#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:42:56 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179932 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/27/7022740.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_7022740
loop_
_publ_author_name
'Vidal, Fernando'
'Dávila, Ma Angeles'
'San Torcuato, Ainhoa'
'Gómez-Sal, Pilar'
'Mosquera, Marta E. G.'
_publ_section_title
;
 Functionalized imido-bridged Ti(IV) complexes as new building blocks for
 supramolecular arrangements: generation of a 1D structure through a
 Mg-Cl···I-C halogen bonding interaction.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7074
_journal_page_last               7084
_journal_paper_doi               10.1039/c3dt32943g
_journal_volume                  42
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C34 H38 Cl2 N4 Ti2'
_chemical_formula_sum            'C34 H38 Cl2 N4 Ti2'
_chemical_formula_weight         669.38
_chemical_name_systematic
;
?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_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             2012-10-05T15:31:14-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                98.36(5)
_cell_angle_beta                 91.79(4)
_cell_angle_gamma                110.62(5)
_cell_formula_units_Z            1
_cell_length_a                   8.472(7)
_cell_length_b                   10.036(8)
_cell_length_c                   10.142(4)
_cell_measurement_reflns_used    276
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      17.35
_cell_measurement_theta_min      3.45
_cell_measurement_wavelength     0.71073
_cell_volume                     795.3(10)
_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)'
_computing_structure_solution    'SIR2002 (Giacovazzo et al, 2003)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.1447
_diffrn_reflns_av_unetI/netI     0.0755
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            19329
_diffrn_reflns_reduction_process
;
Scaled and merged with Sortav
R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.14
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.7
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             348
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.1
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3629
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0952
_refine_ls_R_factor_gt           0.063
_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)+(0.0496P)²+1.9279P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1429
_refine_ls_wR_factor_ref         0.1649
_reflns_number_gt                2684
_reflns_number_total             3629
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c3dt32943g.txt
_cod_data_source_block           2a
_cod_database_code               7022740
loop_
_space_group_symop_operation_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
Ti1 Ti 0.00748(8) 0.63443(7) 0.07208(6) 0.0239(2) Uani 1 1 d .
Cl1 Cl -0.19856(13) 0.70253(11) -0.01842(11) 0.0390(3) Uani 1 1 d .
N1 N -0.1046(4) 0.4329(3) 0.0815(3) 0.0269(7) Uani 1 1 d .
N2 N -0.6468(6) 0.0994(5) 0.5098(5) 0.0584(12) Uani 1 1 d .
C1 C -0.2164(5) 0.3637(4) 0.1710(4) 0.0293(8) Uani 1 1 d .
C2 C -0.1859(5) 0.2589(4) 0.2344(4) 0.0328(9) Uani 1 1 d .
H2 H -0.0914 0.2347 0.2172 0.039 Uiso 1 1 calc R
C3 C -0.2964(6) 0.1911(5) 0.3230(4) 0.0382(10) Uani 1 1 d .
H3 H -0.2754 0.1222 0.3656 0.046 Uiso 1 1 calc R
C4 C -0.4376(5) 0.2261(5) 0.3477(4) 0.0348(9) Uani 1 1 d .
C5 C -0.4697(5) 0.3289(5) 0.2850(4) 0.0365(9) Uani 1 1 d .
H5 H -0.5653 0.3517 0.3018 0.044 Uiso 1 1 calc R
C6 C -0.3599(5) 0.3973(4) 0.1977(4) 0.0335(9) Uani 1 1 d .
H6 H -0.3817 0.4665 0.1561 0.04 Uiso 1 1 calc R
C7 C 0.0453(5) 0.7354(4) 0.3044(4) 0.0316(8) Uani 1 1 d .
C8 C 0.1687(5) 0.6737(4) 0.2762(4) 0.0314(8) Uani 1 1 d .
C9 C 0.2761(5) 0.7516(4) 0.1865(4) 0.0321(8) Uani 1 1 d .
