# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
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# 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 
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data_1ti_a1b2_c5_a_sq
_database_code_depnum_ccdc_archive 'CCDC 1483652'
_audit_update_record             
;
2016-06-06 deposited with the CCDC.
2016-10-17 downloaded from the CCDC.
;
_audit_creation_date             2016-05-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C64 H56 N4 O18 Ti4, 2(C2 H3 N)'
_chemical_formula_sum            'C68 H62 N6 O18 Ti4'
_chemical_formula_weight         1442.83
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 '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 0.0080 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0130 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.3060 0.5280 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.0501(4)
_cell_length_b                   12.0820(4)
_cell_length_c                   23.2457(8)
_cell_angle_alpha                85.061(2)
_cell_angle_beta                 89.175(2)
_cell_angle_gamma                86.151(2)
_cell_volume                     3364.0(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9611
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.59
_cell_measurement_theta_min      2.53
_shelx_estimated_absorpt_T_max   0.993
_shelx_estimated_absorpt_T_min   0.936
_exptl_absorpt_coefficient_mu    0.670
_exptl_absorpt_correction_T_max  0.8624
_exptl_absorpt_correction_T_min  0.7781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0637 before and 0.0473 after correction.
The Ratio of minimum to maximum transmission is 0.9022.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0673
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            57801
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         33.668
_diffrn_reflns_theta_min         2.154
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'φ and ω shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_source                   'Advanced Light Source station 11.3.1'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                14514
_reflns_number_total             20585
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'Bruker APEX2 Bruker-AXS, Madison WI'
_computing_cell_refinement       'SAINT V8.34A Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.34A Bruker-AXS, Madison WI'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     867
_refine_ls_number_reflns         20585
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0518
_refine_ls_restrained_S_all      1.027
_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)+(0.0460P)²+2.2600P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1185
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C34(H34A,H34B), C50(H50A,H50B), C42(H42A,H42B), C10(H10A,H10B),
 C26(H26A,H26B), C35(H35A,H35B), C3(H3A,H3B), C18(H18A,H18B), C58(H58A,H58B),
 C51(H51A,H51B), C19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C45(H45), C46(H46), C44(H44), C47(H47), C24(H24), C23(H23), C12(H12),
 C31(H31), C5(H5), C14(H14), C7(H7), C30(H30), C56(H56), C21(H21), C6(H6),
 C53(H53), C22(H22), C28(H28), C13(H13), C15(H15), C55(H55), C29(H29), C40(H40),
  C63(H63), C54(H54), C37(H37), C39(H39), C38(H38), C60(H60), C62(H62), C61(H61)
2.c Idealised Me refined as rotating group:
 C1AA(H1AA,H1AB,H1AC), C1BA(H1BA,H1BB,H1BC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Ti3 Ti 0.62358(3) 0.41245(3) 0.69230(2) 0.01517(8) Uani 1 1 d . . . . .
Ti1 Ti 0.46051(3) 0.07057(3) 0.83658(2) 0.01446(8) Uani 1 1 d . . . . .
Ti2 Ti 0.29308(3) 0.31128(3) 0.85167(2) 0.01404(8) Uani 1 1 d . . . . .
Ti4 Ti 0.41114(3) 0.30045(3) 0.62172(2) 0.01801(9) Uani 1 1 d . . . . .
O10 O 0.59996(12) 0.27427(11) 0.74484(6) 0.0154(3) Uani 1 1 d . . . . .
O1 O 0.42907(12) 0.12078(12) 0.75317(6) 0.0161(3) Uani 1 1 d . . . . .
O6 O 0.42113(12) 0.37219(11) 0.80583(6) 0.0151(3) Uani 1 1 d . . . . .
O7 O 0.49171(12) 0.48840(12) 0.73785(7) 0.0177(3) Uani 1 1 d . . . . .
O9 O 0.35529(13) 0.36772(12) 0.91490(6) 0.0175(3) Uani 1 1 d . . . . .
O13 O 0.75530(12) 0.33959(12) 0.66769(7) 0.0181(3) Uani 1 1 d . . . . .
O8 O 0.15042(12) 0.30315(12) 0.87993(7) 0.0166(3) Uani 1 1 d . . . . .
O15 O 0.33968(12) 0.32679(12) 0.69855(6) 0.0173(3) Uani 1 1 d . . . . .
O4 O 0.37168(12) -0.04789(12) 0.82634(7) 0.0185(3) Uani 1 1 d . . . . .
O11 O 0.58051(12) 0.18943(12) 0.83280(6) 0.0162(3) Uani 1 1 d . . . . .
O5 O 0.35528(12) 0.16948(12) 0.86238(7) 0.0171(3) Uani 1 1 d . . . . .
O3 O 0.53401(12) 0.00432(12) 0.90025(7) 0.0179(3) Uani 1 1 d . . . . .
O16 O 0.22726(12) 0.28205(12) 0.77224(6) 0.0173(3) Uani 1 1 d . . . . .
O14 O 0.53276(13) 0.37578(13) 0.63735(7) 0.0193(3) Uani 1 1 d . . . . .
O2 O 0.48464(12) 0.15295(12) 0.66203(7) 0.0185(3) Uani 1 1 d . . . . .
O12 O 0.65935(12) 0.55597(12) 0.66940(7) 0.0190(3) Uani 1 1 d . . . . .
O18 O 0.31893(13) 0.42182(13) 0.59312(7) 0.0220(3) Uani 1 1 d . . . . .
O17 O 0.43870(13) 0.23849(14) 0.55393(7) 0.0234(3) Uani 1 1 d . . . . .
N2 N 0.24258(14) 0.49962(14) 0.82526(8) 0.0155(3) Uani 1 1 d . . . . .
N1 N 0.59556(14) -0.02232(14) 0.78405(8) 0.0152(3) Uani 1 1 d . . . . .
N3 N 0.72223(15) 0.42980(14) 0.77591(8) 0.0153(3) Uani 1 1 d . . . . .
N4 N 0.25439(15) 0.20085(15) 0.62590(8) 0.0181(4) Uani 1 1 d . . . . .
C33 C 0.61351(16) 0.26690(17) 0.79885(9) 0.0147(4) Uani 1 1 d . . . . .
C1 C 0.49770(17) 0.10835(17) 0.71221(10) 0.0161(4) Uani 1 1 d . . . . .
C17 C 0.41476(17) 0.45937(16) 0.77150(9) 0.0154(4) Uani 1 1 d . . . . .
C9 C 0.62855(18) -0.05890(17) 0.91413(10) 0.0179(4) Uani 1 1 d . . . . .
C32 C 0.42284(18) 0.45236(17) 0.91616(9) 0.0168(4) Uani 1 1 d . . . . .
C11 C 0.45647(19) -0.14784(17) 0.75214(10) 0.0193(4) Uani 1 1 d . . . . .
C49 C 0.26345(18) 0.27165(17) 0.72186(9) 0.0167(4) Uani 1 1 d . . . . .
C4 C 0.71203(18) -0.07669(17) 0.87234(10) 0.0177(4) Uani 1 1 d . . . . .
C2 C 0.60143(17) 0.03513(17) 0.72522(9) 0.0162(4) Uani 1 1 d . . . . .
H2A H 0.6108 -0.0208 0.6965 0.019 Uiso 1 1 calc R . . . .
H2B H 0.6668 0.0808 0.7222 0.019 Uiso 1 1 calc R . . . .
C16 C 0.36067(19) -0.10194(17) 0.77859(10) 0.0185(4) Uani 1 1 d . . . . .
C34 C 0.67255(18) 0.35841(17) 0.82306(9) 0.0173(4) Uani 1 1 d . . . . .
H34A H 0.6191 0.4041 0.8453 0.021 Uiso 1 1 calc R . . . .
H34B H 0.7317 0.3254 0.8496 0.021 Uiso 1 1 calc R . . . .
C57 C 0.40329(18) 0.15880(19) 0.52217(10) 0.0203(4) Uani 1 1 d . . . . .
C8 C 0.64245(19) -0.10545(18) 0.97069(10) 0.0207(5) Uani 1 1 d . . . . .
H8 H 0.5852 -0.0940 0.9985 0.025 Uiso 1 1 calc R . . . .
C50 C 0.21403(19) 0.18836(19) 0.68648(10) 0.0208(5) Uani 1 1 d . . . . .
H50A H 0.2348 0.1120 0.7035 0.025 Uiso 1 1 calc R . . . .
H50B H 0.1319 0.1996 0.6873 0.025 Uiso 1 1 calc R . . . .
C45 C 0.96225(19) 0.10046(18) 0.75615(11) 0.0227(5) Uani 1 1 d . . . . .
H45 H 1.0078 0.0444 0.7773 0.027 Uiso 1 1 calc R . . . .
C25 C 0.06665(17) 0.37451(17) 0.89537(9) 0.0160(4) Uani 1 1 d . . . . .
C46 C 0.92468(19) 0.08270(18) 0.70206(11) 0.0225(5) Uani 1 1 d . . . . .
H46 H 0.9468 0.0153 0.6856 0.027 Uiso 1 1 calc R . . . .
C43 C 0.86539(17) 0.28156(17) 0.74954(9) 0.0164(4) Uani 1 1 d . . . . .
C42 C 0.84313(17) 0.39530(17) 0.76996(10) 0.0162(4) Uani 1 1 d . . . . .
H42A H 0.8791 0.3972 0.8078 0.019 Uiso 1 1 calc R . . . .
H42B H 0.8779 0.4501 0.7424 0.019 Uiso 1 1 calc R . . . .
C44 C 0.93330(18) 0.20036(18) 0.77964(10) 0.0190(4) Uani 1 1 d . . . . .
H44 H 0.9603 0.2130 0.8166 0.023 Uiso 1 1 calc R . . . .
C48 C 0.82382(17) 0.26148(17) 0.69591(10) 0.0167(4) Uani 1 1 d . . . . .
C10 C 0.56681(18) -0.14014(17) 0.78016(10) 0.0181(4) Uani 1 1 d . . . . .
H10A H 0.5653 -0.1786 0.8195 0.022 Uiso 1 1 calc R . . . .
H10B H 0.6255 -0.1791 0.7577 0.022 Uiso 1 1 calc R . . . .
C26 C 0.26856(18) 0.57381(17) 0.87088(10) 0.0187(4) Uani 1 1 d . . . . .
H26A H 0.2541 0.6522 0.8553 0.022 Uiso 1 1 calc R . . . .
H26B H 0.2174 0.5601 0.9040 0.022 Uiso 1 1 calc R . . . .
C41 C 0.72467(18) 0.63206(17) 0.68703(11) 0.0197(5) Uani 1 1 d . . . . .
C47 C 0.85507(18) 0.16201(17) 0.67150(10) 0.0189(4) Uani 1 1 d . . . . .
H47 H 0.8289 0.1491 0.6345 0.023 Uiso 1 1 calc R . . . .
C36 C 0.75971(18) 0.62722(17) 0.74422(10) 0.0187(4) Uani 1 1 d . . . . .
C35 C 0.71316(18) 0.54836(17) 0.79043(10) 0.0183(4) Uani 1 1 d . . . . .
H35A H 0.7531 0.5538 0.8269 0.022 Uiso 1 1 calc R . . . .
H35B H 0.6339 0.5713 0.7969 0.022 Uiso 1 1 calc R . . . .
C24 C -0.00522(17) 0.34000(18) 0.93984(10) 0.0177(4) Uani 1 1 d . . . . .
H24 H 0.0023 0.2658 0.9573 0.021 Uiso 1 1 calc R . . . .
C23 C -0.08739(18) 0.41419(19) 0.95846(11) 0.0226(5) Uani 1 1 d . . . . .
H23 H -0.1376 0.3902 0.9881 0.027 Uiso 1 1 calc R . . . .
C12 C 0.4463(2) -0.19881(18) 0.70157(10) 0.0222(5) Uani 1 1 d . . . . .
H12 H 0.5110 -0.2299 0.6836 0.027 Uiso 1 1 calc R . . . .
C52 C 0.32252(19) 0.0880(2) 0.54400(10) 0.0213(5) Uani 1 1 d . . . . .
C20 C 0.05320(17) 0.48205(18) 0.86740(10) 0.0176(4) Uani 1 1 d . . . . .
C64 C 0.2133(2) 0.45265(19) 0.60686(10) 0.0228(5) Uani 1 1 d . . . . .
C3 C 0.70648(17) -0.02335(17) 0.81186(10) 0.0172(4) Uani 1 1 d . . . . .
H3A H 0.7276 0.0544 0.8120 0.021 Uiso 1 1 calc R . . . .
H3B H 0.7621 -0.0631 0.7880 0.021 Uiso 1 1 calc R . . . .
C31 C 0.52748(19) 0.4360(2) 0.94022(10) 0.0215(5) Uani 1 1 d . . . . .
H31 H 0.5531 0.3641 0.9565 0.026 Uiso 1 1 calc R . . . .
C18 C 0.30673(18) 0.53005(17) 0.77195(10) 0.0177(4) Uani 1 1 d . . . . .
H18A H 0.3223 0.6097 0.7702 0.021 Uiso 1 1 calc R . . . .
H18B H 0.2625 0.5185 0.7377 0.021 Uiso 1 1 calc R . . . .
C5 C 0.80820(19) -0.13941(18) 0.88984(10) 0.0202(4) Uani 1 1 d . . . . .
H5 H 0.8658 -0.1519 0.8623 0.024 Uiso 1 1 calc R . . . .
C14 C 0.2486(2) -0.16201(19) 0.70400(11) 0.0268(5) Uani 1 1 d . . . . .
H14 H 0.1775 -0.1673 0.6877 0.032 Uiso 1 1 calc R . . . .
C7 C 0.7390(2) -0.16826(19) 0.98662(11) 0.0231(5) Uani 1 1 d . . . . .
H7 H 0.7479 -0.2004 1.0252 0.028 Uiso 1 1 calc R . . . .
C58 C 0.16628(19) 0.26081(19) 0.58825(11) 0.0231(5) Uani 1 1 d . . . . .
H58A H 0.1939 0.2669 0.5479 0.028 Uiso 1 1 calc R . . . .
H58B H 0.1000 0.2164 0.5897 0.028 Uiso 1 1 calc R . . . .
C30 C 0.59502(19) 0.5242(2) 0.94063(10) 0.0242(5) Uani 1 1 d . . . . .
H30 H 0.6665 0.5127 0.9577 0.029 Uiso 1 1 calc R . . . .
C56 C 0.4500(2) 0.1485(2) 0.46785(10) 0.0242(5) Uani 1 1 d . . . . .
H56 H 0.5043 0.1975 0.4535 0.029 Uiso 1 1 calc R . . . .
C21 C -0.02702(18) 0.55577(19) 0.88915(11) 0.0212(5) Uani 1 1 d . . . . .
H21 H -0.0339 0.6306 0.8727 0.025 Uiso 1 1 calc R . . . .
C6 C 0.8225(2) -0.18412(19) 0.94612(11) 0.0241(5) Uani 1 1 d . . . . .
H6 H 0.8897 -0.2258 0.9570 0.029 Uiso 1 1 calc R . . . .
C53 C 0.2903(2) 0.0085(2) 0.50918(11) 0.0275(5) Uani 1 1 d . . . . .
H53 H 0.2346 -0.0396 0.5228 0.033 Uiso 1 1 calc R . . . .
C59 C 0.1326(2) 0.3747(2) 0.60539(11) 0.0241(5) Uani 1 1 d . . . . .
C22 C -0.09729(19) 0.52286(19) 0.93434(11) 0.0245(5) Uani 1 1 d . . . . .
H22 H -0.1516 0.5746 0.9485 0.029 Uiso 1 1 calc R . . . .
C28 C 0.45469(19) 0.64528(19) 0.89223(10) 0.0219(5) Uani 1 1 d . . . . .
H28 H 0.4301 0.7171 0.8755 0.026 Uiso 1 1 calc R . . . .
C13 C 0.3429(2) -0.20529(19) 0.67662(11) 0.0260(5) Uani 1 1 d . . . . .
H13 H 0.3369 -0.2388 0.6414 0.031 Uiso 1 1 calc R . . . .
C51 C 0.27825(19) 0.08795(19) 0.60485(10) 0.0210(5) Uani 1 1 d . . . . .
H51A H 0.2089 0.0483 0.6074 0.025 Uiso 1 1 calc R . . . .
H51B H 0.3329 0.0454 0.6310 0.025 Uiso 1 1 calc R . . . .
C15 C 0.25695(19) -0.11120(18) 0.75487(11) 0.0226(5) Uani 1 1 d . . . . .
H15 H 0.1917 -0.0827 0.7735 0.027 Uiso 1 1 calc R . . . .
C55 C 0.4175(2) 0.0672(2) 0.43472(11) 0.0282(5) Uani 1 1 d . . . . .
H55 H 0.4505 0.0595 0.3978 0.034 Uiso 1 1 calc R . . . .
C29 C 0.55968(19) 0.6289(2) 0.91651(10) 0.0248(5) Uani 1 1 d . . . . .
H29 H 0.6067 0.6889 0.9165 0.030 Uiso 1 1 calc R . . . .
C27 C 0.38502(18) 0.55824(17) 0.89200(9) 0.0175(4) Uani 1 1 d . . . . .
C19 C 0.12076(17) 0.51444(18) 0.81459(10) 0.0183(4) Uani 1 1 d . . . . .
H19A H 0.1020 0.4686 0.7832 0.022 Uiso 1 1 calc R . . . .
H19B H 0.1009 0.5934 0.8015 0.022 Uiso 1 1 calc R . . . .
C40 C 0.7582(2) 0.71654(19) 0.64653(12) 0.0271(5) Uani 1 1 d . . . . .
H40 H 0.7315 0.7215 0.6081 0.032 Uiso 1 1 calc R . . . .
C63 C 0.1838(2) 0.5599(2) 0.62123(12) 0.0320(6) Uani 1 1 d . . . . .
H63 H 0.2388 0.6124 0.6225 0.038 Uiso 1 1 calc R . . . .
C54 C 0.3375(2) -0.0028(2) 0.45497(11) 0.0315(6) Uani 1 1 d . . . . .
H54 H 0.3147 -0.0584 0.4320 0.038 Uiso 1 1 calc R . . . .
C37 C 0.83480(19) 0.70293(18) 0.75854(12) 0.0241(5) Uani 1 1 d . . . . .
H37 H 0.8618 0.6989 0.7969 0.029 Uiso 1 1 calc R . . . .
C39 C 0.8301(2) 0.7925(2) 0.66284(14) 0.0349(7) Uani 1 1 d . . . . .
H39 H 0.8514 0.8509 0.6357 0.042 Uiso 1 1 calc R . . . .
C38 C 0.8711(2) 0.78391(19) 0.71819(13) 0.0315(6) Uani 1 1 d . . . . .
H38 H 0.9240 0.8333 0.7286 0.038 Uiso 1 1 calc R . . . .
C60 C 0.0224(2) 0.4072(2) 0.61812(12) 0.0333(6) Uani 1 1 d . . . . .
H60 H -0.0331 0.3551 0.6172 0.040 Uiso 1 1 calc R . . . .
C62 C 0.0734(3) 0.5901(2) 0.63374(13) 0.0414(7) Uani 1 1 d . . . . .
H62 H 0.0531 0.6635 0.6436 0.050 Uiso 1 1 calc R . . . .
C2AA C 0.1039(2) -0.0914(2) 0.89558(14) 0.0361(6) Uani 1 1 d . . . . .
C61 C -0.0070(2) 0.5140(2) 0.63197(14) 0.0423(8) Uani 1 1 d . . . . .
H61 H -0.0825 0.5353 0.6403 0.051 Uiso 1 1 calc R . . . .
C1AA C 0.1097(3) 0.0244(2) 0.90709(15) 0.0458(8) Uani 1 1 d . . . . .
H1AA H 0.1649 0.0590 0.8813 0.069 Uiso 1 1 calc GR . . . .
H1AB H 0.1313 0.0283 0.9473 0.069 Uiso 1 1 calc GR . . . .
H1AC H 0.0367 0.0639 0.9005 0.069 Uiso 1 1 calc GR . . . .
N1AA N 0.0991(2) -0.1805(2) 0.88598(16) 0.0649(10) Uani 1 1 d . . . . .
N1BA N 0.8355(3) 0.1307(3) 0.93649(16) 0.0680(10) Uani 1 1 d . . . . .
C2BA C 0.7619(3) 0.1424(2) 0.96709(16) 0.0442(8) Uani 1 1 d . . . . .
C1BA C 0.6679(3) 0.1592(3) 1.00504(17) 0.0517(9) Uani 1 1 d . . . . .
H1BA H 0.5990 0.1606 0.9831 0.078 Uiso 1 1 calc GR . . . .
H1BB H 0.6720 0.2302 1.0221 0.078 Uiso 1 1 calc GR . . . .
H1BC H 0.6688 0.0984 1.0358 0.078 Uiso 1 1 calc GR . . . .


_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
Ti3 O10 2.0156(14) . ?
Ti3 O7 2.1003(15) . ?
Ti3 O13 1.8694(15) . ?
Ti3 O14 1.7969(16) . ?
Ti3 O12 1.8468(15) . ?
Ti3 N3 2.3247(19) . ?
Ti1 O1 2.0146(16) . ?
Ti1 O4 1.8768(15) . ?
Ti1 O11 2.1011(15) . ?
Ti1 O5 1.8149(15) . ?
Ti1 O3 1.8314(16) . ?
Ti1 N1 2.3091(17) . ?
Ti2 O6 2.0070(14) . ?
Ti2 O9 1.8601(16) . ?
Ti2 O8 1.8373(15) . ?
Ti2 O5 1.8217(15) . ?
Ti2 O16 2.0868(16) . ?
Ti2 N2 2.3473(17) . ?
Ti4 O15 2.0123(15) . ?
Ti4 O14 1.8329(16) . ?
Ti4 O2 2.0887(16) . ?
Ti4 O18 1.8605(17) . ?
Ti4 O17 1.8188(16) . ?
Ti4 N4 2.3033(18) . ?
O10 C33 1.263(3) . ?
O1 C1 1.264(2) . ?
O6 C17 1.264(2) . ?
O7 C17 1.253(2) . ?
O9 C32 1.352(2) . ?
O13 C48 1.344(3) . ?
O8 C25 1.348(2) . ?
O15 C49 1.260(2) . ?
O4 C16 1.348(3) . ?
O11 C33 1.253(2) . ?
O3 C9 1.355(3) . ?
O16 C49 1.257(3) . ?
O2 C1 1.250(3) . ?
O12 C41 1.343(3) . ?
O18 C64 1.344(3) . ?
O17 C57 1.357(3) . ?
N2 C26 1.496(3) . ?
N2 C18 1.483(3) . ?
N2 C19 1.489(3) . ?
N1 C2 1.482(3) . ?
N1 C10 1.498(3) . ?
N1 C3 1.492(3) . ?
N3 C34 1.480(3) . ?
