##############################################################################
###                                                                        ###
###        Electronic paper (Acta Crystallographica Section E)             ###
###                                                                        ###
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#                                                                            #
# This CIF contains the data in a paper accepted for publication in Acta     #
# Crystallographica Section E. It conforms to the requirements of Notes      #
# for Authors for Section E, and has been peer reviewed under the auspices   #
# of the IUCr Commission on Journals.                                        #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.4.    #
#                                                                            #
# Software is freely available for graphical display of the structure(s) in  #
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data_I
_audit_creation_method     SHELXL-97
_chemical_name_systematic
;
dichlorido[N,N-dimethyl-2-(η⁵-
tetramethylcyclopentadienyl)acetamidinido-κN']titanium(IV)
;
_chemical_name_common     ?
_chemical_formula_moiety     'C13 H20 Cl2 N2 Ti'
_chemical_formula_sum     'C13 H20 Cl2 N2 Ti'
_chemical_formula_iupac     '[Ti (C13 H20 N2) Cl2]'
_chemical_formula_weight     323.11
_chemical_melting_point     ?
_symmetry_cell_setting     orthorhombic
_symmetry_space_group_name_H-M     'P b c a'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x+1/2, -y, z+1/2'
    '-x, y+1/2, -z+1/2'
    'x+1/2, -y+1/2, -z'
    '-x, -y, -z'
    'x-1/2, y, -z-1/2'
    'x, -y-1/2, z-1/2'
    '-x-1/2, y-1/2, z'
_cell_length_a     12.600(5)
_cell_length_b     15.498(6)
_cell_length_c     15.574(5)
_cell_angle_alpha     90.00
_cell_angle_beta     90.00
_cell_angle_gamma     90.00
_cell_volume     3041.1(19)
_cell_formula_units_Z     8
_cell_measurement_reflns_used     4409
_cell_measurement_theta_min     2.462
_cell_measurement_theta_max     26.9515
_cell_measurement_temperature     213(2)
_exptl_crystal_description     block
_exptl_crystal_colour     orange
_exptl_crystal_size_max     0.30
_exptl_crystal_size_mid     0.20
_exptl_crystal_size_min     0.20
_exptl_crystal_density_diffrn     1.411
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     1344
_exptl_absorpt_coefficient_mu     0.899
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details     '(SADABS; Sheldrick, 1997)'
_exptl_absorpt_correction_T_min     0.7742
_exptl_absorpt_correction_T_max     0.8407
_exptl_special_details
;
;
_diffrn_ambient_temperature     213(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Siemens SMART'
_diffrn_measurement_method     ω
_diffrn_detector_area_resol_mean     ?
_diffrn_reflns_number     11691
_diffrn_reflns_av_R_equivalents     0.0367
_diffrn_reflns_av_sigmaI/netI     0.0300
_diffrn_reflns_theta_min     2.46
_diffrn_reflns_theta_max     25.01
_diffrn_reflns_theta_full     25.01
_diffrn_measured_fraction_theta_max     1.000
_diffrn_measured_fraction_theta_full     1.000
_diffrn_reflns_limit_h_min     -14
_diffrn_reflns_limit_h_max     14
_diffrn_reflns_limit_k_min     -18
_diffrn_reflns_limit_k_max     12
_diffrn_reflns_limit_l_min     -18
_diffrn_reflns_limit_l_max     18
_diffrn_standards_number     ?
_diffrn_standards_interval_count     ?
_diffrn_standards_interval_time     ?
_diffrn_standards_decay_%     3.88
_refine_special_details
;
Refinement of F² against ALL reflections. The weighted R-factor
wR and goodness of fit S are based on F², conventional
R-factors R are based on F, with F set to zero for
negative F². The threshold expression of F² >
σ(F²) is used only for calculating R-factors(gt) etc.
and is not relevant to the choice of reflections for refinement.
R-factors based on F² are statistically about twice as large
as those based on F, and R- factors based on ALL data will be
even larger.
