# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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. 
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data_matlv04
_database_code_depnum_ccdc_archive 'CCDC 1820423'
_audit_update_record             
;
2018-01-29 deposited with the CCDC.
2018-04-20 downloaded from the CCDC.
;

_vrf_PLAT301_matlv04             
; 
PROBLEM: _G Main Residue Disorder ..............(Resd  1) .. 3 % 
RESPONSE: One methoxy group is modeled as disordered over two 
positions (0.72:0.28). 
;

_vrf_PLAT860_matlv04             
; 
PROBLEM: _G Number of Least-Squares Restraints ............. 1 
RESPONSE: For the methoxy group disorder the O--C bond lengths 
were restrained to be similar and the anisotropic displacement 
parameters were constrained to be equivalent. 
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            matlv04
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H42 O19 Ti2 V4'
_chemical_formula_sum            'C14 H42 O19 Ti2 V4'
_chemical_formula_weight         814.03

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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

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

_cell_length_a                   10.2851(10)
_cell_length_b                   24.103(2)
_cell_length_c                   12.0280(12)
_cell_angle_alpha                90
_cell_angle_beta                 92.176(2)
_cell_angle_gamma                90
_cell_volume                     2979.6(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.0(5)
_cell_measurement_reflns_used    4016
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      37.49

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.815
_exptl_crystal_F_000             1656
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    1.789
_shelx_estimated_absorpt_T_min   0.468
_shelx_estimated_absorpt_T_max   0.814
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3235
_exptl_absorpt_correction_T_max  0.4995
_exptl_absorpt_process_details   'SADABS (Krause et al., 2015)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100.0(5)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD platform'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            73818
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.893
_diffrn_reflns_theta_max         38.618
_diffrn_reflns_theta_full        37.785
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             16343
_reflns_number_gt                10756
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015b)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_refine_special_details          
; 
One methoxy group is modeled as disordered over two positions 
(0.72:0.28). The O--C bond lengths were restrained to be 
similar and the anisotropic displacement parameters were 
constrained to be equivalent. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0433P)²+2.5745P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         16343
_refine_ls_number_parameters     370
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0503
_refine_ls_wR_factor_ref         0.1256
_refine_ls_wR_factor_gt          0.1135
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.002
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.32428(3) 0.62272(2) 0.06562(3) 0.02298(7) Uani 1 1 d . . . . .
V2 V 0.33612(3) 0.72078(2) 0.26229(3) 0.02310(8) Uani 1 1 d . . . . .
V3 V 0.51519(3) 0.60549(2) 0.29332(3) 0.01637(6) Uani 1 1 d . . . . .
V4 V 0.06769(3) 0.64347(2) 0.22362(3) 0.01953(7) Uani 1 1 d . . . . .
Ti1 Ti 0.26066(3) 0.62674(2) 0.44106(3) 0.01725(6) Uani 1 1 d . . . . .
Ti2 Ti 0.24947(3) 0.53359(2) 0.25614(3) 0.01780(7) Uani 1 1 d . . . . .
O1 O 0.34871(18) 0.62005(9) -0.06531(14) 0.0374(4) Uani 1 1 d . . . . .
O2 O 0.36856(18) 0.78579(6) 0.26536(17) 0.0360(4) Uani 1 1 d . . . . .
O3 O 0.66474(14) 0.59089(7) 0.32118(14) 0.0259(3) Uani 1 1 d . . . . .
O4 O -0.08192(15) 0.65734(8) 0.19700(15) 0.0309(4) Uani 1 1 d . . . . .
O5 O 0.23544(15) 0.62786(7) 0.58345(12) 0.0257(3) Uani 1 1 d . . . . .
O6 O 0.21614(16) 0.46275(6) 0.25352(14) 0.0265(3) Uani 1 1 d . . . . .
O7 O 0.35162(15) 0.70273(6) 0.10189(13) 0.0248(3) Uani 1 1 d . . . . .
O8 O 0.50288(13) 0.60727(6) 0.12767(12) 0.0208(3) Uani 1 1 d . . . . .
O9 O 0.28131(15) 0.54274(7) 0.09707(12) 0.0233(3) Uani 1 1 d D . . . .
O10 O 0.13360(14) 0.63850(7) 0.07031(12) 0.0241(3) Uani 1 1 d . . . . .
O11 O 0.51207(13) 0.68815(6) 0.29303(13) 0.0218(3) Uani 1 1 d . . . . .
O12 O 0.43918(13) 0.52808(5) 0.28286(12) 0.0188(3) Uani 1 1 d . . . . .
O13 O 0.06901(13) 0.55933(6) 0.22797(12) 0.0206(3) Uani 1 1 d . . . . .
O14 O 0.14183(14) 0.72000(6) 0.23577(14) 0.0238(3) Uani 1 1 d . . . . .
O15 O 0.44844(13) 0.60912(6) 0.44970(11) 0.0187(3) Uani 1 1 d . . . . .
O16 O 0.22990(13) 0.54506(5) 0.41865(11) 0.0172(2) Uani 1 1 d . . . . .
O17 O 0.07816(13) 0.63991(6) 0.39159(12) 0.0193(3) Uani 1 1 d . . . . .
O18 O 0.30104(15) 0.70517(6) 0.42323(13) 0.0228(3) Uani 1 1 d . . . . .
O19 O 0.28665(12) 0.62053(5) 0.26764(11) 0.0146(2) Uani 1 1 d . . . . .
C1 C 0.2075(4) 0.62770(13) 0.6970(2) 0.0469(7) Uani 1 1 d . . . . .
H1A H 0.279334 0.645153 0.739958 0.070 Uiso 1 1 calc R U . . .
H1B H 0.196689 0.589383 0.722260 0.070 Uiso 1 1 calc R U . . .
H1C H 0.127086 0.648468 0.707920 0.070 Uiso 1 1 calc R U . . .
C2 C 0.1900(3) 0.40544(10) 0.2487(2) 0.0352(5) Uani 1 1 d . . . . .
H2A H 0.222724 0.390139 0.179597 0.053 Uiso 1 1 calc R U . . .
H2B H 0.095906 0.399345 0.250444 0.053 Uiso 1 1 calc R U . . .
H2C H 0.233208 0.386953 0.312533 0.053 Uiso 1 1 calc R U . . .
C3 C 0.2931(3) 0.74172(11) 0.0245(2) 0.0378(6) Uani 1 1 d . . . . .
H3A H 0.311491 0.779596 0.050262 0.057 Uiso 1 1 calc R U . . .
H3B H 0.198754 0.735820 0.019627 0.057 Uiso 1 1 calc R U . . .
H3C H 0.329074 0.736322 -0.048952 0.057 Uiso 1 1 calc R U . . .
C4 C 0.6063(2) 0.62634(12) 0.0631(2) 0.0357(6) Uani 1 1 d . . . . .
H4A H 0.604854 0.606450 -0.008034 0.054 Uiso 1 1 calc R U . . .
H4B H 0.689356 0.619563 0.103329 0.054 Uiso 1 1 calc R U . . .
H4C H 0.596028 0.666198 0.049216 0.054 Uiso 1 1 calc R U . . .
C5 C 0.2141(6) 0.50881(17) 0.0162(3) 0.0370(10) Uani 0.721(10) 1 d D . P A 1
H5A H 0.229031 0.469618 0.034248 0.055 Uiso 0.721(10) 1 calc R U P A 1
H5B H 0.246420 0.516757 -0.057700 0.055 Uiso 0.721(10) 1 calc R U P A 1
H5C H 0.120659 0.516775 0.016670 0.055 Uiso 0.721(10) 1 calc R U P A 1
C5' C 0.2775(16) 0.5033(4) 0.0126(8) 0.0370(10) Uani 0.279(10) 1 d D . P A 5
H5D H 0.206930 0.476983 0.024784 0.055 Uiso 0.279(10) 1 calc R U P A 5
H5E H 0.360605 0.483426 0.012661 0.055 Uiso 0.279(10) 1 calc R U P A 5
H5F H 0.262371 0.521832 -0.059329 0.055 Uiso 0.279(10) 1 calc R U P A 5
C6 C 0.0473(3) 0.62454(15) -0.0193(2) 0.0484(8) Uani 1 1 d . . . . .
H6A H -0.029668 0.648454 -0.017752 0.073 Uiso 1 1 d R U . . .
H6B H 0.020781 0.585662 -0.012660 0.073 Uiso 1 1 d R U . . .
H6C H 0.090685 0.629893 -0.089629 0.073 Uiso 1 1 d R U . . .
C7 C 0.6203(2) 0.72029(10) 0.2616(2) 0.0335(5) Uani 1 1 d . . . . .
H7A H 0.700032 0.698276 0.271484 0.050 Uiso 1 1 calc R U . . .
H7B H 0.627044 0.753576 0.308262 0.050 Uiso 1 1 calc R U . . .
H7C H 0.608631 0.731208 0.183383 0.050 Uiso 1 1 calc R U . . .
C8 C 0.5128(2) 0.48685(9) 0.2269(2) 0.0288(5) Uani 1 1 d . . . . .
H8A H 0.472384 0.450414 0.236377 0.043 Uiso 1 1 calc R U . . .
H8B H 0.601957 0.486129 0.258532 0.043 Uiso 1 1 calc R U . . .
H8C H 0.514247 0.495812 0.147476 0.043 Uiso 1 1 calc R U . . .
C9 C -0.0396(2) 0.52624(11) 0.2526(3) 0.0379(6) Uani 1 1 d . . . . .
H9A H -0.043122 0.493890 0.203211 0.057 Uiso 1 1 calc R U . . .
H9B H -0.119439 0.548074 0.241481 0.057 Uiso 1 1 calc R U . . .
H9C H -0.031619 0.513819 0.330119 0.057 Uiso 1 1 calc R U . . .
C10 C 0.0681(2) 0.76006(10) 0.2939(2) 0.0320(5) Uani 1 1 d . . . . .
H10A H -0.020636 0.761548 0.261447 0.048 Uiso 1 1 calc R U . . .
H10B H 0.109049 0.796592 0.287825 0.048 Uiso 1 1 calc R U . . .
H10C H 0.065341 0.749538 0.372526 0.048 Uiso 1 1 calc R U . . .
C11 C 0.5341(2) 0.63014(10) 0.5355(2) 0.0309(5) Uani 1 1 d . . . . .
H11A H 0.488821 0.631268 0.605744 0.046 Uiso 1 1 calc R U . . .
H11B H 0.561971 0.667667 0.516058 0.046 Uiso 1 1 calc R U . . .
H11C H 0.610414 0.605941 0.543877 0.046 Uiso 1 1 calc R U . . .
C12 C 0.2743(2) 0.50516(9) 0.49910(18) 0.0241(4) Uani 1 1 d . . . . .
H12A H 0.236063 0.468900 0.480787 0.036 Uiso 1 1 calc R U . . .
H12B H 0.247928 0.516635 0.573093 0.036 Uiso 1 1 calc R U . . .
H12D H 0.369353 0.502550 0.498673 0.036 Uiso 1 1 calc R U . . .
C13 C -0.0270(2) 0.62299(12) 0.4565(2) 0.0321(5) Uani 1 1 d . . . . .
H13A H -0.028167 0.645499 0.524348 0.048 Uiso 1 1 calc R U . . .
H13D H -0.016373 0.583799 0.476629 0.048 Uiso 1 1 calc R U . . .
H13B H -0.108985 0.627964 0.413562 0.048 Uiso 1 1 calc R U . . .
C14 C 0.3368(3) 0.74450(11) 0.5073(2) 0.0400(6) Uani 1 1 d . . . . .
H14D H 0.311835 0.730461 0.579927 0.060 Uiso 1 1 calc R U . . .
H14A H 0.292149 0.779716 0.491667 0.060 Uiso 1 1 calc R U . . .
H14B H 0.431145 0.750399 0.508218 0.060 Uiso 1 1 calc R U . . .


