#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:13:35 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180030 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/24/7032492.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_7032492
loop_
_publ_author_name
'Pop, Alexandra'
'Wang, Lingfang'
'Dorcet, Vincent'
'Roisnel, Thierry'
'Carpentier, Jean-François'
'Silvestru, Anca'
'Sarazin, Yann'
_publ_section_title
;
 On the coordination chemistry of organochalcogenolates R(NMe2)^E(-) and
 R(NMe2)EO(-) (E = S, Se) onto lead(ii) and lighter divalent tetrel
 elements.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16459
_journal_page_last               16474
_journal_paper_doi               10.1039/c4dt02252a
_journal_volume                  43
_journal_year                    2014
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C38 H76 N4 O2 S2 Si4 Sn2'
_chemical_formula_sum            'C38 H76 N4 O2 S2 Si4 Sn2'
_chemical_formula_weight         1034.95
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                101.636(5)
_cell_angle_beta                 104.069(5)
_cell_angle_gamma                93.483(5)
_cell_formula_units_Z            1
_cell_length_a                   8.9518(9)
_cell_length_b                   10.6790(11)
_cell_length_c                   13.8023(15)
_cell_measurement_reflns_used    6710
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      2.36
_cell_measurement_wavelength     0.71073
_cell_volume                     1245.2(2)
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2006)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2006)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2006)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
;
           WinGX publication routines (Farrugia, 2012),
           CRYSCAL (T. Roisnel, local program)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15449
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.1
_exptl_absorpt_coefficient_mu    1.217
_exptl_absorpt_correction_T_max  0.794
_exptl_absorpt_correction_T_min  0.694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.38
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.19
_refine_diff_density_max         2.92
_refine_diff_density_min         -1.557
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.193
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         5620
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.193
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0507
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+16.4656P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1481
_refine_ls_wR_factor_ref         0.1493
_reflns_number_gt                5289
_reflns_number_total             5620
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt02252a2.cif
_cod_data_source_block           9
_cod_depositor_comments
'Adding full bibliography for 7032488--7032503.cif.'
_cod_database_code               7032492
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
Sn1 Sn 0.15785(5) 0.07751(4) 0.10660(3) 0.01452(12) Uani 1 1 d .
S1 S 0.17551(18) 0.39266(15) 0.10762(11) 0.0206(3) Uani 1 1 d .
O1 O -0.0383(5) 0.1133(4) -0.0078(3) 0.0173(8) Uani 1 1 d .
C2 C -0.0756(7) 0.2353(6) -0.0327(5) 0.0203(12) Uani 1 1 d .
C3 C -0.2502(8) 0.2272(6) -0.0752(5) 0.0265(14) Uani 1 1 d .
H3A H -0.2836 0.1597 -0.1383 0.04 Uiso 1 1 calc R
H3B H -0.2774 0.31 -0.0903 0.04 Uiso 1 1 calc R
H3C H -0.3021 0.2067 -0.0246 0.04 Uiso 1 1 calc R
C4 C 0.0057(8) 0.2643(6) -0.1118(5) 0.0249(13) Uani 1 1 d .
H4A H 0.1115 0.2407 -0.0953 0.037 Uiso 1 1 calc R
H4B H 0.0092 0.3564 -0.1111 0.037 Uiso 1 1 calc R
H4C H -0.0513 0.2145 -0.18 0.037 Uiso 1 1 calc R
C5 C -0.0315(7) 0.3424(6) 0.0665(5) 0.0197(12) Uani 1 1 d .
H5A H -0.0643 0.3105 0.1215 0.024 Uiso 1 1 calc R
H5B H -0.0872 0.4174 0.0544 0.024 Uiso 1 1 calc R
C6 C 0.2078(7) 0.4735(6) 0.2376(5) 0.0196(12) Uani 1 1 d .
C7 C 0.0888(8) 0.5090(6) 0.2827(5) 0.0239(13) Uani 1 1 d .
H7 H -0.0158 0.4898 0.2427 0.029 Uiso 1 1 calc R
C8 C 0.1208(9) 0.5724(7) 0.3860(5) 0.0294(15) Uani 1 1 d .
H8 H 0.0388 0.5955 0.4162 0.035 Uiso 1 1 calc R
C9 C 0.2732(10) 0.6011(7) 0.4435(5) 0.0348(17) Uani 1 1 d .
H9 H 0.2965 0.6444 0.5136 0.042 Uiso 1 1 calc R
C10 C 0.3921(8) 0.5666(7) 0.3988(6) 0.0310(15) Uani 1 1 d .
H10 H 0.4963 0.587 0.4394 0.037 Uiso 1 1 calc R
C11 C 0.3639(8) 0.5034(6) 0.2970(5) 0.0236(13) Uani 1 1 d .
