# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_eu2_b
_database_code_depnum_ccdc_archive 'CCDC 1531652'
_audit_update_record             
;
2017-02-27 deposited with the CCDC.
2017-03-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C69 H87 Eu O30 Ti6'
_chemical_formula_sum            'C69 H87 Eu O30 Ti6'
_chemical_formula_weight         1835.74

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -8.9294 11.1857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           174
_space_group_name_H-M_alt        'P -6'
_space_group_name_Hall           'P -6'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'

_cell_length_a                   14.9021(3)
_cell_length_b                   14.9021(3)
_cell_length_c                   23.5900(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4536.8(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9914
_cell_measurement_theta_min      3.42
_cell_measurement_theta_max      66.6

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_F_000             1872
_exptl_transmission_factor_min   0.611
_exptl_transmission_factor_max   1.000
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.220
_exptl_absorpt_coefficient_mu    9.733
_shelx_estimated_absorpt_T_min   0.158
_shelx_estimated_absorpt_T_max   0.223
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.158
_exptl_absorpt_correction_T_max  0.223
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements (SADABS) 
;
_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         '30W microfocus sealed tube, Quazar optics'
_diffrn_measurement_device_type  'Bruker QUEST D8 CCD'
_diffrn_measurement_method       'Thin slice ω and φ scans'
_diffrn_reflns_number            40425
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.424
_diffrn_reflns_theta_max         66.626
_diffrn_reflns_theta_full        66.626
_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 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5463
_reflns_number_gt                5297
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.991
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_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 software package, narrow-frames'
_computing_cell_refinement       'refinement of XYZ centroids > 20sigma(I)'
_computing_data_reduction        
;
 Bruker SAINT software package, narrow frame algorithm
;
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_refine_special_details          
;Refined as a 2-component twin. Residual electron density did not resolve 
into anything meaningful but is presumably disordered solvent. iPr ligands 
restrained and treated as anisotropic., Twin
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0997P)²+7.6717P] 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_abs_structure_details 
;
 Flack x determined using 2453 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5463
_refine_ls_number_parameters     331
_refine_ls_number_restraints     208
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0500
_refine_ls_wR_factor_ref         0.1555
_refine_ls_wR_factor_gt          0.1546
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_restrained_S_all      1.137
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Eu1 Eu 0.666667 0.333333 0.500000 0.0171(3) Uani 1 6 d S T P . .
Eu2 Eu 1.000000 1.000000 1.000000 0.0166(3) Uani 1 6 d S T P . .
Ti1 Ti 0.46541(13) 0.36309(14) 0.56325(7) 0.0280(4) Uani 1 1 d . . . . .
Ti2 Ti 0.80897(13) 0.76144(12) 0.93674(7) 0.0252(4) Uani 1 1 d . . . . .
O1 O 0.5009(6) 0.3075(7) 0.500000 0.0213(18) Uani 1 2 d S TU P . .
O2 O 0.4851(8) 0.4610(8) 0.500000 0.035(2) Uani 1 2 d S TU P C .
O3 O 0.3281(6) 0.2939(7) 0.5643(3) 0.0400(18) Uani 1 1 d D U . . .
O4 O 0.4784(6) 0.4537(6) 0.6226(3) 0.0423(19) Uani 1 1 d . U . . .
O5 O 0.4699(6) 0.2570(6) 0.6153(3) 0.0339(16) Uani 1 1 d . U . . .
O6 O 0.6320(5) 0.4350(5) 0.5756(3) 0.0272(14) Uani 1 1 d . U . . .
O21 O 0.8368(7) 0.8504(7) 1.000000 0.0223(19) Uani 1 2 d S TU P . .
O22 O 0.8353(8) 0.6859(7) 1.000000 0.031(2) Uani 1 2 d S TU P G .
O23 O 0.6718(6) 0.6836(6) 0.9352(3) 0.0383(17) Uani 1 1 d D U . . .
O24 O 0.8300(6) 0.6904(6) 0.8768(3) 0.0354(17) Uani 1 1 d . U . . .
O25 O 0.9756(5) 0.8659(5) 0.9253(3) 0.0242(13) Uani 1 1 d . U . . .
O26 O 0.8048(6) 0.8681(6) 0.8860(3) 0.0318(15) Uani 1 1 d . U . . .
C2 C 0.4809(16) 0.5556(15) 0.500000 0.056(5) Uani 1 2 d S TU P . .
H2A H 0.466350 0.556316 0.541328 0.068 Uiso 0.5 1 calc R U P A -1
C2A C 0.584(2) 0.6450(18) 0.500000 0.082(7) Uani 1 2 d S TU P C .
H2AA H 0.579787 0.708366 0.500000 0.123 Uiso 0.5 1 calc R U P B -1
H2AB H 0.621475 0.643502 0.533920 0.123 Uiso 0.5 1 calc R U P B -1
H2AC H 0.621475 0.643502 0.466080 0.123 Uiso 0.5 1 calc R U P B -1
C2B C 0.384(3) 0.547(3) 0.4787(14) 0.074(10) Uani 0.5 1 d . U P C -1
H2BA H 0.389011 0.614770 0.480388 0.111 Uiso 0.5 1 calc R U P C -1
H2BB H 0.373199 0.522473 0.439336 0.111 Uiso 0.5 1 calc R U P C -1
H2BC H 0.326098 0.497380 0.502083 0.111 Uiso 0.5 1 calc R U P C -1
C3 C 0.2421(19) 0.235(2) 0.6042(11) 0.060(5) Uiso 0.50(2) 1 d D U P D 1
H3 H 0.263894 0.227054 0.643085 0.072 Uiso 0.50(2) 1 calc R U P D 1
C3A C 0.170(3) 0.275(3) 0.603(2) 0.087(6) Uiso 0.50(2) 1 d D U P D 1
H3AA H 0.112495 0.235902 0.629115 0.131 Uiso 0.50(2) 1 calc R U P D 1
H3AB H 0.206167 0.348546 0.613373 0.131 Uiso 0.50(2) 1 calc R U P D 1
H3AC H 0.141793 0.267934 0.564117 0.131 Uiso 0.50(2) 1 calc R U P D 1
C3B C 0.190(3) 0.132(3) 0.5674(16) 0.087(6) Uiso 0.50(2) 1 d D U P D 1
H3BA H 0.127957 0.079389 0.586785 0.131 Uiso 0.50(2) 1 calc R U P D 1
H3BB H 0.171052 0.147033 0.530230 0.131 Uiso 0.50(2) 1 calc R U P D 1
H3BC H 0.239331 0.107559 0.562547 0.131 Uiso 0.50(2) 1 calc R U P D 1
C3' C 0.2146(18) 0.244(2) 0.5645(11) 0.060(5) Uiso 0.50(2) 1 d D U P D 2
H3A' H 0.181304 0.236047 0.526679 0.072 Uiso 0.50(2) 1 calc R U P D 2
C3A' C 0.202(4) 0.316(3) 0.6078(19) 0.087(6) Uiso 0.50(2) 1 d D U P D 2
H3AD H 0.127754 0.292208 0.612871 0.131 Uiso 0.50(2) 1 calc R U P D 2
H3AE H 0.231962 0.314040 0.644278 0.131 Uiso 0.50(2) 1 calc R U P D 2
H3AF H 0.236923 0.387169 0.593258 0.131 Uiso 0.50(2) 1 calc R U P D 2
C3B' C 0.180(3) 0.143(2) 0.5970(16) 0.087(6) Uiso 0.50(2) 1 d D U P D 2
H3BD H 0.104504 0.103547 0.599245 0.131 Uiso 0.50(2) 1 calc R U P D 2
H3BE H 0.204966 0.101440 0.577144 0.131 Uiso 0.50(2) 1 calc R U P D 2
H3BF H 0.209486 0.158838 0.635307 0.131 Uiso 0.50(2) 1 calc R U P D 2
C11 C 0.5508(9) 0.5279(8) 0.6544(5) 0.037(2) Uani 1 1 d . U . . .
C12 C 0.5204(11) 0.5797(10) 0.6924(5) 0.048(3) Uani 1 1 d . U . . .
H12A H 0.450262 0.563889 0.693378 0.058 Uiso 1 1 calc R U . . .
C13 C 0.5919(13) 0.6536(12) 0.7284(6) 0.061(4) Uani 1 1 d . U . . .
H13A H 0.570639 0.688163 0.754363 0.073 Uiso 1 1 calc R U . . .
C14 C 0.6944(14) 0.6780(14) 0.7272(7) 0.070(4) Uani 1 1 d . U . . .
H14A H 0.742983 0.728230 0.752592 0.084 Uiso 1 1 calc R U . . .
C15 C 0.7262(11) 0.6293(11) 0.6890(5) 0.048(3) Uani 1 1 d . U . . .
H15A H 0.797167 0.647928 0.687537 0.058 Uiso 1 1 calc R U . . .
C16 C 0.6547(10) 0.5526(9) 0.6525(5) 0.037(3) Uani 1 1 d . U . . .
C17 C 0.4969(8) 0.1913(8) 0.6119(4) 0.030(2) Uani 1 1 d . U . . .
C22 C 0.8376(19) 0.5915(17) 1.000000 0.061(5) Uani 1 2 d S TU P . .
H22' H 0.823928 0.575974 0.958638 0.073 Uiso 0.5 1 calc R U P E -1
C22A C 0.938(3) 0.613(3) 1.000000 0.106(10) Uani 1 2 d S TU P G .
H22A H 0.982285 0.681055 0.982429 0.159 Uiso 0.5 1 calc R U P F -1
H22B H 0.961017 0.614339 1.039100 0.159 Uiso 0.5 1 calc R U P F -1
H22C H 0.943659 0.559888 0.978471 0.159 Uiso 0.5 1 calc R U P F -1
C22B C 0.746(3) 0.504(2) 1.0204(14) 0.080(11) Uani 0.5 1 d . U P G -1
H22D H 0.686475 0.514092 1.013518 0.121 Uiso 0.5 1 calc R U P G -1
H22E H 0.735087 0.441774 1.000508 0.121 Uiso 0.5 1 calc R U P G -1
H22F H 0.752445 0.496225 1.061138 0.121 Uiso 0.5 1 calc R U P G -1
C23 C 0.6008(17) 0.6381(17) 0.8873(9) 0.056(5) Uiso 0.582(15) 1 d D U P H 1
H23A H 0.637358 0.668855 0.850783 0.067 Uiso 0.582(15) 1 calc R U P H 1
C23A C 0.515(3) 0.664(3) 0.8973(16) 0.095(6) Uiso 0.582(15) 1 d D U P H 1
H23B H 0.464833 0.635276 0.866399 0.143 Uiso 0.582(15) 1 calc R U P H 1
H23C H 0.480883 0.633815 0.933400 0.143 Uiso 0.582(15) 1 calc R U P H 1
H23D H 0.545559 0.739313 0.898552 0.143 Uiso 0.582(15) 1 calc R U P H 1
C23B C 0.554(3) 0.525(2) 0.8865(16) 0.095(6) Uiso 0.582(15) 1 d D U P H 1
H23E H 0.507280 0.496458 0.854056 0.143 Uiso 0.582(15) 1 calc R U P H 1
H23F H 0.609338 0.507338 0.883065 0.143 Uiso 0.582(15) 1 calc R U P H 1
H23G H 0.515825 0.495806 0.921663 0.143 Uiso 0.582(15) 1 calc R U P H 1
C23' C 0.5636(19) 0.641(2) 0.9418(13) 0.056(5) Uiso 0.418(15) 1 d D U P H 2
H23H H 0.541739 0.596778 0.976647 0.067 Uiso 0.418(15) 1 calc R U P H 2
C23C C 0.548(4) 0.730(3) 0.9522(19) 0.095(6) Uiso 0.418(15) 1 d D U P H 2
H23I H 0.473838 0.704916 0.957119 0.143 Uiso 0.418(15) 1 calc R U P H 2
H23J H 0.585437 0.766379 0.986476 0.143 Uiso 0.418(15) 1 calc R U P H 2
H23K H 0.574091 0.777221 0.919732 0.143 Uiso 0.418(15) 1 calc R U P H 2
C23D C 0.506(4) 0.576(4) 0.8939(19) 0.095(6) Uiso 0.418(15) 1 d D U P H 2
H23L H 0.431258 0.547847 0.900192 0.143 Uiso 0.418(15) 1 calc R U P H 2
H23M H 0.526722 0.617123 0.859090 0.143 Uiso 0.418(15) 1 calc R U P H 2
H23N H 0.519725 0.518473 0.890308 0.143 Uiso 0.418(15) 1 calc R U P H 2
C31 C 0.9056(8) 0.6982(8) 0.8435(4) 0.033(2) Uani 1 1 d . U . . .
C32 C 0.8813(11) 0.6216(10) 0.8022(5) 0.049(3) Uani 1 1 d . U . . .
H32A H 0.811915 0.566201 0.798867 0.059 Uiso 1 1 calc R U . . .
C33 C 0.9559(13) 0.6252(12) 0.7665(6) 0.060(4) Uani 1 1 d . U . . .
H33A H 0.938583 0.571304 0.739810 0.073 Uiso 1 1 calc R U . . .
C34 C 1.0582(12) 0.7091(13) 0.7697(6) 0.061(4) Uani 1 1 d . U . . .
H34A H 1.109654 0.714184 0.743985 0.074 Uiso 1 1 calc R U . . .
C35 C 1.0818(11) 0.7820(11) 0.8099(5) 0.048(3) Uani 1 1 d . U . . .
H35A H 1.151430 0.837012 0.812779 0.058 Uiso 1 1 calc R U . . .
C36 C 1.0076(9) 0.7803(9) 0.8480(5) 0.033(2) Uani 1 1 d . U . . .
C37 C 0.8258(8) 0.9610(8) 0.8892(4) 0.0249(19) Uani 1 1 d . 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
Eu1 O1 2.302(8) 2_655 ?
Eu1 O1 2.302(8) 3_665 ?
Eu1 O1 2.302(8) . ?
Eu1 O6 2.555(7) . ?
Eu1 O6 2.555(7) 3_665 ?
Eu1 O6 2.555(7) 5_656 ?
Eu1 O6 2.555(7) 6_666 ?
Eu1 O6 2.555(7) 2_655 ?
Eu1 O6 2.555(7) 4_556 ?
Eu1 Ti1 3.5704(16) 4_556 ?
Eu1 Ti1 3.5704(16) . ?
Eu1 Ti1 3.5705(16) 3_665 ?
Eu2 O21 2.337(9) . ?
Eu2 O21 2.337(9) 3_675 ?
Eu2 O21 2.337(9) 2_765 ?
Eu2 O25 2.549(6) . ?
Eu2 O25 2.549(6) 5_767 ?
Eu2 O25 2.549(6) 3_675 ?
Eu2 O25 2.549(6) 6_677 ?
Eu2 O25 2.549(6) 2_765 ?
Eu2 O25 2.549(6) 4_557 ?
Eu2 Ti2 3.5845(16) 5_767 ?
Eu2 Ti2 3.5845(16) 4_557 ?
Eu2 Ti2 3.5845(16) 6_677 ?
Ti1 O3 1.773(8) . ?
Ti1 O4 1.887(8) . ?
Ti1 O1 1.905(5) . ?
Ti1 O2 2.003(7) . ?
Ti1 O5 2.030(7) . ?
Ti1 O6 2.176(7) . ?
Ti1 Ti1 2.984(3) 4_556 ?
Ti2 O23 1.776(8) . ?
Ti2 O24 1.884(7) . ?
Ti2 O21 1.899(6) . ?
Ti2 O26 2.015(7) . ?
Ti2 O22 2.023(7) . ?
Ti2 O25 2.190(7) . ?
Ti2 Ti2 2.984(3) 4_557 ?
O2 C2 1.44(2) . ?
O3 C3' 1.47(2) . ?
O3 C3 1.47(2) . ?
O4 C11 1.325(14) . ?
O5 C17 1.233(13) . ?
O6 C17 1.297(13) 3_665 ?
O22 C22 1.42(2) . ?
O23 C23' 1.42(2) . ?
O23 C23 1.46(2) . ?
O24 C31 1.330(13) . ?
O25 C37 1.279(12) 2_765 ?
O26 C37 1.260(12) . ?
C2 C2A 1.45(3) . ?
C2 C2B 1.47(4) . ?
C2 H2A 1.0000 . ?
C2A H2AA 0.9800 . ?
C2A H2AB 0.9800 . ?
C2A H2AC 0.9800 . ?
C2B H2BA 0.9800 . ?
C2B H2BB 0.9800 . ?
C2B H2BC 0.9800 . ?
C3 C3A 1.48(3) . ?
C3 C3B 1.58(3) . ?
C3 H3 1.0000 . ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?
C3A H3AC 0.9800 . ?
C3B H3BA 0.9800 . ?
C3B H3BB 0.9800 . ?
C3B H3BC 0.9800 . ?
C3' C3B' 1.53(3) . ?
C3' C3A' 1.57(3) . ?
C3' H3A' 1.0000 . ?
C3A' H3AD 0.9800 . ?
C3A' H3AE 0.9800 . ?
C3A' H3AF 0.9800 . ?
C3B' H3BD 0.9800 . ?
C3B' H3BE 0.9800 . ?
C3B' H3BF 0.9800 . ?
C11 C12 1.399(15) . ?
C11 C16 1.402(17) . ?
C12 C13 1.38(2) . ?
C12 H12A 0.9500 . ?
C13 C14 1.38(2) . ?
C13 H13A 0.9500 . ?
C14 C15 1.380(19) . ?
C14 H14A 0.9500 . ?
C15 C16 1.404(17) . ?
C15 H15A 0.9500 . ?
C16 C17 1.499(15) 3_665 ?
C22 C22A 1.37(4) . ?
C22 C22B 1.42(4) . ?
C22 H22' 1.0000 . ?
C22A H22A 0.9800 . ?
C22A H22B 0.9800 . ?
C22A H22C 0.9800 . ?
C22B H22D 0.9800 . ?
C22B H22E 0.9800 . ?
C22B H22F 0.9800 . ?
C23 C23B 1.47(3) . ?
C23 C23A 1.52(3) . ?
C23 H23A 1.0000 . ?
C23A H23B 0.9800 . ?
C23A H23C 0.9800 . ?
C23A H23D 0.9800 . ?
C23B H23E 0.9800 . ?
C23B H23F 0.9800 . ?
C23B H23G 0.9800 . ?
C23' C23D 1.46(3) . ?
C23' C23C 1.48(3) . ?
C23' H23H 1.0000 . ?
C23C H23I 0.9800 . ?
C23C H23J 0.9800 . ?
C23C H23K 0.9800 . ?
C23D H23L 0.9800 . ?
C23D H23M 0.9800 . ?
C23D H23N 0.9800 . ?
C31 C36 1.401(16) . ?
C31 C32 1.403(15) . ?
C32 C33 1.374(19) . ?
C32 H32A 0.9500 . ?
C33 C34 1.41(2) . ?
C33 H33A 0.9500 . ?
C34 C35 1.350(18) . ?
C34 H34A 0.9500 . ?
C35 C36 1.415(16) . ?
C35 H35A 0.9500 . ?
C36 C37 1.470(14) 2_765 ?

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 Eu1 O1 120.002(1) 2_655 3_665 ?
O1 Eu1 O1 120.000(1) 2_655 . ?
O1 Eu1 O1 119.998(1) 3_665 . ?
O1 Eu1 O6 135.41(16) 2_655 . ?
O1 Eu1 O6 73.0(2) 3_665 . ?
O1 Eu1 O6 65.2(2) . . ?
O1 Eu1 O6 73.0(2) 2_655 3_665 ?
O1 Eu1 O6 65.2(2) 3_665 3_665 ?
O1 Eu1 O6 135.41(16) . 3_665 ?
O6 Eu1 O6 76.6(2) . 3_665 ?
O1 Eu1 O6 65.2(2) 2_655 5_656 ?
O1 Eu1 O6 135.41(16) 3_665 5_656 ?
O1 Eu1 O6 73.0(2) . 5_656 ?
O6 Eu1 O6 138.05(12) . 5_656 ?
O6 Eu1 O6 138.05(12) 3_665 5_656 ?
O1 Eu1 O6 73.0(2) 2_655 6_666 ?
O1 Eu1 O6 65.2(2) 3_665 6_666 ?
O1 Eu1 O6 135.41(16) . 6_666 ?
O6 Eu1 O6 138.05(12) . 6_666 ?
O6 Eu1 O6 88.6(3) 3_665 6_666 ?
O6 Eu1 O6 76.6(2) 5_656 6_666 ?
O1 Eu1 O6 65.2(2) 2_655 2_655 ?
O1 Eu1 O6 135.41(16) 3_665 2_655 ?
O1 Eu1 O6 73.0(2) . 2_655 ?
O6 Eu1 O6 76.6(2) . 2_655 ?
O6 Eu1 O6 76.6(2) 3_665 2_655 ?
O6 Eu1 O6 88.6(3) 5_656 2_655 ?
O6 Eu1 O6 138.05(12) 6_666 2_655 ?
O1 Eu1 O6 135.41(16) 2_655 4_556 ?
O1 Eu1 O6 73.0(2) 3_665 4_556 ?
O1 Eu1 O6 65.2(2) . 4_556 ?
O6 Eu1 O6 88.6(3) . 4_556 ?
O6 Eu1 O6 138.05(12) 3_665 4_556 ?
O6 Eu1 O6 76.6(2) 5_656 4_556 ?
O6 Eu1 O6 76.6(2) 6_666 4_556 ?
O6 Eu1 O6 138.05(12) 2_655 4_556 ?
O1 Eu1 Ti1 130.1(2) 2_655 4_556 ?
O1 Eu1 Ti1 103.5(2) 3_665 4_556 ?
O1 Eu1 Ti1 28.72(12) . 4_556 ?
O6 Eu1 Ti1 77.68(16) . 4_556 ?
O6 Eu1 Ti1 154.04(16) 3_665 4_556 ?
O6 Eu1 Ti1 66.80(15) 5_656 4_556 ?
O6 Eu1 Ti1 108.39(16) 6_666 4_556 ?
O6 Eu1 Ti1 100.93(16) 2_655 4_556 ?
O6 Eu1 Ti1 37.16(16) 4_556 4_556 ?
O1 Eu1 Ti1 130.1(2) 2_655 . ?
O1 Eu1 Ti1 103.5(2) 3_665 . ?
O1 Eu1 Ti1 28.72(12) . . ?
O6 Eu1 Ti1 37.16(16) . . ?
O6 Eu1 Ti1 108.39(16) 3_665 . ?
O6 Eu1 Ti1 100.93(16) 5_656 . ?
O6 Eu1 Ti1 154.04(16) 6_666 . ?
O6 Eu1 Ti1 66.80(15) 2_655 . ?
O6 Eu1 Ti1 77.68(16) 4_556 . ?
Ti1 Eu1 Ti1 49.40(6) 4_556 . ?
O1 Eu1 Ti1 103.5(2) 2_655 3_665 ?
O1 Eu1 Ti1 28.72(12) 3_665 3_665 ?
O1 Eu1 Ti1 130.1(2) . 3_665 ?
O6 Eu1 Ti1 66.80(16) . 3_665 ?
O6 Eu1 Ti1 37.16(16) 3_665 3_665 ?
O6 Eu1 Ti1 154.04(16) 5_656 3_665 ?
O6 Eu1 Ti1 77.68(16) 6_666 3_665 ?
O6 Eu1 Ti1 108.39(16) 2_655 3_665 ?
O6 Eu1 Ti1 100.93(16) 4_556 3_665 ?
Ti1 Eu1 Ti1 125.968(14) 4_556 3_665 ?
Ti1 Eu1 Ti1 103.77(3) . 3_665 ?
O21 Eu2 O21 119.999(4) . 3_675 ?
O21 Eu2 O21 120.001(5) . 2_765 ?
O21 Eu2 O21 120.000(9) 3_675 2_765 ?
O21 Eu2 O25 65.2(2) . . ?
O21 Eu2 O25 136.02(15) 3_675 . ?
O21 Eu2 O25 72.6(2) 2_765 . ?
O21 Eu2 O25 136.02(15) . 5_767 ?
O21 Eu2 O25 72.6(2) 3_675 5_767 ?
O21 Eu2 O25 65.2(2) 2_765 5_767 ?
O25 Eu2 O25 137.62(11) . 5_767 ?
O21 Eu2 O25 72.6(2) . 3_675 ?
O21 Eu2 O25 65.2(2) 3_675 3_675 ?
O21 Eu2 O25 136.02(15) 2_765 3_675 ?
O25 Eu2 O25 77.5(2) . 3_675 ?
O25 Eu2 O25 137.62(11) 5_767 3_675 ?
O21 Eu2 O25 72.6(2) . 6_677 ?
O21 Eu2 O25 65.2(2) 3_675 6_677 ?
O21 Eu2 O25 136.02(15) 2_765 6_677 ?
O25 Eu2 O25 137.62(11) . 6_677 ?
O25 Eu2 O25 77.5(2) 5_767 6_677 ?
O25 Eu2 O25 87.4(3) 3_675 6_677 ?
O21 Eu2 O25 136.02(15) . 2_765 ?
O21 Eu2 O25 72.6(2) 3_675 2_765 ?
O21 Eu2 O25 65.2(2) 2_765 2_765 ?
O25 Eu2 O25 77.5(2) . 2_765 ?
O25 Eu2 O25 87.4(3) 5_767 2_765 ?
O25 Eu2 O25 77.5(2) 3_675 2_765 ?
O25 Eu2 O25 137.62(11) 6_677 2_765 ?
O21 Eu2 O25 65.2(2) . 4_557 ?
O21 Eu2 O25 136.02(14) 3_675 4_557 ?
O21 Eu2 O25 72.6(2) 2_765 4_557 ?
O25 Eu2 O25 87.4(3) . 4_557 ?
O25 Eu2 O25 77.5(2) 5_767 4_557 ?
O25 Eu2 O25 137.62(11) 3_675 4_557 ?
O25 Eu2 O25 77.5(2) 6_677 4_557 ?
O25 Eu2 O25 137.62(11) 2_765 4_557 ?
O21 Eu2 Ti2 130.15(19) . 5_767 ?
O21 Eu2 Ti2 103.5(2) 3_675 5_767 ?
O21 Eu2 Ti2 28.65(12) 2_765 5_767 ?
O25 Eu2 Ti2 100.44(15) . 5_767 ?
O25 Eu2 Ti2 37.23(16) 5_767 5_767 ?
O25 Eu2 Ti2 154.50(15) 3_675 5_767 ?
O25 Eu2 Ti2 109.11(15) 6_677 5_767 ?
O25 Eu2 Ti2 77.24(15) 2_765 5_767 ?
O25 Eu2 Ti2 66.79(15) 4_557 5_767 ?
O21 Eu2 Ti2 28.65(12) . 4_557 ?
O21 Eu2 Ti2 130.1(2) 3_675 4_557 ?
O21 Eu2 Ti2 103.5(2) 2_765 4_557 ?
O25 Eu2 Ti2 77.24(15) . 4_557 ?
O25 Eu2 Ti2 109.11(15) 5_767 4_557 ?
O25 Eu2 Ti2 100.44(16) 3_675 4_557 ?
O25 Eu2 Ti2 66.79(16) 6_677 4_557 ?
O25 Eu2 Ti2 154.50(15) 2_765 4_557 ?
O25 Eu2 Ti2 37.23(16) 4_557 4_557 ?
Ti2 Eu2 Ti2 103.89(3) 5_767 4_557 ?
O21 Eu2 Ti2 103.5(2) . 6_677 ?
O21 Eu2 Ti2 28.65(12) 3_675 6_677 ?
O21 Eu2 Ti2 130.1(2) 2_765 6_677 ?
O25 Eu2 Ti2 154.50(15) . 6_677 ?
O25 Eu2 Ti2 66.79(15) 5_767 6_677 ?
O25 Eu2 Ti2 77.24(15) 3_675 6_677 ?
O25 Eu2 Ti2 37.23(16) 6_677 6_677 ?
O25 Eu2 Ti2 100.44(15) 2_765 6_677 ?
O25 Eu2 Ti2 109.11(15) 4_557 6_677 ?
Ti2 Eu2 Ti2 103.89(3) 5_767 6_677 ?
Ti2 Eu2 Ti2 103.89(3) 4_557 6_677 ?
O3 Ti1 O4 94.6(4) . . ?
O3 Ti1 O1 104.4(4) . . ?
O4 Ti1 O1 160.2(4) . . ?
O3 Ti1 O2 98.1(4) . . ?
O4 Ti1 O2 96.1(4) . . ?
O1 Ti1 O2 76.2(3) . . ?
O3 Ti1 O5 90.9(4) . . ?
O4 Ti1 O5 94.4(3) . . ?
O1 Ti1 O5 90.6(3) . . ?
O2 Ti1 O5 165.6(3) . . ?
O3 Ti1 O6 170.3(3) . . ?
O4 Ti1 O6 82.2(3) . . ?
O1 Ti1 O6 79.8(3) . . ?
O2 Ti1 O6 91.5(4) . . ?
O5 Ti1 O6 80.1(3) . . ?
O3 Ti1 Ti1 90.8(3) . 4_556 ?
O4 Ti1 Ti1 137.9(3) . 4_556 ?
O1 Ti1 Ti1 38.5(2) . 4_556 ?
O2 Ti1 Ti1 41.9(2) . 4_556 ?
O5 Ti1 Ti1 127.3(2) . 4_556 ?
O6 Ti1 Ti1 97.70(18) . 4_556 ?
O3 Ti1 Eu1 137.0(3) . . ?
O4 Ti1 Eu1 127.4(2) . . ?
O1 Ti1 Eu1 35.5(2) . . ?
O2 Ti1 Eu1 87.3(3) . . ?
O5 Ti1 Eu1 78.4(2) . . ?
O6 Ti1 Eu1 45.16(17) . . ?
Ti1 Ti1 Eu1 65.30(3) 4_556 . ?
O23 Ti2 O24 94.5(3) . . ?
O23 Ti2 O21 104.5(4) . . ?
O24 Ti2 O21 160.4(4) . . ?
O23 Ti2 O26 91.3(3) . . ?
O24 Ti2 O26 94.4(3) . . ?
O21 Ti2 O26 89.9(3) . . ?
O23 Ti2 O22 97.6(4) . . ?
O24 Ti2 O22 96.2(3) . . ?
O21 Ti2 O22 76.9(3) . . ?
O26 Ti2 O22 165.5(3) . . ?
O23 Ti2 O25 170.9(3) . . ?
O24 Ti2 O25 81.9(3) . . ?
O21 Ti2 O25 80.0(3) . . ?
O26 Ti2 O25 80.6(3) . . ?
O22 Ti2 O25 91.1(3) . . ?
O23 Ti2 Ti2 91.2(2) . 4_557 ?
O24 Ti2 Ti2 138.6(2) . 4_557 ?
O21 Ti2 Ti2 38.2(2) . 4_557 ?
O26 Ti2 Ti2 126.4(2) . 4_557 ?
O22 Ti2 Ti2 42.5(2) . 4_557 ?
O25 Ti2 Ti2 97.06(17) . 4_557 ?
O23 Ti2 Eu2 137.8(3) . . ?
O24 Ti2 Eu2 126.7(2) . . ?
O21 Ti2 Eu2 36.2(3) . . ?
O26 Ti2 Eu2 77.7(2) . . ?
O22 Ti2 Eu2 88.1(3) . . ?
O25 Ti2 Eu2 44.78(16) . . ?
Ti2 Ti2 Eu2 65.40(3) 4_557 . ?
Ti1 O1 Ti1 103.1(4) 4_556 . ?
Ti1 O1 Eu1 115.8(3) 4_556 . ?
Ti1 O1 Eu1 115.8(3) . . ?
C2 O2 Ti1 130.5(3) . . ?
C2 O2 Ti1 130.5(3) . 4_556 ?
Ti1 O2 Ti1 96.3(4) . 4_556 ?
C3' O3 Ti1 176.0(12) . . ?
C3 O3 Ti1 139.7(12) . . ?
C11 O4 Ti1 140.0(7) . . ?
C17 O5 Ti1 136.8(7) . . ?
C17 O6 Ti1 132.0(7) 3_665 . ?
C17 O6 Eu1 130.2(6) 3_665 . ?
Ti1 O6 Eu1 97.7(2) . . ?
Ti2 O21 Ti2 103.6(5) 4_557 . ?
Ti2 O21 Eu2 115.2(3) 4_557 . ?
Ti2 O21 Eu2 115.2(3) . . ?
C22 O22 Ti2 131.1(3) . 4_557 ?
C22 O22 Ti2 131.1(3) . . ?
Ti2 O22 Ti2 95.1(4) 4_557 . ?
C23' O23 Ti2 166.3(14) . . ?
C23 O23 Ti2 130.5(10) . . ?
C31 O24 Ti2 140.0(7) . . ?
C37 O25 Ti2 130.9(6) 2_765 . ?
C37 O25 Eu2 130.8(6) 2_765 . ?
Ti2 O25 Eu2 98.0(2) . . ?
C37 O26 Ti2 138.0(6) . . ?
O2 C2 C2A 110.7(17) . . ?
O2 C2 C2B 115.7(19) . . ?
C2A C2 C2B 129(2) . . ?
O2 C2 H2A 97.3 . . ?
C2A C2 H2A 97.3 . . ?
C2B C2 H2A 97.3 . . ?
C2 C2A H2AA 109.5 . . ?
C2 C2A H2AB 109.5 . . ?
H2AA C2A H2AB 109.5 . . ?
C2 C2A H2AC 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
C2 C2B H2BA 109.5 . . ?
C2 C2B H2BB 109.5 . . ?
H2BA C2B H2BB 109.5 . . ?
C2 C2B H2BC 109.5 . . ?
H2BA C2B H2BC 109.5 . . ?
H2BB C2B H2BC 109.5 . . ?
O3 C3 C3A 110(3) . . ?
O3 C3 C3B 95(2) . . ?
C3A C3 C3B 106(2) . . ?
O3 C3 H3 114.8 . . ?
C3A C3 H3 114.8 . . ?
C3B C3 H3 114.8 . . ?
C3 C3A H3AA 109.5 . . ?
C3 C3A H3AB 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
C3 C3A H3AC 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
C3 C3B H3BA 109.5 . . ?
C3 C3B H3BB 109.5 . . ?
H3BA C3B H3BB 109.5 . . ?
C3 C3B H3BC 109.5 . . ?
H3BA C3B H3BC 109.5 . . ?
H3BB C3B H3BC 109.5 . . ?
O3 C3' C3B' 104(2) . . ?
O3 C3' C3A' 99(2) . . ?
C3B' C3' C3A' 105(2) . . ?
O3 C3' H3A' 115.7 . . ?
C3B' C3' H3A' 115.7 . . ?
C3A' C3' H3A' 115.7 . . ?
C3' C3A' H3AD 109.5 . . ?
C3' C3A' H3AE 109.5 . . ?
H3AD C3A' H3AE 109.5 . . ?
C3' C3A' H3AF 109.5 . . ?
H3AD C3A' H3AF 109.5 . . ?
H3AE C3A' H3AF 109.5 . . ?
C3' C3B' H3BD 109.5 . . ?
C3' C3B' H3BE 109.5 . . ?
H3BD C3B' H3BE 109.5 . . ?
C3' C3B' H3BF 109.5 . . ?
H3BD C3B' H3BF 109.5 . . ?
H3BE C3B' H3BF 109.5 . . ?
O4 C11 C12 118.0(11) . . ?
O4 C11 C16 122.2(10) . . ?
C12 C11 C16 119.7(11) . . ?
C13 C12 C11 120.2(13) . . ?
C13 C12 H12A 119.9 . . ?
C11 C12 H12A 119.9 . . ?
C12 C13 C14 120.5(12) . . ?
C12 C13 H13A 119.7 . . ?
C14 C13 H13A 119.7 . . ?
C15 C14 C13 120.1(14) . . ?
C15 C14 H14A 120.0 . . ?
C13 C14 H14A 120.0 . . ?
C14 C15 C16 120.6(14) . . ?
C14 C15 H15A 119.7 . . ?
C16 C15 H15A 119.7 . . ?
C11 C16 C15 118.9(11) . . ?
C11 C16 C17 123.2(10) . 3_665 ?
C15 C16 C17 117.9(11) . 3_665 ?
O5 C17 O6 123.2(10) . 2_655 ?
O5 C17 C16 116.7(9) . 2_655 ?
O6 C17 C16 120.1(10) 2_655 2_655 ?
C22A C22 C22B 131(3) . . ?
C22A C22 O22 109(2) . . ?
C22B C22 O22 115(2) . . ?
C22A C22 H22' 97.3 . . ?
C22B C22 H22' 97.3 . . ?
O22 C22 H22' 97.3 . . ?
C22 C22A H22A 109.5 . . ?
C22 C22A H22B 109.5 . . ?
H22A C22A H22B 109.5 . . ?
C22 C22A H22C 109.5 . . ?
H22A C22A H22C 109.5 . . ?
H22B C22A H22C 109.5 . . ?
C22 C22B H22D 109.5 . . ?
C22 C22B H22E 109.5 . . ?
H22D C22B H22E 109.5 . . ?
C22 C22B H22F 109.5 . . ?
H22D C22B H22F 109.5 . . ?
H22E C22B H22F 109.5 . . ?
O23 C23 C23B 111(2) . . ?
O23 C23 C23A 105(2) . . ?
C23B C23 C23A 109(2) . . ?
O23 C23 H23A 110.5 . . ?
C23B C23 H23A 110.5 . . ?
C23A C23 H23A 110.5 . . ?
C23 C23A H23B 109.5 . . ?
C23 C23A H23C 109.5 . . ?
H23B C23A H23C 109.5 . . ?
C23 C23A H23D 109.5 . . ?
H23B C23A H23D 109.5 . . ?
H23C C23A H23D 109.5 . . ?
C23 C23B H23E 109.5 . . ?
C23 C23B H23F 109.5 . . ?
H23E C23B H23F 109.5 . . ?
C23 C23B H23G 109.5 . . ?
H23E C23B H23G 109.5 . . ?
H23F C23B H23G 109.5 . . ?
O23 C23' C23D 112(3) . . ?
O23 C23' C23C 106(3) . . ?
C23D C23' C23C 115(3) . . ?
O23 C23' H23H 108.0 . . ?
C23D C23' H23H 108.0 . . ?
C23C C23' H23H 108.0 . . ?
C23' C23C H23I 109.5 . . ?
C23' C23C H23J 109.5 . . ?
H23I C23C H23J 109.5 . . ?
C23' C23C H23K 109.5 . . ?
H23I C23C H23K 109.5 . . ?
H23J C23C H23K 109.5 . . ?
C23' C23D H23L 109.5 . . ?
C23' C23D H23M 109.5 . . ?
H23L C23D H23M 109.5 . . ?
C23' C23D H23N 109.5 . . ?
H23L C23D H23N 109.5 . . ?
H23M C23D H23N 109.5 . . ?
O24 C31 C36 122.3(9) . . ?
O24 C31 C32 118.4(10) . . ?
C36 C31 C32 119.3(10) . . ?
C33 C32 C31 121.2(12) . . ?
C33 C32 H32A 119.4 . . ?
C31 C32 H32A 119.4 . . ?
C32 C33 C34 119.9(12) . . ?
C32 C33 H33A 120.1 . . ?
C34 C33 H33A 120.1 . . ?
C35 C34 C33 118.8(13) . . ?
C35 C34 H34A 120.6 . . ?
C33 C34 H34A 120.6 . . ?
C34 C35 C36 123.1(13) . . ?
C34 C35 H35A 118.5 . . ?
C36 C35 H35A 118.5 . . ?
C31 C36 C35 117.7(10) . . ?
C31 C36 C37 122.7(9) . 2_765 ?
C35 C36 C37 119.6(10) . 2_765 ?
O26 C37 O25 122.2(9) . 3_675 ?
O26 C37 C36 115.7(9) . 3_675 ?
O25 C37 C36 122.1(9) 3_675 3_675 ?

_refine_diff_density_max         2.399
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.146

####################################################################### 
# 
# 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_ho3_b
_database_code_depnum_ccdc_archive 'CCDC 1504166'
_audit_update_record             
;
2017-02-27 deposited with the CCDC.
2017-03-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C69 H87 Ho O30 Ti6'
_chemical_formula_sum            'C69 H87 Ho O30 Ti6'
_chemical_formula_weight         1848.71

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -14.9734 3.7046 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           174
_space_group_name_H-M_alt        'P -6'
_space_group_name_Hall           'P -6'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'

_cell_length_a                   14.8834(4)
_cell_length_b                   14.8834(4)
_cell_length_c                   23.5900(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4525.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9777
_cell_measurement_theta_min      3.43
_cell_measurement_theta_max      61.6

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_F_000             1880
_exptl_transmission_factor_min   0.688
_exptl_transmission_factor_max   1.000
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.270
_exptl_absorpt_coefficient_mu    6.429
_shelx_estimated_absorpt_T_min   0.218
_shelx_estimated_absorpt_T_max   0.276
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.218
_exptl_absorpt_correction_T_max  0.276
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements (SADABS) 
;
_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         '30W microfocus sealed tube, Quazar optics'
_diffrn_measurement_device_type  'Bruker QUEST D8 CCD'
_diffrn_measurement_method       'Thin slice ω and φ scans'
_diffrn_reflns_number            41759
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_av_R_equivalents  0.0625
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.429
_diffrn_reflns_theta_max         66.780
_diffrn_reflns_theta_full        66.780
_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             5479
_reflns_number_gt                5227
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.990
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.999

_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 software package, narrow-frames'
_computing_cell_refinement       'refinement of XYZ centroids > 20sigma(I)'
_computing_data_reduction        
;
 Bruker SAINT software package, narrow frame algorithm
;
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_refine_special_details          
;Refined as a 2-component twin. Residual electron density did not resolve
into anything meaningful. iPr ligands restrained and treated isotropically 
in order to model the disorder sensibly., Twin
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1360P)²+7.5091P] 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_abs_structure_details 
;
 Flack x determined using 2478 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.419(6)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5479
_refine_ls_number_parameters     326
_refine_ls_number_restraints     202
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0655
_refine_ls_wR_factor_ref         0.1914
_refine_ls_wR_factor_gt          0.1850
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_restrained_S_all      1.100
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Ho1 Ho 0.666667 0.333333 0.500000 0.0251(6) Uani 1 6 d S T P . .
Ho2 Ho 1.000000 1.000000 1.000000 0.0238(6) Uani 1 6 d S T P . .
Ti1 Ti 0.4672(2) 0.3644(2) 0.56293(10) 0.0323(6) Uani 1 1 d . . . . .
Ti2 Ti 0.8099(2) 0.7629(2) 0.93697(9) 0.0297(6) Uani 1 1 d . . . . .
O1 O 0.5040(11) 0.3083(10) 0.500000 0.030(3) Uani 1 2 d S TU P . .
O2 O 0.4874(11) 0.4614(11) 0.500000 0.037(3) Uani 1 2 d S TU P C .
O3 O 0.3291(9) 0.2941(10) 0.5641(4) 0.048(3) Uani 1 1 d D U . . .
O4 O 0.4792(9) 0.4549(9) 0.6212(5) 0.046(3) Uani 1 1 d . U . . .
O5 O 0.4713(9) 0.2598(8) 0.6154(4) 0.039(3) Uani 1 1 d . U . . .
O6 O 0.6328(8) 0.4338(7) 0.5754(4) 0.032(2) Uani 1 1 d . U . . .
O21 O 0.8390(11) 0.8523(11) 1.000000 0.031(3) Uani 1 2 d S TU P . .
O22 O 0.8357(12) 0.6887(9) 1.000000 0.033(3) Uani 1 2 d S TU P G .
O23 O 0.6733(9) 0.6855(8) 0.9365(4) 0.038(2) Uani 1 1 d D U . . .
O24 O 0.8302(9) 0.6934(7) 0.8769(4) 0.042(3) Uani 1 1 d . U . . .
O25 O 0.9768(8) 0.8677(8) 0.9251(4) 0.028(2) Uani 1 1 d . U . . .
O26 O 0.8052(9) 0.8675(8) 0.8857(4) 0.037(2) Uani 1 1 d . U . . .
C2 C 0.482(2) 0.560(2) 0.500000 0.059(7) Uani 1 2 d S TU P . .
H2A H 0.473565 0.560848 0.542047 0.071 Uiso 0.5 1 calc R U P A -1
C2A C 0.593(4) 0.653(3) 0.500000 0.096(12) Uani 1 2 d S TU P C .
H2AA H 0.591405 0.717878 0.500000 0.144 Uiso 0.5 1 calc R U P B -1
H2AB H 0.629828 0.650118 0.533920 0.144 Uiso 0.5 1 calc R U P B -1
H2AC H 0.629828 0.650118 0.466080 0.144 Uiso 0.5 1 calc R U P B -1
C2B C 0.364(4) 0.534(5) 0.487(3) 0.10(2) Uiso 0.5 1 d . . P C -1
H2BA H 0.361663 0.598706 0.486619 0.151 Uiso 0.5 1 calc R U P C -1
H2BB H 0.343277 0.501224 0.449224 0.151 Uiso 0.5 1 calc R U P C -1
H2BC H 0.317363 0.487199 0.515565 0.151 Uiso 0.5 1 calc R U P C -1
C3 C 0.245(2) 0.244(2) 0.6068(12) 0.058(6) Uiso 0.54(3) 1 d D U P D 1
H3 H 0.264817 0.223245 0.642880 0.070 Uiso 0.54(3) 1 calc R U P D 1
C3A C 0.199(4) 0.312(4) 0.614(2) 0.087(8) Uiso 0.54(3) 1 d D U P D 1
H3AA H 0.142619 0.280928 0.641701 0.131 Uiso 0.54(3) 1 calc R U P D 1
H3AB H 0.252126 0.380416 0.626683 0.131 Uiso 0.54(3) 1 calc R U P D 1
H3AC H 0.170825 0.318124 0.577262 0.131 Uiso 0.54(3) 1 calc R U P D 1
C3B C 0.174(4) 0.155(4) 0.5682(18) 0.087(8) Uiso 0.54(3) 1 d D U P D 1
H3BA H 0.202216 0.108886 0.562741 0.131 Uiso 0.54(3) 1 calc R U P D 1
H3BB H 0.104790 0.116301 0.585423 0.131 Uiso 0.54(3) 1 calc R U P D 1
H3BC H 0.168387 0.182732 0.531411 0.131 Uiso 0.54(3) 1 calc R U P D 1
C3' C 0.225(4) 0.229(3) 0.5644(16) 0.058(6) Uiso 0.46(3) 1 d D U P D 2
H3A' H 0.196761 0.220609 0.524967 0.070 Uiso 0.46(3) 1 calc R U P D 2
C3A' C 0.177(5) 0.276(4) 0.601(2) 0.087(8) Uiso 0.46(3) 1 d D U P D 2
H3AD H 0.101157 0.230161 0.602085 0.131 Uiso 0.46(3) 1 calc R U P D 2
H3AE H 0.204170 0.284386 0.639916 0.131 Uiso 0.46(3) 1 calc R U P D 2
H3AF H 0.193161 0.343822 0.586183 0.131 Uiso 0.46(3) 1 calc R U P D 2
C3B' C 0.193(5) 0.125(4) 0.590(2) 0.087(8) Uiso 0.46(3) 1 d D U P D 2
H3BD H 0.116775 0.081968 0.588587 0.131 Uiso 0.46(3) 1 calc R U P D 2
H3BE H 0.223322 0.091249 0.567550 0.131 Uiso 0.46(3) 1 calc R U P D 2
H3BF H 0.216664 0.133568 0.628864 0.131 Uiso 0.46(3) 1 calc R U P D 2
C11 C 0.5520(14) 0.5279(12) 0.6535(7) 0.045(4) Uani 1 1 d . U . . .
C12 C 0.5233(17) 0.5805(15) 0.6932(7) 0.056(5) Uani 1 1 d . U . . .
H12A H 0.453573 0.566152 0.695409 0.067 Uiso 1 1 calc R U . . .
C13 C 0.599(2) 0.654(2) 0.7288(9) 0.074(6) Uani 1 1 d . U . . .
H13A H 0.578793 0.688571 0.755037 0.089 Uiso 1 1 calc R U . . .
C14 C 0.6968(19) 0.6774(19) 0.7286(8) 0.068(6) Uani 1 1 d . U . . .
H14A H 0.745193 0.727039 0.754401 0.082 Uiso 1 1 calc R U . . .
C15 C 0.7269(17) 0.6288(16) 0.6902(8) 0.058(5) Uani 1 1 d . U . . .
H15A H 0.797943 0.647686 0.688398 0.070 Uiso 1 1 calc R U . . .
C16 C 0.6556(13) 0.5512(12) 0.6529(7) 0.038(3) Uani 1 1 d . U . . .
C17 C 0.4966(12) 0.1915(13) 0.6124(7) 0.038(4) Uani 1 1 d . U . . .
C22 C 0.834(3) 0.591(2) 1.000000 0.063(7) Uani 1 2 d S TU P . .
H22' H 0.820190 0.575605 0.958596 0.076 Uiso 0.5 1 calc R U P E -1
C22A C 0.933(5) 0.613(5) 1.000000 0.14(2) Uani 1 2 d S TU P G .
H22A H 0.976130 0.681518 0.982637 0.206 Uiso 0.5 1 calc R U P F -1
H22B H 0.955458 0.614297 1.039086 0.206 Uiso 0.5 1 calc R U P F -1
H22C H 0.938935 0.560567 0.978277 0.206 Uiso 0.5 1 calc R U P F -1
C22B C 0.745(4) 0.504(2) 1.0198(17) 0.080(13) Uani 0.5 1 d . U P G -1
H22D H 0.684537 0.512478 1.013209 0.120 Uiso 0.5 1 calc R U P G -1
H22E H 0.735402 0.442176 0.999736 0.120 Uiso 0.5 1 calc R U P G -1
H22F H 0.751925 0.495906 1.060545 0.120 Uiso 0.5 1 calc R U P G -1
C23 C 0.601(2) 0.642(2) 0.8889(13) 0.060(7) Uiso 0.54(2) 1 d D U P H 1
H23A H 0.638828 0.671818 0.852535 0.072 Uiso 0.54(2) 1 calc R U P H 1
C23A C 0.527(4) 0.680(4) 0.899(2) 0.096(8) Uiso 0.54(2) 1 d D U P H 1
H23B H 0.564473 0.755541 0.899327 0.143 Uiso 0.54(2) 1 calc R U P H 1
H23C H 0.474760 0.654199 0.868842 0.143 Uiso 0.54(2) 1 calc R U P H 1
H23D H 0.492643 0.653534 0.935700 0.143 Uiso 0.54(2) 1 calc R U P H 1
C23B C 0.553(4) 0.530(3) 0.888(2) 0.096(8) Uiso 0.54(2) 1 d D U P H 1
H23E H 0.504915 0.502671 0.855586 0.143 Uiso 0.54(2) 1 calc R U P H 1
H23F H 0.606801 0.511069 0.883561 0.143 Uiso 0.54(2) 1 calc R U P H 1
H23G H 0.514918 0.501259 0.923084 0.143 Uiso 0.54(2) 1 calc R U P H 1
C23' C 0.566(2) 0.654(3) 0.9389(16) 0.060(7) Uiso 0.46(2) 1 d D U P H 2
H23H H 0.539929 0.607635 0.972868 0.072 Uiso 0.46(2) 1 calc R U P H 2
C23C C 0.541(5) 0.736(4) 0.952(2) 0.096(8) Uiso 0.46(2) 1 d D U P H 2
H23I H 0.465589 0.706531 0.952428 0.143 Uiso 0.46(2) 1 calc R U P H 2
H23J H 0.569841 0.766478 0.988940 0.143 Uiso 0.46(2) 1 calc R U P H 2
H23K H 0.571333 0.790263 0.922681 0.143 Uiso 0.46(2) 1 calc R U P H 2
C23D C 0.500(5) 0.588(4) 0.893(2) 0.096(8) Uiso 0.46(2) 1 d D U P H 2
H23L H 0.428302 0.571374 0.898740 0.143 Uiso 0.46(2) 1 calc R U P H 2
H23M H 0.525195 0.624655 0.856431 0.143 Uiso 0.46(2) 1 calc R U P H 2
H23N H 0.502963 0.523556 0.891526 0.143 Uiso 0.46(2) 1 calc R U P H 2
C31 C 0.9050(12) 0.6986(11) 0.8430(6) 0.036(3) Uani 1 1 d . U . . .
C32 C 0.8785(16) 0.6197(15) 0.8033(8) 0.054(4) Uani 1 1 d . U . . .
H32A H 0.809023 0.563966 0.801327 0.065 Uiso 1 1 calc R U . . .
C33 C 0.953(2) 0.6217(18) 0.7662(9) 0.067(5) Uani 1 1 d . U . . .
H33A H 0.936067 0.567017 0.739927 0.081 Uiso 1 1 calc R U . . .
C34 C 1.0565(18) 0.7095(19) 0.7693(9) 0.074(6) Uani 1 1 d . U . . .
H34A H 1.107967 0.715855 0.743203 0.089 Uiso 1 1 calc R U . . .
C35 C 1.0810(15) 0.7846(16) 0.8101(8) 0.054(5) Uani 1 1 d . U . . .
H35A H 1.150455 0.840324 0.812725 0.065 Uiso 1 1 calc R U . . .
C36 C 1.0071(13) 0.7811(12) 0.8477(6) 0.036(3) Uani 1 1 d . U . . .
C37 C 0.8273(13) 0.9599(13) 0.8884(7) 0.035(3) Uani 1 1 d . 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
Ho1 O1 2.257(14) . ?
Ho1 O1 2.257(14) 2_655 ?
Ho1 O1 2.257(14) 3_665 ?
Ho1 O6 2.532(10) 3_665 ?
Ho1 O6 2.532(10) . ?
Ho1 O6 2.532(10) 5_656 ?
Ho1 O6 2.532(10) 6_666 ?
Ho1 O6 2.532(10) 2_655 ?
Ho1 O6 2.532(10) 4_556 ?
Ho1 Ti1 3.550(2) . ?
Ho1 Ti1 3.550(2) 5_656 ?
Ho1 Ti1 3.550(2) 2_655 ?
Ho2 O21 2.304(14) . ?
Ho2 O21 2.304(14) 3_675 ?
Ho2 O21 2.304(14) 2_765 ?
Ho2 O25 2.537(9) 5_767 ?
Ho2 O25 2.537(9) 3_675 ?
Ho2 O25 2.537(9) 6_677 ?
Ho2 O25 2.537(9) 2_765 ?
Ho2 O25 2.537(9) 4_557 ?
Ho2 O25 2.537(9) . ?
Ho2 Ti2 3.561(3) 5_767 ?
Ho2 Ti2 3.561(3) 4_557 ?
Ho2 Ti2 3.561(3) 6_677 ?
Ti1 O3 1.780(12) . ?
Ti1 O4 1.869(11) . ?
Ti1 O1 1.913(9) . ?
Ti1 O2 1.986(9) . ?
Ti1 O5 2.014(11) . ?
Ti1 O6 2.164(11) . ?
Ti1 Ti1 2.969(5) 4_556 ?
Ti2 O23 1.766(12) . ?
Ti2 O24 1.867(10) . ?
Ti2 O21 1.895(10) . ?
Ti2 O22 2.001(9) . ?
Ti2 O26 2.001(11) . ?
Ti2 O25 2.193(10) . ?
Ti2 Ti2 2.974(4) 4_557 ?
O2 C2 1.52(3) . ?
O3 C3' 1.36(5) . ?
O3 C3 1.49(2) . ?
O4 C11 1.33(2) . ?
O5 C17 1.25(2) . ?
O6 C17 1.32(2) 3_665 ?
O22 C22 1.44(3) . ?
O23 C23' 1.43(3) . ?
O23 C23 1.46(3) . ?
O24 C31 1.341(18) . ?
O25 C37 1.281(19) 2_765 ?
O26 C37 1.245(18) . ?
C2 C2A 1.54(5) . ?
C2 C2B 1.62(6) . ?
C2 H2A 1.0000 . ?
C2A H2AA 0.9800 . ?
C2A H2AB 0.9800 . ?
C2A H2AC 0.9800 . ?
C2B H2BA 0.9800 . ?
C2B H2BB 0.9800 . ?
C2B H2BC 0.9800 . ?
C3 C3A 1.48(3) . ?
C3 C3B 1.52(3) . ?
C3 H3 1.0000 . ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?
C3A H3AC 0.9800 . ?
C3B H3BA 0.9800 . ?
C3B H3BB 0.9800 . ?
C3B H3BC 0.9800 . ?
C3' C3B' 1.50(3) . ?
C3' C3A' 1.50(3) . ?
C3' H3A' 1.0000 . ?
C3A' H3AD 0.9800 . ?
C3A' H3AE 0.9800 . ?
C3A' H3AF 0.9800 . ?
C3B' H3BD 0.9800 . ?
C3B' H3BE 0.9800 . ?
C3B' H3BF 0.9800 . ?
C11 C16 1.40(2) . ?
C11 C12 1.42(2) . ?
C12 C13 1.39(3) . ?
C12 H12A 0.9500 . ?
C13 C14 1.31(3) . ?
C13 H13A 0.9500 . ?
C14 C15 1.37(3) . ?
C14 H14A 0.9500 . ?
C15 C16 1.42(3) . ?
C15 H15A 0.9500 . ?
C16 C17 1.48(2) 3_665 ?
C22 C22A 1.34(7) . ?
C22 C22B 1.39(5) . ?
C22 H22' 1.0000 . ?
C22A H22A 0.9800 . ?
C22A H22B 0.9800 . ?
C22A H22C 0.9800 . ?
C22B H22D 0.9800 . ?
C22B H22E 0.9800 . ?
C22B H22F 0.9800 . ?
C23 C23B 1.45(3) . ?
C23 C23A 1.48(3) . ?
C23 H23A 1.0000 . ?
C23A H23B 0.9800 . ?
C23A H23C 0.9800 . ?
C23A H23D 0.9800 . ?
C23B H23E 0.9800 . ?
C23B H23F 0.9800 . ?
C23B H23G 0.9800 . ?
C23' C23D 1.47(3) . ?
C23' C23C 1.47(3) . ?
C23' H23H 1.0000 . ?
C23C H23I 0.9800 . ?
C23C H23J 0.9800 . ?
C23C H23K 0.9800 . ?
C23D H23L 0.9800 . ?
C23D H23M 0.9800 . ?
C23D H23N 0.9800 . ?
C31 C32 1.40(2) . ?
C31 C36 1.40(2) . ?
C32 C33 1.40(3) . ?
C32 H32A 0.9500 . ?
C33 C34 1.44(3) . ?
C33 H33A 0.9500 . ?
C34 C35 1.38(3) . ?
C34 H34A 0.9500 . ?
C35 C36 1.39(2) . ?
C35 H35A 0.9500 . ?
C36 C37 1.48(2) 2_765 ?