;
_reflns_number_total     2677
_reflns_number_gt     2554
_reflns_threshold_expression     I>2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0594
_refine_ls_R_factor_gt     0.0555
_refine_ls_wR_factor_gt     0.1148
_refine_ls_wR_factor_ref     0.1166
_refine_ls_goodness_of_fit_ref     1.269
_refine_ls_restrained_S_all     1.269
_refine_ls_number_reflns     2677
_refine_ls_number_parameters     169
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
          'calc w=1/[σ²(Fo²)+(0.036P)²+4.3005P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     0.001
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     0.379
_refine_diff_density_min     -0.296
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
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'
    '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'
_computing_data_collection     'SMART (Siemens, 1996)'
_computing_cell_refinement     'SAINT (Siemens, 1996)'
_computing_data_reduction     'SAINT (Siemens, 1996)'
_computing_structure_solution     'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement     'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics     'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material     'SHELXL97 (Sheldrick, 2008)'
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_disorder_assembly
    _atom_site_disorder_group
    Ti Ti 0.21528(5) 0.56734(4) 0.10562(4) 0.02449(19) Uani d . 1 . .
    Cl Cl1 0.10277(7) 0.66810(6) 0.04506(6) 0.0396(3) Uani d . 1 . .
    Cl Cl2 0.11570(8) 0.49802(7) 0.20873(6) 0.0416(3) Uani d . 1 . .
    N N1 0.3122(2) 0.63161(19) 0.16445(18) 0.0302(7) Uani d . 1 . .
    N N2 0.4755(2) 0.69295(19) 0.19627(19) 0.0326(7) Uani d . 1 . .
    C C1 0.3752(3) 0.5272(2) 0.0479(2) 0.0289(8) Uani d . 1 . .
    C C2 0.3304(3) 0.4522(2) 0.0835(2) 0.0285(8) Uani d . 1 . .
    C C3 0.2387(3) 0.4307(2) 0.0348(2) 0.0314(8) Uani d . 1 . .
    C C4 0.2270(3) 0.4933(2) -0.0298(2) 0.0313(8) Uani d . 1 . .
    C C5 0.3117(3) 0.5534(2) -0.0221(2) 0.0299(8) Uani d . 1 . .
    C C6 0.4650(3) 0.5788(2) 0.0867(2) 0.0347(9) Uani d . 1 . .
    H H6A 0.5014 0.6123 0.0423 0.042 Uiso calc R 1 . .
    H H6B 0.5166 0.5403 0.1141 0.042 Uiso calc R 1 . .
    C C7 0.4158(3) 0.6384(2) 0.1528(2) 0.0282(8) Uani d . 1 . .
    C C8 0.4285(3) 0.7477(3) 0.2621(3) 0.0458(10) Uani d . 1 . .
    H H8A 0.3529 0.7362 0.2658 0.069 Uiso calc R 1 . .
    H H8B 0.4396 0.8078 0.2473 0.069 Uiso calc R 1 . .
    H H8C 0.4615 0.7356 0.3171 0.069 Uiso calc R 1 . .
    C C9 0.5892(3) 0.7047(3) 0.1806(3) 0.0447(10) Uani d . 1 . .
    H H9A 0.6176 0.6536 0.1531 0.067 Uiso calc R 1 . .
    H H9B 0.6253 0.7141 0.2348 0.067 Uiso calc R 1 . .
    H H9C 0.5999 0.7544 0.1437 0.067 Uiso calc R 1 . .
    C C10 0.3711(3) 0.4014(3) 0.1590(2) 0.0421(10) Uani d . 1 . .
    H H10A 0.4040 0.3486 0.1387 0.063 Uiso calc R 1 . .
    H H10B 0.3125 0.3872 0.1968 0.063 Uiso calc R 1 . .
    H H10C 0.4229 0.4355 0.1900 0.063 Uiso calc R 1 . .
    C C11 0.1708(3) 0.3522(2) 0.0475(3) 0.0442(10) Uani d . 1 . .
    H H11A 0.0967 0.3678 0.0412 0.066 Uiso calc R 1 . .
    H H11B 0.1826 0.3290 0.1046 0.066 Uiso calc R 1 . .
    H H11C 0.1892 0.3090 0.0050 0.066 Uiso calc R 1 . .
