# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Steven Bull'
_publ_contact_author_email       S.D.BULL@BATH.AC.UK

_publ_section_title              
;
An enantiopure pseudo-C3-symmetric titanium
triflate with propeller-like chirality as a catalyst for
asymmetric sulfoxidation reactions
;
loop_
_publ_author_name
'Steven Bull'
'Philip Axe'
'Matthew G. Davidson'
'Matthew D. Jones'
'William L. Mitchell'
;
D.E.J.E.Robinson
;
'John E Warren'

# Attachment 'triflate_5.cif'

data_bath622
_database_code_depnum_ccdc_archive 'CCDC 737968'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C50.50 H72 F3 N O6 S Ti'
_chemical_formula_weight         926.05

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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           Tetragonal
_symmetry_space_group_name_H-M   P4(3)

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x, z+3/4'
'-x, -y, z+1/2'
'y, -x, z+1/4'

_cell_length_a                   14.7440(7)
_cell_length_b                   14.7440(7)
_cell_length_c                   25.1710(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5471.8(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    6231
_cell_measurement_theta_min      2.70
_cell_measurement_theta_max      18.82

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.124
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1980
_exptl_absorpt_coefficient_mu    0.248
_exptl_absorpt_correction_type   'Multi scans'
_exptl_absorpt_correction_T_min  0.687
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'SADABS (Bruker, 2003)'

_exptl_special_details           
;
The structure exhibited severe disorder both in the complex
and in the toluene solvent molecule. The coordination sphere of the metal
and three of the carbon atoms in the arene ring and the oxygen of the phenoxide
in the arene ring are disordered over two positions
around the 3-fold molecular axis. Each of the two parts was refined
independently using PART 1 and PART 2 with the occupcies summed to unity.
The toluene was refined with half occupancy but some small residual
peaks were still observed in the electron density difference
map.
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.69420
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_source         'Station 9.8, Daresbury Laboratory'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_measurement_device_type  'APEX II Bruker diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            46969
_diffrn_reflns_av_R_equivalents  0.0797
_diffrn_reflns_av_sigmaI/netI    0.0695
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         5.70
_diffrn_reflns_theta_max         25.74
_reflns_number_total             11035
_reflns_number_gt                7734
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1348P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.020(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(13)
_refine_ls_number_reflns         11035
_refine_ls_number_parameters     801
_refine_ls_number_restraints     39
_refine_ls_R_factor_all          0.1026
_refine_ls_R_factor_gt           0.0675
_refine_ls_wR_factor_ref         0.2007
_refine_ls_wR_factor_gt          0.1750
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_restrained_S_all      3.939
_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 0.76545(17) 0.25451(19) 0.0058(18) 0.0424(9) Uani 1 1 d . . .
S1 S 0.6173(15) 0.2169(19) -0.0924(19) 0.061(6) Uani 0.62(7) 1 d P A 1
S1A S 0.625(2) 0.174(5) -0.090(3) 0.092(11) Uani 0.38(7) 1 d P A 2
F1 F 0.4690(11) 0.224(2) -0.045(2) 0.205(15) Uani 1 1 d . A .
O1 O 0.7455(13) 0.1616(12) 0.051(2) 0.048(4) Uani 0.73(2) 1 d P B 1
O1A O 0.785(3) 0.143(3) 0.029(3) 0.042(11) Uani 0.27(2) 1 d P B 2
N1 N 0.8786(8) 0.2907(9) 0.0606(19) 0.043(3) Uani 1 1 d . B .
C1 C 0.8592(18) 0.2584(19) 0.115(2) 0.043(6) Uani 0.73(2) 1 d P B 1
H1A H 0.8013 0.2856 0.1266 0.051 Uiso 0.73(2) 1 calc PR B 1
H1B H 0.9076 0.2803 0.1386 0.051 Uiso 0.73(2) 1 calc PR B 1
C11A C 0.822(6) 0.091(5) 0.069(4) 0.045(17) Uani 0.27(2) 1 d P B 2
C1A C 0.947(4) 0.209(4) 0.067(4) 0.053(18) Uani 0.27(2) 1 d P B 2
H1A1 H 0.9735 0.1963 0.0316 0.064 Uiso 0.27(2) 1 calc PR B 2
H1A2 H 0.9969 0.2291 0.0904 0.064 Uiso 0.27(2) 1 calc PR B 2
F2 F 0.4595(11) 0.1484(16) -0.114(2) 0.141(8) Uani 1 1 d . A .
O2 O 0.8508(12) 0.2512(15) -0.045(2) 0.044(4) Uani 0.73(2) 1 d P B 1
O2A O 0.843(4) 0.303(5) -0.043(3) 0.053(14) Uani 0.27(2) 1 d P B 2
C2 C 0.9631(16) 0.2458(18) 0.041(2) 0.046(5) Uani 0.73(2) 1 d P B 1
H2A H 1.0120 0.2558 0.0669 0.055 Uiso 0.73(2) 1 calc PR B 1
H2B H 0.9521 0.1797 0.0387 0.055 Uiso 0.73(2) 1 calc PR B 1
C2A C 0.936(6) 0.368(5) 0.045(4) 0.06(2) Uani 0.27(2) 1 d P B 2
H2A1 H 0.9835 0.3782 0.0725 0.072 Uiso 0.27(2) 1 calc PR B 2
H2A2 H 0.8986 0.4240 0.0430 0.072 Uiso 0.27(2) 1 calc PR B 2
F3 F 0.5203(13) 0.0902(17) -0.048(2) 0.138(7) Uani 1 1 d . A .
O3 O 0.7172(12) 0.3619(14) 0.022(2) 0.046(4) Uani 0.73(2) 1 d P B 1
O3A O 0.704(3) 0.329(3) 0.049(4) 0.048(13) Uani 0.27(2) 1 d P B 2
C3 C 0.8879(18) 0.3938(16) 0.059(2) 0.045(5) Uani 0.73(2) 1 d P B 1
H3 H 0.8878 0.4111 0.0202 0.055 Uiso 0.73(2) 1 calc PR B 1
C3A C 0.847(3) 0.308(6) 0.119(2) 0.046(17) Uani 0.27(2) 1 d PD B 2
H3A H 0.9015 0.3225 0.1406 0.056 Uiso 0.27(2) 1 calc PR B 2
O4 O 0.6623(9) 0.2202(10) -0.0417(19) 0.065(3) Uani 1 1 d . A .
