#------------------------------------------------------------------------------
#$Date: 2015-07-11 00:58:09 +0300 (Sat, 11 Jul 2015) $
#$Revision: 143626 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/51/7035122.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_7035122
loop_
_publ_author_name
'Pedrosa, Sergio'
'Vidal, Fernando'
'Lee, Lucia Myongwon'
'Vargas-Baca, Ignacio'
'Gómez-Sal, Pilar'
'Mosquera, Marta E. G.'
_publ_section_title
;
 Imido-pyridine Ti(iv) compounds: synthesis of unusual imido-amido
 heterobimetallic derivatives.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11119
_journal_page_last               11128
_journal_paper_doi               10.1039/c5dt01320h
_journal_volume                  44
_journal_year                    2015
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C32 H42 Cl2 N4 Ti2'
_chemical_formula_sum            'C32 H42 Cl2 N4 Ti2'
_chemical_formula_weight         649.4
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2012-05-10T18:01:37-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2015-03-27 deposited with the CCDC.
2015-05-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.075(17)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.570(2)
_cell_length_b                   16.1114(13)
_cell_length_c                   10.626(3)
_cell_measurement_reflns_used    245
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      16.34
_cell_measurement_theta_min      3.17
_cell_measurement_wavelength     0.71073
_cell_volume                     1528.8(6)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.01
_diffrn_orient_matrix_UB_12      0
_diffrn_orient_matrix_UB_13      0
_diffrn_orient_matrix_UB_21      0
_diffrn_orient_matrix_UB_22      0.01
_diffrn_orient_matrix_UB_23      0
_diffrn_orient_matrix_UB_31      0
_diffrn_orient_matrix_UB_32      0
_diffrn_orient_matrix_UB_33      0.01
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1192
_diffrn_reflns_av_unetI/netI     0.1135
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10644
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.26
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.726
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.584
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         3490
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.1532
_refine_ls_R_factor_gt           0.0695
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0447P)²+3.3846P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1309
_refine_ls_wR_factor_ref         0.1643
_reflns_number_gt                2031
_reflns_number_total             3490
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c5dt01320h1.cif
_cod_data_source_block           1b
_cod_depositor_comments
'Adding full bibliography for 7035122--7035125.cif.'
_cod_database_code               7035122
loop_
_space_group_symop_operation_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_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 0.53292(9) 0.05127(5) 0.89594(8) 0.0208(2) Uani 1 1 d .
Cl1 Cl 0.33622(14) 0.08907(8) 0.69641(13) 0.0338(3) Uani 1 1 d .
N1 N 0.5373(4) 0.0555(2) 1.0977(4) 0.0238(8) Uani 1 1 d .
N2 N 0.4811(4) 0.1713(2) 0.9740(4) 0.0257(9) Uani 1 1 d .
C1 C 0.5219(5) 0.1398(3) 1.0999(5) 0.0247(10) Uani 1 1 d .
C2 C 0.5462(5) 0.1921(3) 1.2097(5) 0.0299(11) Uani 1 1 d .
H2 H 0.5804 0.1714 1.2973 0.036 Uiso 1 1 calc R
C3 C 0.5179(6) 0.2761(3) 1.1847(5) 0.0339(12) Uani 1 1 d .
H3 H 0.5328 0.312 1.2569 0.041 Uiso 1 1 calc R
C4 C 0.4678(5) 0.3080(3) 1.0544(5) 0.0302(11) Uani 1 1 d .
C5 C 0.4527(5) 0.2518(3) 0.9517(5) 0.0276(11) Uani 1 1 d .
H5 H 0.4214 0.2712 0.8634 0.033 Uiso 1 1 calc R
C6 C 0.7510(5) 0.1350(3) 0.9121(5) 0.0284(11) Uani 1 1 d .
C7 C 0.7970(5) 0.0676(3) 1.0029(5) 0.0296(12) Uani 1 1 d .
C8 C 0.7701(5) -0.0070(3) 0.9275(5) 0.0276(11) Uani 1 1 d .
C9 C 0.7020(5) 0.0147(3) 0.7894(5) 0.0247(10) Uani 1 1 d .
C10 C 0.6911(5) 0.1020(3) 0.7805(5) 0.0257(10) Uani 1 1 d .
C11 C 0.7791(6) 0.2255(3) 0.9464(7) 0.0486(16) Uani 1 1 d .
