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#$Date: 2016-03-21 09:48:01 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178628 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/39/4073941.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_4073941
loop_
_publ_author_name
'Wagner, Harald'
'Wallner, Andreas'
'Fischer, Jelena'
'Flock, Michaela'
'Baumgartner, Judith'
'Marschner, Christoph'
_publ_section_title
;
 Rearrangement of Cyclic Silanes with Aluminum Trichloride
;
_journal_issue                   27
_journal_name_full               Organometallics
_journal_page_first              6704
_journal_paper_doi               10.1021/om7007524
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C24 H72 Si12'
_chemical_formula_weight         697.90
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_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                 118.53(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   19.235(4)
_cell_length_b                   12.713(3)
_cell_length_c                   10.285(2)
_cell_measurement_temperature    100(2)
_cell_volume                     2209.6(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_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  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5959
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.366
_exptl_absorpt_correction_T_max  0.9438
_exptl_absorpt_correction_T_min  0.8857
_exptl_crystal_density_diffrn    1.049
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.576
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2309
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0573
_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)+(0.0776P)²+6.0141P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1552
_refine_ls_wR_factor_ref         0.1592
_reflns_number_gt                2069
_reflns_number_total             2309
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7007524-file001.cif
_cod_data_source_block           9_c2m
_cod_original_cell_volume        2209.5(8)
_cod_database_code               4073941
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, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.2554(5) 0.1405(9) 0.3009(10) 0.073(3) Uani 0.521(7) 1 d PU A 1
H1A H 1.3042 0.1457 0.3957 0.109 Uiso 0.521(7) 1 calc PR A 1
H1B H 1.2163 0.1904 0.2997 0.109 Uiso 0.521(7) 1 calc PR A 1
H1C H 1.2669 0.1570 0.2200 0.109 Uiso 0.521(7) 1 calc PR A 1
C4 C 1.1871(4) 0.1444(6) -0.1219(8) 0.0449(18) Uani 0.521(7) 1 d PU A 1
H4A H 1.2101 0.1485 -0.1885 0.067 Uiso 0.521(7) 1 calc PR A 1
H4B H 1.2271 0.1641 -0.0215 0.067 Uiso 0.521(7) 1 calc PR A 1
H4C H 1.1420 0.1928 -0.1562 0.067 Uiso 0.521(7) 1 calc PR A 1
C5 C 0.9633(7) 0.3728(6) 0.1420(13) 0.084(4) Uani 0.521(7) 1 d PU A 1
H5A H 0.9795 0.4194 0.2276 0.127 Uiso 0.521(7) 1 calc PR A 1
