#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:00:39 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178881 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/10/4111080.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_4111080
loop_
_publ_author_name
'Eric Block'
'Evgeny V. Dikarev'
'Richard S. Glass'
'Jin Jin'
'Bo Li'
'Xiaojie Li'
'Shao-Zhong Zhang'
_publ_section_title
;
 Synthesis, Structure, and Chemistry of New, Mixed Group 14 and 16
 Heterocycles: Nucleophile-Induced Ring Contraction of Mesocyclic
 Dications
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14949
_journal_page_last               14961
_journal_paper_doi               10.1021/ja065037j
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'S2 (C H2)4 (Si (C H3)2)2'
_chemical_formula_sum            'C8 H20 S2 Si2'
_chemical_formula_weight         236.54
_chemical_name_systematic
; 
 3,3,7,7-Tetramethyl-1,5-dithia-3,7-disilocane  
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.9700(10)
_cell_angle_beta                 95.8430(10)
_cell_angle_gamma                106.3500(10)
_cell_formula_units_Z            2
_cell_length_a                   6.6704(5)
_cell_length_b                   9.8045(7)
_cell_length_c                   10.8940(7)
_cell_measurement_reflns_used    4760
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.21
_cell_volume                     667.27(8)
_computing_cell_refinement       'SMART, SAINT'
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXP-93 (Sheldrick, 1993)'
_computing_publication_material  'SHELXCIF-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.904
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '0.3 deg wide ω exposures'
_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  0.0150
_diffrn_reflns_av_sigmaI/netI    0.0206
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5829
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count na
_diffrn_standards_interval_time  na
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.536
_exptl_absorpt_correction_T_max  0.9533
_exptl_absorpt_correction_T_min  0.8776
_exptl_absorpt_correction_type   'multi-scan (SADABS)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             256
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         2987
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0428P)²+0.1721P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0821
_reflns_number_gt                2760
_reflns_number_total             2987
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja065037jsi20060721_015422.cif
_cod_data_source_block           S2Si2C8H20_25a
_cod_database_code               4111080
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
S1 S 0.20738(7) 0.23210(4) 0.59144(4) 0.04548(13) Uani 1 1 d
S2 S 0.67765(6) 0.20198(4) 0.93507(4) 0.04472(13) Uani 1 1 d
Si2 Si 0.26720(6) -0.00580(4) 0.74715(3) 0.02867(11) Uani 1 1 d
Si1 Si 0.65545(6) 0.41888(4) 0.75240(3) 0.03010(11) Uani 1 1 d
C1 C 0.3586(2) 0.37286(16) 0.72248(14) 0.0356(3) Uani 1 1 d
C2 C 0.7560(2) 0.26964(16) 0.79616(14) 0.0351(3) Uani 1 1 d
C3 C 0.3933(2) 0.12388(15) 0.89944(13) 0.0334(3) Uani 1 1 d
C4 C 0.3026(2) 0.07780(16) 0.60320(13) 0.0363(3) Uani 1 1 d
C5 C 0.7639(4) 0.4665(2) 0.60900(18) 0.0536(4) Uani 1 1 d
C6 C 0.7473(3) 0.57372(19) 0.88820(18) 0.0503(4) Uani 1 1 d
C7 C 0.3778(3) -0.16050(18) 0.72807(18) 0.0445(4) Uani 1 1 d
C8 C -0.0191(2) -0.06840(19) 0.75790(19) 0.0435(4) Uani 1 1 d
H1A H 0.300(3) 0.3629(19) 0.7983(17) 0.042(4) Uiso 1 1 d
H1B H 0.339(3) 0.457(2) 0.7004(18) 0.053(5) Uiso 1 1 d
H2A H 0.743(3) 0.193(2) 0.7276(17) 0.045(5) Uiso 1 1 d
H2B H 0.909(3) 0.314(2) 0.8217(17) 0.050(5) Uiso 1 1 d
H3A H 0.327(3) 0.198(2) 0.9119(16) 0.044(5) Uiso 1 1 d
