#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:42:56 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179932 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/27/7022744.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_7022744
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         'C44 H64 Cl2 N2 O6 Ti2'
_chemical_formula_sum            'C44 H64 Cl2 N2 O6 Ti2'
_chemical_formula_weight         883.61
_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             2012-11-21T11:20:10-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                114.228(14)
_cell_angle_beta                 105.391(16)
_cell_angle_gamma                98.180(13)
_cell_formula_units_Z            1
_cell_length_a                   10.332(2)
_cell_length_b                   10.4820(17)
_cell_length_c                   12.136(3)
_cell_measurement_reflns_used    256
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      16.37
_cell_measurement_theta_min      3.36
_cell_measurement_wavelength     0.71073
_cell_volume                     1107.4(5)
_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    'SIR2004 (Giacovazzo et al, 2004)'
_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  0.1058
_diffrn_reflns_av_unetI/netI     0.0595
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            23235
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.09
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.529
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         5078
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_gt           0.0549
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0462P)²+1.6897P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1349
_refine_ls_wR_factor_ref         0.1521
_reflns_number_gt                3929
_reflns_number_total             5078
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c3dt32943g.txt
_cod_data_source_block           2e
_cod_original_cell_volume        1107.4(4)
_cod_database_code               7022744
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 0.11333(5) 0.12415(5) 0.09465(5) 0.02166(15) Uani 1 1 d .
Cl1 Cl 0.13085(10) 0.15846(10) 0.29900(8) 0.0435(2) Uani 1 1 d .
N1 N -0.0845(2) 0.0823(3) 0.0049(2) 0.0248(5) Uani 1 1 d .
O1 O -0.4309(2) 0.2422(3) -0.2075(2) 0.0409(6) Uani 1 1 d .
O2 O -0.2505(3) 0.4777(3) 0.2524(2) 0.0446(6) Uani 1 1 d .
O3 O 0.7815(6) 0.2397(5) 0.4972(6) 0.1140(17) Uani 1 1 d .
C1 C -0.1710(3) 0.1750(3) 0.0118(3) 0.0240(6) Uani 1 1 d .
C2 C -0.2614(3) 0.1658(3) -0.1000(3) 0.0269(6) Uani 1 1 d .
H2 H -0.2661 0.097 -0.1806 0.032 Uiso 1 1 calc R
C3 C -0.3456(3) 0.2604(3) -0.0915(3) 0.0294(6) Uani 1 1 d .
C4 C -0.3390(3) 0.3634(3) 0.0278(3) 0.0341(7) Uani 1 1 d .
H4 H -0.3945 0.4266 0.0332 0.041 Uiso 1 1 calc R
C5 C -0.2485(3) 0.3715(3) 0.1395(3) 0.0319(7) Uani 1 1 d .
C6 C -0.1650(3) 0.2781(3) 0.1340(3) 0.0284(6) Uani 1 1 d .
H6 H -0.1062 0.2833 0.2095 0.034 Uiso 1 1 calc R
C7 C 0.1948(3) 0.3627(3) 0.1167(3) 0.0305(6) Uani 1 1 d .
C8 C 0.3009(3) 0.3473(4) 0.2066(3) 0.0397(8) Uani 1 1 d .
C9 C 0.3507(3) 0.2318(4) 0.1366(4) 0.0422(8) Uani 1 1 d .
C10 C 0.2749(3) 0.1751(4) 0.0037(4) 0.0367(7) Uani 1 1 d .
C11 C 0.1774(3) 0.2566(3) -0.0092(3) 0.0290(6) Uani 1 1 d .
C12 C 0.1213(4) 0.4784(4) 0.1468(4) 0.0469(9) Uani 1 1 d .
H12A H 0.0537 0.4642 0.068 0.07 Uiso 1 1 calc R
H12B H 0.1884 0.5726 0.1877 0.07 Uiso 1 1 calc R
H12C H 0.0745 0.4729 0.204 0.07 Uiso 1 1 calc R
C13 C 0.3592(5) 0.4443(5) 0.3508(4) 0.0711(15) Uani 1 1 d .
H13A H 0.4303 0.4105 0.3903 0.107 Uiso 1 1 calc R
H13B H 0.2853 0.4417 0.3847 0.107 Uiso 1 1 calc R
H13C H 0.3991 0.5426 0.3694 0.107 Uiso 1 1 calc R
C14 C 0.4670(4) 0.1824(6) 0.1958(6) 0.0806(18) Uani 1 1 d .
