#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:08:33 +0100 (lun 21 de mar de 2016) $
#$Revision: 178596 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/07/4070787.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_4070787
loop_
_publ_author_name
'Lim, Young Mook'
'Lee, Myong Euy'
_publ_section_title
;
 An Unexpected Ring Contraction: Phenylsilane to Silacyclopentane
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1000
_journal_paper_doi               10.1021/om701009d
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C23 H56 O Si6'
_chemical_formula_weight         517.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.699(10)
_cell_angle_beta                 82.082(10)
_cell_angle_gamma                71.186(9)
_cell_formula_units_Z            2
_cell_length_a                   9.330(5)
_cell_length_b                   13.422(7)
_cell_length_c                   14.544(8)
_cell_measurement_temperature    293(2)
_cell_volume                     1700.9(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0457
_diffrn_reflns_av_sigmaI/netI    0.0946
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9059
_diffrn_reflns_theta_full        25.56
_diffrn_reflns_theta_max         25.56
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.387
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             858
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         6243
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.1206
_refine_ls_R_factor_gt           0.0660
_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)+(0.0919P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1583
_refine_ls_wR_factor_ref         0.1756
_reflns_number_gt                3544
_reflns_number_total             6243
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om701009d-file003.cif
_cod_data_source_block           d113m
_cod_original_cell_volume        1700.8(16)
_cod_database_code               4070787
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 0.53427(12) 0.29709(8) 0.14411(7) 0.0404(3) Uani 1 1 d .
Si3' Si 0.23198(14) 0.67690(9) 0.28207(8) 0.0477(3) Uani 1 1 d .
Si6' Si 0.63754(14) 0.04574(9) 0.15804(9) 0.0509(3) Uani 1 1 d .
Si5' Si 0.22431(14) 0.12425(9) 0.28827(9) 0.0530(4) Uani 1 1 d .
Si2' Si 0.01036(13) 0.59063(9) 0.18662(8) 0.0471(3) Uani 1 1 d .
Si4' Si 0.38573(14) 0.31028(10) 0.41994(8) 0.0509(3) Uani 1 1 d .
O1' O 0.5285(3) 0.3416(2) 0.03327(18) 0.0495(7) Uani 1 1 d .
C1' C 0.3799(4) 0.3772(3) 0.2228(2) 0.0367(9) Uani 1 1 d .
C6' C 0.3163(4) 0.4818(3) 0.2034(2) 0.0384(9) Uani 1 1 d .
H6'A H 0.3624 0.5110 0.1509 0.046 Uiso 1 1 calc R
C4' C 0.4803(4) 0.1735(3) 0.1738(3) 0.0394(9) Uani 1 1 d .
H4'A H 0.4080 0.1767 0.1298 0.047 Uiso 1 1 calc R
C7' C 0.1816(4) 0.5595(3) 0.2533(3) 0.0393(9) Uani 1 1 d .
H7'A H 0.1576 0.5225 0.3131 0.047 Uiso 1 1 calc R
C3' C 0.3836(4) 0.1870(3) 0.2726(3) 0.0405(9) Uani 1 1 d .
H3'A H 0.4544 0.1470 0.3179 0.049 Uiso 1 1 calc R
C2' C 0.3257(4) 0.3067(3) 0.3006(2) 0.0383(9) Uani 1 1 d .
H2'A H 0.2141 0.3302 0.3059 0.046 Uiso 1 1 calc R
C20' C 0.0518(5) 0.1979(4) 0.3610(4) 0.0759(15) Uani 1 1 d .
H20A H -0.0243 0.1630 0.3656 0.114 Uiso 1 1 calc R
H20B H 0.0128 0.2686 0.3327 0.114 Uiso 1 1 calc R
H20C H 0.0778 0.2001 0.4221 0.114 Uiso 1 1 calc R
C10' C -0.1582(5) 0.6852(4) 0.2471(4) 0.0767(15) Uani 1 1 d .
H10A H -0.2442 0.7004 0.2122 0.115 Uiso 1 1 calc R
H10B H -0.1364 0.7494 0.2517 0.115 Uiso 1 1 calc R
H10C H -0.1810 0.6545 0.3084 0.115 Uiso 1 1 calc R
C8' C 0.4000(6) 0.3636(4) -0.0153(3) 0.0741(14) Uani 1 1 d .
