#------------------------------------------------------------------------------
#$Date: 2016-03-21 08:19:26 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178602 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/13/4071349.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_4071349
loop_
_publ_author_name
'Lorber, Christian'
'Vendier, Laure'
_publ_section_title
;
 Routes to New N-Heterocyclic Carbene Titanium(IV) Imido Complexes
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2774
_journal_paper_doi               10.1021/om800121g
_journal_volume                  27
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C35 H48 Cl2 N4 Ti1'
_chemical_formula_sum            'C35 H48 Cl2 N4 Ti'
_chemical_formula_weight         643.57
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2bc 2ac'
_symmetry_space_group_name_H-M   'P c a b'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.2517(5)
_cell_length_b                   42.872(2)
_cell_length_c                   13.2474(5)
_cell_measurement_reflns_used    7500
_cell_measurement_temperature    180
_cell_measurement_theta_max      29
_cell_measurement_theta_min      2.8213
_cell_measurement_wavelength     0.71073
_cell_volume                     7526.2(5)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
        (compiled Aug 28 2006,13:05:05)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
        (compiled Aug 28 2006,13:05:05)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
        (compiled Aug 28 2006,13:05:05)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       ω-φ
_diffrn_orient_matrix_UB_11      0.0533415254
_diffrn_orient_matrix_UB_12      -0.0049586179
_diffrn_orient_matrix_UB_13      -0.0002372149
_diffrn_orient_matrix_UB_21      -0.0030457022
_diffrn_orient_matrix_UB_22      -0.0391777131
_diffrn_orient_matrix_UB_23      0.0112507177
_diffrn_orient_matrix_UB_31      -0.0039789594
_diffrn_orient_matrix_UB_32      -0.0362073842
_diffrn_orient_matrix_UB_33      -0.0121620394
_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  0.1266
_diffrn_reflns_av_unetI/netI     0.1475
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            50967
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.08
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.396
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
        (compiled Aug 28 2006,13:05:05)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.08
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         6865
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1223
_refine_ls_R_factor_gt           0.0566
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0630P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1313
_refine_ls_wR_factor_ref         0.1625
_reflns_number_gt                3192
_reflns_number_total             6865
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            om800121g-file001.cif
_cod_data_source_block           (3a)
_cod_database_code               4071349
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'x+1/2, -y, -z+1/2'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'-x-1/2, y, z-1/2'
'x-1/2, -y-1/2, 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
C1 C -0.0702(3) 0.09170(10) -0.0686(3) 0.0231(11) Uani 1 1 d .
C2 C -0.1452(3) 0.07718(10) -0.1269(3) 0.0256(11) Uani 1 1 d .
C3 C -0.1662(4) 0.04576(11) -0.1075(4) 0.0407(14) Uani 1 1 d .
H3 H -0.2157 0.0357 -0.145 0.049 Uiso 1 1 calc R
C4 C -0.1146(4) 0.02933(11) -0.0333(4) 0.0416(14) Uani 1 1 d .
H4 H -0.1303 0.0085 -0.021 0.05 Uiso 1 1 calc R
C5 C -0.0411(4) 0.04371(11) 0.0213(4) 0.0349(13) Uani 1 1 d .
H5 H -0.0068 0.0325 0.0706 0.042 Uiso 1 1 calc R
C6 C -0.0160(3) 0.07475(10) 0.0053(3) 0.0233(11) Uani 1 1 d .
C7 C -0.2046(3) 0.09446(11) -0.2055(3) 0.0323(12) Uani 1 1 d .
H7 H -0.1617 0.1114 -0.2302 0.039 Uiso 1 1 calc R
C8 C -0.2335(4) 0.07432(11) -0.2978(4) 0.0524(16) Uani 1 1 d .
H8A H -0.1742 0.0643 -0.324 0.079 Uiso 1 1 calc R
H8B H -0.2624 0.0874 -0.3491 0.079 Uiso 1 1 calc R
H8C H -0.2817 0.0588 -0.2778 0.079 Uiso 1 1 calc R
C9 C -0.2980(4) 0.10938(11) -0.1591(4) 0.0449(14) Uani 1 1 d .
