# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_tiprbut_170704_0m
_database_code_depnum_ccdc_archive 'CCDC 1872957'
loop_
_audit_author_name
_audit_author_address
'Vadim Kessler'
;Swedish University of Agricultural Sciences
Sweden
;
_audit_update_record             
;
2018-10-12 deposited with the CCDC.	2020-02-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H111 O32 P7 Ti5'
_chemical_formula_weight         1632.64

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   27.451(13)
_cell_length_b                   13.802(6)
_cell_length_c                   44.77(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.479(7)
_cell_angle_gamma                90.00
_cell_volume                     16495(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2058
_cell_measurement_theta_min      2.63
_cell_measurement_theta_max      17.77

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6864
_exptl_absorpt_coefficient_mu    0.670
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.7571
_exptl_absorpt_correction_T_max  0.9240
_exptl_absorpt_process_details   'Bruker SADABS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX-II CCD'
_diffrn_measurement_method       'Omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            82518
_diffrn_reflns_av_R_equivalents  0.1164
_diffrn_reflns_av_sigmaI/netI    0.0768
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_theta_min         2.29
_diffrn_reflns_theta_max         25.25
_reflns_number_total             14906
_reflns_number_gt                10002
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0811P)²+186.5712P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         14906
_refine_ls_number_parameters     799
_refine_ls_number_restraints     781
_refine_ls_R_factor_all          0.1336
_refine_ls_R_factor_gt           0.0930
_refine_ls_wR_factor_ref         0.2420
_refine_ls_wR_factor_gt          0.2273
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.13135(5) 0.84729(8) 0.04599(3) 0.0397(3) Uani 1 1 d U . .
Ti2 Ti 0.24117(5) 0.91332(8) 0.08572(3) 0.0403(3) Uani 1 1 d U . .
Ti3 Ti 0.23814(6) 0.67649(9) 0.15869(3) 0.0506(4) Uani 1 1 d U . .
Ti4 Ti 0.13094(6) 0.93873(9) 0.13181(3) 0.0447(3) Uani 1 1 d U . .
Ti5 Ti 0.11885(6) 0.60030(10) 0.11694(3) 0.0504(4) Uani 1 1 d U . .
P1 P 0.24936(8) 0.92321(13) 0.15588(4) 0.0439(5) Uani 1 1 d U . .
P2 P 0.14631(8) 0.60305(12) 0.05008(4) 0.0400(5) Uani 1 1 d U . .
P3 P 0.29401(8) 0.69167(13) 0.10373(4) 0.0419(4) Uani 1 1 d U . .
P4 P 0.05494(8) 0.80188(13) 0.08542(4) 0.0450(5) Uani 1 1 d U . .
P5 P 0.14023(8) 0.72987(14) 0.17474(4) 0.0448(5) Uani 1 1 d U . .
P6 P 0.20496(8) 0.45177(13) 0.15319(4) 0.0441(5) Uani 1 1 d U . .
P7 P 0.14924(9) 1.05457(12) 0.07439(4) 0.0465(5) Uani 1 1 d U . .
O1 O 0.1212(2) 0.9847(3) 0.04981(10) 0.0454(12) Uani 1 1 d U . .
O7 O 0.26447(19) 0.7839(3) 0.09216(10) 0.0417(11) Uani 1 1 d U . .
O11 O 0.18399(18) 0.6689(3) 0.12686(9) 0.0383(10) Uani 1 1 d U . .
O12 O 0.19403(19) 0.6991(3) 0.18691(10) 0.0443(11) Uani 1 1 d U . .
O13 O 0.23885(19) 0.5358(3) 0.16561(11) 0.0455(12) Uani 1 1 d U . .
O2 O 0.06728(19) 0.8209(3) 0.05484(11) 0.0454(11) Uani 1 1 d U . .
O22 O 0.15522(19) 0.4830(3) 0.13400(10) 0.0433(11) Uani 1 1 d U . .
O23 O 0.1277(2) 0.5650(3) 0.07668(10) 0.0440(12) Uani 1 1 d U . .
O26 O 0.2783(2) 0.6090(3) 0.08169(11) 0.0461(12) Uani 1 1 d U . .
O3 O 0.14882(19) 0.7130(3) 0.05005(10) 0.0393(11) Uani 1 1 d U . .
O4 O 0.20124(19) 0.8732(3) 0.04532(10) 0.0408(10) Uani 1 1 d U . .
O27 O 0.2317(3) 0.3817(5) 0.13504(18) 0.0933(15) Uani 1 1 d U . .
O14 O 0.2491(2) 0.8153(3) 0.16088(10) 0.0447(12) Uani 1 1 d U . .
O8 O 0.2047(2) 1.0360(3) 0.08063(10) 0.0448(11) Uani 1 1 d U . .
O17 O 0.1007(2) 1.0102(4) 0.15408(12) 0.0591(14) Uani 1 1 d DU . .
O15 O 0.28867(19) 0.6651(3) 0.13545(10) 0.0441(11) Uani 1 1 d U . .
O30 O 0.11012(19) 0.6466(3) 0.15692(11) 0.0455(11) Uani 1 1 d U . .
O18 O 0.0701(2) 0.8890(3) 0.10631(11) 0.0471(12) Uani 1 1 d U . .
O16 O 0.2984(2) 0.6682(4) 0.19847(11) 0.0540(13) Uani 1 1 d U . .
O5 O 0.16891(18) 0.8635(3) 0.09539(10) 0.0380(10) Uani 1 1 d U . .
O6 O 0.1080(2) 0.8506(3) 0.00614(10) 0.0510(13) Uani 1 1 d U . .
O9 O 0.26884(19) 0.9459(3) 0.12781(10) 0.0437(11) Uani 1 1 d U . .
O19 O 0.1984(2) 0.9678(3) 0.15280(10) 0.0453(11) Uani 1 1 d U . .
O10 O 0.2908(2) 0.9635(3) 0.07249(12) 0.0512(13) Uani 1 1 d U . .
O29 O 0.1974(2) 0.5609(3) 0.04957(11) 0.0511(13) Uani 1 1 d U . .
O24 O 0.0604(2) 0.5223(4) 0.11139(12) 0.0577(14) Uani 1 1 d U . .
O25 O 0.08047(19) 0.7102(3) 0.09925(11) 0.0479(12) Uani 1 1 d U . .
O20 O 0.1308(2) 1.0461(3) 0.10323(11) 0.0484(12) Uani 1 1 d U . .
C7A C 0.1379(3) 1.1767(5) 0.05910(18) 0.0527(19) Uani 1 1 d U . .
C3A C 0.3591(3) 0.7148(6) 0.10621(19) 0.0552(19) Uani 1 1 d U . .
C6A C 0.1944(4) 0.3788(5) 0.18398(17) 0.056(2) Uani 1 1 d U . .
O21 O 0.1362(2) 0.8210(3) 0.15506(10) 0.0450(12) Uani 1 1 d U . .
C2B C 0.1240(3) 0.6035(5) -0.01166(15) 0.054(2) Uani 1 1 d U . .
H2BA H 0.1024 0.5826 -0.0306 0.081 Uiso 1 1 calc R . .
H2BB H 0.1575 0.5810 -0.0106 0.081 Uiso 1 1 calc R . .
H2BC H 0.1239 0.6729 -0.0106 0.081 Uiso 1 1 calc R . .
C7B C 0.1644(4) 1.2474(5) 0.0840(2) 0.067(3) Uani 1 1 d U . .
H7BA H 0.1588 1.3127 0.0766 0.101 Uiso 1 1 calc R . .
H7BB H 0.1997 1.2341 0.0891 0.101 Uiso 1 1 calc R . .
H7BC H 0.1513 1.2398 0.1020 0.101 Uiso 1 1 calc R . .
C1B C 0.2913(4) 1.0884(6) 0.1820(2) 0.086(3) Uani 1 1 d U . .
H1BA H 0.3128 1.1199 0.1993 0.129 Uiso 1 1 calc R . .
H1BB H 0.2581 1.1149 0.1787 0.129 Uiso 1 1 calc R . .
H1BC H 0.3040 1.0986 0.1640 0.129 Uiso 1 1 calc R . .
C3B C 0.3652(4) 0.7549(7) 0.0751(2) 0.072(3) Uani 1 1 d U . .
H3BA H 0.4000 0.7665 0.0761 0.108 Uiso 1 1 calc R . .
H3BB H 0.3469 0.8145 0.0706 0.108 Uiso 1 1 calc R . .
H3BC H 0.3524 0.7087 0.0592 0.108 Uiso 1 1 calc R . .
C5B C 0.1193(5) 0.6705(8) 0.2283(2) 0.085(3) Uani 1 1 d U . .
H5BA H 0.1057 0.6860 0.2456 0.128 Uiso 1 1 calc R . .
H5BB H 0.1540 0.6534 0.2354 0.128 Uiso 1 1 calc R . .
H5BC H 0.1013 0.6169 0.2174 0.128 Uiso 1 1 calc R . .
C41 C 0.2227(3) 0.8457(6) 0.02066(17) 0.055(2) Uani 1 1 d U . .
H41A H 0.2049 0.7903 0.0101 0.066 Uiso 1 1 calc R . .
H41B H 0.2574 0.8271 0.0286 0.066 Uiso 1 1 calc R . .
C2A C 0.1055(3) 0.5623(5) 0.01494(15) 0.0445(17) Uani 1 1 d U . .
C7C C 0.0819(4) 1.1937(6) 0.0502(2) 0.079(3) Uani 1 1 d U . .
H7CA H 0.0753 1.2577 0.0419 0.119 Uiso 1 1 calc R . .
H7CB H 0.0684 1.1872 0.0681 0.119 Uiso 1 1 calc R . .
H7CC H 0.0666 1.1469 0.0351 0.119 Uiso 1 1 calc R . .
C4A C -0.0114(3) 0.7889(6) 0.0800(2) 0.0587(19) Uani 1 1 d U . .
C4B C -0.0239(4) 0.7728(8) 0.1103(2) 0.080(3) Uani 1 1 d U . .
H4BA H -0.0595 0.7652 0.1073 0.120 Uiso 1 1 calc R . .
H4BB H -0.0130 0.8275 0.1234 0.120 Uiso 1 1 calc R . .
H4BC H -0.0073 0.7154 0.1196 0.120 Uiso 1 1 calc R . .
C5A C 0.1145(3) 0.7597(6) 0.20671(18) 0.0580(19) Uani 1 1 d U . .
C7D C 0.1594(5) 1.1841(6) 0.0314(2) 0.078(3) Uani 1 1 d U . .
H7DA H 0.1534 1.2478 0.0228 0.118 Uiso 1 1 calc R . .
H7DB H 0.1439 1.1368 0.0165 0.118 Uiso 1 1 calc R . .
H7DC H 0.1948 1.1724 0.0373 0.118 Uiso 1 1 calc R . .
C6B C 0.1646(4) 0.2881(6) 0.17071(19) 0.069(3) Uani 1 1 d U . .
H6BA H 0.1588 0.2487 0.1872 0.103 Uiso 1 1 calc R . .
H6BB H 0.1833 0.2518 0.1589 0.103 Uiso 1 1 calc R . .
H6BC H 0.1330 0.3073 0.1578 0.103 Uiso 1 1 calc R . .
C6C C 0.2449(4) 0.3490(6) 0.20479(19) 0.067(2) Uani 1 1 d U . .
H6CA H 0.2393 0.3102 0.2214 0.100 Uiso 1 1 calc R . .
H6CB H 0.2635 0.4060 0.2128 0.100 Uiso 1 1 calc R . .
H6CC H 0.2637 0.3122 0.1931 0.100 Uiso 1 1 calc R . .
C2C C 0.1068(4) 0.4509(5) 0.01436(17) 0.062(2) Uani 1 1 d U . .
H2CA H 0.0846 0.4279 -0.0041 0.094 Uiso 1 1 calc R . .
H2CB H 0.0962 0.4259 0.0319 0.094 Uiso 1 1 calc R . .
H2CC H 0.1402 0.4294 0.0150 0.094 Uiso 1 1 calc R . .
C3C C 0.3779(4) 0.7924(7) 0.1308(2) 0.075(3) Uani 1 1 d U . .
H3CA H 0.4128 0.8044 0.1323 0.112 Uiso 1 1 calc R . .
H3CB H 0.3733 0.7699 0.1503 0.112 Uiso 1 1 calc R . .
H3CC H 0.3593 0.8511 0.1253 0.112 Uiso 1 1 calc R . .
C3D C 0.3883(3) 0.6213(7) 0.1137(2) 0.075(3) Uani 1 1 d U . .
H3DA H 0.4232 0.6334 0.1149 0.112 Uiso 1 1 calc R . .
H3DB H 0.3760 0.5744 0.0979 0.112 Uiso 1 1 calc R . .
H3DC H 0.3844 0.5969 0.1331 0.112 Uiso 1 1 calc R . .
C2D C 0.0534(3) 0.5973(6) 0.01391(18) 0.059(2) Uani 1 1 d U . .
H2DA H 0.0312 0.5752 -0.0047 0.088 Uiso 1 1 calc R . .
H2DB H 0.0532 0.6669 0.0145 0.088 Uiso 1 1 calc R . .
H2DC H 0.0425 0.5723 0.0313 0.088 Uiso 1 1 calc R . .
C5C C 0.0601(4) 0.7869(8) 0.1948(2) 0.075(3) Uani 1 1 d U . .
H5CA H 0.0458 0.8035 0.2118 0.112 Uiso 1 1 calc R . .
H5CB H 0.0422 0.7330 0.1839 0.112 Uiso 1 1 calc R . .
H5CC H 0.0577 0.8414 0.1812 0.112 Uiso 1 1 calc R . .
C16 C 0.2944(5) 0.6368(12) 0.2287(2) 0.116(4) Uani 1 1 d U . .
H16A H 0.2683 0.6747 0.2345 0.139 Uiso 1 1 calc R . .
H16B H 0.2834 0.5698 0.2272 0.139 Uiso 1 1 calc R . .
C4C C -0.0292(4) 0.7018(7) 0.0588(2) 0.076(3) Uani 1 1 d U . .
H4CA H -0.0648 0.6944 0.0560 0.114 Uiso 1 1 calc R . .
H4CB H -0.0127 0.6442 0.0680 0.114 Uiso 1 1 calc R . .
H4CC H -0.0213 0.7125 0.0393 0.114 Uiso 1 1 calc R . .
C10 C 0.3119(5) 1.0553(7) 0.0696(3) 0.092(3) Uani 1 1 d U . .
H10A H 0.3207 1.0594 0.0499 0.111 Uiso 1 1 calc R . .
H10B H 0.2871 1.1050 0.0702 0.111 Uiso 1 1 calc R . .
C1C C 0.3419(4) 0.9364(7) 0.1938(2) 0.078(3) Uani 1 1 d U . .
H1CA H 0.3635 0.9671 0.2112 0.117 Uiso 1 1 calc R . .
H1CB H 0.3550 0.9462 0.1759 0.117 Uiso 1 1 calc R . .
H1CC H 0.3401 0.8683 0.1976 0.117 Uiso 1 1 calc R . .
C1D C 0.2673(4) 0.9631(9) 0.2159(2) 0.092(3) Uani 1 1 d U . .
H1DA H 0.2880 0.9932 0.2337 0.139 Uiso 1 1 calc R . .
H1DB H 0.2655 0.8947 0.2194 0.139 Uiso 1 1 calc R . .
H1DC H 0.2342 0.9904 0.2120 0.139 Uiso 1 1 calc R . .
C1A C 0.2896(3) 0.9804(6) 0.18834(18) 0.059(2) Uani 1 1 d U . .
C42 C 0.2202(4) 0.9273(8) -0.0013(2) 0.079(3) Uani 1 1 d U . .
H42A H 0.2351 0.9079 -0.0178 0.118 Uiso 1 1 calc R . .
H42B H 0.2380 0.9820 0.0092 0.118 Uiso 1 1 calc R . .
H42C H 0.1858 0.9447 -0.0095 0.118 Uiso 1 1 calc R . .
C4D C -0.0362(4) 0.8811(7) 0.0652(3) 0.083(3) Uani 1 1 d U . .
H4DA H -0.0719 0.8753 0.0620 0.124 Uiso 1 1 calc R . .
H4DB H -0.0277 0.8910 0.0458 0.124 Uiso 1 1 calc R . .
H4DC H -0.0247 0.9353 0.0784 0.124 Uiso 1 1 calc R . .
C5D C 0.1431(4) 0.8455(7) 0.2239(2) 0.073(3) Uani 1 1 d U . .
H5DA H 0.1294 0.8619 0.2411 0.110 Uiso 1 1 calc R . .
H5DB H 0.1402 0.9001 0.2103 0.110 Uiso 1 1 calc R . .
H5DC H 0.1778 0.8286 0.2311 0.110 Uiso 1 1 calc R . .
C6D C 0.1644(4) 0.4405(6) 0.20173(19) 0.068(2) Uani 1 1 d U . .
H6DA H 0.1581 0.4037 0.2187 0.102 Uiso 1 1 calc R . .
H6DB H 0.1331 0.4587 0.1883 0.102 Uiso 1 1 calc R . .
H6DC H 0.1831 0.4977 0.2094 0.102 Uiso 1 1 calc R . .
C6 C 0.0782(5) 0.9094(8) -0.0161(2) 0.095(3) Uani 1 1 d U . .
H6A H 0.0692 0.9669 -0.0061 0.114 Uiso 1 1 calc R . .
H6B H 0.0978 0.9302 -0.0303 0.114 Uiso 1 1 calc R . .
C24 C 0.0513(4) 0.4238(7) 0.1053(3) 0.091(3) Uani 1 1 d U . .
H24A H 0.0556 0.3899 0.1247 0.109 Uiso 1 1 calc R . .
H24B H 0.0764 0.3993 0.0952 0.109 Uiso 1 1 calc R . .
C241 C 0.0033(5) 0.4006(10) 0.0869(3) 0.129(5) Uani 1 1 d U . .
H24C H 0.0007 0.3318 0.0839 0.194 Uiso 1 1 calc R . .
H24D H -0.0012 0.4324 0.0674 0.194 Uiso 1 1 calc R . .
H24E H -0.0220 0.4220 0.0970 0.194 Uiso 1 1 calc R . .
C191 C 0.3538(7) 1.0725(12) 0.0926(4) 0.168(8) Uani 1 1 d U . .
H19A H 0.3670 1.1354 0.0898 0.252 Uiso 1 1 calc R . .
H19B H 0.3787 1.0241 0.0920 0.252 Uiso 1 1 calc R . .
H19C H 0.3451 1.0702 0.1122 0.252 Uiso 1 1 calc R . .
C161 C 0.3365(6) 0.6432(11) 0.2518(3) 0.124(4) Uani 1 1 d U . .
H16C H 0.3292 0.6214 0.2707 0.186 Uiso 1 1 calc R . .
H16D H 0.3476 0.7094 0.2540 0.186 Uiso 1 1 calc R . .
H16E H 0.3623 0.6035 0.2470 0.186 Uiso 1 1 calc R . .
C61 C 0.0382(6) 0.8696(12) -0.0312(4) 0.155(6) Uani 1 1 d U . .
H61A H 0.0200 0.9147 -0.0461 0.233 Uiso 1 1 calc R . .
H61B H 0.0178 0.8507 -0.0175 0.233 Uiso 1 1 calc R . .
H61C H 0.0465 0.8134 -0.0417 0.233 Uiso 1 1 calc R . .
C17 C 0.0433(9) 1.1047(19) 0.1771(4) 0.239(9) Uani 1 1 d DU . .
H17A H 0.0184 1.1547 0.1730 0.358 Uiso 1 1 calc R . .
H17B H 0.0708 1.1252 0.1934 0.358 Uiso 1 1 calc R . .
H17C H 0.0290 1.0466 0.1832 0.358 Uiso 1 1 calc R . .
C171 C 0.0624(6) 1.0845(11) 0.1480(3) 0.172(7) Uani 1 1 d DU . .
H17D H 0.0347 1.0635 0.1316 0.207 Uiso 1 1 calc R . .
H17E H 0.0760 1.1436 0.1415 0.207 Uiso 1 1 calc R . .
O1A O 0.2905(3) 0.4311(5) 0.10310(17) 0.092(2) Uani 1 1 d DU . .
H1A H 0.2916 0.4880 0.0980 0.138 Uiso 1 1 calc R . .
O2A O 0.3687(3) 0.4030(5) 0.15345(18) 0.0933(15) Uani 1 1 d DU . .
O3A O 0.3738(3) 0.5413(5) 0.19421(18) 0.0933(3) Uani 1 1 d DU . .
H3A H 0.3728 0.4976 0.1817 0.140 Uiso 1 1 calc R . .
C11A C 0.2843(6) 0.3677(9) 0.0753(3) 0.126(4) Uani 1 1 d DU . .
H11A H 0.2810 0.3019 0.0822 0.151 Uiso 1 1 calc R . .
H11B H 0.2523 0.3847 0.0619 0.151 Uiso 1 1 calc R . .
C11B C 0.3173(7) 0.3643(13) 0.0576(3) 0.159(6) Uani 1 1 d DU . .
H21A H 0.3049 0.3223 0.0404 0.238 Uiso 1 1 calc R . .
H21C H 0.3487 0.3399 0.0694 0.238 Uiso 1 1 calc R . .
H21D H 0.3220 0.4282 0.0503 0.238 Uiso 1 1 calc R . .
C21A C 0.3635(8) 0.3020(9) 0.1608(5) 0.168(6) Uani 1 1 d DU . .
H21B H 0.3324 0.2910 0.1670 0.202 Uiso 1 1 calc R . .
H21E H 0.3642 0.2611 0.1433 0.202 Uiso 1 1 calc R . .
C31A C 0.4242(6) 0.5841(17) 0.2018(5) 0.210(7) Uani 1 1 d DU . .
H31A H 0.4252 0.6401 0.2150 0.252 Uiso 1 1 calc R . .
H31B H 0.4341 0.6040 0.1833 0.252 Uiso 1 1 calc R . .
C22B C 0.4052(9) 0.2826(16) 0.1854(5) 0.207(8) Uani 1 1 d U . .
H22A H 0.4043 0.2161 0.1916 0.310 Uiso 1 1 calc R . .
H22B H 0.4039 0.3239 0.2025 0.310 Uiso 1 1 calc R . .
H22C H 0.4356 0.2946 0.1790 0.310 Uiso 1 1 calc R . .
C32B C 0.4611(10) 0.500(2) 0.2194(6) 0.265(9) Uani 1 1 d U . .
H32A H 0.4949 0.5236 0.2248 0.397 Uiso 1 1 calc R . .
H32B H 0.4593 0.4446 0.2062 0.397 Uiso 1 1 calc R . .
H32C H 0.4509 0.4813 0.2377 0.397 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O6 1.750(5) . ?
Ti1 O3 1.912(4) . ?
Ti1 O2 1.925(5) . ?
Ti1 O1 1.931(5) . ?
Ti1 O4 1.959(5) . ?
Ti1 O5 2.223(4) . ?
Ti1 Ti2 3.253(2) . ?
Ti2 O10 1.750(5) . ?
Ti2 O7 1.896(5) . ?
Ti2 O9 1.914(5) . ?
Ti2 O8 1.953(5) . ?
Ti2 O4 1.964(5) . ?
Ti2 O5 2.235(5) . ?
Ti3 O11 1.807(5) . ?
Ti3 O15 1.925(5) . ?
Ti3 O14 1.938(5) . ?
Ti3 O13 1.965(5) . ?
Ti3 O12 1.968(5) . ?
Ti3 O16 2.133(5) . ?
Ti3 P5 3.030(3) . ?
Ti4 O17 1.744(6) . ?
Ti4 O19 1.914(5) . ?
Ti4 O18 1.916(5) . ?
Ti4 O21 1.917(5) . ?
Ti4 O20 1.957(5) . ?
Ti4 O5 2.370(5) . ?
Ti5 O24 1.899(5) . ?
Ti5 O25 1.910(5) . ?
Ti5 O23 1.936(5) . ?
Ti5 O22 1.961(5) . ?
Ti5 O30 1.967(5) . ?
Ti5 O11 1.980(5) . ?
P1 O19 1.505(6) . ?
P1 O14 1.506(5) . ?
P1 O9 1.509(5) . ?
P1 C1A 1.791(8) . ?
P2 O23 1.497(5) . ?
P2 O3 1.520(4) . ?
P2 O29 1.524(6) . ?
P2 C2A 1.795(7) . ?
P3 O26 1.505(5) . ?
P3 O15 1.506(5) . ?
P3 O7 1.533(5) . ?
P3 C3A 1.792(9) . ?
P4 O2 1.508(5) . ?
P4 O25 1.508(5) . ?
P4 O18 1.521(5) . ?
P4 C4A 1.788(9) . ?
P5 O12 1.511(6) . ?
P5 O21 1.524(5) . ?
P5 O30 1.528(5) . ?
P5 C5A 1.785(8) . ?
P6 O22 1.497(5) . ?
P6 O13 1.510(5) . ?
P6 O27 1.554(8) . ?
P6 C6A 1.784(7) . ?
P7 O20 1.497(5) . ?
P7 O8 1.505(6) . ?
P7 O1 1.529(5) . ?
P7 C7A 1.818(7) . ?
O4 C41 1.419(9) . ?
O17 C171 1.4502(11) . ?
O16 C16 1.450(12) . ?
O6 C6 1.393(10) . ?
O10 C10 1.411(9) . ?
O24 C24 1.398(10) . ?
C7A C7D 1.495(12) . ?
C7A C7C 1.512(13) . ?
C7A C7B 1.533(10) . ?
C3A C3D 1.516(12) . ?
C3A C3C 1.537(12) . ?
C3A C3B 1.544(11) . ?
C6A C6D 1.530(12) . ?
C6A C6C 1.535(12) . ?
C6A C6B 1.537(11) . ?
C2B C2A 1.510(10) . ?
C1B C1A 1.520(12) . ?
C5B C5A 1.553(12) . ?
C41 C42 1.486(11) . ?
C2A C2D 1.501(12) . ?
C2A C2C 1.539(9) . ?
C4A C4B 1.491(12) . ?
C4A C4D 1.520(12) . ?
C4A C4C 1.538(12) . ?
C5A C5C 1.512(13) . ?
C5A C5D 1.526(12) . ?
C16 C161 1.363(16) . ?
C10 C191 1.375(17) . ?
C1C C1A 1.525(13) . ?
C1D C1A 1.520(13) . ?
C6 C61 1.273(17) . ?
C24 C241 1.417(14) . ?
C17 C171 1.5396(12) . ?
O1A C11A 1.497(12) . ?
O2A C21A 1.447(9) . ?
O3A C31A 1.471(9) . ?
C11A C11B 1.336(16) . ?
C21A C22B 1.42(2) . ?
C31A C32B 1.62(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Ti1 O3 98.4(2) . . ?
O6 Ti1 O2 94.6(2) . . ?
O3 Ti1 O2 91.0(2) . . ?
O6 Ti1 O1 92.2(2) . . ?
O3 Ti1 O1 169.1(2) . . ?
O2 Ti1 O1 90.5(2) . . ?
O6 Ti1 O4 96.1(2) . . ?
O3 Ti1 O4 87.3(2) . . ?
O2 Ti1 O4 169.3(2) . . ?
O1 Ti1 O4 89.1(2) . . ?
O6 Ti1 O5 170.5(2) . . ?
O3 Ti1 O5 87.42(17) . . ?
O2 Ti1 O5 92.78(19) . . ?
O1 Ti1 O5 81.74(18) . . ?
O4 Ti1 O5 76.59(18) . . ?
O6 Ti1 Ti2 128.5(2) . . ?
O3 Ti1 Ti2 92.27(15) . . ?
O2 Ti1 Ti2 135.65(15) . . ?
O1 Ti1 Ti2 79.12(15) . . ?
O4 Ti1 Ti2 34.01(13) . . ?
O5 Ti1 Ti2 43.28(13) . . ?
O10 Ti2 O7 99.4(2) . . ?
O10 Ti2 O9 94.5(2) . . ?
O7 Ti2 O9 91.7(2) . . ?
O10 Ti2 O8 92.0(2) . . ?
O7 Ti2 O8 168.5(2) . . ?
O9 Ti2 O8 89.2(2) . . ?
O10 Ti2 O4 96.4(2) . . ?
O7 Ti2 O4 88.3(2) . . ?
O9 Ti2 O4 168.9(2) . . ?
O8 Ti2 O4 88.6(2) . . ?
O10 Ti2 O5 169.5(2) . . ?
O7 Ti2 O5 87.92(19) . . ?
O9 Ti2 O5 92.75(19) . . ?
O8 Ti2 O5 80.54(19) . . ?
O4 Ti2 O5 76.20(18) . . ?
O10 Ti2 Ti1 128.40(18) . . ?
O7 Ti2 Ti1 93.21(15) . . ?
O9 Ti2 Ti1 135.13(16) . . ?
O8 Ti2 Ti1 78.15(15) . . ?
O4 Ti2 Ti1 33.92(15) . . ?
O5 Ti2 Ti1 42.99(12) . . ?
O11 Ti3 O15 97.6(2) . . ?
O11 Ti3 O14 100.8(2) . . ?
O15 Ti3 O14 89.2(2) . . ?
O11 Ti3 O13 92.5(2) . . ?
O15 Ti3 O13 91.3(2) . . ?
O14 Ti3 O13 166.6(2) . . ?
O11 Ti3 O12 90.0(2) . . ?
O15 Ti3 O12 171.4(2) . . ?
O14 Ti3 O12 85.6(2) . . ?
O13 Ti3 O12 92.3(2) . . ?
O11 Ti3 O16 172.4(2) . . ?
O15 Ti3 O16 86.0(2) . . ?
O14 Ti3 O16 86.0(2) . . ?
O13 Ti3 O16 80.7(2) . . ?
O12 Ti3 O16 86.9(2) . . ?
O11 Ti3 P5 65.74(16) . . ?
O15 Ti3 P5 159.87(16) . . ?
O14 Ti3 P5 83.31(17) . . ?
O13 Ti3 P5 100.34(17) . . ?
O12 Ti3 P5 25.42(14) . . ?
O16 Ti3 P5 111.93(17) . . ?
O17 Ti4 O19 97.8(2) . . ?
O17 Ti4 O18 94.5(3) . . ?
O19 Ti4 O18 167.6(2) . . ?
O17 Ti4 O21 98.9(2) . . ?
O19 Ti4 O21 88.2(2) . . ?
O18 Ti4 O21 88.0(2) . . ?
O17 Ti4 O20 91.0(2) . . ?
O19 Ti4 O20 90.9(2) . . ?
O18 Ti4 O20 90.7(2) . . ?
O21 Ti4 O20 170.1(2) . . ?
O17 Ti4 O5 170.2(2) . . ?
O19 Ti4 O5 84.23(19) . . ?
O18 Ti4 O5 83.96(19) . . ?
O21 Ti4 O5 90.72(19) . . ?
O20 Ti4 O5 79.42(19) . . ?
O24 Ti5 O25 91.7(2) . . ?
O24 Ti5 O23 91.2(2) . . ?
O25 Ti5 O23 89.5(2) . . ?
O24 Ti5 O22 85.4(2) . . ?
O25 Ti5 O22 176.9(2) . . ?
O23 Ti5 O22 89.5(2) . . ?
O24 Ti5 O30 91.4(2) . . ?
O25 Ti5 O30 87.0(2) . . ?
O23 Ti5 O30 175.6(2) . . ?
O22 Ti5 O30 94.2(2) . . ?
O24 Ti5 O11 172.4(2) . . ?
O25 Ti5 O11 95.5(2) . . ?
O23 Ti5 O11 91.5(2) . . ?
O22 Ti5 O11 87.5(2) . . ?
O30 Ti5 O11 86.3(2) . . ?
O19 P1 O14 112.4(3) . . ?
O19 P1 O9 109.9(3) . . ?
O14 P1 O9 110.1(3) . . ?
O19 P1 C1A 106.2(4) . . ?
O14 P1 C1A 109.8(3) . . ?
O9 P1 C1A 108.3(4) . . ?
O23 P2 O3 112.0(3) . . ?
O23 P2 O29 111.4(3) . . ?
O3 P2 O29 109.8(3) . . ?
O23 P2 C2A 109.2(3) . . ?
O3 P2 C2A 109.3(3) . . ?
O29 P2 C2A 104.8(3) . . ?
O26 P3 O15 110.9(3) . . ?
O26 P3 O7 111.1(3) . . ?
O15 P3 O7 111.2(3) . . ?
O26 P3 C3A 107.8(4) . . ?
O15 P3 C3A 107.4(3) . . ?
O7 P3 C3A 108.3(3) . . ?
O2 P4 O25 109.7(3) . . ?
O2 P4 O18 109.5(3) . . ?
O25 P4 O18 112.1(3) . . ?
O2 P4 C4A 109.3(4) . . ?
O25 P4 C4A 109.5(4) . . ?
O18 P4 C4A 106.7(4) . . ?
O12 P5 O21 111.9(3) . . ?
O12 P5 O30 109.9(3) . . ?
O21 P5 O30 111.2(3) . . ?
O12 P5 C5A 108.1(4) . . ?
O21 P5 C5A 106.5(3) . . ?
O30 P5 C5A 109.0(4) . . ?
O12 P5 Ti3 33.98(18) . . ?
O21 P5 Ti3 90.7(2) . . ?
O30 P5 Ti3 95.5(2) . . ?
C5A P5 Ti3 141.6(3) . . ?
O22 P6 O13 113.1(3) . . ?
O22 P6 O27 111.0(4) . . ?
O13 P6 O27 110.2(4) . . ?
O22 P6 C6A 108.4(4) . . ?
O13 P6 C6A 110.2(3) . . ?
O27 P6 C6A 103.5(4) . . ?
O20 P7 O8 110.9(3) . . ?
O20 P7 O1 110.9(3) . . ?
O8 P7 O1 110.2(3) . . ?
O20 P7 C7A 109.5(3) . . ?
O8 P7 C7A 107.8(4) . . ?
O1 P7 C7A 107.5(3) . . ?
P7 O1 Ti1 128.6(3) . . ?
P3 O7 Ti2 165.1(3) . . ?
Ti3 O11 Ti5 137.6(2) . . ?
P5 O12 Ti3 120.6(3) . . ?
P6 O13 Ti3 135.9(3) . . ?
P4 O2 Ti1 129.0(3) . . ?
P6 O22 Ti5 140.7(3) . . ?
P2 O23 Ti5 142.5(3) . . ?
P2 O3 Ti1 163.3(3) . . ?
C41 O4 Ti1 123.4(5) . . ?
C41 O4 Ti2 123.2(5) . . ?
Ti1 O4 Ti2 112.1(2) . . ?
P1 O14 Ti3 167.4(3) . . ?
P7 O8 Ti2 129.7(3) . . ?
C171 O17 Ti4 135.6(7) . . ?
P3 O15 Ti3 136.9(3) . . ?
P5 O30 Ti5 123.6(3) . . ?
P4 O18 Ti4 136.5(3) . . ?
C16 O16 Ti3 125.6(6) . . ?
Ti1 O5 Ti2 93.73(17) . . ?
Ti1 O5 Ti4 123.5(2) . . ?
Ti2 O5 Ti4 123.42(19) . . ?
C6 O6 Ti1 139.3(6) . . ?
P1 O9 Ti2 129.4(3) . . ?
P1 O19 Ti4 137.0(3) . . ?
C10 O10 Ti2 138.9(6) . . ?
C24 O24 Ti5 133.2(6) . . ?
P4 O25 Ti5 174.4(4) . . ?
P7 O20 Ti4 132.3(3) . . ?
C7D C7A C7C 110.2(8) . . ?
C7D C7A C7B 110.3(7) . . ?
C7C C7A C7B 111.9(7) . . ?
C7D C7A P7 108.0(5) . . ?
C7C C7A P7 108.5(6) . . ?
C7B C7A P7 107.8(5) . . ?
C3D C3A C3C 111.2(8) . . ?
C3D C3A C3B 110.0(8) . . ?
C3C C3A C3B 107.9(7) . . ?
C3D C3A P3 109.3(6) . . ?
C3C C3A P3 109.4(6) . . ?
C3B C3A P3 108.9(6) . . ?
C6D C6A C6C 110.7(7) . . ?
C6D C6A C6B 110.5(8) . . ?
C6C C6A C6B 109.9(7) . . ?
C6D C6A P6 106.9(5) . . ?
C6C C6A P6 109.5(6) . . ?
C6B C6A P6 109.2(5) . . ?
P5 O21 Ti4 177.6(3) . . ?
O4 C41 C42 110.4(7) . . ?
C2D C2A C2B 110.4(6) . . ?
C2D C2A C2C 110.2(7) . . ?
C2B C2A C2C 110.5(6) . . ?
C2D C2A P2 108.8(5) . . ?
C2B C2A P2 108.5(5) . . ?
C2C C2A P2 108.4(5) . . ?
C4B C4A C4D 110.2(9) . . ?
C4B C4A C4C 109.5(8) . . ?
C4D C4A C4C 109.9(8) . . ?
C4B C4A P4 109.5(6) . . ?
C4D C4A P4 108.4(6) . . ?
C4C C4A P4 109.3(7) . . ?
C5C C5A C5D 109.5(8) . . ?
C5C C5A C5B 110.5(8) . . ?
C5D C5A C5B 110.0(8) . . ?
C5C C5A P5 108.5(6) . . ?
C5D C5A P5 109.3(6) . . ?
C5B C5A P5 109.0(6) . . ?
C161 C16 O16 116.9(12) . . ?
C191 C10 O10 112.1(11) . . ?
C1D C1A C1B 110.0(8) . . ?
C1D C1A C1C 110.5(8) . . ?
C1B C1A C1C 110.6(8) . . ?
C1D C1A P1 107.5(6) . . ?
C1B C1A P1 108.7(6) . . ?
C1C C1A P1 109.5(6) . . ?
C61 C6 O6 114.8(12) . . ?
O24 C24 C241 115.6(10) . . ?
O17 C171 C17 110.1(12) . . ?
C11B C11A O1A 123.5(13) . . ?
C22B C21A O2A 104.8(15) . . ?
O3A C31A C32B 105.8(17) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         2.111
_refine_diff_density_min         -2.525
_refine_diff_density_rms         0.117
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_chemical_properties_physical    Moisture-sensitive
####################################################################### 
# 
# 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_tipbu4_170803_0m
_database_code_depnum_ccdc_archive 'CCDC 1872961'
loop_
_audit_author_name
_audit_author_address
'Vadim Kessler'
;Swedish University of Agricultural Sciences
Sweden
;
_audit_update_record             
;
2018-10-12 deposited with the CCDC.	2020-02-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H116 O34 P8 Ti4'
_chemical_formula_weight         1676.77

