#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:42:56 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179932 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/27/7022741.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_7022741
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         'C36 H46 Cl4 N2 O1 Ti2'
_chemical_formula_sum            'C36 H46 Cl4 N2 O Ti2'
_chemical_formula_weight         760.35
_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             2013-02-04T10:51:51-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                109.91(5)
_cell_angle_beta                 95.03(8)
_cell_angle_gamma                111.48(3)
_cell_formula_units_Z            1
_cell_length_a                   8.9380(10)
_cell_length_b                   9.957(2)
_cell_length_c                   11.851(9)
_cell_measurement_reflns_used    236
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      16.56
_cell_measurement_theta_min      3.43
_cell_measurement_wavelength     0.71073
_cell_volume                     895.2(9)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.1086
_diffrn_reflns_av_unetI/netI     0.0604
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17925
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.04
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.776
_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             396
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         4082
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0539
_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)+(0.0480P)²+2.1943P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.135
_refine_ls_wR_factor_ref         0.1506
_reflns_number_gt                3295
_reflns_number_total             4082
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c3dt32943g.txt
_cod_data_source_block           2b
_cod_original_cell_volume        895.1(7)
_cod_database_code               7022741
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 0.04096(6) 0.11638(6) 0.45083(5) 0.01699(16) Uani 1 1 d .
Cl1 Cl -0.18170(10) 0.17267(10) 0.41685(9) 0.0316(2) Uani 1 1 d .
Cl2 Cl -0.30420(14) -0.61418(13) -0.11366(9) 0.0493(3) Uani 1 1 d .
N1 N -0.0528(3) -0.1084(3) 0.3899(2) 0.0181(5) Uani 1 1 d .
C1 C -0.1121(4) -0.2280(4) 0.2687(3) 0.0257(7) Uani 1 1 d .
C2 C -0.2228(5) -0.2286(4) 0.1791(3) 0.0326(8) Uani 1 1 d .
H2 H -0.2582 -0.1483 0.1983 0.039 Uiso 1 1 calc R
C3 C -0.2816(5) -0.3475(5) 0.0611(4) 0.0364(8) Uani 1 1 d .
H3 H -0.3565 -0.3476 0.0014 0.044 Uiso 1 1 calc R
C4 C -0.2285(5) -0.4647(5) 0.0333(3) 0.0360(8) Uani 1 1 d .
C5 C -0.1189(5) -0.4677(4) 0.1191(3) 0.0325(8) Uani 1 1 d .
H5 H -0.0843 -0.5486 0.0984 0.039 Uiso 1 1 calc R
C6 C -0.0597(4) -0.3495(4) 0.2371(3) 0.0307(7) Uani 1 1 d .
H6 H 0.0154 -0.3508 0.2958 0.037 Uiso 1 1 calc R
C7 C 0.3301(4) 0.2358(4) 0.4876(3) 0.0234(6) Uani 1 1 d .
C8 C 0.2677(4) 0.1200(4) 0.3646(3) 0.0236(6) Uani 1 1 d .
C9 C 0.1766(4) 0.1694(4) 0.2966(3) 0.0243(7) Uani 1 1 d .
C10 C 0.1835(4) 0.3147(4) 0.3769(3) 0.0248(7) Uani 1 1 d .
C11 C 0.2795(4) 0.3563(4) 0.4949(3) 0.0248(7) Uani 1 1 d .
C12 C 0.4450(4) 0.2368(5) 0.5882(4) 0.0365(9) Uani 1 1 d .
H12A H 0.4589 0.1406 0.5594 0.055 Uiso 1 1 calc R
H12B H 0.3991 0.2456 0.6592 0.055 Uiso 1 1 calc R
H12C H 0.5506 0.3248 0.6104 0.055 Uiso 1 1 calc R
C13 C 0.3061(5) -0.0201(5) 0.3168(4) 0.0375(9) Uani 1 1 d .
