#------------------------------------------------------------------------------
#$Date: 2019-11-24 06:08:43 +0200 (Sun, 24 Nov 2019) $
#$Revision: 236907 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/08/76/4087664.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4087664
loop_
_publ_author_name
'Nguyen, Trang T.'
'Bertke, Jeffery A.'
'Gray, Danielle L.'
'Hull, Kami L.'
_publ_contact_author
; 
Kami L. Hull 
University of Illinois 
School of Chemical Sciences 
600 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_section_title
;
 Facile C--H, C--F, C--Cl, and C--C Activation by Oxatitanacyclobutene
 Complexes
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4190
_journal_paper_doi               10.1021/acs.organomet.5b00470
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C48 H60 O6 Ti'
_chemical_formula_sum            'C48 H60 O6 Ti'
_chemical_formula_weight         780.86
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
; 
? 
;
_cell_angle_alpha                96.3761(15)
_cell_angle_beta                 90.3364(15)
_cell_angle_gamma                104.8609(16)
_cell_formula_units_Z            2
_cell_length_a                   8.5881(4)
_cell_length_b                   12.7845(6)
_cell_length_c                   19.5964(8)
_cell_measurement_reflns_used    9605
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.39
_cell_measurement_theta_min      2.46
_cell_volume                     2065.42(16)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2014.9-0 (Bruker, 2014)'
_computing_data_reduction
; 
SAINT V8.34A, XPREP v2014/2, SADABS V2014/4, TWINABS V2012/1 
(Bruker, 2012 & 2014) 
;
_computing_molecular_graphics
; 
SHELXTL v2014-4 (Bruker, 2014), CrystalMaker v2.7.7 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'
_computing_structure_refinement  'SHELX-2014-6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELX-2014-4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Bruker D8 Venture/Photon 100'
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  cd46qsa
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0127
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            74631
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.423
_diffrn_reflns_theta_min         2.455
_exptl_absorpt_coefficient_mu    0.256
_exptl_absorpt_correction_T_max  0.99930
_exptl_absorpt_correction_T_min  0.99864
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker, 2014)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             836
_exptl_crystal_id                cd46qsa
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (1 -2 4) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.353
_exptl_crystal_size_mid          0.184
_exptl_crystal_size_min          0.176
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.0491(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     566
_refine_ls_number_reflns         7605
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0452P)²+1.5082P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1020
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7072
_reflns_number_total             7605
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            om5b00470_si_002.cif
_cod_data_source_block           2a
_cod_database_code               4087664
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.915
_shelx_estimated_absorpt_t_max   0.956
_shelxl_version_number           2014/6
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.42643(3) 0.45200(2) 0.77325(2) 0.01919(10) Uani 1 1 d . . . . .
O1 O 0.46603(13) 0.32205(9) 0.80288(5) 0.0214(2) Uani 1 1 d . . . . .
O2 O 0.98025(15) 0.75073(10) 0.88834(6) 0.0306(3) Uani 1 1 d . . . . .
O3 O 0.52599(14) 0.53078(11) 0.70567(6) 0.0282(3) Uani 1 1 d . . . . .
O5 O 0.82780(18) 0.23278(13) 0.49837(7) 0.0457(4) Uani 1 1 d . . . . .
O6 O 0.32137(15) 0.32821(10) 0.68264(6) 0.0309(3) Uani 1 1 d D . . . .
C1 C 0.57916(18) 0.32365(13) 0.85193(8) 0.0192(3) Uani 1 1 d . . . . .
C2 C 0.69032(18) 0.43330(12) 0.86668(7) 0.0180(3) Uani 1 1 d . . . . .
C3 C 0.64474(19) 0.51491(13) 0.83491(8) 0.0196(3) Uani 1 1 d . . . . .
C4 C 0.7469(2) 0.62000(13) 0.84439(8) 0.0221(3) Uani 1 1 d . . . . .
H4A H 0.7184 0.6762 0.8233 0.026 Uiso 1 1 calc R U . . .
C5 C 0.88946(19) 0.64444(13) 0.88394(8) 0.0221(3) Uani 1 1 d . . . . .
C6 C 0.93300(18) 0.56354(13) 0.91546(8) 0.0211(3) Uani 1 1 d . . . . .
H6A H 1.0298 0.5800 0.9428 0.025 Uiso 1 1 calc R U . . .
C7 C 0.83367(18) 0.45865(13) 0.90653(8) 0.0200(3) Uani 1 1 d . . . . .