C12 C 0.4953(8) 0.4653(7) 0.2499(5) 0.0271(14) Uani 1 1 d .
H12A H 0.5925 0.4768 0.3051 0.033 Uiso 1 1 calc R
H12B H 0.4738 0.3731 0.2151 0.033 Uiso 1 1 calc R
N13 N 0.5165(6) 0.5412(6) 0.1762(5) 0.0285(13) Uani 1 1 d .
C14A C 0.6148(9) 0.4787(10) 0.1149(7) 0.047(2) Uani 1 1 d .
H14A H 0.6291 0.5294 0.0654 0.07 Uiso 1 1 calc R
H14B H 0.5653 0.3921 0.0782 0.07 Uiso 1 1 calc R
H14C H 0.7159 0.4727 0.16 0.07 Uiso 1 1 calc R
C15A C 0.5855(10) 0.6707(8) 0.2276(7) 0.043(2) Uani 1 1 d .
H15A H 0.5243 0.709 0.2735 0.064 Uiso 1 1 calc R
H15B H 0.5874 0.7223 0.1766 0.064 Uiso 1 1 calc R
H15C H 0.6917 0.6686 0.2675 0.064 Uiso 1 1 calc R
N1 N 0.0666(6) 0.0802(5) 0.2374(4) 0.0183(10) Uani 1 1 d .
Si1 Si -0.1228(2) 0.07385(17) 0.24861(13) 0.0212(4) Uani 1 1 d .
Si2 Si 0.2146(2) 0.09447(18) 0.34871(13) 0.0224(4) Uani 1 1 d .
C21 C -0.2750(8) 0.0032(8) 0.1262(5) 0.0308(15) Uani 1 1 d .
H21A H -0.2691 0.0546 0.0757 0.046 Uiso 1 1 calc R
H21B H -0.3777 0.0036 0.1394 0.046 Uiso 1 1 calc R
H21C H -0.2576 -0.0854 0.0998 0.046 Uiso 1 1 calc R
C22 C -0.1552(9) -0.0266(8) 0.3405(5) 0.0323(16) Uani 1 1 d .
H22A H -0.1257 -0.1128 0.3194 0.049 Uiso 1 1 calc R
H22B H -0.265 -0.0333 0.3403 0.049 Uiso 1 1 calc R
H22C H -0.0919 0.014 0.4096 0.049 Uiso 1 1 calc R
C23 C -0.1793(9) 0.2379(7) 0.2973(6) 0.0352(17) Uani 1 1 d .
H23A H -0.0973 0.2847 0.3568 0.053 Uiso 1 1 calc R
H23B H -0.2765 0.2278 0.3172 0.053 Uiso 1 1 calc R
H23C H -0.1934 0.2862 0.2431 0.053 Uiso 1 1 calc R
C24 C 0.2409(10) -0.0637(7) 0.3879(6) 0.0365(17) Uani 1 1 d .
H24A H 0.1483 -0.0934 0.4066 0.055 Uiso 1 1 calc R
H24B H 0.3314 -0.0522 0.4469 0.055 Uiso 1 1 calc R
H24C H 0.2569 -0.1277 0.3307 0.055 Uiso 1 1 calc R
C25 C 0.1862(10) 0.2151(8) 0.4606(6) 0.0392(18) Uani 1 1 d .
H25A H 0.1837 0.3002 0.4443 0.059 Uiso 1 1 calc R
H25B H 0.272 0.2184 0.521 0.059 Uiso 1 1 calc R
H25C H 0.0881 0.1895 0.4748 0.059 Uiso 1 1 calc R
C26 C 0.4099(9) 0.1506(9) 0.3343(6) 0.0383(18) Uani 1 1 d .
H26A H 0.4428 0.0829 0.2873 0.057 Uiso 1 1 calc R
H26B H 0.4857 0.1699 0.4014 0.057 Uiso 1 1 calc R
H26C H 0.4028 0.2284 0.3067 0.057 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 0 '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 0.006 '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'
Sn Sn -0.6537 1.4246 '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_3
N1 Sn1 O1 103.09(18) .
N1 Sn1 O1 99.46(17) 2
O1 Sn1 O1 71.78(17) 2
C6 S1 C5 103.9(3) .
C2 O1 Sn1 128.1(3) .
C2 O1 Sn1 122.8(3) 2
Sn1 O1 Sn1 108.22(17) 2
O1 C2 C3 108.6(5) .
O1 C2 C4 110.3(5) .
C3 C2 C4 109.8(5) .
O1 C2 C5 109.4(5) .
C3 C2 C5 106.6(5) .
C4 C2 C5 112.0(5) .
C2 C3 H3A 109.5 .
