#------------------------------------------------------------------------------
#$Date: 2016-03-21 08:52:18 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178613 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/24/4072400.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_4072400
loop_
_publ_author_name
'Zirngast, Michaela'
'Baumgartner, Judith'
'Marschner, Christoph'
_publ_section_title
;
 Synthesis of Cyclic and Bicyclic Polysilanes of Variable Ring Sizes
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              6472
_journal_paper_doi               10.1021/om800842p
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C30 H72 O Si12'
_chemical_formula_weight         785.96
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           72
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-I 2 2c'
_symmetry_space_group_name_H-M   'I b a m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.329(2)
_cell_length_b                   15.447(3)
_cell_length_c                   31.058(6)
_cell_measurement_temperature    200(2)
_cell_volume                     4955.4(17)
_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      200(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker P4'
_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  0.0638
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            18749
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    0.334
_exptl_absorpt_correction_T_max  0.9301
_exptl_absorpt_correction_T_min  0.8723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.054
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.309
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         2587
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.309
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0838
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0523P)²+14.5794P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1703
_refine_ls_wR_factor_ref         0.1746
_reflns_number_gt                2354
_reflns_number_total             2587
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800842p_si_001.cif
_cod_data_source_block           3_463j
_cod_original_cell_volume        4955.2(17)
_cod_original_sg_symbol_H-M      Ibam
_cod_database_code               4072400
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1, y+1, -z+1/2'
'x+1, -y+1, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z'
'-x-1/2, y-1/2, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x, -y, z+1/2'
'-x, y, z+1/2'
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 0.0000 0.5000 0.60453(4) 0.0275(3) Uani 1 2 d S
Si2 Si 0.19719(10) 0.49810(7) 0.56563(3) 0.0297(3) Uani 1 1 d .
Si3 Si 0.20168(13) 0.41976(9) 0.5000 0.0267(3) Uani 1 2 d S
Si4 Si 0.01001(12) 0.62150(7) 0.65079(4) 0.0373(3) Uani 1 1 d .
C1 C 0.3215(4) 0.4437(3) 0.60110(14) 0.0453(11) Uani 1 1 d .
H1A H 0.4056 0.4435 0.5865 0.068 Uiso 1 1 calc R
H1B H 0.2947 0.3840 0.6069 0.068 Uiso 1 1 calc R
H1C H 0.3289 0.4754 0.6283 0.068 Uiso 1 1 calc R
C2 C 0.2597(4) 0.6116(3) 0.55751(14) 0.0429(10) Uani 1 1 d .
H2A H 0.2766 0.6383 0.5856 0.064 Uiso 1 1 calc R
H2B H 0.1949 0.6458 0.5419 0.064 Uiso 1 1 calc R
H2C H 0.3401 0.6097 0.5408 0.064 Uiso 1 1 calc R
C3 C 0.3653(8) 0.3650(6) 0.5000 0.0522(19) Uani 1 2 d S
H31 H 0.369(5) 0.333(3) 0.4760(15) 0.066(16) Uiso 1 1 d .
H32 H 0.437(9) 0.408(6) 0.5000 0.10(3) Uiso 1 2 d S
C4 C 0.0768(9) 0.3316(5) 0.5000 0.0519(18) Uani 1 2 d S
H42 H 0.005(7) 0.360(4) 0.5000 0.04(2) Uiso 1 2 d S
H41 H 0.082(6) 0.298(4) 0.4742(18) 0.11(2) Uiso 1 1 d .
C5 C 0.1723(4) 0.6315(3) 0.67707(14) 0.0530(12) Uani 1 1 d .
H5A H 0.2394 0.6365 0.6549 0.080 Uiso 1 1 calc R
H5B H 0.1889 0.5801 0.6947 0.080 Uiso 1 1 calc R
H5C H 0.1737 0.6832 0.6954 0.080 Uiso 1 1 calc R
C6 C -0.1126(5) 0.6133(3) 0.69519(15) 0.0548(13) Uani 1 1 d .
H6A H -0.1090 0.6657 0.7130 0.082 Uiso 1 1 calc R
H6B H -0.0934 0.5626 0.7131 0.082 Uiso 1 1 calc R
H6C H -0.1993 0.6074 0.6828 0.082 Uiso 1 1 calc R
C7 C -0.0218(5) 0.7245(3) 0.62080(15) 0.0536(12) Uani 1 1 d .
H7A H -0.0150 0.7736 0.6406 0.080 Uiso 1 1 calc R
H7B H -0.1090 0.7227 0.6084 0.080 Uiso 1 1 calc R
H7C H 0.0420 0.7309 0.5977 0.080 Uiso 1 1 calc R
O1 O 0.5000 0.5000 0.7500 0.231(12) Uani 1 4 d S
C8 C 0.5000 0.6530(9) 0.7500 0.179(9) Uani 1 2 d S
C9 C 0.515(4) 0.5788(14) 0.7299(9) 0.306(14) 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'
Si Si 0.0817 0.0704 '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'
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
Si4 Si1 Si4 105.21(8) 2_565 .
