# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_cd214724
_database_code_depnum_ccdc_archive 'CCDC 1040902'
_audit_update_record             
;
2014-12-24 deposited with the CCDC.
2015-03-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H20 I N O'
_chemical_formula_weight         405.26

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.6819(17)
_cell_length_b                   9.4115(15)
_cell_length_c                   17.492(3)
_cell_angle_alpha                90
_cell_angle_beta                 92.723(4)
_cell_angle_gamma                90
_cell_volume                     1756.5(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3882
_cell_measurement_theta_min      4.916
_cell_measurement_theta_max      54.187

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_F_000             808
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.211
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.112
_exptl_absorpt_coefficient_mu    1.825
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5470
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10226
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.331
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3459
_reflns_number_gt                2785
_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       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 ? 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0445P)²+0.7842P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3459
_refine_ls_number_parameters     199
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0396
_refine_ls_wR_factor_ref         0.1034
_refine_ls_wR_factor_gt          0.0968
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
I1 I 0.21738(3) 1.34137(3) 0.04750(2) 0.07361(15) Uani 1 1 d . . . . .
N1 N 0.4272(2) 0.8548(3) 0.10096(14) 0.0411(6) Uani 1 1 d . . . . .
O1 O 0.5905(3) 0.7529(3) 0.22256(15) 0.0733(8) Uani 1 1 d . . . . .
C1 C 0.2080(3) 1.1249(3) 0.07985(18) 0.0423(6) Uani 1 1 d . . . . .
C2 C 0.2881(3) 1.0371(3) 0.04857(16) 0.0408(6) Uani 1 1 d . . . . .
H2 H 0.3408 1.0752 0.0131 0.049 Uiso 1 1 calc R U . . .
C3 C 0.3007(3) 0.8808(3) 0.06580(16) 0.0392(6) Uani 1 1 d . . . . .
H3 H 0.2376 0.8531 0.1019 0.047 Uiso 1 1 calc R U . . .
C4 C 0.2792(3) 0.7988(3) -0.00767(17) 0.0415(6) Uani 1 1 d . . . . .
C5 C 0.1725(3) 0.7172(4) -0.0203(2) 0.0511(8) Uani 1 1 d . . . . .
H5 H 0.1157 0.7083 0.0180 0.061 Uiso 1 1 calc R U . . .
C6 C 0.1499(3) 0.6491(4) -0.0895(2) 0.0585(9) Uani 1 1 d . . . . .
H6 H 0.0778 0.5948 -0.0975 0.070 Uiso 1 1 calc R U . . .
C7 C 0.2334(4) 0.6610(4) -0.1466(2) 0.0598(9) Uani 1 1 d . . . . .
H7 H 0.2177 0.6154 -0.1932 0.072 Uiso 1 1 calc R U . . .
C8 C 0.3397(4) 0.7403(4) -0.1344(2) 0.0638(10) Uani 1 1 d . . . . .
H8 H 0.3972 0.7475 -0.1725 0.077 Uiso 1 1 calc R U . . .
C9 C 0.3620(3) 0.8096(4) -0.06561(19) 0.0543(8) Uani 1 1 d . . . . .
H9 H 0.4340 0.8644 -0.0582 0.065 Uiso 1 1 calc R U . . .
C10 C 0.4497(3) 0.7041(4) 0.1138(2) 0.0566(8) Uani 1 1 d . . . . .
H10A H 0.4437 0.6540 0.0653 0.068 Uiso 1 1 calc R U . . .
H10B H 0.3864 0.6661 0.1461 0.068 Uiso 1 1 calc R U . . .
C11 C 0.5772(4) 0.6811(4) 0.1514(2) 0.0691(11) Uani 1 1 d . . . . .
H11A H 0.5908 0.5802 0.1595 0.083 Uiso 1 1 calc R U . . .
H11B H 0.6405 0.7152 0.1179 0.083 Uiso 1 1 calc R U . . .
C12 C 0.5699(4) 0.8995(5) 0.2106(2) 0.0661(10) Uani 1 1 d . . . . .
H12A H 0.6334 0.9365 0.1782 0.079 Uiso 1 1 calc R U . . .
H12B H 0.5779 0.9486 0.2593 0.079 Uiso 1 1 calc R U . . .
