# Electronic Supplementary Material (ESI) for Organic Chemistry Frontiers.
# This journal is © the Partner Organisations 2014

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#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
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#  except for the purpose of generating routine backup copies
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data_a40103b

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H48 Cl6 O9 Ti3'
_chemical_formula_weight         837.02

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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                   10.354(4)
_cell_length_b                   10.811(4)
_cell_length_c                   18.781(7)
_cell_angle_alpha                77.136(5)
_cell_angle_beta                 88.021(5)
_cell_angle_gamma                64.810(4)
_cell_volume                     1850.4(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2106
_cell_measurement_theta_min      2.17
_cell_measurement_theta_max      23.06

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             864
_exptl_absorpt_coefficient_mu    1.107
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8089
_exptl_absorpt_correction_T_max  0.8515
_exptl_absorpt_process_details   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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7743
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_sigmaI/netI    0.0861
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6366
_reflns_number_gt                3492
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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)+(0.0370P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6366
_refine_ls_number_parameters     379
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0938
_refine_ls_R_factor_gt           0.0516
_refine_ls_wR_factor_ref         0.1131
_refine_ls_wR_factor_gt          0.1046
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.003
_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 0.87052(9) 0.30804(8) 0.33219(4) 0.0450(2) Uani 1 1 d . . .
Ti2 Ti 0.79597(9) 0.23923(9) 0.17043(4) 0.0458(2) Uani 1 1 d . . .
Ti3 Ti 0.52600(9) 0.48959(9) 0.24830(4) 0.0469(3) Uani 1 1 d . . .
O1 O 0.8952(3) 0.2325(3) 0.25810(15) 0.0445(8) Uani 1 1 d . . .
O2 O 0.6307(3) 0.3522(3) 0.19037(15) 0.0457(8) Uani 1 1 d . . .
O3 O 0.6804(3) 0.4433(3) 0.30124(15) 0.0461(8) Uani 1 1 d . . .
O4 O 1.0836(4) 0.1766(3) 0.38229(17) 0.0580(9) Uani 1 1 d . . .
O5 O 0.8346(4) 0.4052(4) 0.43101(17) 0.0680(11) Uani 1 1 d . . .
O6 O 1.0238(4) 0.0857(3) 0.15210(17) 0.0582(9) Uani 1 1 d . . .
O7 O 0.7875(4) 0.0559(3) 0.23520(18) 0.0578(9) Uani 1 1 d . . .
O8 O 0.3442(3) 0.5378(3) 0.17002(18) 0.0602(9) Uani 1 1 d . . .
O9 O 0.5651(3) 0.6319(3) 0.16218(16) 0.0524(9) Uani 1 1 d . . .
Cl1 Cl 0.96396(15) 0.46996(14) 0.28575(8) 0.0683(4) Uani 1 1 d . . .
Cl2 Cl 0.80296(15) 0.14719(13) 0.40868(7) 0.0630(4) Uani 1 1 d . . .
Cl3 Cl 0.71454(17) 0.17728(16) 0.07462(8) 0.0841(5) Uani 1 1 d . . .
Cl4 Cl 0.86278(15) 0.39873(14) 0.09617(7) 0.0695(4) Uani 1 1 d . . .
Cl5 Cl 0.43931(15) 0.35018(15) 0.32343(8) 0.0721(4) Uani 1 1 d . . .
Cl6 Cl 0.38426(16) 0.69224(14) 0.29005(8) 0.0768(5) Uani 1 1 d . . .
C1 C 1.1484(6) 0.0241(5) 0.3946(3) 0.0730(17) Uani 1 1 d . . .
H1A H 1.1270 -0.0045 0.3528 0.088 Uiso 1 1 calc R . .
H1B H 1.1132 -0.0169 0.4377 0.088 Uiso 1 1 calc R . .
C2 C 1.3082(7) -0.0216(7) 0.4055(4) 0.097(2) Uani 1 1 d . . .
H2A H 1.3543 -0.1130 0.4389 0.116 Uiso 1 1 calc R . .
H2B H 1.3531 -0.0247 0.3594 0.116 Uiso 1 1 calc R . .
C3 C 1.3135(7) 0.0891(7) 0.4370(4) 0.110(3) Uani 1 1 d . . .
H3A H 1.3079 0.0679 0.4896 0.132 Uiso 1 1 calc R . .