H8'A H 0.4229 0.3888 -0.0786 0.111 Uiso 1 1 calc R
H8'B H 0.3166 0.4167 0.0140 0.111 Uiso 1 1 calc R
H8'C H 0.3726 0.3004 -0.0144 0.111 Uiso 1 1 calc R
C17' C 0.3723(6) 0.1929(4) 0.5008(3) 0.0759(15) Uani 1 1 d .
H17A H 0.4040 0.1972 0.5599 0.114 Uiso 1 1 calc R
H17B H 0.4370 0.1295 0.4747 0.114 Uiso 1 1 calc R
H17C H 0.2689 0.1917 0.5095 0.114 Uiso 1 1 calc R
C13' C 0.1036(6) 0.7373(4) 0.3839(3) 0.0651(13) Uani 1 1 d .
H13A H 0.1295 0.7972 0.3975 0.098 Uiso 1 1 calc R
H13B H 0.1153 0.6861 0.4371 0.098 Uiso 1 1 calc R
H13C H -0.0001 0.7598 0.3696 0.098 Uiso 1 1 calc R
C19' C 0.1592(5) 0.1178(4) 0.1739(3) 0.0723(14) Uani 1 1 d .
H19A H 0.0787 0.0864 0.1841 0.108 Uiso 1 1 calc R
H19B H 0.2428 0.0759 0.1350 0.108 Uiso 1 1 calc R
H19C H 0.1226 0.1879 0.1439 0.108 Uiso 1 1 calc R
C5' C 0.7264(5) 0.2935(3) 0.1656(3) 0.0562(12) Uani 1 1 d .
H5'A H 0.7388 0.3619 0.1478 0.084 Uiso 1 1 calc R
H5'B H 0.8014 0.2420 0.1295 0.084 Uiso 1 1 calc R
H5'C H 0.7388 0.2749 0.2306 0.084 Uiso 1 1 calc R
C16' C 0.2634(6) 0.4273(3) 0.4806(3) 0.0675(14) Uani 1 1 d .
H16A H 0.2989 0.4255 0.5398 0.101 Uiso 1 1 calc R
H16B H 0.1601 0.4260 0.4899 0.101 Uiso 1 1 calc R
H16C H 0.2681 0.4908 0.4433 0.101 Uiso 1 1 calc R
C22' C 0.5691(6) -0.0643(4) 0.1351(4) 0.0777(15) Uani 1 1 d .
H22A H 0.5136 -0.0436 0.0813 0.116 Uiso 1 1 calc R
H22B H 0.5036 -0.0798 0.1881 0.116 Uiso 1 1 calc R
H22C H 0.6547 -0.1260 0.1242 0.116 Uiso 1 1 calc R
C23' C 0.7454(5) 0.0052(4) 0.2635(3) 0.0739(14) Uani 1 1 d .
H23A H 0.6771 -0.0030 0.3175 0.111 Uiso 1 1 calc R
H23B H 0.7897 0.0585 0.2715 0.111 Uiso 1 1 calc R
H23C H 0.8245 -0.0607 0.2553 0.111 Uiso 1 1 calc R
C14' C 0.2170(6) 0.7788(3) 0.1811(3) 0.0707(14) Uani 1 1 d .
H14A H 0.2828 0.7480 0.1285 0.106 Uiso 1 1 calc R
H14B H 0.2467 0.8361 0.1971 0.106 Uiso 1 1 calc R
H14C H 0.1138 0.8049 0.1658 0.106 Uiso 1 1 calc R
C21' C 0.7703(5) 0.0612(4) 0.0534(3) 0.0765(15) Uani 1 1 d .
H21A H 0.7152 0.0824 -0.0006 0.115 Uiso 1 1 calc R
H21B H 0.8487 -0.0049 0.0451 0.115 Uiso 1 1 calc R
H21C H 0.8154 0.1140 0.0616 0.115 Uiso 1 1 calc R
C12' C 0.4324(5) 0.6338(4) 0.3108(3) 0.0697(14) Uani 1 1 d .