C13 C 0.4422(3) 0.9285(4) 0.17381(17) 0.0493(7) Uani 1 1 d . . . . .
H13A H 0.3782 0.8970 0.2075 0.059 Uiso 1 1 calc R U . . .
H13B H 0.4319 1.0299 0.1658 0.059 Uiso 1 1 calc R U . . .
C14 C 0.1106(3) 1.0902(3) 0.13393(17) 0.0419(6) Uani 1 1 d . . . . .
C15 C 0.1153(4) 1.1476(3) 0.2060(2) 0.0541(8) Uani 1 1 d . . . . .
H15 H 0.1803 1.2086 0.2213 0.065 Uiso 1 1 calc R U . . .
C16 C 0.0225(4) 1.1144(5) 0.2561(2) 0.0681(10) Uani 1 1 d . . . . .
H16 H 0.0255 1.1532 0.3051 0.082 Uiso 1 1 calc R U . . .
C17 C -0.0733(4) 1.0248(5) 0.2339(2) 0.0704(11) Uani 1 1 d . . . . .
H17 H -0.1353 1.0031 0.2676 0.084 Uiso 1 1 calc R U . . .
C18 C -0.0775(3) 0.9678(4) 0.1630(2) 0.0646(10) Uani 1 1 d . . . . .
H18 H -0.1426 0.9066 0.1480 0.078 Uiso 1 1 calc R U . . .
C19 C 0.0134(3) 0.9994(4) 0.11258(19) 0.0513(8) Uani 1 1 d . . . . .
H19 H 0.0094 0.9594 0.0639 0.062 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
I1 C1 2.118(3) . ?
N1 C13 1.453(4) . ?
N1 C10 1.455(4) . ?
N1 C3 1.479(4) . ?
O1 C12 1.411(5) . ?
O1 C11 1.417(5) . ?
C1 C2 1.326(4) . ?
C1 C14 1.476(4) . ?
C2 C3 1.506(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.507(4) . ?
C3 H3 0.9800 . ?
C4 C9 1.380(5) . ?
C4 C5 1.383(4) . ?
C5 C6 1.380(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.375(6) . ?
C6 H6 0.9300 . ?
C7 C8 1.367(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.379(5) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 C11 1.500(5) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.505(5) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.371(5) . ?
C14 C19 1.383(4) . ?
C15 C16 1.390(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.368(6) . ?
C16 H16 0.9300 . ?
C17 C18 1.351(6) . ?
C17 H17 0.9300 . ?
C18 C19 1.374(5) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?

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
C13 N1 C10 108.6(2) . . ?
C13 N1 C3 110.3(2) . . ?
C10 N1 C3 111.5(2) . . ?
C12 O1 C11 109.1(3) . . ?
C2 C1 C14 127.9(3) . . ?
C2 C1 I1 116.7(2) . . ?
C14 C1 I1 115.3(2) . . ?
C1 C2 C3 125.4(3) . . ?
C1 C2 H2 117.3 . . ?
C3 C2 H2 117.3 . . ?
N1 C3 C4 111.6(2) . . ?
N1 C3 C2 108.4(2) . . ?
C4 C3 C2 108.7(2) . . ?
N1 C3 H3 109.3 . . ?
C4 C3 H3 109.3 . . ?
C2 C3 H3 109.3 . . ?
C9 C4 C5 118.4(3) . . ?
C9 C4 C3 120.8(3) . . ?
C5 C4 C3 120.8(3) . . ?
C6 C5 C4 120.5(3) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C7 C6 C5 120.4(3) . . ?
C7 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
C8 C7 C6 119.6(3) . . ?
C8 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
C7 C8 C9 120.1(3) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?
C4 C9 C8 121.1(3) . . ?
C4 C9 H9 119.5 . . ?
C8 C9 H9 119.5 . . ?
N1 C10 C11 110.4(3) . . ?
N1 C10 H10A 109.6 . . ?
C11 C10 H10A 109.6 . . ?
N1 C10 H10B 109.6 . . ?
C11 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
O1 C11 C10 111.5(3) . . ?
O1 C11 H11A 109.3 . . ?
C10 C11 H11A 109.3 . . ?
O1 C11 H11B 109.3 . . ?
C10 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
O1 C12 C13 111.9(3) . . ?
O1 C12 H12A 109.2 . . ?
C13 C12 H12A 109.2 . . ?