H7A H 0.8633 0.4030 0.9278 0.024 Uiso 1 1 calc R U . . .
C8 C 0.58995(19) 0.23694(13) 0.88284(8) 0.0222(3) Uani 1 1 d . . . . .
H8A H 0.6725 0.2517 0.9177 0.027 Uiso 1 1 calc R U . . .
C9 C 0.4915(2) 0.11926(13) 0.87095(9) 0.0249(4) Uani 1 1 d . . . . .
C10 C 0.3185(2) 0.09837(13) 0.89410(10) 0.0285(4) Uani 1 1 d . . . . .
C11 C 0.2192(2) 0.04183(14) 0.84138(11) 0.0341(4) Uani 1 1 d . . . . .
C12 C 0.3143(2) 0.02188(14) 0.78145(10) 0.0351(4) Uani 1 1 d . . . . .
C13 C 0.4709(2) 0.07030(14) 0.79596(10) 0.0313(4) Uani 1 1 d . . . . .
C14 C 1.1130(2) 0.78340(14) 0.93662(9) 0.0291(4) Uani 1 1 d . . . . .
H14A H 1.1643 0.8612 0.9362 0.044 Uiso 1 1 calc R U . . .
H14B H 1.1915 0.7414 0.9242 0.044 Uiso 1 1 calc R U . . .
H14C H 1.0748 0.7701 0.9827 0.044 Uiso 1 1 calc R U . . .
C15 C 0.5786(2) 0.05058(14) 0.91018(10) 0.0321(4) Uani 1 1 d . . . . .
H15A H 0.5849 0.0762 0.9594 0.048 Uiso 1 1 calc R U . . .
H15B H 0.6876 0.0584 0.8933 0.048 Uiso 1 1 calc R U . . .
H15C H 0.5182 -0.0262 0.9027 0.048 Uiso 1 1 calc R U . . .
C16 C 0.2799(2) 0.13028(15) 0.96607(10) 0.0358(4) Uani 1 1 d . . . . .
H16A H 0.3363 0.2067 0.9800 0.054 Uiso 1 1 calc R U . . .
H16B H 0.3147 0.0842 0.9966 0.054 Uiso 1 1 calc R U . . .
H16C H 0.1634 0.1210 0.9691 0.054 Uiso 1 1 calc R U . . .
C17 C 0.0377(2) 0.00360(17) 0.84081(14) 0.0478(6) Uani 1 1 d . . . . .
H17A H 0.0041 -0.0760 0.8311 0.072 Uiso 1 1 calc R U . . .
H17B H -0.0082 0.0361 0.8052 0.072 Uiso 1 1 calc R U . . .
H17C H -0.0006 0.0259 0.8857 0.072 Uiso 1 1 calc R U . . .
C18 C 0.2421(3) -0.04658(17) 0.71564(12) 0.0501(6) Uani 1 1 d . . . . .
H18A H 0.1595 -0.0163 0.6968 0.075 Uiso 1 1 calc R U . . .
H18B H 0.1931 -0.1214 0.7250 0.075 Uiso 1 1 calc R U . . .
H18C H 0.3268 -0.0465 0.6824 0.075 Uiso 1 1 calc R U . . .
C19 C 0.6113(3) 0.07639(19) 0.75104(11) 0.0453(5) Uani 1 1 d . . . . .
H19A H 0.6685 0.1529 0.7492 0.068 Uiso 1 1 calc R U . . .
H19B H 0.5734 0.0421 0.7046 0.068 Uiso 1 1 calc R U . . .
H19C H 0.6845 0.0382 0.7697 0.068 Uiso 1 1 calc R U . . .
C20 C 0.6776(2) 0.57304(17) 0.67678(9) 0.0325(4) Uani 1 1 d . . . . .
H20A H 0.7613 0.5906 0.7149 0.039 Uiso 1 1 calc R U . . .
C21 C 0.6780(2) 0.67793(17) 0.64888(9) 0.0331(4) Uani 1 1 d . . . . .
C22 C 0.5624(2) 0.68405(17) 0.60015(10) 0.0356(4) Uani 1 1 d . . . . .
H22A H 0.4821 0.6198 0.5837 0.043 Uiso 1 1 calc R U . . .
C23 C 0.5614(2) 0.77968(18) 0.57547(11) 0.0413(5) Uani 1 1 d . . . . .
H23A H 0.4811 0.7817 0.5425 0.050 Uiso 1 1 calc R U . . .
