# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2002


data_global
#==============================================================================

_audit_creation_date             31-07-01
_audit_creation_method           from_MolEN_and_SHELXL
_audit_update_record             
; ?
;

_journal_coden_Cambridge         182

loop_
_publ_author_name
'Ian Rothwell'
'Philip E. Fanwick'
'Richard A. Himes'

_publ_contact_author_name        'Ian P. Rothwell'
_publ_contact_author_address     
;    
Department of Chemistry
Purdue University
W. Lafayette
IN 47907
USA
;
_publ_contact_author_email       rothwell@purdue.edu
_publ_contact_author_fax         1(765)4940239
_publ_contact_author_phone       1(765)4945203

_publ_requested_journal          'Chemical Communications'
_publ_requested_category         ?
_publ_requested_coeditor_name    ?

_publ_section_title              
; 
Stereoselective tricyclization of a dienyne by titanium aryloxide centers, 
Unprecedented ring expansion via insertion into a titanium-vinyl bond.
;

_publ_section_references         
;

Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C.,
Guagliardi, A., Moliterni, A.G.G, Polidori, G. Spagna R. (1999). 
J. Appl. Cryst., 32, 115-119

Enraf-Nonius (1993), CAD4 Express, Enraf-Nonius, Delft, The Netherlands.

Johnson, C.K. (1976). ORTEP. Report ORNL-5138.  Oak Ridge National Laboratory,
Tennessee, USA.

Nonius(1998), Collect Users Manual, Nonius 'Delft, The Netherlands.

Otwinowski Z. & Minor, W. (1997). Methods Enzymol., 276, 307-327.

Sheldrick, G.M. (1997). SHELXL97, Program for the Refinement of Crystal
Structures. Univ. of Gottingen, Germany.

Spek A.L.(1997) PLATON. Program. Univ. of Ultrecht,
The Netherlands

Spek A.L.(1997) PLUTON. Molecular Graphics Program. Univ. of Ultrecht, 
The Netherlands
;

data_RH150
_database_code_CSD               197519

# 5. CRYSTAL DATA

_chemical_compound_source        ?
_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_chemical_name_systematic        
; ?
;
_exptl_crystal_density_method    ?

_chemical_formula_sum            'C48 H44 O2 Ti1'
_chemical_formula_structural     ?
_chemical_formula_weight         700.78
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   p-1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.9946(4)
_cell_length_b                   11.7706(4)
_cell_length_c                   13.7377(6)
_cell_angle_alpha                73.1412(15)
_cell_angle_beta                 77.5151(14)
_cell_angle_gamma                84.8318(15)
_cell_volume                     1811.51(18)
_cell_measurement_reflns_used    17419
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_formula_units_Z            2
_exptl_crystal_density_diffrn    1.28
_exptl_crystal_density_meas      ?
_diffrn_radiation_type           MO-K\a
_diffrn_radiation_wavelength     0.71073
_exptl_absorpt_coefficient_mu    0.270
_cell_measurement_temperature    149
_exptl_crystal_F_000             740

# 6. DATA COLLECTION

_diffrn_ambient_temperature      149
_diffrn_measurement_device_type  Nonius_KappaCCD
_exptl_absorpt_correction_type   refined_empirical_(Otwinowski_&_Minor,_1996
_exptl_absorpt_correction_T_min  0.6032
_exptl_absorpt_correction_T_max  0.9681
_diffrn_reflns_number            17419
_diffrn_measured_fraction_theta_max 0.9660
_diffrn_reflns_theta_full        23.3
_reflns_number_total             8326
_reflns_number_gt                7158
_reflns_threshold_expression     >2.0\s(I)
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_theta_min         5.00
_diffrn_reflns_theta_max         27.91
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_max       18

# 7. REFINEMENT DATA

_refine_special_details          
;
Refinement on F^2^ for ALL reflections except for   0 with very negative F^2^
or flagged by the user for potential systematic errors.  Weighted R-factors
wR and all goodnesses 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 observed criterion
of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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_R_factor_gt           0.085
_refine_ls_wR_factor_ref         0.179
_refine_ls_hydrogen_treatment    
;
Chemically significant hydrogens refined isotropically
Others riding
;