O1 C12 H12B 109.2 . . ?
C13 C12 H12B 109.2 . . ?
H12A C12 H12B 107.9 . . ?
N1 C13 C12 110.4(3) . . ?
N1 C13 H13A 109.6 . . ?
C12 C13 H13A 109.6 . . ?
N1 C13 H13B 109.6 . . ?
C12 C13 H13B 109.6 . . ?
H13A C13 H13B 108.1 . . ?
C15 C14 C19 119.1(3) . . ?
C15 C14 C1 120.4(3) . . ?
C19 C14 C1 120.5(3) . . ?
C14 C15 C16 119.7(3) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
C17 C16 C15 120.4(4) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C18 C17 C16 119.9(4) . . ?
C18 C17 H17 120.1 . . ?
C16 C17 H17 120.1 . . ?
C17 C18 C19 120.6(4) . . ?
C17 C18 H18 119.7 . . ?
C19 C18 H18 119.7 . . ?
C18 C19 C14 120.3(3) . . ?
C18 C19 H19 119.8 . . ?
C14 C19 H19 119.8 . . ?

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
C14 C1 C2 C3 -3.6(5) . . . . ?
I1 C1 C2 C3 177.5(2) . . . . ?
C13 N1 C3 C4 -176.6(2) . . . . ?
C10 N1 C3 C4 -55.8(3) . . . . ?
C13 N1 C3 C2 63.7(3) . . . . ?
C10 N1 C3 C2 -175.6(3) . . . . ?
C1 C2 C3 N1 -116.4(3) . . . . ?
C1 C2 C3 C4 122.1(3) . . . . ?
N1 C3 C4 C9 -53.4(4) . . . . ?
C2 C3 C4 C9 66.2(4) . . . . ?
N1 C3 C4 C5 130.3(3) . . . . ?
C2 C3 C4 C5 -110.2(3) . . . . ?
C9 C4 C5 C6 -0.2(5) . . . . ?
C3 C4 C5 C6 176.2(3) . . . . ?
C4 C5 C6 C7 0.2(5) . . . . ?
C5 C6 C7 C8 0.4(6) . . . . ?
C6 C7 C8 C9 -1.0(6) . . . . ?
C5 C4 C9 C8 -0.4(5) . . . . ?
C3 C4 C9 C8 -176.8(3) . . . . ?
C7 C8 C9 C4 1.0(6) . . . . ?
C13 N1 C10 C11 -56.7(4) . . . . ?
C3 N1 C10 C11 -178.5(3) . . . . ?
C12 O1 C11 C10 -58.6(4) . . . . ?
N1 C10 C11 O1 59.1(4) . . . . ?
C11 O1 C12 C13 58.2(4) . . . . ?
C10 N1 C13 C12 56.2(4) . . . . ?
C3 N1 C13 C12 178.7(3) . . . . ?
O1 C12 C13 N1 -58.3(4) . . . . ?
C2 C1 C14 C15 117.9(4) . . . . ?
I1 C1 C14 C15 -63.3(3) . . . . ?
C2 C1 C14 C19 -62.2(4) . . . . ?
I1 C1 C14 C19 116.7(3) . . . . ?
C19 C14 C15 C16 -0.3(5) . . . . ?
C1 C14 C15 C16 179.7(3) . . . . ?
C14 C15 C16 C17 0.0(6) . . . . ?
C15 C16 C17 C18 0.3(6) . . . . ?
C16 C17 C18 C19 -0.2(6) . . . . ?
C17 C18 C19 C14 0.0(5) . . . . ?
C15 C14 C19 C18 0.3(5) . . . . ?
C1 C14 C19 C18 -179.7(3) . . . . ?

_refine_diff_density_max         0.705
_refine_diff_density_min         -0.836
_refine_diff_density_rms         0.097

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_mo_dm14708_0m
_database_code_depnum_ccdc_archive 'CCDC 1040903'
_audit_update_record             
;
2014-12-24 deposited with the CCDC.
2015-03-05 downloaded from the CCDC.