C4 C 0.9783(15) 0.4297(17) 0.082(2) 0.057(6) Uani 0.73(2) 1 d P B 1
H4A H 0.9736 0.4952 0.0884 0.086 Uiso 0.73(2) 1 calc PR B 1
H4B H 1.0281 0.4174 0.0577 0.086 Uiso 0.73(2) 1 calc PR B 1
H4C H 0.9903 0.3990 0.1163 0.086 Uiso 0.73(2) 1 calc PR B 1
C4A C 0.796(8) 0.229(7) 0.145(3) 0.18(9) Uani 0.27(2) 1 d PD B 2
H4A1 H 0.7313 0.2425 0.1465 0.272 Uiso 0.27(2) 1 calc PR B 2
H4A2 H 0.8198 0.2189 0.1807 0.272 Uiso 0.27(2) 1 calc PR B 2
H4A3 H 0.8054 0.1736 0.1235 0.272 Uiso 0.27(2) 1 calc PR B 2
O5 O 0.654(3) 0.155(5) -0.130(3) 0.14(3) Uani 0.62(7) 1 d P A 1
O5A O 0.671(5) 0.108(6) -0.100(4) 0.13(3) Uani 0.38(7) 1 d P A 2
C5 C 0.5090(16) 0.164(2) -0.073(2) 0.089(8) Uani 1 1 d . . .
O6 O 0.589(4) 0.307(3) -0.109(3) 0.16(3) Uani 0.62(7) 1 d P A 1
O6A O 0.623(4) 0.253(6) -0.136(3) 0.11(2) Uani 0.38(7) 1 d P A 2
C11 C 0.788(2) 0.112(2) 0.089(2) 0.049(7) Uani 0.73(2) 1 d P B 1
C12 C 0.8525(15) 0.1584(15) 0.119(2) 0.045(5) Uani 0.73(2) 1 d P B 1
C12A C 0.908(4) 0.123(5) 0.089(3) 0.047(15) Uani 0.27(2) 1 d P B 2
C13 C 0.9095(16) 0.1081(16) 0.154(2) 0.048(6) Uani 0.73(2) 1 d P B 1
H13 H 0.9533 0.1391 0.1745 0.058 Uiso 0.73(2) 1 calc PR B 1
C13A C 0.952(5) 0.072(4) 0.125(4) 0.052(16) Uani 0.27(2) 1 d P B 2
H13A H 1.0158 0.0769 0.1291 0.063 Uiso 0.27(2) 1 calc PR B 2
C14 C 0.9027(13) 0.0124(15) 0.158(2) 0.072(6) Uani 1 1 d . . .
C15 C 0.8303(13) -0.0273(13) 0.130(2) 0.059(4) Uani 1 1 d . B .
H15 H 0.8171 -0.0891 0.1379 0.071 Uiso 1 1 calc R . .
C16 C 0.7761(13) 0.0169(13) 0.093(2) 0.060(5) Uani 1 1 d . . .
C17 C 0.9620(16) -0.0430(16) 0.195(2) 0.076(6) Uani 1 1 d . B .
C18 C 0.6948(13) -0.0270(14) 0.065(2) 0.063(5) Uani 1 1 d . B .
C21 C 0.938(2) 0.276(2) -0.056(2) 0.044(7) Uani 0.73(2) 1 d P B 1
C21A C 0.933(5) 0.322(8) -0.052(4) 0.05(2) Uani 0.27(2) 1 d P B 2
C22 C 0.9956(15) 0.2770(16) -0.012(2) 0.046(5) Uani 0.73(2) 1 d P B 1
C22A C 0.980(5) 0.349(6) -0.009(3) 0.07(2) Uani 0.27(2) 1 d P B 2
C23 C 1.0877(15) 0.3038(19) -0.019(2) 0.048(5) Uani 0.73(2) 1 d P B 1
H23 H 1.1278 0.3021 0.0103 0.057 Uiso 0.73(2) 1 calc PR B 1
C23A C 1.074(5) 0.371(7) -0.012(3) 0.06(2) Uani 0.27(2) 1 d P B 2
H23A H 1.1059 0.4040 0.0142 0.076 Uiso 0.27(2) 1 calc PR B 2
C24 C 1.1205(13) 0.3322(16) -0.068(2) 0.068(5) Uani 1 1 d . . .
C25 C 1.0596(12) 0.3284(13) -0.110(2) 0.056(4) Uani 1 1 d . B .
H25 H 1.0822 0.3428 -0.1442 0.068 Uiso 1 1 calc R . .
C26 C 0.9688(12) 0.3053(13) -0.106(2) 0.054(4) Uani 1 1 d . . .
C27 C 1.2192(14) 0.3587(18) -0.076(2) 0.078(7) Uani 1 1 d . B .
C28 C 0.9073(12) 0.2978(12) -0.154(2) 0.053(4) Uani 1 1 d . B .
C31 C 0.7209(16) 0.4225(16) 0.064(2) 0.042(5) Uani 0.73(2) 1 d P B 1
C31A C 0.709(5) 0.392(6) 0.090(4) 0.049(17) Uani 0.27(2) 1 d P B 2
C32 C 0.8070(14) 0.4399(14) 0.084(2) 0.041(5) Uani 0.73(2) 1 d P B 1
C32A C 0.784(4) 0.390(4) 0.120(3) 0.044(14) Uani 0.27(2) 1 d P B 2
C33 C 0.8144(16) 0.4987(15) 0.127(2) 0.045(5) Uani 0.73(2) 1 d P B 1
H33 H 0.8732 0.5116 0.1403 0.053 Uiso 0.73(2) 1 calc PR B 1
C33A C 0.801(5) 0.462(6) 0.156(4) 0.058(19) Uani 0.27(2) 1 d P B 2
H33A H 0.8498 0.4609 0.1805 0.070 Uiso 0.27(2) 1 calc PR B 2
C34 C 0.7391(12) 0.5400(12) 0.152(2) 0.059(4) Uani 1 1 d . . .
C35 C 0.6559(12) 0.5256(11) 0.127(2) 0.049(4) Uani 1 1 d . B .
H35 H 0.6054 0.5596 0.1390 0.059 Uiso 1 1 calc R . .
C36 C 0.6414(12) 0.4649(11) 0.085(2) 0.053(4) Uani 1 1 d . . .