H3B H 1.4012 0.0994 0.4262 0.132 Uiso 1 1 calc R . .
C4 C 1.1890(7) 0.2167(7) 0.4022(4) 0.113(3) Uani 1 1 d . . .
H4A H 1.1517 0.2781 0.4359 0.136 Uiso 1 1 calc R . .
H4B H 1.2156 0.2668 0.3591 0.136 Uiso 1 1 calc R . .
C5 C 0.8635(11) 0.3397(7) 0.5052(3) 0.149(4) Uani 1 1 d . . .
H5A H 0.8227 0.2723 0.5171 0.179 Uiso 1 1 calc R . .
H5B H 0.9661 0.2893 0.5163 0.179 Uiso 1 1 calc R . .
C6 C 0.8060(11) 0.4387(9) 0.5471(4) 0.160(4) Uani 1 1 d . . .
H6A H 0.8802 0.4580 0.5656 0.192 Uiso 1 1 calc R . .
H6B H 0.7613 0.4050 0.5883 0.192 Uiso 1 1 calc R . .
C7 C 0.6974(10) 0.5683(10) 0.4981(4) 0.178(5) Uani 1 1 d . . .
H7A H 0.6011 0.5786 0.5075 0.213 Uiso 1 1 calc R . .
H7B H 0.7056 0.6515 0.5043 0.213 Uiso 1 1 calc R . .
C8 C 0.7324(10) 0.5451(7) 0.4276(4) 0.138(4) Uani 1 1 d . . .
H8A H 0.7705 0.6097 0.4025 0.166 Uiso 1 1 calc R . .
H8B H 0.6465 0.5635 0.3996 0.166 Uiso 1 1 calc R . .
C9 C 1.0634(7) 0.0438(6) 0.0824(3) 0.089(2) Uani 1 1 d . . .
H9A H 1.0738 -0.0511 0.0864 0.107 Uiso 1 1 calc R . .
H9B H 0.9908 0.1068 0.0436 0.107 Uiso 1 1 calc R . .
C10 C 1.1962(10) 0.0515(12) 0.0678(5) 0.176(5) Uani 1 1 d . . .
H10A H 1.2648 -0.0362 0.0574 0.211 Uiso 1 1 calc R . .
H10B H 1.1826 0.1262 0.0250 0.211 Uiso 1 1 calc R . .
C11 C 1.2496(8) 0.0768(9) 0.1270(5) 0.136(3) Uani 1 1 d . . .
H11A H 1.2642 0.1614 0.1117 0.163 Uiso 1 1 calc R . .
H11B H 1.3408 -0.0010 0.1460 0.163 Uiso 1 1 calc R . .
C12 C 1.1470(6) 0.0931(7) 0.1836(3) 0.0809(18) Uani 1 1 d . . .
H12A H 1.1188 0.1827 0.1965 0.097 Uiso 1 1 calc R . .
H12B H 1.1885 0.0186 0.2273 0.097 Uiso 1 1 calc R . .
C13 C 0.9012(7) -0.0739(6) 0.2664(4) 0.092(2) Uani 1 1 d . . .
H13A H 0.9702 -0.0593 0.2931 0.111 Uiso 1 1 calc R . .
H13B H 0.9492 -0.1209 0.2283 0.111 Uiso 1 1 calc R . .
C14 C 0.8444(8) -0.1605(6) 0.3162(4) 0.112(3) Uani 1 1 d . . .
H14A H 0.8843 -0.1823 0.3659 0.134 Uiso 1 1 calc R . .
H14B H 0.8682 -0.2479 0.3016 0.134 Uiso 1 1 calc R . .
C15 C 0.6871(8) -0.0777(7) 0.3120(4) 0.098(2) Uani 1 1 d . . .
H15A H 0.6569 -0.0448 0.3565 0.117 Uiso 1 1 calc R . .
H15B H 0.6384 -0.1338 0.3048 0.117 Uiso 1 1 calc R . .
C16 C 0.6561(7) 0.0422(6) 0.2482(4) 0.088(2) Uani 1 1 d . . .
H16A H 0.6228 0.0244 0.2056 0.106 Uiso 1 1 calc R . .
H16B H 0.5827 0.1276 0.2586 0.106 Uiso 1 1 calc R . .
C17 C 0.1974(6) 0.6305(6) 0.1783(3) 0.0771(17) Uani 1 1 d . . .