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 Ho1 O1 119.999(5) . 2_655 ?
O1 Ho1 O1 120.001(2) . 3_665 ?
O1 Ho1 O1 120.000(3) 2_655 3_665 ?
O1 Ho1 O6 135.1(2) . 3_665 ?
O1 Ho1 O6 73.1(3) 2_655 3_665 ?
O1 Ho1 O6 65.4(3) 3_665 3_665 ?
O1 Ho1 O6 65.4(3) . . ?
O1 Ho1 O6 135.1(2) 2_655 . ?
O1 Ho1 O6 73.1(3) 3_665 . ?
O6 Ho1 O6 76.1(3) 3_665 . ?
O1 Ho1 O6 73.0(3) . 5_656 ?
O1 Ho1 O6 65.4(3) 2_655 5_656 ?
O1 Ho1 O6 135.1(2) 3_665 5_656 ?
O6 Ho1 O6 138.32(16) 3_665 5_656 ?
O6 Ho1 O6 138.32(16) . 5_656 ?
O1 Ho1 O6 135.1(2) . 6_666 ?
O1 Ho1 O6 73.1(3) 2_655 6_666 ?
O1 Ho1 O6 65.4(3) 3_665 6_666 ?
O6 Ho1 O6 89.3(4) 3_665 6_666 ?
O6 Ho1 O6 138.32(17) . 6_666 ?
O6 Ho1 O6 76.1(3) 5_656 6_666 ?
O1 Ho1 O6 73.0(3) . 2_655 ?
O1 Ho1 O6 65.4(3) 2_655 2_655 ?
O1 Ho1 O6 135.1(2) 3_665 2_655 ?
O6 Ho1 O6 76.1(3) 3_665 2_655 ?
O6 Ho1 O6 76.1(3) . 2_655 ?
O6 Ho1 O6 89.3(4) 5_656 2_655 ?
O6 Ho1 O6 138.32(16) 6_666 2_655 ?
O1 Ho1 O6 65.4(3) . 4_556 ?
O1 Ho1 O6 135.1(2) 2_655 4_556 ?
O1 Ho1 O6 73.1(3) 3_665 4_556 ?
O6 Ho1 O6 138.32(17) 3_665 4_556 ?
O6 Ho1 O6 89.3(4) . 4_556 ?
O6 Ho1 O6 76.1(3) 5_656 4_556 ?
O6 Ho1 O6 76.1(3) 6_666 4_556 ?
O6 Ho1 O6 138.32(16) 2_655 4_556 ?
O1 Ho1 Ti1 28.84(17) . . ?
O1 Ho1 Ti1 130.3(3) 2_655 . ?
O1 Ho1 Ti1 103.3(3) 3_665 . ?
O6 Ho1 Ti1 108.0(2) 3_665 . ?
O6 Ho1 Ti1 37.1(2) . . ?
O6 Ho1 Ti1 101.2(2) 5_656 . ?
O6 Ho1 Ti1 153.7(2) 6_666 . ?
O6 Ho1 Ti1 66.9(2) 2_655 . ?
O6 Ho1 Ti1 77.9(2) 4_556 . ?
O1 Ho1 Ti1 103.3(3) . 5_656 ?
O1 Ho1 Ti1 28.84(17) 2_655 5_656 ?
O1 Ho1 Ti1 130.3(3) 3_665 5_656 ?
O6 Ho1 Ti1 101.2(2) 3_665 5_656 ?
O6 Ho1 Ti1 153.7(2) . 5_656 ?
O6 Ho1 Ti1 37.1(2) 5_656 5_656 ?
O6 Ho1 Ti1 66.9(2) 6_666 5_656 ?
O6 Ho1 Ti1 77.9(2) 2_655 5_656 ?
O6 Ho1 Ti1 108.0(2) 4_556 5_656 ?
Ti1 Ho1 Ti1 125.973(19) . 5_656 ?
O1 Ho1 Ti1 103.3(3) . 2_655 ?
O1 Ho1 Ti1 28.84(17) 2_655 2_655 ?
O1 Ho1 Ti1 130.3(3) 3_665 2_655 ?
O6 Ho1 Ti1 66.9(2) 3_665 2_655 ?
O6 Ho1 Ti1 108.0(2) . 2_655 ?
O6 Ho1 Ti1 77.9(2) 5_656 2_655 ?
O6 Ho1 Ti1 101.2(2) 6_666 2_655 ?
O6 Ho1 Ti1 37.1(2) 2_655 2_655 ?
O6 Ho1 Ti1 153.7(2) 4_556 2_655 ?
Ti1 Ho1 Ti1 103.76(5) . 2_655 ?
Ti1 Ho1 Ti1 49.43(8) 5_656 2_655 ?
O21 Ho2 O21 120.000(6) . 3_675 ?
O21 Ho2 O21 120.001(8) . 2_765 ?
O21 Ho2 O21 120.000(15) 3_675 2_765 ?
O21 Ho2 O25 135.6(2) . 5_767 ?
O21 Ho2 O25 72.5(3) 3_675 5_767 ?
O21 Ho2 O25 65.6(3) 2_765 5_767 ?
O21 Ho2 O25 72.5(3) . 3_675 ?
O21 Ho2 O25 65.6(3) 3_675 3_675 ?
O21 Ho2 O25 135.6(2) 2_765 3_675 ?
O25 Ho2 O25 137.93(16) 5_767 3_675 ?
O21 Ho2 O25 72.5(3) . 6_677 ?
O21 Ho2 O25 65.6(3) 3_675 6_677 ?
O21 Ho2 O25 135.6(2) 2_765 6_677 ?
O25 Ho2 O25 76.9(3) 5_767 6_677 ?
O25 Ho2 O25 88.2(4) 3_675 6_677 ?
O21 Ho2 O25 135.6(2) . 2_765 ?
O21 Ho2 O25 72.5(3) 3_675 2_765 ?
O21 Ho2 O25 65.6(3) 2_765 2_765 ?
O25 Ho2 O25 88.2(4) 5_767 2_765 ?
O25 Ho2 O25 76.9(3) 3_675 2_765 ?
O25 Ho2 O25 137.93(16) 6_677 2_765 ?
O21 Ho2 O25 65.6(3) . 4_557 ?
O21 Ho2 O25 135.6(2) 3_675 4_557 ?
O21 Ho2 O25 72.5(3) 2_765 4_557 ?
O25 Ho2 O25 76.9(3) 5_767 4_557 ?
O25 Ho2 O25 137.93(17) 3_675 4_557 ?
O25 Ho2 O25 76.9(3) 6_677 4_557 ?
O25 Ho2 O25 137.93(16) 2_765 4_557 ?
O21 Ho2 O25 65.6(3) . . ?
O21 Ho2 O25 135.6(2) 3_675 . ?
O21 Ho2 O25 72.5(3) 2_765 . ?
O25 Ho2 O25 137.93(16) 5_767 . ?
O25 Ho2 O25 76.9(3) 3_675 . ?
O25 Ho2 O25 137.93(17) 6_677 . ?
O25 Ho2 O25 76.9(3) 2_765 . ?
O25 Ho2 O25 88.2(4) 4_557 . ?
O21 Ho2 Ti2 130.0(3) . 5_767 ?
O21 Ho2 Ti2 103.6(4) 3_675 5_767 ?
O21 Ho2 Ti2 28.6(2) 2_765 5_767 ?
O25 Ho2 Ti2 37.6(2) 5_767 5_767 ?
O25 Ho2 Ti2 154.5(2) 3_675 5_767 ?
O25 Ho2 Ti2 108.7(2) 6_677 5_767 ?
O25 Ho2 Ti2 77.8(2) 2_765 5_767 ?
O25 Ho2 Ti2 66.3(2) 4_557 5_767 ?
O25 Ho2 Ti2 100.4(2) . 5_767 ?
O21 Ho2 Ti2 28.6(2) . 4_557 ?
O21 Ho2 Ti2 130.0(3) 3_675 4_557 ?
O21 Ho2 Ti2 103.6(4) 2_765 4_557 ?
O25 Ho2 Ti2 108.7(2) 5_767 4_557 ?
O25 Ho2 Ti2 100.4(2) 3_675 4_557 ?
O25 Ho2 Ti2 66.3(2) 6_677 4_557 ?
O25 Ho2 Ti2 154.5(2) 2_765 4_557 ?
O25 Ho2 Ti2 37.6(2) 4_557 4_557 ?
O25 Ho2 Ti2 77.8(2) . 4_557 ?
Ti2 Ho2 Ti2 103.80(4) 5_767 4_557 ?
O21 Ho2 Ti2 103.6(4) . 6_677 ?
O21 Ho2 Ti2 28.6(2) 3_675 6_677 ?
O21 Ho2 Ti2 130.0(4) 2_765 6_677 ?
O25 Ho2 Ti2 66.3(2) 5_767 6_677 ?
O25 Ho2 Ti2 77.8(2) 3_675 6_677 ?
O25 Ho2 Ti2 37.6(2) 6_677 6_677 ?
O25 Ho2 Ti2 100.4(2) 2_765 6_677 ?
O25 Ho2 Ti2 108.7(2) 4_557 6_677 ?
O25 Ho2 Ti2 154.5(2) . 6_677 ?
Ti2 Ho2 Ti2 103.80(4) 5_767 6_677 ?
Ti2 Ho2 Ti2 103.80(4) 4_557 6_677 ?
O3 Ti1 O4 94.5(5) . . ?
O3 Ti1 O1 104.7(6) . . ?
O4 Ti1 O1 160.1(6) . . ?
O3 Ti1 O2 98.6(6) . . ?
O4 Ti1 O2 95.8(5) . . ?
O1 Ti1 O2 76.4(4) . . ?
O3 Ti1 O5 90.5(5) . . ?
O4 Ti1 O5 94.4(5) . . ?
O1 Ti1 O5 90.8(4) . . ?
O2 Ti1 O5 165.8(5) . . ?
O3 Ti1 O6 169.5(5) . . ?
O4 Ti1 O6 83.1(4) . . ?
O1 Ti1 O6 78.9(5) . . ?
O2 Ti1 O6 91.9(5) . . ?
O5 Ti1 O6 79.5(4) . . ?
O3 Ti1 Ti1 90.9(3) . 4_556 ?
O4 Ti1 Ti1 137.3(4) . 4_556 ?
O1 Ti1 Ti1 39.1(3) . 4_556 ?
O2 Ti1 Ti1 41.6(3) . 4_556 ?
O5 Ti1 Ti1 127.9(3) . 4_556 ?
O6 Ti1 Ti1 97.8(3) . 4_556 ?
O3 Ti1 Ho1 136.4(4) . . ?
O4 Ti1 Ho1 128.1(4) . . ?
O1 Ti1 Ho1 34.7(4) . . ?
O2 Ti1 Ho1 87.1(4) . . ?
O5 Ti1 Ho1 78.8(3) . . ?
O6 Ti1 Ho1 44.9(3) . . ?
Ti1 Ti1 Ho1 65.29(4) 4_556 . ?
O23 Ti2 O24 95.0(5) . . ?
O23 Ti2 O21 104.3(5) . . ?
O24 Ti2 O21 160.3(6) . . ?
O23 Ti2 O22 96.9(6) . . ?
O24 Ti2 O22 97.4(5) . . ?
O21 Ti2 O22 76.4(5) . . ?
O23 Ti2 O26 91.6(5) . . ?
O24 Ti2 O26 92.9(5) . . ?
O21 Ti2 O26 90.8(5) . . ?
O22 Ti2 O26 166.0(5) . . ?
O23 Ti2 O25 171.4(4) . . ?
O24 Ti2 O25 81.8(4) . . ?
O21 Ti2 O25 79.7(5) . . ?
O22 Ti2 O25 91.5(5) . . ?
O26 Ti2 O25 80.7(4) . . ?
O23 Ti2 Ti2 90.3(3) . 4_557 ?
O24 Ti2 Ti2 139.4(3) . 4_557 ?
O21 Ti2 Ti2 38.3(4) . 4_557 ?
O22 Ti2 Ti2 42.0(3) . 4_557 ?
O26 Ti2 Ti2 127.2(3) . 4_557 ?
O25 Ti2 Ti2 97.3(2) . 4_557 ?
O23 Ti2 Ho2 137.2(4) . . ?
O24 Ti2 Ho2 126.7(3) . . ?
O21 Ti2 Ho2 35.7(4) . . ?
O22 Ti2 Ho2 87.7(3) . . ?
O26 Ti2 Ho2 78.5(3) . . ?
O25 Ti2 Ho2 44.9(2) . . ?
Ti2 Ti2 Ho2 65.32(4) 4_557 . ?
Ti1 O1 Ti1 101.8(6) . 4_556 ?
Ti1 O1 Ho1 116.5(5) . . ?
Ti1 O1 Ho1 116.5(5) 4_556 . ?
C2 O2 Ti1 130.1(4) . 4_556 ?
C2 O2 Ti1 130.1(4) . . ?
Ti1 O2 Ti1 96.8(6) 4_556 . ?
C3' O3 Ti1 173(2) . . ?
C3 O3 Ti1 137.8(14) . . ?
C11 O4 Ti1 139.3(11) . . ?
C17 O5 Ti1 137.0(11) . . ?
C17 O6 Ti1 130.6(10) 3_665 . ?
C17 O6 Ho1 131.4(10) 3_665 . ?
Ti1 O6 Ho1 97.9(4) . . ?
Ti2 O21 Ti2 103.4(7) . 4_557 ?
Ti2 O21 Ho2 115.7(5) . . ?
Ti2 O21 Ho2 115.7(5) 4_557 . ?
C22 O22 Ti2 130.2(5) . . ?
C22 O22 Ti2 130.2(5) . 4_557 ?
Ti2 O22 Ti2 96.0(6) . 4_557 ?
C23' O23 Ti2 162.0(19) . . ?
C23 O23 Ti2 130.2(15) . . ?
C31 O24 Ti2 141.3(9) . . ?
C37 O25 Ti2 131.1(10) 2_765 . ?
C37 O25 Ho2 131.2(10) 2_765 . ?
Ti2 O25 Ho2 97.4(3) . . ?
C37 O26 Ti2 137.2(12) . . ?
O2 C2 C2A 108(2) . . ?
O2 C2 C2B 110(3) . . ?
C2A C2 C2B 140(3) . . ?
O2 C2 H2A 94.3 . . ?
C2A C2 H2A 94.3 . . ?
C2B C2 H2A 94.3 . . ?
C2 C2A H2AA 109.5 . . ?
C2 C2A H2AB 109.5 . . ?
H2AA C2A H2AB 109.5 . . ?
C2 C2A H2AC 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
C2 C2B H2BA 109.5 . . ?
C2 C2B H2BB 109.5 . . ?
H2BA C2B H2BB 109.5 . . ?
C2 C2B H2BC 109.5 . . ?
H2BA C2B H2BC 109.5 . . ?
H2BB C2B H2BC 109.5 . . ?
C3A C3 O3 107(3) . . ?
C3A C3 C3B 107(2) . . ?
O3 C3 C3B 94(3) . . ?
C3A C3 H3 115.2 . . ?
O3 C3 H3 115.2 . . ?
C3B C3 H3 115.2 . . ?
C3 C3A H3AA 109.5 . . ?
C3 C3A H3AB 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
C3 C3A H3AC 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
C3 C3B H3BA 109.5 . . ?
C3 C3B H3BB 109.5 . . ?
H3BA C3B H3BB 109.5 . . ?
C3 C3B H3BC 109.5 . . ?
H3BA C3B H3BC 109.5 . . ?
H3BB C3B H3BC 109.5 . . ?
O3 C3' C3B' 113(4) . . ?
O3 C3' C3A' 108(4) . . ?
C3B' C3' C3A' 106(2) . . ?
O3 C3' H3A' 109.8 . . ?
C3B' C3' H3A' 109.8 . . ?
C3A' C3' H3A' 109.8 . . ?
C3' C3A' H3AD 109.5 . . ?
C3' C3A' H3AE 109.5 . . ?
H3AD C3A' H3AE 109.5 . . ?
C3' C3A' H3AF 109.5 . . ?
H3AD C3A' H3AF 109.5 . . ?
H3AE C3A' H3AF 109.5 . . ?
C3' C3B' H3BD 109.5 . . ?
C3' C3B' H3BE 109.5 . . ?
H3BD C3B' H3BE 109.5 . . ?
C3' C3B' H3BF 109.5 . . ?
H3BD C3B' H3BF 109.5 . . ?
H3BE C3B' H3BF 109.5 . . ?
O4 C11 C16 122.9(15) . . ?
O4 C11 C12 119.0(17) . . ?
C16 C11 C12 118.1(17) . . ?
C13 C12 C11 119(2) . . ?
C13 C12 H12A 120.6 . . ?
C11 C12 H12A 120.6 . . ?
C14 C13 C12 124(2) . . ?
C14 C13 H13A 117.8 . . ?
C12 C13 H13A 117.8 . . ?
C13 C14 C15 118(2) . . ?
C13 C14 H14A 121.0 . . ?
C15 C14 H14A 121.0 . . ?
C14 C15 C16 122(2) . . ?
C14 C15 H15A 118.9 . . ?
C16 C15 H15A 118.9 . . ?
C11 C16 C15 118.5(16) . . ?
C11 C16 C17 122.8(15) . 3_665 ?
C15 C16 C17 118.6(16) . 3_665 ?
O5 C17 O6 120.9(16) . 2_655 ?
O5 C17 C16 118.0(14) . 2_655 ?
O6 C17 C16 121.0(15) 2_655 2_655 ?
C22A C22 C22B 131(4) . . ?
C22A C22 O22 106(4) . . ?
C22B C22 O22 118(3) . . ?
C22A C22 H22' 97.4 . . ?
C22B C22 H22' 97.4 . . ?
O22 C22 H22' 97.4 . . ?
C22 C22A H22A 109.5 . . ?
C22 C22A H22B 109.5 . . ?
H22A C22A H22B 109.5 . . ?
C22 C22A H22C 109.5 . . ?
H22A C22A H22C 109.5 . . ?
H22B C22A H22C 109.5 . . ?
C22 C22B H22D 109.5 . . ?
C22 C22B H22E 109.5 . . ?
H22D C22B H22E 109.5 . . ?
C22 C22B H22F 109.5 . . ?
H22D C22B H22F 109.5 . . ?
H22E C22B H22F 109.5 . . ?
C23B C23 O23 111(3) . . ?
C23B C23 C23A 114(3) . . ?
O23 C23 C23A 103(3) . . ?
C23B C23 H23A 109.6 . . ?
O23 C23 H23A 109.6 . . ?
C23A C23 H23A 109.6 . . ?
C23 C23A H23B 109.5 . . ?
C23 C23A H23C 109.5 . . ?
H23B C23A H23C 109.5 . . ?
C23 C23A H23D 109.5 . . ?
H23B C23A H23D 109.5 . . ?
H23C C23A H23D 109.5 . . ?
C23 C23B H23E 109.5 . . ?
C23 C23B H23F 109.5 . . ?
H23E C23B H23F 109.5 . . ?
C23 C23B H23G 109.5 . . ?
H23E C23B H23G 109.5 . . ?
H23F C23B H23G 109.5 . . ?
O23 C23' C23D 117(4) . . ?
O23 C23' C23C 116(4) . . ?
C23D C23' C23C 111(3) . . ?
O23 C23' H23H 103.8 . . ?
C23D C23' H23H 103.8 . . ?
C23C C23' H23H 103.8 . . ?
C23' C23C H23I 109.5 . . ?
C23' C23C H23J 109.5 . . ?
H23I C23C H23J 109.5 . . ?
C23' C23C H23K 109.5 . . ?
H23I C23C H23K 109.5 . . ?
H23J C23C H23K 109.5 . . ?
C23' C23D H23L 109.5 . . ?
C23' C23D H23M 109.5 . . ?
H23L C23D H23M 109.5 . . ?
C23' C23D H23N 109.5 . . ?
H23L C23D H23N 109.5 . . ?
H23M C23D H23N 109.5 . . ?
O24 C31 C32 118.4(15) . . ?
O24 C31 C36 120.5(12) . . ?
C32 C31 C36 121.1(15) . . ?
C31 C32 C33 120.9(18) . . ?
C31 C32 H32A 119.5 . . ?
C33 C32 H32A 119.5 . . ?
C32 C33 C34 117.5(18) . . ?
C32 C33 H33A 121.2 . . ?
C34 C33 H33A 121.2 . . ?
C35 C34 C33 120.1(18) . . ?
C35 C34 H34A 119.9 . . ?
C33 C34 H34A 119.9 . . ?
C34 C35 C36 122.0(18) . . ?
C34 C35 H35A 119.0 . . ?
C36 C35 H35A 119.0 . . ?
C35 C36 C31 118.2(15) . . ?
C35 C36 C37 117.9(15) . 2_765 ?
C31 C36 C37 123.8(14) . 2_765 ?
O26 C37 O25 122.6(15) . 3_675 ?
O26 C37 C36 116.3(15) . 3_675 ?
O25 C37 C36 121.1(14) 3_675 3_675 ?

_refine_diff_density_max         3.177
_refine_diff_density_min         -0.844
_refine_diff_density_rms         0.188

####################################################################### 
# 
# 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_er_c
_database_code_depnum_ccdc_archive 'CCDC 1504164'
_audit_update_record             
;
2017-02-27 deposited with the CCDC.
2017-03-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C69 H87 Er O30 Ti6'
_chemical_formula_sum            'C69 H87 Er O30 Ti6'
_chemical_formula_weight         1851.04

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -9.4367 3.9380 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           174
_space_group_name_H-M_alt        'P -6'
_space_group_name_Hall           'P -6'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'

_cell_length_a                   15.0340(3)
_cell_length_b                   15.0340(3)
_cell_length_c                   23.8089(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4660.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9799
_cell_measurement_theta_min      3.39
_cell_measurement_theta_max      66.3

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_F_000             1882
_exptl_transmission_factor_min   0.818
_exptl_transmission_factor_max   1.000
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    6.329
_shelx_estimated_absorpt_T_min   0.413
_shelx_estimated_absorpt_T_max   0.543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.413
_exptl_absorpt_correction_T_max  0.543
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements (SADABS) 
;
_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         '30W microfocus sealed tube, Quazar optics'
_diffrn_measurement_device_type  'Bruker QUEST D8 CCD'
_diffrn_measurement_method       'Thin slice ω and φ scans'
_diffrn_reflns_number            40624
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.394
_diffrn_reflns_theta_max         66.495
_diffrn_reflns_theta_full        66.495
_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 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5643
_reflns_number_gt                5336
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.991
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_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 software package, narrow-frames'
_computing_cell_refinement       'refinement of XYZ centroids > 20sigma(I)'
_computing_data_reduction        
;
 Bruker SAINT software package, narrow frame algorithm
;
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_refine_special_details          
;Refined as a 2-component twin. Floppy iPr ligands restrained and 
treated isotropically. Residual electron density did not refine 
to anything meaningful, presumably disordered solvent., Twin
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1232P)²] 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_abs_structure_details 
;
 Flack x determined using 2498 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.334(6)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5643
_refine_ls_number_parameters     331
_refine_ls_number_restraints     208
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0520
_refine_ls_wR_factor_ref         0.1576
_refine_ls_wR_factor_gt          0.1540
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_restrained_S_all      1.108
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Er1 Er 0.666667 0.333333 0.500000 0.0241(5) Uani 1 6 d S T P . .
Er2 Er 1.000000 1.000000 1.000000 0.0223(4) Uani 1 6 d S T P . .
Ti1 Ti 0.47136(19) 0.36824(19) 0.56247(9) 0.0304(5) Uani 1 1 d . . . . .
Ti2 Ti 0.81995(19) 0.76178(18) 0.93786(9) 0.0312(5) Uani 1 1 d . . . . .
O1 O 0.5078(11) 0.3126(10) 0.500000 0.030(3) Uani 1 2 d S TU P . .
O2 O 0.4934(10) 0.4670(10) 0.500000 0.036(3) Uani 1 2 d S TU P C .
O3 O 0.3365(8) 0.3018(8) 0.5643(4) 0.039(2) Uani 1 1 d D U . . .
O4 O 0.4850(8) 0.4575(8) 0.6210(4) 0.044(3) Uani 1 1 d . U . . .
O5 O 0.4719(9) 0.2626(8) 0.6139(4) 0.041(2) Uani 1 1 d . U . . .
O6 O 0.6363(7) 0.4351(7) 0.5744(4) 0.031(2) Uani 1 1 d . U . . .
O21 O 0.8465(10) 0.8506(9) 1.000000 0.026(3) Uani 1 2 d S TU P . .
O22 O 0.8491(14) 0.6922(8) 1.000000 0.037(3) Uani 1 2 d S TU P G .
O23 O 0.6835(9) 0.6800(9) 0.9387(4) 0.043(3) Uani 1 1 d D U . . .
O24 O 0.8431(10) 0.6935(6) 0.8782(4) 0.043(2) Uani 1 1 d . U . . .
O25 O 0.9839(7) 0.8720(7) 0.9258(3) 0.031(2) Uani 1 1 d . U . . .
O26 O 0.8089(9) 0.8629(9) 0.8867(4) 0.039(2) Uani 1 1 d . U . . .
C2 C 0.486(2) 0.5586(19) 0.500000 0.062(7) Uani 1 2 d S TU P . .
H2A H 0.471336 0.559060 0.540881 0.074 Uiso 0.5 1 calc R U P A -1
C2A C 0.587(3) 0.647(3) 0.500000 0.108(12) Uani 1 2 d S TU P C .
H2AA H 0.635592 0.628745 0.517273 0.163 Uiso 0.5 1 calc R U P B -1
H2AB H 0.608805 0.669447 0.461268 0.163 Uiso 0.5 1 calc R U P B -1
H2AC H 0.587242 0.702211 0.521458 0.163 Uiso 0.5 1 calc R U P B -1
C2B C 0.396(3) 0.553(3) 0.4789(16) 0.074(12) Uani 0.5 1 d . U P C -1
H2BA H 0.337568 0.483125 0.484368 0.111 Uiso 0.5 1 calc R U P C -1
H2BB H 0.382324 0.601945 0.498873 0.111 Uiso 0.5 1 calc R U P C -1
H2BC H 0.403887 0.569180 0.438683 0.111 Uiso 0.5 1 calc R U P C -1
C3 C 0.259(2) 0.263(2) 0.6052(14) 0.071(7) Uiso 0.55(2) 1 d D U P D 1
H3 H 0.293473 0.268348 0.642028 0.085 Uiso 0.55(2) 1 calc R U P D 1
C3A C 0.208(4) 0.321(3) 0.611(2) 0.092(8) Uiso 0.55(2) 1 d D U P D 1
H3AA H 0.257982 0.392434 0.619081 0.138 Uiso 0.55(2) 1 calc R U P D 1
H3AB H 0.172508 0.317283 0.575328 0.138 Uiso 0.55(2) 1 calc R U P D 1
H3AC H 0.157267 0.291984 0.641084 0.138 Uiso 0.55(2) 1 calc R U P D 1
C3B C 0.200(4) 0.158(3) 0.593(2) 0.092(8) Uiso 0.55(2) 1 d D U P D 1
H3BA H 0.143284 0.125769 0.620254 0.138 Uiso 0.55(2) 1 calc R U P D 1
H3BB H 0.171223 0.149600 0.555095 0.138 Uiso 0.55(2) 1 calc R U P D 1
H3BC H 0.242435 0.126340 0.595342 0.138 Uiso 0.55(2) 1 calc R U P D 1
C3' C 0.230(2) 0.236(3) 0.5577(17) 0.071(7) Uiso 0.45(2) 1 d D U P D 2
H3A' H 0.215038 0.250113 0.518936 0.085 Uiso 0.45(2) 1 calc R U P D 2
C3A' C 0.174(4) 0.266(4) 0.593(2) 0.092(8) Uiso 0.45(2) 1 d D U P D 2
H3AD H 0.100368 0.218723 0.587985 0.138 Uiso 0.45(2) 1 calc R U P D 2
H3AE H 0.192577 0.263243 0.632419 0.138 Uiso 0.45(2) 1 calc R U P D 2
H3AF H 0.190768 0.335735 0.583746 0.138 Uiso 0.45(2) 1 calc R U P D 2
C3B' C 0.192(5) 0.127(3) 0.558(2) 0.092(8) Uiso 0.45(2) 1 d D U P D 2
H3BD H 0.117516 0.089678 0.553078 0.138 Uiso 0.45(2) 1 calc R U P D 2
H3BE H 0.224070 0.109319 0.527162 0.138 Uiso 0.45(2) 1 calc R U P D 2
H3BF H 0.209510 0.107055 0.593829 0.138 Uiso 0.45(2) 1 calc R U P D 2
C11 C 0.5582(11) 0.5283(10) 0.6547(6) 0.038(3) Uani 1 1 d . U . . .
C12 C 0.5294(13) 0.5762(13) 0.6946(6) 0.048(4) Uani 1 1 d . U . . .
H12A H 0.459565 0.558669 0.698165 0.058 Uiso 1 1 calc R U . . .
C13 C 0.6047(17) 0.6510(17) 0.7296(7) 0.063(5) Uani 1 1 d . U . . .
H13A H 0.585789 0.687966 0.754586 0.076 Uiso 1 1 calc R U . . .
C14 C 0.7040(17) 0.6723(19) 0.7289(8) 0.071(6) Uani 1 1 d . U . . .
H14A H 0.752780 0.720214 0.754651 0.085 Uiso 1 1 calc R U . . .
C15 C 0.7330(13) 0.6219(13) 0.6892(7) 0.052(4) Uani 1 1 d . U . . .
H15A H 0.801776 0.635183 0.688380 0.062 Uiso 1 1 calc R U . . .
C16 C 0.6597(12) 0.5512(11) 0.6505(6) 0.037(3) Uani 1 1 d . U . . .
C17 C 0.4984(11) 0.1953(11) 0.6110(6) 0.032(3) Uani 1 1 d . U . . .
C22 C 0.860(2) 0.602(2) 1.000000 0.069(7) Uani 1 2 d S TU P . .
H22' H 0.848953 0.586896 0.958835 0.083 Uiso 0.5 1 calc R U P E -1
C22A C 0.976(5) 0.648(5) 1.000000 0.145(18) Uani 1 2 d S TU P G .
H22A H 0.992530 0.593060 1.000000 0.217 Uiso 0.5 1 calc R U P F -1
H22B H 1.004524 0.690657 0.966392 0.217 Uiso 0.5 1 calc R U P F -1
H22C H 1.004524 0.690657 1.033608 0.217 Uiso 0.5 1 calc R U P F -1
C22B C 0.767(5) 0.511(3) 1.0190(16) 0.092(14) Uani 0.5 1 d . U P G -1
H22D H 0.777745 0.452072 1.018362 0.138 Uiso 0.5 1 calc R U P G -1
H22E H 0.751488 0.522621 1.057350 0.138 Uiso 0.5 1 calc R U P G -1
H22F H 0.710250 0.498537 0.994068 0.138 Uiso 0.5 1 calc R U P G -1
C23 C 0.609(2) 0.635(2) 0.8924(12) 0.060(6) Uiso 0.531(18) 1 d D U P H 1
H23A H 0.643534 0.671225 0.856827 0.073 Uiso 0.531(18) 1 calc R U P H 1
C23A C 0.519(3) 0.646(3) 0.9014(18) 0.081(6) Uiso 0.531(18) 1 d D U P H 1
H23B H 0.540796 0.718168 0.906829 0.121 Uiso 0.531(18) 1 calc R U P H 1
H23C H 0.473855 0.619096 0.868593 0.121 Uiso 0.531(18) 1 calc R U P H 1
H23D H 0.482149 0.606459 0.934813 0.121 Uiso 0.531(18) 1 calc R U P H 1
C23B C 0.571(3) 0.525(3) 0.8847(18) 0.081(6) Uiso 0.531(18) 1 d D U P H 1
H23E H 0.628890 0.513846 0.878430 0.121 Uiso 0.531(18) 1 calc R U P H 1
H23F H 0.533264 0.487915 0.918336 0.121 Uiso 0.531(18) 1 calc R U P H 1
H23G H 0.524970 0.500552 0.852116 0.121 Uiso 0.531(18) 1 calc R U P H 1
C23' C 0.576(2) 0.632(3) 0.9375(14) 0.060(6) Uiso 0.469(18) 1 d D U P H 2
H23H H 0.550212 0.589219 0.972249 0.073 Uiso 0.469(18) 1 calc R U P H 2
C23C C 0.550(4) 0.711(3) 0.9421(19) 0.081(6) Uiso 0.469(18) 1 d D U P H 2
H23I H 0.474802 0.679620 0.941390 0.121 Uiso 0.469(18) 1 calc R U P H 2
H23J H 0.576560 0.747905 0.977455 0.121 Uiso 0.469(18) 1 calc R U P H 2
H23K H 0.579619 0.758451 0.910502 0.121 Uiso 0.469(18) 1 calc R U P H 2
C23D C 0.528(4) 0.565(3) 0.8909(18) 0.081(6) Uiso 0.469(18) 1 d D U P H 2
H23L H 0.453037 0.535239 0.893633 0.121 Uiso 0.469(18) 1 calc R U P H 2
H23M H 0.552208 0.604013 0.855816 0.121 Uiso 0.469(18) 1 calc R U P H 2
H23N H 0.544492 0.509947 0.891250 0.121 Uiso 0.469(18) 1 calc R U P H 2
C31 C 0.9178(13) 0.7038(12) 0.8442(6) 0.044(3) Uani 1 1 d . U . . .
C32 C 0.8942(16) 0.6284(16) 0.8040(8) 0.067(5) Uani 1 1 d . U . . .
H32A H 0.826682 0.571381 0.800573 0.080 Uiso 1 1 calc R U . . .
C33 C 0.9715(17) 0.6390(16) 0.7694(8) 0.069(6) Uani 1 1 d . U . . .
H33A H 0.955952 0.586567 0.742523 0.083 Uiso 1 1 calc R U . . .
C34 C 1.0738(16) 0.7235(17) 0.7711(8) 0.071(6) Uani 1 1 d . U . . .
H34A H 1.124889 0.727694 0.745951 0.085 Uiso 1 1 calc R U . . .
C35 C 1.0954(16) 0.7975(15) 0.8098(7) 0.061(5) Uani 1 1 d . U . . .
H35A H 1.162639 0.855493 0.811588 0.073 Uiso 1 1 calc R U . . .
C36 C 1.0185(12) 0.7894(11) 0.8479(6) 0.037(3) Uani 1 1 d . U . . .
C37 C 0.8269(12) 0.9538(13) 0.8900(7) 0.034(3) Uani 1 1 d . 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
Er1 O1 2.248(14) . ?
Er1 O1 2.248(14) 2_655 ?
Er1 O1 2.248(14) 3_665 ?
Er1 O6 2.527(8) . ?
Er1 O6 2.527(8) 3_665 ?
Er1 O6 2.527(8) 5_656 ?
Er1 O6 2.527(8) 6_666 ?
Er1 O6 2.527(8) 2_655 ?
Er1 O6 2.527(8) 4_556 ?
Er1 Ti1 3.557(2) 5_656 ?
Er1 Ti1 3.557(2) 2_655 ?
Er1 Ti1 3.557(2) 3_665 ?
Er2 O21 2.278(13) . ?
Er2 O21 2.278(13) 2_765 ?
Er2 O21 2.278(13) 3_675 ?
Er2 O25 2.534(9) 4_557 ?
Er2 O25 2.534(9) 5_767 ?
Er2 O25 2.534(9) 2_765 ?
Er2 O25 2.534(9) . ?
Er2 O25 2.534(9) 3_675 ?
Er2 O25 2.534(9) 6_677 ?
Er2 Ti2 3.556(2) 5_767 ?
Er2 Ti2 3.556(2) 6_677 ?
Er2 Ti2 3.556(2) 4_557 ?
Ti1 O3 1.756(11) . ?
Ti1 O4 1.874(10) . ?
Ti1 O1 1.916(9) . ?
Ti1 O2 2.009(9) . ?
Ti1 O5 2.009(10) . ?
Ti1 O6 2.179(9) . ?
Ti1 Ti1 2.975(4) 4_556 ?
Ti2 O23 1.789(12) . ?
Ti2 O24 1.884(10) . ?
Ti2 O21 1.897(8) . ?
Ti2 O22 1.983(10) . ?
Ti2 O26 2.018(12) . ?
Ti2 O25 2.195(10) . ?
Ti2 Ti2 2.959(4) 4_557 ?
O2 C2 1.43(3) . ?
O3 C3 1.40(3) . ?
O3 C3' 1.41(3) . ?
O4 C11 1.347(17) . ?
O5 C17 1.260(17) . ?
O6 C17 1.297(18) 3_665 ?
O22 C22 1.45(3) . ?
O23 C23' 1.40(3) . ?
O23 C23 1.47(2) . ?
O24 C31 1.33(2) . ?
O25 C37 1.260(18) 2_765 ?
O26 C37 1.257(17) . ?
C2 C2B 1.42(4) . ?
C2 C2A 1.43(5) . ?
C2 H2A 1.0000 . ?
C2A H2AA 0.9800 . ?
C2A H2AB 0.9800 . ?
C2A H2AC 0.9800 . ?
C2B H2BA 0.9800 . ?
C2B H2BB 0.9800 . ?
C2B H2BC 0.9800 . ?
C3 C3B 1.40(3) . ?
C3 C3A 1.43(3) . ?
C3 H3 1.0000 . ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?
C3A H3AC 0.9800 . ?
C3B H3BA 0.9800 . ?
C3B H3BB 0.9800 . ?
C3B H3BC 0.9800 . ?
C3' C3A' 1.41(3) . ?
C3' C3B' 1.44(3) . ?
C3' H3A' 1.0000 . ?
C3A' H3AD 0.9800 . ?
C3A' H3AE 0.9800 . ?
C3A' H3AF 0.9800 . ?
C3B' H3BD 0.9800 . ?
C3B' H3BE 0.9800 . ?
C3B' H3BF 0.9800 . ?
C11 C12 1.386(19) . ?
C11 C16 1.39(2) . ?
C12 C13 1.40(3) . ?
C12 H12A 0.9500 . ?
C13 C14 1.36(3) . ?
C13 H13A 0.9500 . ?
C14 C15 1.41(3) . ?
C14 H14A 0.9500 . ?
C15 C16 1.42(2) . ?
C15 H15A 0.9500 . ?
C16 C17 1.47(2) 3_665 ?
C22 C22B 1.45(5) . ?
C22 C22A 1.52(7) . ?
C22 H22' 1.0000 . ?
C22A H22A 0.9800 . ?
C22A H22B 0.9800 . ?
C22A H22C 0.9800 . ?
C22B H22D 0.9800 . ?
C22B H22E 0.9800 . ?
C22B H22F 0.9800 . ?
C23 C23B 1.46(3) . ?
C23 C23A 1.46(3) . ?
C23 H23A 1.0000 . ?
C23A H23B 0.9800 . ?
C23A H23C 0.9800 . ?
C23A H23D 0.9800 . ?
C23B H23E 0.9800 . ?
C23B H23F 0.9800 . ?
C23B H23G 0.9800 . ?
C23' C23C 1.43(3) . ?
C23' C23D 1.43(3) . ?
C23' H23H 1.0000 . ?
C23C H23I 0.9800 . ?
C23C H23J 0.9800 . ?
C23C H23K 0.9800 . ?
C23D H23L 0.9800 . ?
C23D H23M 0.9800 . ?
C23D H23N 0.9800 . ?
C31 C32 1.39(2) . ?
C31 C36 1.42(2) . ?
C32 C33 1.37(3) . ?
C32 H32A 0.9500 . ?
C33 C34 1.42(3) . ?
C33 H33A 0.9500 . ?
C34 C35 1.35(3) . ?
C34 H34A 0.9500 . ?
C35 C36 1.43(2) . ?
C35 H35A 0.9500 . ?
C36 C37 1.50(2) 2_765 ?

