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#$Date: 2012-02-24 19:13:23 +0200 (Fri, 24 Feb 2012) $
#$Revision: 34330 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/06/03/4060308.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_4060308
_journal_name_full  'Organometallics'
_journal_year       2005
_publ_section_title
;
 Trapping Unstable Terminal Ta-O Multiple Bonds of Monocyclopentadienyl Tantalum
 Complexes with a Lewis Acid
;
loop_
_publ_author_name
  'Sanchez-Nieves, J.'
  'Frutos, L. M.'
  'Royo, P.'
  'Castano, O.'
  'Herdtweck, E.'
_chemical_formula_sum 'C13 H20 N O5 P Si2 W'
_chemical_formula_weight  541.30
_symmetry_cell_setting  triclinic
_symmetry_space_group_name_H-M  'P -1'
loop_
_symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
_cell_length_a  6.9618(4)
_cell_length_b  9.6073(8)
_cell_length_c  16.1541(9)
_cell_angle_alpha  73.219(3)
_cell_angle_beta  89.975(3)
_cell_angle_gamma  81.823(3)
_cell_volume  1022.98(12)
_cell_formula_units_Z  2
_cell_measurement_temperature  133(2)
_exptl_crystal_density_diffrn  1.757
_diffrn_ambient_temperature  133(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
_atom_site_disorder_assembly
_atom_site_disorder_group
W W 0.261181(10) 0.716083(8) 0.116808(5) 0.01703(2) Uani 1 1 d . . .
N N -0.1900(3) 0.4336(2) 0.24210(13) 0.0367(4) Uani 1 1 d . . .
P P 0.21119(6) 0.46014(5) 0.18983(3) 0.01652(9) Uani 1 1 d . . .
H0 H 0.208(3) 0.382(2) 0.1354(14) 0.025(6) Uiso 1 1 d . . .
Si1 Si 0.27506(8) 0.35607(6) 0.39420(3) 0.02167(10) Uani 1 1 d U . .
Si2 Si 0.41973(8) 0.14789(6) 0.27166(3) 0.02091(10) Uani 1 1 d U . .
O1 O 0.0283(2) 0.70023(19) -0.04908(10) 0.0380(4) Uani 1 1 d . . .
O2 O -0.1250(2) 0.83559(19) 0.19606(12) 0.0451(4) Uani 1 1 d . . .
O3 O 0.2884(2) 1.04673(17) 0.01445(12) 0.0412(4) Uani 1 1 d . . .
O4 O 0.6480(2) 0.59289(17) 0.03919(10) 0.0328(3) Uani 1 1 d . . .
O5 O 0.5215(2) 0.72042(18) 0.27815(10) 0.0349(3) Uani 1 1 d . . .
C1 C 0.1083(3) 0.7053(2) 0.01169(13) 0.0244(4) Uani 1 1 d . . .
C2 C 0.0128(3) 0.7923(2) 0.16746(14) 0.0271(4) Uani 1 1 d . . .
C3 C 0.2853(3) 0.9260(2) 0.05228(14) 0.0273(4) Uani 1 1 d . . .
C4 C 0.5099(3) 0.6370(2) 0.06706(12) 0.0221(4) Uani 1 1 d . . .
C5 C 0.4272(3) 0.7202(2) 0.21995(13) 0.0236(4) Uani 1 1 d . . .
C6 C 0.3553(2) 0.34070(19) 0.28357(11) 0.0174(3) Uani 1 1 d U . .
H6 H 0.4825 0.3789 0.2774 0.021 Uiso 1 1 calc R . .
C7 C 0.1395(3) 0.5418(2) 0.38876(14) 0.0310(4) Uani 1 1 d U . .
H7A H 0.0142 0.5562 0.3575 0.037 Uiso 1 1 calc R . .
H7B H 0.2157 0.6179 0.3584 0.037 Uiso 1 1 calc R . .
H7C H 0.1175 0.5483 0.4475 0.037 Uiso 1 1 calc R . .
C8 C 0.5040(3) 0.3274(3) 0.46181(14) 0.0328(5) Uani 1 1 d U . .
H8A H 0.4714 0.3325 0.5200 0.039 Uiso 1 1 calc R . .
H8B H 0.5828 0.4040 0.4351 0.039 Uiso 1 1 calc R . .
H8C H 0.5775 0.2307 0.4657 0.039 Uiso 1 1 calc R . .
C9 C 0.1132(3) 0.2172(2) 0.44494(14) 0.0307(4) Uani 1 1 d U . .
H9A H 0.1818 0.1181 0.4512 0.037 Uiso 1 1 calc R . .
H9B H -0.0047 0.2345 0.4081 0.037 Uiso 1 1 calc R . .
H9C H 0.0778 0.2265 0.5020 0.037 Uiso 1 1 calc R . .
C10 C 0.5860(3) 0.0301(2) 0.36344(14) 0.0320(5) Uani 1 1 d U . .
H10A H 0.6244 -0.0668 0.3549 0.038 Uiso 1 1 calc R . .