H13A H 0.3698 -0.0246 0.3838 0.056 Uiso 1 1 calc R
H13B H 0.3685 -0.0114 0.2557 0.056 Uiso 1 1 calc R
H13C H 0.2046 -0.1142 0.2801 0.056 Uiso 1 1 calc R
C14 C 0.0922(5) 0.0880(5) 0.1617(3) 0.0402(9) Uani 1 1 d .
H14A H 0.1043 -0.0086 0.1266 0.06 Uiso 1 1 calc R
H14B H 0.1416 0.1551 0.1206 0.06 Uiso 1 1 calc R
H14C H -0.0234 0.0653 0.1514 0.06 Uiso 1 1 calc R
C15 C 0.1121(5) 0.4117(5) 0.3392(4) 0.0383(9) Uani 1 1 d .
H15B H 0.1323 0.505 0.4102 0.057 Uiso 1 1 calc R
H15C H -0.0052 0.3514 0.3051 0.057 Uiso 1 1 calc R
H15A H 0.1633 0.441 0.2782 0.057 Uiso 1 1 calc R
C16 C 0.3272(5) 0.5064(4) 0.6055(4) 0.0391(9) Uani 1 1 d .
H16A H 0.2762 0.5681 0.5859 0.059 Uiso 1 1 calc R
H16B H 0.4455 0.5649 0.6286 0.059 Uiso 1 1 calc R
H16C H 0.2904 0.4827 0.673 0.059 Uiso 1 1 calc R
O1 O 0.6116(12) -0.0677(12) 0.0185(10) 0.084(3) Uani 0.5 1 d P
C22 C 0.6328(9) 0.0707(11) 0.0642(8) 0.098(2) Uani 1 1 d .
H22A H 0.7098 0.1248 0.0247 0.117 Uiso 1 1 calc R
H22B H 0.691 0.1121 0.1501 0.117 Uiso 1 1 calc R
C23 C 0.5054(11) 0.1225(10) 0.0647(9) 0.097(2) Uani 1 1 d .
H23A H 0.4625 0.1149 0.1358 0.116 Uiso 1 1 calc R
H23B H 0.5592 0.234 0.0823 0.116 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'
O O 0.0106 0.006 '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
6 -2 3 0.218
-1 -5 6 0.098
1 9 -11 0.133
-17 -1 0 0.265
0 4 -5 0.156
-1 -7 8 0.107
1 -2 3 1.066
14 -5 13 0.208
-3 0 -2 0.324
1 13 -14 0.142
-1 -1 5 0.1
2 1 -8 0.209
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 84.44(13) . 2_556
N1 Ti1 Cl1 104.25(9) . .
N1 Ti1 Cl1 104.98(11) 2_556 .
N1 Ti1 C7 114.27(12) . .
N1 Ti1 C7 91.95(14) 2_556 .
Cl1 Ti1 C7 139.23(9) . .
N1 Ti1 C8 91.11(12) . .
N1 Ti1 C8 117.04(13) 2_556 .
Cl1 Ti1 C8 136.47(9) . .
C7 Ti1 C8 35.22(12) . .
N1 Ti1 C9 103.27(12) . .
N1 Ti1 C9 149.51(12) 2_556 .
Cl1 Ti1 C9 101.62(10) . .
C7 Ti1 C9 57.85(13) . .
C8 Ti1 C9 34.85(12) . .
N1 Ti1 C11 147.64(11) . .
N1 Ti1 C11 101.18(14) 2_556 .
Cl1 Ti1 C11 104.92(9) . .
C7 Ti1 C11 34.56(12) . .
C8 Ti1 C11 57.76(12) . .
C9 Ti1 C11 57.11(13) . .
N1 Ti1 C10 136.98(12) . .
N1 Ti1 C10 134.12(13) 2_556 .
Cl1 Ti1 C10 85.53(9) . .
C7 Ti1 C10 57.37(12) . .
C8 Ti1 C10 57.53(12) . .
C9 Ti1 C10 34.22(12) . .
C11 Ti1 C10 34.16(12) . .