H3B H 0.361(3) 0.0679(19) 0.9653(17) 0.045(5) Uiso 1 1 d
H4A H 0.444(3) 0.1002(19) 0.5844(17) 0.048(5) Uiso 1 1 d
H4B H 0.212(3) 0.002(2) 0.5322(18) 0.056(5) Uiso 1 1 d
H5A H 0.718(4) 0.393(3) 0.544(3) 0.088(8) Uiso 1 1 d
H5B H 0.735(4) 0.547(3) 0.585(2) 0.092(8) Uiso 1 1 d
H5C H 0.912(5) 0.490(3) 0.616(2) 0.095(8) Uiso 1 1 d
H6A H 0.694(4) 0.648(3) 0.874(2) 0.090(8) Uiso 1 1 d
H6B H 0.881(4) 0.612(2) 0.899(2) 0.069(7) Uiso 1 1 d
H6C H 0.698(3) 0.542(2) 0.961(2) 0.066(6) Uiso 1 1 d
H7A H 0.513(4) -0.134(3) 0.720(2) 0.091(8) Uiso 1 1 d
H7B H 0.360(4) -0.214(3) 0.789(2) 0.085(8) Uiso 1 1 d
H7C H 0.310(4) -0.227(3) 0.656(2) 0.081(7) Uiso 1 1 d
H8A H -0.041(3) -0.106(3) 0.829(2) 0.077(7) Uiso 1 1 d
H8B H -0.095(4) -0.138(3) 0.687(2) 0.084(7) Uiso 1 1 d
H8C H -0.076(4) 0.010(3) 0.765(2) 0.083(7) Uiso 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'
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_publ_flag
C1 S1 C4 105.51(7) y
C1 S1 S2 51.00(5) y
C4 S1 S2 55.12(5) y
C3 S2 C2 105.15(7) y
C3 S2 S1 51.08(5) y
C2 S2 S1 54.86(5) y
C8 Si2 C7 110.92(8) y
C8 Si2 C3 105.22(8) y
C7 Si2 C3 110.64(8) y
C8 Si2 C4 108.82(8) y
C7 Si2 C4 107.17(8) y
C3 Si2 C4 114.09(6) y
C5 Si1 C6 112.07(10) y
C5 Si1 C2 107.58(9) y
C6 Si1 C2 107.43(8) y
C5 Si1 C1 109.34(9) y
C6 Si1 C1 105.83(9) y
C2 Si1 C1 114.67(7) y
S1 C1 Si1 119.87(8) y
S1 C1 H1A 111.9(11) n
Si1 C1 H1A 111.2(10) n
S1 C1 H1B 103.5(12) n
Si1 C1 H1B 102.3(12) n
H1A C1 H1B 106.3(15) n
S2 C2 Si1 117.46(8) y
S2 C2 H2A 112.0(11) n
Si1 C2 H2A 114.1(11) n
S2 C2 H2B 101.7(10) n
Si1 C2 H2B 105.3(11) n
H2A C2 H2B 104.3(15) n
S2 C3 Si2 120.47(8) y
S2 C3 H3A 110.1(11) n
Si2 C3 H3A 110.0(11) n
S2 C3 H3B 102.7(10) n
Si2 C3 H3B 105.6(11) n
H3A C3 H3B 106.7(14) n
S1 C4 Si2 118.36(8) y
S1 C4 H4A 108.6(11) n
Si2 C4 H4A 113.7(11) n
S1 C4 H4B 103.1(11) n
Si2 C4 H4B 105.2(11) n
H4A C4 H4B 106.7(15) n
Si1 C5 H5A 111.9(17) n
Si1 C5 H5B 114.1(16) n
H5A C5 H5B 108(2) n
Si1 C5 H5C 114.4(16) n
H5A C5 H5C 103(2) n
H5B C5 H5C 104(2) n
Si1 C6 H6A 111.3(16) n
Si1 C6 H6B 111.9(15) n
H6A C6 H6B 104(2) n
Si1 C6 H6C 109.0(13) n
H6A C6 H6C 108(2) n
H6B C6 H6C 113(2) n
Si2 C7 H7A 112.5(17) n
Si2 C7 H7B 115.0(16) n
H7A C7 H7B 109(2) n
Si2 C7 H7C 110.9(15) n
H7A C7 H7C 106(2) n
H7B C7 H7C 103(2) n
Si2 C8 H8A 110.9(14) n
Si2 C8 H8B 111.6(15) n
H8A C8 H8B 109(2) n
Si2 C8 H8C 110.7(15) n
H8A C8 H8C 105.5(19) n
H8B C8 H8C 109(2) n
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
S1 C1 1.8081(15) y
S1 C4 1.8147(16) y
S1 S2 4.7347(6) y
S2 C3 1.8093(15) y
S2 C2 1.8116(15) y
Si2 C8 1.8561(16) y
Si2 C7 1.8576(16) y
Si2 C3 1.8795(14) y
Si2 C4 1.8852(15) y
Si1 C5 1.8572(17) y
Si1 C6 1.8601(17) y
Si1 C2 1.8769(15) y
Si1 C1 1.8840(15) y
C1 H1A 0.957(18) n
C1 H1B 0.93(2) n
C2 H2A 0.950(19) n
C2 H2B 0.979(19) n
C3 H3A 0.948(18) n
C3 H3B 0.974(18) n
C4 H4A 0.960(18) n
C4 H4B 0.99(2) n
C5 H5A 0.89(3) n
C5 H5B 0.93(3) n
C5 H5C 0.94(3) n
C6 H6A 0.92(3) n
C6 H6B 0.85(2) n
C6 H6C 0.95(2) n
C7 H7A 0.88(3) n
C7 H7B 0.90(3) n
C7 H7C 0.92(3) n
C8 H8A 0.91(2) n
C8 H8B 0.94(3) n
C8 H8C 0.94(3) n
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_publ_flag
C1 S1 S2 C3 110.95(9) y
C4 S1 S2 C3 -79.37(9) y
C1 S1 S2 C2 -80.75(9) y
C4 S1 S2 C2 88.93(8) y
C4 S1 C1 Si1 49.50(11) y
S2 S1 C1 Si1 58.28(7) y
C5 Si1 C1 S1 56.02(12) n
C6 Si1 C1 S1 176.91(9) n
C2 Si1 C1 S1 -64.87(11) y
C3 S2 C2 Si1 63.55(10) y
S1 S2 C2 Si1 54.14(6) y
C5 Si1 C2 S2 179.26(9) n
C6 Si1 C2 S2 58.42(11) n
C1 Si1 C2 S2 -58.89(11) y
C2 S2 C3 Si2 49.14(10) y
S1 S2 C3 Si2 59.03(7) y
C8 Si2 C3 S2 175.35(9) n
C7 Si2 C3 S2 55.49(11) n
C4 Si2 C3 S2 -65.45(11) y
C1 S1 C4 Si2 62.27(10) y
S2 S1 C4 Si2 53.95(6) y
C8 Si2 C4 S1 59.32(10) n
C7 Si2 C4 S1 179.33(9) n
C3 Si2 C4 S1 -57.83(11) y