C10 C 0.2162(5) 0.8611(4) 0.1597(4) 0.0320(8) Uani 1 1 d .
C11 C 0.0741(5) 0.8518(4) 0.2332(4) 0.0310(8) Uani 1 1 d .
C12 C -0.5539(6) 0.1544(5) 0.4388(4) 0.0413(10) Uani 1 1 d .
C13 C -0.0190(7) 0.9542(5) 0.2436(5) 0.0461(11) Uani 1 1 d .
H13A H 0.0248 1.0233 0.1852 0.069 Uiso 1 1 calc R
H13B H -0.0041 1.0037 0.3342 0.069 Uiso 1 1 calc R
H13C H -0.1373 0.9015 0.2183 0.069 Uiso 1 1 calc R
C14 C -0.0874(6) 0.6950(6) 0.4020(4) 0.0485(12) Uani 1 1 d .
H14A H -0.155 0.7542 0.4014 0.073 Uiso 1 1 calc R
H14B H -0.0332 0.7098 0.4902 0.073 Uiso 1 1 calc R
H14C H -0.1585 0.5953 0.3764 0.073 Uiso 1 1 calc R
C15 C 0.1922(7) 0.5539(5) 0.3366(4) 0.0447(11) Uani 1 1 d .
H15A H 0.2854 0.5325 0.3 0.067 Uiso 1 1 calc R
H15B H 0.0909 0.4695 0.3167 0.067 Uiso 1 1 calc R
H15C H 0.2152 0.5826 0.4318 0.067 Uiso 1 1 calc R
C16 C 0.4334(6) 0.7306(6) 0.1426(5) 0.0462(11) Uani 1 1 d .
H16A H 0.4431 0.6481 0.1747 0.069 Uiso 1 1 calc R
H16B H 0.53 0.8149 0.1782 0.069 Uiso 1 1 calc R
H16C H 0.4283 0.7151 0.0466 0.069 Uiso 1 1 calc R
C17 C 0.2910(7) 0.9701(5) 0.0704(5) 0.0472(12) Uani 1 1 d .
H17A H 0.2265 1.0319 0.0696 0.071 Uiso 1 1 calc R
H17B H 0.2881 0.9211 -0.0188 0.071 Uiso 1 1 calc R
H17C H 0.4061 1.0271 0.1035 0.071 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'
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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-7 -2 1 0.11
-3 6 -1 0.142
3 -5 2 0.164
-2 1 13 0.072
1 0 -12 0.081
11 10 -5 0.063
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 85.36(15) . 2_565
N1 Ti1 Cl1 104.77(11) . .
N1 Ti1 Cl1 104.09(10) 2_565 .
N1 Ti1 C9 117.27(14) . .
N1 Ti1 C9 90.85(15) 2_565 .
Cl1 Ti1 C9 136.40(11) . .
N1 Ti1 C8 91.68(14) . .
N1 Ti1 C8 114.09(15) 2_565 .
Cl1 Ti1 C8 139.49(11) . .
C9 Ti1 C8 35.36(15) . .
N1 Ti1 C10 149.67(13) . .
N1 Ti1 C10 103.18(15) 2_565 .
Cl1 Ti1 C10 101.27(12) . .
C9 Ti1 C10 35.13(14) . .
C8 Ti1 C10 58.17(14) . .
N1 Ti1 C7 100.19(15) . .
N1 Ti1 C7 147.56(14) 2_565 .
Cl1 Ti1 C7 105.24(11) . .
C9 Ti1 C7 58.05(15) . .
C8 Ti1 C7 34.56(14) . .
C10 Ti1 C7 57.54(15) . .
N1 Ti1 C11 133.07(14) . .
N1 Ti1 C11 137.31(15) 2_565 .
Cl1 Ti1 C11 85.39(11) . .
C9 Ti1 C11 57.99(15) . .