;
_audit_creation_date             2014-12-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C16 H26 Al O4 Ti'
_chemical_formula_sum            'C16 H26 Al O4 Ti'
_chemical_formula_weight         357.25
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.6563(14)
_cell_length_b                   9.8287(14)
_cell_length_c                   10.6494(16)
_cell_angle_alpha                64.408(2)
_cell_angle_beta                 74.407(2)
_cell_angle_gamma                73.803(2)
_cell_volume                     862.5(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2356
_cell_measurement_temperature    130
_cell_measurement_theta_max      30.24
_cell_measurement_theta_min      2.34
_shelx_estimated_absorpt_T_max   0.896
_shelx_estimated_absorpt_T_min   0.850
_exptl_absorpt_coefficient_mu    0.561
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6558
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0485 before and 0.0333 after correction.
The Ratio of minimum to maximum transmission is 0.8790.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             378
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0550
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8389
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.524
_diffrn_reflns_theta_min         2.152
_diffrn_ambient_temperature      130
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3793
_reflns_number_total             5183
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.364
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         5183
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0384
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0383P)²+0.0955P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0920
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C14(H14A,H14B), C15(H15A,H15B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C10(H10)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C16(H16A,H16B,H16C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.29108(3) 0.28300(4) 0.41345(3) 0.01721(8) Uani 1 1 d . . . . .
Al1 Al 0.37672(5) 0.42567(6) 0.54601(5) 0.01575(11) Uani 1 1 d . . . . .
O1 O 0.42786(12) 0.61692(13) 0.44162(12) 0.0171(2) Uani 1 1 d . . . . .
O2 O 0.38739(14) 0.85827(16) 0.16105(14) 0.0282(3) Uani 1 1 d . . . . .
O3 O 0.26274(13) 0.44464(15) 0.69503(13) 0.0235(3) Uani 1 1 d . . . . .
O4 O 0.08406(15) 0.26101(18) 1.05260(14) 0.0369(4) Uani 1 1 d . . . . .
C1 C 0.53057(19) 0.3049(2) 0.28024(19) 0.0247(4) Uani 1 1 d . . . . .
H1 H 0.6083 0.3009 0.3214 0.030 Uiso 1 1 calc R . . . .
C2 C 0.4369(2) 0.4378(2) 0.2093(2) 0.0298(4) Uani 1 1 d . . . . .
H2 H 0.4401 0.5399 0.1933 0.036 Uiso 1 1 calc R . . . .
C3 C 0.3371(2) 0.3936(3) 0.1659(2) 0.0355(5) Uani 1 1 d . . . . .
H3 H 0.2598 0.4605 0.1168 0.043 Uiso 1 1 calc R . . . .
C4 C 0.3715(2) 0.2342(3) 0.2076(2) 0.0331(5) Uani 1 1 d . . . . .
H4 H 0.3230 0.1741 0.1899 0.040 Uiso 1 1 calc R . . . .
C5 C 0.4901(2) 0.1780(2) 0.2803(2) 0.0279(4) Uani 1 1 d . . . . .
H5 H 0.5349 0.0733 0.3220 0.033 Uiso 1 1 calc R . . . .
C6 C 0.1861(2) 0.0653(2) 0.5521(2) 0.0261(4) Uani 1 1 d . . . . .
H6 H 0.2461 -0.0337 0.5712 0.031 Uiso 1 1 calc R . . . .
C7 C 0.1134(2) 0.1516(2) 0.4354(2) 0.0276(4) Uani 1 1 d . . . . .
H7 H 0.1141 0.1195 0.3629 0.033 Uiso 1 1 calc R . . . .
C8 C 0.03993(18) 0.2928(2) 0.4442(2) 0.0255(4) Uani 1 1 d . . . . .
H8 H -0.0160 0.3739 0.3780 0.031 Uiso 1 1 calc R . . . .
C9 C 0.06422(18) 0.2924(2) 0.5695(2) 0.0226(4) Uani 1 1 d . . . . .
H9 H 0.0264 0.3730 0.6031 0.027 Uiso 1 1 calc R . . . .
C10 C 0.15364(19) 0.1525(2) 0.6352(2) 0.0228(4) Uani 1 1 d . . . . .
H10 H 0.1868 0.1217 0.7215 0.027 Uiso 1 1 calc R . . . .
C11 C 0.32630(17) 0.75928(19) 0.41149(18) 0.0188(3) Uani 1 1 d . . . . .
H11A H 0.3739 0.8389 0.4067 0.023 Uiso 1 1 calc R . . . .
H11B H 0.2416 0.7480 0.4897 0.023 Uiso 1 1 calc R . . . .