H17A H 0.1864 0.7256 0.1740 0.092 Uiso 1 1 calc R . .
H17B H 0.1668 0.5987 0.2254 0.092 Uiso 1 1 calc R . .
C18 C 0.1139(6) 0.6238(7) 0.1179(3) 0.094(2) Uani 1 1 d . . .
H18A H 0.0173 0.6410 0.1310 0.113 Uiso 1 1 calc R . .
H18B H 0.1095 0.6919 0.0735 0.113 Uiso 1 1 calc R . .
C19 C 0.1933(7) 0.4805(7) 0.1085(4) 0.097(2) Uani 1 1 d . . .
H19A H 0.1584 0.4180 0.1393 0.116 Uiso 1 1 calc R . .
H19B H 0.1828 0.4771 0.0579 0.116 Uiso 1 1 calc R . .
C20 C 0.3417(7) 0.4396(7) 0.1297(4) 0.102(2) Uani 1 1 d . . .
H20A H 0.3838 0.3448 0.1600 0.122 Uiso 1 1 calc R . .
H20B H 0.3957 0.4424 0.0866 0.122 Uiso 1 1 calc R . .
C21 C 0.6353(7) 0.7136(6) 0.1753(3) 0.0792(19) Uani 1 1 d . . .
H21A H 0.7241 0.6536 0.2048 0.095 Uiso 1 1 calc R . .
H21B H 0.5749 0.7831 0.2014 0.095 Uiso 1 1 calc R . .
C22 C 0.6646(8) 0.7826(8) 0.1051(4) 0.105(2) Uani 1 1 d . . .
H22A H 0.7665 0.7420 0.0987 0.126 Uiso 1 1 calc R . .
H22B H 0.6321 0.8820 0.1024 0.126 Uiso 1 1 calc R . .
C23 C 0.5878(7) 0.7620(6) 0.0484(3) 0.0777(18) Uani 1 1 d . . .
H23A H 0.6531 0.7208 0.0131 0.093 Uiso 1 1 calc R . .
H23B H 0.5136 0.8514 0.0229 0.093 Uiso 1 1 calc R . .
C24 C 0.5231(6) 0.6667(5) 0.0843(3) 0.0630(15) Uani 1 1 d . . .
H24A H 0.4198 0.7133 0.0760 0.076 Uiso 1 1 calc R . .
H24B H 0.5589 0.5825 0.0654 0.076 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 O1 1.724(3) . ?
Ti1 O3 1.898(3) . ?
Ti1 O4 2.157(3) . ?
Ti1 O5 2.274(3) . ?
Ti1 Cl2 2.3304(16) . ?
Ti1 Cl1 2.3377(16) . ?
Ti2 O2 1.714(3) . ?
Ti2 O1 1.942(3) . ?
Ti2 O7 2.117(3) . ?
Ti2 Cl4 2.2967(17) . ?
Ti2 O6 2.303(3) . ?
Ti2 Cl3 2.3494(16) . ?
Ti3 O3 1.732(3) . ?
Ti3 O2 1.958(3) . ?
Ti3 O9 2.127(3) . ?
Ti3 O8 2.234(3) . ?
Ti3 Cl5 2.2772(17) . ?
Ti3 Cl6 2.3489(16) . ?
O4 C4 1.421(6) . ?
O4 C1 1.457(5) . ?
O5 C5 1.394(6) . ?
O5 C8 1.418(7) . ?
O6 C12 1.464(6) . ?
O6 C9 1.468(6) . ?
O7 C13 1.406(6) . ?
O7 C16 1.437(6) . ?
O8 C20 1.444(6) . ?
O8 C17 1.448(6) . ?
O9 C21 1.422(5) . ?
O9 C24 1.459(5) . ?
C1 C2 1.518(7) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.469(8) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.461(7) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.385(9) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C7 1.493(9) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.410(9) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.427(9) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.386(9) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.462(8) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.463(8) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.482(8) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.484(7) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.482(7) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.461(8) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.449(7) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.454(7) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.460(7) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.487(7) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ti1 O3 95.29(13) . . ?
O1 Ti1 O4 95.19(13) . . ?
O3 Ti1 O4 169.34(13) . . ?
O1 Ti1 O5 178.65(15) . . ?
O3 Ti1 O5 84.33(13) . . ?
