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#$Date: 2016-03-21 06:28:52 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178513 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/16/4061689.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_4061689
loop_
_publ_author_name
'Esteruelas, M. A.'
'López, A. M. L.'
'Mateo, A. C.'
'Oñate, E.'
_publ_section_title
;
New Titanium Complexes Containing a Cyclopentadienyl Ligand with a Pendant
Aminoalkyl Substituent: Preparation, Behavior of the Amino Group, and Catalytic
Hydroamination of Alkynes
;
_journal_name_full               Organometallics
_journal_paper_doi               10.1021/om050542v
_journal_year                    2005
_chemical_formula_sum            'C33 H49 N3 Ti'
_chemical_formula_weight         535.65
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 112.791(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.038(2)
_cell_length_b                   11.1820(14)
_cell_length_c                   17.564(2)
_cell_measurement_temperature    100(2)
_cell_volume                     3084.9(7)
_diffrn_ambient_temperature      100(2)
_exptl_crystal_density_diffrn    1.153
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4061689
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Ti Ti -0.01043(3) 0.46556(5) 0.74535(3) 0.02762(15) Uani 1 1 d . . .
N1 N -0.05811(14) 0.3780(2) 0.79750(13) 0.0266(6) Uani 1 1 d . . .
N2 N 0.06808(15) 0.3532(2) 0.72865(14) 0.0250(6) Uani 1 1 d . . .
H1 H 0.0621(19) 0.289(2) 0.7454(17) 0.042(11) Uiso 1 1 d . . .
N3 N 0.06025(16) 0.5814(2) 0.85347(14) 0.0338(6) Uani 1 1 d . . .
C1 C -0.09398(18) 0.3168(2) 0.84444(16) 0.0234(7) Uani 1 1 d . . .
C2 C -0.05115(18) 0.2207(2) 0.89430(16) 0.0241(7) Uani 1 1 d . . .
C3 C 0.03471(18) 0.1793(3) 0.89795(17) 0.0292(8) Uani 1 1 d . . .
H3 H 0.0531 0.2364 0.8643 0.035 Uiso 1 1 calc R . .
C4 C 0.02774(19) 0.0557(3) 0.85893(17) 0.0438(9) Uani 1 1 d . . .
H4A H 0.0086 -0.0022 0.8899 0.066 Uiso 1 1 calc R . .
H4B H 0.0835 0.0315 0.8602 0.066 Uiso 1 1 calc R . .
H4C H -0.0134 0.0585 0.8016 0.066 Uiso 1 1 calc R . .
C5 C 0.10326(19) 0.1801(3) 0.98573(17) 0.0419(9) Uani 1 1 d . . .
H5A H 0.1087 0.2610 1.0087 0.063 Uiso 1 1 calc R . .
H5B H 0.1578 0.1552 0.9843 0.063 Uiso 1 1 calc R . .
H5C H 0.0871 0.1246 1.0204 0.063 Uiso 1 1 calc R . .
C6 C -0.08900(19) 0.1598(3) 0.94071(16) 0.0318(8) Uani 1 1 d . . .
H6 H -0.0596 0.0949 0.9747 0.038 Uiso 1 1 calc R . .
C7 C -0.16790(19) 0.1919(3) 0.93819(17) 0.0334(8) Uani 1 1 d . . .
H7 H -0.1937 0.1478 0.9685 0.040 Uiso 1 1 calc R . .
C8 C -0.20915(19) 0.2891(3) 0.89102(16) 0.0305(7) Uani 1 1 d . . .
H8 H -0.2624 0.3134 0.8914 0.037 Uiso 1 1 calc R . .
C9 C -0.17493(18) 0.3520(3) 0.84326(16) 0.0262(7) Uani 1 1 d . . .
C10 C -0.22403(18) 0.4526(3) 0.78806(17) 0.0309(7) Uani 1 1 d . . .
H10 H -0.1817 0.5038 0.7767 0.037 Uiso 1 1 calc R . .
