#------------------------------------------------------------------------------
#$Date: 2016-03-21 08:19:26 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178602 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/13/4071391.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_4071391
loop_
_publ_author_name
'Nikiforov, Grigory B.'
'Roesky, Herbert W.'
'Heisen, Burkhard C.'
'Oswald, Rainer B.'
_publ_section_title
;
 Formation of a Titanium Complex with a TiCHAl2Structural Unit
 from LTiMe3and Trimethylaluminum§
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2544
_journal_paper_doi               10.1021/om800144v
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C32 H50 N2 Ti'
_chemical_formula_weight         510.64
_chemical_name_systematic
;
?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.245(3)
_cell_length_b                   22.068(4)
_cell_length_c                   10.071(2)
_cell_measurement_reflns_used    9559
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      56.91
_cell_measurement_theta_min      4.01
_cell_volume                     3165.9(11)
_computing_cell_refinement       'Bruker SAINT (V. 7.12A, Siemens 2003)'
_computing_data_collection       'Proteum (Version 1.40, Bruker 2002)'
_computing_data_reduction        'Bruker SAINT (V. 7.12A, Siemens 2003)'
_computing_molecular_graphics    'Bruker AXS SHELXTL (V. 6.12)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.602
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker three circle diffractometer'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  'mirror system'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0723
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            18161
_diffrn_reflns_theta_full        57.11
_diffrn_reflns_theta_max         57.11
_diffrn_reflns_theta_min         4.01
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.420
_exptl_absorpt_correction_T_max  0.9094
_exptl_absorpt_correction_T_min  0.7939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.071
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         2180
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0448
_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)+(0.0384P)²+3.2744P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1078
_reflns_number_gt                1771
_reflns_number_total             2180
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800144v-file003.cif
_cod_data_source_block           structure1
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               4071391
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, 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
Ti1 Ti 0.14180(5) 0.7500 0.22871(7) 0.0262(2) Uani 1 2 d S
N1 N 0.08303(15) 0.68312(9) 0.0958(2) 0.0236(5) Uani 1 1 d .
C6 C 0.12144(18) 0.62095(11) 0.0855(3) 0.0242(7) Uani 1 1 d .
C3 C -0.0385(3) 0.7500 0.0052(4) 0.0262(9) Uani 1 2 d S
H3 H -0.1006 0.7500 -0.0292 0.031 Uiso 1 2 calc SR
C4 C 0.00124(18) 0.69220(12) 0.0271(3) 0.0245(6) Uani 1 1 d .
C9 C 0.1932(2) 0.50244(12) 0.0550(3) 0.0346(7) Uani 1 1 d .
H9 H 0.2167 0.4624 0.0442 0.041 Uiso 1 1 calc R
C11 C 0.09076(18) 0.57415(12) 0.1733(3) 0.0265(7) Uani 1 1 d .
C10 C 0.1283(2) 0.51523(12) 0.1551(3) 0.0329(7) Uani 1 1 d .
H10 H 0.1087 0.4835 0.2126 0.039 Uiso 1 1 calc R
C1 C 0.2543(2) 0.68604(14) 0.2745(4) 0.0458(9) Uani 1 1 d .
H1A H 0.2794 0.6947 0.3631 0.069 Uiso 1 1 calc R
H1B H 0.3045 0.6901 0.2085 0.069 Uiso 1 1 calc R
H1C H 0.2295 0.6446 0.2725 0.069 Uiso 1 1 calc R
C8 C 0.2236(2) 0.54907(12) -0.0296(3) 0.0336(7) Uani 1 1 d .
H8 H 0.2678 0.5403 -0.0975 0.040 Uiso 1 1 calc R
C7 C 0.1895(2) 0.60887(12) -0.0155(3) 0.0299(7) Uani 1 1 d .
C12 C 0.0190(2) 0.58528(12) 0.2869(3) 0.0327(7) Uani 1 1 d .
H12 H -0.0047 0.6277 0.2785 0.039 Uiso 1 1 calc R
C5 C -0.0513(2) 0.63799(12) -0.0345(3) 0.0331(7) Uani 1 1 d .
H5A H -0.0098 0.6169 -0.0970 0.050 Uiso 1 1 calc R
H5B H -0.1071 0.6526 -0.0817 0.050 Uiso 1 1 calc R
H5C H -0.0705 0.6100 0.0359 0.050 Uiso 1 1 calc R
C13 C -0.0673(2) 0.54146(14) 0.2793(3) 0.0464(9) Uani 1 1 d .
H13A H -0.0961 0.5443 0.1912 0.070 Uiso 1 1 calc R
H13B H -0.1134 0.5529 0.3470 0.070 Uiso 1 1 calc R
H13C H -0.0464 0.4998 0.2950 0.070 Uiso 1 1 calc R
C2 C 0.0529(3) 0.7500 0.3953(4) 0.0400(11) Uani 1 2 d S
H2A H 0.0725 0.7180 0.4569 0.060 Uiso 0.50 1 calc PR
H2B H -0.0119 0.7426 0.3668 0.060 Uiso 0.50 1 calc PR
H2C H 0.0566 0.7894 0.4399 0.060 Uiso 0.50 1 calc PR
C15 C 0.2257(2) 0.65909(13) -0.1098(3) 0.0450(9) Uani 1 1 d .
H15 H 0.2045 0.6989 -0.0731 0.054 Uiso 1 1 calc R
C14 C 0.0669(2) 0.57892(14) 0.4247(3) 0.0419(8) Uani 1 1 d .
