#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:30:25 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178568 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/77/4067734.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_4067734
loop_
_publ_author_name
'Wallner, Andreas'
'Hlina, Johann'
'Konopa, Tina'
'Wagner, Harald'
'Baumgartner, Judith'
'Marschner, Christoph'
'Flörke, Ulrich'
_publ_section_title
;
 Cyclic and Bicyclic Methylpolysilanes and Some Oligosilanylene-Bridged
 Derivatives
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2660
_journal_paper_doi               10.1021/om901104h
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C38 H114 Si20'
_chemical_formula_weight         1133.09
_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                105.86(3)
_cell_angle_beta                 99.83(3)
_cell_angle_gamma                111.00(3)
_cell_formula_units_Z            1
_cell_length_a                   9.946(2)
_cell_length_b                   13.658(3)
_cell_length_c                   15.241(3)
_cell_measurement_reflns_used    1227
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      45.105
_cell_measurement_theta_min      5.185
_cell_volume                     1774.1(10)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'SMART APEX'
_diffrn_measurement_method       'ω 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  0.0797
_diffrn_reflns_av_sigmaI/netI    0.1551
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14250
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    0.378
_exptl_absorpt_correction_T_max  0.9282
_exptl_absorpt_correction_T_min  0.7994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.060
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             622
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         7139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.1460
_refine_ls_R_factor_gt           0.0812
_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)+(0.0678P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1537
_refine_ls_wR_factor_ref         0.1752
_reflns_number_gt                4011
_reflns_number_total             7139
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om901104h_si_002.cif
_cod_data_source_block           11_318j
_cod_original_cell_volume        1774.3(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4067734
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
Si1 Si 0.38104(15) 0.60552(12) 0.30281(10) 0.0207(3) Uani 1 1 d .
Si2 Si 0.11649(16) 0.50960(12) 0.27006(10) 0.0250(4) Uani 1 1 d .
Si3 Si 0.04102(17) 0.32949(13) 0.28036(11) 0.0316(4) Uani 1 1 d .
Si4 Si 0.11116(18) 0.21309(13) 0.17287(11) 0.0324(4) Uani 1 1 d .
Si5 Si 0.36654(18) 0.30685(13) 0.19180(11) 0.0294(4) Uani 1 1 d .
Si6 Si 0.43886(16) 0.48683(12) 0.18328(10) 0.0247(4) Uani 1 1 d .
Si7 Si 0.47472(15) 0.80199(12) 0.32570(9) 0.0206(3) Uani 1 1 d .
Si8 Si 0.49637(16) 0.90854(12) 0.48568(10) 0.0229(4) Uani 1 1 d .
Si9 Si 0.32952(16) 0.82998(12) 0.20390(10) 0.0237(4) Uani 1 1 d .
Si10 Si 0.72255(16) 0.85721(12) 0.31251(10) 0.0244(4) Uani 1 1 d .
C1 C 0.4727(6) 0.5957(4) 0.4185(3) 0.0263(13) Uani 1 1 d .
H1A H 0.4436 0.6346 0.4709 0.039 Uiso 1 1 calc R
H1B H 0.5827 0.6311 0.4327 0.039 Uiso 1 1 calc R
H1C H 0.4389 0.5164 0.4114 0.039 Uiso 1 1 calc R
C2 C 0.0391(6) 0.5842(5) 0.3568(4) 0.0374(15) Uani 1 1 d .
H2A H 0.0525 0.6562 0.3500 0.056 Uiso 1 1 calc R
H2B H 0.0932 0.5980 0.4222 0.056 Uiso 1 1 calc R
H2C H -0.0685 0.5373 0.3433 0.056 Uiso 1 1 calc R
C3 C 0.0080(6) 0.4870(4) 0.1470(4) 0.0322(14) Uani 1 1 d .
H3A H -0.1004 0.4485 0.1378 0.048 Uiso 1 1 calc R
H3B H 0.0367 0.4408 0.0992 0.048 Uiso 1 1 calc R
H3C H 0.0312 0.5599 0.1398 0.048 Uiso 1 1 calc R
C4 C 0.1150(7) 0.3385(5) 0.4059(4) 0.0424(16) Uani 1 1 d .
