#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:14:48 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179368 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/65/4326521.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_4326521
loop_
_publ_author_name
'Cesar M. Manna'
'Gad Armony'
'Edit Y. Tshuva'
_publ_section_title
;
 New Insights on the Active Species and Mechanism of Cytotoxicity of
 Salan-Ti(IV) Complexes: A Stereochemical Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10284
_journal_page_last               10291
_journal_paper_doi               10.1021/ic201340m
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C44 H56 N4 O6 Ti2, 4(C H2 Cl2)'
_chemical_formula_sum            'C48 H64 Cl8 N4 O6 Ti2'
_chemical_formula_weight         1172.44
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                115.766(2)
_cell_angle_beta                 100.287(2)
_cell_angle_gamma                106.986(2)
_cell_formula_units_Z            1
_cell_length_a                   10.5305(14)
_cell_length_b                   12.5984(17)
_cell_length_c                   12.7306(17)
_cell_measurement_temperature    173(1)
_cell_volume                     1360.0(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(1)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14907
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.736
_exptl_absorpt_correction_T_max  0.9234
_exptl_absorpt_correction_T_min  0.7673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS V2.05'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_description       shapeless
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.132
_refine_diff_density_min         -1.010
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         5841
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0728
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0892P)²+2.8240P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1842
_refine_ls_wR_factor_ref         0.1903
_reflns_number_gt                5152
_reflns_number_total             5841
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201340m_si_002_1.cif
_cod_data_source_block           Ti2(u_O)2(r,r_L1)(s,s_L1)
_cod_database_code               4326521
loop_
_symmetry_equiv_pos_as_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
C1 C 0.5921(3) 0.2235(3) 0.3176(3) 0.0221(6) Uani 1 1 d .
C2 C 0.5450(4) 0.0926(3) 0.2786(3) 0.0280(7) Uani 1 1 d .
H2 H 0.4902 0.0590 0.3176 0.034 Uiso 1 1 calc R
C3 C 0.5776(4) 0.0110(3) 0.1832(4) 0.0316(8) Uani 1 1 d .
H3 H 0.5426 -0.0786 0.1563 0.038 Uiso 1 1 calc R
C4 C 0.6601(4) 0.0575(4) 0.1265(3) 0.0309(8) Uani 1 1 d .
C5 C 0.7083(4) 0.1891(3) 0.1668(3) 0.0283(7) Uani 1 1 d .
H5 H 0.7660 0.2226 0.1294 0.034 Uiso 1 1 calc R
C6 C 0.6741(4) 0.2729(3) 0.2604(3) 0.0248(7) Uani 1 1 d .
C7 C 0.7192(4) 0.4121(3) 0.2940(3) 0.0270(7) Uani 1 1 d .
H7A H 0.7885 0.4321 0.2546 0.032 Uiso 1 1 calc R
H7B H 0.6354 0.4236 0.2601 0.032 Uiso 1 1 calc R
C8 C 0.8489(3) 0.6424(3) 0.4651(3) 0.0236(7) Uani 1 1 d .
H8 H 0.7757 0.6591 0.4208 0.028 Uiso 1 1 calc R
C9 C 0.9788(4) 0.6768(4) 0.4292(4) 0.0357(8) Uani 1 1 d .
H9A H 0.9514 0.6234 0.3376 0.043 Uiso 1 1 calc R
H9B H 1.0509 0.6566 0.4686 0.043 Uiso 1 1 calc R
C10 C 1.0432(5) 0.8203(4) 0.4705(4) 0.0419(10) Uani 1 1 d .
H10A H 1.1288 0.8404 0.4482 0.050 Uiso 1 1 calc R
H10B H 0.9738 0.8397 0.4269 0.050 Uiso 1 1 calc R
C11 C 1.0829(4) 0.9040(4) 0.6113(4) 0.0408(10) Uani 1 1 d .
H11A H 1.1585 0.8901 0.6547 0.049 Uiso 1 1 calc R
H11B H 1.1206 0.9967 0.6366 0.049 Uiso 1 1 calc R
C12 C 0.9547(4) 0.8712(3) 0.6501(4) 0.0325(8) Uani 1 1 d .