N3 C42 1.496(3) . ?
N3 C35 1.496(3) . ?
N4 C50 1.482(3) . ?
N4 C58 1.494(3) . ?
N4 C51 1.497(3) . ?
C33 C34 1.506(3) . ?
C1 C2 1.501(3) . ?
C17 C18 1.509(3) . ?
C9 C4 1.407(3) . ?
C9 C8 1.393(3) . ?
C32 C31 1.382(3) . ?
C32 C27 1.402(3) . ?
C11 C16 1.404(3) . ?
C11 C10 1.501(3) . ?
C11 C12 1.384(3) . ?
C49 C50 1.510(3) . ?
C4 C3 1.496(3) . ?
C4 C5 1.388(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C16 C15 1.389(3) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C57 C52 1.400(3) . ?
C57 C56 1.387(3) . ?
C8 H8 0.9500 . ?
C8 C7 1.382(3) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C45 H45 0.9500 . ?
C45 C46 1.381(4) . ?
C45 C44 1.388(3) . ?
C25 C24 1.393(3) . ?
C25 C20 1.402(3) . ?
C46 H46 0.9500 . ?
C46 C47 1.385(3) . ?
C43 C42 1.498(3) . ?
C43 C44 1.383(3) . ?
C43 C48 1.396(3) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C44 H44 0.9500 . ?
C48 C47 1.399(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.488(3) . ?
C41 C36 1.396(3) . ?
C41 C40 1.404(3) . ?
C47 H47 0.9500 . ?
C36 C35 1.502(3) . ?
C36 C37 1.392(3) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C24 H24 0.9500 . ?
C24 C23 1.381(3) . ?
C23 H23 0.9500 . ?
C23 C22 1.381(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.392(3) . ?
C52 C53 1.387(3) . ?
C52 C51 1.504(3) . ?
C20 C21 1.390(3) . ?
C20 C19 1.501(3) . ?
C64 C59 1.401(3) . ?
C64 C63 1.388(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C31 H31 0.9500 . ?
C31 C30 1.385(3) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C5 H5 0.9500 . ?
C5 C6 1.380(3) . ?
C14 H14 0.9500 . ?
C14 C13 1.388(4) . ?
C14 C15 1.386(4) . ?
C7 H7 0.9500 . ?
C7 C6 1.384(3) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C58 C59 1.494(3) . ?
C30 H30 0.9500 . ?
C30 C29 1.381(4) . ?
C56 H56 0.9500 . ?
C56 C55 1.379(3) . ?
C21 H21 0.9500 . ?
C21 C22 1.388(3) . ?
C6 H6 0.9500 . ?
C53 H53 0.9500 . ?
C53 C54 1.389(3) . ?
C59 C60 1.394(3) . ?
C22 H22 0.9500 . ?
C28 H28 0.9500 . ?
C28 C29 1.388(3) . ?
C28 C27 1.389(3) . ?
C13 H13 0.9500 . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C15 H15 0.9500 . ?
C55 H55 0.9500 . ?
C55 C54 1.376(4) . ?
C29 H29 0.9500 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C40 H40 0.9500 . ?
C40 C39 1.384(4) . ?
C63 H63 0.9500 . ?
C63 C62 1.388(4) . ?
C54 H54 0.9500 . ?
C37 H37 0.9500 . ?
C37 C38 1.384(3) . ?
C39 H39 0.9500 . ?
C39 C38 1.378(4) . ?
C38 H38 0.9500 . ?
C60 H60 0.9500 . ?
C60 C61 1.379(4) . ?
C62 H62 0.9500 . ?
C62 C61 1.383(4) . ?
C2AA C1AA 1.453(4) . ?
C2AA N1AA 1.122(4) . ?
C61 H61 0.9500 . ?
C1AA H1AA 0.9800 . ?
C1AA H1AB 0.9800 . ?
C1AA H1AC 0.9800 . ?
N1BA C2BA 1.138(4) . ?
C2BA C1BA 1.440(5) . ?
C1BA H1BA 0.9800 . ?
C1BA H1BB 0.9800 . ?
C1BA H1BC 0.9800 . ?

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
O10 Ti3 O7 86.13(6) . . ?
O10 Ti3 N3 73.85(6) . . ?
O7 Ti3 N3 83.43(6) . . ?
O13 Ti3 O10 87.29(6) . . ?
O13 Ti3 O7 167.44(7) . . ?
O13 Ti3 N3 84.46(7) . . ?
O14 Ti3 O10 94.03(7) . . ?
O14 Ti3 O7 92.57(7) . . ?
O14 Ti3 O13 98.56(7) . . ?
O14 Ti3 O12 105.20(7) . . ?
O14 Ti3 N3 167.42(7) . . ?
O12 Ti3 O10 159.24(7) . . ?
O12 Ti3 O7 85.29(6) . . ?
O12 Ti3 O13 97.31(7) . . ?
O12 Ti3 N3 86.41(7) . . ?
O1 Ti1 O11 86.86(6) . . ?
O1 Ti1 N1 74.42(6) . . ?
O4 Ti1 O1 86.22(6) . . ?
O4 Ti1 O11 167.28(6) . . ?
O4 Ti1 N1 86.48(6) . . ?
O11 Ti1 N1 81.39(6) . . ?
O5 Ti1 O1 92.75(7) . . ?
O5 Ti1 O4 99.52(7) . . ?
O5 Ti1 O11 91.46(6) . . ?
O5 Ti1 O3 106.81(7) . . ?
O5 Ti1 N1 165.54(7) . . ?
O3 Ti1 O1 159.51(6) . . ?
O3 Ti1 O4 96.25(7) . . ?
O3 Ti1 O11 86.61(6) . . ?
O3 Ti1 N1 85.41(7) . . ?
O6 Ti2 O16 85.97(6) . . ?
O6 Ti2 N2 73.43(6) . . ?
O9 Ti2 O6 86.14(6) . . ?
O9 Ti2 O16 167.72(6) . . ?
O9 Ti2 N2 83.26(6) . . ?
O8 Ti2 O6 158.40(7) . . ?
O8 Ti2 O9 98.02(7) . . ?
O8 Ti2 O16 86.03(6) . . ?
O8 Ti2 N2 85.96(6) . . ?
O5 Ti2 O6 95.38(6) . . ?
O5 Ti2 O9 98.08(7) . . ?
O5 Ti2 O8 104.92(7) . . ?
O5 Ti2 O16 92.01(7) . . ?
O5 Ti2 N2 168.66(6) . . ?
O16 Ti2 N2 85.48(6) . . ?
O15 Ti4 O2 86.88(6) . . ?
O15 Ti4 N4 74.81(6) . . ?
O14 Ti4 O15 92.51(7) . . ?
O14 Ti4 O2 90.94(7) . . ?
O14 Ti4 O18 98.18(7) . . ?
O14 Ti4 N4 166.19(7) . . ?
O2 Ti4 N4 83.06(6) . . ?
O18 Ti4 O15 85.18(7) . . ?
O18 Ti4 O2 168.15(6) . . ?
O18 Ti4 N4 86.37(7) . . ?
O17 Ti4 O15 159.05(7) . . ?
O17 Ti4 O14 107.44(7) . . ?
O17 Ti4 O2 86.48(7) . . ?
O17 Ti4 O18 97.90(8) . . ?
O17 Ti4 N4 84.68(7) . . ?
C33 O10 Ti3 124.08(13) . . ?
C1 O1 Ti1 124.34(14) . . ?
C17 O6 Ti2 124.81(14) . . ?
C17 O7 Ti3 138.07(13) . . ?
C32 O9 Ti2 129.18(13) . . ?
C48 O13 Ti3 130.18(13) . . ?
C25 O8 Ti2 137.32(13) . . ?
C49 O15 Ti4 124.83(14) . . ?
C16 O4 Ti1 128.31(13) . . ?
C33 O11 Ti1 139.30(14) . . ?
Ti1 O5 Ti2 144.86(9) . . ?
C9 O3 Ti1 139.96(14) . . ?
C49 O16 Ti2 136.86(14) . . ?
Ti3 O14 Ti4 145.94(9) . . ?
C1 O2 Ti4 137.89(14) . . ?
C41 O12 Ti3 138.19(15) . . ?
C64 O18 Ti4 130.43(14) . . ?
C57 O17 Ti4 141.33(15) . . ?
C26 N2 Ti2 112.75(13) . . ?
C18 N2 Ti2 106.21(12) . . ?
C18 N2 C26 109.60(16) . . ?
C18 N2 C19 111.02(17) . . ?
C19 N2 Ti2 109.71(12) . . ?
C19 N2 C26 107.59(16) . . ?
C2 N1 Ti1 108.79(12) . . ?
C2 N1 C10 109.55(17) . . ?
C2 N1 C3 109.04(16) . . ?
C10 N1 Ti1 109.90(12) . . ?
C3 N1 Ti1 110.88(13) . . ?
C3 N1 C10 108.67(16) . . ?
C34 N3 Ti3 107.55(13) . . ?
C34 N3 C42 109.43(17) . . ?
C34 N3 C35 109.68(16) . . ?
C42 N3 Ti3 112.46(13) . . ?
C42 N3 C35 107.74(16) . . ?
C35 N3 Ti3 109.96(13) . . ?
C50 N4 Ti4 108.97(13) . . ?
C50 N4 C58 109.93(17) . . ?
C50 N4 C51 109.25(17) . . ?
C58 N4 Ti4 109.72(13) . . ?
C58 N4 C51 107.63(18) . . ?
C51 N4 Ti4 111.32(13) . . ?
O10 C33 C34 116.92(18) . . ?
O11 C33 O10 124.15(19) . . ?
O11 C33 C34 118.93(19) . . ?
O1 C1 C2 117.35(19) . . ?
O2 C1 O1 124.3(2) . . ?
O2 C1 C2 118.35(18) . . ?
O6 C17 C18 116.53(18) . . ?
O7 C17 O6 123.81(19) . . ?
O7 C17 C18 119.66(18) . . ?
O3 C9 C4 120.8(2) . . ?
O3 C9 C8 118.9(2) . . ?
C8 C9 C4 120.3(2) . . ?
O9 C32 C31 121.3(2) . . ?
O9 C32 C27 118.58(19) . . ?
C31 C32 C27 120.1(2) . . ?
C16 C11 C10 118.5(2) . . ?
C12 C11 C16 119.3(2) . . ?
C12 C11 C10 122.3(2) . . ?
O15 C49 C50 117.10(19) . . ?
O16 C49 O15 123.9(2) . . ?
O16 C49 C50 119.01(18) . . ?
C9 C4 C3 123.3(2) . . ?
C5 C4 C9 117.8(2) . . ?
C5 C4 C3 118.61(19) . . ?
N1 C2 C1 110.72(17) . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
O4 C16 C11 119.0(2) . . ?
O4 C16 C15 121.2(2) . . ?
C15 C16 C11 119.8(2) . . ?
N3 C34 C33 110.46(17) . . ?
N3 C34 H34A 109.6 . . ?
N3 C34 H34B 109.6 . . ?
C33 C34 H34A 109.6 . . ?
C33 C34 H34B 109.6 . . ?
H34A C34 H34B 108.1 . . ?
O17 C57 C52 120.8(2) . . ?
O17 C57 C56 118.3(2) . . ?
C56 C57 C52 120.9(2) . . ?
C9 C8 H8 119.8 . . ?
C7 C8 C9 120.4(2) . . ?
C7 C8 H8 119.8 . . ?
N4 C50 C49 110.82(17) . . ?
N4 C50 H50A 109.5 . . ?
N4 C50 H50B 109.5 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 108.1 . . ?
C46 C45 H45 120.0 . . ?
C46 C45 C44 119.9(2) . . ?
C44 C45 H45 120.0 . . ?
O8 C25 C24 118.92(19) . . ?
O8 C25 C20 120.30(19) . . ?
C24 C25 C20 120.78(19) . . ?
C45 C46 H46 119.6 . . ?
C45 C46 C47 120.8(2) . . ?
C47 C46 H46 119.6 . . ?
C44 C43 C42 122.0(2) . . ?
C44 C43 C48 119.6(2) . . ?
C48 C43 C42 118.20(19) . . ?
N3 C42 C43 113.96(17) . . ?
N3 C42 H42A 108.8 . . ?
N3 C42 H42B 108.8 . . ?
C43 C42 H42A 108.8 . . ?
C43 C42 H42B 108.8 . . ?
H42A C42 H42B 107.7 . . ?
C45 C44 H44 119.8 . . ?
C43 C44 C45 120.3(2) . . ?
C43 C44 H44 119.8 . . ?
O13 C48 C43 119.21(18) . . ?
O13 C48 C47 120.6(2) . . ?
C43 C48 C47 120.2(2) . . ?
N1 C10 C11 112.67(17) . . ?
N1 C10 H10A 109.1 . . ?
N1 C10 H10B 109.1 . . ?
C11 C10 H10A 109.1 . . ?
C11 C10 H10B 109.1 . . ?
H10A C10 H10B 107.8 . . ?
N2 C26 H26A 108.7 . . ?
N2 C26 H26B 108.7 . . ?
H26A C26 H26B 107.6 . . ?
C27 C26 N2 114.31(17) . . ?
C27 C26 H26A 108.7 . . ?
C27 C26 H26B 108.7 . . ?
O12 C41 C36 121.06(19) . . ?
O12 C41 C40 118.6(2) . . ?
C36 C41 C40 120.3(2) . . ?
C46 C47 C48 119.1(2) . . ?
C46 C47 H47 120.4 . . ?
C48 C47 H47 120.4 . . ?
C41 C36 C35 121.76(19) . . ?
C37 C36 C41 118.1(2) . . ?
C37 C36 C35 120.0(2) . . ?
N3 C35 C36 113.27(17) . . ?
N3 C35 H35A 108.9 . . ?
N3 C35 H35B 108.9 . . ?
C36 C35 H35A 108.9 . . ?
C36 C35 H35B 108.9 . . ?
H35A C35 H35B 107.7 . . ?
C25 C24 H24 120.2 . . ?
C23 C24 C25 119.6(2) . . ?
C23 C24 H24 120.2 . . ?
C24 C23 H23 119.7 . . ?
C24 C23 C22 120.6(2) . . ?
C22 C23 H23 119.7 . . ?
C11 C12 H12 119.4 . . ?
C11 C12 C13 121.1(2) . . ?
C13 C12 H12 119.4 . . ?
C57 C52 C51 122.8(2) . . ?
C53 C52 C57 117.6(2) . . ?
C53 C52 C51 119.3(2) . . ?
C25 C20 C19 120.78(19) . . ?
C21 C20 C25 117.7(2) . . ?
C21 C20 C19 121.5(2) . . ?
O18 C64 C59 118.6(2) . . ?
O18 C64 C63 121.0(2) . . ?
C63 C64 C59 120.4(2) . . ?
N1 C3 C4 114.88(17) . . ?
N1 C3 H3A 108.5 . . ?
N1 C3 H3B 108.5 . . ?
C4 C3 H3A 108.5 . . ?
C4 C3 H3B 108.5 . . ?
H3A C3 H3B 107.5 . . ?
C32 C31 H31 120.0 . . ?
C32 C31 C30 120.0(2) . . ?
C30 C31 H31 120.0 . . ?
N2 C18 C17 109.86(17) . . ?
N2 C18 H18A 109.7 . . ?
N2 C18 H18B 109.7 . . ?
C17 C18 H18A 109.7 . . ?
C17 C18 H18B 109.7 . . ?
H18A C18 H18B 108.2 . . ?
C4 C5 H5 119.1 . . ?
C6 C5 C4 121.8(2) . . ?
C6 C5 H5 119.1 . . ?
C13 C14 H14 119.6 . . ?
C15 C14 H14 119.6 . . ?
C15 C14 C13 120.8(2) . . ?
C8 C7 H7 120.2 . . ?
C8 C7 C6 119.7(2) . . ?
C6 C7 H7 120.2 . . ?
N4 C58 H58A 108.9 . . ?
N4 C58 H58B 108.9 . . ?
H58A C58 H58B 107.7 . . ?
C59 C58 N4 113.3(2) . . ?
C59 C58 H58A 108.9 . . ?
C59 C58 H58B 108.9 . . ?
C31 C30 H30 119.6 . . ?
C29 C30 C31 120.8(2) . . ?
C29 C30 H30 119.6 . . ?
C57 C56 H56 120.0 . . ?
C55 C56 C57 120.0(2) . . ?
C55 C56 H56 120.0 . . ?
C20 C21 H21 119.2 . . ?
C22 C21 C20 121.7(2) . . ?
C22 C21 H21 119.2 . . ?
C5 C6 C7 120.0(2) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C52 C53 H53 119.2 . . ?
C52 C53 C54 121.7(2) . . ?
C54 C53 H53 119.2 . . ?
C64 C59 C58 119.2(2) . . ?
C60 C59 C64 118.8(2) . . ?
C60 C59 C58 122.0(2) . . ?
C23 C22 C21 119.3(2) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.3 . . ?
C29 C28 H28 119.5 . . ?
C29 C28 C27 121.0(2) . . ?
C27 C28 H28 119.5 . . ?
C12 C13 H13 120.5 . . ?
C14 C13 C12 119.0(2) . . ?
C14 C13 H13 120.5 . . ?
N4 C51 C52 115.01(19) . . ?
N4 C51 H51A 108.5 . . ?
N4 C51 H51B 108.5 . . ?
C52 C51 H51A 108.5 . . ?
C52 C51 H51B 108.5 . . ?
H51A C51 H51B 107.5 . . ?
C16 C15 H15 120.0 . . ?
C14 C15 C16 120.0(2) . . ?
C14 C15 H15 120.0 . . ?
C56 C55 H55 119.9 . . ?
C54 C55 C56 120.2(2) . . ?
C54 C55 H55 119.9 . . ?
C30 C29 C28 119.2(2) . . ?
C30 C29 H29 120.4 . . ?
C28 C29 H29 120.4 . . ?
C32 C27 C26 118.06(19) . . ?
C28 C27 C32 118.9(2) . . ?
C28 C27 C26 122.9(2) . . ?
N2 C19 C20 112.45(18) . . ?
N2 C19 H19A 109.1 . . ?
N2 C19 H19B 109.1 . . ?
C20 C19 H19A 109.1 . . ?
C20 C19 H19B 109.1 . . ?
H19A C19 H19B 107.8 . . ?
C41 C40 H40 120.1 . . ?
C39 C40 C41 119.7(3) . . ?
C39 C40 H40 120.1 . . ?
C64 C63 H63 120.2 . . ?
C62 C63 C64 119.6(3) . . ?
C62 C63 H63 120.2 . . ?
C53 C54 H54 120.2 . . ?
C55 C54 C53 119.6(2) . . ?
C55 C54 H54 120.2 . . ?
C36 C37 H37 119.2 . . ?
C38 C37 C36 121.6(2) . . ?
C38 C37 H37 119.2 . . ?
C40 C39 H39 119.9 . . ?
C38 C39 C40 120.3(2) . . ?
C38 C39 H39 119.9 . . ?
C37 C38 H38 120.1 . . ?
C39 C38 C37 119.7(2) . . ?
C39 C38 H38 120.1 . . ?
C59 C60 H60 119.6 . . ?
C61 C60 C59 120.8(3) . . ?
C61 C60 H60 119.6 . . ?
C63 C62 H62 119.8 . . ?
C61 C62 C63 120.4(3) . . ?
C61 C62 H62 119.8 . . ?
N1AA C2AA C1AA 179.1(4) . . ?
C60 C61 C62 120.0(3) . . ?
C60 C61 H61 120.0 . . ?
C62 C61 H61 120.0 . . ?
C2AA C1AA H1AA 109.5 . . ?
C2AA C1AA H1AB 109.5 . . ?
C2AA C1AA H1AC 109.5 . . ?
H1AA C1AA H1AB 109.5 . . ?
H1AA C1AA H1AC 109.5 . . ?
H1AB C1AA H1AC 109.5 . . ?
N1BA C2BA C1BA 178.8(4) . . ?
C2BA C1BA H1BA 109.5 . . ?
C2BA C1BA H1BB 109.5 . . ?
C2BA C1BA H1BC 109.5 . . ?
H1BA C1BA H1BB 109.5 . . ?
H1BA C1BA H1BC 109.5 . . ?
H1BB C1BA H1BC 109.5 . . ?

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
Ti3 O10 C33 O11 166.75(15) . . . . ?
Ti3 O10 C33 C34 -12.8(2) . . . . ?
Ti3 O7 C17 O6 30.1(3) . . . . ?
Ti3 O7 C17 C18 -149.42(17) . . . . ?
Ti3 O13 C48 C43 -53.3(3) . . . . ?
Ti3 O13 C48 C47 127.91(18) . . . . ?
Ti3 O12 C41 C36 -22.0(3) . . . . ?
Ti3 O12 C41 C40 157.39(17) . . . . ?
Ti3 N3 C34 C33 23.76(19) . . . . ?
Ti3 N3 C42 C43 -52.8(2) . . . . ?
Ti3 N3 C35 C36 -60.8(2) . . . . ?
Ti1 O1 C1 O2 -169.37(15) . . . . ?
Ti1 O1 C1 C2 10.6(2) . . . . ?
Ti1 O4 C16 C11 53.9(3) . . . . ?
Ti1 O4 C16 C15 -125.01(19) . . . . ?
Ti1 O11 C33 O10 -23.2(3) . . . . ?
Ti1 O11 C33 C34 156.31(16) . . . . ?
Ti1 O3 C9 C4 10.3(3) . . . . ?
Ti1 O3 C9 C8 -170.24(16) . . . . ?
Ti1 N1 C2 C1 -18.49(19) . . . . ?
Ti1 N1 C10 C11 59.0(2) . . . . ?
Ti1 N1 C3 C4 58.85(19) . . . . ?
Ti2 O6 C17 O7 -170.54(15) . . . . ?
Ti2 O6 C17 C18 9.0(3) . . . . ?
Ti2 O9 C32 C31 -121.0(2) . . . . ?
Ti2 O9 C32 C27 58.5(2) . . . . ?
Ti2 O8 C25 C24 -147.90(17) . . . . ?
Ti2 O8 C25 C20 31.4(3) . . . . ?
Ti2 O16 C49 O15 -36.6(3) . . . . ?
Ti2 O16 C49 C50 143.19(17) . . . . ?
Ti2 N2 C26 C27 51.5(2) . . . . ?
Ti2 N2 C18 C17 -28.91(19) . . . . ?
Ti2 N2 C19 C20 61.70(19) . . . . ?
Ti4 O15 C49 O16 172.83(15) . . . . ?
Ti4 O15 C49 C50 -7.0(3) . . . . ?
Ti4 O2 C1 O1 32.3(3) . . . . ?
Ti4 O2 C1 C2 -147.68(16) . . . . ?
Ti4 O18 C64 C59 -52.8(3) . . . . ?
Ti4 O18 C64 C63 128.3(2) . . . . ?
Ti4 O17 C57 C52 -5.2(4) . . . . ?