C2 C3 H3B 109.5 .
H3A C3 H3B 109.5 .
C2 C3 H3C 109.5 .
H3A C3 H3C 109.5 .
H3B C3 H3C 109.5 .
C2 C4 H4A 109.5 .
C2 C4 H4B 109.5 .
H4A C4 H4B 109.5 .
C2 C4 H4C 109.5 .
H4A C4 H4C 109.5 .
H4B C4 H4C 109.5 .
C2 C5 S1 111.6(4) .
C2 C5 H5A 109.3 .
S1 C5 H5A 109.3 .
C2 C5 H5B 109.3 .
S1 C5 H5B 109.3 .
H5A C5 H5B 108 .
C7 C6 C11 119.4(6) .
C7 C6 S1 123.4(5) .
C11 C6 S1 117.2(5) .
C6 C7 C8 121.1(6) .
C6 C7 H7 119.5 .
C8 C7 H7 119.5 .
C9 C8 C7 119.2(7) .
C9 C8 H8 120.4 .
C7 C8 H8 120.4 .
C8 C9 C10 120.0(7) .
C8 C9 H9 120 .
C10 C9 H9 120 .
C11 C10 C9 122.1(7) .
C11 C10 H10 119 .
C9 C10 H10 119 .
C10 C11 C6 118.3(6) .
C10 C11 C12 121.3(6) .
C6 C11 C12 120.4(6) .
N13 C12 C11 112.5(6) .
N13 C12 H12A 109.1 .
C11 C12 H12A 109.1 .
N13 C12 H12B 109.1 .
C11 C12 H12B 109.1 .
H12A C12 H12B 107.8 .
C15A N13 C12 111.0(6) .
C15A N13 C14A 110.0(7) .
C12 N13 C14A 109.4(6) .
N13 C14A H14A 109.5 .
N13 C14A H14B 109.5 .
H14A C14A H14B 109.5 .
N13 C14A H14C 109.5 .
H14A C14A H14C 109.5 .
H14B C14A H14C 109.5 .
N13 C15A H15A 109.5 .
N13 C15A H15B 109.5 .
H15A C15A H15B 109.5 .
N13 C15A H15C 109.5 .
H15A C15A H15C 109.5 .
H15B C15A H15C 109.5 .
Si1 N1 Si2 117.5(3) .
Si1 N1 Sn1 131.2(3) .
Si2 N1 Sn1 111.3(3) .
N1 Si1 C21 114.9(3) .
N1 Si1 C22 112.2(3) .
C21 Si1 C22 105.0(3) .
N1 Si1 C23 112.7(3) .
C21 Si1 C23 105.2(4) .
C22 Si1 C23 106.0(4) .
N1 Si2 C25 113.1(3) .
N1 Si2 C26 112.8(3) .
C25 Si2 C26 104.9(4) .
N1 Si2 C24 112.7(3) .
C25 Si2 C24 108.3(4) .
C26 Si2 C24 104.5(4) .
Si1 C21 H21A 109.5 .
Si1 C21 H21B 109.5 .
H21A C21 H21B 109.5 .
Si1 C21 H21C 109.5 .
H21A C21 H21C 109.5 .
H21B C21 H21C 109.5 .
Si1 C22 H22A 109.5 .
Si1 C22 H22B 109.5 .
H22A C22 H22B 109.5 .
Si1 C22 H22C 109.5 .
H22A C22 H22C 109.5 .
H22B C22 H22C 109.5 .
Si1 C23 H23A 109.5 .
Si1 C23 H23B 109.5 .
H23A C23 H23B 109.5 .
Si1 C23 H23C 109.5 .
H23A C23 H23C 109.5 .
H23B C23 H23C 109.5 .
Si2 C24 H24A 109.5 .
Si2 C24 H24B 109.5 .
H24A C24 H24B 109.5 .
Si2 C24 H24C 109.5 .
H24A C24 H24C 109.5 .
H24B C24 H24C 109.5 .
Si2 C25 H25A 109.5 .
Si2 C25 H25B 109.5 .
H25A C25 H25B 109.5 .
Si2 C25 H25C 109.5 .
H25A C25 H25C 109.5 .
H25B C25 H25C 109.5 .
Si2 C26 H26A 109.5 .
Si2 C26 H26B 109.5 .
H26A C26 H26B 109.5 .
Si2 C26 H26C 109.5 .
H26A C26 H26C 109.5 .
H26B C26 H26C 109.5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 N1 2.150(5) .
Sn1 O1 2.168(4) .
Sn1 O1 2.250(4) 2
S1 C6 1.772(6) .
S1 C5 1.813(6) .
O1 C2 1.450(7) .
O1 Sn1 2.250(4) 2
C2 C3 1.521(9) .
