campus Essen, Universitätsstr. 7
         D-45141 Essen, Germany
;
_publ_section_title
;
 Synthesis and X-ray Crystal Structure of Diimidosulfinate Transition
 Metal Complexes
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3421
_journal_paper_doi               10.1021/acs.organomet.5b00407
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C22 H58 Li2 N4 O2 S2 Si4'
_chemical_formula_weight         601.08
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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-2014/7
_cell_angle_alpha                62.694(2)
_cell_angle_beta                 73.265(2)
_cell_angle_gamma                67.081(2)
_cell_formula_units_Z            1
_cell_length_a                   9.9253(5)
_cell_length_b                   10.4660(5)
_cell_length_c                   10.4830(5)
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      30.53
_cell_measurement_theta_min      2.25
_cell_volume                     883.24(8)
_computing_cell_refinement       'BRUKER D8 KAPPA APEX 2 (3.0-2009)'
_computing_data_collection       'BRUKER D8 KAPPA APEX 2 (3.0-2009)'
_computing_data_reduction        'BRUKER D8 KAPPA APEX 2 (3.0-2009)'
_computing_molecular_graphics    'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_publication_material  'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'BRUKER D8 KAPPA APEX 2 (3.0-2009)'
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type
; 
 Bruker D8 KAPPA series II with APEX II area detector system
;
_diffrn_measurement_method
;
 Data collection strategy APEX 2/COSMO
;
_diffrn_radiation_monochromator  'Triumph Goebel mirror'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            23655
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.566
_diffrn_reflns_theta_min         2.206
_exptl_absorpt_coefficient_mu    0.310
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 BRUKER AXS SMART APEX 2 Vers. 3.0-2009
 R.H. Blessing, Acta Cryst. (1995) A51 33-38 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.130
_exptl_crystal_description       block
_exptl_crystal_F_000             328
_exptl_crystal_size_max          0.266
_exptl_crystal_size_mid          0.216
_exptl_crystal_size_min          0.124
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         5227
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0238
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0313P)²+0.2620P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0645
_refine_ls_wR_factor_ref         0.0676
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4643
_reflns_number_total             5227
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            om5b00407_si_002.cif
_cod_data_source_block           mb_158m
_cod_database_code               4086228
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.922
_shelx_estimated_absorpt_t_max   0.963
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
S1 S 0.78952(2) 0.43774(2) -0.00526(2) 0.01232(5) Uani 1 1 d . .
Si1 Si 0.72055(3) 0.49361(3) -0.27743(3) 0.01260(6) Uani 1 1 d . .
Si2 Si 0.83553(3) 0.21355(3) 0.28389(3) 0.01411(6) Uani 1 1 d . .
O1 O 0.56254(7) 0.15415(7) 0.08866(8) 0.01816(14) Uani 1 1 d . .
N1 N 0.66322(8) 0.49479(8) -0.10522(8) 0.01297(14) Uani 1 1 d . .
N2 N 0.72428(8) 0.33726(9) 0.15223(8) 0.01399(14) Uani 1 1 d . .
C1 C 0.91316(10) 0.36780(11) -0.29849(11) 0.01972(18) Uani 1 1 d . .
H1A H 0.9371 0.3654 -0.3950 0.030 Uiso 1 1 calc R U
H1B H 0.9209 0.2656 -0.2246 0.030 Uiso 1 1 calc R U
H1C H 0.9824 0.4065 -0.2869 0.030 Uiso 1 1 calc R U
C2 C 0.59084(11) 0.42962(12) -0.31598(11) 0.02149(19) Uani 1 1 d . .
H2A H 0.4893 0.4921 -0.3002 0.032 Uiso 1 1 calc R U
H2B H 0.6002 0.3239 -0.2512 0.032 Uiso 1 1 calc R U
H2C H 0.6149 0.4392 -0.4168 0.032 Uiso 1 1 calc R U
C3 C 0.71415(11) 0.68764(11) -0.41759(10) 0.02147(19) Uani 1 1 d . .
H3A H 0.7478 0.6840 -0.5137 0.032 Uiso 1 1 calc R U
H3B H 0.7786 0.7257 -0.3980 0.032 Uiso 1 1 calc R U
H3C H 0.6127 0.7548 -0.4144 0.032 Uiso 1 1 calc R U
C4 C 0.72090(12) 0.10540(13) 0.44022(11) 0.0246(2) Uani 1 1 d . .
H4A H 0.6785 0.0570 0.4074 0.037 Uiso 1 1 calc R U
H4B H 0.6412 0.1744 0.4799 0.037 Uiso 1 1 calc R U
H4C H 0.7828 0.0281 0.5154 0.037 Uiso 1 1 calc R U
C5 C 1.00178(11) 0.07828(12) 0.22316(12) 0.02234(19) Uani 1 1 d . .
H5A H 0.9697 0.0166 0.1974 0.034 Uiso 1 1 calc R U
H5B H 1.0625 0.0127 0.3019 0.034 Uiso 1 1 calc R U
H5C H 1.0598 0.1350 0.1385 0.034 Uiso 1 1 calc R U
C6 C 0.90684(12) 0.30971(13) 0.35160(11) 0.0232(2) Uani 1 1 d . .