C12 C 0.27232(18) 0.8117(2) 0.27485(18) 0.0205(3) Uani 1 1 d . . . . .
H12A H 0.2390 0.7267 0.2719 0.025 Uiso 1 1 calc R . . . .
H12B H 0.1885 0.8985 0.2676 0.025 Uiso 1 1 calc R . . . .
C13 C 0.3449(2) 0.9022(3) 0.0291(2) 0.0379(5) Uani 1 1 d . . . . .
H13A H 0.4240 0.9423 -0.0478 0.057 Uiso 1 1 calc GR . . . .
H13B H 0.2564 0.9820 0.0206 0.057 Uiso 1 1 calc GR . . . .
H13C H 0.3252 0.8128 0.0233 0.057 Uiso 1 1 calc GR . . . .
C14 C 0.25364(19) 0.3544(2) 0.83913(19) 0.0263(4) Uani 1 1 d . . . . .
H14A H 0.2930 0.4008 0.8850 0.032 Uiso 1 1 calc R . . . .
H14B H 0.3128 0.2505 0.8532 0.032 Uiso 1 1 calc R . . . .
C15 C 0.09592(19) 0.3430(2) 0.90515(19) 0.0262(4) Uani 1 1 d . . . . .
H15A H 0.0356 0.4473 0.8848 0.031 Uiso 1 1 calc R . . . .
H15B H 0.0589 0.2899 0.8639 0.031 Uiso 1 1 calc R . . . .
C16 C -0.0604(2) 0.2385(3) 1.1170(2) 0.0428(6) Uani 1 1 d . . . . .
H16A H -0.0895 0.1771 1.0798 0.064 Uiso 1 1 calc GR . . . .
H16B H -0.1268 0.3383 1.0965 0.064 Uiso 1 1 calc GR . . . .
H16C H -0.0652 0.1844 1.2194 0.064 Uiso 1 1 calc GR . . . .
H H 0.262(2) 0.458(2) 0.435(2) 0.024(5) Uiso 1 1 d . . . . .
HA H 0.398(2) 0.246(2) 0.541(2) 0.024(5) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 Al1 2.7619(6) . ?
Ti1 C1 2.3785(18) . ?
Ti1 C2 2.391(2) . ?
Ti1 C3 2.343(2) . ?
Ti1 C4 2.3285(19) . ?
Ti1 C5 2.3371(18) . ?
Ti1 C6 2.3370(19) . ?
Ti1 C7 2.3294(18) . ?
Ti1 C8 2.3384(17) . ?
Ti1 C9 2.3729(17) . ?
Ti1 C10 2.3732(18) . ?
Ti1 H 1.767(19) . ?
Ti1 HA 1.776(18) . ?
Al1 Al1 2.8657(10) 2_666 ?
Al1 O1 1.8435(12) 2_666 ?
Al1 O1 1.8521(13) . ?
Al1 O3 1.7224(13) . ?
Al1 H 1.705(19) . ?
Al1 HA 1.745(19) . ?
O1 Al1 1.8435(12) 2_666 ?
O1 C11 1.4277(19) . ?
O2 C12 1.412(2) . ?
O2 C13 1.420(2) . ?
O3 C14 1.394(2) . ?
O4 C15 1.411(2) . ?
O4 C16 1.411(2) . ?
C1 H1 0.9500 . ?
C1 C2 1.396(3) . ?
C1 C5 1.407(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.407(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.396(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.404(3) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C6 C7 1.408(3) . ?
C6 C10 1.404(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.402(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.414(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.399(3) . ?
C10 H10 0.9500 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.505(2) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.509(2) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 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
Al1 Ti1 H 36.5(6) . . ?
Al1 Ti1 HA 37.9(6) . . ?
C1 Ti1 Al1 81.24(5) . . ?
C1 Ti1 C2 34.05(6) . . ?
C1 Ti1 H 94.1(6) . . ?
C1 Ti1 HA 76.2(6) . . ?
C2 Ti1 Al1 83.09(5) . . ?
C2 Ti1 H 75.5(6) . . ?
C2 Ti1 HA 98.3(6) . . ?
C3 Ti1 Al1 115.19(6) . . ?
C3 Ti1 C1 57.31(7) . . ?
C3 Ti1 C2 34.55(7) . . ?