C24 C 0.6778(3) 0.87311(19) 0.59873(11) 0.0469(5) Uani 1 1 d D . . . .
C25 C 0.7922(3) 0.87147(19) 0.64758(12) 0.0484(6) Uani 1 1 d . . . . .
H25A H 0.8711 0.9365 0.6639 0.058 Uiso 1 1 calc R U . . .
C26 C 0.7919(2) 0.7739(2) 0.67298(10) 0.0435(5) Uani 1 1 d . . . . .
H26A H 0.8702 0.7729 0.7072 0.052 Uiso 1 1 calc R U . . .
C27 C 0.7162(2) 0.48527(17) 0.62547(9) 0.0332(4) Uani 1 1 d . . . . .
C28 C 0.7585(2) 0.50019(18) 0.55825(9) 0.0358(4) Uani 1 1 d . . . . .
H28A H 0.7607 0.5678 0.5420 0.043 Uiso 1 1 calc R U . . .
C29 C 0.7981(2) 0.41807(18) 0.51388(9) 0.0373(5) Uani 1 1 d . . . . .
H29A H 0.8271 0.4300 0.4681 0.045 Uiso 1 1 calc R U . . .
C30 C 0.7948(2) 0.32041(19) 0.53695(9) 0.0372(5) Uani 1 1 d . . . . .
C31 C 0.7519(2) 0.30309(19) 0.60469(10) 0.0394(5) Uani 1 1 d . . . . .
H31A H 0.7488 0.2352 0.6208 0.047 Uiso 1 1 calc R U . . .
C32 C 0.7147(2) 0.38538(19) 0.64743(9) 0.0374(5) Uani 1 1 d . . . . .
H32A H 0.6870 0.3736 0.6933 0.045 Uiso 1 1 calc R U . . .
O4 O 0.685(4) 0.9660(12) 0.5662(11) 0.057(3) Uani 0.5 1 d D U P A 1
C33 C 0.5538(5) 0.9876(4) 0.5271(3) 0.0506(12) Uani 0.5 1 d D . P A 1
H33A H 0.5800 1.0651 0.5207 0.076 Uiso 0.5 1 calc R U P A 1
H33B H 0.4539 0.9688 0.5522 0.076 Uiso 0.5 1 calc R U P A 1
H33C H 0.5395 0.9436 0.4822 0.076 Uiso 0.5 1 calc R U P A 1
O4B O 0.677(3) 0.9744(11) 0.5805(11) 0.056(3) Uani 0.5 1 d D U P A 2
C33B C 0.8378(6) 1.0376(4) 0.5787(3) 0.0572(13) Uani 0.5 1 d D . P A 2
H33D H 0.8424 1.0954 0.5493 0.086 Uiso 0.5 1 calc R U P A 2
H33E H 0.9059 0.9910 0.5603 0.086 Uiso 0.5 1 calc R U P A 2
H33F H 0.8765 1.0703 0.6253 0.086 Uiso 0.5 1 calc R U P A 2
C34 C 0.8784(3) 0.2469(2) 0.42991(10) 0.0471(5) Uani 1 1 d . . . . .
H34A H 0.9059 0.1809 0.4091 0.071 Uiso 1 1 calc R U . . .
H34B H 0.9732 0.3091 0.4310 0.071 Uiso 1 1 calc R U . . .
H34C H 0.7909 0.2603 0.4027 0.071 Uiso 1 1 calc R U . . .
