#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:42:56 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179932 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/27/7022743.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_7022743
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         'C17 H22 Cl1 N1 O1 Ti1'
_chemical_formula_sum            'C17 H22 Cl N O Ti'
_chemical_formula_weight         339.71
_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             2013-02-04
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                92.84(3)
_cell_angle_beta                 106.69(3)
_cell_angle_gamma                108.02(2)
_cell_formula_units_Z            2
_cell_length_a                   8.646(3)
_cell_length_b                   9.982(3)
_cell_length_c                   10.590(3)
_cell_measurement_reflns_used    234
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      17.32
_cell_measurement_theta_min      3.23
_cell_measurement_wavelength     0.71073
_cell_volume                     822.9(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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.1365
_diffrn_reflns_av_unetI/netI     0.0698
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16721
_diffrn_reflns_theta_full        26.5
_diffrn_reflns_theta_max         26.5
_diffrn_reflns_theta_min         3.19
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.68
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.691
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3408
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0461P)²+1.2891P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1355
_refine_ls_wR_factor_ref         0.15
_reflns_number_gt                2823
_reflns_number_total             3408
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c3dt32943g.txt
_cod_data_source_block           2d
_cod_original_cell_volume        822.9(4)
_cod_database_code               7022743
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 0.47176(7) 0.11050(5) 0.92840(5) 0.02209(18) Uani 1 1 d .
Cl1 Cl 0.31981(12) 0.21986(9) 1.01688(9) 0.0377(2) Uani 1 1 d .
N1 N 0.3557(3) -0.0923(3) 0.9202(2) 0.0242(5) Uani 1 1 d .
O1 O -0.2874(3) -0.4487(3) 0.5921(3) 0.0419(6) Uani 1 1 d .
C1 C 0.1967(4) -0.1832(3) 0.8355(3) 0.0253(6) Uani 1 1 d .
C2 C 0.0486(4) -0.1452(3) 0.8125(3) 0.0305(7) Uani 1 1 d .
H2 H 0.0568 -0.0571 0.8524 0.037 Uiso 1 1 calc R
C3 C -0.1087(4) -0.2364(4) 0.7316(3) 0.0334(7) Uani 1 1 d .
H3 H -0.2054 -0.2098 0.7193 0.04 Uiso 1 1 calc R
C4 C -0.1247(4) -0.3669(3) 0.6684(3) 0.0306(7) Uani 1 1 d .
C5 C 0.0205(4) -0.4065(4) 0.6878(3) 0.0315(7) Uani 1 1 d .
H5 H 0.0121 -0.4936 0.6454 0.038 Uiso 1 1 calc R
C6 C 0.1779(4) -0.3147(3) 0.7710(3) 0.0298(7) Uani 1 1 d .
H6 H 0.2741 -0.3422 0.784 0.036 Uiso 1 1 calc R
C7 C 0.5122(4) 0.0707(3) 0.7218(3) 0.0301(7) Uani 1 1 d .
C8 C 0.3856(4) 0.1361(4) 0.6978(3) 0.0332(7) Uani 1 1 d .
C9 C 0.4620(5) 0.2762(4) 0.7712(3) 0.0329(7) Uani 1 1 d .
C10 C 0.6357(4) 0.2966(3) 0.8402(3) 0.0314(7) Uani 1 1 d .
C11 C 0.6672(4) 0.1700(4) 0.8090(3) 0.0324(7) Uani 1 1 d .
C12 C 0.4914(6) -0.0748(4) 0.6594(4) 0.0475(10) Uani 1 1 d .
H12A H 0.5972 -0.0933 0.693 0.071 Uiso 1 1 calc R
H12B H 0.4615 -0.079 0.5643 0.071 Uiso 1 1 calc R
H12C H 0.4021 -0.1451 0.6809 0.071 Uiso 1 1 calc R
C13 C 0.2043(5) 0.0741(5) 0.6052(4) 0.0512(10) Uani 1 1 d .
H13A H 0.1459 0.1413 0.6079 0.077 Uiso 1 1 calc R
H13B H 0.146 -0.0122 0.6326 0.077 Uiso 1 1 calc R
H13C H 0.2053 0.0537 0.516 0.077 Uiso 1 1 calc R
C14 C 0.3791(6) 0.3880(5) 0.7667(5) 0.0526(11) Uani 1 1 d .
H14A H 0.2604 0.3478 0.7134 0.079 Uiso 1 1 calc R
H14B H 0.4362 0.4657 0.7282 0.079 Uiso 1 1 calc R
H14C H 0.3873 0.4222 0.8556 0.079 Uiso 1 1 calc R
C15 C 0.7638(6) 0.4320(4) 0.9257(4) 0.0516(11) Uani 1 1 d .
H15A H 0.8728 0.4194 0.9616 0.077 Uiso 1 1 calc R
H15B H 0.7251 0.4557 0.9975 0.077 Uiso 1 1 calc R
H15C H 0.7753 0.5077 0.8728 0.077 Uiso 1 1 calc R
C16 C 0.8386(5) 0.1495(5) 0.8495(4) 0.0500(10) Uani 1 1 d .
H16A H 0.825 0.054 0.8158 0.075 Uiso 1 1 calc R
H16B H 0.8854 0.1653 0.945 0.075 Uiso 1 1 calc R
H16C H 0.915 0.216 0.8134 0.075 Uiso 1 1 calc R
C17 C -0.3144(5) -0.5897(4) 0.5366(4) 0.0425(9) Uani 1 1 d .