H11A H 0.8202 0.232 1.0427 0.073 Uiso 1 1 calc R
H11B H 0.6866 0.2555 0.9106 0.073 Uiso 1 1 calc R
H11C H 0.8487 0.2468 0.908 0.073 Uiso 1 1 calc R
C12 C 0.8763(6) 0.0746(4) 1.1530(5) 0.0480(16) Uani 1 1 d .
H12A H 0.8944 0.0201 1.192 0.072 Uiso 1 1 calc R
H12B H 0.8152 0.1054 1.191 0.072 Uiso 1 1 calc R
H12C H 0.97 0.1028 1.1718 0.072 Uiso 1 1 calc R
C13 C 0.8185(6) -0.0910(3) 0.9863(6) 0.0403(14) Uani 1 1 d .
H13A H 0.8609 -0.0869 1.0828 0.06 Uiso 1 1 calc R
H13B H 0.8922 -0.1126 0.9531 0.06 Uiso 1 1 calc R
H13C H 0.7336 -0.1275 0.9608 0.06 Uiso 1 1 calc R
C14 C 0.6565(6) -0.0440(3) 0.6718(5) 0.0382(13) Uani 1 1 d .
H14A H 0.6746 -0.1 0.7042 0.057 Uiso 1 1 calc R
H14B H 0.7138 -0.0324 0.616 0.057 Uiso 1 1 calc R
H14C H 0.5518 -0.0369 0.6201 0.057 Uiso 1 1 calc R
C15 C 0.6359(6) 0.1526(3) 0.6546(6) 0.0428(14) Uani 1 1 d .
H15A H 0.6008 0.1165 0.5778 0.064 Uiso 1 1 calc R
H15B H 0.7161 0.1864 0.6489 0.064 Uiso 1 1 calc R
H15C H 0.5554 0.1876 0.6561 0.064 Uiso 1 1 calc R
C16 C 0.4375(6) 0.3991(3) 1.0269(6) 0.0443(15) Uani 1 1 d .
H16A H 0.4542 0.4277 1.1103 0.067 Uiso 1 1 calc R
H16B H 0.3356 0.4068 0.9678 0.067 Uiso 1 1 calc R
H16C H 0.5036 0.4208 0.9851 0.067 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 0.0033 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'
Cl Cl 0.1484 0.1585 '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'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-4 1 6 0.103
1 6 3 0.134
-4 -5 1 0.109
0 -4 -3 0.098
19 7 -18 0.128
4 -2 -1 0.108
-4 5 2 0.164
-1 4 -2 0.087
1 -4 2 0.198
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 Ti1 N1 82.52(16) 3_657 .
N1 Ti1 N2 131.21(16) 3_657 .
N1 Ti1 N2 61.60(14) . .
N1 Ti1 Cl1 95.15(12) 3_657 .
N1 Ti1 Cl1 128.17(11) . .
N2 Ti1 Cl1 84.13(11) . .
N1 Ti1 C9 96.04(16) 3_657 .
N1 Ti1 C9 136.25(16) . .
N2 Ti1 C9 132.68(15) . .
Cl1 Ti1 C9 95.57(12) . .
N1 Ti1 C8 88.16(16) 3_657 .
N1 Ti1 C8 101.50(16) . .
N2 Ti1 C8 128.46(16) . .
Cl1 Ti1 C8 130.26(13) . .
C9 Ti1 C8 34.94(16) . .
N1 Ti1 C7 114.84(17) 3_657 .
N1 Ti1 C7 83.29(16) . .
N2 Ti1 C7 93.82(16) . .
Cl1 Ti1 C7 140.21(13) . .
C9 Ti1 C7 57.56(16) . .
C8 Ti1 C7 34.68(17) . .
N1 Ti1 C10 129.39(17) 3_657 .
N1 Ti1 C10 135.50(16) . .
N2 Ti1 C10 99.18(15) . .
Cl1 Ti1 C10 84.20(12) . .
C9 Ti1 C10 34.43(15) . .
C8 Ti1 C10 57.35(16) . .
C7 Ti1 C10 56.80(16) . .
N1 Ti1 C6 145.24(17) 3_657 .
N1 Ti1 C6 101.83(16) . .
N2 Ti1 C6 78.05(15) . .
Cl1 Ti1 C6 107.88(13) . .
C9 Ti1 C6 56.95(16) . .
C8 Ti1 C6 57.10(16) . .
C7 Ti1 C6 34.08(17) . .
C10 Ti1 C6 33.83(16) . .
N1 Ti1 C1 110.55(16) 3_657 .
N1 Ti1 C1 31.23(14) . .