H5B H 0.9089 0.3491 0.1081 0.127 Uiso 0.521(7) 1 calc PR A 1
H5C H 0.9662 0.4110 0.0620 0.127 Uiso 0.521(7) 1 calc PR A 1
C6 C 1.1353(7) 0.3115(9) 0.2457(11) 0.069(3) Uani 0.521(7) 1 d PU A 1
H6A H 1.1515 0.3622 0.3268 0.103 Uiso 0.521(7) 1 calc PR A 1
H6B H 1.1327 0.3466 0.1587 0.103 Uiso 0.521(7) 1 calc PR A 1
H6C H 1.1739 0.2541 0.2763 0.103 Uiso 0.521(7) 1 calc PR A 1
C7 C 1.0363(7) 0.2101(10) 0.3689(10) 0.069(3) Uani 0.521(7) 1 d PU A 1
H7A H 1.0496 0.2695 0.4375 0.104 Uiso 0.521(7) 1 calc PR A 1
H7B H 1.0769 0.1555 0.4134 0.104 Uiso 0.521(7) 1 calc PR A 1
H7C H 0.9848 0.1813 0.3485 0.104 Uiso 0.521(7) 1 calc PR A 1
C11 C 1.2924(5) 0.0866(12) 0.2810(10) 0.082(4) Uani 0.479(7) 1 d PU A 2
H11A H 1.3389 0.0833 0.3793 0.124 Uiso 0.479(7) 1 calc PR A 2
H11B H 1.2729 0.1591 0.2599 0.124 Uiso 0.479(7) 1 calc PR A 2
H11C H 1.3070 0.0633 0.2064 0.124 Uiso 0.479(7) 1 calc PR A 2
C44 C 1.2387(5) 0.0806(8) -0.0605(11) 0.064(3) Uani 0.479(7) 1 d PU A 2
H44A H 1.2575 0.0765 -0.1338 0.095 Uiso 0.479(7) 1 calc PR A 2
H44B H 1.2802 0.0551 0.0352 0.095 Uiso 0.479(7) 1 calc PR A 2
H44C H 1.2260 0.1538 -0.0506 0.095 Uiso 0.479(7) 1 calc PR A 2
C55 C 0.9330(5) 0.3082(6) 0.1746(11) 0.053(2) Uani 0.479(7) 1 d PU A 2
H55A H 0.9435 0.3588 0.2539 0.080 Uiso 0.479(7) 1 calc PR A 2
H55B H 0.9013 0.2499 0.1802 0.080 Uiso 0.479(7) 1 calc PR A 2
H55C H 0.9041 0.3433 0.0785 0.080 Uiso 0.479(7) 1 calc PR A 2
C66 C 1.0908(6) 0.3642(7) 0.1899(11) 0.046(2) Uani 0.479(7) 1 d PU A 2
H66A H 1.1026 0.4123 0.2723 0.069 Uiso 0.479(7) 1 calc PR A 2
H66B H 1.0613 0.4018 0.0960 0.069 Uiso 0.479(7) 1 calc PR A 2
H66C H 1.1404 0.3373 0.1977 0.069 Uiso 0.479(7) 1 calc PR A 2
C77 C 1.0836(7) 0.1969(8) 0.3890(10) 0.052(2) Uani 0.479(7) 1 d PU A 2
H77A H 1.0941 0.2525 0.4621 0.078 Uiso 0.479(7) 1 calc PR A 2
H77B H 1.1338 0.1652 0.4063 0.078 Uiso 0.479(7) 1 calc PR A 2
H77C H 1.0500 0.1428 0.3985 0.078 Uiso 0.479(7) 1 calc PR A 2
Si1 Si 1.09677(6) 0.0000 0.04301(11) 0.0184(3) Uani 1 2 d S . .
Si2 Si 1.0000 0.13340(8) 0.0000 0.0207(3) Uani 1 2 d S . .
Si3 Si 1.21407(7) 0.0000 0.27614(14) 0.0460(4) Uani 1 2 d S . .
Si4 Si 1.15092(6) 0.0000 -0.12061(13) 0.0279(3) Uani 1 2 d S . .
Si5 Si 1.03165(6) 0.25484(7) 0.19684(11) 0.0424(3) Uani 1 1 d . . .
C2 C 1.2038(5) 0.0000 0.4426(7) 0.153(6) Uani 1 2 d S A .
H2A H 1.2564 0.0000 0.5298 0.229 Uiso 1 2 calc SR . .
H2B H 1.1747 -0.0629 0.4439 0.229 Uiso 0.50 1 calc PR . .
H2C H 1.1747 0.0629 0.4439 0.229 Uiso 0.50 1 calc PR . .
C3 C 1.0801(4) 0.0000 -0.3150(7) 0.109(4) Uani 1 2 d S A .
H3A H 1.1082 0.0000 -0.3733 0.164 Uiso 1 2 calc SR . .
H3B H 1.0468 0.0629 -0.3386 0.164 Uiso 0.50 1 calc PR . .
H3C H 1.0468 -0.0629 -0.3387 0.164 Uiso 0.50 1 calc PR . .
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
Si4 Si1 Si3 100.89(6) . .
Si4 Si1 Si2 115.83(4) . 5_755
Si3 Si1 Si2 117.67(4) . 5_755
Si4 Si1 Si2 115.83(4) . .
