# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ym6
_database_code_depnum_ccdc_archive 'CCDC 1055108'
_audit_update_record             
;
2015-03-19 deposited with the CCDC.
2015-05-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H36 Cl2 F4 N2 O2 Ti'
_chemical_formula_sum            'C34 H36 Cl2 F4 N2 O2 Ti'
_chemical_formula_weight         699.45

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'
F F 0.0171 0.0103 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.5330(4)
_cell_length_b                   19.3123(8)
_cell_length_c                   16.1038(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.3484(8)
_cell_angle_gamma                90.00
_cell_volume                     3187.3(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1448
_exptl_absorpt_coefficient_mu    0.494
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8268
_exptl_absorpt_correction_T_max  0.9295
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker X8 APEX II diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            31576
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.36
_diffrn_reflns_theta_max         32.80
_reflns_number_total             10907
_reflns_number_gt                8139
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_reduction        'Bruker SAINT+'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0600P)²+0.7589P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10907
_refine_ls_number_parameters     550
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0454
_refine_ls_wR_factor_ref         0.1134
_refine_ls_wR_factor_gt          0.1033
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.009
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000



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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.43293(2) 0.042281(13) 0.207493(16) 0.01490(6) Uani 1 1 d . . .
Cl1 Cl 0.41179(4) -0.04339(2) 0.10744(3) 0.02873(9) Uani 1 1 d . . .
Cl2 Cl 0.28437(4) 0.00137(2) 0.28043(3) 0.02355(8) Uani 1 1 d . . .
F1 F 0.38261(13) 0.34508(6) 0.16563(8) 0.0444(3) Uani 1 1 d . . .
F2 F 0.16513(11) 0.27989(6) 0.37701(9) 0.0428(3) Uani 1 1 d . . .
F3 F 0.96043(12) 0.17629(8) 0.32826(12) 0.0709(5) Uani 1 1 d . . .
F4 F 0.96673(11) -0.03103(7) 0.18154(10) 0.0537(4) Uani 1 1 d . . .
O1 O 0.57283(10) -0.00010(5) 0.28418(7) 0.0187(2) Uani 1 1 d . . .
O2 O 0.31404(10) 0.10220(5) 0.13827(7) 0.0180(2) Uani 1 1 d . . .
N1 N 0.47573(12) 0.12487(6) 0.30296(8) 0.0165(2) Uani 1 1 d . . .
N2 N 0.56576(11) 0.09450(6) 0.14495(8) 0.0174(2) Uani 1 1 d . . .
C1 C 0.55279(15) 0.11787(8) 0.37894(10) 0.0200(3) Uani 1 1 d . . .
H1 H 0.5585(18) 0.1561(10) 0.4180(12) 0.022(5) Uiso 1 1 d . . .
C2 C 0.63088(15) 0.06008(8) 0.41318(10) 0.0215(3) Uani 1 1 d . . .
C3 C 0.7129(2) 0.06655(10) 0.50370(12) 0.0316(4) Uani 1 1 d . . .
H3B H 0.662(2) 0.0602(12) 0.5445(15) 0.038(6) Uiso 1 1 d . . .
H3A H 0.752(2) 0.1121(13) 0.5112(15) 0.045(7) Uiso 1 1 d . . .
C4 C 0.81825(18) 0.01084(10) 0.52128(12) 0.0320(4) Uani 1 1 d . . .
H4B H 0.882(2) 0.0216(11) 0.4871(14) 0.029(5) Uiso 1 1 d . . .
H4A H 0.861(2) 0.0149(11) 0.5775(14) 0.032(5) Uiso 1 1 d . . .
C5 C 0.75523(19) -0.05915(10) 0.49730(11) 0.0295(4) Uani 1 1 d . . .
H5B H 0.8123(19) -0.0958(10) 0.5127(12) 0.025(5) Uiso 1 1 d . . .
H5A H 0.690(2) -0.0639(12) 0.5249(15) 0.039(6) Uiso 1 1 d . . .
C6 C 0.69847(15) -0.06584(8) 0.40050(10) 0.0224(3) Uani 1 1 d . . .
C7 C 0.63305(13) 0.00133(8) 0.36554(10) 0.0178(3) Uani 1 1 d . . .
C8 C 0.80345(19) -0.08731(11) 0.35118(13) 0.0344(4) Uani 1 1 d . . .
H8B H 0.797(2) -0.0588(13) 0.3019(16) 0.045(6) Uiso 1 1 d . . .
H8A H 0.895(2) -0.0795(12) 0.3878(14) 0.038(6) Uiso 1 1 d . . .
C9 C 0.7730(3) -0.16319(13) 0.32540(18) 0.0519(6) Uani 1 1 d . . .
H9B H 0.809(3) -0.1716(14) 0.2811(18) 0.057(8) Uiso 1 1 d . . .
H9A H 0.812(3) -0.1941(16) 0.376(2) 0.070(9) Uiso 1 1 d . . .
C10 C 0.6257(3) -0.16614(12) 0.30638(16) 0.0462(5) Uani 1 1 d . . .
H10B H 0.586(3) -0.2166(18) 0.305(2) 0.082(10) Uiso 1 1 d . . .
H10A H 0.587(3) -0.1397(15) 0.2491(19) 0.065(8) Uiso 1 1 d . . .
C11 C 0.5951(2) -0.12529(9) 0.37980(13) 0.0309(4) Uani 1 1 d . . .