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   13.546(14)
_cell_length_b                   16.293(17)
_cell_length_c                   18.665(20)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.604(13)
_cell_angle_gamma                90.00
_cell_volume                     4083(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6127
_cell_measurement_theta_min      2.15
_cell_measurement_theta_max      24.21

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1768
_exptl_absorpt_coefficient_mu    0.610
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.8478
_exptl_absorpt_correction_T_max  0.8826
_exptl_absorpt_process_details   'Bruker SADABS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX-II CCD'
_diffrn_measurement_method       'Omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25976
_diffrn_reflns_av_R_equivalents  0.1276
_diffrn_reflns_av_sigmaI/netI    0.0969
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.15
_diffrn_reflns_theta_max         24.34
_reflns_number_total             6592
_reflns_number_gt                3940
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0746P)²+1.1277P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6592
_refine_ls_number_parameters     424
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1185
_refine_ls_R_factor_gt           0.0633
_refine_ls_wR_factor_ref         0.1710
_refine_ls_wR_factor_gt          0.1529
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.101
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.10482(7) 0.86368(5) 0.10466(5) 0.0333(3) Uani 1 1 d . . .
Ti2 Ti -0.13495(7) 0.94724(5) 0.09470(5) 0.0332(3) Uani 1 1 d . . .
P3 P 0.21244(10) 1.03814(7) 0.08703(7) 0.0328(3) Uani 1 1 d . . .
P4 P 0.02497(11) 0.94328(8) 0.24104(7) 0.0361(4) Uani 1 1 d . . .
P5 P 0.10134(11) 0.84862(7) -0.06988(7) 0.0329(3) Uani 1 1 d . . .
P6 P -0.08521(11) 0.75269(7) 0.07835(8) 0.0361(4) Uani 1 1 d . . .
O1 O 0.1375(3) 0.83256(19) 0.00917(18) 0.0376(8) Uani 1 1 d . . .
O6 O -0.2567(3) 0.95198(19) 0.11864(19) 0.0417(9) Uani 1 1 d . . .
O2 O 0.0056(3) 0.92309(18) 0.07693(17) 0.0316(8) Uani 1 1 d . . .
O7 O -0.0782(3) 0.9468(2) 0.19833(18) 0.0407(9) Uani 1 1 d . . .
O12 O -0.0040(3) 0.81809(18) -0.09178(17) 0.0353(8) Uani 1 1 d . . .
O3 O 0.0942(3) 0.88361(19) 0.21062(17) 0.0373(9) Uani 1 1 d . . .
O8 O -0.1084(3) 1.06157(18) 0.08964(19) 0.0379(9) Uani 1 1 d . . .
O4 O 0.0231(3) 0.76172(18) 0.10765(18) 0.0365(8) Uani 1 1 d . . .
O5 O 0.2284(3) 0.78356(19) 0.14740(18) 0.0395(9) Uani 1 1 d . . .
O9 O -0.1471(3) 0.82451(19) 0.09629(19) 0.0396(9) Uani 1 1 d . . .
O11 O -0.0985(3) 0.7364(2) -0.00452(19) 0.0461(10) Uani 1 1 d . . .
O10 O 0.0725(3) 1.0308(2) 0.24964(19) 0.0461(10) Uani 1 1 d . . .
C51 C 0.2887(4) 0.8314(3) -0.0999(3) 0.0485(15) Uani 1 1 d . . .
H51A H 0.3353 0.8045 -0.1266 0.073 Uiso 1 1 calc R . .
H51B H 0.3085 0.8233 -0.0491 0.073 Uiso 1 1 calc R . .
H51C H 0.2877 0.8891 -0.1106 0.073 Uiso 1 1 calc R . .
C3 C 0.3401(4) 1.0712(3) 0.1042(3) 0.0406(13) Uani 1 1 d . . .
C52 C 0.1529(5) 0.8088(4) -0.2008(3) 0.0542(16) Uani 1 1 d . . .
H52A H 0.1978 0.7810 -0.2283 0.081 Uiso 1 1 calc R . .
H52B H 0.1527 0.8664 -0.2115 0.081 Uiso 1 1 calc R . .
H52C H 0.0869 0.7871 -0.2131 0.081 Uiso 1 1 calc R . .
C4 C 0.0106(4) 0.9161(3) 0.3332(3) 0.0394(13) Uani 1 1 d . . .
C53 C 0.1854(5) 0.7036(3) -0.1023(3) 0.0563(17) Uani 1 1 d . . .
H53A H 0.2301 0.6748 -0.1292 0.084 Uiso 1 1 calc R . .
H53B H 0.1192 0.6824 -0.1145 0.084 Uiso 1 1 calc R . .
H53C H 0.2062 0.6965 -0.0515 0.084 Uiso 1 1 calc R . .
C6 C -0.1347(4) 0.6614(3) 0.1155(3) 0.0436(14) Uani 1 1 d . . .
C41 C 0.1110(5) 0.9147(4) 0.3793(3) 0.0595(17) Uani 1 1 d . . .
H41A H 0.1026 0.9004 0.4280 0.089 Uiso 1 1 calc R . .
H41B H 0.1413 0.9679 0.3787 0.089 Uiso 1 1 calc R . .
H41C H 0.1529 0.8747 0.3604 0.089 Uiso 1 1 calc R . .
C50 C 0.2211(5) 0.7055(3) 0.1822(3) 0.0554(16) Uani 1 1 d . . .
H50A H 0.1595 0.7033 0.2034 0.066 Uiso 1 1 calc R . .
H50B H 0.2760 0.6995 0.2208 0.066 Uiso 1 1 calc R . .
C5 C 0.1863(4) 0.7960(3) -0.1211(3) 0.0411(13) Uani 1 1 d . . .
C31 C 0.3453(5) 1.1614(3) 0.0838(4) 0.0653(19) Uani 1 1 d . . .
H31A H 0.4131 1.1798 0.0927 0.098 Uiso 1 1 calc R . .
H31B H 0.3052 1.1932 0.1123 0.098 Uiso 1 1 calc R . .
H31C H 0.3208 1.1681 0.0335 0.098 Uiso 1 1 calc R . .
C501 C 0.2231(5) 0.6366(4) 0.1299(4) 0.072(2) Uani 1 1 d . . .
H50C H 0.2181 0.5853 0.1545 0.108 Uiso 1 1 calc R . .
H50D H 0.2844 0.6381 0.1094 0.108 Uiso 1 1 calc R . .
H50E H 0.1681 0.6419 0.0921 0.108 Uiso 1 1 calc R . .
C42 C -0.0582(5) 0.9789(4) 0.3625(3) 0.0586(17) Uani 1 1 d . . .
H42A H -0.0661 0.9651 0.4114 0.088 Uiso 1 1 calc R . .
H42B H -0.1221 0.9781 0.3332 0.088 Uiso 1 1 calc R . .
H42C H -0.0297 1.0327 0.3612 0.088 Uiso 1 1 calc R . .
C32 C 0.3793(5) 1.0572(4) 0.1838(3) 0.0590(17) Uani 1 1 d . . .
H32A H 0.4474 1.0748 0.1931 0.089 Uiso 1 1 calc R . .
H32B H 0.3752 0.9999 0.1949 0.089 Uiso 1 1 calc R . .
H32C H 0.3399 1.0881 0.2134 0.089 Uiso 1 1 calc R . .
C61 C -0.2428(5) 0.6525(3) 0.0841(4) 0.0617(18) Uani 1 1 d . . .
H61A H -0.2702 0.6045 0.1039 0.093 Uiso 1 1 calc R . .
H61B H -0.2478 0.6473 0.0325 0.093 Uiso 1 1 calc R . .
H61C H -0.2791 0.7001 0.0960 0.093 Uiso 1 1 calc R . .
C43 C -0.0370(5) 0.8316(3) 0.3322(3) 0.0564(16) Uani 1 1 d . . .
H43A H -0.0453 0.8159 0.3805 0.085 Uiso 1 1 calc R . .
H43B H 0.0051 0.7926 0.3124 0.085 Uiso 1 1 calc R . .
H43C H -0.1008 0.8331 0.3028 0.085 Uiso 1 1 calc R . .
C62 C -0.1232(5) 0.6705(4) 0.1967(3) 0.0600(18) Uani 1 1 d . . .
H62A H -0.1494 0.6227 0.2176 0.090 Uiso 1 1 calc R . .
H62B H -0.1590 0.7182 0.2091 0.090 Uiso 1 1 calc R . .
H62C H -0.0539 0.6765 0.2150 0.090 Uiso 1 1 calc R . .
C63 C -0.0765(5) 0.5866(3) 0.0943(4) 0.065(2) Uani 1 1 d . . .
H63A H -0.1023 0.5379 0.1142 0.097 Uiso 1 1 calc R . .
H63B H -0.0074 0.5927 0.1130 0.097 Uiso 1 1 calc R . .
H63C H -0.0835 0.5822 0.0426 0.097 Uiso 1 1 calc R . .
C33 C 0.3995(5) 1.0197(4) 0.0572(3) 0.0545(16) Uani 1 1 d . . .
H33A H 0.4681 1.0360 0.0652 0.082 Uiso 1 1 calc R . .
H33B H 0.3737 1.0278 0.0073 0.082 Uiso 1 1 calc R . .
H33C H 0.3940 0.9628 0.0694 0.082 Uiso 1 1 calc R . .
O13 O 0.1730(3) 1.05551(18) 0.00962(18) 0.0365(8) Uani 1 1 d . . .
O14 O 0.2093(3) 0.94974(18) 0.10948(18) 0.0368(8) Uani 1 1 d . . .
O15 O 0.1509(3) 1.09092(19) 0.13641(17) 0.0386(9) Uani 1 1 d . . .
O16 O 0.4270(3) 0.7967(2) 0.1529(2) 0.0629(12) Uani 1 1 d . . .
H16A H 0.3678 0.7843 0.1486 0.094 Uiso 1 1 calc R . .
O17 O -0.0752(3) 0.7092(2) -0.2018(2) 0.0615(12) Uani 1 1 d . . .
H17A H -0.0789 0.7043 -0.2458 0.092 Uiso 1 1 calc R . .
C17 C -0.1454(5) 0.6569(3) -0.1757(3) 0.0554(16) Uani 1 1 d . . .
H17B H -0.1915 0.6369 -0.2161 0.067 Uiso 1 1 calc R . .
H17C H -0.1834 0.6880 -0.1444 0.067 Uiso 1 1 calc R . .
C16 C 0.4828(5) 0.7300(4) 0.1309(4) 0.0654(19) Uani 1 1 d . . .
H16B H 0.4607 0.6794 0.1511 0.079 Uiso 1 1 calc R . .
H16C H 0.5527 0.7376 0.1488 0.079 Uiso 1 1 calc R . .
C171 C -0.0977(6) 0.5859(4) -0.1348(4) 0.074(2) Uani 1 1 d . . .
H17D H -0.1480 0.5520 -0.1183 0.110 Uiso 1 1 calc R . .
H17E H -0.0532 0.6054 -0.0941 0.110 Uiso 1 1 calc R . .
H17F H -0.0609 0.5544 -0.1658 0.110 Uiso 1 1 calc R . .
C60 C -0.3275(6) 0.9046(4) 0.1505(4) 0.073(2) Uani 1 1 d . . .
H60A H -0.3879 0.9001 0.1165 0.088 Uiso 1 1 calc R . .
H60B H -0.3012 0.8496 0.1598 0.088 Uiso 1 1 calc R . .
C601 C -0.3510(7) 0.9383(5) 0.2154(4) 0.098(3) Uani 1 1 d . . .
H60C H -0.3991 0.9040 0.2344 0.147 Uiso 1 1 calc R . .
H60D H -0.3782 0.9923 0.2065 0.147 Uiso 1 1 calc R . .
H60E H -0.2918 0.9415 0.2498 0.147 Uiso 1 1 calc R . .
C161 C 0.4697(6) 0.7241(5) 0.0503(4) 0.089(3) Uani 1 1 d . . .
H16D H 0.5084 0.6791 0.0360 0.134 Uiso 1 1 calc R . .
H16E H 0.4917 0.7742 0.0304 0.134 Uiso 1 1 calc R . .
H16F H 0.4007 0.7153 0.0327 0.134 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O2 1.682(4) . ?
Ti1 O1 1.959(4) . ?
Ti1 O14 1.986(4) . ?
Ti1 O4 2.001(4) . ?
Ti1 O3 2.028(4) . ?
Ti1 O5 2.189(4) . ?
Ti2 O6 1.767(4) . ?
Ti2 O8 1.902(4) . ?
Ti2 O13 1.948(4) 3_575 ?
Ti2 O7 1.984(4) . ?
Ti2 O9 2.007(4) . ?
Ti2 O2 2.014(4) . ?
P3 O13 1.500(4) . ?
P3 O14 1.502(4) . ?
P3 O15 1.577(4) . ?
P3 C3 1.799(6) . ?
P4 O3 1.513(4) . ?
P4 O7 1.516(4) . ?
P4 O10 1.564(4) . ?
P4 C4 1.811(5) . ?
P5 O1 1.515(4) . ?
P5 O12 1.515(4) . ?
P5 O8 1.515(3) 3_575 ?
P5 C5 1.808(5) . ?
P6 O9 1.503(4) . ?
P6 O4 1.504(4) . ?
P6 O11 1.556(4) . ?
P6 C6 1.806(5) . ?
O6 C60 1.421(7) . ?
O8 P5 1.515(3) 3_575 ?
O5 C50 1.438(6) . ?
C51 C5 1.506(8) . ?
C3 C33 1.518(8) . ?
C3 C31 1.523(7) . ?
C3 C32 1.527(8) . ?
C52 C5 1.509(8) . ?
C4 C41 1.509(8) . ?
C4 C43 1.519(7) . ?
C4 C42 1.533(8) . ?
C53 C5 1.546(7) . ?
C6 C62 1.510(8) . ?
C6 C61 1.510(9) . ?
C6 C63 1.532(7) . ?
C50 C501 1.490(8) . ?
O13 Ti2 1.948(4) 3_575 ?
O16 C16 1.416(7) . ?
O17 C17 1.411(7) . ?
C17 C171 1.486(9) . ?
C16 C161 1.494(9) . ?
C60 C601 1.406(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
O2 Ti1 O1 97.86(16) . . ?
O2 Ti1 O14 98.25(17) . . ?
O1 Ti1 O14 88.77(14) . . ?
O2 Ti1 O4 93.67(17) . . ?
O1 Ti1 O4 90.16(14) . . ?
O14 Ti1 O4 168.07(15) . . ?
O2 Ti1 O3 92.92(15) . . ?
O1 Ti1 O3 169.21(15) . . ?
O14 Ti1 O3 89.13(14) . . ?
O4 Ti1 O3 89.71(14) . . ?
O2 Ti1 O5 175.80(15) . . ?
O1 Ti1 O5 85.60(14) . . ?
O14 Ti1 O5 84.17(15) . . ?
O4 Ti1 O5 83.90(15) . . ?
O3 Ti1 O5 83.66(14) . . ?
O6 Ti2 O8 99.13(15) . . ?
O6 Ti2 O13 96.99(17) . 3_575 ?
O8 Ti2 O13 89.97(14) . 3_575 ?
O6 Ti2 O7 90.45(17) . . ?
O8 Ti2 O7 90.05(14) . . ?
O13 Ti2 O7 172.47(15) 3_575 . ?
O6 Ti2 O9 87.64(15) . . ?
O8 Ti2 O9 173.22(16) . . ?
O13 Ti2 O9 88.88(14) 3_575 . ?
O7 Ti2 O9 90.21(14) . . ?
O6 Ti2 O2 169.95(14) . . ?
O8 Ti2 O2 89.67(14) . . ?
O13 Ti2 O2 87.79(14) 3_575 . ?
O7 Ti2 O2 84.68(14) . . ?
O9 Ti2 O2 83.61(13) . . ?
O13 P3 O14 115.47(19) . . ?
O13 P3 O15 108.2(2) . . ?
O14 P3 O15 108.8(2) . . ?
O13 P3 C3 109.1(2) . . ?
O14 P3 C3 107.4(2) . . ?
O15 P3 C3 107.6(2) . . ?
O3 P4 O7 113.7(2) . . ?
O3 P4 O10 110.9(2) . . ?
O7 P4 O10 111.0(2) . . ?
O3 P4 C4 110.4(2) . . ?
O7 P4 C4 107.5(2) . . ?
O10 P4 C4 102.7(2) . . ?
O1 P5 O12 112.18(19) . . ?
O1 P5 O8 112.41(19) . 3_575 ?
O12 P5 O8 109.8(2) . 3_575 ?
O1 P5 C5 106.7(2) . . ?
O12 P5 C5 110.1(2) . . ?
O8 P5 C5 105.3(2) 3_575 . ?
O9 P6 O4 112.9(2) . . ?
O9 P6 O11 111.1(2) . . ?
O4 P6 O11 110.9(2) . . ?
O9 P6 C6 108.0(2) . . ?
O4 P6 C6 109.6(2) . . ?
O11 P6 C6 104.0(2) . . ?
P5 O1 Ti1 139.4(2) . . ?
C60 O6 Ti2 141.8(4) . . ?
Ti1 O2 Ti2 142.79(19) . . ?
P4 O7 Ti2 136.4(2) . . ?
P4 O3 Ti1 126.6(2) . . ?
P5 O8 Ti2 167.5(2) 3_575 . ?
P6 O4 Ti1 126.0(2) . . ?
C50 O5 Ti1 126.7(3) . . ?
P6 O9 Ti2 136.3(2) . . ?
C33 C3 C31 110.1(5) . . ?
C33 C3 C32 109.7(5) . . ?
C31 C3 C32 111.4(5) . . ?
C33 C3 P3 107.6(4) . . ?
C31 C3 P3 108.6(4) . . ?
C32 C3 P3 109.3(4) . . ?
C41 C4 C43 110.0(5) . . ?
C41 C4 C42 110.6(5) . . ?
C43 C4 C42 109.3(5) . . ?
C41 C4 P4 110.1(4) . . ?
C43 C4 P4 108.0(4) . . ?
C42 C4 P4 108.8(4) . . ?
C62 C6 C61 111.4(5) . . ?
C62 C6 C63 110.4(5) . . ?
C61 C6 C63 109.2(5) . . ?
C62 C6 P6 108.1(4) . . ?
C61 C6 P6 108.7(4) . . ?
C63 C6 P6 109.1(4) . . ?
O5 C50 C501 111.3(5) . . ?
C51 C5 C52 110.6(4) . . ?
C51 C5 C53 110.4(5) . . ?
C52 C5 C53 110.4(5) . . ?
C51 C5 P5 107.9(4) . . ?
C52 C5 P5 109.0(4) . . ?
C53 C5 P5 108.4(4) . . ?
P3 O13 Ti2 166.5(2) . 3_575 ?
P3 O14 Ti1 135.3(2) . . ?
O17 C17 C171 112.3(6) . . ?
O16 C16 C161 110.2(6) . . ?
C601 C60 O6 113.0(6) . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        24.34
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.926
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.112
####################################################################### 
# 
# 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_tiacopbu
_database_code_depnum_ccdc_archive 'CCDC 1872958'
loop_
_audit_author_name
_audit_author_address
'Vadim Kessler'
;Swedish University of Agricultural Sciences
Sweden
;
_audit_update_record             
;
2018-10-12 deposited with the CCDC.	2020-02-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H92 O24 P4 Ti4'
_chemical_formula_weight         1368.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C2/c  '

