Supplementary Material (ESI) for Dalton Transactions
This journal is © The Royal Society of Chemistry 2004

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Dr Andreas Danopoulos'
_publ_contact_author_address     
;
Department of Chemistry
University of Southampton
Highfield
Southampton
Hampshire
SO17 1BJ
UNITED KINGDOM
;

_publ_contact_author_email       AD1@SOTON.AC.UK

_publ_section_title              
;
Zirconium and titanium amido complexes with
3,3-dimethyl-1,5-diaza-8-oxacyclodecane; facile C-H activation of the
macrocyclic rim
;
_publ_requested_category         fm
loop_
_publ_author_name
'Andreas Danopoulos'
'Robin M. Porter'
'Gillian Reid'
'Lisa R. Titcomb'

data_Zr(N2O)2
_database_code_depnum_ccdc_archive 'CCDC 253241'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H36 N4 O2 Zr'
_chemical_formula_sum            'C18 H36 N4 O2 Zr'
_chemical_formula_weight         431.73

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'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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                   10.2993(18)
_cell_length_b                   11.2657(13)
_cell_length_c                   17.012(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.041(9)
_cell_angle_gamma                90.00
_cell_volume                     1973.9(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    3909
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             912
_exptl_absorpt_coefficient_mu    0.576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8290
_exptl_absorpt_correction_T_max  0.9446
_exptl_absorpt_process_details   'SADABS V2.10 (Sheldrick, G.M., 2003)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11501
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_sigmaI/netI    0.0505
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.00
_diffrn_reflns_theta_max         27.56
_reflns_number_total             4492
_reflns_number_gt                3811
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_solution    'DIRDIF99 (Beurskens, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  
;
PLATON (Spek, 2003)
ENCIFER (Allen, 2004)
;

