#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/61/4076101.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_4076101
loop_
_publ_author_name
'Wang, Cun'
'Erker, Gerhard'
'Kehr, Gerald'
'Wedeking, Katrin'
'Fröhlich, Roland'
_publ_section_title
;
 Synthesis, Structural Features, and Formation of Organometallic Derivates
 of C1-Bridged Cp/Amido Titanium and Zirconium “CpCN-Constrained
 Geometry” Systems
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              4760
_journal_paper_doi               10.1021/om0505918
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C17.5 H19 Cl2 N O Ti'
_chemical_formula_weight         378.14
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.13(1)
_cell_angle_beta                 95.52(1)
_cell_angle_gamma                112.59(1)
_cell_formula_units_Z            2
_cell_length_a                   8.739(1)
_cell_length_b                   9.758(1)
_cell_length_c                   11.401(1)
_cell_measurement_temperature    198(2)
_cell_volume                     891.77(17)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP (BrukerAXS, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      198(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode Nonius FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9961
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    0.781
_exptl_absorpt_correction_T_max  0.9260
_exptl_absorpt_correction_T_min  0.7717
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             390
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         4219
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0354
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0414P)²+0.3467P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0940
_reflns_number_gt                3787
_reflns_number_total             4219
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0505918si20050713_115732.cif
_cod_data_source_block           erk2810
_cod_original_cell_volume        891.77(16)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C17.50 H19 Cl2 N O Ti'
_cod_database_code               4076101
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.31227(3) 0.75534(3) 0.11804(2) 0.03696(10) Uani 1 1 d . . .
Cl1 Cl 0.10802(6) 0.81729(5) 0.02774(4) 0.05388(13) Uani 1 1 d . . .
Cl2 Cl 0.44706(5) 0.94732(4) 0.25679(4) 0.04794(12) Uani 1 1 d . . .
O1 O -0.33053(13) 0.45539(12) 0.46720(10) 0.0419(3) Uani 1 1 d . . .
N1 N 0.20254(15) 0.57814(13) 0.19969(11) 0.0344(3) Uani 1 1 d . . .
C1 C 0.3772(2) 0.55840(18) 0.07565(14) 0.0413(3) Uani 1 1 d . . .
C2 C 0.5301(2) 0.6772(2) 0.11474(17) 0.0493(4) Uani 1 1 d . . .
H2 H 0.6010 0.6821 0.1847 0.059 Uiso 1 1 calc R . .
C3 C 0.5588(3) 0.7871(2) 0.03139(19) 0.0586(5) Uani 1 1 d . . .
H3 H 0.6520 0.8793 0.0359 0.070 Uiso 1 1 calc R . .
C4 C 0.4255(3) 0.7364(2) -0.05941(17) 0.0563(5) Uani 1 1 d . . .
H4 H 0.4127 0.7884 -0.1267 0.068 Uiso 1 1 calc R . .
C5 C 0.3145(2) 0.5947(2) -0.03297(14) 0.0471(4) Uani 1 1 d . . .
H5 H 0.2145 0.5341 -0.0801 0.057 Uiso 1 1 calc R . .
C6 C 0.2614(2) 0.46338(17) 0.15960(13) 0.0380(3) Uani 1 1 d . . .
H6 H 0.1672 0.3791 0.1145 0.046 Uiso 1 1 calc R . .
C7 C 0.3454(2) 0.4053(2) 0.25781(16) 0.0506(4) Uani 1 1 d . . .
H7A H 0.4434 0.4875 0.2969 0.076 Uiso 1 1 calc R . .
H7B H 0.3803 0.3299 0.2245 0.076 Uiso 1 1 calc R . .
H7C H 0.2669 0.3607 0.3154 0.076 Uiso 1 1 calc R . .
C8 C 0.06769(17) 0.54069(15) 0.26796(12) 0.0320(3) Uani 1 1 d . . .
C9 C 0.03054(18) 0.65411(15) 0.31869(13) 0.0357(3) Uani 1 1 d . . .
H9 H 0.0979 0.7549 0.3082 0.043 Uiso 1 1 calc R . .
C10 C -0.10264(18) 0.62154(16) 0.38382(14) 0.0375(3) Uani 1 1 d . . .
H10 H -0.1265 0.7001 0.4172 0.045 Uiso 1 1 calc R . .
C11 C -0.20256(17) 0.47461(15) 0.40113(12) 0.0329(3) Uani 1 1 d . . .
C12 C -0.16714(19) 0.36055(15) 0.35178(13) 0.0370(3) Uani 1 1 d . . .
H12 H -0.2345 0.2599 0.3631 0.044 Uiso 1 1 calc R . .
C13 C -0.03312(19) 0.39349(16) 0.28583(14) 0.0376(3) Uani 1 1 d . . .