_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
V1 O1 1.6054(17) . ?
V1 O8 1.9915(15) . ?
V1 O7 1.9947(17) . ?
V1 O10 2.0005(15) . ?
V1 O9 2.0168(16) . ?
V1 O19 2.4755(13) . ?
V2 O2 1.6022(16) . ?
V2 O7 1.9901(17) . ?
V2 O11 1.9947(15) . ?
V2 O14 2.0117(16) . ?
V2 O18 2.0180(16) . ?
V2 O19 2.4707(13) . ?
V3 O3 1.6009(15) . ?
V3 O8 1.9922(15) . ?
V3 O11 1.9926(15) . ?
V3 O12 2.0251(14) . ?
V3 O15 2.0285(15) . ?
V3 O19 2.3868(13) . ?
V4 O4 1.5952(15) . ?
V4 O10 1.9924(15) . ?
V4 O14 1.9992(16) . ?
V4 O17 2.0209(15) . ?
V4 O13 2.0288(15) . ?
V4 O19 2.3595(13) . ?
Ti1 O5 1.7421(15) . ?
Ti1 O18 1.9489(15) . ?
Ti1 O17 1.9731(14) . ?
Ti1 O15 1.9764(14) . ?
Ti1 O16 2.0107(14) . ?
Ti1 O19 2.1183(13) . ?
Ti2 O6 1.7417(15) . ?
Ti2 O9 1.9658(15) . ?
Ti2 O12 1.9699(14) . ?
Ti2 O13 1.9740(14) . ?
Ti2 O16 1.9919(14) . ?
Ti2 O19 2.1336(13) . ?
O5 C1 1.406(3) . ?
O6 C2 1.408(3) . ?
O7 C3 1.438(3) . ?
O8 C4 1.417(3) . ?
O9 C5' 1.391(7) . ?
O9 C5 1.429(4) . ?
O10 C6 1.410(3) . ?
O11 C7 1.419(2) . ?
O12 C8 1.433(2) . ?
O13 C9 1.413(3) . ?
O14 C10 1.427(3) . ?
O15 C11 1.425(2) . ?
O16 C12 1.427(2) . ?
O17 C13 1.418(2) . ?
O18 C14 1.425(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C5' H5D 0.9800 . ?
C5' H5E 0.9800 . ?
C5' H5F 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12D 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13D 0.9800 . ?
C13 H13B 0.9800 . ?
C14 H14D 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O8 100.58(8) . . ?
O1 V1 O7 103.13(9) . . ?
O8 V1 O7 88.77(6) . . ?
O1 V1 O10 103.03(8) . . ?
O8 V1 O10 156.39(6) . . ?
O7 V1 O10 86.58(7) . . ?
O1 V1 O9 100.91(9) . . ?
O8 V1 O9 87.50(6) . . ?
O7 V1 O9 155.95(6) . . ?
O10 V1 O9 87.38(7) . . ?
O1 V1 O19 176.48(8) . . ?
O8 V1 O19 78.73(5) . . ?
O7 V1 O19 80.33(5) . . ?
O10 V1 O19 77.67(5) . . ?
O9 V1 O19 75.64(5) . . ?
O2 V2 O7 102.23(9) . . ?
O2 V2 O11 101.22(8) . . ?
O7 V2 O11 89.31(6) . . ?
O2 V2 O14 102.56(8) . . ?
O7 V2 O14 87.70(7) . . ?
O11 V2 O14 156.12(6) . . ?
O2 V2 O18 101.83(9) . . ?
O7 V2 O18 155.93(6) . . ?
O11 V2 O18 86.71(6) . . ?
O14 V2 O18 86.42(7) . . ?
O2 V2 O19 177.19(8) . . ?
O7 V2 O19 80.54(5) . . ?
O11 V2 O19 78.22(5) . . ?
O14 V2 O19 77.92(5) . . ?
O18 V2 O19 75.41(5) . . ?
O3 V3 O8 103.77(7) . . ?
O3 V3 O11 103.62(7) . . ?
O8 V3 O11 88.65(6) . . ?
O3 V3 O12 100.14(7) . . ?
O8 V3 O12 87.01(6) . . ?
O11 V3 O12 156.20(6) . . ?
O3 V3 O15 99.89(7) . . ?
O8 V3 O15 156.29(6) . . ?
O11 V3 O15 87.28(6) . . ?
O12 V3 O15 87.36(6) . . ?
O3 V3 O19 173.79(7) . . ?
O8 V3 O19 80.93(5) . . ?
O11 V3 O19 80.34(5) . . ?
O12 V3 O19 75.87(5) . . ?
O15 V3 O19 75.36(5) . . ?
O4 V4 O10 100.74(8) . . ?
O4 V4 O14 100.58(8) . . ?
O10 V4 O14 88.91(7) . . ?
O4 V4 O17 102.94(8) . . ?
O10 V4 O17 156.30(6) . . ?
O14 V4 O17 87.73(6) . . ?
O4 V4 O13 102.72(8) . . ?
O10 V4 O13 87.79(6) . . ?
O14 V4 O13 156.68(6) . . ?
O17 V4 O13 86.09(6) . . ?
O4 V4 O19 177.94(7) . . ?
O10 V4 O19 80.69(5) . . ?
O14 V4 O19 80.89(5) . . ?
O17 V4 O19 75.61(5) . . ?
O13 V4 O19 75.79(5) . . ?
O5 Ti1 O18 97.67(7) . . ?
O5 Ti1 O17 96.81(7) . . ?
O18 Ti1 O17 90.86(6) . . ?
O5 Ti1 O15 97.66(7) . . ?
O18 Ti1 O15 90.13(6) . . ?
O17 Ti1 O15 165.23(6) . . ?
O5 Ti1 O16 96.79(7) . . ?
O18 Ti1 O16 165.49(6) . . ?
O17 Ti1 O16 88.52(6) . . ?
O15 Ti1 O16 86.85(6) . . ?
O5 Ti1 O19 176.57(7) . . ?
O18 Ti1 O19 85.69(6) . . ?
O17 Ti1 O19 82.45(5) . . ?
O15 Ti1 O19 82.94(5) . . ?
O16 Ti1 O19 79.85(5) . . ?
O6 Ti2 O9 97.60(7) . . ?
O6 Ti2 O12 97.46(7) . . ?
O9 Ti2 O12 88.04(6) . . ?
O6 Ti2 O13 97.00(7) . . ?
O9 Ti2 O13 89.31(6) . . ?
O12 Ti2 O13 165.52(6) . . ?
O6 Ti2 O16 97.27(7) . . ?
O9 Ti2 O16 165.10(6) . . ?
O12 Ti2 O16 89.17(6) . . ?
O13 Ti2 O16 89.74(6) . . ?
O6 Ti2 O19 177.10(7) . . ?
O9 Ti2 O19 85.23(6) . . ?
O12 Ti2 O19 83.20(5) . . ?
O13 Ti2 O19 82.39(5) . . ?
O16 Ti2 O19 79.90(5) . . ?
C1 O5 Ti1 176.63(19) . . ?
C2 O6 Ti2 178.60(17) . . ?
C3 O7 V2 115.92(16) . . ?
C3 O7 V1 115.99(16) . . ?
V2 O7 V1 114.05(7) . . ?
C4 O8 V1 115.74(14) . . ?
C4 O8 V3 122.34(14) . . ?
V1 O8 V3 113.67(7) . . ?
C5' O9 Ti2 129.3(5) . . ?
C5 O9 Ti2 120.3(2) . . ?
C5' O9 V1 121.1(5) . . ?
C5 O9 V1 121.6(2) . . ?
Ti2 O9 V1 109.61(7) . . ?
C6 O10 V4 119.68(16) . . ?
C6 O10 V1 121.48(15) . . ?
V4 O10 V1 113.95(7) . . ?
C7 O11 V3 122.24(14) . . ?
C7 O11 V2 116.79(13) . . ?
V3 O11 V2 114.14(7) . . ?
C8 O12 Ti2 120.51(13) . . ?
C8 O12 V3 117.31(13) . . ?
Ti2 O12 V3 109.01(6) . . ?
C9 O13 Ti2 122.17(15) . . ?
C9 O13 V4 124.40(14) . . ?
Ti2 O13 V4 108.90(6) . . ?
C10 O14 V4 116.86(14) . . ?
C10 O14 V2 117.32(15) . . ?
V4 O14 V2 113.20(7) . . ?
C11 O15 Ti1 122.54(13) . . ?
C11 O15 V3 117.75(14) . . ?
Ti1 O15 V3 108.96(6) . . ?
C12 O16 Ti2 122.03(13) . . ?
C12 O16 Ti1 121.63(13) . . ?
Ti2 O16 Ti1 104.25(6) . . ?
C13 O17 Ti1 121.61(13) . . ?
C13 O17 V4 123.39(13) . . ?
Ti1 O17 V4 108.80(6) . . ?
C14 O18 Ti1 128.16(16) . . ?
C14 O18 V2 120.41(15) . . ?
Ti1 O18 V2 109.45(7) . . ?
Ti1 O19 Ti2 95.99(5) . . ?
Ti1 O19 V4 92.83(5) . . ?
Ti2 O19 V4 92.78(5) . . ?
Ti1 O19 V3 92.51(5) . . ?
Ti2 O19 V3 91.86(5) . . ?
V4 O19 V3 172.53(6) . . ?
Ti1 O19 V2 89.44(5) . . ?
Ti2 O19 V2 174.51(6) . . ?
V4 O19 V2 87.75(4) . . ?
V3 O19 V2 87.08(4) . . ?
Ti1 O19 V1 174.45(6) . . ?
Ti2 O19 V1 89.52(5) . . ?
V4 O19 V1 87.61(4) . . ?
V3 O19 V1 86.58(4) . . ?
V2 O19 V1 85.04(4) . . ?
O5 C1 H1A 109.5 . . ?
O5 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O5 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O6 C2 H2A 109.5 . . ?
O6 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
O6 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O7 C3 H3A 109.5 . . ?
O7 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
O7 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O8 C4 H4A 109.5 . . ?
O8 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
O8 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O9 C5 H5A 109.5 . . ?
O9 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
O9 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O9 C5' H5D 109.5 . . ?
O9 C5' H5E 109.5 . . ?
H5D C5' H5E 109.5 . . ?
O9 C5' H5F 109.5 . . ?
H5D C5' H5F 109.5 . . ?
H5E C5' H5F 109.5 . . ?
O10 C6 H6A 109.3 . . ?
O10 C6 H6B 109.6 . . ?
H6A C6 H6B 109.5 . . ?
O10 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O11 C7 H7A 109.5 . . ?
O11 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
O11 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O12 C8 H8A 109.5 . . ?
O12 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O12 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O13 C9 H9A 109.5 . . ?
O13 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
O13 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O14 C10 H10A 109.5 . . ?
O14 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
O14 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O15 C11 H11A 109.5 . . ?
O15 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
O15 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O16 C12 H12A 109.5 . . ?
O16 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O16 C12 H12D 109.5 . . ?
H12A C12 H12D 109.5 . . ?
H12B C12 H12D 109.5 . . ?
O17 C13 H13A 109.5 . . ?
O17 C13 H13D 109.5 . . ?
H13A C13 H13D 109.5 . . ?
O17 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13D C13 H13B 109.5 . . ?
O18 C14 H14D 109.5 . . ?
O18 C14 H14A 109.5 . . ?
H14D C14 H14A 109.5 . . ?
O18 C14 H14B 109.5 . . ?
H14D C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?