Si4 Si1 Si2 109.73(4) 2_565 .
Si4 Si1 Si2 106.38(4) . .
Si4 Si1 Si2 106.39(4) 2_565 2_565
Si4 Si1 Si2 109.73(4) . 2_565
Si2 Si1 Si2 118.65(8) . 2_565
C2 Si2 C1 105.0(2) . .
C2 Si2 Si1 110.57(14) . .
C1 Si2 Si1 107.02(15) . .
C2 Si2 Si3 110.67(14) . .
C1 Si2 Si3 105.13(15) . .
Si1 Si2 Si3 117.50(6) . .
C4 Si3 C3 106.9(4) . .
C4 Si3 Si2 110.92(13) . 10_556
C3 Si3 Si2 104.24(15) . 10_556
C4 Si3 Si2 110.92(13) . .
C3 Si3 Si2 104.24(15) . .
Si2 Si3 Si2 118.56(8) 10_556 .
C5 Si4 C7 107.7(2) . .
C5 Si4 C6 106.8(2) . .
C7 Si4 C6 107.7(2) . .
C5 Si4 Si1 111.69(16) . .
C7 Si4 Si1 111.35(15) . .
C6 Si4 Si1 111.32(16) . .
C9 O1 C9 55.6(19) 8_456 2_665
C9 O1 C9 126(2) 8_456 7_546
C9 O1 C9 167(3) 2_665 7_546
C9 O1 C9 167(3) 8_456 .
C9 O1 C9 126(2) 2_665 .
C9 O1 C9 55.6(19) 7_546 .
C9 C8 C9 58(2) . 7_546
C9 C9 C8 60.8(10) 7_546 .
C9 C9 O1 62.2(9) 7_546 .
C8 C9 O1 123.0(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 Si4 2.3659(14) 2_565
Si1 Si4 2.3659(14) .
Si1 Si2 2.3683(13) .
Si1 Si2 2.3684(13) 2_565
Si2 C2 1.885(4) .
Si2 C1 1.889(4) .
Si2 Si3 2.3710(13) .
Si3 C4 1.876(7) .
Si3 C3 1.890(7) .
Si3 Si2 2.3709(13) 10_556
Si4 C5 1.871(5) .
Si4 C7 1.872(4) .
Si4 C6 1.876(5) .
O1 C9 1.38(2) 8_456
O1 C9 1.38(2) 2_665
O1 C9 1.38(2) 7_546
O1 C9 1.38(2) .
C8 C9 1.31(2) .
C8 C9 1.31(2) 7_546
C9 C9 1.28(4) 7_546
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
Si4 Si1 Si2 C2 -144.26(15) 2_565 .
Si4 Si1 Si2 C2 -30.93(16) . .
Si2 Si1 Si2 C2 93.23(15) 2_565 .
Si4 Si1 Si2 C1 -30.44(17) 2_565 .
Si4 Si1 Si2 C1 82.88(16) . .
Si2 Si1 Si2 C1 -152.95(16) 2_565 .
Si4 Si1 Si2 Si3 87.40(8) 2_565 .
Si4 Si1 Si2 Si3 -159.27(6) . .
Si2 Si1 Si2 Si3 -35.11(5) 2_565 .
C2 Si2 Si3 C4 -153.9(3) . .
C1 Si2 Si3 C4 93.3(3) . .
Si1 Si2 Si3 C4 -25.6(3) . .
C2 Si2 Si3 C3 91.5(3) . .
C1 Si2 Si3 C3 -21.4(3) . .
Si1 Si2 Si3 C3 -140.2(3) . .
C2 Si2 Si3 Si2 -23.82(18) . 10_556
C1 Si2 Si3 Si2 -136.67(16) . 10_556
Si1 Si2 Si3 Si2 104.47(8) . 10_556
Si4 Si1 Si4 C5 73.34(17) 2_565 .
Si2 Si1 Si4 C5 -43.06(18) . .
Si2 Si1 Si4 C5 -172.58(17) 2_565 .
Si4 Si1 Si4 C7 -166.22(19) 2_565 .
Si2 Si1 Si4 C7 77.38(19) . .
Si2 Si1 Si4 C7 -52.14(19) 2_565 .
Si4 Si1 Si4 C6 -46.00(18) 2_565 .
Si2 Si1 Si4 C6 -162.39(19) . .
Si2 Si1 Si4 C6 68.09(19) 2_565 .
C9 C8 C9 O1 -0.001(6) 7_546 .
C9 O1 C9 C9 -102(3) 8_456 7_546
C9 O1 C9 C9 164(4) 2_665 7_546
C9 O1 C9 C8 -102(3) 8_456 .
C9 O1 C9 C8 164(4) 2_665 .
C9 O1 C9 C8 0.001(7) 7_546 .