H13 H -0.0096 0.3148 0.2524 0.045 Uiso 1 1 calc R . .
C14 C -0.4332(2) 0.30688(19) 0.48969(16) 0.0471(4) Uani 1 1 d . . .
H14A H -0.4782 0.2478 0.4147 0.071 Uiso 1 1 calc R . .
H14B H -0.5253 0.3076 0.5321 0.071 Uiso 1 1 calc R . .
H14C H -0.3666 0.2631 0.5378 0.071 Uiso 1 1 calc R . .
C15 C -0.8432(3) 0.0169(2) 0.5424(4) 0.0866(9) Uani 1 1 d . . .
H15 H -0.7317 0.0296 0.5684 0.104 Uiso 1 1 calc R . .
C16 C -0.8757(3) 0.0246(2) 0.4274(4) 0.0842(9) Uani 1 1 d . . .
H16 H -0.7873 0.0414 0.3799 0.101 Uiso 1 1 calc R A 1
C17A C -1.047(2) 0.0082(17) 0.3654(10) 0.0645(17) Uani 0.50 1 d P . 1
C18 C -1.0720(8) 0.0023(5) 0.2665(5) 0.0781(14) Uani 0.50 1 d P B 1
H18A H -1.1108 -0.1014 0.2359 0.117 Uiso 0.50 1 calc PR B 1
H18B H -0.9692 0.0617 0.2333 0.117 Uiso 0.50 1 calc PR B 1
H18C H -1.1579 0.0413 0.2441 0.117 Uiso 0.50 1 calc PR B 1
C17B C -1.019(2) 0.0063(17) 0.3999(11) 0.0645(17) Uani 0.50 1 d P . 2
H17B H -1.0423 0.0082 0.3170 0.077 Uiso 0.50 1 calc PR . 2
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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 Ti C1 63.90(5) . .
N1 Ti Cl1 106.43(4) . .
C1 Ti Cl1 128.61(5) . .
N1 Ti Cl2 107.97(4) . .
C1 Ti Cl2 128.12(5) . .
Cl1 Ti Cl2 103.20(2) . .
N1 Ti C2 86.40(6) . .
C1 Ti C2 36.07(6) . .
Cl1 Ti C2 152.18(5) . .
Cl2 Ti C2 95.77(5) . .
N1 Ti C5 85.72(6) . .
C1 Ti C5 35.99(6) . .
Cl1 Ti C5 96.52(5) . .
Cl2 Ti C5 151.31(5) . .
C2 Ti C5 59.17(7) . .
N1 Ti C4 119.60(6) . .
C1 Ti C4 59.16(6) . .
Cl1 Ti C4 94.09(6) . .
Cl2 Ti C4 121.74(6) . .
C2 Ti C4 58.38(7) . .
C5 Ti C4 34.99(6) . .
N1 Ti C3 120.10(6) . .
C1 Ti C3 59.14(7) . .
Cl1 Ti C3 122.34(6) . .
Cl2 Ti C3 93.43(6) . .
C2 Ti C3 35.09(7) . .
C5 Ti C3 58.17(7) . .
C4 Ti C3 34.51(8) . .
C11 O1 C14 117.45(12) . .
C8 N1 C6 120.64(12) . .
C8 N1 Ti 130.80(10) . .
C6 N1 Ti 107.55(9) . .
C5 C1 C2 107.57(15) . .
C5 C1 C6 121.40(15) . .
C2 C1 C6 122.94(15) . .
C5 C1 Ti 74.04(10) . .
C2 C1 Ti 73.93(10) . .
C6 C1 Ti 92.15(9) . .
C3 C2 C1 107.94(17) . .
C3 C2 Ti 74.82(11) . .
C1 C2 Ti 70.01(9) . .
C4 C3 C2 108.18(17) . .
C4 C3 Ti 72.72(11) . .
C2 C3 Ti 70.09(10) . .
C3 C4 C5 107.97(17) . .
C3 C4 Ti 72.77(10) . .
C5 C4 Ti 70.22(9) . .
C4 C5 C1 108.32(17) . .
C4 C5 Ti 74.78(10) . .
C1 C5 Ti 69.97(9) . .
N1 C6 C7 114.32(13) . .
N1 C6 C1 96.41(11) . .
C7 C6 C1 114.89(14) . .
C9 C8 C13 118.20(13) . .
C9 C8 N1 119.22(12) . .
C13 C8 N1 122.57(13) . .
C10 C9 C8 120.82(13) . .
C9 C10 C11 120.63(13) . .
O1 C11 C12 125.01(13) . .
O1 C11 C10 115.64(13) . .
C12 C11 C10 119.35(13) . .