H11B H 0.508(2) -0.1061(12) 0.3656(15) 0.041(6) Uiso 1 1 d . . .
H11A H 0.612(2) -0.1546(13) 0.4311(16) 0.046(7) Uiso 1 1 d . . .
C12 C 0.40406(14) 0.18877(7) 0.29028(10) 0.0176(3) Uani 1 1 d . . .
C13 C 0.42676(16) 0.23660(8) 0.23092(10) 0.0218(3) Uani 1 1 d . . .
H13 H 0.4876(19) 0.2282(10) 0.1975(13) 0.025(5) Uiso 1 1 d . . .
C14 C 0.35935(18) 0.29846(8) 0.22336(11) 0.0264(3) Uani 1 1 d . . .
C15 C 0.27001(17) 0.31548(9) 0.27081(12) 0.0291(4) Uani 1 1 d . . .
H15 H 0.225(2) 0.3560(11) 0.2660(14) 0.035(6) Uiso 1 1 d . . .
C16 C 0.25004(16) 0.26602(9) 0.32786(12) 0.0269(3) Uani 1 1 d . . .
C17 C 0.31365(16) 0.20269(8) 0.33883(11) 0.0231(3) Uani 1 1 d . . .
H17 H 0.297(2) 0.1719(11) 0.3762(13) 0.029(5) Uiso 1 1 d . . .
C18 C 0.53188(15) 0.13037(8) 0.07435(10) 0.0203(3) Uani 1 1 d . . .
H18 H 0.6040(18) 0.1477(9) 0.0494(12) 0.021(5) Uiso 1 1 d . . .
C19 C 0.40298(15) 0.14800(8) 0.02980(10) 0.0204(3) Uani 1 1 d . . .
C20 C 0.38704(18) 0.18818(11) -0.05276(12) 0.0305(4) Uani 1 1 d . . .
H20B H 0.463(2) 0.2188(12) -0.0499(14) 0.041(6) Uiso 1 1 d . . .
H20A H 0.387(2) 0.1548(13) -0.0987(16) 0.049(7) Uiso 1 1 d . . .
C21 C 0.25897(17) 0.22779(10) -0.07251(12) 0.0292(4) Uani 1 1 d . . .
H31B H 0.246(2) 0.2512(12) -0.1307(16) 0.045(6) Uiso 1 1 d . . .
H31A H 0.2653(19) 0.2651(11) -0.0303(14) 0.029(5) Uiso 1 1 d . . .
C22 C 0.14673(17) 0.17999(9) -0.06839(11) 0.0260(3) Uani 1 1 d . . .
H22B H 0.149(2) 0.1412(12) -0.1069(14) 0.037(6) Uiso 1 1 d . . .
H22A H 0.065(2) 0.2039(11) -0.0882(13) 0.031(5) Uiso 1 1 d . . .
C23 C 0.15752(14) 0.15069(7) 0.02189(10) 0.0179(3) Uani 1 1 d . . .
C24 C 0.29768(14) 0.13330(7) 0.06398(9) 0.0165(3) Uani 1 1 d . . .
C25 C 0.06983(16) 0.08626(9) 0.01918(12) 0.0255(3) Uani 1 1 d . . .
H25B H 0.0902(19) 0.0654(10) 0.0765(13) 0.024(5) Uiso 1 1 d . . .
H25A H 0.086(2) 0.0512(11) -0.0223(14) 0.029(5) Uiso 1 1 d . . .
C26 C -0.06813(17) 0.11620(10) 0.00120(13) 0.0318(4) Uani 1 1 d . . .
H26B H -0.131(2) 0.0853(12) 0.0174(14) 0.041(6) Uiso 1 1 d . . .
H26A H -0.102(2) 0.1254(11) -0.0620(15) 0.038(6) Uiso 1 1 d . . .
C27 C -0.05305(17) 0.18608(11) 0.04833(13) 0.0343(4) Uani 1 1 d . . .
H27B H -0.100(2) 0.2241(12) 0.0114(14) 0.036(6) Uiso 1 1 d . . .
H27A H -0.093(2) 0.1845(13) 0.0981(16) 0.050(7) Uiso 1 1 d . . .
C28 C 0.09573(16) 0.20056(9) 0.07674(12) 0.0258(3) Uani 1 1 d . . .
H28B H 0.1283(19) 0.1876(10) 0.1365(13) 0.025(5) Uiso 1 1 d . . .
H28A H 0.1210(19) 0.2497(11) 0.0671(13) 0.028(5) Uiso 1 1 d . . .
C29 C 0.70336(13) 0.08755(8) 0.18050(10) 0.0180(3) Uani 1 1 d . . .
C30 C 0.76664(17) 0.13710(9) 0.23694(13) 0.0306(4) Uani 1 1 d . . .
H30 H 0.724(2) 0.1748(13) 0.2499(16) 0.046(7) Uiso 1 1 d . . .
C31 C 0.89821(17) 0.12775(10) 0.27302(13) 0.0338(4) Uani 1 1 d . . .
C32 C 0.96906(16) 0.07272(9) 0.25495(12) 0.0268(3) Uani 1 1 d . . .
H32 H 1.053(2) 0.0706(12) 0.2764(14) 0.039(6) Uiso 1 1 d . . .
C33 C 0.90124(16) 0.02495(9) 0.19875(12) 0.0276(3) Uani 1 1 d . . .
C34 C 0.76977(16) 0.03045(9) 0.16034(11) 0.0259(3) Uani 1 1 d . . .
H34 H 0.724(2) -0.0037(11) 0.1232(14) 0.034(6) Uiso 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O2 1.8722(10) . ?
Ti1 O1 1.8777(11) . ?
Ti1 N2 2.1539(12) . ?
Ti1 N1 2.1888(13) . ?
Ti1 Cl1 2.2842(5) . ?
Ti1 Cl2 2.3024(4) . ?
F1 C14 1.357(2) . ?
F2 C16 1.351(2) . ?
F3 C31 1.353(2) . ?
F4 C33 1.3453(19) . ?
O1 C7 1.3176(18) . ?
O2 C24 1.3140(17) . ?
N1 C1 1.310(2) . ?
N1 C12 1.4364(18) . ?
N2 C18 1.309(2) . ?
N2 C29 1.4364(18) . ?
C1 C2 1.420(2) . ?
C2 C7 1.373(2) . ?
C2 C3 1.518(2) . ?
C3 C4 1.525(3) . ?
C4 C5 1.516(3) . ?
C5 C6 1.541(2) . ?
C6 C7 1.515(2) . ?
C6 C8 1.559(2) . ?
C6 C11 1.564(2) . ?
C8 C9 1.537(3) . ?
C9 C10 1.512(4) . ?
C10 C11 1.516(3) . ?
C12 C13 1.389(2) . ?
C12 C17 1.391(2) . ?
C13 C14 1.381(2) . ?
C14 C15 1.382(3) . ?
C15 C16 1.375(3) . ?
C16 C17 1.386(2) . ?
C18 C19 1.423(2) . ?
C19 C24 1.377(2) . ?
C19 C20 1.515(2) . ?
C20 C21 1.519(2) . ?
C21 C22 1.513(2) . ?
C22 C23 1.540(2) . ?
C23 C24 1.513(2) . ?
C23 C25 1.544(2) . ?
C23 C28 1.548(2) . ?
C25 C26 1.528(2) . ?
C26 C27 1.538(3) . ?
C27 C28 1.553(2) . ?
C29 C30 1.381(2) . ?
C29 C34 1.384(2) . ?
C30 C31 1.385(2) . ?
C31 C32 1.368(2) . ?
C32 C33 1.372(3) . ?
C33 C34 1.384(2) . ?

