#------------------------------------------------------------------------------
#$Date: 2016-02-21 01:03:34 +0100 (dom 21 de feb de 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/89/2238911.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2238911
loop_
_publ_author_name
'Zaitsev, Kirill V.'
'Karlov, Sergey S.'
'Piskun, Yulia A.'
'Vasilenko, Irina V.'
'Churakov, Andrei V.'
_publ_section_title
;
 Di-μ-oxido-bis({2,2'-[ethane-1,2-diylbis(nitrilomethanylylidene)]diphenolato}titanium(IV))
 chloroform disolvate
;
_journal_coeditor_code           QK2062
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m635
_journal_page_last               m636
_journal_paper_doi               10.1107/S1600536813029656
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Ti2 (C16 H16 N2 O2)2 O2], 2C H Cl3'
_chemical_formula_moiety         'C32 H32 N4 O6 Ti2, 2(C H Cl3)'
_chemical_formula_sum            'C34 H34 Cl6 N4 O6 Ti2'
_chemical_formula_weight         903.15
_chemical_name_systematic
'Di-μ-oxido-bis({2,2'-[ethane-1,2-diylbis(nitrilomethanylylidene)]diphenolato}titanium(IV)) chloroform disolvate'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                117.075(4)
_cell_angle_beta                 93.113(4)
_cell_angle_gamma                110.463(4)
_cell_formula_units_Z            1
_cell_length_a                   10.237(3)
_cell_length_b                   10.356(3)
_cell_length_c                   10.936(3)
_cell_measurement_reflns_used    1919
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.730
_cell_measurement_theta_min      2.197
_cell_volume                     935.0(5)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0563
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_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            8213
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.906
_exptl_absorpt_correction_T_max  0.9910
_exptl_absorpt_correction_T_min  0.9310
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.430
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         3668
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0393P)²+0.3887P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0920
_reflns_number_gt                2761
_reflns_number_total             3668
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            qk2062.cif
_cod_data_source_block           I
_cod_original_cell_volume        935.0(4)
_cod_database_code               2238911
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Ti Ti1 0.50658(5) 0.65403(6) 0.05634(5) 0.01468(14) Uani d . 1 1
O O1 0.6684(2) 0.7828(2) 0.21655(19) 0.0185(4) Uani d . 1 1
O O2 0.3932(2) 0.7673(2) 0.13984(19) 0.0186(4) Uani d . 1 1
O O3 0.4197(2) 0.4842(2) 0.07711(19) 0.0179(4) Uani d . 1 1
N N1 0.6242(2) 0.8318(3) -0.0058(2) 0.0166(5) Uani d . 1 1
N N2 0.3580(3) 0.5823(3) -0.1413(3) 0.0198(5) Uani d . 1 1