_refine_special_details          
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0350P)^2^+0.2620P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4492
_refine_ls_number_parameters     231
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0339
_refine_ls_wR_factor_ref         0.0745
_refine_ls_wR_factor_gt          0.0700
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_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
C1 C 0.1065(3) -0.0930(3) 0.32463(19) 0.0241(7) Uani 1 1 d . . .
H1A H 0.0415 -0.1573 0.3201 0.029 Uiso 1 1 calc R . .
H1B H 0.1066 -0.0639 0.3795 0.029 Uiso 1 1 calc R . .
C2 C 0.2426(4) -0.1400(2) 0.30238(15) 0.0214(6) Uani 1 1 d . . .
H2A H 0.3097 -0.0885 0.3264 0.026 Uiso 1 1 calc R . .
H2B H 0.2538 -0.2211 0.3237 0.026 Uiso 1 1 calc R . .
C3 C 0.1854(3) -0.2382(2) 0.18040(17) 0.0172(6) Uani 1 1 d . . .
H3A H 0.1030 -0.2468 0.2098 0.021 Uiso 1 1 calc R . .
H3B H 0.2344 -0.3130 0.1872 0.021 Uiso 1 1 calc R . .
C4 C 0.1516(3) -0.2261(3) 0.09304(19) 0.0176(7) Uani 1 1 d . . .
C5 C 0.0497(3) -0.1283(3) 0.07725(18) 0.0187(7) Uani 1 1 d . . .
H5A H 0.0380 -0.1210 0.0197 0.022 Uiso 1 1 calc R . .
H5B H -0.0343 -0.1546 0.0996 0.022 Uiso 1 1 calc R . .
C6 C -0.0315(3) 0.0433(3) 0.1489(2) 0.0196(8) Uani 1 1 d . . .
H6A H -0.1112 0.0287 0.1178 0.023 Uiso 1 1 calc R . .
H6B H -0.0188 0.1302 0.1529 0.023 Uiso 1 1 calc R . .
C7 C -0.0476(3) -0.0092(3) 0.23116(19) 0.0210(7) Uani 1 1 d . . .
H7A H -0.1165 0.0337 0.2601 0.025 Uiso 1 1 calc R . .
H7B H -0.0723 -0.0940 0.2276 0.025 Uiso 1 1 calc R . .
C8 C 0.2724(3) -0.2083(3) 0.04245(17) 0.0225(8) Uani 1 1 d . . .
H8A H 0.3385 -0.2668 0.0572 0.034 Uiso 1 1 calc R . .
H8B H 0.3067 -0.1281 0.0508 0.034 Uiso 1 1 calc R . .
H8C H 0.2496 -0.2185 -0.0131 0.034 Uiso 1 1 calc R . .
C9 C 0.0871(3) -0.3438(3) 0.06801(19) 0.0226(7) Uani 1 1 d . . .
H9A H 0.0615 -0.3389 0.0126 0.034 Uiso 1 1 calc R . .
H9B H 0.0101 -0.3580 0.1005 0.034 Uiso 1 1 calc R . .
H9C H 0.1488 -0.4092 0.0750 0.034 Uiso 1 1 calc R . .
C10 C 0.4311(3) 0.1551(3) 0.30900(17) 0.0255(8) Uani 1 1 d . . .
H10A H 0.4937 0.2185 0.2953 0.031 Uiso 1 1 calc R . .
H10B H 0.4467 0.1306 0.3641 0.031 Uiso 1 1 calc R . .
C11 C 0.2910(3) 0.2002(3) 0.29910(17) 0.0238(8) Uani 1 1 d . . .
H11A H 0.2313 0.1478 0.3286 0.029 Uiso 1 1 calc R . .
H11B H 0.2840 0.2811 0.3215 0.029 Uiso 1 1 calc R . .
C12 C 0.3212(3) 0.2982(2) 0.17473(18) 0.0185(6) Uani 1 1 d . . .
H12A H 0.4087 0.3061 0.1984 0.022 Uiso 1 1 calc R . .
H12B H 0.2745 0.3735 0.1846 0.022 Uiso 1 1 calc R . .
C13 C 0.3378(3) 0.2843(3) 0.08523(18) 0.0172(7) Uani 1 1 d . . .
C14 C 0.4328(3) 0.1838(3) 0.06279(19) 0.0201(7) Uani 1 1 d . . .
H14A H 0.4331 0.1762 0.0048 0.024 Uiso 1 1 calc R . .
H14B H 0.5212 0.2079 0.0791 0.024 Uiso 1 1 calc R . .
C15 C 0.5209(3) 0.0081(3) 0.1267(2) 0.0216(8) Uani 1 1 d . . .
H15A H 0.5937 0.0184 0.0894 0.026 Uiso 1 1 calc R . .
H15B H 0.5035 -0.0780 0.1319 0.026 Uiso 1 1 calc R . .