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

_cell_length_a                   25.010(5)
_cell_length_b                   13.950(3)
_cell_length_c                   22.820(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.44(3)
_cell_angle_gamma                90.00
_cell_volume                     7190(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9073
_cell_measurement_theta_min      2.3170
_cell_measurement_theta_max      24.9173

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2880
_exptl_absorpt_coefficient_mu    0.582
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.8446
_exptl_absorpt_correction_T_max  0.8924
_exptl_absorpt_process_details   'Bruker SADABS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX-II CCD'
_diffrn_measurement_method       'Omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28268
_diffrn_reflns_av_R_equivalents  0.0871
_diffrn_reflns_av_sigmaI/netI    0.0703
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.16
_diffrn_reflns_theta_max         25.16
_reflns_number_total             6291
_reflns_number_gt                4068
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT, SADABS and XPREP'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0704P)²+22.7266P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00089(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         6291
_refine_ls_number_parameters     362
_refine_ls_number_restraints     310
_refine_ls_R_factor_all          0.1185
_refine_ls_R_factor_gt           0.0860
_refine_ls_wR_factor_ref         0.2584
_refine_ls_wR_factor_gt          0.2398
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.09217(4) 0.74250(7) 0.23473(5) 0.0464(3) Uani 1 1 d U . .
Ti2 Ti 0.06754(6) 0.47847(9) 0.37273(6) 0.0657(4) Uani 1 1 d U . .
P3 P 0.04948(6) 0.71453(11) 0.35748(7) 0.0467(4) Uani 1 1 d U . .
P4 P 0.07640(7) 0.50221(10) 0.22817(8) 0.0514(4) Uani 1 1 d U . .
O6 O 0.06656(17) 0.7249(3) 0.30081(17) 0.0504(9) Uani 1 1 d U . .
O4 O 0.01472(17) 0.7413(3) 0.16427(19) 0.0526(9) Uani 1 1 d U . .
O7 O 0.07232(18) 0.4919(3) 0.29304(19) 0.0591(10) Uani 1 1 d U . .
O5 O 0.17524(19) 0.7282(3) 0.3022(2) 0.0679(12) Uani 1 1 d U . .
O2 O 0.09729(19) 0.6017(3) 0.2220(2) 0.0587(10) Uani 1 1 d U . .
O11 O 0.12954(19) 0.7494(3) 0.1717(2) 0.0592(10) Uani 1 1 d U . .
O9 O 0.05603(19) 0.4504(3) 0.4534(2) 0.0617(11) Uani 1 1 d U . .
O3 O 0.0986(2) 0.8703(3) 0.2402(2) 0.0688(12) Uani 1 1 d U . .
O10 O 0.1460(2) 0.4751(3) 0.4239(2) 0.0748(12) Uani 1 1 d U . .
O12 O 0.0653(2) 0.3374(3) 0.3630(2) 0.0764(13) Uani 1 1 d U . .
O1 O 0.0629(2) 0.6153(3) 0.3873(2) 0.0630(11) Uani 1 1 d U . .
O8 O -0.0201(2) 0.4759(3) 0.3289(2) 0.0683(11) Uani 1 1 d U . .
C4 C 0.1819(3) 0.7286(5) 0.1796(4) 0.0681(17) Uani 1 1 d U . .
C9 C 0.0473(4) 0.3767(6) 0.4778(4) 0.081(2) Uani 1 1 d U . .
C3 C 0.2266(3) 0.7047(5) 0.2402(4) 0.0763(18) Uani 1 1 d U . .
H3A H 0.2623 0.6840 0.2410 0.092 Uiso 1 1 calc R . .
C6 C 0.1327(3) 0.4175(5) 0.2309(4) 0.0726(18) Uani 1 1 d U . .
C15 C 0.0924(3) 0.8007(5) 0.4203(3) 0.0697(17) Uani 1 1 d U . .
C5 C 0.1912(4) 0.7342(8) 0.1198(4) 0.111(3) Uani 1 1 d U . .
H5A H 0.1547 0.7514 0.0838 0.167 Uiso 1 1 calc R . .
H5B H 0.2043 0.6731 0.1117 0.167 Uiso 1 1 calc R . .
H5C H 0.2207 0.7819 0.1253 0.167 Uiso 1 1 calc R . .
C2 C 0.2234(3) 0.7086(5) 0.2979(4) 0.0665(16) Uani 1 1 d U . .
C8 C 0.0453(5) 0.2861(6) 0.4485(5) 0.104(3) Uani 1 1 d U . .
H8B H 0.0347 0.2338 0.4665 0.124 Uiso 1 1 calc R . .
C10 C 0.1257(7) 0.9533(8) 0.2320(6) 0.147(5) Uani 1 1 d U . .
H10 H 0.1549 0.9198 0.2216 0.177 Uiso 1 1 calc R . .
C6A C 0.1122(4) 0.3164(5) 0.2351(5) 0.107(3) Uani 1 1 d U . .
H6AA H 0.1419 0.2715 0.2368 0.160 Uiso 1 1 calc R . .
H6AB H 0.0759 0.3035 0.1977 0.160 Uiso 1 1 calc R . .
H6AC H 0.1059 0.3103 0.2736 0.160 Uiso 1 1 calc R . .
C1 C 0.2744(4) 0.6894(6) 0.3590(4) 0.097(3) Uani 1 1 d U . .
H1A H 0.2630 0.6946 0.3941 0.146 Uiso 1 1 calc R . .
H1B H 0.3050 0.7351 0.3651 0.146 Uiso 1 1 calc R . .
H1C H 0.2888 0.6259 0.3582 0.146 Uiso 1 1 calc R . .
C15A C 0.0772(4) 0.7950(7) 0.4766(4) 0.105(3) Uani 1 1 d U . .
H15A H 0.1005 0.8405 0.5090 0.157 Uiso 1 1 calc R . .
H15B H 0.0852 0.7316 0.4946 0.157 Uiso 1 1 calc R . .
H15C H 0.0359 0.8093 0.4624 0.157 Uiso 1 1 calc R . .
C6B C 0.1886(4) 0.4392(6) 0.2889(5) 0.098(2) Uani 1 1 d U . .
H6BA H 0.2189 0.3954 0.2909 0.147 Uiso 1 1 calc R . .
H6BB H 0.1822 0.4327 0.3274 0.147 Uiso 1 1 calc R . .
H6BC H 0.2007 0.5036 0.2860 0.147 Uiso 1 1 calc R . .
C7 C 0.0577(4) 0.2674(6) 0.3956(5) 0.094(2) Uani 1 1 d U . .
C14A C 0.2383(7) 0.4041(11) 0.4785(8) 0.197(5) Uani 1 1 d DU . .
H14A H 0.2210 0.3536 0.4475 0.295 Uiso 1 1 calc R . .
H14B H 0.2627 0.3768 0.5201 0.295 Uiso 1 1 calc R . .
H14C H 0.2620 0.4443 0.4648 0.295 Uiso 1 1 calc R . .
C13 C 0.0406(4) 0.3886(7) 0.5402(4) 0.108(3) Uani 1 1 d U . .
H13A H 0.0437 0.4553 0.5516 0.161 Uiso 1 1 calc R . .
H13B H 0.0713 0.3534 0.5743 0.161 Uiso 1 1 calc R . .
H13C H 0.0027 0.3648 0.5344 0.161 Uiso 1 1 calc R . .
C14 C 0.1913(7) 0.4613(12) 0.4833(5) 0.181(5) Uani 1 1 d U . .
H14D H 0.1734 0.4121 0.5000 0.217 Uiso 1 1 calc R . .
C6C C 0.1400(5) 0.4275(7) 0.1677(5) 0.109(3) Uani 1 1 d U . .
H6CA H 0.1700 0.3839 0.1684 0.164 Uiso 1 1 calc R . .
H6CB H 0.1514 0.4920 0.1637 0.164 Uiso 1 1 calc R . .
H6CC H 0.1031 0.4128 0.1314 0.164 Uiso 1 1 calc R . .
C14B C 0.2073(7) 0.5316(10) 0.5356(7) 0.185(4) Uani 1 1 d DU . .
H14E H 0.1721 0.5621 0.5335 0.278 Uiso 1 1 calc R . .
H14F H 0.2331 0.5790 0.5309 0.278 Uiso 1 1 calc R . .
H14G H 0.2273 0.4999 0.5767 0.278 Uiso 1 1 calc R . .
C15C C 0.0802(5) 0.9003(6) 0.3907(5) 0.113(3) Uani 1 1 d U . .
H15D H 0.1030 0.9464 0.4230 0.170 Uiso 1 1 calc R . .
H15E H 0.0388 0.9146 0.3753 0.170 Uiso 1 1 calc R . .
H15F H 0.0911 0.9028 0.3552 0.170 Uiso 1 1 calc R . .
C15B C 0.1580(4) 0.7765(7) 0.4424(4) 0.111(3) Uani 1 1 d U . .
H15G H 0.1819 0.8210 0.4754 0.167 Uiso 1 1 calc R . .
H15H H 0.1677 0.7808 0.4061 0.167 Uiso 1 1 calc R . .
H15I H 0.1656 0.7126 0.4597 0.167 Uiso 1 1 calc R . .
C10A C 0.1648(9) 0.9947(11) 0.2850(8) 0.265(11) Uani 1 1 d U . .
H10A H 0.1810 1.0500 0.2734 0.397 Uiso 1 1 calc R . .
H10B H 0.1961 0.9503 0.3084 0.397 Uiso 1 1 calc R . .
H10C H 0.1459 1.0141 0.3118 0.397 Uiso 1 1 calc R . .
C11 C 0.0543(7) 0.1729(7) 0.3675(6) 0.177(6) Uani 1 1 d U . .
H11A H 0.0645 0.1773 0.3316 0.265 Uiso 1 1 calc R . .
H11B H 0.0147 0.1486 0.3527 0.265 Uiso 1 1 calc R . .
H11C H 0.0814 0.1305 0.3997 0.265 Uiso 1 1 calc R . .
C10B C 0.0978(6) 0.9998(11) 0.1720(7) 0.173(4) Uani 1 1 d U . .
H10D H 0.1205 1.0549 0.1716 0.259 Uiso 1 1 calc R . .
H10E H 0.0588 1.0197 0.1655 0.259 Uiso 1 1 calc R . .
H10F H 0.0947 0.9566 0.1380 0.259 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O3 1.790(4) . ?
Ti1 O6 1.890(4) . ?
Ti1 O4 1.914(4) . ?
Ti1 O5 1.995(4) . ?
Ti1 O2 1.997(4) . ?
Ti1 O11 2.026(4) . ?
Ti2 O10 1.801(5) . ?
Ti2 O7 1.882(4) . ?
Ti2 O1 1.949(4) . ?
Ti2 O12 1.978(4) . ?
Ti2 O8 1.981(5) . ?
Ti2 O9 2.020(4) . ?
P3 O4 1.510(4) 2 ?
P3 O1 1.516(4) . ?
P3 O6 1.533(4) . ?
P3 C15 1.825(6) . ?
P4 O8 1.496(5) 2 ?
P4 O2 1.511(4) . ?
P4 O7 1.534(4) . ?
P4 C6 1.818(6) . ?
O4 P3 1.510(4) 2 ?
O5 C2 1.278(8) . ?
O11 C4 1.275(8) . ?
O9 C9 1.231(8) . ?
O3 C10 1.393(10) . ?
O10 C14 1.356(11) . ?
O12 C7 1.290(9) . ?
O8 P4 1.496(5) 2 ?
C4 C3 1.395(10) . ?
C4 C5 1.482(10) . ?
C9 C8 1.422(11) . ?
C9 C13 1.513(10) . ?
C3 C2 1.356(10) . ?
C6 C6B 1.486(11) . ?
C6 C6C 1.537(11) . ?
C6 C6A 1.518(10) . ?
C15 C15A 1.490(11) . ?
C15 C15C 1.516(11) . ?
C15 C15B 1.534(11) . ?
C2 C1 1.454(10) . ?
C8 C7 1.393(12) . ?
C10 C10A 1.319(15) . ?
C10 C10B 1.400(15) . ?
C7 C11 1.451(12) . ?
C14A C14 1.463(17) . ?
C14A C14B 2.516(10) . ?
C14 C14B 1.462(16) . ?

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
O3 Ti1 O6 97.15(19) . . ?
O3 Ti1 O4 95.44(19) . . ?
O6 Ti1 O4 95.83(17) . . ?
O3 Ti1 O5 90.8(2) . . ?
O6 Ti1 O5 88.22(18) . . ?
O4 Ti1 O5 172.07(19) . . ?
O3 Ti1 O2 168.6(2) . . ?
O6 Ti1 O2 93.03(17) . . ?
O4 Ti1 O2 88.54(17) . . ?
O5 Ti1 O2 84.43(18) . . ?
O3 Ti1 O11 86.98(19) . . ?
O6 Ti1 O11 171.84(18) . . ?
O4 Ti1 O11 90.75(17) . . ?
O5 Ti1 O11 84.68(19) . . ?
O2 Ti1 O11 82.29(17) . . ?
O10 Ti2 O7 97.2(2) . . ?
O10 Ti2 O1 92.5(2) . . ?
O7 Ti2 O1 95.79(17) . . ?
O10 Ti2 O12 91.0(2) . . ?
O7 Ti2 O12 90.08(19) . . ?
O1 Ti2 O12 172.7(2) . . ?
O10 Ti2 O8 170.9(2) . . ?
O7 Ti2 O8 91.72(19) . . ?
O1 Ti2 O8 88.25(19) . . ?
O12 Ti2 O8 87.3(2) . . ?
O10 Ti2 O9 86.9(2) . . ?
O7 Ti2 O9 173.1(2) . . ?
O1 Ti2 O9 89.55(18) . . ?
O12 Ti2 O9 84.28(18) . . ?
O8 Ti2 O9 84.04(18) . . ?
O4 P3 O1 111.9(2) 2 . ?
O4 P3 O6 110.0(2) 2 . ?
O1 P3 O6 112.2(2) . . ?
O4 P3 C15 106.2(3) 2 . ?
O1 P3 C15 107.9(3) . . ?
O6 P3 C15 108.5(3) . . ?
O8 P4 O2 112.2(3) 2 . ?
O8 P4 O7 112.9(3) 2 . ?
O2 P4 O7 110.2(2) . . ?
O8 P4 C6 107.2(3) 2 . ?
O2 P4 C6 107.9(3) . . ?
O7 P4 C6 106.1(3) . . ?
P3 O6 Ti1 176.1(3) . . ?
P3 O4 Ti1 145.9(3) 2 . ?
P4 O7 Ti2 179.7(3) . . ?
C2 O5 Ti1 131.7(5) . . ?
P4 O2 Ti1 147.5(3) . . ?
C4 O11 Ti1 130.3(4) . . ?
C9 O9 Ti2 134.1(5) . . ?
C10 O3 Ti1 148.4(7) . . ?
C14 O10 Ti2 149.4(8) . . ?
C7 O12 Ti2 133.9(5) . . ?
P3 O1 Ti2 146.7(3) . . ?
P4 O8 Ti2 149.1(3) 2 . ?
O11 C4 C3 122.2(6) . . ?
O11 C4 C5 114.6(7) . . ?
C3 C4 C5 123.2(7) . . ?
O9 C9 C8 120.4(7) . . ?
O9 C9 C13 116.5(7) . . ?
C8 C9 C13 123.0(7) . . ?
C2 C3 C4 126.5(7) . . ?
C6B C6 C6C 111.9(7) . . ?
C6B C6 C6A 110.3(7) . . ?
C6C C6 C6A 108.9(7) . . ?
C6B C6 P4 108.4(5) . . ?
C6C C6 P4 108.1(5) . . ?
C6A C6 P4 109.2(5) . . ?
C15A C15 C15C 110.8(7) . . ?
C15A C15 C15B 109.8(7) . . ?
C15C C15 C15B 109.3(8) . . ?
C15A C15 P3 111.1(6) . . ?
C15C C15 P3 108.4(5) . . ?
C15B C15 P3 107.4(5) . . ?
O5 C2 C3 122.3(6) . . ?
O5 C2 C1 115.7(7) . . ?
C3 C2 C1 122.0(7) . . ?
C7 C8 C9 126.7(8) . . ?
C10A C10 C10B 123.7(12) . . ?
C10A C10 O3 116.9(10) . . ?
C10B C10 O3 116.7(11) . . ?
O12 C7 C8 120.0(7) . . ?
O12 C7 C11 115.4(9) . . ?
C8 C7 C11 124.0(9) . . ?
C14 C14A C14B 30.7(7) . . ?
O10 C14 C14A 110.9(12) . . ?
O10 C14 C14B 122.6(12) . . ?
C14A C14 C14B 118.6(12) . . ?
C14 C14B C14A 30.7(7) . . ?