_refine_diff_density_max         1.488
_refine_diff_density_min         -1.014
_refine_diff_density_rms         0.113

####################################################################### 
# 
# 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_matlv10
_database_code_depnum_ccdc_archive 'CCDC 1825306'
_audit_update_record             
;
2018-02-22 deposited with the CCDC.
2018-04-20 downloaded from the CCDC.
;

_vrf_DIFMX02_matlv10             
; 
PROBLEM: _C  The maximum difference density is > 0.1*ZMAX*0.75 
            The relevant atom site should be identified. 
RESPONSE: There are residual peaks ranging from 1.00 to 1.97 
electrons per \%A^3^ near the metal centers of the cationic 
cluster containing atoms Ti2, Ti3, V4, V5, and V6. These peaks 
are likely due to a very minor component of disorder for the 
cluster for which only the metal center positions are found 
above the noise. This disorder was not modeled. 
;

_vrf_PLAT971_matlv10             
; 
PROBLEM: _C Check Calcd Residual Density  0.77A From  V7   1.89 eA-3 
         _C Check Calcd Residual Density  0.68A From  V5   1.69 eA-3 
RESPONSE: See response above to alert DIFMX02. 
;

_vrf_PLAT301_matlv10             
; 
PROBLEM: _G Main Residue Disorder ..............(Resd  1) .. 97% 
         _G Main Residue Disorder ..............(Resd  2) .. 5% 
RESPONSE: Methyl group C4 is modeled as disordered over two 
positions (0.51(1):0.49(1)). The cluster containing atoms Ti2, Ti3, 
V4, V5, and V6 is modeled as disordered over a crystallographic 
mirror plane (0.50:0.50). 
;

_vrf_PLAT302_matlv10             
; 
PROBLEM: _G Anion/Solvent/Minor-Residue Disorder (Resd  3-12) .. 100% 
RESPONSE: Both tetrachloroaluminate anions are modeled as disordered 
over crystallographic mirror planes (0.50:0.50), and the anion containing
Al2 is additionally modeled as disordered over three general positions 
(0.708(3):0.168(3):0.124(3)). All cocrystallized THF solvent molecules 
are modeled as disordered over crystallographic mirror planes (0.50:0.50), 
and the THF molecule containing atom O30 is additionally modeled as
disordered over two general positions (0.71(2):0.29(2)). 
;

_vrf_PLAT860_matlv10             
; 
PROBLEM: _G Number of Least-Squares Restraints ............. 269 
RESPONSE: For each disorder model, analogous bond lengths and angles 
among the different positions were restrained to be similar. Anisotropic 
displacement parameters for proximal and symmetry related atoms were 
restrained to be similar and/or constrained to be equivalent. 
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            matlv10
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H42 Cl O18 Ti2 V4, Al Cl4, 1.5(C4 H8 O)'
_chemical_formula_sum            'C20 H54 Al Cl5 O19.50 Ti2 V4'
_chemical_formula_weight         1110.42

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'
Al Al 0.0645 0.0514 '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'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 21/m'
_space_group_name_Hall           '-P 2yb'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

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

_cell_length_a                   19.3992(19)
_cell_length_b                   11.6179(11)
_cell_length_c                   19.5185(19)
_cell_angle_alpha                90
_cell_angle_beta                 96.728(2)
_cell_angle_gamma                90
_cell_volume                     4368.7(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.0(5)
_cell_measurement_reflns_used    3926
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      30.37

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_F_000             2256
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    1.560
_shelx_estimated_absorpt_T_min   0.574
_shelx_estimated_absorpt_T_max   0.800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4178
_exptl_absorpt_correction_T_max  0.4935
_exptl_absorpt_process_details   'SADABS-2016/2 (Krause et al., 2015)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100.0(5)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD platform'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            110728
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_av_R_equivalents  0.0771
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.044
_diffrn_reflns_theta_max         30.542
_diffrn_reflns_theta_full        30.508
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             13948
_reflns_number_gt                8655
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'APEX3 (Bruker, 2017)'
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2015a)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2015b)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_refine_special_details          
; 
There are residual peaks ranging from 1.00 to 1.97 electrons per 
Å³ near the metal centers of the cationic cluster containing 
atoms Ti2, Ti3, V4, V5, and V6. These peaks are likely due to a 
very minor component of disorder for the cluster for which only 
the metal center positions are found above the noise. This disorder 
was not modeled. 
  
Methyl group C4 is modeled as disordered over two positions 
(0.51(1):0.49(1)). The cluster containing atoms Ti2, Ti3, V4, V5, 
and V6 is modeled as disordered over a crystallographic mirror 
plane (0.50:0.50). Both tetrachloroaluminate anions are modeled
as disordered over crystallographic mirror planes (0.50:0.50), and
the anion containing Al2 is additionally modeled as disordered over
three general positions (0.708(3):0.168(3):0.124(3)). All cocrystallized
THF solvent molecules are modeled as disordered over crystallographic
mirror planes (0.50:0.50), and the THF molecule containing atom O30
is additionally modeled as disordered over two general positions
(0.71(2):0.29(2)). 
  