C16 C 0.5588(3) 0.0588(3) 0.2065(2) 0.0249(8) Uani 1 1 d . . .
H16A H 0.6301 0.0114 0.2298 0.030 Uiso 1 1 calc R . .
H16B H 0.5891 0.1417 0.2006 0.030 Uiso 1 1 calc R . .
C17 C 0.3986(3) 0.4002(3) 0.05582(19) 0.0235(7) Uani 1 1 d . . .
H17A H 0.4788 0.4160 0.0851 0.035 Uiso 1 1 calc R . .
H17B H 0.3375 0.4658 0.0639 0.035 Uiso 1 1 calc R . .
H17C H 0.4185 0.3931 -0.0003 0.035 Uiso 1 1 calc R . .
C18 C 0.2062(3) 0.2682(3) 0.04437(19) 0.0237(7) Uani 1 1 d . . .
H18A H 0.1484 0.3337 0.0590 0.036 Uiso 1 1 calc R . .
H18B H 0.1674 0.1927 0.0608 0.036 Uiso 1 1 calc R . .
H18C H 0.2186 0.2680 -0.0127 0.036 Uiso 1 1 calc R . .
N1 N 0.2606(3) -0.1424(2) 0.21776(12) 0.0160(5) Uani 1 1 d . . .
N2 N 0.0799(3) -0.0100(2) 0.10913(15) 0.0168(5) Uani 1 1 d . . .
N3 N 0.2523(3) 0.20286(18) 0.21649(11) 0.0171(5) Uani 1 1 d . . .
N4 N 0.4060(3) 0.0674(2) 0.09627(15) 0.0172(6) Uani 1 1 d . . .
O1 O 0.0747(2) 0.0029(2) 0.27129(14) 0.0198(5) Uani 1 1 d . . .
O2 O 0.4463(2) 0.0549(2) 0.25670(14) 0.0217(5) Uani 1 1 d . . .
Zr1 Zr 0.25008(4) 0.03009(2) 0.169713(12) 0.01411(7) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0320(18) 0.0208(16) 0.0194(15) 0.0061(14) 0.0086(15) 0.0051(15)
C2 0.0265(15) 0.0198(13) 0.0178(12) 0.0046(11) -0.0003(19) -0.0018(19)
C3 0.0140(15) 0.0150(14) 0.0226(17) 0.0038(13) 0.0040(14) -0.0003(12)
C4 0.0143(15) 0.0153(15) 0.0231(17) -0.0008(13) 0.0021(13) -0.0025(13)
C5 0.0161(15) 0.0210(16) 0.0192(16) -0.0009(13) -0.0001(13) -0.0029(14)
C6 0.0133(16) 0.0175(16) 0.028(2) 0.0005(14) 0.0020(15) 0.0026(13)
C7 0.0169(17) 0.0162(15) 0.0298(17) -0.0007(14) 0.0091(14) 0.0010(14)
C8 0.025(2) 0.0204(14) 0.0220(14) -0.0019(12) 0.0061(14) -0.0008(15)
C9 0.0214(17) 0.0236(17) 0.0229(16) -0.0027(14) -0.0015(14) 0.0001(15)
C10 0.0354(19) 0.0229(17) 0.0182(16) -0.0002(13) -0.0044(14) -0.0029(16)
C11 0.033(2) 0.0199(15) 0.0189(14) -0.0035(13) 0.0046(13) -0.0062(14)
C12 0.0193(16) 0.0147(14) 0.0215(15) -0.0018(13) 0.0052(15) -0.0010(12)
C13 0.0184(16) 0.0174(15) 0.0158(15) 0.0032(13) 0.0036(13) -0.0019(13)
C14 0.0201(16) 0.0178(16) 0.0225(16) 0.0030(13) 0.0047(14) -0.0008(13)
C15 0.0135(18) 0.0213(16) 0.030(2) 0.0024(16) 0.0017(15) -0.0011(15)
C16 0.0129(16) 0.0272(18) 0.0347(19) 0.0047(16) -0.0015(15) 0.0013(15)
C17 0.0251(18) 0.0182(17) 0.0273(17) 0.0038(14) -0.0004(14) -0.0053(15)
C18 0.0225(17) 0.0251(17) 0.0235(16) 0.0048(14) -0.0010(14) -0.0024(14)
N1 0.0172(13) 0.0157(10) 0.0151(10) 0.0020(9) -0.0004(14) -0.0012(14)
N2 0.0142(14) 0.0161(13) 0.0201(13) -0.0009(11) -0.0009(11) -0.0024(12)
N3 0.0194(11) 0.0168(11) 0.0153(10) -0.0009(8) -0.0020(17) -0.0034(16)
N4 0.0146(14) 0.0180(14) 0.0188(14) -0.0004(11) 0.0031(11) -0.0008(12)
O1 0.0183(12) 0.0184(10) 0.0228(12) 0.0022(10) 0.0037(10) 0.0002(10)
O2 0.0215(13) 0.0217(11) 0.0218(12) -0.0012(10) -0.0025(10) -0.0024(10)
Zr1 0.01303(12) 0.01431(12) 0.01500(11) 0.00097(11) 0.0018(4) -0.00118(13)