H H2 0.374(3) 0.509(4) -0.198(3) 0.030 Uiso d . 1 1
C C11 0.7673(3) 0.9337(3) 0.2842(3) 0.0166(6) Uani d . 1 1
C C12 0.8403(3) 1.0016(3) 0.4247(3) 0.0217(6) Uani d . 1 1
H H12 0.8190 0.9395 0.4696 0.026 Uiso calc R 1 1
C C13 0.9432(3) 1.1579(4) 0.4998(3) 0.0285(7) Uani d . 1 1
H H13 0.9911 1.2026 0.5960 0.034 Uiso calc R 1 1
C C14 0.9772(3) 1.2501(4) 0.4359(3) 0.0328(8) Uani d . 1 1
H H14 1.0475 1.3578 0.4879 0.039 Uiso calc R 1 1
C C15 0.9077(3) 1.1837(4) 0.2962(3) 0.0274(7) Uani d . 1 1
H H15 0.9326 1.2463 0.2519 0.033 Uiso calc R 1 1
C C16 0.8012(3) 1.0262(3) 0.2176(3) 0.0191(6) Uani d . 1 1
C C17 0.7329(3) 0.9660(3) 0.0716(3) 0.0186(6) Uani d . 1 1
H H17 0.7713 1.0303 0.0308 0.022 Uiso calc R 1 1
C C18 0.5634(3) 0.7824(4) -0.1528(3) 0.0226(7) Uani d . 1 1
H H18A 0.5968 0.7047 -0.2195 0.027 Uiso calc R 1 1
H H18B 0.5944 0.8762 -0.1659 0.027 Uiso calc R 1 1
C C21 0.2627(3) 0.7615(3) 0.1055(3) 0.0190(6) Uani d . 1 1
C C22 0.2212(3) 0.8734(4) 0.2051(3) 0.0236(7) Uani d . 1 1
H H22 0.2850 0.9515 0.2964 0.028 Uiso calc R 1 1
C C23 0.0879(3) 0.8713(4) 0.1718(4) 0.0303(8) Uani d . 1 1
H H23 0.0617 0.9490 0.2401 0.036 Uiso calc R 1 1
C C24 -0.0073(3) 0.7581(4) 0.0410(4) 0.0323(8) Uani d . 1 1
H H24 -0.0991 0.7565 0.0192 0.039 Uiso calc R 1 1
C C25 0.0326(3) 0.6466(4) -0.0583(3) 0.0268(7) Uani d . 1 1
H H25 -0.0333 0.5679 -0.1484 0.032 Uiso calc R 1 1
C C26 0.1668(3) 0.6469(3) -0.0294(3) 0.0210(6) Uani d . 1 1
C C27 0.2045(3) 0.5213(3) -0.1398(3) 0.0243(7) Uani d . 1 1
H H27A 0.1818 0.4316 -0.1214 0.029 Uiso calc R 1 1
H H27B 0.1437 0.4789 -0.2346 0.029 Uiso calc R 1 1
C C28 0.4012(3) 0.7066(3) -0.1807(3) 0.0232(7) Uani d . 1 1
H H28A 0.3675 0.7892 -0.1244 0.028 Uiso calc R 1 1
H H28B 0.3562 0.6586 -0.2825 0.028 Uiso calc R 1 1
C C1 0.4183(3) 0.6758(4) 0.4095(3) 0.0325(8) Uani d . 1 1
H H1 0.4220 0.6818 0.3210 0.039 Uiso calc R 1 1
Cl Cl1 0.26515(9) 0.50389(11) 0.37249(10) 0.0455(3) Uani d . 1 1
Cl Cl2 0.40908(11) 0.84731(11) 0.54051(11) 0.0507(3) Uani d . 1 1
Cl Cl3 0.57585(8) 0.66277(9) 0.46628(8) 0.0301(2) Uani d . 1 1
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 0.0000 0.0000 '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 0.0060 '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_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O3 Ti1 O1 . . 101.11(8)
O3 Ti1 O2 . . 98.43(9)
O1 Ti1 O2 . . 95.69(8)
O3 Ti1 O3 . 2_665 82.80(9)
O1 Ti1 O3 . 2_665 100.23(8)
O2 Ti1 O3 . 2_665 163.49(8)
O3 Ti1 N2 . . 100.65(9)
O1 Ti1 N2 . . 158.23(9)
O2 Ti1 N2 . . 81.27(9)
O3 Ti1 N2 2_665 . 82.33(9)
O3 Ti1 N1 . . 168.80(8)
O1 Ti1 N1 . . 82.93(8)
O2 Ti1 N1 . . 91.50(8)
O3 Ti1 N1 2_665 . 86.21(8)
N2 Ti1 N1 . . 75.64(9)
O3 Ti1 Ti1 . 2_665 43.20(6)
O1 Ti1 Ti1 . 2_665 104.27(6)
O2 Ti1 Ti1 . 2_665 139.09(7)
O3 Ti1 Ti1 2_665 2_665 39.60(5)
N2 Ti1 Ti1 . 2_665 91.53(7)
N1 Ti1 Ti1 . 2_665 125.78(6)
C11 O1 Ti1 . . 136.03(17)
C21 O2 Ti1 . . 138.85(18)
Ti1 O3 Ti1 . 2_665 97.20(9)