H12A H 0.8845 0.8961 0.6154 0.039 Uiso 1 1 calc R
H12B H 0.9854 0.9223 0.7422 0.039 Uiso 1 1 calc R
C13 C 0.8844(3) 0.7271(3) 0.6049(3) 0.0235(7) Uani 1 1 d .
H13 H 0.9530 0.7063 0.6491 0.028 Uiso 1 1 calc R
C14 C 0.7728(4) 0.7462(3) 0.7667(3) 0.0235(7) Uani 1 1 d .
H14A H 0.6791 0.7196 0.7757 0.028 Uiso 1 1 calc R
H14B H 0.8168 0.8420 0.8096 0.028 Uiso 1 1 calc R
C15 C 0.8646(3) 0.7037(3) 0.8286(3) 0.0222(6) Uani 1 1 d .
C16 C 0.9607(4) 0.7907(3) 0.9508(3) 0.0271(7) Uani 1 1 d .
H16 H 0.9700 0.8775 0.9910 0.033 Uiso 1 1 calc R
C17 C 1.0430(4) 0.7554(4) 1.0157(3) 0.0313(8) Uani 1 1 d .
C18 C 1.0296(4) 0.6285(4) 0.9545(3) 0.0298(7) Uani 1 1 d .
H18 H 1.0859 0.6023 0.9966 0.036 Uiso 1 1 calc R
C19 C 0.9359(4) 0.5396(3) 0.8333(3) 0.0257(7) Uani 1 1 d .
H19 H 0.9287 0.4533 0.7936 0.031 Uiso 1 1 calc R
C20 C 0.8517(3) 0.5752(3) 0.7686(3) 0.0214(6) Uani 1 1 d .
C21 C 0.6979(5) -0.0313(4) 0.0242(4) 0.0416(10) Uani 1 1 d .
H21A H 0.7428 -0.0759 0.0539 0.062 Uiso 1 1 calc R
H21B H 0.7638 0.0199 0.0011 0.062 Uiso 1 1 calc R
H21C H 0.6114 -0.0954 -0.0488 0.062 Uiso 1 1 calc R
C22 C 1.1441(5) 0.8529(4) 1.1487(4) 0.0490(11) Uani 1 1 d .
H22A H 1.1348 0.8129 1.1995 0.073 Uiso 1 1 calc R
H22B H 1.1211 0.9282 1.1827 0.073 Uiso 1 1 calc R
H22C H 1.2418 0.8809 1.1500 0.073 Uiso 1 1 calc R
C23 C 0.7012(5) 0.5914(5) 0.0179(5) 0.0573(13) Uani 1 1 d .
H23A H 0.6631 0.5035 0.0057 0.069 Uiso 1 1 calc R
H23B H 0.7807 0.5997 -0.0138 0.069 Uiso 1 1 calc R
C24 C 0.5161(6) 0.2497(6) 0.6351(6) 0.0697(16) Uani 1 1 d .
H24A H 0.5795 0.2536 0.5868 0.084 Uiso 1 1 calc R
H24B H 0.4918 0.3251 0.6577 0.084 Uiso 1 1 calc R
Cl1 Cl 0.57096(18) 0.6076(2) -0.0672(2) 0.1097(8) Uani 1 1 d .
Cl2 Cl 0.7645(3) 0.7033(3) 0.17316(19) 0.1630(14) Uani 1 1 d .
Cl3 Cl 0.36016(16) 0.10697(18) 0.54052(18) 0.0887(6) Uani 1 1 d .
Cl4 Cl 0.60537(19) 0.26203(18) 0.76820(18) 0.0912(6) Uani 1 1 d .
N1 N 0.7842(3) 0.5042(3) 0.4305(3) 0.0217(6) Uani 1 1 d .
H1N H 0.845(5) 0.489(4) 0.460(4) 0.033 Uiso 1 1 d .
N2 N 0.7518(3) 0.6906(3) 0.6318(3) 0.0209(5) Uani 1 1 d .
H2N H 0.705(5) 0.717(4) 0.604(4) 0.031 Uiso 1 1 d .
O1 O 0.4811(2) 0.4797(2) 0.5844(2) 0.0209(5) Uani 1 1 d .
O2 O 0.5548(2) 0.3000(2) 0.4085(2) 0.0232(5) Uani 1 1 d .
O4 O 0.7608(2) 0.4870(2) 0.6514(2) 0.0234(5) Uani 1 1 d .
