#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/91/2239106.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_2239106
loop_
_publ_author_name
'Haehnel, Martin'
'Spannenberg, Anke'
'Rosenthal, Uwe'
_publ_section_title
;
 Bis(μ₂-isopropylimido-κ²N:N)bis[(η⁵-cyclopentadienyl)(ethenolato-κO)titanium(IV)]
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m16
_journal_paper_doi               10.1107/S1600536813033072
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Ti2 (C5 H5)2 (C3 H7 N)2 (C2 H3 O)2]'
_chemical_formula_moiety         'C20 H30 N2 O2 Ti2'
_chemical_formula_sum            'C20 H30 N2 O2 Ti2'
_chemical_formula_weight         426.26
_chemical_name_systematic
Bis(μ₂-isopropylimido-κ²N:N)bis[(η⁵-cyclopentadienyl)(ethenolato-κO)titanium(IV)]
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 106.593(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8746(4)
_cell_length_b                   9.7484(2)
_cell_length_c                   16.3264(4)
_cell_measurement_reflns_used    4113
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.5
_cell_measurement_theta_min      2.53
_cell_volume                     2116.27(9)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2005)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2005)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2005)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0140
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32869
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.70
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.770
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.365
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         4625
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0238
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0485P)²+0.2691P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0693
_reflns_number_gt                4211
_reflns_number_total             4625
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            pk2508sup1.cf
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2239106
_cod_database_fobs_code          2239106
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_type_symbol
_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_symmetry_multiplicity
C C1 1.00508(9) 0.81266(12) 0.07526(8) 0.0264(2) Uani d . 1 1
H H1 1.0139 0.8211 0.0199 0.032 Uiso calc R 1 1
C C2 1.04722(11) 0.90582(14) 0.13237(9) 0.0398(3) Uani d . 1 1
H H2A 1.0400 0.9008 0.1884 0.048 Uiso calc R 1 1
H H2B 1.0849 0.9783 0.1176 0.048 Uiso calc R 1 1
C C3 1.10447(9) 0.42926(12) 0.16322(7) 0.0237(2) Uani d . 1 1
H H3 1.0485 0.4372 0.1903 0.028 Uiso calc R 1 1
C C4 1.14785(12) 0.28630(14) 0.18057(9) 0.0406(3) Uani d . 1 1
H H4A 1.0950 0.2187 0.1567 0.061 Uiso calc R 1 1
H H4B 1.1743 0.2723 0.2424 0.061 Uiso calc R 1 1