Ti4 O17 C57 C56 175.44(18) . . . . ?
Ti4 N4 C50 C49 17.5(2) . . . . ?
Ti4 N4 C58 C59 -59.9(2) . . . . ?
Ti4 N4 C51 C52 -58.3(2) . . . . ?
O10 Ti3 O13 C48 -29.31(17) . . . . ?
O10 Ti3 O14 Ti4 28.02(17) . . . . ?
O10 Ti3 O12 C41 26.5(3) . . . . ?
O10 C33 C34 N3 -10.6(3) . . . . ?
O1 Ti1 O4 C16 33.78(17) . . . . ?
O1 Ti1 O5 Ti2 -40.72(17) . . . . ?
O1 Ti1 O3 C9 -3.2(3) . . . . ?
O1 C1 C2 N1 7.8(3) . . . . ?
O6 Ti2 O9 C32 24.85(17) . . . . ?
O6 Ti2 O8 C25 -35.4(3) . . . . ?
O6 Ti2 O5 Ti1 -19.02(17) . . . . ?
O6 C17 C18 N2 17.0(3) . . . . ?
O7 Ti3 O13 C48 29.1(4) . . . . ?
O7 Ti3 O14 Ti4 -58.27(17) . . . . ?
O7 Ti3 O12 C41 92.4(2) . . . . ?
O7 C17 C18 N2 -163.45(18) . . . . ?
O9 Ti2 O8 C25 64.5(2) . . . . ?
O9 Ti2 O5 Ti1 -105.87(16) . . . . ?
O9 C32 C31 C30 179.68(19) . . . . ?
O9 C32 C27 C26 5.3(3) . . . . ?
O9 C32 C27 C28 -178.90(19) . . . . ?
O13 Ti3 O14 Ti4 115.88(17) . . . . ?
O13 Ti3 O12 C41 -75.3(2) . . . . ?
O13 C48 C47 C46 -179.20(18) . . . . ?
O8 Ti2 O9 C32 -133.84(17) . . . . ?
O8 Ti2 O5 Ti1 153.55(15) . . . . ?
O8 C25 C24 C23 176.2(2) . . . . ?
O8 C25 C20 C21 -173.29(19) . . . . ?
O8 C25 C20 C19 8.8(3) . . . . ?
O15 Ti4 O14 Ti3 31.53(17) . . . . ?
O15 Ti4 O18 C64 -37.9(2) . . . . ?
O15 Ti4 O17 C57 1.0(4) . . . . ?
O15 C49 C50 N4 -9.1(3) . . . . ?
O4 Ti1 O5 Ti2 -127.34(16) . . . . ?
O4 Ti1 O3 C9 92.8(2) . . . . ?
O4 C16 C15 C14 176.5(2) . . . . ?
O11 Ti1 O4 C16 -23.4(4) . . . . ?
O11 Ti1 O5 Ti2 46.20(16) . . . . ?
O11 Ti1 O3 C9 -74.8(2) . . . . ?
O11 C33 C34 N3 169.80(18) . . . . ?
O5 Ti1 O4 C16 125.93(17) . . . . ?
O5 Ti1 O3 C9 -165.3(2) . . . . ?
O5 Ti2 O9 C32 119.74(17) . . . . ?
O5 Ti2 O8 C25 165.1(2) . . . . ?
O3 Ti1 O4 C16 -125.80(17) . . . . ?
O3 Ti1 O5 Ti2 133.10(16) . . . . ?
O3 C9 C4 C3 3.7(3) . . . . ?
O3 C9 C4 C5 178.06(19) . . . . ?
O3 C9 C8 C7 -178.5(2) . . . . ?
O16 Ti2 O9 C32 -25.2(4) . . . . ?
O16 Ti2 O8 C25 -103.9(2) . . . . ?
O16 Ti2 O5 Ti1 67.11(16) . . . . ?
O16 C49 C50 N4 171.05(19) . . . . ?
O14 Ti3 O13 C48 -122.99(17) . . . . ?
O14 Ti3 O12 C41 -176.3(2) . . . . ?
O14 Ti4 O18 C64 -129.8(2) . . . . ?
O14 Ti4 O17 C57 162.6(2) . . . . ?
O2 Ti4 O14 Ti3 -55.39(17) . . . . ?
O2 Ti4 O18 C64 10.2(5) . . . . ?
O2 Ti4 O17 C57 72.7(2) . . . . ?
O2 C1 C2 N1 -172.27(17) . . . . ?
O12 Ti3 O13 C48 130.36(17) . . . . ?
O12 Ti3 O14 Ti4 -144.08(16) . . . . ?
O12 C41 C36 C35 -9.3(3) . . . . ?
O12 C41 C36 C37 174.68(19) . . . . ?
O12 C41 C40 C39 -176.6(2) . . . . ?
O18 Ti4 O14 Ti3 117.02(17) . . . . ?
O18 Ti4 O17 C57 -96.2(2) . . . . ?
O18 C64 C59 C58 -0.5(3) . . . . ?
O18 C64 C59 C60 -178.3(2) . . . . ?
O18 C64 C63 C62 178.3(2) . . . . ?
O17 Ti4 O14 Ti3 -141.99(16) . . . . ?
O17 Ti4 O18 C64 121.2(2) . . . . ?
O17 C57 C52 C53 -180.0(2) . . . . ?
O17 C57 C52 C51 -5.9(3) . . . . ?
O17 C57 C56 C55 178.9(2) . . . . ?
N2 Ti2 O9 C32 -48.90(17) . . . . ?
N2 Ti2 O8 C25 -18.2(2) . . . . ?
N2 Ti2 O5 Ti1 -9.8(5) . . . . ?
N2 C26 C27 C32 -58.6(3) . . . . ?
N2 C26 C27 C28 125.7(2) . . . . ?
N1 Ti1 O4 C16 -40.82(18) . . . . ?
N1 Ti1 O5 Ti2 -13.7(4) . . . . ?
N1 Ti1 O3 C9 6.8(2) . . . . ?
N3 Ti3 O13 C48 44.71(17) . . . . ?
N3 Ti3 O14 Ti4 12.8(4) . . . . ?
N3 Ti3 O12 C41 8.7(2) . . . . ?
N4 Ti4 O14 Ti3 8.5(4) . . . . ?
N4 Ti4 O18 C64 37.1(2) . . . . ?
N4 Ti4 O17 C57 -10.6(2) . . . . ?
N4 C58 C59 C64 58.2(3) . . . . ?
N4 C58 C59 C60 -124.0(2) . . . . ?
C9 C4 C3 N1 -43.0(3) . . . . ?
C9 C4 C5 C6 0.5(3) . . . . ?
C9 C8 C7 C6 0.5(3) . . . . ?
C32 C31 C30 C29 -0.9(3) . . . . ?
C11 C16 C15 C14 -2.4(3) . . . . ?
C11 C12 C13 C14 -1.5(3) . . . . ?
C4 C9 C8 C7 0.9(3) . . . . ?
C4 C5 C6 C7 1.0(3) . . . . ?
C2 N1 C10 C11 -60.5(2) . . . . ?
C2 N1 C3 C4 178.61(17) . . . . ?
C16 C11 C10 N1 -61.5(3) . . . . ?
C16 C11 C12 C13 0.0(3) . . . . ?
C34 N3 C42 C43 66.6(2) . . . . ?
C34 N3 C35 C36 -178.88(18) . . . . ?
C57 C52 C53 C54 1.2(4) . . . . ?
C57 C52 C51 N4 42.5(3) . . . . ?
C57 C56 C55 C54 1.1(4) . . . . ?
C8 C9 C4 C3 -175.77(19) . . . . ?
C8 C9 C4 C5 -1.4(3) . . . . ?
C8 C7 C6 C5 -1.5(3) . . . . ?
C50 N4 C58 C59 59.9(2) . . . . ?
C50 N4 C51 C52 -178.71(19) . . . . ?
C45 C46 C47 C48 0.6(3) . . . . ?
C25 C24 C23 C22 -1.5(3) . . . . ?
C25 C20 C21 C22 -4.5(3) . . . . ?
C25 C20 C19 N2 -57.7(3) . . . . ?
C46 C45 C44 C43 1.1(3) . . . . ?
C43 C48 C47 C46 2.0(3) . . . . ?
C42 N3 C34 C33 -98.7(2) . . . . ?
C42 N3 C35 C36 62.1(2) . . . . ?
C42 C43 C44 C45 -172.61(19) . . . . ?
C42 C43 C48 O13 -7.5(3) . . . . ?
C42 C43 C48 C47 171.24(18) . . . . ?
C44 C45 C46 C47 -2.2(3) . . . . ?
C44 C43 C42 N3 -125.9(2) . . . . ?
C44 C43 C48 O13 178.12(18) . . . . ?
C44 C43 C48 C47 -3.1(3) . . . . ?
C48 C43 C42 N3 59.9(3) . . . . ?
C48 C43 C44 C45 1.5(3) . . . . ?
C10 N1 C2 C1 101.66(19) . . . . ?
C10 N1 C3 C4 -62.0(2) . . . . ?
C10 C11 C16 O4 3.3(3) . . . . ?
C10 C11 C16 C15 -177.71(19) . . . . ?
C10 C11 C12 C13 179.7(2) . . . . ?
C26 N2 C18 C17 93.2(2) . . . . ?
C26 N2 C19 C20 -61.3(2) . . . . ?
C41 C36 C35 N3 54.1(3) . . . . ?
C41 C36 C37 C38 2.5(3) . . . . ?
C41 C40 C39 C38 1.6(4) . . . . ?
C36 C41 C40 C39 2.8(3) . . . . ?
C36 C37 C38 C39 1.8(4) . . . . ?
C35 N3 C34 C33 143.32(18) . . . . ?
C35 N3 C42 C43 -174.17(18) . . . . ?
C35 C36 C37 C38 -173.6(2) . . . . ?
C24 C25 C20 C21 6.0(3) . . . . ?
C24 C25 C20 C19 -171.9(2) . . . . ?
C24 C23 C22 C21 3.0(4) . . . . ?
C12 C11 C16 O4 -176.94(19) . . . . ?
C12 C11 C16 C15 2.0(3) . . . . ?
C12 C11 C10 N1 118.8(2) . . . . ?
C52 C57 C56 C55 -0.5(4) . . . . ?
C52 C53 C54 C55 -0.7(4) . . . . ?
C20 C25 C24 C23 -3.1(3) . . . . ?
C20 C21 C22 C23 0.1(4) . . . . ?
C64 C59 C60 C61 -0.1(4) . . . . ?
C64 C63 C62 C61 0.0(4) . . . . ?
C3 N1 C2 C1 -139.53(17) . . . . ?
C3 N1 C10 C11 -179.49(18) . . . . ?
C3 C4 C5 C6 175.1(2) . . . . ?
C31 C32 C27 C26 -175.20(19) . . . . ?
C31 C32 C27 C28 0.6(3) . . . . ?
C31 C30 C29 C28 0.7(3) . . . . ?
C18 N2 C26 C27 -66.6(2) . . . . ?
C18 N2 C19 C20 178.79(17) . . . . ?
C5 C4 C3 N1 142.69(19) . . . . ?
C58 N4 C50 C49 -102.7(2) . . . . ?
C58 N4 C51 C52 62.0(2) . . . . ?
C58 C59 C60 C61 -177.8(3) . . . . ?
C56 C57 C52 C53 -0.7(3) . . . . ?
C56 C57 C52 C51 173.4(2) . . . . ?
C56 C55 C54 C53 -0.5(4) . . . . ?
C21 C20 C19 N2 124.5(2) . . . . ?
C53 C52 C51 N4 -143.5(2) . . . . ?
C59 C64 C63 C62 -0.5(4) . . . . ?
C59 C60 C61 C62 -0.5(5) . . . . ?
C13 C14 C15 C16 0.8(3) . . . . ?
C51 N4 C50 C49 139.37(19) . . . . ?
C51 N4 C58 C59 178.82(18) . . . . ?
C51 C52 C53 C54 -173.1(2) . . . . ?
C15 C14 C13 C12 1.2(4) . . . . ?
C29 C28 C27 C32 -0.8(3) . . . . ?
C29 C28 C27 C26 174.8(2) . . . . ?
C27 C32 C31 C30 0.2(3) . . . . ?
C27 C28 C29 C30 0.1(3) . . . . ?
C19 N2 C26 C27 172.59(18) . . . . ?
C19 N2 C18 C17 -148.12(17) . . . . ?
C19 C20 C21 C22 173.4(2) . . . . ?
C40 C41 C36 C35 171.3(2) . . . . ?
C40 C41 C36 C37 -4.7(3) . . . . ?
C40 C39 C38 C37 -3.9(4) . . . . ?
C63 C64 C59 C58 178.4(2) . . . . ?
C63 C64 C59 C60 0.5(4) . . . . ?
C63 C62 C61 C60 0.5(5) . . . . ?
C37 C36 C35 N3 -129.9(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_final_sq
_database_code_depnum_ccdc_archive 'CCDC 1483653'
_audit_update_record             
;
2016-06-06 deposited with the CCDC.
2016-10-17 downloaded from the CCDC.
;
_audit_creation_date             2016-05-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C72 H72 N4 O18 Ti4, 2(C2 H4 O0.5)'
_chemical_formula_sum            'C76 H80 N4 O19 Ti4'
_chemical_formula_weight         1545.04
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -4'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'

_cell_length_a                   13.8620(5)
_cell_length_b                   13.8620(5)
_cell_length_c                   23.4683(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4509.6(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9994
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.11
_cell_measurement_theta_min      2.71
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.402
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.7022
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0566 before and 0.0469 after correction.
The Ratio of minimum to maximum transmission is 0.9419.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            36957
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.117
_diffrn_reflns_theta_min         2.708
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.946
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                4688
_reflns_number_total             4978
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker APEX2 v2014.9-0 (Bruker, 2014)'
_computing_data_collection       'Bruker APEX2 v2014.9-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details 
;
 Flack x determined using 2190 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.033(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         4978
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0381
_refine_ls_restrained_S_all      1.068
_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)+(0.0886P)²+0.5197P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1145
_refine_special_details          SQUEEZE
# start Validation Reply Form
_vrf_PLAT987_final_sq            
;
PROBLEM: The Flack x is >> 0 - Do a BASF/TWIN Refinement Please Check
RESPONSE: The Flack parameter is close to zero [0.033(7)].
;
# end Validation Reply Form
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: O1AA(0.25) C2AA(0.5) H2AA(0.5) H2AB(0.5) C1AA(0.5) H1AA(0.5)
 H1AB(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B), C10(H10A,H10B), C2AA(H2AA,H2AB), C1AA(H1AA,H1AB)
3.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C14(H14), C7(H7), C8(H8), C12(H12), C15(H15)
3.c Idealised Me refined as rotating group:
 C13A(H13A,H13B,H13C), C6A(H6AB,H6AC,H6AA)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.46638(4) 0.62147(4) 0.60581(2) 0.01548(16) Uani 1 1 d . . . . .
O4 O 0.57215(18) 0.69051(17) 0.63440(10) 0.0210(5) Uani 1 1 d . . . . .
O2 O 0.56587(16) 0.65009(17) 0.44104(9) 0.0171(5) Uani 1 1 d . . . . .
O1 O 0.54239(16) 0.61360(16) 0.53267(10) 0.0154(4) Uani 1 1 d . . . . .
O3 O 0.37660(18) 0.66697(17) 0.65686(10) 0.0202(5) Uani 1 1 d . . . . .
O5 O 0.5000 0.5000 0.62896(14) 0.0182(7) Uani 1 2 d S T P . .
C5 C 0.2413(3) 0.8897(3) 0.63257(17) 0.0255(7) Uani 1 1 d . . . . .
H5 H 0.2241 0.9316 0.6022 0.031 Uiso 1 1 calc R . . . .
N1 N 0.4301(2) 0.7609(2) 0.55473(12) 0.0176(6) Uani 1 1 d . . . . .
C4 C 0.2963(2) 0.8085(2) 0.62071(14) 0.0203(7) Uani 1 1 d . . . . .
C13 C 0.7563(3) 0.8729(3) 0.5462(2) 0.0325(9) Uani 1 1 d . . . . .
C6 C 0.2103(3) 0.9118(3) 0.68754(18) 0.0331(9) Uani 1 1 d . . . . .
C9 C 0.3219(2) 0.7465(3) 0.66528(15) 0.0214(7) Uani 1 1 d . . . . .
C13A C 0.8223(4) 0.9365(3) 0.5097(2) 0.0454(12) Uani 1 1 d . . . . .
H13A H 0.7943 0.9439 0.4716 0.068 Uiso 1 1 calc GR . . . .
H13B H 0.8860 0.9061 0.5066 0.068 Uiso 1 1 calc GR . . . .
H13C H 0.8290 1.0000 0.5276 0.068 Uiso 1 1 calc GR . . . .
C16 C 0.6325(2) 0.7509(2) 0.60741(15) 0.0211(6) Uani 1 1 d . . . . .
C14 C 0.7936(3) 0.8001(3) 0.58052(19) 0.0313(9) Uani 1 1 d . . . . .
H14 H 0.8614 0.7919 0.5834 0.038 Uiso 1 1 calc R . . . .
C7 C 0.2359(3) 0.8492(3) 0.73122(18) 0.0365(10) Uani 1 1 d . . . . .
H7 H 0.2155 0.8629 0.7690 0.044 Uiso 1 1 calc R . . . .
C3 C 0.3252(3) 0.7871(3) 0.56028(14) 0.0205(7) Uani 1 1 d . . . . .
H3A H 0.3117 0.8443 0.5363 0.025 Uiso 1 1 calc R . . . .
H3B H 0.2854 0.7331 0.5458 0.025 Uiso 1 1 calc R . . . .
C2 C 0.4535(3) 0.7435(2) 0.49357(14) 0.0190(7) Uani 1 1 d . . . . .
H2A H 0.4800 0.8032 0.4765 0.023 Uiso 1 1 calc R . . . .
H2B H 0.3940 0.7262 0.4726 0.023 Uiso 1 1 calc R . . . .
C8 C 0.2903(3) 0.7679(3) 0.72111(16) 0.0291(8) Uani 1 1 d . . . . .
H8 H 0.3066 0.7261 0.7517 0.035 Uiso 1 1 calc R . . . .
C12 C 0.6572(3) 0.8871(3) 0.54478(18) 0.0294(8) Uani 1 1 d . . . . .
H12 H 0.6316 0.9388 0.5230 0.035 Uiso 1 1 calc R . . . .
C1 C 0.5257(2) 0.6637(2) 0.48824(13) 0.0155(6) Uani 1 1 d . . . . .
C15 C 0.7322(3) 0.7391(3) 0.61068(18) 0.0279(8) Uani 1 1 d . . . . .
H15 H 0.7585 0.6892 0.6337 0.033 Uiso 1 1 calc R . . . .
C6A C 0.1500(4) 1.0006(4) 0.6992(2) 0.0455(11) Uani 1 1 d . . . . .
H6AB H 0.1765 1.0555 0.6781 0.068 Uiso 1 1 calc GR . . . .
H6AC H 0.1511 1.0149 0.7401 0.068 Uiso 1 1 calc GR . . . .
H6AA H 0.0834 0.9890 0.6870 0.068 Uiso 1 1 calc GR . . . .
C11 C 0.5945(3) 0.8267(3) 0.57484(16) 0.0225(7) Uani 1 1 d . . . . .
C10 C 0.4883(3) 0.8449(3) 0.57616(16) 0.0221(7) Uani 1 1 d . . . . .
H10A H 0.4736 0.9022 0.5526 0.027 Uiso 1 1 calc R . . . .
H10B H 0.4686 0.8594 0.6158 0.027 Uiso 1 1 calc R . . . .
O1AA O 0.5000 1.0000 0.6762(3) 0.0358(19) Uani 0.5 2 d S T P . .
C2AA C 0.5487(8) 0.9751(7) 0.7734(4) 0.041(2) Uani 0.5 1 d . . . . .
H2AA H 0.5513 0.9225 0.8019 0.050 Uiso 0.5 1 calc R . . . .
H2AB H 0.6019 1.0211 0.7806 0.050 Uiso 0.5 1 calc R . . . .
C1AA C 0.5515(7) 0.9354(6) 0.7118(3) 0.0351(19) Uani 0.5 1 d . . . . .
H1AA H 0.6192 0.9299 0.6987 0.042 Uiso 0.5 1 calc R . . . .
H1AB H 0.5217 0.8706 0.7104 0.042 Uiso 0.5 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 O4 1.875(2) . ?
Ti1 O2 2.100(2) 4_656 ?
Ti1 O1 2.017(2) . ?
Ti1 O3 1.839(2) . ?
Ti1 O5 1.8296(11) . ?
Ti1 N1 2.330(3) . ?
O4 C16 1.342(4) . ?
O2 Ti1 2.100(2) 3_566 ?
O2 C1 1.254(4) . ?
O1 C1 1.274(4) . ?
O3 C9 1.353(4) . ?
O5 Ti1 1.8295(11) 2_665 ?
C5 H5 0.9500 . ?
C5 C4 1.388(5) . ?
C5 C6 1.393(6) . ?
N1 C3 1.505(4) . ?
N1 C2 1.491(4) . ?
N1 C10 1.502(4) . ?
C4 C9 1.400(5) . ?
C4 C3 1.503(5) . ?
C13 C13A 1.532(6) . ?
C13 C14 1.392(7) . ?
C13 C12 1.388(6) . ?
C6 C7 1.389(7) . ?
C6 C6A 1.513(6) . ?
C9 C8 1.413(5) . ?
C13A H13A 0.9800 . ?
C13A H13B 0.9800 . ?
C13A H13C 0.9800 . ?
C16 C15 1.395(5) . ?
C16 C11 1.403(5) . ?
C14 H14 0.9500 . ?
C14 C15 1.392(6) . ?
C7 H7 0.9500 . ?
C7 C8 1.377(6) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C1 1.497(4) . ?
C8 H8 0.9500 . ?
C12 H12 0.9500 . ?
C12 C11 1.398(5) . ?
C15 H15 0.9500 . ?
C6A H6AB 0.9800 . ?
C6A H6AC 0.9800 . ?
C6A H6AA 0.9800 . ?
C11 C10 1.494(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
O1AA C1AA 1.418(9) 2_675 ?
O1AA C1AA 1.418(9) . ?
C2AA C2AA 1.52(2) 2_675 ?
C2AA H2AA 0.9900 . ?
C2AA H2AB 0.9900 . ?
C2AA C1AA 1.547(12) . ?
C1AA H1AA 0.9900 . ?
C1AA H1AB 0.9900 . ?

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
O4 Ti1 O2 167.39(10) . 4_656 ?
O4 Ti1 O1 85.62(10) . . ?
O4 Ti1 N1 85.94(10) . . ?
O2 Ti1 N1 82.49(9) 4_656 . ?
O1 Ti1 O2 86.34(9) . 4_656 ?