C11 C12 C13 119.98(13) . .
C12 C13 C8 121.02(13) . .
C16 C15 C17A 129.5(5) . 2_356
C16 C15 C17B 111.5(4) . 2_356
C17A C15 C17B 18.0(7) 2_356 2_356
C15 C16 C17B 112.1(8) . .
C15 C16 C17A 124.4(7) . .
C17B C16 C17A 12.4(13) . .
C18 C17A C15 131.8(14) . 2_356
C18 C17A C16 121.6(17) . .
C15 C17A C16 106.1(6) 2_356 .
C16 C17B C15 136.4(9) . 2_356
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti N1 1.9332(13) .
Ti C1 2.2589(16) .
Ti Cl1 2.2608(6) .
Ti Cl2 2.2866(6) .
Ti C2 2.3098(18) .
Ti C5 2.3116(17) .
Ti C4 2.3703(17) .
Ti C3 2.3710(18) .
O1 C11 1.3638(17) .
O1 C14 1.4251(19) .
N1 C8 1.4089(18) .
N1 C6 1.4816(18) .
C1 C5 1.413(2) .
C1 C2 1.415(2) .
C1 C6 1.517(2) .
C2 C3 1.412(3) .
C3 C4 1.406(3) .
C4 C5 1.409(3) .
C6 C7 1.517(2) .
C8 C9 1.3970(19) .
C8 C13 1.3982(19) .
C9 C10 1.378(2) .
C10 C11 1.393(2) .
C11 C12 1.387(2) .
C12 C13 1.389(2) .
C15 C16 1.324(4) .
C15 C17A 1.45(2) 2_356
C15 C17B 1.37(2) 2_356
C16 C17B 1.201(18) .
C16 C17A 1.540(15) .
C17A C18 1.124(12) .
C17A C15 1.45(2) 2_356
C17B C15 1.37(2) 2_356
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
_geom_torsion_site_symmetry_4
C1 Ti N1 C8 -168.38(14) . .
Cl1 Ti N1 C8 -42.93(13) . .
Cl2 Ti N1 C8 67.30(13) . .
C2 Ti N1 C8 162.20(13) . .
C5 Ti N1 C8 -138.48(13) . .
C4 Ti N1 C8 -147.59(12) . .
C3 Ti N1 C8 172.42(12) . .
C1 Ti N1 C6 -0.12(9) . .
Cl1 Ti N1 C6 125.32(9) . .
Cl2 Ti N1 C6 -124.44(9) . .
C2 Ti N1 C6 -29.54(10) . .
C5 Ti N1 C6 29.78(10) . .
C4 Ti N1 C6 20.67(12) . .
C3 Ti N1 C6 -19.33(12) . .
N1 Ti C1 C5 122.22(11) . .
Cl1 Ti C1 C5 31.54(12) . .
Cl2 Ti C1 C5 -144.79(9) . .
C2 Ti C1 C5 -114.15(15) . .
C4 Ti C1 C5 -36.71(11) . .
C3 Ti C1 C5 -77.14(12) . .
N1 Ti C1 C2 -123.63(12) . .
Cl1 Ti C1 C2 145.69(9) . .
Cl2 Ti C1 C2 -30.64(12) . .
C5 Ti C1 C2 114.15(15) . .
C4 Ti C1 C2 77.43(12) . .
C3 Ti C1 C2 37.01(11) . .
N1 Ti C1 C6 0.12(8) . .
Cl1 Ti C1 C6 -90.56(10) . .
Cl2 Ti C1 C6 93.11(9) . .
C2 Ti C1 C6 123.74(15) . .
C5 Ti C1 C6 -122.11(15) . .
C4 Ti C1 C6 -158.82(12) . .
C3 Ti C1 C6 160.76(13) . .
C5 C1 C2 C3 1.21(19) . .
C6 C1 C2 C3 -147.69(16) . .
Ti C1 C2 C3 -65.75(13) . .
C5 C1 C2 Ti 66.96(11) . .
C6 C1 C2 Ti -81.94(14) . .
N1 Ti C2 C3 164.52(12) . .
C1 Ti C2 C3 116.00(16) . .
Cl1 Ti C2 C3 45.32(17) . .
Cl2 Ti C2 C3 -87.76(11) . .
C5 Ti C2 C3 77.36(12) . .
C4 Ti C2 C3 36.20(12) . .
N1 Ti C2 C1 48.52(10) . .
Cl1 Ti C2 C1 -70.68(15) . .
Cl2 Ti C2 C1 156.24(9) . .
C5 Ti C2 C1 -38.64(10) . .
C4 Ti C2 C1 -79.80(11) . .
C3 Ti C2 C1 -116.00(16) . .
C1 C2 C3 C4 -0.6(2) . .