H6A H 0.9766 0.3581 0.2750 0.035 Uiso 1 1 calc R U
H6B H 0.9570 0.2350 0.4362 0.035 Uiso 1 1 calc R U
H6C H 0.8242 0.3862 0.3790 0.035 Uiso 1 1 calc R U
C7 C 0.77240(11) 0.60675(11) 0.01287(11) 0.01975(18) Uani 1 1 d . .
H7A H 0.7978 0.6812 -0.0823 0.030 Uiso 1 1 calc R U
H7B H 0.8395 0.5826 0.0789 0.030 Uiso 1 1 calc R U
H7C H 0.6706 0.6484 0.0518 0.030 Uiso 1 1 calc R U
C8 C 0.70705(10) 0.07167(10) 0.03824(10) 0.01798(17) Uani 1 1 d . .
H8A H 0.7831 0.1146 0.0314 0.022 Uiso 1 1 calc R U
H8B H 0.7082 0.0757 -0.0583 0.022 Uiso 1 1 calc R U
C9 C 0.73542(11) -0.08923(11) 0.14982(11) 0.02007(18) Uani 1 1 d . .
H9A H 0.7768 -0.1031 0.2323 0.024 Uiso 1 1 calc R U
H9B H 0.8031 -0.1620 0.1066 0.024 Uiso 1 1 calc R U
C10 C 0.58033(11) -0.10536(11) 0.19618(11) 0.01987(18) Uani 1 1 d . .
H10A H 0.5519 -0.1249 0.1252 0.024 Uiso 1 1 calc R U
H10B H 0.5722 -0.1873 0.2930 0.024 Uiso 1 1 calc R U
C11 C 0.48738(11) 0.04783(11) 0.19914(11) 0.02148(19) Uani 1 1 d . .
H11A H 0.3868 0.0745 0.1777 0.026 Uiso 1 1 calc R U
H11B H 0.4796 0.0477 0.2955 0.026 Uiso 1 1 calc R U
Li1 Li 0.54515(18) 0.35360(18) 0.08102(18) 0.0165(3) Uani 1 1 d . .
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'
Li Li -0.0003 0.0001 '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'
O O 0.0106 0.0060 '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'
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
N2 S1 N1 103.94(4) . .
N2 S1 C7 103.62(4) . .
N1 S1 C7 102.83(4) . .
N2 S1 Li1 49.58(4) . .
N1 S1 Li1 54.60(4) . .
C7 S1 Li1 115.91(5) . .
N1 Si1 C2 108.42(4) . .
N1 Si1 C1 112.92(4) . .
C2 Si1 C1 109.34(5) . .
N1 Si1 C3 110.95(4) . .
C2 Si1 C3 107.63(5) . .
C1 Si1 C3 107.44(5) . .
N2 Si2 C4 107.06(4) . .
N2 Si2 C6 113.07(4) . .
C4 Si2 C6 107.44(5) . .
N2 Si2 C5 113.28(4) . .
C4 Si2 C5 109.37(5) . .
C6 Si2 C5 106.47(5) . .
C8 O1 C11 109.15(7) . .
C8 O1 Li1 115.98(7) . .
C11 O1 Li1 126.28(7) . .
S1 N1 Si1 117.58(4) . .
S1 N1 Li1 123.27(6) . 2_665
Si1 N1 Li1 114.30(6) . 2_665
S1 N1 Li1 88.11(5) . .
Si1 N1 Li1 128.50(6) . .
Li1 N1 Li1 76.79(7) 2_665 .
S1 N2 Si2 121.19(5) . .
S1 N2 Li1 93.64(6) . .
Si2 N2 Li1 139.13(6) . .
O1 C8 C9 105.57(7) . .
C8 C9 C10 101.60(8) . .
C11 C10 C9 101.87(8) . .
O1 C11 C10 105.95(8) . .
O1 Li1 N2 109.80(8) . .
O1 Li1 N1 119.97(8) . 2_665
N2 Li1 N1 122.88(8) . 2_665
O1 Li1 N1 117.99(8) . .
N2 Li1 N1 73.94(6) . .
N1 Li1 N1 103.21(7) 2_665 .
O1 Li1 Li1 141.19(11) . 2_665
N2 Li1 Li1 101.56(9) . 2_665
N1 Li1 Li1 53.12(6) 2_665 2_665
N1 Li1 Li1 50.09(6) . 2_665
O1 Li1 S1 117.94(7) . .
N2 Li1 S1 36.79(3) . .
N1 Li1 S1 121.25(7) 2_665 .
N1 Li1 S1 37.29(3) . .
Li1 Li1 S1 75.82(7) 2_665 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S1 N2 1.6039(8) .
S1 N1 1.6202(8) .
S1 C7 1.8027(10) .
S1 Li1 2.6730(16) .
Si1 N1 1.7339(8) .
Si1 C2 1.8678(10) .
Si1 C1 1.8710(10) .
Si1 C3 1.8715(10) .
Si2 N2 1.7103(8) .
Si2 C4 1.8678(10) .
Si2 C6 1.8753(10) .
Si2 C5 1.8801(10) .
O1 C8 1.4490(11) .
O1 C11 1.4501(11) .
O1 Li1 1.9919(17) .
N1 Li1 2.0906(18) 2_665
N1 Li1 2.1800(17) .
N2 Li1 2.0390(18) .
C8 C9 1.5154(13) .
C9 C10 1.5266(14) .
C10 C11 1.5165(14) .
Li1 N1 2.0906(18) 2_665
Li1 Li1 2.653(3) 2_665