_refine_ls_number_reflns         8313
_refine_ls_number_parameters     525
_refine_ls_number_restraints     0
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_weighting_scheme      'calc '
_refine_ls_weighting_details     
'1/[\s^2^(Fo^2^)+(0.0586P)^2^+3.9213P] where P=(Fo^2^+2Fc^2^)/3  '

_refine_ls_shift/su_max          0.009
_refine_diff_density_max         0.75
_refine_diff_density_min         -0.63
_refine_ls_extinction_method     none
_atom_type_scat_source           
'International Tables for Crystallography (Vol C)'

# 8. COMPUTING DATA

_computing_data_collection       Collect_(Nonius,_1998)
_computing_cell_refinement       DENZO/SCALEPACK_(Otwinowski,_1996)
_computing_data_reduction        DENZO/SCALEPACK_(Otwinowski,_1996)
_computing_structure_solution    Direct_methods_(SIR97,_Altomare_et_al.,_1997)
_computing_structure_refinement  SHELX97_(Sheldrick,_1997)
_computing_molecular_graphics    
;
ORTEP (Johnson, 1976)
PLUTON (Spek, 1991)
;
_computing_publication_material  CIF_VAX_MolEN_(Fair,_1990)

# 9. ATOMIC COORDINATES AND THERMAL PARAMETERS

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
Ti 0.70179(5) 0.28979(5) 0.69006(5) 0.02316(17) Uani ?
O(3) 0.5768(2) 0.1978(2) 0.74424(17) 0.0285(7) Uani ?
O(4) 0.74186(19) 0.40500(19) 0.56915(17) 0.0237(7) Uani ?
C(11) 0.8429(3) 0.0876(3) 0.8013(3) 0.0340(11) Uani ?
C(12) 0.9108(3) 0.1417(3) 0.8563(3) 0.0294(11) Uani ?
C(13) 1.0274(4) 0.0805(4) 0.8541(3) 0.0368(11) Uani ?
C(14) 1.0326(4) 0.0010(4) 0.7818(4) 0.0443(16) Uani ?
C(15) 0.9116(4) -0.0304(4) 0.7961(4) 0.0487(16) Uani ?
C(16) 0.8393(4) 0.1705(3) 0.6932(3) 0.0346(13) Uani ?
C(21) 0.7527(4) 0.2860(4) 0.9075(3) 0.0410(14) Uani ?
C(22) 0.8737(3) 0.2278(3) 0.9003(3) 0.0311(11) Uani ?
C(23) 0.9399(4) 0.2801(4) 0.9588(3) 0.0446(15) Uani ?
C(25) 0.7489(5) 0.3582(6) 0.9854(5) 0.084(3) Uani ?
C(26) 0.7300(4) 0.3622(3) 0.8031(3) 0.0327(12) Uani ?
C(31) 0.4999(3) 0.1157(3) 0.7521(2) 0.0242(10) Uani ?
C(32) 0.4063(3) 0.0923(3) 0.8354(3) 0.0245(10) Uani ?
C(33) 0.3309(3) 0.0051(3) 0.8422(3) 0.0278(10) Uani ?