C11 C -0.2837(2) 0.4021(3) 0.70578(19) 0.0556(10) Uani 1 1 d . . .
H11A H -0.2515 0.3514 0.6827 0.083 Uiso 1 1 calc R . .
H11B H -0.3101 0.4679 0.6676 0.083 Uiso 1 1 calc R . .
H11C H -0.3281 0.3544 0.7139 0.083 Uiso 1 1 calc R . .
C12 C -0.2723(2) 0.5333(3) 0.82445(19) 0.0584(10) Uani 1 1 d . . .
H12A H -0.3172 0.4873 0.8328 0.088 Uiso 1 1 calc R . .
H12B H -0.2977 0.5997 0.7865 0.088 Uiso 1 1 calc R . .
H12C H -0.2329 0.5650 0.8775 0.088 Uiso 1 1 calc R . .
C13 C 0.09934(18) 0.3278(3) 0.66546(16) 0.0233(7) Uani 1 1 d . . .
C14 C 0.05720(18) 0.2427(3) 0.60446(16) 0.0261(7) Uani 1 1 d . . .
C15 C -0.02314(18) 0.1798(3) 0.60034(17) 0.0315(8) Uani 1 1 d . . .
H15 H -0.0434 0.2216 0.6397 0.038 Uiso 1 1 calc R . .
C16 C -0.09466(19) 0.1865(3) 0.51495(18) 0.0516(10) Uani 1 1 d . . .
H16A H -0.1033 0.2699 0.4964 0.077 Uiso 1 1 calc R . .
H16B H -0.1473 0.1551 0.5176 0.077 Uiso 1 1 calc R . .
H16C H -0.0794 0.1388 0.4760 0.077 Uiso 1 1 calc R . .
C17 C -0.00513(19) 0.0503(3) 0.62861(18) 0.0437(9) Uani 1 1 d . . .
H17A H 0.0146 0.0066 0.5910 0.066 Uiso 1 1 calc R . .
H17B H -0.0573 0.0132 0.6283 0.066 Uiso 1 1 calc R . .
H17C H 0.0389 0.0479 0.6847 0.066 Uiso 1 1 calc R . .
C18 C 0.09188(19) 0.2150(3) 0.54592(16) 0.0318(8) Uani 1 1 d . . .
H18 H 0.0651 0.1562 0.5050 0.038 Uiso 1 1 calc R . .
C19 C 0.16382(19) 0.2716(3) 0.54677(17) 0.0331(8) Uani 1 1 d . . .
H19 H 0.1869 0.2507 0.5073 0.040 Uiso 1 1 calc R . .
C20 C 0.20241(18) 0.3583(3) 0.60476(16) 0.0303(7) Uani 1 1 d . . .
H20 H 0.2510 0.3987 0.6036 0.036 Uiso 1 1 calc R . .
C21 C 0.17158(18) 0.3884(2) 0.66547(16) 0.0235(7) Uani 1 1 d . . .
C22 C 0.21737(17) 0.4786(3) 0.73161(16) 0.0282(7) Uani 1 1 d . . .
H22 H 0.1737 0.5145 0.7498 0.034 Uiso 1 1 calc R . .
C23 C 0.28263(18) 0.4165(2) 0.80692(16) 0.0334(8) Uani 1 1 d . . .
H23A H 0.2538 0.3576 0.8284 0.050 Uiso 1 1 calc R . .
H23B H 0.3110 0.4760 0.8497 0.050 Uiso 1 1 calc R . .
H23C H 0.3250 0.3760 0.7910 0.050 Uiso 1 1 calc R . .
C24 C 0.25771(18) 0.5817(3) 0.70288(17) 0.0403(9) Uani 1 1 d . . .
H24A H 0.3049 0.5514 0.6897 0.060 Uiso 1 1 calc R . .
H24B H 0.2792 0.6416 0.7469 0.060 Uiso 1 1 calc R . .
H24C H 0.2149 0.6185 0.6536 0.060 Uiso 1 1 calc R . .