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
_geom_angle_publ_flag
O2 Ti1 O1 167.53(5) . . ?
O2 Ti1 N2 81.35(5) . . ?
O1 Ti1 N2 90.90(5) . . ?
O2 Ti1 N1 88.21(5) . . ?
O1 Ti1 N1 81.53(5) . . ?
N2 Ti1 N1 86.36(5) . . ?
O2 Ti1 Cl1 94.86(4) . . ?
O1 Ti1 Cl1 94.71(4) . . ?
N2 Ti1 Cl1 88.70(4) . . ?
N1 Ti1 Cl1 173.73(3) . . ?
O2 Ti1 Cl2 94.35(3) . . ?
O1 Ti1 Cl2 92.15(3) . . ?
N2 Ti1 Cl2 172.11(4) . . ?
N1 Ti1 Cl2 86.89(3) . . ?
Cl1 Ti1 Cl2 98.296(18) . . ?
C7 O1 Ti1 140.30(10) . . ?
C24 O2 Ti1 138.92(9) . . ?
C1 N1 C12 114.42(13) . . ?
C1 N1 Ti1 124.30(10) . . ?
C12 N1 Ti1 120.66(9) . . ?
C18 N2 C29 116.31(12) . . ?
C18 N2 Ti1 125.30(10) . . ?
C29 N2 Ti1 118.33(9) . . ?
N1 C1 C2 128.48(15) . . ?
C7 C2 C1 121.03(14) . . ?
C7 C2 C3 121.69(14) . . ?
C1 C2 C3 117.27(14) . . ?
C2 C3 C4 110.40(15) . . ?
C5 C4 C3 108.95(15) . . ?
C4 C5 C6 112.17(14) . . ?
C7 C6 C5 109.94(14) . . ?
C7 C6 C8 110.71(13) . . ?
C5 C6 C8 112.49(14) . . ?
C7 C6 C11 108.34(13) . . ?
C5 C6 C11 111.44(14) . . ?
C8 C6 C11 103.71(14) . . ?
O1 C7 C2 120.44(13) . . ?
O1 C7 C6 115.14(13) . . ?
C2 C7 C6 124.39(14) . . ?
C9 C8 C6 105.24(17) . . ?
C10 C9 C8 103.37(17) . . ?
C9 C10 C11 102.42(19) . . ?
C10 C11 C6 106.58(16) . . ?
C13 C12 C17 120.49(14) . . ?
C13 C12 N1 120.05(13) . . ?
C17 C12 N1 119.45(13) . . ?
C14 C13 C12 117.98(15) . . ?
F1 C14 C13 117.65(16) . . ?
F1 C14 C15 118.35(15) . . ?
C13 C14 C15 124.00(16) . . ?
C16 C15 C14 115.65(15) . . ?
F2 C16 C15 118.55(15) . . ?
F2 C16 C17 117.78(16) . . ?
C15 C16 C17 123.66(16) . . ?
C16 C17 C12 118.19(15) . . ?
N2 C18 C19 127.00(13) . . ?
C24 C19 C18 120.81(14) . . ?
C24 C19 C20 121.35(14) . . ?
C18 C19 C20 117.68(13) . . ?
C19 C20 C21 110.77(14) . . ?
C22 C21 C20 110.40(15) . . ?
C21 C22 C23 112.17(14) . . ?
C24 C23 C22 110.87(12) . . ?
C24 C23 C25 110.43(12) . . ?
C22 C23 C25 110.86(13) . . ?
C24 C23 C28 112.19(13) . . ?
C22 C23 C28 111.17(13) . . ?
C25 C23 C28 100.94(13) . . ?
O2 C24 C19 120.65(13) . . ?
O2 C24 C23 114.75(12) . . ?
C19 C24 C23 124.60(13) . . ?
C26 C25 C23 103.71(13) . . ?
C25 C26 C27 104.66(14) . . ?
C26 C27 C28 106.59(14) . . ?
C23 C28 C27 104.38(14) . . ?
C30 C29 C34 120.88(15) . . ?
C30 C29 N2 119.14(14) . . ?
C34 C29 N2 119.94(14) . . ?
C29 C30 C31 118.03(16) . . ?
F3 C31 C32 118.22(16) . . ?
F3 C31 C30 118.12(16) . . ?
C32 C31 C30 123.65(17) . . ?
C31 C32 C33 115.87(16) . . ?
F4 C33 C32 117.56(15) . . ?
F4 C33 C34 118.51(16) . . ?
C32 C33 C34 123.92(16) . . ?
C33 C34 C29 117.65(15) . . ?