H4A H 0.0882 0.3902 0.4500 0.064 Uiso 1 1 calc R
H4B H 0.2251 0.3663 0.4233 0.064 Uiso 1 1 calc R
H4C H 0.0704 0.2636 0.4096 0.064 Uiso 1 1 calc R
C5 C -0.1704(6) 0.2666(5) 0.2484(5) 0.057(2) Uani 1 1 d .
H5A H -0.2086 0.1881 0.2441 0.086 Uiso 1 1 calc R
H5B H -0.2123 0.2697 0.1867 0.086 Uiso 1 1 calc R
H5C H -0.2008 0.3093 0.2978 0.086 Uiso 1 1 calc R
C6 C -0.0010(7) 0.1755(5) 0.0472(4) 0.0554(19) Uani 1 1 d .
H6A H 0.0353 0.1320 0.0027 0.083 Uiso 1 1 calc R
H6B H 0.0107 0.2445 0.0349 0.083 Uiso 1 1 calc R
H6C H -0.1078 0.1304 0.0380 0.083 Uiso 1 1 calc R
C7 C 0.0761(6) 0.0789(4) 0.1949(4) 0.0396(15) Uani 1 1 d .
H7A H -0.0323 0.0365 0.1833 0.059 Uiso 1 1 calc R
H7B H 0.1302 0.0963 0.2613 0.059 Uiso 1 1 calc R
H7C H 0.1120 0.0336 0.1517 0.059 Uiso 1 1 calc R
C8 C 0.4159(7) 0.2236(5) 0.0910(4) 0.0426(16) Uani 1 1 d .
H8A H 0.5251 0.2588 0.1016 0.064 Uiso 1 1 calc R
H8B H 0.3633 0.2228 0.0301 0.064 Uiso 1 1 calc R
H8C H 0.3847 0.1463 0.0892 0.064 Uiso 1 1 calc R
C9 C 0.4793(6) 0.3116(5) 0.3065(4) 0.0362(14) Uani 1 1 d .
H9A H 0.4806 0.2382 0.2974 0.054 Uiso 1 1 calc R
H9B H 0.4333 0.3299 0.3569 0.054 Uiso 1 1 calc R
H9C H 0.5829 0.3694 0.3249 0.054 Uiso 1 1 calc R
C10 C 0.6468(6) 0.5302(5) 0.1983(4) 0.0361(14) Uani 1 1 d .
H10A H 0.6600 0.4752 0.1479 0.054 Uiso 1 1 calc R
H10B H 0.6965 0.5331 0.2609 0.054 Uiso 1 1 calc R
H10C H 0.6919 0.6046 0.1939 0.054 Uiso 1 1 calc R
C11 C 0.3451(6) 0.4669(4) 0.0567(3) 0.0303(13) Uani 1 1 d .
H11A H 0.3959 0.5355 0.0442 0.045 Uiso 1 1 calc R
H11B H 0.2387 0.4514 0.0487 0.045 Uiso 1 1 calc R
H11C H 0.3520 0.4034 0.0117 0.045 Uiso 1 1 calc R
C12 C 0.6757(6) 0.9207(5) 0.5627(3) 0.0317(13) Uani 1 1 d .
H12A H 0.6868 0.9576 0.6301 0.047 Uiso 1 1 calc R
H12B H 0.7621 0.9655 0.5460 0.047 Uiso 1 1 calc R
H12C H 0.6713 0.8454 0.5520 0.047 Uiso 1 1 calc R
C13 C 0.3376(6) 0.8268(4) 0.5257(4) 0.0321(14) Uani 1 1 d .
H13A H 0.3308 0.7507 0.5136 0.048 Uiso 1 1 calc R
H13B H 0.2424 0.8223 0.4900 0.048 Uiso 1 1 calc R
H13C H 0.3570 0.8649 0.5941 0.048 Uiso 1 1 calc R
C14 C 0.4305(6) 0.9726(4) 0.1984(4) 0.0294(13) Uani 1 1 d .