For each disorder model, analogous bond lengths and angles among 
the different positions were restrained to be similar. Anisotropic 
displacement parameters for proximal and symmetry related atoms were 
restrained to be similar and/or constrained to be equivalent. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0658P)²+8.8422P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_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         13948
_refine_ls_number_parameters     735
_refine_ls_number_restraints     269
_refine_ls_R_factor_all          0.1021
_refine_ls_R_factor_gt           0.0582
_refine_ls_wR_factor_ref         0.1670
_refine_ls_wR_factor_gt          0.1417
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.002
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.38252(4) 0.250000 0.28872(4) 0.02095(16) Uani 1 2 d S T P A .
V2 V 0.48262(3) 0.39238(5) 0.19161(3) 0.02458(13) Uani 1 1 d . . . . .
V3 V 0.41008(4) 0.250000 0.06148(4) 0.02417(17) Uani 1 2 d S T P A .
Ti1 Ti 0.31476(3) 0.38691(5) 0.15189(3) 0.02450(13) Uani 1 1 d . . . . .
Cl1 Cl 0.42658(8) 0.250000 -0.05556(6) 0.0434(3) Uani 1 2 d S T P . .
O1 O 0.37617(17) 0.250000 0.36960(17) 0.0296(8) Uani 1 2 d S T P . .
O2 O 0.53967(14) 0.4891(2) 0.20440(13) 0.0377(6) Uani 1 1 d . . . . .
O3 O 0.25165(14) 0.4916(3) 0.13611(13) 0.0380(6) Uani 1 1 d . . . . .
O4 O 0.39807(13) 0.4869(2) 0.17061(12) 0.0306(5) Uani 1 1 d . . . . .
O5 O 0.45533(12) 0.3713(2) 0.28367(11) 0.0255(5) Uani 1 1 d . . . . .
O6 O 0.31295(12) 0.3684(2) 0.25096(11) 0.0258(5) Uani 1 1 d D . . . .
O7 O 0.48127(13) 0.3682(2) 0.09248(12) 0.0302(5) Uani 1 1 d . . . . .
O8 O 0.33732(13) 0.3699(2) 0.05584(12) 0.0333(6) Uani 1 1 d . . . . .
O9 O 0.53693(17) 0.250000 0.20754(17) 0.0275(7) Uani 1 2 d S T P . .
O10 O 0.25312(17) 0.250000 0.13584(16) 0.0286(8) Uani 1 2 d S T P . .
O11 O 0.38954(15) 0.250000 0.16731(15) 0.0195(6) Uani 1 2 d S T P . .
C1 C 0.1958(3) 0.5711(5) 0.1242(3) 0.0620(15) Uani 1 1 d . . . . .
H1A H 0.213962 0.649831 0.128161 0.093 Uiso 1 1 calc R U . . .
H1B H 0.163376 0.559050 0.158460 0.093 Uiso 1 1 calc R U . . .
H1C H 0.171552 0.559222 0.077819 0.093 Uiso 1 1 calc R U . . .
C2 C 0.4026(3) 0.6024(4) 0.1486(3) 0.0641(16) Uani 1 1 d . . . . .
H2A H 0.428155 0.605471 0.108219 0.096 Uiso 1 1 calc R U . . .
H2B H 0.426902 0.648492 0.185952 0.096 Uiso 1 1 calc R U . . .
H2C H 0.355733 0.633349 0.136353 0.096 Uiso 1 1 calc R U . . .
C3 C 0.4516(2) 0.4714(4) 0.32641(19) 0.0391(9) Uani 1 1 d . . . . .
H3D H 0.494252 0.516569 0.326402 0.059 Uiso 1 1 calc R U . . .
H3E H 0.446369 0.447347 0.373657 0.059 Uiso 1 1 calc R U . . .
H3F H 0.411637 0.518422 0.308315 0.059 Uiso 1 1 calc R U . . .
C4 C 0.2712(5) 0.4337(9) 0.2940(4) 0.0377(16) Uani 0.485(10) 1 d D . P A 1
H4A H 0.293641 0.433534 0.341715 0.057 Uiso 0.485(10) 1 calc R U P A 1
H4B H 0.225068 0.398693 0.292364 0.057 Uiso 0.485(10) 1 calc R U P A 1
H4C H 0.266614 0.513146 0.277207 0.057 Uiso 0.485(10) 1 calc R U P A 1
C4' C 0.2476(4) 0.3809(9) 0.2797(5) 0.0377(16) Uani 0.515(10) 1 d D . P A 5
H4D H 0.224743 0.452255 0.262619 0.057 Uiso 0.515(10) 1 calc R U P A 5
H4E H 0.256374 0.383505 0.330123 0.057 Uiso 0.515(10) 1 calc R U P A 5
H4F H 0.217459 0.315192 0.265644 0.057 Uiso 0.515(10) 1 calc R U P A 5
C5 C 0.5428(2) 0.3969(4) 0.0616(2) 0.0415(10) Uani 1 1 d . . . . .
H5D H 0.550803 0.480135 0.065020 0.062 Uiso 1 1 calc R U . . .
H5E H 0.536765 0.374098 0.012920 0.062 Uiso 1 1 calc R U . . .
H5F H 0.582675 0.356190 0.085759 0.062 Uiso 1 1 calc R U . . .
C6 C 0.3172(3) 0.4480(4) 0.00178(19) 0.0466(11) Uani 1 1 d . . . . .
H6D H 0.332156 0.418708 -0.041205 0.070 Uiso 1 1 calc R U . . .
H6E H 0.338960 0.522927 0.012777 0.070 Uiso 1 1 calc R U . . .
H6F H 0.266629 0.456585 -0.003770 0.070 Uiso 1 1 calc R U . . .
C7 C 0.5936(3) 0.250000 0.2630(3) 0.0395(13) Uani 1 2 d S T P . .
H7D H 0.611355 0.171467 0.270403 0.059 Uiso 0.5 1 calc R U P . .
H7E H 0.576930 0.278403 0.305335 0.059 Uiso 0.5 1 calc R U P . .
H7F H 0.630860 0.300129 0.250611 0.059 Uiso 0.5 1 calc R U P . .
C8 C 0.1918(3) 0.250000 0.0863(3) 0.0400(14) Uani 1 2 d S T P . .
H8D H 0.203063 0.282576 0.042602 0.060 Uiso 0.5 1 calc R U P . .
H8E H 0.155604 0.296543 0.103852 0.060 Uiso 0.5 1 calc R U P . .
H8F H 0.175144 0.170882 0.078633 0.060 Uiso 0.5 1 calc R U P . .
V4 V 0.23510(5) 0.2522(10) 0.51022(5) 0.0284(4) Uani 0.5 1 d D . P B -1
V5 V 0.1338(4) 0.1203(7) 0.60737(17) 0.0287(3) Uani 0.5 1 d . . P B -1
V6 V 0.3086(4) 0.1152(8) 0.6462(2) 0.0273(2) Uani 0.5 1 d D . P B -1
V7 V 0.3016(4) 0.3997(8) 0.6495(2) 0.0273(2) Uani 0.5 1 d D . P B -1
Ti2 Ti 0.20364(6) 0.2410(19) 0.73865(5) 0.0219(17) Uani 0.5 1 d D . P B -1
Ti3 Ti 0.1428(5) 0.3926(7) 0.60716(18) 0.0287(3) Uani 0.5 1 d D . P B -1
Cl2 Cl 0.05485(15) -0.0159(3) 0.58548(16) 0.0631(7) Uani 0.5 1 d . . P B -1
O12 O 0.2449(2) 0.2646(17) 0.43093(19) 0.027(3) Uani 0.5 1 d D . P B -1
O13 O 0.3707(5) 0.0208(9) 0.6574(4) 0.0342(10) Uani 0.5 1 d D . P B -1
O14 O 0.3566(5) 0.5056(8) 0.6569(4) 0.0342(10) Uani 0.5 1 d D . P B -1
O15 O 0.1916(2) 0.238(3) 0.8251(2) 0.029(4) Uani 0.5 1 d D U P B -1
O16 O 0.0853(4) 0.5042(8) 0.5900(5) 0.0631(7) Uani 0.5 1 d D . P B -1
O17 O 0.1661(5) 0.1257(12) 0.5133(5) 0.0283(11) Uani 0.5 1 d D . P B -1
O18 O 0.3032(5) 0.1475(13) 0.5434(4) 0.0256(13) Uani 0.5 1 d D . P B -1
O19 O 0.2999(4) 0.3729(13) 0.5470(4) 0.0256(13) Uani 0.5 1 d D . P B -1
O20 O 0.1631(5) 0.3565(12) 0.5077(5) 0.0283(11) Uani 0.5 1 d D . P B -1
O21 O 0.2107(3) 0.0142(6) 0.6262(4) 0.0264(6) Uani 0.5 1 d D . P B -1
O22 O 0.36056(19) 0.2630(6) 0.66338(19) 0.0264(6) Uani 0.5 1 d D . P B -1
O23 O 0.2277(3) 0.4854(6) 0.6247(4) 0.0264(6) Uani 0.5 1 d D . P B -1
O24 O 0.0767(2) 0.2659(5) 0.5887(2) 0.0264(6) Uani 0.5 1 d D . P B -1
O25 O 0.1283(5) 0.1436(11) 0.7077(4) 0.0254(12) Uani 0.5 1 d D . P B -1
O26 O 0.2717(9) 0.1252(11) 0.7383(6) 0.0256(9) Uani 0.5 1 d D . P B -1
O27 O 0.2781(9) 0.3639(11) 0.7448(6) 0.0256(9) Uani 0.5 1 d D . P B -1
O28 O 0.1365(5) 0.3818(11) 0.7062(4) 0.0254(12) Uani 0.5 1 d D . P B -1
O29 O 0.21278(17) 0.250000 0.63021(15) 0.0220(6) Uani 1 2 d S T P . .
C9 C 0.1884(5) 0.267(2) 0.8968(4) 0.057(5) Uani 0.5 1 d D U P B -1
H9A H 0.151715 0.221616 0.914488 0.085 Uiso 0.5 1 calc R U P B -1
H9B H 0.178292 0.349079 0.900904 0.085 Uiso 0.5 1 calc R U P B -1
H9C H 0.233093 0.249244 0.923575 0.085 Uiso 0.5 1 calc R U P B -1
C10 C 0.0346(6) 0.6014(11) 0.5796(5) 0.0631(7) Uani 0.5 1 d D . P B -1
H10A H 0.003258 0.588553 0.537102 0.095 Uiso 0.5 1 calc R U P B -1
H10B H 0.059704 0.673845 0.575940 0.095 Uiso 0.5 1 calc R U P B -1
H10C H 0.007472 0.605339 0.618866 0.095 Uiso 0.5 1 calc R U P B -1
C11 C 0.1631(5) 0.0357(8) 0.4640(4) 0.0458(15) Uani 0.5 1 d D . P B -1
H11A H 0.203997 -0.013852 0.473821 0.069 Uiso 0.5 1 calc R U P B -1
H11B H 0.162404 0.068583 0.417700 0.069 Uiso 0.5 1 calc R U P B -1
H11C H 0.120995 -0.009941 0.466426 0.069 Uiso 0.5 1 calc R U P B -1
C12 C 0.3190(5) 0.0529(7) 0.4991(4) 0.0400(13) Uani 0.5 1 d D . P B -1
H12A H 0.278616 0.002097 0.490771 0.060 Uiso 0.5 1 calc R U P B -1
H12B H 0.358662 0.009398 0.521567 0.060 Uiso 0.5 1 calc R U P B -1
H12C H 0.330518 0.083588 0.455039 0.060 Uiso 0.5 1 calc R U P B -1
C13 C 0.3677(4) 0.3759(8) 0.5211(4) 0.0400(13) Uani 0.5 1 d D . P B -1
H13A H 0.397597 0.315879 0.543941 0.060 Uiso 0.5 1 calc R U P B -1
H13B H 0.389220 0.451392 0.530805 0.060 Uiso 0.5 1 calc R U P B -1
H13C H 0.361764 0.362425 0.471183 0.060 Uiso 0.5 1 calc R U P B -1
C14 C 0.1143(5) 0.3774(8) 0.4497(4) 0.0458(15) Uani 0.5 1 d D . P B -1
H14A H 0.138567 0.387461 0.408851 0.069 Uiso 0.5 1 calc R U P B -1