C37 C 0.7501(14) 0.6059(13) 0.197(2) 0.063(5) Uani 1 1 d . B .
C38 C 0.5496(11) 0.4509(12) 0.059(2) 0.051(4) Uani 1 1 d . B .
C41 C 1.004(5) -0.122(5) 0.166(3) 0.13(3) Uani 0.61(7) 1 d PU B 1
H41A H 1.0451 -0.1541 0.1903 0.190 Uiso 0.61(7) 1 calc PR B 1
H41B H 1.0376 -0.1001 0.1353 0.190 Uiso 0.61(7) 1 calc PR B 1
H41C H 0.9559 -0.1636 0.1545 0.190 Uiso 0.61(7) 1 calc PR B 1
C41A C 0.925(7) -0.129(7) 0.214(6) 0.12(4) Uani 0.39(7) 1 d PU B 2
H41D H 0.8900 -0.1580 0.1852 0.186 Uiso 0.39(7) 1 calc PR B 2
H41E H 0.8854 -0.1183 0.2443 0.186 Uiso 0.39(7) 1 calc PR B 2
H41F H 0.9748 -0.1694 0.2243 0.186 Uiso 0.39(7) 1 calc PR B 2
C42 C 0.901(3) -0.082(4) 0.241(3) 0.083(14) Uani 0.61(7) 1 d PU B 1
H42A H 0.8520 -0.1192 0.2260 0.125 Uiso 0.61(7) 1 calc PR B 1
H42B H 0.8743 -0.0318 0.2614 0.125 Uiso 0.61(7) 1 calc PR B 1
H42C H 0.9379 -0.1196 0.2648 0.125 Uiso 0.61(7) 1 calc PR B 1
C42A C 0.955(13) 0.018(8) 0.255(6) 0.18(6) Uani 0.39(7) 1 d PU B 2
H42D H 0.8912 0.0264 0.2650 0.277 Uiso 0.39(7) 1 calc PR B 2
H42E H 0.9845 0.0768 0.2513 0.277 Uiso 0.39(7) 1 calc PR B 2
H42F H 0.9857 -0.0167 0.2835 0.277 Uiso 0.39(7) 1 calc PR B 2
C43 C 1.033(5) 0.013(4) 0.221(4) 0.13(3) Uani 0.61(7) 1 d PU B 1
H43A H 1.0039 0.0588 0.2439 0.200 Uiso 0.61(7) 1 calc PR B 1
H43B H 1.0700 0.0433 0.1943 0.200 Uiso 0.61(7) 1 calc PR B 1
H43C H 1.0716 -0.0260 0.2433 0.200 Uiso 0.61(7) 1 calc PR B 1
C43A C 1.062(6) -0.046(14) 0.164(6) 0.18(6) Uani 0.39(7) 1 d PU B 2
H43D H 1.0982 -0.0961 0.1779 0.276 Uiso 0.39(7) 1 calc PR B 2
H43E H 1.0935 0.0112 0.1688 0.276 Uiso 0.39(7) 1 calc PR B 2
H43F H 1.0514 -0.0562 0.1255 0.276 Uiso 0.39(7) 1 calc PR B 2
C44 C 0.6789(19) -0.1238(17) 0.087(2) 0.091(8) Uani 1 1 d . . .
H44A H 0.6665 -0.1208 0.1251 0.136 Uiso 1 1 calc R B .
H44B H 0.7331 -0.1608 0.0807 0.136 Uiso 1 1 calc R . .
H44C H 0.6270 -0.1513 0.0687 0.136 Uiso 1 1 calc R . .
C45 C 0.6088(16) 0.025(2) 0.075(2) 0.093(7) Uani 1 1 d . . .
H45A H 0.6167 0.0877 0.0629 0.140 Uiso 1 1 calc R B .
H45B H 0.5946 0.0242 0.1128 0.140 Uiso 1 1 calc R . .
H45C H 0.5591 -0.0033 0.0549 0.140 Uiso 1 1 calc R . .
C46 C 0.7132(16) -0.0371(14) 0.006(2) 0.074(5) Uani 1 1 d . . .
H46A H 0.6612 -0.0665 -0.0113 0.111 Uiso 1 1 calc R B .
H46B H 0.7676 -0.0741 0.0004 0.111 Uiso 1 1 calc R . .
H46C H 0.7225 0.0230 -0.0100 0.111 Uiso 1 1 calc R . .
C47 C 1.2735(16) 0.354(3) -0.026(2) 0.133(14) Uani 1 1 d . . .
H47A H 1.2605 0.2964 -0.0077 0.199 Uiso 1 1 calc R B .
H47B H 1.2571 0.4046 -0.0027 0.199 Uiso 1 1 calc R . .
H47C H 1.3383 0.3569 -0.0344 0.199 Uiso 1 1 calc R . .
C48 C 1.2634(18) 0.295(2) -0.115(2) 0.099(8) Uani 1 1 d . . .
H48A H 1.3211 0.3205 -0.1274 0.148 Uiso 1 1 calc R B .
H48B H 1.2232 0.2858 -0.1459 0.148 Uiso 1 1 calc R . .
H48C H 1.2746 0.2362 -0.0980 0.148 Uiso 1 1 calc R . .
C49 C 1.2206(17) 0.4557(18) -0.101(2) 0.092(8) Uani 1 1 d . . .
H49A H 1.1887 0.4981 -0.0779 0.139 Uiso 1 1 calc R B .
H49B H 1.1904 0.4542 -0.1361 0.139 Uiso 1 1 calc R . .
H49C H 1.2835 0.4756 -0.1059 0.139 Uiso 1 1 calc R . .
C50 C 0.9586(15) 0.3220(15) -0.206(2) 0.066(5) Uani 1 1 d . . .
H50A H 0.9785 0.3854 -0.2044 0.098 Uiso 1 1 calc R B .
H50B H 0.9182 0.3136 -0.2365 0.098 Uiso 1 1 calc R . .
H50C H 1.0116 0.2824 -0.2097 0.098 Uiso 1 1 calc R . .
C51 C 0.8720(14) 0.2006(13) -0.161(2) 0.067(5) Uani 1 1 d . . .
H51A H 0.9233 0.1592 -0.1658 0.101 Uiso 1 1 calc R B .
H51B H 0.8319 0.1975 -0.1917 0.101 Uiso 1 1 calc R . .
H51C H 0.8382 0.1830 -0.1288 0.101 Uiso 1 1 calc R . .