C35 C 0.2735(12) 0.3554(9) 0.6180(5) 0.041(2) Uani 0.516(7) 1 d D U P B 1
H35A H 0.2095 0.4097 0.6261 0.049 Uiso 0.516(7) 1 calc R U P B 1
H35B H 0.3704 0.3881 0.5930 0.049 Uiso 0.516(7) 1 calc R U P B 1
C36 C 0.1798(6) 0.2604(6) 0.5777(3) 0.0364(12) Uani 0.516(7) 1 d D U P B 1
H36A H 0.1870 0.2666 0.5278 0.044 Uiso 0.516(7) 1 calc R U P B 1
H36B H 0.0654 0.2422 0.5904 0.044 Uiso 0.516(7) 1 calc R U P B 1
C37 C 0.2777(7) 0.1711(4) 0.6023(2) 0.0450(12) Uani 0.516(7) 1 d D U P B 1
H37A H 0.2099 0.0952 0.5951 0.054 Uiso 0.516(7) 1 calc R U P B 1
H37B H 0.3802 0.1760 0.5784 0.054 Uiso 0.516(7) 1 calc R U P B 1
C38 C 0.305(2) 0.2124(7) 0.6762(6) 0.033(2) Uani 0.516(7) 1 d D U P B 1
H38A H 0.2136 0.1760 0.7028 0.040 Uiso 0.516(7) 1 calc R U P B 1
H38B H 0.4048 0.1975 0.6940 0.040 Uiso 0.516(7) 1 calc R U P B 1
C35B C 0.3147(11) 0.3554(8) 0.6113(4) 0.0310(17) Uani 0.484(7) 1 d D U P B 2
H35C H 0.2541 0.4111 0.6084 0.037 Uiso 0.484(7) 1 calc R U P B 2
H35D H 0.4246 0.3832 0.5946 0.037 Uiso 0.484(7) 1 calc R U P B 2
C36B C 0.2331(11) 0.2541(7) 0.5720(4) 0.0612(19) Uani 0.484(7) 1 d D U P B 2
H36C H 0.3082 0.2304 0.5393 0.073 Uiso 0.484(7) 1 calc R U P B 2
H36D H 0.1416 0.2648 0.5450 0.073 Uiso 0.484(7) 1 calc R U P B 2
C37B C 0.1719(6) 0.1678(4) 0.6183(2) 0.0412(12) Uani 0.484(7) 1 d D U P B 2
H37C H 0.1811 0.0956 0.5974 0.049 Uiso 0.484(7) 1 calc R U P B 2
H37D H 0.0584 0.1629 0.6300 0.049 Uiso 0.484(7) 1 calc R U P B 2
C38B C 0.285(2) 0.2097(8) 0.6805(7) 0.039(2) Uani 0.484(7) 1 d D U P B 2
H38C H 0.2317 0.1854 0.7228 0.047 Uiso 0.484(7) 1 calc R U P B 2
H38D H 0.3838 0.1841 0.6753 0.047 Uiso 0.484(7) 1 calc R U P B 2
C39 C 0.23372(19) 0.44221(14) 0.86105(8) 0.0226(3) Uani 1 1 d . . . . .
C40 C 0.3386(2) 0.54844(14) 0.87146(8) 0.0234(3) Uani 1 1 d . . . . .
C41 C 0.3176(2) 0.60279(13) 0.81377(9) 0.0241(3) Uani 1 1 d . . . . .
C42 C 0.20123(19) 0.53018(14) 0.76845(8) 0.0243(3) Uani 1 1 d . . . . .
C43 C 0.14906(19) 0.43031(14) 0.79745(8) 0.0232(3) Uani 1 1 d . . . . .
C44 C 0.2150(2) 0.35879(15) 0.91033(9) 0.0313(4) Uani 1 1 d . . . . .
H44A H 0.3189 0.3663 0.9339 0.047 Uiso 1 1 calc R U . . .
H44B H 0.1784 0.2857 0.8851 0.047 Uiso 1 1 calc R U . . .
H44C H 0.1355 0.3697 0.9442 0.047 Uiso 1 1 calc R U . . .
C45 C 0.4318(2) 0.59883(16) 0.93701(9) 0.0326(4) Uani 1 1 d . . . . .
H45A H 0.4930 0.5497 0.9516 0.049 Uiso 1 1 calc R U . . .
H45B H 0.3571 0.6114 0.9727 0.049 Uiso 1 1 calc R U . . .
H45C H 0.5064 0.6684 0.9296 0.049 Uiso 1 1 calc R U . . .
C46 C 0.3980(2) 0.71841(15) 0.80273(11) 0.0347(4) Uani 1 1 d . . . . .
H46A H 0.4817 0.7501 0.8387 0.052 Uiso 1 1 calc R U . . .
H46B H 0.3177 0.7609 0.8045 0.052 Uiso 1 1 calc R U . . .
H46C H 0.4470 0.7196 0.7577 0.052 Uiso 1 1 calc R U . . .
C47 C 0.1381(2) 0.56015(18) 0.70384(10) 0.0363(4) Uani 1 1 d . . . . .
H47A H 0.0675 0.4950 0.6781 0.054 Uiso 1 1 calc R U . . .
H47B H 0.2286 0.5907 0.6756 0.054 Uiso 1 1 calc R U . . .
H47C H 0.0770 0.6143 0.7156 0.054 Uiso 1 1 calc R U . . .