O1 Ti1 N1 73.71(10) . . ?
O3 Ti1 O4 96.95(11) . . ?
O3 Ti1 O2 86.94(10) . 4_656 ?
O3 Ti1 O1 157.88(11) . . ?
O3 Ti1 N1 84.53(10) . . ?
O5 Ti1 O4 99.46(9) . . ?
O5 Ti1 O2 90.77(8) . 4_656 ?
O5 Ti1 O1 94.01(11) . . ?
O5 Ti1 O3 107.14(11) . . ?
O5 Ti1 N1 166.27(12) . . ?
C16 O4 Ti1 129.5(2) . . ?
C1 O2 Ti1 137.8(2) . 3_566 ?
C1 O1 Ti1 124.9(2) . . ?
C9 O3 Ti1 138.9(2) . . ?
Ti1 O5 Ti1 145.46(19) 2_665 . ?
C4 C5 H5 118.9 . . ?
C4 C5 C6 122.2(4) . . ?
C6 C5 H5 118.9 . . ?
C3 N1 Ti1 111.3(2) . . ?
C2 N1 Ti1 108.3(2) . . ?
C2 N1 C3 109.4(3) . . ?
C2 N1 C10 109.3(3) . . ?
C10 N1 Ti1 110.8(2) . . ?
C10 N1 C3 107.6(3) . . ?
C5 C4 C9 119.2(3) . . ?
C5 C4 C3 119.7(3) . . ?
C9 C4 C3 121.0(3) . . ?
C14 C13 C13A 121.3(4) . . ?
C12 C13 C13A 119.8(4) . . ?
C12 C13 C14 118.9(4) . . ?
C5 C6 C6A 121.1(4) . . ?
C7 C6 C5 117.9(4) . . ?
C7 C6 C6A 121.0(4) . . ?
O3 C9 C4 122.3(3) . . ?
O3 C9 C8 118.7(3) . . ?
C4 C9 C8 119.1(3) . . ?
C13 C13A H13A 109.5 . . ?
C13 C13A H13B 109.5 . . ?
C13 C13A H13C 109.5 . . ?
H13A C13A H13B 109.5 . . ?
H13A C13A H13C 109.5 . . ?
H13B C13A H13C 109.5 . . ?
O4 C16 C15 121.3(3) . . ?
O4 C16 C11 119.4(3) . . ?
C15 C16 C11 119.3(3) . . ?
C13 C14 H14 119.7 . . ?
C13 C14 C15 120.5(4) . . ?
C15 C14 H14 119.7 . . ?
C6 C7 H7 119.2 . . ?
C8 C7 C6 121.6(4) . . ?
C8 C7 H7 119.2 . . ?
N1 C3 H3A 109.0 . . ?
N1 C3 H3B 109.0 . . ?
C4 C3 N1 112.8(3) . . ?
C4 C3 H3A 109.0 . . ?
C4 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
N1 C2 H2A 109.6 . . ?
N1 C2 H2B 109.6 . . ?
N1 C2 C1 110.2(3) . . ?
H2A C2 H2B 108.1 . . ?
C1 C2 H2A 109.6 . . ?
C1 C2 H2B 109.6 . . ?
C9 C8 H8 120.0 . . ?
C7 C8 C9 120.1(4) . . ?
C7 C8 H8 120.0 . . ?
C13 C12 H12 119.4 . . ?
C13 C12 C11 121.3(4) . . ?
C11 C12 H12 119.4 . . ?
O2 C1 O1 124.1(3) . . ?
O2 C1 C2 118.8(3) . . ?
O1 C1 C2 117.1(3) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 C16 120.5(4) . . ?
C14 C15 H15 119.8 . . ?
C6 C6A H6AB 109.5 . . ?
C6 C6A H6AC 109.5 . . ?
C6 C6A H6AA 109.5 . . ?
H6AB C6A H6AC 109.5 . . ?
H6AB C6A H6AA 109.5 . . ?
H6AC C6A H6AA 109.5 . . ?
C16 C11 C10 119.0(3) . . ?
C12 C11 C16 119.3(3) . . ?
C12 C11 C10 121.5(4) . . ?
N1 C10 H10A 109.0 . . ?
N1 C10 H10B 109.0 . . ?
C11 C10 N1 113.1(3) . . ?
C11 C10 H10A 109.0 . . ?
C11 C10 H10B 109.0 . . ?
H10A C10 H10B 107.8 . . ?
C1AA O1AA C1AA 107.7(9) . 2_675 ?
C2AA C2AA H2AA 111.6 2_675 . ?
C2AA C2AA H2AB 111.6 2_675 . ?
C2AA C2AA C1AA 100.6(6) 2_675 . ?
H2AA C2AA H2AB 109.4 . . ?
C1AA C2AA H2AA 111.6 . . ?
C1AA C2AA H2AB 111.6 . . ?
O1AA C1AA C2AA 108.3(7) . . ?
O1AA C1AA H1AA 110.0 . . ?
O1AA C1AA H1AB 110.0 . . ?
C2AA C1AA H1AA 110.0 . . ?
C2AA C1AA H1AB 110.0 . . ?
H1AA C1AA H1AB 108.4 . . ?

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
Ti1 O4 C16 C15 -127.9(3) . . . . ?
Ti1 O4 C16 C11 51.5(4) . . . . ?
Ti1 O2 C1 O1 31.7(5) 3_566 . . . ?
Ti1 O2 C1 C2 -148.3(3) 3_566 . . . ?
Ti1 O1 C1 O2 -171.1(2) . . . . ?
Ti1 O1 C1 C2 8.9(4) . . . . ?
Ti1 O3 C9 C4 24.2(5) . . . . ?
Ti1 O3 C9 C8 -155.4(3) . . . . ?
Ti1 N1 C3 C4 61.9(3) . . . . ?
Ti1 N1 C2 C1 -22.5(3) . . . . ?
Ti1 N1 C10 C11 56.1(3) . . . . ?
O4 Ti1 O3 C9 79.3(3) . . . . ?
O4 Ti1 O5 Ti1 -115.57(8) . . . 2_665 ?
O4 C16 C15 C14 177.4(3) . . . . ?
O4 C16 C11 C12 -177.3(3) . . . . ?
O4 C16 C11 C10 6.6(5) . . . . ?
O2 Ti1 O4 C16 -17.6(7) 4_656 . . . ?
O2 Ti1 O3 C9 -88.7(3) 4_656 . . . ?
O2 Ti1 O5 Ti1 57.04(6) 4_656 . . 2_665 ?
O1 Ti1 O4 C16 33.0(3) . . . . ?
O1 Ti1 O3 C9 -16.2(5) . . . . ?
O1 Ti1 O5 Ti1 -29.35(7) . . . 2_665 ?
O3 Ti1 O4 C16 -124.9(3) . . . . ?
O3 Ti1 O5 Ti1 144.07(8) . . . 2_665 ?
O3 C9 C8 C7 178.9(4) . . . . ?
O5 Ti1 O4 C16 126.3(3) . . . . ?
O5 Ti1 O3 C9 -178.6(3) . . . . ?
C5 C4 C9 O3 -179.0(3) . . . . ?
C5 C4 C9 C8 0.5(5) . . . . ?
C5 C4 C3 N1 133.6(3) . . . . ?
C5 C6 C7 C8 0.1(7) . . . . ?
N1 Ti1 O4 C16 -41.0(3) . . . . ?
N1 Ti1 O3 C9 -6.0(3) . . . . ?
N1 Ti1 O5 Ti1 -3.3(3) . . . 2_665 ?
N1 C2 C1 O2 -168.2(3) . . . . ?
N1 C2 C1 O1 11.9(4) . . . . ?
C4 C5 C6 C7 -0.3(6) . . . . ?
C4 C5 C6 C6A -179.8(4) . . . . ?
C4 C9 C8 C7 -0.7(6) . . . . ?
C13 C14 C15 C16 -0.7(6) . . . . ?
C13 C12 C11 C16 0.5(6) . . . . ?
C13 C12 C11 C10 176.5(3) . . . . ?
C6 C5 C4 C9 -0.1(5) . . . . ?
C6 C5 C4 C3 178.3(4) . . . . ?
C6 C7 C8 C9 0.3(7) . . . . ?
C9 C4 C3 N1 -48.1(4) . . . . ?
C13A C13 C14 C15 -176.0(4) . . . . ?
C13A C13 C12 C11 176.1(4) . . . . ?
C16 C11 C10 N1 -61.3(4) . . . . ?
C14 C13 C12 C11 -3.2(6) . . . . ?
C3 N1 C2 C1 -144.1(3) . . . . ?
C3 N1 C10 C11 178.0(3) . . . . ?
C3 C4 C9 O3 2.7(5) . . . . ?
C3 C4 C9 C8 -177.8(3) . . . . ?
C2 N1 C3 C4 -178.4(3) . . . . ?
C2 N1 C10 C11 -63.2(4) . . . . ?
C12 C13 C14 C15 3.3(6) . . . . ?
C12 C11 C10 N1 122.7(4) . . . . ?
C15 C16 C11 C12 2.1(5) . . . . ?
C15 C16 C11 C10 -174.0(3) . . . . ?
C6A C6 C7 C8 179.6(4) . . . . ?
C11 C16 C15 C14 -2.1(5) . . . . ?
C10 N1 C3 C4 -59.7(4) . . . . ?
C10 N1 C2 C1 98.3(3) . . . . ?
C2AA C2AA C1AA O1AA 31.7(12) 2_675 . . . ?
C1AA O1AA C1AA C2AA -12.2(5) 2_675 . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_final
_database_code_depnum_ccdc_archive 'CCDC 1483654'
_audit_update_record             
;
2016-06-06 deposited with the CCDC.
2016-10-17 downloaded from the CCDC.
;
_audit_creation_date             2016-05-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C96 H120 N4 O18 Ti4, 12(C7 H8)'
_chemical_formula_sum            'C180 H216 N4 O18 Ti4'
_chemical_formula_weight         2915.16
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -4'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'

_cell_length_a                   19.5294(8)
_cell_length_b                   19.5294(8)
_cell_length_c                   20.7148(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7900.6(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9816
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.87
_cell_measurement_theta_min      2.46
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.261
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0707 before and 0.0563 after correction.
The Ratio of minimum to maximum transmission is 0.8645.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3112
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            57486
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.142
_diffrn_reflns_theta_min         2.458
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.940
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                7467
_reflns_number_total             8746
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Bruker APEX2 v2014.9-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details 
;
 Flack x determined using 3339 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         8746
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0383
_refine_ls_restrained_S_all      1.078
_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)+(0.0550P)²+4.4970P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.1036
_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.

 The disordered toluene "B" solvent molecule was refined anisotropically over
 two positions (C1BA-C7BA and C1BB-C7BB) using idealised positions for all
 atoms. Occupancies for each molecule were refined freely against each other.

 The disordered toluene "C" solvent molecule was refined anisotropically over
 two positions (C1CA-C7CA and C1CB-C7CB) using idealised positions for all
 atoms. Occupancies for each molecule were refined freely against each other.
 The EADP constraint about molecule C1BB-C7BB allowed for stable refinement.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C4CB) = Uanis(C3CB) = Uanis(C1CB) = Uanis(C2CB) = Uanis(C7CB) =
Uanis(C6CB) = Uanis(C5CB)
3. Others
 Sof(C1BA)=Sof(H1BD)=Sof(H1BE)=Sof(H1BF)=Sof(C2BA)=Sof(C7BA)=Sof(H7BA)=
 Sof(C6BA)=Sof(H6BE)=Sof(C5BA)=Sof(H5BA)=Sof(C4BA)=Sof(H4BA)=Sof(C3BA)=
 Sof(H3BA)=1-FVAR(1)
 Sof(C1BB)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=Sof(C2BB)=Sof(C7BB)=Sof(H7BB)=
 Sof(C6BB)=Sof(H6BD)=Sof(C5BB)=Sof(H5BB)=Sof(C4BB)=Sof(H4BB)=Sof(C3BB)=
 Sof(H3BB)=FVAR(1)
 Sof(C1CB)=Sof(H1CD)=Sof(H1CE)=Sof(H1CF)=Sof(C2CB)=Sof(C7CB)=Sof(H7CB)=
 Sof(C6CB)=Sof(H6CE)=Sof(C5CB)=Sof(H5CB)=Sof(C4CB)=Sof(H4CB)=Sof(C3CB)=
 Sof(H3CB)=1-FVAR(2)
 Sof(C1CA)=Sof(H1CA)=Sof(H1CB)=Sof(H1CC)=Sof(C4CA)=Sof(H4CA)=Sof(C3CA)=
 Sof(H3CA)=Sof(C8CA)=Sof(C7CA)=Sof(H7CA)=Sof(C6CA)=Sof(H6CD)=Sof(C5CA)=
 Sof(H5CA)=FVAR(2)
4.a Free rotating group:
 C1BB(C2BB,C7BB,C6BB,C5BB,C4BB,C3BB), C1BA(C2BA,C7BA,C6BA,C5BA,C4BA,C3BA,C5,C6,
 C6A,C6D,C6C,C6B), C1CA(C4CA,C3CA,C8CA,C7CA,C6CA,C5CA), C1CB(C2CB,C7CB,C6CB,
 C5CB,C4CB,C3CB)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C10(H10A,H10B)
4.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C8(H8), C7(H7), C15(H15), C14(H14), C7AA(H7AA), C3AA(H3AA),
 C4AA(H4AA), C5AA(H5AA), C6AA(H6AA), C7BB(H7BB), C6BB(H6BD), C5BB(H5BB),
 C4BB(H4BB), C3BB(H3BB), C7BA(H7BA), C6BA(H6BE), C5BA(H5BA), C4BA(H4BA),
 C3BA(H3BA), C5(H5), C4CA(H4CA), C3CA(H3CA), C7CA(H7CA), C6CA(H6CD), C5CA(H5CA),
  C7CB(H7CB), C6CB(H6CE), C5CB(H5CB), C4CB(H4CB), C3CB(H3CB)
4.d Idealised Me refined as rotating group:
 C13C(H13A,H13B,H13C), C13D(H13D,H13E,H13F), C13B(H13G,H13H,H13I), C1AA(H1AA,
 H1AB,H1AC), C1BB(H1BA,H1BB,H1BC), C1BA(H1BD,H1BE,H1BF), C6D(H6DA,H6DB,H6DC),
 C6C(H6CA,H6CB,H6CC), C6B(H6BA,H6BB,H6BC), C1CA(H1CA,H1CB,H1CC), C1CB(H1CD,H1CE,
 H1CF)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.50337(3) 0.58909(3) 0.62004(2) 0.01520(12) Uani 1 1 d . . . . .
O4 O 0.41914(11) 0.61811(11) 0.65244(10) 0.0199(5) Uani 1 1 d . . . . .
O1 O 0.45144(10) 0.57088(10) 0.53707(10) 0.0160(4) Uani 1 1 d . . . . .
O5 O 0.5000 0.5000 0.64558(14) 0.0181(6) Uani 1 2 d S T P . .
O2 O 0.42803(11) 0.59253(11) 0.43364(10) 0.0172(4) Uani 1 1 d . . . . .
O3 O 0.55838(11) 0.63533(11) 0.67770(10) 0.0189(4) Uani 1 1 d . . . . .
N1 N 0.50319(13) 0.69235(13) 0.56221(12) 0.0157(5) Uani 1 1 d . . . . .
C12 C 0.32357(17) 0.74184(16) 0.55739(15) 0.0214(7) Uani 1 1 d . . . . .
H12 H 0.3320 0.7824 0.5333 0.026 Uiso 1 1 calc R . . . .
C8 C 0.60815(17) 0.71647(16) 0.74833(15) 0.0205(6) Uani 1 1 d . . . . .
H8 H 0.6060 0.6841 0.7825 0.025 Uiso 1 1 calc R . . . .
C7 C 0.63456(17) 0.78090(17) 0.75977(15) 0.0233(7) Uani 1 1 d . . . . .
H7 H 0.6508 0.7918 0.8017 0.028 Uiso 1 1 calc R . . . .
C4 C 0.58924(16) 0.74618(16) 0.63660(14) 0.0191(6) Uani 1 1 d . . . . .
C2AA C 0.4451(2) 0.5902(2) 0.8764(2) 0.0385(9) Uani 1 1 d . . . . .
C2 C 0.48893(16) 0.67665(15) 0.49351(14) 0.0168(6) Uani 1 1 d . . . . .
H2A H 0.5324 0.6757 0.4690 0.020 Uiso 1 1 calc R . . . .
H2B H 0.4596 0.7130 0.4749 0.020 Uiso 1 1 calc R . . . .
C9 C 0.58448(15) 0.69822(16) 0.68690(15) 0.0180(6) Uani 1 1 d . . . . .
C11 C 0.37819(16) 0.70936(16) 0.58741(15) 0.0192(6) Uani 1 1 d . . . . .
C3 C 0.57092(16) 0.72744(15) 0.56822(15) 0.0186(6) Uani 1 1 d . . . . .
H3A H 0.5702 0.7696 0.5417 0.022 Uiso 1 1 calc R . . . .
H3B H 0.6069 0.6970 0.5506 0.022 Uiso 1 1 calc R . . . .
C16 C 0.36632(16) 0.64947(15) 0.62327(16) 0.0193(6) Uani 1 1 d . . . . .
C10 C 0.44876(16) 0.73950(16) 0.58785(15) 0.0191(6) Uani 1 1 d . . . . .
H10A H 0.4607 0.7524 0.6327 0.023 Uiso 1 1 calc R . . . .
H10B H 0.4486 0.7819 0.5616 0.023 Uiso 1 1 calc R . . . .
C15 C 0.29994(17) 0.62380(17) 0.62817(16) 0.0238(7) Uani 1 1 d . . . . .
H15 H 0.2914 0.5833 0.6523 0.029 Uiso 1 1 calc R . . . .
C14 C 0.24648(17) 0.65752(18) 0.59773(16) 0.0258(7) Uani 1 1 d . . . . .
H14 H 0.2015 0.6396 0.6018 0.031 Uiso 1 1 calc R . . . .
C13 C 0.25628(17) 0.71671(17) 0.56145(16) 0.0238(7) Uani 1 1 d . . . . .
C1 C 0.45356(15) 0.60854(15) 0.48739(14) 0.0164(6) Uani 1 1 d . . . . .
C13C C 0.12961(19) 0.7159(2) 0.5316(2) 0.0404(9) Uani 1 1 d . . . . .
H13A H 0.1362 0.6717 0.5101 0.061 Uiso 1 1 calc GR . . . .
H13B H 0.0939 0.7419 0.5091 0.061 Uiso 1 1 calc GR . . . .
H13C H 0.1157 0.7082 0.5765 0.061 Uiso 1 1 calc GR . . . .
C7AA C 0.4074(3) 0.5553(2) 0.9224(2) 0.0500(12) Uani 1 1 d . . . . .
H7AA H 0.4118 0.5671 0.9667 0.060 Uiso 1 1 calc R . . . .
C13D C 0.2141(2) 0.7726(2) 0.45937(19) 0.0357(9) Uani 1 1 d . . . . .
H13D H 0.2564 0.7995 0.4572 0.053 Uiso 1 1 calc GR . . . .
H13E H 0.1764 0.7989 0.4402 0.053 Uiso 1 1 calc GR . . . .
H13F H 0.2201 0.7297 0.4355 0.053 Uiso 1 1 calc GR . . . .
C13B C 0.1877(2) 0.8233(2) 0.5673(2) 0.0406(10) Uani 1 1 d . . . . .
H13G H 0.1775 0.8131 0.6126 0.061 Uiso 1 1 calc GR . . . .
H13H H 0.1496 0.8492 0.5484 0.061 Uiso 1 1 calc GR . . . .
H13I H 0.2298 0.8505 0.5646 0.061 Uiso 1 1 calc GR . . . .
C13A C 0.19721(18) 0.75653(19) 0.53023(18) 0.0294(8) Uani 1 1 d . . . . .
C1AA C 0.4936(3) 0.6466(3) 0.8961(2) 0.0581(13) Uani 1 1 d . . . . .
H1AA H 0.4798 0.6647 0.9383 0.087 Uiso 1 1 calc GR . . . .
H1AB H 0.4921 0.6835 0.8640 0.087 Uiso 1 1 calc GR . . . .
H1AC H 0.5402 0.6284 0.8989 0.087 Uiso 1 1 calc GR . . . .
C3AA C 0.4377(2) 0.5725(3) 0.8123(2) 0.0513(12) Uani 1 1 d . . . . .
H3AA H 0.4625 0.5967 0.7801 0.062 Uiso 1 1 calc R . . . .
C4AA C 0.3947(3) 0.5199(3) 0.7945(2) 0.0597(14) Uani 1 1 d . . . . .
H4AA H 0.3908 0.5077 0.7503 0.072 Uiso 1 1 calc R . . . .
C5AA C 0.3574(3) 0.4849(3) 0.8398(3) 0.0620(14) Uani 1 1 d . . . . .
H5AA H 0.3279 0.4485 0.8275 0.074 Uiso 1 1 calc R . . . .
C6AA C 0.3640(3) 0.5040(3) 0.9046(3) 0.0641(15) Uani 1 1 d . . . . .
H6AA H 0.3378 0.4810 0.9366 0.077 Uiso 1 1 calc R . . . .