C3 Ti1 C9 128.74(7) . . ?
C3 Ti1 C10 153.55(7) . . ?
C3 Ti1 H 95.0(6) . . ?
C3 Ti1 HA 131.6(6) . . ?
C4 Ti1 Al1 137.52(5) . . ?
C4 Ti1 C1 57.56(6) . . ?
C4 Ti1 C2 57.45(7) . . ?
C4 Ti1 C3 34.78(8) . . ?
C4 Ti1 C5 35.02(7) . . ?
C4 Ti1 C6 97.40(7) . . ?
C4 Ti1 C7 79.82(7) . . ?
C4 Ti1 C8 100.19(7) . . ?
C4 Ti1 C9 134.43(7) . . ?
C4 Ti1 C10 131.92(7) . . ?
C4 Ti1 H 129.2(6) . . ?
C4 Ti1 HA 126.7(6) . . ?
C5 Ti1 Al1 112.01(5) . . ?
C5 Ti1 C1 34.70(7) . . ?
C5 Ti1 C2 57.46(7) . . ?
C5 Ti1 C3 58.00(7) . . ?
C5 Ti1 C8 131.01(7) . . ?
C5 Ti1 C9 156.47(7) . . ?
C5 Ti1 C10 128.09(7) . . ?
C5 Ti1 H 128.5(6) . . ?
C5 Ti1 HA 91.8(6) . . ?
C6 Ti1 Al1 118.82(5) . . ?
C6 Ti1 C1 130.21(7) . . ?
C6 Ti1 C2 154.27(7) . . ?
C6 Ti1 C3 125.98(8) . . ?
C6 Ti1 C5 99.35(7) . . ?
C6 Ti1 C8 58.40(7) . . ?
C6 Ti1 C9 57.74(6) . . ?
C6 Ti1 C10 34.68(6) . . ?
C6 Ti1 H 130.1(6) . . ?
C6 Ti1 HA 93.1(6) . . ?
C7 Ti1 Al1 142.66(5) . . ?
C7 Ti1 C1 134.74(7) . . ?
C7 Ti1 C2 131.19(7) . . ?
C7 Ti1 C3 96.72(7) . . ?
C7 Ti1 C5 100.93(7) . . ?
C7 Ti1 C6 35.12(7) . . ?
C7 Ti1 C8 34.96(7) . . ?
C7 Ti1 C9 57.74(7) . . ?
C7 Ti1 C10 57.66(7) . . ?
C7 Ti1 H 127.1(6) . . ?
C7 Ti1 HA 127.8(6) . . ?
C8 Ti1 Al1 116.94(5) . . ?
C8 Ti1 C1 154.87(7) . . ?
C8 Ti1 C2 126.25(7) . . ?
C8 Ti1 C3 97.95(7) . . ?
C8 Ti1 C9 34.91(6) . . ?
C8 Ti1 C10 57.76(7) . . ?
C8 Ti1 H 92.4(6) . . ?
C8 Ti1 HA 128.9(6) . . ?
C9 Ti1 Al1 86.26(5) . . ?
C9 Ti1 C1 167.45(6) . . ?
C9 Ti1 C2 143.08(7) . . ?
C9 Ti1 C10 34.29(6) . . ?
C9 Ti1 H 75.0(6) . . ?
C9 Ti1 HA 94.6(6) . . ?
C10 Ti1 Al1 87.44(5) . . ?
C10 Ti1 C1 144.99(6) . . ?
C10 Ti1 C2 170.47(7) . . ?
C10 Ti1 H 96.2(6) . . ?
C10 Ti1 HA 74.6(6) . . ?
H Ti1 HA 74.3(9) . . ?
Ti1 Al1 Al1 128.12(3) . 2_666 ?
Ti1 Al1 H 38.1(6) . . ?
Ti1 Al1 HA 38.7(6) . . ?
Al1 Al1 H 122.2(7) 2_666 . ?
Al1 Al1 HA 120.1(6) 2_666 . ?
O1 Al1 Ti1 119.45(4) . . ?
O1 Al1 Ti1 117.75(4) 2_666 . ?
O1 Al1 Al1 39.05(4) . 2_666 ?
O1 Al1 Al1 39.26(4) 2_666 2_666 ?
O1 Al1 O1 78.31(6) 2_666 . ?
O1 Al1 H 92.1(7) . . ?