C(34) 0.3473(3) -0.0578(3) 0.7684(3) 0.0319(11) Uani ?
C(35) 0.4395(3) -0.0331(3) 0.6861(3) 0.0288(10) Uani ?
C(36) 0.5171(3) 0.0537(3) 0.6761(2) 0.0255(10) Uani ?
C(41) 0.7463(3) 0.5153(3) 0.5017(2) 0.0207(9) Uani ?
C(42) 0.6668(3) 0.6036(3) 0.5259(2) 0.0219(9) Uani ?
C(43) 0.6763(3) 0.7190(3) 0.4590(3) 0.0260(10) Uani ?
C(44) 0.7588(3) 0.7459(3) 0.3690(3) 0.0298(11) Uani ?
C(45) 0.8347(3) 0.6571(3) 0.3453(3) 0.0268(10) Uani ?
C(46) 0.8305(3) 0.5408(3) 0.4101(2) 0.0231(9) Uani ?
C(24A) 0.8642(14) 0.3894(10) 0.9735(8) 0.036(3) Uani ?
C(24B) 0.8552(16) 0.3476(16) 1.0186(13) 0.076(7) Uani ?
C(321) 0.3841(3) 0.1579(3) 0.9162(3) 0.0258(10) Uani ?
C(322) 0.4626(3) 0.1537(3) 0.9777(3) 0.0344(12) Uani ?
C(323) 0.4392(4) 0.2099(4) 1.0559(3) 0.0437(14) Uani ?
C(324) 0.3380(4) 0.2738(4) 1.0723(3) 0.0415(12) Uani ?
C(325) 0.2589(3) 0.2791(4) 1.0114(3) 0.0378(12) Uani ?
C(326) 0.2811(3) 0.2204(3) 0.9345(3) 0.0329(11) Uani ?
C(361) 0.6152(3) 0.0790(3) 0.5868(3) 0.0267(10) Uani ?
C(362) 0.6286(3) 0.1923(3) 0.5170(3) 0.0279(10) Uani ?
C(363) 0.7210(3) 0.2165(3) 0.4346(3) 0.0330(11) Uani ?
C(364) 0.8023(4) 0.1279(4) 0.4215(3) 0.0403(12) Uani ?
C(365) 0.7896(4) 0.0149(4) 0.4891(3) 0.0447(14) Uani ?
C(366) 0.6966(4) -0.0099(3) 0.5709(3) 0.0369(11) Uani ?
C(421) 0.5740(3) 0.5752(3) 0.6194(2) 0.0224(9) Uani ?
C(422) 0.5556(3) 0.6429(3) 0.6902(3) 0.0320(11) Uani ?
C(423) 0.4680(4) 0.6166(4) 0.7764(3) 0.0414(12) Uani ?
C(424) 0.3969(3) 0.5237(3) 0.7938(3) 0.0367(12) Uani ?
C(425) 0.4131(3) 0.4564(3) 0.7237(3) 0.0291(11) Uani ?
C(426) 0.5009(3) 0.4825(3) 0.6378(3) 0.0246(10) Uani ?
C(461) 0.9156(3) 0.4499(3) 0.3810(3) 0.0241(10) Uani ?
C(462) 0.9333(3) 0.4353(3) 0.2818(3) 0.0331(11) Uani ?
C(463) 1.0169(4) 0.3557(4) 0.2516(3) 0.0426(12) Uani ?
C(464) 1.0857(3) 0.2922(4) 0.3191(3) 0.0405(14) Uani ?
C(465) 1.0684(3) 0.3056(3) 0.4179(3) 0.0348(11) Uani ?
C(466) 0.9830(3) 0.3836(3) 0.4494(3) 0.0266(10) Uani ?
H(11) 0.754(4) 0.069(4) 0.842(3) 0.047(12) Uiso ?
H(21) 0.688(5) 0.207(5) 0.938(4) 0.085(18) Uiso ?