C48 C 0.0192(2) 0.33229(16) 0.76920(10) 0.0325(4) Uani 1 1 d . . . . .
H48A H 0.0130 0.3283 0.7190 0.049 Uiso 1 1 calc R U . . .
H48B H -0.0844 0.3380 0.7878 0.049 Uiso 1 1 calc R U . . .
H48C H 0.0439 0.2664 0.7824 0.049 Uiso 1 1 calc R U . . .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1.00 0.00 0.00 0.0810
-1.00 0.00 0.00 0.1760
0.00 1.00 0.00 0.0840
0.00 -1.00 0.00 0.0870
0.00 0.00 1.00 0.0400
0.00 0.00 -1.00 0.0870
-2.00 2.00 1.00 0.1340
2.00 -2.00 -1.00 0.1170
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
O3 Ti1 O1 128.15(5) . .
O3 Ti1 C3 87.91(6) . .
O1 Ti1 C3 77.52(5) . .
O3 Ti1 O6 82.59(5) . .
O1 Ti1 O6 79.06(4) . .
C3 Ti1 O6 141.01(5) . .
O3 Ti1 C43 123.01(5) . .
O1 Ti1 C43 101.97(5) . .
C3 Ti1 C43 132.95(6) . .
O6 Ti1 C43 82.29(5) . .
O3 Ti1 C39 145.27(6) . .
O1 Ti1 C39 86.54(5) . .
C3 Ti1 C39 99.75(6) . .
O6 Ti1 C39 109.47(6) . .
C43 Ti1 C39 34.46(5) . .
O3 Ti1 C42 91.29(5) . .
O1 Ti1 C42 136.58(6) . .
C3 Ti1 C42 127.40(6) . .
O6 Ti1 C42 90.67(5) . .
C43 Ti1 C42 34.61(6) . .
C39 Ti1 C42 57.18(5) . .
O3 Ti1 C40 118.14(6) . .
O1 Ti1 C40 106.87(5) . .
C3 Ti1 C40 77.54(6) . .
O6 Ti1 C40 139.58(5) . .
C43 Ti1 C40 57.29(6) . .
C39 Ti1 C40 34.43(6) . .
C42 Ti1 C40 57.01(6) . .
O3 Ti1 C41 88.79(6) . .
O1 Ti1 C41 140.82(5) . .
C3 Ti1 C41 93.41(6) . .
O6 Ti1 C41 123.91(5) . .
C43 Ti1 C41 57.16(6) . .
C39 Ti1 C41 57.15(6) . .
C42 Ti1 C41 34.01(6) . .
C40 Ti1 C41 34.45(6) . .
C1 O1 Ti1 123.33(10) . .
C5 O2 C14 117.56(13) . .
C20 O3 Ti1 143.86(11) . .
C30 O5 C34 117.30(18) . .
C35 O6 C38 108.2(6) . .
C38B O6 C35B 108.3(6) . .
C35 O6 Ti1 124.1(4) . .
C38 O6 Ti1 127.4(4) . .
C38B O6 Ti1 126.6(4) . .
C35B O6 Ti1 123.7(4) . .
C8 C1 O1 124.69(14) . .
C8 C1 C2 124.18(14) . .
O1 C1 C2 111.13(13) . .
C7 C2 C3 120.14(14) . .
C7 C2 C1 125.33(14) . .
C3 C2 C1 114.50(13) . .
C4 C3 C2 117.87(14) . .
C4 C3 Ti1 129.81(11) . .
C2 C3 Ti1 112.23(11) . .
C5 C4 C3 121.62(15) . .
C5 C4 H4A 119.2 . .
C3 C4 H4A 119.2 . .
O2 C5 C6 124.09(14) . .
O2 C5 C4 115.80(14) . .
C6 C5 C4 120.12(15) . .
C7 C6 C5 119.20(14) . .
C7 C6 H6A 120.4 . .
C5 C6 H6A 120.4 . .
C6 C7 C2 121.06(14) . .
C6 C7 H7A 119.5 . .
C2 C7 H7A 119.5 . .
C1 C8 C9 130.35(14) . .
C1 C8 H8A 114.8 . .
C9 C8 H8A 114.8 . .
C8 C9 C10 115.40(14) . .
C8 C9 C13 114.58(15) . .
C10 C9 C13 102.77(14) . .
C8 C9 C15 107.80(13) . .
C10 C9 C15 108.26(14) . .
C13 C9 C15 107.64(14) . .
C11 C10 C16 129.43(18) . .