    C C12 0.1436(3) 0.4946(3) -0.0985(3) 0.0448(10) Uani d . 1 . .
    H H12A 0.1733 0.4725 -0.1516 0.067 Uiso calc R 1 . .
    H H12B 0.1194 0.5534 -0.1073 0.067 Uiso calc R 1 . .
    H H12C 0.0842 0.4588 -0.0812 0.067 Uiso calc R 1 . .
    C C13 0.3304(3) 0.6293(3) -0.0800(2) 0.0438(10) Uani d . 1 . .
    H H13A 0.3836 0.6667 -0.0547 0.066 Uiso calc R 1 . .
    H H13B 0.2647 0.6611 -0.0872 0.066 Uiso calc R 1 . .
    H H13C 0.3550 0.6091 -0.1355 0.066 Uiso calc R 1 . .
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
    Ti 0.0217(3) 0.0269(3) 0.0249(3) 0.0006(3) 0.0008(2) -0.0016(3)
    Cl1 0.0328(5) 0.0388(5) 0.0471(6) 0.0091(4) -0.0028(4) 0.0043(4)
    Cl2 0.0404(5) 0.0474(6) 0.0370(5) -0.0053(5) 0.0098(4) 0.0072(4)
    N1 0.0284(16) 0.0325(16) 0.0296(15) 0.0011(13) 0.0017(13) -0.0100(13)
    N2 0.0275(16) 0.0341(17) 0.0362(17) -0.0027(13) -0.0056(13) -0.0058(14)
    C1 0.0254(18) 0.0333(19) 0.0281(18) 0.0029(15) 0.0048(14) -0.0097(16)
    C2 0.0273(18) 0.0292(18) 0.0292(18) 0.0055(15) 0.0010(15) -0.0057(15)
    C3 0.0316(19) 0.0304(19) 0.0322(19) 0.0039(16) -0.0029(16) -0.0050(16)
    C4 0.034(2) 0.0330(19) 0.0270(18) 0.0037(16) -0.0009(15) -0.0057(16)
    C5 0.0337(19) 0.0284(18) 0.0275(18) 0.0008(16) 0.0073(15) -0.0039(15)
    C6 0.0242(18) 0.040(2) 0.040(2) -0.0016(16) 0.0036(16) -0.0100(17)
    C7 0.0259(18) 0.0284(18) 0.0302(19) 0.0013(15) -0.0026(15) -0.0004(15)
    C8 0.049(2) 0.041(2) 0.047(2) -0.002(2) -0.010(2) -0.018(2)
    C9 0.035(2) 0.045(2) 0.054(3) -0.0144(19) -0.0090(19) 0.000(2)
    C10 0.044(2) 0.041(2) 0.041(2) 0.0107(19) -0.0116(19) 0.0001(19)
    C11 0.045(2) 0.034(2) 0.054(3) -0.0069(19) -0.009(2) -0.0018(19)
    C12 0.052(3) 0.049(2) 0.034(2) -0.003(2) -0.0164(19) -0.0002(19)
    C13 0.053(3) 0.042(2) 0.036(2) -0.001(2) 0.0120(19) 0.0009(18)
_geom_special_details
;
All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes.
;
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
    Ti N1 . 1.823(3) ?
    Ti C1 . 2.292(3) ?
    Ti Cl2 . 2.3036(12) ?
    Ti Cl1 . 2.3104(12) ?
    Ti C2 . 2.325(3) ?
    Ti C5 . 2.341(3) ?
    Ti C4 . 2.405(3) ?
    Ti C3 . 2.406(4) ?
    N1 C7 . 1.322(4) ?
    N2 C7 . 1.319(4) ?
    N2 C8 . 1.457(5) ?
    N2 C9 . 1.464(5) ?
    C1 C2 . 1.406(5) ?
    C1 C5 . 1.412(5) ?
    C1 C6 . 1.512(5) ?
    C2 C3 . 1.422(5) ?
    C2 C10 . 1.504(5) ?
    C3 C4 . 1.405(5) ?
    C3 C11 . 1.500(5) ?