H10B H 0.5190 0.0190 0.4178 0.038 Uiso 1 1 calc R . .
H10C H 0.7018 0.0763 0.3658 0.038 Uiso 1 1 calc R . .
C11 C 0.1942(3) 0.0656(2) 0.26610(15) 0.0321(5) Uani 1 1 d U . .
H11A H 0.1051 0.1326 0.2201 0.039 Uiso 1 1 calc R . .
H11B H 0.1312 0.0498 0.3217 0.039 Uiso 1 1 calc R . .
H11C H 0.2279 -0.0286 0.2536 0.039 Uiso 1 1 calc R . .
C12 C 0.5538(3) 0.1627(3) 0.17020(14) 0.0342(5) Uani 1 1 d U . .
H12A H 0.6622 0.2175 0.1704 0.041 Uiso 1 1 calc R . .
H12B H 0.4656 0.2144 0.1201 0.041 Uiso 1 1 calc R . .
H12C H 0.6041 0.0640 0.1668 0.041 Uiso 1 1 calc R . .
C13 C -0.0360(3) 0.4402(2) 0.22160(13) 0.0235(4) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
W 0.01575(4) 0.01504(4) 0.01936(4) -0.00395(3) 0.00147(2) -0.00150(2)
N 0.0265(10) 0.0383(11) 0.0426(12) -0.0068(9) -0.0004(8) -0.0061(8)
P 0.0159(2) 0.0161(2) 0.0177(2) -0.00515(17) 0.00028(15) -0.00250(17)
Si1 0.0244(3) 0.0239(3) 0.0178(3) -0.0074(2) 0.00223(18) -0.0045(2)
Si2 0.0241(3) 0.0172(2) 0.0201(3) -0.00514(19) -0.00080(18) 0.0010(2)
O1 0.0322(8) 0.0521(10) 0.0302(9) -0.0128(7) -0.0067(6) -0.0063(7)
O2 0.0320(9) 0.0371(10) 0.0631(12) -0.0138(9) 0.0178(8) 0.0038(7)
O3 0.0368(9) 0.0211(8) 0.0566(11) 0.0025(7) 0.0051(7) -0.0038(7)
O4 0.0272(8) 0.0378(9) 0.0299(8) -0.0083(7) 0.0064(6) 0.0036(6)
O5 0.0323(8) 0.0460(10) 0.0323(9) -0.0185(7) -0.0017(6) -0.0096(7)
C1 0.0202(9) 0.0243(10) 0.0268(10) -0.0049(8) 0.0033(7) -0.0026(7)
C2 0.0250(10) 0.0196(10) 0.0349(12) -0.0056(8) 0.0033(8) -0.0024(8)
C3 0.0216(9) 0.0256(11) 0.0331(11) -0.0069(8) 0.0015(7) -0.0009(8)
C4 0.0237(9) 0.0211(9) 0.0190(9) -0.0021(7) 0.0000(7) -0.0029(7)
C5 0.0237(9) 0.0220(10) 0.0274(10) -0.0105(8) 0.0069(7) -0.0042(7)
C6 0.0163(8) 0.0184(9) 0.0168(9) -0.0040(6) 0.0000(6) -0.0024(6)
C7 0.0384(12) 0.0295(11) 0.0285(11) -0.0142(9) 0.0097(8) -0.0042(9)
C8 0.0379(12) 0.0372(12) 0.0264(11) -0.0129(9) -0.0059(8) -0.0074(9)
C9 0.0336(11) 0.0331(12) 0.0245(11) -0.0059(9) 0.0069(8) -0.0074(9)
C10 0.0368(12) 0.0248(11) 0.0296(11) -0.0051(8) -0.0078(8) 0.0050(9)
C11 0.0366(12) 0.0234(11) 0.0397(13) -0.0141(9) -0.0020(9) -0.0051(9)
C12 0.0405(12) 0.0335(12) 0.0267(11) -0.0110(9) 0.0070(9) 0.0053(10)
C13 0.0227(9) 0.0196(9) 0.0264(10) -0.0034(7) -0.0038(7) -0.0042(7)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W C3 2.016(2) . ?
W C1 2.040(2) . ?
W C5 2.041(2) . ?
W C2 2.045(2) . ?
W C4 2.0491(19) . ?
W P 2.4753(5) . ?
N C13 1.127(3) . ?
P C6 1.8129(18) . ?
P C13 1.816(2) . ?
Si1 C8 1.874(2) . ?
Si1 C7 1.874(2) . ?
Si1 C9 1.875(2) . ?
Si1 C6 1.9121(18) . ?
Si2 C10 1.865(2) . ?
Si2 C12 1.865(2) . ?
Si2 C11 1.869(2) . ?
Si2 C6 1.9076(18) . ?
O1 C1 1.146(2) . ?
O2 C2 1.142(2) . ?
O3 C3 1.148(3) . ?
O4 C4 1.140(2) . ?
O5 C5 1.148(2) . ?
_cod_database_code 4060308