C1BB C 0.5208(3) 0.8972(5) 0.4522(6) 0.095(6) Uani 0.492(8) 1 d . . . A 1
H1BA H 0.5255 0.8553 0.4266 0.143 Uiso 0.492(8) 1 calc GR . . A 1
H1BB H 0.5431 0.8908 0.4942 0.143 Uiso 0.492(8) 1 calc GR . . A 1
H1BC H 0.5425 0.9354 0.4293 0.143 Uiso 0.492(8) 1 calc GR . . A 1
C2BB C 0.4460(3) 0.9127(3) 0.4623(3) 0.045(3) Uani 0.492(8) 1 d G . . A 1
C7BB C 0.4011(4) 0.9181(4) 0.4098(3) 0.062(5) Uani 0.492(8) 1 d G . . A 1
H7BB H 0.4180 0.9107 0.3673 0.074 Uiso 0.492(8) 1 calc R . . A 1
C6BB C 0.3320(4) 0.9339(4) 0.4188(4) 0.060(3) Uani 0.492(8) 1 d G . . A 1
H6BD H 0.3023 0.9372 0.3826 0.072 Uiso 0.492(8) 1 calc R . . A 1
C5BB C 0.3065(3) 0.9449(3) 0.4809(4) 0.065(4) Uani 0.492(8) 1 d G . . A 1
H5BB H 0.2596 0.9559 0.4872 0.077 Uiso 0.492(8) 1 calc R . . A 1
C4BB C 0.3507(4) 0.9395(4) 0.5338(3) 0.082(6) Uani 0.492(8) 1 d G . . A 1
H4BB H 0.3337 0.9467 0.5762 0.099 Uiso 0.492(8) 1 calc R . . A 1
C3BB C 0.4196(4) 0.9236(4) 0.5244(3) 0.059(4) Uani 0.492(8) 1 d G . . A 1
H3BB H 0.4492 0.9201 0.5607 0.071 Uiso 0.492(8) 1 calc R . . A 1
C1BA C 0.5214(2) 0.8988(2) 0.38755(10) 0.081(4) Uani 0.508(8) 1 d . . . A 2
H1BD H 0.5226 0.8498 0.3775 0.121 Uiso 0.508(8) 1 calc GR . . A 2
H1BE H 0.5666 0.9135 0.4027 0.121 Uiso 0.508(8) 1 calc GR . . A 2
H1BF H 0.5092 0.9246 0.3486 0.121 Uiso 0.508(8) 1 calc GR . . A 2
C2BA C 0.4690(2) 0.9120(2) 0.43951(13) 0.058(4) Uani 0.508(8) 1 d G . . A 2
C7BA C 0.3989(2) 0.9142(2) 0.42500(17) 0.057(4) Uani 0.508(8) 1 d G . . A 2
H7BA H 0.3842 0.9062 0.3819 0.069 Uiso 0.508(8) 1 calc R . . A 2
C6BA C 0.35043(19) 0.9280(2) 0.4727(2) 0.075(4) Uani 0.508(8) 1 d G . . A 2
H6BE H 0.3032 0.9295 0.4620 0.090 Uiso 0.508(8) 1 calc R . . A 2
C5BA C 0.37124(15) 0.9397(2) 0.53632(19) 0.079(6) Uani 0.508(8) 1 d G . . A 2
H5BA H 0.3383 0.9491 0.5689 0.094 Uiso 0.508(8) 1 calc R . . A 2
C4BA C 0.44086(14) 0.93747(17) 0.55162(15) 0.076(4) Uani 0.508(8) 1 d G . . A 2
H4BA H 0.4554 0.9453 0.5947 0.092 Uiso 0.508(8) 1 calc R . . A 2
C3BA C 0.48915(16) 0.92367(16) 0.50356(13) 0.059(3) Uani 0.508(8) 1 d G . . A 2
H3BA H 0.5364 0.9222 0.5144 0.071 Uiso 0.508(8) 1 calc R . . A 2
C5 C 0.61501(10) 0.81139(8) 0.65013(9) 0.0197(6) Uani 1 1 d G . . . .
H5 H 0.6169 0.8441 0.6162 0.024 Uiso 1 1 calc R . . . .
C6 C 0.63796(9) 0.83049(7) 0.71112(8) 0.0219(7) Uani 1 1 d G . . . .
C6A C 0.66700(8) 0.90210(8) 0.72466(7) 0.0274(8) Uani 1 1 d G . . . .
C6D C 0.74365(8) 0.89621(12) 0.73880(10) 0.0388(9) Uani 1 1 d G . . . .
H6DA H 0.7507 0.8663 0.7762 0.058 Uiso 1 1 calc GR . . . .
H6DB H 0.7623 0.9417 0.7482 0.058 Uiso 1 1 calc GR . . . .
H6DC H 0.7671 0.8769 0.7011 0.058 Uiso 1 1 calc GR . . . .
C6C C 0.65686(11) 0.95064(8) 0.66770(9) 0.0402(10) Uani 1 1 d G . . . .
H6CA H 0.6798 0.9320 0.6295 0.060 Uiso 1 1 calc GR . . . .
H6CB H 0.6764 0.9955 0.6782 0.060 Uiso 1 1 calc GR . . . .
H6CC H 0.6078 0.9556 0.6588 0.060 Uiso 1 1 calc GR . . . .
C6B C 0.62955(11) 0.93363(12) 0.78351(8) 0.0340(8) Uani 1 1 d G . . . .
H6BA H 0.5804 0.9365 0.7744 0.051 Uiso 1 1 calc GR . . . .
H6BB H 0.6475 0.9796 0.7918 0.051 Uiso 1 1 calc GR . . . .
H6BC H 0.6370 0.9047 0.8215 0.051 Uiso 1 1 calc GR . . . .
C1CA C 0.2625(2) 0.8305(4) 0.2908(3) 0.099(4) Uani 0.727(9) 1 d . . . B 1
H1CA H 0.2578 0.8753 0.3118 0.149 Uiso 0.727(9) 1 calc GR . . B 1
H1CB H 0.2376 0.7960 0.3159 0.149 Uiso 0.727(9) 1 calc GR . . B 1
H1CC H 0.2435 0.8328 0.2471 0.149 Uiso 0.727(9) 1 calc GR . . B 1
C4CA C 0.4431(2) 0.8332(3) 0.2332(3) 0.064(2) Uani 0.727(9) 1 d G . . B 1
H4CA H 0.4703 0.8593 0.2043 0.076 Uiso 0.727(9) 1 calc R . . B 1
C3CA C 0.3744(2) 0.8501(2) 0.2446(2) 0.0504(18) Uani 0.727(9) 1 d G . . B 1
H3CA H 0.3548 0.8882 0.2229 0.060 Uiso 0.727(9) 1 calc R . . B 1
C8CA C 0.33443(18) 0.8120(2) 0.28744(18) 0.0494(18) Uani 0.727(9) 1 d G . . B 1
C7CA C 0.3626(2) 0.7559(2) 0.3197(2) 0.0512(19) Uani 0.727(9) 1 d G . . B 1
H7CA H 0.3355 0.7300 0.3489 0.061 Uiso 0.727(9) 1 calc R . . B 1
C6CA C 0.4308(3) 0.7382(3) 0.3086(3) 0.067(2) Uani 0.727(9) 1 d G . . B 1
H6CD H 0.4503 0.7000 0.3302 0.080 Uiso 0.727(9) 1 calc R . . B 1
C5CA C 0.4705(2) 0.7765(3) 0.2658(3) 0.081(3) Uani 0.727(9) 1 d G . . B 1
H5CA H 0.5169 0.7640 0.2586 0.097 Uiso 0.727(9) 1 calc R . . B 1
C1CB C 0.4457(9) 0.8742(8) 0.1989(7) 0.061(3) Uani 0.273(9) 1 d . . . B 2
H1CD H 0.4089 0.9010 0.1789 0.092 Uiso 0.273(9) 1 calc GR . . B 2
H1CE H 0.4695 0.8476 0.1657 0.092 Uiso 0.273(9) 1 calc GR . . B 2
H1CF H 0.4782 0.9052 0.2200 0.092 Uiso 0.273(9) 1 calc GR . . B 2
C2CB C 0.4156(6) 0.8262(6) 0.2483(5) 0.061(3) Uani 0.273(9) 1 d G . . B 2
C7CB C 0.3450(6) 0.8261(7) 0.2612(6) 0.061(3) Uani 0.273(9) 1 d G . . B 2
H7CB H 0.3158 0.8559 0.2377 0.073 Uiso 0.273(9) 1 calc R . . B 2
C6CB C 0.3172(6) 0.7828(9) 0.3080(6) 0.061(3) Uani 0.273(9) 1 d G . . B 2
H6CE H 0.2693 0.7835 0.3162 0.073 Uiso 0.273(9) 1 calc R . . B 2
C5CB C 0.3595(8) 0.7386(8) 0.3429(6) 0.061(3) Uani 0.273(9) 1 d G . . B 2
H5CB H 0.3406 0.7092 0.3748 0.073 Uiso 0.273(9) 1 calc R . . B 2
C4CB C 0.4298(8) 0.7380(9) 0.3304(8) 0.061(3) Uani 0.273(9) 1 d G . . B 2
H4CB H 0.4589 0.7080 0.3539 0.073 Uiso 0.273(9) 1 calc R . . B 2
C3CB C 0.4574(6) 0.7814(9) 0.2836(7) 0.061(3) Uani 0.273(9) 1 d G . . B 2
H3CB H 0.5052 0.7806 0.2755 0.073 Uiso 0.273(9) 1 calc R . . B 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
Ti1 O4 1.865(2) . ?
Ti1 O1 2.027(2) . ?
Ti1 O5 1.8198(10) . ?
Ti1 O2 2.093(2) 3_566 ?
Ti1 O3 1.843(2) . ?
Ti1 N1 2.346(3) . ?
O4 C16 1.343(4) . ?
O1 C1 1.265(4) . ?
O5 Ti1 1.8198(10) 2_665 ?
O2 Ti1 2.093(2) 4_656 ?
O2 C1 1.259(4) . ?
O3 C9 1.343(4) . ?
N1 C2 1.482(4) . ?
N1 C3 1.495(4) . ?
N1 C10 1.503(4) . ?
C12 H12 0.9500 . ?
C12 C11 1.388(4) . ?
C12 C13 1.405(5) . ?
C8 H8 0.9500 . ?
C8 C7 1.380(5) . ?
C8 C9 1.400(4) . ?
C7 H7 0.9500 . ?
C7 C6 1.399(4) . ?
C4 C9 1.404(4) . ?
C4 C3 1.506(4) . ?
C4 C5 1.398(3) . ?
C2AA C7AA 1.385(6) . ?
C2AA C1AA 1.508(7) . ?
C2AA C3AA 1.380(7) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C1 1.504(4) . ?
C11 C16 1.405(5) . ?
C11 C10 1.499(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C16 C15 1.394(4) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C15 H15 0.9500 . ?
C15 C14 1.386(5) . ?
C14 H14 0.9500 . ?
C14 C13 1.392(5) . ?
C13 C13A 1.534(5) . ?
C13C H13A 0.9800 . ?
C13C H13B 0.9800 . ?
C13C H13C 0.9800 . ?
C13C C13A 1.541(5) . ?
C7AA H7AA 0.9500 . ?
C7AA C6AA 1.362(8) . ?
C13D H13D 0.9800 . ?
C13D H13E 0.9800 . ?
C13D H13F 0.9800 . ?
C13D C13A 1.537(5) . ?
C13B H13G 0.9800 . ?
C13B H13H 0.9800 . ?
C13B H13I 0.9800 . ?
C13B C13A 1.525(5) . ?
C1AA H1AA 0.9800 . ?
C1AA H1AB 0.9800 . ?
C1AA H1AC 0.9800 . ?
C3AA H3AA 0.9500 . ?
C3AA C4AA 1.377(8) . ?
C4AA H4AA 0.9500 . ?
C4AA C5AA 1.370(7) . ?
C5AA H5AA 0.9500 . ?
C5AA C6AA 1.399(7) . ?
C6AA H6AA 0.9500 . ?
C1BB H1BA 0.9800 . ?
C1BB H1BB 0.9800 . ?
C1BB H1BC 0.9800 . ?
C1BB C2BB 1.5078 . ?
C2BB C7BB 1.4015 . ?
C2BB C3BB 1.4018 . ?
C7BB H7BB 0.9500 . ?
C7BB C6BB 1.3968 . ?
C6BB H6BD 0.9500 . ?
C6BB C5BB 1.3961 . ?
C5BB H5BB 0.9500 . ?
C5BB C4BB 1.3973 . ?
C4BB H4BB 0.9500 . ?
C4BB C3BB 1.3962 . ?
C3BB H3BB 0.9500 . ?
C1BA H1BD 0.9800 . ?
C1BA H1BE 0.9800 . ?
C1BA H1BF 0.9800 . ?
C1BA C2BA 1.5075 . ?
C2BA C7BA 1.4017 . ?
C2BA C3BA 1.4026 . ?
C7BA H7BA 0.9500 . ?
C7BA C6BA 1.3960 . ?
C6BA H6BE 0.9500 . ?
C6BA C5BA 1.3969 . ?
C5BA H5BA 0.9500 . ?
C5BA C4BA 1.3968 . ?
C4BA H4BA 0.9500 . ?
C4BA C3BA 1.3976 . ?
C3BA H3BA 0.9500 . ?
C5 H5 0.9500 . ?
C5 C6 1.3915 . ?
C6 C6A 1.5350 . ?
C6A C6D 1.5296 . ?
C6A C6C 1.5264 . ?
C6A C6B 1.5493 . ?
C6D H6DA 0.9800 . ?
C6D H6DB 0.9800 . ?
C6D H6DC 0.9800 . ?
C6C H6CA 0.9800 . ?
C6C H6CB 0.9800 . ?
C6C H6CC 0.9800 . ?
C6B H6BA 0.9800 . ?
C6B H6BB 0.9800 . ?
C6B H6BC 0.9800 . ?
C1CA H1CA 0.9800 . ?
C1CA H1CB 0.9800 . ?
C1CA H1CC 0.9800 . ?
C1CA C8CA 1.4526 . ?
C4CA H4CA 0.9500 . ?
C4CA C3CA 1.4016 . ?
C4CA C5CA 1.4025 . ?
C3CA H3CA 0.9500 . ?
C3CA C8CA 1.3972 . ?
C8CA C7CA 1.3954 . ?
C7CA H7CA 0.9500 . ?
C7CA C6CA 1.3963 . ?
C6CA H6CD 0.9500 . ?
C6CA C5CA 1.3947 . ?
C5CA H5CA 0.9500 . ?
C1CB H1CD 0.9800 . ?
C1CB H1CE 0.9800 . ?
C1CB H1CF 0.9800 . ?
C1CB C2CB 1.5072 . ?
C2CB C7CB 1.4030 . ?
C2CB C3CB 1.4018 . ?
C7CB H7CB 0.9500 . ?
C7CB C6CB 1.3964 . ?
C6CB H6CE 0.9500 . ?
C6CB C5CB 1.3958 . ?
C5CB H5CB 0.9500 . ?
C5CB C4CB 1.3973 . ?
C4CB H4CB 0.9500 . ?
C4CB C3CB 1.3968 . ?
C3CB H3CB 0.9500 . ?

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
O4 Ti1 O1 85.25(9) . . ?
O4 Ti1 O2 166.82(9) . 3_566 ?
O4 Ti1 N1 85.48(9) . . ?
O1 Ti1 O2 86.43(8) . 3_566 ?
O1 Ti1 N1 73.57(8) . . ?
O5 Ti1 O4 98.86(8) . . ?
O5 Ti1 O1 93.48(10) . . ?
O5 Ti1 O2 91.82(8) . 3_566 ?
O5 Ti1 O3 107.52(10) . . ?
O5 Ti1 N1 166.04(11) . . ?
O2 Ti1 N1 82.38(8) 3_566 . ?
O3 Ti1 O4 97.59(10) . . ?
O3 Ti1 O1 158.00(9) . . ?
O3 Ti1 O2 86.42(9) . 3_566 ?
O3 Ti1 N1 84.88(9) . . ?
C16 O4 Ti1 130.86(19) . . ?
C1 O1 Ti1 124.83(19) . . ?
Ti1 O5 Ti1 146.19(18) 2_665 . ?
C1 O2 Ti1 137.7(2) . 4_656 ?
C9 O3 Ti1 139.6(2) . . ?
C2 N1 Ti1 108.22(18) . . ?
C2 N1 C3 109.9(2) . . ?
C2 N1 C10 109.5(2) . . ?
C3 N1 Ti1 110.50(18) . . ?
C3 N1 C10 108.4(2) . . ?
C10 N1 Ti1 110.31(18) . . ?
C11 C12 H12 118.9 . . ?
C11 C12 C13 122.2(3) . . ?
C13 C12 H12 118.9 . . ?
C7 C8 H8 119.6 . . ?
C7 C8 C9 120.8(3) . . ?
C9 C8 H8 119.6 . . ?
C8 C7 H7 119.2 . . ?
C8 C7 C6 121.7(3) . . ?
C6 C7 H7 119.2 . . ?
C9 C4 C3 121.3(3) . . ?
C5 C4 C9 118.9(3) . . ?
C5 C4 C3 119.7(2) . . ?
C7AA C2AA C1AA 120.5(4) . . ?
C3AA C2AA C7AA 118.9(4) . . ?
C3AA C2AA C1AA 120.7(4) . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
N1 C2 C1 110.5(2) . . ?
H2A C2 H2B 108.1 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
O3 C9 C8 119.1(3) . . ?
O3 C9 C4 122.0(3) . . ?
C8 C9 C4 118.9(3) . . ?
C12 C11 C16 119.4(3) . . ?
C12 C11 C10 122.0(3) . . ?
C16 C11 C10 118.4(3) . . ?
N1 C3 C4 113.6(2) . . ?
N1 C3 H3A 108.9 . . ?
N1 C3 H3B 108.9 . . ?
C4 C3 H3A 108.9 . . ?
C4 C3 H3B 108.9 . . ?
H3A C3 H3B 107.7 . . ?
O4 C16 C11 119.4(3) . . ?
O4 C16 C15 121.2(3) . . ?
C15 C16 C11 119.4(3) . . ?
N1 C10 H10A 108.7 . . ?
N1 C10 H10B 108.7 . . ?
C11 C10 N1 114.0(2) . . ?
C11 C10 H10A 108.7 . . ?
C11 C10 H10B 108.7 . . ?
H10A C10 H10B 107.6 . . ?
C16 C15 H15 120.1 . . ?
C14 C15 C16 119.8(3) . . ?
C14 C15 H15 120.1 . . ?
C15 C14 H14 118.8 . . ?
C15 C14 C13 122.5(3) . . ?
C13 C14 H14 118.8 . . ?
C12 C13 C13A 120.1(3) . . ?
C14 C13 C12 116.8(3) . . ?
C14 C13 C13A 123.0(3) . . ?
O1 C1 C2 117.4(3) . . ?
O2 C1 O1 124.2(3) . . ?
O2 C1 C2 118.4(3) . . ?
H13A C13C H13B 109.5 . . ?
H13A C13C H13C 109.5 . . ?
H13B C13C H13C 109.5 . . ?
C13A C13C H13A 109.5 . . ?
C13A C13C H13B 109.5 . . ?
C13A C13C H13C 109.5 . . ?
C2AA C7AA H7AA 119.8 . . ?
C6AA C7AA C2AA 120.4(5) . . ?
C6AA C7AA H7AA 119.8 . . ?
H13D C13D H13E 109.5 . . ?
H13D C13D H13F 109.5 . . ?
H13E C13D H13F 109.5 . . ?
C13A C13D H13D 109.5 . . ?
C13A C13D H13E 109.5 . . ?
C13A C13D H13F 109.5 . . ?
H13G C13B H13H 109.5 . . ?
H13G C13B H13I 109.5 . . ?
H13H C13B H13I 109.5 . . ?
C13A C13B H13G 109.5 . . ?
C13A C13B H13H 109.5 . . ?
C13A C13B H13I 109.5 . . ?
C13 C13A C13C 112.0(3) . . ?
C13 C13A C13D 110.2(3) . . ?
C13D C13A C13C 107.8(3) . . ?
C13B C13A C13 108.3(3) . . ?
C13B C13A C13C 109.1(3) . . ?
C13B C13A C13D 109.4(3) . . ?
C2AA C1AA H1AA 109.5 . . ?
C2AA C1AA H1AB 109.5 . . ?
C2AA C1AA H1AC 109.5 . . ?
H1AA C1AA H1AB 109.5 . . ?
H1AA C1AA H1AC 109.5 . . ?
H1AB C1AA H1AC 109.5 . . ?
C2AA C3AA H3AA 119.7 . . ?
C4AA C3AA C2AA 120.5(4) . . ?
C4AA C3AA H3AA 119.7 . . ?
C3AA C4AA H4AA 119.5 . . ?
C5AA C4AA C3AA 120.9(5) . . ?
C5AA C4AA H4AA 119.5 . . ?
C4AA C5AA H5AA 120.9 . . ?
C4AA C5AA C6AA 118.3(5) . . ?
C6AA C5AA H5AA 120.9 . . ?
C7AA C6AA C5AA 120.9(5) . . ?
C7AA C6AA H6AA 119.5 . . ?
C5AA C6AA H6AA 119.5 . . ?
H1BA C1BB H1BB 109.5 . . ?
H1BA C1BB H1BC 109.5 . . ?
H1BB C1BB H1BC 109.5 . . ?
C2BB C1BB H1BA 109.5 . . ?
C2BB C1BB H1BB 109.5 . . ?
C2BB C1BB H1BC 109.5 . . ?
C7BB C2BB C1BB 120.9 . . ?
C7BB C2BB C3BB 118.2 . . ?
C3BB C2BB C1BB 120.9 . . ?
C2BB C7BB H7BB 119.5 . . ?
C6BB C7BB C2BB 121.0 . . ?
C6BB C7BB H7BB 119.5 . . ?
C7BB C6BB H6BD 119.9 . . ?
C5BB C6BB C7BB 120.2 . . ?
C5BB C6BB H6BD 119.9 . . ?
C6BB C5BB H5BB 120.3 . . ?
C6BB C5BB C4BB 119.4 . . ?
C4BB C5BB H5BB 120.3 . . ?
C5BB C4BB H4BB 119.9 . . ?
C3BB C4BB C5BB 120.2 . . ?
C3BB C4BB H4BB 119.9 . . ?
C2BB C3BB H3BB 119.5 . . ?
C4BB C3BB C2BB 121.0 . . ?
C4BB C3BB H3BB 119.5 . . ?
H1BD C1BA H1BE 109.5 . . ?
H1BD C1BA H1BF 109.5 . . ?
H1BE C1BA H1BF 109.5 . . ?
C2BA C1BA H1BD 109.5 . . ?
C2BA C1BA H1BE 109.5 . . ?
C2BA C1BA H1BF 109.5 . . ?
C7BA C2BA C1BA 121.0 . . ?
C7BA C2BA C3BA 118.1 . . ?
C3BA C2BA C1BA 120.8 . . ?
C2BA C7BA H7BA 119.4 . . ?
C6BA C7BA C2BA 121.1 . . ?
C6BA C7BA H7BA 119.4 . . ?
C7BA C6BA H6BE 119.9 . . ?
C7BA C6BA C5BA 120.1 . . ?
C5BA C6BA H6BE 119.9 . . ?
C6BA C5BA H5BA 120.3 . . ?
C4BA C5BA C6BA 119.5 . . ?
C4BA C5BA H5BA 120.3 . . ?
C5BA C4BA H4BA 120.0 . . ?
C5BA C4BA C3BA 120.1 . . ?
C3BA C4BA H4BA 120.0 . . ?
C2BA C3BA H3BA 119.5 . . ?
C4BA C3BA C2BA 121.1 . . ?
C4BA C3BA H3BA 119.5 . . ?
C4 C5 H5 118.6 . . ?
C6 C5 C4 122.84(16) . . ?
C6 C5 H5 118.6 . . ?
C7 C6 C6A 121.10(16) . . ?
C5 C6 C7 116.94(16) . . ?
C5 C6 C6A 121.9 . . ?
C6 C6A C6B 109.4 . . ?
C6D C6A C6 109.2 . . ?
C6D C6A C6B 109.9 . . ?
C6C C6A C6 112.1 . . ?
C6C C6A C6D 108.8 . . ?
C6C C6A C6B 107.5 . . ?
C6A C6D H6DA 109.5 . . ?
C6A C6D H6DB 109.5 . . ?