O4 Ti1 O5 85.23(13) . . ?
O1 Ti1 Cl2 95.43(11) . . ?
O3 Ti1 Cl2 94.79(10) . . ?
O4 Ti1 Cl2 86.16(10) . . ?
O5 Ti1 Cl2 83.32(10) . . ?
O1 Ti1 Cl1 97.88(11) . . ?
O3 Ti1 Cl1 92.24(10) . . ?
O4 Ti1 Cl1 84.38(10) . . ?
O5 Ti1 Cl1 83.44(10) . . ?
Cl2 Ti1 Cl1 164.30(6) . . ?
O2 Ti2 O1 94.90(13) . . ?
O2 Ti2 O7 95.11(14) . . ?
O1 Ti2 O7 83.24(13) . . ?
O2 Ti2 Cl4 99.37(11) . . ?
O1 Ti2 Cl4 94.29(10) . . ?
O7 Ti2 Cl4 165.48(11) . . ?
O2 Ti2 O6 175.86(13) . . ?
O1 Ti2 O6 81.03(12) . . ?
O7 Ti2 O6 83.69(13) . . ?
Cl4 Ti2 O6 81.79(9) . . ?
O2 Ti2 Cl3 96.40(11) . . ?
O1 Ti2 Cl3 163.53(10) . . ?
O7 Ti2 Cl3 83.86(10) . . ?
Cl4 Ti2 Cl3 95.64(7) . . ?
O6 Ti2 Cl3 87.42(10) . . ?
O3 Ti3 O2 91.30(13) . . ?
O3 Ti3 O9 95.07(13) . . ?
O2 Ti3 O9 83.76(13) . . ?
O3 Ti3 O8 173.12(14) . . ?
O2 Ti3 O8 82.24(12) . . ?
O9 Ti3 O8 81.93(13) . . ?
O3 Ti3 Cl5 98.09(11) . . ?
O2 Ti3 Cl5 95.30(10) . . ?
O9 Ti3 Cl5 166.83(10) . . ?
O8 Ti3 Cl5 84.93(10) . . ?
O3 Ti3 Cl6 96.62(11) . . ?
O2 Ti3 Cl6 166.19(10) . . ?
O9 Ti3 Cl6 84.28(10) . . ?
O8 Ti3 Cl6 89.26(10) . . ?
Cl5 Ti3 Cl6 94.77(7) . . ?
Ti1 O1 Ti2 142.24(17) . . ?
Ti2 O2 Ti3 145.69(17) . . ?
Ti3 O3 Ti1 146.89(17) . . ?
C4 O4 C1 107.9(4) . . ?
C4 O4 Ti1 128.9(3) . . ?
C1 O4 Ti1 122.9(3) . . ?
C5 O5 C8 105.8(5) . . ?
C5 O5 Ti1 129.4(4) . . ?
C8 O5 Ti1 121.6(3) . . ?
C12 O6 C9 107.7(4) . . ?
C12 O6 Ti2 119.5(3) . . ?
C9 O6 Ti2 122.8(3) . . ?
C13 O7 C16 108.1(4) . . ?
C13 O7 Ti2 128.7(4) . . ?
C16 O7 Ti2 123.0(3) . . ?
C20 O8 C17 107.6(4) . . ?
C20 O8 Ti3 123.2(3) . . ?
C17 O8 Ti3 123.2(3) . . ?
C21 O9 C24 109.7(4) . . ?
C21 O9 Ti3 122.2(3) . . ?
C24 O9 Ti3 128.1(3) . . ?
O4 C1 C2 105.4(5) . . ?
O4 C1 H1A 110.7 . . ?
C2 C1 H1A 110.7 . . ?
O4 C1 H1B 110.7 . . ?
C2 C1 H1B 110.7 . . ?
H1A C1 H1B 108.8 . . ?
C3 C2 C1 102.3(5) . . ?
C3 C2 H2A 111.3 . . ?
C1 C2 H2A 111.3 . . ?
C3 C2 H2B 111.3 . . ?
C1 C2 H2B 111.3 . . ?
H2A C2 H2B 109.2 . . ?
C4 C3 C2 104.9(6) . . ?
C4 C3 H3A 110.8 . . ?
C2 C3 H3A 110.8 . . ?
C4 C3 H3B 110.8 . . ?
C2 C3 H3B 110.8 . . ?