O1 Al1 H 142.4(7) 2_666 . ?
O1 Al1 HA 142.4(7) . . ?
O1 Al1 HA 89.0(6) 2_666 . ?
O3 Al1 Ti1 117.74(5) . . ?
O3 Al1 Al1 113.90(5) . 2_666 ?
O3 Al1 O1 103.97(6) . . ?
O3 Al1 O1 112.78(6) . 2_666 ?
O3 Al1 H 104.8(7) . . ?
O3 Al1 HA 113.6(7) . . ?
H Al1 HA 76.6(9) . . ?
Al1 O1 Al1 101.69(6) 2_666 . ?
C11 O1 Al1 124.54(10) . . ?
C11 O1 Al1 129.88(10) . 2_666 ?
C12 O2 C13 111.55(14) . . ?
C14 O3 Al1 133.67(12) . . ?
C15 O4 C16 111.72(15) . . ?
Ti1 C1 H1 121.4 . . ?
C2 C1 Ti1 73.46(10) . . ?
C2 C1 H1 125.8 . . ?
C2 C1 C5 108.36(17) . . ?
C5 C1 Ti1 71.04(10) . . ?
C5 C1 H1 125.8 . . ?
Ti1 C2 H2 122.2 . . ?
C1 C2 Ti1 72.49(11) . . ?
C1 C2 H2 126.1 . . ?
C1 C2 C3 107.78(19) . . ?
C3 C2 Ti1 70.88(11) . . ?
C3 C2 H2 126.1 . . ?
Ti1 C3 H3 119.3 . . ?
C2 C3 Ti1 74.58(11) . . ?
C2 C3 H3 126.0 . . ?
C4 C3 Ti1 72.03(11) . . ?
C4 C3 C2 108.08(17) . . ?
C4 C3 H3 126.0 . . ?
Ti1 C4 H4 119.9 . . ?
C3 C4 Ti1 73.19(11) . . ?
C3 C4 H4 125.9 . . ?
C3 C4 C5 108.27(18) . . ?
C5 C4 Ti1 72.82(11) . . ?
C5 C4 H4 125.9 . . ?
Ti1 C5 H5 119.2 . . ?
C1 C5 Ti1 74.26(10) . . ?
C1 C5 H5 126.3 . . ?
C4 C5 Ti1 72.16(11) . . ?
C4 C5 C1 107.49(18) . . ?
C4 C5 H5 126.3 . . ?
Ti1 C6 H6 119.4 . . ?
C7 C6 Ti1 72.14(11) . . ?
C7 C6 H6 126.3 . . ?
C10 C6 Ti1 74.07(11) . . ?
C10 C6 H6 126.3 . . ?
C10 C6 C7 107.50(16) . . ?
Ti1 C7 H7 120.4 . . ?
C6 C7 Ti1 72.74(10) . . ?
C6 C7 H7 125.7 . . ?
C8 C7 Ti1 72.87(10) . . ?
C8 C7 C6 108.53(17) . . ?
C8 C7 H7 125.7 . . ?
Ti1 C8 H8 119.6 . . ?
C7 C8 Ti1 72.17(10) . . ?
C7 C8 H8 126.3 . . ?
C7 C8 C9 107.48(16) . . ?
C9 C8 Ti1 73.87(10) . . ?
C9 C8 H8 126.3 . . ?
Ti1 C9 H9 121.6 . . ?
C8 C9 Ti1 71.21(10) . . ?
C8 C9 H9 126.0 . . ?
C10 C9 Ti1 72.87(10) . . ?
C10 C9 C8 108.02(16) . . ?
C10 C9 H9 126.0 . . ?
Ti1 C10 H10 121.8 . . ?
C6 C10 Ti1 71.25(11) . . ?
C6 C10 H10 125.8 . . ?
C9 C10 Ti1 72.84(10) . . ?
C9 C10 C6 108.45(16) . . ?
C9 C10 H10 125.8 . . ?
O1 C11 H11A 109.0 . . ?
O1 C11 H11B 109.0 . . ?
O1 C11 C12 112.79(14) . . ?
H11A C11 H11B 107.8 . . ?
C12 C11 H11A 109.0 . . ?
C12 C11 H11B 109.0 . . ?
O2 C12 C11 108.97(13) . . ?
O2 C12 H12A 109.9 . . ?