H14A H 0.0899 0.5374 0.4358 0.063 Uiso 1 1 calc R
H14B H 0.0213 0.5882 0.4947 0.063 Uiso 1 1 calc R
H14C H 0.1198 0.6072 0.4305 0.063 Uiso 1 1 calc R
C17 C 0.1841(3) 0.65286(18) -0.2504(4) 0.0675(12) Uani 1 1 d .
H17A H 0.2014 0.6134 -0.2876 0.101 Uiso 1 1 calc R
H17B H 0.2087 0.6852 -0.3072 0.101 Uiso 1 1 calc R
H17C H 0.1155 0.6560 -0.2457 0.101 Uiso 1 1 calc R
C16 C 0.3356(2) 0.66043(16) -0.1159(4) 0.0578(10) Uani 1 1 d .
H16A H 0.3586 0.6223 -0.1538 0.087 Uiso 1 1 calc R
H16B H 0.3609 0.6655 -0.0261 0.087 Uiso 1 1 calc R
H16C H 0.3560 0.6944 -0.1717 0.087 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 0.0181 0.0091 '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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C2 Ti1 N1 105.12(11) . .
C2 Ti1 N1 105.12(11) . 7_575
N1 Ti1 N1 86.14(11) . 7_575
C2 Ti1 C1 105.87(14) . 7_575
N1 Ti1 C1 148.88(12) . 7_575
N1 Ti1 C1 88.50(10) 7_575 7_575
C2 Ti1 C1 105.87(14) . .
N1 Ti1 C1 88.50(10) . .
N1 Ti1 C1 148.88(12) 7_575 .
C1 Ti1 C1 80.48(16) 7_575 .
C4 N1 C6 114.5(2) . .
C4 N1 Ti1 122.84(16) . .
C6 N1 Ti1 122.20(16) . .
C11 C6 C7 120.9(2) . .
C11 C6 N1 120.9(2) . .
C7 C6 N1 118.2(2) . .
C4 C3 C4 129.0(4) 7_575 .
N1 C4 C3 123.5(2) . .
N1 C4 C5 120.2(2) . .
C3 C4 C5 116.3(2) . .
C10 C9 C8 119.6(3) . .
C10 C11 C6 117.9(3) . .
C10 C11 C12 119.2(2) . .
C6 C11 C12 122.9(2) . .
C9 C10 C11 121.9(3) . .
C9 C8 C7 121.2(3) . .
C8 C7 C6 118.6(2) . .
C8 C7 C15 119.5(3) . .
C6 C7 C15 121.9(2) . .
C14 C12 C11 110.8(2) . .
C14 C12 C13 109.4(2) . .
C11 C12 C13 112.5(2) . .
C17 C15 C7 111.8(3) . .
C17 C15 C16 110.5(3) . .
C7 C15 C16 111.8(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 C2 2.102(4) .
Ti1 N1 2.161(2) .
Ti1 N1 2.161(2) 7_575
Ti1 C1 2.185(3) 7_575
Ti1 C1 2.185(3) .
N1 C4 1.370(3) .
N1 C6 1.481(3) .
C6 C11 1.428(4) .
C6 C7 1.430(4) .
C3 C4 1.413(3) 7_575
C3 C4 1.413(3) .
C4 C5 1.542(4) .
C9 C10 1.397(4) .
C9 C8 1.404(4) .
C11 C10 1.418(4) .
C11 C12 1.553(4) .
C8 C7 1.413(4) .
C7 C15 1.548(4) .
C12 C14 1.552(4) .
C12 C13 1.566(4) .
C15 C17 1.541(5) .
C15 C16 1.566(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
_geom_torsion_site_symmetry_1
C2 Ti1 N1 C4 72.0(2) .
N1 Ti1 N1 C4 -32.7(2) 7_575
C1 Ti1 N1 C4 -113.3(2) 7_575
C1 Ti1 N1 C4 178.0(2) .
C2 Ti1 N1 C6 -99.8(2) .
N1 Ti1 N1 C6 155.54(15) 7_575
C1 Ti1 N1 C6 74.9(3) 7_575
C1 Ti1 N1 C6 6.2(2) .
C4 N1 C6 C11 -86.0(3) .
Ti1 N1 C6 C11 86.5(3) .
C4 N1 C6 C7 93.5(3) .
Ti1 N1 C6 C7 -94.1(3) .
C6 N1 C4 C3 -168.9(3) .
Ti1 N1 C4 C3 18.7(4) .
C6 N1 C4 C5 9.3(3) .
Ti1 N1 C4 C5 -163.06(19) .
C4 C3 C4 N1 11.1(6) 7_575
C4 C3 C4 C5 -167.2(3) 7_575
C7 C6 C11 C10 -1.4(4) .
N1 C6 C11 C10 178.0(2) .
C7 C6 C11 C12 178.4(2) .
N1 C6 C11 C12 -2.2(4) .
C8 C9 C10 C11 0.8(4) .
C6 C11 C10 C9 -0.1(4) .
C12 C11 C10 C9 -179.8(2) .
C10 C9 C8 C7 -0.1(4) .
C9 C8 C7 C6 -1.3(4) .
C9 C8 C7 C15 179.3(3) .
C11 C6 C7 C8 2.0(4) .
N1 C6 C7 C8 -177.4(2) .
C11 C6 C7 C15 -178.5(3) .
N1 C6 C7 C15 2.1(4) .
C10 C11 C12 C14 68.0(3) .
C6 C11 C12 C14 -111.8(3) .
C10 C11 C12 C13 -54.9(3) .
C6 C11 C12 C13 125.3(3) .
C8 C7 C15 C17 73.8(4) .
C6 C7 C15 C17 -105.7(3) .
C8 C7 C15 C16 -50.7(4) .
C6 C7 C15 C16 129.9(3) .