H3A C3 H3B 108.9 . . ?
O4 C4 C3 107.9(5) . . ?
O4 C4 H4A 110.1 . . ?
C3 C4 H4A 110.1 . . ?
O4 C4 H4B 110.1 . . ?
C3 C4 H4B 110.1 . . ?
H4A C4 H4B 108.4 . . ?
C6 C5 O5 110.1(6) . . ?
C6 C5 H5A 109.6 . . ?
O5 C5 H5A 109.6 . . ?
C6 C5 H5B 109.6 . . ?
O5 C5 H5B 109.6 . . ?
H5A C5 H5B 108.2 . . ?
C5 C6 C7 106.7(7) . . ?
C5 C6 H6A 110.4 . . ?
C7 C6 H6A 110.4 . . ?
C5 C6 H6B 110.4 . . ?
C7 C6 H6B 110.4 . . ?
H6A C6 H6B 108.6 . . ?
C8 C7 C6 103.0(7) . . ?
C8 C7 H7A 111.2 . . ?
C6 C7 H7A 111.2 . . ?
C8 C7 H7B 111.2 . . ?
C6 C7 H7B 111.2 . . ?
H7A C7 H7B 109.1 . . ?
C7 C8 O5 111.3(6) . . ?
C7 C8 H8A 109.4 . . ?
O5 C8 H8A 109.4 . . ?
C7 C8 H8B 109.4 . . ?
O5 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
C10 C9 O6 105.8(6) . . ?
C10 C9 H9A 110.6 . . ?
O6 C9 H9A 110.6 . . ?
C10 C9 H9B 110.6 . . ?
O6 C9 H9B 110.6 . . ?
H9A C9 H9B 108.7 . . ?
C11 C10 C9 111.0(7) . . ?
C11 C10 H10A 109.4 . . ?
C9 C10 H10A 109.4 . . ?
C11 C10 H10B 109.4 . . ?
C9 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
C10 C11 C12 108.7(7) . . ?
C10 C11 H11A 109.9 . . ?
C12 C11 H11A 109.9 . . ?
C10 C11 H11B 109.9 . . ?
C12 C11 H11B 109.9 . . ?
H11A C11 H11B 108.3 . . ?
C11 C12 O6 105.8(5) . . ?
C11 C12 H12A 110.6 . . ?
O6 C12 H12A 110.6 . . ?
C11 C12 H12B 110.6 . . ?
O6 C12 H12B 110.6 . . ?
H12A C12 H12B 108.7 . . ?
O7 C13 C14 108.8(5) . . ?
O7 C13 H13A 109.9 . . ?
C14 C13 H13A 109.9 . . ?
O7 C13 H13B 109.9 . . ?
C14 C13 H13B 109.9 . . ?
H13A C13 H13B 108.3 . . ?
C13 C14 C15 106.7(5) . . ?
C13 C14 H14A 110.4 . . ?
C15 C14 H14A 110.4 . . ?
C13 C14 H14B 110.4 . . ?
C15 C14 H14B 110.4 . . ?
H14A C14 H14B 108.6 . . ?
C14 C15 C16 104.9(5) . . ?
C14 C15 H15A 110.8 . . ?
C16 C15 H15A 110.8 . . ?
C14 C15 H15B 110.8 . . ?
C16 C15 H15B 110.8 . . ?
H15A C15 H15B 108.9 . . ?
O7 C16 C15 106.7(5) . . ?
O7 C16 H16A 110.4 . . ?
C15 C16 H16A 110.4 . . ?
O7 C16 H16B 110.4 . . ?
C15 C16 H16B 110.4 . . ?
H16A C16 H16B 108.6 . . ?
O8 C17 C18 104.7(5) . . ?
O8 C17 H17A 110.8 . . ?
C18 C17 H17A 110.8 . . ?
O8 C17 H17B 110.8 . . ?
C18 C17 H17B 110.8 . . ?
H17A C17 H17B 108.9 . . ?
C19 C18 C17 103.7(5) . . ?
C19 C18 H18A 111.0 . . ?
C17 C18 H18A 111.0 . . ?
C19 C18 H18B 111.0 . . ?
C17 C18 H18B 111.0 . . ?
H18A C18 H18B 109.0 . . ?
C20 C19 C18 106.3(5) . . ?
C20 C19 H19A 110.5 . . ?