C6A C6D H6DC 109.5 . . ?
H6DA C6D H6DB 109.5 . . ?
H6DA C6D H6DC 109.5 . . ?
H6DB C6D H6DC 109.5 . . ?
C6A C6C H6CA 109.5 . . ?
C6A C6C H6CB 109.5 . . ?
C6A C6C H6CC 109.5 . . ?
H6CA C6C H6CB 109.5 . . ?
H6CA C6C H6CC 109.5 . . ?
H6CB C6C H6CC 109.5 . . ?
C6A C6B H6BA 109.5 . . ?
C6A C6B H6BB 109.5 . . ?
C6A C6B H6BC 109.5 . . ?
H6BA C6B H6BB 109.5 . . ?
H6BA C6B H6BC 109.5 . . ?
H6BB C6B H6BC 109.5 . . ?
H1CA C1CA H1CB 109.5 . . ?
H1CA C1CA H1CC 109.5 . . ?
H1CB C1CA H1CC 109.5 . . ?
C8CA C1CA H1CA 109.5 . . ?
C8CA C1CA H1CB 109.5 . . ?
C8CA C1CA H1CC 109.5 . . ?
C3CA C4CA H4CA 121.0 . . ?
C3CA C4CA C5CA 118.1 . . ?
C5CA C4CA H4CA 121.0 . . ?
C4CA C3CA H3CA 119.5 . . ?
C8CA C3CA C4CA 121.1 . . ?
C8CA C3CA H3CA 119.5 . . ?
C3CA C8CA C1CA 116.0 . . ?
C7CA C8CA C1CA 123.6 . . ?
C7CA C8CA C3CA 120.1 . . ?
C8CA C7CA H7CA 120.3 . . ?
C8CA C7CA C6CA 119.4 . . ?
C6CA C7CA H7CA 120.3 . . ?
C7CA C6CA H6CD 119.9 . . ?
C5CA C6CA C7CA 120.2 . . ?
C5CA C6CA H6CD 119.9 . . ?
C4CA C5CA H5CA 119.5 . . ?
C6CA C5CA C4CA 121.1 . . ?
C6CA C5CA H5CA 119.5 . . ?
H1CD C1CB H1CE 109.5 . . ?
H1CD C1CB H1CF 109.5 . . ?
H1CE C1CB H1CF 109.5 . . ?
C2CB C1CB H1CD 109.5 . . ?
C2CB C1CB H1CE 109.5 . . ?
C2CB C1CB H1CF 109.5 . . ?
C7CB C2CB C1CB 120.9 . . ?
C3CB C2CB C1CB 120.9 . . ?
C3CB C2CB C7CB 118.2 . . ?
C2CB C7CB H7CB 119.5 . . ?
C6CB C7CB C2CB 121.0 . . ?
C6CB C7CB H7CB 119.5 . . ?
C7CB C6CB H6CE 119.9 . . ?
C5CB C6CB C7CB 120.2 . . ?
C5CB C6CB H6CE 119.9 . . ?
C6CB C5CB H5CB 120.3 . . ?
C6CB C5CB C4CB 119.5 . . ?
C4CB C5CB H5CB 120.3 . . ?
C5CB C4CB H4CB 119.9 . . ?
C3CB C4CB C5CB 120.1 . . ?
C3CB C4CB H4CB 119.9 . . ?
C2CB C3CB H3CB 119.5 . . ?
C4CB C3CB C2CB 121.1 . . ?
C4CB C3CB H3CB 119.5 . . ?

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
Ti1 O4 C16 C11 -52.2(4) . . . . ?
Ti1 O4 C16 C15 128.0(3) . . . . ?
Ti1 O1 C1 O2 170.8(2) . . . . ?
Ti1 O1 C1 C2 -9.2(4) . . . . ?
Ti1 O2 C1 O1 -32.0(5) 4_656 . . . ?
Ti1 O2 C1 C2 148.0(2) 4_656 . . . ?
Ti1 O3 C9 C8 161.0(2) . . . . ?
Ti1 O3 C9 C4 -19.5(5) . . . . ?
Ti1 N1 C2 C1 21.8(3) . . . . ?
Ti1 N1 C3 C4 -61.3(3) . . . . ?
Ti1 N1 C10 C11 -56.3(3) . . . . ?
O4 Ti1 O5 Ti1 115.34(7) . . . 2_665 ?
O4 Ti1 O3 C9 -81.5(3) . . . . ?
O4 C16 C15 C14 179.7(3) . . . . ?
O1 Ti1 O4 C16 -33.1(3) . . . . ?
O1 Ti1 O5 Ti1 29.61(6) . . . 2_665 ?
O1 Ti1 O3 C9 14.6(5) . . . . ?
O5 Ti1 O4 C16 -125.9(3) . . . . ?
O5 Ti1 O3 C9 176.7(3) . . . . ?
O2 Ti1 O4 C16 17.9(6) 3_566 . . . ?
O2 Ti1 O5 Ti1 -56.92(6) 3_566 . . 2_665 ?
O2 Ti1 O3 C9 85.9(3) 3_566 . . . ?
O3 Ti1 O4 C16 124.9(3) . . . . ?
O3 Ti1 O5 Ti1 -143.74(8) . . . 2_665 ?
N1 Ti1 O4 C16 40.7(3) . . . . ?
N1 Ti1 O5 Ti1 8.1(3) . . . 2_665 ?
N1 Ti1 O3 C9 3.2(3) . . . . ?
N1 C2 C1 O1 -11.2(4) . . . . ?
N1 C2 C1 O2 168.7(3) . . . . ?
C12 C11 C16 O4 -179.9(3) . . . . ?
C12 C11 C16 C15 -0.1(5) . . . . ?
C12 C11 C10 N1 -125.4(3) . . . . ?
C12 C13 C13A C13C 171.9(3) . . . . ?
C12 C13 C13A C13D 51.9(4) . . . . ?
C12 C13 C13A C13B -67.7(4) . . . . ?
C8 C7 C6 C5 -1.5(4) . . . . ?
C8 C7 C6 C6A 179.6(2) . . . . ?
C7 C8 C9 O3 -179.2(3) . . . . ?
C7 C8 C9 C4 1.2(5) . . . . ?
C7 C6 C6A C6D 67.2(2) . . . . ?
C7 C6 C6A C6C -172.2(2) . . . . ?
C7 C6 C6A C6B -53.1(2) . . . . ?
C4 C5 C6 C7 0.2(2) . . . . ?
C4 C5 C6 C6A 179.1(2) . . . . ?
C2AA C7AA C6AA C5AA 1.1(9) . . . . ?
C2AA C3AA C4AA C5AA 1.2(8) . . . . ?
C2 N1 C3 C4 179.3(2) . . . . ?
C2 N1 C10 C11 62.6(3) . . . . ?
C9 C8 C7 C6 0.8(5) . . . . ?
C9 C4 C3 N1 49.3(4) . . . . ?
C9 C4 C5 C6 1.7(3) . . . . ?
C11 C12 C13 C14 0.6(5) . . . . ?
C11 C12 C13 C13A 176.9(3) . . . . ?
C11 C16 C15 C14 0.0(5) . . . . ?
C3 N1 C2 C1 142.6(2) . . . . ?
C3 N1 C10 C11 -177.4(3) . . . . ?
C3 C4 C9 O3 -5.4(5) . . . . ?
C3 C4 C9 C8 174.1(3) . . . . ?
C3 C4 C5 C6 -174.87(19) . . . . ?
C16 C11 C10 N1 60.1(4) . . . . ?
C16 C15 C14 C13 0.5(5) . . . . ?
C10 N1 C2 C1 -98.5(3) . . . . ?
C10 N1 C3 C4 59.7(3) . . . . ?
C10 C11 C16 O4 -5.3(4) . . . . ?
C10 C11 C16 C15 174.5(3) . . . . ?
C15 C14 C13 C12 -0.7(5) . . . . ?
C15 C14 C13 C13A -176.9(3) . . . . ?
C14 C13 C13A C13C -12.0(5) . . . . ?
C14 C13 C13A C13D -132.0(3) . . . . ?
C14 C13 C13A C13B 108.4(4) . . . . ?
C13 C12 C11 C16 -0.2(5) . . . . ?
C13 C12 C11 C10 -174.6(3) . . . . ?
C7AA C2AA C3AA C4AA -1.4(7) . . . . ?
C1AA C2AA C7AA C6AA -179.5(5) . . . . ?
C1AA C2AA C3AA C4AA 178.4(5) . . . . ?
C3AA C2AA C7AA C6AA 0.3(7) . . . . ?
C3AA C4AA C5AA C6AA 0.2(9) . . . . ?
C4AA C5AA C6AA C7AA -1.3(9) . . . . ?
C1BB C2BB C7BB C6BB -178.6 . . . . ?
C1BB C2BB C3BB C4BB 178.5 . . . . ?
C2BB C7BB C6BB C5BB 0.1 . . . . ?
C7BB C2BB C3BB C4BB -0.2 . . . . ?
C7BB C6BB C5BB C4BB -0.3 . . . . ?
C6BB C5BB C4BB C3BB 0.3 . . . . ?
C5BB C4BB C3BB C2BB 0.0 . . . . ?
C3BB C2BB C7BB C6BB 0.2 . . . . ?
C1BA C2BA C7BA C6BA -178.4 . . . . ?
C1BA C2BA C3BA C4BA 178.5 . . . . ?
C2BA C7BA C6BA C5BA -0.2 . . . . ?
C7BA C2BA C3BA C4BA -0.2 . . . . ?
C7BA C6BA C5BA C4BA 0.0 . . . . ?
C6BA C5BA C4BA C3BA 0.0 . . . . ?
C5BA C4BA C3BA C2BA 0.1 . . . . ?
C3BA C2BA C7BA C6BA 0.3 . . . . ?
C5 C4 C9 O3 178.1(3) . . . . ?
C5 C4 C9 C8 -2.4(4) . . . . ?
C5 C4 C3 N1 -134.2(3) . . . . ?
C5 C6 C6A C6D -111.6 . . . . ?
C5 C6 C6A C6C 9.0 . . . . ?
C5 C6 C6A C6B 128.1 . . . . ?
C1CA C8CA C7CA C6CA 173.9 . . . . ?
C4CA C3CA C8CA C1CA -174.6 . . . . ?
C4CA C3CA C8CA C7CA -0.1 . . . . ?
C3CA C4CA C5CA C6CA -0.3 . . . . ?
C3CA C8CA C7CA C6CA -0.2 . . . . ?
C8CA C7CA C6CA C5CA 0.2 . . . . ?
C7CA C6CA C5CA C4CA 0.0 . . . . ?
C5CA C4CA C3CA C8CA 0.3 . . . . ?
C1CB C2CB C7CB C6CB -178.5 . . . . ?
C1CB C2CB C3CB C4CB 178.5 . . . . ?
C2CB C7CB C6CB C5CB -0.1 . . . . ?
C7CB C2CB C3CB C4CB -0.2 . . . . ?
C7CB C6CB C5CB C4CB -0.1 . . . . ?
C6CB C5CB C4CB C3CB 0.2 . . . . ?
C5CB C4CB C3CB C2CB 0.0 . . . . ?
C3CB C2CB C7CB C6CB 0.3 . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_1ti_a1f_a5_a_sq
_database_code_depnum_ccdc_archive 'CCDC 1483655'
_audit_update_record             
;
2016-06-06 deposited with the CCDC.
2016-10-17 downloaded from the CCDC.
;
_audit_creation_date             2016-05-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C64 H48 F8 N4 O18 Ti4'
_chemical_formula_sum            'C64 H48 F8 N4 O18 Ti4'
_chemical_formula_weight         1504.66
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0080 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0130 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.3060 0.5280 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_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                   12.3528(5)
_cell_length_b                   28.6409(12)
_cell_length_c                   19.2930(8)
_cell_angle_alpha                90
_cell_angle_beta                 95.215(2)
_cell_angle_gamma                90
_cell_volume                     6797.5(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.85
_cell_measurement_theta_min      2.19
_shelx_estimated_absorpt_T_max   0.997
_shelx_estimated_absorpt_T_min   0.967
_exptl_absorpt_coefficient_mu    0.681
_exptl_absorpt_correction_T_max  0.7448
_exptl_absorpt_correction_T_min  0.5976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1407 before and 0.0873 after correction.
The Ratio of minimum to maximum transmission is 0.8024.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             3056
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.005
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1533
_diffrn_reflns_av_unetI/netI     0.0665
_diffrn_reflns_Laue_measured_fraction_full 0.584
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            107298
_diffrn_reflns_point_group_measured_fraction_full 0.584
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         22.885
_diffrn_reflns_theta_min         2.194
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.584
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'φ and ω shutterless scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_source                   'Advanced Light Source station 11.3.1'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5287
_reflns_number_total             7186
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_data_collection       'Bruker APEX2 Bruker-AXS, Madison WI'
_computing_cell_refinement       'SAINT V8.34A Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.34A Bruker-AXS, Madison WI'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     883
_refine_ls_number_reflns         7186
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0457
_refine_ls_restrained_S_all      1.017
_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)+(0.0250P)²+14.8570P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1101
_refine_special_details          SQUEEZE
# start Validation Reply Form
_vrf_THETM01_1ti_a1f_a5_a_sq     
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Data were trimmed to 0.9963 Ang resolution with Rmerge 0.1533 and
I/sig of 9.8. Data collected beyond this limit were too weak.
;
# end Validation Reply Form
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C50(H50A,H50B), C18(H18A,H18B), C58(H58A,H58B), C2(H2A,H2B), C34(H34A,H34B),
 C10(H10A,H10B), C51(H51A,H51B), C3(H3A,H3B), C26(H26A,H26B), C19(H19A,H19B),
 C42(H42A,H42B), C35(H35A,H35B)
2.b Aromatic/amide H refined with riding coordinates:
 C53(H53), C8(H8), C63(H63), C60(H60), C7(H7), C56(H56), C14(H14), C15(H15),
 C47(H47), C21(H21), C62(H62), C12(H12), C44(H44), C5(H5), C28(H28), C40(H40),
 C55(H55), C46(H46), C24(H24), C23(H23), C31(H31), C30(H30), C39(H39), C37(H37)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.51178(7) 0.36191(3) 0.58202(5) 0.0297(3) Uani 1 1 d . . . . .
Ti2 Ti 0.73701(8) 0.29363(3) 0.63019(5) 0.0328(3) Uani 1 1 d . . . . .
Ti3 Ti 0.58048(8) 0.36581(3) 0.86813(5) 0.0338(3) Uani 1 1 d . . . . .
Ti4 Ti 0.43705(8) 0.26374(3) 0.82085(5) 0.0304(3) Uani 1 1 d . . . . .
O1 O 0.4563(3) 0.32127(11) 0.65612(16) 0.0277(8) Uani 1 1 d . . . . .
F7 F -0.0230(3) 0.12463(12) 0.81376(16) 0.0534(9) Uani 1 1 d . . . . .
O2 O 0.3602(3) 0.30947(12) 0.74683(17) 0.0320(9) Uani 1 1 d . . . . .
O11 O 0.5759(3) 0.40514(11) 0.66336(19) 0.0320(9) Uani 1 1 d . . . . .
O4 O 0.4258(3) 0.32560(12) 0.51822(16) 0.0315(9) Uani 1 1 d . . . . .
O10 O 0.5412(3) 0.37783(11) 0.76691(17) 0.0296(8) Uani 1 1 d . . . . .
O16 O 0.6152(3) 0.24726(11) 0.65253(17) 0.0290(8) Uani 1 1 d . . . . .
O15 O 0.5572(3) 0.26008(11) 0.75674(17) 0.0288(8) Uani 1 1 d . . . . .
O6 O 0.7143(3) 0.32624(11) 0.72045(18) 0.0306(9) Uani 1 1 d . . . . .
F8 F 0.7439(3) 0.07003(12) 0.77258(17) 0.0602(10) Uani 1 1 d . . . . .
O17 O 0.3020(3) 0.25372(12) 0.85071(16) 0.0319(9) Uani 1 1 d . . . . .
O8 O 0.7777(3) 0.24810(12) 0.57233(17) 0.0360(9) Uani 1 1 d . . . . .
O18 O 0.5070(3) 0.21414(12) 0.86772(16) 0.0338(9) Uani 1 1 d . . . . .
O12 O 0.6571(3) 0.37161(12) 0.95340(18) 0.0399(10) Uani 1 1 d . . . . .
O7 O 0.7114(3) 0.32814(12) 0.83544(18) 0.0348(9) Uani 1 1 d . . . . .
O13 O 0.4778(3) 0.41145(12) 0.88315(18) 0.0371(9) Uani 1 1 d . . . . .
O14 O 0.4984(3) 0.31307(11) 0.86952(16) 0.0339(9) Uani 1 1 d . . . . .
O3 O 0.5172(3) 0.41186(12) 0.52433(17) 0.0333(9) Uani 1 1 d . . . . .
F2 F 0.0601(3) 0.22633(13) 0.55632(18) 0.0698(11) Uani 1 1 d . . . . .
O5 O 0.6391(3) 0.33053(12) 0.58041(16) 0.0330(9) Uani 1 1 d . . . . .
O9 O 0.8611(3) 0.33139(13) 0.62842(19) 0.0409(10) Uani 1 1 d . . . . .
F1 F 0.2327(3) 0.53541(13) 0.39360(19) 0.0693(11) Uani 1 1 d . . . . .
F6 F 0.3433(3) 0.55763(12) 0.7171(2) 0.0725(11) Uani 1 1 d . . . . .
F4 F 1.1332(3) 0.38703(13) 0.8503(2) 0.0746(11) Uani 1 1 d . . . . .
N2 N 0.8353(3) 0.25090(15) 0.7172(2) 0.0329(11) Uani 1 1 d . . . . .
F3 F 0.9362(4) 0.07022(12) 0.57384(18) 0.0777(12) Uani 1 1 d . . . . .
N4 N 0.3831(3) 0.20737(14) 0.73622(19) 0.0274(10) Uani 1 1 d . . . . .
N1 N 0.3433(3) 0.39316(14) 0.6071(2) 0.0305(11) Uani 1 1 d . . . . .
N3 N 0.6862(3) 0.43008(14) 0.8386(2) 0.0335(11) Uani 1 1 d . . . . .
F5 F 0.9259(4) 0.49238(17) 1.1030(2) 0.0997(15) Uani 1 1 d . . . . .
C33 C 0.5970(4) 0.40187(18) 0.7284(3) 0.0309(13) Uani 1 1 d . . . . .
C49 C 0.5464(4) 0.24307(17) 0.6961(3) 0.0274(13) Uani 1 1 d . . . . .
C50 C 0.4444(4) 0.21684(18) 0.6751(3) 0.0299(13) Uani 1 1 d . . . . .
H50A H 0.3986 0.2353 0.6403 0.036 Uiso 1 1 calc R . . . .
H50B H 0.4626 0.1869 0.6531 0.036 Uiso 1 1 calc R . . . .
C52 C 0.1987(4) 0.19962(18) 0.7768(3) 0.0306(13) Uani 1 1 d . . . . .
C18 C 0.7994(4) 0.26443(18) 0.7856(3) 0.0322(13) Uani 1 1 d . . . . .
H18A H 0.8637 0.2679 0.8198 0.039 Uiso 1 1 calc R . . . .
H18B H 0.7528 0.2395 0.8024 0.039 Uiso 1 1 calc R . . . .
C1 C 0.3849(4) 0.33333(18) 0.6951(3) 0.0290(13) Uani 1 1 d . . . . .
C59 C 0.5223(4) 0.15044(18) 0.7901(3) 0.0325(14) Uani 1 1 d . . . . .
C16 C 0.3353(4) 0.30094(19) 0.5262(3) 0.0324(14) Uani 1 1 d . . . . .
C17 C 0.7376(4) 0.30914(19) 0.7808(3) 0.0329(14) Uani 1 1 d . . . . .
C58 C 0.4070(4) 0.15855(18) 0.7624(3) 0.0348(14) Uani 1 1 d . . . . .
H58A H 0.3594 0.1516 0.7996 0.042 Uiso 1 1 calc R . . . .
H58B H 0.3883 0.1364 0.7238 0.042 Uiso 1 1 calc R . . . .
C64 C 0.5674(5) 0.17832(18) 0.8458(3) 0.0320(14) Uani 1 1 d . . . . .
C2 C 0.3268(4) 0.37811(17) 0.6793(3) 0.0301(13) Uani 1 1 d . . . . .
H2A H 0.3549 0.4024 0.7128 0.036 Uiso 1 1 calc R . . . .
H2B H 0.2482 0.3740 0.6840 0.036 Uiso 1 1 calc R . . . .
C34 C 0.6940(4) 0.42671(18) 0.7633(3) 0.0354(14) Uani 1 1 d . . . . .
H34A H 0.7610 0.4096 0.7545 0.043 Uiso 1 1 calc R . . . .
H34B H 0.6986 0.4584 0.7434 0.043 Uiso 1 1 calc R . . . .
C11 C 0.2468(4) 0.3234(2) 0.5519(3) 0.0346(14) Uani 1 1 d . . . . .
C53 C 0.1176(4) 0.16624(19) 0.7692(3) 0.0368(14) Uani 1 1 d . . . . .
H53 H 0.1046 0.1493 0.7269 0.044 Uiso 1 1 calc R . . . .
C48 C 0.4424(5) 0.44841(18) 0.8441(3) 0.0336(14) Uani 1 1 d . . . . .
C20 C 0.8416(4) 0.18012(19) 0.6372(3) 0.0346(14) Uani 1 1 d . . . . .
C10 C 0.2513(4) 0.37540(19) 0.5600(3) 0.0345(14) Uani 1 1 d . . . . .
H10A H 0.2553 0.3895 0.5135 0.041 Uiso 1 1 calc R . . . .
H10B H 0.1826 0.3860 0.5776 0.041 Uiso 1 1 calc R . . . .
C51 C 0.2642(4) 0.21079(18) 0.7168(3) 0.0311(13) Uani 1 1 d . . . . .
H51A H 0.2437 0.1890 0.6781 0.037 Uiso 1 1 calc R . . . .
H51B H 0.2465 0.2428 0.7002 0.037 Uiso 1 1 calc R . . . .
C4 C 0.3606(5) 0.45988(18) 0.5279(3) 0.0362(14) Uani 1 1 d . . . . .
C8 C 0.4599(5) 0.45724(18) 0.4251(3) 0.0376(14) Uani 1 1 d . . . . .
H8 H 0.5185 0.4455 0.4016 0.045 Uiso 1 1 calc R . . . .
C3 C 0.3473(5) 0.44510(18) 0.6013(3) 0.0362(14) Uani 1 1 d . . . . .
H3A H 0.4088 0.4572 0.6326 0.043 Uiso 1 1 calc R . . . .
H3B H 0.2793 0.4586 0.6162 0.043 Uiso 1 1 calc R . . . .
C57 C 0.2197(4) 0.22270(19) 0.8403(3) 0.0339(14) Uani 1 1 d . . . . .