_diffrn_measured_fraction_theta_max 0.975
_diffrn_reflns_theta_full        25.16
_diffrn_measured_fraction_theta_full 0.975
_refine_diff_density_max         1.038
_refine_diff_density_min         -0.994
_refine_diff_density_rms         0.097
####################################################################### 
# 
# 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_tipbunw
_database_code_depnum_ccdc_archive 'CCDC 1872959'
loop_
_audit_author_name
_audit_author_address
'Vadim Kessler'
;Swedish University of Agricultural Sciences
Sweden
;
_audit_update_record             
;
2018-10-12 deposited with the CCDC.	2020-02-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H69 O16 P Ti4'
_chemical_formula_weight         884.40

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.918(5)
_cell_length_b                   11.667(6)
_cell_length_c                   19.845(10)
_cell_angle_alpha                98.141(6)
_cell_angle_beta                 90.067(6)
_cell_angle_gamma                116.790(5)
_cell_volume                     2227.9(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7538
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      28.18

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             936
_exptl_absorpt_coefficient_mu    0.784
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.8526
_exptl_absorpt_correction_T_max  0.9257
_exptl_absorpt_process_details   'Bruker SADABS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX-II CCD'
_diffrn_measurement_method       'Omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20031
_diffrn_reflns_av_R_equivalents  0.0695
_diffrn_reflns_av_sigmaI/netI    0.0805
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.27
_diffrn_reflns_theta_max         25.02
_reflns_number_total             7704
_reflns_number_gt                4722
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0228P)²+14.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7704
_refine_ls_number_parameters     571
_refine_ls_number_restraints     999
_refine_ls_R_factor_all          0.1383
_refine_ls_R_factor_gt           0.0947
_refine_ls_wR_factor_ref         0.2175
_refine_ls_wR_factor_gt          0.2007
_refine_ls_goodness_of_fit_ref   0.843
_refine_ls_restrained_S_all      0.876
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.67805(13) 0.85493(12) 0.16558(6) 0.0630(4) Uani 1 1 d U . .
Ti2 Ti 0.74915(13) 0.62479(12) 0.19108(6) 0.0641(4) Uani 1 1 d U . .
Ti3 Ti 0.88854(13) 0.89703(12) 0.29063(7) 0.0680(4) Uani 1 1 d U . .
Ti4 Ti 0.4995(2) 0.6494(2) 0.26044(11) 0.0624(7) Uani 0.548(3) 1 d PU . .
P1 P 0.7353(2) 0.6378(2) 0.34576(10) 0.0758(6) Uani 1 1 d U . .
O1 O 0.7032(4) 0.7646(4) 0.2418(2) 0.0555(9) Uani 1 1 d U . .
O2 O 0.7376(5) 0.7209(5) 0.1199(2) 0.0697(11) Uani 1 1 d U . .
O3 O 0.8703(5) 0.9734(4) 0.2113(2) 0.0731(11) Uani 1 1 d U . .
O4 O 0.6300(9) 0.9739(9) 0.2076(5) 0.077(2) Uani 0.548(3) 1 d PDU . .
O5 O 0.5091(10) 0.7434(9) 0.1228(5) 0.082(2) Uani 0.548(3) 1 d PU . .
O7 O 0.9330(5) 0.7706(5) 0.2253(2) 0.0737(12) Uani 1 1 d DU . .
O8 O 0.8083(6) 0.5193(6) 0.1452(3) 0.0957(17) Uani 1 1 d U . .
O9 O 0.7479(6) 0.5631(5) 0.2791(2) 0.0854(14) Uani 1 1 d U . .
O10 O 0.5549(6) 0.5209(6) 0.1934(4) 0.0999(16) Uani 1 1 d U . .
O11 O 0.8540(6) 0.7748(5) 0.3571(2) 0.0849(14) Uani 1 1 d U . .
O12 O 0.8010(6) 0.9732(6) 0.3447(3) 0.1032(16) Uani 1 1 d U . .
O13 O 1.0603(5) 1.0025(6) 0.3186(3) 0.1009(17) Uani 1 1 d U . .
O16 O 0.3280(8) 0.5208(7) 0.2581(5) 0.071(2) Uani 0.548(3) 1 d PU . .
C0C C 0.7458(12) 0.5560(9) 0.4135(4) 0.100(2) Uani 1 1 d U . .
C7 C 1.0719(18) 0.7853(19) 0.2099(10) 0.090(4) Uani 0.538(8) 1 d PU . .
C4 C 0.5115(12) 0.9877(12) 0.2310(6) 0.134(3) Uani 1 1 d DU . .
C14 C 0.5009(17) 0.8781(15) 0.3723(8) 0.074(2) Uani 0.548(3) 1 d PU . .
C5 C 0.3873(12) 0.6335(12) 0.1108(6) 0.137(4) Uani 1 1 d U . .
C1A C 0.6250(14) 0.4173(10) 0.4024(5) 0.146(4) Uani 1 1 d U . .
H1AA H 0.6299 0.3726 0.4386 0.219 Uiso 1 1 calc R . .
H1AB H 0.6303 0.3708 0.3595 0.219 Uiso 1 1 calc R . .
H1AC H 0.5395 0.4222 0.4024 0.219 Uiso 1 1 calc R . .
C2 C 0.7281(9) 0.6773(9) 0.0471(4) 0.092(2) Uani 1 1 d U . .
H2A H 0.6705 0.7052 0.0237 0.111 Uiso 1 1 calc R . .
H2B H 0.6860 0.5831 0.0380 0.111 Uiso 1 1 calc R . .
C8 C 0.8244(14) 0.4028(12) 0.1349(8) 0.179(6) Uani 1 1 d U . .
H8A H 0.8213 0.3742 0.1788 0.214 Uiso 1 1 calc R . .
H8B H 0.7461 0.3358 0.1060 0.214 Uiso 1 1 calc R . .
C13 C 1.242(5) 1.131(6) 0.336(3) 0.196(14) Uani 0.40(3) 1 d PU . .
C81 C 0.9383(13) 0.4108(12) 0.1073(6) 0.143(4) Uani 1 1 d U . .
H81A H 0.9384 0.3278 0.1031 0.215 Uiso 1 1 calc R . .
H81B H 1.0172 0.4748 0.1359 0.215 Uiso 1 1 calc R . .
H81C H 0.9415 0.4354 0.0630 0.215 Uiso 1 1 calc R . .
C71 C 1.1598(15) 0.789(3) 0.1933(13) 0.149(7) Uani 0.538(8) 1 d PDU . .
C6 C 0.6546(11) 0.9895(10) 0.0509(5) 0.114(3) Uani 1 1 d U . .
C101 C 0.4417(11) 0.3173(10) 0.1253(5) 0.113(3) Uani 1 1 d U . .
C41 C 0.5787(15) 1.1116(14) 0.2666(7) 0.170(4) Uani 1 1 d U . .
H41A H 0.5141 1.1456 0.2761 0.255 Uiso 1 1 calc R . .
H41B H 0.6482 1.1659 0.2398 0.255 Uiso 1 1 calc R . .
H41C H 0.6209 1.1103 0.3087 0.255 Uiso 1 1 calc R . .
C121 C 0.8516(16) 1.1531(14) 0.4161(7) 0.174(4) Uani 1 1 d U . .
H12A H 0.8731 1.1989 0.4621 0.261 Uiso 1 1 calc R . .
H12B H 0.7716 1.1545 0.3969 0.261 Uiso 1 1 calc R . .
H12C H 0.9279 1.1942 0.3893 0.261 Uiso 1 1 calc R . .
C61 C 0.7507(13) 1.0299(10) -0.0030(5) 0.131(4) Uani 1 1 d U . .
H61A H 0.7203 1.0713 -0.0330 0.197 Uiso 1 1 calc R . .
H61B H 0.7536 0.9550 -0.0285 0.197 Uiso 1 1 calc R . .
H61C H 0.8409 1.0900 0.0174 0.197 Uiso 1 1 calc R . .
C10A C 0.4900(14) 0.3834(13) 0.1958(8) 0.077(3) Uani 0.538(8) 1 d PU . .
C1B C 0.7364(15) 0.6325(11) 0.4816(4) 0.144(4) Uani 1 1 d U . .
H1BA H 0.7425 0.5899 0.5185 0.216 Uiso 1 1 calc R . .
H1BB H 0.6502 0.6359 0.4810 0.216 Uiso 1 1 calc R . .
H1BC H 0.8106 0.7192 0.4876 0.216 Uiso 1 1 calc R . .
C131 C 1.183(5) 1.024(5) 0.412(2) 0.177(12) Uani 0.40(3) 1 d PU . .
C12 C 0.8255(15) 1.0245(13) 0.4162(7) 0.152(3) Uani 1 1 d U . .
H12D H 0.7456 0.9788 0.4408 0.183 Uiso 1 1 calc R . .
H12E H 0.9042 1.0199 0.4360 0.183 Uiso 1 1 calc R . .
Ti4A Ti 0.5740(3) 0.7941(3) 0.31072(14) 0.0672(8) Uani 0.452(3) 1 d PU . .
C3 C 0.9504(9) 1.1056(8) 0.2028(5) 0.103(3) Uani 1 1 d U . .
H3A H 0.9859 1.1593 0.2472 0.124 Uiso 1 1 calc R . .
H3B H 0.8930 1.1355 0.1811 0.124 Uiso 1 1 calc R . .
O16A O 0.4125(12) 0.6613(11) 0.2786(6) 0.0753(19) Uani 0.452(3) 1 d PU . .
C31 C 1.0642(11) 1.1186(12) 0.1613(6) 0.145(5) Uani 1 1 d U . .
H31A H 1.1180 1.2083 0.1566 0.218 Uiso 1 1 calc R . .
H31B H 1.0288 1.0673 0.1170 0.218 Uiso 1 1 calc R . .
H31C H 1.1209 1.0889 0.1828 0.218 Uiso 1 1 calc R . .
C1C C 0.8821(14) 0.5510(13) 0.4142(6) 0.150(4) Uani 1 1 d U . .
H1CA H 0.8881 0.5075 0.4507 0.225 Uiso 1 1 calc R . .
H1CB H 0.9561 0.6380 0.4208 0.225 Uiso 1 1 calc R . .
H1CC H 0.8885 0.5045 0.3715 0.225 Uiso 1 1 calc R . .
C51 C 0.3263(14) 0.6744(14) 0.0669(7) 0.160(5) Uani 1 1 d U . .
H51A H 0.2700 0.6028 0.0322 0.240 Uiso 1 1 calc R . .
H51B H 0.3957 0.7419 0.0459 0.240 Uiso 1 1 calc R . .
H51C H 0.2701 0.7075 0.0912 0.240 Uiso 1 1 calc R . .
C141 C 0.397(2) 0.780(2) 0.4306(10) 0.116(5) Uani 0.548(3) 1 d PU . .
C161 C 0.198(2) 0.448(2) 0.3401(10) 0.252(11) Uani 1 1 d U . .
H16A H 0.1031 0.3907 0.3448 0.378 Uiso 1 1 calc R . .
H16B H 0.2324 0.5172 0.3785 0.378 Uiso 1 1 calc R . .
H16C H 0.2506 0.4007 0.3385 0.378 Uiso 1 1 calc R . .
C16 C 0.2075(14) 0.4928(14) 0.2889(9) 0.171(6) Uani 1 1 d U . .
O5A O 0.4892(9) 0.7161(9) 0.1740(5) 0.0572(16) Uani 0.452(3) 1 d PU . .
C14A C 0.385(2) 0.8402(19) 0.4103(10) 0.082(3) Uani 0.452(3) 1 d PU . .
C71C C 1.113(2) 0.722(2) 0.2626(13) 0.108(5) Uani 0.462(8) 1 d PU . .
O14A O 0.5073(14) 0.8398(12) 0.3833(7) 0.078(2) Uani 0.452(3) 1 d PU . .
C7C C 1.046(2) 0.728(3) 0.2482(13) 0.095(5) Uani 0.462(8) 1 d PU . .
C14B C 0.394(3) 0.802(3) 0.4743(13) 0.131(8) Uani 0.452(3) 1 d PU . .
C13C C 1.171(3) 1.086(3) 0.3578(16) 0.165(10) Uani 0.60(3) 1 d PU . .
C13D C 1.275(3) 1.097(3) 0.3828(17) 0.182(11) Uani 0.60(3) 1 d PU . .
C21 C 0.8657(11) 0.7313(12) 0.0212(5) 0.121(4) Uani 1 1 d U . .
H21A H 0.8584 0.7008 -0.0269 0.182 Uiso 1 1 calc R . .
H21B H 0.9225 0.7037 0.0445 0.182 Uiso 1 1 calc R . .
H21C H 0.9062 0.8245 0.0292 0.182 Uiso 1 1 calc R . .
O14 O 0.4694(10) 0.7667(9) 0.3166(4) 0.0714(15) Uani 0.548(3) 1 d PU . .
O4A O 0.5845(11) 0.9058(11) 0.2400(6) 0.0709(18) Uani 0.452(3) 1 d PU . .
O6A O 0.7133(13) 0.9690(13) 0.1059(6) 0.090(3) Uani 0.538(8) 1 d PU . .
O15B O 0.6146(15) 0.6804(14) 0.3584(7) 0.087(2) Uani 0.452(3) 1 d PU . .
O6B O 0.6847(14) 0.8930(13) 0.0817(6) 0.077(3) Uani 0.462(8) 1 d PU . .
O15A O 0.5829(12) 0.6132(11) 0.3378(5) 0.084(2) Uani 0.548(3) 1 d PU . .
C10B C 0.574(2) 0.4985(18) 0.1518(9) 0.082(3) Uani 0.462(8) 1 d PU . .


_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 O6B 1.776(12) . ?
Ti1 O4 1.797(8) . ?
Ti1 O5 1.826(10) . ?
Ti1 O6A 1.819(11) . ?
Ti1 O4A 1.969(10) . ?
Ti1 O5A 1.993(9) . ?
Ti1 O3 2.040(5) . ?
Ti1 O1 2.045(4) . ?
Ti1 O2 2.051(4) . ?
Ti1 Ti4A 3.154(3) . ?
Ti1 Ti4 3.188(3) . ?
Ti1 Ti3 3.210(2) . ?
Ti2 O8 1.777(5) . ?
Ti2 O10 1.915(6) . ?
Ti2 C10B 1.890(19) . ?
Ti2 O2 1.961(5) . ?
Ti2 O9 1.978(5) . ?
Ti2 O7 1.994(5) . ?
Ti2 O1 2.050(4) . ?
Ti2 Ti4 3.164(3) . ?
Ti2 Ti3 3.189(2) . ?
Ti3 O13 1.750(5) . ?
Ti3 O12 1.831(5) . ?
Ti3 O3 1.968(5) . ?
Ti3 O11 1.990(5) . ?
Ti3 O7 2.049(4) . ?
Ti3 O1 2.043(4) . ?
Ti3 Ti4A 3.133(4) . ?
Ti4 O16A 1.076(11) . ?
Ti4 Ti4A 1.670(4) . ?
Ti4 O14 1.788(9) . ?
Ti4 O16 1.791(8) . ?
Ti4 O15A 1.973(11) . ?
Ti4 O5A 2.004(10) . ?
Ti4 O1 2.083(5) . ?
Ti4 O15B 2.208(14) . ?
Ti4 O10 2.153(7) . ?
P1 O9 1.521(5) . ?
P1 O11 1.522(6) . ?
P1 O15A 1.559(12) . ?
P1 O15B 1.612(14) . ?
P1 C0C 1.787(9) . ?
O1 Ti4A 2.071(5) . ?
O2 C2 1.450(8) . ?
O3 C3 1.424(9) . ?
O4 O4A 1.039(12) . ?
O4 C4 1.442(8) . ?
O5 O5A 1.102(11) . ?
O5 C5 1.359(13) . ?
O7 C7C 1.61(2) . ?
O7 C7 1.484(16) . ?
O8 C8 1.435(12) . ?
O10 C10B 0.885(16) . ?
O10 C10A 1.441(14) . ?
O12 C12 1.434(13) . ?
O12 Ti4A 2.428(7) . ?
O13 C13C 1.32(2) . ?
O16 C16 1.372(14) . ?
O16 O16A 1.467(13) . ?
C0C C1C 1.516(15) . ?
C0C C1B 1.541(12) . ?
C0C C1A 1.543(14) . ?
C7 C7C 1.04(2) . ?
C7 C71 0.998(18) . ?
C7 C71C 1.53(3) . ?
C4 C41 1.372(16) . ?
C4 O4A 1.520(14) . ?
C14 O14A 0.554(18) . ?
C14 C14A 1.40(2) . ?
C14 O14 1.490(18) . ?
C14 C141 1.77(2) . ?
C14 Ti4A 1.861(16) . ?
C5 C51 1.355(15) . ?
C5 O5A 1.558(14) . ?
C2 C21 1.469(12) . ?
C8 C81 1.329(15) . ?
C13 C13C 0.88(6) . ?
C13 C13D 1.18(6) . ?
C71 C7C 1.63(3) . ?
C71 C71C 1.65(3) . ?
C6 O6A 1.368(14) . ?
C6 C61 1.471(13) . ?
C6 O6B 1.509(15) . ?
C101 C10A 1.468(17) . ?
C101 C10B 1.94(2) . ?
C121 C12 1.395(16) . ?
C10A C10B 1.62(2) . ?
C131 C13D 1.20(5) . ?
C131 C13C 1.41(5) . ?
Ti4A O14 1.049(9) . ?
Ti4A O14A 1.738(13) . ?
Ti4A O16A 1.781(12) . ?
Ti4A O15B 1.932(14) . ?
Ti4A O4A 2.017(12) . ?
Ti4A O15A 2.293(11) . ?
C3 C31 1.454(13) . ?
O16A O14 1.230(12) . ?
C141 C14B 0.87(3) . ?
C141 C14A 0.91(2) . ?
C141 O14A 1.50(2) . ?
C161 C16 1.19(2) . ?
C14A O14A 1.44(2) . ?
C14A C14B 1.42(3) . ?
C71C C7C 0.82(2) . ?
O14A O14 1.418(15) . ?
C13C C13D 1.19(4) . ?
O6A O6B 0.863(13) . ?
O15B O15A 0.752(15) . ?

