#------------------------------------------------------------------------------
#$Date: 2008-01-28 19:31:05 +0000 (Mon, 28 Jan 2008) $
#$Revision: 38 $
#$URL: svn://www.crystallography.net/cod/cif/8/8000068.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_8000068
loop_
_publ_author_name
'Hidenori Koshikawa'
'Masaaki Okazaki'
'Shun-ichi Matsumoto'
'Keiji Ueno'
'Hiromi Tobita'
'Hiroshi Ogino'
_publ_section_title
;
 Synthesis and Structure of a Base-stabilized Silyl(silylene)tantalum
 Complex
;
_journal_issue                   10
_journal_name_full               'Chemistry Letters'
_journal_page_first              1412
_journal_volume                  34
_journal_year                    2005
_chemical_formula_moiety         'C15 H35 O Si2 Ta '
_chemical_formula_sum            'C15 H35 O Si2 Ta '
_chemical_formula_weight         468.56
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 102.482(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.090(1)
_cell_length_b                   13.081(2)
_cell_length_c                   17.396(2)
_cell_measurement_reflns_used    15968
_cell_measurement_temperature    150.2
_cell_measurement_theta_max      26.8
_cell_measurement_theta_min      1.2
_cell_volume                     1797.4(5)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    'DIRDIF94 (PATTY)'
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9541
_diffrn_measured_fraction_theta_max 0.9541
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.052
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12703
_diffrn_reflns_theta_full        26.88
_diffrn_reflns_theta_max         26.88
_exptl_absorpt_coefficient_mu    6.233
_exptl_absorpt_correction_T_max  0.829
_exptl_absorpt_correction_T_min  0.514
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.02
_refine_diff_density_min         -1.55
_refine_ls_abs_structure_Flack   0.00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.213
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3704
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.0069
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.04900(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0882
_reflns_number_gt                3209
_reflns_number_total             3704
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,1/2+y,1/2-z
-x,-y,-z
1/2+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_calc_flag
Ta(1) Ta 0.09320(2) 0.23418(1) -0.002995(9) 0.01386(6) Uani 1.00 d
Si(1) Si 0.1323(2) 0.3707(1) -0.10665(7) 0.0176(3) Uani 1.00 d
Si(2) Si 0.1439(2) 0.1534(1) -0.13231(7) 0.0168(3) Uani 1.00 d
O(1) O 0.1481(5) 0.2781(3) -0.1869(2) 0.0225(8) Uani 1.00 d