_diffrn_measured_fraction_theta_max 0.922
_diffrn_reflns_theta_full        32.80
_diffrn_measured_fraction_theta_full 0.922
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.065
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ym3
_database_code_depnum_ccdc_archive 'CCDC 1055109'
_audit_update_record             
;
2015-03-19 deposited with the CCDC.
2015-05-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H30 Cl2 F10 N2 O2 Ti, C7 H7'
_chemical_formula_sum            'C41 H37 Cl2 F10 N2 O2 Ti'
_chemical_formula_weight         898.53

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'
F F 0.0171 0.0103 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

loop_
_symmetry_equiv_pos_as_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'

_cell_length_a                   26.090(4)
_cell_length_b                   9.2839(11)
_cell_length_c                   16.883(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.216(5)
_cell_angle_gamma                90.00
_cell_volume                     3906.3(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1836
_exptl_absorpt_coefficient_mu    0.443
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8426
_exptl_absorpt_correction_T_max  0.8785
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14139
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0359
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.34
_diffrn_reflns_theta_max         28.28
_reflns_number_total             4732
_reflns_number_gt                3694
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0542P)²+1.0650P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    riding
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4732
_refine_ls_number_parameters     267
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0342
_refine_ls_wR_factor_ref         0.0979
_refine_ls_wR_factor_gt          0.0914
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000