H14A H 0.5243 0.9785 0.1832 0.044 Uiso 1 1 calc R
H14B H 0.4542 1.0308 0.2604 0.044 Uiso 1 1 calc R
H14C H 0.3659 0.9828 0.1489 0.044 Uiso 1 1 calc R
C15 C 0.1413(5) 0.8131(4) 0.2191(4) 0.0308(13) Uani 1 1 d .
H15A H 0.0865 0.8290 0.1691 0.046 Uiso 1 1 calc R
H15B H 0.1550 0.8656 0.2820 0.046 Uiso 1 1 calc R
H15C H 0.0835 0.7357 0.2144 0.046 Uiso 1 1 calc R
C16 C 0.2948(6) 0.7261(4) 0.0835(3) 0.0317(14) Uani 1 1 d .
H16A H 0.2385 0.6496 0.0812 0.048 Uiso 1 1 calc R
H16B H 0.3916 0.7339 0.0723 0.048 Uiso 1 1 calc R
H16C H 0.2361 0.7406 0.0341 0.048 Uiso 1 1 calc R
C17 C 0.7113(6) 0.8090(4) 0.1824(3) 0.0296(13) Uani 1 1 d .
H17A H 0.8094 0.8128 0.1762 0.044 Uiso 1 1 calc R
H17B H 0.6844 0.8577 0.1533 0.044 Uiso 1 1 calc R
H17C H 0.6343 0.7312 0.1497 0.044 Uiso 1 1 calc R
C18 C 0.8330(5) 0.8004(4) 0.3790(4) 0.0322(14) Uani 1 1 d .
H18A H 0.7715 0.7203 0.3640 0.048 Uiso 1 1 calc R
H18B H 0.8605 0.8414 0.4478 0.048 Uiso 1 1 calc R
H18C H 0.9247 0.8099 0.3599 0.048 Uiso 1 1 calc R
C19 C 0.8392(6) 1.0144(4) 0.3624(4) 0.0339(14) Uani 1 1 d .
H19A H 0.8474 1.0443 0.4303 0.051 Uiso 1 1 calc R
H19B H 0.7906 1.0495 0.3276 0.051 Uiso 1 1 calc R
H19C H 0.9402 1.0313 0.3552 0.051 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'
Si Si 0.0817 0.0704 '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
C1 Si1 Si2 107.00(18) . .
C1 Si1 Si6 103.87(16) . .
Si2 Si1 Si6 104.15(8) . .
C1 Si1 Si7 107.04(17) . .
Si2 Si1 Si7 115.45(8) . .
Si6 Si1 Si7 118.28(8) . .
C3 Si2 C2 106.8(2) . .
C3 Si2 Si3 105.94(18) . .
C2 Si2 Si3 104.2(2) . .
C3 Si2 Si1 112.92(18) . .
C2 Si2 Si1 113.35(18) . .
Si3 Si2 Si1 112.90(8) . .
C5 Si3 C4 107.3(3) . .
C5 Si3 Si4 108.8(2) . .
C4 Si3 Si4 110.8(2) . .
C5 Si3 Si2 106.2(2) . .
C4 Si3 Si2 111.6(2) . .
Si4 Si3 Si2 111.89(9) . .
C6 Si4 C7 107.8(3) . .
C6 Si4 Si5 109.8(2) . .
C7 Si4 Si5 108.90(19) . .
C6 Si4 Si3 110.4(2) . .
C7 Si4 Si3 111.0(2) . .
Si5 Si4 Si3 108.98(9) . .
C9 Si5 C8 107.1(3) . .
C9 Si5 Si4 109.16(19) . .
C8 Si5 Si4 108.9(2) . .
C9 Si5 Si6 111.6(2) . .
C8 Si5 Si6 105.49(19) . .
Si4 Si5 Si6 114.28(9) . .
C10 Si6 C11 107.7(2) . .