C52 C 0.8271(13) 0.3631(14) -0.150(2) 0.063(5) Uani 1 1 d . . .
H52A H 0.7927 0.3498 -0.1176 0.094 Uiso 1 1 calc R B .
H52B H 0.7876 0.3558 -0.1810 0.094 Uiso 1 1 calc R . .
H52C H 0.8495 0.4256 -0.1486 0.094 Uiso 1 1 calc R . .
C53 C 0.779(4) 0.544(3) 0.246(2) 0.099(16) Uani 0.62(5) 1 d P B 1
H53A H 0.7682 0.5774 0.2794 0.148 Uiso 0.62(5) 1 calc PR B 1
H53B H 0.8433 0.5290 0.2433 0.148 Uiso 0.62(5) 1 calc PR B 1
H53C H 0.7426 0.4886 0.2461 0.148 Uiso 0.62(5) 1 calc PR B 1
C53A C 0.842(4) 0.614(4) 0.222(3) 0.070(18) Uani 0.38(5) 1 d P B 2
H53D H 0.8431 0.6663 0.2456 0.106 Uiso 0.38(5) 1 calc PR B 2
H53E H 0.8870 0.6221 0.1935 0.106 Uiso 0.38(5) 1 calc PR B 2
H53F H 0.8555 0.5586 0.2417 0.106 Uiso 0.38(5) 1 calc PR B 2
C54 C 0.827(4) 0.673(3) 0.185(3) 0.12(2) Uani 0.62(5) 1 d P B 1
H54A H 0.8093 0.7102 0.1541 0.177 Uiso 0.62(5) 1 calc PR B 1
H54B H 0.8821 0.6391 0.1762 0.177 Uiso 0.62(5) 1 calc PR B 1
H54C H 0.8377 0.7119 0.2155 0.177 Uiso 0.62(5) 1 calc PR B 1
C54A C 0.727(4) 0.705(4) 0.174(3) 0.071(19) Uani 0.38(5) 1 d P B 2
H54D H 0.6612 0.7107 0.1690 0.107 Uiso 0.38(5) 1 calc PR B 2
H54E H 0.7572 0.7125 0.1393 0.107 Uiso 0.38(5) 1 calc PR B 2
H54F H 0.7483 0.7517 0.1984 0.107 Uiso 0.38(5) 1 calc PR B 2
C55 C 0.667(4) 0.653(4) 0.212(3) 0.10(2) Uani 0.62(5) 1 d P B 1
H55A H 0.6797 0.6987 0.2393 0.154 Uiso 0.62(5) 1 calc PR B 1
H55B H 0.6223 0.6096 0.2256 0.154 Uiso 0.62(5) 1 calc PR B 1
H55C H 0.6416 0.6835 0.1804 0.154 Uiso 0.62(5) 1 calc PR B 1
C55A C 0.678(6) 0.589(9) 0.241(4) 0.11(4) Uani 0.38(5) 1 d P B 2
H55D H 0.6620 0.6470 0.2576 0.172 Uiso 0.38(5) 1 calc PR B 2
H55E H 0.7034 0.5482 0.2679 0.172 Uiso 0.38(5) 1 calc PR B 2
H55F H 0.6244 0.5617 0.2250 0.172 Uiso 0.38(5) 1 calc PR B 2
C56 C 0.5538(13) 0.4672(15) 0.000(2) 0.067(5) Uani 1 1 d . . .
H56A H 0.5796 0.5273 -0.0073 0.100 Uiso 1 1 calc R B .
H56B H 0.4925 0.4640 -0.0152 0.100 Uiso 1 1 calc R . .
H56C H 0.5920 0.4207 -0.0169 0.100 Uiso 1 1 calc R . .
C57 C 0.5176(15) 0.3541(15) 0.071(2) 0.073(6) Uani 1 1 d . . .
H57A H 0.5535 0.3114 0.0493 0.110 Uiso 1 1 calc R B .
H57B H 0.4534 0.3484 0.0609 0.110 Uiso 1 1 calc R . .
H57C H 0.5253 0.3404 0.1083 0.110 Uiso 1 1 calc R . .
C58 C 0.4777(13) 0.5144(18) 0.083(2) 0.076(6) Uani 1 1 d . . .
H58A H 0.4709 0.5014 0.1213 0.114 Uiso 1 1 calc R B .
H58B H 0.4196 0.5048 0.0653 0.114 Uiso 1 1 calc R . .
H58C H 0.4969 0.5776 0.0787 0.114 Uiso 1 1 calc R . .
C61 C 0.898(3) 0.591(3) -0.029(3) 0.16(3) Uiso 0.50 1 d PGD . .
C62 C 0.989(4) 0.564(3) -0.030(3) 0.15(3) Uiso 0.50 1 d PG . .
H62 H 1.0074 0.5165 -0.0530 0.181 Uiso 0.50 1 calc PR . .
C63 C 1.052(3) 0.607(4) 0.003(3) 0.17(3) Uiso 0.50 1 d PG . .
H63 H 1.1134 0.5885 0.0019 0.203 Uiso 0.50 1 calc PR . .
C64 C 1.024(3) 0.676(3) 0.036(3) 0.109(18) Uiso 0.50 1 d PG . .
H64 H 1.0672 0.7054 0.0586 0.131 Uiso 0.50 1 calc PR . .
C65 C 0.934(4) 0.703(3) 0.037(3) 0.18(4) Uiso 0.50 1 d PG . .
H65 H 0.9150 0.7503 0.0605 0.215 Uiso 0.50 1 calc PR . .
C66 C 0.871(3) 0.660(4) 0.005(3) 0.14(2) Uiso 0.50 1 d PG . .
H66 H 0.8090 0.6783 0.0057 0.171 Uiso 0.50 1 calc PR . .
C67 C 0.810(4) 0.561(6) -0.049(4) 0.23(6) Uiso 0.50 1 d PGD . .
H67A H 0.7633 0.6038 -0.0376 0.344 Uiso 0.50 1 calc PR . .
H67B H 0.7966 0.5005 -0.0360 0.344 Uiso 0.50 1 calc PR . .