H9A H -0.343 0.0934 -0.1358 0.067 Uiso 1 1 calc R
H9B H -0.3316 0.1219 -0.209 0.067 Uiso 1 1 calc R
H9C H -0.2784 0.1223 -0.1033 0.067 Uiso 1 1 calc R
C10 C 0.0654(3) 0.09057(10) 0.0664(4) 0.0295(12) Uani 1 1 d .
H10 H 0.0939 0.1074 0.0251 0.035 Uiso 1 1 calc R
C11 C 0.1523(4) 0.06881(12) 0.0969(4) 0.0474(15) Uani 1 1 d .
H11A H 0.1283 0.0538 0.1449 0.071 Uiso 1 1 calc R
H11B H 0.2057 0.0809 0.1267 0.071 Uiso 1 1 calc R
H11C H 0.1773 0.0582 0.0382 0.071 Uiso 1 1 calc R
C12 C 0.0197(4) 0.10545(12) 0.1619(3) 0.0451(14) Uani 1 1 d .
H12A H -0.0359 0.1186 0.1433 0.068 Uiso 1 1 calc R
H12B H 0.0702 0.1177 0.1955 0.068 Uiso 1 1 calc R
H12C H -0.0036 0.0893 0.2065 0.068 Uiso 1 1 calc R
C13 C 0.0716(3) 0.17044(10) -0.2192(3) 0.0215(11) Uani 1 1 d .
C14 C 0.1735(4) 0.19286(11) -0.3352(4) 0.0357(13) Uani 1 1 d .
H14 H 0.2047 0.208 -0.3746 0.043 Uiso 1 1 calc R
C15 C 0.1889(4) 0.16239(12) -0.3395(4) 0.0431(14) Uani 1 1 d .
H15 H 0.234 0.1522 -0.3819 0.052 Uiso 1 1 calc R
C16 C 0.0693(3) 0.22866(10) -0.2327(3) 0.0238(11) Uani 1 1 d .
C17 C 0.1257(3) 0.24507(10) -0.1627(3) 0.0237(11) Uani 1 1 d .
C18 C 0.0937(4) 0.27489(10) -0.1373(3) 0.0274(11) Uani 1 1 d .
H18 H 0.13 0.2863 -0.09 0.033 Uiso 1 1 calc R
C19 C 0.0091(4) 0.28791(11) -0.1811(4) 0.0377(13) Uani 1 1 d .
C20 C -0.0419(4) 0.27102(12) -0.2539(4) 0.0357(13) Uani 1 1 d .
H20 H -0.0978 0.28 -0.2847 0.043 Uiso 1 1 calc R
C21 C -0.0133(4) 0.24136(11) -0.2827(3) 0.0312(12) Uani 1 1 d .
C22 C 0.2217(3) 0.23280(11) -0.1171(4) 0.0379(13) Uani 1 1 d .
H22A H 0.2315 0.2115 -0.1375 0.057 Uiso 1 1 calc R
H22B H 0.2174 0.2338 -0.0448 0.057 Uiso 1 1 calc R
H22C H 0.2776 0.2452 -0.1398 0.057 Uiso 1 1 calc R
C23 C -0.0637(4) 0.22475(13) -0.3693(4) 0.0502(16) Uani 1 1 d .
H23A H -0.1258 0.2351 -0.3857 0.075 Uiso 1 1 calc R
H23B H -0.0775 0.2036 -0.3504 0.075 Uiso 1 1 calc R
H23C H -0.0199 0.225 -0.427 0.075 Uiso 1 1 calc R
C24 C -0.0239(5) 0.32055(12) -0.1505(5) 0.069(2) Uani 1 1 d .
H24A H -0.0637 0.3194 -0.0901 0.104 Uiso 1 1 calc R
H24B H -0.0634 0.3296 -0.2037 0.104 Uiso 1 1 calc R
H24C H 0.0346 0.3332 -0.1384 0.104 Uiso 1 1 calc R
C25 C 0.1212(3) 0.11550(10) -0.2585(3) 0.0249(11) Uani 1 1 d .