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 Er1 O1 120.000(6) . 2_655 ?
O1 Er1 O1 120.000(2) . 3_665 ?
O1 Er1 O1 120.000(3) 2_655 3_665 ?
O1 Er1 O6 65.4(3) . . ?
O1 Er1 O6 135.2(2) 2_655 . ?
O1 Er1 O6 73.0(3) 3_665 . ?
O1 Er1 O6 135.2(2) . 3_665 ?
O1 Er1 O6 73.0(3) 2_655 3_665 ?
O1 Er1 O6 65.4(3) 3_665 3_665 ?
O6 Er1 O6 76.3(3) . 3_665 ?
O1 Er1 O6 73.0(3) . 5_656 ?
O1 Er1 O6 65.4(3) 2_655 5_656 ?
O1 Er1 O6 135.2(2) 3_665 5_656 ?
O6 Er1 O6 138.21(16) . 5_656 ?
O6 Er1 O6 138.21(15) 3_665 5_656 ?
O1 Er1 O6 135.2(2) . 6_666 ?
O1 Er1 O6 73.0(3) 2_655 6_666 ?
O1 Er1 O6 65.4(3) 3_665 6_666 ?
O6 Er1 O6 138.21(16) . 6_666 ?
O6 Er1 O6 89.0(4) 3_665 6_666 ?
O6 Er1 O6 76.3(3) 5_656 6_666 ?
O1 Er1 O6 73.0(3) . 2_655 ?
O1 Er1 O6 65.4(3) 2_655 2_655 ?
O1 Er1 O6 135.2(2) 3_665 2_655 ?
O6 Er1 O6 76.3(3) . 2_655 ?
O6 Er1 O6 76.3(3) 3_665 2_655 ?
O6 Er1 O6 89.0(4) 5_656 2_655 ?
O6 Er1 O6 138.21(15) 6_666 2_655 ?
O1 Er1 O6 65.4(3) . 4_556 ?
O1 Er1 O6 135.2(2) 2_655 4_556 ?
O1 Er1 O6 73.0(3) 3_665 4_556 ?
O6 Er1 O6 89.0(4) . 4_556 ?
O6 Er1 O6 138.21(16) 3_665 4_556 ?
O6 Er1 O6 76.3(3) 5_656 4_556 ?
O6 Er1 O6 76.3(3) 6_666 4_556 ?
O6 Er1 O6 138.21(16) 2_655 4_556 ?
O1 Er1 Ti1 103.6(3) . 5_656 ?
O1 Er1 Ti1 28.66(17) 2_655 5_656 ?
O1 Er1 Ti1 130.0(3) 3_665 5_656 ?
O6 Er1 Ti1 154.0(2) . 5_656 ?
O6 Er1 Ti1 100.9(2) 3_665 5_656 ?
O6 Er1 Ti1 37.4(2) 5_656 5_656 ?
O6 Er1 Ti1 66.6(2) 6_666 5_656 ?
O6 Er1 Ti1 78.0(2) 2_655 5_656 ?
O6 Er1 Ti1 108.2(2) 4_556 5_656 ?
O1 Er1 Ti1 103.6(3) . 2_655 ?
O1 Er1 Ti1 28.66(17) 2_655 2_655 ?
O1 Er1 Ti1 130.0(3) 3_665 2_655 ?
O6 Er1 Ti1 108.2(2) . 2_655 ?
O6 Er1 Ti1 66.6(2) 3_665 2_655 ?
O6 Er1 Ti1 78.0(2) 5_656 2_655 ?
O6 Er1 Ti1 100.9(2) 6_666 2_655 ?
O6 Er1 Ti1 37.4(2) 2_655 2_655 ?
O6 Er1 Ti1 154.0(2) 4_556 2_655 ?
Ti1 Er1 Ti1 49.44(7) 5_656 2_655 ?
O1 Er1 Ti1 130.0(3) . 3_665 ?
O1 Er1 Ti1 103.6(3) 2_655 3_665 ?
O1 Er1 Ti1 28.66(17) 3_665 3_665 ?
O6 Er1 Ti1 66.6(2) . 3_665 ?
O6 Er1 Ti1 37.4(2) 3_665 3_665 ?
O6 Er1 Ti1 154.0(2) 5_656 3_665 ?
O6 Er1 Ti1 78.0(2) 6_666 3_665 ?
O6 Er1 Ti1 108.2(2) 2_655 3_665 ?
O6 Er1 Ti1 100.9(2) 4_556 3_665 ?
Ti1 Er1 Ti1 125.976(17) 5_656 3_665 ?
Ti1 Er1 Ti1 103.75(4) 2_655 3_665 ?
O21 Er2 O21 120.000(6) . 2_765 ?
O21 Er2 O21 120.000(6) . 3_675 ?
O21 Er2 O21 120.000(5) 2_765 3_675 ?
O21 Er2 O25 65.5(3) . 4_557 ?
O21 Er2 O25 72.6(3) 2_765 4_557 ?
O21 Er2 O25 135.5(2) 3_675 4_557 ?
O21 Er2 O25 135.5(2) . 5_767 ?
O21 Er2 O25 65.5(3) 2_765 5_767 ?
O21 Er2 O25 72.6(3) 3_675 5_767 ?
O25 Er2 O25 76.7(3) 4_557 5_767 ?
O21 Er2 O25 135.5(2) . 2_765 ?
O21 Er2 O25 65.5(3) 2_765 2_765 ?
O21 Er2 O25 72.6(3) 3_675 2_765 ?
O25 Er2 O25 138.01(15) 4_557 2_765 ?
O25 Er2 O25 88.5(4) 5_767 2_765 ?
O21 Er2 O25 65.5(3) . . ?
O21 Er2 O25 72.6(3) 2_765 . ?
O21 Er2 O25 135.5(2) 3_675 . ?
O25 Er2 O25 88.5(4) 4_557 . ?
O25 Er2 O25 138.01(15) 5_767 . ?
O25 Er2 O25 76.7(3) 2_765 . ?
O21 Er2 O25 72.6(3) . 3_675 ?
O21 Er2 O25 135.5(2) 2_765 3_675 ?
O21 Er2 O25 65.5(3) 3_675 3_675 ?
O25 Er2 O25 138.01(15) 4_557 3_675 ?
O25 Er2 O25 138.01(15) 5_767 3_675 ?
O25 Er2 O25 76.7(3) 2_765 3_675 ?
O25 Er2 O25 76.7(3) . 3_675 ?
O21 Er2 O25 72.6(3) . 6_677 ?
O21 Er2 O25 135.5(2) 2_765 6_677 ?
O21 Er2 O25 65.5(3) 3_675 6_677 ?
O25 Er2 O25 76.7(3) 4_557 6_677 ?
O25 Er2 O25 76.7(3) 5_767 6_677 ?
O25 Er2 O25 138.01(15) 2_765 6_677 ?
O25 Er2 O25 138.01(15) . 6_677 ?
O25 Er2 O25 88.5(4) 3_675 6_677 ?
O21 Er2 Ti2 129.9(3) . 5_767 ?
O21 Er2 Ti2 28.50(18) 2_765 5_767 ?
O21 Er2 Ti2 103.7(3) 3_675 5_767 ?
O25 Er2 Ti2 66.3(2) 4_557 5_767 ?
O25 Er2 Ti2 37.8(2) 5_767 5_767 ?
O25 Er2 Ti2 77.9(2) 2_765 5_767 ?
O25 Er2 Ti2 100.3(2) . 5_767 ?
O25 Er2 Ti2 154.4(2) 3_675 5_767 ?
O25 Er2 Ti2 108.8(2) 6_677 5_767 ?
O21 Er2 Ti2 103.7(3) . 6_677 ?
O21 Er2 Ti2 129.9(3) 2_765 6_677 ?
O21 Er2 Ti2 28.50(17) 3_675 6_677 ?
O25 Er2 Ti2 108.8(2) 4_557 6_677 ?
O25 Er2 Ti2 66.3(2) 5_767 6_677 ?
O25 Er2 Ti2 100.3(2) 2_765 6_677 ?
O25 Er2 Ti2 154.4(2) . 6_677 ?
O25 Er2 Ti2 77.9(2) 3_675 6_677 ?
O25 Er2 Ti2 37.8(2) 6_677 6_677 ?
Ti2 Er2 Ti2 103.91(4) 5_767 6_677 ?
O21 Er2 Ti2 28.50(17) . 4_557 ?
O21 Er2 Ti2 103.7(3) 2_765 4_557 ?
O21 Er2 Ti2 129.9(3) 3_675 4_557 ?
O25 Er2 Ti2 37.8(2) 4_557 4_557 ?
O25 Er2 Ti2 108.8(2) 5_767 4_557 ?
O25 Er2 Ti2 154.4(2) 2_765 4_557 ?
O25 Er2 Ti2 77.9(2) . 4_557 ?
O25 Er2 Ti2 100.3(2) 3_675 4_557 ?
O25 Er2 Ti2 66.3(2) 6_677 4_557 ?
Ti2 Er2 Ti2 103.91(4) 5_767 4_557 ?
Ti2 Er2 Ti2 103.91(4) 6_677 4_557 ?
O3 Ti1 O4 94.1(5) . . ?
O3 Ti1 O1 105.8(5) . . ?
O4 Ti1 O1 159.6(5) . . ?
O3 Ti1 O2 99.0(5) . . ?
O4 Ti1 O2 95.9(5) . . ?
O1 Ti1 O2 76.7(4) . . ?
O3 Ti1 O5 89.7(5) . . ?
O4 Ti1 O5 94.0(5) . . ?
O1 Ti1 O5 90.7(4) . . ?
O2 Ti1 O5 166.3(5) . . ?
O3 Ti1 O6 169.4(4) . . ?
O4 Ti1 O6 83.2(4) . . ?
O1 Ti1 O6 78.1(5) . . ?
O2 Ti1 O6 91.5(4) . . ?
O5 Ti1 O6 80.3(4) . . ?
O3 Ti1 Ti1 91.4(3) . 4_556 ?
O4 Ti1 Ti1 138.1(3) . 4_556 ?
O1 Ti1 Ti1 39.1(3) . 4_556 ?
O2 Ti1 Ti1 42.2(3) . 4_556 ?
O5 Ti1 Ti1 127.6(3) . 4_556 ?
O6 Ti1 Ti1 97.5(2) . 4_556 ?
O3 Ti1 Er1 136.9(4) . . ?
O4 Ti1 Er1 127.9(3) . . ?
O1 Ti1 Er1 34.2(4) . . ?
O2 Ti1 Er1 87.5(3) . . ?
O5 Ti1 Er1 79.0(3) . . ?
O6 Ti1 Er1 44.7(2) . . ?
Ti1 Ti1 Er1 65.28(4) 4_556 . ?
O23 Ti2 O24 95.4(5) . . ?
O23 Ti2 O21 103.9(5) . . ?
O24 Ti2 O21 160.1(6) . . ?
O23 Ti2 O22 96.3(6) . . ?
O24 Ti2 O22 97.2(4) . . ?
O21 Ti2 O22 76.4(4) . . ?
O23 Ti2 O26 91.5(5) . . ?
O24 Ti2 O26 93.6(4) . . ?
O21 Ti2 O26 90.4(5) . . ?
O22 Ti2 O26 166.0(4) . . ?
O23 Ti2 O25 171.6(4) . . ?
O24 Ti2 O25 82.5(4) . . ?
O21 Ti2 O25 79.0(5) . . ?
O22 Ti2 O25 92.0(6) . . ?
O26 Ti2 O25 80.6(4) . . ?
O23 Ti2 Ti2 89.4(3) . 4_557 ?
O24 Ti2 Ti2 138.9(3) . 4_557 ?
O21 Ti2 Ti2 38.8(3) . 4_557 ?
O22 Ti2 Ti2 41.8(3) . 4_557 ?
O26 Ti2 Ti2 127.1(3) . 4_557 ?
O25 Ti2 Ti2 97.5(2) . 4_557 ?
O23 Ti2 Er2 136.2(4) . . ?
O24 Ti2 Er2 127.4(4) . . ?
O21 Ti2 Er2 35.0(4) . . ?
O22 Ti2 Er2 87.9(3) . . ?
O26 Ti2 Er2 78.5(3) . . ?
O25 Ti2 Er2 45.0(2) . . ?
Ti2 Ti2 Er2 65.42(4) 4_557 . ?
Ti1 O1 Ti1 101.8(6) 4_556 . ?
Ti1 O1 Er1 117.1(5) 4_556 . ?
Ti1 O1 Er1 117.1(5) . . ?
C2 O2 Ti1 130.3(4) . 4_556 ?
C2 O2 Ti1 130.3(4) . . ?
Ti1 O2 Ti1 95.5(6) 4_556 . ?
C3 O3 Ti1 137.4(16) . . ?
C3' O3 Ti1 168.5(18) . . ?
C11 O4 Ti1 139.6(9) . . ?
C17 O5 Ti1 136.7(11) . . ?
C17 O6 Ti1 130.0(8) 3_665 . ?
C17 O6 Er1 131.9(8) 3_665 . ?
Ti1 O6 Er1 97.9(3) . . ?
Ti2 O21 Ti2 102.5(6) 4_557 . ?
Ti2 O21 Er2 116.5(5) 4_557 . ?
Ti2 O21 Er2 116.5(5) . . ?
C22 O22 Ti2 130.8(3) . 4_557 ?
C22 O22 Ti2 130.8(3) . . ?
Ti2 O22 Ti2 96.5(6) 4_557 . ?
C23' O23 Ti2 169.8(17) . . ?
C23 O23 Ti2 130.9(13) . . ?
C31 O24 Ti2 140.5(9) . . ?
C37 O25 Ti2 130.2(10) 2_765 . ?
C37 O25 Er2 132.3(10) 2_765 . ?
Ti2 O25 Er2 97.3(3) . . ?
C37 O26 Ti2 136.8(12) . . ?
C2B C2 C2A 127(3) . . ?
C2B C2 O2 118(2) . . ?
C2A C2 O2 110(3) . . ?
C2B C2 H2A 97.6 . . ?
C2A C2 H2A 97.6 . . ?
O2 C2 H2A 97.6 . . ?
C2 C2A H2AA 109.5 . . ?
C2 C2A H2AB 109.5 . . ?
H2AA C2A H2AB 109.5 . . ?
C2 C2A H2AC 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
C2 C2B H2BA 109.5 . . ?
C2 C2B H2BB 109.5 . . ?
H2BA C2B H2BB 109.5 . . ?
C2 C2B H2BC 109.5 . . ?
H2BA C2B H2BC 109.5 . . ?
H2BB C2B H2BC 109.5 . . ?
C3B C3 O3 105(3) . . ?
C3B C3 C3A 118(3) . . ?
O3 C3 C3A 113(3) . . ?
C3B C3 H3 106.7 . . ?
O3 C3 H3 106.7 . . ?
C3A C3 H3 106.7 . . ?
C3 C3A H3AA 109.5 . . ?
C3 C3A H3AB 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
C3 C3A H3AC 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
C3 C3B H3BA 109.5 . . ?
C3 C3B H3BB 109.5 . . ?
H3BA C3B H3BB 109.5 . . ?
C3 C3B H3BC 109.5 . . ?
H3BA C3B H3BC 109.5 . . ?
H3BB C3B H3BC 109.5 . . ?
O3 C3' C3A' 111(3) . . ?
O3 C3' C3B' 118(4) . . ?
C3A' C3' C3B' 114(3) . . ?
O3 C3' H3A' 104.4 . . ?
C3A' C3' H3A' 104.4 . . ?
C3B' C3' H3A' 104.4 . . ?
C3' C3A' H3AD 109.5 . . ?
C3' C3A' H3AE 109.5 . . ?
H3AD C3A' H3AE 109.5 . . ?
C3' C3A' H3AF 109.5 . . ?
H3AD C3A' H3AF 109.5 . . ?
H3AE C3A' H3AF 109.5 . . ?
C3' C3B' H3BD 109.5 . . ?
C3' C3B' H3BE 109.5 . . ?
H3BD C3B' H3BE 109.5 . . ?
C3' C3B' H3BF 109.5 . . ?
H3BD C3B' H3BF 109.5 . . ?
H3BE C3B' H3BF 109.5 . . ?
O4 C11 C12 118.3(13) . . ?
O4 C11 C16 121.0(12) . . ?
C12 C11 C16 120.7(14) . . ?
C11 C12 C13 119.1(16) . . ?
C11 C12 H12A 120.4 . . ?
C13 C12 H12A 120.4 . . ?
C14 C13 C12 122.2(17) . . ?
C14 C13 H13A 118.9 . . ?
C12 C13 H13A 118.9 . . ?
C13 C14 C15 118.6(19) . . ?
C13 C14 H14A 120.7 . . ?
C15 C14 H14A 120.7 . . ?
C14 C15 C16 120.3(17) . . ?
C14 C15 H15A 119.8 . . ?
C16 C15 H15A 119.8 . . ?
C11 C16 C15 118.8(14) . . ?
C11 C16 C17 124.7(13) . 3_665 ?
C15 C16 C17 116.4(14) . 3_665 ?
O5 C17 O6 121.7(14) . 2_655 ?
O5 C17 C16 116.9(13) . 2_655 ?
O6 C17 C16 121.4(12) 2_655 2_655 ?
O22 C22 C22B 112(3) . . ?
O22 C22 C22A 102(3) . . ?
C22B C22 C22A 141(4) . . ?
O22 C22 H22' 97.2 . . ?
C22B C22 H22' 97.2 . . ?
C22A C22 H22' 97.2 . . ?
C22 C22A H22A 109.5 . . ?
C22 C22A H22B 109.5 . . ?
H22A C22A H22B 109.5 . . ?
C22 C22A H22C 109.5 . . ?
H22A C22A H22C 109.5 . . ?
H22B C22A H22C 109.5 . . ?
C22 C22B H22D 109.5 . . ?
C22 C22B H22E 109.5 . . ?
H22D C22B H22E 109.5 . . ?
C22 C22B H22F 109.5 . . ?
H22D C22B H22F 109.5 . . ?
H22E C22B H22F 109.5 . . ?
C23B C23 C23A 106(2) . . ?
C23B C23 O23 113(3) . . ?
C23A C23 O23 112(3) . . ?
C23B C23 H23A 108.5 . . ?
C23A C23 H23A 108.5 . . ?
O23 C23 H23A 108.5 . . ?
C23 C23A H23B 109.5 . . ?
C23 C23A H23C 109.5 . . ?
H23B C23A H23C 109.5 . . ?
C23 C23A H23D 109.5 . . ?
H23B C23A H23D 109.5 . . ?
H23C C23A H23D 109.5 . . ?
C23 C23B H23E 109.5 . . ?
C23 C23B H23F 109.5 . . ?
H23E C23B H23F 109.5 . . ?
C23 C23B H23G 109.5 . . ?
H23E C23B H23G 109.5 . . ?
H23F C23B H23G 109.5 . . ?
O23 C23' C23C 107(3) . . ?
O23 C23' C23D 115(3) . . ?
C23C C23' C23D 113(3) . . ?
O23 C23' H23H 106.9 . . ?
C23C C23' H23H 106.9 . . ?
C23D C23' H23H 106.9 . . ?
C23' C23C H23I 109.5 . . ?
C23' C23C H23J 109.5 . . ?
H23I C23C H23J 109.5 . . ?
C23' C23C H23K 109.5 . . ?
H23I C23C H23K 109.5 . . ?
H23J C23C H23K 109.5 . . ?
C23' C23D H23L 109.5 . . ?
C23' C23D H23M 109.5 . . ?
H23L C23D H23M 109.5 . . ?
C23' C23D H23N 109.5 . . ?
H23L C23D H23N 109.5 . . ?
H23M C23D H23N 109.5 . . ?
O24 C31 C32 118.0(15) . . ?
O24 C31 C36 121.7(13) . . ?
C32 C31 C36 120.3(16) . . ?
C33 C32 C31 117.7(18) . . ?
C33 C32 H32A 121.1 . . ?
C31 C32 H32A 121.1 . . ?
C32 C33 C34 124.3(17) . . ?
C32 C33 H33A 117.8 . . ?
C34 C33 H33A 117.8 . . ?
C35 C34 C33 117.4(19) . . ?
C35 C34 H34A 121.3 . . ?
C33 C34 H34A 121.3 . . ?
C34 C35 C36 120.8(19) . . ?
C34 C35 H35A 119.6 . . ?
C36 C35 H35A 119.6 . . ?
C31 C36 C35 119.4(14) . . ?
C31 C36 C37 121.8(13) . 2_765 ?
C35 C36 C37 118.9(15) . 2_765 ?
O26 C37 O25 122.0(15) . 3_675 ?
O26 C37 C36 114.6(15) . 3_675 ?
O25 C37 C36 123.4(14) 3_675 3_675 ?

_refine_diff_density_max         1.776
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.175

####################################################################### 
# 
# 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_dy_b
_database_code_depnum_ccdc_archive 'CCDC 1504163'
_audit_update_record             
;
2017-02-27 deposited with the CCDC.
2017-03-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C69 H87 Dy O30 Ti6'
_chemical_formula_sum            'C69 H87 Dy O30 Ti6'
_chemical_formula_weight         1846.28

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -9.8046 9.8477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           174
_space_group_name_H-M_alt        'P -6'
_space_group_name_Hall           'P -6'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'

_cell_length_a                   14.9065(3)
_cell_length_b                   14.9065(3)
_cell_length_c                   23.6229(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4545.8(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9449
_cell_measurement_theta_min      3.42
_cell_measurement_theta_max      65.1

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_F_000             1878
_exptl_transmission_factor_min   0.747
_exptl_transmission_factor_max   1.000
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    9.172
_shelx_estimated_absorpt_T_min   0.261
_shelx_estimated_absorpt_T_max   0.289
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.261
_exptl_absorpt_correction_T_max  0.289
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements (SADABS) 
;

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         '30W microfocus sealed tube, Quazar optics'
_diffrn_measurement_device_type  'Bruker QUEST D8 CCD'
_diffrn_measurement_method       'Thin slice ω and φ scans'
_diffrn_reflns_number            26874
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.423
_diffrn_reflns_theta_max         65.170
_diffrn_reflns_theta_full        65.170
_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 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             5239
_reflns_number_gt                4938
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.974
_reflns_Friedel_fraction_max     0.983
_reflns_Friedel_fraction_full    0.983

_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 software package, narrow-frames'
_computing_cell_refinement       'refinement of XYZ centroids > 20sigma(I)'
_computing_data_reduction        
;
Bruker SAINT software package, narrow frame algorithm
;
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_refine_special_details          
;Refined as a 2-component twin. Residual electron density did not resolve
into anything meaningful - presumably solvent.
 The iPr groups have been restrained and modelled isotropically as they are
 floppy., Twin
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1246P)²] 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_abs_structure_details 
;
 Flack x determined using 2242 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.021(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5239
_refine_ls_number_parameters     331
_refine_ls_number_restraints     208
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0550
_refine_ls_wR_factor_ref         0.1647
_refine_ls_wR_factor_gt          0.1594
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_restrained_S_all      1.107
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Dy1 Dy 0.333333 0.666667 0.500000 0.0240(5) Uani 1 6 d S T P . .
Dy2 Dy 0.000000 0.000000 0.000000 0.0236(5) Uani 1 6 d S T P . .
Ti1 Ti 0.5330(2) 0.6357(2) 0.43712(10) 0.0318(6) Uani 1 1 d . . . . .
Ti2 Ti 0.1891(2) 0.23758(19) 0.06295(9) 0.0306(5) Uani 1 1 d . . . . .
O1 O 0.4972(10) 0.6921(10) 0.500000 0.030(3) Uani 1 2 d S TU P . .
O2 O 0.5134(10) 0.5391(10) 0.500000 0.037(3) Uani 1 2 d S TU P C .
O3 O 0.6704(8) 0.7059(9) 0.4361(4) 0.045(3) Uani 1 1 d D U . . .
O4 O 0.5211(8) 0.5460(9) 0.3781(5) 0.046(3) Uani 1 1 d . U . . .
O5 O 0.5290(8) 0.7414(8) 0.3851(4) 0.040(2) Uani 1 1 d . U . . .
O6 O 0.3665(7) 0.5648(7) 0.4246(4) 0.0303(19) Uani 1 1 d . U . . .
O21 O 0.1614(11) 0.1474(10) 0.000000 0.031(3) Uani 1 2 d S TU P . .
O22 O 0.1627(13) 0.3112(9) 0.000000 0.037(3) Uani 1 2 d S TU P G .
O23 O 0.3254(8) 0.3161(9) 0.0637(3) 0.040(2) Uani 1 1 d D U . . .
O24 O 0.1679(8) 0.3067(7) 0.1228(4) 0.043(3) Uani 1 1 d . U . . .
O25 O 0.0231(7) 0.1327(7) 0.0750(3) 0.0285(19) Uani 1 1 d . U . . .
O26 O 0.1948(9) 0.1330(9) 0.1141(4) 0.038(2) Uani 1 1 d . U . . .
C2 C 0.518(2) 0.441(2) 0.500000 0.061(7) Uani 1 2 d S TU P . .
H2A H 0.526460 0.440539 0.458055 0.073 Uiso 0.5 1 calc R U P A -1
C2A C 0.411(3) 0.352(3) 0.500000 0.086(9) Uani 1 2 d S TU P C .
H2AA H 0.412874 0.287325 0.500000 0.129 Uiso 0.5 1 calc R U P B -1
H2AB H 0.374287 0.354794 0.533872 0.129 Uiso 0.5 1 calc R U P B -1
H2AC H 0.374287 0.354794 0.466128 0.129 Uiso 0.5 1 calc R U P B -1
C2B C 0.628(4) 0.461(4) 0.514(2) 0.092(18) Uani 0.5 1 d . U P C -1
H2BA H 0.678570 0.534826 0.507712 0.138 Uiso 0.5 1 calc R U P C -1
H2BB H 0.630946 0.443080 0.553258 0.138 Uiso 0.5 1 calc R U P C -1
H2BC H 0.644688 0.419052 0.488815 0.138 Uiso 0.5 1 calc R U P C -1
C3 C 0.756(2) 0.759(2) 0.3947(11) 0.059(6) Uiso 0.58(3) 1 d D U P D 1
H3 H 0.733008 0.775503 0.358231 0.071 Uiso 0.58(3) 1 calc R U P D 1
C3A C 0.806(4) 0.697(4) 0.388(2) 0.091(8) Uiso 0.58(3) 1 d D U P D 1
H3AA H 0.863162 0.731387 0.360216 0.137 Uiso 0.58(3) 1 calc R U P D 1
H3AB H 0.834140 0.690961 0.424016 0.137 Uiso 0.58(3) 1 calc R U P D 1
H3AC H 0.756012 0.628160 0.373597 0.137 Uiso 0.58(3) 1 calc R U P D 1
C3B C 0.824(4) 0.853(3) 0.4296(17) 0.091(8) Uiso 0.58(3) 1 d D U P D 1
H3BA H 0.789891 0.894537 0.434510 0.137 Uiso 0.58(3) 1 calc R U P D 1
H3BB H 0.835360 0.831473 0.466771 0.137 Uiso 0.58(3) 1 calc R U P D 1
H3BC H 0.890214 0.894589 0.410347 0.137 Uiso 0.58(3) 1 calc R U P D 1
C3' C 0.779(2) 0.777(3) 0.4358(16) 0.059(6) Uiso 0.42(3) 1 d D U P D 2
H3A' H 0.806709 0.790595 0.475324 0.071 Uiso 0.42(3) 1 calc R U P D 2
C3A' C 0.827(6) 0.730(5) 0.402(3) 0.091(8) Uiso 0.42(3) 1 d D U P D 2
H3AD H 0.902078 0.776642 0.400426 0.137 Uiso 0.42(3) 1 calc R U P D 2
H3AE H 0.812061 0.663989 0.419067 0.137 Uiso 0.42(3) 1 calc R U P D 2
H3AF H 0.798786 0.717193 0.363292 0.137 Uiso 0.42(3) 1 calc R U P D 2
C3B' C 0.801(6) 0.875(4) 0.408(2) 0.091(8) Uiso 0.42(3) 1 d D U P D 2
H3BD H 0.876056 0.923405 0.408716 0.137 Uiso 0.42(3) 1 calc R U P D 2
H3BE H 0.776142 0.861572 0.369321 0.137 Uiso 0.42(3) 1 calc R U P D 2
H3BF H 0.766136 0.905973 0.429217 0.137 Uiso 0.42(3) 1 calc R U P D 2
C11 C 0.4491(14) 0.4725(12) 0.3454(7) 0.047(4) Uani 1 1 d . U . . .
C12 C 0.4762(16) 0.4206(14) 0.3069(6) 0.052(4) Uani 1 1 d . U . . .
H12A H 0.545586 0.434360 0.305182 0.063 Uiso 1 1 calc R U . . .
C13 C 0.4024(17) 0.3485(18) 0.2707(7) 0.065(5) Uani 1 1 d . U . . .
H13A H 0.422966 0.314262 0.244217 0.078 Uiso 1 1 calc R U . . .
C14 C 0.304(2) 0.325(2) 0.2714(9) 0.077(6) Uani 1 1 d . U . . .
H14A H 0.256073 0.276892 0.245123 0.093 Uiso 1 1 calc R U . . .
C15 C 0.2732(16) 0.3718(15) 0.3104(7) 0.056(4) Uani 1 1 d . U . . .
H15A H 0.202232 0.352814 0.312313 0.067 Uiso 1 1 calc R U . . .
C16 C 0.3446(13) 0.4476(12) 0.3478(6) 0.039(3) Uani 1 1 d . U . . .
C17 C 0.5025(12) 0.8095(12) 0.3881(6) 0.036(3) Uani 1 1 d . U . . .
C22 C 0.164(3) 0.409(2) 0.000000 0.065(7) Uani 1 2 d S TU P . .
H22' H 0.178895 0.427042 0.041046 0.078 Uiso 0.5 1 calc R U P E -1
C22A C 0.052(5) 0.374(5) 0.000000 0.15(2) Uani 1 2 d S TU P G .
H22A H 0.014217 0.308517 0.020716 0.218 Uiso 0.5 1 calc R U P F -1
H22B H 0.040184 0.426412 0.018373 0.218 Uiso 0.5 1 calc R U P F -1
H22C H 0.026422 0.363932 -0.039089 0.218 Uiso 0.5 1 calc R U P F -1
C22B C 0.248(5) 0.494(3) -0.0226(17) 0.086(12) Uani 0.5 1 d . U P G -1
H22D H 0.238261 0.554520 -0.019663 0.130 Uiso 0.5 1 calc R U P G -1
H22E H 0.310624 0.508273 -0.001771 0.130 Uiso 0.5 1 calc R U P G -1
H22F H 0.255595 0.481348 -0.062474 0.130 Uiso 0.5 1 calc R U P G -1
C23 C 0.396(2) 0.357(2) 0.1126(12) 0.060(6) Uiso 0.546(19) 1 d D U P H 1
H23A H 0.358620 0.325667 0.148876 0.072 Uiso 0.546(19) 1 calc R U P H 1
C23A C 0.471(4) 0.322(4) 0.099(2) 0.102(8) Uiso 0.546(19) 1 d D U P H 1
H23B H 0.434623 0.245822 0.097867 0.153 Uiso 0.546(19) 1 calc R U P H 1
H23C H 0.502502 0.349269 0.061955 0.153 Uiso 0.546(19) 1 calc R U P H 1
H23D H 0.525093 0.346800 0.127997 0.153 Uiso 0.546(19) 1 calc R U P H 1
C23B C 0.448(4) 0.469(3) 0.114(2) 0.102(8) Uiso 0.546(19) 1 d D U P H 1
H23E H 0.494182 0.494085 0.147318 0.153 Uiso 0.546(19) 1 calc R U P H 1
H23F H 0.488284 0.497432 0.079766 0.153 Uiso 0.546(19) 1 calc R U P H 1
H23G H 0.396195 0.491001 0.117607 0.153 Uiso 0.546(19) 1 calc R U P H 1
C23' C 0.433(2) 0.351(3) 0.0585(15) 0.060(6) Uiso 0.454(19) 1 d D U P H 2
H23H H 0.458782 0.399174 0.025526 0.072 Uiso 0.454(19) 1 calc R U P H 2
C23C C 0.457(5) 0.268(4) 0.046(2) 0.102(8) Uiso 0.454(19) 1 d D U P H 2
H23I H 0.532524 0.298497 0.043312 0.153 Uiso 0.454(19) 1 calc R U P H 2
H23J H 0.430741 0.217034 0.076830 0.153 Uiso 0.454(19) 1 calc R U P H 2
H23K H 0.424796 0.234521 0.010406 0.153 Uiso 0.454(19) 1 calc R U P H 2
C23D C 0.493(5) 0.410(4) 0.108(2) 0.102(8) Uiso 0.454(19) 1 d D U P H 2
H23L H 0.566269 0.431867 0.102417 0.153 Uiso 0.454(19) 1 calc R U P H 2
H23M H 0.485430 0.471142 0.112846 0.153 Uiso 0.454(19) 1 calc R U P H 2
H23N H 0.467317 0.366426 0.141961 0.153 Uiso 0.454(19) 1 calc R U P H 2
C31 C 0.0942(12) 0.3023(11) 0.1561(5) 0.037(3) Uani 1 1 d . U . . .
C32 C 0.1182(16) 0.3782(15) 0.1968(8) 0.059(4) Uani 1 1 d . U . . .
H32A H 0.187486 0.433780 0.199524 0.070 Uiso 1 1 calc R U . . .
C33 C 0.0439(19) 0.3756(17) 0.2338(8) 0.069(5) Uani 1 1 d . U . . .
H33A H 0.061079 0.430075 0.260110 0.083 Uiso 1 1 calc R U . . .
C34 C -0.0598(19) 0.2879(19) 0.2309(9) 0.077(6) Uani 1 1 d . U . . .
H34A H -0.111321 0.281701 0.256823 0.092 Uiso 1 1 calc R U . . .
C35 C -0.0831(16) 0.2132(16) 0.1902(8) 0.058(5) Uani 1 1 d . U . . .
H35A H -0.151988 0.156765 0.187723 0.069 Uiso 1 1 calc R U . . .
C36 C -0.0088(12) 0.2179(12) 0.1526(7) 0.039(3) Uani 1 1 d . U . . .
C37 C 0.1732(12) 0.0413(12) 0.1110(6) 0.032(3) Uani 1 1 d . 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
Dy1 O1 2.277(13) . ?
Dy1 O1 2.277(13) 2_665 ?
Dy1 O1 2.277(13) 3_565 ?
Dy1 O6 2.545(8) . ?
Dy1 O6 2.545(8) 3_565 ?
Dy1 O6 2.545(8) 5_666 ?
Dy1 O6 2.545(8) 6_566 ?
Dy1 O6 2.545(9) 2_665 ?
Dy1 O6 2.545(8) 4_556 ?
Dy1 Ti1 3.557(2) 5_666 ?
Dy1 Ti1 3.557(2) 2_665 ?
Dy1 Ti1 3.557(2) 3_565 ?
Dy2 O21 2.309(13) 3 ?
Dy2 O21 2.309(13) . ?
Dy2 O21 2.309(13) 2 ?
Dy2 O25 2.547(8) 4 ?
Dy2 O25 2.547(8) 5 ?
Dy2 O25 2.547(8) 2 ?
Dy2 O25 2.547(8) . ?
Dy2 O25 2.547(8) 3 ?
Dy2 O25 2.547(8) 6 ?
Dy2 Ti2 3.566(2) . ?
Dy2 Ti2 3.566(2) 5 ?
Dy2 Ti2 3.566(2) 6 ?
Ti1 O3 1.774(11) . ?
Ti1 O4 1.878(11) . ?
Ti1 O1 1.910(8) . ?
Ti1 O2 1.987(9) . ?
Ti1 O5 2.022(10) . ?
Ti1 O6 2.178(10) . ?
Ti1 Ti1 2.971(5) 4_556 ?
Ti2 O23 1.767(11) . ?
Ti2 O24 1.867(10) . ?
Ti2 O21 1.906(9) . ?
Ti2 O22 2.001(10) . ?
Ti2 O26 2.007(11) . ?
Ti2 O25 2.185(10) . ?
Ti2 Ti2 2.974(4) 4 ?
O2 C2 1.49(3) . ?
O3 C3' 1.42(3) . ?
O3 C3 1.48(2) . ?
O4 C11 1.33(2) . ?
O5 C17 1.26(2) . ?
O6 C17 1.284(18) 3_565 ?
O22 C22 1.45(3) . ?
O23 C23' 1.42(3) . ?
O23 C23 1.47(2) . ?
O24 C31 1.326(18) . ?
O25 C37 1.279(17) 2 ?
O26 C37 1.240(16) . ?
C2 C2A 1.48(4) . ?
C2 C2B 1.55(5) . ?
C2 H2A 1.0000 . ?
C2A H2AA 0.9800 . ?
C2A H2AB 0.9800 . ?
C2A H2AC 0.9800 . ?
C2B H2BA 0.9800 . ?
C2B H2BB 0.9800 . ?
C2B H2BC 0.9800 . ?
C3 C3A 1.47(3) . ?
C3 C3B 1.50(3) . ?
C3 H3 1.0000 . ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?
C3A H3AC 0.9800 . ?
C3B H3BA 0.9800 . ?
C3B H3BB 0.9800 . ?
C3B H3BC 0.9800 . ?
C3' C3B' 1.47(3) . ?
C3' C3A' 1.47(3) . ?
C3' H3A' 1.0000 . ?
C3A' H3AD 0.9800 . ?
C3A' H3AE 0.9800 . ?
C3A' H3AF 0.9800 . ?
C3B' H3BD 0.9800 . ?
C3B' H3BE 0.9800 . ?
C3B' H3BF 0.9800 . ?
C11 C12 1.38(2) . ?
C11 C16 1.41(2) . ?
C12 C13 1.38(3) . ?
C12 H12A 0.9500 . ?
C13 C14 1.32(3) . ?
C13 H13A 0.9500 . ?
C14 C15 1.37(3) . ?
C14 H14A 0.9500 . ?
C15 C16 1.41(2) . ?
C15 H15A 0.9500 . ?
C16 C17 1.48(2) 3_565 ?
C22 C22B 1.37(5) . ?
C22 C22A 1.48(7) . ?
C22 H22' 1.0000 . ?
C22A H22A 0.9800 . ?
C22A H22B 0.9800 . ?
C22A H22C 0.9800 . ?
C22B H22D 0.9800 . ?
C22B H22E 0.9800 . ?
C22B H22F 0.9800 . ?
C23 C23B 1.45(3) . ?
C23 C23A 1.49(3) . ?
C23 H23A 1.0000 . ?
C23A H23B 0.9800 . ?
C23A H23C 0.9800 . ?
C23A H23D 0.9800 . ?
C23B H23E 0.9800 . ?
C23B H23F 0.9800 . ?
C23B H23G 0.9800 . ?
C23' C23C 1.47(3) . ?
C23' C23D 1.47(3) . ?
C23' H23H 1.0000 . ?
C23C H23I 0.9800 . ?
C23C H23J 0.9800 . ?
C23C H23K 0.9800 . ?
C23D H23L 0.9800 . ?
C23D H23M 0.9800 . ?
C23D H23N 0.9800 . ?
C31 C32 1.39(2) . ?
C31 C36 1.42(2) . ?
C32 C33 1.40(3) . ?
C32 H32A 0.9500 . ?
C33 C34 1.44(3) . ?
C33 H33A 0.9500 . ?
C34 C35 1.38(3) . ?
C34 H34A 0.9500 . ?
C35 C36 1.39(2) . ?
C35 H35A 0.9500 . ?
C36 C37 1.49(2) 2 ?

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 Dy1 O1 119.999(7) . 2_665 ?
O1 Dy1 O1 120.001(2) . 3_565 ?
O1 Dy1 O1 120.000(2) 2_665 3_565 ?
O1 Dy1 O6 65.6(3) . . ?
O1 Dy1 O6 135.3(2) 2_665 . ?
O1 Dy1 O6 72.7(3) 3_565 . ?
O1 Dy1 O6 135.3(2) . 3_565 ?
O1 Dy1 O6 72.7(3) 2_665 3_565 ?
O1 Dy1 O6 65.6(3) 3_565 3_565 ?
O6 Dy1 O6 76.4(3) . 3_565 ?
O1 Dy1 O6 72.7(3) . 5_666 ?
O1 Dy1 O6 65.6(3) 2_665 5_666 ?
O1 Dy1 O6 135.3(2) 3_565 5_666 ?
O6 Dy1 O6 138.18(15) . 5_666 ?
O6 Dy1 O6 138.18(15) 3_565 5_666 ?
O1 Dy1 O6 135.3(2) . 6_566 ?
O1 Dy1 O6 72.7(3) 2_665 6_566 ?
O1 Dy1 O6 65.6(3) 3_565 6_566 ?
O6 Dy1 O6 138.18(16) . 6_566 ?
O6 Dy1 O6 88.9(4) 3_565 6_566 ?
O6 Dy1 O6 76.4(3) 5_666 6_566 ?
O1 Dy1 O6 72.7(3) . 2_665 ?
O1 Dy1 O6 65.6(3) 2_665 2_665 ?
O1 Dy1 O6 135.3(2) 3_565 2_665 ?
O6 Dy1 O6 76.4(3) . 2_665 ?
O6 Dy1 O6 76.4(3) 3_565 2_665 ?
O6 Dy1 O6 88.9(4) 5_666 2_665 ?
O6 Dy1 O6 138.18(15) 6_566 2_665 ?
O1 Dy1 O6 65.6(3) . 4_556 ?
O1 Dy1 O6 135.3(2) 2_665 4_556 ?
O1 Dy1 O6 72.7(3) 3_565 4_556 ?
O6 Dy1 O6 88.9(4) . 4_556 ?
O6 Dy1 O6 138.18(16) 3_565 4_556 ?
O6 Dy1 O6 76.4(3) 5_666 4_556 ?
O6 Dy1 O6 76.4(3) 6_566 4_556 ?
O6 Dy1 O6 138.18(16) 2_665 4_556 ?
O1 Dy1 Ti1 103.2(3) . 5_666 ?
O1 Dy1 Ti1 28.83(17) 2_665 5_666 ?
O1 Dy1 Ti1 130.3(3) 3_565 5_666 ?
O6 Dy1 Ti1 154.0(2) . 5_666 ?
O6 Dy1 Ti1 100.8(2) 3_565 5_666 ?
O6 Dy1 Ti1 37.4(2) 5_666 5_666 ?
O6 Dy1 Ti1 66.6(2) 6_566 5_666 ?
O6 Dy1 Ti1 77.9(2) 2_665 5_666 ?
O6 Dy1 Ti1 108.3(2) 4_556 5_666 ?
O1 Dy1 Ti1 103.2(3) . 2_665 ?
O1 Dy1 Ti1 28.83(17) 2_665 2_665 ?
O1 Dy1 Ti1 130.3(3) 3_565 2_665 ?
O6 Dy1 Ti1 108.3(2) . 2_665 ?
O6 Dy1 Ti1 66.6(2) 3_565 2_665 ?
O6 Dy1 Ti1 77.9(2) 5_666 2_665 ?
O6 Dy1 Ti1 100.8(2) 6_566 2_665 ?
O6 Dy1 Ti1 37.4(2) 2_665 2_665 ?
O6 Dy1 Ti1 154.0(2) 4_556 2_665 ?
Ti1 Dy1 Ti1 49.36(8) 5_666 2_665 ?
O1 Dy1 Ti1 130.3(3) . 3_565 ?
O1 Dy1 Ti1 103.2(3) 2_665 3_565 ?
O1 Dy1 Ti1 28.83(17) 3_565 3_565 ?
O6 Dy1 Ti1 66.6(2) . 3_565 ?
O6 Dy1 Ti1 37.4(2) 3_565 3_565 ?
O6 Dy1 Ti1 154.0(2) 5_666 3_565 ?
O6 Dy1 Ti1 77.9(2) 6_566 3_565 ?
O6 Dy1 Ti1 108.3(2) 2_665 3_565 ?
O6 Dy1 Ti1 100.8(2) 4_556 3_565 ?
Ti1 Dy1 Ti1 125.958(18) 5_666 3_565 ?
Ti1 Dy1 Ti1 103.79(4) 2_665 3_565 ?
O21 Dy2 O21 120.0 3 . ?
O21 Dy2 O21 120.0 3 2 ?
O21 Dy2 O21 120.0 . 2 ?
O21 Dy2 O25 135.7(2) 3 4 ?
O21 Dy2 O25 65.7(3) . 4 ?
O21 Dy2 O25 72.3(3) 2 4 ?
O21 Dy2 O25 72.3(3) 3 5 ?
O21 Dy2 O25 135.7(2) . 5 ?
O21 Dy2 O25 65.7(3) 2 5 ?
O25 Dy2 O25 77.0(3) 4 5 ?
O21 Dy2 O25 72.3(3) 3 2 ?
O21 Dy2 O25 135.7(2) . 2 ?
O21 Dy2 O25 65.7(3) 2 2 ?
O25 Dy2 O25 137.88(15) 4 2 ?
O25 Dy2 O25 88.1(4) 5 2 ?
O21 Dy2 O25 135.7(2) 3 . ?
O21 Dy2 O25 65.7(3) . . ?
O21 Dy2 O25 72.3(3) 2 . ?
O25 Dy2 O25 88.1(4) 4 . ?
O25 Dy2 O25 137.88(15) 5 . ?
O25 Dy2 O25 77.0(3) 2 . ?
O21 Dy2 O25 65.7(3) 3 3 ?
O21 Dy2 O25 72.3(3) . 3 ?
O21 Dy2 O25 135.7(2) 2 3 ?
O25 Dy2 O25 137.88(15) 4 3 ?
O25 Dy2 O25 137.87(15) 5 3 ?
O25 Dy2 O25 77.0(3) 2 3 ?
O25 Dy2 O25 77.0(3) . 3 ?
O21 Dy2 O25 65.7(3) 3 6 ?
O21 Dy2 O25 72.3(3) . 6 ?
O21 Dy2 O25 135.7(2) 2 6 ?
O25 Dy2 O25 77.0(3) 4 6 ?
O25 Dy2 O25 77.0(3) 5 6 ?
O25 Dy2 O25 137.87(15) 2 6 ?
O25 Dy2 O25 137.88(15) . 6 ?
O25 Dy2 O25 88.1(4) 3 6 ?
O21 Dy2 Ti2 130.5(3) 3 . ?
O21 Dy2 Ti2 28.91(19) . . ?
O21 Dy2 Ti2 103.1(3) 2 . ?
O25 Dy2 Ti2 77.6(2) 4 . ?
O25 Dy2 Ti2 154.4(2) 5 . ?
O25 Dy2 Ti2 108.8(2) 2 . ?
O25 Dy2 Ti2 37.4(2) . . ?
O25 Dy2 Ti2 66.6(2) 3 . ?
O25 Dy2 Ti2 100.5(2) 6 . ?
O21 Dy2 Ti2 103.1(3) 3 5 ?
O21 Dy2 Ti2 130.5(3) . 5 ?
O21 Dy2 Ti2 28.91(19) 2 5 ?
O25 Dy2 Ti2 66.6(2) 4 5 ?
O25 Dy2 Ti2 37.4(2) 5 5 ?
O25 Dy2 Ti2 77.6(2) 2 5 ?
O25 Dy2 Ti2 100.5(2) . 5 ?
O25 Dy2 Ti2 154.4(2) 3 5 ?
O25 Dy2 Ti2 108.8(2) 6 5 ?
Ti2 Dy2 Ti2 125.940(16) . 5 ?
O21 Dy2 Ti2 28.91(19) 3 6 ?
O21 Dy2 Ti2 103.1(3) . 6 ?
O21 Dy2 Ti2 130.5(3) 2 6 ?
O25 Dy2 Ti2 108.8(2) 4 6 ?
O25 Dy2 Ti2 66.6(2) 5 6 ?
O25 Dy2 Ti2 100.5(2) 2 6 ?
O25 Dy2 Ti2 154.4(2) . 6 ?
O25 Dy2 Ti2 77.6(2) 3 6 ?
O25 Dy2 Ti2 37.4(2) 6 6 ?
Ti2 Dy2 Ti2 125.941(16) . 6 ?
Ti2 Dy2 Ti2 103.84(4) 5 6 ?
O3 Ti1 O4 94.6(5) . . ?
O3 Ti1 O1 104.2(5) . . ?
O4 Ti1 O1 160.6(5) . . ?
O3 Ti1 O2 98.4(5) . . ?
O4 Ti1 O2 96.4(5) . . ?
O1 Ti1 O2 76.4(4) . . ?
O3 Ti1 O5 90.5(5) . . ?
O4 Ti1 O5 94.3(5) . . ?
O1 Ti1 O5 90.4(4) . . ?
O2 Ti1 O5 165.6(4) . . ?
O3 Ti1 O6 169.8(4) . . ?
O4 Ti1 O6 82.8(4) . . ?
O1 Ti1 O6 79.5(5) . . ?
O2 Ti1 O6 91.8(5) . . ?
O5 Ti1 O6 79.9(4) . . ?
O3 Ti1 Ti1 90.7(3) . 4_556 ?
O4 Ti1 Ti1 137.9(4) . 4_556 ?
O1 Ti1 Ti1 38.9(3) . 4_556 ?
O2 Ti1 Ti1 41.6(3) . 4_556 ?
O5 Ti1 Ti1 127.4(3) . 4_556 ?
O6 Ti1 Ti1 97.8(2) . 4_556 ?
O3 Ti1 Dy1 136.3(4) . . ?
O4 Ti1 Dy1 128.0(4) . . ?
O1 Ti1 Dy1 35.1(4) . . ?
O2 Ti1 Dy1 87.3(3) . . ?
O5 Ti1 Dy1 78.5(3) . . ?
O6 Ti1 Dy1 45.2(2) . . ?
Ti1 Ti1 Dy1 65.32(4) 4_556 . ?
O23 Ti2 O24 94.8(5) . . ?
O23 Ti2 O21 104.3(5) . . ?
O24 Ti2 O21 160.6(6) . . ?
O23 Ti2 O22 96.9(5) . . ?
O24 Ti2 O22 97.2(5) . . ?
O21 Ti2 O22 77.0(4) . . ?
O23 Ti2 O26 91.5(5) . . ?
O24 Ti2 O26 93.3(5) . . ?
O21 Ti2 O26 90.0(5) . . ?
O22 Ti2 O26 165.9(4) . . ?
O23 Ti2 O25 171.2(4) . . ?
O24 Ti2 O25 81.5(4) . . ?
O21 Ti2 O25 80.1(5) . . ?
O22 Ti2 O25 91.5(5) . . ?
O26 Ti2 O25 80.7(4) . . ?
O23 Ti2 Ti2 90.6(3) . 4 ?
O24 Ti2 Ti2 139.2(3) . 4 ?
O21 Ti2 Ti2 38.7(3) . 4 ?
O22 Ti2 Ti2 42.0(3) . 4 ?
O26 Ti2 Ti2 127.0(3) . 4 ?
O25 Ti2 Ti2 97.5(2) . 4 ?
O23 Ti2 Dy2 137.6(4) . . ?
O24 Ti2 Dy2 126.6(3) . . ?
O21 Ti2 Dy2 35.8(4) . . ?
O22 Ti2 Dy2 87.7(3) . . ?
O26 Ti2 Dy2 78.4(3) . . ?
O25 Ti2 Dy2 45.1(2) . . ?
Ti2 Ti2 Dy2 65.35(3) 4 . ?
Ti1 O1 Ti1 102.1(6) 4_556 . ?
Ti1 O1 Dy1 116.1(5) 4_556 . ?
Ti1 O1 Dy1 116.1(5) . . ?
C2 O2 Ti1 130.3(4) . 4_556 ?
C2 O2 Ti1 130.3(4) . . ?
Ti1 O2 Ti1 96.8(6) 4_556 . ?
C3' O3 Ti1 170(2) . . ?
C3 O3 Ti1 138.8(13) . . ?
C11 O4 Ti1 140.0(10) . . ?
C17 O5 Ti1 137.3(10) . . ?
C17 O6 Ti1 130.2(9) 3_565 . ?
C17 O6 Dy1 132.2(10) 3_565 . ?
Ti1 O6 Dy1 97.4(3) . . ?
Ti2 O21 Ti2 102.6(6) . 4 ?
Ti2 O21 Dy2 115.2(5) . . ?
Ti2 O21 Dy2 115.2(5) 4 . ?
C22 O22 Ti2 130.2(4) . . ?
C22 O22 Ti2 130.2(4) . 4 ?
Ti2 O22 Ti2 96.0(6) . 4 ?
C23' O23 Ti2 162.4(18) . . ?
C23 O23 Ti2 128.9(13) . . ?
C31 O24 Ti2 141.9(9) . . ?
C37 O25 Ti2 132.0(9) 2 . ?
C37 O25 Dy2 130.3(9) 2 . ?
Ti2 O25 Dy2 97.5(3) . . ?
C37 O26 Ti2 137.2(11) . . ?
C2A C2 O2 109(2) . . ?
C2A C2 C2B 137(3) . . ?
O2 C2 C2B 112(2) . . ?
C2A C2 H2A 94.5 . . ?
O2 C2 H2A 94.5 . . ?
C2B C2 H2A 94.5 . . ?
C2 C2A H2AA 109.5 . . ?
C2 C2A H2AB 109.5 . . ?
H2AA C2A H2AB 109.5 . . ?
C2 C2A H2AC 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
C2 C2B H2BA 109.5 . . ?
C2 C2B H2BB 109.5 . . ?
H2BA C2B H2BB 109.5 . . ?
C2 C2B H2BC 109.5 . . ?
H2BA C2B H2BC 109.5 . . ?
H2BB C2B H2BC 109.5 . . ?
C3A C3 O3 108(3) . . ?
C3A C3 C3B 109(2) . . ?
O3 C3 C3B 98(2) . . ?
C3A C3 H3 113.4 . . ?
O3 C3 H3 113.4 . . ?
C3B C3 H3 113.4 . . ?
C3 C3A H3AA 109.5 . . ?
C3 C3A H3AB 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
C3 C3A H3AC 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
C3 C3B H3BA 109.5 . . ?
C3 C3B H3BB 109.5 . . ?
H3BA C3B H3BB 109.5 . . ?
C3 C3B H3BC 109.5 . . ?
H3BA C3B H3BC 109.5 . . ?
H3BB C3B H3BC 109.5 . . ?
O3 C3' C3B' 111(4) . . ?
O3 C3' C3A' 107(4) . . ?
C3B' C3' C3A' 108(2) . . ?
O3 C3' H3A' 110.4 . . ?
C3B' C3' H3A' 110.4 . . ?
C3A' C3' H3A' 110.4 . . ?
C3' C3A' H3AD 109.5 . . ?
C3' C3A' H3AE 109.5 . . ?
H3AD C3A' H3AE 109.5 . . ?
C3' C3A' H3AF 109.5 . . ?
H3AD C3A' H3AF 109.5 . . ?
H3AE C3A' H3AF 109.5 . . ?
C3' C3B' H3BD 109.5 . . ?
C3' C3B' H3BE 109.5 . . ?
H3BD C3B' H3BE 109.5 . . ?
C3' C3B' H3BF 109.5 . . ?
H3BD C3B' H3BF 109.5 . . ?
H3BE C3B' H3BF 109.5 . . ?
O4 C11 C12 120.1(16) . . ?
O4 C11 C16 121.6(14) . . ?
C12 C11 C16 118.3(17) . . ?
C11 C12 C13 120.1(19) . . ?
C11 C12 H12A 120.0 . . ?
C13 C12 H12A 120.0 . . ?
C14 C13 C12 122.7(19) . . ?
C14 C13 H13A 118.6 . . ?
C12 C13 H13A 118.6 . . ?
C13 C14 C15 119(2) . . ?
C13 C14 H14A 120.5 . . ?
C15 C14 H14A 120.5 . . ?
C14 C15 C16 121(2) . . ?
C14 C15 H15A 119.4 . . ?
C16 C15 H15A 119.4 . . ?
C15 C16 C11 118.5(16) . . ?
C15 C16 C17 118.8(15) . 3_565 ?
C11 C16 C17 122.6(14) . 3_565 ?
O5 C17 O6 120.7(15) . 2_665 ?
O5 C17 C16 116.8(13) . 2_665 ?
O6 C17 C16 122.5(14) 2_665 2_665 ?
C22B C22 O22 119(3) . . ?
C22B C22 C22A 133(4) . . ?
O22 C22 C22A 101(3) . . ?
C22B C22 H22' 98.9 . . ?
O22 C22 H22' 98.9 . . ?
C22A C22 H22' 98.9 . . ?
C22 C22A H22A 109.5 . . ?
C22 C22A H22B 109.5 . . ?
H22A C22A H22B 109.5 . . ?
C22 C22A H22C 109.5 . . ?
H22A C22A H22C 109.5 . . ?
H22B C22A H22C 109.5 . . ?
C22 C22B H22D 109.5 . . ?
C22 C22B H22E 109.5 . . ?
H22D C22B H22E 109.5 . . ?
C22 C22B H22F 109.5 . . ?
H22D C22B H22F 109.5 . . ?
H22E C22B H22F 109.5 . . ?
C23B C23 O23 111(3) . . ?
C23B C23 C23A 111(2) . . ?
O23 C23 C23A 101(3) . . ?
C23B C23 H23A 111.3 . . ?
O23 C23 H23A 111.3 . . ?
C23A C23 H23A 111.3 . . ?
C23 C23A H23B 109.5 . . ?
C23 C23A H23C 109.5 . . ?
H23B C23A H23C 109.5 . . ?
C23 C23A H23D 109.5 . . ?
H23B C23A H23D 109.5 . . ?
H23C C23A H23D 109.5 . . ?
C23 C23B H23E 109.5 . . ?
C23 C23B H23F 109.5 . . ?
H23E C23B H23F 109.5 . . ?
C23 C23B H23G 109.5 . . ?
H23E C23B H23G 109.5 . . ?
H23F C23B H23G 109.5 . . ?
O23 C23' C23C 115(4) . . ?
O23 C23' C23D 113(4) . . ?
C23C C23' C23D 109(3) . . ?
O23 C23' H23H 106.6 . . ?
C23C C23' H23H 106.6 . . ?
C23D C23' H23H 106.6 . . ?
C23' C23C H23I 109.5 . . ?
C23' C23C H23J 109.5 . . ?
H23I C23C H23J 109.5 . . ?
C23' C23C H23K 109.5 . . ?
H23I C23C H23K 109.5 . . ?
H23J C23C H23K 109.5 . . ?
C23' C23D H23L 109.5 . . ?
C23' C23D H23M 109.5 . . ?
H23L C23D H23M 109.5 . . ?
C23' C23D H23N 109.5 . . ?
H23L C23D H23N 109.5 . . ?
H23M C23D H23N 109.5 . . ?
O24 C31 C32 120.1(14) . . ?
O24 C31 C36 120.8(12) . . ?
C32 C31 C36 119.1(15) . . ?
C31 C32 C33 122.3(18) . . ?
C31 C32 H32A 118.9 . . ?
C33 C32 H32A 118.9 . . ?
C32 C33 C34 118.1(18) . . ?
C32 C33 H33A 121.0 . . ?
C34 C33 H33A 121.0 . . ?
C35 C34 C33 119.3(19) . . ?
C35 C34 H34A 120.4 . . ?
C33 C34 H34A 120.4 . . ?
C34 C35 C36 122.1(19) . . ?
C34 C35 H35A 119.0 . . ?
C36 C35 H35A 119.0 . . ?
C35 C36 C31 119.2(15) . . ?
C35 C36 C37 118.0(15) . 2 ?
C31 C36 C37 122.8(13) . 2 ?
O26 C37 O25 123.5(14) . 3 ?
O26 C37 C36 115.7(14) . 3 ?
O25 C37 C36 120.8(13) 3 3 ?