H(33) 0.2685 -0.0113 0.8971 0.0330 Uiso calc
H(34) 0.2967 -0.1160 0.7744 0.0380 Uiso calc
H(35) 0.4502 -0.0747 0.6365 0.0350 Uiso calc
H(43) 0.6260 0.7788 0.4754 0.0310 Uiso calc
H(44) 0.7635 0.8227 0.3247 0.0360 Uiso calc
H(45) 0.8900 0.6755 0.2845 0.0320 Uiso calc
H(13A) 1.031(4) 0.031(4) 0.927(4) 0.055(13) Uiso ?
H(13B) 1.099(5) 0.147(5) 0.824(4) 0.087(18) Uiso ?
H(14A) 1.032(3) 0.058(3) 0.695(3) 0.031(10) Uiso ?
H(14B) 1.082(4) -0.069(4) 0.796(3) 0.051(13) Uiso ?
H(15A) 0.888(4) -0.095(5) 0.867(4) 0.063(14) Uiso ?
H(15B) 0.895(4) -0.065(4) 0.734(4) 0.060(14) Uiso ?
H(16A) 0.820(4) 0.137(4) 0.651(4) 0.055(14) Uiso ?
H(16B) 0.919(3) 0.189(3) 0.691(3) 0.029(10) Uiso ?
H(23A) 0.956(5) 0.217(5) 1.018(5) 0.082(18) Uiso ?
H(23B) 1.023(7) 0.318(8) 0.908(7) 0.16(3) Uiso ?
H(24A) 0.8747 0.4095 1.0345 0.0440 Uiso calc
H(24B) 0.8838 0.4573 0.9135 0.0440 Uiso calc
H(24C) 0.8445 0.3067 1.0921 0.0910 Uiso calc
H(24D) 0.8833 0.4259 1.0078 0.0910 Uiso calc
H(25A) 0.7001 0.4287 0.9699 0.1010 Uiso calc
H(25B) 0.7202 0.3108 1.0557 0.1010 Uiso calc
H(26A) 0.802(5) 0.405(5) 0.785(4) 0.082(18) Uiso ?
H(26B) 0.657(4) 0.406(4) 0.810(3) 0.044(12) Uiso ?
H(322) 0.5319 0.1126 0.9665 0.0410 Uiso calc
H(323) 0.4921 0.2046 1.0976 0.0520 Uiso calc
H(324) 0.3232 0.3129 1.1239 0.0500 Uiso calc
H(325) 0.1905 0.3220 1.0219 0.0450 Uiso calc
H(326) 0.2267 0.2229 0.8949 0.0390 Uiso calc
H(362) 0.5747 0.2523 0.5261 0.0330 Uiso calc
H(363) 0.7285 0.2920 0.3882 0.0390 Uiso calc
H(364) 0.8654 0.1445 0.3672 0.0480 Uiso calc
H(365) 0.8438 -0.0447 0.4796 0.0530 Uiso calc
H(366) 0.6882 -0.0863 0.6155 0.0440 Uiso calc
H(422) 0.6025 0.7060 0.6792 0.0380 Uiso calc
H(423) 0.4569 0.6620 0.8232 0.0490 Uiso calc
H(424) 0.3385 0.5064 0.8522 0.0440 Uiso calc
H(425) 0.3652 0.3942 0.7345 0.0350 Uiso calc
H(426) 0.5115 0.4370 0.5911 0.0290 Uiso calc
H(462) 0.8889 0.4791 0.2353 0.0400 Uiso calc
H(463) 1.0266 0.3451 0.1858 0.0510 Uiso calc
H(464) 1.1432 0.2408 0.2980 0.0490 Uiso calc
H(465) 1.1139 0.2625 0.4637 0.0420 Uiso calc
H(466) 0.9711 0.3913 0.5164 0.0320 Uiso calc