C17 N1 C18 . . 119.5(2)
C17 N1 Ti1 . . 127.32(19)
C18 N1 Ti1 . . 113.18(17)
C28 N2 C27 . . 113.9(2)
C28 N2 Ti1 . . 112.28(17)
C27 N2 Ti1 . . 112.94(17)
C28 N2 H2 . . 107(2)
C27 N2 H2 . . 109(2)
Ti1 N2 H2 . . 100(2)
O1 C11 C12 . . 118.7(2)
O1 C11 C16 . . 122.2(2)
C12 C11 C16 . . 119.1(3)
C13 C12 C11 . . 120.9(3)
C13 C12 H12 . . 119.5
C11 C12 H12 . . 119.5
C12 C13 C14 . . 120.5(3)
C12 C13 H13 . . 119.7
C14 C13 H13 . . 119.7
C15 C14 C13 . . 119.2(3)
C15 C14 H14 . . 120.4
C13 C14 H14 . . 120.4
C14 C15 C16 . . 121.7(3)
C14 C15 H15 . . 119.2
C16 C15 H15 . . 119.2
C15 C16 C11 . . 118.5(3)
C15 C16 C17 . . 118.2(3)
C11 C16 C17 . . 123.4(3)
N1 C17 C16 . . 124.0(3)
N1 C17 H17 . . 118.0
C16 C17 H17 . . 118.0
N1 C18 C28 . . 107.2(2)
N1 C18 H18A . . 110.3
C28 C18 H18A . . 110.3
N1 C18 H18B . . 110.3
C28 C18 H18B . . 110.3
H18A C18 H18B . . 108.5
O2 C21 C22 . . 119.4(3)
O2 C21 C26 . . 121.7(3)
C22 C21 C26 . . 118.9(3)
C23 C22 C21 . . 120.6(3)
C23 C22 H22 . . 119.7
C21 C22 H22 . . 119.7
C24 C23 C22 . . 120.8(3)
C24 C23 H23 . . 119.6
C22 C23 H23 . . 119.6
C23 C24 C25 . . 119.2(3)
C23 C24 H24 . . 120.4
C25 C24 H24 . . 120.4
C24 C25 C26 . . 121.6(3)
C24 C25 H25 . . 119.2
C26 C25 H25 . . 119.2
C25 C26 C21 . . 118.9(3)
C25 C26 C27 . . 119.7(3)
C21 C26 C27 . . 121.3(2)
N2 C27 C26 . . 113.1(2)
N2 C27 H27A . . 109.0
C26 C27 H27A . . 109.0
N2 C27 H27B . . 109.0
C26 C27 H27B . . 109.0
H27A C27 H27B . . 107.8
N2 C28 C18 . . 109.8(2)
N2 C28 H28A . . 109.7
C18 C28 H28A . . 109.7
N2 C28 H28B . . 109.7
C18 C28 H28B . . 109.7
H28A C28 H28B . . 108.2
Cl2 C1 Cl1 . . 110.39(17)
Cl2 C1 Cl3 . . 109.84(18)
Cl1 C1 Cl3 . . 109.57(18)
Cl2 C1 H1 . . 109.0
Cl1 C1 H1 . . 109.0
Cl3 C1 H1 . . 109.0
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Ti1 O3 . 1.7962(19)
Ti1 O1 . 1.8991(19)
Ti1 O2 . 1.9102(19)
Ti1 O3 2_665 1.9292(19)
Ti1 N2 . 2.220(2)
Ti1 N1 . 2.232(2)
Ti1 Ti1 2_665 2.7958(12)
O1 C11 . 1.332(3)
O2 C21 . 1.341(3)
O3 Ti1 2_665 1.9292(19)
N1 C17 . 1.277(3)
N1 C18 . 1.468(3)
N2 C28 . 1.471(4)
N2 C27 . 1.479(4)
N2 H2 . 0.81(3)
C11 C12 . 1.393(4)
C11 C16 . 1.414(4)
C12 C13 . 1.382(4)
C12 H12 . 0.9500
C13 C14 . 1.386(4)
C13 H13 . 0.9500
C14 C15 . 1.378(4)
C14 H14 . 0.9500
C15 C16 . 1.403(4)
C15 H15 . 0.9500
C16 C17 . 1.447(4)
C17 H17 . 0.9500
C18 C28 . 1.511(4)
C18 H18A . 0.9900
C18 H18B . 0.9900
C21 C22 . 1.399(4)
C21 C26 . 1.408(4)
C22 C23 . 1.383(4)
C22 H22 . 0.9500
C23 C24 . 1.376(5)
C23 H23 . 0.9500
C24 C25 . 1.384(4)
C24 H24 . 0.9500
C25 C26 . 1.392(4)
C25 H25 . 0.9500
C26 C27 . 1.507(4)
C27 H27A . 0.9900
C27 H27B . 0.9900
C28 H28A . 0.9900
C28 H28B . 0.9900
C1 Cl2 . 1.742(3)
C1 Cl1 . 1.765(3)
C1 Cl3 . 1.767(3)
C1 H1 . 1.0000
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N2 H2 Cl3 2_665 0.81(3) 2.84(3) 3.575(3) 151(3)
C1 H1 O2 . 1.00 2.55 3.506(4) 159.6
C1 H1 O3 . 1.00 2.51 3.257(4) 131.4
C17 H17 Cg2 2_675 0.95 2.81 3.754(4) 174
C23 H23 Cg1 1_455 0.95 2.86 3.747(4) 156