H14B H 0.087981 0.447304 0.457372 0.069 Uiso 0.5 1 calc R U P B -1
H14C H 0.082401 0.311917 0.442648 0.069 Uiso 0.5 1 calc R U P B -1
C15 C 0.2197(16) -0.1089(10) 0.624(2) 0.073(3) Uani 0.5 1 d D . P B -1
H15A H 0.265048 -0.126758 0.609369 0.109 Uiso 0.5 1 calc R U P B -1
H15B H 0.182945 -0.142677 0.591727 0.109 Uiso 0.5 1 calc R U P B -1
H15C H 0.217300 -0.140896 0.670370 0.109 Uiso 0.5 1 calc R U P B -1
C16 C 0.4152(3) 0.252(3) 0.7206(3) 0.043(2) Uani 0.5 1 d D . P B -1
H16A H 0.452444 0.306984 0.714453 0.065 Uiso 0.5 1 calc R U P B -1
H16B H 0.433679 0.173798 0.722002 0.065 Uiso 0.5 1 calc R U P B -1
H16C H 0.396238 0.269080 0.763905 0.065 Uiso 0.5 1 calc R U P B -1
C17 C 0.2222(16) 0.6087(10) 0.628(2) 0.073(3) Uani 0.5 1 d D . P B -1
H17A H 0.187275 0.629435 0.658515 0.109 Uiso 0.5 1 calc R U P B -1
H17B H 0.208308 0.639429 0.581869 0.109 Uiso 0.5 1 calc R U P B -1
H17C H 0.267182 0.641244 0.646555 0.109 Uiso 0.5 1 calc R U P B -1
C18 C 0.0020(3) 0.263(7) 0.5860(5) 0.069(10) Uani 0.5 1 d D . P B -1
H18A H -0.011952 0.301905 0.626816 0.104 Uiso 0.5 1 calc R U P B -1
H18B H -0.013835 0.183071 0.585174 0.104 Uiso 0.5 1 calc R U P B -1
H18C H -0.018764 0.302760 0.544310 0.104 Uiso 0.5 1 calc R U P B -1
C19 C 0.1020(5) 0.0503(10) 0.7473(5) 0.0463(18) Uani 0.5 1 d D . P B -1
H19A H 0.102787 0.074128 0.795591 0.069 Uiso 0.5 1 calc R U P B -1
H19B H 0.131371 -0.017868 0.744808 0.069 Uiso 0.5 1 calc R U P B -1
H19C H 0.054308 0.031959 0.728280 0.069 Uiso 0.5 1 calc R U P B -1
C20 C 0.2970(5) 0.0667(10) 0.8018(5) 0.0348(13) Uani 0.5 1 d D . P B -1
H20A H 0.323947 0.120630 0.832888 0.052 Uiso 0.5 1 calc R U P B -1
H20B H 0.326552 0.002078 0.791522 0.052 Uiso 0.5 1 calc R U P B -1
H20C H 0.257544 0.037900 0.823839 0.052 Uiso 0.5 1 calc R U P B -1
C21 C 0.2800(6) 0.4660(10) 0.7872(5) 0.0348(13) Uani 0.5 1 d D . P B -1
H21A H 0.325632 0.502591 0.788541 0.052 Uiso 0.5 1 calc R U P B -1
H21B H 0.271530 0.444867 0.834109 0.052 Uiso 0.5 1 calc R U P B -1
H21C H 0.244024 0.519931 0.767747 0.052 Uiso 0.5 1 calc R U P B -1
C22 C 0.0788(5) 0.4049(11) 0.7452(5) 0.0463(18) Uani 0.5 1 d D . P B -1
H22A H 0.047888 0.461824 0.720592 0.069 Uiso 0.5 1 calc R U P B -1
H22B H 0.096470 0.435013 0.790811 0.069 Uiso 0.5 1 calc R U P B -1
H22C H 0.053071 0.333514 0.750578 0.069 Uiso 0.5 1 calc R U P B -1
Al1 Al 0.17307(12) 0.7732(2) 0.32661(11) 0.0388(10) Uani 0.5 1 d D . P C -1
Cl3 Cl 0.1230(3) 0.6129(4) 0.3005(3) 0.0480(8) Uani 0.5 1 d D . P C -1
Cl4 Cl 0.26935(10) 0.7811(2) 0.28281(12) 0.0541(8) Uani 0.5 1 d D . P C -1
Cl5 Cl 0.19118(15) 0.7875(3) 0.43590(11) 0.0723(10) Uani 0.5 1 d D . P C -1
Cl6 Cl 0.1066(3) 0.9082(5) 0.2854(3) 0.0585(12) Uani 0.5 1 d D . P C -1
Al2 Al 0.20579(18) 0.7492(11) 0.91598(17) 0.0289(7) Uani 0.3542(14) 1 d D U P D
-1
Cl7 Cl 0.1512(5) 0.5900(6) 0.9213(4) 0.0329(6) Uani 0.3542(14) 1 d D . P D -1
Cl8 Cl 0.1402(4) 0.8943(6) 0.9278(4) 0.0329(6) Uani 0.3542(14) 1 d D . P D -1
Cl9 Cl 0.2470(3) 0.7620(11) 0.82001(19) 0.0756(18) Uani 0.3542(14) 1 d D . P D
-1
Cl10 Cl 0.28912(14) 0.752(2) 0.99809(18) 0.0511(8) Uani 0.3542(14) 1 d D U P D
-1
Al2' Al 0.1888(6) 0.7586(17) 0.9035(6) 0.030(3) Uani 0.0839(13) 1 d D U P E -5
Cl7' Cl 0.1272(8) 0.6151(17) 0.9275(11) 0.0329(6) Uani 0.0839(13) 1 d D . P E
-5
Cl8' Cl 0.1417(13) 0.915(2) 0.9312(15) 0.0329(6) Uani 0.0839(13) 1 d D . P E -5
Cl9' Cl 0.1960(10) 0.759(3) 0.7954(6) 0.0756(18) Uani 0.0839(13) 1 d D . P E -5
Cl0' Cl 0.2902(5) 0.745(3) 0.9590(8) 0.0511(8) Uani 0.0839(13) 1 d D . P E -5
Al2" Al 0.1834(6) 0.750000 0.8883(7) 0.027(3) Uani 0.124(2) 2 d DS TU P F 6
Cl7" Cl 0.1410(13) 0.5995(17) 0.9303(13) 0.0329(6) Uani 0.0619(12) 1 d D . P F
6
Cl8" Cl 0.1410(13) 0.9003(18) 0.9305(13) 0.0329(6) Uani 0.0619(12) 1 d D . P F
6
Cl9" Cl 0.1592(9) 0.750000 0.7791(6) 0.0756(18) Uani 0.124(2) 2 d DS T P F 6
Cl0" Cl 0.2933(6) 0.750000 0.9141(9) 0.0511(8) Uani 0.124(2) 2 d DS T P F 6
O30 O -0.0659(7) 0.8030(10) 0.7150(5) 0.103(4) Uani 0.353(8) 1 d D . P G -1
C23 C -0.0169(19) 0.706(3) 0.7278(10) 0.093(6) Uani 0.353(8) 1 d D . P G -1
H23A H -0.030665 0.640504 0.696437 0.111 Uiso 0.353(8) 1 calc R U P G -1
H23B H 0.030928 0.729507 0.721429 0.111 Uiso 0.353(8) 1 calc R U P G -1
C24 C -0.0219(14) 0.675(2) 0.7985(9) 0.073(6) Uani 0.353(8) 1 d D . P G -1
H24A H 0.019825 0.633542 0.820024 0.088 Uiso 0.353(8) 1 calc R U P G -1
H24B H -0.064114 0.629470 0.803936 0.088 Uiso 0.353(8) 1 calc R U P G -1
C25 C -0.0265(14) 0.808(3) 0.8274(10) 0.088(7) Uani 0.353(8) 1 d D . P G -1
H25A H -0.034891 0.811508 0.876440 0.105 Uiso 0.353(8) 1 calc R U P G -1
H25B H 0.014867 0.854759 0.820259 0.105 Uiso 0.353(8) 1 calc R U P G -1
C26 C -0.0868(13) 0.840(3) 0.7810(7) 0.092(6) Uani 0.353(8) 1 d D . P G -1
H26A H -0.095466 0.923876 0.781732 0.110 Uiso 0.353(8) 1 calc R U P G -1
H26B H -0.128762 0.798451 0.791946 0.110 Uiso 0.353(8) 1 calc R U P G -1
O31 O 0.4631(6) 0.6438(8) 0.4810(5) 0.091(3) Uani 0.5 1 d D . P H -1
C27 C 0.4514(6) 0.6945(9) 0.5429(6) 0.066(3) Uani 0.5 1 d D . P H -1
H27A H 0.493898 0.733941 0.564062 0.079 Uiso 0.5 1 calc R U P H -1
H27B H 0.438290 0.635345 0.575544 0.079 Uiso 0.5 1 calc R U P H -1
C28 C 0.3936(7) 0.7797(8) 0.5274(6) 0.075(4) Uani 0.5 1 d D . P H -1
H28A H 0.396679 0.842950 0.561590 0.090 Uiso 0.5 1 calc R U P H -1
H28B H 0.347519 0.742323 0.525672 0.090 Uiso 0.5 1 calc R U P H -1
C29 C 0.4076(10) 0.8224(12) 0.4563(7) 0.090(5) Uani 0.5 1 d D . P H -1
H29A H 0.364350 0.847104 0.428206 0.108 Uiso 0.5 1 calc R U P H -1
H29B H 0.441326 0.886735 0.459928 0.108 Uiso 0.5 1 calc R U P H -1
C30 C 0.4377(10) 0.7156(10) 0.4267(6) 0.105(6) Uani 0.5 1 d D . P H -1
H30A H 0.401307 0.675242 0.395872 0.126 Uiso 0.5 1 calc R U P H -1
H30B H 0.475611 0.737202 0.399395 0.126 Uiso 0.5 1 calc R U P H -1
O32 O -0.0564(3) 0.7678(12) 0.0119(3) 0.044(3) Uani 0.5 1 d D . P I -1
C31 C -0.0041(6) 0.8320(10) 0.0511(8) 0.061(3) Uani 0.5 1 d D . P I -1
H31A H -0.024661 0.880543 0.085137 0.073 Uiso 0.5 1 calc R U P I -1
H31B H 0.019653 0.882876 0.020593 0.073 Uiso 0.5 1 calc R U P I -1
C32 C 0.0471(4) 0.748(3) 0.0878(5) 0.068(3) Uani 0.5 1 d D . P I -1
H32A H 0.055789 0.766187 0.137599 0.082 Uiso 0.5 1 calc R U P I -1
H32B H 0.091743 0.750198 0.067904 0.082 Uiso 0.5 1 calc R U P I -1
C33 C 0.0128(6) 0.6316(12) 0.0765(7) 0.068(4) Uani 0.5 1 d D . P I -1
H33A H -0.014460 0.611388 0.114569 0.082 Uiso 0.5 1 calc R U P I -1
H33B H 0.047344 0.570299 0.071482 0.082 Uiso 0.5 1 calc R U P I -1
C34 C -0.0340(5) 0.6515(9) 0.0092(5) 0.049(2) Uani 0.5 1 d D . P I -1
H34A H -0.008037 0.639102 -0.030922 0.059 Uiso 0.5 1 calc R U P I -1
H34B H -0.074204 0.598462 0.005538 0.059 Uiso 0.5 1 calc R U P I -1
O30' O -0.0659(7) 0.8030(10) 0.7150(5) 0.103(4) Uani 0.147(8) 1 d D . P G -5
C23' C -0.017(4) 0.707(6) 0.7116(17) 0.093(6) Uani 0.147(8) 1 d D . P G -5
H23C H -0.040748 0.631603 0.707430 0.111 Uiso 0.147(8) 1 calc R U P G -5
H23D H 0.011560 0.716220 0.672866 0.111 Uiso 0.147(8) 1 calc R U P G -5
C24' C 0.0249(16) 0.719(4) 0.7773(15) 0.073(6) Uani 0.147(8) 1 d D . P G -5
H24C H 0.053712 0.789241 0.780302 0.088 Uiso 0.147(8) 1 calc R U P G -5
H24D H 0.054311 0.650355 0.789569 0.088 Uiso 0.147(8) 1 calc R U P G -5
C25' C -0.0419(19) 0.728(5) 0.8228(14) 0.088(7) Uani 0.147(8) 1 d D . P G -5
H25C H -0.073895 0.661398 0.815612 0.105 Uiso 0.147(8) 1 calc R U P G -5
H25D H -0.027652 0.739859 0.872682 0.105 Uiso 0.147(8) 1 calc R U P G -5
C26' C -0.069(4) 0.830(6) 0.7882(10) 0.092(6) Uani 0.147(8) 1 d D . P G -5
H26C H -0.040006 0.898134 0.802603 0.110 Uiso 0.147(8) 1 calc R U P G -5
H26D H -0.117314 0.845200 0.797413 0.110 Uiso 0.147(8) 1 calc R U P G -5