C18 C19 H19A 110.5 . . ?
C20 C19 H19B 110.5 . . ?
C18 C19 H19B 110.5 . . ?
H19A C19 H19B 108.7 . . ?
O8 C20 C19 107.3(5) . . ?
O8 C20 H20A 110.3 . . ?
C19 C20 H20A 110.3 . . ?
O8 C20 H20B 110.3 . . ?
C19 C20 H20B 110.3 . . ?
H20A C20 H20B 108.5 . . ?
O9 C21 C22 108.4(5) . . ?
O9 C21 H21A 110.0 . . ?
C22 C21 H21A 110.0 . . ?
O9 C21 H21B 110.0 . . ?
C22 C21 H21B 110.0 . . ?
H21A C21 H21B 108.4 . . ?
C21 C22 C23 107.2(5) . . ?
C21 C22 H22A 110.3 . . ?
C23 C22 H22A 110.3 . . ?
C21 C22 H22B 110.3 . . ?
C23 C22 H22B 110.3 . . ?
H22A C22 H22B 108.5 . . ?
C22 C23 C24 108.1(5) . . ?
C22 C23 H23A 110.1 . . ?
C24 C23 H23A 110.1 . . ?
C22 C23 H23B 110.1 . . ?
C24 C23 H23B 110.1 . . ?
H23A C23 H23B 108.4 . . ?
O9 C24 C23 105.6(4) . . ?
O9 C24 H24A 110.6 . . ?
C23 C24 H24A 110.6 . . ?
O9 C24 H24B 110.6 . . ?
C23 C24 H24B 110.6 . . ?
H24A C24 H24B 108.7 . . ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.076
_database_code_depnum_ccdc_archive 'CCDC 1000407'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_a40425b

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H44 Cl6 O6 Ti2'
_chemical_formula_weight         809.15

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca

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

_cell_length_a                   13.085(5)
_cell_length_b                   12.063(5)
_cell_length_c                   23.777(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3753(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2787
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      25.22

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1672
_exptl_absorpt_coefficient_mu    0.890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8780
_exptl_absorpt_correction_T_max  0.9162
_exptl_absorpt_process_details   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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14899
_diffrn_reflns_av_R_equivalents  0.0740
_diffrn_reflns_av_sigmaI/netI    0.0678
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.71
_diffrn_reflns_theta_max         25.10
_reflns_number_total             3348
_reflns_number_gt                1595
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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)+(0.0921P)²+0.0665P] where P=(Fo²+2Fc²)/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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3348
_refine_ls_number_parameters     199
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1282
_refine_ls_R_factor_gt           0.0641
_refine_ls_wR_factor_ref         0.1906
_refine_ls_wR_factor_gt          0.1683
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.001
_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 0.06646(7) 0.39167(9) 0.86699(4) 0.0630(4) Uani 1 1 d . . .
O1 O 0.1157(3) 0.3111(3) 0.78973(16) 0.0732(11) Uani 1 1 d . . .
O2 O 0.2262(3) 0.3765(3) 0.88156(16) 0.0684(10) Uani 1 1 d . . .
O3 O 0.0390(3) 0.4557(4) 0.93109(15) 0.0738(12) Uani 1 1 d . . .
Cl1 Cl 0.10630(14) 0.55782(14) 0.82347(8) 0.0934(6) Uani 1 1 d . . .
Cl2 Cl 0.05286(14) 0.21728(17) 0.90655(9) 0.1058(7) Uani 1 1 d . . .
Cl3 Cl -0.09324(12) 0.38700(17) 0.83118(8) 0.1025(7) Uani 1 1 d . . .
C1 C -0.0180(5) 0.4829(9) 0.9749(3) 0.124(3) Uani 1 1 d . . .
H1 H -0.0273 0.4060 0.9872 0.149 Uiso 1 1 calc R . .
C2 C -0.1316(4) 0.5005(6) 0.9621(2) 0.0713(17) Uani 1 1 d . . .
C3 C -0.1641(5) 0.5947(5) 0.9363(3) 0.0760(18) Uani 1 1 d . . .
H3 H -0.1176 0.6510 0.9286 0.091 Uiso 1 1 calc R . .
C4 C -0.2644(5) 0.6076(6) 0.9215(3) 0.0853(19) Uani 1 1 d . . .