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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.0000 0.14970(4) 0.2500 0.01638(10) Uani 1 2 d S . .
Cl1 Cl 0.020957(17) 0.32052(4) 0.16688(3) 0.02472(11) Uani 1 1 d . . .
F1 F -0.11066(5) 0.40697(11) 0.12528(7) 0.0338(3) Uani 1 1 d . . .
F2 F -0.17992(5) 0.57673(11) 0.17344(8) 0.0405(3) Uani 1 1 d . . .
F3 F -0.23012(5) 0.47693(13) 0.28166(8) 0.0449(3) Uani 1 1 d . . .
F4 F -0.20964(5) 0.20533(13) 0.34381(8) 0.0416(3) Uani 1 1 d . . .
F5 F -0.14045(5) 0.03428(11) 0.29605(7) 0.0367(3) Uani 1 1 d . . .
O1 O 0.00252(5) 0.00344(12) 0.17366(8) 0.0249(3) Uani 1 1 d . . .
N1 N -0.08492(5) 0.12717(13) 0.18780(8) 0.0187(3) Uani 1 1 d . . .
C1 C -0.10695(7) 0.02188(16) 0.13601(10) 0.0215(3) Uani 1 1 d . . .
H1A H -0.1450 0.0219 0.1164 0.026 Uiso 1 1 calc R . .
C2 C -0.08125(7) -0.09022(16) 0.10612(11) 0.0217(3) Uani 1 1 d . . .
C3 C -0.11651(8) -0.2013(2) 0.04929(13) 0.0335(4) Uani 1 1 d . . .
H3C H -0.1478 -0.1525 0.0109 0.040 Uiso 1 1 calc R . .
H3D H -0.1300 -0.2707 0.0829 0.040 Uiso 1 1 calc R . .
C4 C -0.08586(8) -0.28192(19) -0.00053(12) 0.0313(4) Uani 1 1 d . . .
H4C H -0.0786 -0.2169 -0.0425 0.038 Uiso 1 1 calc R . .
H4D H -0.1076 -0.3639 -0.0299 0.038 Uiso 1 1 calc R . .
C5 C -0.03299(8) -0.33722(17) 0.05769(12) 0.0276(4) Uani 1 1 d . . .
H5C H -0.0148 -0.3975 0.0257 0.033 Uiso 1 1 calc R . .
H5D H -0.0407 -0.3989 0.1007 0.033 Uiso 1 1 calc R . .
C6 C 0.00494(7) -0.21494(15) 0.10023(10) 0.0200(3) Uani 1 1 d . . .
C7 C 0.05158(8) -0.27249(17) 0.17377(11) 0.0257(4) Uani 1 1 d . . .
H7C H 0.0675 -0.1938 0.2129 0.031 Uiso 1 1 calc R . .
H7D H 0.0387 -0.3489 0.2041 0.031 Uiso 1 1 calc R . .
C8 C 0.09273(8) -0.33314(19) 0.13333(13) 0.0329(4) Uani 1 1 d . . .
H8C H 0.1297 -0.3116 0.1681 0.040 Uiso 1 1 calc R . .
H8D H 0.0887 -0.4389 0.1267 0.040 Uiso 1 1 calc R . .
C9 C 0.08152(8) -0.2603(2) 0.04864(13) 0.0338(4) Uani 1 1 d . . .
H9C H 0.0707 -0.3325 0.0036 0.041 Uiso 1 1 calc R . .
H9D H 0.1139 -0.2094 0.0442 0.041 Uiso 1 1 calc R . .
C10 C 0.03579(7) -0.15304(17) 0.04259(11) 0.0238(4) Uani 1 1 d . . .
H10C H 0.0121 -0.1461 -0.0152 0.029 Uiso 1 1 calc R . .
H10D H 0.0502 -0.0562 0.0614 0.029 Uiso 1 1 calc R . .
C11 C -0.02636(7) -0.09744(15) 0.12752(10) 0.0188(3) Uani 1 1 d . . .
C12 C -0.12403(7) 0.21574(16) 0.20868(10) 0.0201(3) Uani 1 1 d . . .
C13 C -0.13474(7) 0.35494(17) 0.17872(11) 0.0228(3) Uani 1 1 d . . .
C14 C -0.17012(8) 0.44225(18) 0.20334(12) 0.0282(4) Uani 1 1 d . . .
C15 C -0.19562(7) 0.39203(19) 0.25824(12) 0.0289(4) Uani 1 1 d . . .
C16 C -0.18566(8) 0.2544(2) 0.28918(12) 0.0283(4) Uani 1 1 d . . .
C17 C -0.15029(7) 0.16786(17) 0.26413(11) 0.0246(4) Uani 1 1 d . . .
C1S C -0.22793(10) 0.1522(3) -0.04211(16) 0.0540(6) Uani 1 1 d . . .
H1SA H -0.2126 0.0850 -0.0710 0.065 Uiso 1 1 calc R . .
C2S C -0.22355(10) 0.2958(3) -0.05444(17) 0.0551(7) Uani 1 1 d . . .
H2SA H -0.2054 0.3277 -0.0923 0.066 Uiso 1 1 calc R . .
C3S C -0.24515(9) 0.3967(3) -0.01278(16) 0.0519(6) Uani 1 1 d . . .
C4S C -0.23983(18) 0.5433(5) -0.0254(3) 0.0452(11) Uani 0.50 1 d P . .
H4SA H -0.2199 0.5573 -0.0657 0.068 Uiso 0.50 1 calc PR . .
H4SB H -0.2204 0.5890 0.0272 0.068 Uiso 0.50 1 calc PR . .
H4SC H -0.2755 0.5869 -0.0466 0.068 Uiso 0.50 1 calc PR . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O1 1.8867(11) . ?
Ti1 O1 1.8867(11) 2 ?
Ti1 N1 2.1629(14) . ?
Ti1 N1 2.1629(14) 2 ?
Ti1 Cl1 2.2887(5) . ?
Ti1 Cl1 2.2888(5) 2 ?
F1 C13 1.333(2) . ?
F2 C14 1.3426(19) . ?
F3 C15 1.3411(19) . ?
F4 C16 1.338(2) . ?
F5 C17 1.3463(18) . ?
O1 C11 1.3056(18) . ?
N1 C1 1.324(2) . ?
N1 C12 1.433(2) . ?
C1 C2 1.410(2) . ?
C2 C11 1.371(2) . ?
C2 C3 1.519(2) . ?
C3 C4 1.518(2) . ?
C4 C5 1.526(3) . ?
C5 C6 1.537(2) . ?
C6 C11 1.514(2) . ?
C6 C10 1.546(2) . ?
C6 C7 1.554(2) . ?
C7 C8 1.540(2) . ?
C8 C9 1.530(3) . ?
C9 C10 1.534(2) . ?
C12 C13 1.386(2) . ?
C12 C17 1.387(2) . ?
C13 C14 1.382(2) . ?
C14 C15 1.373(3) . ?
C15 C16 1.376(3) . ?
C16 C17 1.381(2) . ?
C1S C2S 1.359(4) . ?
C1S C3S 1.394(4) 7_455 ?
C2S C3S 1.387(4) . ?
C3S C4S 1.391(5) . ?
C3S C1S 1.394(4) 7_455 ?

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
_geom_angle_publ_flag
O1 Ti1 O1 87.94(8) . 2 ?
O1 Ti1 N1 80.60(5) . . ?
O1 Ti1 N1 91.38(5) 2 . ?
O1 Ti1 N1 91.39(5) . 2 ?
O1 Ti1 N1 80.60(5) 2 2 ?
N1 Ti1 N1 168.90(7) . 2 ?
O1 Ti1 Cl1 90.96(4) . . ?
O1 Ti1 Cl1 168.70(4) 2 . ?
N1 Ti1 Cl1 99.53(4) . . ?
N1 Ti1 Cl1 88.19(4) 2 . ?
O1 Ti1 Cl1 168.70(4) . 2 ?
O1 Ti1 Cl1 90.96(4) 2 2 ?
N1 Ti1 Cl1 88.19(4) . 2 ?
N1 Ti1 Cl1 99.53(4) 2 2 ?
Cl1 Ti1 Cl1 92.27(3) . 2 ?
C11 O1 Ti1 142.48(11) . . ?
C1 N1 C12 112.61(14) . . ?
C1 N1 Ti1 125.04(11) . . ?
C12 N1 Ti1 121.78(10) . . ?
N1 C1 C2 128.45(16) . . ?
C11 C2 C1 120.81(15) . . ?
C11 C2 C3 121.56(14) . . ?
C1 C2 C3 117.63(15) . . ?
C2 C3 C4 111.40(15) . . ?
C3 C4 C5 109.44(16) . . ?
C4 C5 C6 112.74(13) . . ?
C11 C6 C5 110.11(14) . . ?
C11 C6 C10 110.61(12) . . ?
C5 C6 C10 111.32(14) . . ?
C11 C6 C7 111.72(13) . . ?
C5 C6 C7 111.29(13) . . ?
C10 C6 C7 101.56(14) . . ?
C8 C7 C6 104.80(14) . . ?
C9 C8 C7 106.70(14) . . ?
C8 C9 C10 106.19(15) . . ?
C9 C10 C6 104.87(13) . . ?
O1 C11 C2 119.72(14) . . ?
O1 C11 C6 115.49(14) . . ?
C2 C11 C6 124.78(14) . . ?
C13 C12 C17 117.30(15) . . ?
C13 C12 N1 121.78(15) . . ?
C17 C12 N1 120.80(14) . . ?
F1 C13 C14 118.79(14) . . ?
F1 C13 C12 120.02(14) . . ?
C14 C13 C12 121.19(16) . . ?
F2 C14 C15 119.56(16) . . ?
F2 C14 C13 120.15(17) . . ?
C15 C14 C13 120.29(16) . . ?
F3 C15 C14 120.09(16) . . ?
F3 C15 C16 120.11(17) . . ?
C14 C15 C16 119.80(16) . . ?
F4 C16 C15 120.22(16) . . ?
F4 C16 C17 120.29(16) . . ?
C15 C16 C17 119.48(17) . . ?
F5 C17 C16 118.61(16) . . ?
F5 C17 C12 119.45(15) . . ?
C16 C17 C12 121.93(15) . . ?
C2S C1S C3S 120.2(3) . 7_455 ?
C1S C2S C3S 121.3(3) . . ?
C2S C3S C4S 120.6(3) . . ?
C2S C3S C1S 118.5(3) . 7_455 ?
C4S C3S C1S 120.9(3) . 7_455 ?