C(1) C -0.1785(6) 0.3219(4) -0.0206(3) 0.024(1) Uani 1.00 d
C(2) C -0.1908(6) 0.2407(4) -0.0801(3) 0.023(1) Uani 1.00 d
C(3) C -0.1728(6) 0.1408(4) -0.0387(3) 0.025(1) Uani 1.00 d
C(4) C -0.1471(6) 0.1628(4) 0.0439(3) 0.026(1) Uani 1.00 d
C(5) C -0.1512(7) 0.2740(4) 0.0549(3) 0.025(1) Uani 1.00 d
C(6) C 0.3399(6) 0.3201(4) 0.0741(3) 0.026(1) Uani 1.00 d
C(7) C 0.3983(6) 0.2441(4) 0.0239(3) 0.023(1) Uani 1.00 d
C(8) C 0.3556(6) 0.1422(4) 0.0489(3) 0.025(1) Uani 1.00 d
C(9) C 0.2683(6) 0.1551(4) 0.1125(3) 0.024(1) Uani 1.00 d
C(10) C 0.2594(7) 0.2645(4) 0.1274(3) 0.026(1) Uani 1.00 d
C(11) C -0.0436(7) 0.4609(4) -0.1594(3) 0.027(1) Uani 1.00 d
C(12) C 0.3353(7) 0.4507(4) -0.1037(3) 0.026(1) Uani 1.00 d
C(13) C -0.0228(6) 0.0774(4) -0.2070(3) 0.025(1) Uani 1.00 d
C(14) C 0.3547(6) 0.0931(4) -0.1473(3) 0.028(1) Uani 1.00 d
C(15) C 0.1950(7) 0.2965(5) -0.2629(3) 0.030(1) Uani 1.00 d
H(1) H -0.1973 0.3934 -0.0315 0.0282 Uiso 1.00 calc
H(2) H -0.2206 0.2506 -0.1355 0.0276 Uiso 1.00 calc
H(3) H -0.1873 0.0755 -0.0632 0.0309 Uiso 1.00 calc
H(4) H -0.1386 0.1123 0.0846 0.0311 Uiso 1.00 calc
H(5) H -0.1453 0.3077 0.1043 0.0307 Uiso 1.00 calc
H(6) H 0.3622 0.3918 0.0747 0.0313 Uiso 1.00 calc
H(7) H 0.4658 0.2586 -0.0141 0.0286 Uiso 1.00 calc
H(8) H 0.3887 0.0785 0.0294 0.0306 Uiso 1.00 calc
H(9) H 0.2325 0.1015 0.1433 0.0293 Uiso 1.00 calc
H(10) H 0.2155 0.2945 0.1693 0.0315 Uiso 1.00 calc
H(11) H -0.0642 0.5123 -0.1229 0.0327 Uiso 1.00 calc
H(12) H -0.1455 0.4234 -0.1773 0.0327 Uiso 1.00 calc
H(13) H -0.0110 0.4931 -0.2022 0.0327 Uiso 1.00 calc
H(14) H 0.3463 0.5022 -0.0639 0.0335 Uiso 1.00 calc
H(15) H 0.3324 0.4820 -0.1529 0.0335 Uiso 1.00 calc
H(16) H 0.4335 0.4072 -0.0910 0.0335 Uiso 1.00 calc
H(17) H -0.1287 0.1133 -0.2168 0.0316 Uiso 1.00 calc
H(18) H 0.0129 0.0707 -0.2554 0.0316 Uiso 1.00 calc
H(19) H -0.0384 0.0118 -0.1868 0.0316 Uiso 1.00 calc
H(20) H 0.3514 0.0856 -0.2020 0.0350 Uiso 1.00 calc
H(21) H 0.4476 0.1372 -0.1250 0.0350 Uiso 1.00 calc
H(22) H 0.3719 0.0286 -0.1223 0.0350 Uiso 1.00 calc
H(23) H 0.1172 0.3436 -0.2932 0.0368 Uiso 1.00 calc
H(24) H 0.1930 0.2345 -0.2911 0.0368 Uiso 1.00 calc
H(25) H 0.3063 0.3253 -0.2545 0.0368 Uiso 1.00 calc
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ta(1) 0.0132(1) 0.0152(1) 0.0129(1) -0.00174(7) 0.00204(7) 0.00080(6)
Si(1) 0.0190(6) 0.0163(6) 0.0176(6) -0.0010(5) 0.0044(5) 0.0011(4)
Si(2) 0.0175(6) 0.0172(6) 0.0150(6) -0.0003(5) 0.0018(4) -0.0017(4)
O(1) 0.028(2) 0.022(2) 0.019(2) -0.002(1) 0.009(1) 0.000(1)
C(1) 0.012(2) 0.032(3) 0.028(2) 0.004(2) 0.007(2) 0.000(2)