    C4 C5 . 1.422(5) ?
    C4 C12 . 1.500(5) ?
    C5 C13 . 1.500(5) ?
    C6 C7 . 1.515(5) ?
    C6 H6A . 0.9800 ?
    C6 H6B . 0.9800 ?
    C8 H8A . 0.9700 ?
    C8 H8B . 0.9700 ?
    C8 H8C . 0.9700 ?
    C9 H9A . 0.9700 ?
    C9 H9B . 0.9700 ?
    C9 H9C . 0.9700 ?
    C10 H10A . 0.9700 ?
    C10 H10B . 0.9700 ?
    C10 H10C . 0.9700 ?
    C11 H11A . 0.9700 ?
    C11 H11B . 0.9700 ?
    C11 H11C . 0.9700 ?
    C12 H12A . 0.9700 ?
    C12 H12B . 0.9700 ?
    C12 H12C . 0.9700 ?
    C13 H13A . 0.9700 ?
    C13 H13B . 0.9700 ?
    C13 H13C . 0.9700 ?
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
    _geom_angle_publ_flag
    N1 Ti C1 . . 75.92(13) ?
    N1 Ti Cl2 . . 105.63(10) ?
    C1 Ti Cl2 . . 128.71(10) ?
    N1 Ti Cl1 . . 104.29(10) ?
    C1 Ti Cl1 . . 124.25(10) ?
    Cl2 Ti Cl1 . . 105.40(5) ?
    N1 Ti C2 . . 94.34(13) ?
    C1 Ti C2 . . 35.44(13) ?
    Cl2 Ti C2 . . 94.88(10) ?
    Cl1 Ti C2 . . 147.26(9) ?
    N1 Ti C5 . . 97.46(13) ?
    C1 Ti C5 . . 35.48(12) ?
    Cl2 Ti C5 . . 146.31(9) ?
    Cl1 Ti C5 . . 91.94(10) ?
    C2 Ti C5 . . 58.66(12) ?
    N1 Ti C4 . . 131.33(13) ?
    C1 Ti C4 . . 58.19(12) ?
    Cl2 Ti C4 . . 114.96(10) ?
    Cl1 Ti C4 . . 90.13(9) ?
    C2 Ti C4 . . 57.72(12) ?
    C5 Ti C4 . . 34.83(12) ?
    N1 Ti C3 . . 128.99(13) ?
    C1 Ti C3 . . 58.23(12) ?
    Cl2 Ti C3 . . 88.61(10) ?
    Cl1 Ti C3 . . 118.89(9) ?
    C2 Ti C3 . . 34.93(12) ?
    C5 Ti C3 . . 57.70(12) ?
    C4 Ti C3 . . 33.97(12) ?
    C7 N1 Ti . . 129.5(2) ?
    C7 N2 C8 . . 120.2(3) ?
    C7 N2 C9 . . 123.5(3) ?
    C8 N2 C9 . . 116.3(3) ?
    C2 C1 C5 . . 108.4(3) ?
    C2 C1 C6 . . 125.4(3) ?
    C5 C1 C6 . . 125.5(3) ?
    C2 C1 Ti . . 73.55(19) ?
    C5 C1 Ti . . 74.12(19) ?
    C6 C1 Ti . . 110.9(2) ?
    C1 C2 C3 . . 108.0(3) ?
    C1 C2 C10 . . 127.2(3) ?
    C3 C2 C10 . . 124.8(3) ?
    C1 C2 Ti . . 71.01(19) ?
    C3 C2 Ti . . 75.7(2) ?
    C10 C2 Ti . . 119.9(2) ?
    C4 C3 C2 . . 107.8(3) ?
    C4 C3 C11 . . 126.4(3) ?
    C2 C3 C11 . . 125.7(3) ?
    C4 C3 Ti . . 73.0(2) ?
    C2 C3 Ti . . 69.41(19) ?
    C11 C3 Ti . . 125.7(3) ?
    C3 C4 C5 . . 108.3(3) ?
    C3 C4 C12 . . 126.4(3) ?
    C5 C4 C12 . . 125.2(3) ?