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
O6B Ti1 O4 98.6(5) . . ?
O6B Ti1 O5 74.7(6) . . ?
O4 Ti1 O5 96.6(4) . . ?
O6B Ti1 O6A 27.7(4) . . ?
O4 Ti1 O6A 75.7(5) . . ?
O5 Ti1 O6A 92.8(5) . . ?
O6B Ti1 O4A 125.6(5) . . ?
O4 Ti1 O4A 31.6(4) . . ?
O5 Ti1 O4A 88.5(5) . . ?
O6A Ti1 O4A 106.6(5) . . ?
O6B Ti1 O5A 107.7(5) . . ?
O4 Ti1 O5A 89.3(4) . . ?
O5 Ti1 O5A 33.2(3) . . ?
O6A Ti1 O5A 122.3(5) . . ?
O4A Ti1 O5A 67.1(4) . . ?
O6B Ti1 O3 105.0(5) . . ?
O4 Ti1 O3 86.2(3) . . ?
O5 Ti1 O3 177.2(3) . . ?
O6A Ti1 O3 87.8(4) . . ?
O4A Ti1 O3 94.0(3) . . ?
O5A Ti1 O3 147.3(3) . . ?
O6B Ti1 O1 156.4(4) . . ?
O4 Ti1 O1 104.8(3) . . ?
O5 Ti1 O1 105.2(3) . . ?
O6A Ti1 O1 161.7(4) . . ?
O4A Ti1 O1 77.6(4) . . ?
O5A Ti1 O1 75.9(3) . . ?
O3 Ti1 O1 73.98(18) . . ?
O6B Ti1 O2 82.6(4) . . ?
O4 Ti1 O2 178.3(3) . . ?
O5 Ti1 O2 84.9(3) . . ?
O6A Ti1 O2 105.0(5) . . ?
O4A Ti1 O2 148.0(4) . . ?
O5A Ti1 O2 91.6(3) . . ?
O3 Ti1 O2 92.3(2) . . ?
O1 Ti1 O2 74.01(17) . . ?
O6B Ti1 Ti4A 160.9(4) . . ?
O4 Ti1 Ti4A 68.5(3) . . ?
O5 Ti1 Ti4A 92.3(3) . . ?
O6A Ti1 Ti4A 144.2(4) . . ?
O4A Ti1 Ti4A 38.2(3) . . ?
O5A Ti1 Ti4A 59.7(3) . . ?
O3 Ti1 Ti4A 88.70(15) . . ?
O1 Ti1 Ti4A 40.27(12) . . ?
O2 Ti1 Ti4A 110.72(15) . . ?
O6B Ti1 Ti4 143.6(5) . . ?
O4 Ti1 Ti4 91.7(3) . . ?
O5 Ti1 Ti4 69.5(3) . . ?
O6A Ti1 Ti4 157.2(4) . . ?
O4A Ti1 Ti4 60.3(3) . . ?
O5A Ti1 Ti4 37.2(3) . . ?
O3 Ti1 Ti4 110.52(15) . . ?
O1 Ti1 Ti4 39.87(12) . . ?
O2 Ti1 Ti4 88.17(15) . . ?
Ti4A Ti1 Ti4 30.52(7) . . ?
O6B Ti1 Ti3 138.3(4) . . ?
O4 Ti1 Ti3 93.2(3) . . ?
O5 Ti1 Ti3 143.4(3) . . ?
O6A Ti1 Ti3 123.8(4) . . ?
O4A Ti1 Ti3 81.8(3) . . ?
O5A Ti1 Ti3 112.2(3) . . ?
O3 Ti1 Ti3 36.01(14) . . ?
O1 Ti1 Ti3 38.24(11) . . ?
O2 Ti1 Ti3 85.07(13) . . ?
Ti4A Ti1 Ti3 58.97(7) . . ?
Ti4 Ti1 Ti3 75.05(6) . . ?
O8 Ti2 O10 105.3(3) . . ?
O8 Ti2 C10B 84.4(6) . . ?
O10 Ti2 C10B 26.9(5) . . ?
O8 Ti2 O2 101.1(2) . . ?
O10 Ti2 O2 96.2(3) . . ?
C10B Ti2 O2 83.8(6) . . ?
O8 Ti2 O9 94.9(2) . . ?
O10 Ti2 O9 81.0(3) . . ?
C10B Ti2 O9 99.5(6) . . ?
O2 Ti2 O9 163.91(19) . . ?
O8 Ti2 O7 97.4(2) . . ?
O10 Ti2 O7 154.9(2) . . ?
C10B Ti2 O7 173.6(6) . . ?
O2 Ti2 O7 89.8(2) . . ?
O9 Ti2 O7 86.5(2) . . ?
O8 Ti2 O1 173.0(3) . . ?
O10 Ti2 O1 81.4(2) . . ?
C10B Ti2 O1 101.4(6) . . ?
O2 Ti2 O1 75.84(17) . . ?
O9 Ti2 O1 88.07(19) . . ?
O7 Ti2 O1 76.43(17) . . ?
O8 Ti2 Ti4 146.5(2) . . ?
O10 Ti2 Ti4 41.7(2) . . ?
C10B Ti2 Ti4 65.5(6) . . ?
O2 Ti2 Ti4 90.47(14) . . ?
O9 Ti2 Ti4 76.83(18) . . ?
O7 Ti2 Ti4 114.13(14) . . ?
O1 Ti2 Ti4 40.43(12) . . ?
O8 Ti2 Ti3 135.6(2) . . ?
O10 Ti2 Ti3 117.2(2) . . ?
C10B Ti2 Ti3 140.0(6) . . ?
O2 Ti2 Ti3 87.12(14) . . ?
O9 Ti2 Ti3 80.25(15) . . ?
O7 Ti2 Ti3 38.56(12) . . ?
O1 Ti2 Ti3 38.75(12) . . ?
Ti4 Ti2 Ti3 75.69(6) . . ?
O8 Ti2 Ti1 138.8(2) . . ?
O10 Ti2 Ti1 86.2(2) . . ?
C10B Ti2 Ti1 90.8(6) . . ?
O2 Ti2 Ti1 37.74(12) . . ?
O9 Ti2 Ti1 126.19(15) . . ?
O7 Ti2 Ti1 83.76(15) . . ?
O1 Ti2 Ti1 38.23(12) . . ?
Ti4 Ti2 Ti1 59.98(5) . . ?
Ti3 Ti2 Ti1 60.18(5) . . ?
O13 Ti3 O12 100.5(3) . . ?
O13 Ti3 O3 99.8(3) . . ?
O12 Ti3 O3 92.9(2) . . ?
O13 Ti3 O11 97.2(3) . . ?
O12 Ti3 O11 88.5(3) . . ?
O3 Ti3 O11 162.4(2) . . ?
O13 Ti3 O7 94.8(2) . . ?
O12 Ti3 O7 164.3(3) . . ?
O3 Ti3 O7 88.0(2) . . ?
O11 Ti3 O7 86.0(2) . . ?
O13 Ti3 O1 169.1(2) . . ?
O12 Ti3 O1 89.6(2) . . ?
O3 Ti3 O1 75.57(18) . . ?
O11 Ti3 O1 86.90(19) . . ?
O7 Ti3 O1 75.38(17) . . ?
O13 Ti3 Ti4A 150.1(2) . . ?
O12 Ti3 Ti4A 50.6(2) . . ?
O3 Ti3 Ti4A 90.61(15) . . ?
O11 Ti3 Ti4A 76.72(18) . . ?
O7 Ti3 Ti4A 113.65(15) . . ?
O1 Ti3 Ti4A 40.72(12) . . ?
O13 Ti3 Ti2 132.0(2) . . ?
O12 Ti3 Ti2 127.0(2) . . ?
O3 Ti3 Ti2 85.91(15) . . ?
O11 Ti3 Ti2 79.32(14) . . ?
O7 Ti3 Ti2 37.34(13) . . ?
O1 Ti3 Ti2 38.90(11) . . ?
Ti4A Ti3 Ti2 76.39(6) . . ?
O13 Ti3 Ti1 137.2(2) . . ?
O12 Ti3 Ti1 88.11(19) . . ?
O3 Ti3 Ti1 37.57(13) . . ?
O11 Ti3 Ti1 125.07(16) . . ?
O7 Ti3 Ti1 83.06(14) . . ?
O1 Ti3 Ti1 38.28(12) . . ?
Ti4A Ti3 Ti1 59.62(7) . . ?
Ti2 Ti3 Ti1 60.31(4) . . ?
O16A Ti4 Ti4A 77.5(6) . . ?
O16A Ti4 O14 42.4(6) . . ?
Ti4A Ti4 O14 35.1(3) . . ?
O16A Ti4 O16 54.9(6) . . ?
Ti4A Ti4 O16 129.5(3) . . ?
O14 Ti4 O16 95.6(4) . . ?
O16A Ti4 O15A 106.9(7) . . ?
Ti4A Ti4 O15A 77.5(4) . . ?
O14 Ti4 O15A 90.4(4) . . ?
O16 Ti4 O15A 99.0(5) . . ?
O16A Ti4 O5A 91.9(7) . . ?
Ti4A Ti4 O5A 96.7(3) . . ?
O14 Ti4 O5A 96.6(4) . . ?
O16 Ti4 O5A 100.6(4) . . ?
O15A Ti4 O5A 158.4(4) . . ?
O16A Ti4 O1 138.8(6) . . ?
Ti4A Ti4 O1 65.91(16) . . ?
O14 Ti4 O1 99.6(3) . . ?
O16 Ti4 O1 164.6(3) . . ?
O15A Ti4 O1 83.8(4) . . ?
O5A Ti4 O1 74.9(3) . . ?
O16A Ti4 O15B 100.3(7) . . ?
Ti4A Ti4 O15B 57.8(4) . . ?
O14 Ti4 O15B 74.0(5) . . ?
O16 Ti4 O15B 110.9(5) . . ?
O15A Ti4 O15B 19.7(4) . . ?
O5A Ti4 O15B 147.7(5) . . ?
O1 Ti4 O15B 76.4(4) . . ?
O16A Ti4 O10 142.6(7) . . ?
Ti4A Ti4 O10 139.8(2) . . ?
O14 Ti4 O10 174.8(4) . . ?
O16 Ti4 O10 89.6(3) . . ?
O15A Ti4 O10 88.4(4) . . ?
O5A Ti4 O10 82.8(3) . . ?
O1 Ti4 O10 75.3(2) . . ?
O15B Ti4 O10 103.8(4) . . ?
O16A Ti4 Ti2 173.3(6) . . ?
Ti4A Ti4 Ti2 103.59(15) . . ?
O14 Ti4 Ti2 138.5(3) . . ?
O16 Ti4 Ti2 125.7(3) . . ?
O15A Ti4 Ti2 79.8(3) . . ?
O5A Ti4 Ti2 81.4(3) . . ?
O1 Ti4 Ti2 39.65(12) . . ?
O15B Ti4 Ti2 85.8(4) . . ?
O10 Ti4 Ti2 36.32(17) . . ?
O16A Ti4 Ti1 113.7(6) . . ?
Ti4A Ti4 Ti1 73.61(13) . . ?
O14 Ti4 Ti1 93.2(3) . . ?
O16 Ti4 Ti1 137.5(3) . . ?
O15A Ti4 Ti1 122.5(4) . . ?
O5A Ti4 Ti1 37.0(3) . . ?
O1 Ti4 Ti1 39.01(12) . . ?
O15B Ti4 Ti1 111.5(4) . . ?
O10 Ti4 Ti1 83.25(19) . . ?
Ti2 Ti4 Ti1 60.80(6) . . ?
O9 P1 O11 109.5(3) . . ?
O9 P1 O15A 101.7(5) . . ?
O11 P1 O15A 121.5(5) . . ?
O9 P1 O15B 124.0(6) . . ?
O11 P1 O15B 96.3(6) . . ?
O15A P1 O15B 27.4(6) . . ?
O9 P1 C0C 108.0(4) . . ?
O11 P1 C0C 108.8(4) . . ?
O15A P1 C0C 106.6(5) . . ?
O15B P1 C0C 109.0(6) . . ?
Ti1 O1 Ti3 103.48(18) . . ?
Ti1 O1 Ti2 103.44(18) . . ?
Ti3 O1 Ti2 102.35(18) . . ?
Ti1 O1 Ti4A 100.06(19) . . ?
Ti3 O1 Ti4A 99.21(18) . . ?
Ti2 O1 Ti4A 143.2(2) . . ?
Ti1 O1 Ti4 101.13(19) . . ?
Ti3 O1 Ti4 141.7(2) . . ?
Ti2 O1 Ti4 99.92(18) . . ?
Ti4A O1 Ti4 47.41(14) . . ?
C2 O2 Ti2 125.1(5) . . ?
C2 O2 Ti1 125.5(5) . . ?
Ti2 O2 Ti1 106.46(19) . . ?
C3 O3 Ti3 125.3(5) . . ?
C3 O3 Ti1 124.5(5) . . ?
Ti3 O3 Ti1 106.4(2) . . ?
O4A O4 C4 73.5(9) . . ?
O4A O4 Ti1 83.4(8) . . ?
C4 O4 Ti1 141.5(8) . . ?
O5A O5 C5 77.8(9) . . ?
O5A O5 Ti1 81.7(7) . . ?
C5 O5 Ti1 156.6(9) . . ?
C7C O7 C7 38.9(9) . . ?
C7C O7 Ti2 115.6(9) . . ?
C7 O7 Ti2 129.1(7) . . ?
C7C O7 Ti3 120.5(9) . . ?
C7 O7 Ti3 126.7(7) . . ?
Ti2 O7 Ti3 104.1(2) . . ?
C8 O8 Ti2 152.2(8) . . ?
P1 O9 Ti2 121.3(3) . . ?
C10B O10 C10A 84.8(15) . . ?
C10B O10 Ti2 74.9(14) . . ?
C10A O10 Ti2 124.1(7) . . ?
C10B O10 Ti4 147.4(15) . . ?
C10A O10 Ti4 120.6(7) . . ?
Ti2 O10 Ti4 101.9(3) . . ?
P1 O11 Ti3 122.4(3) . . ?
C12 O12 Ti3 129.8(7) . . ?
C12 O12 Ti4A 115.0(7) . . ?
Ti3 O12 Ti4A 93.7(2) . . ?
C13C O13 Ti3 161.6(15) . . ?
C16 O16 O16A 104.8(9) . . ?
C16 O16 Ti4 140.2(9) . . ?
O16A O16 Ti4 36.9(5) . . ?
C1C C0C C1B 109.5(9) . . ?
C1C C0C C1A 110.5(9) . . ?
C1B C0C C1A 109.9(10) . . ?
C1C C0C P1 109.4(8) . . ?
C1B C0C P1 108.5(6) . . ?
C1A C0C P1 109.0(7) . . ?
C7C C7 C71 107(3) . . ?
C7C C7 O7 76.9(18) . . ?
C71 C7 O7 172(2) . . ?
C7C C7 C71C 30.0(14) . . ?
C71 C7 C71C 78(2) . . ?
O7 C7 C71C 106.4(17) . . ?
C41 C4 O4 98.4(11) . . ?
C41 C4 O4A 113.1(12) . . ?
O4 C4 O4A 41.0(5) . . ?
O14A C14 C14A 83(3) . . ?
O14A C14 O14 72(3) . . ?
C14A C14 O14 105.8(14) . . ?
O14A C14 C141 52(3) . . ?
C14A C14 C141 30.8(10) . . ?
O14 C14 C141 94.6(11) . . ?
O14A C14 Ti4A 69(3) . . ?
C14A C14 Ti4A 136.1(13) . . ?
O14 C14 Ti4A 34.3(5) . . ?
C141 C14 Ti4A 113.8(11) . . ?
O5 C5 C51 97.4(11) . . ?
O5 C5 O5A 43.7(5) . . ?
C51 C5 O5A 127.6(12) . . ?
O2 C2 C21 110.1(7) . . ?
C81 C8 O8 116.7(13) . . ?
C13C C13 C13D 68(6) . . ?
C7 C71 C7C 37.4(15) . . ?
C7 C71 C71C 65.6(18) . . ?
C7C C71 C71C 29.0(9) . . ?
O6A C6 C61 111.6(10) . . ?
O6A C6 O6B 34.5(6) . . ?
C61 C6 O6B 105.4(9) . . ?
C10A C101 C10B 54.8(9) . . ?
C101 C10A O10 106.6(11) . . ?
C101 C10A C10B 77.6(10) . . ?
O10 C10A C10B 32.9(6) . . ?
C13D C131 C13C 53(3) . . ?
C121 C12 O12 101.9(11) . . ?
O14 Ti4A Ti4 78.6(5) . . ?
O14 Ti4A O14A 54.6(6) . . ?
Ti4 Ti4A O14A 125.4(5) . . ?
O14 Ti4A O16A 42.4(6) . . ?
Ti4 Ti4A O16A 36.2(4) . . ?
O14A Ti4A O16A 93.3(6) . . ?
O14 Ti4A C14 53.1(7) . . ?
Ti4 Ti4A C14 131.1(5) . . ?
O14A Ti4A C14 17.3(6) . . ?
O16A Ti4A C14 95.3(7) . . ?
O14 Ti4A O15B 105.0(7) . . ?
Ti4 Ti4A O15B 75.2(5) . . ?
O14A Ti4A O15B 90.2(6) . . ?
O16A Ti4A O15B 89.8(6) . . ?
C14 Ti4A O15B 107.4(6) . . ?
O14 Ti4A O4A 93.0(6) . . ?
Ti4 Ti4A O4A 98.2(3) . . ?
O14A Ti4A O4A 109.5(5) . . ?
O16A Ti4A O4A 96.4(5) . . ?
C14 Ti4A O4A 92.2(6) . . ?
O15B Ti4A O4A 158.9(5) . . ?
O14 Ti4A O1 141.1(6) . . ?
Ti4 Ti4A O1 66.68(16) . . ?
O14A Ti4A O1 164.1(5) . . ?
O16A Ti4A O1 101.0(4) . . ?
C14 Ti4A O1 160.7(5) . . ?
O15B Ti4A O1 83.0(4) . . ?
O4A Ti4A O1 76.0(3) . . ?
O14 Ti4A O15A 99.3(6) . . ?
Ti4 Ti4A O15A 57.1(3) . . ?
O14A Ti4A O15A 100.9(5) . . ?
O16A Ti4A O15A 74.8(5) . . ?
C14 Ti4A O15A 118.0(6) . . ?
O15B Ti4A O15A 18.0(5) . . ?
O4A Ti4A O15A 148.9(4) . . ?
O1 Ti4A O15A 76.6(3) . . ?
O14 Ti4A O12 141.4(6) . . ?
Ti4 Ti4A O12 140.0(2) . . ?
O14A Ti4A O12 91.5(5) . . ?
O16A Ti4A O12 175.0(4) . . ?
C14 Ti4A O12 88.8(5) . . ?
O15B Ti4A O12 91.6(5) . . ?
O4A Ti4A O12 80.7(4) . . ?
O1 Ti4A O12 74.40(19) . . ?
O15A Ti4A O12 105.6(4) . . ?
O14 Ti4A Ti3 175.4(5) . . ?
Ti4 Ti4A Ti3 104.30(15) . . ?
O14A Ti4A Ti3 124.5(5) . . ?
O16A Ti4A Ti3 140.2(4) . . ?
C14 Ti4A Ti3 124.4(5) . . ?
O15B Ti4A Ti3 79.3(5) . . ?
O4A Ti4A Ti3 83.1(3) . . ?
O1 Ti4A Ti3 40.07(12) . . ?
O15A Ti4A Ti3 85.3(3) . . ?
O12 Ti4A Ti3 35.68(13) . . ?
O14 Ti4A Ti1 116.5(5) . . ?
Ti4 Ti4A Ti1 75.86(12) . . ?
O14A Ti4A Ti1 146.4(4) . . ?
O16A Ti4A Ti1 94.9(4) . . ?
C14 Ti4A Ti1 129.2(5) . . ?
O15B Ti4A Ti1 122.3(4) . . ?
O4A Ti4A Ti1 37.2(3) . . ?
O1 Ti4A Ti1 39.67(13) . . ?
O15A Ti4A Ti1 112.8(3) . . ?
O12 Ti4A Ti1 80.33(16) . . ?
Ti3 Ti4A Ti1 61.40(6) . . ?
O3 C3 C31 110.4(8) . . ?
Ti4 O16A O14 101.4(10) . . ?
Ti4 O16A O16 88.2(8) . . ?
O14 O16A O16 158.4(11) . . ?
Ti4 O16A Ti4A 66.3(6) . . ?
O14 O16A Ti4A 35.1(6) . . ?
O16 O16A Ti4A 149.0(9) . . ?
C14B C141 C14A 105(4) . . ?
C14B C141 O14A 131(3) . . ?
C14A C141 O14A 68.5(18) . . ?
C14B C141 C14 128(3) . . ?
C14A C141 C14 51.5(17) . . ?
O14A C141 C14 17.0(7) . . ?
C161 C16 O16 115.3(19) . . ?
O5 O5A C5 58.5(8) . . ?
O5 O5A Ti1 65.1(7) . . ?
C5 O5A Ti1 122.5(7) . . ?
O5 O5A Ti4 161.8(9) . . ?
C5 O5A Ti4 124.5(7) . . ?
Ti1 O5A Ti4 105.8(4) . . ?
C141 C14A C14 98(2) . . ?
C141 C14A O14A 75.4(19) . . ?
C14 C14A O14A 22.4(8) . . ?
C141 C14A C14B 36(2) . . ?
C14 C14A C14B 117.6(19) . . ?
O14A C14A C14B 98.7(18) . . ?
C7C C71C C7 39(2) . . ?
C7C C71C C71 74(3) . . ?
C7 C71C C71 36.3(9) . . ?
C14 O14A O14 86(3) . . ?
C14 O14A C14A 74(3) . . ?
O14 O14A C14A 107.4(12) . . ?
C14 O14A C141 110(3) . . ?
O14 O14A C141 111.0(13) . . ?
C14A O14A C141 36.1(10) . . ?
C14 O14A Ti4A 94(3) . . ?
O14 O14A Ti4A 37.1(5) . . ?
C14A O14A Ti4A 144.2(12) . . ?
C141 O14A Ti4A 139.8(12) . . ?
C71C C7C C7 111(3) . . ?
C71C C7C O7 169(3) . . ?
C7 C7C O7 64.2(17) . . ?
C71C C7C C71 77(3) . . ?
C7 C7C C71 35.9(14) . . ?
O7 C7C C71 99.8(18) . . ?
C141 C14B C14A 38(2) . . ?
C13 C13C C13D 68(5) . . ?
C13 C13C O13 115(5) . . ?
C13D C13C O13 142(3) . . ?
C13 C13C C131 122(6) . . ?
C13D C13C C131 54(2) . . ?
O13 C13C C131 107(3) . . ?
C131 C13D C13C 72(3) . . ?
C131 C13D C13 116(4) . . ?
C13C C13D C13 44(3) . . ?
Ti4A O14 O16A 102.4(9) . . ?
Ti4A O14 O14A 88.3(8) . . ?
O16A O14 O14A 150.1(11) . . ?
Ti4A O14 C14 92.6(9) . . ?
O16A O14 C14 163.5(12) . . ?
O14A O14 C14 21.8(7) . . ?
Ti4A O14 Ti4 66.3(5) . . ?
O16A O14 Ti4 36.2(6) . . ?
O14A O14 Ti4 141.6(8) . . ?
C14 O14 Ti4 157.4(9) . . ?
O4 O4A C4 65.5(8) . . ?
O4 O4A Ti1 65.0(7) . . ?
C4 O4A Ti1 122.0(8) . . ?
O4 O4A Ti4A 157.7(10) . . ?
C4 O4A Ti4A 131.8(8) . . ?
Ti1 O4A Ti4A 104.6(5) . . ?
O6B O6A C6 81.7(14) . . ?
O6B O6A Ti1 73.4(12) . . ?
C6 O6A Ti1 141.7(10) . . ?
O15A O15B P1 72.3(16) . . ?
O15A O15B Ti4A 109.2(18) . . ?
P1 O15B Ti4A 127.8(8) . . ?
O15A O15B Ti4 62.2(15) . . ?
P1 O15B Ti4 109.8(7) . . ?
Ti4A O15B Ti4 47.0(3) . . ?
O6A O6B C6 63.8(12) . . ?
O6A O6B Ti1 78.9(13) . . ?
C6 O6B Ti1 133.0(9) . . ?
O15B O15A P1 80.3(17) . . ?
O15B O15A Ti4 98.1(17) . . ?
P1 O15A Ti4 125.4(6) . . ?
O15B O15A Ti4A 52.7(15) . . ?
P1 O15A Ti4A 110.2(6) . . ?
Ti4 O15A Ti4A 45.3(2) . . ?
O10 C10B C10A 62.2(14) . . ?
O10 C10B C101 105.1(18) . . ?
C10A C10B C101 47.6(8) . . ?
O10 C10B Ti2 78.2(13) . . ?
C10A C10B Ti2 115.5(12) . . ?
C101 C10B Ti2 149.5(12) . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.801
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.083
####################################################################### 
# 
# 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_tipbu41_170804_0m
_database_code_depnum_ccdc_archive 'CCDC 1872960'
loop_
_audit_author_name
_audit_author_address
'Vadim Kessler'
;Swedish University of Agricultural Sciences
Sweden
;
_audit_update_record             
;
2018-10-12 deposited with the CCDC.	2020-02-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H116 O34 P8 Ti4'
_chemical_formula_weight         1676.77

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   12.921(4)
_cell_length_b                   20.151(6)
_cell_length_c                   17.426(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.719(8)
_cell_angle_gamma                90.00
_cell_volume                     4368(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7543
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      26.20

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1768
_exptl_absorpt_coefficient_mu    0.570
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.8211
_exptl_absorpt_correction_T_max  0.8945
_exptl_absorpt_process_details   'Bruker SADABS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX-II CCD'
_diffrn_measurement_method       'Omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            38586
_diffrn_reflns_av_R_equivalents  0.1768
_diffrn_reflns_av_sigmaI/netI    0.1217
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.36
_diffrn_reflns_theta_max         25.25
_reflns_number_total             7714
_reflns_number_gt                4454
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0443P)²+26.4334P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7714
_refine_ls_number_parameters     414
_refine_ls_number_restraints     364
_refine_ls_R_factor_all          0.1658
_refine_ls_R_factor_gt           0.1043
_refine_ls_wR_factor_ref         0.2476
_refine_ls_wR_factor_gt          0.2303
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_restrained_S_all      1.154
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.37680(13) 0.42094(6) 0.57613(8) 0.0335(4) Uani 1 1 d U . .
Ti2 Ti 0.33813(14) 0.57669(7) 0.35468(8) 0.0364(4) Uani 1 1 d U . .
P3 P 0.30794(18) 0.58308(9) 0.53459(11) 0.0310(5) Uani 1 1 d U . .
P4 P 0.32617(18) 0.41855(9) 0.37217(11) 0.0302(5) Uani 1 1 d U . .
P5 P 0.5309(2) 0.28940(9) 0.59317(12) 0.0348(5) Uani 1 1 d U . .
P6 P 0.4873(2) 0.54565(10) 0.24079(12) 0.0381(6) Uani 1 1 d U . .
O1 O 0.5322(5) 0.4430(2) 0.5884(3) 0.0320(12) Uani 1 1 d U . .
O6 O 0.2792(5) 0.4853(2) 0.3388(3) 0.0359(13) Uani 1 1 d U . .
O7 O 0.2730(5) 0.5870(3) 0.4441(3) 0.0395(14) Uani 1 1 d U . .
O2 O 0.3539(5) 0.4146(3) 0.4625(3) 0.0368(13) Uani 1 1 d U . .
O3 O 0.4276(5) 0.3268(2) 0.5873(3) 0.0381(13) Uani 1 1 d U . .
O8 O 0.1857(6) 0.6065(3) 0.2780(4) 0.0511(16) Uani 1 1 d U . .
O4 O 0.2455(5) 0.3913(3) 0.5793(4) 0.0491(15) Uani 1 1 d U . .
O9 O 0.3821(5) 0.5681(3) 0.2523(3) 0.0441(14) Uani 1 1 d U . .
O10 O 0.4272(5) 0.4022(3) 0.3435(3) 0.0407(13) Uani 1 1 d U . .
O5 O 0.4180(5) 0.4293(3) 0.6948(3) 0.0402(14) Uani 1 1 d U . .
C51 C 0.5152(10) 0.2200(4) 0.7227(5) 0.054(3) Uani 1 1 d U . .
H51A H 0.5102 0.1780 0.7474 0.081 Uiso 1 1 calc R . .
H51B H 0.4527 0.2461 0.7218 0.081 Uiso 1 1 calc R . .
H51C H 0.5784 0.2429 0.7524 0.081 Uiso 1 1 calc R . .
C4 C 0.2235(8) 0.3547(4) 0.3326(5) 0.045(2) Uani 1 1 d U . .
O11 O 0.5435(6) 0.2716(3) 0.5086(3) 0.0447(16) Uani 1 1 d U . .
C5 C 0.5218(8) 0.2086(4) 0.6364(5) 0.043(2) Uani 1 1 d U . .
O12 O 0.4011(5) 0.6320(2) 0.5706(3) 0.0339(13) Uani 1 1 d U . .
C6 C 0.4994(9) 0.5730(4) 0.1449(5) 0.053(2) Uani 1 1 d U . .
C52 C 0.6227(9) 0.1682(4) 0.6378(6) 0.055(2) Uani 1 1 d U . .
H52A H 0.6180 0.1255 0.6609 0.082 Uiso 1 1 calc R . .
H52B H 0.6850 0.1912 0.6690 0.082 Uiso 1 1 calc R . .
H52C H 0.6282 0.1627 0.5843 0.082 Uiso 1 1 calc R . .
O13 O 0.4879(10) 0.4682(5) 0.2339(6) 0.109(2) Uani 1 1 d U . .
C53 C 0.4201(9) 0.1736(4) 0.5884(6) 0.057(2) Uani 1 1 d U . .
H53A H 0.4149 0.1309 0.6113 0.086 Uiso 1 1 calc R . .
H53B H 0.4230 0.1683 0.5343 0.086 Uiso 1 1 calc R . .
H53C H 0.3584 0.1998 0.5894 0.086 Uiso 1 1 calc R . .
C31 C 0.1628(10) 0.6780(5) 0.5401(8) 0.070(3) Uani 1 1 d U . .
H31A H 0.1018 0.6923 0.5573 0.104 Uiso 1 1 calc R . .
H31B H 0.1455 0.6796 0.4830 0.104 Uiso 1 1 calc R . .
H31C H 0.2227 0.7068 0.5623 0.104 Uiso 1 1 calc R . .
C61 C 0.4058(12) 0.5447(6) 0.0775(6) 0.084(4) Uani 1 1 d U . .
H61A H 0.4132 0.5593 0.0268 0.125 Uiso 1 1 calc R . .
H61B H 0.3386 0.5601 0.0843 0.125 Uiso 1 1 calc R . .
H61C H 0.4076 0.4971 0.0795 0.125 Uiso 1 1 calc R . .
C62 C 0.4963(10) 0.6480(4) 0.1423(6) 0.063(3) Uani 1 1 d U . .
H62A H 0.5028 0.6630 0.0916 0.094 Uiso 1 1 calc R . .
H62B H 0.5548 0.6654 0.1839 0.094 Uiso 1 1 calc R . .
H62C H 0.4294 0.6633 0.1500 0.094 Uiso 1 1 calc R . .
C3 C 0.1919(8) 0.6074(4) 0.5682(5) 0.0407(19) Uani 1 1 d U . .
C41 C 0.2728(10) 0.2875(4) 0.3655(7) 0.063(3) Uani 1 1 d U . .
H41A H 0.2219 0.2527 0.3455 0.094 Uiso 1 1 calc R . .
H41B H 0.2907 0.2881 0.4226 0.094 Uiso 1 1 calc R . .
H41C H 0.3367 0.2798 0.3487 0.094 Uiso 1 1 calc R . .
C32 C 0.2239(9) 0.6038(6) 0.6594(6) 0.064(3) Uani 1 1 d U . .
H32A H 0.1637 0.6165 0.6786 0.096 Uiso 1 1 calc R . .
H32B H 0.2829 0.6334 0.6806 0.096 Uiso 1 1 calc R . .
H32C H 0.2450 0.5593 0.6761 0.096 Uiso 1 1 calc R . .
C33 C 0.0994(8) 0.5608(5) 0.5311(7) 0.057(3) Uani 1 1 d U . .
H33A H 0.0376 0.5729 0.5485 0.085 Uiso 1 1 calc R . .
H33B H 0.1198 0.5160 0.5472 0.085 Uiso 1 1 calc R . .
H33C H 0.0823 0.5639 0.4740 0.085 Uiso 1 1 calc R . .
O15 O 0.3405(5) 0.5137(2) 0.5664(3) 0.0380(13) Uani 1 1 d U . .
O14 O 0.6305(5) 0.3263(2) 0.6421(3) 0.0353(13) Uani 1 1 d U . .
C42 C 0.1254(9) 0.3704(5) 0.3608(7) 0.062(3) Uani 1 1 d U . .
H42A H 0.0705 0.3380 0.3399 0.094 Uiso 1 1 calc R . .
H42B H 0.0991 0.4137 0.3424 0.094 Uiso 1 1 calc R . .
H42C H 0.1443 0.3695 0.4180 0.094 Uiso 1 1 calc R . .
C43 C 0.1982(10) 0.3557(5) 0.2426(6) 0.062(3) Uani 1 1 d U . .
H43A H 0.1445 0.3228 0.2207 0.093 Uiso 1 1 calc R . .
H43B H 0.2622 0.3460 0.2268 0.093 Uiso 1 1 calc R . .
H43C H 0.1717 0.3987 0.2232 0.093 Uiso 1 1 calc R . .
C63 C 0.6087(12) 0.5476(5) 0.1333(6) 0.076(3) Uani 1 1 d U . .
H63A H 0.6155 0.5618 0.0823 0.113 Uiso 1 1 calc R . .
H63B H 0.6106 0.5000 0.1358 0.113 Uiso 1 1 calc R . .
H63C H 0.6671 0.5653 0.1746 0.113 Uiso 1 1 calc R . .
C40 C 0.2174(16) 0.3436(10) 0.6242(12) 0.158(8) Uani 1 1 d DU . .
H40A H 0.2266 0.3627 0.6767 0.190 Uiso 1 1 calc R . .
H40B H 0.2713 0.3090 0.6304 0.190 Uiso 1 1 calc R . .
C801 C 0.1054(18) 0.7125(9) 0.2484(16) 0.181(10) Uani 1 1 d U . .
H80A H 0.0946 0.7489 0.2115 0.271 Uiso 1 1 calc R . .
H80B H 0.1421 0.7280 0.3008 0.271 Uiso 1 1 calc R . .
H80C H 0.0370 0.6942 0.2490 0.271 Uiso 1 1 calc R . .
C80 C 0.1633(13) 0.6667(7) 0.2264(9) 0.096(4) Uani 1 1 d U . .
H80D H 0.2314 0.6862 0.2250 0.115 Uiso 1 1 calc R . .
H80E H 0.1266 0.6530 0.1726 0.115 Uiso 1 1 calc R . .
C401 C 0.1101(14) 0.3089(10) 0.6036(13) 0.147(6) Uani 1 1 d DU . .
H40M H 0.1085 0.2774 0.6446 0.220 Uiso 1 1 calc R . .
H40N H 0.0995 0.2861 0.5537 0.220 Uiso 1 1 calc R . .
H40C H 0.0540 0.3410 0.5994 0.220 Uiso 1 1 calc R . .
O16 O 0.0313(10) 0.5248(5) 0.1906(7) 0.0407(13) Uani 0.482(12) 1 d PDU . .
H16A H 0.0644 0.5483 0.2276 0.061 Uiso 0.482(12) 1 calc PR . .
C161 C -0.0638(17) 0.4999(11) 0.2078(16) 0.086(7) Uani 0.482(12) 1 d PDU . .
H16M H -0.1172 0.5350 0.1976 0.103 Uiso 0.482(12) 1 calc PR . .
H16C H -0.0468 0.4893 0.2641 0.103 Uiso 0.482(12) 1 calc PR . .
C162 C -0.114(2) 0.4377(12) 0.1597(17) 0.106(10) Uani 0.482(12) 1 d PDU . .
H16D H -0.1778 0.4250 0.1749 0.158 Uiso 0.482(12) 1 calc PR . .
H16E H -0.0635 0.4019 0.1708 0.158 Uiso 0.482(12) 1 calc PR . .
H16F H -0.1334 0.4476 0.1038 0.158 Uiso 0.482(12) 1 calc PR . .
C171 C 0.107(3) 0.3534(11) -0.017(2) 0.198(16) Uani 0.61(3) 1 d PDU . .
H17A H 0.0323 0.3582 -0.0468 0.237 Uiso 0.61(3) 1 calc PR . .
H17Y H 0.1089 0.3281 0.0305 0.237 Uiso 0.61(3) 1 calc PR . .
C172 C 0.164(5) 0.3122(18) -0.068(3) 0.29(3) Uani 0.61(3) 1 d PDU . .
O17 O 0.1485(9) 0.4179(5) 0.0070(6) 0.109(2) Uani 1 1 d DU . .
H17E H 0.1218 0.4320 0.0415 0.163 Uiso 0.61(3) 1 calc PR . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O4 1.813(7) . ?
Ti1 O15 1.924(5) . ?
Ti1 O2 1.925(5) . ?
Ti1 O3 2.000(5) . ?
Ti1 O5 1.999(5) . ?
Ti1 O1 2.011(6) . ?
Ti2 O1 1.745(6) 3_666 ?
Ti2 O7 1.972(6) . ?
Ti2 O6 1.983(5) . ?
Ti2 O14 1.995(5) 3_666 ?
Ti2 O9 2.021(6) . ?
Ti2 O8 2.144(7) . ?
P3 O7 1.521(6) . ?
P3 O15 1.520(5) . ?
P3 O12 1.551(6) . ?
P3 C3 1.818(9) . ?
P4 O2 1.519(5) . ?
P4 O6 1.525(5) . ?
P4 O10 1.554(6) . ?
P4 C4 1.842(9) . ?
P5 O3 1.512(6) . ?
P5 O14 1.530(6) . ?
P5 O11 1.567(5) . ?
P5 C5 1.812(8) . ?
P6 O5 1.505(6) 3_666 ?
P6 O9 1.497(7) . ?
P6 O13 1.566(10) . ?
P6 C6 1.806(8) . ?
O1 Ti2 1.745(6) 3_666 ?
O8 C80 1.490(15) . ?
O4 C40 1.351(15) . ?
O5 P6 1.505(6) 3_666 ?
C51 C5 1.546(11) . ?
C4 C43 1.513(13) . ?
C4 C42 1.512(14) . ?
C4 C41 1.540(13) . ?
C5 C53 1.525(14) . ?
C5 C52 1.531(14) . ?
C6 C62 1.514(12) . ?
C6 C61 1.549(15) . ?
C6 C63 1.565(16) . ?
C31 C3 1.518(13) . ?
C3 C32 1.531(13) . ?
C3 C33 1.521(13) . ?
O14 Ti2 1.995(5) 3_666 ?
C40 C401 1.507(10) . ?
C801 C80 1.31(2) . ?
O16 C161 1.432(16) . ?
C161 C162 1.550(10) . ?
C171 O17 1.425(18) . ?
C171 C172 1.541(10) . ?