C(2) 0.011(2) 0.034(3) 0.024(2) -0.003(2) 0.004(2) 0.002(2)
C(3) 0.014(2) 0.029(3) 0.031(2) -0.003(2) 0.005(2) -0.002(2)
C(4) 0.018(2) 0.031(2) 0.030(2) -0.002(2) 0.009(2) 0.007(2)
C(5) 0.020(3) 0.035(2) 0.027(2) -0.002(2) 0.016(2) -0.001(2)
C(6) 0.022(3) 0.028(3) 0.026(2) -0.011(2) 0.000(2) -0.007(2)
C(7) 0.006(2) 0.040(3) 0.022(2) -0.003(2) 0.001(2) 0.000(2)
C(8) 0.019(2) 0.032(3) 0.021(2) 0.008(2) -0.004(2) 0.002(2)
C(9) 0.026(3) 0.029(2) 0.014(2) -0.001(2) -0.003(2) 0.010(2)
C(10) 0.026(3) 0.033(2) 0.016(2) -0.003(2) -0.003(2) -0.005(2)
C(11) 0.028(3) 0.023(3) 0.028(3) 0.007(2) 0.004(2) 0.007(2)
C(12) 0.027(2) 0.024(3) 0.030(3) -0.009(2) 0.008(2) 0.001(2)
C(13) 0.027(3) 0.025(3) 0.019(2) -0.002(2) 0.001(2) -0.003(2)
C(14) 0.020(2) 0.033(3) 0.032(3) 0.003(2) 0.007(2) -0.007(2)
C(15) 0.043(3) 0.035(3) 0.015(2) -0.009(3) 0.010(2) -0.003(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
Si Si 0.082 0.070
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
O O 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Ta Ta -0.705 6.523
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
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
Si(1) Ta(1) Si(2) 67.30(4) yes
Si(1) Ta(1) C(1) 80.3(1) yes
Si(1) Ta(1) C(2) 80.4(1) yes
Si(1) Ta(1) C(3) 113.6(1) yes
Si(1) Ta(1) C(4) 135.7(1) yes
Si(1) Ta(1) C(5) 111.5(1) yes
Si(1) Ta(1) C(6) 81.8(1) yes
Si(1) Ta(1) C(7) 79.9(1) yes
Si(1) Ta(1) C(8) 111.6(1) yes
Si(1) Ta(1) C(9) 136.8(1) yes
Si(1) Ta(1) C(10) 114.4(1) yes
Si(2) Ta(1) C(1) 112.9(1) yes
Si(2) Ta(1) C(2) 80.9(1) yes
Si(2) Ta(1) C(3) 82.6(1) yes
Si(2) Ta(1) C(4) 114.7(1) yes
Si(2) Ta(1) C(5) 137.0(1) yes
Si(2) Ta(1) C(6) 113.7(1) yes
Si(2) Ta(1) C(7) 81.0(2) yes
Si(2) Ta(1) C(8) 80.3(1) yes
Si(2) Ta(1) C(9) 111.8(1) yes
Si(2) Ta(1) C(10) 136.3(2) yes
C(1) Ta(1) C(2) 35.4(2) yes
C(1) Ta(1) C(3) 58.8(2) yes
C(1) Ta(1) C(4) 57.5(2) yes
C(1) Ta(1) C(5) 33.9(2) yes
C(1) Ta(1) C(6) 117.5(2) yes
C(1) Ta(1) C(7) 148.7(2) yes
C(1) Ta(1) C(8) 165.4(2) yes
C(1) Ta(1) C(9) 130.8(2) yes
C(1) Ta(1) C(10) 110.2(2) yes
C(2) Ta(1) C(3) 35.7(2) yes
C(2) Ta(1) C(4) 57.8(2) yes
C(2) Ta(1) C(5) 57.6(2) yes
C(2) Ta(1) C(6) 150.1(2) yes
C(2) Ta(1) C(7) 157.2(2) yes
C(2) Ta(1) C(8) 151.3(2) yes
C(2) Ta(1) C(9) 142.7(2) yes
C(2) Ta(1) C(10) 142.5(2) yes
C(3) Ta(1) C(4) 34.2(2) yes
C(3) Ta(1) C(5) 57.8(2) yes
C(3) Ta(1) C(6) 161.6(2) yes
C(3) Ta(1) C(7) 152.4(2) yes
C(3) Ta(1) C(8) 119.9(2) yes
C(3) Ta(1) C(9) 108.8(2) yes
C(3) Ta(1) C(10) 127.3(2) yes
C(4) Ta(1) C(5) 34.8(2) yes
C(4) Ta(1) C(6) 127.5(2) yes
C(4) Ta(1) C(7) 143.8(2) yes
C(4) Ta(1) C(8) 112.2(2) yes
C(4) Ta(1) C(9) 85.7(2) yes