O2 C12 H12B 109.9 . . ?
C11 C12 H12A 109.9 . . ?
C11 C12 H12B 109.9 . . ?
H12A C12 H12B 108.3 . . ?
O2 C13 H13A 109.5 . . ?
O2 C13 H13B 109.5 . . ?
O2 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O3 C14 H14A 109.8 . . ?
O3 C14 H14B 109.8 . . ?
O3 C14 C15 109.52(14) . . ?
H14A C14 H14B 108.2 . . ?
C15 C14 H14A 109.8 . . ?
C15 C14 H14B 109.8 . . ?
O4 C15 C14 110.04(15) . . ?
O4 C15 H15A 109.7 . . ?
O4 C15 H15B 109.7 . . ?
C14 C15 H15A 109.7 . . ?
C14 C15 H15B 109.7 . . ?
H15A C15 H15B 108.2 . . ?
O4 C16 H16A 109.5 . . ?
O4 C16 H16B 109.5 . . ?
O4 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ti1 Al1 O1 Al1 -115.42(5) . . . 2_666 ?
Ti1 Al1 O1 C11 85.00(12) . . . . ?
Ti1 Al1 O3 C14 91.62(16) . . . . ?
Ti1 C1 C2 C3 -62.49(13) . . . . ?
Ti1 C1 C5 C4 65.00(13) . . . . ?
Ti1 C2 C3 C4 -64.74(14) . . . . ?
Ti1 C3 C4 C5 -64.87(14) . . . . ?
Ti1 C4 C5 C1 -66.41(13) . . . . ?
Ti1 C6 C7 C8 -64.57(13) . . . . ?
Ti1 C6 C10 C9 63.79(12) . . . . ?
Ti1 C7 C8 C9 -65.97(12) . . . . ?
Ti1 C8 C9 C10 -64.03(12) . . . . ?
Ti1 C9 C10 C6 -62.77(13) . . . . ?
Al1 Al1 O1 C11 -159.58(15) 2_666 . . . ?
Al1 Al1 O3 C14 -93.61(16) 2_666 . . . ?
Al1 O1 C11 C12 115.15(14) 2_666 . . . ?
Al1 O1 C11 C12 -91.29(15) . . . . ?
Al1 O3 C14 C15 -134.79(15) . . . . ?
O1 Al1 O1 Al1 0.000(0) 2_666 . . 2_666 ?
O1 Al1 O1 C11 -159.58(15) 2_666 . . . ?
O1 Al1 O3 C14 -50.70(18) 2_666 . . . ?
O1 Al1 O3 C14 -133.70(16) . . . . ?
O1 C11 C12 O2 -70.80(18) . . . . ?
O3 Al1 O1 Al1 110.86(6) . . . 2_666 ?
O3 Al1 O1 C11 -48.72(13) . . . . ?
O3 C14 C15 O4 -175.90(16) . . . . ?
C1 C2 C3 Ti1 63.54(13) . . . . ?
C1 C2 C3 C4 -1.2(2) . . . . ?
C2 C1 C5 Ti1 -64.45(13) . . . . ?
C2 C1 C5 C4 0.5(2) . . . . ?
C2 C3 C4 Ti1 66.42(14) . . . . ?
C2 C3 C4 C5 1.5(2) . . . . ?
C3 C4 C5 Ti1 65.11(14) . . . . ?
C3 C4 C5 C1 -1.3(2) . . . . ?
C5 C1 C2 Ti1 62.89(13) . . . . ?
C5 C1 C2 C3 0.4(2) . . . . ?
C6 C7 C8 Ti1 64.49(13) . . . . ?
C6 C7 C8 C9 -1.5(2) . . . . ?
C7 C6 C10 Ti1 -64.89(13) . . . . ?
C7 C6 C10 C9 -1.1(2) . . . . ?
C7 C8 C9 Ti1 64.83(12) . . . . ?
C7 C8 C9 C10 0.8(2) . . . . ?
C8 C9 C10 Ti1 62.95(12) . . . . ?
C8 C9 C10 C6 0.2(2) . . . . ?
C10 C6 C7 Ti1 66.18(13) . . . . ?
C10 C6 C7 C8 1.6(2) . . . . ?
C13 O2 C12 C11 177.21(15) . . . . ?
C16 O4 C15 C14 -175.84(18) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