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 O15 96.6(3) . . ?
O4 Ti1 O2 97.2(3) . . ?
O15 Ti1 O2 90.5(2) . . ?
O4 Ti1 O3 88.3(3) . . ?
O15 Ti1 O3 175.1(3) . . ?
O2 Ti1 O3 89.5(2) . . ?
O4 Ti1 O5 89.2(3) . . ?
O15 Ti1 O5 90.0(2) . . ?
O2 Ti1 O5 173.6(3) . . ?
O3 Ti1 O5 89.5(2) . . ?
O4 Ti1 O1 170.1(2) . . ?
O15 Ti1 O1 90.4(2) . . ?
O2 Ti1 O1 89.7(2) . . ?
O3 Ti1 O1 84.7(2) . . ?
O5 Ti1 O1 83.8(2) . . ?
O1 Ti2 O7 97.2(2) 3_666 . ?
O1 Ti2 O6 98.1(2) 3_666 . ?
O7 Ti2 O6 88.8(2) . . ?
O1 Ti2 O14 92.9(2) 3_666 3_666 ?
O7 Ti2 O14 90.1(2) . 3_666 ?
O6 Ti2 O14 169.0(2) . 3_666 ?
O1 Ti2 O9 91.5(3) 3_666 . ?
O7 Ti2 O9 171.3(3) . . ?
O6 Ti2 O9 89.2(2) . . ?
O14 Ti2 O9 90.3(2) 3_666 . ?
O1 Ti2 O8 174.6(3) 3_666 . ?
O7 Ti2 O8 86.9(3) . . ?
O6 Ti2 O8 85.4(2) . . ?
O14 Ti2 O8 83.6(2) 3_666 . ?
O9 Ti2 O8 84.5(3) . . ?
O7 P3 O15 113.6(3) . . ?
O7 P3 O12 111.5(3) . . ?
O15 P3 O12 109.2(3) . . ?
O7 P3 C3 106.3(4) . . ?
O15 P3 C3 107.5(4) . . ?
O12 P3 C3 108.4(3) . . ?
O2 P4 O6 113.6(3) . . ?
O2 P4 O10 109.8(3) . . ?
O6 P4 O10 110.3(3) . . ?
O2 P4 C4 107.1(4) . . ?
O6 P4 C4 107.5(4) . . ?
O10 P4 C4 108.3(4) . . ?
O3 P5 O14 113.0(3) . . ?
O3 P5 O11 111.4(3) . . ?
O14 P5 O11 110.4(3) . . ?
O3 P5 C5 108.7(4) . . ?
O14 P5 C5 110.1(4) . . ?
O11 P5 C5 102.7(3) . . ?
O5 P6 O9 112.5(3) 3_666 . ?
O5 P6 O13 111.8(5) 3_666 . ?
O9 P6 O13 109.6(5) . . ?
O5 P6 C6 109.3(4) 3_666 . ?
O9 P6 C6 110.0(4) . . ?
O13 P6 C6 103.2(5) . . ?
Ti2 O1 Ti1 142.0(3) 3_666 . ?
P4 O6 Ti2 131.9(4) . . ?
P3 O7 Ti2 138.1(4) . . ?
P4 O2 Ti1 171.8(4) . . ?
P5 O3 Ti1 137.7(4) . . ?
C80 O8 Ti2 126.8(8) . . ?
C40 O4 Ti1 130.7(10) . . ?
P6 O9 Ti2 128.9(3) . . ?
P6 O5 Ti1 137.3(4) 3_666 . ?
C43 C4 C42 111.7(9) . . ?
C43 C4 C41 110.4(8) . . ?
C42 C4 C41 111.3(9) . . ?
C43 C4 P4 108.1(7) . . ?
C42 C4 P4 108.3(6) . . ?
C41 C4 P4 106.9(7) . . ?
C53 C5 C52 111.5(7) . . ?
C53 C5 C51 109.6(8) . . ?
C52 C5 C51 109.6(8) . . ?
C53 C5 P5 109.3(6) . . ?
C52 C5 P5 109.4(6) . . ?
C51 C5 P5 107.3(5) . . ?
C62 C6 C61 109.7(9) . . ?
C62 C6 C63 109.9(9) . . ?
C61 C6 C63 109.2(9) . . ?
C62 C6 P6 108.9(6) . . ?
C61 C6 P6 110.1(7) . . ?
C63 C6 P6 109.1(7) . . ?
C32 C3 C31 110.7(8) . . ?
C32 C3 C33 111.8(8) . . ?
C31 C3 C33 110.1(9) . . ?
C32 C3 P3 107.9(7) . . ?
C31 C3 P3 107.6(7) . . ?
C33 C3 P3 108.5(6) . . ?
P3 O15 Ti1 164.2(4) . . ?
P5 O14 Ti2 128.7(3) . 3_666 ?
O4 C40 C401 124.5(17) . . ?
C801 C80 O8 115.5(16) . . ?
O16 C161 C162 115.5(13) . . ?
O17 C171 C172 117.7(15) . . ?

_diffrn_measured_fraction_theta_max 0.975
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.975
_refine_diff_density_max         2.699
_refine_diff_density_min         -2.720
_refine_diff_density_rms         0.130
####################################################################### 
# 
# 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_titbpp1to1_26juna_0m
_database_code_depnum_ccdc_archive 'CCDC 1872963'
loop_
_audit_author_name
_audit_author_address
'Vadim Kessler'
;Swedish University of Agricultural Sciences
Sweden
;
_audit_update_record             
;
2018-10-12 deposited with the CCDC.	2020-02-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H128 O36 P2 Ti10'
_chemical_formula_weight         1870.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1


loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.667(5)
_cell_length_b                   12.635(7)
_cell_length_c                   17.668(9)
_cell_angle_alpha                94.311(12)
_cell_angle_beta                 105.875(10)
_cell_angle_gamma                111.946(10)
_cell_volume                     2277(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2960
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      16.61

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             978
_exptl_absorpt_coefficient_mu    0.934
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.7800
_exptl_absorpt_correction_T_max  0.9124
_exptl_absorpt_process_details   'Bruker SADABS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX-II CCD'
_diffrn_measurement_method       'Omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            50732
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0312
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.22
_diffrn_reflns_theta_max         25.02
_reflns_number_total             7996
_reflns_number_gt                5468
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0944P)²+6.3754P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7996
_refine_ls_number_parameters     451
_refine_ls_number_restraints     50
_refine_ls_R_factor_all          0.1143
_refine_ls_R_factor_gt           0.0804
_refine_ls_wR_factor_ref         0.2262
_refine_ls_wR_factor_gt          0.2055
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_restrained_S_all      1.000
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.12605(12) 0.41534(10) 0.30137(7) 0.0745(4) Uani 1 1 d . . .
Ti2 Ti -0.06975(12) 0.42758(10) 0.40896(7) 0.0725(4) Uani 1 1 d . . .
Ti3 Ti -0.20276(13) 0.17439(10) 0.27784(7) 0.0789(4) Uani 1 1 d . . .
Ti4 Ti -0.06351(14) 0.22189(11) 0.14215(7) 0.0845(4) Uani 1 1 d . . .
Ti5 Ti -0.15238(14) 0.41162(11) 0.21565(7) 0.0819(4) Uani 1 1 d . . .
P6 P 0.0604(2) 0.15104(16) 0.29507(11) 0.0810(5) Uani 1 1 d . . .
O1 O -0.0626(4) 0.3005(3) 0.2463(2) 0.0694(10) Uani 1 1 d . . .
O15 O 0.0874(4) 0.4538(4) 0.3909(2) 0.0748(11) Uani 1 1 d . . .
O16 O 0.0395(5) 0.5112(4) 0.2407(3) 0.0833(12) Uani 1 1 d D . .
O17 O -0.0131(4) 0.5846(4) 0.4758(2) 0.0748(11) Uani 1 1 d D . .
O3 O 0.0286(5) 0.1312(4) 0.2040(3) 0.0867(13) Uani 1 1 d . . .
O14 O -0.1426(4) 0.4684(4) 0.3153(3) 0.0799(12) Uani 1 1 d . . .
O8 O 0.1547(4) 0.2783(4) 0.3334(3) 0.0791(12) Uani 1 1 d . . .
O4 O -0.0661(5) 0.1157(4) 0.3160(3) 0.0804(12) Uani 1 1 d . . .
O11 O -0.1597(4) 0.2688(4) 0.3717(2) 0.0781(12) Uani 1 1 d . . .
O10 O 0.1123(5) 0.3496(4) 0.1822(3) 0.0860(13) Uani 1 1 d . . .
O5 O -0.2981(5) 0.2640(4) 0.2154(3) 0.0879(13) Uani 1 1 d . . .
O2 O -0.1470(5) 0.3274(5) 0.1080(3) 0.0948(15) Uani 1 1 d . . .
O6 O -0.2306(6) 0.4914(5) 0.1582(3) 0.1127(18) Uani 1 1 d D . .
O9 O -0.2179(5) 0.1088(4) 0.1582(3) 0.0954(15) Uani 1 1 d D . .
O7 O 0.2930(5) 0.5104(5) 0.3272(3) 0.0982(15) Uani 1 1 d D . .
C1 C 0.1415(9) 0.0600(7) 0.3343(5) 0.102(2) Uani 1 1 d . . .
O13 O -0.3400(6) 0.0495(4) 0.2795(3) 0.1095(17) Uani 1 1 d D . .
C1A C 0.0459(11) -0.0681(8) 0.2968(6) 0.136(4) Uani 1 1 d . . .
H1AA H 0.0866 -0.1185 0.3165 0.204 Uiso 1 1 calc R . .
H1AB H 0.0236 -0.0798 0.2394 0.204 Uiso 1 1 calc R . .
H1AC H -0.0320 -0.0856 0.3111 0.204 Uiso 1 1 calc R . .
C1B C 0.2665(10) 0.0907(9) 0.3118(6) 0.137(4) Uani 1 1 d . . .
H1BA H 0.3095 0.0423 0.3324 0.205 Uiso 1 1 calc R . .
H1BB H 0.3239 0.1710 0.3346 0.205 Uiso 1 1 calc R . .
H1BC H 0.2445 0.0782 0.2545 0.205 Uiso 1 1 calc R . .
C12A C -0.0151(13) 0.6955(11) 0.4482(8) 0.163(4) Uani 1 1 d DU . .
H12A H 0.0524 0.7645 0.4862 0.196 Uiso 1 1 calc R . .
H12B H -0.0050 0.6981 0.3956 0.196 Uiso 1 1 calc R . .
C2 C -0.1714(11) 0.3630(9) 0.0314(5) 0.126(3) Uani 1 1 d D . .
H2A H -0.1140 0.3514 0.0041 0.152 Uiso 1 1 calc R . .
H2B H -0.1545 0.4449 0.0394 0.152 Uiso 1 1 calc R . .
C1C C 0.1771(10) 0.0812(9) 0.4265(6) 0.137(3) Uani 1 1 d U . .
H1CA H 0.2200 0.0328 0.4474 0.205 Uiso 1 1 calc R . .
H1CB H 0.0989 0.0624 0.4406 0.205 Uiso 1 1 calc R . .
H1CC H 0.2345 0.1615 0.4489 0.205 Uiso 1 1 calc R . .
C9 C 0.0882(13) 0.6332(8) 0.2605(7) 0.152(4) Uani 1 1 d D . .
H9A H 0.1448 0.6601 0.3160 0.182 Uiso 1 1 calc R . .
H9B H 0.0159 0.6557 0.2553 0.182 Uiso 1 1 calc R . .
C6 C 0.2172(11) 0.3378(10) 0.1618(6) 0.139(4) Uani 1 1 d D . .
H6A H 0.1889 0.2584 0.1346 0.167 Uiso 1 1 calc R . .
H6B H 0.2893 0.3535 0.2105 0.167 Uiso 1 1 calc R . .
C8 C -0.4248(14) 0.2597(13) 0.2151(9) 0.182(5) Uani 1 1 d D . .
H8A H -0.4470 0.2214 0.2579 0.219 Uiso 1 1 calc R . .
H8B H -0.4161 0.3389 0.2278 0.219 Uiso 1 1 calc R . .
C15 C -0.3547(12) 0.3050(11) 0.4451(8) 0.163(5) Uani 1 1 d D . .
H15A H -0.3811 0.2575 0.3924 0.195 Uiso 1 1 calc R . .
H15B H -0.4245 0.3283 0.4466 0.195 Uiso 1 1 calc R . .
C15A C -0.3410(17) 0.2336(15) 0.5050(11) 0.236(8) Uani 1 1 d D . .
H15C H -0.4221 0.1667 0.4936 0.354 Uiso 1 1 calc R . .
H15D H -0.3187 0.2784 0.5573 0.354 Uiso 1 1 calc R . .
H15E H -0.2733 0.2086 0.5036 0.354 Uiso 1 1 calc R . .
C2A C -0.3086(12) 0.2926(12) -0.0172(7) 0.185(6) Uani 1 1 d D . .
H2AA H -0.3265 0.3150 -0.0684 0.277 Uiso 1 1 calc R . .
H2AB H -0.3647 0.3050 0.0101 0.277 Uiso 1 1 calc R . .
H2AC H -0.3244 0.2117 -0.0249 0.277 Uiso 1 1 calc R . .
C8B C -0.5283(16) 0.2035(18) 0.1442(10) 0.266(11) Uani 1 1 d D . .
H8BA H -0.6068 0.2047 0.1509 0.398 Uiso 1 1 calc R . .
H8BB H -0.5397 0.1243 0.1312 0.398 Uiso 1 1 calc R . .
H8BC H -0.5100 0.2426 0.1016 0.398 Uiso 1 1 calc R . .
C12 C -0.1338(15) 0.6843(15) 0.4463(9) 0.228(8) Uani 1 1 d D . .
H12C H -0.1472 0.7509 0.4303 0.342 Uiso 1 1 calc R . .
H12D H -0.1417 0.6789 0.4987 0.342 Uiso 1 1 calc R . .
H12E H -0.1981 0.6151 0.4085 0.342 Uiso 1 1 calc R . .
C7 C -0.4030(19) -0.0528(16) 0.3166(13) 0.310(13) Uani 1 1 d D . .
H7A H -0.3711 -0.1133 0.3144 0.372 Uiso 1 1 calc R . .
H7B H -0.4062 -0.0312 0.3696 0.372 Uiso 1 1 calc R . .
O40 O -0.0725(6) 0.1630(5) 0.0460(3) 0.1148(19) Uani 1 1 d D . .
C29A C 0.2608(16) 0.4156(15) 0.1112(9) 0.220(7) Uani 1 1 d D . .
H29A H 0.3332 0.4071 0.0999 0.331 Uiso 1 1 calc R . .
H29B H 0.2878 0.4942 0.1378 0.331 Uiso 1 1 calc R . .
H29C H 0.1907 0.3977 0.0619 0.331 Uiso 1 1 calc R . .
C50A C 0.4322(14) 0.5364(18) 0.3648(12) 0.281(11) Uani 1 1 d D . .
H50A H 0.4660 0.5875 0.4169 0.337 Uiso 1 1 calc R . .
H50B H 0.4431 0.4651 0.3723 0.337 Uiso 1 1 calc R . .
O18B O -0.2395(5) 0.4077(4) 0.4544(3) 0.0934(14) Uani 1 1 d D . .
C9A C 0.1596(16) 0.6878(14) 0.2098(10) 0.220(7) Uani 1 1 d DU . .
H9AA H 0.1922 0.7708 0.2252 0.330 Uiso 1 1 calc R . .
H9AB H 0.1031 0.6630 0.1550 0.330 Uiso 1 1 calc R . .
H9AC H 0.2317 0.6661 0.2151 0.330 Uiso 1 1 calc R . .
C62 C -0.2756(18) 0.5820(15) 0.1690(11) 0.242(9) Uani 1 1 d D . .
H62A H -0.2007 0.6566 0.1877 0.290 Uiso 1 1 calc R . .
H62B H -0.3168 0.5695 0.2103 0.290 Uiso 1 1 calc R . .
C62B C -0.373(2) 0.587(2) 0.0918(12) 0.45(2) Uani 1 1 d D . .
H62C H -0.4025 0.6456 0.1033 0.672 Uiso 1 1 calc R . .
H62D H -0.4467 0.5124 0.0722 0.672 Uiso 1 1 calc R . .
H62E H -0.3311 0.6044 0.0518 0.672 Uiso 1 1 calc R . .
C50B C 0.500(4) 0.590(3) 0.315(2) 0.56(2) Uani 1 1 d DU . .
H50C H 0.5919 0.6167 0.3410 0.836 Uiso 1 1 calc R . .
H50D H 0.4799 0.6557 0.3024 0.836 Uiso 1 1 calc R . .
H50E H 0.4734 0.5359 0.2657 0.836 Uiso 1 1 calc R . .
C60A C -0.3355(17) 0.0055(16) 0.0964(10) 0.258(11) Uani 1 1 d D . .
H60A H -0.4171 -0.0146 0.1077 0.310 Uiso 1 1 calc R . .
H60B H -0.3467 0.0130 0.0409 0.310 Uiso 1 1 calc R . .
C60C C -0.2730(19) -0.0611(17) 0.1214(12) 0.235(8) Uani 1 1 d D . .
H60C H -0.3247 -0.1397 0.0922 0.353 Uiso 1 1 calc R . .
H60D H -0.2588 -0.0590 0.1777 0.353 Uiso 1 1 calc R . .
H60E H -0.1903 -0.0324 0.1121 0.353 Uiso 1 1 calc R . .
C26A C -0.052(2) 0.1384(17) -0.0298(7) 0.288(12) Uani 1 1 d D . .
H26A H -0.0486 0.2010 -0.0589 0.346 Uiso 1 1 calc R . .
H26X H 0.0298 0.1294 -0.0206 0.346 Uiso 1 1 calc R . .
C26B C -0.153(3) 0.040(2) -0.0706(15) 0.49(3) Uani 1 1 d D . .
H26V H -0.1437 0.0184 -0.1213 0.734 Uiso 1 1 calc R . .
H26C H -0.2321 0.0508 -0.0796 0.734 Uiso 1 1 calc R . .
H26D H -0.1550 -0.0205 -0.0404 0.734 Uiso 1 1 calc R . .
C7A C -0.520(4) -0.073(6) 0.251(3) 0.79(3) Uani 1 1 d DU . .
H7A1 H -0.5932 -0.1349 0.2575 1.178 Uiso 1 1 calc R . .
H7A2 H -0.5090 -0.0941 0.2012 1.178 Uiso 1 1 calc R . .
H7A3 H -0.5349 -0.0033 0.2517 1.178 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O7 1.769(5) . ?
Ti1 O15 1.838(4) . ?
Ti1 O8 1.976(4) . ?
Ti1 O1 2.031(4) . ?
Ti1 O16 2.038(5) . ?
Ti1 O10 2.144(4) . ?
Ti1 Ti5 3.167(2) . ?
Ti1 Ti4 3.209(2) . ?
Ti1 Ti2 3.3838(19) . ?
Ti2 O11 1.846(4) . ?
Ti2 O14 1.848(5) . ?
Ti2 O15 1.859(5) . ?
Ti2 O17 2.002(4) . ?
Ti2 O17 2.047(4) 2_566 ?
Ti2 O18B 2.271(5) . ?
Ti2 Ti2 3.220(3) 2_566 ?
Ti2 Ti5 3.253(2) . ?
Ti2 Ti3 3.349(2) . ?
Ti3 O13 1.788(5) . ?
Ti3 O11 1.796(4) . ?
Ti3 O4 1.979(5) . ?
Ti3 O5 2.048(5) . ?
Ti3 O1 2.051(4) . ?
Ti3 O9 2.147(5) . ?
Ti3 Ti5 3.173(2) . ?
Ti3 Ti4 3.219(2) . ?
Ti4 O40 1.762(5) . ?
Ti4 O9 1.945(6) . ?
Ti4 O2 1.965(5) . ?
Ti4 O10 1.968(5) . ?
Ti4 O1 2.020(4) . ?
Ti4 O3 2.031(5) . ?
Ti4 Ti5 3.261(2) . ?
Ti5 O6 1.793(5) . ?
Ti5 O14 1.807(4) . ?
Ti5 O5 1.998(5) . ?
Ti5 O16 2.015(5) . ?
Ti5 O1 2.066(4) . ?
Ti5 O2 2.136(5) . ?
P6 O3 1.528(5) . ?
P6 O4 1.531(5) . ?
P6 O8 1.537(5) . ?
P6 C1 1.808(8) . ?
O16 C9 1.407(10) . ?
O17 C12A 1.523(11) . ?
O17 Ti2 2.046(4) 2_566 ?
O10 C6 1.421(10) . ?
O5 C8 1.458(14) . ?
O2 C2 1.447(9) . ?
O6 C62 1.446(12) . ?
O9 C60A 1.550(16) . ?
O7 C50A 1.471(15) . ?
C1 C1B 1.534(12) . ?
C1 C1C 1.543(12) . ?
C1 C1A 1.546(12) . ?
O13 C7 1.525(14) . ?
C12A C12 1.328(13) . ?
C2 C2A 1.470(12) . ?
C9 C9A 1.430(13) . ?
C6 C29A 1.425(12) . ?
C8 C8B 1.389(14) . ?
C15 O18B 1.435(11) . ?
C15 C15A 1.456(14) . ?
C7 C7A 1.45(2) . ?
O40 C26A 1.457(8) . ?
C50A C50B 1.394(19) . ?
C62 C62B 1.5394(12) . ?
C60A C60C 1.331(14) . ?
C26A C26B 1.327(18) . ?