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ti 0.0319(3) 0.0182(3) 0.0208(3) -0.0015(2) -0.0062(2) -0.0067(2)
O(3) 0.0370(14) 0.0250(12) 0.0240(12) -0.0098(10) -0.0015(10) -0.0082(10)
O(4) 0.0251(12) 0.0204(11) 0.0248(12) -0.0006(9) -0.0041(9) -0.0055(9)
C(11) 0.031(2) 0.0323(19) 0.036(2) -0.0026(16) -0.0024(16) -0.0081(16)
C(12) 0.0257(18) 0.0332(19) 0.0266(18) 0.0029(14) -0.0055(14) -0.0052(15)
C(13) 0.042(2) 0.039(2) 0.0248(19) 0.0138(18) -0.0084(17) -0.0049(16)
C(14) 0.049(3) 0.035(2) 0.049(3) 0.0154(19) -0.012(2) -0.0150(19)
C(15) 0.061(3) 0.025(2) 0.058(3) -0.0015(19) -0.012(2) -0.008(2)
C(16) 0.049(3) 0.0304(19) 0.0281(19) 0.0053(17) -0.0119(18) -0.0125(16)
C(21) 0.040(2) 0.054(3) 0.032(2) 0.0099(19) -0.0075(17) -0.0197(19)
C(22) 0.0303(19) 0.0338(19) 0.0304(19) 0.0010(15) -0.0092(15) -0.0092(15)
C(23) 0.051(3) 0.058(3) 0.032(2) 0.013(2) -0.019(2) -0.020(2)
C(25) 0.090(4) 0.126(5) 0.070(4) 0.061(4) -0.048(3) -0.075(4)
C(26) 0.038(2) 0.033(2) 0.035(2) 0.0088(17) -0.0145(17) -0.0194(16)
C(31) 0.0331(19) 0.0160(15) 0.0243(16) -0.0034(13) -0.0082(14) -0.0042(12)
C(32) 0.0313(18) 0.0189(15) 0.0238(17) 0.0007(13) -0.0084(14) -0.0049(13)
C(33) 0.0271(18) 0.0260(17) 0.0292(18) -0.0026(14) -0.0082(14) -0.0037(14)
C(34) 0.039(2) 0.0225(17) 0.038(2) -0.0037(15) -0.0150(17) -0.0079(15)
C(35) 0.041(2) 0.0204(16) 0.0280(18) -0.0010(14) -0.0120(15) -0.0074(13)
C(36) 0.038(2) 0.0178(15) 0.0213(16) -0.0005(14) -0.0081(14) -0.0049(12)
C(41) 0.0246(17) 0.0177(15) 0.0223(16) -0.0027(12) -0.0090(13) -0.0055(12)
C(42) 0.0222(16) 0.0214(15) 0.0249(16) -0.0017(12) -0.0083(13) -0.0077(13)
C(43) 0.0253(17) 0.0205(16) 0.0327(18) 0.0016(13) -0.0091(14) -0.0062(14)
C(44) 0.0298(19) 0.0234(17) 0.0321(19) -0.0021(14) -0.0089(15) 0.0009(14)
C(45) 0.0290(18) 0.0250(17) 0.0239(17) -0.0028(14) -0.0052(14) -0.0022(13)
C(46) 0.0233(17) 0.0247(16) 0.0231(16) -0.0008(13) -0.0073(13) -0.0074(13)
C(24A) 0.055(6) 0.034(5) 0.028(5) -0.013(5) -0.007(5) -0.018(4)
C(24B) 0.058(8) 0.096(14) 0.091(12) 0.012(10) -0.006(10) -0.065(10)
C(321) 0.0301(18) 0.0243(16) 0.0218(16) -0.0052(14) -0.0018(14) -0.0056(13)
C(322) 0.035(2) 0.037(2) 0.036(2) 0.0028(16) -0.0108(16) -0.0162(16)
C(323) 0.047(2) 0.052(3) 0.041(2) 0.003(2) -0.0170(19) -0.022(2)
C(324) 0.050(2) 0.046(2) 0.034(2) -0.0087(19) -0.0013(18) -0.0228(18)
C(325) 0.034(2) 0.043(2) 0.038(2) 0.0005(17) 0.0004(17) -0.0197(18)
C(326) 0.0303(19) 0.038(2) 0.0319(19) 0.0011(16) -0.0052(15) -0.0136(16)
C(361) 0.037(2) 0.0233(16) 0.0238(17) -0.0048(14) -0.0083(14) -0.0101(13)
C(362) 0.037(2) 0.0251(17) 0.0254(17) -0.0034(14) -0.0087(15) -0.0102(14)
C(363) 0.046(2) 0.0299(18) 0.0263(18) -0.0102(16) -0.0067(16) -0.0106(15)
C(364) 0.048(2) 0.042(2) 0.035(2) -0.0115(18) 0.0031(18) -0.0221(18)
C(365) 0.053(3) 0.033(2) 0.049(2) 0.0031(18) 0.004(2) -0.0243(19)
C(366) 0.053(2) 0.0207(17) 0.038(2) -0.0011(16) -0.0046(18) -0.0131(15)
C(421) 0.0215(16) 0.0203(15) 0.0262(17) 0.0009(12) -0.0063(13) -0.0072(13)
C(422) 0.035(2) 0.0248(17) 0.040(2) -0.0064(15) -0.0024(16) -0.0168(15)
C(423) 0.049(2) 0.037(2) 0.043(2) -0.0036(18) 0.0029(19) -0.0267(18)
C(424) 0.036(2) 0.041(2) 0.032(2) -0.0045(17) 0.0060(16) -0.0169(17)
C(425) 0.0291(19) 0.0269(17) 0.0326(19) -0.0034(14) -0.0073(15) -0.0086(15)
C(426) 0.0278(18) 0.0245(16) 0.0241(17) -0.0010(13) -0.0072(14) -0.0093(13)
C(461) 0.0234(17) 0.0234(16) 0.0254(17) -0.0029(13) -0.0014(13) -0.0084(13)
C(462) 0.037(2) 0.0339(19) 0.0280(18) -0.0020(16) -0.0038(16) -0.0095(15)
C(463) 0.043(2) 0.049(2) 0.037(2) -0.0045(19) 0.0052(18) -0.0227(19)
C(464) 0.032(2) 0.036(2) 0.055(3) 0.0022(17) 0.0006(19) -0.0225(19)
C(465) 0.032(2) 0.0265(18) 0.048(2) 0.0022(15) -0.0103(17) -0.0129(16)
C(466) 0.0271(18) 0.0227(16) 0.0316(18) -0.0033(13) -0.0059(14) -0.0091(14)