H12A H 0.4991 0.6023 0.2587 0.105 Uiso 1 1 calc R
H12B H 0.4435 0.5829 0.3642 0.105 Uiso 1 1 calc R
H12C H 0.4579 0.6938 0.3243 0.105 Uiso 1 1 calc R
C18' C 0.2910(6) -0.0111(4) 0.3499(4) 0.0848(17) Uani 1 1 d .
H18A H 0.2108 -0.0426 0.3574 0.127 Uiso 1 1 calc R
H18B H 0.3184 -0.0061 0.4100 0.127 Uiso 1 1 calc R
H18C H 0.3780 -0.0539 0.3139 0.127 Uiso 1 1 calc R
C11' C -0.0359(6) 0.4659(4) 0.1846(4) 0.0896(18) Uani 1 1 d .
H11A H -0.1225 0.4799 0.1505 0.134 Uiso 1 1 calc R
H11B H -0.0589 0.4387 0.2473 0.134 Uiso 1 1 calc R
H11C H 0.0497 0.4148 0.1550 0.134 Uiso 1 1 calc R
C15' C 0.5885(6) 0.3083(5) 0.4097(3) 0.098(2) Uani 1 1 d .
H15A H 0.6166 0.3102 0.4704 0.148 Uiso 1 1 calc R
H15B H 0.6001 0.3688 0.3702 0.148 Uiso 1 1 calc R
H15C H 0.6530 0.2450 0.3833 0.148 Uiso 1 1 calc R
C9' C 0.0443(6) 0.6427(4) 0.0637(3) 0.0835(16) Uani 1 1 d .
H9'A H -0.0460 0.6568 0.0332 0.125 Uiso 1 1 calc R
H9'B H 0.1269 0.5913 0.0321 0.125 Uiso 1 1 calc R
H9'C H 0.0695 0.7068 0.0624 0.125 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'
O O 0.0106 0.0060 '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
O1' Si1' C1' 114.15(16)
O1' Si1' C5' 102.29(17)
C1' Si1' C5' 113.83(19)
O1' Si1' C4' 113.92(16)
C1' Si1' C4' 95.26(16)
C5' Si1' C4' 118.08(19)
C12' Si3' C14' 107.1(2)
C12' Si3' C13' 109.0(2)
C14' Si3' C13' 109.2(2)
C12' Si3' C7' 109.79(19)
C14' Si3' C7' 111.44(19)
C13' Si3' C7' 110.16(18)
C21' Si6' C22' 104.5(2)
C21' Si6' C23' 109.3(2)
C22' Si6' C23' 109.4(2)
C21' Si6' C4' 110.11(19)
C22' Si6' C4' 113.4(2)
C23' Si6' C4' 109.97(19)
C20' Si5' C19' 106.0(2)
C20' Si5' C18' 105.8(2)
C19' Si5' C18' 110.4(2)
C20' Si5' C3' 113.49(19)
C19' Si5' C3' 111.39(19)
C18' Si5' C3' 109.6(2)
C9' Si2' C10' 110.1(2)
C9' Si2' C11' 107.5(3)
C10' Si2' C11' 107.4(2)
C9' Si2' C7' 113.0(2)
C10' Si2' C7' 110.5(2)
C11' Si2' C7' 108.1(2)
C16' Si4' C15' 109.2(3)
C16' Si4' C17' 105.3(2)
C15' Si4' C17' 106.6(3)
C16' Si4' C2' 112.88(19)
C15' Si4' C2' 110.7(2)
C17' Si4' C2' 111.89(19)
C8' O1' Si1' 124.1(3)
C6' C1' C2' 127.0(3)
C6' C1' Si1' 121.9(3)
C2' C1' Si1' 110.5(2)
C1' C6' C7' 130.4(3)
C3' C4' Si1' 105.3(2)
C3' C4' Si6' 117.5(2)
Si1' C4' Si6' 116.4(2)
C6' C7' Si2' 109.4(2)
C6' C7' Si3' 111.6(2)
Si2' C7' Si3' 116.14(19)
C4' C3' C2' 113.3(3)
C4' C3' Si5' 113.5(2)
C2' C3' Si5' 112.6(2)
C1' C2' C3' 109.4(3)