_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
C1 O1 1.449(4) . ?
C1 C2 1.545(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N1 1.452(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N1 1.472(4) . ?
C3 C4 1.532(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C8 1.527(4) . ?
C4 C9 1.542(4) . ?
C4 C5 1.545(4) . ?
C5 N2 1.472(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 N2 1.462(4) . ?
C6 C7 1.528(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 O1 1.439(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 O2 1.446(4) . ?
C10 C11 1.538(4) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 N3 1.461(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 N3 1.471(4) . ?
C12 C13 1.540(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C17 1.533(4) . ?
C13 C18 1.534(4) . ?
C13 C14 1.544(4) . ?
C14 N4 1.456(4) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 N4 1.454(4) . ?
C15 C16 1.524(5) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 O2 1.441(4) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
N1 Zr1 2.111(2) . ?
N2 Zr1 2.082(3) . ?
N3 Zr1 2.103(2) . ?
N4 Zr1 2.078(3) . ?
O1 Zr1 2.519(2) . ?
O2 Zr1 2.519(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
O1 C1 C2 107.9(2) . . ?
O1 C1 H1A 110.1 . . ?
C2 C1 H1A 110.1 . . ?
O1 C1 H1B 110.1 . . ?
C2 C1 H1B 110.1 . . ?
H1A C1 H1B 108.4 . . ?
N1 C2 C1 111.5(3) . . ?
N1 C2 H2A 109.3 . . ?
C1 C2 H2A 109.3 . . ?
N1 C2 H2B 109.3 . . ?
C1 C2 H2B 109.3 . . ?
H2A C2 H2B 108.0 . . ?
N1 C3 C4 118.2(2) . . ?
N1 C3 H3A 107.8 . . ?
C4 C3 H3A 107.8 . . ?
N1 C3 H3B 107.8 . . ?
C4 C3 H3B 107.8 . . ?
H3A C3 H3B 107.1 . . ?
C8 C4 C3 112.0(2) . . ?
C8 C4 C9 108.0(2) . . ?
C3 C4 C9 106.8(2) . . ?
C8 C4 C5 111.2(2) . . ?
C3 C4 C5 112.7(2) . . ?
C9 C4 C5 105.8(2) . . ?
N2 C5 C4 116.0(3) . . ?
N2 C5 H5A 108.3 . . ?
C4 C5 H5A 108.3 . . ?
N2 C5 H5B 108.3 . . ?
C4 C5 H5B 108.3 . . ?
H5A C5 H5B 107.4 . . ?
N2 C6 C7 110.5(3) . . ?
N2 C6 H6A 109.6 . . ?
C7 C6 H6A 109.6 . . ?
N2 C6 H6B 109.6 . . ?
C7 C6 H6B 109.6 . . ?
H6A C6 H6B 108.1 . . ?
O1 C7 C6 107.6(3) . . ?
O1 C7 H7A 110.2 . . ?
C6 C7 H7A 110.2 . . ?
O1 C7 H7B 110.2 . . ?
C6 C7 H7B 110.2 . . ?
H7A C7 H7B 108.5 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O2 C10 C11 107.0(2) . . ?
O2 C10 H10A 110.3 . . ?
C11 C10 H10A 110.3 . . ?
O2 C10 H10B 110.3 . . ?
C11 C10 H10B 110.3 . . ?
H10A C10 H10B 108.6 . . ?
N3 C11 C10 111.6(3) . . ?
N3 C11 H11A 109.3 . . ?
C10 C11 H11A 109.3 . . ?
N3 C11 H11B 109.3 . . ?
C10 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
N3 C12 C13 117.2(2) . . ?
N3 C12 H12A 108.0 . . ?
C13 C12 H12A 108.0 . . ?
N3 C12 H12B 108.0 . . ?
C13 C12 H12B 108.0 . . ?
H12A C12 H12B 107.2 . . ?
C17 C13 C18 108.3(3) . . ?
C17 C13 C12 106.4(2) . . ?
C18 C13 C12 111.2(3) . . ?
C17 C13 C14 106.6(2) . . ?
C18 C13 C14 111.2(2) . . ?
C12 C13 C14 112.9(3) . . ?
N4 C14 C13 116.3(2) . . ?
N4 C14 H14A 108.2 . . ?
C13 C14 H14A 108.2 . . ?
N4 C14 H14B 108.2 . . ?
C13 C14 H14B 108.2 . . ?
H14A C14 H14B 107.4 . . ?
N4 C15 C16 110.7(3) . . ?
N4 C15 H15A 109.5 . . ?
C16 C15 H15A 109.5 . . ?
N4 C15 H15B 109.5 . . ?
C16 C15 H15B 109.5 . . ?
H15A C15 H15B 108.1 . . ?
O2 C16 C15 108.1(3) . . ?
O2 C16 H16A 110.1 . . ?
C15 C16 H16A 110.1 . . ?
O2 C16 H16B 110.1 . . ?
C15 C16 H16B 110.1 . . ?
H16A C16 H16B 108.4 . . ?
C13 C17 H17A 109.5 . . ?
C13 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C13 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C13 C18 H18A 109.5 . . ?
C13 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C13 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C2 N1 C3 112.0(3) . . ?
C2 N1 Zr1 111.09(17) . . ?
C3 N1 Zr1 118.72(19) . . ?
C6 N2 C5 112.1(3) . . ?
C6 N2 Zr1 110.0(2) . . ?
C5 N2 Zr1 123.8(2) . . ?
C11 N3 C12 110.4(3) . . ?