_refine_diff_density_max         3.585
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.159

####################################################################### 
# 
# 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_ce_c_sq
_database_code_depnum_ccdc_archive 'CCDC 1504173'
_audit_update_record             
;
2017-02-27 deposited with the CCDC.
2017-03-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C69 H87 Ce O30 Ti6'
_chemical_formula_sum            'C69 H87 Ce O30 Ti6'
_chemical_formula_weight         1823.90

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -1.8482 9.6596 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           174
_space_group_name_H-M_alt        'P -6'
_space_group_name_Hall           'P -6'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'

_cell_length_a                   15.0280(4)
_cell_length_b                   15.0280(4)
_cell_length_c                   23.6224(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4620.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9439
_cell_measurement_theta_min      3.40
_cell_measurement_theta_max      61.1

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_F_000             1862
_exptl_transmission_factor_min   0.778
_exptl_transmission_factor_max   1.000
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    8.505
_shelx_estimated_absorpt_T_min   0.295
_shelx_estimated_absorpt_T_max   0.362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.295
_exptl_absorpt_correction_T_max  0.362
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements (SADABS) 
;
_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         '30W microfocus sealed tube, Quazar optics'
_diffrn_measurement_device_type  'Bruker QUEST D8 CCD'
_diffrn_measurement_method       'Thin slice ω and φ scans'
_diffrn_reflns_number            102688
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         7.773
_diffrn_reflns_theta_max         61.315
_diffrn_reflns_theta_full        61.315
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             4874
_reflns_number_gt                4697
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.989
_reflns_Friedel_fraction_max     0.993
_reflns_Friedel_fraction_full    0.993

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 software package, narrow-frames'
_computing_cell_refinement       'refinement of XYZ centroids > 20sigma(I)'
_computing_data_reduction        
;
 Bruker SAINT software package, narrow frame algorithm
;
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_refine_special_details          
;Refined as a 2-component twin. Residual electron density did not resolve
into anything meaningful - presumably solvent and thus was treated with SQUEEZE.
 The iPr groups have been restrained and modelled isotropically as they are
 floppy., Twin,SQUEEZE
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1386P)²+18.2437P] 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_abs_structure_details 
;
 Flack x determined using 2248 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.515(15)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4874
_refine_ls_number_parameters     331
_refine_ls_number_restraints     136
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0688
_refine_ls_wR_factor_ref         0.1910
_refine_ls_wR_factor_gt          0.1884
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Ce1 Ce 0.666667 0.333333 0.500000 0.0221(6) Uani 1 6 d S T P . .
Ce2 Ce 1.000000 1.000000 1.000000 0.0227(7) Uani 1 6 d S T P . .
Ti1 Ti 0.4662(3) 0.3657(3) 0.56365(14) 0.0313(8) Uani 1 1 d . . . . .
Ti2 Ti 0.8119(3) 0.7605(3) 0.93665(13) 0.0338(8) Uani 1 1 d . . . . .
O1 O 0.4984(13) 0.3108(14) 0.500000 0.030(4) Uani 1 2 d S T P . .
O2 O 0.4846(13) 0.4610(13) 0.500000 0.036(4) Uani 1 2 d S T P C .
O3 O 0.3307(11) 0.2996(12) 0.5658(5) 0.049(4) Uani 1 1 d D . . . .
O4 O 0.4821(11) 0.4561(12) 0.6237(6) 0.050(4) Uani 1 1 d . . . . .
O5 O 0.4714(12) 0.2591(10) 0.6138(6) 0.042(4) Uani 1 1 d . . . . .
O6 O 0.6318(11) 0.4363(10) 0.5748(5) 0.038(3) Uani 1 1 d . . . . .
O21 O 0.8317(18) 0.8483(15) 1.000000 0.037(5) Uani 1 2 d S T P . .
O22 O 0.837(2) 0.6874(14) 1.000000 0.050(5) Uani 1 2 d S T P G .
O23 O 0.6770(13) 0.6810(12) 0.9340(5) 0.049(4) Uani 1 1 d D . . . .
O24 O 0.8332(13) 0.6935(11) 0.8774(6) 0.050(4) Uani 1 1 d . . . . .
O25 O 0.9777(12) 0.8637(11) 0.9252(5) 0.036(3) Uani 1 1 d . . . . .
O26 O 0.8058(13) 0.8662(13) 0.8860(7) 0.045(4) Uani 1 1 d . . . . .
C2 C 0.482(3) 0.561(3) 0.500000 0.070(11) Uani 1 2 d S TU P . .
H2A H 0.470373 0.562063 0.541635 0.084 Uiso 0.5 1 calc R U P A -1
C2A C 0.587(3) 0.643(3) 0.500000 0.080(12) Uani 1 2 d S TU P C .
H2AA H 0.630352 0.617981 0.516574 0.120 Uiso 0.5 1 calc R U P B -1
H2AB H 0.608804 0.665253 0.461031 0.120 Uiso 0.5 1 calc R U P B -1
H2AC H 0.592856 0.700238 0.522395 0.120 Uiso 0.5 1 calc R U P B -1
C2B C 0.378(5) 0.543(5) 0.482(3) 0.10(2) Uani 0.5 1 d . U P C -1
H2BA H 0.325896 0.472308 0.490699 0.146 Uiso 0.5 1 calc R U P C -1
H2BB H 0.363039 0.590606 0.502770 0.146 Uiso 0.5 1 calc R U P C -1
H2BC H 0.378987 0.555621 0.441406 0.146 Uiso 0.5 1 calc R U P C -1
C3 C 0.252(2) 0.261(3) 0.6077(16) 0.057(8) Uiso 0.57(3) 1 d D U P D 1
H3 H 0.285119 0.267579 0.645442 0.068 Uiso 0.57(3) 1 calc R U P D 1
C3A C 0.193(4) 0.311(4) 0.611(3) 0.087(9) Uiso 0.57(3) 1 d D U P D 1
H3AA H 0.141052 0.279697 0.640514 0.130 Uiso 0.57(3) 1 calc R U P D 1
H3AB H 0.238392 0.384241 0.619299 0.130 Uiso 0.57(3) 1 calc R U P D 1
H3AC H 0.158928 0.304604 0.574261 0.130 Uiso 0.57(3) 1 calc R U P D 1
C3B C 0.186(4) 0.154(3) 0.597(2) 0.087(9) Uiso 0.57(3) 1 d D U P D 1
H3BA H 0.130704 0.124946 0.624810 0.130 Uiso 0.57(3) 1 calc R U P D 1
H3BB H 0.155931 0.145270 0.558686 0.130 Uiso 0.57(3) 1 calc R U P D 1
H3BC H 0.225330 0.118258 0.598515 0.130 Uiso 0.57(3) 1 calc R U P D 1
C3' C 0.230(3) 0.216(3) 0.568(2) 0.057(8) Uiso 0.43(3) 1 d D U P D 2
H3A' H 0.215428 0.232788 0.529060 0.068 Uiso 0.43(3) 1 calc R U P D 2
C3A' C 0.166(5) 0.249(5) 0.593(3) 0.087(9) Uiso 0.43(3) 1 d D U P D 2
H3AD H 0.206564 0.322555 0.601463 0.130 Uiso 0.43(3) 1 calc R U P D 2
H3AE H 0.109777 0.236005 0.567450 0.130 Uiso 0.43(3) 1 calc R U P D 2
H3AF H 0.137586 0.210917 0.628602 0.130 Uiso 0.43(3) 1 calc R U P D 2
C3B' C 0.176(5) 0.111(4) 0.555(3) 0.087(9) Uiso 0.43(3) 1 d D U P D 2
H3BD H 0.103490 0.082459 0.563518 0.130 Uiso 0.43(3) 1 calc R U P D 2
H3BE H 0.184456 0.100846 0.514506 0.130 Uiso 0.43(3) 1 calc R U P D 2
H3BF H 0.203841 0.075154 0.577504 0.130 Uiso 0.43(3) 1 calc R U P D 2
C11 C 0.5550(17) 0.5318(17) 0.6558(9) 0.045(5) Uani 1 1 d . U . . .
C12 C 0.529(2) 0.5807(19) 0.6933(10) 0.058(6) Uani 1 1 d . U . . .
H12A H 0.460283 0.566974 0.695362 0.069 Uiso 1 1 calc R U . . .
C13 C 0.601(2) 0.650(3) 0.7286(12) 0.075(8) Uani 1 1 d . U . . .
H13A H 0.578869 0.680717 0.755971 0.089 Uiso 1 1 calc R U . . .
C14 C 0.700(3) 0.679(3) 0.7287(13) 0.078(8) Uani 1 1 d . U . . .
H14A H 0.747014 0.731007 0.753565 0.094 Uiso 1 1 calc R U . . .
C15 C 0.730(2) 0.628(2) 0.6890(11) 0.066(7) Uani 1 1 d . U . . .
H15A H 0.800017 0.644124 0.687515 0.079 Uiso 1 1 calc R U . . .
C16 C 0.6585(17) 0.5556(17) 0.6525(9) 0.043(5) Uani 1 1 d . U . . .
C17 C 0.4935(17) 0.1880(17) 0.6119(10) 0.036(5) Uani 1 1 d . U . . .
C22 C 0.838(4) 0.594(4) 1.000000 0.077(12) Uani 1 2 d S TU P . .
H22' H 0.822866 0.576013 0.959100 0.093 Uiso 0.5 1 calc R U P E -1
C22A C 0.952(6) 0.628(6) 1.000000 0.14(2) Uani 1 2 d S TU P G .
H22A H 0.989815 0.691441 0.977956 0.214 Uiso 0.5 1 calc R U P F -1
H22B H 0.977576 0.640383 1.039003 0.214 Uiso 0.5 1 calc R U P F -1
H22C H 0.961666 0.574013 0.983041 0.214 Uiso 0.5 1 calc R U P F -1
C22B C 0.753(8) 0.514(6) 1.023(3) 0.12(3) Uani 0.5 1 d . U P G -1
H22D H 0.759422 0.452403 1.021758 0.187 Uiso 0.5 1 calc R U P G -1
H22E H 0.746720 0.530122 1.062748 0.187 Uiso 0.5 1 calc R U P G -1
H22F H 0.692292 0.502479 1.002000 0.187 Uiso 0.5 1 calc R U P G -1
C23 C 0.603(3) 0.632(3) 0.8890(18) 0.077(11) Uiso 0.54(3) 1 d D U P H 1
H23A H 0.636923 0.667827 0.852791 0.092 Uiso 0.54(3) 1 calc R U P H 1
C23A C 0.511(4) 0.638(4) 0.896(2) 0.078(8) Uiso 0.54(3) 1 d D U P H 1
H23B H 0.529077 0.710152 0.899847 0.117 Uiso 0.54(3) 1 calc R U P H 1
H23C H 0.467338 0.608714 0.862202 0.117 Uiso 0.54(3) 1 calc R U P H 1
H23D H 0.473893 0.599489 0.929383 0.117 Uiso 0.54(3) 1 calc R U P H 1
C23B C 0.572(4) 0.525(3) 0.883(2) 0.078(8) Uiso 0.54(3) 1 d D U P H 1
H23E H 0.632686 0.517851 0.878392 0.117 Uiso 0.54(3) 1 calc R U P H 1
H23F H 0.534025 0.487787 0.916924 0.117 Uiso 0.54(3) 1 calc R U P H 1
H23G H 0.527469 0.497011 0.849743 0.117 Uiso 0.54(3) 1 calc R U P H 1
C23' C 0.568(3) 0.626(4) 0.940(2) 0.077(11) Uiso 0.46(3) 1 d D U P H 2
H23H H 0.545266 0.587954 0.976856 0.092 Uiso 0.46(3) 1 calc R U P H 2
C23C C 0.561(6) 0.716(4) 0.939(3) 0.078(8) Uiso 0.46(3) 1 d D U P H 2
H23I H 0.488566 0.697650 0.942906 0.117 Uiso 0.46(3) 1 calc R U P H 2
H23J H 0.600392 0.760760 0.970707 0.117 Uiso 0.46(3) 1 calc R U P H 2
H23K H 0.588179 0.752391 0.903311 0.117 Uiso 0.46(3) 1 calc R U P H 2
C23D C 0.515(5) 0.562(4) 0.893(3) 0.078(8) Uiso 0.46(3) 1 d D U P H 2
H23L H 0.519922 0.500009 0.893342 0.117 Uiso 0.46(3) 1 calc R U P H 2
H23M H 0.442121 0.543559 0.894298 0.117 Uiso 0.46(3) 1 calc R U P H 2
H23N H 0.545148 0.600271 0.857465 0.117 Uiso 0.46(3) 1 calc R U P H 2
C31 C 0.910(2) 0.7001(18) 0.8430(10) 0.055(6) Uani 1 1 d . U . . .
C32 C 0.886(2) 0.624(2) 0.8031(10) 0.060(6) Uani 1 1 d . U . . .
H32A H 0.818820 0.566336 0.800460 0.072 Uiso 1 1 calc R U . . .
C33 C 0.963(3) 0.632(3) 0.7670(12) 0.077(8) Uani 1 1 d . U . . .
H33A H 0.945451 0.580443 0.739046 0.092 Uiso 1 1 calc R U . . .
C34 C 1.064(3) 0.711(3) 0.7694(14) 0.084(9) Uani 1 1 d . U . . .
H34A H 1.116657 0.713399 0.745805 0.101 Uiso 1 1 calc R U . . .
C35 C 1.083(2) 0.787(2) 0.8093(10) 0.057(6) Uani 1 1 d . U . . .
H35A H 1.150245 0.845555 0.810319 0.068 Uiso 1 1 calc R U . . .
C36 C 1.0107(16) 0.7841(16) 0.8479(8) 0.037(5) Uani 1 1 d . U . . .
C37 C 0.827(2) 0.959(2) 0.8900(11) 0.043(6) Uani 1 1 d . 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
Ce1 O1 2.378(17) 2_655 ?
Ce1 O1 2.378(17) . ?
Ce1 O1 2.378(17) 3_665 ?
Ce1 O6 2.569(13) 3_665 ?
Ce1 O6 2.569(13) 5_656 ?
Ce1 O6 2.569(13) 6_666 ?
Ce1 O6 2.569(13) 2_655 ?
Ce1 O6 2.569(13) 4_556 ?
Ce1 O6 2.570(13) . ?
Ce1 Ti1 3.611(3) . ?
Ce1 Ti1 3.611(3) 5_656 ?
Ce1 Ti1 3.611(3) 2_655 ?
Ce2 O21 2.41(2) . ?
Ce2 O21 2.41(2) 3_675 ?
Ce2 O21 2.41(2) 2_765 ?
Ce2 O25 2.597(12) 5_767 ?
Ce2 O25 2.597(12) 3_675 ?
Ce2 O25 2.597(12) 6_677 ?
Ce2 O25 2.597(12) 2_765 ?
Ce2 O25 2.597(12) 4_557 ?
Ce2 O25 2.597(12) . ?
Ce2 Ti2 3.607(3) 6_677 ?
Ce2 Ti2 3.607(3) 3_675 ?
Ce2 Ti2 3.607(4) . ?
Ti1 O3 1.765(14) . ?
Ti1 O1 1.890(11) . ?
Ti1 O4 1.896(15) . ?
Ti1 O2 1.998(12) . ?
Ti1 O5 2.026(14) . ?
Ti1 O6 2.178(15) . ?
Ti1 Ti1 3.007(6) 4_556 ?
Ti2 O23 1.765(17) . ?
Ti2 O24 1.844(15) . ?
Ti2 O21 1.917(13) . ?
Ti2 O22 2.004(14) . ?
Ti2 O26 2.027(17) . ?
Ti2 O25 2.196(16) . ?
Ti2 Ti2 2.993(6) 4_557 ?
O2 C2 1.52(4) . ?
O3 C3' 1.40(3) . ?
O3 C3 1.42(3) . ?
O4 C11 1.35(3) . ?
O5 C17 1.27(3) . ?
O6 C17 1.33(3) 3_665 ?
O22 C22 1.40(5) . ?
O23 C23' 1.43(3) . ?
O23 C23 1.44(3) . ?
O24 C31 1.37(3) . ?
O25 C37 1.24(3) 2_765 ?
O26 C37 1.27(3) . ?
C2 C2A 1.44(6) . ?
C2 C2B 1.50(7) . ?
C2 H2A 1.0000 . ?
C2A H2AA 0.9800 . ?
C2A H2AB 0.9800 . ?
C2A H2AC 0.9800 . ?
C2B H2BA 0.9800 . ?
C2B H2BB 0.9800 . ?
C2B H2BC 0.9800 . ?
C3 C3B 1.43(3) . ?
C3 C3A 1.43(3) . ?
C3 H3 1.0000 . ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?
C3A H3AC 0.9800 . ?
C3B H3BA 0.9800 . ?
C3B H3BB 0.9800 . ?
C3B H3BC 0.9800 . ?
C3' C3B' 1.40(3) . ?
C3' C3A' 1.43(3) . ?
C3' H3A' 1.0000 . ?
C3A' H3AD 0.9800 . ?
C3A' H3AE 0.9800 . ?
C3A' H3AF 0.9800 . ?
C3B' H3BD 0.9800 . ?
C3B' H3BE 0.9800 . ?
C3B' H3BF 0.9800 . ?
C11 C12 1.33(3) . ?
C11 C16 1.41(3) . ?
C12 C13 1.35(4) . ?
C12 H12A 0.9500 . ?
C13 C14 1.31(4) . ?
C13 H13A 0.9500 . ?
C14 C15 1.43(4) . ?
C14 H14A 0.9500 . ?
C15 C16 1.39(3) . ?
C15 H15A 0.9500 . ?
C16 C17 1.47(3) 3_665 ?
C22 C22B 1.36(9) . ?
C22 C22A 1.52(8) . ?
C22 H22' 1.0000 . ?
C22A H22A 0.9800 . ?
C22A H22B 0.9800 . ?
C22A H22C 0.9800 . ?
C22B H22D 0.9800 . ?
C22B H22E 0.9800 . ?
C22B H22F 0.9800 . ?
C23 C23A 1.44(3) . ?
C23 C23B 1.44(3) . ?
C23 H23A 1.0000 . ?
C23A H23B 0.9800 . ?
C23A H23C 0.9800 . ?
C23A H23D 0.9800 . ?
C23B H23E 0.9800 . ?
C23B H23F 0.9800 . ?
C23B H23G 0.9800 . ?
C23' C23C 1.42(3) . ?
C23' C23D 1.43(3) . ?
C23' H23H 1.0000 . ?
C23C H23I 0.9800 . ?
C23C H23J 0.9800 . ?
C23C H23K 0.9800 . ?
C23D H23L 0.9800 . ?
C23D H23M 0.9800 . ?
C23D H23N 0.9800 . ?
C31 C32 1.39(3) . ?
C31 C36 1.41(3) . ?
C32 C33 1.39(4) . ?
C32 H32A 0.9500 . ?
C33 C34 1.38(4) . ?
C33 H33A 0.9500 . ?
C34 C35 1.40(4) . ?
C34 H34A 0.9500 . ?
C35 C36 1.40(3) . ?
C35 H35A 0.9500 . ?
C36 C37 1.49(3) 2_765 ?

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 Ce1 O1 119.999(2) 2_655 . ?
O1 Ce1 O1 120.002(3) 2_655 3_665 ?
O1 Ce1 O1 119.999(2) . 3_665 ?
O1 Ce1 O6 73.5(4) 2_655 3_665 ?
O1 Ce1 O6 136.1(3) . 3_665 ?
O1 Ce1 O6 64.1(4) 3_665 3_665 ?
O1 Ce1 O6 64.1(4) 2_655 5_656 ?
O1 Ce1 O6 73.5(4) . 5_656 ?
O1 Ce1 O6 136.1(3) 3_665 5_656 ?
O6 Ce1 O6 137.4(2) 3_665 5_656 ?
O1 Ce1 O6 73.5(4) 2_655 6_666 ?
O1 Ce1 O6 136.1(3) . 6_666 ?
O1 Ce1 O6 64.1(4) 3_665 6_666 ?
O6 Ce1 O6 86.9(6) 3_665 6_666 ?
O6 Ce1 O6 77.9(4) 5_656 6_666 ?
O1 Ce1 O6 64.1(4) 2_655 2_655 ?
O1 Ce1 O6 73.5(4) . 2_655 ?
O1 Ce1 O6 136.1(3) 3_665 2_655 ?
O6 Ce1 O6 77.9(4) 3_665 2_655 ?
O6 Ce1 O6 86.9(6) 5_656 2_655 ?
O6 Ce1 O6 137.4(2) 6_666 2_655 ?
O1 Ce1 O6 136.1(3) 2_655 4_556 ?
O1 Ce1 O6 64.1(4) . 4_556 ?
O1 Ce1 O6 73.5(4) 3_665 4_556 ?
O6 Ce1 O6 137.4(2) 3_665 4_556 ?
O6 Ce1 O6 77.9(4) 5_656 4_556 ?
O6 Ce1 O6 77.9(4) 6_666 4_556 ?
O6 Ce1 O6 137.4(2) 2_655 4_556 ?
O1 Ce1 O6 136.1(3) 2_655 . ?
O1 Ce1 O6 64.1(4) . . ?
O1 Ce1 O6 73.5(4) 3_665 . ?
O6 Ce1 O6 77.9(4) 3_665 . ?
O6 Ce1 O6 137.4(2) 5_656 . ?
O6 Ce1 O6 137.4(2) 6_666 . ?
O6 Ce1 O6 77.9(4) 2_655 . ?
O6 Ce1 O6 86.9(6) 4_556 . ?
O1 Ce1 Ti1 129.5(4) 2_655 . ?
O1 Ce1 Ti1 28.3(2) . . ?
O1 Ce1 Ti1 104.1(4) 3_665 . ?
O6 Ce1 Ti1 109.1(3) 3_665 . ?
O6 Ce1 Ti1 100.9(3) 5_656 . ?
O6 Ce1 Ti1 154.2(3) 6_666 . ?
O6 Ce1 Ti1 67.4(3) 2_655 . ?
O6 Ce1 Ti1 76.7(3) 4_556 . ?
O6 Ce1 Ti1 36.6(3) . . ?
O1 Ce1 Ti1 28.3(2) 2_655 5_656 ?
O1 Ce1 Ti1 104.1(4) . 5_656 ?
O1 Ce1 Ti1 129.6(4) 3_665 5_656 ?
O6 Ce1 Ti1 100.9(3) 3_665 5_656 ?
O6 Ce1 Ti1 36.6(3) 5_656 5_656 ?
O6 Ce1 Ti1 67.4(3) 6_666 5_656 ?
O6 Ce1 Ti1 76.7(3) 2_655 5_656 ?
O6 Ce1 Ti1 109.1(3) 4_556 5_656 ?
O6 Ce1 Ti1 154.2(3) . 5_656 ?
Ti1 Ce1 Ti1 125.92(2) . 5_656 ?
O1 Ce1 Ti1 28.3(2) 2_655 2_655 ?
O1 Ce1 Ti1 104.1(4) . 2_655 ?
O1 Ce1 Ti1 129.6(4) 3_665 2_655 ?
O6 Ce1 Ti1 67.4(3) 3_665 2_655 ?
O6 Ce1 Ti1 76.7(3) 5_656 2_655 ?
O6 Ce1 Ti1 100.9(3) 6_666 2_655 ?
O6 Ce1 Ti1 36.6(3) 2_655 2_655 ?
O6 Ce1 Ti1 154.2(3) 4_556 2_655 ?
O6 Ce1 Ti1 109.1(3) . 2_655 ?
Ti1 Ce1 Ti1 103.88(6) . 2_655 ?
Ti1 Ce1 Ti1 49.22(10) 5_656 2_655 ?
O21 Ce2 O21 120.001(8) . 3_675 ?
O21 Ce2 O21 119.999(11) . 2_765 ?
O21 Ce2 O21 120.000(18) 3_675 2_765 ?
O21 Ce2 O25 137.0(3) . 5_767 ?
O21 Ce2 O25 71.0(5) 3_675 5_767 ?
O21 Ce2 O25 66.0(5) 2_765 5_767 ?
O21 Ce2 O25 71.0(5) . 3_675 ?
O21 Ce2 O25 66.0(5) 3_675 3_675 ?
O21 Ce2 O25 137.0(3) 2_765 3_675 ?
O25 Ce2 O25 137.0(2) 5_767 3_675 ?
O21 Ce2 O25 71.0(5) . 6_677 ?
O21 Ce2 O25 66.0(5) 3_675 6_677 ?
O21 Ce2 O25 137.0(3) 2_765 6_677 ?
O25 Ce2 O25 78.8(4) 5_767 6_677 ?
O25 Ce2 O25 85.8(6) 3_675 6_677 ?
O21 Ce2 O25 137.0(3) . 2_765 ?
O21 Ce2 O25 71.0(5) 3_675 2_765 ?
O21 Ce2 O25 66.0(5) 2_765 2_765 ?
O25 Ce2 O25 85.8(6) 5_767 2_765 ?
O25 Ce2 O25 78.8(4) 3_675 2_765 ?
O25 Ce2 O25 137.0(2) 6_677 2_765 ?
O21 Ce2 O25 66.0(5) . 4_557 ?
O21 Ce2 O25 137.0(3) 3_675 4_557 ?
O21 Ce2 O25 71.0(5) 2_765 4_557 ?
O25 Ce2 O25 78.8(4) 5_767 4_557 ?
O25 Ce2 O25 137.0(2) 3_675 4_557 ?
O25 Ce2 O25 78.8(4) 6_677 4_557 ?
O25 Ce2 O25 137.0(2) 2_765 4_557 ?
O21 Ce2 O25 66.0(5) . . ?
O21 Ce2 O25 137.0(3) 3_675 . ?
O21 Ce2 O25 71.0(5) 2_765 . ?
O25 Ce2 O25 137.0(2) 5_767 . ?
O25 Ce2 O25 78.8(4) 3_675 . ?
O25 Ce2 O25 137.0(2) 6_677 . ?
O25 Ce2 O25 78.8(4) 2_765 . ?
O25 Ce2 O25 85.8(6) 4_557 . ?
O21 Ce2 Ti2 101.9(5) . 6_677 ?
O21 Ce2 Ti2 29.5(3) 3_675 6_677 ?
O21 Ce2 Ti2 131.6(4) 2_765 6_677 ?
O25 Ce2 Ti2 66.9(3) 5_767 6_677 ?
O25 Ce2 Ti2 76.6(3) 3_675 6_677 ?
O25 Ce2 Ti2 37.2(3) 6_677 6_677 ?
O25 Ce2 Ti2 99.9(3) 2_765 6_677 ?
O25 Ce2 Ti2 110.0(3) 4_557 6_677 ?
O25 Ce2 Ti2 155.0(3) . 6_677 ?
O21 Ce2 Ti2 101.9(5) . 3_675 ?
O21 Ce2 Ti2 29.5(3) 3_675 3_675 ?
O21 Ce2 Ti2 131.6(4) 2_765 3_675 ?
O25 Ce2 Ti2 99.9(3) 5_767 3_675 ?
O25 Ce2 Ti2 37.2(3) 3_675 3_675 ?
O25 Ce2 Ti2 76.6(3) 6_677 3_675 ?
O25 Ce2 Ti2 66.9(3) 2_765 3_675 ?
O25 Ce2 Ti2 155.0(3) 4_557 3_675 ?
O25 Ce2 Ti2 110.0(3) . 3_675 ?
Ti2 Ce2 Ti2 49.02(10) 6_677 3_675 ?
O21 Ce2 Ti2 29.5(3) . . ?
O21 Ce2 Ti2 131.6(4) 3_675 . ?
O21 Ce2 Ti2 101.9(5) 2_765 . ?
O25 Ce2 Ti2 155.0(3) 5_767 . ?
O25 Ce2 Ti2 66.9(3) 3_675 . ?
O25 Ce2 Ti2 99.9(3) 6_677 . ?
O25 Ce2 Ti2 110.0(3) 2_765 . ?
O25 Ce2 Ti2 76.6(3) 4_557 . ?
O25 Ce2 Ti2 37.2(3) . . ?
Ti2 Ce2 Ti2 125.88(2) 6_677 . ?
Ti2 Ce2 Ti2 103.99(6) 3_675 . ?
O3 Ti1 O1 104.6(7) . . ?
O3 Ti1 O4 94.5(7) . . ?
O1 Ti1 O4 160.1(7) . . ?
O3 Ti1 O2 97.6(7) . . ?
O1 Ti1 O2 75.0(6) . . ?
O4 Ti1 O2 97.3(7) . . ?
O3 Ti1 O5 91.6(7) . . ?
O1 Ti1 O5 90.0(6) . . ?
O4 Ti1 O5 95.1(6) . . ?
O2 Ti1 O5 163.9(6) . . ?
O3 Ti1 O6 170.5(6) . . ?
O1 Ti1 O6 80.2(6) . . ?
O4 Ti1 O6 81.7(6) . . ?
O2 Ti1 O6 91.5(6) . . ?
O5 Ti1 O6 80.1(6) . . ?
O3 Ti1 Ti1 91.7(4) . 4_556 ?
O1 Ti1 Ti1 37.3(4) . 4_556 ?
O4 Ti1 Ti1 138.5(5) . 4_556 ?
O2 Ti1 Ti1 41.2(4) . 4_556 ?
O5 Ti1 Ti1 125.8(4) . 4_556 ?
O6 Ti1 Ti1 96.9(3) . 4_556 ?
O3 Ti1 Ce1 137.9(5) . . ?
O1 Ti1 Ce1 36.6(5) . . ?
O4 Ti1 Ce1 126.4(5) . . ?
O2 Ti1 Ce1 87.6(5) . . ?
O5 Ti1 Ce1 76.8(4) . . ?
O6 Ti1 Ce1 44.7(4) . . ?
Ti1 Ti1 Ce1 65.39(5) 4_556 . ?
O23 Ti2 O24 93.3(7) . . ?
O23 Ti2 O21 102.9(8) . . ?
O24 Ti2 O21 163.5(9) . . ?
O23 Ti2 O22 97.2(9) . . ?
O24 Ti2 O22 97.7(7) . . ?
O21 Ti2 O22 77.8(6) . . ?
O23 Ti2 O26 91.3(7) . . ?
O24 Ti2 O26 93.9(7) . . ?
O21 Ti2 O26 88.5(7) . . ?
O22 Ti2 O26 165.2(7) . . ?
O23 Ti2 O25 170.7(5) . . ?
O24 Ti2 O25 81.2(6) . . ?
O21 Ti2 O25 83.1(8) . . ?
O22 Ti2 O25 91.1(9) . . ?
O26 Ti2 O25 81.6(6) . . ?
O23 Ti2 Ti2 92.0(4) . 4_557 ?
O24 Ti2 Ti2 139.4(5) . 4_557 ?
O21 Ti2 Ti2 38.7(5) . 4_557 ?
O22 Ti2 Ti2 41.7(4) . 4_557 ?
O26 Ti2 Ti2 126.2(5) . 4_557 ?
O25 Ti2 Ti2 97.1(3) . 4_557 ?
O23 Ti2 Ce2 138.7(5) . . ?
O24 Ti2 Ce2 126.6(5) . . ?
O21 Ti2 Ce2 38.3(6) . . ?
O22 Ti2 Ce2 88.2(6) . . ?
O26 Ti2 Ce2 77.5(5) . . ?
O25 Ti2 Ce2 45.6(3) . . ?
Ti2 Ti2 Ce2 65.49(5) 4_557 . ?
Ti1 O1 Ti1 105.4(9) 4_556 . ?
Ti1 O1 Ce1 115.1(6) 4_556 . ?
Ti1 O1 Ce1 115.1(6) . . ?
C2 O2 Ti1 130.1(5) . 4_556 ?
C2 O2 Ti1 130.1(5) . . ?
Ti1 O2 Ti1 97.6(8) 4_556 . ?
C3' O3 Ti1 158(3) . . ?
C3 O3 Ti1 137.6(18) . . ?
C11 O4 Ti1 141.5(13) . . ?
C17 O5 Ti1 140.9(16) . . ?
C17 O6 Ti1 130.5(13) 3_665 . ?
C17 O6 Ce1 130.7(13) 3_665 . ?
Ti1 O6 Ce1 98.7(5) . . ?
Ti2 O21 Ti2 102.6(9) 4_557 . ?
Ti2 O21 Ce2 112.2(8) 4_557 . ?
Ti2 O21 Ce2 112.2(8) . . ?
C22 O22 Ti2 130.2(6) . 4_557 ?
C22 O22 Ti2 130.2(6) . . ?
Ti2 O22 Ti2 96.6(9) 4_557 . ?
C23' O23 Ti2 171(2) . . ?
C23 O23 Ti2 134(2) . . ?
C31 O24 Ti2 141.1(14) . . ?
C37 O25 Ti2 133.5(16) 2_765 . ?
C37 O25 Ce2 128.5(16) 2_765 . ?
Ti2 O25 Ce2 97.3(4) . . ?
C37 O26 Ti2 137.0(19) . . ?
C2A C2 C2B 138(4) . . ?
C2A C2 O2 106(3) . . ?
C2B C2 O2 111(3) . . ?
C2A C2 H2A 96.2 . . ?
C2B C2 H2A 96.2 . . ?
O2 C2 H2A 96.2 . . ?
C2 C2A H2AA 109.5 . . ?
C2 C2A H2AB 109.5 . . ?
H2AA C2A H2AB 109.5 . . ?
C2 C2A H2AC 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
C2 C2B H2BA 109.5 . . ?
C2 C2B H2BB 109.5 . . ?
H2BA C2B H2BB 109.5 . . ?
C2 C2B H2BC 109.5 . . ?
H2BA C2B H2BC 109.5 . . ?
H2BB C2B H2BC 109.5 . . ?
O3 C3 C3B 108(3) . . ?
O3 C3 C3A 115(4) . . ?
C3B C3 C3A 110(3) . . ?
O3 C3 H3 108.1 . . ?
C3B C3 H3 108.1 . . ?
C3A C3 H3 108.1 . . ?
C3 C3A H3AA 109.5 . . ?
C3 C3A H3AB 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
C3 C3A H3AC 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
C3 C3B H3BA 109.5 . . ?
C3 C3B H3BB 109.5 . . ?
H3BA C3B H3BB 109.5 . . ?
C3 C3B H3BC 109.5 . . ?
H3BA C3B H3BC 109.5 . . ?
H3BB C3B H3BC 109.5 . . ?
C3B' C3' O3 140(4) . . ?
C3B' C3' C3A' 112(3) . . ?
O3 C3' C3A' 108(4) . . ?
C3B' C3' H3A' 91.1 . . ?
O3 C3' H3A' 91.1 . . ?
C3A' C3' H3A' 91.1 . . ?
C3' C3A' H3AD 109.5 . . ?
C3' C3A' H3AE 109.5 . . ?
H3AD C3A' H3AE 109.5 . . ?
C3' C3A' H3AF 109.5 . . ?
H3AD C3A' H3AF 109.5 . . ?
H3AE C3A' H3AF 109.5 . . ?
C3' C3B' H3BD 109.5 . . ?
C3' C3B' H3BE 109.5 . . ?
H3BD C3B' H3BE 109.5 . . ?
C3' C3B' H3BF 109.5 . . ?
H3BD C3B' H3BF 109.5 . . ?
H3BE C3B' H3BF 109.5 . . ?
C12 C11 O4 120(2) . . ?
C12 C11 C16 119(2) . . ?
O4 C11 C16 121(2) . . ?
C11 C12 C13 120(3) . . ?
C11 C12 H12A 120.2 . . ?
C13 C12 H12A 120.2 . . ?
C14 C13 C12 127(3) . . ?
C14 C13 H13A 116.7 . . ?
C12 C13 H13A 116.7 . . ?
C13 C14 C15 116(3) . . ?
C13 C14 H14A 122.2 . . ?
C15 C14 H14A 122.2 . . ?
C16 C15 C14 120(3) . . ?
C16 C15 H15A 120.1 . . ?
C14 C15 H15A 120.1 . . ?
C15 C16 C11 119(2) . . ?
C15 C16 C17 118(2) . 3_665 ?
C11 C16 C17 123(2) . 3_665 ?
O5 C17 O6 119(2) . 2_655 ?
O5 C17 C16 119(2) . 2_655 ?
O6 C17 C16 122.3(19) 2_655 2_655 ?
C22B C22 O22 114(6) . . ?
C22B C22 C22A 134(6) . . ?
O22 C22 C22A 104(4) . . ?
C22B C22 H22' 99.2 . . ?
O22 C22 H22' 99.2 . . ?
C22A C22 H22' 99.2 . . ?
C22 C22A H22A 109.5 . . ?
C22 C22A H22B 109.5 . . ?
H22A C22A H22B 109.5 . . ?
C22 C22A H22C 109.5 . . ?
H22A C22A H22C 109.5 . . ?
H22B C22A H22C 109.5 . . ?
C22 C22B H22D 109.5 . . ?
C22 C22B H22E 109.5 . . ?
H22D C22B H22E 109.5 . . ?
C22 C22B H22F 109.5 . . ?
H22D C22B H22F 109.5 . . ?
H22E C22B H22F 109.5 . . ?
C23A C23 C23B 107(3) . . ?
C23A C23 O23 114(4) . . ?
C23B C23 O23 112(4) . . ?
C23A C23 H23A 107.9 . . ?
C23B C23 H23A 107.9 . . ?
O23 C23 H23A 107.9 . . ?
C23 C23A H23B 109.5 . . ?
C23 C23A H23C 109.5 . . ?
H23B C23A H23C 109.5 . . ?
C23 C23A H23D 109.5 . . ?
H23B C23A H23D 109.5 . . ?
H23C C23A H23D 109.5 . . ?
C23 C23B H23E 109.5 . . ?
C23 C23B H23F 109.5 . . ?
H23E C23B H23F 109.5 . . ?
C23 C23B H23G 109.5 . . ?
H23E C23B H23G 109.5 . . ?
H23F C23B H23G 109.5 . . ?
C23C C23' O23 93(4) . . ?
C23C C23' C23D 110(3) . . ?
O23 C23' C23D 114(5) . . ?
C23C C23' H23H 112.7 . . ?
O23 C23' H23H 112.7 . . ?
C23D C23' H23H 112.7 . . ?
C23' C23C H23I 109.5 . . ?
C23' C23C H23J 109.5 . . ?
H23I C23C H23J 109.5 . . ?
C23' C23C H23K 109.5 . . ?
H23I C23C H23K 109.5 . . ?
H23J C23C H23K 109.5 . . ?
C23' C23D H23L 109.5 . . ?
C23' C23D H23M 109.5 . . ?
H23L C23D H23M 109.5 . . ?
C23' C23D H23N 109.5 . . ?
H23L C23D H23N 109.5 . . ?
H23M C23D H23N 109.5 . . ?
O24 C31 C32 119(2) . . ?
O24 C31 C36 120(2) . . ?
C32 C31 C36 121(2) . . ?
C33 C32 C31 119(3) . . ?
C33 C32 H32A 120.5 . . ?
C31 C32 H32A 120.5 . . ?
C34 C33 C32 124(3) . . ?
C34 C33 H33A 118.0 . . ?
C32 C33 H33A 118.0 . . ?
C33 C34 C35 115(3) . . ?
C33 C34 H34A 122.7 . . ?
C35 C34 H34A 122.7 . . ?
C34 C35 C36 125(3) . . ?
C34 C35 H35A 117.4 . . ?
C36 C35 H35A 117.4 . . ?
C35 C36 C31 116(2) . . ?
C35 C36 C37 120(2) . 2_765 ?
C31 C36 C37 123(2) . 2_765 ?
O25 C37 O26 126(3) 3_675 . ?
O25 C37 C36 120(2) 3_675 3_675 ?
O26 C37 C36 114(2) . 3_675 ?

_refine_diff_density_max         2.590
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.087






####################################################################### 
# 
# 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_tb_b
_database_code_depnum_ccdc_archive 'CCDC 1504169'
_audit_update_record             
;
2017-02-27 deposited with the CCDC.
2017-03-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT094_tb_b                
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....      10.56 Report
RESPONSE: There is a large amount of residual electron density that did not resolve into anything meaningful. It is presumably disordered solvent, as the NMR and elemental analysis of the complex is in excellent agreement with the crystallographic formula.
;
# Added during the CSD deposition process: Monday 27 February 2017 10:24 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C69 H87 O30 Tb Ti6'
_chemical_formula_sum            'C69 H87 O30 Tb Ti6'
_chemical_formula_weight         1842.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -9.1472 9.1891 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           174
_space_group_name_H-M_alt        'P -6'
_space_group_name_Hall           'P -6'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'

_cell_length_a                   14.9365(3)
_cell_length_b                   14.9365(3)
_cell_length_c                   23.6008(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4559.9(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9908
_cell_measurement_theta_min      3.416
_cell_measurement_theta_max      66.6

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_F_000             1876
_exptl_transmission_factor_min   0.636
_exptl_transmission_factor_max   1.000
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    8.574
_shelx_estimated_absorpt_T_min   0.190
_shelx_estimated_absorpt_T_max   0.293
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.190
_exptl_absorpt_correction_T_max  0.293
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements (SADABS) 
;

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         '30W microfocus sealed tube, Quazar optics'
_diffrn_measurement_device_type  'Bruker QUEST D8 CCD'
_diffrn_measurement_method       'Thin slice ω and φ scans'
_diffrn_reflns_number            39344
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_av_R_equivalents  0.0553
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.417
_diffrn_reflns_theta_max         66.641
_diffrn_reflns_theta_full        66.641
_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             5531
_reflns_number_gt                5296
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.989
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

_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 software package, narrow-frames'

_computing_cell_refinement       'refinement of XYZ centroids > 20sigma(I)'

_computing_data_reduction        
;
 
Bruker SAINT software package, narrow frame algorithm

;


_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_refine_special_details          
;Refined as a 2-component twin. Residual electron density did not resolve 
into anything meaningful and is presumably disordered solvent. iPr ligands
were modelled using restraints and by keeping them isotropic., Twin
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1458P)²+8.4982P] 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_abs_structure_details 
;
 Flack x determined using 2507 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.152(6)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5531
_refine_ls_number_parameters     331
_refine_ls_number_restraints     212
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0684
_refine_ls_wR_factor_ref         0.1949
_refine_ls_wR_factor_gt          0.1920
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.095
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Tb1 Tb 0.666667 0.333333 0.500000 0.0208(6) Uani 1 6 d S T P . .
Tb2 Tb 1.000000 1.000000 1.000000 0.0202(5) Uani 1 6 d S T P . .
Ti1 Ti 0.4673(2) 0.3650(2) 0.56302(12) 0.0297(7) Uani 1 1 d . . . . .
Ti2 Ti 0.8108(2) 0.7624(2) 0.93696(11) 0.0284(6) Uani 1 1 d . . . . .
O1 O 0.5039(12) 0.3089(12) 0.500000 0.028(3) Uani 1 2 d S TU P . .
O2 O 0.4880(12) 0.4623(12) 0.500000 0.035(4) Uani 1 2 d S TU P C .
O3 O 0.3300(9) 0.2956(10) 0.5642(5) 0.042(3) Uani 1 1 d D U . . .
O4 O 0.4819(10) 0.4545(11) 0.6221(5) 0.043(3) Uani 1 1 d . U . . .
O5 O 0.4704(10) 0.2598(9) 0.6146(5) 0.039(3) Uani 1 1 d . U . . .
O6 O 0.6328(9) 0.4354(8) 0.5749(5) 0.030(2) Uani 1 1 d . U . . .
O21 O 0.8371(13) 0.8514(13) 1.000000 0.032(4) Uani 1 2 d S TU P . .
O22 O 0.8340(14) 0.6881(11) 1.000000 0.034(3) Uani 1 2 d S TU P G .
O23 O 0.6748(10) 0.6844(10) 0.9364(4) 0.041(3) Uani 1 1 d D U . . .
O24 O 0.8308(10) 0.6927(9) 0.8769(5) 0.041(3) Uani 1 1 d . U . . .
O25 O 0.9780(9) 0.8685(9) 0.9252(4) 0.028(2) Uani 1 1 d . U . . .
O26 O 0.8069(11) 0.8693(10) 0.8855(5) 0.038(3) Uani 1 1 d . U . . .
C2 C 0.485(2) 0.560(2) 0.500000 0.051(7) Uani 1 2 d S TU P . .
H2A H 0.478414 0.560671 0.542173 0.061 Uiso 0.5 1 calc R U P A -1
C2A C 0.588(3) 0.650(3) 0.500000 0.081(11) Uani 1 2 d S TU P C .
H2AA H 0.582815 0.713157 0.500000 0.121 Uiso 0.5 1 calc R U P B -1
H2AB H 0.625064 0.649012 0.533904 0.121 Uiso 0.5 1 calc R U P B -1
H2AC H 0.625064 0.649011 0.466096 0.121 Uiso 0.5 1 calc R U P B -1
C2B C 0.362(5) 0.533(4) 0.489(4) 0.09(2) Uani 0.5 1 d . U P C -1
H2BA H 0.314954 0.458966 0.493860 0.132 Uiso 0.5 1 calc R U P C -1
H2BB H 0.344626 0.571020 0.517266 0.132 Uiso 0.5 1 calc R U P C -1
H2BC H 0.355406 0.554653 0.451134 0.132 Uiso 0.5 1 calc R U P C -1
C3 C 0.250(2) 0.251(2) 0.6072(14) 0.055(7) Uiso 0.52(2) 1 d D U P D 1
H3 H 0.284046 0.256034 0.644597 0.066 Uiso 0.52(2) 1 calc R U P D 1
C3A C 0.193(3) 0.304(4) 0.611(2) 0.074(8) Uiso 0.52(2) 1 d D U P D 1
H3AA H 0.240478 0.376848 0.619668 0.111 Uiso 0.52(2) 1 calc R U P D 1
H3AB H 0.158881 0.298351 0.574627 0.111 Uiso 0.52(2) 1 calc R U P D 1
H3AC H 0.141249 0.272740 0.640896 0.111 Uiso 0.52(2) 1 calc R U P D 1
C3B C 0.183(3) 0.144(2) 0.594(2) 0.074(8) Uiso 0.52(2) 1 d D U P D 1
H3BA H 0.224040 0.109004 0.592000 0.111 Uiso 0.52(2) 1 calc R U P D 1
H3BB H 0.131394 0.112053 0.624298 0.111 Uiso 0.52(2) 1 calc R U P D 1
H3BC H 0.149026 0.137663 0.558029 0.111 Uiso 0.52(2) 1 calc R U P D 1
C3' C 0.224(2) 0.220(2) 0.5592(17) 0.055(7) Uiso 0.48(2) 1 d D U P D 2
H3A' H 0.206782 0.229851 0.519658 0.066 Uiso 0.48(2) 1 calc R U P D 2
C3A' C 0.162(3) 0.245(4) 0.593(2) 0.074(8) Uiso 0.48(2) 1 d D U P D 2
H3AD H 0.185985 0.319539 0.589927 0.111 Uiso 0.48(2) 1 calc R U P D 2
H3AE H 0.089711 0.205806 0.580429 0.111 Uiso 0.48(2) 1 calc R U P D 2
H3AF H 0.165969 0.228517 0.632924 0.111 Uiso 0.48(2) 1 calc R U P D 2
C3B' C 0.197(3) 0.117(2) 0.561(2) 0.074(8) Uiso 0.48(2) 1 d D U P D 2
H3BD H 0.122184 0.074097 0.556623 0.111 Uiso 0.48(2) 1 calc R U P D 2
H3BE H 0.231355 0.102818 0.529241 0.111 Uiso 0.48(2) 1 calc R U P D 2
H3BF H 0.219188 0.101997 0.596638 0.111 Uiso 0.48(2) 1 calc R U P D 2
C11 C 0.5536(16) 0.5290(14) 0.6539(8) 0.043(4) Uani 1 1 d . U . . .
C12 C 0.5271(19) 0.5806(16) 0.6938(8) 0.052(5) Uani 1 1 d . U . . .
H12A H 0.458022 0.567218 0.696595 0.062 Uiso 1 1 calc R U . . .
C13 C 0.601(2) 0.650(2) 0.7284(10) 0.072(7) Uani 1 1 d . U . . .
H13A H 0.579738 0.680692 0.756478 0.087 Uiso 1 1 calc R U . . .
C14 C 0.698(2) 0.679(2) 0.7277(10) 0.067(6) Uani 1 1 d . U . . .
H14A H 0.745816 0.731910 0.751937 0.080 Uiso 1 1 calc R U . . .
C15 C 0.729(2) 0.6290(19) 0.6898(9) 0.060(6) Uani 1 1 d . U . . .
H15A H 0.799666 0.646090 0.688848 0.071 Uiso 1 1 calc R U . . .
C16 C 0.6563(15) 0.5519(15) 0.6522(7) 0.039(4) Uani 1 1 d . U . . .
C17 C 0.4981(15) 0.1922(16) 0.6122(8) 0.040(4) Uani 1 1 d . U . . .
C22 C 0.838(3) 0.594(3) 1.000000 0.066(9) Uani 1 2 d S TU P . .
H22' H 0.825303 0.577390 0.958676 0.080 Uiso 0.5 1 calc R U P E -1
C22A C 0.956(6) 0.642(7) 1.000000 0.16(3) Uani 1 2 d S TU P G .
H22A H 0.987676 0.706617 0.978503 0.243 Uiso 0.5 1 calc R U P F -1
H22B H 0.981703 0.655779 1.039084 0.243 Uiso 0.5 1 calc R U P F -1
H22C H 0.974401 0.593635 0.982413 0.243 Uiso 0.5 1 calc R U P F -1
C22B C 0.749(6) 0.507(3) 1.0210(18) 0.080(14) Uani 0.5 1 d . U P G -1
H22D H 0.758728 0.446522 1.019421 0.120 Uiso 0.5 1 calc R U P G -1
H22E H 0.737676 0.519377 1.060411 0.120 Uiso 0.5 1 calc R U P G -1
H22F H 0.689263 0.493744 0.998016 0.120 Uiso 0.5 1 calc R U P G -1
C23 C 0.604(3) 0.642(3) 0.8889(16) 0.066(9) Uiso 0.49(2) 1 d D U P H 1
H23A H 0.641433 0.674643 0.853003 0.079 Uiso 0.49(2) 1 calc R U P H 1
C23A C 0.518(4) 0.660(4) 0.896(2) 0.075(7) Uiso 0.49(2) 1 d D U P H 1
H23B H 0.471064 0.630756 0.863407 0.113 Uiso 0.49(2) 1 calc R U P H 1
H23C H 0.480970 0.627434 0.930795 0.113 Uiso 0.49(2) 1 calc R U P H 1
H23D H 0.544376 0.734719 0.897597 0.113 Uiso 0.49(2) 1 calc R U P H 1
C23B C 0.560(4) 0.530(3) 0.885(2) 0.075(7) Uiso 0.49(2) 1 d D U P H 1
H23E H 0.616126 0.514540 0.880319 0.113 Uiso 0.49(2) 1 calc R U P H 1
H23F H 0.521605 0.497530 0.919659 0.113 Uiso 0.49(2) 1 calc R U P H 1
H23G H 0.513660 0.503876 0.852306 0.113 Uiso 0.49(2) 1 calc R U P H 1
C23' C 0.567(2) 0.632(3) 0.9399(17) 0.066(9) Uiso 0.51(2) 1 d D U P H 2
H23H H 0.542572 0.593757 0.976609 0.079 Uiso 0.51(2) 1 calc R U P H 2
C23C C 0.552(5) 0.717(4) 0.939(2) 0.075(7) Uiso 0.51(2) 1 d D U P H 2
H23I H 0.478426 0.693972 0.940746 0.113 Uiso 0.51(2) 1 calc R U P H 2
H23J H 0.588127 0.762734 0.970834 0.113 Uiso 0.51(2) 1 calc R U P H 2
H23K H 0.580691 0.755724 0.903181 0.113 Uiso 0.51(2) 1 calc R U P H 2
C23D C 0.518(4) 0.565(4) 0.893(2) 0.075(7) Uiso 0.51(2) 1 d D U P H 2
H23L H 0.443171 0.529760 0.897373 0.113 Uiso 0.51(2) 1 calc R U P H 2
H23M H 0.538348 0.604989 0.857741 0.113 Uiso 0.51(2) 1 calc R U P H 2
H23N H 0.540416 0.512866 0.891218 0.113 Uiso 0.51(2) 1 calc R U P H 2
C31 C 0.9046(15) 0.6987(13) 0.8435(7) 0.039(4) Uani 1 1 d . U . . .
C32 C 0.8807(18) 0.6213(19) 0.8038(9) 0.057(5) Uani 1 1 d . U . . .
H32A H 0.812691 0.563305 0.802619 0.069 Uiso 1 1 calc R U . . .
C33 C 0.955(2) 0.627(2) 0.7655(10) 0.068(6) Uani 1 1 d . U . . .
H33A H 0.936374 0.575166 0.737480 0.081 Uiso 1 1 calc R U . . .
C34 C 1.061(2) 0.713(2) 0.7688(12) 0.081(8) Uani 1 1 d . U . . .
H34A H 1.112816 0.718754 0.743547 0.097 Uiso 1 1 calc R U . . .
C35 C 1.0823(19) 0.7862(18) 0.8099(9) 0.055(5) Uani 1 1 d . U . . .
H35A H 1.150988 0.842570 0.813051 0.066 Uiso 1 1 calc R U . . .
C36 C 1.0081(15) 0.7813(14) 0.8472(8) 0.038(4) Uani 1 1 d . U . . .
C37 C 0.8261(14) 0.9603(14) 0.8887(7) 0.030(4) Uani 1 1 d . 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
Tb1 O1 2.270(15) 2_655 ?
Tb1 O1 2.270(15) 3_665 ?
Tb1 O1 2.270(15) . ?
Tb1 O6 2.545(11) . ?
Tb1 O6 2.545(11) 3_665 ?
Tb1 O6 2.545(11) 5_656 ?
Tb1 O6 2.545(11) 6_666 ?
Tb1 O6 2.545(11) 2_655 ?
Tb1 O6 2.545(11) 4_556 ?
Tb1 Ti1 3.565(3) 4_556 ?
Tb1 Ti1 3.565(3) 3_665 ?
Tb1 Ti1 3.565(3) 6_666 ?
Tb2 O21 2.334(16) 3_675 ?
Tb2 O21 2.334(16) 2_765 ?
Tb2 O21 2.334(17) . ?
Tb2 O25 2.536(10) 5_767 ?
Tb2 O25 2.536(10) 3_675 ?
Tb2 O25 2.536(10) 6_677 ?
Tb2 O25 2.536(10) 4_557 ?
Tb2 O25 2.536(10) 2_765 ?
Tb2 O25 2.536(10) . ?
Tb2 Ti2 3.573(3) 5_767 ?
Tb2 Ti2 3.573(3) 2_765 ?
Tb2 Ti2 3.573(3) 4_557 ?
Ti1 O3 1.776(13) . ?
Ti1 O4 1.867(13) . ?
Ti1 O1 1.917(9) . ?
Ti1 O2 1.993(11) . ?
Ti1 O5 2.006(12) . ?
Ti1 O6 2.167(12) . ?
Ti1 Ti1 2.975(6) 4_556 ?
Ti2 O23 1.765(14) . ?
Ti2 O24 1.869(11) . ?
Ti2 O21 1.901(11) . ?
Ti2 O22 1.988(11) . ?
Ti2 O26 2.029(13) . ?
Ti2 O25 2.207(12) . ?
Ti2 Ti2 2.976(5) 4_557 ?
O2 C2 1.49(3) . ?
O3 C3' 1.41(3) . ?
O3 C3 1.45(3) . ?
O4 C11 1.33(2) . ?
O5 C17 1.27(2) . ?
O6 C17 1.30(2) 3_665 ?
O22 C22 1.44(5) . ?
O23 C23' 1.40(3) . ?
O23 C23 1.45(3) . ?
O24 C31 1.32(2) . ?
O25 C37 1.28(2) 2_765 ?
O26 C37 1.24(2) . ?
C2 C2A 1.45(5) . ?
C2 C2B 1.69(6) . ?
C2 H2A 1.0000 . ?
C2A H2AA 0.9800 . ?
C2A H2AB 0.9800 . ?
C2A H2AC 0.9800 . ?
C2B H2BA 0.9800 . ?
C2B H2BB 0.9800 . ?
C2B H2BC 0.9800 . ?
C3 C3B 1.43(3) . ?
C3 C3A 1.43(3) . ?
C3 H3 1.0000 . ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?
C3A H3AC 0.9800 . ?
C3B H3BA 0.9800 . ?
C3B H3BB 0.9800 . ?
C3B H3BC 0.9800 . ?
C3' C3B' 1.38(3) . ?
C3' C3A' 1.42(3) . ?
C3' H3A' 1.0000 . ?
C3A' H3AD 0.9800 . ?
C3A' H3AE 0.9800 . ?
C3A' H3AF 0.9800 . ?
C3B' H3BD 0.9800 . ?
C3B' H3BE 0.9800 . ?
C3B' H3BF 0.9800 . ?
C11 C12 1.39(3) . ?
C11 C16 1.40(3) . ?
C12 C13 1.35(4) . ?
C12 H12A 0.9500 . ?
C13 C14 1.28(4) . ?
C13 H13A 0.9500 . ?
C14 C15 1.38(3) . ?
C14 H14A 0.9500 . ?
C15 C16 1.43(3) . ?
C15 H15A 0.9500 . ?
C16 C17 1.48(3) 3_665 ?
C22 C22B 1.40(7) . ?
C22 C22A 1.54(9) . ?
C22 H22' 1.0000 . ?
C22A H22A 0.9800 . ?
C22A H22B 0.9800 . ?
C22A H22C 0.9800 . ?
C22B H22D 0.9800 . ?
C22B H22E 0.9800 . ?
C22B H22F 0.9800 . ?
C23 C23A 1.45(3) . ?
C23 C23B 1.45(3) . ?
C23 H23A 1.0000 . ?
C23A H23B 0.9800 . ?
C23A H23C 0.9800 . ?
C23A H23D 0.9800 . ?
C23B H23E 0.9800 . ?
C23B H23F 0.9800 . ?
C23B H23G 0.9800 . ?
C23' C23C 1.40(3) . ?
C23' C23D 1.43(3) . ?
C23' H23H 1.0000 . ?
C23C H23I 0.9800 . ?
C23C H23J 0.9800 . ?
C23C H23K 0.9800 . ?
C23D H23L 0.9800 . ?
C23D H23M 0.9800 . ?
C23D H23N 0.9800 . ?
C31 C32 1.39(3) . ?
C31 C36 1.42(3) . ?
C32 C33 1.40(3) . ?
C32 H32A 0.9500 . ?
C33 C34 1.46(4) . ?
C33 H33A 0.9500 . ?
C34 C35 1.37(3) . ?
C34 H34A 0.9500 . ?
C35 C36 1.39(3) . ?
C35 H35A 0.9500 . ?
C36 C37 1.48(2) 2_765 ?