Ti1 Ti 0.62151(6) 0.47801(5) 0.52427(5) 0.01787(17) Uani 1 1 d .
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O2 C1 C2 119.0(3) . .
O2 C1 C6 121.5(3) . .
C2 C1 C6 119.5(3) . .
C3 C2 C1 120.4(3) . .
C3 C2 H2 119.8 . .
C1 C2 H2 119.8 . .
C4 C3 C2 121.3(3) . .
C4 C3 H3 119.4 . .
C2 C3 H3 119.4 . .
C3 C4 C5 118.1(3) . .
C3 C4 C21 121.1(3) . .
C5 C4 C21 120.7(3) . .
C4 C5 C6 121.8(3) . .
C4 C5 H5 119.1 . .
C6 C5 H5 119.1 . .
C5 C6 C1 118.8(3) . .
C5 C6 C7 119.9(3) . .
C1 C6 C7 121.2(3) . .
N1 C7 C6 112.4(3) . .
N1 C7 H7A 109.1 . .
C6 C7 H7A 109.1 . .
N1 C7 H7B 109.1 . .
C6 C7 H7B 109.1 . .
H7A C7 H7B 107.9 . .
N1 C8 C9 113.8(3) . .
N1 C8 C13 107.9(3) . .
C9 C8 C13 111.2(3) . .
N1 C8 H8 107.9 . .
C9 C8 H8 107.9 . .
C13 C8 H8 107.9 . .
C8 C9 C10 111.4(3) . .
C8 C9 H9A 109.3 . .
C10 C9 H9A 109.3 . .
C8 C9 H9B 109.3 . .
C10 C9 H9B 109.3 . .
H9A C9 H9B 108.0 . .
C11 C10 C9 110.0(3) . .
C11 C10 H10A 109.7 . .
C9 C10 H10A 109.7 . .
C11 C10 H10B 109.7 . .
C9 C10 H10B 109.7 . .
H10A C10 H10B 108.2 . .
C12 C11 C10 111.2(3) . .
C12 C11 H11A 109.4 . .
C10 C11 H11A 109.4 . .
C12 C11 H11B 109.4 . .
C10 C11 H11B 109.4 . .
H11A C11 H11B 108.0 . .
C11 C12 C13 112.0(3) . .
C11 C12 H12A 109.2 . .
C13 C12 H12A 109.2 . .
C11 C12 H12B 109.2 . .
C13 C12 H12B 109.2 . .
H12A C12 H12B 107.9 . .
N2 C13 C8 108.0(3) . .
N2 C13 C12 113.1(3) . .
C8 C13 C12 111.8(3) . .
N2 C13 H13 107.9 . .
C8 C13 H13 107.9 . .
C12 C13 H13 107.9 . .
N2 C14 C15 112.7(3) . .
N2 C14 H14A 109.1 . .
C15 C14 H14A 109.1 . .
N2 C14 H14B 109.1 . .
C15 C14 H14B 109.1 . .
H14A C14 H14B 107.8 . .
C16 C15 C20 118.7(3) . .
C16 C15 C14 119.9(3) . .
C20 C15 C14 121.4(3) . .
C17 C16 C15 122.7(3) . .
C17 C16 H16 118.7 . .
C15 C16 H16 118.7 . .
C16 C17 C18 117.7(3) . .
C16 C17 C22 120.6(4) . .
C18 C17 C22 121.7(3) . .
C19 C18 C17 121.3(3) . .
C19 C18 H18 119.4 . .
C17 C18 H18 119.4 . .
C18 C19 C20 120.8(3) . .
C18 C19 H19 119.6 . .
C20 C19 H19 119.6 . .
O4 C20 C19 119.8(3) . .
O4 C20 C15 121.4(3) . .
C19 C20 C15 118.8(3) . .
C4 C21 H21A 109.5 . .
C4 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
C4 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
C17 C22 H22A 109.5 . .
C17 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
C17 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
Cl2 C23 Cl1 113.1(4) . .
Cl2 C23 H23A 109.0 . .
Cl1 C23 H23A 109.0 . .
Cl2 C23 H23B 109.0 . .
Cl1 C23 H23B 109.0 . .
H23A C23 H23B 107.8 . .