C11 N3 Zr1 110.36(17) . . ?
C12 N3 Zr1 119.87(18) . . ?
C15 N4 C14 113.5(3) . . ?
C15 N4 Zr1 108.8(2) . . ?
C14 N4 Zr1 124.3(2) . . ?
C7 O1 C1 115.1(2) . . ?
C7 O1 Zr1 108.30(17) . . ?
C1 O1 Zr1 111.00(17) . . ?
C16 O2 C10 115.3(3) . . ?
C16 O2 Zr1 107.51(18) . . ?
C10 O2 Zr1 111.17(18) . . ?
N4 Zr1 N2 113.37(10) . . ?
N4 Zr1 N3 91.85(11) . . ?
N2 Zr1 N3 113.40(12) . . ?
N4 Zr1 N1 112.30(11) . . ?
N2 Zr1 N1 92.00(11) . . ?
N3 Zr1 N1 134.83(8) . . ?
N4 Zr1 O1 172.57(9) . . ?
N2 Zr1 O1 73.12(9) . . ?
N3 Zr1 O1 81.97(9) . . ?
N1 Zr1 O1 70.08(9) . . ?
N4 Zr1 O2 73.20(9) . . ?
N2 Zr1 O2 171.62(9) . . ?
N3 Zr1 O2 70.52(10) . . ?
N1 Zr1 O2 80.43(9) . . ?
O1 Zr1 O2 100.70(7) . . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 N1 -38.8(3) . . . . ?
N1 C3 C4 C8 55.8(3) . . . . ?
N1 C3 C4 C9 173.8(3) . . . . ?
N1 C3 C4 C5 -70.4(4) . . . . ?
C8 C4 C5 N2 -73.2(3) . . . . ?
C3 C4 C5 N2 53.5(3) . . . . ?
C9 C4 C5 N2 169.8(3) . . . . ?
N2 C6 C7 O1 53.2(3) . . . . ?
O2 C10 C11 N3 -42.7(3) . . . . ?
N3 C12 C13 C17 174.0(3) . . . . ?
N3 C12 C13 C18 56.4(4) . . . . ?
N3 C12 C13 C14 -69.4(4) . . . . ?
C17 C13 C14 N4 170.1(3) . . . . ?
C18 C13 C14 N4 -72.1(3) . . . . ?
C12 C13 C14 N4 53.7(4) . . . . ?
N4 C15 C16 O2 52.6(4) . . . . ?
C1 C2 N1 C3 -72.6(3) . . . . ?
C1 C2 N1 Zr1 62.7(3) . . . . ?
C4 C3 N1 C2 157.4(3) . . . . ?
C4 C3 N1 Zr1 25.8(4) . . . . ?
C7 C6 N2 C5 78.8(3) . . . . ?
C7 C6 N2 Zr1 -63.2(3) . . . . ?
C4 C5 N2 C6 -134.2(3) . . . . ?
C4 C5 N2 Zr1 1.6(4) . . . . ?
C10 C11 N3 C12 -70.8(3) . . . . ?
C10 C11 N3 Zr1 64.0(3) . . . . ?
C13 C12 N3 C11 155.6(3) . . . . ?
C13 C12 N3 Zr1 25.7(4) . . . . ?
C16 C15 N4 C14 78.0(3) . . . . ?
C16 C15 N4 Zr1 -64.9(3) . . . . ?
C13 C14 N4 C15 -135.6(3) . . . . ?
C13 C14 N4 Zr1 0.6(4) . . . . ?
C6 C7 O1 C1 -145.3(3) . . . . ?
C6 C7 O1 Zr1 -20.4(3) . . . . ?
C2 C1 O1 C7 126.7(3) . . . . ?
C2 C1 O1 Zr1 3.3(3) . . . . ?
C15 C16 O2 C10 -142.4(3) . . . . ?
C15 C16 O2 Zr1 -17.7(3) . . . . ?
C11 C10 O2 C16 129.9(3) . . . . ?
C11 C10 O2 Zr1 7.2(3) . . . . ?
C15 N4 Zr1 N2 -136.8(2) . . . . ?
C14 N4 Zr1 N2 85.3(3) . . . . ?
C15 N4 Zr1 N3 106.7(2) . . . . ?
C14 N4 Zr1 N3 -31.2(3) . . . . ?
C15 N4 Zr1 N1 -34.2(2) . . . . ?
C14 N4 Zr1 N1 -172.1(2) . . . . ?
C15 N4 Zr1 O2 37.7(2) . . . . ?
C14 N4 Zr1 O2 -100.2(3) . . . . ?
C6 N2 Zr1 N4 -140.60(18) . . . . ?
C5 N2 Zr1 N4 82.8(3) . . . . ?
C6 N2 Zr1 N3 -37.6(2) . . . . ?
C5 N2 Zr1 N3 -174.2(2) . . . . ?
C6 N2 Zr1 N1 104.0(2) . . . . ?
C5 N2 Zr1 N1 -32.6(2) . . . . ?
C6 N2 Zr1 O1 35.54(19) . . . . ?
C5 N2 Zr1 O1 -101.1(2) . . . . ?
C11 N3 Zr1 N4 -112.6(2) . . . . ?
C12 N3 Zr1 N4 17.3(3) . . . . ?
C11 N3 Zr1 N2 130.8(2) . . . . ?
C12 N3 Zr1 N2 -99.3(3) . . . . ?
C11 N3 Zr1 N1 11.9(4) . . . . ?
C12 N3 Zr1 N1 141.8(2) . . . . ?
C11 N3 Zr1 O1 63.2(2) . . . . ?
C12 N3 Zr1 O1 -166.9(3) . . . . ?
C11 N3 Zr1 O2 -41.2(2) . . . . ?
C12 N3 Zr1 O2 88.7(3) . . . . ?
C2 N1 Zr1 N4 130.0(3) . . . . ?
C3 N1 Zr1 N4 -98.0(2) . . . . ?
C2 N1 Zr1 N2 -113.7(3) . . . . ?
C3 N1 Zr1 N2 18.3(2) . . . . ?
C2 N1 Zr1 N3 12.8(4) . . . . ?
C3 N1 Zr1 N3 144.8(2) . . . . ?
C2 N1 Zr1 O1 -42.4(3) . . . . ?
C3 N1 Zr1 O1 89.5(2) . . . . ?
C2 N1 Zr1 O2 62.7(3) . . . . ?
C3 N1 Zr1 O2 -165.3(2) . . . . ?
C7 O1 Zr1 N2 -7.57(18) . . . . ?
C1 O1 Zr1 N2 119.7(2) . . . . ?
C7 O1 Zr1 N3 109.93(19) . . . . ?
C1 O1 Zr1 N3 -122.8(2) . . . . ?
C7 O1 Zr1 N1 -106.1(2) . . . . ?
C1 O1 Zr1 N1 21.1(2) . . . . ?
C7 O1 Zr1 O2 178.25(17) . . . . ?
C1 O1 Zr1 O2 -54.5(2) . . . . ?
C16 O2 Zr1 N4 -10.48(19) . . . . ?
C10 O2 Zr1 N4 116.6(2) . . . . ?
C16 O2 Zr1 N3 -108.7(2) . . . . ?
C10 O2 Zr1 N3 18.45(18) . . . . ?
C16 O2 Zr1 N1 106.4(2) . . . . ?
C10 O2 Zr1 N1 -126.4(2) . . . . ?
C16 O2 Zr1 O1 173.90(18) . . . . ?
C10 O2 Zr1 O1 -59.0(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.087