C10 Si6 Si5 100.69(19) . .
C11 Si6 Si5 107.06(18) . .
C10 Si6 Si1 115.07(18) . .
C11 Si6 Si1 114.09(17) . .
Si5 Si6 Si1 111.15(8) . .
Si9 Si7 Si10 107.87(8) . .
Si9 Si7 Si8 115.17(8) . .
Si10 Si7 Si8 106.84(8) . .
Si9 Si7 Si1 110.68(8) . .
Si10 Si7 Si1 106.22(8) . .
Si8 Si7 Si1 109.60(8) . .
C13 Si8 C12 106.7(2) . .
C13 Si8 Si8 107.68(19) . 2_676
C12 Si8 Si8 109.64(19) . 2_676
C13 Si8 Si7 110.27(17) . .
C12 Si8 Si7 105.14(17) . .
Si8 Si8 Si7 116.97(10) 2_676 .
C15 Si9 C16 107.2(2) . .
C15 Si9 C14 109.3(2) . .
C16 Si9 C14 105.7(2) . .
C15 Si9 Si7 111.97(18) . .
C16 Si9 Si7 111.08(18) . .
C14 Si9 Si7 111.39(18) . .
C18 Si10 C17 110.6(2) . .
C18 Si10 C19 105.1(2) . .
C17 Si10 C19 106.1(2) . .
C18 Si10 Si7 112.13(18) . .
C17 Si10 Si7 108.89(18) . .
C19 Si10 Si7 113.74(18) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 C1 1.904(5) .
Si1 Si2 2.369(2) .
Si1 Si6 2.385(2) .
Si1 Si7 2.403(2) .
Si2 C3 1.879(5) .
Si2 C2 1.885(5) .
Si2 Si3 2.360(2) .
Si3 C5 1.878(6) .
Si3 C4 1.882(6) .
Si3 Si4 2.337(2) .
Si4 C6 1.871(6) .
Si4 C7 1.875(5) .
Si4 Si5 2.322(2) .
Si5 C9 1.880(5) .
Si5 C8 1.896(5) .
Si5 Si6 2.349(2) .
Si6 C10 1.889(5) .
Si6 C11 1.892(5) .
Si7 Si9 2.355(2) .
Si7 Si10 2.368(2) .
Si7 Si8 2.401(2) .
Si8 C13 1.884(5) .
Si8 C12 1.884(5) .
Si8 Si8 2.388(3) 2_676
Si9 C15 1.865(5) .
Si9 C16 1.873(5) .
Si9 C14 1.877(5) .
Si10 C18 1.869(5) .
Si10 C17 1.881(5) .
Si10 C19 1.886(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_4
C1 Si1 Si2 C3 -169.2(2) .
Si6 Si1 Si2 C3 -59.61(19) .
Si7 Si1 Si2 C3 71.8(2) .
C1 Si1 Si2 C2 69.1(3) .
Si6 Si1 Si2 C2 178.7(2) .
Si7 Si1 Si2 C2 -49.9(2) .
C1 Si1 Si2 Si3 -49.07(18) .
Si6 Si1 Si2 Si3 60.54(10) .
Si7 Si1 Si2 Si3 -168.08(8) .
C3 Si2 Si3 C5 -54.2(3) .
C2 Si2 Si3 C5 58.3(3) .
Si1 Si2 Si3 C5 -178.2(2) .
C3 Si2 Si3 C4 -170.8(3) .
C2 Si2 Si3 C4 -58.3(3) .
Si1 Si2 Si3 C4 65.1(2) .
C3 Si2 Si3 Si4 64.41(19) .
C2 Si2 Si3 Si4 176.91(18) .
Si1 Si2 Si3 Si4 -59.67(11) .
C5 Si3 Si4 C6 48.0(3) .
C4 Si3 Si4 C6 165.8(3) .
Si2 Si3 Si4 C6 -69.0(2) .
C5 Si3 Si4 C7 -71.5(3) .
C4 Si3 Si4 C7 46.3(3) .