Si3 Si1 Si2 117.67(4) . .
Si2 Si1 Si2 90.02(5) 5_755 .
Si5 Si2 Si5 99.21(6) . 2_755
Si5 Si2 Si1 118.41(3) . 5_755
Si5 Si2 Si1 116.16(4) 2_755 5_755
Si5 Si2 Si1 116.15(4) . .
Si5 Si2 Si1 118.41(4) 2_755 .
Si1 Si2 Si1 89.98(5) 5_755 .
C2 Si3 C11 115.4(4) . .
C2 Si3 C11 115.4(4) . 6
C11 Si3 C11 73.1(10) . 6
C2 Si3 C1 95.7(3) . 6
C11 Si3 C1 105.6(7) . 6
C11 Si3 C1 33.1(5) 6 6
C2 Si3 C1 95.7(3) . .
C11 Si3 C1 33.1(5) . .
C11 Si3 C1 105.6(7) 6 .
C1 Si3 C1 136.6(6) 6 .
C2 Si3 Si1 118.2(3) . .
C11 Si3 Si1 113.3(3) . .
C11 Si3 Si1 113.3(3) 6 .
C1 Si3 Si1 105.5(3) 6 .
C1 Si3 Si1 105.5(3) . .
C3 Si4 C44 117.7(4) . 6
C3 Si4 C44 117.7(4) . .
C44 Si4 C44 68.8(8) 6 .
C3 Si4 C4 94.3(2) . .
C44 Si4 C4 104.8(5) 6 .
C44 Si4 C4 36.8(4) . .
C3 Si4 C4 94.3(2) . 6
C44 Si4 C4 36.8(4) 6 6
C44 Si4 C4 104.8(5) . 6
C4 Si4 C4 138.2(5) . 6
C3 Si4 Si1 115.6(2) . .
C44 Si4 Si1 114.4(3) 6 .
C44 Si4 Si1 114.4(3) . .
C4 Si4 Si1 106.4(2) . .
C4 Si4 Si1 106.4(2) 6 .
C66 Si5 C7 122.4(4) . .
C66 Si5 C77 108.1(5) . .
C7 Si5 C77 26.4(4) . .
C66 Si5 C5 75.0(4) . .
C7 Si5 C5 104.0(5) . .
C77 Si5 C5 124.5(4) . .
C66 Si5 C55 109.0(4) . .
C7 Si5 C55 79.2(5) . .
C77 Si5 C55 105.2(4) . .
C5 Si5 C55 34.9(3) . .
C66 Si5 C6 31.2(4) . .
C7 Si5 C6 107.2(4) . .
C77 Si5 C6 84.8(5) . .
C5 Si5 C6 105.3(5) . .
C55 Si5 C6 136.9(5) . .
C66 Si5 Si2 111.9(3) . .
C7 Si5 Si2 119.9(4) . .
C77 Si5 Si2 115.4(3) . .
C5 Si5 Si2 113.6(3) . .
C55 Si5 Si2 106.9(3) . .
C6 Si5 Si2 105.9(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 Si3 1.922(10) .
C4 Si4 1.966(7) .
C5 Si5 1.894(10) .
C6 Si5 1.947(9) .
C7 Si5 1.820(8) .
C11 Si3 1.848(9) .
C44 Si4 1.813(7) .
C55 Si5 1.923(7) .
C66 Si5 1.820(7) .
C77 Si5 1.887(9) .
Si1 Si4 2.3645(14) .
Si1 Si3 2.3814(19) .
Si1 Si2 2.3979(10) 5_755
Si1 Si2 2.3979(10) .
Si2 Si5 2.3822(11) .
Si2 Si5 2.3822(11) 2_755
Si2 Si1 2.3979(10) 5_755
Si3 C2 1.815(7) .
Si3 C11 1.848(9) 6
Si3 C1 1.922(10) 6
Si4 C3 1.803(6) .