#==END

data_[Ti(N2O)*(Benzyl)]2
_database_code_depnum_ccdc_archive 'CCDC 253242'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H48 N4 O2 Ti2'
_chemical_formula_sum            'C32 H48 N4 O2 Ti2'
_chemical_formula_weight         616.54

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c
_symmetry_space_group_name_Hall  '-P 2ybc'

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                   9.0291(5)
_cell_length_b                   10.7445(6)
_cell_length_c                   15.7401(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.12(1)
_cell_angle_gamma                90.00
_cell_volume                     1526.99(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    5955
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             656
_exptl_absorpt_coefficient_mu    0.558
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6906
_exptl_absorpt_correction_T_max  0.9515
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
;
Bruker-Nonius 95mm CCD camera on \k-goniostat
;
_diffrn_measurement_method       '\f & \w scans'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7242
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_av_sigmaI/netI    0.0896
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.95
_diffrn_reflns_theta_max         27.48
_reflns_number_total             3345
_reflns_number_gt                2387
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_cell_refinement       
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'
_computing_data_reduction        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'
_computing_structure_solution    'DIRDIF99 (Beurskens, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  
;
PLATON (Spek, 2003)
ENCIFER (Allen, 2004)
;

_refine_special_details          
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0368P)^2^+1.2563P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3345
_refine_ls_number_parameters     183
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0531
_refine_ls_wR_factor_ref         0.1214
_refine_ls_wR_factor_gt          0.1079
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_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
C1 C 0.2094(3) 0.0348(3) -0.13668(17) 0.0192(6) Uani 1 1 d . . .
H1A H 0.2124 -0.0572 -0.1400 0.023 Uiso 1 1 calc R . .
H1B H 0.2763 0.0682 -0.1809 0.023 Uiso 1 1 calc R . .
C2 C 0.0523(3) 0.0794(3) -0.15383(16) 0.0162(6) Uani 1 1 d . . .
H2A H 0.0528 0.1698 -0.1660 0.019 Uiso 1 1 calc R . .
H2B H 0.0113 0.0357 -0.2040 0.019 Uiso 1 1 calc R . .
C3 C -0.1282(3) 0.1517(3) -0.03866(16) 0.0167(6) Uani 1 1 d . . .
H3 H -0.2156 0.1200 -0.0063 0.020 Uiso 1 1 calc R . .
C4 C -0.1493(3) 0.2844(3) -0.07371(17) 0.0186(6) Uani 1 1 d . . .
C5 C 0.0018(3) 0.3519(3) -0.08283(17) 0.0189(6) Uani 1 1 d . . .
H5A H 0.0272 0.3595 -0.1438 0.023 Uiso 1 1 calc R . .
H5B H -0.0057 0.4367 -0.0588 0.023 Uiso 1 1 calc R . .
C6 C 0.2652(3) 0.2977(3) -0.07608(18) 0.0217(7) Uani 1 1 d . . .
H6A H 0.3133 0.3738 -0.0537 0.026 Uiso 1 1 calc R . .
H6B H 0.2570 0.3054 -0.1386 0.026 Uiso 1 1 calc R . .
C7 C 0.3567(3) 0.1835(3) -0.05299(18) 0.0210(7) Uani 1 1 d . . .