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
O7 Ti1 O15 101.9(2) . . ?
O7 Ti1 O8 96.5(2) . . ?
O15 Ti1 O8 95.39(19) . . ?
O7 Ti1 O1 166.9(2) . . ?
O15 Ti1 O1 90.86(18) . . ?
O8 Ti1 O1 85.01(18) . . ?
O7 Ti1 O16 100.8(2) . . ?
O15 Ti1 O16 90.95(19) . . ?
O8 Ti1 O16 159.9(2) . . ?
O1 Ti1 O16 75.85(18) . . ?
O7 Ti1 O10 93.5(2) . . ?
O15 Ti1 O10 163.8(2) . . ?
O8 Ti1 O10 87.67(18) . . ?
O1 Ti1 O10 73.53(17) . . ?
O16 Ti1 O10 81.22(18) . . ?
O7 Ti1 Ti5 139.06(19) . . ?
O15 Ti1 Ti5 81.02(14) . . ?
O8 Ti1 Ti5 124.13(15) . . ?
O1 Ti1 Ti5 39.77(12) . . ?
O16 Ti1 Ti5 38.34(14) . . ?
O10 Ti1 Ti5 84.10(14) . . ?
O7 Ti1 Ti4 129.89(18) . . ?
O15 Ti1 Ti4 128.19(15) . . ?
O8 Ti1 Ti4 79.90(14) . . ?
O1 Ti1 Ti4 37.48(11) . . ?
O16 Ti1 Ti4 81.21(14) . . ?
O10 Ti1 Ti4 36.77(14) . . ?
Ti5 Ti1 Ti4 61.51(4) . . ?
O7 Ti1 Ti2 124.51(18) . . ?
O15 Ti1 Ti2 23.90(14) . . ?
O8 Ti1 Ti2 98.89(13) . . ?
O1 Ti1 Ti2 67.79(11) . . ?
O16 Ti1 Ti2 79.61(13) . . ?
O10 Ti1 Ti2 139.91(14) . . ?
Ti5 Ti1 Ti2 59.44(5) . . ?
Ti4 Ti1 Ti2 105.26(6) . . ?
O11 Ti2 O14 95.7(2) . . ?
O11 Ti2 O15 101.23(19) . . ?
O14 Ti2 O15 95.0(2) . . ?
O11 Ti2 O17 158.67(19) . . ?
O14 Ti2 O17 93.31(18) . . ?
O15 Ti2 O17 97.17(18) . . ?
O11 Ti2 O17 94.90(19) . 2_566 ?
O14 Ti2 O17 167.68(17) . 2_566 ?
O15 Ti2 O17 89.04(19) . 2_566 ?
O17 Ti2 O17 74.61(18) . 2_566 ?
O11 Ti2 O18B 83.78(19) . . ?
O14 Ti2 O18B 93.4(2) . . ?
O15 Ti2 O18B 169.79(19) . . ?
O17 Ti2 O18B 76.42(19) . . ?
O17 Ti2 O18B 81.63(19) 2_566 . ?
O11 Ti2 Ti2 129.30(15) . 2_566 ?
O14 Ti2 Ti2 131.05(15) . 2_566 ?
O15 Ti2 Ti2 93.84(14) . 2_566 ?
O17 Ti2 Ti2 37.78(12) . 2_566 ?
O17 Ti2 Ti2 36.82(11) 2_566 2_566 ?
O18B Ti2 Ti2 76.20(14) . 2_566 ?
O11 Ti2 Ti5 78.65(14) . . ?
O14 Ti2 Ti5 26.78(13) . . ?
O15 Ti2 Ti5 78.32(13) . . ?
O17 Ti2 Ti5 115.92(13) . . ?
O17 Ti2 Ti5 164.26(12) 2_566 . ?
O18B Ti2 Ti5 111.55(15) . . ?
Ti2 Ti2 Ti5 152.06(7) 2_566 . ?
O11 Ti2 Ti3 22.81(13) . . ?
O14 Ti2 Ti3 78.48(14) . . ?
O15 Ti2 Ti3 87.92(13) . . ?
O17 Ti2 Ti3 170.72(13) . . ?
O17 Ti2 Ti3 113.37(12) 2_566 . ?
O18B Ti2 Ti3 99.54(14) . . ?
Ti2 Ti2 Ti3 149.95(7) 2_566 . ?
Ti5 Ti2 Ti3 57.43(4) . . ?
O11 Ti2 Ti1 86.45(13) . . ?
O14 Ti2 Ti1 78.17(14) . . ?
O15 Ti2 Ti1 23.61(12) . . ?
O17 Ti2 Ti1 114.35(14) . . ?
O17 Ti2 Ti1 108.71(13) 2_566 . ?
O18B Ti2 Ti1 166.39(14) . . ?
Ti2 Ti2 Ti1 117.39(7) 2_566 . ?
Ti5 Ti2 Ti1 56.96(4) . . ?
Ti3 Ti2 Ti1 68.51(4) . . ?
O13 Ti3 O11 102.8(2) . . ?
O13 Ti3 O4 98.2(2) . . ?
O11 Ti3 O4 95.2(2) . . ?
O13 Ti3 O5 99.8(3) . . ?
O11 Ti3 O5 92.2(2) . . ?
O4 Ti3 O5 158.5(2) . . ?
O13 Ti3 O1 165.9(2) . . ?
O11 Ti3 O1 90.68(18) . . ?
O4 Ti3 O1 84.55(18) . . ?
O5 Ti3 O1 75.19(19) . . ?
O13 Ti3 O9 93.6(2) . . ?
O11 Ti3 O9 162.9(2) . . ?
O4 Ti3 O9 86.9(2) . . ?
O5 Ti3 O9 80.4(2) . . ?
O1 Ti3 O9 72.62(18) . . ?
O13 Ti3 Ti5 137.5(2) . . ?
O11 Ti3 Ti5 81.59(15) . . ?
O4 Ti3 Ti5 123.76(14) . . ?
O5 Ti3 Ti5 37.79(14) . . ?
O1 Ti3 Ti5 39.74(12) . . ?
O9 Ti3 Ti5 83.19(15) . . ?
O13 Ti3 Ti4 129.33(18) . . ?
O11 Ti3 Ti4 127.86(15) . . ?
O4 Ti3 Ti4 79.09(13) . . ?
O5 Ti3 Ti4 80.44(14) . . ?
O1 Ti3 Ti4 37.40(11) . . ?
O9 Ti3 Ti4 35.96(15) . . ?
Ti5 Ti3 Ti4 61.34(4) . . ?
O13 Ti3 Ti2 124.19(18) . . ?
O11 Ti3 Ti2 23.48(14) . . ?
O4 Ti3 Ti2 99.92(14) . . ?
O5 Ti3 Ti2 79.45(14) . . ?
O1 Ti3 Ti2 68.46(11) . . ?
O9 Ti3 Ti2 139.52(15) . . ?
Ti5 Ti3 Ti2 59.77(5) . . ?
Ti4 Ti3 Ti2 105.84(5) . . ?
O40 Ti4 O9 103.2(3) . . ?
O40 Ti4 O2 96.9(2) . . ?
O9 Ti4 O2 93.9(2) . . ?
O40 Ti4 O10 102.8(2) . . ?
O9 Ti4 O10 152.2(2) . . ?
O2 Ti4 O10 92.7(2) . . ?
O40 Ti4 O1 173.6(2) . . ?
O9 Ti4 O1 77.66(18) . . ?
O2 Ti4 O1 76.70(17) . . ?
O10 Ti4 O1 77.66(18) . . ?
O40 Ti4 O3 96.7(2) . . ?
O9 Ti4 O3 84.0(2) . . ?
O2 Ti4 O3 166.34(18) . . ?
O10 Ti4 O3 83.3(2) . . ?
O1 Ti4 O3 89.68(17) . . ?
O40 Ti4 Ti1 143.4(2) . . ?
O9 Ti4 Ti1 112.50(14) . . ?
O2 Ti4 Ti1 88.73(15) . . ?
O10 Ti4 Ti1 40.71(13) . . ?
O1 Ti4 Ti1 37.72(12) . . ?
O3 Ti4 Ti1 79.68(13) . . ?
O40 Ti4 Ti3 143.5(2) . . ?
O9 Ti4 Ti3 40.41(13) . . ?
O2 Ti4 Ti3 89.70(15) . . ?
O10 Ti4 Ti3 112.77(13) . . ?
O1 Ti4 Ti3 38.07(12) . . ?
O3 Ti4 Ti3 79.95(14) . . ?
Ti1 Ti4 Ti3 72.25(5) . . ?
O40 Ti4 Ti5 136.1(2) . . ?
O9 Ti4 Ti5 83.87(15) . . ?
O2 Ti4 Ti5 39.18(13) . . ?
O10 Ti4 Ti5 84.30(14) . . ?
O1 Ti4 Ti5 37.54(12) . . ?
O3 Ti4 Ti5 127.22(13) . . ?
Ti1 Ti4 Ti5 58.61(5) . . ?
Ti3 Ti4 Ti5 58.63(4) . . ?
O6 Ti5 O14 100.2(2) . . ?
O6 Ti5 O5 105.1(3) . . ?
O14 Ti5 O5 89.0(2) . . ?
O6 Ti5 O16 103.5(3) . . ?
O14 Ti5 O16 90.0(2) . . ?
O5 Ti5 O16 151.0(2) . . ?
O6 Ti5 O1 161.8(2) . . ?
O14 Ti5 O1 98.00(18) . . ?
O5 Ti5 O1 75.93(19) . . ?
O16 Ti5 O1 75.57(18) . . ?
O6 Ti5 O2 89.7(2) . . ?
O14 Ti5 O2 170.1(2) . . ?
O5 Ti5 O2 88.6(2) . . ?
O16 Ti5 O2 87.5(2) . . ?
O1 Ti5 O2 72.10(17) . . ?
O6 Ti5 Ti1 142.3(2) . . ?
O14 Ti5 Ti1 85.01(15) . . ?
O5 Ti5 Ti1 112.30(15) . . ?
O16 Ti5 Ti1 38.85(13) . . ?
O1 Ti5 Ti1 38.97(12) . . ?
O2 Ti5 Ti1 86.99(14) . . ?
O6 Ti5 Ti3 144.0(2) . . ?
O14 Ti5 Ti3 84.11(15) . . ?
O5 Ti5 Ti3 38.91(15) . . ?
O16 Ti5 Ti3 112.26(14) . . ?
O1 Ti5 Ti3 39.40(12) . . ?
O2 Ti5 Ti3 88.01(15) . . ?
Ti1 Ti5 Ti3 73.42(4) . . ?
O6 Ti5 Ti2 127.61(17) . . ?
O14 Ti5 Ti2 27.43(14) . . ?
O5 Ti5 Ti2 82.59(14) . . ?
O16 Ti5 Ti2 83.30(13) . . ?
O1 Ti5 Ti2 70.56(11) . . ?
O2 Ti5 Ti2 142.66(14) . . ?
Ti1 Ti5 Ti2 63.59(4) . . ?
Ti3 Ti5 Ti2 62.80(4) . . ?
O6 Ti5 Ti4 125.26(18) . . ?
O14 Ti5 Ti4 134.56(15) . . ?
O5 Ti5 Ti4 80.03(14) . . ?
O16 Ti5 Ti4 80.18(13) . . ?
O1 Ti5 Ti4 36.57(11) . . ?
O2 Ti5 Ti4 35.54(13) . . ?
Ti1 Ti5 Ti4 59.88(4) . . ?
Ti3 Ti5 Ti4 60.03(5) . . ?
Ti2 Ti5 Ti4 107.13(5) . . ?
O3 P6 O4 109.8(3) . . ?
O3 P6 O8 110.3(3) . . ?
O4 P6 O8 112.0(2) . . ?
O3 P6 C1 108.8(3) . . ?
O4 P6 C1 108.2(4) . . ?
O8 P6 C1 107.7(4) . . ?
Ti4 O1 Ti1 104.79(18) . . ?
Ti4 O1 Ti3 104.53(18) . . ?
Ti1 O1 Ti3 136.4(2) . . ?
Ti4 O1 Ti5 105.90(18) . . ?
Ti1 O1 Ti5 101.26(18) . . ?
Ti3 O1 Ti5 100.86(18) . . ?
Ti1 O15 Ti2 132.5(2) . . ?
C9 O16 Ti5 120.6(6) . . ?
C9 O16 Ti1 124.0(6) . . ?
Ti5 O16 Ti1 102.8(2) . . ?
C12A O17 Ti2 128.7(6) . . ?
C12A O17 Ti2 125.6(6) . 2_566 ?
Ti2 O17 Ti2 105.39(18) . 2_566 ?
P6 O3 Ti4 118.1(2) . . ?
Ti5 O14 Ti2 125.8(2) . . ?
P6 O8 Ti1 124.9(3) . . ?
P6 O4 Ti3 125.6(3) . . ?
Ti3 O11 Ti2 133.7(2) . . ?
C6 O10 Ti4 120.2(6) . . ?
C6 O10 Ti1 123.9(5) . . ?
Ti4 O10 Ti1 102.53(19) . . ?
C8 O5 Ti5 122.0(7) . . ?
C8 O5 Ti3 125.6(7) . . ?
Ti5 O5 Ti3 103.3(2) . . ?
C2 O2 Ti4 127.9(5) . . ?
C2 O2 Ti5 125.3(5) . . ?
Ti4 O2 Ti5 105.3(2) . . ?
C62 O6 Ti5 140.5(8) . . ?
C60A O9 Ti4 128.9(7) . . ?
C60A O9 Ti3 126.9(7) . . ?
Ti4 O9 Ti3 103.6(2) . . ?
C50A O7 Ti1 150.5(10) . . ?
C1B C1 C1C 109.4(8) . . ?
C1B C1 C1A 110.6(7) . . ?
C1C C1 C1A 110.3(8) . . ?
C1B C1 P6 109.4(6) . . ?
C1C C1 P6 109.4(6) . . ?
C1A C1 P6 107.7(6) . . ?
C7 O13 Ti3 151.8(9) . . ?
C12 C12A O17 101.1(12) . . ?
O2 C2 C2A 108.4(9) . . ?
O16 C9 C9A 111.6(11) . . ?
O10 C6 C29A 111.6(11) . . ?
C8B C8 O5 116.4(14) . . ?
O18B C15 C15A 115.3(12) . . ?
C7A C7 O13 84(3) . . ?
C26A O40 Ti4 166.5(9) . . ?
C50B C50A O7 108(3) . . ?
C15 O18B Ti2 129.0(6) . . ?
O6 C62 C62B 113.3(16) . . ?
C60C C60A O9 87.2(14) . . ?
C26B C26A O40 105.4(17) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.724
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.092
####################################################################### 
# 
# 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_ti_tbup_5b
_database_code_depnum_ccdc_archive 'CCDC 1872962'
loop_
_audit_author_name
_audit_author_address
'Vadim Kessler'
;Swedish University of Agricultural Sciences
Sweden
;
_audit_update_record             
;
2018-10-12 deposited with the CCDC.	2020-02-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H91 O26 P4 Ti6'
_chemical_formula_weight         1375.39

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1


loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.141(3)
_cell_length_b                   14.492(4)
_cell_length_c                   19.519(8)
_cell_angle_alpha                96.504(4)
_cell_angle_beta                 99.449(5)
_cell_angle_gamma                113.033(3)
_cell_volume                     3309.3(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9031
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      24.08

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1438
_exptl_absorpt_coefficient_mu    0.854
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.8084
_exptl_absorpt_correction_T_max  0.8614
_exptl_absorpt_process_details   'Bruker SADABS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX-II CCD'
_diffrn_measurement_method       'Omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30157
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.24
_diffrn_reflns_theta_max         24.15
_reflns_number_total             10497
_reflns_number_gt                7909
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'