H H4C 1.2023 0.2753 0.1539 0.061 Uiso calc R 1 1
C C5 1.18229(11) 0.53813(14) 0.20265(8) 0.0344(3) Uani d . 1 1
H H5A 1.2402 0.5285 0.1801 0.052 Uiso calc R 1 1
H H5B 1.2043 0.5268 0.2649 0.052 Uiso calc R 1 1
H H5C 1.1526 0.6294 0.1884 0.052 Uiso calc R 1 1
C C6 0.83879(9) 0.43737(12) 0.13292(7) 0.0252(2) Uani d . 1 1
H H6 0.8677 0.4425 0.1931 0.030 Uiso calc R 1 1
C C7 0.77320(9) 0.53364(12) 0.08185(8) 0.0273(2) Uani d . 1 1
H H7 0.7498 0.6153 0.1015 0.033 Uiso calc R 1 1
C C8 0.74794(9) 0.48839(13) -0.00364(8) 0.0273(2) Uani d . 1 1
H H8 0.7049 0.5344 -0.0516 0.033 Uiso calc R 1 1
C C9 0.79764(8) 0.36312(12) -0.00555(7) 0.0249(2) Uani d . 1 1
H H9 0.7938 0.3094 -0.0549 0.030 Uiso calc R 1 1
C C10 0.85404(8) 0.33132(12) 0.07872(7) 0.0241(2) Uani d . 1 1
H H10 0.8951 0.2525 0.0961 0.029 Uiso calc R 1 1
C C11 0.49256(11) -0.21964(14) 0.14913(8) 0.0350(3) Uani d . 1 1
H H11 0.4293 -0.2371 0.1088 0.042 Uiso calc R 1 1
C C12 0.54472(15) -0.32585(17) 0.18746(11) 0.0544(4) Uani d . 1 1
H H12A 0.6083 -0.3125 0.2281 0.065 Uiso calc R 1 1
H H12B 0.5188 -0.4160 0.1745 0.065 Uiso calc R 1 1
C C13 0.69659(8) -0.08443(12) 0.03329(7) 0.0232(2) Uani d . 1 1
H H13 0.6907 -0.1851 0.0212 0.028 Uiso calc R 1 1
C C14 0.75543(10) -0.02130(15) -0.02278(9) 0.0331(3) Uani d . 1 1
H H14A 0.7197 -0.0378 -0.0830 0.050 Uiso calc R 1 1
H H14B 0.8224 -0.0631 -0.0093 0.050 Uiso calc R 1 1
H H14C 0.7622 0.0777 -0.0122 0.050 Uiso calc R 1 1
C C15 0.75381(10) -0.06547(16) 0.12745(8) 0.0356(3) Uani d . 1 1
H H15A 0.7647 0.0326 0.1400 0.053 Uiso calc R 1 1
H H15B 0.8189 -0.1123 0.1397 0.053 Uiso calc R 1 1
H H15C 0.7146 -0.1045 0.1631 0.053 Uiso calc R 1 1
C C16 0.59925(10) 0.27006(13) 0.09822(8) 0.0324(3) Uani d . 1 1
H H16 0.6481 0.2876 0.0689 0.039 Uiso calc R 1 1
C C17 0.61833(10) 0.21581(14) 0.18150(8) 0.0344(3) Uani d . 1 1
H H17 0.6823 0.1899 0.2179 0.041 Uiso calc R 1 1
C C18 0.52699(10) 0.20677(13) 0.20118(7) 0.0311(3) Uani d . 1 1
H H18 0.5181 0.1745 0.2535 0.037 Uiso calc R 1 1
C C19 0.45087(9) 0.25346(12) 0.13058(8) 0.0278(2) Uani d . 1 1
H H19 0.3812 0.2576 0.1264 0.033 Uiso calc R 1 1
C C20 0.49548(10) 0.29353(12) 0.06639(8) 0.0290(2) Uani d . 1 1
H H20 0.4614 0.3297 0.0118 0.035 Uiso calc R 1 1
N N1 1.06135(7) 0.44839(9) 0.07062(6) 0.02088(18) Uani d . 1 1
N N2 0.59469(7) -0.02696(9) 0.01025(6) 0.02089(19) Uani d . 1 1
O O1 0.95030(6) 0.70628(8) 0.08943(5) 0.02590(17) Uani d . 1 1
O O2 0.52192(6) -0.08863(9) 0.16262(5) 0.02749(18) Uani d . 1 1
Ti Ti1 0.924511(14) 0.532856(19) 0.036855(12) 0.01873(7) Uani d . 1 1
Ti Ti2 0.520839(14) 0.05278(2) 0.083057(12) 0.01907(7) Uani d . 1 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
C2 C1 O1 . . 124.77(11)
C2 C1 H1 . . 117.6
O1 C1 H1 . . 117.6
C1 C2 H2A . . 120.0
C1 C2 H2B . . 120.0
H2A C2 H2B . . 120.0
N1 C3 C4 . . 109.44(10)
N1 C3 C5 . . 112.22(9)