H14A H 0.5004 0.2388 0.2884 0.121 Uiso 1 1 calc R
H14B H 0.5423 0.1959 0.1656 0.121 Uiso 1 1 calc R
H14C H 0.4328 0.081 0.1714 0.121 Uiso 1 1 calc R
C15 C 0.2995(6) 0.0596(4) -0.1049(5) 0.0689(15) Uani 1 1 d .
H15A H 0.2335 0.0416 -0.1859 0.103 Uiso 1 1 calc R
H15B H 0.2878 -0.0286 -0.0973 0.103 Uiso 1 1 calc R
H15C H 0.393 0.0914 -0.1015 0.103 Uiso 1 1 calc R
C16 C 0.0838(4) 0.2409(4) -0.1340(3) 0.0447(8) Uani 1 1 d .
H16A H 0.0919 0.1604 -0.2049 0.067 Uiso 1 1 calc R
H16B H 0.1108 0.329 -0.1395 0.067 Uiso 1 1 calc R
H16C H -0.0114 0.2233 -0.1378 0.067 Uiso 1 1 calc R
C18 C -0.5175(4) 0.3381(4) -0.2047(4) 0.0454(9) Uani 1 1 d .
H18A H -0.572 0.3142 -0.2917 0.068 Uiso 1 1 calc R
H18B H -0.4594 0.4372 -0.1604 0.068 Uiso 1 1 calc R
H18C H -0.5789 0.3271 -0.1601 0.068 Uiso 1 1 calc R
C19 C -0.1622(5) 0.4893(4) 0.3707(4) 0.0523(10) Uani 1 1 d .
H19A H -0.1724 0.5668 0.4425 0.078 Uiso 1 1 calc R
H19B H -0.0665 0.5099 0.3763 0.078 Uiso 1 1 calc R
H19C H -0.1884 0.399 0.3729 0.078 Uiso 1 1 calc R
C20 C 0.8841(7) 0.1658(6) 0.4992(6) 0.0831(16) Uani 1 1 d .
H20A H 0.9613 0.2193 0.5816 0.1 Uiso 1 1 calc R
H20B H 0.92 0.1572 0.4311 0.1 Uiso 1 1 calc R
C21 C 0.8203(6) 0.0206(6) 0.4798(6) 0.0785(15) Uani 1 1 d .
H21A H 0.8829 -0.0057 0.5366 0.094 Uiso 1 1 calc R
H21B H 0.796 -0.0528 0.3908 0.094 Uiso 1 1 calc R
C22 C 0.6922(6) 0.0367(7) 0.5129(7) 0.0894(18) Uani 1 1 d .
H22A H 0.6127 -0.0476 0.451 0.107 Uiso 1 1 calc R
H22B H 0.7071 0.0467 0.5988 0.107 Uiso 1 1 calc R
C23 C 0.6693(9) 0.1622(8) 0.5082(11) 0.134(3) Uani 1 1 d .
H23A H 0.5853 0.1354 0.4348 0.161 Uiso 1 1 calc R
H23B H 0.6544 0.2239 0.5862 0.161 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
3 -1 -7 0.177
-6 11 -7 0.146
0 -1 2 0.136
3 -5 2 0.161
14 -1 -9 0.112
1 3 -3 0.177
-3 1 1 0.157
-4 -9 10 0.09
-11 1 -1 0.091
1 0 3 0.226
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 85.38(10) 2 .
N1 Ti1 Cl1 104.62(8) 2 .
N1 Ti1 Cl1 104.42(8) . .
N1 Ti1 C10 90.66(11) 2 .
N1 Ti1 C10 119.95(12) . .
Cl1 Ti1 C10 134.15(10) . .
N1 Ti1 C11 112.43(11) 2 .
N1 Ti1 C11 93.05(10) . .
Cl1 Ti1 C11 140.10(8) . .
C10 Ti1 C11 35.33(11) . .
N1 Ti1 C9 104.55(12) 2 .
N1 Ti1 C9 150.85(11) . .
Cl1 Ti1 C9 99.51(10) . .
C10 Ti1 C9 34.69(13) . .
C11 Ti1 C9 57.80(11) . .
N1 Ti1 C7 146.40(10) 2 .
N1 Ti1 C7 99.60(10) . .
Cl1 Ti1 C7 106.17(8) . .
C10 Ti1 C7 57.93(11) . .
C11 Ti1 C7 34.61(11) . .
C9 Ti1 C7 57.26(11) . .
N1 Ti1 C8 138.92(12) 2 .
N1 Ti1 C8 131.54(11) . .