_diffrn_measured_fraction_theta_max 0.972
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_full 0.972
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.054
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ym1
_database_code_depnum_ccdc_archive 'CCDC 1055110'
_audit_update_record             
;
2015-03-19 deposited with the CCDC.
2015-05-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H38 Cl2 F6 N2 O2 Ti'
_chemical_formula_sum            'C36 H38 Cl2 F6 N2 O2 Ti'
_chemical_formula_weight         763.48

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'
F F 0.0171 0.0103 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.5392(15)
_cell_length_b                   12.9101(17)
_cell_length_c                   29.846(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.051(4)
_cell_angle_gamma                90.00
_cell_volume                     4020.9(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1576
_exptl_absorpt_coefficient_mu    0.405
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8549
_exptl_absorpt_correction_T_max  0.9235
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART diffractometer'
_diffrn_measurement_method       '0.3 deg. phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            39315
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.51
_diffrn_reflns_theta_max         26.37
_reflns_number_total             8206
_reflns_number_gt                6249
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
Solvent toluene molecule is badly disordered and was SQEEZEd
;
# SQUEEZE RESULTS 
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 395 78 ' '
2 0.000 0.500 0.500 395 78 ' '
_platon_squeeze_details          
;
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0674P)²+2.5472P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    riding
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8206
_refine_ls_number_parameters     442
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0485
_refine_ls_wR_factor_ref         0.1309
_refine_ls_wR_factor_gt          0.1222
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.69847(4) 0.61698(3) 0.159316(14) 0.01905(12) Uani 1 1 d . . .
Cl1 Cl 0.66106(7) 0.63214(5) 0.23216(2) 0.03300(17) Uani 1 1 d . . .
Cl2 Cl 0.88276(6) 0.71256(4) 0.16359(2) 0.02881(16) Uani 1 1 d . . .
F1 F 0.7978(2) 0.70426(17) -0.00453(7) 0.0670(6) Uani 1 1 d . . .
F2 F 0.6780(3) 0.57141(14) -0.00717(6) 0.0690(7) Uani 1 1 d . . .
F3 F 0.5943(2) 0.71824(16) -0.02025(6) 0.0658(6) Uani 1 1 d . . .
F4 F 0.36090(16) 0.32030(14) 0.17774(6) 0.0457(4) Uani 1 1 d . . .
F5 F 0.33045(16) 0.38309(12) 0.11061(6) 0.0428(4) Uani 1 1 d . . .
F6 F 0.44942(16) 0.25209(12) 0.12401(6) 0.0413(4) Uani 1 1 d . . .
O1 O 0.78403(16) 0.49161(12) 0.16834(6) 0.0224(4) Uani 1 1 d . . .
O2 O 0.59171(16) 0.72730(12) 0.13864(5) 0.0216(4) Uani 1 1 d . . .
N1 N 0.53665(19) 0.50901(14) 0.14636(7) 0.0203(4) Uani 1 1 d . . .
N2 N 0.7069(2) 0.60869(15) 0.08526(7) 0.0235(4) Uani 1 1 d . . .
C1 C 0.7678(2) 0.39759(17) 0.18299(8) 0.0224(5) Uani 1 1 d . . .
C2 C 0.8889(2) 0.34971(18) 0.20729(9) 0.0253(5) Uani 1 1 d . . .
C3 C 1.0067(3) 0.3724(2) 0.18348(11) 0.0367(7) Uani 1 1 d . . .
H3A H 1.0295 0.3109 0.1665 0.044 Uiso 1 1 calc R . .
H3B H 0.9894 0.4312 0.1622 0.044 Uiso 1 1 calc R . .
C4 C 1.1129(4) 0.3988(3) 0.22108(15) 0.0683(11) Uani 1 1 d . . .
H4A H 1.1519 0.3353 0.2356 0.082 Uiso 1 1 calc R . .
H4B H 1.1805 0.4402 0.2095 0.082 Uiso 1 1 calc R . .
C5 C 1.0479(3) 0.4599(3) 0.25319(14) 0.0565(9) Uani 1 1 d . . .
H5A H 1.0357 0.5325 0.2428 0.068 Uiso 1 1 calc R . .
H5B H 1.0989 0.4596 0.2837 0.068 Uiso 1 1 calc R . .
C6 C 0.9199(3) 0.4073(2) 0.25404(9) 0.0313(6) Uani 1 1 d . . .
H6A H 0.8528 0.4591 0.2576 0.038 Uiso 1 1 calc R . .
H6B H 0.9251 0.3573 0.2794 0.038 Uiso 1 1 calc R . .
C7 C 0.8714(3) 0.23352(19) 0.21409(10) 0.0342(6) Uani 1 1 d . . .
H7A H 0.8738 0.1969 0.1851 0.041 Uiso 1 1 calc R . .
H7B H 0.9425 0.2070 0.2363 0.041 Uiso 1 1 calc R . .
C8 C 0.7455(3) 0.2124(2) 0.23080(10) 0.0352(7) Uani 1 1 d . . .
H8A H 0.7405 0.2527 0.2587 0.042 Uiso 1 1 calc R . .
H8B H 0.7395 0.1379 0.2382 0.042 Uiso 1 1 calc R . .
C9 C 0.6350(3) 0.24204(19) 0.19480(10) 0.0328(6) Uani 1 1 d . . .
H9A H 0.5535 0.2362 0.2075 0.039 Uiso 1 1 calc R . .
H9B H 0.6314 0.1931 0.1691 0.039 Uiso 1 1 calc R . .
C10 C 0.6488(2) 0.35258(17) 0.17753(8) 0.0231(5) Uani 1 1 d . . .
C11 C 0.5398(2) 0.40870(18) 0.15546(8) 0.0221(5) Uani 1 1 d . . .
C12 C 0.4187(3) 0.3416(2) 0.14203(10) 0.0315(6) Uani 1 1 d . . .
C13 C 0.4168(2) 0.56093(17) 0.13152(8) 0.0218(5) Uani 1 1 d . . .
C14 C 0.3380(3) 0.5840(2) 0.16344(10) 0.0313(6) Uani 1 1 d . . .
H14A H 0.3624 0.5655 0.1942 0.038 Uiso 1 1 calc R . .
C15 C 0.2231(3) 0.6345(2) 0.14996(11) 0.0402(7) Uani 1 1 d . . .
H15A H 0.1673 0.6493 0.1715 0.048 Uiso 1 1 calc R . .
C16 C 0.1894(3) 0.6636(2) 0.10537(12) 0.0421(8) Uani 1 1 d . . .
H16A H 0.1107 0.6986 0.0964 0.051 Uiso 1 1 calc R . .
C17 C 0.2694(3) 0.6419(2) 0.07398(11) 0.0378(7) Uani 1 1 d . . .
H17A H 0.2459 0.6623 0.0434 0.045 Uiso 1 1 calc R . .
C18 C 0.3840(3) 0.5907(2) 0.08676(9) 0.0297(6) Uani 1 1 d . . .
H18A H 0.4397 0.5761 0.0651 0.036 Uiso 1 1 calc R . .
C19 C 0.5918(2) 0.80206(17) 0.10906(8) 0.0235(5) Uani 1 1 d . . .
C20 C 0.5397(3) 0.90267(18) 0.12505(9) 0.0269(6) Uani 1 1 d . . .
C21 C 0.6331(3) 0.94092(19) 0.16734(10) 0.0320(6) Uani 1 1 d . . .
H21A H 0.6983 0.8873 0.1772 0.038 Uiso 1 1 calc R . .
H21B H 0.6775 1.0051 0.1601 0.038 Uiso 1 1 calc R . .
C22 C 0.5500(3) 0.9613(3) 0.20426(12) 0.0517(9) Uani 1 1 d . . .
H22A H 0.5991 0.9498 0.2346 0.062 Uiso 1 1 calc R . .
H22B H 0.5169 1.0332 0.2025 0.062 Uiso 1 1 calc R . .
C23 C 0.4432(4) 0.8852(3) 0.19491(13) 0.0602(10) Uani 1 1 d . . .
H23A H 0.3681 0.9074 0.2090 0.072 Uiso 1 1 calc R . .