C4 C3 C5 . . 111.57(10)
N1 C3 H3 . . 107.8
C4 C3 H3 . . 107.8
C5 C3 H3 . . 107.8
C3 C4 H4A . . 109.5
C3 C4 H4B . . 109.5
H4A C4 H4B . . 109.5
C3 C4 H4C . . 109.5
H4A C4 H4C . . 109.5
H4B C4 H4C . . 109.5
C3 C5 H5A . . 109.5
C3 C5 H5B . . 109.5
H5A C5 H5B . . 109.5
C3 C5 H5C . . 109.5
H5A C5 H5C . . 109.5
H5B C5 H5C . . 109.5
C7 C6 C10 . . 107.71(10)
C7 C6 Ti1 . . 73.25(6)
C10 C6 Ti1 . . 71.67(6)
C7 C6 H6 . . 126.1
C10 C6 H6 . . 126.1
Ti1 C6 H6 . . 120.7
C6 C7 C8 . . 108.34(11)
C6 C7 Ti1 . . 72.91(7)
C8 C7 Ti1 . . 71.91(7)
C6 C7 H7 . . 125.8
C8 C7 H7 . . 125.8
Ti1 C7 H7 . . 121.1
C9 C8 C7 . . 107.98(10)
C9 C8 Ti1 . . 72.13(6)
C7 C8 Ti1 . . 73.96(7)
C9 C8 H8 . . 126.0
C7 C8 H8 . . 126.0
Ti1 C8 H8 . . 119.7
C8 C9 C10 . . 107.96(10)
C8 C9 Ti1 . . 73.47(6)
C10 C9 Ti1 . . 73.11(6)
C8 C9 H9 . . 126.0
C10 C9 H9 . . 126.0
Ti1 C9 H9 . . 119.3
C9 C10 C6 . . 108.01(10)
C9 C10 Ti1 . . 72.37(6)
C6 C10 Ti1 . . 73.96(6)
C9 C10 H10 . . 126.0
C6 C10 H10 . . 126.0
Ti1 C10 H10 . . 119.5
C12 C11 O2 . . 124.91(14)
C12 C11 H11 . . 117.5
O2 C11 H11 . . 117.5
C11 C12 H12A . . 120.0
C11 C12 H12B . . 120.0
H12A C12 H12B . . 120.0
N2 C13 C14 . . 109.58(9)
N2 C13 C15 . . 113.45(9)
C14 C13 C15 . . 110.07(10)
N2 C13 H13 . . 107.9
C14 C13 H13 . . 107.9
C15 C13 H13 . . 107.9
C13 C14 H14A . . 109.5
C13 C14 H14B . . 109.5
H14A C14 H14B . . 109.5
C13 C14 H14C . . 109.5
H14A C14 H14C . . 109.5
H14B C14 H14C . . 109.5
C13 C15 H15A . . 109.5
C13 C15 H15B . . 109.5
H15A C15 H15B . . 109.5
C13 C15 H15C . . 109.5
H15A C15 H15C . . 109.5
H15B C15 H15C . . 109.5
C20 C16 C17 . . 107.95(11)
C20 C16 Ti2 . . 73.39(7)
C17 C16 Ti2 . . 73.68(7)
C20 C16 H16 . . 126.0
C17 C16 H16 . . 126.0
Ti2 C16 H16 . . 118.8
C18 C17 C16 . . 108.20(11)
C18 C17 Ti2 . . 74.68(7)
C16 C17 Ti2 . . 71.73(7)
C18 C17 H17 . . 125.9
C16 C17 H17 . . 125.9
Ti2 C17 H17 . . 119.5
C17 C18 C19 . . 108.13(11)
C17 C18 Ti2 . . 71.60(7)
C19 C18 Ti2 . . 72.50(7)
C17 C18 H18 . . 125.9
C19 C18 H18 . . 125.9
Ti2 C18 H18 . . 121.7
C18 C19 C20 . . 108.23(11)
C18 C19 Ti2 . . 73.87(7)
C20 C19 Ti2 . . 71.58(7)
C18 C19 H19 . . 125.9
C20 C19 H19 . . 125.9
Ti2 C19 H19 . . 120.4
C16 C20 C19 . . 107.48(11)
C16 C20 Ti2 . . 72.18(7)
C19 C20 Ti2 . . 74.01(7)
C16 C20 H20 . . 126.3
C19 C20 H20 . . 126.3
Ti2 C20 H20 . . 119.4
C3 N1 Ti1 . 3_765 151.07(8)
C3 N1 Ti1 . . 114.31(7)
Ti1 N1 Ti1 3_765 . 92.75(4)
C13 N2 Ti2 . 3_655 133.70(7)
C13 N2 Ti2 . . 129.43(7)
Ti2 N2 Ti2 3_655 . 94.16(4)
C1 O1 Ti1 . . 131.09(7)
C11 O2 Ti2 . . 129.76(8)
N1 Ti1 O1 3_765 . 106.79(4)
N1 Ti1 N1 3_765 . 87.25(4)
O1 Ti1 N1 . . 101.68(4)
N1 Ti1 C9 3_765 . 93.65(4)
O1 Ti1 C9 . . 142.01(4)
N1 Ti1 C9 . . 111.16(4)
N1 Ti1 C10 3_765 . 121.55(4)
O1 Ti1 C10 . . 130.56(4)
N1 Ti1 C10 . . 90.95(4)
C9 Ti1 C10 . . 34.52(4)
N1 Ti1 C8 3_765 . 97.76(4)
O1 Ti1 C8 . . 109.60(4)
N1 Ti1 C8 . . 145.17(4)
C9 Ti1 C8 . . 34.40(4)