# 10. MOLECULAR GEOMETRY

_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_publ_flag
Ti O(4) 1.815(2) YES
Ti O(3) 1.821(2) YES
Ti C(16) 2.067(4) YES
Ti C(26) 2.073(4) YES
O(3) C(31) 1.361(4) YES
O(4) C(41) 1.357(4) YES
C(11) H(11) 1.10(4) YES
C(11) C(12) 1.510(5) YES
C(11) C(16) 1.529(5) YES
C(11) C(15) 1.561(6) YES
C(12) C(22) 1.322(5) YES
C(12) C(13) 1.513(5) YES
C(13) H(13A) 1.01(5) YES
C(13) H(13B) 1.14(6) YES
C(13) C(14) 1.540(6) YES
C(14) H(14B) 0.97(5) YES
C(14) H(14A) 1.19(4) YES
C(14) C(15) 1.487(6) YES
C(15) H(15A) 1.05(5) YES
C(15) H(15B) 1.10(5) YES
C(16) H(16A) 0.87(5) YES
C(16) H(16B) 0.99(4) YES
C(21) H(21) 1.19(6) YES
C(21) C(26) 1.522(6) YES
C(21) C(25) 1.538(6) YES
C(21) C(22) 1.543(5) YES
C(22) C(23) 1.519(5) YES
C(23) H(23A) 0.97(6) YES
C(23) H(23B) 1.14(9) YES
C(23) C(24B) 1.486(16) YES
C(23) C(24A) 1.543(15) YES
C(24A) C(25) 1.426(16) YES
C(24B) C(25) 1.429(19) YES
C(26) H(26B) 0.97(4) YES
C(26) H(26A) 0.98(6) YES
C(31) C(32) 1.401(5) YES
C(31) C(36) 1.410(4) YES
C(32) C(33) 1.399(5) YES
C(32) C(321) 1.494(4) YES
C(33) C(34) 1.391(5) YES
C(34) C(35) 1.383(5) YES
C(35) C(36) 1.401(5) YES
C(36) C(361) 1.485(5) YES
C(41) C(46) 1.407(4) YES
C(41) C(42) 1.409(4) YES
C(42) C(43) 1.401(4) YES
C(42) C(421) 1.483(4) YES
C(43) C(44) 1.382(5) YES
C(44) C(45) 1.386(5) YES
C(45) C(46) 1.399(5) YES
C(46) C(461) 1.491(4) YES
C(321) C(322) 1.383(5) YES
C(321) C(326) 1.393(5) YES
C(322) C(323) 1.385(5) YES
C(323) C(324) 1.380(6) YES
C(324) C(325) 1.380(6) YES
C(325) C(326) 1.390(5) YES
C(361) C(366) 1.397(5) YES
C(361) C(362) 1.398(5) YES
C(362) C(363) 1.386(5) YES
C(363) C(364) 1.385(6) YES
C(364) C(365) 1.384(6) YES
C(365) C(366) 1.385(6) YES
C(421) C(426) 1.393(4) YES
C(421) C(422) 1.398(4) YES
C(422) C(423) 1.382(5) YES
C(423) C(424) 1.381(5) YES
C(424) C(425) 1.388(5) YES
C(425) C(426) 1.381(5) YES
C(461) C(466) 1.390(5) YES
C(461) C(462) 1.391(5) YES
C(462) C(463) 1.389(5) YES
C(463) C(464) 1.384(6) YES
C(464) C(465) 1.381(6) YES
C(465) C(466) 1.396(5) YES