C11 C10 C9 108.63(17) . .
C16 C10 C9 121.74(16) . .
C10 C11 C12 109.77(16) . .
C10 C11 C17 127.2(2) . .
C12 C11 C17 123.03(18) . .
C13 C12 C11 109.58(16) . .
C13 C12 C18 126.8(2) . .
C11 C12 C18 123.54(19) . .
C12 C13 C19 129.26(18) . .
C12 C13 C9 109.02(17) . .
C19 C13 C9 121.68(16) . .
O2 C14 H14A 109.5 . .
O2 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
O2 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C9 C15 H15A 109.5 . .
C9 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C9 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C10 C16 H16A 109.5 . .
C10 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C10 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C11 C17 H17A 109.5 . .
C11 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C11 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C12 C18 H18A 109.5 . .
C12 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C12 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
C13 C19 H19A 109.5 . .
C13 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
C13 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
O3 C20 C21 109.43(14) . .
O3 C20 C27 109.44(15) . .
C21 C20 C27 115.45(15) . .
O3 C20 H20A 107.4 . .
C21 C20 H20A 107.4 . .
C27 C20 H20A 107.4 . .
C26 C21 C22 117.6(2) . .
C26 C21 C20 120.48(18) . .
C22 C21 C20 121.93(17) . .
C23 C22 C21 121.92(19) . .
C23 C22 H22A 119.0 . .
C21 C22 H22A 119.0 . .
C22 C23 C24 119.5(2) . .
C22 C23 H23A 120.2 . .
C24 C23 H23A 120.2 . .
C25 C24 C23 120.6(2) . .
C25 C24 O4B 116.2(12) . .
C23 C24 O4B 122.8(12) . .
C25 C24 O4 121.4(13) . .
C23 C24 O4 117.6(13) . .
C24 C25 C26 119.6(2) . .
C24 C25 H25A 120.2 . .
C26 C25 H25A 120.2 . .
C21 C26 C25 120.7(2) . .
C21 C26 H26A 119.6 . .
C25 C26 H26A 119.6 . .
C32 C27 C28 117.56(18) . .
C32 C27 C20 118.51(16) . .
C28 C27 C20 123.90(19) . .
C27 C28 C29 121.6(2) . .
C27 C28 H28A 119.2 . .
C29 C28 H28A 119.2 . .
C30 C29 C28 119.43(18) . .
C30 C29 H29A 120.3 . .
C28 C29 H29A 120.3 . .
C29 C30 O5 125.19(17) . .
C29 C30 C31 120.09(19) . .
O5 C30 C31 114.7(2) . .
C32 C31 C30 119.4(2) . .
C32 C31 H31A 120.3 . .
C30 C31 H31A 120.3 . .
C31 C32 C27 121.94(18) . .
C31 C32 H32A 119.0 . .
C27 C32 H32A 119.0 . .
C24 O4 C33 126(2) . .
O4 C33 C33 166.3(10) . 2_676
O4 C33 H33A 109.5 . .
C33 C33 H33A 67.1 2_676 .
O4 C33 H33B 109.5 . .
C33 C33 H33B 83.9 2_676 .
H33A C33 H33B 109.5 . .
O4 C33 H33C 109.5 . .
C33 C33 H33C 61.6 2_676 .
H33A C33 H33C 109.5 . .
H33B C33 H33C 109.5 . .
C24 O4B C33B 108.9(16) . .
O4B C33B H33D 109.5 . .
O4B C33B H33E 109.5 . .
H33D C33B H33E 109.5 . .
O4B C33B H33F 109.5 . .
H33D C33B H33F 109.5 . .
H33E C33B H33F 109.5 . .
O5 C34 H34A 109.5 . .
O5 C34 H34B 109.5 . .
H34A C34 H34B 109.5 . .
O5 C34 H34C 109.5 . .
H34A C34 H34C 109.5 . .
H34B C34 H34C 109.5 . .
C36 C35 O6 110.2(7) . .
C36 C35 H35A 109.6 . .
O6 C35 H35A 109.6 . .
C36 C35 H35B 109.6 . .
O6 C35 H35B 109.6 . .
H35A C35 H35B 108.1 . .
C35 C36 C37 97.8(5) . .
C35 C36 H36A 112.2 . .
C37 C36 H36A 112.2 . .
C35 C36 H36B 112.2 . .
C37 C36 H36B 112.2 . .
H36A C36 H36B 109.8 . .