H23B H 0.4705 0.8157 0.2065 0.072 Uiso 1 1 calc R . .
C24 C 0.4117(3) 0.8842(2) 0.14366(11) 0.0356(7) Uani 1 1 d . . .
H24A H 0.3495 0.9396 0.1333 0.043 Uiso 1 1 calc R . .
H24B H 0.3743 0.8167 0.1331 0.043 Uiso 1 1 calc R . .
C25 C 0.5245(3) 0.9834(2) 0.08715(11) 0.0418(7) Uani 1 1 d . . .
H25A H 0.4451 0.9691 0.0662 0.050 Uiso 1 1 calc R . .
H25B H 0.5167 1.0531 0.1003 0.050 Uiso 1 1 calc R . .
C26 C 0.6376(4) 0.9817(2) 0.06131(12) 0.0485(8) Uani 1 1 d . . .
H26A H 0.7180 0.9900 0.0825 0.058 Uiso 1 1 calc R . .
H26B H 0.6310 1.0397 0.0394 0.058 Uiso 1 1 calc R . .
C27 C 0.6392(4) 0.8790(2) 0.03635(11) 0.0467(8) Uani 1 1 d . . .
H27A H 0.7178 0.8748 0.0217 0.056 Uiso 1 1 calc R . .
H27B H 0.5644 0.8755 0.0123 0.056 Uiso 1 1 calc R . .
C28 C 0.6355(3) 0.78713(19) 0.06841(9) 0.0287(6) Uani 1 1 d . . .
C29 C 0.6779(2) 0.68507(19) 0.05658(8) 0.0261(6) Uani 1 1 d . . .
C30 C 0.6877(4) 0.6690(2) 0.00603(10) 0.0433(8) Uani 1 1 d . . .
C31 C 0.7676(3) 0.5150(2) 0.07214(8) 0.0283(6) Uani 1 1 d . . .
C32 C 0.8968(3) 0.5178(3) 0.06945(11) 0.0485(8) Uani 1 1 d . . .
H32A H 0.9421 0.5815 0.0735 0.058 Uiso 1 1 calc R . .
C33 C 0.9607(4) 0.4284(4) 0.06090(14) 0.0763(14) Uani 1 1 d . . .
H33A H 1.0497 0.4306 0.0588 0.092 Uiso 1 1 calc R . .
C34 C 0.8961(5) 0.3365(4) 0.05550(13) 0.0805(16) Uani 1 1 d . . .
H34A H 0.9406 0.2749 0.0499 0.097 Uiso 1 1 calc R . .
C35 C 0.7664(5) 0.3328(2) 0.05819(11) 0.0640(12) Uani 1 1 d . . .
H35A H 0.7221 0.2687 0.0544 0.077 Uiso 1 1 calc R . .
C36 C 0.7003(3) 0.4229(2) 0.06646(10) 0.0402(7) Uani 1 1 d . . .
H36A H 0.6109 0.4209 0.0682 0.048 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O1 1.8541(16) . ?
Ti1 O2 1.8657(16) . ?
Ti1 N1 2.195(2) . ?
Ti1 N2 2.227(2) . ?
Ti1 Cl1 2.2717(8) . ?
Ti1 Cl2 2.2896(8) . ?
F1 C30 1.325(4) . ?
F2 C30 1.320(3) . ?
F3 C30 1.331(4) . ?
F4 C12 1.329(3) . ?
F5 C12 1.337(3) . ?
F6 C12 1.333(3) . ?
O1 C1 1.310(3) . ?
O2 C19 1.308(3) . ?
N1 C11 1.323(3) . ?
N1 C13 1.444(3) . ?
N2 C29 1.313(3) . ?
N2 C31 1.447(3) . ?
C1 C10 1.370(4) . ?
C1 C2 1.509(3) . ?
C2 C7 1.528(3) . ?
C2 C3 1.542(4) . ?
C2 C6 1.574(4) . ?
C3 C4 1.509(5) . ?
C4 C5 1.481(5) . ?
C5 C6 1.514(4) . ?
C7 C8 1.506(4) . ?
C8 C9 1.519(4) . ?
C9 C10 1.531(3) . ?
C10 C11 1.438(4) . ?
C11 C12 1.548(4) . ?
C13 C14 1.381(4) . ?
C13 C18 1.387(4) . ?
C14 C15 1.384(4) . ?
C15 C16 1.380(5) . ?
C16 C17 1.374(5) . ?
C17 C18 1.383(4) . ?
C19 C28 1.371(4) . ?
C19 C20 1.513(3) . ?
C20 C25 1.530(4) . ?
C20 C24 1.548(4) . ?
C20 C21 1.568(4) . ?
C21 C22 1.524(4) . ?
C22 C23 1.491(5) . ?
C23 C24 1.519(5) . ?
C25 C26 1.507(5) . ?
C26 C27 1.522(4) . ?
C27 C28 1.528(4) . ?
C28 C29 1.451(3) . ?
C29 C30 1.540(4) . ?
C31 C32 1.377(4) . ?
C31 C36 1.383(4) . ?
C32 C33 1.379(5) . ?
C33 C34 1.366(7) . ?
C34 C35 1.381(7) . ?
C35 C36 1.396(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
_geom_angle_publ_flag
O1 Ti1 O2 166.66(7) . . ?
O1 Ti1 N1 79.70(7) . . ?
O2 Ti1 N1 90.51(7) . . ?
O1 Ti1 N2 90.92(7) . . ?
O2 Ti1 N2 79.31(7) . . ?
N1 Ti1 N2 86.14(7) . . ?
O1 Ti1 Cl1 94.71(6) . . ?
O2 Ti1 Cl1 94.21(6) . . ?
N1 Ti1 Cl1 89.34(6) . . ?
N2 Ti1 Cl1 172.05(6) . . ?
O1 Ti1 Cl2 94.06(6) . . ?
O2 Ti1 Cl2 94.28(6) . . ?
N1 Ti1 Cl2 169.86(6) . . ?
N2 Ti1 Cl2 85.97(6) . . ?
Cl1 Ti1 Cl2 99.20(3) . . ?
C1 O1 Ti1 140.70(16) . . ?
C19 O2 Ti1 136.82(16) . . ?
C11 N1 C13 120.9(2) . . ?
C11 N1 Ti1 126.11(17) . . ?
C13 N1 Ti1 112.60(13) . . ?
C29 N2 C31 121.5(2) . . ?
C29 N2 Ti1 124.95(16) . . ?
C31 N2 Ti1 112.91(15) . . ?
O1 C1 C10 120.9(2) . . ?
O1 C1 C2 113.5(2) . . ?
C10 C1 C2 125.5(2) . . ?
C1 C2 C7 110.9(2) . . ?
C1 C2 C3 112.5(2) . . ?
C7 C2 C3 111.5(2) . . ?
C1 C2 C6 106.8(2) . . ?
C7 C2 C6 111.1(2) . . ?
C3 C2 C6 103.8(2) . . ?
C4 C3 C2 105.2(3) . . ?
C5 C4 C3 103.8(3) . . ?
C4 C5 C6 105.4(3) . . ?
C5 C6 C2 105.8(2) . . ?
C8 C7 C2 110.5(2) . . ?
C7 C8 C9 110.1(2) . . ?
C8 C9 C10 111.9(2) . . ?
C1 C10 C11 120.0(2) . . ?
C1 C10 C9 118.9(2) . . ?
C11 C10 C9 121.1(2) . . ?
N1 C11 C10 125.6(2) . . ?
N1 C11 C12 119.9(2) . . ?
C10 C11 C12 114.4(2) . . ?
F4 C12 F6 108.0(2) . . ?
F4 C12 F5 107.1(2) . . ?
F6 C12 F5 104.4(2) . . ?
F4 C12 C11 111.2(2) . . ?
F6 C12 C11 110.6(2) . . ?
F5 C12 C11 115.1(2) . . ?
C14 C13 C18 120.8(2) . . ?
C14 C13 N1 118.2(2) . . ?
C18 C13 N1 120.9(2) . . ?
C13 C14 C15 119.1(3) . . ?
C16 C15 C14 120.3(3) . . ?
C17 C16 C15 120.1(3) . . ?
C16 C17 C18 120.3(3) . . ?
C17 C18 C13 119.2(3) . . ?
O2 C19 C28 121.7(2) . . ?
O2 C19 C20 112.7(2) . . ?
C28 C19 C20 125.6(2) . . ?
C19 C20 C25 110.9(2) . . ?
C19 C20 C24 110.7(2) . . ?
C25 C20 C24 111.3(2) . . ?
C19 C20 C21 108.1(2) . . ?
C25 C20 C21 111.7(2) . . ?
C24 C20 C21 103.9(2) . . ?
C22 C21 C20 106.1(2) . . ?
C23 C22 C21 104.3(3) . . ?
C22 C23 C24 104.3(3) . . ?
C23 C24 C20 106.4(2) . . ?
C26 C25 C20 111.1(2) . . ?
C25 C26 C27 109.1(3) . . ?
C26 C27 C28 111.5(2) . . ?
C19 C28 C29 119.8(2) . . ?
C19 C28 C27 119.1(2) . . ?
C29 C28 C27 121.1(2) . . ?
N2 C29 C28 125.1(2) . . ?
N2 C29 C30 119.7(2) . . ?
C28 C29 C30 115.2(2) . . ?
F2 C30 F1 106.9(3) . . ?
F2 C30 F3 105.0(3) . . ?
F1 C30 F3 107.2(3) . . ?
F2 C30 C29 114.1(2) . . ?
F1 C30 C29 111.6(3) . . ?
F3 C30 C29 111.6(3) . . ?
C32 C31 C36 120.7(3) . . ?
C32 C31 N2 118.2(3) . . ?
C36 C31 N2 120.9(3) . . ?
C31 C32 C33 120.1(4) . . ?
C34 C33 C32 120.1(4) . . ?
C33 C34 C35 120.3(3) . . ?
C34 C35 C36 120.3(4) . . ?
C31 C36 C35 118.5(3) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.942
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.062
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ym2
_database_code_depnum_ccdc_archive 'CCDC 1055111'
_audit_update_record             
;
2015-03-19 deposited with the CCDC.
2015-05-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H34 Cl2 F10 N2 O2 Ti'
_chemical_formula_sum            'C36 H34 Cl2 F10 N2 O2 Ti'
_chemical_formula_weight         835.45