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
O(4) Ti O(3) 132.30(11) YES
O(4) Ti C(16) 104.48(13) YES
O(3) Ti C(16) 104.73(15) YES
O(4) Ti C(26) 104.51(14) YES
O(3) Ti C(26) 108.11(14) YES
C(16) Ti C(26) 97.41(16) YES
C(31) O(3) Ti 158.3(2) YES
C(41) O(4) Ti 158.0(2) YES
H(11) C(11) C(12) 114(2) YES
H(11) C(11) C(16) 107(2) YES
C(12) C(11) C(16) 110.2(3) YES
H(11) C(11) C(15) 111(2) YES
C(12) C(11) C(15) 102.7(3) YES
C(16) C(11) C(15) 112.0(3) YES
C(22) C(12) C(11) 125.4(3) YES
C(22) C(12) C(13) 125.6(3) YES
C(11) C(12) C(13) 109.0(3) YES
H(13A) C(13) H(13B) 110(4) YES
H(13A) C(13) C(12) 108(3) YES
H(13B) C(13) C(12) 112(3) YES
H(13A) C(13) C(14) 111(3) YES
H(13B) C(13) C(14) 111(3) YES
C(12) C(13) C(14) 104.5(3) YES
H(14B) C(14) H(14A) 120(3) YES
H(14B) C(14) C(15) 112(3) YES
H(14A) C(14) C(15) 90.9(18) YES
H(14B) C(14) C(13) 115(3) YES
H(14A) C(14) C(13) 111.6(18) YES
C(15) C(14) C(13) 103.8(3) YES
H(15A) C(15) H(15B) 108(4) YES
H(15A) C(15) C(14) 110(3) YES
H(15B) C(15) C(14) 114(2) YES
H(15A) C(15) C(11) 109(3) YES
H(15B) C(15) C(11) 112(3) YES
C(14) C(15) C(11) 103.9(3) YES
H(16A) C(16) H(16B) 124(4) YES
H(16A) C(16) C(11) 115(3) YES
H(16B) C(16) C(11) 86(2) YES
H(16A) C(16) Ti 95(3) YES
H(16B) C(16) Ti 126(2) YES
C(11) C(16) Ti 113.7(3) YES
H(21) C(21) C(26) 107(3) YES
H(21) C(21) C(25) 114(3) YES
C(26) C(21) C(25) 112.9(4) YES
H(21) C(21) C(22) 106(3) YES
C(26) C(21) C(22) 113.0(3) YES
C(25) C(21) C(22) 103.2(3) YES
C(12) C(22) C(23) 125.8(3) YES
C(12) C(22) C(21) 125.7(3) YES
C(23) C(22) C(21) 108.4(3) YES
H(23A) C(23) H(23B) 109(5) YES
H(23A) C(23) C(24B) 96(3) YES
H(23B) C(23) C(24B) 123(4) YES
H(23A) C(23) C(22) 108(3) YES
H(23B) C(23) C(22) 112(4) YES
C(24B) C(23) C(22) 106.5(8) YES
H(23A) C(23) C(24A) 121(3) YES
H(23B) C(23) C(24A) 105(4) YES
C(24B) C(23) C(24A) 25.3(7) YES
C(22) C(23) C(24A) 102.0(6) YES
C(25) C(24A) C(23) 106.7(7) YES
C(25) C(24B) C(23) 109.7(11) YES
C(24A) C(25) C(24B) 26.9(7) YES
C(24A) C(25) C(21) 105.1(6) YES
C(24B) C(25) C(21) 110.9(7) YES