H4 H -0.2861 0.6719 0.9036 0.102 Uiso 1 1 calc R . .
C5 C -0.3312(5) 0.5265(7) 0.9332(3) 0.087(2) Uani 1 1 d . . .
H5 H -0.3998 0.5364 0.9242 0.104 Uiso 1 1 calc R . .
C6 C -0.3013(5) 0.4308(7) 0.9577(4) 0.108(3) Uani 1 1 d . . .
H6 H -0.3478 0.3741 0.9645 0.130 Uiso 1 1 calc R . .
C7 C -0.2001(5) 0.4197(6) 0.9723(3) 0.101(2) Uani 1 1 d . . .
H7 H -0.1785 0.3546 0.9895 0.121 Uiso 1 1 calc R . .
C8 C 0.1339(11) 0.1995(8) 0.7794(4) 0.188(6) Uani 1 1 d . . .
H8A H 0.0699 0.1588 0.7797 0.225 Uiso 1 1 calc R . .
H8B H 0.1779 0.1691 0.8084 0.225 Uiso 1 1 calc R . .
C9 C 0.1834(9) 0.1888(8) 0.7239(4) 0.156(4) Uani 1 1 d . . .
H9A H 0.2566 0.2002 0.7265 0.187 Uiso 1 1 calc R . .
H9B H 0.1701 0.1168 0.7073 0.187 Uiso 1 1 calc R . .
C10 C 0.1360(7) 0.2742(9) 0.6930(4) 0.137(3) Uani 1 1 d . . .
H10A H 0.0743 0.2473 0.6750 0.165 Uiso 1 1 calc R . .
H10B H 0.1818 0.3025 0.6643 0.165 Uiso 1 1 calc R . .
C11 C 0.1111(11) 0.3624(8) 0.7346(3) 0.187(6) Uani 1 1 d . . .
H11A H 0.1601 0.4225 0.7320 0.225 Uiso 1 1 calc R . .
H11B H 0.0434 0.3919 0.7276 0.225 Uiso 1 1 calc R . .
C12 C 0.3104(7) 0.4130(11) 0.8454(5) 0.208(6) Uani 1 1 d . . .
H12A H 0.3015 0.4895 0.8338 0.250 Uiso 1 1 calc R . .
H12B H 0.3163 0.3666 0.8123 0.250 Uiso 1 1 calc R . .
C13 C 0.4011(7) 0.4005(10) 0.8828(6) 0.193(6) Uani 1 1 d . . .
H13A H 0.4578 0.3714 0.8610 0.232 Uiso 1 1 calc R . .
H13B H 0.4208 0.4727 0.8970 0.232 Uiso 1 1 calc R . .
C14 C 0.3834(6) 0.3353(11) 0.9244(4) 0.156(5) Uani 1 1 d . . .
H14A H 0.4094 0.3667 0.9591 0.187 Uiso 1 1 calc R . .
H14B H 0.4151 0.2636 0.9184 0.187 Uiso 1 1 calc R . .
C15 C 0.2741(7) 0.3252(11) 0.9264(4) 0.190(5) Uani 1 1 d . . .
H15A H 0.2560 0.2472 0.9265 0.228 Uiso 1 1 calc R . .
H15B H 0.2494 0.3576 0.9612 0.228 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 1.746(4) . ?
Ti1 O2 2.127(4) . ?
Ti1 O1 2.176(4) . ?
Ti1 Cl3 2.2572(19) . ?
Ti1 Cl2 2.311(2) . ?
Ti1 Cl1 2.315(2) . ?
O1 C8 1.389(9) . ?
O1 C11 1.451(9) . ?
O2 C15 1.382(9) . ?
O2 C12 1.465(9) . ?
O3 C1 1.322(7) . ?
C1 C1 1.348(13) 5_567 ?
C1 C2 1.532(8) . ?
C1 H1 0.9800 . ?
C2 C7 1.347(9) . ?
C2 C3 1.360(8) . ?
C3 C4 1.368(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.340(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.351(9) . ?
C5 H5 0.9300 . ?
C6 C7 1.375(9) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.475(12) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.409(11) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.488(10) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.490(13) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.285(12) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.436(11) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?

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 O2 95.65(16) . . ?
O3 Ti1 O1 174.57(16) . . ?
O2 Ti1 O1 78.92(15) . . ?