Ti C2 C3 C4 -63.16(14) . .
C1 C2 C3 Ti 62.60(11) . .
N1 Ti C3 C4 99.48(13) . .
C1 Ti C3 C4 79.35(13) . .
Cl1 Ti C3 C4 -39.46(13) . .
Cl2 Ti C3 C4 -147.44(11) . .
C2 Ti C3 C4 117.41(17) . .
C5 Ti C3 C4 36.95(11) . .
N1 Ti C3 C2 -17.93(14) . .
C1 Ti C3 C2 -38.06(11) . .
Cl1 Ti C3 C2 -156.87(10) . .
Cl2 Ti C3 C2 95.15(11) . .
C5 Ti C3 C2 -80.45(12) . .
C4 Ti C3 C2 -117.41(17) . .
C2 C3 C4 C5 -0.3(2) . .
Ti C3 C4 C5 -61.78(13) . .
C2 C3 C4 Ti 61.47(13) . .
N1 Ti C4 C3 -101.06(13) . .
C1 Ti C4 C3 -79.27(13) . .
Cl1 Ti C4 C3 147.43(12) . .
Cl2 Ti C4 C3 39.17(14) . .
C2 Ti C4 C3 -36.83(12) . .
C5 Ti C4 C3 -117.04(18) . .
N1 Ti C4 C5 15.98(14) . .
C1 Ti C4 C5 37.78(11) . .
Cl1 Ti C4 C5 -95.53(11) . .
Cl2 Ti C4 C5 156.21(10) . .
C2 Ti C4 C5 80.22(12) . .
C3 Ti C4 C5 117.04(18) . .
C3 C4 C5 C1 1.1(2) . .
Ti C4 C5 C1 -62.36(11) . .
C3 C4 C5 Ti 63.42(13) . .
C2 C1 C5 C4 -1.40(19) . .
C6 C1 C5 C4 148.07(15) . .
Ti C1 C5 C4 65.48(12) . .
C2 C1 C5 Ti -66.88(11) . .
C6 C1 C5 Ti 82.59(13) . .
N1 Ti C5 C4 -166.11(12) . .
C1 Ti C5 C4 -116.48(16) . .
Cl1 Ti C5 C4 87.82(12) . .
Cl2 Ti C5 C4 -45.61(17) . .
C2 Ti C5 C4 -77.75(13) . .
C3 Ti C5 C4 -36.43(12) . .
N1 Ti C5 C1 -49.63(10) . .
Cl1 Ti C5 C1 -155.70(9) . .
Cl2 Ti C5 C1 70.88(14) . .
C2 Ti C5 C1 38.73(10) . .
C4 Ti C5 C1 116.48(16) . .
C3 Ti C5 C1 80.05(12) . .
C8 N1 C6 C7 -69.12(18) . .
Ti N1 C6 C7 121.19(13) . .
C8 N1 C6 C1 169.85(13) . .
Ti N1 C6 C1 0.17(12) . .
C5 C1 C6 N1 -72.71(17) . .
C2 C1 C6 N1 72.05(18) . .
Ti C1 C6 N1 -0.14(10) . .
C5 C1 C6 C7 166.70(15) . .
C2 C1 C6 C7 -48.5(2) . .
Ti C1 C6 C7 -120.73(12) . .
C6 N1 C8 C9 170.79(13) . .
Ti N1 C8 C9 -22.2(2) . .
C6 N1 C8 C13 -10.2(2) . .
Ti N1 C8 C13 156.74(12) . .
C13 C8 C9 C10 -0.5(2) . .
N1 C8 C9 C10 178.56(14) . .
C8 C9 C10 C11 0.4(2) . .
C14 O1 C11 C12 1.6(2) . .
C14 O1 C11 C10 -178.37(14) . .
C9 C10 C11 O1 179.85(14) . .
C9 C10 C11 C12 -0.2(2) . .
O1 C11 C12 C13 179.96(14) . .
C10 C11 C12 C13 0.0(2) . .
C11 C12 C13 C8 0.0(2) . .
C9 C8 C13 C12 0.3(2) . .
N1 C8 C13 C12 -178.71(14) . .
C17A C15 C16 C17B -0.7(4) 2_356 .
C17B C15 C16 C17B -1.6(15) 2_356 .
C17A C15 C16 C17A 0.3(15) 2_356 .
C17B C15 C16 C17A -0.6(3) 2_356 .
C15 C16 C17A C18 -172.7(9) . .
C17B C16 C17A C18 -168(7) . .
C15 C16 C17A C15 -0.3(12) . 2_356
C17B C16 C17A C15 4(5) . 2_356
C15 C16 C17B C15 2(2) . 2_356
C17A C16 C17B C15 -174(8) . 2_356