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 Tb1 O1 120.000(3) 2_655 3_665 ?
O1 Tb1 O1 120.000(2) 2_655 . ?
O1 Tb1 O1 119.999(2) 3_665 . ?
O1 Tb1 O6 135.7(2) 2_655 . ?
O1 Tb1 O6 72.9(4) 3_665 . ?
O1 Tb1 O6 65.1(4) . . ?
O1 Tb1 O6 72.9(4) 2_655 3_665 ?
O1 Tb1 O6 65.1(4) 3_665 3_665 ?
O1 Tb1 O6 135.7(2) . 3_665 ?
O6 Tb1 O6 77.1(4) . 3_665 ?
O1 Tb1 O6 65.1(4) 2_655 5_656 ?
O1 Tb1 O6 135.7(2) 3_665 5_656 ?
O1 Tb1 O6 72.9(4) . 5_656 ?
O6 Tb1 O6 137.85(18) . 5_656 ?
O6 Tb1 O6 137.85(18) 3_665 5_656 ?
O1 Tb1 O6 72.9(4) 2_655 6_666 ?
O1 Tb1 O6 65.1(4) 3_665 6_666 ?
O1 Tb1 O6 135.7(2) . 6_666 ?
O6 Tb1 O6 137.85(19) . 6_666 ?
O6 Tb1 O6 88.0(5) 3_665 6_666 ?
O6 Tb1 O6 77.0(4) 5_656 6_666 ?
O1 Tb1 O6 65.1(4) 2_655 2_655 ?
O1 Tb1 O6 135.7(2) 3_665 2_655 ?
O1 Tb1 O6 72.9(4) . 2_655 ?
O6 Tb1 O6 77.0(4) . 2_655 ?
O6 Tb1 O6 77.0(4) 3_665 2_655 ?
O6 Tb1 O6 88.0(5) 5_656 2_655 ?
O6 Tb1 O6 137.85(18) 6_666 2_655 ?
O1 Tb1 O6 135.7(2) 2_655 4_556 ?
O1 Tb1 O6 72.9(4) 3_665 4_556 ?
O1 Tb1 O6 65.1(4) . 4_556 ?
O6 Tb1 O6 88.0(5) . 4_556 ?
O6 Tb1 O6 137.85(18) 3_665 4_556 ?
O6 Tb1 O6 77.0(4) 5_656 4_556 ?
O6 Tb1 O6 77.0(4) 6_666 4_556 ?
O6 Tb1 O6 137.85(18) 2_655 4_556 ?
O1 Tb1 Ti1 130.2(3) 2_655 4_556 ?
O1 Tb1 Ti1 103.4(3) 3_665 4_556 ?
O1 Tb1 Ti1 28.75(19) . 4_556 ?
O6 Tb1 Ti1 77.4(3) . 4_556 ?
O6 Tb1 Ti1 154.1(2) 3_665 4_556 ?
O6 Tb1 Ti1 67.0(3) 5_656 4_556 ?
O6 Tb1 Ti1 108.7(2) 6_666 4_556 ?
O6 Tb1 Ti1 100.9(2) 2_655 4_556 ?
O6 Tb1 Ti1 37.0(3) 4_556 4_556 ?
O1 Tb1 Ti1 103.4(3) 2_655 3_665 ?
O1 Tb1 Ti1 28.75(19) 3_665 3_665 ?
O1 Tb1 Ti1 130.2(3) . 3_665 ?
O6 Tb1 Ti1 67.0(3) . 3_665 ?
O6 Tb1 Ti1 37.0(3) 3_665 3_665 ?
O6 Tb1 Ti1 154.1(2) 5_656 3_665 ?
O6 Tb1 Ti1 77.4(3) 6_666 3_665 ?
O6 Tb1 Ti1 108.7(2) 2_655 3_665 ?
O6 Tb1 Ti1 100.9(3) 4_556 3_665 ?
Ti1 Tb1 Ti1 125.95(2) 4_556 3_665 ?
O1 Tb1 Ti1 103.4(3) 2_655 6_666 ?
O1 Tb1 Ti1 28.75(19) 3_665 6_666 ?
O1 Tb1 Ti1 130.2(3) . 6_666 ?
O6 Tb1 Ti1 100.9(3) . 6_666 ?
O6 Tb1 Ti1 77.4(3) 3_665 6_666 ?
O6 Tb1 Ti1 108.7(2) 5_656 6_666 ?
O6 Tb1 Ti1 37.0(3) 6_666 6_666 ?
O6 Tb1 Ti1 154.1(2) 2_655 6_666 ?
O6 Tb1 Ti1 67.0(3) 4_556 6_666 ?
Ti1 Tb1 Ti1 103.83(5) 4_556 6_666 ?
Ti1 Tb1 Ti1 49.31(9) 3_665 6_666 ?
O21 Tb2 O21 120.000(17) 3_675 2_765 ?
O21 Tb2 O21 119.999(7) 3_675 . ?
O21 Tb2 O21 120.001(5) 2_765 . ?
O21 Tb2 O25 71.9(4) 3_675 5_767 ?
O21 Tb2 O25 66.1(4) 2_765 5_767 ?
O21 Tb2 O25 135.7(2) . 5_767 ?
O21 Tb2 O25 66.1(4) 3_675 3_675 ?
O21 Tb2 O25 135.7(2) 2_765 3_675 ?
O21 Tb2 O25 71.9(4) . 3_675 ?
O25 Tb2 O25 137.90(18) 5_767 3_675 ?
O21 Tb2 O25 66.1(4) 3_675 6_677 ?
O21 Tb2 O25 135.7(2) 2_765 6_677 ?
O21 Tb2 O25 71.9(4) . 6_677 ?
O25 Tb2 O25 76.9(4) 5_767 6_677 ?
O25 Tb2 O25 88.2(5) 3_675 6_677 ?
O21 Tb2 O25 135.7(2) 3_675 4_557 ?
O21 Tb2 O25 71.9(4) 2_765 4_557 ?
O21 Tb2 O25 66.1(4) . 4_557 ?
O25 Tb2 O25 76.9(4) 5_767 4_557 ?
O25 Tb2 O25 137.90(19) 3_675 4_557 ?
O25 Tb2 O25 76.9(4) 6_677 4_557 ?
O21 Tb2 O25 71.9(4) 3_675 2_765 ?
O21 Tb2 O25 66.1(4) 2_765 2_765 ?
O21 Tb2 O25 135.7(2) . 2_765 ?
O25 Tb2 O25 88.2(5) 5_767 2_765 ?
O25 Tb2 O25 76.9(4) 3_675 2_765 ?
O25 Tb2 O25 137.90(18) 6_677 2_765 ?
O25 Tb2 O25 137.90(18) 4_557 2_765 ?
O21 Tb2 O25 135.7(2) 3_675 . ?
O21 Tb2 O25 71.9(4) 2_765 . ?
O21 Tb2 O25 66.1(4) . . ?
O25 Tb2 O25 137.90(18) 5_767 . ?
O25 Tb2 O25 76.9(4) 3_675 . ?
O25 Tb2 O25 137.90(19) 6_677 . ?
O25 Tb2 O25 88.2(5) 4_557 . ?
O25 Tb2 O25 76.9(4) 2_765 . ?
O21 Tb2 Ti2 103.0(4) 3_675 5_767 ?
O21 Tb2 Ti2 28.9(2) 2_765 5_767 ?
O21 Tb2 Ti2 130.6(4) . 5_767 ?
O25 Tb2 Ti2 37.8(3) 5_767 5_767 ?
O25 Tb2 Ti2 154.6(3) 3_675 5_767 ?
O25 Tb2 Ti2 108.9(2) 6_677 5_767 ?
O25 Tb2 Ti2 66.3(3) 4_557 5_767 ?
O25 Tb2 Ti2 77.8(2) 2_765 5_767 ?
O25 Tb2 Ti2 100.2(3) . 5_767 ?
O21 Tb2 Ti2 103.0(4) 3_675 2_765 ?
O21 Tb2 Ti2 28.9(2) 2_765 2_765 ?
O21 Tb2 Ti2 130.6(4) . 2_765 ?
O25 Tb2 Ti2 77.8(2) 5_767 2_765 ?
O25 Tb2 Ti2 108.9(2) 3_675 2_765 ?
O25 Tb2 Ti2 154.6(3) 6_677 2_765 ?
O25 Tb2 Ti2 100.2(3) 4_557 2_765 ?
O25 Tb2 Ti2 37.8(3) 2_765 2_765 ?
O25 Tb2 Ti2 66.3(3) . 2_765 ?
Ti2 Tb2 Ti2 49.22(9) 5_767 2_765 ?
O21 Tb2 Ti2 130.6(4) 3_675 4_557 ?
O21 Tb2 Ti2 103.0(4) 2_765 4_557 ?
O21 Tb2 Ti2 28.9(2) . 4_557 ?
O25 Tb2 Ti2 108.9(3) 5_767 4_557 ?
O25 Tb2 Ti2 100.2(3) 3_675 4_557 ?
O25 Tb2 Ti2 66.3(3) 6_677 4_557 ?
O25 Tb2 Ti2 37.8(3) 4_557 4_557 ?
O25 Tb2 Ti2 154.6(3) 2_765 4_557 ?
O25 Tb2 Ti2 77.8(3) . 4_557 ?
Ti2 Tb2 Ti2 103.88(5) 5_767 4_557 ?
Ti2 Tb2 Ti2 125.93(2) 2_765 4_557 ?
O3 Ti1 O4 95.3(6) . . ?
O3 Ti1 O1 104.8(6) . . ?
O4 Ti1 O1 159.4(6) . . ?
O3 Ti1 O2 98.6(6) . . ?
O4 Ti1 O2 96.6(6) . . ?
O1 Ti1 O2 76.5(5) . . ?
O3 Ti1 O5 90.3(6) . . ?
O4 Ti1 O5 93.9(5) . . ?
O1 Ti1 O5 90.3(5) . . ?
O2 Ti1 O5 165.5(5) . . ?
O3 Ti1 O6 170.1(5) . . ?
O4 Ti1 O6 81.9(5) . . ?
O1 Ti1 O6 78.9(5) . . ?
O2 Ti1 O6 91.1(6) . . ?
O5 Ti1 O6 80.4(5) . . ?
O3 Ti1 Ti1 90.9(4) . 4_556 ?
O4 Ti1 Ti1 138.3(4) . 4_556 ?
O1 Ti1 Ti1 39.1(3) . 4_556 ?
O2 Ti1 Ti1 41.7(3) . 4_556 ?
O5 Ti1 Ti1 127.3(3) . 4_556 ?
O6 Ti1 Ti1 97.4(3) . 4_556 ?
O3 Ti1 Tb1 136.6(4) . . ?
O4 Ti1 Tb1 126.9(4) . . ?
O1 Ti1 Tb1 34.7(4) . . ?
O2 Ti1 Tb1 87.2(4) . . ?
O5 Ti1 Tb1 78.5(4) . . ?
O6 Ti1 Tb1 45.0(3) . . ?
Ti1 Ti1 Tb1 65.34(5) 4_556 . ?
O23 Ti2 O24 94.5(6) . . ?
O23 Ti2 O21 103.6(7) . . ?
O24 Ti2 O21 161.5(7) . . ?
O23 Ti2 O22 95.8(7) . . ?
O24 Ti2 O22 97.7(5) . . ?
O21 Ti2 O22 76.8(6) . . ?
O23 Ti2 O26 92.2(6) . . ?
O24 Ti2 O26 93.5(5) . . ?
O21 Ti2 O26 89.7(6) . . ?
O22 Ti2 O26 165.6(5) . . ?
O23 Ti2 O25 171.4(5) . . ?
O24 Ti2 O25 82.3(5) . . ?
O21 Ti2 O25 80.3(6) . . ?
O22 Ti2 O25 92.5(6) . . ?
O26 Ti2 O25 80.1(5) . . ?
O23 Ti2 Ti2 90.5(3) . 4_557 ?
O24 Ti2 Ti2 139.3(4) . 4_557 ?
O21 Ti2 Ti2 38.5(4) . 4_557 ?
O22 Ti2 Ti2 41.6(3) . 4_557 ?
O26 Ti2 Ti2 126.7(4) . 4_557 ?
O25 Ti2 Ti2 97.2(3) . 4_557 ?
O23 Ti2 Tb2 137.4(4) . . ?
O24 Ti2 Tb2 127.0(4) . . ?
O21 Ti2 Tb2 36.4(5) . . ?
O22 Ti2 Tb2 88.3(4) . . ?
O26 Ti2 Tb2 77.7(4) . . ?
O25 Ti2 Tb2 44.7(3) . . ?
Ti2 Ti2 Tb2 65.39(4) 4_557 . ?
Ti1 O1 Ti1 101.8(7) 4_556 . ?
Ti1 O1 Tb1 116.5(5) 4_556 . ?
Ti1 O1 Tb1 116.5(5) . . ?
C2 O2 Ti1 130.4(5) . 4_556 ?
C2 O2 Ti1 130.4(5) . . ?
Ti1 O2 Ti1 96.5(7) 4_556 . ?
C3' O3 Ti1 165.2(16) . . ?
C3 O3 Ti1 136.3(16) . . ?
C11 O4 Ti1 141.3(12) . . ?
C17 O5 Ti1 137.8(13) . . ?
C17 O6 Ti1 130.9(12) 3_665 . ?
C17 O6 Tb1 130.8(12) 3_665 . ?
Ti1 O6 Tb1 98.0(4) . . ?
Ti2 O21 Ti2 103.0(8) 4_557 . ?
Ti2 O21 Tb2 114.7(6) 4_557 . ?
Ti2 O21 Tb2 114.7(6) . . ?
C22 O22 Ti2 130.6(4) . 4_557 ?
C22 O22 Ti2 130.6(4) . . ?
Ti2 O22 Ti2 96.9(7) 4_557 . ?
C23' O23 Ti2 173.1(19) . . ?
C23 O23 Ti2 130.0(18) . . ?
C31 O24 Ti2 140.8(11) . . ?
C37 O25 Ti2 129.6(11) 2_765 . ?
C37 O25 Tb2 132.7(11) 2_765 . ?
Ti2 O25 Tb2 97.5(4) . . ?
C37 O26 Ti2 137.9(13) . . ?
C2A C2 O2 112(3) . . ?
C2A C2 C2B 138(3) . . ?
O2 C2 C2B 109(3) . . ?
C2A C2 H2A 93.1 . . ?
O2 C2 H2A 93.1 . . ?
C2B C2 H2A 93.1 . . ?
C2 C2A H2AA 109.5 . . ?
C2 C2A H2AB 109.5 . . ?
H2AA C2A H2AB 109.5 . . ?
C2 C2A H2AC 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
C2 C2B H2BA 109.5 . . ?
C2 C2B H2BB 109.5 . . ?
H2BA C2B H2BB 109.5 . . ?
C2 C2B H2BC 109.5 . . ?
H2BA C2B H2BC 109.5 . . ?
H2BB C2B H2BC 109.5 . . ?
C3B C3 C3A 111(3) . . ?
C3B C3 O3 109(2) . . ?
C3A C3 O3 112(2) . . ?
C3B C3 H3 108.6 . . ?
C3A C3 H3 108.6 . . ?
O3 C3 H3 108.6 . . ?
C3 C3A H3AA 109.5 . . ?
C3 C3A H3AB 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
C3 C3A H3AC 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
C3 C3B H3BA 109.5 . . ?
C3 C3B H3BB 109.5 . . ?
H3BA C3B H3BB 109.5 . . ?
C3 C3B H3BC 109.5 . . ?
H3BA C3B H3BC 109.5 . . ?
H3BB C3B H3BC 109.5 . . ?
C3B' C3' O3 118(3) . . ?
C3B' C3' C3A' 115(3) . . ?
O3 C3' C3A' 111(2) . . ?
C3B' C3' H3A' 103.4 . . ?
O3 C3' H3A' 103.4 . . ?
C3A' C3' H3A' 103.4 . . ?
C3' C3A' H3AD 109.5 . . ?
C3' C3A' H3AE 109.5 . . ?
H3AD C3A' H3AE 109.5 . . ?
C3' C3A' H3AF 109.5 . . ?
H3AD C3A' H3AF 109.5 . . ?
H3AE C3A' H3AF 109.5 . . ?
C3' C3B' H3BD 109.5 . . ?
C3' C3B' H3BE 109.5 . . ?
H3BD C3B' H3BE 109.5 . . ?
C3' C3B' H3BF 109.5 . . ?
H3BD C3B' H3BF 109.5 . . ?
H3BE C3B' H3BF 109.5 . . ?
O4 C11 C12 120.9(19) . . ?
O4 C11 C16 121.1(17) . . ?
C12 C11 C16 117.8(19) . . ?
C13 C12 C11 119(2) . . ?
C13 C12 H12A 120.6 . . ?
C11 C12 H12A 120.6 . . ?
C14 C13 C12 127(2) . . ?
C14 C13 H13A 116.4 . . ?
C12 C13 H13A 116.4 . . ?
C13 C14 C15 117(3) . . ?
C13 C14 H14A 121.5 . . ?
C15 C14 H14A 121.5 . . ?
C14 C15 C16 120(2) . . ?
C14 C15 H15A 119.8 . . ?
C16 C15 H15A 119.8 . . ?
C11 C16 C15 118.7(19) . . ?
C11 C16 C17 123.1(17) . 3_665 ?
C15 C16 C17 118.2(19) . 3_665 ?
O5 C17 O6 121.6(18) . 2_655 ?
O5 C17 C16 117.2(17) . 2_655 ?
O6 C17 C16 121.1(18) 2_655 2_655 ?
C22B C22 O22 115(4) . . ?
C22B C22 C22A 140(5) . . ?
O22 C22 C22A 98(4) . . ?
C22B C22 H22' 98.3 . . ?
O22 C22 H22' 98.3 . . ?
C22A C22 H22' 98.3 . . ?
C22 C22A H22A 109.5 . . ?
C22 C22A H22B 109.5 . . ?
H22A C22A H22B 109.5 . . ?
C22 C22A H22C 109.5 . . ?
H22A C22A H22C 109.5 . . ?
H22B C22A H22C 109.5 . . ?
C22 C22B H22D 109.5 . . ?
C22 C22B H22E 109.5 . . ?
H22D C22B H22E 109.5 . . ?
C22 C22B H22F 109.5 . . ?
H22D C22B H22F 109.5 . . ?
H22E C22B H22F 109.5 . . ?
C23A C23 O23 111(4) . . ?
C23A C23 C23B 107(3) . . ?
O23 C23 C23B 111(4) . . ?
C23A C23 H23A 109.3 . . ?
O23 C23 H23A 109.3 . . ?
C23B C23 H23A 109.3 . . ?
C23 C23A H23B 109.5 . . ?
C23 C23A H23C 109.5 . . ?
H23B C23A H23C 109.5 . . ?
C23 C23A H23D 109.5 . . ?
H23B C23A H23D 109.5 . . ?
H23C C23A H23D 109.5 . . ?
C23 C23B H23E 109.5 . . ?
C23 C23B H23F 109.5 . . ?
H23E C23B H23F 109.5 . . ?
C23 C23B H23G 109.5 . . ?
H23E C23B H23G 109.5 . . ?
H23F C23B H23G 109.5 . . ?
O23 C23' C23C 98(4) . . ?
O23 C23' C23D 113(4) . . ?
C23C C23' C23D 112(3) . . ?
O23 C23' H23H 111.1 . . ?
C23C C23' H23H 111.1 . . ?
C23D C23' H23H 111.1 . . ?
C23' C23C H23I 109.5 . . ?
C23' C23C H23J 109.5 . . ?
H23I C23C H23J 109.5 . . ?
C23' C23C H23K 109.5 . . ?
H23I C23C H23K 109.5 . . ?
H23J C23C H23K 109.5 . . ?
C23' C23D H23L 109.5 . . ?
C23' C23D H23M 109.5 . . ?
H23L C23D H23M 109.5 . . ?
C23' C23D H23N 109.5 . . ?
H23L C23D H23N 109.5 . . ?
H23M C23D H23N 109.5 . . ?
O24 C31 C32 119.2(18) . . ?
O24 C31 C36 122.2(15) . . ?
C32 C31 C36 118.6(18) . . ?
C31 C32 C33 121(2) . . ?
C31 C32 H32A 119.4 . . ?
C33 C32 H32A 119.4 . . ?
C32 C33 C34 120(2) . . ?
C32 C33 H33A 120.1 . . ?
C34 C33 H33A 120.1 . . ?
C35 C34 C33 117(2) . . ?
C35 C34 H34A 121.4 . . ?
C33 C34 H34A 121.4 . . ?
C34 C35 C36 123(2) . . ?
C34 C35 H35A 118.6 . . ?
C36 C35 H35A 118.6 . . ?
C35 C36 C31 120.2(18) . . ?
C35 C36 C37 118.0(18) . 2_765 ?
C31 C36 C37 121.8(16) . 2_765 ?
O26 C37 O25 120.6(17) . 3_675 ?
O26 C37 C36 116.2(17) . 3_675 ?
O25 C37 C36 123.2(16) 3_675 3_675 ?

_refine_diff_density_max         6.042
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.188

####################################################################### 
# 
# 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_sm_b_sq
_database_code_depnum_ccdc_archive 'CCDC 1504172'
_audit_update_record             
;
2017-02-27 deposited with the CCDC.
2017-03-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C69 H87 O30 Sm Ti6'
_chemical_formula_sum            'C69 H87 O30 Sm Ti6'
_chemical_formula_weight         1834.13

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -5.3236 12.2178 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           174
_space_group_name_H-M_alt        'P -6'
_space_group_name_Hall           'P -6'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'

_cell_length_a                   14.9683(4)
_cell_length_b                   14.9683(4)
_cell_length_c                   23.6974(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4598.1(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9582
_cell_measurement_theta_min      3.41
_cell_measurement_theta_max      66.6

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_F_000             1870
_exptl_transmission_factor_min   0.791
_exptl_transmission_factor_max   1.000
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    9.516
_shelx_estimated_absorpt_T_min   0.240
_shelx_estimated_absorpt_T_max   0.349
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.240
_exptl_absorpt_correction_T_max  0.349
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements (SADABS) 
;
_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         '30W microfocus sealed tube, Quazar optics'
_diffrn_measurement_device_type  'Bruker QUEST D8 CCD'
_diffrn_measurement_method       'Thin slice ω and φ scans'
_diffrn_reflns_number            104538
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.409
_diffrn_reflns_theta_max         66.858
_diffrn_reflns_theta_full        66.858
_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 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5582
_reflns_number_gt                5380
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.988
_reflns_Friedel_fraction_max     0.996
_reflns_Friedel_fraction_full    0.997

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 software package, narrow-frames'
_computing_cell_refinement       'refinement of XYZ centroids > 20sigma(I)'
_computing_data_reduction        
;
 Bruker SAINT software package, narrow frame algorithm
;
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_refine_special_details          
;Refined as a 2-component twin. Residual electron density did not resolve into
anything meaningful but is presumably disordered solvent and so was treated with
SQUEEZE. The disorder in the iPr ligands could be modelled satifactorily by 
applying restraints and keeping them isotropic., Twin,SQUEEZE
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0597P)²+4.3518P] 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_abs_structure_details 
;
 Flack x determined using 2572 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5582
_refine_ls_number_parameters     331
_refine_ls_number_restraints     212
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0377
_refine_ls_wR_factor_ref         0.1018
_refine_ls_wR_factor_gt          0.1000
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_restrained_S_all      1.130
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Sm1 Sm 0.666667 0.333333 0.500000 0.0221(3) Uani 1 6 d S T P . .
Sm2 Sm 1.000000 1.000000 1.000000 0.0248(3) Uani 1 6 d S T P . .
Ti1 Ti 0.46690(14) 0.36487(14) 0.56302(7) 0.0321(4) Uani 1 1 d . . . . .
Ti2 Ti 0.81234(15) 0.76152(15) 0.93691(7) 0.0361(4) Uani 1 1 d . . . . .
O1 O 0.5014(7) 0.3097(7) 0.500000 0.0258(18) Uani 1 2 d S TU P . .
O2 O 0.4860(7) 0.4616(7) 0.500000 0.036(2) Uani 1 2 d S TU P C .
O3 O 0.3302(5) 0.2961(6) 0.5644(3) 0.0465(18) Uani 1 1 d D U . . .
O4 O 0.4811(5) 0.4548(6) 0.6223(3) 0.0448(18) Uani 1 1 d . U . . .
O5 O 0.4712(6) 0.2595(5) 0.6140(3) 0.0389(18) Uani 1 1 d . U . . .
O6 O 0.6325(5) 0.4353(5) 0.5746(2) 0.0295(13) Uani 1 1 d . U . . .
O21 O 0.8360(8) 0.8502(8) 1.000000 0.036(2) Uani 1 2 d S TU P . .
O22 O 0.8379(10) 0.6884(7) 1.000000 0.044(2) Uani 1 2 d S TU P G .
O23 O 0.6756(6) 0.6821(6) 0.9354(3) 0.0465(19) Uani 1 1 d D U . . .
O24 O 0.8346(7) 0.6932(5) 0.8771(3) 0.0486(19) Uani 1 1 d . U . . .
O25 O 0.9785(5) 0.8669(5) 0.9253(3) 0.0336(15) Uani 1 1 d . U . . .
O26 O 0.8065(7) 0.8671(7) 0.8863(4) 0.044(2) Uani 1 1 d . U . . .
C2 C 0.4822(14) 0.5579(12) 0.500000 0.061(5) Uani 1 2 d S TU P . .
H2A H 0.473309 0.558435 0.541798 0.073 Uiso 0.5 1 calc R U P A -1
C2A C 0.5856(19) 0.6471(17) 0.500000 0.088(7) Uani 1 2 d S TU P C .
H2AA H 0.581326 0.710358 0.500000 0.132 Uiso 0.5 1 calc R U P B -1
H2AB H 0.622639 0.645616 0.533766 0.132 Uiso 0.5 1 calc R U P B -1
H2AC H 0.622639 0.645616 0.466234 0.132 Uiso 0.5 1 calc R U P B -1
C2B C 0.372(3) 0.539(3) 0.4861(19) 0.110(16) Uani 0.5 1 d . U P C -1
H2BA H 0.321310 0.465384 0.491486 0.165 Uiso 0.5 1 calc R U P C -1
H2BB H 0.355377 0.580347 0.511160 0.165 Uiso 0.5 1 calc R U P C -1
H2BC H 0.369736 0.557846 0.446760 0.165 Uiso 0.5 1 calc R U P C -1
C3 C 0.2498(16) 0.2532(16) 0.6063(10) 0.066(5) Uiso 0.553(16) 1 d D U P D 1
H3 H 0.282872 0.258896 0.643807 0.079 Uiso 0.553(16) 1 calc R U P D 1
C3A C 0.195(2) 0.311(2) 0.6094(13) 0.083(5) Uiso 0.553(16) 1 d D U P D 1
H3AA H 0.244884 0.383633 0.617220 0.125 Uiso 0.553(16) 1 calc R U P D 1
H3AB H 0.160960 0.305373 0.573319 0.125 Uiso 0.553(16) 1 calc R U P D 1
H3AC H 0.143997 0.282790 0.639615 0.125 Uiso 0.553(16) 1 calc R U P D 1
C3B C 0.182(2) 0.1466(17) 0.5950(13) 0.083(5) Uiso 0.553(16) 1 d D U P D 1
H3BA H 0.127766 0.117483 0.623490 0.125 Uiso 0.553(16) 1 calc R U P D 1
H3BB H 0.151700 0.138617 0.557493 0.125 Uiso 0.553(16) 1 calc R U P D 1
H3BC H 0.221661 0.110196 0.596122 0.125 Uiso 0.553(16) 1 calc R U P D 1
C3' C 0.2268(17) 0.2242(18) 0.5614(13) 0.066(5) Uiso 0.447(16) 1 d D U P D 2
H3A' H 0.208202 0.234349 0.522319 0.079 Uiso 0.447(16) 1 calc R U P D 2
C3A' C 0.167(2) 0.254(3) 0.5963(15) 0.083(5) Uiso 0.447(16) 1 d D U P D 2
H3AD H 0.093496 0.201996 0.593498 0.125 Uiso 0.447(16) 1 calc R U P D 2
H3AE H 0.189199 0.260120 0.635662 0.125 Uiso 0.447(16) 1 calc R U P D 2
H3AF H 0.176909 0.320891 0.583424 0.125 Uiso 0.447(16) 1 calc R U P D 2
C3B' C 0.194(3) 0.1194(18) 0.5622(16) 0.083(5) Uiso 0.447(16) 1 d D U P D 2
H3BD H 0.119028 0.079433 0.559756 0.125 Uiso 0.447(16) 1 calc R U P D 2
H3BE H 0.224538 0.102593 0.530091 0.125 Uiso 0.447(16) 1 calc R U P D 2
H3BF H 0.216986 0.102501 0.597457 0.125 Uiso 0.447(16) 1 calc R U P D 2
C11 C 0.5538(9) 0.5287(8) 0.6547(5) 0.045(3) Uani 1 1 d . U . . .
C12 C 0.5263(11) 0.5790(10) 0.6938(5) 0.059(4) Uani 1 1 d . U . . .
H12A H 0.456351 0.562361 0.696506 0.071 Uiso 1 1 calc R U . . .
C13 C 0.5975(13) 0.6514(14) 0.7282(6) 0.077(4) Uani 1 1 d . U . . .
H13A H 0.576514 0.685952 0.753943 0.092 Uiso 1 1 calc R U . . .
C14 C 0.6959(14) 0.6761(14) 0.7273(6) 0.077(4) Uani 1 1 d . U . . .
H14A H 0.743758 0.726579 0.752586 0.092 Uiso 1 1 calc R U . . .
C15 C 0.7288(11) 0.6274(11) 0.6890(5) 0.060(3) Uani 1 1 d . U . . .
H15A H 0.799103 0.644707 0.688160 0.072 Uiso 1 1 calc R U . . .
C16 C 0.6574(9) 0.5529(9) 0.6519(5) 0.043(3) Uani 1 1 d . U . . .
C17 C 0.4979(9) 0.1915(9) 0.6112(5) 0.040(3) Uani 1 1 d . U . . .
C22 C 0.8406(19) 0.5929(18) 1.000000 0.075(6) Uani 1 2 d S TU P . .
H22' H 0.824150 0.573360 0.959401 0.090 Uiso 0.5 1 calc R U P E -1
C22A C 0.954(3) 0.625(3) 1.000000 0.175(16) Uani 1 2 d S TU P G .
H22A H 0.992764 0.686902 0.976989 0.263 Uiso 0.5 1 calc R U P F -1
H22B H 0.980461 0.638890 1.038764 0.263 Uiso 0.5 1 calc R U P F -1
H22C H 0.962489 0.568753 0.984248 0.263 Uiso 0.5 1 calc R U P F -1
C22B C 0.750(3) 0.510(2) 1.0256(13) 0.098(10) Uani 0.5 1 d . U P G -1
H22D H 0.753714 0.447077 1.024921 0.147 Uiso 0.5 1 calc R U P G -1
H22E H 0.744376 0.528417 1.064708 0.147 Uiso 0.5 1 calc R U P G -1
H22F H 0.688510 0.499304 1.004491 0.147 Uiso 0.5 1 calc R U P G -1
C23 C 0.6031(19) 0.6392(19) 0.8880(11) 0.075(6) Uiso 0.508(14) 1 d D U P H 1
H23A H 0.639309 0.672897 0.852049 0.091 Uiso 0.508(14) 1 calc R U P H 1
C23A C 0.516(3) 0.656(3) 0.8963(14) 0.086(5) Uiso 0.508(14) 1 d D U P H 1
H23B H 0.468394 0.626878 0.864356 0.129 Uiso 0.508(14) 1 calc R U P H 1
H23C H 0.479921 0.621916 0.931251 0.129 Uiso 0.508(14) 1 calc R U P H 1
H23D H 0.541079 0.730044 0.898971 0.129 Uiso 0.508(14) 1 calc R U P H 1
C23B C 0.564(3) 0.528(2) 0.8847(14) 0.086(5) Uiso 0.508(14) 1 d D U P H 1
H23E H 0.622054 0.515370 0.879114 0.129 Uiso 0.508(14) 1 calc R U P H 1
H23F H 0.528375 0.494595 0.919900 0.129 Uiso 0.508(14) 1 calc R U P H 1
H23G H 0.516022 0.498251 0.852995 0.129 Uiso 0.508(14) 1 calc R U P H 1
C23' C 0.5656(18) 0.635(2) 0.9380(12) 0.075(6) Uiso 0.492(14) 1 d D U P H 2
H23H H 0.539457 0.595575 0.974082 0.091 Uiso 0.492(14) 1 calc R U P H 2
C23C C 0.555(3) 0.719(2) 0.9388(14) 0.086(5) Uiso 0.492(14) 1 d D U P H 2
H23I H 0.481495 0.697986 0.940559 0.129 Uiso 0.492(14) 1 calc R U P H 2
H23J H 0.590331 0.761395 0.971925 0.129 Uiso 0.492(14) 1 calc R U P H 2
H23K H 0.585178 0.759885 0.904455 0.129 Uiso 0.492(14) 1 calc R U P H 2
C23D C 0.513(3) 0.568(2) 0.8905(13) 0.086(5) Uiso 0.492(14) 1 d D U P H 2
H23L H 0.522650 0.508108 0.891565 0.129 Uiso 0.492(14) 1 calc R U P H 2
H23M H 0.439166 0.545111 0.892608 0.129 Uiso 0.492(14) 1 calc R U P H 2
H23N H 0.541412 0.606192 0.855288 0.129 Uiso 0.492(14) 1 calc R U P H 2
C31 C 0.9090(10) 0.7003(9) 0.8437(5) 0.048(3) Uani 1 1 d . U . . .
C32 C 0.8870(12) 0.6242(11) 0.8036(6) 0.066(4) Uani 1 1 d . U . . .
H32A H 0.819681 0.565515 0.802020 0.079 Uiso 1 1 calc R U . . .
C33 C 0.9612(15) 0.6325(13) 0.7662(6) 0.081(5) Uani 1 1 d . U . . .
H33A H 0.943174 0.581465 0.737801 0.097 Uiso 1 1 calc R U . . .
C34 C 1.0608(14) 0.7132(13) 0.7692(6) 0.083(5) Uani 1 1 d . U . . .
H34A H 1.111951 0.717694 0.743754 0.100 Uiso 1 1 calc R U . . .
C35 C 1.0856(12) 0.7891(11) 0.8109(5) 0.062(4) Uani 1 1 d . U . . .
H35A H 1.154293 0.845185 0.813581 0.074 Uiso 1 1 calc R U . . .
C36 C 1.0110(9) 0.7835(9) 0.8482(5) 0.044(3) Uani 1 1 d . U . . .
C37 C 0.8261(9) 0.9590(9) 0.8892(5) 0.035(2) Uani 1 1 d . 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
Sm1 O1 2.317(9) 2_655 ?
Sm1 O1 2.317(9) . ?
Sm1 O1 2.317(9) 3_665 ?
Sm1 O6 2.550(6) . ?
Sm1 O6 2.550(6) 3_665 ?
Sm1 O6 2.550(6) 5_656 ?
Sm1 O6 2.550(6) 6_666 ?
Sm1 O6 2.550(6) 2_655 ?
Sm1 O6 2.550(6) 4_556 ?
Sm1 Ti1 3.5784(16) 4_556 ?
Sm1 Ti1 3.5785(16) . ?
Sm1 Ti1 3.5785(17) 3_665 ?
Sm2 O21 2.355(10) 3_675 ?
Sm2 O21 2.355(10) 2_765 ?
Sm2 O21 2.355(10) . ?
Sm2 O25 2.562(6) 3_675 ?
Sm2 O25 2.562(6) 6_677 ?
Sm2 O25 2.562(6) 5_767 ?
Sm2 O25 2.562(6) 2_765 ?
Sm2 O25 2.562(6) 4_557 ?
Sm2 O25 2.562(6) . ?
Sm2 Ti2 3.5834(18) 6_677 ?
Sm2 Ti2 3.5834(18) 3_675 ?
Sm2 Ti2 3.5834(18) . ?
Ti1 O3 1.772(7) . ?
Ti1 O4 1.883(7) . ?
Ti1 O1 1.899(5) . ?
Ti1 O2 1.999(6) . ?
Ti1 O5 2.013(7) . ?
Ti1 O6 2.171(7) . ?
Ti1 Ti1 2.987(3) 4_556 ?
Ti2 O23 1.780(8) . ?
Ti2 O24 1.872(8) . ?
Ti2 O21 1.911(6) . ?
Ti2 O22 1.999(8) . ?
Ti2 O26 2.020(9) . ?
Ti2 O25 2.197(8) . ?
Ti2 Ti2 2.990(3) 4_557 ?
O2 C2 1.470(18) . ?
O3 C3' 1.38(2) . ?
O3 C3 1.44(2) . ?
O4 C11 1.339(13) . ?
O5 C17 1.267(15) . ?
O6 C17 1.293(13) 3_665 ?
O22 C22 1.45(3) . ?
O23 C23' 1.43(2) . ?
O23 C23 1.47(2) . ?
O24 C31 1.327(14) . ?
O25 C37 1.267(14) 2_765 ?
O26 C37 1.258(12) . ?
C2 C2A 1.45(3) . ?
C2 C2B 1.56(4) . ?
C2 H2A 1.0000 . ?
C2A H2AA 0.9800 . ?
C2A H2AB 0.9800 . ?
C2A H2AC 0.9800 . ?
C2B H2BA 0.9800 . ?
C2B H2BB 0.9800 . ?
C2B H2BC 0.9800 . ?
C3 C3B 1.42(2) . ?
C3 C3A 1.45(2) . ?
C3 H3 1.0000 . ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?
C3A H3AC 0.9800 . ?
C3B H3BA 0.9800 . ?
C3B H3BB 0.9800 . ?
C3B H3BC 0.9800 . ?
C3' C3B' 1.39(2) . ?
C3' C3A' 1.45(2) . ?
C3' H3A' 1.0000 . ?
C3A' H3AD 0.9800 . ?
C3A' H3AE 0.9800 . ?
C3A' H3AF 0.9800 . ?
C3B' H3BD 0.9800 . ?
C3B' H3BE 0.9800 . ?
C3B' H3BF 0.9800 . ?
C11 C12 1.379(15) . ?
C11 C16 1.407(17) . ?
C12 C13 1.35(2) . ?
C12 H12A 0.9500 . ?
C13 C14 1.33(2) . ?
C13 H13A 0.9500 . ?
C14 C15 1.398(19) . ?
C14 H14A 0.9500 . ?
C15 C16 1.403(17) . ?
C15 H15A 0.9500 . ?
C16 C17 1.488(16) 3_665 ?
C22 C22B 1.44(4) . ?
C22 C22A 1.52(5) . ?
C22 H22' 1.0000 . ?
C22A H22A 0.9800 . ?
C22A H22B 0.9800 . ?
C22A H22C 0.9800 . ?
C22B H22D 0.9800 . ?
C22B H22E 0.9800 . ?
C22B H22F 0.9800 . ?
C23 C23A 1.46(3) . ?
C23 C23B 1.47(3) . ?
C23 H23A 1.0000 . ?
C23A H23B 0.9800 . ?
C23A H23C 0.9800 . ?
C23A H23D 0.9800 . ?
C23B H23E 0.9800 . ?
C23B H23F 0.9800 . ?
C23B H23G 0.9800 . ?
C23' C23C 1.35(3) . ?
C23' C23D 1.45(3) . ?
C23' H23H 1.0000 . ?
C23C H23I 0.9800 . ?
C23C H23J 0.9800 . ?
C23C H23K 0.9800 . ?
C23D H23L 0.9800 . ?
C23D H23M 0.9800 . ?
C23D H23N 0.9800 . ?
C31 C32 1.390(16) . ?
C31 C36 1.412(17) . ?
C32 C33 1.38(2) . ?
C32 H32A 0.9500 . ?
C33 C34 1.37(2) . ?
C33 H33A 0.9500 . ?
C34 C35 1.408(18) . ?
C34 H34A 0.9500 . ?
C35 C36 1.393(16) . ?
C35 H35A 0.9500 . ?
C36 C37 1.467(16) 2_765 ?

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 Sm1 O1 120.000(1) 2_655 . ?
O1 Sm1 O1 120.000(2) 2_655 3_665 ?
O1 Sm1 O1 120.000(1) . 3_665 ?
O1 Sm1 O6 135.73(14) 2_655 . ?
O1 Sm1 O6 64.7(2) . . ?
O1 Sm1 O6 73.2(2) 3_665 . ?
O1 Sm1 O6 73.2(2) 2_655 3_665 ?
O1 Sm1 O6 135.73(14) . 3_665 ?
O1 Sm1 O6 64.7(2) 3_665 3_665 ?
O6 Sm1 O6 77.2(2) . 3_665 ?
O1 Sm1 O6 64.7(2) 2_655 5_656 ?
O1 Sm1 O6 73.2(2) . 5_656 ?
O1 Sm1 O6 135.73(14) 3_665 5_656 ?
O6 Sm1 O6 137.77(10) . 5_656 ?
O6 Sm1 O6 137.77(10) 3_665 5_656 ?
O1 Sm1 O6 73.2(2) 2_655 6_666 ?
O1 Sm1 O6 135.73(14) . 6_666 ?
O1 Sm1 O6 64.7(2) 3_665 6_666 ?
O6 Sm1 O6 137.77(11) . 6_666 ?
O6 Sm1 O6 87.8(3) 3_665 6_666 ?
O6 Sm1 O6 77.2(2) 5_656 6_666 ?
O1 Sm1 O6 64.7(2) 2_655 2_655 ?
O1 Sm1 O6 73.2(2) . 2_655 ?
O1 Sm1 O6 135.73(14) 3_665 2_655 ?
O6 Sm1 O6 77.2(2) . 2_655 ?
O6 Sm1 O6 77.2(2) 3_665 2_655 ?
O6 Sm1 O6 87.8(3) 5_656 2_655 ?
O6 Sm1 O6 137.77(10) 6_666 2_655 ?
O1 Sm1 O6 135.73(14) 2_655 4_556 ?
O1 Sm1 O6 64.7(2) . 4_556 ?
O1 Sm1 O6 73.2(2) 3_665 4_556 ?
O6 Sm1 O6 87.8(3) . 4_556 ?
O6 Sm1 O6 137.77(11) 3_665 4_556 ?
O6 Sm1 O6 77.2(2) 5_656 4_556 ?
O6 Sm1 O6 77.2(2) 6_666 4_556 ?
O6 Sm1 O6 137.77(11) 2_655 4_556 ?
O1 Sm1 Ti1 129.85(19) 2_655 4_556 ?
O1 Sm1 Ti1 28.54(11) . 4_556 ?
O1 Sm1 Ti1 103.8(2) 3_665 4_556 ?
O6 Sm1 Ti1 77.24(14) . 4_556 ?
O6 Sm1 Ti1 154.15(14) 3_665 4_556 ?
O6 Sm1 Ti1 67.06(14) 5_656 4_556 ?
O6 Sm1 Ti1 108.73(14) 6_666 4_556 ?
O6 Sm1 Ti1 100.90(14) 2_655 4_556 ?
O6 Sm1 Ti1 36.91(15) 4_556 4_556 ?
O1 Sm1 Ti1 129.85(19) 2_655 . ?
O1 Sm1 Ti1 28.54(11) . . ?
O1 Sm1 Ti1 103.8(2) 3_665 . ?
O6 Sm1 Ti1 36.91(15) . . ?
O6 Sm1 Ti1 108.73(14) 3_665 . ?
O6 Sm1 Ti1 100.90(14) 5_656 . ?
O6 Sm1 Ti1 154.15(14) 6_666 . ?
O6 Sm1 Ti1 67.06(14) 2_655 . ?
O6 Sm1 Ti1 77.24(14) 4_556 . ?
Ti1 Sm1 Ti1 49.33(5) 4_556 . ?
O1 Sm1 Ti1 103.8(2) 2_655 3_665 ?
O1 Sm1 Ti1 129.85(18) . 3_665 ?
O1 Sm1 Ti1 28.54(11) 3_665 3_665 ?
O6 Sm1 Ti1 67.07(14) . 3_665 ?
O6 Sm1 Ti1 36.91(15) 3_665 3_665 ?
O6 Sm1 Ti1 154.15(14) 5_656 3_665 ?
O6 Sm1 Ti1 77.24(15) 6_666 3_665 ?
O6 Sm1 Ti1 108.73(14) 2_655 3_665 ?
O6 Sm1 Ti1 100.90(14) 4_556 3_665 ?
Ti1 Sm1 Ti1 125.952(13) 4_556 3_665 ?
Ti1 Sm1 Ti1 103.81(3) . 3_665 ?
O21 Sm2 O21 120.000(10) 3_675 2_765 ?
O21 Sm2 O21 119.999(4) 3_675 . ?
O21 Sm2 O21 120.001(3) 2_765 . ?
O21 Sm2 O25 66.0(2) 3_675 3_675 ?
O21 Sm2 O25 136.16(15) 2_765 3_675 ?
O21 Sm2 O25 71.6(2) . 3_675 ?
O21 Sm2 O25 66.0(2) 3_675 6_677 ?
O21 Sm2 O25 136.16(15) 2_765 6_677 ?
O21 Sm2 O25 71.6(2) . 6_677 ?
O25 Sm2 O25 87.4(3) 3_675 6_677 ?
O21 Sm2 O25 71.6(2) 3_675 5_767 ?
O21 Sm2 O25 66.0(2) 2_765 5_767 ?
O21 Sm2 O25 136.16(15) . 5_767 ?
O25 Sm2 O25 137.61(11) 3_675 5_767 ?
O25 Sm2 O25 77.6(2) 6_677 5_767 ?
O21 Sm2 O25 71.6(2) 3_675 2_765 ?
O21 Sm2 O25 66.0(2) 2_765 2_765 ?
O21 Sm2 O25 136.16(15) . 2_765 ?
O25 Sm2 O25 77.6(2) 3_675 2_765 ?
O25 Sm2 O25 137.61(11) 6_677 2_765 ?
O25 Sm2 O25 87.4(3) 5_767 2_765 ?
O21 Sm2 O25 136.16(15) 3_675 4_557 ?
O21 Sm2 O25 71.6(2) 2_765 4_557 ?
O21 Sm2 O25 66.0(2) . 4_557 ?
O25 Sm2 O25 137.61(12) 3_675 4_557 ?
O25 Sm2 O25 77.6(2) 6_677 4_557 ?
O25 Sm2 O25 77.6(2) 5_767 4_557 ?
O25 Sm2 O25 137.60(11) 2_765 4_557 ?
O21 Sm2 O25 136.16(15) 3_675 . ?
O21 Sm2 O25 71.6(2) 2_765 . ?
O21 Sm2 O25 66.0(2) . . ?
O25 Sm2 O25 77.6(2) 3_675 . ?
O25 Sm2 O25 137.60(12) 6_677 . ?
O25 Sm2 O25 137.60(11) 5_767 . ?
O25 Sm2 O25 77.6(2) 2_765 . ?
O25 Sm2 O25 87.4(3) 4_557 . ?
O21 Sm2 Ti2 29.19(14) 3_675 6_677 ?
O21 Sm2 Ti2 130.9(2) 2_765 6_677 ?
O21 Sm2 Ti2 102.6(2) . 6_677 ?
O25 Sm2 Ti2 77.43(15) 3_675 6_677 ?
O25 Sm2 Ti2 37.44(16) 6_677 6_677 ?
O25 Sm2 Ti2 66.51(16) 5_767 6_677 ?
O25 Sm2 Ti2 100.24(16) 2_765 6_677 ?
O25 Sm2 Ti2 109.16(15) 4_557 6_677 ?
O25 Sm2 Ti2 154.75(16) . 6_677 ?
O21 Sm2 Ti2 29.19(14) 3_675 3_675 ?
O21 Sm2 Ti2 130.9(2) 2_765 3_675 ?
O21 Sm2 Ti2 102.6(2) . 3_675 ?
O25 Sm2 Ti2 37.44(16) 3_675 3_675 ?
O25 Sm2 Ti2 77.43(15) 6_677 3_675 ?
O25 Sm2 Ti2 100.24(16) 5_767 3_675 ?
O25 Sm2 Ti2 66.51(16) 2_765 3_675 ?
O25 Sm2 Ti2 154.75(16) 4_557 3_675 ?
O25 Sm2 Ti2 109.16(15) . 3_675 ?
Ti2 Sm2 Ti2 49.32(6) 6_677 3_675 ?
O21 Sm2 Ti2 130.9(2) 3_675 . ?
O21 Sm2 Ti2 102.6(3) 2_765 . ?
O21 Sm2 Ti2 29.19(14) . . ?
O25 Sm2 Ti2 66.51(16) 3_675 . ?
O25 Sm2 Ti2 100.23(16) 6_677 . ?
O25 Sm2 Ti2 154.75(16) 5_767 . ?
O25 Sm2 Ti2 109.16(15) 2_765 . ?
O25 Sm2 Ti2 77.43(16) 4_557 . ?
O25 Sm2 Ti2 37.44(16) . . ?
Ti2 Sm2 Ti2 125.947(13) 6_677 . ?
Ti2 Sm2 Ti2 103.82(3) 3_675 . ?
O3 Ti1 O4 94.9(3) . . ?
O3 Ti1 O1 104.4(4) . . ?
O4 Ti1 O1 160.0(4) . . ?
O3 Ti1 O2 98.1(4) . . ?
O4 Ti1 O2 96.6(3) . . ?
O1 Ti1 O2 75.9(3) . . ?
O3 Ti1 O5 90.7(3) . . ?
O4 Ti1 O5 94.4(3) . . ?
O1 Ti1 O5 90.5(3) . . ?
O2 Ti1 O5 165.3(3) . . ?
O3 Ti1 O6 170.2(3) . . ?
O4 Ti1 O6 82.2(3) . . ?
O1 Ti1 O6 79.5(3) . . ?
O2 Ti1 O6 91.6(3) . . ?
O5 Ti1 O6 80.2(3) . . ?
O3 Ti1 Ti1 91.1(2) . 4_556 ?
O4 Ti1 Ti1 138.3(2) . 4_556 ?
O1 Ti1 Ti1 38.2(2) . 4_556 ?
O2 Ti1 Ti1 41.7(2) . 4_556 ?
O5 Ti1 Ti1 126.9(2) . 4_556 ?
O6 Ti1 Ti1 97.27(16) . 4_556 ?
O3 Ti1 Sm1 136.8(3) . . ?
O4 Ti1 Sm1 127.1(2) . . ?
O1 Ti1 Sm1 35.7(2) . . ?
O2 Ti1 Sm1 87.6(2) . . ?
O5 Ti1 Sm1 77.9(2) . . ?
O6 Ti1 Sm1 44.84(16) . . ?
Ti1 Ti1 Sm1 65.33(3) 4_556 . ?
O23 Ti2 O24 94.5(4) . . ?
O23 Ti2 O21 103.4(4) . . ?
O24 Ti2 O21 161.7(4) . . ?
O23 Ti2 O22 96.9(4) . . ?
O24 Ti2 O22 97.6(4) . . ?
O21 Ti2 O22 77.0(3) . . ?
O23 Ti2 O26 91.5(4) . . ?
O24 Ti2 O26 93.8(4) . . ?
O21 Ti2 O26 89.2(4) . . ?
O22 Ti2 O26 165.2(3) . . ?
O23 Ti2 O25 171.0(3) . . ?
O24 Ti2 O25 81.4(3) . . ?
O21 Ti2 O25 81.3(4) . . ?
O22 Ti2 O25 91.6(4) . . ?
O26 Ti2 O25 80.8(3) . . ?
O23 Ti2 Ti2 91.1(2) . 4_557 ?
O24 Ti2 Ti2 139.2(2) . 4_557 ?
O21 Ti2 Ti2 38.5(2) . 4_557 ?
O22 Ti2 Ti2 41.6(2) . 4_557 ?
O26 Ti2 Ti2 126.4(3) . 4_557 ?
O25 Ti2 Ti2 97.18(17) . 4_557 ?
O23 Ti2 Sm2 137.8(3) . . ?
O24 Ti2 Sm2 126.5(3) . . ?
O21 Ti2 Sm2 37.0(3) . . ?
O22 Ti2 Sm2 87.9(3) . . ?
O26 Ti2 Sm2 77.7(3) . . ?
O25 Ti2 Sm2 45.16(16) . . ?
Ti2 Ti2 Sm2 65.34(3) 4_557 . ?
Ti1 O1 Ti1 103.7(4) 4_556 . ?
Ti1 O1 Sm1 115.8(3) 4_556 . ?
Ti1 O1 Sm1 115.8(3) . . ?
C2 O2 Ti1 130.4(3) . . ?
C2 O2 Ti1 130.4(3) . 4_556 ?
Ti1 O2 Ti1 96.7(4) . 4_556 ?
C3' O3 Ti1 166.9(12) . . ?
C3 O3 Ti1 137.5(11) . . ?
C11 O4 Ti1 140.6(7) . . ?
C17 O5 Ti1 138.1(8) . . ?
C17 O6 Ti1 130.9(7) 3_665 . ?
C17 O6 Sm1 130.6(7) 3_665 . ?
Ti1 O6 Sm1 98.2(2) . . ?
Ti2 O21 Ti2 102.9(5) . 4_557 ?
Ti2 O21 Sm2 113.9(4) . . ?
Ti2 O21 Sm2 113.9(4) 4_557 . ?
C22 O22 Ti2 130.3(3) . 4_557 ?
C22 O22 Ti2 130.3(3) . . ?
Ti2 O22 Ti2 96.8(5) 4_557 . ?
C23' O23 Ti2 169.4(13) . . ?
C23 O23 Ti2 131.2(12) . . ?
C31 O24 Ti2 141.2(7) . . ?
C37 O25 Ti2 131.0(7) 2_765 . ?
C37 O25 Sm2 131.2(7) 2_765 . ?
Ti2 O25 Sm2 97.4(2) . . ?
C37 O26 Ti2 138.3(10) . . ?
C2A C2 O2 110.9(16) . . ?
C2A C2 C2B 135(2) . . ?
O2 C2 C2B 111.9(17) . . ?
C2A C2 H2A 94.5 . . ?
O2 C2 H2A 94.5 . . ?
C2B C2 H2A 94.5 . . ?
C2 C2A H2AA 109.5 . . ?
C2 C2A H2AB 109.5 . . ?
H2AA C2A H2AB 109.5 . . ?
C2 C2A H2AC 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
C2 C2B H2BA 109.5 . . ?
C2 C2B H2BB 109.5 . . ?
H2BA C2B H2BB 109.5 . . ?
C2 C2B H2BC 109.5 . . ?
H2BA C2B H2BC 109.5 . . ?
H2BB C2B H2BC 109.5 . . ?
C3B C3 O3 109.5(17) . . ?
C3B C3 C3A 113(2) . . ?
O3 C3 C3A 111.1(18) . . ?
C3B C3 H3 107.8 . . ?
O3 C3 H3 107.8 . . ?
C3A C3 H3 107.8 . . ?
C3 C3A H3AA 109.5 . . ?
C3 C3A H3AB 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
C3 C3A H3AC 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
C3 C3B H3BA 109.5 . . ?
C3 C3B H3BB 109.5 . . ?
H3BA C3B H3BB 109.5 . . ?
C3 C3B H3BC 109.5 . . ?
H3BA C3B H3BC 109.5 . . ?
H3BB C3B H3BC 109.5 . . ?
O3 C3' C3B' 120(2) . . ?
O3 C3' C3A' 111(2) . . ?
C3B' C3' C3A' 115(2) . . ?
O3 C3' H3A' 102.6 . . ?
C3B' C3' H3A' 102.6 . . ?
C3A' C3' H3A' 102.6 . . ?
C3' C3A' H3AD 109.5 . . ?
C3' C3A' H3AE 109.5 . . ?
H3AD C3A' H3AE 109.5 . . ?
C3' C3A' H3AF 109.5 . . ?
H3AD C3A' H3AF 109.5 . . ?
H3AE C3A' H3AF 109.5 . . ?
C3' C3B' H3BD 109.5 . . ?
C3' C3B' H3BE 109.5 . . ?
H3BD C3B' H3BE 109.5 . . ?
C3' C3B' H3BF 109.5 . . ?
H3BD C3B' H3BF 109.5 . . ?
H3BE C3B' H3BF 109.5 . . ?
O4 C11 C12 119.6(11) . . ?
O4 C11 C16 121.4(10) . . ?
C12 C11 C16 118.8(12) . . ?
C13 C12 C11 120.8(14) . . ?
C13 C12 H12A 119.6 . . ?
C11 C12 H12A 119.6 . . ?
C14 C13 C12 122.4(14) . . ?
C14 C13 H13A 118.8 . . ?
C12 C13 H13A 118.8 . . ?
C13 C14 C15 119.7(15) . . ?
C13 C14 H14A 120.1 . . ?
C15 C14 H14A 120.1 . . ?
C14 C15 C16 119.6(13) . . ?
C14 C15 H15A 120.2 . . ?
C16 C15 H15A 120.2 . . ?
C15 C16 C11 118.6(11) . . ?
C15 C16 C17 119.0(11) . 3_665 ?
C11 C16 C17 122.4(10) . 3_665 ?
O5 C17 O6 121.8(11) . 2_655 ?
O5 C17 C16 116.1(10) . 2_655 ?
O6 C17 C16 122.1(10) 2_655 2_655 ?
C22B C22 O22 111(2) . . ?
C22B C22 C22A 134(3) . . ?
O22 C22 C22A 106(2) . . ?
C22B C22 H22' 99.5 . . ?
O22 C22 H22' 99.5 . . ?
C22A C22 H22' 99.5 . . ?
C22 C22A H22A 109.5 . . ?
C22 C22A H22B 109.5 . . ?
H22A C22A H22B 109.5 . . ?
C22 C22A H22C 109.5 . . ?
H22A C22A H22C 109.5 . . ?
H22B C22A H22C 109.5 . . ?
C22 C22B H22D 109.5 . . ?
C22 C22B H22E 109.5 . . ?
H22D C22B H22E 109.5 . . ?
C22 C22B H22F 109.5 . . ?
H22D C22B H22F 109.5 . . ?
H22E C22B H22F 109.5 . . ?
C23A C23 O23 111(2) . . ?
C23A C23 C23B 109(2) . . ?
O23 C23 C23B 109(2) . . ?
C23A C23 H23A 109.6 . . ?
O23 C23 H23A 109.6 . . ?
C23B C23 H23A 109.6 . . ?
C23 C23A H23B 109.5 . . ?
C23 C23A H23C 109.5 . . ?
H23B C23A H23C 109.5 . . ?
C23 C23A H23D 109.5 . . ?
H23B C23A H23D 109.5 . . ?
H23C C23A H23D 109.5 . . ?
C23 C23B H23E 109.5 . . ?
C23 C23B H23F 109.5 . . ?
H23E C23B H23F 109.5 . . ?
C23 C23B H23G 109.5 . . ?
H23E C23B H23G 109.5 . . ?
H23F C23B H23G 109.5 . . ?
C23C C23' O23 101(2) . . ?
C23C C23' C23D 112(2) . . ?
O23 C23' C23D 114(2) . . ?
C23C C23' H23H 110.0 . . ?
O23 C23' H23H 110.0 . . ?
C23D C23' H23H 110.0 . . ?
C23' C23C H23I 109.5 . . ?
C23' C23C H23J 109.5 . . ?
H23I C23C H23J 109.5 . . ?
C23' C23C H23K 109.5 . . ?
H23I C23C H23K 109.5 . . ?
H23J C23C H23K 109.5 . . ?
C23' C23D H23L 109.5 . . ?
C23' C23D H23M 109.5 . . ?
H23L C23D H23M 109.5 . . ?
C23' C23D H23N 109.5 . . ?
H23L C23D H23N 109.5 . . ?
H23M C23D H23N 109.5 . . ?
O24 C31 C32 119.7(12) . . ?
O24 C31 C36 121.4(10) . . ?
C32 C31 C36 118.9(12) . . ?
C33 C32 C31 121.0(14) . . ?
C33 C32 H32A 119.5 . . ?
C31 C32 H32A 119.5 . . ?
C34 C33 C32 121.2(13) . . ?
C34 C33 H33A 119.4 . . ?
C32 C33 H33A 119.4 . . ?
C33 C34 C35 118.6(14) . . ?
C33 C34 H34A 120.7 . . ?
C35 C34 H34A 120.7 . . ?
C36 C35 C34 121.1(14) . . ?
C36 C35 H35A 119.5 . . ?
C34 C35 H35A 119.5 . . ?
C35 C36 C31 119.1(11) . . ?
C35 C36 C37 118.3(11) . 2_765 ?
C31 C36 C37 122.5(10) . 2_765 ?
O26 C37 O25 121.9(12) . 3_675 ?
O26 C37 C36 115.8(11) . 3_675 ?
O25 C37 C36 122.4(10) 3_675 3_675 ?