C38 C37 C36 99.2(6) . .
C38 C37 H37A 111.9 . .
C36 C37 H37A 111.9 . .
C38 C37 H37B 111.9 . .
C36 C37 H37B 111.9 . .
H37A C37 H37B 109.6 . .
O6 C38 C37 107.5(6) . .
O6 C38 H38A 110.2 . .
C37 C38 H38A 110.2 . .
O6 C38 H38B 110.2 . .
C37 C38 H38B 110.2 . .
H38A C38 H38B 108.5 . .
C36B C35B O6 104.5(6) . .
C36B C35B H35C 110.9 . .
O6 C35B H35C 110.9 . .
C36B C35B H35D 110.9 . .
O6 C35B H35D 110.9 . .
H35C C35B H35D 108.9 . .
C35B C36B C37B 110.7(6) . .
C35B C36B H36C 109.5 . .
C37B C36B H36C 109.5 . .
C35B C36B H36D 109.5 . .
C37B C36B H36D 109.5 . .
H36C C36B H36D 108.1 . .
C36B C37B C38B 101.4(7) . .
C36B C37B H37C 111.5 . .
C38B C37B H37C 111.5 . .
C36B C37B H37D 111.5 . .
C38B C37B H37D 111.5 . .
H37C C37B H37D 109.3 . .
O6 C38B C37B 104.2(7) . .
O6 C38B H38C 110.9 . .
C37B C38B H38C 110.9 . .
O6 C38B H38D 110.9 . .
C37B C38B H38D 110.9 . .
H38C C38B H38D 108.9 . .
C43 C39 C40 108.30(14) . .
C43 C39 C44 126.53(16) . .
C40 C39 C44 125.16(15) . .
C43 C39 Ti1 72.69(9) . .
C40 C39 Ti1 73.36(9) . .
C44 C39 Ti1 120.86(11) . .
C39 C40 C41 107.73(14) . .
C39 C40 C45 124.89(16) . .
C41 C40 C45 126.61(16) . .
C39 C40 Ti1 72.22(9) . .
C41 C40 Ti1 73.19(9) . .
C45 C40 Ti1 128.04(11) . .
C42 C41 C40 107.97(15) . .
C42 C41 C46 124.61(16) . .
C40 C41 C46 127.38(16) . .
C42 C41 Ti1 72.56(9) . .
C40 C41 Ti1 72.36(9) . .
C46 C41 Ti1 122.70(11) . .
C41 C42 C43 108.28(14) . .
C41 C42 C47 123.89(16) . .
C43 C42 C47 127.68(17) . .
C41 C42 Ti1 73.43(9) . .
C43 C42 Ti1 72.06(9) . .
C47 C42 Ti1 123.94(11) . .
C39 C43 C42 107.72(15) . .
C39 C43 C48 125.25(16) . .
C42 C43 C48 126.88(15) . .
C39 C43 Ti1 72.85(9) . .
C42 C43 Ti1 73.33(9) . .
C48 C43 Ti1 122.95(11) . .
C39 C44 H44A 109.5 . .
C39 C44 H44B 109.5 . .
H44A C44 H44B 109.5 . .
C39 C44 H44C 109.5 . .
H44A C44 H44C 109.5 . .
H44B C44 H44C 109.5 . .
C40 C45 H45A 109.5 . .
C40 C45 H45B 109.5 . .
H45A C45 H45B 109.5 . .
C40 C45 H45C 109.5 . .
H45A C45 H45C 109.5 . .
H45B C45 H45C 109.5 . .
C41 C46 H46A 109.5 . .
C41 C46 H46B 109.5 . .
H46A C46 H46B 109.5 . .
C41 C46 H46C 109.5 . .
H46A C46 H46C 109.5 . .
H46B C46 H46C 109.5 . .
C42 C47 H47A 109.5 . .
C42 C47 H47B 109.5 . .
H47A C47 H47B 109.5 . .
C42 C47 H47C 109.5 . .
H47A C47 H47C 109.5 . .
H47B C47 H47C 109.5 . .
C43 C48 H48A 109.5 . .
C43 C48 H48B 109.5 . .
H48A C48 H48B 109.5 . .
C43 C48 H48C 109.5 . .
H48A C48 H48C 109.5 . .
H48B C48 H48C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 O3 1.8351(12) .
Ti1 O1 1.9273(11) .
Ti1 C3 2.1461(16) .
Ti1 O6 2.2575(12) .
Ti1 C43 2.3832(16) .
