#------------------------------------------------------------------------------
#$Date: 2015-10-09 13:16:57 +0300 (Fri, 09 Oct 2015) $
#$Revision: 161602 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/62/7036229.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_7036229
loop_
_publ_author_name
'Zhao, Tiankun'
'Grützke, Martin'
'Götz, Kathrin H'
'Druzhenko, Tetiana'
'Huhn, Thomas'
_publ_section_title
;
 Synthesis and X-ray structure analysis of cytotoxic heptacoordinate
 sulfonamide salan titanium(iv)-bis-chelates.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16475
_journal_page_last               16485
_journal_paper_doi               10.1039/c5dt01618e
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C25 H25 N3 O6 Ti'
_chemical_formula_weight         511.38
_chemical_melting_point          449
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-07-05 deposited with the CCDC.
2015-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.497(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7824(13)
_cell_length_b                   14.9183(9)
_cell_length_c                   8.6437(7)
_cell_measurement_reflns_used    16892
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.69
_cell_measurement_theta_min      1.83
_cell_volume                     2163.3(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1342
_diffrn_reflns_av_unetI/netI     0.1260
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            14886
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.261
_diffrn_reflns_theta_min         1.827
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    0.447
_exptl_absorpt_correction_T_max  0.9415
_exptl_absorpt_correction_T_min  0.6640
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
'X-SHAPE 2.07 (03-Aug-2005) Stoe & Cie, Darmstadt, Germany'
;
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1064
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetone, DCM'
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.293
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         2181
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0564P)²+1.4636P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0916
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1909
_reflns_number_total             2181
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt01618e2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7036228--7036229.cif.'
_cod_database_code               7036229
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
C1 C 0.63086(10) 0.70807(11) 0.4821(2) 0.0192(3) Uani 1 1 d . . .
C2 C 0.64775(10) 0.71127(12) 0.6416(2) 0.0213(4) Uani 1 1 d . . .
H2 H 0.6183 0.7503 0.7054 0.026 Uiso 1 1 calc R U .
C3 C 0.70732(10) 0.65775(12) 0.7069(2) 0.0235(4) Uani 1 1 d . . .
H3 H 0.7192 0.6609 0.8148 0.028 Uiso 1 1 calc R U .
C4 C 0.74969(10) 0.59933(12) 0.6139(2) 0.0230(4) Uani 1 1 d . . .
H4 H 0.7896 0.5615 0.6585 0.028 Uiso 1 1 calc R U .
C5 C 0.73335(10) 0.59682(12) 0.4565(2) 0.0232(4) Uani 1 1 d . . .
H5 H 0.7623 0.5566 0.3938 0.028 Uiso 1 1 calc R U .
C6 C 0.67556(9) 0.65169(12) 0.3875(2) 0.0200(4) Uani 1 1 d . . .
C7 C 0.66019(10) 0.64950(12) 0.2154(2) 0.0212(4) Uani 1 1 d . . .
H7A H 0.6801 0.7057 0.1694 0.025 Uiso 1 1 calc R U .
H7B H 0.6902 0.5990 0.1706 0.025 Uiso 1 1 calc R U .
C8 C 0.54484(10) 0.55639(11) 0.2499(2) 0.0213(4) Uani 1 1 d . . .
H8A H 0.5663 0.5536 0.3575 0.026 Uiso 1 1 calc R U .
H8B H 0.5640 0.5031 0.1937 0.026 Uiso 1 1 calc R U .
C9 C 0.56720(11) 0.62832(12) 0.0035(2) 0.0240(4) Uani 1 1 d . . .
H9A H 0.6010 0.5784 -0.0280 0.036 Uiso 1 1 calc R U .
H9B H 0.5848 0.6836 -0.0465 0.036 Uiso 1 1 calc R U .
H9C H 0.5117 0.6159 -0.0275 0.036 Uiso 1 1 calc R U .
C10 C 0.55277(9) 0.95695(11) 0.16534(19) 0.0185(3) Uani 1 1 d . . .
C11 C 0.60465(10) 0.89324(11) 0.07903(19) 0.0194(3) Uani 1 1 d . . .
C12 C 0.5000 1.09620(17) 0.2500 0.0251(5) Uani 1 2 d S T P
H12 H 0.5000 1.1599 0.2500 0.030 Uiso 1 2 calc R U P
C13 C 0.55435(10) 1.05007(12) 0.1617(2) 0.0225(4) Uani 1 1 d . . .
H13 H 0.5916 1.0812 0.1006 0.027 Uiso 1 1 calc R U .
N1 N 0.57330(8) 0.63908(10) 0.17370(16) 0.0190(3) Uani 1 1 d . . .
N2 N 0.5000 0.91270(13) 0.2500 0.0168(4) Uani 1 2 d S T P
O1 O 0.57050(7) 0.75706(8) 0.41990(14) 0.0189(3) Uani 1 1 d . . .
O2 O 0.58532(7) 0.81057(8) 0.10518(14) 0.0198(3) Uani 1 1 d . . .
O3 O 0.65741(7) 0.91909(9) -0.00433(15) 0.0262(3) Uani 1 1 d . . .
Ti1 Ti 0.5000 0.76669(3) 0.2500 0.01570(14) Uani 1 2 d S T P
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'
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
O1 C1 C2 120.29(15) . .
O1 C1 C6 119.93(15) . .
C2 C1 C6 119.76(15) . .
C3 C2 C1 120.38(16) . .
C2 C3 C4 119.90(16) . .
C5 C4 C3 119.61(16) . .
C4 C5 C6 121.63(16) . .
C5 C6 C1 118.66(16) . .