_refine_diff_density_max         3.028
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.086



####################################################################### 
# 
# 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_eu1_a
_database_code_depnum_ccdc_archive 'CCDC 1504165'
_audit_update_record             
;
2017-02-27 deposited with the CCDC.
2017-03-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C69 H87 Eu O30 Ti6'
_chemical_formula_sum            'C69 H87 Eu O30 Ti6'
_chemical_formula_weight         1835.74

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -8.9294 11.1857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

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

_cell_length_a                   14.9147(4)
_cell_length_b                   22.5136(6)
_cell_length_c                   25.0990(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8427.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9960
_cell_measurement_theta_min      2.64
_cell_measurement_theta_max      72.28

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_F_000             3744
_exptl_transmission_factor_min   0.649
_exptl_transmission_factor_max   1.000
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.170
_exptl_absorpt_coefficient_mu    10.479
_shelx_estimated_absorpt_T_min   0.188
_shelx_estimated_absorpt_T_max   0.269
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.188
_exptl_absorpt_correction_T_max  0.269
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements (SADABS) 
;
_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         '30W microfocus sealed tube, Quazar optics'
_diffrn_measurement_device_type  'Bruker QUEST D8 CCD'
_diffrn_measurement_method       'Thin slice ω and φ scans'
_diffrn_reflns_number            57628
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.636
_diffrn_reflns_theta_max         72.297
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8537
_reflns_number_gt                7327
_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 software package, narrow-frames'
_computing_cell_refinement       'refinement of XYZ centroids > 20sigma(I)'
_computing_data_reduction        
;
 Bruker SAINT software package, narrow frame algorithm
;
_computing_structure_solution    'SHELXT-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          
;
iso-propyl groups placed on mirror planes for ease, resulting in 
some odd looking groups. Formula confirmed by elemental analysis.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0427P)²+12.3905P] 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         8537
_refine_ls_number_parameters     559
_refine_ls_number_restraints     273
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0385
_refine_ls_wR_factor_ref         0.0971
_refine_ls_wR_factor_gt          0.0909
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.003
_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
Ti1 Ti 0.45106(4) 0.31640(3) 0.40159(2) 0.02903(14) Uani 1 1 d . . . . .
Ti2 Ti 0.10757(4) 0.31603(3) 0.49707(2) 0.02669(13) Uani 1 1 d . . . . .
Ti3 Ti 0.41702(4) 0.31611(3) 0.62455(2) 0.02676(13) Uani 1 1 d . . . . .
Eu01 Eu 0.32438(2) 0.2500 0.50736(2) 0.01803(7) Uani 1 2 d S T P . .
O1 O 0.44767(18) 0.31858(12) 0.33111(10) 0.0427(6) Uani 1 1 d . . . . .
O2 O 0.52286(16) 0.31850(12) 0.65580(10) 0.0411(6) Uani 1 1 d . . . . .
O3 O 0.00561(16) 0.31672(12) 0.53296(11) 0.0391(6) Uani 1 1 d . . . . .
O4 O 0.5396(2) 0.2500 0.40858(14) 0.0335(8) Uani 1 2 d S T P . .
O5 O 0.42541(18) 0.2500 0.57793(11) 0.0219(6) Uani 1 2 d S T P . .
O6 O 0.3634(2) 0.2500 0.66733(13) 0.0358(8) Uani 1 2 d S T P . .
O7 O 0.0770(2) 0.2500 0.44642(13) 0.0300(7) Uani 1 2 d S T P . .
O8 O 0.17087(18) 0.2500 0.52511(12) 0.0224(6) Uani 1 2 d S T P . .
O9 O 0.3781(2) 0.2500 0.42014(11) 0.0237(6) Uani 1 2 d S T P . .
O10 O 0.53458(17) 0.37860(12) 0.40805(10) 0.0404(6) Uani 1 1 d . . . . .
O11 O 0.45765(16) 0.37066(11) 0.56677(9) 0.0341(5) Uani 1 1 d . . . . .
O12 O 0.44124(14) 0.32942(10) 0.48735(9) 0.0269(5) Uani 1 1 d . . . . .
O20 O 0.36855(16) 0.37837(12) 0.66571(10) 0.0370(6) Uani 1 1 d . . . . .
O21 O 0.16542(15) 0.36966(11) 0.55190(9) 0.0319(5) Uani 1 1 d . . . . .
O22 O 0.29131(14) 0.32776(10) 0.58066(9) 0.0266(5) Uani 1 1 d . . . . .
O30 O 0.07313(16) 0.37914(11) 0.45213(10) 0.0361(6) Uani 1 1 d . . . . .
O31 O 0.34083(16) 0.36937(11) 0.40514(10) 0.0344(5) Uani 1 1 d . . . . .
O32 O 0.23659(14) 0.32964(10) 0.45748(9) 0.0252(5) Uani 1 1 d . . . . .
C1 C 0.4533(10) 0.3608(7) 0.2901(5) 0.079(4) Uani 0.504(18) 1 d . U P A 1
H1A H 0.4375 0.3998 0.3066 0.095 Uiso 0.504(18) 1 calc R U P A 1
C1B C 0.3890(15) 0.3506(8) 0.2497(5) 0.102(6) Uani 0.504(18) 1 d . U P A 1
H1BA H 0.3952 0.3810 0.2219 0.153 Uiso 0.504(18) 1 calc R U P A 1
H1BB H 0.3986 0.3112 0.2341 0.153 Uiso 0.504(18) 1 calc R U P A 1
H1BC H 0.3286 0.3526 0.2650 0.153 Uiso 0.504(18) 1 calc R U P A 1
C1A C 0.5464(15) 0.3669(10) 0.2703(7) 0.132(8) Uani 0.504(18) 1 d . U P A 1
H1AA H 0.5481 0.3966 0.2418 0.198 Uiso 0.504(18) 1 calc R U P A 1
H1AB H 0.5855 0.3795 0.2995 0.198 Uiso 0.504(18) 1 calc R U P A 1
H1AC H 0.5671 0.3286 0.2564 0.198 Uiso 0.504(18) 1 calc R U P A 1
C1' C 0.4341(10) 0.3247(8) 0.2771(5) 0.079(4) Uani 0.496(18) 1 d . U P A 2
H1'A H 0.4638 0.2916 0.2573 0.095 Uiso 0.496(18) 1 calc R U P A 2
C1B' C 0.3331(14) 0.3254(11) 0.2654(9) 0.133(8) Uani 0.496(18) 1 d . U P A 2
H1BD H 0.3235 0.3298 0.2270 0.200 Uiso 0.496(18) 1 calc R U P A 2
H1BE H 0.3062 0.2881 0.2776 0.200 Uiso 0.496(18) 1 calc R U P A 2
H1BF H 0.3052 0.3588 0.2841 0.200 Uiso 0.496(18) 1 calc R U P A 2
C1A' C 0.4809(19) 0.3854(10) 0.2640(10) 0.164(9) Uani 0.496(18) 1 d . U P A 2
H1AD H 0.4748 0.3939 0.2259 0.246 Uiso 0.496(18) 1 calc R U P A 2
H1AE H 0.4525 0.4172 0.2846 0.246 Uiso 0.496(18) 1 calc R U P A 2
H1AF H 0.5446 0.3830 0.2733 0.246 Uiso 0.496(18) 1 calc R U P A 2
C3 C -0.0610(4) 0.3497(4) 0.5568(3) 0.109(2) Uani 1 1 d . U . . .
H3A H -0.0288 0.3887 0.5577 0.131 Uiso 1 1 calc R U . . .
C3B C -0.0657(5) 0.3395(3) 0.6145(3) 0.107(3) Uani 1 1 d . U . . .
H3BA H -0.1138 0.3638 0.6298 0.161 Uiso 1 1 calc R U . . .
H3BB H -0.0781 0.2975 0.6214 0.161 Uiso 1 1 calc R U . . .
H3BC H -0.0085 0.3505 0.6309 0.161 Uiso 1 1 calc R U . . .
C3A C -0.1331(5) 0.3671(4) 0.5260(4) 0.146(4) Uani 1 1 d . U . . .
H3AA H -0.1750 0.3901 0.5479 0.218 Uiso 1 1 calc R U . . .
H3AB H -0.1118 0.3917 0.4964 0.218 Uiso 1 1 calc R U . . .
H3AC H -0.1636 0.3319 0.5119 0.218 Uiso 1 1 calc R U . . .
C4 C 0.6373(4) 0.2500 0.4013(3) 0.0587(17) Uani 1 2 d S TU P . .
H4A H 0.6373 0.2056 0.4013 0.070 Uiso 0.5 1 calc R U P B -1
C4A C 0.6806(6) 0.2500 0.4519(5) 0.135(5) Uani 1 2 d S TU P . .
H4AA H 0.6354 0.2500 0.4802 0.203 Uiso 0.5 1 calc R U P C -1
H4AB H 0.7182 0.2145 0.4551 0.203 Uiso 0.5 1 calc R U P C -1
H4AC H 0.7182 0.2855 0.4551 0.203 Uiso 0.5 1 calc R U P C -1
C4B C 0.6632(7) 0.2500 0.3499(6) 0.206(7) Uani 1 2 d S TU P . .
H4BA H 0.6102 0.2500 0.3269 0.309 Uiso 0.5 1 calc R U P D -1
H4BB H 0.6992 0.2855 0.3428 0.309 Uiso 0.5 1 calc R U P D -1
H4BC H 0.6992 0.2145 0.3428 0.309 Uiso 0.5 1 calc R U P D -1
C6 C 0.3110(6) 0.2500 0.7161(3) 0.079(2) Uani 1 2 d S TU P . .
H6A H 0.3110 0.2944 0.7161 0.095 Uiso 0.5 1 calc R U P E -1
C6A C 0.2156(6) 0.2500 0.7030(4) 0.133(5) Uani 1 2 d S TU P . .
H6AA H 0.2082 0.2500 0.6642 0.199 Uiso 0.5 1 calc R U P F -1
H6AB H 0.1872 0.2145 0.7180 0.199 Uiso 0.5 1 calc R U P F -1
H6AC H 0.1872 0.2855 0.7180 0.199 Uiso 0.5 1 calc R U P F -1
C6B C 0.3587(11) 0.2500 0.7593(4) 0.183(7) Uani 1 2 d S TU P . .
H6BA H 0.3189 0.2500 0.7903 0.274 Uiso 0.5 1 calc R U P G -1
H6BB H 0.3966 0.2145 0.7601 0.274 Uiso 0.5 1 calc R U P G -1
H6BC H 0.3966 0.2855 0.7601 0.274 Uiso 0.5 1 calc R U P G -1
C7 C 0.0285(4) 0.2500 0.3967(2) 0.0562(17) Uani 1 2 d S TU P . .
H7A H 0.0285 0.2056 0.3967 0.067 Uiso 0.5 1 calc R U P H -1
C7B C 0.0904(7) 0.2500 0.3524(3) 0.114(4) Uani 1 2 d S TU P . .
H7BA H 0.1521 0.2500 0.3660 0.171 Uiso 0.5 1 calc R U P I -1
H7BB H 0.0806 0.2145 0.3307 0.171 Uiso 0.5 1 calc R U P I -1
H7BC H 0.0806 0.2855 0.3307 0.171 Uiso 0.5 1 calc R U P I -1
C7A C -0.0600(7) 0.2500 0.4000(5) 0.181(6) Uani 1 2 d S TU P . .
H7AA H -0.0858 0.2500 0.3641 0.271 Uiso 0.5 1 calc R U P J -1
H7AB H -0.0799 0.2145 0.4192 0.271 Uiso 0.5 1 calc R U P J -1
H7AC H -0.0799 0.2855 0.4192 0.271 Uiso 0.5 1 calc R U P J -1
C11 C 0.5711(2) 0.41288(17) 0.44521(16) 0.0380(8) Uani 1 1 d . U . . .
C12 C 0.6395(3) 0.4522(2) 0.4302(2) 0.0580(12) Uani 1 1 d . U . . .
H12A H 0.6595 0.4535 0.3943 0.070 Uiso 1 1 calc R U . . .
C13 C 0.6774(4) 0.4888(2) 0.4677(2) 0.0754(17) Uani 1 1 d . U . . .
H13A H 0.7241 0.5151 0.4574 0.090 Uiso 1 1 calc R U . . .
C14 C 0.6494(4) 0.4883(3) 0.5196(2) 0.0801(18) Uani 1 1 d . U . . .
H14A H 0.6757 0.5145 0.5447 0.096 Uiso 1 1 calc R U . . .
C15 C 0.5830(3) 0.4496(2) 0.53525(19) 0.0571(12) Uani 1 1 d . U . . .
H15A H 0.5638 0.4493 0.5713 0.068 Uiso 1 1 calc R U . . .
C16 C 0.5435(2) 0.41070(16) 0.49854(14) 0.0347(8) Uani 1 1 d . U . . .
C17 C 0.4769(2) 0.36787(15) 0.51775(14) 0.0282(7) Uani 1 1 d . U . . .
C21 C 0.3008(2) 0.41556(16) 0.66481(14) 0.0336(8) Uani 1 1 d . U . . .
C22 C 0.2999(3) 0.46136(19) 0.70240(16) 0.0458(10) Uani 1 1 d . U . . .
H22A H 0.3477 0.4647 0.7273 0.055 Uiso 1 1 calc R U . . .
C23 C 0.2304(3) 0.5018(2) 0.70370(19) 0.0604(13) Uani 1 1 d . U . . .
H23A H 0.2306 0.5328 0.7293 0.072 Uiso 1 1 calc R U . . .
C24 C 0.1608(3) 0.4971(2) 0.6679(2) 0.0596(13) Uani 1 1 d . U . . .
H24A H 0.1125 0.5246 0.6693 0.072 Uiso 1 1 calc R U . . .
C25 C 0.1611(3) 0.45284(19) 0.63034(17) 0.0446(10) Uani 1 1 d . U . . .
H25A H 0.1131 0.4504 0.6055 0.054 Uiso 1 1 calc R U . . .
C26 C 0.2305(2) 0.41137(16) 0.62786(14) 0.0321(7) Uani 1 1 d . U . . .
C27 C 0.2298(2) 0.36641(15) 0.58475(13) 0.0274(7) Uani 1 1 d . U . . .
C31 C 0.1086(2) 0.41515(16) 0.41674(14) 0.0350(8) Uani 1 1 d . U . . .
C32 C 0.0535(3) 0.45865(19) 0.39382(17) 0.0480(10) Uani 1 1 d . U . . .
H32A H -0.0078 0.4609 0.4039 0.058 Uiso 1 1 calc R U . . .
C33 C 0.0865(3) 0.4979(2) 0.35721(19) 0.0558(12) Uani 1 1 d . U . . .
H33A H 0.0480 0.5269 0.3421 0.067 Uiso 1 1 calc R U . . .
C34 C 0.1756(3) 0.4957(2) 0.34187(18) 0.0549(11) Uani 1 1 d . U . . .
H34A H 0.1985 0.5235 0.3169 0.066 Uiso 1 1 calc R U . . .
C35 C 0.2309(3) 0.45266(17) 0.36343(15) 0.0416(9) Uani 1 1 d . U . . .
H35A H 0.2919 0.4508 0.3527 0.050 Uiso 1 1 calc R U . . .
C36 C 0.1986(2) 0.41190(15) 0.40065(13) 0.0304(7) Uani 1 1 d . U . . .
C37 C 0.2616(2) 0.36736(14) 0.42280(13) 0.0266(7) Uani 1 1 d . U . . .
C2 C 0.5725(6) 0.3664(5) 0.6814(4) 0.077(3) Uani 0.585(7) 1 d D U P K 1
H2A H 0.5480 0.4041 0.6662 0.093 Uiso 0.585(7) 1 calc R U P K 1
C2A C 0.6683(12) 0.3609(12) 0.6597(8) 0.105(7) Uani 0.585(7) 1 d D U P K 1
H2AA H 0.6665 0.3582 0.6208 0.157 Uiso 0.585(7) 1 calc R U P K 1
H2AB H 0.7032 0.3959 0.6703 0.157 Uiso 0.585(7) 1 calc R U P K 1
H2AC H 0.6965 0.3251 0.6743 0.157 Uiso 0.585(7) 1 calc R U P K 1
C2B C 0.5605(8) 0.3709(6) 0.7374(4) 0.108(5) Uani 0.585(7) 1 d D U P K 1
H2BA H 0.5962 0.4041 0.7511 0.162 Uiso 0.585(7) 1 calc R U P K 1
H2BB H 0.4970 0.3777 0.7453 0.162 Uiso 0.585(7) 1 calc R U P K 1
H2BC H 0.5801 0.3339 0.7544 0.162 Uiso 0.585(7) 1 calc R U P K 1
C2' C 0.6193(7) 0.3091(6) 0.6586(5) 0.064(3) Uani 0.415(7) 1 d . U P K 2
H2'A H 0.6321 0.2761 0.6842 0.076 Uiso 0.415(7) 1 calc R U P K 2
C2B' C 0.6580(9) 0.2924(7) 0.6028(6) 0.085(4) Uani 0.415(7) 1 d . U P K 2
H2BD H 0.7228 0.2863 0.6057 0.127 Uiso 0.415(7) 1 calc R U P K 2
H2BE H 0.6295 0.2558 0.5902 0.127 Uiso 0.415(7) 1 calc R U P K 2
H2BF H 0.6458 0.3247 0.5776 0.127 Uiso 0.415(7) 1 calc R U P K 2
C2A' C 0.6535(19) 0.3667(16) 0.6815(11) 0.101(9) Uani 0.415(7) 1 d . U P K 2
H2AD H 0.7189 0.3648 0.6850 0.151 Uiso 0.415(7) 1 calc R U P K 2
H2AE H 0.6372 0.3995 0.6578 0.151 Uiso 0.415(7) 1 calc R U P K 2
H2AF H 0.6266 0.3732 0.7166 0.151 Uiso 0.415(7) 1 calc R U P K 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O1 1.770(3) . ?
Ti1 O10 1.881(3) . ?
Ti1 O9 1.9066(19) . ?
Ti1 O4 2.002(2) . ?
Ti1 O31 2.033(2) . ?
Ti1 O12 2.177(2) . ?
Ti1 Ti1 2.9897(12) 7_565 ?
Ti1 Eu01 3.5850(6) . ?
Ti2 O3 1.767(2) . ?
Ti2 O30 1.885(2) . ?
Ti2 O8 1.8965(18) . ?
Ti2 O7 2.008(2) . ?
Ti2 O21 2.024(2) . ?
Ti2 O32 2.187(2) . ?
Ti2 Ti2 2.9732(12) 7_565 ?
Ti2 Eu01 3.5685(6) . ?
Ti3 O2 1.764(2) . ?
Ti3 O20 1.885(2) . ?
Ti3 O5 1.8974(18) . ?
Ti3 O11 1.995(2) . ?
Ti3 O6 2.002(2) . ?
Ti3 O22 2.190(2) . ?
Ti3 Ti3 2.9767(12) 7_565 ?
Ti3 Eu01 3.5742(6) . ?
Eu01 O5 2.325(3) . ?
Eu01 O9 2.331(3) . ?
Eu01 O8 2.333(3) . ?
Eu01 O12 2.547(2) 7_565 ?
Eu01 O12 2.547(2) . ?
Eu01 O32 2.549(2) 7_565 ?
Eu01 O32 2.549(2) . ?
Eu01 O22 2.587(2) . ?
Eu01 O22 2.587(2) 7_565 ?
Eu01 Ti2 3.5685(6) 7_565 ?
O1 C1' 1.377(12) . ?
O1 C1 1.402(11) . ?
O2 C2' 1.456(11) . ?
O2 C2 1.458(10) . ?
O3 C3 1.377(6) . ?
O4 C4 1.469(6) . ?
O4 Ti1 2.003(2) 7_565 ?
O5 Ti3 1.8974(18) 7_565 ?
O6 C6 1.453(8) . ?
O6 Ti3 2.002(2) 7_565 ?
O7 C7 1.443(6) . ?
O7 Ti2 2.008(2) 7_565 ?
O8 Ti2 1.8966(18) 7_565 ?
O9 Ti1 1.9066(19) 7_565 ?
O10 C11 1.327(5) . ?
O11 C17 1.265(4) . ?
O12 C17 1.270(4) . ?
O20 C21 1.313(4) . ?
O21 C27 1.267(4) . ?
O22 C27 1.269(4) . ?
O30 C31 1.314(4) . ?
O31 C37 1.263(4) . ?
O32 C37 1.272(4) . ?
C1 C1B 1.42(2) . ?
C1 C1A 1.48(2) . ?
C1 H1A 1.0000 . ?
C1B H1BA 0.9800 . ?
C1B H1BB 0.9800 . ?
C1B H1BC 0.9800 . ?
C1A H1AA 0.9800 . ?
C1A H1AB 0.9800 . ?
C1A H1AC 0.9800 . ?
C1' C1B' 1.53(2) . ?
C1' C1A' 1.57(3) . ?
C1' H1'A 1.0000 . ?
C1B' H1BD 0.9800 . ?
C1B' H1BE 0.9800 . ?
C1B' H1BF 0.9800 . ?
C1A' H1AD 0.9800 . ?
C1A' H1AE 0.9800 . ?
C1A' H1AF 0.9800 . ?
C3 C3A 1.382(9) . ?
C3 C3B 1.468(9) . ?
C3 H3A 1.0000 . ?
C3B H3BA 0.9800 . ?
C3B H3BB 0.9800 . ?
C3B H3BC 0.9800 . ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?
C3A H3AC 0.9800 . ?
C4 C4B 1.345(14) . ?
C4 C4A 1.425(12) . ?
C4 H4A 1.0000 . ?
C4A H4AA 0.9800 . ?
C4A H4AB 0.9800 . ?
C4A H4AC 0.9800 . ?
C4B H4BA 0.9800 . ?
C4B H4BB 0.9800 . ?
C4B H4BC 0.9800 . ?
C6 C6B 1.295(14) . ?
C6 C6A 1.462(13) . ?
C6 H6A 1.0000 . ?
C6A H6AA 0.9800 . ?
C6A H6AB 0.9800 . ?
C6A H6AC 0.9800 . ?
C6B H6BA 0.9800 . ?
C6B H6BB 0.9800 . ?
C6B H6BC 0.9800 . ?
C7 C7A 1.323(12) . ?
C7 C7B 1.445(11) . ?
C7 H7A 1.0000 . ?
C7B H7BA 0.9800 . ?
C7B H7BB 0.9800 . ?
C7B H7BC 0.9800 . ?
C7A H7AA 0.9800 . ?
C7A H7AB 0.9800 . ?
C7A H7AC 0.9800 . ?
C11 C16 1.401(5) . ?
C11 C12 1.403(5) . ?
C12 C13 1.372(7) . ?
C12 H12A 0.9500 . ?
C13 C14 1.367(8) . ?
C13 H13A 0.9500 . ?
C14 C15 1.376(6) . ?
C14 H14A 0.9500 . ?
C15 C16 1.401(5) . ?
C15 H15A 0.9500 . ?
C16 C17 1.467(5) . ?
C21 C22 1.398(5) . ?
C21 C26 1.402(5) . ?
C22 C23 1.380(6) . ?
C22 H22A 0.9500 . ?
C23 C24 1.377(6) . ?
C23 H23A 0.9500 . ?
C24 C25 1.372(6) . ?
C24 H24A 0.9500 . ?
C25 C26 1.396(5) . ?
C25 H25A 0.9500 . ?
C26 C27 1.482(5) . ?
C31 C32 1.402(5) . ?
C31 C36 1.403(5) . ?
C32 C33 1.367(6) . ?
C32 H32A 0.9500 . ?
C33 C34 1.384(7) . ?
C33 H33A 0.9500 . ?
C34 C35 1.384(6) . ?
C34 H34A 0.9500 . ?
C35 C36 1.395(5) . ?
C35 H35A 0.9500 . ?
C36 C37 1.482(4) . ?
C2 C2B 1.419(13) . ?
C2 C2A 1.534(18) . ?
C2 H2A 1.0000 . ?
C2A H2AA 0.9800 . ?
C2A H2AB 0.9800 . ?
C2A H2AC 0.9800 . ?
C2B H2BA 0.9800 . ?
C2B H2BB 0.9800 . ?
C2B H2BC 0.9800 . ?
C2' C2A' 1.51(3) . ?
C2' C2B' 1.559(19) . ?
C2' H2'A 1.0000 . ?
C2B' C2B' 1.91(3) 7_565 ?
C2B' H2BD 0.9800 . ?
C2B' H2BE 0.9800 . ?
C2B' H2BF 0.9800 . ?
C2A' H2AD 0.9800 . ?
C2A' H2AE 0.9800 . ?
C2A' H2AF 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 Ti1 O10 94.84(12) . . ?
O1 Ti1 O9 104.45(13) . . ?
O10 Ti1 O9 160.13(12) . . ?
O1 Ti1 O4 97.30(14) . . ?
O10 Ti1 O4 96.39(11) . . ?
O9 Ti1 O4 76.69(10) . . ?
O1 Ti1 O31 90.26(12) . . ?
O10 Ti1 O31 95.45(11) . . ?
O9 Ti1 O31 89.30(10) . . ?
O4 Ti1 O31 165.34(10) . . ?
O1 Ti1 O12 169.16(11) . . ?
O10 Ti1 O12 81.90(10) . . ?
O9 Ti1 O12 79.97(10) . . ?
O4 Ti1 O12 93.34(12) . . ?
O31 Ti1 O12 79.82(9) . . ?
O1 Ti1 Ti1 91.59(9) . 7_565 ?
O10 Ti1 Ti1 138.11(9) . 7_565 ?
O9 Ti1 Ti1 38.37(7) . 7_565 ?
O4 Ti1 Ti1 41.71(7) . 7_565 ?
O31 Ti1 Ti1 125.92(7) . 7_565 ?
O12 Ti1 Ti1 97.74(6) . 7_565 ?
O1 Ti1 Eu01 137.43(9) . . ?
O10 Ti1 Eu01 126.55(8) . . ?
O9 Ti1 Eu01 36.05(8) . . ?
O4 Ti1 Eu01 88.36(9) . . ?
O31 Ti1 Eu01 77.64(7) . . ?
O12 Ti1 Eu01 44.65(6) . . ?
Ti1 Ti1 Eu01 65.357(10) 7_565 . ?
O3 Ti2 O30 93.66(12) . . ?
O3 Ti2 O8 104.25(13) . . ?
O30 Ti2 O8 161.50(12) . . ?
O3 Ti2 O7 97.70(13) . . ?
O30 Ti2 O7 96.74(11) . . ?
O8 Ti2 O7 76.56(10) . . ?
O3 Ti2 O21 90.86(11) . . ?
O30 Ti2 O21 94.20(11) . . ?
O8 Ti2 O21 90.17(10) . . ?
O7 Ti2 O21 165.62(10) . . ?
O3 Ti2 O32 170.82(11) . . ?
O30 Ti2 O32 82.09(9) . . ?
O8 Ti2 O32 80.82(10) . . ?
O7 Ti2 O32 90.90(11) . . ?
O21 Ti2 O32 81.39(9) . . ?
O3 Ti2 Ti2 90.51(9) . 7_565 ?
O30 Ti2 Ti2 138.90(8) . 7_565 ?
O8 Ti2 Ti2 38.39(7) . 7_565 ?
O7 Ti2 Ti2 42.25(7) . 7_565 ?
O21 Ti2 Ti2 126.63(7) . 7_565 ?
O32 Ti2 Ti2 98.05(6) . 7_565 ?
O3 Ti2 Eu01 138.28(9) . . ?
O30 Ti2 Eu01 127.17(8) . . ?
O8 Ti2 Eu01 36.43(8) . . ?
O7 Ti2 Eu01 86.73(8) . . ?
O21 Ti2 Eu01 79.22(6) . . ?
O32 Ti2 Eu01 45.09(6) . . ?
Ti2 Ti2 Eu01 65.381(10) 7_565 . ?
O2 Ti3 O20 94.41(12) . . ?
O2 Ti3 O5 103.84(12) . . ?
O20 Ti3 O5 161.15(12) . . ?
O2 Ti3 O11 91.87(12) . . ?
O20 Ti3 O11 93.27(11) . . ?
O5 Ti3 O11 90.84(10) . . ?
O2 Ti3 O6 98.14(14) . . ?
O20 Ti3 O6 96.07(11) . . ?
O5 Ti3 O6 76.93(10) . . ?
O11 Ti3 O6 165.72(11) . . ?
O2 Ti3 O22 170.49(12) . . ?
O20 Ti3 O22 81.85(9) . . ?
O5 Ti3 O22 80.81(10) . . ?
O11 Ti3 O22 79.67(9) . . ?
O6 Ti3 O22 90.98(12) . . ?
O2 Ti3 Ti3 91.75(9) . 7_565 ?
O20 Ti3 Ti3 138.03(8) . 7_565 ?
O5 Ti3 Ti3 38.33(7) . 7_565 ?
O11 Ti3 Ti3 128.01(7) . 7_565 ?
O6 Ti3 Ti3 41.97(7) . 7_565 ?
O22 Ti3 Ti3 96.88(6) . 7_565 ?
O2 Ti3 Eu01 136.44(9) . . ?
O20 Ti3 Eu01 127.75(7) . . ?
O5 Ti3 Eu01 36.04(8) . . ?
O11 Ti3 Eu01 77.03(7) . . ?
O6 Ti3 Eu01 88.71(9) . . ?
O22 Ti3 Eu01 45.98(6) . . ?
Ti3 Ti3 Eu01 65.392(10) 7_565 . ?
O5 Eu01 O9 119.51(10) . . ?
O5 Eu01 O8 119.38(10) . . ?
O9 Eu01 O8 121.11(10) . . ?
O5 Eu01 O12 72.95(7) . 7_565 ?
O9 Eu01 O12 65.14(7) . 7_565 ?
O8 Eu01 O12 135.18(5) . 7_565 ?
O5 Eu01 O12 72.95(7) . . ?
O9 Eu01 O12 65.14(7) . . ?
O8 Eu01 O12 135.18(5) . . ?
O12 Eu01 O12 89.18(10) 7_565 . ?
O5 Eu01 O32 134.99(5) . 7_565 ?
O9 Eu01 O32 73.45(7) . 7_565 ?
O8 Eu01 O32 65.77(7) . 7_565 ?
O12 Eu01 O32 76.16(7) 7_565 7_565 ?
O12 Eu01 O32 138.46(7) . 7_565 ?
O5 Eu01 O32 134.99(5) . . ?
O9 Eu01 O32 73.46(7) . . ?
O8 Eu01 O32 65.77(7) . . ?
O12 Eu01 O32 138.46(7) 7_565 . ?
O12 Eu01 O32 76.16(7) . . ?
O32 Eu01 O32 89.40(10) 7_565 . ?
O5 Eu01 O22 65.29(7) . . ?
O9 Eu01 O22 137.16(5) . . ?
O8 Eu01 O22 71.16(7) . . ?
O12 Eu01 O22 138.23(7) 7_565 . ?
O12 Eu01 O22 78.21(7) . . ?
O32 Eu01 O22 136.67(7) 7_565 . ?
O32 Eu01 O22 77.02(7) . . ?
O5 Eu01 O22 65.29(7) . 7_565 ?
O9 Eu01 O22 137.16(5) . 7_565 ?
O8 Eu01 O22 71.16(7) . 7_565 ?
O12 Eu01 O22 78.21(7) 7_565 7_565 ?
O12 Eu01 O22 138.23(7) . 7_565 ?
O32 Eu01 O22 77.02(7) 7_565 7_565 ?
O32 Eu01 O22 136.67(7) . 7_565 ?
O22 Eu01 O22 85.18(10) . 7_565 ?
O5 Eu01 Ti2 129.97(6) . . ?
O9 Eu01 Ti2 104.09(7) . . ?
O8 Eu01 Ti2 28.87(4) . . ?
O12 Eu01 Ti2 153.93(5) 7_565 . ?
O12 Eu01 Ti2 108.26(5) . . ?
O32 Eu01 Ti2 77.99(5) 7_565 . ?
O32 Eu01 Ti2 37.43(5) . . ?
O22 Eu01 Ti2 66.22(5) . . ?
O22 Eu01 Ti2 99.24(5) 7_565 . ?
O5 Eu01 Ti2 129.97(6) . 7_565 ?
O9 Eu01 Ti2 104.09(7) . 7_565 ?
O8 Eu01 Ti2 28.87(4) . 7_565 ?
O12 Eu01 Ti2 108.26(5) 7_565 7_565 ?
O12 Eu01 Ti2 153.93(5) . 7_565 ?
O32 Eu01 Ti2 37.43(5) 7_565 7_565 ?
O32 Eu01 Ti2 77.99(5) . 7_565 ?
O22 Eu01 Ti2 99.24(5) . 7_565 ?
O22 Eu01 Ti2 66.22(5) 7_565 7_565 ?
Ti2 Eu01 Ti2 49.240(19) . 7_565 ?
O5 Eu01 Ti3 28.69(4) . . ?
O9 Eu01 Ti3 129.78(6) . . ?
O8 Eu01 Ti3 102.84(7) . . ?
O12 Eu01 Ti3 100.96(5) 7_565 . ?
O12 Eu01 Ti3 66.76(5) . . ?
O32 Eu01 Ti3 153.60(5) 7_565 . ?
O32 Eu01 Ti3 108.05(5) . . ?
O22 Eu01 Ti3 37.51(5) . . ?
O22 Eu01 Ti3 76.72(5) 7_565 . ?
Ti2 Eu01 Ti3 103.675(14) . . ?
Ti2 Eu01 Ti3 125.687(14) 7_565 . ?
C1' O1 Ti1 172.0(6) . . ?
C1 O1 Ti1 138.6(8) . . ?
C2' O2 Ti3 154.3(6) . . ?
C2 O2 Ti3 132.3(5) . . ?
C3 O3 Ti2 147.9(4) . . ?
C4 O4 Ti1 130.05(10) . . ?
C4 O4 Ti1 130.05(10) . 7_565 ?
Ti1 O4 Ti1 96.57(14) . 7_565 ?
Ti3 O5 Ti3 103.34(14) . 7_565 ?
Ti3 O5 Eu01 115.28(9) . . ?
Ti3 O5 Eu01 115.28(9) 7_565 . ?
C6 O6 Ti3 131.83(8) . 7_565 ?
C6 O6 Ti3 131.84(8) . . ?
Ti3 O6 Ti3 96.06(14) 7_565 . ?
C7 O7 Ti2 131.40(9) . . ?
C7 O7 Ti2 131.40(9) . 7_565 ?
Ti2 O7 Ti2 95.50(13) . 7_565 ?
Ti2 O8 Ti2 103.23(14) . 7_565 ?
Ti2 O8 Eu01 114.70(10) . . ?
Ti2 O8 Eu01 114.70(10) 7_565 . ?
Ti1 O9 Ti1 103.26(14) . 7_565 ?
Ti1 O9 Eu01 115.18(10) . . ?
Ti1 O9 Eu01 115.18(10) 7_565 . ?
C11 O10 Ti1 139.9(2) . . ?
C17 O11 Ti3 138.2(2) . . ?
C17 O12 Ti1 131.1(2) . . ?
C17 O12 Eu01 130.3(2) . . ?
Ti1 O12 Eu01 98.42(8) . . ?
C21 O20 Ti3 139.5(2) . . ?
C27 O21 Ti2 136.9(2) . . ?
C27 O22 Ti3 131.4(2) . . ?
C27 O22 Eu01 131.3(2) . . ?
Ti3 O22 Eu01 96.51(8) . . ?
C31 O30 Ti2 139.4(2) . . ?
C37 O31 Ti1 138.7(2) . . ?
C37 O32 Ti2 131.5(2) . . ?
C37 O32 Eu01 130.95(19) . . ?
Ti2 O32 Eu01 97.48(8) . . ?
O1 C1 C1B 112.1(12) . . ?
O1 C1 C1A 111.4(13) . . ?
C1B C1 C1A 114.1(15) . . ?
O1 C1 H1A 106.2 . . ?
C1B C1 H1A 106.2 . . ?
C1A C1 H1A 106.2 . . ?
C1 C1B H1BA 109.5 . . ?
C1 C1B H1BB 109.5 . . ?
H1BA C1B H1BB 109.5 . . ?
C1 C1B H1BC 109.5 . . ?
H1BA C1B H1BC 109.5 . . ?
H1BB C1B H1BC 109.5 . . ?
C1 C1A H1AA 109.5 . . ?
C1 C1A H1AB 109.5 . . ?
H1AA C1A H1AB 109.5 . . ?
C1 C1A H1AC 109.5 . . ?
H1AA C1A H1AC 109.5 . . ?
H1AB C1A H1AC 109.5 . . ?
O1 C1' C1B' 109.5(13) . . ?
O1 C1' C1A' 103.2(14) . . ?
C1B' C1' C1A' 112.8(15) . . ?
O1 C1' H1'A 110.4 . . ?
C1B' C1' H1'A 110.4 . . ?
C1A' C1' H1'A 110.4 . . ?
C1' C1B' H1BD 109.5 . . ?
C1' C1B' H1BE 109.5 . . ?
H1BD C1B' H1BE 109.5 . . ?
C1' C1B' H1BF 109.5 . . ?
H1BD C1B' H1BF 109.5 . . ?
H1BE C1B' H1BF 109.5 . . ?
C1' C1A' H1AD 109.5 . . ?
C1' C1A' H1AE 109.5 . . ?
H1AD C1A' H1AE 109.5 . . ?
C1' C1A' H1AF 109.5 . . ?
H1AD C1A' H1AF 109.5 . . ?
H1AE C1A' H1AF 109.5 . . ?
O3 C3 C3A 118.1(6) . . ?
O3 C3 C3B 112.3(6) . . ?
C3A C3 C3B 124.0(6) . . ?
O3 C3 H3A 97.9 . . ?
C3A C3 H3A 97.9 . . ?
C3B C3 H3A 97.9 . . ?
C3 C3B H3BA 109.5 . . ?
C3 C3B H3BB 109.5 . . ?
H3BA C3B H3BB 109.5 . . ?
C3 C3B H3BC 109.5 . . ?
H3BA C3B H3BC 109.5 . . ?
H3BB C3B H3BC 109.5 . . ?
C3 C3A H3AA 109.5 . . ?
C3 C3A H3AB 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
C3 C3A H3AC 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
C4B C4 C4A 136.3(8) . . ?
C4B C4 O4 113.9(7) . . ?
C4A C4 O4 109.8(6) . . ?
C4B C4 H4A 90.0 . . ?
C4A C4 H4A 90.0 . . ?
O4 C4 H4A 90.0 . . ?
C4 C4A H4AA 109.5 . . ?
C4 C4A H4AB 109.5 . . ?
H4AA C4A H4AB 109.5 . . ?
C4 C4A H4AC 109.5 . . ?
H4AA C4A H4AC 109.5 . . ?
H4AB C4A H4AC 109.5 . . ?
C4 C4B H4BA 109.5 . . ?
C4 C4B H4BB 109.5 . . ?
H4BA C4B H4BB 109.5 . . ?
C4 C4B H4BC 109.5 . . ?
H4BA C4B H4BC 109.5 . . ?
H4BB C4B H4BC 109.5 . . ?
C6B C6 O6 114.2(9) . . ?
C6B C6 C6A 136.3(10) . . ?
O6 C6 C6A 109.5(7) . . ?
C6B C6 H6A 90.0 . . ?
O6 C6 H6A 90.0 . . ?
C6A C6 H6A 90.0 . . ?
C6 C6A H6AA 109.5 . . ?
C6 C6A H6AB 109.5 . . ?
H6AA C6A H6AB 109.5 . . ?
C6 C6A H6AC 109.5 . . ?
H6AA C6A H6AC 109.5 . . ?
H6AB C6A H6AC 109.5 . . ?
C6 C6B H6BA 109.5 . . ?
C6 C6B H6BB 109.5 . . ?
H6BA C6B H6BB 109.5 . . ?
C6 C6B H6BC 109.5 . . ?
H6BA C6B H6BC 109.5 . . ?
H6BB C6B H6BC 109.5 . . ?
C7A C7 O7 116.5(7) . . ?
C7A C7 C7B 133.4(8) . . ?
O7 C7 C7B 110.1(6) . . ?
C7A C7 H7A 90.0 . . ?
O7 C7 H7A 90.0 . . ?
C7B C7 H7A 90.0 . . ?
C7 C7B H7BA 109.5 . . ?
C7 C7B H7BB 109.5 . . ?
H7BA C7B H7BB 109.5 . . ?
C7 C7B H7BC 109.5 . . ?
H7BA C7B H7BC 109.5 . . ?
H7BB C7B H7BC 109.5 . . ?
C7 C7A H7AA 109.5 . . ?
C7 C7A H7AB 109.5 . . ?
H7AA C7A H7AB 109.5 . . ?
C7 C7A H7AC 109.5 . . ?
H7AA C7A H7AC 109.5 . . ?
H7AB C7A H7AC 109.5 . . ?
O10 C11 C16 122.1(3) . . ?
O10 C11 C12 118.5(4) . . ?
C16 C11 C12 119.4(4) . . ?
C13 C12 C11 119.7(4) . . ?
C13 C12 H12A 120.2 . . ?
C11 C12 H12A 120.2 . . ?
C14 C13 C12 121.4(4) . . ?
C14 C13 H13A 119.3 . . ?
C12 C13 H13A 119.3 . . ?
C13 C14 C15 119.9(5) . . ?
C13 C14 H14A 120.0 . . ?
C15 C14 H14A 120.0 . . ?
C14 C15 C16 120.6(5) . . ?
C14 C15 H15A 119.7 . . ?
C16 C15 H15A 119.7 . . ?
C11 C16 C15 118.9(3) . . ?
C11 C16 C17 122.4(3) . . ?
C15 C16 C17 118.7(3) . . ?
O11 C17 O12 121.6(3) . . ?
O11 C17 C16 116.2(3) . . ?
O12 C17 C16 122.3(3) . . ?
O20 C21 C22 117.7(3) . . ?
O20 C21 C26 122.9(3) . . ?
C22 C21 C26 119.3(3) . . ?
C23 C22 C21 120.6(4) . . ?
C23 C22 H22A 119.7 . . ?
C21 C22 H22A 119.7 . . ?
C24 C23 C22 120.1(4) . . ?
C24 C23 H23A 120.0 . . ?
C22 C23 H23A 120.0 . . ?
C25 C24 C23 120.1(4) . . ?
C25 C24 H24A 119.9 . . ?
C23 C24 H24A 119.9 . . ?
C24 C25 C26 121.2(4) . . ?
C24 C25 H25A 119.4 . . ?
C26 C25 H25A 119.4 . . ?
C25 C26 C21 118.7(3) . . ?
C25 C26 C27 118.9(3) . . ?
C21 C26 C27 122.3(3) . . ?
O21 C27 O22 122.3(3) . . ?
O21 C27 C26 116.2(3) . . ?
O22 C27 C26 121.5(3) . . ?
O30 C31 C32 118.1(4) . . ?
O30 C31 C36 123.2(3) . . ?
C32 C31 C36 118.7(4) . . ?
C33 C32 C31 121.0(4) . . ?
C33 C32 H32A 119.5 . . ?
C31 C32 H32A 119.5 . . ?
C32 C33 C34 120.8(4) . . ?
C32 C33 H33A 119.6 . . ?
C34 C33 H33A 119.6 . . ?
C35 C34 C33 119.2(4) . . ?
C35 C34 H34A 120.4 . . ?
C33 C34 H34A 120.4 . . ?
C34 C35 C36 121.1(4) . . ?
C34 C35 H35A 119.4 . . ?
C36 C35 H35A 119.4 . . ?
C35 C36 C31 119.3(3) . . ?
C35 C36 C37 118.5(3) . . ?
C31 C36 C37 122.2(3) . . ?
O31 C37 O32 122.6(3) . . ?
O31 C37 C36 115.9(3) . . ?
O32 C37 C36 121.5(3) . . ?
C2B C2 O2 115.2(8) . . ?
C2B C2 C2A 118.3(11) . . ?
O2 C2 C2A 104.9(11) . . ?
C2B C2 H2A 105.8 . . ?
O2 C2 H2A 105.8 . . ?
C2A C2 H2A 105.8 . . ?
C2 C2A H2AA 109.5 . . ?
C2 C2A H2AB 109.5 . . ?
H2AA C2A H2AB 109.5 . . ?
C2 C2A H2AC 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
C2 C2B H2BA 109.5 . . ?
C2 C2B H2BB 109.5 . . ?
H2BA C2B H2BB 109.5 . . ?
C2 C2B H2BC 109.5 . . ?
H2BA C2B H2BC 109.5 . . ?
H2BB C2B H2BC 109.5 . . ?
O2 C2' C2A' 103.1(14) . . ?
O2 C2' C2B' 110.9(9) . . ?
C2A' C2' C2B' 115.1(15) . . ?
O2 C2' H2'A 109.1 . . ?
C2A' C2' H2'A 109.1 . . ?
C2B' C2' H2'A 109.1 . . ?
C2' C2B' C2B' 103.9(7) . 7_565 ?
C2' C2B' H2BD 109.5 . . ?
C2B' C2B' H2BD 81.9 7_565 . ?
C2' C2B' H2BE 109.5 . . ?
C2B' C2B' H2BE 32.8 7_565 . ?
H2BD C2B' H2BE 109.5 . . ?
C2' C2B' H2BF 109.5 . . ?
C2B' C2B' H2BF 137.8 7_565 . ?
H2BD C2B' H2BF 109.5 . . ?
H2BE C2B' H2BF 109.5 . . ?
C2' C2A' H2AD 109.5 . . ?
C2' C2A' H2AE 109.5 . . ?
H2AD C2A' H2AE 109.5 . . ?
C2' C2A' H2AF 109.5 . . ?
H2AD C2A' H2AF 109.5 . . ?
H2AE C2A' H2AF 109.5 . . ?