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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0217P)²+5.3604P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10497
_refine_ls_number_parameters     667
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0481
_refine_ls_wR_factor_ref         0.1076
_refine_ls_wR_factor_gt          0.1019
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.48159(6) 0.96185(6) 0.27138(4) 0.04810(19) Uani 1 1 d . . .
Ti2 Ti 0.26035(6) 0.97690(5) 0.30003(4) 0.04607(18) Uani 1 1 d . . .
Ti3 Ti 0.29001(6) 0.85070(5) 0.13098(3) 0.04592(18) Uani 1 1 d . . .
Ti4 Ti 0.23594(6) 0.61444(6) 0.18520(4) 0.0524(2) Uani 1 1 d . . .
Ti5 Ti 0.01259(6) 0.62462(6) 0.24007(4) 0.0563(2) Uani 1 1 d . . .
Ti6 Ti 0.21824(7) 0.61286(6) 0.35140(4) 0.0592(2) Uani 1 1 d . . .
P7 P 0.13339(9) 0.78515(9) 0.38293(6) 0.0517(3) Uani 1 1 d . . .
P8 P 0.38241(10) 1.08538(8) 0.19001(6) 0.0550(3) Uani 1 1 d . . .
P9 P 0.45311(9) 0.73871(9) 0.31419(6) 0.0537(3) Uani 1 1 d . . .
P10 P 0.05308(9) 0.82773(9) 0.16894(6) 0.0515(3) Uani 1 1 d . . .
O1 O 0.31315(19) 0.89898(18) 0.23535(12) 0.0416(6) Uani 1 1 d . . .
O15 O 0.19545(19) 0.69147(18) 0.26852(12) 0.0442(6) Uani 1 1 d . . .
O2 O 0.4577(2) 0.8887(2) 0.17405(13) 0.0487(6) Uani 1 1 d . . .
O16 O 0.0604(2) 0.5553(2) 0.16762(14) 0.0595(7) Uani 1 1 d . . .
O3 O 0.4232(2) 1.0171(2) 0.34670(12) 0.0507(7) Uani 1 1 d . . .
O17 O 0.3969(2) 0.6777(2) 0.23933(14) 0.0560(7) Uani 1 1 d . . .
O7 O 0.2188(2) 0.8737(2) 0.35979(13) 0.0506(6) Uani 1 1 d . . .
O8 O 0.1093(2) 0.9042(2) 0.23828(13) 0.0514(7) Uani 1 1 d . . .
O4 O 0.4794(2) 0.8506(2) 0.31814(13) 0.0553(7) Uani 1 1 d . . .
O11 O 0.2515(2) 0.7126(2) 0.13826(13) 0.0508(6) Uani 1 1 d . . .
O18 O 0.0490(2) 0.5458(2) 0.31138(16) 0.0649(8) Uani 1 1 d . . .
O21 O -0.0009(2) 0.7191(2) 0.18232(14) 0.0585(7) Uani 1 1 d . . .
O19 O 0.2216(2) 0.5281(2) 0.26913(16) 0.0649(8) Uani 1 1 d . . .
O12 O 0.1327(2) 0.8324(2) 0.12018(13) 0.0541(7) Uani 1 1 d . . .
O24 O 0.1895(2) 0.7167(2) 0.40948(13) 0.0570(7) Uani 1 1 d . . .
O9 O 0.3018(2) 1.0804(2) 0.23950(14) 0.0551(7) Uani 1 1 d . . .
O22 O 0.0285(2) 0.7229(2) 0.32290(14) 0.0548(7) Uani 1 1 d . . .
O13 O 0.3296(2) 0.9999(2) 0.12538(13) 0.0558(7) Uani 1 1 d . . .
O10 O 0.2349(2) 1.0662(2) 0.35759(15) 0.0630(8) Uani 1 1 d . . .
O5 O 0.4917(2) 1.0842(2) 0.23097(14) 0.0563(7) Uani 1 1 d . . .
O6 O 0.6337(2) 1.0263(2) 0.29865(15) 0.0639(8) Uani 1 1 d . . .
O25 O 0.3793(2) 0.6961(2) 0.36609(14) 0.0583(7) Uani 1 1 d . . .
O20 O 0.2422(3) 0.5184(2) 0.12261(16) 0.0711(8) Uani 1 1 d . . .
O14 O 0.2950(2) 0.8339(2) 0.03964(13) 0.0595(7) Uani 1 1 d . . .
O23 O -0.1333(2) 0.5473(2) 0.22005(18) 0.0805(10) Uani 1 1 d . . .
O26 O 0.2254(3) 0.5402(3) 0.41588(17) 0.0825(10) Uani 1 1 d . . .
C7 C 0.0840(4) 0.8340(4) 0.4543(2) 0.0687(13) Uani 1 1 d . . .
C8 C 0.4187(4) 1.2056(4) 0.1605(3) 0.0724(13) Uani 1 1 d . . .
C9 C 0.5866(4) 0.7290(4) 0.3424(2) 0.0709(13) Uani 1 1 d . . .
C14 C 0.3091(5) 0.8868(5) -0.0165(3) 0.0904(17) Uani 1 1 d . . .
H14A H 0.3306 0.8510 -0.0526 0.108 Uiso 1 1 calc R . .
H14B H 0.3702 0.9545 0.0007 0.108 Uiso 1 1 calc R . .
C122 C 0.5301(5) 0.8056(6) 0.0940(3) 0.122(2) Uani 1 1 d . . .
H12A H 0.5894 0.8185 0.0686 0.183 Uiso 1 1 calc R . .
H12B H 0.4577 0.7745 0.0610 0.183 Uiso 1 1 calc R . .
H12C H 0.5348 0.7604 0.1255 0.183 Uiso 1 1 calc R . .
C16 C 0.7258(4) 1.1170(4) 0.2960(3) 0.0992(19) Uani 1 1 d . . .
H16A H 0.7508 1.1632 0.3414 0.119 Uiso 1 1 calc R . .
H16B H 0.7002 1.1499 0.2606 0.119 Uiso 1 1 calc R . .
C9A C 0.6634(4) 0.7745(5) 0.2934(3) 0.0978(19) Uani 1 1 d . . .
H9AA H 0.7345 0.7699 0.3078 0.147 Uiso 1 1 calc R . .
H9AB H 0.6767 0.8449 0.2956 0.147 Uiso 1 1 calc R . .
H9AC H 0.6276 0.7374 0.2457 0.147 Uiso 1 1 calc R . .
C12 C 0.5427(4) 0.9008(5) 0.1343(3) 0.0891(17) Uani 1 1 d . . .
H12D H 0.6169 0.9326 0.1666 0.107 Uiso 1 1 calc R . .
H12E H 0.5394 0.9465 0.1021 0.107 Uiso 1 1 calc R . .
C113 C 0.4786(4) 1.0579(5) 0.4194(3) 0.0948(18) Uani 1 1 d . . .
H11A H 0.5286 1.0256 0.4339 0.114 Uiso 1 1 calc R . .
H11B H 0.4220 1.0418 0.4477 0.114 Uiso 1 1 calc R . .
C10A C -0.1391(4) 0.8558(5) 0.1727(3) 0.1000(19) Uani 1 1 d . . .
H10A H -0.1981 0.8725 0.1495 0.150 Uiso 1 1 calc R . .
H10B H -0.0978 0.9047 0.2159 0.150 Uiso 1 1 calc R . .
H10C H -0.1721 0.7887 0.1832 0.150 Uiso 1 1 calc R . .
C7A C 0.0142(6) 0.7458(5) 0.4857(3) 0.126(3) Uani 1 1 d . . .
H7AA H -0.0121 0.7713 0.5235 0.189 Uiso 1 1 calc R . .
H7AB H 0.0602 0.7125 0.5038 0.189 Uiso 1 1 calc R . .
H7AC H -0.0498 0.6979 0.4497 0.189 Uiso 1 1 calc R . .
C121 C 0.3786(7) 0.5004(6) 0.0635(4) 0.155(3) Uani 1 1 d . . .
H12F H 0.3933 0.4920 0.0172 0.233 Uiso 1 1 calc R . .
H12G H 0.3779 0.4436 0.0847 0.233 Uiso 1 1 calc R . .
H12H H 0.4370 0.5627 0.0924 0.233 Uiso 1 1 calc R . .
C10 C -0.0578(4) 0.8584(4) 0.1240(2) 0.0701(13) Uani 1 1 d . . .
C131 C 0.5434(6) 1.1663(6) 0.4331(4) 0.161(4) Uani 1 1 d . . .
H13A H 0.5787 1.1901 0.4827 0.241 Uiso 1 1 calc R . .
H13B H 0.4941 1.1989 0.4197 0.241 Uiso 1 1 calc R . .
H13C H 0.6008 1.1826 0.4062 0.241 Uiso 1 1 calc R . .
C10B C -0.1212(5) 0.7804(5) 0.0553(3) 0.111(2) Uani 1 1 d . . .
H10D H -0.1800 0.7964 0.0311 0.166 Uiso 1 1 calc R . .
H10E H -0.1543 0.7132 0.0659 0.166 Uiso 1 1 calc R . .
H10F H -0.0691 0.7822 0.0257 0.166 Uiso 1 1 calc R . .
C120 C 0.2713(6) 0.5048(6) 0.0580(3) 0.137(3) Uani 1 1 d . . .
H12I H 0.2132 0.4419 0.0283 0.165 Uiso 1 1 calc R . .
H12J H 0.2719 0.5606 0.0347 0.165 Uiso 1 1 calc R . .
C119 C 0.2449(7) 0.4331(6) 0.2654(5) 0.153(3) Uani 1 1 d U . .
H11C H 0.3053 0.4405 0.2409 0.183 Uiso 1 1 calc R . .
H11D H 0.2685 0.4236 0.3128 0.183 Uiso 1 1 calc R . .
C115 C 0.2050(6) 0.8962(6) -0.0483(3) 0.134(3) Uani 1 1 d . . .
H11J H 0.2181 0.9329 -0.0863 0.201 Uiso 1 1 calc R . .
H11E H 0.1841 0.9326 -0.0130 0.201 Uiso 1 1 calc R . .
H11F H 0.1447 0.8293 -0.0664 0.201 Uiso 1 1 calc R . .
C10C C -0.0017(5) 0.9652(5) 0.1086(3) 0.110(2) Uani 1 1 d . . .
H10G H -0.0588 0.9836 0.0848 0.164 Uiso 1 1 calc R . .
H10H H 0.0502 0.9661 0.0790 0.164 Uiso 1 1 calc R . .
H10I H 0.0390 1.0132 0.1523 0.164 Uiso 1 1 calc R . .
C8A C 0.3095(6) 1.2037(4) 0.1172(3) 0.117(2) Uani 1 1 d . . .
H8AA H 0.3261 1.2667 0.1006 0.175 Uiso 1 1 calc R . .
H8AB H 0.2556 1.1954 0.1464 0.175 Uiso 1 1 calc R . .
H8AC H 0.2781 1.1476 0.0775 0.175 Uiso 1 1 calc R . .
C8B C 0.4681(5) 1.2919(4) 0.2250(3) 0.0964(18) Uani 1 1 d . . .
H8BA H 0.4883 1.3563 0.2099 0.145 Uiso 1 1 calc R . .
H8BB H 0.5345 1.2902 0.2528 0.145 Uiso 1 1 calc R . .
H8BC H 0.4127 1.2838 0.2530 0.145 Uiso 1 1 calc R . .
C192 C 0.1535(10) 0.3558(9) 0.2321(6) 0.236(5) Uani 1 1 d U . .
H19A H 0.1662 0.2948 0.2305 0.354 Uiso 1 1 calc R . .
H19B H 0.1321 0.3647 0.1847 0.354 Uiso 1 1 calc R . .
H19C H 0.0937 0.3499 0.2561 0.354 Uiso 1 1 calc R . .
C161 C 0.8204(5) 1.1001(6) 0.2793(4) 0.157(3) Uani 1 1 d . . .
H16C H 0.8806 1.1643 0.2788 0.236 Uiso 1 1 calc R . .
H16D H 0.7970 1.0564 0.2335 0.236 Uiso 1 1 calc R . .
H16E H 0.8467 1.0681 0.3143 0.236 Uiso 1 1 calc R . .
C116 C -0.0086(4) 0.5104(4) 0.0967(3) 0.0861(16) Uani 1 1 d . . .
H11G H 0.0390 0.5288 0.0630 0.103 Uiso 1 1 calc R . .
H11H H -0.0649 0.5380 0.0878 0.103 Uiso 1 1 calc R . .
C7B C 0.1871(5) 0.9132(5) 0.5092(3) 0.115(2) Uani 1 1 d . . .
H7BA H 0.1623 0.9396 0.5474 0.173 Uiso 1 1 calc R . .
H7BB H 0.2287 0.9681 0.4876 0.173 Uiso 1 1 calc R . .
H7BC H 0.2352 0.8817 0.5272 0.173 Uiso 1 1 calc R . .
C8C C 0.5065(6) 1.2169(4) 0.1157(3) 0.113(2) Uani 1 1 d . . .
H8CA H 0.5268 1.2807 0.0998 0.169 Uiso 1 1 calc R . .
H8CB H 0.4748 1.1616 0.0754 0.169 Uiso 1 1 calc R . .
H8CC H 0.5729 1.2154 0.1437 0.169 Uiso 1 1 calc R . .
C117 C -0.0658(6) 0.3999(5) 0.0861(4) 0.149(3) Uani 1 1 d . . .
H11I H -0.1104 0.3729 0.0385 0.224 Uiso 1 1 calc R . .
H11X H -0.1145 0.3814 0.1187 0.224 Uiso 1 1 calc R . .
H11K H -0.0103 0.3722 0.0943 0.224 Uiso 1 1 calc R . .
C7C C 0.0108(5) 0.8860(5) 0.4238(3) 0.0968(18) Uani 1 1 d . . .
H7CA H -0.0162 0.9123 0.4609 0.145 Uiso 1 1 calc R . .
H7CB H -0.0527 0.8373 0.3879 0.145 Uiso 1 1 calc R . .
H7CC H 0.0553 0.9413 0.4035 0.145 Uiso 1 1 calc R . .
C9B C 0.6410(5) 0.7886(6) 0.4174(3) 0.123(3) Uani 1 1 d . . .
H9BA H 0.7118 0.7841 0.4331 0.185 Uiso 1 1 calc R . .
H9BB H 0.5912 0.7606 0.4479 0.185 Uiso 1 1 calc R . .
H9BC H 0.6546 0.8589 0.4188 0.185 Uiso 1 1 calc R . .
C111 C 0.1363(9) 1.1629(8) 0.3639(6) 0.206(4) Uani 1 1 d U . .
H11L H 0.1409 1.2311 0.3691 0.309 Uiso 1 1 calc R . .
H11M H 0.1070 1.1322 0.4017 0.309 Uiso 1 1 calc R . .
H11N H 0.0867 1.1232 0.3193 0.309 Uiso 1 1 calc R . .
C9C C 0.5627(5) 0.6157(5) 0.3380(4) 0.117(2) Uani 1 1 d . . .
H9CA H 0.6328 0.6097 0.3529 0.176 Uiso 1 1 calc R . .
H9CB H 0.5277 0.5796 0.2900 0.176 Uiso 1 1 calc R . .
H9CC H 0.5127 0.5870 0.3682 0.176 Uiso 1 1 calc R . .
C110 C 0.2394(7) 1.1658(6) 0.3663(4) 0.128(2) Uani 1 1 d . . .
H11O H 0.2896 1.2057 0.4115 0.154 Uiso 1 1 calc R . .
H11P H 0.2701 1.1988 0.3291 0.154 Uiso 1 1 calc R . .
C126 C 0.2343(9) 0.5157(9) 0.4829(5) 0.220(5) Uani 1 1 d D . .
H12K H 0.2175 0.5611 0.5151 0.264 Uiso 1 1 calc R . .
H12L H 0.1807 0.4460 0.4805 0.264 Uiso 1 1 calc R . .
C181 C -0.0321(7) 0.5000(7) 0.3572(5) 0.151(3) Uani 1 1 d U . .
H18A H 0.0084 0.5187 0.4064 0.182 Uiso 1 1 calc R . .
H18B H -0.0902 0.5259 0.3527 0.182 Uiso 1 1 calc R . .
C124 C -0.3076(7) 0.5314(7) 0.1571(6) 0.200(5) Uani 1 1 d . . .
H12Y H -0.3862 0.5011 0.1591 0.300 Uiso 1 1 calc R . .
H12W H -0.2984 0.5014 0.1135 0.300 Uiso 1 1 calc R . .
H12X H -0.2831 0.6037 0.1597 0.300 Uiso 1 1 calc R . .
C123 C -0.2481(6) 0.5156(9) 0.2091(6) 0.224(6) Uani 1 1 d . . .
H12Z H -0.2800 0.4423 0.2066 0.269 Uiso 1 1 calc R . .
H12N H -0.2620 0.5452 0.2517 0.269 Uiso 1 1 calc R . .
C182 C -0.0782(9) 0.4024(7) 0.3373(6) 0.236(6) Uani 1 1 d . . .
H18R H -0.1304 0.3725 0.3660 0.353 Uiso 1 1 calc R . .
H18C H -0.0204 0.3772 0.3423 0.353 Uiso 1 1 calc R . .
H18D H -0.1183 0.3845 0.2885 0.353 Uiso 1 1 calc R . .
C127 C 0.3564(10) 0.5274(13) 0.5096(8) 0.366(11) Uani 1 1 d D . .
H12M H 0.3635 0.5077 0.5548 0.550 Uiso 1 1 calc R . .
H12P H 0.4086 0.5974 0.5141 0.550 Uiso 1 1 calc R . .
H12Q H 0.3734 0.4845 0.4764 0.550 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O6 1.797(3) . ?
Ti1 O4 1.934(3) . ?
Ti1 O2 1.979(3) . ?
Ti1 O5 1.988(3) . ?
Ti1 O3 1.993(3) . ?
Ti1 O1 1.997(2) . ?
Ti1 P8 3.0359(14) . ?
Ti1 Ti2 3.1329(12) . ?
Ti1 Ti3 3.1629(13) . ?
Ti2 O10 1.784(3) . ?
Ti2 O8 1.947(3) . ?
Ti2 O7 1.965(3) . ?
Ti2 O9 1.979(3) . ?
Ti2 O1 1.982(2) . ?
Ti2 O3 2.004(3) . ?
Ti3 O14 1.788(3) . ?
Ti3 O11 1.892(3) . ?
Ti3 O12 1.950(3) . ?
Ti3 O1 2.010(2) . ?
Ti3 O13 2.037(3) . ?
Ti3 O2 2.050(3) . ?
Ti4 O11 1.742(3) . ?
Ti4 O20 1.782(3) . ?
Ti4 O17 1.990(3) . ?
Ti4 O16 2.074(3) . ?
Ti4 O15 2.124(3) . ?
Ti4 O19 2.160(3) . ?
Ti4 Ti6 3.2922(16) . ?
Ti4 Ti5 3.3344(13) . ?
Ti5 O23 1.748(3) . ?
Ti5 O21 1.911(3) . ?
Ti5 O22 1.954(3) . ?
Ti5 O16 1.967(3) . ?
Ti5 O18 2.010(3) . ?
Ti5 O15 2.154(2) . ?
Ti5 Ti6 3.2512(13) . ?
Ti6 O26 1.744(3) . ?
Ti6 O19 1.926(3) . ?
Ti6 O25 1.934(3) . ?
Ti6 O24 1.972(3) . ?
Ti6 O18 2.017(3) . ?
Ti6 O15 2.128(2) . ?
P7 O7 1.510(3) . ?
P7 O22 1.531(3) . ?
P7 O24 1.536(3) . ?
P7 C7 1.815(4) . ?
P8 O13 1.515(3) . ?
P8 O5 1.532(3) . ?
P8 O9 1.533(3) . ?
P8 C8 1.806(5) . ?
P9 O4 1.510(3) . ?
P9 O17 1.518(3) . ?
P9 O25 1.531(3) . ?
P9 C9 1.815(4) . ?
P10 O8 1.516(3) . ?
P10 O12 1.514(3) . ?
P10 O21 1.526(3) . ?
P10 C10 1.807(4) . ?
O2 C12 1.429(5) . ?
O16 C116 1.443(5) . ?
O3 C113 1.424(5) . ?
O18 C181 1.506(8) . ?
O19 C119 1.518(8) . ?
O10 C110 1.410(7) . ?
O6 C16 1.410(5) . ?
O20 C120 1.391(7) . ?
O14 C14 1.403(5) . ?
O23 C123 1.365(8) . ?
O26 C126 1.393(9) . ?
C7 C7A 1.515(7) . ?
C7 C7C 1.526(7) . ?
C7 C7B 1.526(7) . ?
C8 C8B 1.520(7) . ?
C8 C8C 1.530(7) . ?
C8 C8A 1.529(7) . ?
C9 C9B 1.512(7) . ?
C9 C9A 1.520(6) . ?
C9 C9C 1.535(7) . ?
C14 C115 1.470(7) . ?
C122 C12 1.444(7) . ?
C16 C161 1.437(8) . ?
C113 C131 1.430(9) . ?
C10A C10 1.534(7) . ?
C121 C120 1.423(8) . ?
C10 C10C 1.521(7) . ?
C10 C10B 1.524(7) . ?
C119 C192 1.284(11) . ?
C116 C117 1.451(7) . ?
C111 C110 1.332(10) . ?
C126 C127 1.5383(11) . ?
C181 C182 1.283(10) . ?
C124 C123 1.275(10) . ?

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
O6 Ti1 O4 91.69(12) . . ?
O6 Ti1 O2 102.50(12) . . ?
O4 Ti1 O2 96.39(11) . . ?
O6 Ti1 O5 85.36(12) . . ?
O4 Ti1 O5 175.17(12) . . ?
O2 Ti1 O5 87.99(11) . . ?
O6 Ti1 O3 105.68(12) . . ?
O4 Ti1 O3 91.40(11) . . ?
O2 Ti1 O3 150.49(10) . . ?
O5 Ti1 O3 85.74(11) . . ?
O6 Ti1 O1 174.92(12) . . ?
O4 Ti1 O1 93.29(11) . . ?
O2 Ti1 O1 75.94(10) . . ?
O5 Ti1 O1 89.74(10) . . ?
O3 Ti1 O1 75.23(10) . . ?
O6 Ti1 P8 111.60(10) . . ?
O4 Ti1 P8 156.61(8) . . ?
O2 Ti1 P8 81.23(8) . . ?
O5 Ti1 P8 26.28(8) . . ?
O3 Ti1 P8 80.46(8) . . ?
O1 Ti1 P8 63.48(7) . . ?
O6 Ti1 Ti2 141.75(10) . . ?
O4 Ti1 Ti2 100.19(8) . . ?
O2 Ti1 Ti2 111.99(7) . . ?
O5 Ti1 Ti2 79.96(8) . . ?
O3 Ti1 Ti2 38.51(7) . . ?
O1 Ti1 Ti2 37.89(7) . . ?
P8 Ti1 Ti2 60.20(3) . . ?
O6 Ti1 Ti3 139.31(10) . . ?
O4 Ti1 Ti3 103.31(9) . . ?
O2 Ti1 Ti3 39.07(7) . . ?
O5 Ti1 Ti3 81.38(8) . . ?
O3 Ti1 Ti3 111.43(8) . . ?
O1 Ti1 Ti3 38.02(7) . . ?
P8 Ti1 Ti3 60.59(3) . . ?
Ti2 Ti1 Ti3 72.92(3) . . ?
O10 Ti2 O8 99.54(12) . . ?
O10 Ti2 O7 92.92(13) . . ?
O8 Ti2 O7 88.90(11) . . ?
O10 Ti2 O9 87.27(13) . . ?
O8 Ti2 O9 90.92(11) . . ?
O7 Ti2 O9 179.76(13) . . ?
O10 Ti2 O1 169.81(12) . . ?
O8 Ti2 O1 87.56(10) . . ?
O7 Ti2 O1 94.53(11) . . ?
O9 Ti2 O1 85.30(11) . . ?
O10 Ti2 O3 98.03(12) . . ?
O8 Ti2 O3 162.27(11) . . ?
O7 Ti2 O3 87.82(11) . . ?
O9 Ti2 O3 92.30(11) . . ?
O1 Ti2 O3 75.34(10) . . ?
O10 Ti2 Ti1 133.42(10) . . ?
O8 Ti2 Ti1 125.47(8) . . ?
O7 Ti2 Ti1 98.69(8) . . ?
O9 Ti2 Ti1 81.29(8) . . ?
O1 Ti2 Ti1 38.24(7) . . ?
O3 Ti2 Ti1 38.28(7) . . ?
O14 Ti3 O11 95.88(12) . . ?
O14 Ti3 O12 99.05(12) . . ?
O11 Ti3 O12 92.11(11) . . ?
O14 Ti3 O1 167.47(12) . . ?
O11 Ti3 O1 94.15(10) . . ?
O12 Ti3 O1 88.05(10) . . ?
O14 Ti3 O13 85.52(12) . . ?
O11 Ti3 O13 178.47(11) . . ?
O12 Ti3 O13 87.05(11) . . ?
O1 Ti3 O13 84.54(10) . . ?
O14 Ti3 O2 98.19(11) . . ?
O11 Ti3 O2 90.95(11) . . ?
O12 Ti3 O2 162.09(11) . . ?
O1 Ti3 O2 74.13(9) . . ?
O13 Ti3 O2 89.46(11) . . ?
O14 Ti3 Ti1 132.30(10) . . ?
O11 Ti3 Ti1 100.15(8) . . ?
O12 Ti3 Ti1 124.65(8) . . ?
O1 Ti3 Ti1 37.74(7) . . ?
O13 Ti3 Ti1 79.30(8) . . ?
O2 Ti3 Ti1 37.49(7) . . ?
O11 Ti4 O20 102.51(14) . . ?
O11 Ti4 O17 94.56(12) . . ?
O20 Ti4 O17 99.19(13) . . ?
O11 Ti4 O16 96.24(12) . . ?
O20 Ti4 O16 96.80(13) . . ?
O17 Ti4 O16 158.28(11) . . ?
O11 Ti4 O15 91.31(11) . . ?
O20 Ti4 O15 163.48(13) . . ?
O17 Ti4 O15 88.54(10) . . ?
O16 Ti4 O15 72.44(10) . . ?
O11 Ti4 O19 162.67(12) . . ?
O20 Ti4 O19 94.65(13) . . ?
O17 Ti4 O19 80.19(11) . . ?
O16 Ti4 O19 83.95(11) . . ?
O15 Ti4 O19 72.16(10) . . ?
O11 Ti4 Ti6 128.76(9) . . ?
O20 Ti4 Ti6 128.60(11) . . ?
O17 Ti4 Ti6 75.90(8) . . ?
O16 Ti4 Ti6 82.65(8) . . ?
O15 Ti4 Ti6 39.32(7) . . ?
O19 Ti4 Ti6 33.97(8) . . ?
O11 Ti4 Ti5 93.78(9) . . ?
O20 Ti4 Ti5 129.43(11) . . ?
O17 Ti4 Ti5 127.10(8) . . ?
O16 Ti4 Ti5 33.36(8) . . ?
O15 Ti4 Ti5 39.11(7) . . ?
O19 Ti4 Ti5 76.82(8) . . ?
Ti6 Ti4 Ti5 58.76(2) . . ?
O23 Ti5 O21 94.33(14) . . ?
O23 Ti5 O22 101.45(14) . . ?
O21 Ti5 O22 88.56(12) . . ?
O23 Ti5 O16 100.59(14) . . ?
O21 Ti5 O16 92.04(12) . . ?
O22 Ti5 O16 157.84(11) . . ?
O23 Ti5 O18 93.80(14) . . ?
O21 Ti5 O18 170.34(12) . . ?
O22 Ti5 O18 84.73(12) . . ?
O16 Ti5 O18 91.57(12) . . ?
O23 Ti5 O15 168.22(14) . . ?
O21 Ti5 O15 96.24(10) . . ?
O22 Ti5 O15 84.02(10) . . ?
O16 Ti5 O15 73.89(10) . . ?
O18 Ti5 O15 76.18(10) . . ?
O23 Ti5 Ti6 130.04(12) . . ?
O21 Ti5 Ti6 135.32(9) . . ?
O22 Ti5 Ti6 78.80(8) . . ?
O16 Ti5 Ti6 85.31(9) . . ?
O18 Ti5 Ti6 36.24(8) . . ?
O15 Ti5 Ti6 40.31(6) . . ?
O23 Ti5 Ti4 135.49(12) . . ?
O21 Ti5 Ti4 93.96(9) . . ?
O22 Ti5 Ti4 122.41(8) . . ?
O16 Ti5 Ti4 35.45(8) . . ?
O18 Ti5 Ti4 83.84(9) . . ?
O15 Ti5 Ti4 38.47(7) . . ?
Ti6 Ti5 Ti4 59.97(3) . . ?
O26 Ti6 O19 101.35(15) . . ?
O26 Ti6 O25 97.88(14) . . ?
O19 Ti6 O25 90.55(13) . . ?
O26 Ti6 O24 97.05(14) . . ?
O19 Ti6 O24 160.00(12) . . ?
O25 Ti6 O24 94.64(12) . . ?
O26 Ti6 O18 98.69(14) . . ?
O19 Ti6 O18 83.62(13) . . ?
O25 Ti6 O18 163.22(11) . . ?
O24 Ti6 O18 85.94(12) . . ?
O26 Ti6 O15 175.07(14) . . ?
O19 Ti6 O15 76.80(11) . . ?
O25 Ti6 O15 86.74(10) . . ?
O24 Ti6 O15 84.22(10) . . ?
O18 Ti6 O15 76.62(10) . . ?
O26 Ti6 Ti5 134.57(12) . . ?
O19 Ti6 Ti5 81.83(9) . . ?
O25 Ti6 Ti5 127.52(8) . . ?
O24 Ti6 Ti5 79.69(8) . . ?
O18 Ti6 Ti5 36.10(8) . . ?
O15 Ti6 Ti5 40.90(7) . . ?
O26 Ti6 Ti4 139.71(12) . . ?
O19 Ti6 Ti4 38.81(8) . . ?
O25 Ti6 Ti4 80.79(8) . . ?
O24 Ti6 Ti4 123.24(8) . . ?
O18 Ti6 Ti4 84.88(9) . . ?
O15 Ti6 Ti4 39.22(7) . . ?
Ti5 Ti6 Ti4 61.27(3) . . ?
O7 P7 O22 111.57(15) . . ?
O7 P7 O24 109.68(15) . . ?
O22 P7 O24 110.44(16) . . ?
O7 P7 C7 109.28(19) . . ?
O22 P7 C7 106.68(19) . . ?
O24 P7 C7 109.12(19) . . ?
O13 P8 O5 110.00(16) . . ?
O13 P8 O9 113.11(16) . . ?
O5 P8 O9 109.74(16) . . ?
O13 P8 C8 108.3(2) . . ?
O5 P8 C8 108.3(2) . . ?
O9 P8 C8 107.3(2) . . ?
O13 P8 Ti1 91.56(11) . . ?
O5 P8 Ti1 35.08(10) . . ?
O9 P8 Ti1 91.75(11) . . ?
C8 P8 Ti1 143.34(18) . . ?
O4 P9 O17 111.65(15) . . ?
O4 P9 O25 109.88(16) . . ?
O17 P9 O25 111.24(16) . . ?
O4 P9 C9 107.6(2) . . ?
O17 P9 C9 108.8(2) . . ?
O25 P9 C9 107.50(18) . . ?
O8 P10 O12 113.66(15) . . ?
O8 P10 O21 110.71(16) . . ?
O12 P10 O21 109.25(16) . . ?
O8 P10 C10 106.89(19) . . ?
O12 P10 C10 107.59(19) . . ?
O21 P10 C10 108.6(2) . . ?
Ti2 O1 Ti1 103.86(11) . . ?
Ti2 O1 Ti3 139.19(12) . . ?
Ti1 O1 Ti3 104.24(11) . . ?
Ti4 O15 Ti6 101.47(11) . . ?
Ti4 O15 Ti5 102.42(10) . . ?
Ti6 O15 Ti5 98.79(10) . . ?
C12 O2 Ti1 126.3(3) . . ?
C12 O2 Ti3 124.8(3) . . ?
Ti1 O2 Ti3 103.43(11) . . ?
C116 O16 Ti5 122.3(3) . . ?
C116 O16 Ti4 120.0(3) . . ?
Ti5 O16 Ti4 111.19(12) . . ?
C113 O3 Ti1 127.5(3) . . ?
C113 O3 Ti2 128.4(3) . . ?
Ti1 O3 Ti2 103.22(11) . . ?
P9 O17 Ti4 132.13(16) . . ?
P7 O7 Ti2 152.36(16) . . ?
P10 O8 Ti2 138.20(16) . . ?
P9 O4 Ti1 149.79(18) . . ?
Ti4 O11 Ti3 153.57(15) . . ?
C181 O18 Ti6 121.0(4) . . ?
C181 O18 Ti5 120.4(4) . . ?
Ti6 O18 Ti5 107.66(12) . . ?
P10 O21 Ti5 146.02(17) . . ?
C119 O19 Ti6 128.3(4) . . ?
C119 O19 Ti4 122.4(4) . . ?
Ti6 O19 Ti4 107.22(13) . . ?
P10 O12 Ti3 136.22(16) . . ?
P7 O24 Ti6 127.16(16) . . ?
P8 O9 Ti2 123.08(16) . . ?
P7 O22 Ti5 128.60(16) . . ?
P8 O13 Ti3 122.86(15) . . ?
C110 O10 Ti2 142.2(4) . . ?
P8 O5 Ti1 118.64(15) . . ?
C16 O6 Ti1 141.6(3) . . ?
P9 O25 Ti6 131.53(16) . . ?
C120 O20 Ti4 141.1(4) . . ?
C14 O14 Ti3 141.7(3) . . ?
C123 O23 Ti5 162.3(6) . . ?
C126 O26 Ti6 158.3(6) . . ?
C7A C7 C7C 109.9(5) . . ?
C7A C7 C7B 111.9(5) . . ?
C7C C7 C7B 108.9(5) . . ?
C7A C7 P7 109.1(4) . . ?
C7C C7 P7 108.4(3) . . ?
C7B C7 P7 108.5(3) . . ?
C8B C8 C8C 110.1(5) . . ?
C8B C8 C8A 110.4(5) . . ?
C8C C8 C8A 111.3(5) . . ?
C8B C8 P8 108.8(3) . . ?
C8C C8 P8 108.6(4) . . ?
C8A C8 P8 107.5(4) . . ?
C9B C9 C9A 109.9(5) . . ?
C9B C9 C9C 111.2(5) . . ?
C9A C9 C9C 109.9(5) . . ?
C9B C9 P9 108.4(3) . . ?
C9A C9 P9 108.7(3) . . ?
C9C C9 P9 108.8(4) . . ?
O14 C14 C115 112.1(5) . . ?
O6 C16 C161 113.2(5) . . ?
O2 C12 C122 113.3(5) . . ?
O3 C113 C131 112.7(6) . . ?
C10C C10 C10A 110.3(5) . . ?
C10C C10 C10B 110.5(5) . . ?
C10A C10 C10B 110.4(4) . . ?
C10C C10 P10 107.6(3) . . ?
C10A C10 P10 108.8(3) . . ?
C10B C10 P10 109.1(3) . . ?
C121 C120 O20 114.3(6) . . ?
C192 C119 O19 108.5(8) . . ?
O16 C116 C117 111.9(5) . . ?
C111 C110 O10 110.7(8) . . ?
C127 C126 O26 108.1(8) . . ?
C182 C181 O18 108.8(9) . . ?
C124 C123 O23 123.5(9) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        24.15
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.851
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.059