C26 C 0.0573(4) 0.09880(11) -0.3205(4) 0.0328(12) Uani 1 1 d .
C27 C 0.0560(4) 0.06657(11) -0.3115(4) 0.0382(13) Uani 1 1 d .
H27 H 0.0147 0.0549 -0.3538 0.046 Uiso 1 1 calc R
C28 C 0.1156(4) 0.05152(11) -0.2400(4) 0.0366(13) Uani 1 1 d .
C29 C 0.1786(4) 0.06860(11) -0.1802(4) 0.0343(13) Uani 1 1 d .
H29 H 0.2193 0.0584 -0.1336 0.041 Uiso 1 1 calc R
C30 C 0.1833(3) 0.10100(11) -0.1872(3) 0.0315(12) Uani 1 1 d .
C31 C -0.0065(4) 0.11452(11) -0.3998(4) 0.0481(15) Uani 1 1 d .
H31A H -0.0406 0.1321 -0.3706 0.072 Uiso 1 1 calc R
H31B H -0.0554 0.1 -0.4253 0.072 Uiso 1 1 calc R
H31C H 0.0359 0.1215 -0.4541 0.072 Uiso 1 1 calc R
C32 C 0.1114(5) 0.01688(11) -0.2296(4) 0.0616(18) Uani 1 1 d .
H32A H 0.1591 0.0103 -0.1793 0.092 Uiso 1 1 calc R
H32B H 0.1278 0.0074 -0.2931 0.092 Uiso 1 1 calc R
H32C H 0.0447 0.0107 -0.2096 0.092 Uiso 1 1 calc R
C33 C 0.2562(4) 0.11930(11) -0.1234(4) 0.0393(13) Uani 1 1 d .
H33A H 0.3044 0.1295 -0.1662 0.059 Uiso 1 1 calc R
H33B H 0.2908 0.1054 -0.0782 0.059 Uiso 1 1 calc R
H33C H 0.22 0.1346 -0.085 0.059 Uiso 1 1 calc R
C34 C -0.1407(4) 0.20925(11) 0.0635(4) 0.0415(14) Uani 1 1 d .
H34A H -0.1874 0.2165 0.0132 0.062 Uiso 1 1 calc R
H34B H -0.0778 0.2201 0.0562 0.062 Uiso 1 1 calc R
H34C H -0.1679 0.2131 0.1294 0.062 Uiso 1 1 calc R
C35 C -0.2180(4) 0.15849(12) 0.0673(3) 0.0391(14) Uani 1 1 d .
H35A H -0.2455 0.1643 0.1317 0.059 Uiso 1 1 calc R
H35B H -0.205 0.1365 0.0664 0.059 Uiso 1 1 calc R
H35C H -0.2653 0.1636 0.015 0.059 Uiso 1 1 calc R
N1 N -0.0499(3) 0.12352(8) -0.0819(3) 0.0207(9) Uani 1 1 d .
N2 N 0.1024(3) 0.19782(8) -0.2614(3) 0.0277(9) Uani 1 1 d .
N3 N 0.1266(3) 0.14868(8) -0.2703(3) 0.0282(10) Uani 1 1 d .
N4 N -0.1239(3) 0.17537(8) 0.0504(3) 0.0263(9) Uani 1 1 d .
H4A H -0.0835 0.1698 0.103 0.032 Uiso 1 1 calc R
Cl1 Cl 0.09916(9) 0.17770(3) 0.01886(9) 0.0329(3) Uani 1 1 d .
Cl2 Cl -0.17047(8) 0.18368(3) -0.17743(8) 0.0286(3) Uani 1 1 d .
Ti1 Ti -0.03592(6) 0.162916(17) -0.08731(6) 0.0196(2) Uani 1 1 d .