C(4) Ta(1) C(10) 94.1(2) yes
C(5) Ta(1) C(6) 108.3(2) yes
C(5) Ta(1) C(7) 141.9(2) yes
C(5) Ta(1) C(8) 131.7(2) yes
C(5) Ta(1) C(9) 97.4(2) yes
C(5) Ta(1) C(10) 85.1(2) yes
C(6) Ta(1) C(7) 35.3(2) yes
C(6) Ta(1) C(8) 58.5(2) yes
C(6) Ta(1) C(9) 58.4(2) yes
C(6) Ta(1) C(10) 34.7(2) yes
C(7) Ta(1) C(8) 35.2(2) yes
C(7) Ta(1) C(9) 58.2(2) yes
C(7) Ta(1) C(10) 57.9(2) yes
C(8) Ta(1) C(9) 34.6(2) yes
C(8) Ta(1) C(10) 57.8(2) yes
C(9) Ta(1) C(10) 35.1(2) yes
Ta(1) Si(1) O(1) 96.3(1) yes
Ta(1) Si(1) C(11) 124.3(2) yes
Ta(1) Si(1) C(12) 125.5(2) yes
O(1) Si(1) C(11) 101.8(2) yes
O(1) Si(1) C(12) 100.1(2) yes
C(11) Si(1) C(12) 102.5(3) yes
Ta(1) Si(2) O(1) 96.1(1) yes
Ta(1) Si(2) C(13) 125.0(2) yes
Ta(1) Si(2) C(14) 126.0(2) yes
O(1) Si(2) C(13) 101.1(2) yes
O(1) Si(2) C(14) 99.8(2) yes
C(13) Si(2) C(14) 101.9(2) yes
Si(1) O(1) Si(2) 99.9(2) yes
Si(1) O(1) C(15) 129.4(4) yes
Si(2) O(1) C(15) 128.9(4) yes
Ta(1) C(1) C(2) 70.8(3) yes
Ta(1) C(1) C(5) 73.9(3) yes
C(2) C(1) C(5) 107.7(5) yes
Ta(1) C(2) C(1) 73.8(3) yes
Ta(1) C(2) C(3) 73.5(3) yes
C(1) C(2) C(3) 108.0(5) yes
Ta(1) C(3) C(2) 70.8(3) yes
Ta(1) C(3) C(4) 73.5(3) yes
C(2) C(3) C(4) 106.8(5) yes
Ta(1) C(4) C(3) 72.3(3) yes
Ta(1) C(4) C(5) 73.0(3) yes
C(3) C(4) C(5) 109.0(5) yes
Ta(1) C(5) C(1) 72.3(3) yes
Ta(1) C(5) C(4) 72.2(3) yes
C(1) C(5) C(4) 108.6(5) yes
Ta(1) C(6) C(7) 71.9(3) yes
Ta(1) C(6) C(10) 71.9(3) yes
C(7) C(6) C(10) 106.9(5) yes
Ta(1) C(7) C(6) 72.8(3) yes
Ta(1) C(7) C(8) 73.3(3) yes
C(6) C(7) C(8) 108.2(5) yes
Ta(1) C(8) C(7) 71.6(3) yes
Ta(1) C(8) C(9) 72.3(3) yes
C(7) C(8) C(9) 107.9(5) yes
Ta(1) C(9) C(8) 73.1(3) yes
Ta(1) C(9) C(10) 71.7(3) yes
C(8) C(9) C(10) 107.5(5) yes
Ta(1) C(10) C(6) 73.4(3) yes
Ta(1) C(10) C(9) 73.2(3) yes
C(6) C(10) C(9) 109.6(5) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Ta(1) Si(1) 2.605(1) yes
Ta(1) Si(2) 2.597(1) yes
Ta(1) C(1) 2.440(5) yes
Ta(1) C(2) 2.399(6) yes
Ta(1) C(3) 2.435(5) yes
Ta(1) C(4) 2.450(5) yes
Ta(1) C(5) 2.461(6) yes
Ta(1) C(6) 2.426(5) yes
Ta(1) C(7) 2.414(5) yes
Ta(1) C(8) 2.437(5) yes
Ta(1) C(9) 2.426(5) yes
Ta(1) C(10) 2.406(5) yes
Si(1) O(1) 1.873(4) yes
Si(1) C(11) 1.922(6) yes
Si(1) C(12) 1.939(6) yes
Si(2) O(1) 1.891(4) yes
Si(2) C(13) 1.933(5) yes
Si(2) C(14) 1.947(6) yes
O(1) C(15) 1.473(6) yes
C(1) C(2) 1.472(8) yes
C(1) C(5) 1.428(8) yes
C(2) C(3) 1.484(8) yes
C(3) C(4) 1.435(8) yes
C(4) C(5) 1.469(9) yes
C(6) C(7) 1.467(8) yes
C(6) C(10) 1.439(8) yes
C(7) C(8) 1.467(8) yes
C(8) C(9) 1.445(8) yes
C(9) C(10) 1.459(8) yes
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
Ta(1) Si(1) 2.605(1) .
Ta(1) Si(2) 2.597(1) .
C(5) C(7) 3.588(8) 1_455