Si4 C44 1.813(7) 6
Si4 C4 1.966(7) 6
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 Si5 -119.04(5) . .
Si3 Si1 Si2 Si5 0.36(6) . .
Si2 Si1 Si2 Si5 122.00(4) 5_755 .
Si4 Si1 Si2 Si5 -1.10(6) . 2_755
Si3 Si1 Si2 Si5 118.30(6) . 2_755
Si2 Si1 Si2 Si5 -120.07(5) 5_755 2_755
Si4 Si1 Si2 Si1 118.96(6) . 5_755
Si3 Si1 Si2 Si1 -121.64(6) . 5_755
Si2 Si1 Si2 Si1 0.0 5_755 5_755
Si4 Si1 Si3 C2 180.0 . .
Si2 Si1 Si3 C2 -52.99(4) 5_755 .
Si2 Si1 Si3 C2 52.99(4) . .
Si4 Si1 Si3 C11 40.4(6) . .
Si2 Si1 Si3 C11 167.5(6) 5_755 .
Si2 Si1 Si3 C11 -86.6(6) . .
Si4 Si1 Si3 C11 -40.4(6) . 6
Si2 Si1 Si3 C11 86.6(6) 5_755 6
Si2 Si1 Si3 C11 -167.5(6) . 6
Si4 Si1 Si3 C1 -74.6(3) . 6
Si2 Si1 Si3 C1 52.4(3) 5_755 6
Si2 Si1 Si3 C1 158.4(3) . 6
Si4 Si1 Si3 C1 74.6(3) . .
Si2 Si1 Si3 C1 -158.4(3) 5_755 .
Si2 Si1 Si3 C1 -52.4(3) . .
Si3 Si1 Si4 C3 180.0 . .
Si2 Si1 Si4 C3 51.79(4) 5_755 .
Si2 Si1 Si4 C3 -51.79(4) . .
Si3 Si1 Si4 C44 38.3(4) . 6
Si2 Si1 Si4 C44 -89.9(4) 5_755 6
Si2 Si1 Si4 C44 166.6(4) . 6
Si3 Si1 Si4 C44 -38.3(4) . .
Si2 Si1 Si4 C44 -166.6(4) 5_755 .
Si2 Si1 Si4 C44 89.9(4) . .
Si3 Si1 Si4 C4 -76.8(2) . .
Si2 Si1 Si4 C4 155.0(2) 5_755 .
Si2 Si1 Si4 C4 51.4(2) . .
Si3 Si1 Si4 C4 76.8(2) . 6
Si2 Si1 Si4 C4 -51.4(2) 5_755 6
Si2 Si1 Si4 C4 -155.0(2) . 6
Si5 Si2 Si5 C66 -42.3(4) 2_755 .
Si1 Si2 Si5 C66 -168.9(4) 5_755 .
Si1 Si2 Si5 C66 85.8(4) . .
Si5 Si2 Si5 C7 164.0(5) 2_755 .
Si1 Si2 Si5 C7 37.5(5) 5_755 .
Si1 Si2 Si5 C7 -67.9(5) . .
Si5 Si2 Si5 C77 -166.5(4) 2_755 .
Si1 Si2 Si5 C77 66.9(4) 5_755 .
Si1 Si2 Si5 C77 -38.4(4) . .
Si5 Si2 Si5 C5 40.3(3) 2_755 .
Si1 Si2 Si5 C5 -86.3(3) 5_755 .
Si1 Si2 Si5 C5 168.4(3) . .
Si5 Si2 Si5 C55 76.9(3) 2_755 .
Si1 Si2 Si5 C55 -49.6(3) 5_755 .
Si1 Si2 Si5 C55 -155.0(3) . .
Si5 Si2 Si5 C6 -74.8(4) 2_755 .
Si1 Si2 Si5 C6 158.7(4) 5_755 .
Si1 Si2 Si5 C6 53.3(4) . .