H(26B) C(26) H(26A) 119(4) YES
H(26B) C(26) C(21) 112(3) YES
H(26A) C(26) C(21) 94(3) YES
H(26B) C(26) Ti 97(2) YES
H(26A) C(26) Ti 115(3) YES
C(21) C(26) Ti 122.6(3) YES
O(3) C(31) C(32) 120.3(3) YES
O(3) C(31) C(36) 118.9(3) YES
C(32) C(31) C(36) 120.8(3) YES
C(33) C(32) C(31) 118.6(3) YES
C(33) C(32) C(321) 119.2(3) YES
C(31) C(32) C(321) 122.3(3) YES
C(34) C(33) C(32) 121.4(3) YES
C(35) C(34) C(33) 119.5(3) YES
C(34) C(35) C(36) 121.1(3) YES
C(35) C(36) C(31) 118.7(3) YES
C(35) C(36) C(361) 120.0(3) YES
C(31) C(36) C(361) 121.2(3) YES
O(4) C(41) C(46) 120.1(3) YES
O(4) C(41) C(42) 118.9(3) YES
C(46) C(41) C(42) 121.0(3) YES
C(43) C(42) C(41) 118.5(3) YES
C(43) C(42) C(421) 120.5(3) YES
C(41) C(42) C(421) 121.0(3) YES
C(44) C(43) C(42) 121.2(3) YES
C(43) C(44) C(45) 119.3(3) YES
C(44) C(45) C(46) 121.9(3) YES
C(45) C(46) C(41) 118.0(3) YES
C(45) C(46) C(461) 119.3(3) YES
C(41) C(46) C(461) 122.7(3) YES
C(322) C(321) C(326) 118.4(3) YES
C(322) C(321) C(32) 121.1(3) YES
C(326) C(321) C(32) 120.4(3) YES
C(321) C(322) C(323) 120.8(4) YES
C(324) C(323) C(322) 120.5(4) YES
C(323) C(324) C(325) 119.3(3) YES
C(324) C(325) C(326) 120.2(4) YES
C(325) C(326) C(321) 120.7(4) YES
C(366) C(361) C(362) 118.5(3) YES
C(366) C(361) C(36) 120.7(3) YES
C(362) C(361) C(36) 120.8(3) YES
C(363) C(362) C(361) 120.8(3) YES
C(364) C(363) C(362) 119.9(3) YES
C(365) C(364) C(363) 120.0(4) YES
C(364) C(365) C(366) 120.3(4) YES
C(365) C(366) C(361) 120.5(3) YES
C(426) C(421) C(422) 118.1(3) YES
C(426) C(421) C(42) 121.1(3) YES
C(422) C(421) C(42) 120.8(3) YES
C(423) C(422) C(421) 120.4(3) YES
C(424) C(423) C(422) 120.7(3) YES
C(423) C(424) C(425) 119.7(3) YES
C(426) C(425) C(424) 119.5(3) YES
C(425) C(426) C(421) 121.6(3) YES
C(466) C(461) C(462) 118.9(3) YES
C(466) C(461) C(46) 121.1(3) YES
C(462) C(461) C(46) 119.8(3) YES
C(463) C(462) C(461) 120.5(4) YES
C(464) C(463) C(462) 120.4(4) YES
C(465) C(464) C(463) 119.5(3) YES
C(464) C(465) C(466) 120.4(4) YES
C(461) C(466) C(465) 120.3(3) YES