C63 C 0.6704(4) 0.1687(2) 0.8759(3) 0.0368(14) Uani 1 1 d . . . . .
H63 H 0.7012 0.1877 0.9129 0.044 Uiso 1 1 calc R . . . .
C26 C 0.9529(4) 0.26194(19) 0.7140(3) 0.0387(14) Uani 1 1 d . . . . .
H26A H 0.9963 0.2426 0.7488 0.046 Uiso 1 1 calc R . . . .
H26B H 0.9741 0.2532 0.6674 0.046 Uiso 1 1 calc R . . . .
C60 C 0.5836(5) 0.11419(19) 0.7657(3) 0.0351(14) Uani 1 1 d . . . . .
H60 H 0.5561 0.0957 0.7272 0.042 Uiso 1 1 calc R . . . .
C32 C 0.9320(5) 0.3457(2) 0.6815(3) 0.0403(15) Uani 1 1 d . . . . .
C25 C 0.8164(4) 0.2039(2) 0.5747(3) 0.0353(14) Uani 1 1 d . . . . .
C41 C 0.7257(5) 0.4021(2) 0.9892(3) 0.0409(15) Uani 1 1 d . . . . .
C7 C 0.3885(5) 0.4885(2) 0.3926(3) 0.0415(15) Uani 1 1 d . . . . .
H7 H 0.3974 0.4988 0.3467 0.050 Uiso 1 1 calc R . . . .
C43 C 0.5204(5) 0.48032(19) 0.8247(3) 0.0386(15) Uani 1 1 d . . . . .
C56 C 0.1540(5) 0.21314(19) 0.8941(3) 0.0392(15) Uani 1 1 d . . . . .
H56 H 0.1663 0.2291 0.9372 0.047 Uiso 1 1 calc R . . . .
C27 C 0.9799(5) 0.3116(2) 0.7270(3) 0.0393(15) Uani 1 1 d . . . . .
C14 C 0.2341(5) 0.2291(2) 0.5174(3) 0.0438(16) Uani 1 1 d . . . . .
H14 H 0.2279 0.1972 0.5042 0.053 Uiso 1 1 calc R . . . .
C15 C 0.3277(5) 0.2538(2) 0.5087(3) 0.0400(15) Uani 1 1 d . . . . .
H15 H 0.3875 0.2386 0.4907 0.048 Uiso 1 1 calc R . . . .
C9 C 0.4464(4) 0.44263(18) 0.4928(3) 0.0330(14) Uani 1 1 d . . . . .
C19 C 0.8171(4) 0.19962(18) 0.7072(3) 0.0343(14) Uani 1 1 d . . . . .
H19A H 0.7402 0.1927 0.7139 0.041 Uiso 1 1 calc R . . . .
H19B H 0.8626 0.1829 0.7441 0.041 Uiso 1 1 calc R . . . .
C47 C 0.3347(5) 0.4544(2) 0.8224(3) 0.0451(16) Uani 1 1 d . . . . .
H47 H 0.2828 0.4328 0.8367 0.054 Uiso 1 1 calc R . . . .
C61 C 0.6839(5) 0.1060(2) 0.7985(3) 0.0441(16) Uani 1 1 d . . . . .
C21 C 0.8825(5) 0.1352(2) 0.6357(3) 0.0453(16) Uani 1 1 d . . . . .
H21 H 0.9007 0.1187 0.6779 0.054 Uiso 1 1 calc R . . . .
C62 C 0.7289(5) 0.1321(2) 0.8531(3) 0.0432(15) Uani 1 1 d . . . . .
H62 H 0.7992 0.1250 0.8746 0.052 Uiso 1 1 calc R . . . .
C42 C 0.6345(5) 0.47564(19) 0.8552(3) 0.0445(16) Uani 1 1 d . . . . .
H42A H 0.6363 0.4789 0.9064 0.053 Uiso 1 1 calc R . . . .
H42B H 0.6779 0.5015 0.8378 0.053 Uiso 1 1 calc R . . . .
C36 C 0.7938(5) 0.4310(2) 0.9548(3) 0.0456(16) Uani 1 1 d . . . . .
C12 C 0.1531(5) 0.2980(2) 0.5623(3) 0.0401(15) Uani 1 1 d . . . . .
H12 H 0.0927 0.3125 0.5806 0.048 Uiso 1 1 calc R . . . .
C44 C 0.4858(5) 0.5170(2) 0.7813(3) 0.0429(15) Uani 1 1 d . . . . .
H44 H 0.5369 0.5387 0.7663 0.052 Uiso 1 1 calc R . . . .
C35 C 0.7955(5) 0.4283(2) 0.8769(3) 0.0425(15) Uani 1 1 d . . . . .
H35A H 0.8395 0.4545 0.8612 0.051 Uiso 1 1 calc R . . . .
H35B H 0.8315 0.3988 0.8649 0.051 Uiso 1 1 calc R . . . .
C5 C 0.2892(5) 0.4916(2) 0.4942(3) 0.0466(16) Uani 1 1 d . . . . .
H5 H 0.2307 0.5041 0.5170 0.056 Uiso 1 1 calc R . . . .
C54 C 0.0570(5) 0.1580(2) 0.8230(3) 0.0417(15) Uani 1 1 d . . . . .
C28 C 1.0481(5) 0.3263(2) 0.7833(3) 0.0463(16) Uani 1 1 d . . . . .
H28 H 1.0809 0.3040 0.8149 0.056 Uiso 1 1 calc R . . . .
C40 C 0.7250(5) 0.4034(2) 1.0617(3) 0.0487(16) Uani 1 1 d . . . . .
H40 H 0.6773 0.3839 1.0846 0.058 Uiso 1 1 calc R . . . .
C55 C 0.0709(5) 0.1804(2) 0.8847(3) 0.0432(15) Uani 1 1 d . . . . .
H55 H 0.0253 0.1739 0.9207 0.052 Uiso 1 1 calc R . . . .
C46 C 0.3006(5) 0.4915(2) 0.7801(3) 0.0505(17) Uani 1 1 d . . . . .
H46 H 0.2259 0.4959 0.7652 0.061 Uiso 1 1 calc R . . . .
C24 C 0.8326(5) 0.1825(2) 0.5117(3) 0.0437(15) Uani 1 1 d . . . . .
H24 H 0.8165 0.1988 0.4692 0.052 Uiso 1 1 calc R . . . .
C13 C 0.1506(5) 0.2513(2) 0.5453(3) 0.0504(17) Uani 1 1 d . . . . .
C23 C 0.8723(5) 0.1372(2) 0.5112(3) 0.0570(18) Uani 1 1 d . . . . .
H23 H 0.8824 0.1221 0.4685 0.068 Uiso 1 1 calc R . . . .
C22 C 0.8967(5) 0.1146(2) 0.5734(3) 0.0527(17) Uani 1 1 d . . . . .
C6 C 0.3047(5) 0.5046(2) 0.4269(3) 0.0493(17) Uani 1 1 d . . . . .
C31 C 0.9574(5) 0.3930(2) 0.6913(3) 0.0488(17) Uani 1 1 d . . . . .
H31 H 0.9275 0.4157 0.6591 0.059 Uiso 1 1 calc R . . . .
C29 C 1.0691(5) 0.3733(3) 0.7941(3) 0.0550(18) Uani 1 1 d . . . . .
C45 C 0.3782(6) 0.5217(2) 0.7604(3) 0.0503(17) Uani 1 1 d . . . . .
C30 C 1.0267(5) 0.4064(2) 0.7484(4) 0.0533(17) Uani 1 1 d . . . . .
H30 H 1.0447 0.4384 0.7557 0.064 Uiso 1 1 calc R . . . .
C39 C 0.7943(6) 0.4334(3) 1.0992(3) 0.0629(19) Uani 1 1 d . . . . .
H39 H 0.7972 0.4340 1.1486 0.075 Uiso 1 1 calc R . . . .
C37 C 0.8608(5) 0.4619(2) 0.9932(3) 0.0593(19) Uani 1 1 d . . . . .
H37 H 0.9072 0.4824 0.9709 0.071 Uiso 1 1 calc R . . . .
C38 C 0.8590(6) 0.4625(3) 1.0652(4) 0.069(2) Uani 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 O1 2.012(3) . ?
Ti1 O11 2.097(4) . ?
Ti1 O4 1.867(4) . ?
Ti1 O3 1.817(3) . ?
Ti1 O5 1.815(3) . ?
Ti1 N1 2.356(4) . ?
Ti2 O16 2.081(3) . ?
Ti2 O6 2.018(3) . ?
Ti2 O8 1.817(4) . ?
Ti2 O5 1.814(3) . ?
Ti2 O9 1.878(4) . ?
Ti2 N2 2.328(4) . ?
Ti3 O10 1.999(3) . ?
Ti3 O12 1.829(4) . ?
Ti3 O7 2.089(4) . ?
Ti3 O13 1.862(4) . ?
Ti3 O14 1.821(3) . ?
Ti3 N3 2.357(4) . ?
Ti4 O2 2.100(4) . ?
Ti4 O15 2.019(3) . ?
Ti4 O17 1.837(3) . ?
Ti4 O18 1.855(3) . ?
Ti4 O14 1.823(3) . ?
Ti4 N4 2.349(4) . ?
O1 C1 1.258(6) . ?
F7 C54 1.376(6) . ?
O2 C1 1.270(6) . ?
O11 C33 1.262(6) . ?
O4 C16 1.344(6) . ?
O10 C33 1.262(6) . ?
O16 C49 1.254(6) . ?
O15 C49 1.264(6) . ?
O6 C17 1.272(6) . ?
F8 C61 1.389(6) . ?
O17 C57 1.351(6) . ?
O8 C25 1.352(6) . ?
O18 C64 1.358(6) . ?
O12 C41 1.360(6) . ?
O7 C17 1.254(6) . ?
O13 C48 1.349(6) . ?
O3 C9 1.347(6) . ?
F2 C13 1.361(6) . ?
O9 C32 1.350(7) . ?
F1 C6 1.370(6) . ?
F6 C45 1.369(7) . ?
F4 C29 1.343(7) . ?
N2 C18 1.482(6) . ?
N2 C26 1.493(6) . ?
N2 C19 1.496(6) . ?
F3 C22 1.362(7) . ?
N4 C50 1.484(6) . ?
N4 C58 1.506(6) . ?
N4 C51 1.485(6) . ?
N1 C2 1.491(6) . ?
N1 C10 1.479(6) . ?
N1 C3 1.493(6) . ?
N3 C34 1.467(6) . ?
N3 C42 1.500(7) . ?
N3 C35 1.480(7) . ?
F5 C38 1.357(7) . ?
C33 C34 1.499(7) . ?
C49 C50 1.491(7) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C52 C53 1.383(7) . ?
C52 C51 1.505(7) . ?
C52 C57 1.395(7) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C17 1.489(7) . ?
C1 C2 1.487(7) . ?
C59 C58 1.493(7) . ?
C59 C64 1.412(7) . ?
C59 C60 1.392(7) . ?
C16 C11 1.397(7) . ?
C16 C15 1.392(7) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C64 C63 1.378(7) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C11 C10 1.498(7) . ?
C11 C12 1.397(7) . ?
C53 H53 0.9500 . ?
C53 C54 1.354(7) . ?
C48 C43 1.403(8) . ?
C48 C47 1.368(8) . ?
C20 C25 1.396(7) . ?
C20 C19 1.518(7) . ?
C20 C21 1.384(7) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C4 C3 1.501(7) . ?
C4 C9 1.399(7) . ?
C4 C5 1.386(7) . ?
C8 H8 0.9500 . ?
C8 C7 1.367(7) . ?
C8 C9 1.396(7) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C57 C56 1.401(7) . ?
C63 H63 0.9500 . ?
C63 C62 1.368(8) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.478(8) . ?
C60 H60 0.9500 . ?
C60 C61 1.360(8) . ?
C32 C27 1.405(8) . ?
C32 C31 1.401(8) . ?
C25 C24 1.391(7) . ?
C41 C36 1.392(8) . ?
C41 C40 1.400(8) . ?
C7 H7 0.9500 . ?
C7 C6 1.359(8) . ?
C43 C42 1.483(8) . ?
C43 C44 1.387(8) . ?
C56 H56 0.9500 . ?
C56 C55 1.391(8) . ?
C27 C28 1.377(8) . ?
C14 H14 0.9500 . ?
C14 C15 1.379(8) . ?
C14 C13 1.364(8) . ?
C15 H15 0.9500 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C47 H47 0.9500 . ?
C47 C46 1.383(8) . ?
C61 C62 1.367(8) . ?
C21 H21 0.9500 . ?
C21 C22 1.365(8) . ?
C62 H62 0.9500 . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C36 C35 1.507(8) . ?
C36 C37 1.381(8) . ?
C12 H12 0.9500 . ?
C12 C13 1.375(8) . ?
C44 H44 0.9500 . ?
C44 C45 1.360(8) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C5 H5 0.9500 . ?
C5 C6 1.381(8) . ?
C54 C55 1.349(8) . ?
C28 H28 0.9500 . ?
C28 C29 1.381(8) . ?
C40 H40 0.9500 . ?
C40 C39 1.371(8) . ?
C55 H55 0.9500 . ?
C46 H46 0.9500 . ?
C46 C45 1.371(8) . ?
C24 H24 0.9500 . ?
C24 C23 1.386(8) . ?
C23 H23 0.9500 . ?
C23 C22 1.372(8) . ?
C31 H31 0.9500 . ?
C31 C30 1.387(8) . ?
C29 C30 1.367(9) . ?
C30 H30 0.9500 . ?
C39 H39 0.9500 . ?
C39 C38 1.363(9) . ?
C37 H37 0.9500 . ?
C37 C38 1.390(9) . ?

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 O11 86.54(13) . . ?
O1 Ti1 N1 73.12(14) . . ?
O11 Ti1 N1 84.43(14) . . ?
O4 Ti1 O1 86.35(14) . . ?
O4 Ti1 O11 167.36(14) . . ?
O4 Ti1 N1 83.51(15) . . ?
O3 Ti1 O1 157.61(15) . . ?
O3 Ti1 O11 87.77(15) . . ?
O3 Ti1 O4 94.89(15) . . ?
O3 Ti1 N1 84.78(15) . . ?
O5 Ti1 O1 94.43(14) . . ?
O5 Ti1 O11 92.06(14) . . ?
O5 Ti1 O4 98.90(15) . . ?
O5 Ti1 O3 107.41(15) . . ?
O5 Ti1 N1 167.22(15) . . ?
O16 Ti2 N2 81.64(14) . . ?
O6 Ti2 O16 87.52(13) . . ?
O6 Ti2 N2 74.07(14) . . ?
O8 Ti2 O16 85.10(15) . . ?
O8 Ti2 O6 158.48(15) . . ?
O8 Ti2 O9 97.49(16) . . ?
O8 Ti2 N2 84.86(15) . . ?
O5 Ti2 O16 91.26(14) . . ?
O5 Ti2 O6 92.80(15) . . ?
O5 Ti2 O8 107.53(16) . . ?
O5 Ti2 O9 99.24(16) . . ?
O5 Ti2 N2 165.24(15) . . ?
O9 Ti2 O16 167.82(15) . . ?
O9 Ti2 O6 85.81(15) . . ?
O9 Ti2 N2 86.73(16) . . ?
O10 Ti3 O7 85.40(14) . . ?
O10 Ti3 N3 73.71(14) . . ?
O12 Ti3 O10 157.33(16) . . ?
O12 Ti3 O7 88.11(15) . . ?
O12 Ti3 O13 95.74(16) . . ?
O12 Ti3 N3 83.93(15) . . ?
O7 Ti3 N3 82.48(14) . . ?
O13 Ti3 O10 85.58(15) . . ?
O13 Ti3 O7 165.11(15) . . ?
O13 Ti3 N3 83.64(15) . . ?
O14 Ti3 O10 94.09(15) . . ?
O14 Ti3 O12 107.77(16) . . ?
O14 Ti3 O7 91.35(14) . . ?
O14 Ti3 O13 101.08(16) . . ?
O14 Ti3 N3 166.67(15) . . ?
O2 Ti4 N4 82.75(13) . . ?
O15 Ti4 O2 85.88(13) . . ?
O15 Ti4 N4 73.53(14) . . ?
O17 Ti4 O2 86.74(14) . . ?
O17 Ti4 O15 157.42(15) . . ?
O17 Ti4 O18 97.11(15) . . ?
O17 Ti4 N4 84.39(14) . . ?
O18 Ti4 O2 166.17(14) . . ?
O18 Ti4 O15 85.58(14) . . ?
O18 Ti4 N4 84.42(14) . . ?
O14 Ti4 O2 90.47(14) . . ?
O14 Ti4 O15 93.52(15) . . ?
O14 Ti4 O17 107.86(15) . . ?
O14 Ti4 O18 100.89(15) . . ?
O14 Ti4 N4 165.71(14) . . ?
C1 O1 Ti1 124.6(3) . . ?
C1 O2 Ti4 138.1(3) . . ?
C33 O11 Ti1 136.9(3) . . ?
C16 O4 Ti1 130.3(3) . . ?
C33 O10 Ti3 124.9(3) . . ?
C49 O16 Ti2 138.3(3) . . ?
C49 O15 Ti4 124.5(3) . . ?
C17 O6 Ti2 125.0(3) . . ?
C57 O17 Ti4 138.5(3) . . ?
C25 O8 Ti2 140.2(3) . . ?
C64 O18 Ti4 132.1(3) . . ?
C41 O12 Ti3 139.7(3) . . ?
C17 O7 Ti3 138.0(3) . . ?
C48 O13 Ti3 130.9(3) . . ?
Ti3 O14 Ti4 147.29(19) . . ?
C9 O3 Ti1 137.1(3) . . ?
Ti2 O5 Ti1 144.77(19) . . ?
C32 O9 Ti2 129.4(3) . . ?
C18 N2 Ti2 109.0(3) . . ?
C18 N2 C26 110.6(4) . . ?
C18 N2 C19 108.5(4) . . ?
C26 N2 Ti2 107.7(3) . . ?
C26 N2 C19 109.8(4) . . ?
C19 N2 Ti2 111.1(3) . . ?
C50 N4 Ti4 107.1(3) . . ?
C50 N4 C58 109.7(4) . . ?
C50 N4 C51 110.6(4) . . ?
C58 N4 Ti4 111.7(3) . . ?
C51 N4 Ti4 109.9(3) . . ?
C51 N4 C58 107.8(4) . . ?
C2 N1 Ti1 106.3(3) . . ?
C2 N1 C3 111.5(4) . . ?
C10 N1 Ti1 112.8(3) . . ?
C10 N1 C2 108.2(4) . . ?
C10 N1 C3 109.0(4) . . ?
C3 N1 Ti1 109.1(3) . . ?
C34 N3 Ti3 106.0(3) . . ?
C34 N3 C42 109.7(4) . . ?
C34 N3 C35 110.6(4) . . ?
C42 N3 Ti3 111.8(3) . . ?
C35 N3 Ti3 110.6(3) . . ?
C35 N3 C42 108.1(4) . . ?
O11 C33 C34 119.7(5) . . ?
O10 C33 O11 123.4(5) . . ?
O10 C33 C34 116.9(5) . . ?
O16 C49 O15 124.3(5) . . ?
O16 C49 C50 118.3(5) . . ?
O15 C49 C50 117.5(5) . . ?
N4 C50 C49 110.8(4) . . ?
N4 C50 H50A 109.5 . . ?
N4 C50 H50B 109.5 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 108.1 . . ?
C53 C52 C51 120.0(5) . . ?
C53 C52 C57 119.7(5) . . ?
C57 C52 C51 120.3(5) . . ?
N2 C18 H18A 109.4 . . ?
N2 C18 H18B 109.4 . . ?
N2 C18 C17 111.3(4) . . ?
H18A C18 H18B 108.0 . . ?
C17 C18 H18A 109.4 . . ?
C17 C18 H18B 109.4 . . ?
O1 C1 O2 123.6(5) . . ?
O1 C1 C2 117.8(4) . . ?
O2 C1 C2 118.6(5) . . ?
C64 C59 C58 118.8(5) . . ?
C60 C59 C58 121.7(5) . . ?
C60 C59 C64 119.3(5) . . ?
O4 C16 C11 119.0(5) . . ?
O4 C16 C15 121.4(5) . . ?
C15 C16 C11 119.6(5) . . ?
O6 C17 C18 117.4(5) . . ?
O7 C17 O6 123.2(5) . . ?
O7 C17 C18 119.4(5) . . ?
N4 C58 H58A 108.6 . . ?
N4 C58 H58B 108.6 . . ?
C59 C58 N4 114.6(4) . . ?
C59 C58 H58A 108.6 . . ?
C59 C58 H58B 108.6 . . ?
H58A C58 H58B 107.6 . . ?
O18 C64 C59 118.3(5) . . ?
O18 C64 C63 122.2(5) . . ?
C63 C64 C59 119.5(5) . . ?
N1 C2 H2A 109.7 . . ?
N1 C2 H2B 109.7 . . ?
C1 C2 N1 109.6(4) . . ?
C1 C2 H2A 109.7 . . ?
C1 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
N3 C34 C33 110.7(4) . . ?
N3 C34 H34A 109.5 . . ?
N3 C34 H34B 109.5 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 108.1 . . ?
C16 C11 C10 118.1(5) . . ?
C12 C11 C16 119.8(5) . . ?
C12 C11 C10 121.7(5) . . ?
C52 C53 H53 120.5 . . ?
C54 C53 C52 119.0(5) . . ?
C54 C53 H53 120.5 . . ?
O13 C48 C43 117.6(5) . . ?
O13 C48 C47 121.8(5) . . ?
C47 C48 C43 120.6(5) . . ?
C25 C20 C19 122.9(5) . . ?
C21 C20 C25 119.3(5) . . ?
C21 C20 C19 117.6(5) . . ?
N1 C10 C11 115.1(4) . . ?
N1 C10 H10A 108.5 . . ?
N1 C10 H10B 108.5 . . ?
C11 C10 H10A 108.5 . . ?
C11 C10 H10B 108.5 . . ?
H10A C10 H10B 107.5 . . ?
N4 C51 C52 112.4(4) . . ?
N4 C51 H51A 109.1 . . ?
N4 C51 H51B 109.1 . . ?
C52 C51 H51A 109.1 . . ?
C52 C51 H51B 109.1 . . ?
H51A C51 H51B 107.9 . . ?
C9 C4 C3 120.7(5) . . ?
C5 C4 C3 120.5(5) . . ?
C5 C4 C9 118.8(5) . . ?
C7 C8 H8 120.1 . . ?
C7 C8 C9 119.9(5) . . ?
C9 C8 H8 120.1 . . ?
N1 C3 C4 111.0(4) . . ?
N1 C3 H3A 109.4 . . ?
N1 C3 H3B 109.4 . . ?
C4 C3 H3A 109.4 . . ?