Cl4 C24 Cl3 113.5(3) . .
Cl4 C24 H24A 108.9 . .
Cl3 C24 H24A 108.9 . .
Cl4 C24 H24B 108.9 . .
Cl3 C24 H24B 108.9 . .
H24A C24 H24B 107.7 . .
C7 N1 C8 113.3(3) . .
C7 N1 Ti1 110.8(2) . .
C8 N1 Ti1 109.39(19) . .
C7 N1 H1N 110(3) . .
C8 N1 H1N 108(3) . .
Ti1 N1 H1N 106(3) . .
C13 N2 C14 114.7(3) . .
C13 N2 Ti1 112.65(19) . .
C14 N2 Ti1 111.0(2) . .
C13 N2 H2N 105(3) . .
C14 N2 H2N 109(3) . .
Ti1 N2 H2N 104(3) . .
Ti1 O1 Ti1 96.70(10) . 2_666
C1 O2 Ti1 137.0(2) . .
C20 O4 Ti1 138.1(2) . .
O1 Ti1 O2 100.92(10) . .
O1 Ti1 O4 102.04(10) . .
O2 Ti1 O4 97.15(10) . .
O1 Ti1 O1 83.30(10) . 2_666
O2 Ti1 O1 97.19(10) . 2_666
O4 Ti1 O1 163.44(10) . 2_666
O1 Ti1 N2 97.34(10) . .
O2 Ti1 N2 161.55(10) . .
O4 Ti1 N2 81.45(10) . .
O1 Ti1 N2 82.32(10) 2_666 .
O1 Ti1 N1 166.28(10) . .
O2 Ti1 N1 85.27(10) . .
O4 Ti1 N1 89.18(10) . .
O1 Ti1 N1 83.78(10) 2_666 .
N2 Ti1 N1 76.34(10) . .
O1 Ti1 Ti1 43.94(7) . 2_666
O2 Ti1 Ti1 102.03(8) . 2_666
O4 Ti1 Ti1 143.41(8) . 2_666
O1 Ti1 Ti1 39.37(6) 2_666 2_666
N2 Ti1 Ti1 89.32(8) . 2_666
N1 Ti1 Ti1 123.00(8) . 2_666
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O2 1.355(4) .
C1 C2 1.391(5) .
C1 C6 1.402(5) .
C2 C3 1.385(5) .
C2 H2 0.9500 .
C3 C4 1.384(5) .
C3 H3 0.9500 .
C4 C5 1.395(5) .
C4 C21 1.511(5) .
C5 C6 1.395(5) .
C5 H5 0.9500 .
C6 C7 1.508(5) .
C7 N1 1.481(4) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 N1 1.490(4) .
C8 C9 1.522(5) .
C8 C13 1.524(5) .
C8 H8 1.0000 .
C9 C10 1.528(5) .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 C11 1.526(6) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 C12 1.525(5) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 C13 1.526(5) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 N2 1.486(4) .
C13 H13 1.0000 .
C14 N2 1.490(4) .
C14 C15 1.497(5) .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C15 C16 1.397(5) .
C15 C20 1.408(4) .
C16 C17 1.386(5) .
C16 H16 0.9500 .
C17 C18 1.388(5) .
C17 C22 1.514(5) .
C18 C19 1.385(5) .
C18 H18 0.9500 .
C19 C20 1.400(5) .
C19 H19 0.9500 .
C20 O4 1.343(4) .
C21 H21A 0.9800 .
C21 H21B 0.9800 .
C21 H21C 0.9800 .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C22 H22C 0.9800 .
C23 Cl2 1.702(6) .
C23 Cl1 1.709(6) .
C23 H23A 0.9900 .
C23 H23B 0.9900 .
C24 Cl4 1.701(6) .
C24 Cl3 1.751(6) .
C24 H24A 0.9900 .
C24 H24B 0.9900 .
N1 Ti1 2.283(3) .
N1 H1N 0.80(4) .
N2 Ti1 2.219(3) .
N2 H2N 0.78(4) .
O1 Ti1 1.784(2) .
O1 Ti1 1.951(2) 2_666
O2 Ti1 1.879(2) .
O4 Ti1 1.918(2) .
Ti1 O1 1.951(2) 2_666
Ti1 Ti1 2.7928(11) 2_666