H67C H 0.8124 0.5603 -0.0883 0.344 Uiso 0.50 1 calc PR . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ti1 0.0401(14) 0.0485(16) 0.0386(14) -0.0025(11) -0.0040(13) 0.0020(12)
S1 0.073(8) 0.069(10) 0.042(6) -0.004(6) -0.014(5) -0.013(7)
S1A 0.067(11) 0.10(3) 0.11(2) -0.048(18) -0.041(11) 0.023(15)
F1 0.065(9) 0.28(3) 0.27(3) -0.19(3) -0.022(13) 0.042(13)
O1 0.046(10) 0.052(10) 0.047(11) 0.004(8) -0.004(8) -0.005(8)
O1A 0.04(3) 0.04(2) 0.05(3) 0.00(2) -0.02(2) 0.004(18)
N1 0.040(7) 0.047(7) 0.044(7) 0.000(6) -0.001(6) -0.001(5)
C1 0.047(13) 0.043(13) 0.038(12) 0.004(11) -0.007(9) -0.005(12)
C11A 0.05(4) 0.05(4) 0.04(4) 0.00(3) -0.02(3) -0.01(3)
C1A 0.04(3) 0.03(3) 0.09(6) 0.00(3) -0.01(3) -0.01(3)
F2 0.085(10) 0.20(2) 0.140(15) -0.065(14) -0.056(11) 0.003(11)
O2 0.044(9) 0.051(11) 0.038(9) 0.000(9) -0.004(6) 0.000(9)
O2A 0.06(3) 0.06(3) 0.04(3) 0.01(3) -0.02(2) -0.02(3)
C2 0.046(12) 0.045(13) 0.048(14) 0.000(11) -0.003(10) 0.006(10)
C2A 0.07(5) 0.06(4) 0.06(5) 0.03(3) 0.00(4) 0.00(4)
F3 0.096(11) 0.165(18) 0.153(18) 0.036(15) -0.017(12) -0.039(12)
O3 0.043(9) 0.049(11) 0.046(11) -0.005(8) -0.008(7) 0.005(7)
O3A 0.03(2) 0.04(3) 0.08(4) -0.02(3) -0.01(2) 0.004(19)
C3 0.046(13) 0.046(13) 0.045(13) 0.002(10) -0.009(11) -0.005(11)
C3A 0.03(3) 0.06(5) 0.04(4) 0.01(4) -0.01(3) -0.01(3)
O4 0.055(7) 0.090(9) 0.048(8) -0.008(7) -0.011(6) -0.002(7)
C4 0.043(12) 0.059(14) 0.070(16) -0.002(12) -0.007(11) -0.006(10)
C4A 0.10(10) 0.3(2) 0.18(17) -0.11(16) -0.07(11) 0.06(12)
O5 0.10(3) 0.25(7) 0.08(3) -0.12(4) 0.05(2) -0.08(4)
O5A 0.12(5) 0.19(7) 0.07(4) -0.02(4) 0.00(3) 0.10(5)
C5 0.062(13) 0.12(2) 0.086(18) -0.036(16) -0.008(12) 0.009(14)
O6 0.21(5) 0.09(3) 0.18(5) 0.04(3) -0.12(5) -0.01(3)
O6A 0.13(5) 0.12(6) 0.07(4) -0.01(4) -0.04(3) 0.01(4)
C11 0.048(15) 0.057(16) 0.043(17) 0.001(12) 0.002(12) -0.001(12)
C12 0.053(12) 0.045(11) 0.037(11) 0.000(9) -0.007(9) -0.006(9)
C12A 0.03(3) 0.07(4) 0.04(3) 0.00(3) 0.01(2) -0.01(3)
C13 0.051(13) 0.048(12) 0.045(13) 0.007(10) -0.009(10) -0.005(10)
C13A 0.05(4) 0.04(3) 0.07(4) 0.01(3) 0.00(3) 0.00(3)
C14 0.058(11) 0.074(13) 0.083(14) 0.029(11) -0.018(10) -0.022(10)
C15 0.057(10) 0.051(10) 0.070(12) 0.011(9) -0.001(9) -0.009(8)
C16 0.058(10) 0.058(10) 0.066(12) 0.011(9) -0.010(9) -0.009(8)
C17 0.076(13) 0.079(14) 0.074(14) 0.024(11) -0.020(11) -0.006(11)
C18 0.053(10) 0.071(12) 0.065(12) 0.005(9) -0.001(9) -0.018(9)
C21 0.040(13) 0.041(14) 0.050(15) -0.004(13) -0.005(10) 0.006(13)
C21A 0.03(3) 0.08(6) 0.04(4) -0.01(5) -0.01(3) -0.01(5)
C22 0.050(12) 0.043(12) 0.045(12) -0.005(9) -0.006(9) 0.011(10)
C22A 0.07(5) 0.09(6) 0.05(4) 0.02(4) 0.00(3) 0.00(4)
C23 0.040(11) 0.054(14) 0.049(13) 0.006(11) -0.008(9) 0.003(10)
C23A 0.06(4) 0.09(6) 0.04(4) 0.02(4) -0.01(3) -0.02(4)
C24 0.052(10) 0.090(14) 0.062(12) 0.017(10) -0.007(9) 0.001(9)
C25 0.050(9) 0.064(11) 0.055(10) 0.015(8) 0.005(8) 0.010(8)
C26 0.050(9) 0.063(10) 0.047(10) 0.007(8) -0.002(7) 0.009(8)
C27 0.051(10) 0.108(17) 0.075(14) 0.031(13) -0.002(10) -0.002(11)
C28 0.060(10) 0.060(10) 0.039(9) 0.000(7) -0.001(7) 0.012(8)
C31 0.052(13) 0.043(13) 0.032(13) 0.000(10) -0.004(11) 0.000(10)
C31A 0.06(4) 0.06(4) 0.03(4) -0.01(3) -0.01(3) 0.01(3)
C32 0.042(11) 0.040(10) 0.042(12) 0.007(9) -0.004(9) 0.003(8)
C32A 0.04(3) 0.05(3) 0.04(3) 0.00(3) 0.00(2) 0.01(2)
C33 0.051(12) 0.039(11) 0.044(13) 0.006(10) -0.006(10) -0.006(9)
C33A 0.06(4) 0.08(5) 0.04(4) -0.02(4) 0.00(3) -0.02(3)
