#------------------------------------------------------------------------------
#$Date: 2011-09-17 23:27:16 +0300 (Sat, 17 Sep 2011) $
#$Revision: 26029 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/2013268.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_2013268
_journal_name_full  'Acta Crystallographica, Section C'
_journal_year  2003
_journal_volume  59
_journal_page_first  m109
_journal_page_last  m111
_publ_section_title
;
Ansa-[(tert-butylamino)(isodicyclopentadienyl)dimethylsilane]Zr(NMe~2~)~2~
prepared by an amine-elimination reaction
;
loop_
_publ_author_name
  'Gallucci, Judith C.'
  "Gentil, S\'ebastien"
  'Pirio, Nadine'
  'Meunier, Philippe'
  'Gallou, Fabrice'
  'Paquette, Leo A.'
_chemical_name_common
;
Ansa-[(tert-butylamino)(isodicyclopentadienyl)dimethylsilane]Zr(NMe~2~)~2~
;
_chemical_formula_moiety  'C20 H37 N3 Si Zr'
_chemical_formula_sum  'C20 H37 N3 Si Zr'
_chemical_formula_structural  '[Zr (C16 H25 N Si) (C2 H6 N)2]'
_chemical_formula_iupac  '[Zr (C16 H25 N Si) (C2 H6 N)2]'
_chemical_formula_weight  438.84
_symmetry_cell_setting  orthorhombic
_symmetry_space_group_name_H-M  'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
loop_
_symmetry_equiv_pos_as_xyz
  'x, y, z'
  'x+1/2, -y+1/2, -z'
  '-x, y+1/2, -z+1/2'
  '-x+1/2, -y, z+1/2'
  '-x, -y, -z'
  '-x-1/2, y-1/2, z'
  'x, -y-1/2, z-1/2'
  'x-1/2, y, -z-1/2'
_cell_length_a  10.5930(10)
_cell_length_b  15.134(2)
_cell_length_c  28.592(3)
_cell_angle_alpha  90
_cell_angle_beta  90
_cell_angle_gamma  90
_cell_volume  4583.7(9)
_cell_formula_units_Z  8
_cell_measurement_temperature  150(2)
_exptl_crystal_density_diffrn  1.272
_diffrn_ambient_temperature  150(2)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
  Zr 0.52498(2) 0.619386(15) 0.620355(8) 0.01794(9) Uani d . 1 . . Zr
  Si 0.25163(6) 0.56073(4) 0.62692(2) 0.01937(16) Uani d . 1 . . Si
  N1 0.39431(19) 0.53359(13) 0.65236(7) 0.0211(4) Uani d . 1 . . N
  N2 0.6881(2) 0.55190(16) 0.60438(8) 0.0320(5) Uani d . 1 . . N
  N3 0.5715(3) 0.70843(15) 0.67145(9) 0.0406(6) Uani d . 1 . . N
  C1 0.4905(2) 0.66138(16) 0.53311(8) 0.0194(5) Uani d . 1 . . C
  C2 0.4012(2) 0.59733(15) 0.54545(8) 0.0193(5) Uani d . 1 . . C
  H2 0.3952 0.5396 0.5326 0.023 Uiso calc R 1 . . H
  C3 0.3203(2) 0.63358(15) 0.58090(8) 0.0178(5) Uani d . 1 . . C
  C4 0.3603(2) 0.72356(15) 0.58790(8) 0.0192(5) Uani d . 1 . . C
  H4 0.3218 0.7653 0.6082 0.023 Uiso calc R 1 . . H
  C5 0.4666(2) 0.73885(15) 0.55939(8) 0.0193(5) Uani d . 1 . . C
  C6 0.5513(2) 0.81018(17) 0.54014(9) 0.0254(6) Uani d . 1 . . C
  H6 0.5685 0.8614 0.5613 0.030 Uiso calc R 1 . . H
  C7 0.4975(3) 0.83286(18) 0.49097(10) 0.0311(7) Uani d . 1 . . C
  H7A 0.4059 0.8455 0.4926 0.037 Uiso calc R 1 . . H