C25 C -0.0294(2) 0.6666(3) 0.69430(19) 0.0359(8) Uani 1 1 d . . .
C26 C 0.0050(2) 0.6057(3) 0.64497(18) 0.0369(8) Uani 1 1 d . . .
H26 H 0.0584 0.6212 0.6417 0.044 Uiso 1 1 calc R . .
C27 C -0.0536(2) 0.5177(3) 0.60124(17) 0.0404(9) Uani 1 1 d . . .
H27 H -0.0465 0.4624 0.5634 0.048 Uiso 1 1 calc R . .
C28 C -0.12479(19) 0.5249(3) 0.62280(17) 0.0369(8) Uani 1 1 d . . .
H28 H -0.1740 0.4757 0.6025 0.044 Uiso 1 1 calc R . .
C29 C -0.10941(19) 0.6188(3) 0.68009(19) 0.0381(8) Uani 1 1 d . . .
H29 H -0.1471 0.6451 0.7048 0.046 Uiso 1 1 calc R . .
C30 C 0.0172(2) 0.7569(3) 0.7601(2) 0.0473(9) Uani 1 1 d . . .
H30A H -0.0227 0.7933 0.7821 0.057 Uiso 1 1 calc R . .
H30B H 0.0402 0.8213 0.7360 0.057 Uiso 1 1 calc R . .
C31 C 0.0900(2) 0.6951(3) 0.8299(2) 0.0437(9) Uani 1 1 d . . .
H31A H 0.1372 0.6784 0.8118 0.052 Uiso 1 1 calc R . .
H31B H 0.1119 0.7488 0.8785 0.052 Uiso 1 1 calc R . .
C32 C 0.13488(19) 0.5160(3) 0.91187(16) 0.0398(8) Uani 1 1 d . . .
H32A H 0.1741 0.4973 0.8849 0.060 Uiso 1 1 calc R . .
H32B H 0.1159 0.4416 0.9288 0.060 Uiso 1 1 calc R . .
H32C H 0.1641 0.5658 0.9606 0.060 Uiso 1 1 calc R . .
C33 C 0.0041(2) 0.6093(3) 0.89805(18) 0.0440(9) Uani 1 1 d . . .
H33A H 0.0350 0.6597 0.9460 0.066 Uiso 1 1 calc R . .
H33B H -0.0132 0.5348 0.9166 0.066 Uiso 1 1 calc R . .
H33C H -0.0466 0.6519 0.8610 0.066 Uiso 1 1 calc R . .
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
Ti N1 1.742(2) . ?
Ti N2 1.939(2) . ?
Ti N3 2.227(2) . ?
Ti C29 2.365(3) . ?
Ti C28 2.371(3) . ?
Ti C25 2.395(3) . ?
Ti C27 2.418(3) . ?
Ti C26 2.448(3) . ?
N1 C1 1.383(3) . ?
N2 C13 1.433(3) . ?
N2 H1 0.80(3) . ?
N3 C32 1.481(3) . ?
N3 C33 1.485(3) . ?
N3 C31 1.486(3) . ?
C1 C2 1.400(4) . ?
C1 C9 1.427(4) . ?
C2 C6 1.397(3) . ?
C2 C3 1.512(4) . ?
C3 C4 1.526(4) . ?
C3 C5 1.532(4) . ?
C3 H3 1.0000 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.375(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.382(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.385(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.508(4) . ?
C10 C11 1.517(4) . ?
C10 C12 1.519(4) . ?
C10 H10 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.404(4) . ?
C13 C21 1.405(4) . ?
C14 C18 1.405(3) . ?
C14 C15 1.516(4) . ?
C15 C17 1.523(4) . ?
C15 C16 1.524(4) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.374(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.376(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.400(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.507(4) . ?
C22 C24 1.525(3) . ?
C22 C23 1.526(3) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C29 1.394(4) . ?
C25 C26 1.396(4) . ?
C25 C30 1.508(4) . ?
C26 C27 1.400(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.406(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.407(4) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C30 C31 1.530(4) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