C2 C4 1.521(9) .
C2 C5 1.546(8) .
C3 H3A 0.98 .
C3 H3B 0.98 .
C3 H3C 0.98 .
C4 H4A 0.98 .
C4 H4B 0.98 .
C4 H4C 0.98 .
C5 H5A 0.99 .
C5 H5B 0.99 .
C6 C7 1.394(9) .
C6 C11 1.417(9) .
C7 C8 1.402(9) .
C7 H7 0.95 .
C8 C9 1.381(11) .
C8 H8 0.95 .
C9 C10 1.387(11) .
C9 H9 0.95 .
C10 C11 1.385(10) .
C10 H10 0.95 .
C11 C12 1.514(9) .
C12 N13 1.462(9) .
C12 H12A 0.99 .
C12 H12B 0.99 .
N13 C15A 1.443(10) .
N13 C14A 1.464(10) .
C14A H14A 0.98 .
C14A H14B 0.98 .
C14A H14C 0.98 .
C15A H15A 0.98 .
C15A H15B 0.98 .
C15A H15C 0.98 .
N1 Si1 1.738(5) .
N1 Si2 1.741(5) .
Si1 C21 1.876(7) .
Si1 C22 1.879(7) .
Si1 C23 1.891(8) .
Si2 C25 1.880(8) .
Si2 C26 1.883(8) .
Si2 C24 1.886(8) .
C21 H21A 0.98 .
C21 H21B 0.98 .
C21 H21C 0.98 .
C22 H22A 0.98 .
C22 H22B 0.98 .
C22 H22C 0.98 .
C23 H23A 0.98 .
C23 H23B 0.98 .
C23 H23C 0.98 .
C24 H24A 0.98 .
C24 H24B 0.98 .
C24 H24C 0.98 .
C25 H25A 0.98 .
C25 H25B 0.98 .
C25 H25C 0.98 .
C26 H26A 0.98 .
C26 H26B 0.98 .
C26 H26C 0.98 .
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 Sn1 O1 C2 94.8(5) . .
O1 Sn1 O1 C2 -169.4(5) 2 .
N1 Sn1 O1 Sn1 -95.8(2) . 2
O1 Sn1 O1 Sn1 0 2 2
Sn1 O1 C2 C3 -152.6(4) . .
Sn1 O1 C2 C3 39.4(6) 2 .
Sn1 O1 C2 C4 87.0(6) . .
Sn1 O1 C2 C4 -81.0(6) 2 .
Sn1 O1 C2 C5 -36.6(7) . .
Sn1 O1 C2 C5 155.4(4) 2 .
O1 C2 C5 S1 77.9(5) . .
C3 C2 C5 S1 -164.8(4) . .
C4 C2 C5 S1 -44.7(6) . .
C6 S1 C5 C2 -162.2(4) . .
C5 S1 C6 C7 -12.0(6) . .
C5 S1 C6 C11 168.4(5) . .
C11 C6 C7 C8 -0.7(10) . .
S1 C6 C7 C8 179.8(5) . .
C6 C7 C8 C9 0.6(11) . .
C7 C8 C9 C10 -0.2(11) . .
C8 C9 C10 C11 0.0(12) . .
C9 C10 C11 C6 -0.1(11) . .
C9 C10 C11 C12 -179.4(7) . .
C7 C6 C11 C10 0.4(9) . .
S1 C6 C11 C10 180.0(5) . .
C7 C6 C11 C12 179.7(6) . .
S1 C6 C11 C12 -0.7(8) . .
C10 C11 C12 N13 -110.0(7) . .
C6 C11 C12 N13 70.7(8) . .
C11 C12 N13 C15A 73.2(7) . .
C11 C12 N13 C14A -165.2(6) . .
O1 Sn1 N1 Si1 13.9(4) . .
O1 Sn1 N1 Si1 -59.5(4) 2 .
O1 Sn1 N1 Si2 -164.7(2) . .
O1 Sn1 N1 Si2 121.9(3) 2 .
Si2 N1 Si1 C21 -159.9(3) . .
Sn1 N1 Si1 C21 21.5(5) . .
Si2 N1 Si1 C22 -40.1(4) . .
Sn1 N1 Si1 C22 141.3(4) . .
Si2 N1 Si1 C23 79.5(4) . .
Sn1 N1 Si1 C23 -99.0(4) . .
Si1 N1 Si2 C25 -43.6(5) . .
Sn1 N1 Si2 C25 135.2(3) . .
Si1 N1 Si2 C26 -162.4(4) . .
Sn1 N1 Si2 C26 16.5(4) . .
Si1 N1 Si2 C24 79.6(4) . .
Sn1 N1 Si2 C24 -101.5(4) . .