H17A H -0.4332 -0.6352 0.4855 0.064 Uiso 1 1 calc R
H17B H -0.283 -0.6427 0.607 0.064 Uiso 1 1 calc R
H17C H -0.2451 -0.5866 0.4796 0.064 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
-5 4 13 0.216
1 3 2 0.161
2 -1 -5 0.144
-4 -3 3 0.13
0 1 0 0.092
0 -1 0 0.15
1 -12 1 0.165
-6 10 9 0.161
0 3 -1 0.164
-2 -3 6 0.202
16 -3 2 0.15
-14 2 1 0.163
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 85.85(12) 2_657 .
N1 Ti1 Cl1 104.62(8) 2_657 .
N1 Ti1 Cl1 104.49(8) . .
N1 Ti1 C11 91.12(12) 2_657 .
N1 Ti1 C11 115.92(12) . .
Cl1 Ti1 C11 137.58(9) . .
N1 Ti1 C7 115.38(12) 2_657 .
N1 Ti1 C7 91.31(11) . .
Cl1 Ti1 C7 137.92(9) . .
C11 Ti1 C7 35.18(12) . .
N1 Ti1 C10 101.51(12) 2_657 .
N1 Ti1 C10 148.93(11) . .
Cl1 Ti1 C10 102.73(9) . .
C11 Ti1 C10 34.92(12) . .
C7 Ti1 C10 58.13(12) . .
N1 Ti1 C8 148.25(12) 2_657 .
N1 Ti1 C8 101.31(12) . .
Cl1 Ti1 C8 103.40(9) . .
C11 Ti1 C8 57.79(12) . .
C7 Ti1 C8 34.62(12) . .
C10 Ti1 C8 57.55(12) . .
N1 Ti1 C9 135.09(12) 2_657 .
N1 Ti1 C9 134.80(12) . .
Cl1 Ti1 C9 85.18(9) . .
C11 Ti1 C9 57.55(12) . .
C7 Ti1 C9 57.59(12) . .
C10 Ti1 C9 34.38(12) . .
C8 Ti1 C9 34.46(12) . .
N1 Ti1 Ti1 43.42(8) 2_657 2_657
N1 Ti1 Ti1 42.43(8) . 2_657
Cl1 Ti1 Ti1 110.07(4) . 2_657
C11 Ti1 Ti1 108.33(9) . 2_657
C7 Ti1 Ti1 107.80(9) . 2_657
C10 Ti1 Ti1 136.49(9) . 2_657
C8 Ti1 Ti1 135.27(9) . 2_657
C9 Ti1 Ti1 164.73(9) . 2_657
C1 N1 Ti1 135.3(2) . 2_657
C1 N1 Ti1 130.4(2) . .
Ti1 N1 Ti1 94.15(12) 2_657 .
C4 O1 C17 117.9(3) . .
C6 C1 N1 121.7(3) . .
C6 C1 C2 117.1(3) . .
N1 C1 C2 121.2(3) . .
C3 C2 C1 121.1(3) . .
C2 C3 C4 120.9(3) . .
O1 C4 C3 115.6(3) . .
O1 C4 C5 125.1(3) . .
C3 C4 C5 119.3(3) . .
C6 C5 C4 119.3(3) . .
C5 C6 C1 122.3(3) . .
C8 C7 C11 108.0(3) . .
C8 C7 C12 126.4(3) . .
C11 C7 C12 125.4(3) . .
C8 C7 Ti1 74.44(18) . .
C11 C7 Ti1 72.28(18) . .
C12 C7 Ti1 122.2(2) . .
C7 C8 C9 107.9(3) . .
C7 C8 C13 126.8(3) . .
C9 C8 C13 125.2(4) . .
C7 C8 Ti1 70.94(18) . .
C9 C8 Ti1 73.36(19) . .
C13 C8 Ti1 124.1(2) . .
C10 C9 C8 108.0(3) . .
C10 C9 C14 125.4(4) . .
C8 C9 C14 126.3(4) . .
C10 C9 Ti1 71.53(18) . .
C8 C9 Ti1 72.17(18) . .
C14 C9 Ti1 126.3(2) . .
C9 C10 C11 107.9(3) . .
C9 C10 C15 125.2(3) . .
C11 C10 C15 126.9(3) . .
C9 C10 Ti1 74.09(19) . .
C11 C10 Ti1 71.34(18) . .
C15 C10 Ti1 122.5(2) . .
C10 C11 C7 108.1(3) . .
C10 C11 C16 126.0(4) . .
C7 C11 C16 125.7(3) . .
C10 C11 Ti1 73.73(18) . .
C7 C11 Ti1 72.54(18) . .
C16 C11 Ti1 124.3(2) . .
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) 2_657
Ti1 N1 1.947(3) .
Ti1 Cl1 2.2996(11) .
Ti1 C11 2.343(3) .
Ti1 C7 2.346(3) .
Ti1 C10 2.373(3) .
Ti1 C8 2.391(3) .
Ti1 C9 2.407(3) .
Ti1 Ti1 2.8244(14) 2_657
N1 C1 1.399(4) .
N1 Ti1 1.911(3) 2_657
O1 C4 1.367(4) .
O1 C17 1.421(4) .
C1 C6 1.390(4) .
C1 C2 1.405(4) .
C2 C3 1.378(5) .
C3 C4 1.383(5) .
C4 C5 1.394(5) .
C5 C6 1.388(5) .
C7 C8 1.410(5) .
C7 C11 1.417(5) .
C7 C12 1.501(5) .
C8 C9 1.421(5) .
C8 C13 1.502(5) .
C9 C10 1.413(5) .
C9 C14 1.498(5) .
C10 C11 1.415(5) .
C10 C15 1.500(5) .
C11 C16 1.501(5) .