    C3 C4 Ti . . 73.1(2) ?
    C5 C4 Ti . . 70.10(19) ?
    C12 C4 Ti . . 125.2(3) ?
    C1 C5 C4 . . 107.5(3) ?
    C1 C5 C13 . . 126.9(3) ?
    C4 C5 C13 . . 125.5(3) ?
    C1 C5 Ti . . 70.40(19) ?
    C4 C5 Ti . . 75.1(2) ?
    C13 C5 Ti . . 121.3(2) ?
    C1 C6 C7 . . 106.7(3) ?
    C1 C6 H6A . . 110.4 ?
    C7 C6 H6A . . 110.4 ?
    C1 C6 H6B . . 110.4 ?
    C7 C6 H6B . . 110.4 ?
    H6A C6 H6B . . 108.6 ?
    N2 C7 N1 . . 122.9(3) ?
    N2 C7 C6 . . 120.4(3) ?
    N1 C7 C6 . . 116.7(3) ?
    N2 C8 H8A . . 109.5 ?
    N2 C8 H8B . . 109.5 ?
    H8A C8 H8B . . 109.5 ?
    N2 C8 H8C . . 109.5 ?
    H8A C8 H8C . . 109.5 ?
    H8B C8 H8C . . 109.5 ?
    N2 C9 H9A . . 109.5 ?
    N2 C9 H9B . . 109.5 ?
    H9A C9 H9B . . 109.5 ?
    N2 C9 H9C . . 109.5 ?
    H9A C9 H9C . . 109.5 ?
    H9B C9 H9C . . 109.5 ?
    C2 C10 H10A . . 109.5 ?
    C2 C10 H10B . . 109.5 ?
    H10A C10 H10B . . 109.5 ?
    C2 C10 H10C . . 109.5 ?
    H10A C10 H10C . . 109.5 ?
    H10B C10 H10C . . 109.5 ?
    C3 C11 H11A . . 109.5 ?
    C3 C11 H11B . . 109.5 ?
    H11A C11 H11B . . 109.5 ?
    C3 C11 H11C . . 109.5 ?
    H11A C11 H11C . . 109.5 ?
    H11B C11 H11C . . 109.5 ?
    C4 C12 H12A . . 109.5 ?
    C4 C12 H12B . . 109.5 ?
    H12A C12 H12B . . 109.5 ?
    C4 C12 H12C . . 109.5 ?
    H12A C12 H12C . . 109.5 ?
    H12B C12 H12C . . 109.5 ?
    C5 C13 H13A . . 109.5 ?
    C5 C13 H13B . . 109.5 ?
    H13A C13 H13B . . 109.5 ?
    C5 C13 H13C . . 109.5 ?
    H13A C13 H13C . . 109.5 ?
    H13B C13 H13C . . 109.5 ?
data_global
_journal_date_recd_electronic     2009-04-22
_journal_date_accepted     2009-04-28
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2009
_journal_volume     65
_journal_issue      6
_journal_page_first     m611
_journal_page_last     m611
_journal_paper_category     QM
_journal_coeditor_code     CV2554
_publ_contact_author_name     'Donglong Guo'
_publ_contact_author_address
;
School of Life Science and Technology, Shanxi University, Taiyuan 030006, P. R.
 China
;
_publ_contact_author_email     mszhou@sxu.edu.cn
_publ_contact_author_fax     ?
_publ_contact_author_phone     ?
_publ_section_title
;
The ansa-bridged cyclopentadienyl titanium complex
[{η⁵-C₅Me₄CH₂-C(NMe₂)=N}TiCl₂]
;
loop_
    _publ_author_name
    _publ_author_footnote
    _publ_author_address
    'Guo, Donglong' .
;
School of Life Science and Technology
Shanxi University
Taiyuan 030006
People's Republic of China
;
    'Tong, Hong-Bo' .
;
Institute of Applied Chemistry
Shanxi University
Taiyuan 030006
People's Republic of China
;
    'Zhou, Meisu' .
;
Institute of Applied Chemistry
Shanxi University
Taiyuan 030006
People's Republic of China
;
_publ_section_synopsis     .