  H7B 0.5413 0.8846 0.4773 0.037 Uiso calc R 1 . . H
  C8 0.5235(3) 0.74808(19) 0.46191(9) 0.0315(6) Uani d . 1 . . C
  H8A 0.5791 0.7610 0.4349 0.038 Uiso calc R 1 . . H
  H8B 0.4438 0.7218 0.4503 0.038 Uiso calc R 1 . . H
  C9 0.5899(2) 0.68537(17) 0.49730(9) 0.0252(6) Uani d . 1 . . C
  H9 0.6387 0.6351 0.4836 0.030 Uiso calc R 1 . . H
  C10 0.6671(2) 0.75396(17) 0.52568(9) 0.0269(6) Uani d . 1 . . C
  H10A 0.7110 0.7274 0.5528 0.032 Uiso calc R 1 . . H
  H10B 0.7277 0.7872 0.5061 0.032 Uiso calc R 1 . . H
  C11 0.1415(3) 0.62432(18) 0.66512(10) 0.0327(6) Uani d . 1 . . C
  H11A 0.1039 0.5846 0.6883 0.049 Uiso calc R 1 . . H
  H11B 0.0745 0.6505 0.6459 0.049 Uiso calc R 1 . . H
  H11C 0.1881 0.6713 0.6812 0.049 Uiso calc R 1 . . H
  C12 0.1610(3) 0.46851(17) 0.59900(10) 0.0305(6) Uani d . 1 . . C
  H12A 0.0924 0.4931 0.5800 0.046 Uiso calc R 1 . . H
  H12B 0.1255 0.4303 0.6234 0.046 Uiso calc R 1 . . H
  H12C 0.2176 0.4339 0.5790 0.046 Uiso calc R 1 . . H
  C13 0.4185(3) 0.46247(18) 0.68666(10) 0.0345(7) Uani d D 1 . . C
  C14A 0.5416(4) 0.4785(3) 0.71187(14) 0.0490(13) Uani d P 0.821(6) A 1 C
  H14A 0.6099 0.4843 0.6890 0.073 Uiso calc PR 0.821(6) A 1 H
  H14B 0.5594 0.4287 0.7328 0.073 Uiso calc PR 0.821(6) A 1 H
  H14C 0.5354 0.5330 0.7302 0.073 Uiso calc PR 0.821(6) A 1 H
  C15A 0.4411(5) 0.3758(2) 0.65758(16) 0.0510(13) Uani d P 0.821(6) A 1 C
  H15A 0.5109 0.3851 0.6356 0.076 Uiso calc PR 0.821(6) A 1 H
  H15B 0.3643 0.3609 0.6402 0.076 Uiso calc PR 0.821(6) A 1 H
  H15C 0.4624 0.3272 0.6788 0.076 Uiso calc PR 0.821(6) A 1 H
  C16A 0.3117(4) 0.4483(4) 0.71881(17) 0.0646(17) Uani d P 0.821(6) A 1 C
  H16A 0.3312 0.3991 0.7399 0.097 Uiso calc PR 0.821(6) A 1 H
  H16B 0.2357 0.4343 0.7007 0.097 Uiso calc PR 0.821(6) A 1 H
  H16C 0.2973 0.5020 0.7372 0.097 Uiso calc PR 0.821(6) A 1 H
  C14B 0.402(2) 0.5159(13) 0.7350(6) 0.059(6) Uiso d PD 0.179(6) A 2 C
  H14D 0.3264 0.5532 0.7331 0.089 Uiso calc PR 0.179(6) A 2 H
  H14E 0.4762 0.5530 0.7403 0.089 Uiso calc PR 0.179(6) A 2 H
  H14F 0.3927 0.4739 0.7608 0.089 Uiso calc PR 0.179(6) A 2 H
  C15B 0.5513(17) 0.4164(17) 0.6908(10) 0.077(8) Uiso d PD 0.179(6) A 2 C
  H15D 0.6180 0.4610 0.6882 0.116 Uiso calc PR 0.179(6) A 2 H
  H15E 0.5608 0.3729 0.6657 0.116 Uiso calc PR 0.179(6) A 2 H
  H15F 0.5578 0.3866 0.7212 0.116 Uiso calc PR 0.179(6) A 2 H
  C16B 0.3047(16) 0.3961(12) 0.6934(7) 0.047(5) Uiso d PD 0.179(6) A 2 C
  H16D 0.3036 0.3536 0.6675 0.071 Uiso calc PR 0.179(6) A 2 H
  H16E 0.2251 0.4291 0.6938 0.071 Uiso calc PR 0.179(6) A 2 H
  H16F 0.3148 0.3643 0.7230 0.071 Uiso calc PR 0.179(6) A 2 H
  C17 0.6999(3) 0.4869(2) 0.56820(13) 0.0598(10) Uani d . 1 . . C
  H17A 0.6200 0.4823 0.5511 0.090 Uiso calc R 1 . . H