_refine_diff_density_max         0.741
_refine_diff_density_min         -0.777
_refine_diff_density_rms         0.075

####################################################################### 
# 
# 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_gd_c
_database_code_depnum_ccdc_archive 'CCDC 1504168'
_audit_update_record             
;
2017-02-27 deposited with the CCDC.
2017-03-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C69 H87 Gd O30 Ti6'
_chemical_formula_sum            'C69 H87 Gd O30 Ti6'
_chemical_formula_weight         1841.03

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -8.8380 11.9157 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           174
_space_group_name_H-M_alt        'P -6'
_space_group_name_Hall           'P -6'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'

_cell_length_a                   14.9227(4)
_cell_length_b                   14.9227(4)
_cell_length_c                   23.5803(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4547.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9985
_cell_measurement_theta_min      3.42
_cell_measurement_theta_max      66.7

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_F_000             1874
_exptl_transmission_factor_min   0.520
_exptl_transmission_factor_max   1.000
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    9.490
_shelx_estimated_absorpt_T_min   0.157
_shelx_estimated_absorpt_T_max   0.253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.157
_exptl_absorpt_correction_T_max  0.253
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements (SADABS) 
;
_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         '30W microfocus sealed tube, Quazar optics'
_diffrn_measurement_device_type  'Bruker QUEST D8 CCD'
_diffrn_measurement_method       'Thin slice ω and φ scans'
_diffrn_reflns_number            29382
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_av_R_equivalents  0.0659
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.420
_diffrn_reflns_theta_max         66.722
_diffrn_reflns_theta_full        66.722
_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 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             5479
_reflns_number_gt                5264
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.983
_reflns_Friedel_fraction_max     0.992
_reflns_Friedel_fraction_full    0.992

_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 software package, narrow-frames'
_computing_cell_refinement       'refinement of XYZ centroids > 20sigma(I)'
_computing_data_reduction        
;
 Bruker SAINT software package, narrow frame algorithm
;
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_refine_special_details          
;Refined as a 2-component twin. Residual electron density did not refine
into anything meaningful and is presumably disordered solvent thus was
ignored. iPr ligands disordered - treated isotropically and restrained., Twin
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1289P)²+14.5673P] 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_abs_structure_details 
;
 Flack x determined using 2453 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.151(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5479
_refine_ls_number_parameters     331
_refine_ls_number_restraints     210
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0698
_refine_ls_wR_factor_ref         0.1961
_refine_ls_wR_factor_gt          0.1918
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_restrained_S_all      1.116
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Gd1 Gd 0.666667 0.333333 0.500000 0.0169(6) Uani 1 6 d S T P . .
Gd2 Gd 1.000000 1.000000 1.000000 0.0175(6) Uani 1 6 d S T P . .
Ti1 Ti 0.4664(3) 0.3641(3) 0.56302(12) 0.0263(7) Uani 1 1 d . . . . .
Ti2 Ti 0.8093(2) 0.7621(2) 0.93680(12) 0.0259(7) Uani 1 1 d . . . . .
O1 O 0.5013(12) 0.3087(13) 0.500000 0.023(3) Uani 1 2 d S TU P . .
O2 O 0.4864(13) 0.4615(12) 0.500000 0.031(4) Uani 1 2 d S TU P C .
O3 O 0.3294(10) 0.2950(10) 0.5641(5) 0.037(3) Uani 1 1 d D U . . .
O4 O 0.4789(10) 0.4538(11) 0.6217(6) 0.040(3) Uani 1 1 d . U . . .
O5 O 0.4706(11) 0.2576(10) 0.6152(6) 0.035(3) Uani 1 1 d . U . . .
O6 O 0.6333(10) 0.4354(9) 0.5756(5) 0.030(3) Uani 1 1 d . U . . .
O21 O 0.8371(14) 0.8522(12) 1.000000 0.029(4) Uani 1 2 d S TU P . .
O22 O 0.8337(15) 0.6867(11) 1.000000 0.032(4) Uani 1 2 d S TU P G .
O23 O 0.6733(10) 0.6848(10) 0.9357(5) 0.034(3) Uani 1 1 d D U . . .
O24 O 0.8302(10) 0.6927(9) 0.8770(5) 0.038(3) Uani 1 1 d . U . . .
O25 O 0.9753(9) 0.8669(9) 0.9251(5) 0.026(2) Uani 1 1 d . U . . .
O26 O 0.8051(11) 0.8668(11) 0.8863(6) 0.031(3) Uani 1 1 d . U . . .
C2 C 0.479(2) 0.559(2) 0.500000 0.055(8) Uani 1 2 d DS TU P . .
H2A H 0.471223 0.559134 0.542130 0.067 Uiso 0.5 1 calc R U P A -1
C2A C 0.586(3) 0.649(3) 0.500000 0.079(12) Uani 1 2 d DS TU P C .
H2AA H 0.634277 0.625287 0.510390 0.118 Uiso 0.5 1 calc R U P B -1
H2AB H 0.602506 0.679528 0.462086 0.118 Uiso 0.5 1 calc R U P B -1
H2AC H 0.590513 0.700004 0.527524 0.118 Uiso 0.5 1 calc R U P B -1
C2B C 0.372(4) 0.539(5) 0.489(4) 0.09(2) Uani 0.5 1 d D U P C -1
H2BA H 0.322535 0.465050 0.493936 0.140 Uiso 0.5 1 calc R U P C -1
H2BB H 0.355850 0.579413 0.515134 0.140 Uiso 0.5 1 calc R U P C -1
H2BC H 0.367843 0.558937 0.449696 0.140 Uiso 0.5 1 calc R U P C -1
C3 C 0.251(3) 0.256(3) 0.6097(14) 0.060(9) Uiso 0.49(3) 1 d D U P D 1
H3 H 0.262558 0.227123 0.645546 0.072 Uiso 0.49(3) 1 calc R U P D 1
C3A C 0.206(5) 0.325(5) 0.611(3) 0.069(7) Uiso 0.49(3) 1 d D U P D 1
H3AA H 0.222658 0.361955 0.647177 0.103 Uiso 0.49(3) 1 calc R U P D 1
H3AB H 0.233915 0.374235 0.579722 0.103 Uiso 0.49(3) 1 calc R U P D 1
H3AC H 0.130210 0.282852 0.607103 0.103 Uiso 0.49(3) 1 calc R U P D 1
C3B C 0.228(5) 0.198(4) 0.5568(19) 0.069(7) Uiso 0.49(3) 1 d D U P D 1
H3BA H 0.158658 0.136696 0.558928 0.103 Uiso 0.49(3) 1 calc R U P D 1
H3BB H 0.230339 0.241959 0.525277 0.103 Uiso 0.49(3) 1 calc R U P D 1
H3BC H 0.279157 0.176188 0.550439 0.103 Uiso 0.49(3) 1 calc R U P D 1
C3' C 0.222(4) 0.243(3) 0.5665(18) 0.060(9) Uiso 0.51(3) 1 d D U P D 2
H3A' H 0.194359 0.242318 0.527856 0.072 Uiso 0.51(3) 1 calc R U P D 2
C3A' C 0.179(5) 0.286(4) 0.607(2) 0.069(7) Uiso 0.51(3) 1 d D U P D 2
H3AD H 0.103398 0.245426 0.606296 0.103 Uiso 0.51(3) 1 calc R U P D 2
H3AE H 0.203895 0.284725 0.645339 0.103 Uiso 0.51(3) 1 calc R U P D 2
H3AF H 0.201488 0.358106 0.596591 0.103 Uiso 0.51(3) 1 calc R U P D 2
C3B' C 0.187(5) 0.133(3) 0.584(2) 0.069(7) Uiso 0.51(3) 1 d D U P D 2
H3BD H 0.111678 0.093636 0.585976 0.103 Uiso 0.51(3) 1 calc R U P D 2
H3BE H 0.211211 0.101156 0.555719 0.103 Uiso 0.51(3) 1 calc R U P D 2
H3BF H 0.216649 0.132874 0.620990 0.103 Uiso 0.51(3) 1 calc R U P D 2
C11 C 0.5525(17) 0.5284(15) 0.6538(9) 0.043(5) Uani 1 1 d . U . . .
C12 C 0.522(2) 0.5810(17) 0.6927(8) 0.049(5) Uani 1 1 d . U . . .
H12A H 0.452843 0.566804 0.694241 0.059 Uiso 1 1 calc R U . . .
C13 C 0.596(2) 0.652(3) 0.7276(11) 0.069(7) Uani 1 1 d . U . . .
H13A H 0.575015 0.686546 0.753973 0.083 Uiso 1 1 calc R U . . .
C14 C 0.696(2) 0.678(3) 0.7277(11) 0.070(7) Uani 1 1 d . U . . .
H14A H 0.743910 0.729721 0.752902 0.083 Uiso 1 1 calc R U . . .
C15 C 0.728(2) 0.6281(18) 0.6901(9) 0.051(6) Uani 1 1 d . U . . .
H15A H 0.798711 0.645659 0.689616 0.061 Uiso 1 1 calc R U . . .
C16 C 0.6565(15) 0.5506(15) 0.6523(9) 0.035(4) Uani 1 1 d . U . . .
C17 C 0.4955(16) 0.1891(15) 0.6124(8) 0.030(4) Uani 1 1 d . U . . .
C22 C 0.835(3) 0.592(3) 1.000000 0.065(10) Uani 1 2 d S TU P . .
H22' H 0.822300 0.575712 0.958605 0.079 Uiso 0.5 1 calc R U P E -1
C22A C 0.945(7) 0.631(7) 1.000000 0.16(3) Uani 1 2 d S TU P G .
H22A H 0.958170 0.572821 1.000000 0.245 Uiso 0.5 1 calc R U P F -1
H22B H 0.975600 0.673175 0.966066 0.245 Uiso 0.5 1 calc R U P F -1
H22C H 0.975601 0.673175 1.033934 0.245 Uiso 0.5 1 calc R U P F -1
C22B C 0.739(5) 0.505(4) 1.021(2) 0.075(16) Uani 0.5 1 d . U P G -1
H22D H 0.743388 0.441755 1.020472 0.113 Uiso 0.5 1 calc R U P G -1
H22E H 0.727148 0.519269 1.060345 0.113 Uiso 0.5 1 calc R U P G -1
H22F H 0.681040 0.495736 0.997358 0.113 Uiso 0.5 1 calc R U P G -1
C23 C 0.599(3) 0.641(3) 0.8881(17) 0.065(10) Uiso 0.53(2) 1 d D U P H 1
H23A H 0.635937 0.671442 0.851584 0.078 Uiso 0.53(2) 1 calc R U P H 1
C23A C 0.519(5) 0.669(5) 0.898(3) 0.087(10) Uiso 0.53(2) 1 d D U P H 1
H23B H 0.551215 0.744309 0.898079 0.131 Uiso 0.53(2) 1 calc R U P H 1
H23C H 0.468004 0.640186 0.867080 0.131 Uiso 0.53(2) 1 calc R U P H 1
H23D H 0.485229 0.640624 0.934088 0.131 Uiso 0.53(2) 1 calc R U P H 1
C23B C 0.557(5) 0.528(4) 0.887(3) 0.087(10) Uiso 0.53(2) 1 d D U P H 1
H23E H 0.612499 0.512898 0.880542 0.131 Uiso 0.53(2) 1 calc R U P H 1
H23F H 0.522906 0.498338 0.923306 0.131 Uiso 0.53(2) 1 calc R U P H 1
H23G H 0.505680 0.497901 0.856298 0.131 Uiso 0.53(2) 1 calc R U P H 1
C23' C 0.565(3) 0.654(4) 0.935(2) 0.065(10) Uiso 0.47(2) 1 d D U P H 2
H23H H 0.537261 0.606295 0.968452 0.078 Uiso 0.47(2) 1 calc R U P H 2
C23C C 0.554(6) 0.742(5) 0.954(3) 0.087(10) Uiso 0.47(2) 1 d D U P H 2
H23I H 0.480361 0.722070 0.953835 0.131 Uiso 0.47(2) 1 calc R U P H 2
H23J H 0.581467 0.762235 0.992464 0.131 Uiso 0.47(2) 1 calc R U P H 2
H23K H 0.591949 0.800626 0.928177 0.131 Uiso 0.47(2) 1 calc R U P H 2
C23D C 0.488(5) 0.596(5) 0.891(3) 0.087(10) Uiso 0.47(2) 1 d D U P H 2
H23L H 0.420769 0.586621 0.902096 0.131 Uiso 0.47(2) 1 calc R U P H 2
H23M H 0.510126 0.634527 0.855155 0.131 Uiso 0.47(2) 1 calc R U P H 2
H23N H 0.482742 0.528309 0.886012 0.131 Uiso 0.47(2) 1 calc R U P H 2
C31 C 0.9050(15) 0.6977(13) 0.8434(7) 0.032(4) Uani 1 1 d . U . . .
C32 C 0.882(2) 0.6227(19) 0.8038(10) 0.051(5) Uani 1 1 d . U . . .
H32A H 0.813212 0.566307 0.801528 0.061 Uiso 1 1 calc R U . . .
C33 C 0.957(2) 0.626(2) 0.7661(10) 0.061(6) Uani 1 1 d . U . . .
H33A H 0.939171 0.572133 0.739170 0.073 Uiso 1 1 calc R U . . .
C34 C 1.056(2) 0.709(2) 0.7697(11) 0.068(7) Uani 1 1 d . U . . .
H34A H 1.106844 0.713221 0.743892 0.082 Uiso 1 1 calc R U . . .
C35 C 1.0831(19) 0.786(2) 0.8099(9) 0.048(5) Uani 1 1 d . U . . .
H35A H 1.151705 0.843069 0.811226 0.058 Uiso 1 1 calc R U . . .
C36 C 1.0088(15) 0.7793(14) 0.8483(8) 0.033(4) Uani 1 1 d . U . . .
C37 C 0.8292(15) 0.9604(16) 0.8888(9) 0.031(4) Uani 1 1 d . 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
Gd1 O1 2.305(15) 2_655 ?
Gd1 O1 2.305(15) 3_665 ?
Gd1 O1 2.305(15) . ?
Gd1 O6 2.550(12) 3_665 ?
Gd1 O6 2.550(12) 6_666 ?
Gd1 O6 2.550(12) 5_656 ?
Gd1 O6 2.550(12) 2_655 ?
Gd1 O6 2.550(12) . ?
Gd1 O6 2.550(12) 4_556 ?
Gd1 Ti1 3.567(3) 5_656 ?
Gd1 Ti1 3.567(3) 2_655 ?
Gd1 Ti1 3.567(3) 3_665 ?
Gd2 O21 2.326(17) . ?
Gd2 O21 2.326(17) 3_675 ?
Gd2 O21 2.326(17) 2_765 ?
Gd2 O25 2.543(11) 3_675 ?
Gd2 O25 2.543(11) 6_677 ?
Gd2 O25 2.543(11) 5_767 ?
Gd2 O25 2.543(11) 2_765 ?
Gd2 O25 2.543(11) 4_557 ?
Gd2 O25 2.543(11) . ?
Gd2 Ti2 3.580(3) 6_677 ?
Gd2 Ti2 3.580(3) 3_675 ?
Gd2 Ti2 3.580(3) . ?
Ti1 O3 1.770(14) . ?
Ti1 O4 1.867(14) . ?
Ti1 O1 1.896(10) . ?
Ti1 O2 1.994(11) . ?
Ti1 O5 2.036(13) . ?
Ti1 O6 2.185(13) . ?
Ti1 Ti1 2.972(6) 4_556 ?
Ti2 O23 1.763(14) . ?
Ti2 O24 1.866(13) . ?
Ti2 O21 1.909(11) . ?
Ti2 O26 1.989(14) . ?
Ti2 O22 2.008(12) . ?
Ti2 O25 2.187(13) . ?
Ti2 Ti2 2.980(6) 4_557 ?
O2 C2 1.51(3) . ?
O3 C3' 1.39(5) . ?
O3 C3 1.48(3) . ?
O3 C3B 1.49(6) . ?
O4 C11 1.34(2) . ?
O5 C17 1.25(2) . ?
O6 C17 1.30(2) 3_665 ?
O22 C22 1.43(4) . ?
O23 C23' 1.45(3) . ?
O23 C23 1.48(3) . ?
O24 C31 1.34(2) . ?
O25 C37 1.28(2) 2_765 ?
O26 C37 1.26(2) . ?
C2 C2A 1.48(3) . ?
C2 C2B 1.49(3) . ?
C2 H2A 1.0000 . ?
C2A H2AA 0.9800 . ?
C2A H2AB 0.9800 . ?
C2A H2AC 0.9800 . ?
C2B H2BA 0.9800 . ?
C2B H2BB 0.9800 . ?
C2B H2BC 0.9800 . ?
C3 C3B 1.46(3) . ?
C3 C3A 1.49(3) . ?
C3 H3 1.0000 . ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?
C3A H3AC 0.9800 . ?
C3B H3BA 0.9800 . ?
C3B H3BB 0.9800 . ?
C3B H3BC 0.9800 . ?
C3' C3A' 1.47(3) . ?
C3' C3B' 1.51(3) . ?
C3' H3A' 1.0000 . ?
C3A' H3AD 0.9800 . ?
C3A' H3AE 0.9800 . ?
C3A' H3AF 0.9800 . ?
C3B' H3BD 0.9800 . ?
C3B' H3BE 0.9800 . ?
C3B' H3BF 0.9800 . ?
C11 C16 1.42(3) . ?
C11 C12 1.42(3) . ?
C12 C13 1.36(4) . ?
C12 H12A 0.9500 . ?
C13 C14 1.34(4) . ?
C13 H13A 0.9500 . ?
C14 C15 1.39(3) . ?
C14 H14A 0.9500 . ?
C15 C16 1.43(3) . ?
C15 H15A 0.9500 . ?
C16 C17 1.43(3) 3_665 ?
C22 C22A 1.44(9) . ?
C22 C22B 1.46(7) . ?
C22 H22' 1.0000 . ?
C22A H22A 0.9800 . ?
C22A H22B 0.9800 . ?
C22A H22C 0.9800 . ?
C22B H22D 0.9800 . ?
C22B H22E 0.9800 . ?
C22B H22F 0.9800 . ?
C23 C23A 1.47(3) . ?
C23 C23B 1.47(3) . ?
C23 H23A 1.0000 . ?
C23A H23B 0.9800 . ?
C23A H23C 0.9800 . ?
C23A H23D 0.9800 . ?
C23B H23E 0.9800 . ?
C23B H23F 0.9800 . ?
C23B H23G 0.9800 . ?
C23' C23C 1.47(3) . ?
C23' C23D 1.47(3) . ?
C23' H23H 1.0000 . ?
C23C H23I 0.9800 . ?
C23C H23J 0.9800 . ?
C23C H23K 0.9800 . ?
C23D H23L 0.9800 . ?
C23D H23M 0.9800 . ?
C23D H23N 0.9800 . ?
C31 C32 1.36(3) . ?
C31 C36 1.42(3) . ?
C32 C33 1.41(3) . ?
C32 H32A 0.9500 . ?
C33 C34 1.38(4) . ?
C33 H33A 0.9500 . ?
C34 C35 1.39(3) . ?
C34 H34A 0.9500 . ?
C35 C36 1.40(3) . ?
C35 H35A 0.9500 . ?
C36 C37 1.52(3) 2_765 ?

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 Gd1 O1 120.000(2) 2_655 3_665 ?
O1 Gd1 O1 119.999(2) 2_655 . ?
O1 Gd1 O1 120.001(2) 3_665 . ?
O1 Gd1 O6 72.9(4) 2_655 3_665 ?
O1 Gd1 O6 65.3(4) 3_665 3_665 ?
O1 Gd1 O6 135.4(3) . 3_665 ?
O1 Gd1 O6 72.9(4) 2_655 6_666 ?
O1 Gd1 O6 65.3(4) 3_665 6_666 ?
O1 Gd1 O6 135.4(3) . 6_666 ?
O6 Gd1 O6 88.7(5) 3_665 6_666 ?
O1 Gd1 O6 65.3(4) 2_655 5_656 ?
O1 Gd1 O6 135.4(3) 3_665 5_656 ?
O1 Gd1 O6 72.9(4) . 5_656 ?
O6 Gd1 O6 138.1(2) 3_665 5_656 ?
O6 Gd1 O6 76.6(4) 6_666 5_656 ?
O1 Gd1 O6 65.3(4) 2_655 2_655 ?
O1 Gd1 O6 135.4(3) 3_665 2_655 ?
O1 Gd1 O6 72.9(4) . 2_655 ?
O6 Gd1 O6 76.6(4) 3_665 2_655 ?
O6 Gd1 O6 138.1(2) 6_666 2_655 ?
O6 Gd1 O6 88.7(5) 5_656 2_655 ?
O1 Gd1 O6 135.4(3) 2_655 . ?
O1 Gd1 O6 72.9(4) 3_665 . ?
O1 Gd1 O6 65.3(4) . . ?
O6 Gd1 O6 76.6(4) 3_665 . ?
O6 Gd1 O6 138.1(2) 6_666 . ?
O6 Gd1 O6 138.1(2) 5_656 . ?
O6 Gd1 O6 76.6(4) 2_655 . ?
O1 Gd1 O6 135.4(3) 2_655 4_556 ?
O1 Gd1 O6 72.9(4) 3_665 4_556 ?
O1 Gd1 O6 65.3(4) . 4_556 ?
O6 Gd1 O6 138.1(2) 3_665 4_556 ?
O6 Gd1 O6 76.6(4) 6_666 4_556 ?
O6 Gd1 O6 76.6(4) 5_656 4_556 ?
O6 Gd1 O6 138.1(2) 2_655 4_556 ?
O6 Gd1 O6 88.7(5) . 4_556 ?
O1 Gd1 Ti1 28.6(2) 2_655 5_656 ?
O1 Gd1 Ti1 130.0(4) 3_665 5_656 ?
O1 Gd1 Ti1 103.6(4) . 5_656 ?
O6 Gd1 Ti1 100.7(3) 3_665 5_656 ?
O6 Gd1 Ti1 66.7(3) 6_666 5_656 ?
O6 Gd1 Ti1 37.4(3) 5_656 5_656 ?
O6 Gd1 Ti1 77.8(3) 2_655 5_656 ?
O6 Gd1 Ti1 154.1(3) . 5_656 ?
O6 Gd1 Ti1 108.5(3) 4_556 5_656 ?
O1 Gd1 Ti1 28.6(2) 2_655 2_655 ?
O1 Gd1 Ti1 130.0(4) 3_665 2_655 ?
O1 Gd1 Ti1 103.6(4) . 2_655 ?
O6 Gd1 Ti1 66.7(3) 3_665 2_655 ?
O6 Gd1 Ti1 100.7(3) 6_666 2_655 ?
O6 Gd1 Ti1 77.8(3) 5_656 2_655 ?
O6 Gd1 Ti1 37.4(3) 2_655 2_655 ?
O6 Gd1 Ti1 108.5(3) . 2_655 ?
O6 Gd1 Ti1 154.1(3) 4_556 2_655 ?
Ti1 Gd1 Ti1 49.24(10) 5_656 2_655 ?
O1 Gd1 Ti1 103.6(4) 2_655 3_665 ?
O1 Gd1 Ti1 28.6(2) 3_665 3_665 ?
O1 Gd1 Ti1 130.0(4) . 3_665 ?
O6 Gd1 Ti1 37.4(3) 3_665 3_665 ?
O6 Gd1 Ti1 77.8(3) 6_666 3_665 ?
O6 Gd1 Ti1 154.1(3) 5_656 3_665 ?
O6 Gd1 Ti1 108.5(3) 2_655 3_665 ?
O6 Gd1 Ti1 66.7(3) . 3_665 ?
O6 Gd1 Ti1 100.7(3) 4_556 3_665 ?
Ti1 Gd1 Ti1 125.93(2) 5_656 3_665 ?
Ti1 Gd1 Ti1 103.87(6) 2_655 3_665 ?
O21 Gd2 O21 119.999(7) . 3_675 ?
O21 Gd2 O21 120.001(10) . 2_765 ?
O21 Gd2 O21 120.000(17) 3_675 2_765 ?
O21 Gd2 O25 72.4(4) . 3_675 ?
O21 Gd2 O25 65.5(4) 3_675 3_675 ?
O21 Gd2 O25 135.8(3) 2_765 3_675 ?
O21 Gd2 O25 72.4(4) . 6_677 ?
O21 Gd2 O25 65.5(4) 3_675 6_677 ?
O21 Gd2 O25 135.8(3) 2_765 6_677 ?
O25 Gd2 O25 87.9(5) 3_675 6_677 ?
O21 Gd2 O25 135.8(3) . 5_767 ?
O21 Gd2 O25 72.4(4) 3_675 5_767 ?
O21 Gd2 O25 65.5(4) 2_765 5_767 ?
O25 Gd2 O25 137.8(2) 3_675 5_767 ?
O25 Gd2 O25 77.1(4) 6_677 5_767 ?
O21 Gd2 O25 135.8(3) . 2_765 ?
O21 Gd2 O25 72.4(4) 3_675 2_765 ?
O21 Gd2 O25 65.5(4) 2_765 2_765 ?
O25 Gd2 O25 77.1(4) 3_675 2_765 ?
O25 Gd2 O25 137.8(2) 6_677 2_765 ?
O25 Gd2 O25 87.9(5) 5_767 2_765 ?
O21 Gd2 O25 65.5(4) . 4_557 ?
O21 Gd2 O25 135.8(3) 3_675 4_557 ?
O21 Gd2 O25 72.4(4) 2_765 4_557 ?
O25 Gd2 O25 137.8(2) 3_675 4_557 ?
O25 Gd2 O25 77.1(4) 6_677 4_557 ?
O25 Gd2 O25 77.1(4) 5_767 4_557 ?
O25 Gd2 O25 137.8(2) 2_765 4_557 ?
O21 Gd2 O25 65.5(4) . . ?
O21 Gd2 O25 135.8(3) 3_675 . ?
O21 Gd2 O25 72.4(4) 2_765 . ?
O25 Gd2 O25 77.1(4) 3_675 . ?
O25 Gd2 O25 137.8(2) 6_677 . ?
O25 Gd2 O25 137.8(2) 5_767 . ?
O25 Gd2 O25 77.1(4) 2_765 . ?
O25 Gd2 O25 87.9(5) 4_557 . ?
O21 Gd2 Ti2 103.1(4) . 6_677 ?
O21 Gd2 Ti2 28.9(2) 3_675 6_677 ?
O21 Gd2 Ti2 130.5(4) 2_765 6_677 ?
O25 Gd2 Ti2 77.4(3) 3_675 6_677 ?
O25 Gd2 Ti2 37.2(3) 6_677 6_677 ?
O25 Gd2 Ti2 66.8(3) 5_767 6_677 ?
O25 Gd2 Ti2 100.6(3) 2_765 6_677 ?
O25 Gd2 Ti2 108.8(3) 4_557 6_677 ?
O25 Gd2 Ti2 154.2(3) . 6_677 ?
O21 Gd2 Ti2 103.1(4) . 3_675 ?
O21 Gd2 Ti2 28.9(2) 3_675 3_675 ?
O21 Gd2 Ti2 130.5(4) 2_765 3_675 ?
O25 Gd2 Ti2 37.2(3) 3_675 3_675 ?
O25 Gd2 Ti2 77.4(3) 6_677 3_675 ?
O25 Gd2 Ti2 100.6(3) 5_767 3_675 ?
O25 Gd2 Ti2 66.8(3) 2_765 3_675 ?
O25 Gd2 Ti2 154.2(3) 4_557 3_675 ?
O25 Gd2 Ti2 108.8(3) . 3_675 ?
Ti2 Gd2 Ti2 49.19(9) 6_677 3_675 ?
O21 Gd2 Ti2 28.9(2) . . ?
O21 Gd2 Ti2 130.5(4) 3_675 . ?
O21 Gd2 Ti2 103.1(4) 2_765 . ?
O25 Gd2 Ti2 66.8(3) 3_675 . ?
O25 Gd2 Ti2 100.6(3) 6_677 . ?
O25 Gd2 Ti2 154.2(3) 5_767 . ?
O25 Gd2 Ti2 108.8(3) 2_765 . ?
O25 Gd2 Ti2 77.4(3) 4_557 . ?
O25 Gd2 Ti2 37.2(3) . . ?
Ti2 Gd2 Ti2 125.92(2) 6_677 . ?
Ti2 Gd2 Ti2 103.90(6) 3_675 . ?
O3 Ti1 O4 94.6(6) . . ?
O3 Ti1 O1 104.2(6) . . ?
O4 Ti1 O1 160.4(7) . . ?
O3 Ti1 O2 98.3(7) . . ?
O4 Ti1 O2 96.0(6) . . ?
O1 Ti1 O2 76.1(5) . . ?
O3 Ti1 O5 90.8(6) . . ?
O4 Ti1 O5 94.6(6) . . ?
O1 Ti1 O5 90.6(5) . . ?
O2 Ti1 O5 165.4(6) . . ?
O3 Ti1 O6 170.0(5) . . ?
O4 Ti1 O6 82.5(5) . . ?
O1 Ti1 O6 79.8(6) . . ?
O2 Ti1 O6 91.6(6) . . ?
O5 Ti1 O6 80.0(5) . . ?
O3 Ti1 Ti1 90.8(4) . 4_556 ?
O4 Ti1 Ti1 137.8(4) . 4_556 ?
O1 Ti1 Ti1 38.4(4) . 4_556 ?
O2 Ti1 Ti1 41.8(3) . 4_556 ?
O5 Ti1 Ti1 127.2(4) . 4_556 ?
O6 Ti1 Ti1 97.8(3) . 4_556 ?
O3 Ti1 Gd1 136.8(4) . . ?
O4 Ti1 Gd1 127.7(4) . . ?
O1 Ti1 Gd1 35.6(4) . . ?
O2 Ti1 Gd1 87.3(4) . . ?
O5 Ti1 Gd1 78.3(4) . . ?
O6 Ti1 Gd1 45.1(3) . . ?
Ti1 Ti1 Gd1 65.38(5) 4_556 . ?
O23 Ti2 O24 94.7(6) . . ?
O23 Ti2 O21 104.3(7) . . ?
O24 Ti2 O21 160.6(7) . . ?
O23 Ti2 O26 91.6(6) . . ?
O24 Ti2 O26 93.6(6) . . ?
O21 Ti2 O26 89.7(6) . . ?
O23 Ti2 O22 96.7(7) . . ?
O24 Ti2 O22 97.0(6) . . ?
O21 Ti2 O22 77.2(6) . . ?
O26 Ti2 O22 165.9(6) . . ?
O23 Ti2 O25 170.9(5) . . ?
O24 Ti2 O25 81.8(5) . . ?
O21 Ti2 O25 79.9(6) . . ?
O26 Ti2 O25 80.4(5) . . ?
O22 Ti2 O25 92.0(6) . . ?
O23 Ti2 Ti2 90.9(4) . 4_557 ?
O24 Ti2 Ti2 139.1(4) . 4_557 ?
O21 Ti2 Ti2 38.7(4) . 4_557 ?
O26 Ti2 Ti2 126.8(4) . 4_557 ?
O22 Ti2 Ti2 42.1(4) . 4_557 ?
O25 Ti2 Ti2 97.2(3) . 4_557 ?
O23 Ti2 Gd2 137.7(5) . . ?
O24 Ti2 Gd2 126.5(4) . . ?
O21 Ti2 Gd2 36.0(5) . . ?
O26 Ti2 Gd2 78.0(4) . . ?
O22 Ti2 Gd2 88.3(4) . . ?
O25 Ti2 Gd2 44.7(3) . . ?
Ti2 Ti2 Gd2 65.40(5) 4_557 . ?
Ti1 O1 Ti1 103.2(7) . 4_556 ?
Ti1 O1 Gd1 115.9(5) . . ?
Ti1 O1 Gd1 115.9(5) 4_556 . ?
C2 O2 Ti1 130.1(5) . . ?
C2 O2 Ti1 130.1(5) . 4_556 ?
Ti1 O2 Ti1 96.4(7) . 4_556 ?
C3 O3 C3B 58.7(17) . . ?
C3' O3 Ti1 178(2) . . ?
C3 O3 Ti1 134.1(18) . . ?
C3B O3 Ti1 152(2) . . ?
C11 O4 Ti1 139.5(13) . . ?
C17 O5 Ti1 138.0(14) . . ?
C17 O6 Ti1 130.0(12) 3_665 . ?
C17 O6 Gd1 132.4(12) 3_665 . ?
Ti1 O6 Gd1 97.5(4) . . ?
Ti2 O21 Ti2 102.7(8) . 4_557 ?
Ti2 O21 Gd2 115.1(6) . . ?
Ti2 O21 Gd2 115.1(6) 4_557 . ?
C22 O22 Ti2 130.8(5) . 4_557 ?
C22 O22 Ti2 130.8(5) . . ?
Ti2 O22 Ti2 95.8(8) 4_557 . ?
C23' O23 Ti2 161(2) . . ?
C23 O23 Ti2 131.5(19) . . ?
C31 O24 Ti2 141.5(12) . . ?
C37 O25 Ti2 132.2(12) 2_765 . ?
C37 O25 Gd2 129.4(12) 2_765 . ?
Ti2 O25 Gd2 98.1(4) . . ?
C37 O26 Ti2 137.8(15) . . ?
C2A C2 C2B 138(4) . . ?
C2A C2 O2 108(3) . . ?
C2B C2 O2 113(3) . . ?
C2A C2 H2A 93.9 . . ?
C2B C2 H2A 93.9 . . ?
O2 C2 H2A 93.9 . . ?
C2 C2A H2AA 109.5 . . ?
C2 C2A H2AB 109.5 . . ?
H2AA C2A H2AB 109.5 . . ?
C2 C2A H2AC 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
C2 C2B H2BA 109.5 . . ?
C2 C2B H2BB 109.5 . . ?
H2BA C2B H2BB 109.5 . . ?
C2 C2B H2BC 109.5 . . ?
H2BA C2B H2BC 109.5 . . ?
H2BB C2B H2BC 109.5 . . ?
C3B C3 O3 61(3) . . ?
C3B C3 C3A 112(3) . . ?
O3 C3 C3A 107(3) . . ?
C3B C3 H3 120.8 . . ?
O3 C3 H3 120.8 . . ?
C3A C3 H3 120.8 . . ?
C3 C3A H3AA 109.5 . . ?
C3 C3A H3AB 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
C3 C3A H3AC 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
C3 C3B O3 60.1(19) . . ?
C3 C3B H3BA 109.5 . . ?
O3 C3B H3BA 169.6 . . ?
C3 C3B H3BB 109.5 . . ?
O3 C3B H3BB 75.9 . . ?
H3BA C3B H3BB 109.5 . . ?
C3 C3B H3BC 109.5 . . ?
O3 C3B H3BC 75.9 . . ?
H3BA C3B H3BC 109.5 . . ?
H3BB C3B H3BC 109.5 . . ?
O3 C3' C3A' 114(4) . . ?
O3 C3' C3B' 107(4) . . ?
C3A' C3' C3B' 108(3) . . ?
O3 C3' H3A' 108.9 . . ?
C3A' C3' H3A' 108.9 . . ?
C3B' C3' H3A' 108.9 . . ?
C3' C3A' H3AD 109.5 . . ?
C3' C3A' H3AE 109.5 . . ?
H3AD C3A' H3AE 109.5 . . ?
C3' C3A' H3AF 109.5 . . ?
H3AD C3A' H3AF 109.5 . . ?
H3AE C3A' H3AF 109.5 . . ?
C3' C3B' H3BD 109.5 . . ?
C3' C3B' H3BE 109.5 . . ?
H3BD C3B' H3BE 109.5 . . ?
C3' C3B' H3BF 109.5 . . ?
H3BD C3B' H3BF 109.5 . . ?
H3BE C3B' H3BF 109.5 . . ?
O4 C11 C16 121.7(18) . . ?
O4 C11 C12 118(2) . . ?
C16 C11 C12 120(2) . . ?
C13 C12 C11 118(2) . . ?
C13 C12 H12A 121.0 . . ?
C11 C12 H12A 121.0 . . ?
C14 C13 C12 125(3) . . ?
C14 C13 H13A 117.5 . . ?
C12 C13 H13A 117.5 . . ?
C13 C14 C15 118(3) . . ?
C13 C14 H14A 120.8 . . ?
C15 C14 H14A 120.8 . . ?
C14 C15 C16 121(2) . . ?
C14 C15 H15A 119.5 . . ?
C16 C15 H15A 119.5 . . ?
C11 C16 C15 117.5(19) . . ?
C11 C16 C17 123.2(19) . 3_665 ?
C15 C16 C17 119.2(19) . 3_665 ?
O5 C17 O6 119.7(19) . 2_655 ?
O5 C17 C16 117.6(18) . 2_655 ?
O6 C17 C16 122.6(17) 2_655 2_655 ?
O22 C22 C22A 100(5) . . ?
O22 C22 C22B 113(4) . . ?
C22A C22 C22B 141(5) . . ?
O22 C22 H22' 98.0 . . ?
C22A C22 H22' 98.0 . . ?
C22B C22 H22' 98.0 . . ?
C22 C22A H22A 109.5 . . ?
C22 C22A H22B 109.5 . . ?
H22A C22A H22B 109.5 . . ?
C22 C22A H22C 109.5 . . ?
H22A C22A H22C 109.5 . . ?
H22B C22A H22C 109.5 . . ?
C22 C22B H22D 109.5 . . ?
C22 C22B H22E 109.5 . . ?
H22D C22B H22E 109.5 . . ?
C22 C22B H22F 109.5 . . ?
H22D C22B H22F 109.5 . . ?
H22E C22B H22F 109.5 . . ?
C23A C23 C23B 112(3) . . ?
C23A C23 O23 107(4) . . ?
C23B C23 O23 109(4) . . ?
C23A C23 H23A 109.6 . . ?
C23B C23 H23A 109.6 . . ?
O23 C23 H23A 109.6 . . ?
C23 C23A H23B 109.5 . . ?
C23 C23A H23C 109.5 . . ?
H23B C23A H23C 109.5 . . ?
C23 C23A H23D 109.5 . . ?
H23B C23A H23D 109.5 . . ?
H23C C23A H23D 109.5 . . ?
C23 C23B H23E 109.5 . . ?
C23 C23B H23F 109.5 . . ?
H23E C23B H23F 109.5 . . ?
C23 C23B H23G 109.5 . . ?
H23E C23B H23G 109.5 . . ?
H23F C23B H23G 109.5 . . ?
O23 C23' C23C 109(4) . . ?
O23 C23' C23D 127(5) . . ?
C23C C23' C23D 110(3) . . ?
O23 C23' H23H 102.4 . . ?
C23C C23' H23H 102.4 . . ?
C23D C23' H23H 102.4 . . ?
C23' C23C H23I 109.5 . . ?
C23' C23C H23J 109.5 . . ?
H23I C23C H23J 109.5 . . ?
C23' C23C H23K 109.5 . . ?
H23I C23C H23K 109.5 . . ?
H23J C23C H23K 109.5 . . ?
C23' C23D H23L 109.5 . . ?
C23' C23D H23M 109.5 . . ?
H23L C23D H23M 109.5 . . ?
C23' C23D H23N 109.5 . . ?
H23L C23D H23N 109.5 . . ?
H23M C23D H23N 109.5 . . ?
O24 C31 C32 120.0(18) . . ?
O24 C31 C36 121.4(15) . . ?
C32 C31 C36 118.6(18) . . ?
C31 C32 C33 122(2) . . ?
C31 C32 H32A 118.8 . . ?
C33 C32 H32A 118.8 . . ?
C34 C33 C32 118(2) . . ?
C34 C33 H33A 121.1 . . ?
C32 C33 H33A 121.1 . . ?
C33 C34 C35 122(2) . . ?
C33 C34 H34A 119.2 . . ?
C35 C34 H34A 119.2 . . ?
C34 C35 C36 119(2) . . ?
C34 C35 H35A 120.3 . . ?
C36 C35 H35A 120.3 . . ?
C35 C36 C31 119.8(18) . . ?
C35 C36 C37 117.8(19) . 2_765 ?
C31 C36 C37 121.9(17) . 2_765 ?
O26 C37 O25 124.2(19) . 3_675 ?
O26 C37 C36 114.9(18) . 3_675 ?
O25 C37 C36 120.7(18) 3_675 3_675 ?

_refine_diff_density_max         5.413
_refine_diff_density_min         -1.326
_refine_diff_density_rms         0.196

####################################################################### 
# 
# 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_nd_b
_database_code_depnum_ccdc_archive 'CCDC 1504167'
_audit_update_record             
;
2017-02-27 deposited with the CCDC.
2017-03-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT094_nd_b                
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       8.44 Report
RESPONSE: There is a large amount of residual electron density that did not resolve into anything meaningful. It is presumably disordered solvent, as the NMR and elemental analysis of the complex is in excellent agreement with the crystallographic formula.
;
# Added during the CSD deposition process: Monday 27 February 2017 10:24 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C69 H87 Nd O30 Ti6'
_chemical_formula_sum            'C69 H87 Nd O30 Ti6'
_chemical_formula_weight         1828.02

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -3.1807 10.9079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           174
_space_group_name_H-M_alt        'P -6'
_space_group_name_Hall           'P -6'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'

_cell_length_a                   14.9289(4)
_cell_length_b                   14.9289(4)
_cell_length_c                   23.5597(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4547.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9985
_cell_measurement_theta_min      3.4
_cell_measurement_theta_max      61.6

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_F_000             1866
_exptl_transmission_factor_min   0.792
_exptl_transmission_factor_max   1.00
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    9.130
_shelx_estimated_absorpt_T_min   0.341
_shelx_estimated_absorpt_T_max   0.407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.341
_exptl_absorpt_correction_T_max  0.407
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements (SADABS) 
;
_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         '30W microfocus sealed tube, Quazar optics'
_diffrn_measurement_device_type  'Bruker QUEST D8 CCD'
_diffrn_measurement_method       'Thin slice ω and φ scans'
_diffrn_reflns_number            26755
_diffrn_reflns_av_unetI/netI     0.0677
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.418
_diffrn_reflns_theta_max         61.253
_diffrn_reflns_theta_full        61.253
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             4755
_reflns_number_gt                4263
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.983
_reflns_Friedel_fraction_max     0.993
_reflns_Friedel_fraction_full    0.992

_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 software package, narrow-frames'
_computing_cell_refinement       'refinement of XYZ centroids > 20sigma(I)'
_computing_data_reduction        
;
 Bruker SAINT software package, narrow frame algorithm
;
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_refine_special_details          
;Refined as a 2-component twin. Residual electron density did not
resolve into anything meaningful but is presumably disordered solvent.
iPr ligands disordered but resolve acceptably when restrained and treated
 as isotropic., Twin
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1167P)²+0.5826P] 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_abs_structure_details 
;
 Flack x determined using 1864 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.024(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4755
_refine_ls_number_parameters     331
_refine_ls_number_restraints     212
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0603
_refine_ls_wR_factor_ref         0.1729
_refine_ls_wR_factor_gt          0.1638
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_restrained_S_all      1.109
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Nd1 Nd 0.666667 0.333333 0.500000 0.0214(7) Uani 1 6 d S T P . .
Nd2 Nd 1.000000 1.000000 1.000000 0.0217(7) Uani 1 6 d S T P . .
Ti1 Ti 0.4645(3) 0.3631(3) 0.56348(14) 0.0311(9) Uani 1 1 d . . . . .
Ti2 Ti 0.8082(3) 0.7612(3) 0.93666(13) 0.0313(8) Uani 1 1 d . . . . .
O1 O 0.4990(14) 0.3069(14) 0.500000 0.030(4) Uani 1 2 d S TU P . .
O2 O 0.4835(13) 0.4594(13) 0.500000 0.035(5) Uani 1 2 d S TU P C .
O3 O 0.3282(11) 0.2946(11) 0.5648(6) 0.046(4) Uani 1 1 d D U . . .
O4 O 0.4781(11) 0.4535(11) 0.6224(6) 0.050(4) Uani 1 1 d . U . . .
O5 O 0.4691(11) 0.2563(10) 0.6143(6) 0.038(3) Uani 1 1 d . U . . .
O6 O 0.6315(10) 0.4363(9) 0.5755(5) 0.032(3) Uani 1 1 d . U . . .
O21 O 0.8320(14) 0.8489(14) 1.000000 0.029(4) Uani 1 2 d S TU P . .
O22 O 0.8326(15) 0.6872(12) 1.000000 0.034(4) Uani 1 2 d S TU P G .
O23 O 0.6717(10) 0.6819(11) 0.9354(5) 0.036(3) Uani 1 1 d D U . . .
O24 O 0.8281(9) 0.6922(9) 0.8765(5) 0.034(3) Uani 1 1 d . U . . .
O25 O 0.9748(10) 0.8652(10) 0.9254(5) 0.029(3) Uani 1 1 d . U . . .
O26 O 0.8060(11) 0.8694(12) 0.8852(6) 0.038(4) Uani 1 1 d . U . . .
C2 C 0.479(3) 0.559(2) 0.500000 0.058(9) Uani 1 2 d S TU P . .
H2A H 0.466963 0.560159 0.541744 0.070 Uiso 0.5 1 calc R U P A -1
C2A C 0.588(3) 0.653(4) 0.500000 0.085(12) Uani 1 2 d S TU P C .
H2AA H 0.636015 0.632338 0.515321 0.128 Uiso 0.5 1 calc R U P B -1
H2AB H 0.607784 0.677929 0.461075 0.128 Uiso 0.5 1 calc R U P B -1
H2AC H 0.589459 0.707523 0.523604 0.128 Uiso 0.5 1 calc R U P B -1
C2B C 0.374(4) 0.542(4) 0.482(2) 0.072(18) Uani 0.5 1 d . U P C -1
H2BA H 0.321570 0.469352 0.489004 0.109 Uiso 0.5 1 calc R U P C -1
H2BB H 0.356995 0.586952 0.504167 0.109 Uiso 0.5 1 calc R U P C -1
H2BC H 0.375320 0.557358 0.441638 0.109 Uiso 0.5 1 calc R U P C -1
C3 C 0.247(3) 0.249(3) 0.6057(17) 0.081(12) Uiso 0.53(3) 1 d D U P D 1
H3 H 0.278942 0.250696 0.643153 0.097 Uiso 0.53(3) 1 calc R U P D 1
C3A C 0.194(3) 0.306(4) 0.612(2) 0.076(8) Uiso 0.53(3) 1 d D U P D 1
H3AA H 0.243807 0.378129 0.621202 0.114 Uiso 0.53(3) 1 calc R U P D 1
H3AB H 0.159104 0.303862 0.575986 0.114 Uiso 0.53(3) 1 calc R U P D 1
H3AC H 0.142313 0.275636 0.642102 0.114 Uiso 0.53(3) 1 calc R U P D 1
C3B C 0.180(3) 0.144(3) 0.592(2) 0.076(8) Uiso 0.53(3) 1 d D U P D 1
H3BA H 0.123902 0.112353 0.619973 0.114 Uiso 0.53(3) 1 calc R U P D 1
H3BB H 0.150164 0.138574 0.554113 0.114 Uiso 0.53(3) 1 calc R U P D 1
H3BC H 0.218768 0.106799 0.592106 0.114 Uiso 0.53(3) 1 calc R U P D 1
C3' C 0.220(2) 0.231(3) 0.557(2) 0.081(12) Uiso 0.47(3) 1 d D U P D 2
H3A' H 0.205604 0.250440 0.519154 0.097 Uiso 0.47(3) 1 calc R U P D 2
C3A' C 0.162(3) 0.255(4) 0.596(2) 0.076(8) Uiso 0.47(3) 1 d D U P D 2
H3AD H 0.189794 0.329572 0.596752 0.114 Uiso 0.47(3) 1 calc R U P D 2
H3AE H 0.089268 0.220440 0.583362 0.114 Uiso 0.47(3) 1 calc R U P D 2
H3AF H 0.165407 0.230034 0.633787 0.114 Uiso 0.47(3) 1 calc R U P D 2
C3B' C 0.185(3) 0.124(3) 0.553(3) 0.076(8) Uiso 0.47(3) 1 d D U P D 2
H3BD H 0.227935 0.113146 0.526012 0.114 Uiso 0.47(3) 1 calc R U P D 2
H3BE H 0.188918 0.097696 0.590425 0.114 Uiso 0.47(3) 1 calc R U P D 2
H3BF H 0.112779 0.088102 0.539999 0.114 Uiso 0.47(3) 1 calc R U P D 2
C11 C 0.5517(17) 0.5290(15) 0.6545(9) 0.041(5) Uani 1 1 d . U . . .
C12 C 0.521(2) 0.5801(18) 0.6926(8) 0.051(6) Uani 1 1 d . U . . .
H12A H 0.451898 0.566490 0.694217 0.061 Uiso 1 1 calc R U . . .
C13 C 0.597(2) 0.652(2) 0.7279(11) 0.071(8) Uani 1 1 d . U . . .
H13A H 0.576586 0.684171 0.755563 0.085 Uiso 1 1 calc R U . . .
C14 C 0.692(2) 0.678(2) 0.7269(11) 0.064(7) Uani 1 1 d . U . . .
H14A H 0.739001 0.729059 0.752720 0.077 Uiso 1 1 calc R U . . .
C15 C 0.7276(19) 0.6333(18) 0.6879(9) 0.052(6) Uani 1 1 d . U . . .
H15A H 0.799282 0.655815 0.684928 0.063 Uiso 1 1 calc R U . . .
C16 C 0.6545(17) 0.5531(16) 0.6528(8) 0.037(5) Uani 1 1 d . U . . .
C17 C 0.4951(16) 0.1895(17) 0.6128(9) 0.032(5) Uani 1 1 d . U . . .
C22 C 0.835(3) 0.592(3) 1.000000 0.060(9) Uani 1 2 d S TU P . .
H22' H 0.821923 0.576705 0.958548 0.073 Uiso 0.5 1 calc R U P E -1
C22A C 0.951(5) 0.632(5) 1.000000 0.14(2) Uani 1 2 d S TU P G .
H22A H 0.987375 0.699605 0.981399 0.207 Uiso 0.5 1 calc R U P F -1
H22B H 0.975510 0.638312 1.039201 0.207 Uiso 0.5 1 calc R U P F -1
H22C H 0.964796 0.582964 0.979401 0.207 Uiso 0.5 1 calc R U P F -1
C22B C 0.751(6) 0.504(4) 1.020(2) 0.092(18) Uani 0.5 1 d . U P G -1
H22D H 0.763730 0.446357 1.017227 0.139 Uiso 0.5 1 calc R U P G -1
H22E H 0.738366 0.514337 1.059746 0.139 Uiso 0.5 1 calc R U P G -1
H22F H 0.689596 0.489177 0.997316 0.139 Uiso 0.5 1 calc R U P G -1
C23 C 0.600(3) 0.639(3) 0.8879(15) 0.066(10) Uiso 0.54(2) 1 d D U P H 1
H23A H 0.636010 0.673978 0.851942 0.079 Uiso 0.54(2) 1 calc R U P H 1
C23A C 0.508(4) 0.649(4) 0.895(2) 0.086(9) Uiso 0.54(2) 1 d D U P H 1
H23B H 0.462127 0.618777 0.862645 0.130 Uiso 0.54(2) 1 calc R U P H 1
H23C H 0.471447 0.612145 0.930000 0.130 Uiso 0.54(2) 1 calc R U P H 1
H23D H 0.528924 0.722075 0.898819 0.130 Uiso 0.54(2) 1 calc R U P H 1
C23B C 0.561(4) 0.527(3) 0.883(2) 0.086(9) Uiso 0.54(2) 1 d D U P H 1
H23E H 0.512868 0.499262 0.850691 0.130 Uiso 0.54(2) 1 calc R U P H 1
H23F H 0.618922 0.514992 0.876544 0.130 Uiso 0.54(2) 1 calc R U P H 1
H23G H 0.524709 0.492250 0.917808 0.130 Uiso 0.54(2) 1 calc R U P H 1
C23' C 0.563(2) 0.633(4) 0.939(2) 0.066(10) Uiso 0.46(2) 1 d D U P H 2
H23H H 0.537714 0.592086 0.974968 0.079 Uiso 0.46(2) 1 calc R U P H 2
C23C C 0.556(6) 0.723(4) 0.942(3) 0.086(9) Uiso 0.46(2) 1 d D U P H 2
H23I H 0.482660 0.704281 0.944686 0.130 Uiso 0.46(2) 1 calc R U P H 2
H23J H 0.592930 0.763406 0.975442 0.130 Uiso 0.46(2) 1 calc R U P H 2
H23K H 0.585964 0.764853 0.907695 0.130 Uiso 0.46(2) 1 calc R U P H 2
C23D C 0.507(5) 0.570(4) 0.891(2) 0.086(9) Uiso 0.46(2) 1 d D U P H 2
H23L H 0.432109 0.539333 0.897789 0.130 Uiso 0.46(2) 1 calc R U P H 2
H23M H 0.525971 0.612803 0.856824 0.130 Uiso 0.46(2) 1 calc R U P H 2
H23N H 0.523054 0.514531 0.885945 0.130 Uiso 0.46(2) 1 calc R U P H 2
C31 C 0.9045(17) 0.6988(16) 0.8432(8) 0.042(5) Uani 1 1 d . U . . .
C32 C 0.8789(18) 0.6200(18) 0.8028(9) 0.052(6) Uani 1 1 d . U . . .
H32A H 0.810018 0.563590 0.800996 0.063 Uiso 1 1 calc R U . . .
C33 C 0.952(2) 0.624(2) 0.7662(9) 0.060(7) Uani 1 1 d . U . . .
H33A H 0.931864 0.570974 0.738337 0.072 Uiso 1 1 calc R U . . .
C34 C 1.061(2) 0.709(2) 0.7693(11) 0.073(8) Uani 1 1 d . U . . .
H34A H 1.113387 0.710514 0.745588 0.087 Uiso 1 1 calc R U . . .
C35 C 1.082(2) 0.7839(18) 0.8084(9) 0.051(6) Uani 1 1 d . U . . .
H35A H 1.149117 0.842780 0.809275 0.061 Uiso 1 1 calc R U . . .
C36 C 1.0069(16) 0.7785(16) 0.8481(10) 0.038(5) Uani 1 1 d . U . . .
C37 C 0.8256(18) 0.9622(18) 0.8901(10) 0.035(5) Uani 1 1 d . 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
Nd1 O1 2.332(18) 2_655 ?
Nd1 O1 2.332(18) . ?
Nd1 O1 2.332(18) 3_665 ?
Nd1 O6 2.571(12) . ?
Nd1 O6 2.571(12) 3_665 ?
Nd1 O6 2.571(12) 5_656 ?
Nd1 O6 2.571(12) 6_666 ?
Nd1 O6 2.571(12) 2_655 ?
Nd1 O6 2.571(12) 4_556 ?
Nd1 Ti1 3.589(3) 4_556 ?
Nd1 Ti1 3.589(3) 3_665 ?
Nd1 Ti1 3.589(3) 6_666 ?
Nd2 O21 2.391(18) 3_675 ?
Nd2 O21 2.391(18) 2_765 ?
Nd2 O21 2.391(19) . ?
Nd2 O25 2.554(11) . ?
Nd2 O25 2.554(11) 5_767 ?
Nd2 O25 2.554(11) 3_675 ?
Nd2 O25 2.554(11) 6_677 ?
Nd2 O25 2.554(11) 2_765 ?
Nd2 O25 2.554(11) 4_557 ?
Nd2 Ti2 3.596(3) 5_767 ?
Nd2 Ti2 3.596(3) 4_557 ?
Nd2 Ti2 3.596(3) 6_677 ?
Ti1 O3 1.763(14) . ?
Ti1 O4 1.875(14) . ?
Ti1 O1 1.906(11) . ?
Ti1 O2 1.995(11) . ?
Ti1 O5 2.022(14) . ?
Ti1 O6 2.183(14) . ?
Ti1 Ti1 2.991(7) 4_556 ?
Ti2 O23 1.773(13) . ?
Ti2 O24 1.861(12) . ?
Ti2 O21 1.898(12) . ?
Ti2 O22 1.995(13) . ?
Ti2 O26 2.033(15) . ?
Ti2 O25 2.192(14) . ?
Ti2 Ti2 2.985(6) 4_557 ?
O2 C2 1.53(4) . ?
O3 C3' 1.42(3) . ?
O3 C3 1.43(3) . ?
O4 C11 1.35(2) . ?
O5 C17 1.24(3) . ?
O6 C17 1.32(2) 3_665 ?
O22 C22 1.43(4) . ?
O23 C23' 1.41(3) . ?
O23 C23 1.46(3) . ?
O24 C31 1.35(2) . ?
O25 C37 1.27(3) 2_765 ?
O26 C37 1.27(2) . ?
C2 C2B 1.51(6) . ?
C2 C2A 1.52(6) . ?
C2 H2A 1.0000 . ?
C2A H2AA 0.9800 . ?
C2A H2AB 0.9800 . ?
C2A H2AC 0.9800 . ?
C2B H2BA 0.9800 . ?
C2B H2BB 0.9800 . ?
C2B H2BC 0.9800 . ?
C3 C3B 1.41(3) . ?
C3 C3A 1.43(3) . ?
C3 H3 1.0000 . ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?
C3A H3AC 0.9800 . ?
C3B H3BA 0.9800 . ?
C3B H3BB 0.9800 . ?
C3B H3BC 0.9800 . ?
C3' C3B' 1.41(3) . ?
C3' C3A' 1.42(3) . ?
C3' H3A' 1.0000 . ?
C3A' H3AD 0.9800 . ?
C3A' H3AE 0.9800 . ?
C3A' H3AF 0.9800 . ?
C3B' H3BD 0.9800 . ?
C3B' H3BE 0.9800 . ?
C3B' H3BF 0.9800 . ?
C11 C16 1.39(3) . ?
C11 C12 1.39(3) . ?
C12 C13 1.38(4) . ?
C12 H12A 0.9500 . ?
C13 C14 1.26(4) . ?
C13 H13A 0.9500 . ?
C14 C15 1.39(3) . ?
C14 H14A 0.9500 . ?
C15 C16 1.42(3) . ?
C15 H15A 0.9500 . ?
C16 C17 1.48(3) 3_665 ?
C22 C22B 1.37(7) . ?
C22 C22A 1.53(7) . ?
C22 H22' 1.0000 . ?
C22A H22A 0.9800 . ?
C22A H22B 0.9800 . ?
C22A H22C 0.9800 . ?
C22B H22D 0.9800 . ?
C22B H22E 0.9800 . ?
C22B H22F 0.9800 . ?
C23 C23A 1.47(3) . ?
C23 C23B 1.47(3) . ?
C23 H23A 1.0000 . ?
C23A H23B 0.9800 . ?
C23A H23C 0.9800 . ?
C23A H23D 0.9800 . ?
C23B H23E 0.9800 . ?
C23B H23F 0.9800 . ?
C23B H23G 0.9800 . ?
C23' C23C 1.41(3) . ?
C23' C23D 1.44(3) . ?
C23' H23H 1.0000 . ?
C23C H23I 0.9800 . ?
C23C H23J 0.9800 . ?
C23C H23K 0.9800 . ?
C23D H23L 0.9800 . ?
C23D H23M 0.9800 . ?
C23D H23N 0.9800 . ?
C31 C36 1.40(3) . ?
C31 C32 1.41(3) . ?
C32 C33 1.37(3) . ?
C32 H32A 0.9500 . ?
C33 C34 1.49(4) . ?
C33 H33A 0.9500 . ?
C34 C35 1.36(3) . ?
C34 H34A 0.9500 . ?
C35 C36 1.43(3) . ?
C35 H35A 0.9500 . ?
C36 C37 1.49(3) 2_765 ?