_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
V1 O1 1.598(3) . ?
V1 O5 2.006(2) 4_565 ?
V1 O5 2.006(2) . ?
V1 O6 2.006(2) . ?
V1 O6 2.006(2) 4_565 ?
V1 O11 2.390(3) . ?
V1 Ti1 3.2508(9) . ?
V1 Ti1 3.2508(9) 4_565 ?
V2 O2 1.577(3) . ?
V2 O5 1.947(2) . ?
V2 O7 1.952(2) . ?
V2 O9 1.9662(18) . ?
V2 O4 1.976(3) . ?
V2 O11 2.454(2) . ?
V2 Ti1 3.2584(9) . ?
V3 O8 1.977(3) 4_565 ?
V3 O8 1.977(3) . ?
V3 O7 1.991(3) . ?
V3 O7 1.991(3) 4_565 ?
V3 O11 2.149(3) . ?
V3 Cl1 2.3437(15) . ?
V3 Ti1 3.1348(9) . ?
V3 Ti1 3.1349(9) 4_565 ?
Ti1 O3 1.727(3) . ?
Ti1 O6 1.950(2) . ?
Ti1 O8 1.984(2) . ?
Ti1 O4 1.989(3) . ?
Ti1 O10 1.993(2) . ?
Ti1 O11 2.150(2) . ?
Ti1 Ti1 3.1812(13) 4_565 ?
O3 C1 1.422(5) . ?
O4 C2 1.415(5) . ?
O5 C3 1.438(4) . ?
O6 C4 1.449(6) . ?
O6 C4' 1.453(6) . ?
O7 C5 1.438(4) . ?
O8 C6 1.412(4) . ?
O9 C7 1.449(6) . ?
O10 C8 1.443(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3D 0.9800 . ?
C3 H3E 0.9800 . ?
C3 H3F 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C4' H4D 0.9800 . ?
C4' H4E 0.9800 . ?
C4' H4F 0.9800 . ?
C5 H5D 0.9800 . ?
C5 H5E 0.9800 . ?
C5 H5F 0.9800 . ?
C6 H6D 0.9800 . ?
C6 H6E 0.9800 . ?
C6 H6F 0.9800 . ?
C7 H7D 0.9800 . ?
C7 H7E 0.9800 . ?
C7 H7F 0.9800 . ?
C7 H7D 0.980(14) 4_565 ?
C7 H7E 0.98(3) 4_565 ?
C7 H7F 0.98(4) 4_565 ?
C8 H8D 0.9800 . ?
C8 H8E 0.9800 . ?
C8 H8F 0.9800 . ?
C8 H8D 0.98(3) 4_565 ?
C8 H8E 0.98(4) 4_565 ?
C8 H8F 0.980(9) 4_565 ?
V4 O12 1.588(4) . ?
V4 O20 1.845(15) . ?
V4 O18 1.856(15) . ?
V4 O19 1.962(15) . ?
V4 O17 1.995(16) . ?
V4 O29 2.431(3) . ?
V4 Ti3 3.200(12) . ?
V5 O21 1.937(7) . ?
V5 O25 1.993(7) . ?
V5 O17 2.009(11) . ?
V5 O24 2.032(6) . ?
V5 O29 2.158(11) . ?
V5 Cl2 2.209(11) . ?
V5 Ti2 3.091(12) . ?
V5 Ti3 3.1686(17) . ?
V6 O13 1.624(6) . ?
V6 O22 2.000(8) . ?
V6 O26 2.014(15) . ?
V6 O18 2.033(8) . ?
V6 O21 2.226(7) . ?
V6 O29 2.422(12) . ?
V6 Ti2 3.224(15) . ?
V7 O14 1.624(6) . ?
V7 O23 1.766(7) . ?
V7 O22 1.957(7) . ?
V7 O27 2.010(15) . ?
V7 O19 2.020(9) . ?
V7 O29 2.447(12) . ?
V7 Ti3 3.096(11) . ?
Ti2 O15 1.731(4) . ?
Ti2 O26 1.89(2) . ?
Ti2 O25 1.89(2) . ?
Ti2 O27 2.02(2) . ?
Ti2 O28 2.14(2) . ?
Ti2 O29 2.147(3) . ?
Ti2 Ti3 3.220(14) . ?
Ti3 O16 1.717(10) . ?
Ti3 O28 1.956(8) . ?
Ti3 O24 1.958(5) . ?
Ti3 O23 1.965(7) . ?
Ti3 O20 2.068(10) . ?
Ti3 O29 2.156(12) . ?
O15 C9 1.446(13) . ?
O16 C10 1.496(12) . ?
O17 C11 1.418(13) . ?
O18 C12 1.453(13) . ?
O19 C13 1.465(10) . ?
O20 C14 1.409(11) . ?
O21 C15 1.442(10) . ?
O22 C16 1.452(8) . ?
O23 C17 1.438(11) . ?
O24 C18 1.443(7) . ?
O25 C19 1.457(12) . ?
O26 C20 1.447(12) . ?
O27 C21 1.446(11) . ?
O28 C22 1.450(10) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
Al1 Cl6 2.127(4) . ?
Al1 Cl5 2.127(3) . ?
Al1 Cl3 2.134(4) . ?
Al1 Cl4 2.145(3) . ?
Al2 Cl9 2.126(4) . ?
Al2 Cl10 2.139(4) . ?
Al2 Cl7 2.139(6) . ?
Al2 Cl8 2.141(6) . ?
Al2' Cl9' 2.131(7) . ?
Al2' Cl7' 2.136(8) . ?
Al2' Cl8' 2.136(8) . ?
Al2' Cl0' 2.137(7) . ?
Al2" Cl9" 2.127(7) . ?
Al2" Cl0" 2.133(7) . ?
Al2" Cl8" 2.136(8) . ?
Al2" Cl8" 2.136(8) 4_575 ?
Al2" Cl7" 2.136(8) . ?
Al2" Cl7" 2.136(8) 4_575 ?
Cl7" Cl8" 0.01(6) 4_575 ?
O30 C26 1.460(14) . ?
O30 C23 1.480(14) . ?
C23 C24 1.44(3) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.66(2) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.44(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
O31 C27 1.388(12) . ?
O31 C30 1.393(13) . ?
C27 C28 1.500(12) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.529(17) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.513(14) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
O32 C31 1.410(11) . ?
O32 C34 1.422(13) . ?
C31 C32 1.511(19) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.51(3) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.524(13) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
O30' C26' 1.472(18) . ?
O30' C23' 1.477(17) . ?
C23' C24' 1.44(3) . ?
C23' H23C 0.9900 . ?
C23' H23D 0.9900 . ?
C24' C25' 1.66(3) . ?
C24' H24C 0.9900 . ?
C24' H24D 0.9900 . ?
C25' C26' 1.44(3) . ?
C25' H25C 0.9900 . ?
C25' H25D 0.9900 . ?
C26' H26C 0.9900 . ?
C26' H26D 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O5 100.65(11) . 4_565 ?
O1 V1 O5 100.64(11) . . ?
O5 V1 O5 89.26(14) 4_565 . ?
O1 V1 O6 103.69(11) . . ?
O5 V1 O6 155.66(10) 4_565 . ?
O5 V1 O6 86.99(10) . . ?
O1 V1 O6 103.69(11) . 4_565 ?
O5 V1 O6 86.99(10) 4_565 4_565 ?
O5 V1 O6 155.66(10) . 4_565 ?
O6 V1 O6 86.59(14) . 4_565 ?
O1 V1 O11 178.86(15) . . ?
O5 V1 O11 80.15(8) 4_565 . ?
O5 V1 O11 80.15(8) . . ?
O6 V1 O11 75.51(8) . . ?
O6 V1 O11 75.51(8) 4_565 . ?
O1 V1 Ti1 137.83(9) . . ?
O5 V1 Ti1 121.51(7) 4_565 . ?
O5 V1 Ti1 80.52(7) . . ?
O6 V1 Ti1 34.18(6) . . ?
O6 V1 Ti1 81.02(7) 4_565 . ?
O11 V1 Ti1 41.39(5) . . ?
O1 V1 Ti1 137.83(9) . 4_565 ?
O5 V1 Ti1 80.52(7) 4_565 4_565 ?
O5 V1 Ti1 121.51(7) . 4_565 ?
O6 V1 Ti1 81.01(7) . 4_565 ?
O6 V1 Ti1 34.18(6) 4_565 4_565 ?
O11 V1 Ti1 41.39(5) . 4_565 ?
Ti1 V1 Ti1 58.59(3) . 4_565 ?
O2 V2 O5 101.85(12) . . ?
O2 V2 O7 100.79(12) . . ?
O5 V2 O7 157.35(10) . . ?
O2 V2 O9 102.80(13) . . ?
O5 V2 O9 86.94(12) . . ?
O7 V2 O9 88.88(12) . . ?
O2 V2 O4 100.77(13) . . ?
O5 V2 O4 87.28(10) . . ?
O7 V2 O4 87.71(10) . . ?
O9 V2 O4 156.41(11) . . ?
O2 V2 O11 176.56(12) . . ?
O5 V2 O11 79.63(10) . . ?
O7 V2 O11 77.72(10) . . ?
O9 V2 O11 80.33(9) . . ?
O4 V2 O11 76.14(9) . . ?
O2 V2 Ti1 135.64(11) . . ?
O5 V2 Ti1 81.08(7) . . ?
O7 V2 Ti1 82.21(8) . . ?
O9 V2 Ti1 121.55(8) . . ?
O4 V2 Ti1 34.87(7) . . ?
O11 V2 Ti1 41.29(5) . . ?
O8 V3 O8 89.59(17) 4_565 . ?
O8 V3 O7 165.53(10) 4_565 . ?
O8 V3 O7 89.78(11) . . ?
O8 V3 O7 89.78(11) 4_565 4_565 ?
O8 V3 O7 165.53(10) . 4_565 ?
O7 V3 O7 87.23(15) . 4_565 ?
O8 V3 O11 80.90(9) 4_565 . ?
O8 V3 O11 80.91(9) . . ?
O7 V3 O11 84.72(9) . . ?
O7 V3 O11 84.72(9) 4_565 . ?
O8 V3 Cl1 97.12(8) 4_565 . ?
O8 V3 Cl1 97.12(8) . . ?
O7 V3 Cl1 97.30(8) . . ?
O7 V3 Cl1 97.31(8) 4_565 . ?
O11 V3 Cl1 177.19(10) . . ?
O8 V3 Ti1 85.67(8) 4_565 . ?
O8 V3 Ti1 37.76(7) . . ?
O7 V3 Ti1 85.00(7) . . ?
O7 V3 Ti1 127.79(7) 4_565 . ?
O11 V3 Ti1 43.19(6) . . ?
Cl1 V3 Ti1 134.88(4) . . ?
O8 V3 Ti1 37.76(7) 4_565 4_565 ?
O8 V3 Ti1 85.67(8) . 4_565 ?
O7 V3 Ti1 127.80(7) . 4_565 ?
O7 V3 Ti1 85.00(7) 4_565 4_565 ?
O11 V3 Ti1 43.20(6) . 4_565 ?
Cl1 V3 Ti1 134.88(4) . 4_565 ?
Ti1 V3 Ti1 60.98(3) . 4_565 ?
O3 Ti1 O6 99.19(11) . . ?
O3 Ti1 O8 97.58(11) . . ?
O6 Ti1 O8 163.23(10) . . ?
O3 Ti1 O4 99.51(13) . . ?
O6 Ti1 O4 89.47(10) . . ?
O8 Ti1 O4 88.13(11) . . ?
O3 Ti1 O10 97.71(13) . . ?
O6 Ti1 O10 89.30(12) . . ?
O8 Ti1 O10 88.09(12) . . ?
O4 Ti1 O10 162.71(11) . . ?
O3 Ti1 O11 176.56(12) . . ?
O6 Ti1 O11 82.52(10) . . ?
O8 Ti1 O11 80.71(11) . . ?
O4 Ti1 O11 83.45(9) . . ?
O10 Ti1 O11 79.29(10) . . ?
O3 Ti1 V3 135.18(9) . . ?
O6 Ti1 V3 125.63(7) . . ?
O8 Ti1 V3 37.60(7) . . ?
O4 Ti1 V3 83.08(7) . . ?
O10 Ti1 V3 83.64(9) . . ?
O11 Ti1 V3 43.17(8) . . ?
O3 Ti1 Ti1 134.74(10) . 4_565 ?
O6 Ti1 Ti1 83.67(7) . 4_565 ?
O8 Ti1 Ti1 84.28(8) . 4_565 ?
O4 Ti1 Ti1 125.73(7) . 4_565 ?
O10 Ti1 Ti1 37.04(7) . 4_565 ?
O11 Ti1 Ti1 42.29(6) . 4_565 ?
V3 Ti1 Ti1 59.510(14) . 4_565 ?
O3 Ti1 V1 134.49(9) . . ?
O6 Ti1 V1 35.30(7) . . ?
O8 Ti1 V1 127.93(8) . . ?
O4 Ti1 V1 83.87(7) . . ?
O10 Ti1 V1 85.18(8) . . ?
O11 Ti1 V1 47.30(8) . . ?
V3 Ti1 V1 90.33(2) . . ?
Ti1 Ti1 V1 60.707(13) 4_565 . ?
O3 Ti1 V2 134.13(11) . . ?
O6 Ti1 V2 84.25(7) . . ?
O8 Ti1 V2 84.37(8) . . ?
O4 Ti1 V2 34.62(7) . . ?
O10 Ti1 V2 128.14(8) . . ?
O11 Ti1 V2 48.86(6) . . ?
V3 Ti1 V2 60.32(2) . . ?
Ti1 Ti1 V2 91.119(15) 4_565 . ?
V1 Ti1 V2 61.148(19) . . ?
C1 O3 Ti1 175.5(3) . . ?
C2 O4 V2 120.7(3) . . ?
C2 O4 Ti1 125.1(3) . . ?
V2 O4 Ti1 110.51(12) . . ?
C3 O5 V2 118.1(2) . . ?
C3 O5 V1 117.1(2) . . ?
V2 O5 V1 113.76(11) . . ?
C4 O6 Ti1 126.4(4) . . ?
C4' O6 Ti1 119.3(4) . . ?
C4 O6 V1 122.9(4) . . ?
C4' O6 V1 120.5(4) . . ?
Ti1 O6 V1 110.51(11) . . ?
C5 O7 V2 117.8(2) . . ?
C5 O7 V3 127.8(2) . . ?
V2 O7 V3 109.19(11) . . ?
C6 O8 V3 128.9(2) . . ?
C6 O8 Ti1 124.7(2) . . ?
V3 O8 Ti1 104.64(11) . . ?
C7 O9 V2 117.62(12) . 4_565 ?
C7 O9 V2 117.62(12) . . ?
V2 O9 V2 114.55(16) 4_565 . ?
C8 O10 Ti1 122.54(12) . 4_565 ?
C8 O10 Ti1 122.54(12) . . ?
Ti1 O10 Ti1 105.93(15) 4_565 . ?
V3 O11 Ti1 93.64(10) . . ?
V3 O11 Ti1 93.64(10) . 4_565 ?
Ti1 O11 Ti1 95.43(12) . 4_565 ?