  H17B 0.7206 0.4296 0.5822 0.090 Uiso calc R 1 . . H
  H17C 0.7672 0.5044 0.5466 0.090 Uiso calc R 1 . . H
  C18 0.8094(3) 0.5652(3) 0.62702(14) 0.0591(10) Uani d . 1 . . C
  H18A 0.8011 0.6106 0.6513 0.089 Uiso calc R 1 . . H
  H18B 0.8716 0.5843 0.6038 0.089 Uiso calc R 1 . . H
  H18C 0.8372 0.5097 0.6413 0.089 Uiso calc R 1 . . H
  C19 0.4956(4) 0.7295(3) 0.71455(13) 0.0662(11) Uani d . 1 . . C
  H19A 0.4311 0.6840 0.7192 0.099 Uiso calc R 1 . . H
  H19B 0.4547 0.7872 0.7107 0.099 Uiso calc R 1 . . H
  H19C 0.5516 0.7312 0.7418 0.099 Uiso calc R 1 . . H
  C20 0.6559(5) 0.7791(3) 0.66411(14) 0.0848(16) Uani d . 1 . . C
  H20A 0.7010 0.7702 0.6346 0.127 Uiso calc R 1 . . H
  H20B 0.7167 0.7816 0.6899 0.127 Uiso calc R 1 . . H
  H20C 0.6086 0.8347 0.6628 0.127 Uiso calc R 1 . . H
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
  Zr 0.01658(14) 0.01852(14) 0.01872(14) -0.00120(9) -0.00261(9) 0.00062(9)
  Si 0.0180(3) 0.0171(3) 0.0230(3) -0.0016(3) 0.0015(3) 0.0024(3)
  N1 0.0229(11) 0.0210(10) 0.0195(11) -0.0002(9) -0.0018(9) 0.0039(8)
  N2 0.0217(12) 0.0413(14) 0.0329(12) 0.0086(10) 0.0004(10) 0.0044(11)
  N3 0.0570(16) 0.0265(12) 0.0382(14) -0.0043(12) -0.0197(13) -0.0057(11)
  C1 0.0192(13) 0.0216(13) 0.0174(12) 0.0026(10) -0.0011(10) 0.0017(10)
  C2 0.0222(13) 0.0186(12) 0.0169(12) 0.0003(10) -0.0048(10) -0.0007(9)
  C3 0.0150(12) 0.0184(12) 0.0199(12) -0.0002(9) -0.0032(10) 0.0028(9)
  C4 0.0175(12) 0.0170(12) 0.0233(13) 0.0027(10) 0.0007(10) 0.0017(10)
  C5 0.0174(12) 0.0184(12) 0.0219(12) -0.0004(10) -0.0020(10) 0.0038(10)
  C6 0.0214(14) 0.0224(13) 0.0324(15) -0.0043(10) 0.0021(11) 0.0043(11)
  C7 0.0257(15) 0.0312(15) 0.0364(16) -0.0033(11) 0.0016(12) 0.0167(13)
  C8 0.0278(15) 0.0429(16) 0.0237(14) -0.0047(13) 0.0047(11) 0.0100(12)
  C9 0.0218(14) 0.0301(14) 0.0237(13) 0.0009(11) 0.0056(11) 0.0007(11)
  C10 0.0185(13) 0.0322(14) 0.0300(14) -0.0032(11) 0.0028(11) 0.0072(12)
  C11 0.0286(15) 0.0322(15) 0.0372(16) 0.0029(12) 0.0101(13) 0.0045(12)
  C12 0.0273(15) 0.0251(14) 0.0391(16) -0.0057(11) -0.0044(12) 0.0046(12)
  C13 0.0350(16) 0.0318(15) 0.0367(16) -0.0028(13) -0.0091(13) 0.0172(12)
  C14A 0.059(3) 0.045(2) 0.043(2) -0.003(2) -0.026(2) 0.0227(19)
  C15A 0.070(3) 0.0232(19) 0.060(3) 0.0045(19) -0.020(2) 0.0098(17)
  C16A 0.056(3) 0.080(4) 0.057(3) 0.014(3) 0.016(2) 0.048(3)
  C17 0.051(2) 0.071(2) 0.057(2) 0.0331(19) -0.0021(18) -0.0169(19)
  C18 0.0292(17) 0.064(2) 0.084(3) 0.0085(17) -0.0139(18) 0.009(2)
  C19 0.091(3) 0.058(2) 0.049(2) -0.001(2) -0.003(2) -0.0160(19)
  C20 0.137(4) 0.071(3) 0.046(2) -0.059(3) -0.005(2) -0.011(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
  Zr N3 . 2.048(2) yes
  Zr N2 . 2.059(2) yes
  Zr N1 . 2.107(2) yes
  Zr C3 . 2.454(2) ?