N1 Ti1 Ti1 42.23(9) . 2_556
N1 Ti1 Ti1 42.21(9) 2_556 2_556
Cl1 Ti1 Ti1 109.92(5) . 2_556
C7 Ti1 Ti1 107.48(10) . 2_556
C8 Ti1 Ti1 108.67(9) . 2_556
C9 Ti1 Ti1 137.46(9) . 2_556
C11 Ti1 Ti1 134.52(10) . 2_556
C10 Ti1 Ti1 164.50(8) . 2_556
C1 N1 Ti1 132.3(2) . .
C1 N1 Ti1 132.1(2) . 2_556
Ti1 N1 Ti1 95.56(13) . 2_556
C2 C1 C6 118.5(3) . .
C2 C1 N1 121.2(3) . .
C6 C1 N1 120.3(3) . .
C1 C2 C3 120.7(3) . .
C4 C3 C2 119.3(4) . .
C5 C4 C3 121.6(4) . .
C5 C4 Cl2 119.3(3) . .
C3 C4 Cl2 119.1(3) . .
C4 C5 C6 119.5(4) . .
C5 C6 C1 120.4(3) . .
C11 C7 C8 108.3(3) . .
C11 C7 C12 126.2(3) . .
C8 C7 C12 125.2(3) . .
C11 C7 Ti1 74.93(18) . .
C8 C7 Ti1 72.4(2) . .
C12 C7 Ti1 123.5(2) . .
C9 C8 C7 107.5(3) . .
C9 C8 C13 127.6(3) . .
C7 C8 C13 124.7(3) . .
C9 C8 Ti1 74.05(18) . .
C7 C8 Ti1 72.35(19) . .
C13 C8 Ti1 123.0(2) . .
C10 C9 C8 108.2(3) . .
C10 C9 C14 124.7(3) . .
C8 C9 C14 127.0(3) . .
C10 C9 Ti1 74.15(19) . .
C8 C9 Ti1 71.09(18) . .
C14 C9 Ti1 122.6(2) . .
C9 C10 C11 108.0(3) . .
C9 C10 C15 125.1(3) . .
C11 C10 C15 126.8(3) . .
C9 C10 Ti1 71.63(18) . .
C11 C10 Ti1 72.34(19) . .
C15 C10 Ti1 125.3(2) . .
C7 C11 C10 108.0(3) . .
C7 C11 C16 126.2(3) . .
C10 C11 C16 125.8(3) . .
C7 C11 Ti1 70.51(17) . .
C10 C11 Ti1 73.5(2) . .
C16 C11 Ti1 124.4(2) . .
C23 O1 C22 101.4(9) 2_655 .
O1 C22 C23 124.9(8) . .
O1 C22 C23 38.4(5) . 2_655
C23 C22 C23 90.9(6) . 2_655
O1 C23 C22 124.7(9) 2_655 .
O1 C23 C22 40.2(6) 2_655 2_655
C22 C23 C22 89.1(6) . 2_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 N1 1.911(3) .
Ti1 N1 1.911(3) 2_556
Ti1 Cl1 2.2949(11) .
Ti1 C7 2.341(3) .
Ti1 C8 2.342(3) .
Ti1 C9 2.380(4) .
Ti1 C11 2.398(3) .
Ti1 C10 2.413(3) .
Ti1 Ti1 2.8306(16) 2_556
Cl2 C4 1.731(4) .
N1 C1 1.415(4) .
N1 Ti1 1.911(3) 2_556
C1 C2 1.384(5) .
C1 C6 1.400(5) .
C2 C3 1.386(5) .
C3 C4 1.367(6) .
C4 C5 1.364(6) .
C5 C6 1.383(5) .
C7 C11 1.409(5) .
C7 C8 1.417(5) .
C7 C12 1.498(5) .
C8 C9 1.415(5) .
C8 C13 1.494(5) .
C9 C10 1.411(5) .
C9 C14 1.497(5) .
C10 C11 1.413(5) .
C10 C15 1.495(5) .
C11 C16 1.495(5) .
O1 C23 1.183(11) 2_655
O1 C22 1.230(11) .
C22 C23 1.410(10) .
C22 C23 1.867(12) 2_655
C23 O1 1.183(11) 2_655
C23 C22 1.867(12) 2_655