V3 O11 V1 172.64(15) . . ?
Ti1 O11 V1 91.31(9) . . ?
Ti1 O11 V1 91.31(9) 4_565 . ?
V3 O11 V2 88.32(9) . . ?
Ti1 O11 V2 89.86(3) . . ?
Ti1 O11 V2 174.23(12) 4_565 . ?
V1 O11 V2 86.24(9) . . ?
V3 O11 V2 88.32(9) . 4_565 ?
Ti1 O11 V2 174.23(12) . 4_565 ?
Ti1 O11 V2 89.86(3) 4_565 4_565 ?
V1 O11 V2 86.24(9) . 4_565 ?
V2 O11 V2 84.77(10) . 4_565 ?
O3 C1 H1A 109.5 . . ?
O3 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O3 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O4 C2 H2A 109.5 . . ?
O4 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
O4 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O5 C3 H3D 109.5 . . ?
O5 C3 H3E 109.5 . . ?
H3D C3 H3E 109.5 . . ?
O5 C3 H3F 109.5 . . ?
H3D C3 H3F 109.5 . . ?
H3E C3 H3F 109.5 . . ?
O6 C4 H4A 109.5 . . ?
O6 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
O6 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O6 C4' H4D 109.5 . . ?
O6 C4' H4E 109.5 . . ?
H4D C4' H4E 109.5 . . ?
O6 C4' H4F 109.5 . . ?
H4D C4' H4F 109.5 . . ?
H4E C4' H4F 109.5 . . ?
O7 C5 H5D 109.5 . . ?
O7 C5 H5E 109.5 . . ?
H5D C5 H5E 109.5 . . ?
O7 C5 H5F 109.5 . . ?
H5D C5 H5F 109.5 . . ?
H5E C5 H5F 109.5 . . ?
O8 C6 H6D 109.5 . . ?
O8 C6 H6E 109.5 . . ?
H6D C6 H6E 109.5 . . ?
O8 C6 H6F 109.5 . . ?
H6D C6 H6F 109.5 . . ?
H6E C6 H6F 109.5 . . ?
O9 C7 H7D 109.5 . . ?
O9 C7 H7E 109.5 . . ?
H7D C7 H7E 109.5 . . ?
O9 C7 H7F 109.5 . . ?
H7D C7 H7F 109.5 . . ?
H7E C7 H7F 109.5 . . ?
O9 C7 H7D 109.5(3) . 4_565 ?
O9 C7 H7E 109.5(7) . 4_565 ?
H7D C7 H7E 109.5 4_565 4_565 ?
O9 C7 H7F 109.5(9) . 4_565 ?
H7D C7 H7F 109.5 4_565 4_565 ?
H7E C7 H7F 109.5 4_565 4_565 ?
O10 C8 H8D 109.5 . . ?
O10 C8 H8E 109.5 . . ?
H8D C8 H8E 109.5 . . ?
O10 C8 H8F 109.5 . . ?
H8D C8 H8F 109.5 . . ?
H8E C8 H8F 109.5 . . ?
O10 C8 H8D 109.5(7) . 4_565 ?
O10 C8 H8E 109.5(9) . 4_565 ?
H8D C8 H8E 109.5 4_565 4_565 ?
O10 C8 H8F 109.47(18) . 4_565 ?
H8D C8 H8F 109.5 4_565 4_565 ?
H8E C8 H8F 109.5 4_565 4_565 ?
O12 V4 O20 95.3(7) . . ?
O12 V4 O18 103.8(6) . . ?
O20 V4 O18 160.9(4) . . ?
O12 V4 O19 98.5(7) . . ?
O20 V4 O19 89.5(7) . . ?
O18 V4 O19 86.66(18) . . ?
O12 V4 O17 104.7(7) . . ?
O20 V4 O17 88.6(2) . . ?
O18 V4 O17 87.7(6) . . ?
O19 V4 O17 156.8(4) . . ?
O12 V4 O29 174.3(8) . . ?
O20 V4 O29 79.2(3) . . ?
O18 V4 O29 81.8(3) . . ?
O19 V4 O29 80.4(3) . . ?
O17 V4 O29 76.5(3) . . ?
O12 V4 Ti3 132.0(7) . . ?
O20 V4 Ti3 37.5(3) . . ?
O18 V4 Ti3 123.5(3) . . ?
O19 V4 Ti3 78.4(3) . . ?
O17 V4 Ti3 86.2(4) . . ?
O29 V4 Ti3 42.33(17) . . ?
O21 V5 O25 91.7(3) . . ?
O21 V5 O17 83.0(4) . . ?
O25 V5 O17 162.3(8) . . ?
O21 V5 O24 162.9(7) . . ?
O25 V5 O24 88.4(3) . . ?
O17 V5 O24 91.8(4) . . ?
O21 V5 O29 83.8(4) . . ?
O25 V5 O29 79.7(5) . . ?
O17 V5 O29 83.0(6) . . ?
O24 V5 O29 79.3(3) . . ?
O21 V5 Cl2 94.7(4) . . ?
O25 V5 Cl2 99.9(6) . . ?
O17 V5 Cl2 97.4(5) . . ?
O24 V5 Cl2 102.1(4) . . ?
O29 V5 Cl2 178.48(18) . . ?
O21 V5 Ti2 83.0(4) . . ?
O25 V5 Ti2 36.1(5) . . ?
O17 V5 Ti2 126.2(6) . . ?
O24 V5 Ti2 87.0(4) . . ?
O29 V5 Ti2 44.0(3) . . ?
Cl2 V5 Ti2 135.4(4) . . ?
O21 V5 Ti3 126.5(7) . . ?
O25 V5 Ti3 82.8(4) . . ?
O17 V5 Ti3 86.8(6) . . ?
O24 V5 Ti3 36.62(13) . . ?
O29 V5 Ti3 42.7(3) . . ?
Cl2 V5 Ti3 138.8(4) . . ?
Ti2 V5 Ti3 61.9(4) . . ?
O13 V6 O22 101.9(4) . . ?
O13 V6 O26 104.8(6) . . ?
O22 V6 O26 91.5(5) . . ?
O13 V6 O18 102.0(7) . . ?
O22 V6 O18 88.4(4) . . ?
O26 V6 O18 152.6(9) . . ?
O13 V6 O21 105.7(5) . . ?
O22 V6 O21 152.2(7) . . ?
O26 V6 O21 78.6(4) . . ?
O18 V6 O21 88.8(3) . . ?
O13 V6 O29 177.8(3) . . ?
O22 V6 O29 80.2(4) . . ?
O26 V6 O29 74.4(7) . . ?
O18 V6 O29 78.6(5) . . ?
O21 V6 O29 72.1(3) . . ?
O13 V6 Ti2 137.6(4) . . ?
O22 V6 Ti2 81.7(5) . . ?
O26 V6 Ti2 33.0(6) . . ?
O18 V6 Ti2 120.4(6) . . ?
O21 V6 Ti2 75.9(4) . . ?
O29 V6 Ti2 41.8(3) . . ?
O14 V7 O23 95.8(5) . . ?
O14 V7 O22 103.6(4) . . ?
O23 V7 O22 159.7(7) . . ?
O14 V7 O27 107.0(6) . . ?
O23 V7 O27 96.0(5) . . ?
O22 V7 O27 84.0(4) . . ?
O14 V7 O19 98.1(7) . . ?
O23 V7 O19 84.1(4) . . ?
O22 V7 O19 87.4(4) . . ?
O27 V7 O19 154.8(9) . . ?
O14 V7 O29 174.9(4) . . ?
O23 V7 O29 79.9(4) . . ?
O22 V7 O29 80.4(4) . . ?
O27 V7 O29 76.3(7) . . ?
O19 V7 O29 78.9(5) . . ?
O14 V7 Ti3 131.8(4) . . ?
O23 V7 Ti3 36.0(3) . . ?
O22 V7 Ti3 124.2(5) . . ?
O27 V7 Ti3 85.1(6) . . ?
O19 V7 Ti3 80.3(3) . . ?
O29 V7 Ti3 43.9(2) . . ?
O15 Ti2 O26 99.5(12) . . ?
O15 Ti2 O25 96.5(10) . . ?
O26 Ti2 O25 95.0(10) . . ?
O15 Ti2 O27 97.6(11) . . ?
O26 Ti2 O27 90.47(18) . . ?
O25 Ti2 O27 163.8(6) . . ?
O15 Ti2 O28 98.9(12) . . ?
O26 Ti2 O28 161.2(5) . . ?
O25 Ti2 O28 86.7(3) . . ?
O27 Ti2 O28 83.3(9) . . ?
O15 Ti2 O29 176.5(10) . . ?
O26 Ti2 O29 83.8(5) . . ?
O25 Ti2 O29 82.2(4) . . ?
O27 Ti2 O29 83.3(5) . . ?
O28 Ti2 O29 77.8(4) . . ?
O15 Ti2 V5 134.8(11) . . ?
O26 Ti2 V5 85.0(6) . . ?
O25 Ti2 V5 38.4(3) . . ?
O27 Ti2 V5 127.5(5) . . ?
O28 Ti2 V5 84.8(2) . . ?
O29 Ti2 V5 44.2(3) . . ?
O15 Ti2 Ti3 135.0(12) . . ?
O26 Ti2 Ti3 125.4(4) . . ?
O25 Ti2 Ti3 82.8(3) . . ?
O27 Ti2 Ti3 81.6(6) . . ?
O28 Ti2 Ti3 36.2(3) . . ?
O29 Ti2 Ti3 41.6(3) . . ?
V5 Ti2 Ti3 60.23(6) . . ?
O15 Ti2 V6 134.7(11) . . ?
O26 Ti2 V6 35.5(4) . . ?
O25 Ti2 V6 93.7(6) . . ?
O27 Ti2 V6 82.0(4) . . ?
O28 Ti2 V6 125.7(3) . . ?
O29 Ti2 V6 48.7(2) . . ?
V5 Ti2 V6 64.8(3) . . ?
Ti3 Ti2 V6 89.9(2) . . ?
O16 Ti3 O28 97.3(7) . . ?
O16 Ti3 O24 97.8(5) . . ?
O28 Ti3 O24 91.1(3) . . ?
O16 Ti3 O23 97.6(4) . . ?
O28 Ti3 O23 90.6(3) . . ?
O24 Ti3 O23 164.2(7) . . ?
O16 Ti3 O20 99.3(6) . . ?
O28 Ti3 O20 162.9(9) . . ?
O24 Ti3 O20 82.4(4) . . ?
O23 Ti3 O20 91.6(4) . . ?
O16 Ti3 O29 178.3(4) . . ?
O28 Ti3 O29 81.7(5) . . ?
O24 Ti3 O29 81.0(3) . . ?
O23 Ti3 O29 83.7(4) . . ?
O20 Ti3 O29 81.7(6) . . ?
O16 Ti3 V7 129.4(4) . . ?
O28 Ti3 V7 85.0(4) . . ?
O24 Ti3 V7 132.8(5) . . ?
O23 Ti3 V7 31.9(3) . . ?
O20 Ti3 V7 87.9(4) . . ?
O29 Ti3 V7 51.8(3) . . ?
O16 Ti3 V5 136.0(5) . . ?
O28 Ti3 V5 85.7(4) . . ?
O24 Ti3 V5 38.25(15) . . ?
O23 Ti3 V5 126.4(7) . . ?
O20 Ti3 V5 79.4(5) . . ?
O29 Ti3 V5 42.8(3) . . ?
V7 Ti3 V5 94.6(5) . . ?
O16 Ti3 V4 131.7(4) . . ?
O28 Ti3 V4 131.0(7) . . ?
O24 Ti3 V4 84.7(3) . . ?
O23 Ti3 V4 82.4(4) . . ?
O20 Ti3 V4 32.9(4) . . ?
O29 Ti3 V4 49.4(3) . . ?
V7 Ti3 V4 64.1(2) . . ?
V5 Ti3 V4 61.7(4) . . ?
O16 Ti3 Ti2 137.5(5) . . ?
O28 Ti3 Ti2 40.2(5) . . ?
O24 Ti3 Ti2 84.7(4) . . ?
O23 Ti3 Ti2 86.5(4) . . ?
O20 Ti3 Ti2 123.0(7) . . ?
O29 Ti3 Ti2 41.4(3) . . ?
V7 Ti3 Ti2 62.7(3) . . ?
V5 Ti3 Ti2 57.9(4) . . ?
V4 Ti3 Ti2 90.8(4) . . ?
C9 O15 Ti2 165(3) . . ?
C10 O16 Ti3 176.6(8) . . ?
C11 O17 V4 119.8(7) . . ?
C11 O17 V5 127.3(9) . . ?
V4 O17 V5 109.4(7) . . ?
C12 O18 V4 118.6(7) . . ?
C12 O18 V6 117.3(9) . . ?
V4 O18 V6 114.7(7) . . ?
C13 O19 V4 117.0(6) . . ?
C13 O19 V7 115.3(6) . . ?
V4 O19 V7 114.1(7) . . ?
C14 O20 V4 124.7(7) . . ?
C14 O20 Ti3 122.4(8) . . ?
V4 O20 Ti3 109.6(7) . . ?
C15 O21 V5 136.0(14) . . ?
C15 O21 V6 115.1(14) . . ?
V5 O21 V6 108.7(5) . . ?
C16 O22 V7 122.5(13) . . ?
C16 O22 V6 111.3(13) . . ?
V7 O22 V6 113.51(18) . . ?
C17 O23 V7 127.6(15) . . ?
C17 O23 Ti3 119.3(14) . . ?
V7 O23 Ti3 112.1(6) . . ?
C18 O24 Ti3 131(3) . . ?
C18 O24 V5 121(3) . . ?
Ti3 O24 V5 105.13(18) . . ?
C19 O25 Ti2 125.5(7) . . ?
C19 O25 V5 118.9(9) . . ?
Ti2 O25 V5 105.4(6) . . ?
C20 O26 Ti2 120.0(9) . . ?
C20 O26 V6 128.1(12) . . ?
Ti2 O26 V6 111.5(8) . . ?
C21 O27 V7 111.5(9) . . ?
C21 O27 Ti2 125.7(11) . . ?
V7 O27 Ti2 109.3(8) . . ?
C22 O28 Ti3 130.4(9) . . ?
C22 O28 Ti2 117.8(6) . . ?
Ti3 O28 Ti2 103.6(7) . . ?
Ti2 O29 Ti3 96.9(5) . . ?
Ti2 O29 V5 91.8(4) . . ?
Ti3 O29 V5 94.54(14) . . ?
Ti2 O29 V6 89.5(4) . . ?
Ti3 O29 V6 168.16(17) . . ?
V5 O29 V6 95.18(11) . . ?
Ti2 O29 V4 174.1(3) . . ?
Ti3 O29 V4 88.3(3) . . ?
V5 O29 V4 90.6(2) . . ?
V6 O29 V4 84.9(2) . . ?
Ti2 O29 V7 91.2(5) . . ?
Ti3 O29 V7 84.30(11) . . ?
V5 O29 V7 176.9(2) . . ?
V6 O29 V7 85.65(11) . . ?
V4 O29 V7 86.5(2) . . ?
O15 C9 H9A 109.5 . . ?
O15 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
O15 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O16 C10 H10A 109.5 . . ?
O16 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
O16 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O17 C11 H11A 109.5 . . ?
O17 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
O17 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O18 C12 H12A 109.5 . . ?