  Zr C4 . 2.528(2) ?
  Zr C2 . 2.533(2) ?
  Zr C5 . 2.587(2) ?
  Zr C1 . 2.600(2) ?
  Zr Si . 3.0343(7) ?
  Si N1 . 1.727(2) yes
  Si C3 . 1.864(2) yes
  Si C11 . 1.866(3) ?
  Si C12 . 1.873(3) ?
  N1 C13 . 1.478(3) yes
  N2 C17 . 1.433(4) yes
  N2 C18 . 1.452(4) yes
  N3 C20 . 1.410(4) yes
  N3 C19 . 1.506(5) yes
  C1 C2 . 1.399(3) ?
  C1 C5 . 1.415(3) ?
  C1 C9 . 1.513(3) ?
  C2 C3 . 1.437(3) ?
  C2 H2 . 0.95 ?
  C3 C4 . 1.440(3) ?
  C4 C5 . 1.409(3) ?
  C4 H4 . 0.95 ?
  C5 C6 . 1.508(3) ?
  C6 C10 . 1.549(4) ?
  C6 C7 . 1.555(4) ?
  C6 H6 . 1.00 ?
  C7 C8 . 1.553(4) ?
  C7 H7A . 0.99 ?
  C7 H7B . 0.99 ?
  C8 C9 . 1.555(4) ?
  C8 H8A . 0.99 ?
  C8 H8B . 0.99 ?
  C9 C10 . 1.550(4) ?
  C9 H9 . 1.00 ?
  C10 H10A . 0.99 ?
  C10 H10B . 0.99 ?
  C11 H11A . 0.98 ?
  C11 H11B . 0.98 ?
  C11 H11C . 0.98 ?
  C12 H12A . 0.98 ?
  C12 H12B . 0.98 ?
  C12 H12C . 0.98 ?
  C13 C16A . 1.473(5) ?
  C13 C14A . 1.509(5) ?
  C13 C15A . 1.572(5) ?
  C13 C15B . 1.575(14) ?
  C13 C16B . 1.582(13) ?
  C13 C14B . 1.610(13) ?
  C14A H14A . 0.98 ?
  C14A H14B . 0.98 ?
  C14A H14C . 0.98 ?
  C15A H15A . 0.98 ?
  C15A H15B . 0.98 ?
  C15A H15C . 0.98 ?
  C16A H16A . 0.98 ?
  C16A H16B . 0.98 ?
  C16A H16C . 0.98 ?
  C14B H14D . 0.98 ?
  C14B H14E . 0.98 ?
  C14B H14F . 0.98 ?
  C15B H15D . 0.98 ?
  C15B H15E . 0.98 ?
  C15B H15F . 0.98 ?
  C16B H16D . 0.98 ?
  C16B H16E . 0.98 ?
  C16B H16F . 0.98 ?
  C17 H17A . 0.98 ?
  C17 H17B . 0.98 ?
  C17 H17C . 0.98 ?
  C18 H18A . 0.98 ?
  C18 H18B . 0.98 ?
  C18 H18C . 0.98 ?
  C19 H19A . 0.98 ?
  C19 H19B . 0.98 ?
  C19 H19C . 0.98 ?
  C20 H20A . 0.98 ?
  C20 H20B . 0.98 ?
  C20 H20C . 0.98 ?
_cod_database_code 2013268