C34 0.055(10) 0.046(9) 0.074(13) -0.014(8) -0.010(9) 0.002(8)
C35 0.053(9) 0.041(8) 0.053(10) -0.004(7) 0.001(7) -0.002(7)
C36 0.054(10) 0.042(8) 0.063(11) -0.004(8) -0.005(8) -0.004(7)
C37 0.075(12) 0.060(11) 0.055(11) -0.011(9) -0.009(9) -0.004(9)
C38 0.044(8) 0.058(10) 0.052(10) -0.003(8) 0.001(7) 0.002(7)
C41 0.12(5) 0.14(5) 0.12(4) 0.02(4) 0.00(4) 0.06(4)
C41A 0.12(7) 0.08(5) 0.18(10) 0.06(6) -0.03(7) 0.01(5)
C42 0.07(2) 0.07(3) 0.10(4) 0.03(2) -0.02(2) 0.00(2)
C42A 0.28(14) 0.12(7) 0.15(10) -0.04(7) -0.12(10) 0.00(9)
C43 0.12(4) 0.11(4) 0.17(6) 0.07(4) -0.11(5) -0.03(3)
C43A 0.07(5) 0.34(16) 0.15(9) 0.09(10) -0.01(5) 0.00(8)
C44 0.100(17) 0.088(16) 0.085(16) 0.018(13) -0.022(13) -0.055(14)
C45 0.062(13) 0.12(2) 0.095(18) 0.003(16) -0.005(12) -0.002(13)
C46 0.085(13) 0.072(12) 0.064(12) 0.000(11) 0.000(12) -0.017(10)
C47 0.047(12) 0.26(4) 0.095(19) 0.05(2) -0.011(12) -0.020(18)
C48 0.070(15) 0.097(18) 0.13(2) 0.007(18) 0.008(15) 0.008(13)
C49 0.070(14) 0.089(17) 0.12(2) 0.012(15) 0.011(14) -0.011(12)
C50 0.079(13) 0.075(12) 0.044(10) 0.004(9) 0.004(9) 0.001(10)
C51 0.073(12) 0.061(11) 0.067(12) 0.002(9) 0.009(10) 0.010(9)
C52 0.065(11) 0.066(11) 0.057(11) 0.000(9) -0.013(9) 0.017(9)
C53 0.14(4) 0.10(3) 0.06(2) 0.00(2) -0.03(2) 0.03(3)
C53A 0.08(4) 0.06(3) 0.08(4) -0.01(3) -0.02(3) -0.01(3)
C54 0.15(5) 0.08(3) 0.12(4) -0.03(3) -0.03(3) -0.04(3)
C54A 0.07(4) 0.06(3) 0.08(4) -0.01(3) -0.03(3) 0.00(3)
C55 0.13(4) 0.10(4) 0.08(3) -0.05(3) -0.04(3) 0.04(3)
C55A 0.09(5) 0.19(10) 0.06(4) -0.04(5) 0.01(4) -0.07(6)
C56 0.061(10) 0.081(13) 0.058(12) -0.009(10) -0.001(9) 0.010(9)
C57 0.066(12) 0.072(13) 0.081(14) 0.002(11) -0.006(10) -0.024(10)
C58 0.054(11) 0.106(17) 0.068(14) -0.021(12) -0.001(9) 0.011(11)

_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 O1A 1.77(4) . ?
Ti1 O3 1.785(19) . ?
Ti1 O3A 1.79(5) . ?
Ti1 O2 1.800(18) . ?
Ti1 O1 1.811(17) . ?
Ti1 O2A 1.82(5) . ?
Ti1 O4 2.000(12) . ?
Ti1 N1 2.230(13) . ?
S1 O5 1.42(4) . ?
S1 O4 1.439(18) . ?
S1 O6 1.46(4) . ?
S1 C5 1.84(3) . ?
S1A O5A 1.21(8) . ?
S1A O4 1.50(3) . ?
S1A O6A 1.64(9) . ?
S1A C5 1.77(5) . ?
F1 C5 1.27(3) . ?
O1 C11 1.36(3) . ?
O1A C11A 1.38(8) . ?
N1 C1 1.47(3) . ?
N1 C2A 1.47(7) . ?
N1 C2 1.50(3) . ?
N1 C3 1.53(3) . ?
N1 C3A 1.55(7) . ?
N1 C1A 1.57(7) . ?
C1 C12 1.48(4) . ?
C11A C16 1.42(8) . ?
C11A C12A 1.43(9) . ?
C1A C12A 1.50(10) . ?
F2 C5 1.28(3) . ?
O2 C21 1.36(4) . ?
O2A C21A 1.37(9) . ?
C2 C22 1.48(4) . ?
C2A C22A 1.54(12) . ?
F3 C5 1.28(4) . ?
O3 C31 1.37(3) . ?
O3A C31A 1.39(8) . ?
C3 C32 1.51(4) . ?
C3 C4 1.56(3) . ?
C3A C32A 1.52(10) . ?
C3A C4A 1.5400(8) . ?
C11 C12 1.39(4) . ?
C11 C16 1.41(3) . ?
C12 C13 1.41(3) . ?
C12A C13A 1.36(9) . ?
C13 C14 1.42(3) . ?
C13A C14 1.40(7) . ?
C14 C15 1.39(3) . ?
C14 C17 1.52(3) . ?
C15 C16 1.39(3) . ?
C16 C18 1.54(3) . ?
C17 C41A 1.46(8) . ?
C17 C43 1.49(5) . ?
C17 C41 1.50(6) . ?
C17 C42 1.58(5) . ?
C17 C43A 1.67(11) . ?
C17 C42A 1.77(12) . ?
C18 C45 1.50(3) . ?
C18 C46 1.53(3) . ?
C18 C44 1.55(3) . ?
C21 C22 1.39(4) . ?
C21 C26 1.41(4) . ?
C21A C22A 1.35(11) . ?
C21A C26 1.48(9) . ?
C22 C23 1.43(3) . ?
C22A C23A 1.42(11) . ?
C23 C24 1.37(3) . ?
C23A C24 1.66(9) . ?
C24 C25 1.40(3) . ?
C24 C27 1.52(3) . ?
C25 C26 1.38(3) . ?
C26 C28 1.52(2) . ?
C27 C47 1.50(4) . ?
C27 C48 1.51(4) . ?
C27 C49 1.56(3) . ?
C28 C52 1.53(2) . ?
C28 C51 1.53(3) . ?
C28 C50 1.55(3) . ?
C31 C32 1.39(3) . ?
C31 C36 1.44(3) . ?
C31A C32A 1.35(9) . ?
C31A C36 1.47(7) . ?