C1' C2' Si4' 114.9(3)
C3' C2' Si4' 109.5(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Si1' O1' 1.648(3)
Si1' C1' 1.844(4)
Si1' C5' 1.846(4)
Si1' C4' 1.867(4)
Si3' C12' 1.861(5)
Si3' C14' 1.863(4)
Si3' C13' 1.864(4)
Si3' C7' 1.892(4)
Si6' C21' 1.860(5)
Si6' C22' 1.869(5)
Si6' C23' 1.876(5)
Si6' C4' 1.879(4)
Si5' C20' 1.859(5)
Si5' C19' 1.868(5)
Si5' C18' 1.871(5)
Si5' C3' 1.907(4)
Si2' C9' 1.858(5)
Si2' C10' 1.864(5)
Si2' C11' 1.864(5)
Si2' C7' 1.887(4)
Si4' C16' 1.862(4)
Si4' C15' 1.869(5)
Si4' C17' 1.870(4)
Si4' C2' 1.907(4)
O1' C8' 1.406(5)
C1' C6' 1.345(5)
C1' C2' 1.520(5)
C6' C7' 1.513(5)
C4' C3' 1.586(5)
C3' C2' 1.608(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
C1' Si1' O1' C8' -53.1(4)
C5' Si1' O1' C8' -176.5(3)
C4' Si1' O1' C8' 54.9(4)
O1' Si1' C1' C6' -29.7(4)
C5' Si1' C1' C6' 87.2(4)
C4' Si1' C1' C6' -148.9(3)
O1' Si1' C1' C2' 142.6(2)
C5' Si1' C1' C2' -100.5(3)
C4' Si1' C1' C2' 23.4(3)
C2' C1' C6' C7' 3.2(7)
Si1' C1' C6' C7' 174.2(3)
O1' Si1' C4' C3' -141.2(2)
C1' Si1' C4' C3' -21.8(3)
C5' Si1' C4' C3' 98.8(3)
O1' Si1' C4' Si6' 86.7(2)
C1' Si1' C4' Si6' -153.9(2)
C5' Si1' C4' Si6' -33.3(3)
C21' Si6' C4' C3' -163.0(3)
C22' Si6' C4' C3' 80.3(3)
C23' Si6' C4' C3' -42.5(3)
C21' Si6' C4' Si1' -36.8(3)
C22' Si6' C4' Si1' -153.5(2)
C23' Si6' C4' Si1' 83.7(3)
C1' C6' C7' Si2' -103.1(4)
C1' C6' C7' Si3' 127.0(4)
C9' Si2' C7' C6' -56.6(3)
C10' Si2' C7' C6' 179.4(3)
C11' Si2' C7' C6' 62.2(3)
C9' Si2' C7' Si3' 70.8(3)
C10' Si2' C7' Si3' -53.2(3)
C11' Si2' C7' Si3' -170.4(2)
C12' Si3' C7' C6' -34.9(3)
C14' Si3' C7' C6' 83.6(3)
C13' Si3' C7' C6' -155.0(3)
C12' Si3' C7' Si2' -161.3(2)
C14' Si3' C7' Si2' -42.7(3)
C13' Si3' C7' Si2' 78.6(3)
Si1' C4' C3' C2' 15.7(4)
Si6' C4' C3' C2' 147.1(3)
Si1' C4' C3' Si5' 145.70(19)
Si6' C4' C3' Si5' -82.8(3)
C20' Si5' C3' C4' -146.0(3)
C19' Si5' C3' C4' -26.5(3)
C18' Si5' C3' C4' 96.0(3)
C20' Si5' C3' C2' -15.6(3)
C19' Si5' C3' C2' 103.9(3)
C18' Si5' C3' C2' -133.6(3)
C6' C1' C2' C3' 155.2(4)
Si1' C1' C2' C3' -16.6(4)
C6' C1' C2' Si4' -81.2(4)
Si1' C1' C2' Si4' 107.0(2)
C4' C3' C2' C1' 0.2(4)
Si5' C3' C2' C1' -130.3(3)
C4' C3' C2' Si4' -126.6(3)
Si5' C3' C2' Si4' 102.9(2)
C16' Si4' C2' C1' 80.2(3)
C15' Si4' C2' C1' -42.5(4)
C17' Si4' C2' C1' -161.2(3)
C16' Si4' C2' C3' -156.2(3)
C15' Si4' C2' C3' 81.1(3)
C17' Si4' C2' C3' -37.6(3)