Ti1 C39 2.3854(16) .
Ti1 C42 2.3998(15) .
Ti1 C40 2.4002(16) .
Ti1 C41 2.4109(16) .
O1 C1 1.3575(18) .
O2 C5 1.375(2) .
O2 C14 1.423(2) .
O3 C20 1.423(2) .
O5 C30 1.373(2) .
O5 C34 1.429(2) .
O6 C35 1.435(9) .
O6 C38 1.442(9) .
O6 C38B 1.461(10) .
O6 C35B 1.482(9) .
C1 C8 1.344(2) .
C1 C2 1.477(2) .
C2 C7 1.399(2) .
C2 C3 1.407(2) .
C3 C4 1.395(2) .
C4 C5 1.392(2) .
C4 H4A 0.9500 .
C5 C6 1.389(2) .
C6 C7 1.384(2) .
C6 H6A 0.9500 .
C7 H7A 0.9500 .
C8 C9 1.517(2) .
C8 H8A 0.9500 .
C9 C10 1.522(2) .
C9 C13 1.523(2) .
C9 C15 1.549(2) .
C10 C11 1.351(3) .
C10 C16 1.487(3) .
C11 C12 1.471(3) .
C11 C17 1.509(3) .
C12 C13 1.343(3) .
C12 C18 1.508(3) .
C13 C19 1.488(3) .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
C19 H19A 0.9800 .
C19 H19B 0.9800 .
C19 H19C 0.9800 .
C20 C21 1.503(3) .
C20 C27 1.524(3) .
C20 H20A 1.0000 .
C21 C26 1.392(3) .
C21 C22 1.396(3) .
C22 C23 1.366(3) .
C22 H22A 0.9500 .
C23 C24 1.376(3) .
C23 H23A 0.9500 .
C24 C25 1.374(3) .
C24 O4B 1.383(6) .
C24 O4 1.397(6) .
C25 C26 1.392(3) .
C25 H25A 0.9500 .
C26 H26A 0.9500 .
C27 C32 1.389(3) .
C27 C28 1.389(3) .
C28 C29 1.399(3) .
C28 H28A 0.9500 .
C29 C30 1.368(3) .
C29 H29A 0.9500 .
C30 C31 1.406(3) .
C31 C32 1.375(3) .
C31 H31A 0.9500 .
C32 H32A 0.9500 .
O4 C33 1.46(3) .
C33 C33 1.515(8) 2_676
C33 H33A 0.9800 .
C33 H33B 0.9800 .
C33 H33C 0.9800 .
O4B C33B 1.41(3) .
C33B H33D 0.9800 .
C33B H33E 0.9800 .
C33B H33F 0.9800 .
C34 H34A 0.9800 .
C34 H34B 0.9800 .
C34 H34C 0.9800 .
C35 C36 1.423(9) .
C35 H35A 0.9900 .
C35 H35B 0.9900 .
C36 C37 1.689(7) .
C36 H36A 0.9900 .
C36 H36B 0.9900 .
C37 C38 1.481(10) .
C37 H37A 0.9900 .
C37 H37B 0.9900 .
C38 H38A 0.9900 .
C38 H38B 0.9900 .
C35B C36B 1.438(9) .
C35B H35C 0.9900 .
C35B H35D 0.9900 .
C36B C37B 1.500(9) .
C36B H36C 0.9900 .
C36B H36D 0.9900 .
C37B C38B 1.511(11) .
C37B H37C 0.9900 .
C37B H37D 0.9900 .
C38B H38C 0.9900 .
C38B H38D 0.9900 .
C39 C43 1.413(2) .
C39 C40 1.416(2) .
C39 C44 1.496(2) .
C40 C41 1.425(2) .
C40 C45 1.499(2) .
C41 C42 1.407(2) .
C41 C46 1.503(2) .
C42 C43 1.423(2) .
C42 C47 1.500(2) .
C43 C48 1.498(2) .
C44 H44A 0.9800 .
C44 H44B 0.9800 .
C44 H44C 0.9800 .
C45 H45A 0.9800 .
C45 H45B 0.9800 .
C45 H45C 0.9800 .
C46 H46A 0.9800 .
C46 H46B 0.9800 .
C46 H46C 0.9800 .
C47 H47A 0.9800 .
C47 H47B 0.9800 .
C47 H47C 0.9800 .
C48 H48A 0.9800 .
C48 H48B 0.9800 .
C48 H48C 0.9800 .