N2 Ti1 C1 30.91(14) . .
Cl1 Ti1 C1 110.23(11) . .
C9 Ti1 C1 140.28(16) . .
C8 Ti1 C1 114.81(16) . .
C7 Ti1 C1 84.11(16) . .
C10 Ti1 C1 117.04(16) . .
C6 Ti1 C1 85.92(16) . .
N1 Ti1 Ti1 44.71(12) 3_657 3_657
N1 Ti1 Ti1 37.81(10) . 3_657
N2 Ti1 Ti1 94.01(11) . 3_657
Cl1 Ti1 Ti1 119.61(6) . 3_657
C9 Ti1 Ti1 125.28(12) . 3_657
C8 Ti1 Ti1 96.99(12) . 3_657
C7 Ti1 Ti1 100.19(13) . 3_657
C10 Ti1 Ti1 153.97(12) . 3_657
C6 Ti1 Ti1 130.80(13) . 3_657
C1 Ti1 Ti1 67.07(11) . 3_657
C1 N1 Ti1 151.3(3) . 3_657
C1 N1 Ti1 94.9(3) . .
Ti1 N1 Ti1 97.48(16) 3_657 .
C5 N2 C1 120.7(4) . .
C5 N2 Ti1 147.0(3) . .
C1 N2 Ti1 91.1(3) . .
N2 C1 N1 110.6(4) . .
N2 C1 C2 120.4(4) . .
N1 C1 C2 129.0(5) . .
N2 C1 Ti1 58.0(2) . .
N1 C1 Ti1 53.9(2) . .
C2 C1 Ti1 167.8(3) . .
C1 C2 C3 117.9(5) . .
C2 C3 C4 121.7(5) . .
C5 C4 C3 116.3(4) . .
C5 C4 C16 121.8(5) . .
C3 C4 C16 121.8(5) . .
N2 C5 C4 122.8(5) . .
C10 C6 C7 107.6(4) . .
C10 C6 C11 125.4(5) . .
C7 C6 C11 126.5(5) . .
C10 C6 Ti1 71.9(3) . .
C7 C6 Ti1 70.8(3) . .
C11 C6 Ti1 128.9(3) . .
C8 C7 C6 108.6(4) . .
C8 C7 C12 125.7(5) . .
C6 C7 C12 125.5(5) . .
C8 C7 Ti1 72.0(3) . .
C6 C7 Ti1 75.1(3) . .
C12 C7 Ti1 123.9(3) . .
C7 C8 C9 107.3(4) . .
C7 C8 C13 124.6(5) . .
C9 C8 C13 127.9(5) . .
C7 C8 Ti1 73.3(3) . .
C9 C8 Ti1 72.3(3) . .
C13 C8 Ti1 123.9(3) . .
C10 C9 C8 108.1(4) . .
C10 C9 C14 125.4(4) . .
C8 C9 C14 126.4(4) . .
C10 C9 Ti1 74.7(3) . .
C8 C9 Ti1 72.8(3) . .
C14 C9 Ti1 120.8(3) . .
C6 C10 C9 108.4(4) . .
C6 C10 C15 124.7(5) . .
C9 C10 C15 126.8(5) . .
C6 C10 Ti1 74.3(3) . .
C9 C10 Ti1 70.9(3) . .
C15 C10 Ti1 123.9(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 N1 1.857(4) 3_657
Ti1 N1 2.131(4) .
Ti1 N2 2.229(4) .
Ti1 Cl1 2.3536(16) .
Ti1 C9 2.359(4) .
Ti1 C8 2.366(4) .
Ti1 C7 2.383(5) .
Ti1 C10 2.409(4) .
Ti1 C6 2.439(4) .
Ti1 C1 2.628(5) .
Ti1 Ti1 3.0030(17) 3_657
N1 C1 1.368(6) .
N1 Ti1 1.857(4) 3_657
N2 C5 1.328(6) .
N2 C1 1.350(6) .
C1 C2 1.389(7) .
C2 C3 1.387(7) .
C3 C4 1.390(7) .
C4 C5 1.386(7) .
C4 C16 1.504(6) .
C6 C10 1.411(7) .
C6 C7 1.414(7) .
C6 C11 1.503(7) .
C7 C8 1.416(7) .
C7 C12 1.505(7) .
C8 C9 1.419(7) .
C8 C13 1.492(7) .
C9 C10 1.412(6) .
C9 C14 1.501(7) .
C10 C15 1.492(7) .