O18 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O18 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O19 C13 H13A 109.5 . . ?
O19 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
O19 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O20 C14 H14A 109.5 . . ?
O20 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O20 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O21 C15 H15A 109.5 . . ?
O21 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O21 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O22 C16 H16A 109.5 . . ?
O22 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O22 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O23 C17 H17A 109.5 . . ?
O23 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O23 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O24 C18 H18A 109.5 . . ?
O24 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O24 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O25 C19 H19A 109.5 . . ?
O25 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O25 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O26 C20 H20A 109.5 . . ?
O26 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O26 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O27 C21 H21A 109.5 . . ?
O27 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O27 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O28 C22 H22A 109.5 . . ?
O28 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
O28 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Cl6 Al1 Cl5 110.1(2) . . ?
Cl6 Al1 Cl3 108.33(14) . . ?
Cl5 Al1 Cl3 108.95(19) . . ?
Cl6 Al1 Cl4 109.6(2) . . ?
Cl5 Al1 Cl4 110.30(14) . . ?
Cl3 Al1 Cl4 109.59(19) . . ?
Cl9 Al2 Cl10 109.3(2) . . ?
Cl9 Al2 Cl7 110.0(5) . . ?
Cl10 Al2 Cl7 108.1(5) . . ?
Cl9 Al2 Cl8 109.2(5) . . ?
Cl10 Al2 Cl8 108.3(5) . . ?
Cl7 Al2 Cl8 111.8(2) . . ?
Cl9' Al2' Cl7' 108.9(6) . . ?
Cl9' Al2' Cl8' 109.1(6) . . ?
Cl7' Al2' Cl8' 110.0(7) . . ?
Cl9' Al2' Cl0' 109.9(6) . . ?
Cl7' Al2' Cl0' 109.7(6) . . ?
Cl8' Al2' Cl0' 109.3(6) . . ?
Cl9" Al2" Cl0" 109.5(6) . . ?
Cl9" Al2" Cl8" 109.7(7) . . ?
Cl0" Al2" Cl8" 109.2(7) . . ?
Cl9" Al2" Cl8" 109.7(7) . 4_575 ?
Cl0" Al2" Cl8" 109.2(7) . 4_575 ?
Cl8" Al2" Cl8" 109.7(17) . 4_575 ?
Cl9" Al2" Cl7" 109.5(7) . . ?
Cl0" Al2" Cl7" 109.2(7) . . ?
Cl8" Al2" Cl7" 109.8(7) . . ?
Cl8" Al2" Cl7" 0.1(15) 4_575 . ?
C26 O30 C23 108.4(13) . . ?
C24 C23 O30 103.8(16) . . ?
C24 C23 H23A 111.0 . . ?
O30 C23 H23A 111.0 . . ?
C24 C23 H23B 111.0 . . ?
O30 C23 H23B 111.0 . . ?
H23A C23 H23B 109.0 . . ?
C23 C24 C25 96.0(17) . . ?
C23 C24 H24A 112.5 . . ?
C25 C24 H24A 112.5 . . ?
C23 C24 H24B 112.5 . . ?
C25 C24 H24B 112.5 . . ?
H24A C24 H24B 110.1 . . ?
C26 C25 C24 95.6(18) . . ?
C26 C25 H25A 112.6 . . ?
C24 C25 H25A 112.6 . . ?
C26 C25 H25B 112.6 . . ?
C24 C25 H25B 112.6 . . ?
H25A C25 H25B 110.1 . . ?
C25 C26 O30 101.0(13) . . ?
C25 C26 H26A 111.6 . . ?
O30 C26 H26A 111.6 . . ?
C25 C26 H26B 111.6 . . ?
O30 C26 H26B 111.6 . . ?
H26A C26 H26B 109.4 . . ?
C27 O31 C30 109.2(10) . . ?
O31 C27 C28 107.4(8) . . ?
O31 C27 H27A 110.2 . . ?
C28 C27 H27A 110.2 . . ?
O31 C27 H27B 110.2 . . ?
C28 C27 H27B 110.2 . . ?
H27A C27 H27B 108.5 . . ?
C27 C28 C29 100.9(9) . . ?
C27 C28 H28A 111.6 . . ?
C29 C28 H28A 111.6 . . ?
C27 C28 H28B 111.6 . . ?
C29 C28 H28B 111.6 . . ?
H28A C28 H28B 109.4 . . ?
C30 C29 C28 101.4(9) . . ?
C30 C29 H29A 111.5 . . ?
C28 C29 H29A 111.5 . . ?
C30 C29 H29B 111.5 . . ?
C28 C29 H29B 111.5 . . ?
H29A C29 H29B 109.3 . . ?
O31 C30 C29 108.6(9) . . ?
O31 C30 H30A 110.0 . . ?
C29 C30 H30A 110.0 . . ?
O31 C30 H30B 110.0 . . ?
C29 C30 H30B 110.0 . . ?
H30A C30 H30B 108.4 . . ?
C31 O32 C34 108.6(8) . . ?
O32 C31 C32 107.8(12) . . ?
O32 C31 H31A 110.1 . . ?
C32 C31 H31A 110.1 . . ?
O32 C31 H31B 110.1 . . ?
C32 C31 H31B 110.1 . . ?
H31A C31 H31B 108.5 . . ?
C31 C32 C33 104.8(9) . . ?
C31 C32 H32A 110.8 . . ?
C33 C32 H32A 110.8 . . ?
C31 C32 H32B 110.8 . . ?
C33 C32 H32B 110.8 . . ?
H32A C32 H32B 108.9 . . ?
C32 C33 C34 101.4(8) . . ?
C32 C33 H33A 111.5 . . ?
C34 C33 H33A 111.5 . . ?
C32 C33 H33B 111.5 . . ?
C34 C33 H33B 111.5 . . ?
H33A C33 H33B 109.3 . . ?
O32 C34 C33 105.4(9) . . ?
O32 C34 H34A 110.7 . . ?
C33 C34 H34A 110.7 . . ?
O32 C34 H34B 110.7 . . ?
C33 C34 H34B 110.7 . . ?
H34A C34 H34B 108.8 . . ?
C26' O30' C23' 107.8(18) . . ?
C24' C23' O30' 101(2) . . ?
C24' C23' H23C 111.6 . . ?
O30' C23' H23C 111.6 . . ?
C24' C23' H23D 111.6 . . ?
O30' C23' H23D 111.6 . . ?
H23C C23' H23D 109.4 . . ?
C23' C24' C25' 95(3) . . ?
C23' C24' H24C 112.7 . . ?
C25' C24' H24C 112.7 . . ?
C23' C24' H24D 112.7 . . ?
C25' C24' H24D 112.7 . . ?
H24C C24' H24D 110.2 . . ?
C26' C25' C24' 94(2) . . ?
C26' C25' H25C 113.0 . . ?
C24' C25' H25C 113.0 . . ?
C26' C25' H25D 113.0 . . ?
C24' C25' H25D 113.0 . . ?
H25C C25' H25D 110.4 . . ?
C25' C26' O30' 103(2) . . ?
C25' C26' H26C 111.2 . . ?
O30' C26' H26C 111.2 . . ?
C25' C26' H26D 111.2 . . ?
O30' C26' H26D 111.2 . . ?
H26C C26' H26D 109.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O26 Ti2 O15 C9 117(5) . . . . ?
O25 Ti2 O15 C9 -147(5) . . . . ?
O27 Ti2 O15 C9 25(5) . . . . ?
O28 Ti2 O15 C9 -60(5) . . . . ?
V5 Ti2 O15 C9 -151(4) . . . . ?
Ti3 Ti2 O15 C9 -61(4) . . . . ?
V6 Ti2 O15 C9 111(6) . . . . ?
O12 V4 O18 C12 -36.7(10) . . . . ?
O20 V4 O18 C12 147(2) . . . . ?
O19 V4 O18 C12 -134.6(7) . . . . ?
O17 V4 O18 C12 67.9(7) . . . . ?
O29 V4 O18 C12 144.6(7) . . . . ?
Ti3 V4 O18 C12 151.8(6) . . . . ?
O12 V4 O18 V6 177.7(8) . . . . ?
O20 V4 O18 V6 1(3) . . . . ?
O19 V4 O18 V6 79.7(7) . . . . ?
O17 V4 O18 V6 -77.8(6) . . . . ?
O29 V4 O18 V6 -1.1(5) . . . . ?
Ti3 V4 O18 V6 6.1(9) . . . . ?
O12 V4 O20 C14 30.5(13) . . . . ?
O18 V4 O20 C14 -152.8(19) . . . . ?
O19 V4 O20 C14 129.0(11) . . . . ?
O17 V4 O20 C14 -74.1(9) . . . . ?
O29 V4 O20 C14 -150.7(11) . . . . ?
Ti3 V4 O20 C14 -159.7(15) . . . . ?
O12 V4 O20 Ti3 -169.8(7) . . . . ?
O18 V4 O20 Ti3 7(3) . . . . ?
O19 V4 O20 Ti3 -71.3(6) . . . . ?
O17 V4 O20 Ti3 85.6(7) . . . . ?
O29 V4 O20 Ti3 9.0(5) . . . . ?
O14 V7 O23 C17 -12(2) . . . . ?
O22 V7 O23 C17 -176(2) . . . . ?
O27 V7 O23 C17 95(2) . . . . ?
O19 V7 O23 C17 -110(2) . . . . ?
O29 V7 O23 C17 170(2) . . . . ?
Ti3 V7 O23 C17 168(2) . . . . ?
O14 V7 O23 Ti3 179.1(5) . . . . ?
O22 V7 O23 Ti3 15.9(18) . . . . ?
O27 V7 O23 Ti3 -73.1(7) . . . . ?
O19 V7 O23 Ti3 81.5(7) . . . . ?
O29 V7 O23 Ti3 1.8(4) . . . . ?
O15 Ti2 O25 C19 -31.3(15) . . . . ?
O26 Ti2 O25 C19 69.0(8) . . . . ?
O27 Ti2 O25 C19 178(3) . . . . ?
O28 Ti2 O25 C19 -129.8(7) . . . . ?
O29 Ti2 O25 C19 152.0(7) . . . . ?
V5 Ti2 O25 C19 144.4(9) . . . . ?
Ti3 Ti2 O25 C19 -166.0(7) . . . . ?
V6 Ti2 O25 C19 104.6(6) . . . . ?
O15 Ti2 O25 V5 -175.6(12) . . . . ?
O26 Ti2 O25 V5 -75.4(6) . . . . ?
O27 Ti2 O25 V5 34(3) . . . . ?
O28 Ti2 O25 V5 85.8(5) . . . . ?
O29 Ti2 O25 V5 7.7(6) . . . . ?
Ti3 Ti2 O25 V5 49.7(5) . . . . ?
V6 Ti2 O25 V5 -39.8(5) . . . . ?
O15 Ti2 O26 C20 -0.5(15) . . . . ?
O25 Ti2 O26 C20 -98.0(9) . . . . ?
O27 Ti2 O26 C20 97.2(9) . . . . ?
O28 Ti2 O26 C20 168(2) . . . . ?
O29 Ti2 O26 C20 -179.6(9) . . . . ?
V5 Ti2 O26 C20 -135.1(9) . . . . ?
Ti3 Ti2 O26 C20 177.2(7) . . . . ?
V6 Ti2 O26 C20 172.6(13) . . . . ?
O15 Ti2 O26 V6 -173.1(11) . . . . ?
O25 Ti2 O26 V6 89.4(6) . . . . ?
O27 Ti2 O26 V6 -75.4(6) . . . . ?
O28 Ti2 O26 V6 -5(3) . . . . ?
O29 Ti2 O26 V6 7.8(7) . . . . ?
V5 Ti2 O26 V6 52.3(6) . . . . ?
Ti3 Ti2 O26 V6 4.6(11) . . . . ?
C26 O30 C23 C24 11(3) . . . . ?
O30 C23 C24 C25 -40(4) . . . . ?
C23 C24 C25 C26 57(3) . . . . ?
C24 C25 C26 O30 -50(3) . . . . ?
C23 O30 C26 C25 28(3) . . . . ?
C30 O31 C27 C28 21.7(15) . . . . ?
O31 C27 C28 C29 -34.2(12) . . . . ?
C27 C28 C29 C30 32.4(17) . . . . ?
C27 O31 C30 C29 1(2) . . . . ?
C28 C29 C30 O31 -22(2) . . . . ?
C34 O32 C31 C32 -12.6(13) . . . . ?
O32 C31 C32 C33 -10.0(13) . . . . ?
C31 C32 C33 C34 26.5(13) . . . . ?
C31 O32 C34 C33 30.1(13) . . . . ?
C32 C33 C34 O32 -34.7(13) . . . . ?
C26' O30' C23' C24' -23(6) . . . . ?
O30' C23' C24' C25' 49(5) . . . . ?
C23' C24' C25' C26' -61(5) . . . . ?
C24' C25' C26' O30' 46(5) . . . . ?
C23' O30' C26' C25' -19(5) . . . . ?

_refine_diff_density_max         1.971
_refine_diff_density_min         -1.239
_refine_diff_density_rms         0.111