Cl1 Ti1 C8 85.03(9) . .
C10 Ti1 C8 57.72(13) . .
C11 Ti1 C8 57.35(11) . .
C9 Ti1 C8 34.59(13) . .
C7 Ti1 C8 34.04(11) . .
N1 Ti1 Ti1 42.74(7) 2 2
N1 Ti1 Ti1 42.64(7) . 2
Cl1 Ti1 Ti1 109.94(4) . 2
C10 Ti1 Ti1 110.35(9) . 2
C11 Ti1 Ti1 107.19(8) . 2
C9 Ti1 Ti1 139.94(11) . 2
C7 Ti1 Ti1 132.81(8) . 2
C8 Ti1 Ti1 164.54(9) . 2
C1 N1 Ti1 134.49(19) . 2
C1 N1 Ti1 130.88(19) . .
Ti1 N1 Ti1 94.62(10) 2 .
C3 O1 C18 117.6(3) . .
C5 O2 C19 117.1(3) . .
C23 O3 C20 107.4(5) . .
C2 C1 N1 120.5(3) . .
C2 C1 C6 120.1(3) . .
N1 C1 C6 119.3(3) . .
C1 C2 C3 119.9(3) . .
O1 C3 C4 124.3(3) . .
O1 C3 C2 115.2(3) . .
C4 C3 C2 120.5(3) . .
C3 C4 C5 119.3(3) . .
O2 C5 C6 124.2(3) . .
O2 C5 C4 114.3(3) . .
C6 C5 C4 121.4(3) . .
C5 C6 C1 118.7(3) . .
C8 C7 C11 108.2(3) . .
C8 C7 C12 126.3(3) . .
C11 C7 C12 125.3(3) . .
C8 C7 Ti1 73.08(17) . .
C11 C7 Ti1 71.14(16) . .
C12 C7 Ti1 125.5(2) . .
C7 C8 C9 108.0(3) . .
C7 C8 C13 125.8(4) . .
C9 C8 C13 126.0(4) . .
C7 C8 Ti1 72.88(17) . .
C9 C8 Ti1 71.50(18) . .
C13 C8 Ti1 125.1(3) . .
C10 C9 C8 108.4(3) . .
C10 C9 C14 126.4(4) . .
C8 C9 C14 125.2(4) . .
C10 C9 Ti1 71.60(17) . .
C8 C9 Ti1 73.90(18) . .
C14 C9 Ti1 121.5(2) . .
C9 C10 C11 107.6(3) . .
C9 C10 C15 126.4(4) . .
C11 C10 C15 125.8(4) . .
C9 C10 Ti1 73.71(19) . .
C11 C10 Ti1 72.93(16) . .
C15 C10 Ti1 122.9(2) . .
C7 C11 C10 107.8(3) . .
C7 C11 C16 126.4(3) . .
C10 C11 C16 125.6(3) . .
C7 C11 Ti1 74.25(17) . .
C10 C11 Ti1 71.75(17) . .
C16 C11 Ti1 123.9(2) . .
O3 C20 C21 108.3(5) . .
C20 C21 C22 103.4(5) . .
C23 C22 C21 105.5(5) . .
O3 C23 C22 111.7(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 N1 1.927(2) 2
Ti1 N1 1.930(2) .
Ti1 Cl1 2.3074(11) .
Ti1 C10 2.345(3) .
Ti1 C11 2.360(3) .
Ti1 C9 2.372(3) .
Ti1 C7 2.401(3) .
Ti1 C8 2.403(3) .
Ti1 Ti1 2.8351(13) 2
N1 C1 1.404(3) .
N1 Ti1 1.927(2) 2
O1 C3 1.367(4) .
O1 C18 1.434(4) .
O2 C5 1.373(4) .
O2 C19 1.427(5) .
O3 C23 1.388(7) .
O3 C20 1.399(7) .
C1 C2 1.384(4) .
C1 C6 1.410(4) .
C2 C3 1.399(4) .
C3 C4 1.383(4) .
C4 C5 1.389(5) .
C5 C6 1.387(4) .
C7 C8 1.406(5) .
C7 C11 1.417(4) .
C7 C12 1.492(4) .
C8 C9 1.420(5) .
C8 C13 1.505(5) .
C9 C10 1.406(5) .
C9 C14 1.501(5) .
C10 C11 1.428(4) .
C10 C15 1.491(5) .
C11 C16 1.493(5) .
C20 C21 1.464(7) .
C21 C22 1.494(7) .
C22 C23 1.390(8) .