C4 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
O17 C57 C52 121.3(5) . . ?
O17 C57 C56 119.8(5) . . ?
C52 C57 C56 118.9(5) . . ?
C64 C63 H63 119.6 . . ?
C62 C63 C64 120.9(5) . . ?
C62 C63 H63 119.6 . . ?
N2 C26 H26A 108.8 . . ?
N2 C26 H26B 108.8 . . ?
H26A C26 H26B 107.7 . . ?
C27 C26 N2 113.7(4) . . ?
C27 C26 H26A 108.8 . . ?
C27 C26 H26B 108.8 . . ?
C59 C60 H60 120.9 . . ?
C61 C60 C59 118.2(5) . . ?
C61 C60 H60 120.9 . . ?
O9 C32 C27 118.1(5) . . ?
O9 C32 C31 121.1(6) . . ?
C31 C32 C27 120.7(6) . . ?
O8 C25 C20 122.4(5) . . ?
O8 C25 C24 117.5(5) . . ?
C24 C25 C20 120.0(5) . . ?
O12 C41 C36 121.0(5) . . ?
O12 C41 C40 117.7(5) . . ?
C36 C41 C40 121.2(6) . . ?
C8 C7 H7 120.4 . . ?
C6 C7 C8 119.1(5) . . ?
C6 C7 H7 120.4 . . ?
C48 C43 C42 119.1(5) . . ?
C44 C43 C48 118.3(5) . . ?
C44 C43 C42 122.5(5) . . ?
C57 C56 H56 119.8 . . ?
C55 C56 C57 120.4(5) . . ?
C55 C56 H56 119.8 . . ?
C32 C27 C26 119.1(5) . . ?
C28 C27 C26 122.7(5) . . ?
C28 C27 C32 118.2(5) . . ?
C15 C14 H14 120.7 . . ?
C13 C14 H14 120.7 . . ?
C13 C14 C15 118.7(6) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 C16 120.5(6) . . ?
C14 C15 H15 119.8 . . ?
O3 C9 C4 120.1(5) . . ?
O3 C9 C8 119.4(5) . . ?
C8 C9 C4 120.5(5) . . ?
N2 C19 C20 115.8(4) . . ?
N2 C19 H19A 108.3 . . ?
N2 C19 H19B 108.3 . . ?
C20 C19 H19A 108.3 . . ?
C20 C19 H19B 108.3 . . ?
H19A C19 H19B 107.4 . . ?
C48 C47 H47 119.6 . . ?
C48 C47 C46 120.8(6) . . ?
C46 C47 H47 119.6 . . ?
C60 C61 F8 117.0(6) . . ?
C60 C61 C62 123.7(5) . . ?
C62 C61 F8 119.3(5) . . ?
C20 C21 H21 120.1 . . ?
C22 C21 C20 119.7(5) . . ?
C22 C21 H21 120.1 . . ?
C63 C62 H62 120.8 . . ?
C61 C62 C63 118.4(5) . . ?
C61 C62 H62 120.8 . . ?
N3 C42 H42A 108.8 . . ?
N3 C42 H42B 108.8 . . ?
C43 C42 N3 113.6(4) . . ?
C43 C42 H42A 108.8 . . ?
C43 C42 H42B 108.8 . . ?
H42A C42 H42B 107.7 . . ?
C41 C36 C35 120.6(5) . . ?
C37 C36 C41 118.9(6) . . ?
C37 C36 C35 120.5(6) . . ?
C11 C12 H12 120.9 . . ?
C13 C12 C11 118.2(5) . . ?
C13 C12 H12 120.9 . . ?
C43 C44 H44 120.2 . . ?
C45 C44 C43 119.6(6) . . ?
C45 C44 H44 120.2 . . ?
N3 C35 C36 113.7(5) . . ?
N3 C35 H35A 108.8 . . ?
N3 C35 H35B 108.8 . . ?
C36 C35 H35A 108.8 . . ?
C36 C35 H35B 108.8 . . ?
H35A C35 H35B 107.7 . . ?
C4 C5 H5 120.6 . . ?
C6 C5 C4 118.7(6) . . ?
C6 C5 H5 120.6 . . ?
C53 C54 F7 117.5(5) . . ?
C55 C54 F7 118.5(5) . . ?
C55 C54 C53 124.0(6) . . ?
C27 C28 H28 119.7 . . ?
C27 C28 C29 120.6(6) . . ?
C29 C28 H28 119.7 . . ?
C41 C40 H40 120.5 . . ?
C39 C40 C41 119.0(6) . . ?
C39 C40 H40 120.5 . . ?
C56 C55 H55 121.1 . . ?
C54 C55 C56 117.9(5) . . ?
C54 C55 H55 121.1 . . ?
C47 C46 H46 121.1 . . ?
C45 C46 C47 117.8(6) . . ?
C45 C46 H46 121.1 . . ?
C25 C24 H24 120.1 . . ?
C23 C24 C25 119.9(5) . . ?
C23 C24 H24 120.1 . . ?
F2 C13 C14 118.5(6) . . ?
F2 C13 C12 118.3(6) . . ?
C14 C13 C12 123.1(6) . . ?
C24 C23 H23 120.5 . . ?
C22 C23 C24 119.0(6) . . ?
C22 C23 H23 120.5 . . ?
F3 C22 C21 118.1(5) . . ?
F3 C22 C23 119.8(6) . . ?
C21 C22 C23 122.1(6) . . ?
F1 C6 C5 118.4(6) . . ?
C7 C6 F1 118.7(5) . . ?
C7 C6 C5 122.9(6) . . ?
C32 C31 H31 120.4 . . ?
C30 C31 C32 119.3(6) . . ?
C30 C31 H31 120.4 . . ?
F4 C29 C28 119.8(6) . . ?
F4 C29 C30 118.6(6) . . ?
C30 C29 C28 121.6(6) . . ?
F6 C45 C46 117.0(6) . . ?
C44 C45 F6 120.0(6) . . ?
C44 C45 C46 122.9(6) . . ?
C31 C30 H30 120.3 . . ?
C29 C30 C31 119.5(6) . . ?
C29 C30 H30 120.3 . . ?
C40 C39 H39 120.2 . . ?
C38 C39 C40 119.5(6) . . ?
C38 C39 H39 120.2 . . ?
C36 C37 H37 120.6 . . ?
C36 C37 C38 118.7(6) . . ?
C38 C37 H37 120.6 . . ?
F5 C38 C39 118.8(6) . . ?
F5 C38 C37 118.7(7) . . ?
C39 C38 C37 122.5(6) . . ?

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
Ti1 O1 C1 O2 -171.3(3) . . . . ?
Ti1 O1 C1 C2 8.5(6) . . . . ?
Ti1 O11 C33 O10 -33.8(8) . . . . ?
Ti1 O11 C33 C34 145.1(4) . . . . ?
Ti1 O4 C16 C11 54.4(6) . . . . ?
Ti1 O4 C16 C15 -126.2(4) . . . . ?
Ti1 O3 C9 C4 38.9(7) . . . . ?
Ti1 O3 C9 C8 -141.4(4) . . . . ?
Ti1 N1 C2 C1 -27.9(5) . . . . ?
Ti1 N1 C10 C11 49.8(5) . . . . ?
Ti1 N1 C3 C4 64.6(5) . . . . ?
Ti2 O16 C49 O15 -26.6(8) . . . . ?
Ti2 O16 C49 C50 152.7(4) . . . . ?
Ti2 O6 C17 O7 -171.8(4) . . . . ?
Ti2 O6 C17 C18 8.4(6) . . . . ?
Ti2 O8 C25 C20 -2.9(8) . . . . ?
Ti2 O8 C25 C24 178.2(4) . . . . ?
Ti2 O9 C32 C27 52.8(6) . . . . ?
Ti2 O9 C32 C31 -127.2(5) . . . . ?
Ti2 N2 C18 C17 -16.2(5) . . . . ?
Ti2 N2 C26 C27 61.9(5) . . . . ?
Ti2 N2 C19 C20 55.8(5) . . . . ?
Ti3 O10 C33 O11 172.8(3) . . . . ?
Ti3 O10 C33 C34 -6.1(6) . . . . ?
Ti3 O12 C41 C36 -29.6(8) . . . . ?
Ti3 O12 C41 C40 150.1(4) . . . . ?
Ti3 O7 C17 O6 37.0(8) . . . . ?
Ti3 O7 C17 C18 -143.3(4) . . . . ?
Ti3 O13 C48 C43 -55.2(6) . . . . ?
Ti3 O13 C48 C47 123.3(5) . . . . ?
Ti3 N3 C34 C33 27.5(5) . . . . ?
Ti3 N3 C42 C43 -53.2(5) . . . . ?
Ti3 N3 C35 C36 -62.2(5) . . . . ?
Ti4 O2 C1 O1 31.3(8) . . . . ?
Ti4 O2 C1 C2 -148.6(4) . . . . ?
Ti4 O15 C49 O16 168.4(3) . . . . ?
Ti4 O15 C49 C50 -10.8(6) . . . . ?
Ti4 O17 C57 C52 -30.4(8) . . . . ?
Ti4 O17 C57 C56 149.3(4) . . . . ?
Ti4 O18 C64 C59 -53.2(6) . . . . ?
Ti4 O18 C64 C63 126.5(5) . . . . ?
Ti4 N4 C50 C49 23.5(4) . . . . ?
Ti4 N4 C58 C59 -53.9(5) . . . . ?
Ti4 N4 C51 C52 -64.1(5) . . . . ?
O1 Ti1 O4 C16 25.8(4) . . . . ?
O1 Ti1 O3 C9 -28.8(7) . . . . ?
O1 Ti1 O5 Ti2 -24.6(4) . . . . ?
O1 C1 C2 N1 16.6(6) . . . . ?
F7 C54 C55 C56 178.2(5) . . . . ?
O2 Ti4 O17 C57 95.6(5) . . . . ?
O2 Ti4 O18 C64 20.9(9) . . . . ?
O2 Ti4 O14 Ti3 -54.2(4) . . . . ?
O2 C1 C2 N1 -163.5(4) . . . . ?
O11 Ti1 O4 C16 -30.1(9) . . . . ?
O11 Ti1 O3 C9 -104.1(5) . . . . ?
O11 Ti1 O5 Ti2 62.1(4) . . . . ?
O11 C33 C34 N3 163.3(4) . . . . ?
O4 Ti1 O3 C9 63.5(5) . . . . ?
O4 Ti1 O5 Ti2 -111.6(4) . . . . ?
O4 C16 C11 C10 8.4(7) . . . . ?
O4 C16 C11 C12 -178.2(4) . . . . ?
O4 C16 C15 C14 179.9(5) . . . . ?
O10 Ti3 O12 C41 20.7(8) . . . . ?
O10 Ti3 O13 C48 -27.6(4) . . . . ?
O10 Ti3 O14 Ti4 26.5(4) . . . . ?
O10 C33 C34 N3 -17.8(6) . . . . ?
O16 Ti2 O8 C25 -64.1(5) . . . . ?
O16 Ti2 O5 Ti1 52.7(4) . . . . ?
O16 Ti2 O9 C32 -20.2(10) . . . . ?
O16 C49 C50 N4 168.9(4) . . . . ?
O15 Ti4 O17 C57 24.5(7) . . . . ?
O15 Ti4 O18 C64 -31.0(4) . . . . ?
O15 Ti4 O14 Ti3 31.7(4) . . . . ?
O15 C49 C50 N4 -11.8(6) . . . . ?
O6 Ti2 O8 C25 6.3(8) . . . . ?
O6 Ti2 O5 Ti1 -34.9(4) . . . . ?
O6 Ti2 O9 C32 36.8(4) . . . . ?
F8 C61 C62 C63 177.1(5) . . . . ?
O17 Ti4 O18 C64 126.4(4) . . . . ?
O17 Ti4 O14 Ti3 -140.9(4) . . . . ?
O17 C57 C56 C55 -178.3(5) . . . . ?
O8 Ti2 O5 Ti1 138.0(3) . . . . ?
O8 Ti2 O9 C32 -121.9(4) . . . . ?
O8 C25 C24 C23 179.9(5) . . . . ?
O18 Ti4 O17 C57 -71.1(5) . . . . ?
O18 Ti4 O14 Ti3 117.9(4) . . . . ?
O18 C64 C63 C62 179.4(5) . . . . ?
O12 Ti3 O13 C48 129.7(4) . . . . ?
O12 Ti3 O14 Ti4 -147.4(4) . . . . ?
O12 C41 C36 C35 -1.8(8) . . . . ?
O12 C41 C36 C37 178.9(5) . . . . ?
O12 C41 C40 C39 179.2(5) . . . . ?
O7 Ti3 O12 C41 94.0(5) . . . . ?
O7 Ti3 O13 C48 25.3(9) . . . . ?
O7 Ti3 O14 Ti4 -59.0(4) . . . . ?
O13 Ti3 O12 C41 -71.5(5) . . . . ?
O13 Ti3 O14 Ti4 112.8(4) . . . . ?
O13 C48 C43 C42 -8.0(7) . . . . ?
O13 C48 C43 C44 176.4(4) . . . . ?
O13 C48 C47 C46 -177.4(5) . . . . ?
O14 Ti3 O12 C41 -175.1(5) . . . . ?
O14 Ti3 O13 C48 -120.9(4) . . . . ?
O14 Ti4 O17 C57 -175.0(5) . . . . ?
O14 Ti4 O18 C64 -123.8(4) . . . . ?
O3 Ti1 O4 C16 -131.8(4) . . . . ?
O3 Ti1 O5 Ti2 150.4(3) . . . . ?
O5 Ti1 O4 C16 119.7(4) . . . . ?
O5 Ti1 O3 C9 164.4(5) . . . . ?
O5 Ti2 O8 C25 -153.9(5) . . . . ?
O5 Ti2 O9 C32 128.9(4) . . . . ?
O9 Ti2 O8 C25 103.9(5) . . . . ?
O9 Ti2 O5 Ti1 -121.1(4) . . . . ?
O9 C32 C27 C26 1.4(7) . . . . ?
O9 C32 C27 C28 -176.8(5) . . . . ?
O9 C32 C31 C30 177.0(5) . . . . ?
F4 C29 C30 C31 -177.9(5) . . . . ?
N2 Ti2 O8 C25 17.9(5) . . . . ?
N2 Ti2 O5 Ti1 -8.1(9) . . . . ?
N2 Ti2 O9 C32 -37.5(4) . . . . ?
N2 C18 C17 O6 7.4(6) . . . . ?
N2 C18 C17 O7 -172.3(4) . . . . ?
N2 C26 C27 C32 -61.7(6) . . . . ?
N2 C26 C27 C28 116.3(6) . . . . ?
N4 Ti4 O17 C57 12.5(5) . . . . ?
N4 Ti4 O18 C64 42.8(4) . . . . ?
N4 Ti4 O14 Ti3 7.2(9) . . . . ?
N1 Ti1 O4 C16 -47.6(4) . . . . ?
N1 Ti1 O3 C9 -19.5(5) . . . . ?
N1 Ti1 O5 Ti2 -11.6(10) . . . . ?
N3 Ti3 O12 C41 11.4(5) . . . . ?
N3 Ti3 O13 C48 46.5(4) . . . . ?
N3 Ti3 O14 Ti4 3.1(10) . . . . ?
C50 N4 C58 C59 64.7(5) . . . . ?
C50 N4 C51 C52 177.8(4) . . . . ?
C52 C53 C54 F7 180.0(5) . . . . ?
C52 C53 C54 C55 -0.4(9) . . . . ?
C52 C57 C56 C55 1.5(8) . . . . ?
C18 N2 C26 C27 -57.2(6) . . . . ?
C18 N2 C19 C20 175.6(4) . . . . ?
C59 C64 C63 C62 -0.9(8) . . . . ?
C59 C60 C61 F8 -179.2(5) . . . . ?
C59 C60 C61 C62 -1.6(9) . . . . ?
C16 C11 C10 N1 -59.4(6) . . . . ?
C16 C11 C12 C13 -1.3(8) . . . . ?
C58 N4 C50 C49 -97.9(5) . . . . ?
C58 N4 C51 C52 57.9(5) . . . . ?
C58 C59 C64 O18 -5.8(7) . . . . ?
C58 C59 C64 C63 174.5(5) . . . . ?
C58 C59 C60 C61 -173.1(5) . . . . ?
C64 C59 C58 N4 58.3(6) . . . . ?
C64 C59 C60 C61 2.3(8) . . . . ?
C64 C63 C62 C61 1.6(8) . . . . ?
C2 N1 C10 C11 -67.4(5) . . . . ?
C2 N1 C3 C4 -178.3(4) . . . . ?
C34 N3 C42 C43 64.1(6) . . . . ?
C34 N3 C35 C36 -179.3(4) . . . . ?
C11 C16 C15 C14 -0.7(8) . . . . ?
C11 C12 C13 F2 179.1(5) . . . . ?
C11 C12 C13 C14 -1.5(9) . . . . ?
C53 C52 C51 N4 -126.9(5) . . . . ?
C53 C52 C57 O17 176.5(5) . . . . ?
C53 C52 C57 C56 -3.2(8) . . . . ?
C53 C54 C55 C56 -1.4(9) . . . . ?
C48 C43 C42 N3 61.0(7) . . . . ?
C48 C43 C44 C45 1.6(8) . . . . ?
C48 C47 C46 C45 0.4(8) . . . . ?
C20 C25 C24 C23 1.0(9) . . . . ?
C20 C21 C22 F3 -179.4(5) . . . . ?
C20 C21 C22 C23 0.4(10) . . . . ?
C10 N1 C2 C1 93.4(5) . . . . ?
C10 N1 C3 C4 -59.0(5) . . . . ?
C10 C11 C12 C13 171.8(5) . . . . ?
C51 N4 C50 C49 143.3(4) . . . . ?
C51 N4 C58 C59 -174.8(4) . . . . ?
C51 C52 C53 C54 -177.5(5) . . . . ?
C51 C52 C57 O17 -3.2(7) . . . . ?
C51 C52 C57 C56 177.0(5) . . . . ?
C4 C5 C6 F1 179.1(5) . . . . ?
C4 C5 C6 C7 -1.5(9) . . . . ?
C8 C7 C6 F1 -179.2(5) . . . . ?
C8 C7 C6 C5 1.4(9) . . . . ?
C3 N1 C2 C1 -146.7(4) . . . . ?
C3 N1 C10 C11 171.2(4) . . . . ?
C3 C4 C9 O3 1.1(8) . . . . ?
C3 C4 C9 C8 -178.6(5) . . . . ?
C3 C4 C5 C6 179.5(5) . . . . ?
C57 C52 C53 C54 2.7(8) . . . . ?
C57 C52 C51 N4 52.9(6) . . . . ?
C57 C56 C55 C54 0.8(8) . . . . ?
C26 N2 C18 C17 102.1(5) . . . . ?
C26 N2 C19 C20 -63.3(6) . . . . ?
C26 C27 C28 C29 -178.6(5) . . . . ?
C60 C59 C58 N4 -126.2(5) . . . . ?
C60 C59 C64 O18 178.6(4) . . . . ?
C60 C59 C64 C63 -1.1(7) . . . . ?
C60 C61 C62 C63 -0.4(9) . . . . ?
C32 C27 C28 C29 -0.5(8) . . . . ?
C32 C31 C30 C29 0.1(9) . . . . ?
C25 C20 C19 N2 -39.3(7) . . . . ?
C25 C20 C21 C22 -0.6(9) . . . . ?
C25 C24 C23 C22 -1.1(9) . . . . ?
C41 C36 C35 N3 49.8(7) . . . . ?
C41 C36 C37 C38 1.0(9) . . . . ?
C41 C40 C39 C38 2.6(10) . . . . ?
C7 C8 C9 O3 -180.0(5) . . . . ?
C7 C8 C9 C4 -0.3(8) . . . . ?
C43 C48 C47 C46 1.1(8) . . . . ?
C43 C44 C45 F6 -179.5(5) . . . . ?
C43 C44 C45 C46 -0.2(9) . . . . ?
C27 C32 C31 C30 -3.0(8) . . . . ?
C27 C28 C29 F4 178.1(5) . . . . ?
C27 C28 C29 C30 -2.5(9) . . . . ?
C15 C16 C11 C10 -171.0(5) . . . . ?
C15 C16 C11 C12 2.4(7) . . . . ?
C15 C14 C13 F2 -177.4(5) . . . . ?
C15 C14 C13 C12 3.2(9) . . . . ?
C9 C4 C3 N1 -54.4(7) . . . . ?
C9 C4 C5 C6 0.7(8) . . . . ?
C9 C8 C7 C6 -0.5(8) . . . . ?
C19 N2 C18 C17 -137.4(4) . . . . ?
C19 N2 C26 C27 -177.0(4) . . . . ?
C19 C20 C25 O8 6.5(8) . . . . ?
C19 C20 C25 C24 -174.6(5) . . . . ?
C19 C20 C21 C22 174.1(5) . . . . ?
C47 C48 C43 C42 173.5(5) . . . . ?
C47 C48 C43 C44 -2.1(8) . . . . ?
C47 C46 C45 F6 178.5(5) . . . . ?
C47 C46 C45 C44 -0.9(9) . . . . ?
C21 C20 C25 O8 -179.0(5) . . . . ?
C21 C20 C25 C24 -0.1(8) . . . . ?
C21 C20 C19 N2 146.2(5) . . . . ?
C42 N3 C34 C33 -93.3(5) . . . . ?
C42 N3 C35 C36 60.5(6) . . . . ?
C42 C43 C44 C45 -173.8(5) . . . . ?
C36 C41 C40 C39 -1.1(9) . . . . ?
C36 C37 C38 F5 179.1(6) . . . . ?
C36 C37 C38 C39 0.5(11) . . . . ?
C12 C11 C10 N1 127.4(5) . . . . ?
C44 C43 C42 N3 -123.7(5) . . . . ?
C35 N3 C34 C33 147.5(4) . . . . ?
C35 N3 C42 C43 -175.2(5) . . . . ?
C35 C36 C37 C38 -178.3(6) . . . . ?
C5 C4 C3 N1 126.8(5) . . . . ?
C5 C4 C9 O3 179.9(5) . . . . ?
C5 C4 C9 C8 0.2(8) . . . . ?
C28 C29 C30 C31 2.7(9) . . . . ?
C40 C41 C36 C35 178.5(5) . . . . ?
C40 C41 C36 C37 -0.8(9) . . . . ?
C40 C39 C38 F5 179.1(6) . . . . ?
C40 C39 C38 C37 -2.4(11) . . . . ?
C24 C23 C22 F3 -179.7(6) . . . . ?
C24 C23 C22 C21 0.4(10) . . . . ?
C13 C14 C15 C16 -2.0(8) . . . . ?
C31 C32 C27 C26 -178.6(5) . . . . ?
C31 C32 C27 C28 3.2(8) . . . . ?
C37 C36 C35 N3 -130.9(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