C8 Ti1 C11 57.55(14) . .
C10 Ti1 C11 34.60(15) . .
C7 Ti1 C11 34.31(13) . .
N1 Ti1 Ti1 42.73(10) . 2_565
N1 Ti1 Ti1 42.63(10) 2_565 2_565
Cl1 Ti1 Ti1 109.81(7) . 2_565
C9 Ti1 Ti1 108.74(12) . 2_565
C8 Ti1 Ti1 107.32(11) . 2_565
C10 Ti1 Ti1 137.88(12) . 2_565
C7 Ti1 Ti1 134.01(11) . 2_565
C11 Ti1 Ti1 164.67(10) . 2_565
C1 N1 Ti1 131.4(3) . .
C1 N1 Ti1 134.0(3) . 2_565
Ti1 N1 Ti1 94.64(15) . 2_565
C6 C1 C2 118.8(4) . .
C6 C1 N1 120.7(3) . .
C2 C1 N1 120.5(4) . .
C3 C2 C1 120.2(4) . .
C4 C3 C2 119.9(4) . .
C3 C4 C5 120.5(4) . .
C3 C4 C12 119.9(4) . .
C5 C4 C12 119.6(4) . .
C6 C5 C4 120.0(4) . .
C5 C6 C1 120.6(4) . .
C8 C7 C11 108.4(4) . .
C8 C7 C14 126.9(4) . .
C11 C7 C14 124.6(4) . .
C8 C7 Ti1 71.1(2) . .
C11 C7 Ti1 73.5(2) . .
C14 C7 Ti1 125.1(3) . .
C7 C8 C9 108.2(3) . .
C7 C8 C15 126.4(4) . .
C9 C8 C15 125.2(4) . .
C7 C8 Ti1 74.3(2) . .
C9 C8 Ti1 71.9(2) . .
C15 C8 Ti1 122.8(3) . .
C10 C9 C8 107.4(4) . .
C10 C9 C16 127.0(4) . .
C8 C9 C16 125.3(4) . .
C10 C9 Ti1 73.3(2) . .
C8 C9 Ti1 72.8(2) . .
C16 C9 Ti1 124.6(3) . .
C9 C10 C11 108.4(3) . .
C9 C10 C17 126.2(4) . .
C11 C10 C17 125.5(4) . .
C9 C10 Ti1 71.5(2) . .
C11 C10 Ti1 74.5(2) . .
C17 C10 Ti1 120.7(3) . .
C7 C11 C10 107.7(3) . .
C7 C11 C13 125.9(4) . .
C10 C11 C13 126.3(4) . .
C7 C11 Ti1 72.2(2) . .
C10 C11 Ti1 70.9(2) . .
C13 C11 Ti1 126.4(3) . .
N2 C12 C4 178.8(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 N1 1.926(4) .
Ti1 N1 1.930(3) 2_565
Ti1 Cl1 2.2976(18) .
Ti1 C9 2.337(4) .
Ti1 C8 2.348(4) .
Ti1 C10 2.360(4) .
Ti1 C7 2.390(4) .
Ti1 C11 2.406(4) .
Ti1 Ti1 2.834(3) 2_565
N1 C1 1.407(5) .
N1 Ti1 1.930(3) 2_565
N2 C12 1.135(6) .
C1 C6 1.396(6) .
C1 C2 1.401(5) .
C2 C3 1.388(6) .
C3 C4 1.380(6) .
C4 C5 1.386(6) .
C4 C12 1.447(6) .
C5 C6 1.378(6) .
C7 C8 1.408(6) .
C7 C11 1.414(6) .
C7 C14 1.507(6) .
C8 C9 1.423(6) .
C8 C15 1.495(5) .
C9 C10 1.418(6) .
C9 C16 1.492(6) .
C10 C11 1.418(6) .
C10 C17 1.501(6) .
C11 C13 1.495(6) .