H7A H 0.4373 0.1722 -0.0948 0.025 Uiso 1 1 calc R . .
H7B H 0.4018 0.1948 0.0039 0.025 Uiso 1 1 calc R . .
C8 C -0.2349(3) 0.2827(3) -0.15908(17) 0.0214(7) Uani 1 1 d . . .
H8A H -0.1783 0.2355 -0.2012 0.032 Uiso 1 1 calc R . .
H8B H -0.2489 0.3682 -0.1792 0.032 Uiso 1 1 calc R . .
H8C H -0.3317 0.2434 -0.1508 0.032 Uiso 1 1 calc R . .
C9 C -0.2463(3) 0.3529(3) -0.00808(18) 0.0218(7) Uani 1 1 d . . .
H9A H -0.3410 0.3093 -0.0020 0.033 Uiso 1 1 calc R . .
H9B H -0.2644 0.4383 -0.0274 0.033 Uiso 1 1 calc R . .
H9C H -0.1952 0.3548 0.0469 0.033 Uiso 1 1 calc R . .
C10 C 0.0308(3) 0.2196(3) 0.15033(16) 0.0174(6) Uani 1 1 d . . .
H10A H -0.0196 0.3012 0.1464 0.021 Uiso 1 1 calc R . .
H10B H -0.0191 0.1645 0.1918 0.021 Uiso 1 1 calc R . .
C11 C 0.1916(3) 0.2284(3) 0.16226(16) 0.0179(6) Uani 1 1 d . . .
C12 C 0.2693(3) 0.3394(3) 0.14550(17) 0.0230(7) Uani 1 1 d . . .
H12 H 0.2147 0.4115 0.1299 0.028 Uiso 1 1 calc R . .
C13 C 0.4215(4) 0.3474(3) 0.15091(18) 0.0275(8) Uani 1 1 d . . .
H13 H 0.4696 0.4245 0.1404 0.033 Uiso 1 1 calc R . .
C14 C 0.5051(4) 0.2422(4) 0.17182(19) 0.0302(8) Uani 1 1 d . . .
H14 H 0.6100 0.2468 0.1750 0.036 Uiso 1 1 calc R . .
C15 C 0.4324(3) 0.1312(4) 0.18776(18) 0.0295(8) Uani 1 1 d . . .
H15 H 0.4880 0.0593 0.2025 0.035 Uiso 1 1 calc R . .
C16 C 0.2792(3) 0.1237(3) 0.18250(17) 0.0228(7) Uani 1 1 d . . .
H16 H 0.2320 0.0462 0.1928 0.027 Uiso 1 1 calc R . .
N1 N -0.0410(2) 0.0539(2) -0.07846(13) 0.0152(5) Uani 1 1 d . . .
N2 N 0.1185(3) 0.2830(2) -0.03868(14) 0.0170(5) Uani 1 1 d . . .
O1 O 0.2617(2) 0.07465(19) -0.05275(11) 0.0178(4) Uani 1 1 d . . .
Ti1 Ti 0.07256(6) 0.13109(5) 0.02598(3) 0.01457(15) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0224(16) 0.0246(18) 0.0106(13) -0.0029(11) 0.0029(11) -0.0022(14)
C2 0.0190(15) 0.0208(16) 0.0089(12) -0.0005(11) 0.0010(11) -0.0027(13)
C3 0.0164(14) 0.0220(17) 0.0118(13) -0.0011(11) 0.0006(11) -0.0013(13)
C4 0.0234(16) 0.0177(17) 0.0146(14) 0.0016(11) -0.0008(11) 0.0018(13)
C5 0.0200(15) 0.0212(17) 0.0154(13) 0.0031(12) 0.0017(11) -0.0010(13)
C6 0.0214(16) 0.0274(19) 0.0162(14) 0.0009(12) 0.0032(12) -0.0097(14)
C7 0.0171(15) 0.0269(18) 0.0190(15) -0.0014(12) 0.0023(12) -0.0063(14)
C8 0.0205(16) 0.0243(18) 0.0194(15) 0.0038(12) -0.0006(12) 0.0002(14)
C9 0.0247(17) 0.0208(18) 0.0198(15) 0.0015(12) 0.0038(12) 0.0024(14)
C10 0.0206(16) 0.0195(16) 0.0121(13) -0.0020(11) 0.0017(11) 0.0023(13)
C11 0.0241(16) 0.0222(17) 0.0075(12) -0.0040(11) 0.0017(11) -0.0007(13)
C12 0.0276(17) 0.0281(19) 0.0135(14) -0.0009(12) -0.0011(12) -0.0012(14)
C13 0.0311(18) 0.034(2) 0.0179(15) -0.0025(13) -0.0015(13) -0.0100(16)
C14 0.0187(17) 0.052(2) 0.0196(15) -0.0023(15) -0.0043(13) -0.0019(16)
C15 0.0244(17) 0.043(2) 0.0213(15) 0.0008(15) -0.0018(13) 0.0095(17)
C16 0.0255(17) 0.0283(19) 0.0145(14) -0.0011(12) -0.0005(12) 0.0021(15)
N1 0.0161(12) 0.0211(14) 0.0082(10) 0.0001(9) 0.0006(9) -0.0010(11)
N2 0.0167(13) 0.0199(14) 0.0142(11) 0.0014(10) 0.0015(9) -0.0021(11)
O1 0.0177(10) 0.0234(12) 0.0122(9) 0.0005(8) 0.0018(8) -0.0030(9)
Ti1 0.0161(3) 0.0184(3) 0.0092(2) 0.0001(2) 0.00162(18) -0.0009(2)