O3 Ti1 Cl3 98.60(13) . . ?
O2 Ti1 Cl3 165.75(12) . . ?
O1 Ti1 Cl3 86.83(12) . . ?
O3 Ti1 Cl2 91.79(16) . . ?
O2 Ti1 Cl2 86.03(12) . . ?
O1 Ti1 Cl2 87.71(13) . . ?
Cl3 Ti1 Cl2 93.41(8) . . ?
O3 Ti1 Cl1 93.09(16) . . ?
O2 Ti1 Cl1 85.77(12) . . ?
O1 Ti1 Cl1 86.71(12) . . ?
Cl3 Ti1 Cl1 93.53(8) . . ?
Cl2 Ti1 Cl1 170.84(8) . . ?
C8 O1 C11 105.1(6) . . ?
C8 O1 Ti1 129.3(5) . . ?
C11 O1 Ti1 124.1(4) . . ?
C15 O2 C12 104.2(7) . . ?
C15 O2 Ti1 127.6(4) . . ?
C12 O2 Ti1 128.1(5) . . ?
C1 O3 Ti1 156.0(4) . . ?
O3 C1 C1 125.3(8) . 5_567 ?
O3 C1 C2 115.2(5) . . ?
C1 C1 C2 118.1(8) 5_567 . ?
O3 C1 H1 94.0 . . ?
C1 C1 H1 94.0 5_567 . ?
C2 C1 H1 94.0 . . ?
C7 C2 C3 118.5(6) . . ?
C7 C2 C1 120.7(7) . . ?
C3 C2 C1 120.6(7) . . ?
C2 C3 C4 120.7(6) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C5 C4 C3 119.3(6) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 121.6(6) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C5 C6 C7 118.1(7) . . ?
C5 C6 H6 120.9 . . ?
C7 C6 H6 120.9 . . ?
C2 C7 C6 121.7(7) . . ?
C2 C7 H7 119.1 . . ?
C6 C7 H7 119.1 . . ?
O1 C8 C9 108.6(8) . . ?
O1 C8 H8A 110.0 . . ?
C9 C8 H8A 110.0 . . ?
O1 C8 H8B 110.0 . . ?
C9 C8 H8B 110.0 . . ?
H8A C8 H8B 108.4 . . ?
C10 C9 C8 102.0(8) . . ?
C10 C9 H9A 111.4 . . ?
C8 C9 H9A 111.4 . . ?
C10 C9 H9B 111.4 . . ?
C8 C9 H9B 111.4 . . ?
H9A C9 H9B 109.2 . . ?
C9 C10 C11 105.8(8) . . ?
C9 C10 H10A 110.6 . . ?
C11 C10 H10A 110.6 . . ?
C9 C10 H10B 110.6 . . ?
C11 C10 H10B 110.6 . . ?
H10A C10 H10B 108.7 . . ?
O1 C11 C10 106.7(7) . . ?
O1 C11 H11A 110.4 . . ?
C10 C11 H11A 110.4 . . ?
O1 C11 H11B 110.4 . . ?
C10 C11 H11B 110.4 . . ?
H11A C11 H11B 108.6 . . ?
O2 C12 C13 102.6(9) . . ?
O2 C12 H12A 111.2 . . ?
C13 C12 H12A 111.2 . . ?
O2 C12 H12B 111.2 . . ?
C13 C12 H12B 111.2 . . ?
H12A C12 H12B 109.2 . . ?
C14 C13 C12 112.2(9) . . ?
C14 C13 H13A 109.2 . . ?
C12 C13 H13A 109.2 . . ?
C14 C13 H13B 109.2 . . ?
C12 C13 H13B 109.2 . . ?
H13A C13 H13B 107.9 . . ?
C13 C14 C15 104.9(8) . . ?
C13 C14 H14A 110.8 . . ?
C15 C14 H14A 110.8 . . ?
C13 C14 H14B 110.8 . . ?
C15 C14 H14B 110.8 . . ?
H14A C14 H14B 108.8 . . ?
O2 C15 C14 112.8(8) . . ?
O2 C15 H15A 109.0 . . ?
C14 C15 H15A 109.0 . . ?
O2 C15 H15B 109.0 . . ?
C14 C15 H15B 109.0 . . ?
H15A C15 H15B 107.8 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.825
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.073
_database_code_depnum_ccdc_archive 'CCDC 1000408'