C32 C33 1.40(3) . ?
C32A C33A 1.42(9) . ?
C33 C34 1.41(3) . ?
C33A C34 1.47(9) . ?
C34 C35 1.39(2) . ?
C34 C37 1.52(3) . ?
C35 C36 1.39(2) . ?
C36 C38 1.51(2) . ?
C37 C55 1.46(5) . ?
C37 C53A 1.49(6) . ?
C37 C54 1.53(5) . ?
C37 C55A 1.54(7) . ?
C37 C53 1.58(4) . ?
C37 C54A 1.61(6) . ?
C38 C56 1.53(3) . ?
C38 C57 1.53(3) . ?
C38 C58 1.54(3) . ?
C61 C62 1.3900 . ?
C61 C66 1.3900 . ?
C61 C67 1.4591 . ?
C62 C63 1.3900 . ?
C63 C64 1.3900 . ?
C64 C65 1.3900 . ?
C65 C66 1.3900 . ?

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
O1A Ti1 O3 144(2) . . ?
O1A Ti1 O3A 117(3) . . ?
O3 Ti1 O3A 27.3(19) . . ?
O1A Ti1 O2 96(2) . . ?
O3 Ti1 O2 118.0(10) . . ?
O3A Ti1 O2 143(2) . . ?
O1A Ti1 O1 27.3(17) . . ?
O3 Ti1 O1 117.2(10) . . ?
O3A Ti1 O1 90(2) . . ?
O2 Ti1 O1 123.1(9) . . ?
O1A Ti1 O2A 119(3) . . ?
O3 Ti1 O2A 93(2) . . ?
O3A Ti1 O2A 119(3) . . ?
O2 Ti1 O2A 24.9(19) . . ?
O1 Ti1 O2A 146(2) . . ?
O1A Ti1 O4 95.0(14) . . ?
O3 Ti1 O4 93.5(7) . . ?
O3A Ti1 O4 97.5(15) . . ?
O2 Ti1 O4 95.6(7) . . ?
O1 Ti1 O4 93.7(7) . . ?
O2A Ti1 O4 100.1(16) . . ?
O1A Ti1 N1 84.0(13) . . ?
O3 Ti1 N1 86.6(7) . . ?
O3A Ti1 N1 81.9(15) . . ?
O2 Ti1 N1 85.8(7) . . ?
O1 Ti1 N1 84.9(6) . . ?
O2A Ti1 N1 81.5(16) . . ?
O4 Ti1 N1 178.4(6) . . ?
O5 S1 O4 116(3) . . ?
O5 S1 O6 120(4) . . ?
O4 S1 O6 111(2) . . ?
O5 S1 C5 103.5(18) . . ?
O4 S1 C5 100.4(13) . . ?
O6 S1 C5 102(3) . . ?
O5A S1A O4 109(4) . . ?
O5A S1A O6A 116(5) . . ?
O4 S1A O6A 105(4) . . ?
O5A S1A C5 122(6) . . ?
O4 S1A C5 101(2) . . ?
O6A S1A C5 102(3) . . ?
C11 O1 Ti1 141.0(17) . . ?
C11A O1A Ti1 145(4) . . ?
C1 N1 C2A 127(4) . . ?
C1 N1 C2 109.3(17) . . ?
C2A N1 C2 77(4) . . ?
C1 N1 C3 111.8(17) . . ?
C2A N1 C3 34(4) . . ?
C2 N1 C3 110.7(17) . . ?
C1 N1 C3A 29(3) . . ?
C2A N1 C3A 107(5) . . ?
C2 N1 C3A 130(3) . . ?
C3 N1 C3A 84(4) . . ?
C1 N1 C1A 78(4) . . ?
C2A N1 C1A 104(5) . . ?
C2 N1 C1A 33(3) . . ?
C3 N1 C1A 135(3) . . ?
C3A N1 C1A 103(4) . . ?
C1 N1 Ti1 110.4(12) . . ?
C2A N1 Ti1 117(3) . . ?
C2 N1 Ti1 108.0(12) . . ?
C3 N1 Ti1 106.5(11) . . ?
C3A N1 Ti1 113.3(19) . . ?
C1A N1 Ti1 111(3) . . ?
N1 C1 C12 114(2) . . ?
O1A C11A C16 123(5) . . ?
O1A C11A C12A 115(6) . . ?
C16 C11A C12A 122(5) . . ?
C12A C1A N1 116(5) . . ?
C21 O2 Ti1 142.2(18) . . ?
C21A O2A Ti1 143(5) . . ?
C22 C2 N1 115.6(19) . . ?
N1 C2A C22A 109(7) . . ?
C31 O3 Ti1 137.8(16) . . ?
C31A O3A Ti1 146(4) . . ?
C32 C3 N1 111.3(18) . . ?
C32 C3 C4 111(2) . . ?
N1 C3 C4 113.7(19) . . ?
C32A C3A C4A 107(7) . . ?
C32A C3A N1 110(5) . . ?
C4A C3A N1 115(7) . . ?
S1 O4 S1A 25.3(17) . . ?
S1 O4 Ti1 152.8(11) . . ?
S1A O4 Ti1 151.6(14) . . ?
F1 C5 F3 111(3) . . ?
F1 C5 F2 108(2) . . ?
F3 C5 F2 108(3) . . ?
F1 C5 S1A 122(3) . . ?
F3 C5 S1A 94(3) . . ?
F2 C5 S1A 112(2) . . ?
F1 C5 S1 105(2) . . ?
F3 C5 S1 112(2) . . ?
F2 C5 S1 111(2) . . ?
S1A C5 S1 20.5(15) . . ?
O1 C11 C12 115(2) . . ?
O1 C11 C16 122(2) . . ?
C12 C11 C16 122(2) . . ?
C11 C12 C13 118(2) . . ?
C11 C12 C1 119(2) . . ?
C13 C12 C1 122(2) . . ?
C13A C12A C11A 118(6) . . ?
C13A C12A C1A 122(6) . . ?
C11A C12A C1A 120(6) . . ?
C12 C13 C14 121(2) . . ?
C12A C13A C14 120(6) . . ?
C15 C14 C13A 112(3) . . ?
C15 C14 C13 116.0(18) . . ?
C13A C14 C13 45(3) . . ?
C15 C14 C17 121.0(18) . . ?
C13A C14 C17 113(3) . . ?
C13 C14 C17 122.5(19) . . ?