_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
C1 O1 1.466(3) . ?
C1 C2 1.521(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N1 1.482(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N1 1.456(4) . ?
C3 C4 1.540(4) . ?
C3 Ti1 2.089(3) . ?
C3 H3 1.0000 . ?
C4 C9 1.543(4) . ?
C4 C8 1.549(4) . ?
C4 C5 1.552(4) . ?
C5 N2 1.463(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 N2 1.459(4) . ?
C6 C7 1.523(4) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 O1 1.450(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.467(4) . ?
C10 Ti1 2.209(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.409(4) . ?
C11 C16 1.410(4) . ?
C11 Ti1 2.616(3) . ?
C12 C13 1.380(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.398(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.385(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.388(4) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
N1 Ti1 2.106(2) . ?
N1 Ti1 2.171(2) 3 ?
N2 Ti1 1.968(2) . ?
O1 Ti1 2.1975(19) . ?
Ti1 N1 2.171(2) 3 ?
Ti1 Ti1 3.2118(10) 3 ?

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 C1 C2 111.5(2) . . ?
O1 C1 H1A 109.3 . . ?
C2 C1 H1A 109.3 . . ?
O1 C1 H1B 109.3 . . ?
C2 C1 H1B 109.3 . . ?
H1A C1 H1B 108.0 . . ?
N1 C2 C1 109.3(2) . . ?
N1 C2 H2A 109.8 . . ?
C1 C2 H2A 109.8 . . ?
N1 C2 H2B 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.3 . . ?
N1 C3 C4 125.5(2) . . ?
N1 C3 Ti1 70.32(14) . . ?
C4 C3 Ti1 112.31(19) . . ?
N1 C3 H3 113.6 . . ?
C4 C3 H3 113.6 . . ?
Ti1 C3 H3 113.6 . . ?
C3 C4 C9 105.8(2) . . ?
C3 C4 C8 111.2(2) . . ?
C9 C4 C8 107.7(2) . . ?
C3 C4 C5 110.9(2) . . ?
C9 C4 C5 109.8(2) . . ?
C8 C4 C5 111.2(2) . . ?
N2 C5 C4 110.7(2) . . ?
N2 C5 H5A 109.5 . . ?
C4 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
N2 C6 C7 108.0(2) . . ?
N2 C6 H6A 110.1 . . ?
C7 C6 H6A 110.1 . . ?
N2 C6 H6B 110.1 . . ?
C7 C6 H6B 110.1 . . ?
H6A C6 H6B 108.4 . . ?
O1 C7 C6 109.3(2) . . ?
O1 C7 H7A 109.8 . . ?
C6 C7 H7A 109.8 . . ?
O1 C7 H7B 109.8 . . ?
C6 C7 H7B 109.8 . . ?
H7A C7 H7B 108.3 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 Ti1 88.30(16) . . ?
C11 C10 H10A 113.9 . . ?
Ti1 C10 H10A 113.9 . . ?
C11 C10 H10B 113.9 . . ?
Ti1 C10 H10B 113.9 . . ?
H10A C10 H10B 111.1 . . ?
C12 C11 C16 116.0(3) . . ?
C12 C11 C10 121.6(3) . . ?
C16 C11 C10 122.1(3) . . ?
C12 C11 Ti1 112.88(18) . . ?
C16 C11 Ti1 95.49(18) . . ?
C10 C11 Ti1 57.60(14) . . ?
C13 C12 C11 122.5(3) . . ?
C13 C12 H12 118.7 . . ?
C11 C12 H12 118.7 . . ?
C12 C13 C14 120.1(3) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C15 C14 C13 118.9(3) . . ?
C15 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?
C14 C15 C16 120.8(3) . . ?
C14 C15 H15 119.6 . . ?
C16 C15 H15 119.6 . . ?
C15 C16 C11 121.7(3) . . ?
C15 C16 H16 119.2 . . ?
C11 C16 H16 119.2 . . ?
C3 N1 C2 121.3(2) . . ?
C3 N1 Ti1 69.05(14) . . ?
C2 N1 Ti1 105.99(16) . . ?
C3 N1 Ti1 115.20(17) . 3 ?
C2 N1 Ti1 123.32(18) . 3 ?
Ti1 N1 Ti1 97.34(9) . 3 ?
C6 N2 C5 114.0(2) . . ?
C6 N2 Ti1 119.42(19) . . ?
C5 N2 Ti1 120.85(18) . . ?
C7 O1 C1 115.0(2) . . ?
C7 O1 Ti1 103.83(16) . . ?
C1 O1 Ti1 109.85(15) . . ?
N2 Ti1 C3 81.01(11) . . ?
N2 Ti1 N1 91.48(9) . . ?
C3 Ti1 N1 40.62(10) . . ?
N2 Ti1 N1 169.66(9) . 3 ?
C3 Ti1 N1 99.68(10) . 3 ?
N1 Ti1 N1 82.66(9) . 3 ?
N2 Ti1 O1 76.83(9) . . ?
C3 Ti1 O1 115.43(9) . . ?
N1 Ti1 O1 80.14(8) . . ?
N1 Ti1 O1 93.71(8) 3 . ?
N2 Ti1 C10 97.92(11) . . ?
C3 Ti1 C10 103.66(11) . . ?
N1 Ti1 C10 141.02(10) . . ?
N1 Ti1 C10 91.96(10) 3 . ?
O1 Ti1 C10 138.83(9) . . ?
N2 Ti1 C11 90.33(9) . . ?
C3 Ti1 C11 135.39(10) . . ?
N1 Ti1 C11 175.09(9) . . ?
N1 Ti1 C11 96.20(9) 3 . ?
O1 Ti1 C11 104.72(8) . . ?
C10 Ti1 C11 34.11(9) . . ?
N2 Ti1 Ti1 133.00(7) . 3 ?
C3 Ti1 Ti1 67.42(8) . 3 ?
N1 Ti1 Ti1 42.10(6) . 3 ?
N1 Ti1 Ti1 40.56(6) 3 3 ?
O1 Ti1 Ti1 86.07(6) . 3 ?
C10 Ti1 Ti1 122.19(8) . 3 ?
C11 Ti1 Ti1 136.57(7) . 3 ?

_diffrn_measured_fraction_theta_max 0.958
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.958
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.084

#==END