Si2 Si3 Si4 C7 171.5(2) .
C5 Si3 Si4 Si5 168.6(2) .
C4 Si3 Si4 Si5 -73.6(2) .
Si2 Si3 Si4 Si5 51.62(11) .
C6 Si4 Si5 C9 -165.9(3) .
C7 Si4 Si5 C9 -48.0(3) .
Si3 Si4 Si5 C9 73.1(2) .
C6 Si4 Si5 C8 -49.3(3) .
C7 Si4 Si5 C8 68.5(3) .
Si3 Si4 Si5 C8 -170.3(2) .
C6 Si4 Si5 Si6 68.4(2) .
C7 Si4 Si5 Si6 -173.81(19) .
Si3 Si4 Si5 Si6 -52.62(11) .
C9 Si5 Si6 C10 57.0(3) .
C8 Si5 Si6 C10 -59.0(3) .
Si4 Si5 Si6 C10 -178.55(18) .
C9 Si5 Si6 C11 169.4(2) .
C8 Si5 Si6 C11 53.5(3) .
Si4 Si5 Si6 C11 -66.12(19) .
C9 Si5 Si6 Si1 -65.4(2) .
C8 Si5 Si6 Si1 178.7(2) .
Si4 Si5 Si6 Si1 59.08(11) .
C1 Si1 Si6 C10 -60.7(3) .
Si2 Si1 Si6 C10 -172.6(2) .
Si7 Si1 Si6 C10 57.7(2) .
C1 Si1 Si6 C11 174.1(3) .
Si2 Si1 Si6 C11 62.2(2) .
Si7 Si1 Si6 C11 -67.5(2) .
C1 Si1 Si6 Si5 52.90(19) .
Si2 Si1 Si6 Si5 -59.00(10) .
Si7 Si1 Si6 Si5 171.30(8) .
C1 Si1 Si7 Si9 -166.46(17) .
Si2 Si1 Si7 Si9 -47.47(10) .
Si6 Si1 Si7 Si9 76.82(10) .
C1 Si1 Si7 Si10 76.71(18) .
Si2 Si1 Si7 Si10 -164.30(7) .
Si6 Si1 Si7 Si10 -40.01(10) .
C1 Si1 Si7 Si8 -38.36(18) .
Si2 Si1 Si7 Si8 80.62(10) .
Si6 Si1 Si7 Si8 -155.08(8) .
Si9 Si7 Si8 C13 89.5(2) .
Si10 Si7 Si8 C13 -150.79(19) .
Si1 Si7 Si8 C13 -36.1(2) .
Si9 Si7 Si8 C12 -155.91(19) .
Si10 Si7 Si8 C12 -36.1(2) .
Si1 Si7 Si8 C12 78.5(2) .
Si9 Si7 Si8 Si8 -34.01(13) 2_676
Si10 Si7 Si8 Si8 85.75(12) 2_676
Si1 Si7 Si8 Si8 -159.57(9) 2_676
Si10 Si7 Si9 C15 -170.19(19) .
Si8 Si7 Si9 C15 -51.0(2) .
Si1 Si7 Si9 C15 74.01(19) .
Si10 Si7 Si9 C16 70.0(2) .
Si8 Si7 Si9 C16 -170.77(19) .
Si1 Si7 Si9 C16 -45.8(2) .
Si10 Si7 Si9 C14 -47.5(2) .
Si8 Si7 Si9 C14 71.7(2) .
Si1 Si7 Si9 C14 -163.30(19) .
Si9 Si7 Si10 C18 -162.81(19) .
Si8 Si7 Si10 C18 72.8(2) .
Si1 Si7 Si10 C18 -44.1(2) .
Si9 Si7 Si10 C17 -40.03(19) .
Si8 Si7 Si10 C17 -164.39(18) .
Si1 Si7 Si10 C17 78.67(19) .
Si9 Si7 Si10 C19 78.1(2) .
Si8 Si7 Si10 C19 -46.3(2) .
Si1 Si7 Si10 C19 -163.24(19) .