C5 C6 C7 120.73(15) . .
C1 C6 C7 120.60(15) . .
N1 C7 C6 112.35(14) . .
N1 C8 C8 109.53(11) . 2_655
N2 C10 C13 121.26(16) . .
N2 C10 C11 111.13(15) . .
C13 C10 C11 127.61(16) . .
O3 C11 O2 126.37(16) . .
O3 C11 C10 122.24(16) . .
O2 C11 C10 111.39(14) . .
C13 C12 C13 120.5(2) 2_655 .
C12 C13 C10 118.05(17) . .
C9 N1 C8 109.64(13) . .
C9 N1 C7 106.93(13) . .
C8 N1 C7 107.55(13) . .
C9 N1 Ti1 109.92(10) . .
C8 N1 Ti1 111.67(10) . .
C7 N1 Ti1 110.99(10) . .
C10 N2 C10 120.9(2) . 2_655
C10 N2 Ti1 119.57(10) . .
C10 N2 Ti1 119.57(10) 2_655 .
C1 O1 Ti1 143.98(11) . .
C11 O2 Ti1 126.62(11) . .
O1 Ti1 O1 171.17(7) 2_655 .
O1 Ti1 O2 89.00(5) 2_655 .
O1 Ti1 O2 93.84(5) . .
O1 Ti1 O2 93.84(5) 2_655 2_655
O1 Ti1 O2 89.00(5) . 2_655
O2 Ti1 O2 142.47(7) . 2_655
O1 Ti1 N2 94.42(4) 2_655 .
O1 Ti1 N2 94.41(4) . .
O2 Ti1 N2 71.23(3) . .
O2 Ti1 N2 71.23(3) 2_655 .
O1 Ti1 N1 92.41(5) 2_655 .
O1 Ti1 N1 80.46(5) . .
O2 Ti1 N1 73.05(5) . .
O2 Ti1 N1 143.95(5) 2_655 .
N2 Ti1 N1 143.46(3) . .
O1 Ti1 N1 80.46(5) 2_655 2_655
O1 Ti1 N1 92.41(5) . 2_655
O2 Ti1 N1 143.95(5) . 2_655
O2 Ti1 N1 73.05(5) 2_655 2_655
N2 Ti1 N1 143.46(3) . 2_655
N1 Ti1 N1 73.08(7) . 2_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.349(2) .
C1 C2 1.401(2) .
C1 C6 1.404(2) .
C2 C3 1.388(2) .
C3 C4 1.393(3) .
C4 C5 1.382(3) .
C5 C6 1.391(2) .
C6 C7 1.503(2) .
C7 N1 1.501(2) .
C8 N1 1.483(2) .
C8 C8 1.505(3) 2_655
C9 N1 1.480(2) .
C10 N2 1.3376(19) .
C10 C13 1.390(2) .
C10 C11 1.501(2) .
C11 O3 1.219(2) .
C11 O2 1.297(2) .
C12 C13 1.387(2) 2_655
C12 C13 1.387(2) .
N1 Ti1 2.3695(14) .
N2 C10 1.3377(19) 2_655
N2 Ti1 2.178(2) .
O1 Ti1 1.8672(11) .
O2 Ti1 2.0345(12) .
Ti1 O1 1.8672(11) 2_655
Ti1 O2 2.0345(12) 2_655
Ti1 N1 2.3695(14) 2_655
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O1 C1 C2 C3 176.93(15) . .
C6 C1 C2 C3 -1.3(3) . .
C1 C2 C3 C4 -1.1(3) . .
C2 C3 C4 C5 1.6(3) . .
C3 C4 C5 C6 0.3(3) . .
C4 C5 C6 C1 -2.6(3) . .
C4 C5 C6 C7 178.46(16) . .
O1 C1 C6 C5 -175.10(15) . .
C2 C1 C6 C5 3.1(2) . .
O1 C1 C6 C7 3.8(2) . .
C2 C1 C6 C7 -177.98(15) . .
C5 C6 C7 N1 129.86(16) . .
C1 C6 C7 N1 -49.0(2) . .
N2 C10 C11 O3 -179.34(13) . .
C13 C10 C11 O3 1.9(3) . .
N2 C10 C11 O2 0.92(17) . .
C13 C10 C11 O2 -177.82(15) . .
C13 C12 C13 C10 -0.32(10) 2_655 .
N2 C10 C13 C12 0.7(2) . .
C11 C10 C13 C12 179.29(13) . .
C8 C8 N1 C9 -80.01(19) 2_655 .
C8 C8 N1 C7 164.07(16) 2_655 .
C8 C8 N1 Ti1 42.07(18) 2_655 .
C6 C7 N1 C9 -174.18(14) . .
C6 C7 N1 C8 -56.48(17) . .
C6 C7 N1 Ti1 65.94(15) . .
C13 C10 N2 C10 -0.34(11) . 2_655
C11 C10 N2 C10 -179.17(14) . 2_655
C13 C10 N2 Ti1 179.66(11) . .
C11 C10 N2 Ti1 0.83(14) . .
C2 C1 O1 Ti1 -158.12(14) . .
C6 C1 O1 Ti1 20.1(3) . .
O3 C11 O2 Ti1 177.66(13) . .
C10 C11 O2 Ti1 -2.61(18) . .
C1 O1 Ti1 O2 -73.39(19) . .
C1 O1 Ti1 O2 144.08(18) . 2_655
C1 O1 Ti1 N2 -144.83(18) . .
C1 O1 Ti1 N1 -1.30(18) . .
C1 O1 Ti1 N1 71.09(18) . 2_655