C10 Ti1 C8 . . 57.08(4)
N1 Ti1 C6 3_765 . 150.56(4)
O1 Ti1 C6 . . 96.60(4)
N1 Ti1 C6 . . 105.55(4)
C9 Ti1 C6 . . 57.12(4)
C10 Ti1 C6 . . 34.37(4)
C8 Ti1 C6 . . 56.77(4)
N1 Ti1 C7 3_765 . 129.22(4)
O1 Ti1 C7 . . 85.81(4)
N1 Ti1 C7 . . 139.30(4)
C9 Ti1 C7 . . 56.86(4)
C10 Ti1 C7 . . 56.70(4)
C8 Ti1 C7 . . 34.13(4)
C6 Ti1 C7 . . 33.84(4)
N1 Ti1 Ti1 3_765 3_765 46.02(3)
O1 Ti1 Ti1 . 3_765 109.66(3)
N1 Ti1 Ti1 . 3_765 41.24(3)
C9 Ti1 Ti1 . 3_765 107.58(3)
C10 Ti1 Ti1 . 3_765 110.93(3)
C8 Ti1 Ti1 . 3_765 132.88(3)
C6 Ti1 Ti1 . 3_765 140.16(3)
C7 Ti1 Ti1 . 3_765 164.44(3)
N2 Ti2 O2 3_655 . 107.20(4)
N2 Ti2 N2 3_655 . 85.84(4)
O2 Ti2 N2 . . 103.11(4)
N2 Ti2 C16 3_655 . 117.65(4)
O2 Ti2 C16 . . 131.96(4)
N2 Ti2 C16 . . 96.63(4)
N2 Ti2 C20 3_655 . 88.59(4)
O2 Ti2 C20 . . 140.36(4)
N2 Ti2 C20 . . 114.35(4)
C16 Ti2 C20 . . 34.43(5)
N2 Ti2 C17 3_655 . 145.09(4)
O2 Ti2 C17 . . 97.53(4)
N2 Ti2 C17 . . 112.49(4)
C16 Ti2 C17 . . 34.59(5)
C20 Ti2 C17 . . 57.08(5)
N2 Ti2 C19 3_655 . 92.34(4)
O2 Ti2 C19 . . 107.19(4)
N2 Ti2 C19 . . 148.75(4)
C16 Ti2 C19 . . 56.89(4)
C20 Ti2 C19 . . 34.41(4)
C17 Ti2 C19 . . 56.31(4)
N2 Ti2 C18 3_655 . 123.60(4)
O2 Ti2 C18 . . 85.03(4)
N2 Ti2 C18 . . 146.12(4)
C16 Ti2 C18 . . 56.71(4)
C20 Ti2 C18 . . 56.67(4)
C17 Ti2 C18 . . 33.72(5)
C19 Ti2 C18 . . 33.63(4)
N2 Ti2 Ti2 3_655 3_655 43.66(3)
O2 Ti2 Ti2 . 3_655 110.86(3)
N2 Ti2 Ti2 . 3_655 42.18(3)
C16 Ti2 Ti2 . 3_655 113.10(3)
C20 Ti2 Ti2 . 3_655 105.60(3)
C17 Ti2 Ti2 . 3_655 144.77(4)
C19 Ti2 Ti2 . 3_655 128.26(3)
C18 Ti2 Ti2 . 3_655 161.30(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C1 C2 . 1.3133(18)
C1 O1 . 1.3443(14)
C1 H1 . 0.9500
C2 H2A . 0.9500
C2 H2B . 0.9500
C3 N1 . 1.4703(14)
C3 C4 . 1.5124(17)
C3 C5 . 1.5197(17)
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 . 1.4039(17)
C6 C10 . 1.4155(16)
C6 Ti1 . 2.4096(11)
C6 H6 . 0.9500
C7 C8 . 1.4093(18)
C7 Ti1 . 2.4140(12)
C7 H7 . 0.9500
C8 C9 . 1.4071(17)
C8 Ti1 . 2.3878(11)
C8 H8 . 0.9500
C9 C10 . 1.4094(16)
C9 Ti1 . 2.3706(11)
C9 H9 . 0.9500
C10 Ti1 . 2.3801(11)
C10 H10 . 0.9500
C11 C12 . 1.315(2)
C11 O2 . 1.3395(16)
C11 H11 . 0.9500
C12 H12A . 0.9500
C12 H12B . 0.9500
C13 N2 . 1.4665(14)
C13 C14 . 1.5198(16)
C13 C15 . 1.5267(16)
C13 H13 . 1.0000
C14 H14A . 0.9800
C14 H14B . 0.9800
C14 H14C . 0.9800
C15 H15A . 0.9800
C15 H15B . 0.9800
C15 H15C . 0.9800
C16 C20 . 1.4028(18)
C16 C17 . 1.4118(19)
C16 Ti2 . 2.3617(12)
C16 H16 . 0.9500
C17 C18 . 1.3963(19)
C17 Ti2 . 2.3869(12)
C17 H17 . 0.9500
C18 C19 . 1.3986(18)
C18 Ti2 . 2.4262(11)
C18 H18 . 0.9500
C19 C20 . 1.4158(16)
C19 Ti2 . 2.4087(11)
C19 H19 . 0.9500
C20 Ti2 . 2.3773(12)
C20 H20 . 0.9500
N1 Ti1 3_765 1.8296(9)
N1 Ti1 . 1.9972(10)
N2 Ti2 3_655 1.8864(9)
N2 Ti2 . 1.9398(9)
O1 Ti1 . 1.8834(8)
O2 Ti2 . 1.8913(8)
Ti1 N1 3_765 1.8296(9)
Ti1 Ti1 3_765 2.7725(4)
Ti2 N2 3_655 1.8864(9)
Ti2 Ti2 3_655 2.8022(4)