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'
F F 0.0171 0.0103 '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'

_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   P6(1)22

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'-x, -y, z+1/2'
'y, -x+y, z+5/6'
'x-y, x, z+1/6'
'y, x, -z+1/3'
'x-y, -y, -z'
'-x, -x+y, -z+2/3'
'-y, -x, -z+5/6'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/6'

_cell_length_a                   13.5188(16)
_cell_length_b                   13.5188(16)
_cell_length_c                   33.888(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     5363.6(13)
_cell_formula_units_Z            6
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       'flat rod'
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2556
_exptl_absorpt_coefficient_mu    0.478
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8699
_exptl_absorpt_correction_T_max  0.9765
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17307
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_sigmaI/netI    0.0539
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.51
_diffrn_reflns_theta_max         24.63
_reflns_number_total             2819
_reflns_number_gt                2326
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0430P)²+0.0216P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    riding
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(4)
_refine_ls_number_reflns         2819
_refine_ls_number_parameters     240
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0422
_refine_ls_wR_factor_ref         0.0836
_refine_ls_wR_factor_gt          0.0788
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.091
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.00921(6) 0.50460(3) 0.0833 0.02077(19) Uani 1 2 d S . .
Cl1 Cl -0.12199(7) 0.53062(7) 0.05001(2) 0.0312(2) Uani 1 1 d . . .
F1 F 0.24862(17) 0.81630(17) -0.02638(6) 0.0474(6) Uani 1 1 d . . .
F2 F 0.33342(15) 0.71851(15) -0.03012(6) 0.0391(5) Uani 1 1 d . . .
F3 F 0.35282(15) 0.81521(16) 0.02151(6) 0.0449(6) Uani 1 1 d . . .
F4 F 0.06008(15) 0.79182(16) 0.01984(6) 0.0381(5) Uani 1 1 d . . .
F5 F 0.29637(14) 0.74486(15) 0.10981(5) 0.0350(5) Uani 1 1 d . . .
O1 O 0.03608(16) 0.42814(16) 0.04276(6) 0.0232(5) Uani 1 1 d . . .
N1 N 0.1388(2) 0.65212(19) 0.04795(7) 0.0214(6) Uani 1 1 d . . .
C1 C 0.1712(2) 0.6443(3) 0.01205(9) 0.0225(8) Uani 1 1 d . . .
C2 C 0.1170(2) 0.5444(3) -0.01241(9) 0.0221(8) Uani 1 1 d . . .
C3 C 0.0503(2) 0.4399(3) 0.00424(9) 0.0224(7) Uani 1 1 d . . .
C4 C -0.0149(3) 0.3275(3) -0.01822(9) 0.0253(8) Uani 1 1 d . . .
C5 C 0.0204(3) 0.3449(3) -0.06158(9) 0.0323(9) Uani 1 1 d . . .
H5A H 0.0945 0.3473 -0.0643 0.039 Uiso 1 1 calc R . .
H5B H -0.0371 0.2792 -0.0771 0.039 Uiso 1 1 calc R . .
C6 C 0.0314(3) 0.4533(3) -0.07794(10) 0.0370(9) Uani 1 1 d . . .
H6A H -0.0406 0.4542 -0.0736 0.044 Uiso 1 1 calc R . .
H6B H 0.0459 0.4575 -0.1067 0.044 Uiso 1 1 calc R . .
C7 C 0.1296(3) 0.5553(3) -0.05746(9) 0.0310(8) Uani 1 1 d . . .
H7A H 0.1315 0.6262 -0.0660 0.037 Uiso 1 1 calc R . .
H7B H 0.2027 0.5607 -0.0653 0.037 Uiso 1 1 calc R . .
C8 C 0.2763(3) 0.7494(3) -0.00570(10) 0.0310(9) Uani 1 1 d . . .
C9 C 0.1762(3) 0.7632(3) 0.06445(9) 0.0221(8) Uani 1 1 d . . .
C10 C 0.1329(3) 0.8303(3) 0.05103(10) 0.0273(8) Uani 1 1 d . . .
C11 C 0.1621(3) 0.9346(3) 0.06667(10) 0.0355(9) Uani 1 1 d . . .
H11A H 0.1315 0.9787 0.0561 0.043 Uiso 1 1 calc R . .
C12 C 0.2370(3) 0.9744(3) 0.09813(10) 0.0369(9) Uani 1 1 d . . .
H12A H 0.2579 1.0466 0.1094 0.044 Uiso 1 1 calc R . .
C13 C 0.2817(3) 0.9101(3) 0.11329(10) 0.0321(9) Uani 1 1 d . . .
H13A H 0.3328 0.9369 0.1351 0.039 Uiso 1 1 calc R . .
C14 C 0.2509(3) 0.8073(3) 0.09629(9) 0.0268(8) Uani 1 1 d . . .
C15 C -0.1452(3) 0.2817(3) -0.01357(10) 0.0359(9) Uani 1 1 d . . .
H15A H -0.1593 0.3273 0.0061 0.043 Uiso 1 1 calc R . .
H15B H -0.1792 0.2850 -0.0391 0.043 Uiso 1 1 calc R . .
C16 C -0.1960(3) 0.1584(3) 0.00021(12) 0.0537(12) Uani 1 1 d . . .
H16A H -0.2652 0.1351 0.0164 0.064 Uiso 1 1 calc R . .
H16B H -0.2163 0.1060 -0.0226 0.064 Uiso 1 1 calc R . .
C17 C -0.1034(4) 0.1579(3) 0.02432(14) 0.0679(14) Uani 1 1 d . . .
H17A H -0.1155 0.0797 0.0268 0.082 Uiso 1 1 calc R . .
H17B H -0.1000 0.1891 0.0510 0.082 Uiso 1 1 calc R . .
C18 C 0.0040(3) 0.2339(3) 0.00126(10) 0.0345(9) Uani 1 1 d . . .
H18A H 0.0170 0.1893 -0.0192 0.041 Uiso 1 1 calc R . .
H18B H 0.0711 0.2692 0.0190 0.041 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O1 1.862(2) . ?
Ti1 O1 1.862(2) 12_565 ?
Ti1 N1 2.234(2) . ?
Ti1 N1 2.234(2) 12_565 ?
Ti1 Cl1 2.2735(10) . ?
Ti1 Cl1 2.2736(10) 12_565 ?
F1 C8 1.337(4) . ?
F2 C8 1.333(4) . ?
F3 C8 1.339(4) . ?
F4 C10 1.359(4) . ?
F5 C14 1.349(4) . ?
O1 C3 1.317(3) . ?
N1 C1 1.315(4) . ?
N1 C9 1.437(4) . ?
C1 C2 1.435(4) . ?
C1 C8 1.542(4) . ?
C2 C3 1.362(4) . ?
C2 C7 1.535(4) . ?
C3 C4 1.524(4) . ?
C4 C5 1.526(4) . ?
C4 C18 1.557(5) . ?
C4 C15 1.556(4) . ?
C5 C6 1.503(4) . ?
C6 C7 1.522(4) . ?
C9 C10 1.379(4) . ?
C9 C14 1.392(4) . ?
C10 C11 1.367(5) . ?
C11 C12 1.380(5) . ?
C12 C13 1.383(5) . ?
C13 C14 1.363(5) . ?
C15 C16 1.523(5) . ?
C16 C17 1.497(6) . ?
C17 C18 1.511(5) . ?

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
_geom_angle_publ_flag
O1 Ti1 O1 160.54(12) . 12_565 ?
O1 Ti1 N1 79.38(9) . . ?
O1 Ti1 N1 87.42(9) 12_565 . ?
O1 Ti1 N1 87.42(9) . 12_565 ?
O1 Ti1 N1 79.38(9) 12_565 12_565 ?
N1 Ti1 N1 94.47(13) . 12_565 ?
O1 Ti1 Cl1 95.91(7) . . ?
O1 Ti1 Cl1 97.20(6) 12_565 . ?
N1 Ti1 Cl1 85.37(6) . . ?
N1 Ti1 Cl1 176.58(7) 12_565 . ?
O1 Ti1 Cl1 97.21(6) . 12_565 ?
O1 Ti1 Cl1 95.90(7) 12_565 12_565 ?
N1 Ti1 Cl1 176.58(7) . 12_565 ?
N1 Ti1 Cl1 85.37(6) 12_565 12_565 ?
Cl1 Ti1 Cl1 94.99(5) . 12_565 ?
C3 O1 Ti1 136.2(2) . . ?
C1 N1 C9 119.1(2) . . ?
C1 N1 Ti1 124.7(2) . . ?
C9 N1 Ti1 115.69(18) . . ?
N1 C1 C2 125.2(3) . . ?
N1 C1 C8 118.5(3) . . ?
C2 C1 C8 116.3(3) . . ?
C3 C2 C1 119.9(3) . . ?
C3 C2 C7 119.7(3) . . ?
C1 C2 C7 120.3(3) . . ?
O1 C3 C2 121.1(3) . . ?
O1 C3 C4 113.4(3) . . ?
C2 C3 C4 125.4(3) . . ?
C5 C4 C3 110.3(3) . . ?
C5 C4 C18 111.5(3) . . ?
C3 C4 C18 110.5(3) . . ?
C5 C4 C15 111.3(3) . . ?
C3 C4 C15 108.8(2) . . ?
C18 C4 C15 104.3(3) . . ?
C6 C5 C4 112.1(3) . . ?
C5 C6 C7 109.3(3) . . ?
C6 C7 C2 111.2(3) . . ?
F2 C8 F1 106.8(3) . . ?
F2 C8 F3 105.0(3) . . ?
F1 C8 F3 107.2(3) . . ?
F2 C8 C1 111.4(3) . . ?
F1 C8 C1 112.8(3) . . ?
F3 C8 C1 113.2(3) . . ?
C10 C9 C14 115.4(3) . . ?
C10 C9 N1 121.0(3) . . ?
C14 C9 N1 123.4(3) . . ?
F4 C10 C11 118.5(3) . . ?
F4 C10 C9 118.0(3) . . ?
C11 C10 C9 123.5(3) . . ?
C10 C11 C12 118.7(3) . . ?
C13 C12 C11 120.5(3) . . ?
C14 C13 C12 118.5(3) . . ?
F5 C14 C13 119.4(3) . . ?
F5 C14 C9 117.1(3) . . ?
C13 C14 C9 123.5(3) . . ?
C16 C15 C4 105.6(3) . . ?
C17 C16 C15 104.6(3) . . ?
C16 C17 C18 103.6(3) . . ?
C17 C18 C4 106.2(3) . . ?

_diffrn_measured_fraction_theta_max 0.955
_diffrn_reflns_theta_full        24.63
_diffrn_measured_fraction_theta_full 0.955
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.046