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 0 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
N1 C1 C2 119.9(4)
N1 C1 C6 119.3(4)
C2 C1 C6 120.8(4)
C3 C2 C1 117.8(4)
C3 C2 C7 119.9(4)
C1 C2 C7 122.3(4)
C4 C3 C2 121.4(5)
C5 C4 C3 119.9(5)
C4 C5 C6 121.6(5)
C5 C6 C1 118.5(4)
C5 C6 C10 121.3(4)
C1 C6 C10 120.2(4)
C2 C7 C9 110.7(4)
C2 C7 C8 113.8(4)
C9 C7 C8 110.6(4)
C6 C10 C11 113.8(4)
C6 C10 C12 110.2(4)
C11 C10 C12 109.3(4)
N2 C13 N3 103.0(4)
N2 C13 Ti1 128.6(3)
N3 C13 Ti1 128.2(3)
C15 C14 N2 106.8(4)
C14 C15 N3 107.6(4)
C17 C16 C21 123.1(4)
C17 C16 N2 118.6(4)
C21 C16 N2 118.2(4)
C16 C17 C18 117.8(4)
C16 C17 C22 123.3(4)
C18 C17 C22 118.9(4)
C19 C18 C17 121.3(4)
C18 C19 C20 118.6(5)
C18 C19 C24 119.6(5)
C20 C19 C24 121.8(5)
C21 C20 C19 122.8(5)
C20 C21 C16 116.4(4)
C20 C21 C23 121.7(5)
C16 C21 C23 121.8(5)
C26 C25 C30 122.2(4)
C26 C25 N3 118.7(4)
C30 C25 N3 119.1(4)
C25 C26 C27 118.2(5)
C25 C26 C31 121.8(4)
C27 C26 C31 119.9(4)
C26 C27 C28 120.9(5)
C29 C28 C27 119.6(5)
C29 C28 C32 120.2(5)
C27 C28 C32 120.2(5)
C28 C29 C30 121.6(5)
C29 C30 C25 117.5(4)
C29 C30 C33 120.7(5)
C25 C30 C33 121.7(4)
C1 N1 Ti1 173.2(3)
C13 N2 C14 111.3(4)
C13 N2 C16 126.1(4)
C14 N2 C16 122.5(4)
C13 N3 C15 111.2(4)
C13 N3 C25 126.7(4)
C15 N3 C25 122.0(4)
C35 N4 C34 109.9(4)
C35 N4 Ti1 117.0(3)
C34 N4 Ti1 114.2(3)
N1 Ti1 N4 98.41(15)
N1 Ti1 C13 103.96(16)
N4 Ti1 C13 157.05(15)
N1 Ti1 Cl2 108.58(13)
N4 Ti1 Cl2 85.84(10)
C13 Ti1 Cl2 91.81(11)
N1 Ti1 Cl1 108.89(12)
N4 Ti1 Cl1 81.08(10)
C13 Ti1 Cl1 86.84(11)
Cl2 Ti1 Cl1 141.67(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 N1 1.401(5)
C1 C2 1.404(6)
C1 C6 1.415(6)
C2 C3 1.400(6)
C2 C7 1.500(6)
C3 C4 1.388(6)
C4 C5 1.362(6)
C5 C6 1.388(6)
C6 C10 1.510(6)
C7 C9 1.523(6)
C7 C8 1.546(6)
C10 C11 1.536(6)
C10 C12 1.541(6)
C13 N2 1.363(5)
C13 N3 1.364(5)
C13 Ti1 2.277(4)
C14 C15 1.323(6)
C14 N2 1.374(5)
C15 N3 1.366(5)
C16 C17 1.384(6)
C16 C21 1.391(6)
C16 N2 1.444(5)
C17 C18 1.388(6)
C17 C22 1.504(6)
C18 C19 1.380(6)
C19 C20 1.382(7)
C19 C24 1.521(6)
C20 C21 1.381(6)
C21 C23 1.506(6)
C25 C26 1.381(6)
C25 C30 1.398(6)
C25 N3 1.433(5)
C26 C27 1.387(6)
C26 C31 1.507(6)
C27 C28 1.391(7)
C28 C29 1.364(6)
C28 C32 1.492(6)
C29 C30 1.394(6)
C30 C33 1.505(6)
C34 N4 1.480(5)
C35 N4 1.459(5)
N1 Ti1 1.701(3)
N4 Ti1 2.230(3)
Cl1 Ti1 2.3631(14)
Cl2 Ti1 2.3231(13)