C16 C15 C14 124.8(17) . . ?
C15 C16 C11 116.0(19) . . ?
C15 C16 C11A 112(3) . . ?
C11 C16 C11A 31(3) . . ?
C15 C16 C18 124.1(17) . . ?
C11 C16 C18 118.9(19) . . ?
C11A C16 C18 120(3) . . ?
C41A C17 C43 127(5) . . ?
C41A C17 C41 69(6) . . ?
C43 C17 C41 111(5) . . ?
C41A C17 C14 117(4) . . ?
C43 C17 C14 112(2) . . ?
C41 C17 C14 111(3) . . ?
C41A C17 C42 40(5) . . ?
C43 C17 C42 106(4) . . ?
C41 C17 C42 108(4) . . ?
C14 C17 C42 109(2) . . ?
C41A C17 C43A 117(9) . . ?
C43 C17 C43A 67(7) . . ?
C41 C17 C43A 52(7) . . ?
C14 C17 C43A 103(4) . . ?
C42 C17 C43A 147(5) . . ?
C41A C17 C42A 98(8) . . ?
C43 C17 C42A 51(6) . . ?
C41 C17 C42A 146(5) . . ?
C14 C17 C42A 103(4) . . ?
C42 C17 C42A 61(6) . . ?
C43A C17 C42A 118(9) . . ?
C45 C18 C46 111.0(19) . . ?
C45 C18 C16 111.7(19) . . ?
C46 C18 C16 110.8(16) . . ?
C45 C18 C44 107(2) . . ?
C46 C18 C44 106.5(19) . . ?
C16 C18 C44 110.1(17) . . ?
O2 C21 C22 115(3) . . ?
O2 C21 C26 124(3) . . ?
C22 C21 C26 121(3) . . ?
C22A C21A O2A 115(7) . . ?
C22A C21A C26 127(7) . . ?
O2A C21A C26 118(6) . . ?
C21 C22 C23 119(2) . . ?
C21 C22 C2 121(2) . . ?
C23 C22 C2 120.8(19) . . ?
C21A C22A C23A 121(7) . . ?
C21A C22A C2A 123(7) . . ?
C23A C22A C2A 115(7) . . ?
C24 C23 C22 122(2) . . ?
C22A C23A C24 112(6) . . ?
C23 C24 C25 116.0(18) . . ?
C23 C24 C27 122.8(18) . . ?
C25 C24 C27 120.9(18) . . ?
C23 C24 C23A 38(3) . . ?
C25 C24 C23A 113(3) . . ?
C27 C24 C23A 115(3) . . ?
C26 C25 C24 125.2(17) . . ?
C25 C26 C21 116.8(19) . . ?
C25 C26 C21A 112(3) . . ?
C21 C26 C21A 27(4) . . ?
C25 C26 C28 122.4(16) . . ?
C21 C26 C28 120.2(19) . . ?
C21A C26 C28 122(3) . . ?
C47 C27 C48 107(2) . . ?
C47 C27 C24 112.0(19) . . ?
C48 C27 C24 110(2) . . ?
C47 C27 C49 112(3) . . ?
C48 C27 C49 108(2) . . ?
C24 C27 C49 107.8(17) . . ?
C26 C28 C52 111.0(15) . . ?
C26 C28 C51 110.8(16) . . ?
C52 C28 C51 109.4(16) . . ?
C26 C28 C50 111.4(15) . . ?
C52 C28 C50 107.0(15) . . ?
C51 C28 C50 107.0(15) . . ?
O3 C31 C32 115(2) . . ?
O3 C31 C36 122.6(19) . . ?
C32 C31 C36 122(2) . . ?
C32A C31A O3A 117(6) . . ?
C32A C31A C36 129(5) . . ?
O3A C31A C36 113(5) . . ?
C31 C32 C33 118(2) . . ?
C31 C32 C3 119(2) . . ?
C33 C32 C3 122.8(19) . . ?
C31A C32A C33A 119(6) . . ?
C31A C32A C3A 121(6) . . ?
C33A C32A C3A 120(6) . . ?
C32 C33 C34 123(2) . . ?
C32A C33A C34 116(6) . . ?
C35 C34 C33 115.4(17) . . ?
C35 C34 C33A 118(3) . . ?
C33 C34 C33A 37(3) . . ?
C35 C34 C37 122.2(16) . . ?
C33 C34 C37 121.8(17) . . ?
C33A C34 C37 112(3) . . ?
C34 C35 C36 124.8(16) . . ?
C35 C36 C31 116.0(17) . . ?
C35 C36 C31A 108(3) . . ?
C31 C36 C31A 33(3) . . ?
C35 C36 C38 123.1(16) . . ?
C31 C36 C38 120.5(17) . . ?
C31A C36 C38 123(3) . . ?
C55 C37 C53A 129(3) . . ?
C55 C37 C34 114(2) . . ?
C53A C37 C34 117(3) . . ?
C55 C37 C54 111(4) . . ?
C53A C37 C54 51(3) . . ?
C34 C37 C54 109(3) . . ?
C55 C37 C55A 47(5) . . ?
C53A C37 C55A 110(5) . . ?
C34 C37 C55A 111(3) . . ?
C54 C37 C55A 139(4) . . ?
C55 C37 C53 108(3) . . ?
C53A C37 C53 59(3) . . ?
C34 C37 C53 105(2) . . ?
C54 C37 C53 110(3) . . ?
C55A C37 C53 63(5) . . ?
C55 C37 C54A 59(4) . . ?
C53A C37 C54A 106(3) . . ?
C34 C37 C54A 106(2) . . ?
C54 C37 C54A 60(3) . . ?
C55A C37 C54A 105(6) . . ?
C53 C37 C54A 150(3) . . ?
C36 C38 C56 111.4(15) . . ?
C36 C38 C57 109.0(15) . . ?
C56 C38 C57 109.8(17) . . ?
C36 C38 C58 111.5(15) . . ?
C56 C38 C58 108.5(16) . . ?
C57 C38 C58 106.5(17) . . ?
C62 C61 C66 120.0 . . ?
C62 C61 C67 139.4 . . ?
C66 C61 C67 100.1 . . ?
C63 C62 C61 120.0 . . ?
C62 C63 C64 120.0 . . ?
C65 C64 C63 120.0 . . ?
C64 C65 C66 120.0 . . ?
C65 C66 C61 120.0 . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        25.74
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.051