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 Nd1 O1 120.000(3) 2_655 . ?
O1 Nd1 O1 120.002(3) 2_655 3_665 ?
O1 Nd1 O1 119.998(2) . 3_665 ?
O1 Nd1 O6 135.9(3) 2_655 . ?
O1 Nd1 O6 65.1(4) . . ?
O1 Nd1 O6 72.7(4) 3_665 . ?
O1 Nd1 O6 72.7(4) 2_655 3_665 ?
O1 Nd1 O6 135.9(3) . 3_665 ?
O1 Nd1 O6 65.1(4) 3_665 3_665 ?
O6 Nd1 O6 77.4(4) . 3_665 ?
O1 Nd1 O6 65.1(4) 2_655 5_656 ?
O1 Nd1 O6 72.7(4) . 5_656 ?
O1 Nd1 O6 135.9(3) 3_665 5_656 ?
O6 Nd1 O6 137.7(2) . 5_656 ?
O6 Nd1 O6 137.68(19) 3_665 5_656 ?
O1 Nd1 O6 72.7(4) 2_655 6_666 ?
O1 Nd1 O6 135.9(3) . 6_666 ?
O1 Nd1 O6 65.1(4) 3_665 6_666 ?
O6 Nd1 O6 137.7(2) . 6_666 ?
O6 Nd1 O6 87.6(5) 3_665 6_666 ?
O6 Nd1 O6 77.4(4) 5_656 6_666 ?
O1 Nd1 O6 65.1(4) 2_655 2_655 ?
O1 Nd1 O6 72.7(4) . 2_655 ?
O1 Nd1 O6 135.9(3) 3_665 2_655 ?
O6 Nd1 O6 77.4(4) . 2_655 ?
O6 Nd1 O6 77.4(4) 3_665 2_655 ?
O6 Nd1 O6 87.6(5) 5_656 2_655 ?
O6 Nd1 O6 137.68(19) 6_666 2_655 ?
O1 Nd1 O6 135.9(3) 2_655 4_556 ?
O1 Nd1 O6 65.1(4) . 4_556 ?
O1 Nd1 O6 72.7(4) 3_665 4_556 ?
O6 Nd1 O6 87.6(5) . 4_556 ?
O6 Nd1 O6 137.7(2) 3_665 4_556 ?
O6 Nd1 O6 77.4(4) 5_656 4_556 ?
O6 Nd1 O6 77.4(4) 6_666 4_556 ?
O6 Nd1 O6 137.7(2) 2_655 4_556 ?
O1 Nd1 Ti1 130.2(4) 2_655 4_556 ?
O1 Nd1 Ti1 28.7(2) . 4_556 ?
O1 Nd1 Ti1 103.4(4) 3_665 4_556 ?
O6 Nd1 Ti1 77.2(3) . 4_556 ?
O6 Nd1 Ti1 154.3(3) 3_665 4_556 ?
O6 Nd1 Ti1 66.9(3) 5_656 4_556 ?
O6 Nd1 Ti1 108.9(3) 6_666 4_556 ?
O6 Nd1 Ti1 100.7(3) 2_655 4_556 ?
O6 Nd1 Ti1 37.1(3) 4_556 4_556 ?
O1 Nd1 Ti1 103.4(4) 2_655 3_665 ?
O1 Nd1 Ti1 130.2(4) . 3_665 ?
O1 Nd1 Ti1 28.7(2) 3_665 3_665 ?
O6 Nd1 Ti1 66.9(3) . 3_665 ?
O6 Nd1 Ti1 37.1(3) 3_665 3_665 ?
O6 Nd1 Ti1 154.3(3) 5_656 3_665 ?
O6 Nd1 Ti1 77.2(3) 6_666 3_665 ?
O6 Nd1 Ti1 108.9(3) 2_655 3_665 ?
O6 Nd1 Ti1 100.7(3) 4_556 3_665 ?
Ti1 Nd1 Ti1 125.93(3) 4_556 3_665 ?
O1 Nd1 Ti1 103.4(4) 2_655 6_666 ?
O1 Nd1 Ti1 130.2(4) . 6_666 ?
O1 Nd1 Ti1 28.7(2) 3_665 6_666 ?
O6 Nd1 Ti1 100.7(3) . 6_666 ?
O6 Nd1 Ti1 77.2(3) 3_665 6_666 ?
O6 Nd1 Ti1 108.9(3) 5_656 6_666 ?
O6 Nd1 Ti1 37.1(3) 6_666 6_666 ?
O6 Nd1 Ti1 154.3(3) 2_655 6_666 ?
O6 Nd1 Ti1 66.9(3) 4_556 6_666 ?
Ti1 Nd1 Ti1 103.86(6) 4_556 6_666 ?
Ti1 Nd1 Ti1 49.26(11) 3_665 6_666 ?
O21 Nd2 O21 120.000(17) 3_675 2_765 ?
O21 Nd2 O21 120.000(7) 3_675 . ?
O21 Nd2 O21 120.000(6) 2_765 . ?
O21 Nd2 O25 136.3(3) 3_675 . ?
O21 Nd2 O25 72.1(4) 2_765 . ?
O21 Nd2 O25 65.5(4) . . ?
O21 Nd2 O25 72.1(4) 3_675 5_767 ?
O21 Nd2 O25 65.5(4) 2_765 5_767 ?
O21 Nd2 O25 136.3(3) . 5_767 ?
O25 Nd2 O25 137.5(2) . 5_767 ?
O21 Nd2 O25 65.5(4) 3_675 3_675 ?
O21 Nd2 O25 136.3(3) 2_765 3_675 ?
O21 Nd2 O25 72.1(4) . 3_675 ?
O25 Nd2 O25 77.8(4) . 3_675 ?
O25 Nd2 O25 137.5(2) 5_767 3_675 ?
O21 Nd2 O25 65.5(4) 3_675 6_677 ?
O21 Nd2 O25 136.3(3) 2_765 6_677 ?
O21 Nd2 O25 72.1(4) . 6_677 ?
O25 Nd2 O25 137.5(2) . 6_677 ?
O25 Nd2 O25 77.8(4) 5_767 6_677 ?
O25 Nd2 O25 87.0(6) 3_675 6_677 ?
O21 Nd2 O25 72.1(4) 3_675 2_765 ?
O21 Nd2 O25 65.5(4) 2_765 2_765 ?
O21 Nd2 O25 136.3(3) . 2_765 ?
O25 Nd2 O25 77.8(4) . 2_765 ?
O25 Nd2 O25 87.0(6) 5_767 2_765 ?
O25 Nd2 O25 77.8(4) 3_675 2_765 ?
O25 Nd2 O25 137.5(2) 6_677 2_765 ?
O21 Nd2 O25 136.3(3) 3_675 4_557 ?
O21 Nd2 O25 72.1(4) 2_765 4_557 ?
O21 Nd2 O25 65.5(4) . 4_557 ?
O25 Nd2 O25 87.0(6) . 4_557 ?
O25 Nd2 O25 77.8(4) 5_767 4_557 ?
O25 Nd2 O25 137.5(2) 3_675 4_557 ?
O25 Nd2 O25 77.8(4) 6_677 4_557 ?
O25 Nd2 O25 137.5(2) 2_765 4_557 ?
O21 Nd2 Ti2 102.8(4) 3_675 5_767 ?
O21 Nd2 Ti2 29.0(3) 2_765 5_767 ?
O21 Nd2 Ti2 130.8(4) . 5_767 ?
O25 Nd2 Ti2 100.4(3) . 5_767 ?
O25 Nd2 Ti2 37.1(3) 5_767 5_767 ?
O25 Nd2 Ti2 154.5(3) 3_675 5_767 ?
O25 Nd2 Ti2 109.3(3) 6_677 5_767 ?
O25 Nd2 Ti2 76.9(3) 2_765 5_767 ?
O25 Nd2 Ti2 67.0(3) 4_557 5_767 ?
O21 Nd2 Ti2 130.8(4) 3_675 4_557 ?
O21 Nd2 Ti2 102.8(4) 2_765 4_557 ?
O21 Nd2 Ti2 29.0(2) . 4_557 ?
O25 Nd2 Ti2 76.9(3) . 4_557 ?
O25 Nd2 Ti2 109.3(3) 5_767 4_557 ?
O25 Nd2 Ti2 100.4(3) 3_675 4_557 ?
O25 Nd2 Ti2 67.0(3) 6_677 4_557 ?
O25 Nd2 Ti2 154.5(3) 2_765 4_557 ?
O25 Nd2 Ti2 37.1(3) 4_557 4_557 ?
Ti2 Nd2 Ti2 103.98(6) 5_767 4_557 ?
O21 Nd2 Ti2 29.0(2) 3_675 6_677 ?
O21 Nd2 Ti2 130.8(4) 2_765 6_677 ?
O21 Nd2 Ti2 102.8(4) . 6_677 ?
O25 Nd2 Ti2 154.5(3) . 6_677 ?
O25 Nd2 Ti2 67.0(3) 5_767 6_677 ?
O25 Nd2 Ti2 76.9(3) 3_675 6_677 ?
O25 Nd2 Ti2 37.1(3) 6_677 6_677 ?
O25 Nd2 Ti2 100.4(3) 2_765 6_677 ?
O25 Nd2 Ti2 109.3(3) 4_557 6_677 ?
Ti2 Nd2 Ti2 103.98(6) 5_767 6_677 ?
Ti2 Nd2 Ti2 103.98(6) 4_557 6_677 ?
O3 Ti1 O4 94.7(7) . . ?
O3 Ti1 O1 104.2(7) . . ?
O4 Ti1 O1 160.3(7) . . ?
O3 Ti1 O2 97.9(7) . . ?
O4 Ti1 O2 96.3(6) . . ?
O1 Ti1 O2 75.9(6) . . ?
O3 Ti1 O5 91.0(6) . . ?
O4 Ti1 O5 95.5(6) . . ?
O1 Ti1 O5 89.7(6) . . ?
O2 Ti1 O5 164.5(6) . . ?
O3 Ti1 O6 170.5(5) . . ?
O4 Ti1 O6 81.9(6) . . ?
O1 Ti1 O6 80.2(6) . . ?
O2 Ti1 O6 91.2(6) . . ?
O5 Ti1 O6 80.7(5) . . ?
O3 Ti1 Ti1 91.0(5) . 4_556 ?
O4 Ti1 Ti1 137.7(5) . 4_556 ?
O1 Ti1 Ti1 38.3(4) . 4_556 ?
O2 Ti1 Ti1 41.4(4) . 4_556 ?
O5 Ti1 Ti1 126.3(4) . 4_556 ?
O6 Ti1 Ti1 97.5(3) . 4_556 ?
O3 Ti1 Nd1 137.2(5) . . ?
O4 Ti1 Nd1 127.1(5) . . ?
O1 Ti1 Nd1 35.9(5) . . ?
O2 Ti1 Nd1 87.2(4) . . ?
O5 Ti1 Nd1 77.7(4) . . ?
O6 Ti1 Nd1 45.2(3) . . ?
Ti1 Ti1 Nd1 65.37(5) 4_556 . ?
O23 Ti2 O24 93.8(6) . . ?
O23 Ti2 O21 103.3(7) . . ?
O24 Ti2 O21 162.5(7) . . ?
O23 Ti2 O22 96.3(7) . . ?
O24 Ti2 O22 98.1(6) . . ?
O21 Ti2 O22 76.7(6) . . ?
O23 Ti2 O26 92.9(6) . . ?
O24 Ti2 O26 93.2(6) . . ?
O21 Ti2 O26 89.6(6) . . ?
O22 Ti2 O26 165.0(6) . . ?
O23 Ti2 O25 171.6(5) . . ?
O24 Ti2 O25 82.0(5) . . ?
O21 Ti2 O25 81.5(6) . . ?
O22 Ti2 O25 91.5(6) . . ?
O26 Ti2 O25 80.1(6) . . ?
O23 Ti2 Ti2 90.9(4) . 4_557 ?
O24 Ti2 Ti2 139.6(4) . 4_557 ?
O21 Ti2 Ti2 38.2(5) . 4_557 ?
O22 Ti2 Ti2 41.6(4) . 4_557 ?
O26 Ti2 Ti2 126.6(4) . 4_557 ?
O25 Ti2 Ti2 97.0(3) . 4_557 ?
O23 Ti2 Nd2 138.4(5) . . ?
O24 Ti2 Nd2 126.6(4) . . ?
O21 Ti2 Nd2 37.6(5) . . ?
O22 Ti2 Nd2 87.9(4) . . ?
O26 Ti2 Nd2 77.4(4) . . ?
O25 Ti2 Nd2 44.7(3) . . ?
Ti2 Ti2 Nd2 65.48(5) 4_557 . ?
Ti1 O1 Ti1 103.4(9) 4_556 . ?
Ti1 O1 Nd1 115.4(6) 4_556 . ?
Ti1 O1 Nd1 115.4(6) . . ?
C2 O2 Ti1 130.1(5) . . ?
C2 O2 Ti1 130.1(5) . 4_556 ?
Ti1 O2 Ti1 97.1(7) . 4_556 ?
C3' O3 Ti1 170(2) . . ?
C3 O3 Ti1 139(2) . . ?
C11 O4 Ti1 140.1(13) . . ?
C17 O5 Ti1 140.0(15) . . ?
C17 O6 Ti1 131.8(13) 3_665 . ?
C17 O6 Nd1 130.3(13) 3_665 . ?
Ti1 O6 Nd1 97.7(4) . . ?
Ti2 O21 Ti2 103.7(9) 4_557 . ?
Ti2 O21 Nd2 113.4(6) 4_557 . ?
Ti2 O21 Nd2 113.4(6) . . ?
C22 O22 Ti2 130.3(5) . 4_557 ?
C22 O22 Ti2 130.3(5) . . ?
Ti2 O22 Ti2 96.8(8) 4_557 . ?
C23' O23 Ti2 171(2) . . ?
C23 O23 Ti2 130.7(18) . . ?
C31 O24 Ti2 140.1(12) . . ?
C37 O25 Ti2 131.0(13) 2_765 . ?
C37 O25 Nd2 130.6(13) 2_765 . ?
Ti2 O25 Nd2 98.2(4) . . ?
C37 O26 Ti2 136.5(17) . . ?
C2B C2 C2A 134(3) . . ?
C2B C2 O2 112(3) . . ?
C2A C2 O2 110(3) . . ?
C2B C2 H2A 96.0 . . ?
C2A C2 H2A 96.0 . . ?
O2 C2 H2A 96.0 . . ?
C2 C2A H2AA 109.5 . . ?
C2 C2A H2AB 109.5 . . ?
H2AA C2A H2AB 109.5 . . ?
C2 C2A H2AC 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
C2 C2B H2BA 109.5 . . ?
C2 C2B H2BB 109.5 . . ?
H2BA C2B H2BB 109.5 . . ?
C2 C2B H2BC 109.5 . . ?
H2BA C2B H2BC 109.5 . . ?
H2BB C2B H2BC 109.5 . . ?
C3B C3 O3 110(3) . . ?
C3B C3 C3A 113(3) . . ?
O3 C3 C3A 112(3) . . ?
C3B C3 H3 107.3 . . ?
O3 C3 H3 107.3 . . ?
C3A C3 H3 107.3 . . ?
C3 C3A H3AA 109.5 . . ?
C3 C3A H3AB 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
C3 C3A H3AC 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
C3 C3B H3BA 109.5 . . ?
C3 C3B H3BB 109.5 . . ?
H3BA C3B H3BB 109.5 . . ?
C3 C3B H3BC 109.5 . . ?
H3BA C3B H3BC 109.5 . . ?
H3BB C3B H3BC 109.5 . . ?
C3B' C3' C3A' 113(3) . . ?
C3B' C3' O3 115(3) . . ?
C3A' C3' O3 113(3) . . ?
C3B' C3' H3A' 104.7 . . ?
C3A' C3' H3A' 104.7 . . ?
O3 C3' H3A' 104.7 . . ?
C3' C3A' H3AD 109.5 . . ?
C3' C3A' H3AE 109.5 . . ?
H3AD C3A' H3AE 109.5 . . ?
C3' C3A' H3AF 109.5 . . ?
H3AD C3A' H3AF 109.5 . . ?
H3AE C3A' H3AF 109.5 . . ?
C3' C3B' H3BD 109.5 . . ?
C3' C3B' H3BE 109.5 . . ?
H3BD C3B' H3BE 109.5 . . ?
C3' C3B' H3BF 109.5 . . ?
H3BD C3B' H3BF 109.5 . . ?
H3BE C3B' H3BF 109.5 . . ?
O4 C11 C16 122.2(18) . . ?
O4 C11 C12 118(2) . . ?
C16 C11 C12 120(2) . . ?
C13 C12 C11 116(3) . . ?
C13 C12 H12A 121.8 . . ?
C11 C12 H12A 121.8 . . ?
C14 C13 C12 126(3) . . ?
C14 C13 H13A 117.0 . . ?
C12 C13 H13A 117.0 . . ?
C13 C14 C15 120(3) . . ?
C13 C14 H14A 120.0 . . ?
C15 C14 H14A 120.0 . . ?
C14 C15 C16 118(2) . . ?
C14 C15 H15A 120.8 . . ?
C16 C15 H15A 120.8 . . ?
C11 C16 C15 119(2) . . ?
C11 C16 C17 123.6(19) . 3_665 ?
C15 C16 C17 117(2) . 3_665 ?
O5 C17 O6 121(2) . 2_655 ?
O5 C17 C16 119.3(19) . 2_655 ?
O6 C17 C16 119.9(19) 2_655 2_655 ?
C22B C22 O22 119(4) . . ?
C22B C22 C22A 134(5) . . ?
O22 C22 C22A 102(4) . . ?
C22B C22 H22' 97.8 . . ?
O22 C22 H22' 97.8 . . ?
C22A C22 H22' 97.8 . . ?
C22 C22A H22A 109.5 . . ?
C22 C22A H22B 109.5 . . ?
H22A C22A H22B 109.5 . . ?
C22 C22A H22C 109.5 . . ?
H22A C22A H22C 109.5 . . ?
H22B C22A H22C 109.5 . . ?
C22 C22B H22D 109.5 . . ?
C22 C22B H22E 109.5 . . ?
H22D C22B H22E 109.5 . . ?
C22 C22B H22F 109.5 . . ?
H22D C22B H22F 109.5 . . ?
H22E C22B H22F 109.5 . . ?
O23 C23 C23A 112(3) . . ?
O23 C23 C23B 111(3) . . ?
C23A C23 C23B 105(2) . . ?
O23 C23 H23A 109.5 . . ?
C23A C23 H23A 109.5 . . ?
C23B C23 H23A 109.5 . . ?
C23 C23A H23B 109.5 . . ?
C23 C23A H23C 109.5 . . ?
H23B C23A H23C 109.5 . . ?
C23 C23A H23D 109.5 . . ?
H23B C23A H23D 109.5 . . ?
H23C C23A H23D 109.5 . . ?
C23 C23B H23E 109.5 . . ?
C23 C23B H23F 109.5 . . ?
H23E C23B H23F 109.5 . . ?
C23 C23B H23G 109.5 . . ?
H23E C23B H23G 109.5 . . ?
H23F C23B H23G 109.5 . . ?
O23 C23' C23C 97(4) . . ?
O23 C23' C23D 116(4) . . ?
C23C C23' C23D 111(3) . . ?
O23 C23' H23H 110.6 . . ?
C23C C23' H23H 110.6 . . ?
C23D C23' H23H 110.6 . . ?
C23' C23C H23I 109.5 . . ?
C23' C23C H23J 109.5 . . ?
H23I C23C H23J 109.5 . . ?
C23' C23C H23K 109.5 . . ?
H23I C23C H23K 109.5 . . ?
H23J C23C H23K 109.5 . . ?
C23' C23D H23L 109.5 . . ?
C23' C23D H23M 109.5 . . ?
H23L C23D H23M 109.5 . . ?
C23' C23D H23N 109.5 . . ?
H23L C23D H23N 109.5 . . ?
H23M C23D H23N 109.5 . . ?
O24 C31 C36 122.8(17) . . ?
O24 C31 C32 117.8(19) . . ?
C36 C31 C32 119(2) . . ?
C33 C32 C31 121(2) . . ?
C33 C32 H32A 119.5 . . ?
C31 C32 H32A 119.5 . . ?
C32 C33 C34 121(2) . . ?
C32 C33 H33A 119.6 . . ?
C34 C33 H33A 119.6 . . ?
C35 C34 C33 116(2) . . ?
C35 C34 H34A 122.1 . . ?
C33 C34 H34A 122.1 . . ?
C34 C35 C36 123(2) . . ?
C34 C35 H35A 118.4 . . ?
C36 C35 H35A 118.4 . . ?
C31 C36 C35 119(2) . . ?
C31 C36 C37 121.4(19) . 2_765 ?
C35 C36 C37 119(2) . 2_765 ?
O25 C37 O26 123(2) 3_675 . ?
O25 C37 C36 122.5(19) 3_675 3_675 ?
O26 C37 C36 114(2) . 3_675 ?

_refine_diff_density_max         4.636
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.159

####################################################################### 
# 
# 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_pr_c
_database_code_depnum_ccdc_archive 'CCDC 1504170'
_audit_update_record             
;
2017-02-27 deposited with the CCDC.
2017-03-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C69 H87 O30 Pr Ti6'
_chemical_formula_sum            'C69 H87 O30 Pr Ti6'
_chemical_formula_weight         1824.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -2.4164 10.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           174
_space_group_name_H-M_alt        'P -6'
_space_group_name_Hall           'P -6'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'

_cell_length_a                   14.9478(6)
_cell_length_b                   14.9478(6)
_cell_length_c                   23.5581(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4558.5(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9476
_cell_measurement_theta_min      3.31
_cell_measurement_theta_max      64.2

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_F_000             1864
_exptl_transmission_factor_min   0.726
_exptl_transmission_factor_max   1.000
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    8.862
_shelx_estimated_absorpt_T_min   0.270
_shelx_estimated_absorpt_T_max   0.370
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.270
_exptl_absorpt_correction_T_max  0.370
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements (SADABS) 
;
_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         '30W microfocus sealed tube, Quazar optics'
_diffrn_measurement_device_type  'Bruker QUEST D8 CCD'
_diffrn_measurement_method       'Thin slice ω and φ scans'
_diffrn_reflns_number            39041
_diffrn_reflns_av_unetI/netI     0.0603
_diffrn_reflns_av_R_equivalents  0.1004
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.414
_diffrn_reflns_theta_max         65.308
_diffrn_reflns_theta_full        65.308
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             5331
_reflns_number_gt                4840
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.984
_reflns_Friedel_fraction_max     0.993
_reflns_Friedel_fraction_full    0.993

_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 software package, narrow-frames'
_computing_cell_refinement       'refinement of XYZ centroids > 20sigma(I)'
_computing_data_reduction        
;
 Bruker SAINT software package, narrow frame algorithm
;
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_refine_special_details          
;Refined as a 2-component twin. Residual electron density did not resolve 
into anything meaningful and is presumably disordered solvent. iPr ligands 
modelled by dfixing and keeping isotropic., Twin
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1525P)²+10.9642P] 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_abs_structure_details 
;
 Flack x determined using 2158 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.037(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5331
_refine_ls_number_parameters     331
_refine_ls_number_restraints     208
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0792
_refine_ls_wR_factor_ref         0.2215
_refine_ls_wR_factor_gt          0.2114
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_restrained_S_all      1.120
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Pr1 Pr 0.666667 0.333333 0.500000 0.0184(8) Uani 1 6 d S T P . .
Pr2 Pr 1.000000 1.000000 1.000000 0.0177(8) Uani 1 6 d S T P . .
Ti1 Ti 0.4649(3) 0.3640(3) 0.56378(16) 0.0278(9) Uani 1 1 d . . . . .
Ti2 Ti 0.8074(3) 0.7614(3) 0.93650(15) 0.0266(9) Uani 1 1 d . . . . .
O1 O 0.4979(16) 0.3077(16) 0.500000 0.026(4) Uani 1 2 d S TU P . .
O2 O 0.4835(14) 0.4591(15) 0.500000 0.028(5) Uani 1 2 d S TU P C .
O3 O 0.3287(12) 0.2961(12) 0.5650(6) 0.040(4) Uani 1 1 d D U . . .
O4 O 0.4800(12) 0.4541(13) 0.6237(7) 0.042(4) Uani 1 1 d . U . . .
O5 O 0.4712(12) 0.2575(11) 0.6142(6) 0.033(4) Uani 1 1 d . U . . .
O6 O 0.6318(11) 0.4360(11) 0.5750(6) 0.029(3) Uani 1 1 d . U . . .
O21 O 0.8300(15) 0.8509(16) 1.000000 0.028(5) Uani 1 2 d S TU P . .
O22 O 0.8314(17) 0.6878(13) 1.000000 0.030(4) Uani 1 2 d S TU P G .
O23 O 0.6717(11) 0.6829(12) 0.9340(6) 0.033(4) Uani 1 1 d D U . . .
O24 O 0.8279(11) 0.6932(11) 0.8762(6) 0.035(4) Uani 1 1 d . U . . .
O25 O 0.9751(11) 0.8637(11) 0.9243(6) 0.027(3) Uani 1 1 d . U . . .
O26 O 0.8042(14) 0.8695(13) 0.8848(8) 0.039(4) Uani 1 1 d . U . . .
C2 C 0.479(3) 0.560(3) 0.500000 0.050(9) Uani 1 2 d S TU P . .
H2A H 0.474311 0.560898 0.542311 0.060 Uiso 0.5 1 calc R U P A -1
C2A C 0.589(4) 0.650(4) 0.500000 0.079(14) Uani 1 2 d S TU P C .
H2AA H 0.588480 0.715074 0.500000 0.118 Uiso 0.5 1 calc R U P B -1
H2AB H 0.625068 0.646233 0.533966 0.118 Uiso 0.5 1 calc R U P B -1
H2AC H 0.625068 0.646233 0.466034 0.118 Uiso 0.5 1 calc R U P B -1
C2B C 0.354(5) 0.528(5) 0.491(5) 0.08(2) Uani 0.5 1 d . U P C -1
H2BA H 0.310099 0.452981 0.496091 0.124 Uiso 0.5 1 calc R U P C -1
H2BB H 0.335834 0.563963 0.519309 0.124 Uiso 0.5 1 calc R U P C -1
H2BC H 0.344701 0.547280 0.452891 0.124 Uiso 0.5 1 calc R U P C -1
C3 C 0.249(2) 0.252(3) 0.6060(15) 0.036(7) Uiso 0.55(3) 1 d D U P D 1
H3 H 0.281332 0.253960 0.643426 0.043 Uiso 0.55(3) 1 calc R U P D 1
C3A C 0.191(5) 0.303(4) 0.613(3) 0.075(10) Uiso 0.55(3) 1 d D U P D 1
H3AA H 0.236761 0.374974 0.623377 0.112 Uiso 0.55(3) 1 calc R U P D 1
H3AB H 0.155636 0.299695 0.577093 0.112 Uiso 0.55(3) 1 calc R U P D 1
H3AC H 0.138947 0.268173 0.642776 0.112 Uiso 0.55(3) 1 calc R U P D 1
C3B C 0.185(5) 0.148(3) 0.591(3) 0.075(10) Uiso 0.55(3) 1 d D U P D 1
H3BA H 0.128749 0.114898 0.618327 0.112 Uiso 0.55(3) 1 calc R U P D 1
H3BB H 0.156870 0.144425 0.552909 0.112 Uiso 0.55(3) 1 calc R U P D 1
H3BC H 0.225948 0.113410 0.590905 0.112 Uiso 0.55(3) 1 calc R U P D 1
C3' C 0.228(2) 0.213(3) 0.566(2) 0.036(7) Uiso 0.45(3) 1 d D U P D 2
H3A' H 0.240887 0.186422 0.602392 0.043 Uiso 0.45(3) 1 calc R U P D 2
C3A' C 0.167(5) 0.247(5) 0.594(3) 0.075(10) Uiso 0.45(3) 1 d D U P D 2
H3AD H 0.211663 0.317493 0.608643 0.112 Uiso 0.45(3) 1 calc R U P D 2
H3AE H 0.116502 0.247112 0.567765 0.112 Uiso 0.45(3) 1 calc R U P D 2
H3AF H 0.130654 0.201000 0.626205 0.112 Uiso 0.45(3) 1 calc R U P D 2
C3B' C 0.168(5) 0.114(4) 0.545(3) 0.075(10) Uiso 0.45(3) 1 d D U P D 2
H3BD H 0.096524 0.084753 0.559043 0.112 Uiso 0.45(3) 1 calc R U P D 2
H3BE H 0.167841 0.115456 0.503644 0.112 Uiso 0.91(6) 2 calc R U P D 2
H3BF H 0.195549 0.070187 0.558193 0.112 Uiso 0.45(3) 1 calc R U P D 2
C11 C 0.553(2) 0.5298(18) 0.6552(11) 0.039(5) Uani 1 1 d . U . . .
C12 C 0.523(2) 0.5819(19) 0.6923(10) 0.042(6) Uani 1 1 d . U . . .
H12A H 0.454243 0.568231 0.693670 0.050 Uiso 1 1 calc R U . . .
C13 C 0.598(3) 0.654(3) 0.7271(13) 0.062(8) Uani 1 1 d . U . . .
H13A H 0.577171 0.688153 0.753481 0.075 Uiso 1 1 calc R U . . .
C14 C 0.693(3) 0.681(3) 0.7274(13) 0.062(8) Uani 1 1 d . U . . .
H14A H 0.740407 0.732217 0.752747 0.074 Uiso 1 1 calc R U . . .
C15 C 0.728(2) 0.631(2) 0.6887(12) 0.054(7) Uani 1 1 d . U . . .
H15A H 0.798409 0.649235 0.686790 0.065 Uiso 1 1 calc R U . . .
C16 C 0.6530(19) 0.5540(17) 0.6532(10) 0.034(5) Uani 1 1 d . U . . .
C17 C 0.4959(17) 0.1879(19) 0.6124(10) 0.030(5) Uani 1 1 d . U . . .
C22 C 0.836(4) 0.591(4) 1.000000 0.068(12) Uani 1 2 d S TU P . .
H22' H 0.825850 0.577892 0.958221 0.082 Uiso 0.5 1 calc R U P E -1
C22A C 0.958(9) 0.647(10) 1.000000 0.20(5) Uani 1 2 d S TU P G .
H22A H 0.986521 0.712809 0.979511 0.296 Uiso 0.5 1 calc R U P F -1
H22B H 0.983591 0.660313 1.039207 0.296 Uiso 0.5 1 calc R U P F -1
H22C H 0.980383 0.602847 0.981282 0.296 Uiso 0.5 1 calc R U P F -1
C22B C 0.745(7) 0.507(5) 1.016(3) 0.09(2) Uani 0.5 1 d . U P G -1
H22D H 0.752323 0.445715 1.015659 0.130 Uiso 0.5 1 calc R U P G -1
H22E H 0.728061 0.518219 1.055068 0.130 Uiso 0.5 1 calc R U P G -1
H22F H 0.689843 0.497891 0.990469 0.130 Uiso 0.5 1 calc R U P G -1
C23 C 0.602(3) 0.640(4) 0.887(2) 0.064(11) Uiso 0.46(3) 1 d D U P H 1
H23A H 0.639889 0.675180 0.851549 0.077 Uiso 0.46(3) 1 calc R U P H 1
C23A C 0.518(5) 0.659(5) 0.894(3) 0.068(8) Uiso 0.46(3) 1 d D U P H 1
H23B H 0.544337 0.733006 0.898374 0.102 Uiso 0.46(3) 1 calc R U P H 1
H23C H 0.473037 0.633633 0.860362 0.102 Uiso 0.46(3) 1 calc R U P H 1
H23D H 0.477798 0.622220 0.927676 0.102 Uiso 0.46(3) 1 calc R U P H 1
C23B C 0.561(5) 0.532(4) 0.881(3) 0.068(8) Uiso 0.46(3) 1 d D U P H 1
H23E H 0.617086 0.517169 0.876012 0.102 Uiso 0.46(3) 1 calc R U P H 1
H23F H 0.520380 0.496158 0.914610 0.102 Uiso 0.46(3) 1 calc R U P H 1
H23G H 0.515619 0.507572 0.847296 0.102 Uiso 0.46(3) 1 calc R U P H 1
C23' C 0.564(2) 0.632(3) 0.938(2) 0.064(11) Uiso 0.54(3) 1 d D U P H 2
H23H H 0.539334 0.592753 0.974484 0.077 Uiso 0.54(3) 1 calc R U P H 2
C23C C 0.566(5) 0.725(4) 0.940(2) 0.068(8) Uiso 0.54(3) 1 d D U P H 2
H23I H 0.495275 0.712162 0.943691 0.102 Uiso 0.54(3) 1 calc R U P H 2
H23J H 0.606255 0.764143 0.973535 0.102 Uiso 0.54(3) 1 calc R U P H 2
H23K H 0.597898 0.764439 0.905819 0.102 Uiso 0.54(3) 1 calc R U P H 2
C23D C 0.503(5) 0.574(4) 0.891(2) 0.068(8) Uiso 0.54(3) 1 d D U P H 2
H23L H 0.501290 0.507644 0.889455 0.102 Uiso 0.54(3) 1 calc R U P H 2
H23M H 0.432303 0.561370 0.896114 0.102 Uiso 0.54(3) 1 calc R U P H 2
H23N H 0.532231 0.612474 0.856127 0.102 Uiso 0.54(3) 1 calc R U P H 2
C31 C 0.9039(19) 0.6976(17) 0.8427(10) 0.037(5) Uani 1 1 d . U . . .
C32 C 0.879(2) 0.621(2) 0.8036(12) 0.047(6) Uani 1 1 d . U . . .
H32A H 0.810273 0.564276 0.802303 0.057 Uiso 1 1 calc R U . . .
C33 C 0.953(3) 0.624(2) 0.7654(12) 0.059(7) Uani 1 1 d . U . . .
H33A H 0.934376 0.571329 0.737654 0.070 Uiso 1 1 calc R U . . .
C34 C 1.056(3) 0.708(3) 0.7699(14) 0.069(9) Uani 1 1 d . U . . .
H34A H 1.108269 0.712875 0.744857 0.083 Uiso 1 1 calc R U . . .
C35 C 1.080(2) 0.782(2) 0.8099(10) 0.044(6) Uani 1 1 d . U . . .
H35A H 1.149177 0.838143 0.811926 0.053 Uiso 1 1 calc R U . . .
C36 C 1.0062(18) 0.7790(18) 0.8488(11) 0.035(5) Uani 1 1 d . U . . .
C37 C 0.8257(17) 0.9606(18) 0.8894(10) 0.026(5) Uani 1 1 d . 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
Pr1 O1 2.35(2) . ?
Pr1 O1 2.35(2) 2_655 ?
Pr1 O1 2.35(2) 3_665 ?
Pr1 O6 2.558(14) 3_665 ?
Pr1 O6 2.558(14) 5_656 ?
Pr1 O6 2.558(14) 6_666 ?
Pr1 O6 2.558(14) 2_655 ?
Pr1 O6 2.558(14) 4_556 ?
Pr1 O6 2.558(14) . ?
Pr1 Ti1 3.598(4) 5_656 ?
Pr1 Ti1 3.598(4) 2_655 ?
Pr1 Ti1 3.598(4) 3_665 ?
Pr2 O21 2.400(19) 3_675 ?
Pr2 O21 2.400(19) 2_765 ?
Pr2 O21 2.400(19) . ?
Pr2 O25 2.591(13) . ?
Pr2 O25 2.591(13) 5_767 ?
Pr2 O25 2.591(13) 3_675 ?
Pr2 O25 2.591(13) 6_677 ?
Pr2 O25 2.591(13) 2_765 ?
Pr2 O25 2.591(13) 4_557 ?
Pr2 Ti2 3.602(4) . ?
Pr2 Ti2 3.602(4) 5_767 ?
Pr2 Ti2 3.602(4) 4_557 ?
Ti1 O3 1.764(16) . ?
Ti1 O4 1.886(17) . ?
Ti1 O1 1.904(12) . ?
Ti1 O2 1.990(13) . ?
Ti1 O5 2.026(15) . ?
Ti1 O6 2.183(15) . ?
Ti1 Ti1 3.005(7) 4_556 ?
Ti2 O23 1.765(15) . ?
Ti2 O24 1.861(14) . ?
Ti2 O21 1.920(15) . ?
Ti2 O22 1.993(13) . ?
Ti2 O26 2.043(18) . ?
Ti2 O25 2.208(16) . ?
Ti2 Ti2 2.992(7) 4_557 ?
O2 C2 1.55(4) . ?
O3 C3' 1.40(3) . ?
O3 C3 1.42(3) . ?
O4 C11 1.34(3) . ?
O5 C17 1.27(3) . ?
O6 C17 1.31(3) 3_665 ?
O22 C22 1.48(6) . ?
O23 C23' 1.39(3) . ?
O23 C23 1.43(3) . ?
O24 C31 1.36(3) . ?
O25 C37 1.26(3) 2_765 ?
O26 C37 1.24(3) . ?
C2 C2A 1.51(6) . ?
C2 C2B 1.69(8) . ?
C2 H2A 1.0000 . ?
C2A H2AA 0.9800 . ?
C2A H2AB 0.9800 . ?
C2A H2AC 0.9800 . ?
C2B H2BA 0.9800 . ?
C2B H2BB 0.9800 . ?
C2B H2BC 0.9800 . ?
C3 C3B 1.40(3) . ?
C3 C3A 1.42(3) . ?
C3 H3 1.0000 . ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?
C3A H3AC 0.9800 . ?
C3B H3BA 0.9800 . ?
C3B H3BB 0.9800 . ?
C3B H3BC 0.9800 . ?
C3' C3B' 1.39(3) . ?
C3' C3A' 1.41(3) . ?
C3' H3A' 1.0000 . ?
C3A' H3AD 0.9800 . ?
C3A' H3AE 0.9800 . ?
C3A' H3AF 0.9800 . ?
C3B' H3BD 0.9800 . ?
C3B' H3BE 0.9800 . ?
C3B' H3BF 0.9800 . ?
C11 C16 1.35(4) . ?
C11 C12 1.38(3) . ?
C12 C13 1.37(4) . ?
C12 H12A 0.9500 . ?
C13 C14 1.27(4) . ?
C13 H13A 0.9500 . ?
C14 C15 1.42(4) . ?
C14 H14A 0.9500 . ?
C15 C16 1.41(4) . ?
C15 H15A 0.9500 . ?
C16 C17 1.50(3) 3_665 ?
C22 C22B 1.36(9) . ?
C22 C22A 1.59(12) . ?
C22 H22' 1.0000 . ?
C22A H22A 0.9800 . ?
C22A H22B 0.9800 . ?
C22A H22C 0.9800 . ?
C22B H22D 0.9800 . ?
C22B H22E 0.9800 . ?
C22B H22F 0.9800 . ?
C23 C23B 1.42(3) . ?
C23 C23A 1.43(3) . ?
C23 H23A 1.0000 . ?
C23A H23B 0.9800 . ?
C23A H23C 0.9800 . ?
C23A H23D 0.9800 . ?
C23B H23E 0.9800 . ?
C23B H23F 0.9800 . ?
C23B H23G 0.9800 . ?
C23' C23C 1.38(3) . ?
C23' C23D 1.42(3) . ?
C23' H23H 1.0000 . ?
C23C H23I 0.9800 . ?
C23C H23J 0.9800 . ?
C23C H23K 0.9800 . ?
C23D H23L 0.9800 . ?
C23D H23M 0.9800 . ?
C23D H23N 0.9800 . ?
C31 C32 1.37(3) . ?
C31 C36 1.41(3) . ?
C32 C33 1.41(4) . ?
C32 H32A 0.9500 . ?
C33 C34 1.43(5) . ?
C33 H33A 0.9500 . ?
C34 C35 1.35(4) . ?
C34 H34A 0.9500 . ?
C35 C36 1.42(3) . ?
C35 H35A 0.9500 . ?
C36 C37 1.48(3) 2_765 ?

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 Pr1 O1 120.000(8) . 2_655 ?
O1 Pr1 O1 120.000(1) . 3_665 ?
O1 Pr1 O1 120.000(3) 2_655 3_665 ?
O1 Pr1 O6 136.0(3) . 3_665 ?
O1 Pr1 O6 72.9(5) 2_655 3_665 ?
O1 Pr1 O6 64.8(5) 3_665 3_665 ?
O1 Pr1 O6 72.9(5) . 5_656 ?
O1 Pr1 O6 64.8(5) 2_655 5_656 ?
O1 Pr1 O6 136.0(3) 3_665 5_656 ?
O6 Pr1 O6 137.6(2) 3_665 5_656 ?
O1 Pr1 O6 136.0(3) . 6_666 ?
O1 Pr1 O6 72.9(5) 2_655 6_666 ?
O1 Pr1 O6 64.8(5) 3_665 6_666 ?
O6 Pr1 O6 87.3(6) 3_665 6_666 ?
O6 Pr1 O6 77.6(5) 5_656 6_666 ?
O1 Pr1 O6 72.9(5) . 2_655 ?
O1 Pr1 O6 64.8(5) 2_655 2_655 ?
O1 Pr1 O6 136.0(3) 3_665 2_655 ?
O6 Pr1 O6 77.6(5) 3_665 2_655 ?
O6 Pr1 O6 87.3(6) 5_656 2_655 ?
O6 Pr1 O6 137.6(2) 6_666 2_655 ?
O1 Pr1 O6 64.8(5) . 4_556 ?
O1 Pr1 O6 136.0(3) 2_655 4_556 ?
O1 Pr1 O6 72.9(5) 3_665 4_556 ?
O6 Pr1 O6 137.6(2) 3_665 4_556 ?
O6 Pr1 O6 77.6(5) 5_656 4_556 ?
O6 Pr1 O6 77.6(5) 6_666 4_556 ?
O6 Pr1 O6 137.6(2) 2_655 4_556 ?
O1 Pr1 O6 64.8(5) . . ?
O1 Pr1 O6 136.0(3) 2_655 . ?
O1 Pr1 O6 72.9(5) 3_665 . ?
O6 Pr1 O6 77.6(5) 3_665 . ?
O6 Pr1 O6 137.6(2) 5_656 . ?
O6 Pr1 O6 137.6(2) 6_666 . ?
O6 Pr1 O6 77.6(5) 2_655 . ?
O6 Pr1 O6 87.3(6) 4_556 . ?
O1 Pr1 Ti1 103.5(5) . 5_656 ?
O1 Pr1 Ti1 28.7(3) 2_655 5_656 ?
O1 Pr1 Ti1 130.1(4) 3_665 5_656 ?
O6 Pr1 Ti1 100.7(3) 3_665 5_656 ?
O6 Pr1 Ti1 36.9(3) 5_656 5_656 ?
O6 Pr1 Ti1 67.0(3) 6_666 5_656 ?
O6 Pr1 Ti1 77.1(3) 2_655 5_656 ?
O6 Pr1 Ti1 109.0(3) 4_556 5_656 ?
O6 Pr1 Ti1 154.4(3) . 5_656 ?
O1 Pr1 Ti1 103.5(5) . 2_655 ?
O1 Pr1 Ti1 28.7(3) 2_655 2_655 ?
O1 Pr1 Ti1 130.1(4) 3_665 2_655 ?
O6 Pr1 Ti1 67.0(3) 3_665 2_655 ?
O6 Pr1 Ti1 77.1(3) 5_656 2_655 ?
O6 Pr1 Ti1 100.7(3) 6_666 2_655 ?
O6 Pr1 Ti1 36.9(3) 2_655 2_655 ?
O6 Pr1 Ti1 154.4(3) 4_556 2_655 ?
O6 Pr1 Ti1 109.0(3) . 2_655 ?
Ti1 Pr1 Ti1 49.36(12) 5_656 2_655 ?
O1 Pr1 Ti1 130.1(4) . 3_665 ?
O1 Pr1 Ti1 103.5(5) 2_655 3_665 ?
O1 Pr1 Ti1 28.7(3) 3_665 3_665 ?
O6 Pr1 Ti1 36.9(3) 3_665 3_665 ?
O6 Pr1 Ti1 154.4(3) 5_656 3_665 ?
O6 Pr1 Ti1 77.1(3) 6_666 3_665 ?
O6 Pr1 Ti1 109.0(3) 2_655 3_665 ?
O6 Pr1 Ti1 100.7(3) 4_556 3_665 ?
O6 Pr1 Ti1 67.0(3) . 3_665 ?
Ti1 Pr1 Ti1 125.96(3) 5_656 3_665 ?
Ti1 Pr1 Ti1 103.79(7) 2_655 3_665 ?
O21 Pr2 O21 120.00(2) 3_675 2_765 ?
O21 Pr2 O21 119.999(7) 3_675 . ?
O21 Pr2 O21 120.001(7) 2_765 . ?
O21 Pr2 O25 136.4(3) 3_675 . ?
O21 Pr2 O25 71.1(5) 2_765 . ?
O21 Pr2 O25 66.5(5) . . ?
O21 Pr2 O25 71.1(5) 3_675 5_767 ?
O21 Pr2 O25 66.5(5) 2_765 5_767 ?
O21 Pr2 O25 136.4(3) . 5_767 ?
O25 Pr2 O25 137.5(2) . 5_767 ?
O21 Pr2 O25 66.5(5) 3_675 3_675 ?
O21 Pr2 O25 136.4(3) 2_765 3_675 ?
O21 Pr2 O25 71.1(5) . 3_675 ?
O25 Pr2 O25 77.8(5) . 3_675 ?
O25 Pr2 O25 137.5(2) 5_767 3_675 ?
O21 Pr2 O25 66.5(5) 3_675 6_677 ?
O21 Pr2 O25 136.4(3) 2_765 6_677 ?
O21 Pr2 O25 71.1(5) . 6_677 ?
O25 Pr2 O25 137.5(2) . 6_677 ?
O25 Pr2 O25 77.8(5) 5_767 6_677 ?
O25 Pr2 O25 87.0(6) 3_675 6_677 ?
O21 Pr2 O25 71.1(5) 3_675 2_765 ?
O21 Pr2 O25 66.5(5) 2_765 2_765 ?
O21 Pr2 O25 136.4(3) . 2_765 ?
O25 Pr2 O25 77.8(5) . 2_765 ?
O25 Pr2 O25 87.0(7) 5_767 2_765 ?
O25 Pr2 O25 77.8(5) 3_675 2_765 ?
O25 Pr2 O25 137.5(2) 6_677 2_765 ?
O21 Pr2 O25 136.4(3) 3_675 4_557 ?
O21 Pr2 O25 71.1(5) 2_765 4_557 ?
O21 Pr2 O25 66.5(5) . 4_557 ?
O25 Pr2 O25 87.0(6) . 4_557 ?
O25 Pr2 O25 77.8(5) 5_767 4_557 ?
O25 Pr2 O25 137.5(2) 3_675 4_557 ?
O25 Pr2 O25 77.8(5) 6_677 4_557 ?
O25 Pr2 O25 137.5(2) 2_765 4_557 ?
O21 Pr2 Ti2 131.6(5) 3_675 . ?
O21 Pr2 Ti2 101.9(5) 2_765 . ?
O21 Pr2 Ti2 29.5(3) . . ?
O25 Pr2 Ti2 37.5(3) . . ?
O25 Pr2 Ti2 154.8(3) 5_767 . ?
O25 Pr2 Ti2 66.6(3) 3_675 . ?
O25 Pr2 Ti2 100.1(3) 6_677 . ?
O25 Pr2 Ti2 109.4(3) 2_765 . ?
O25 Pr2 Ti2 77.2(3) 4_557 . ?
O21 Pr2 Ti2 101.9(5) 3_675 5_767 ?
O21 Pr2 Ti2 29.5(3) 2_765 5_767 ?
O21 Pr2 Ti2 131.6(5) . 5_767 ?
O25 Pr2 Ti2 100.1(3) . 5_767 ?
O25 Pr2 Ti2 37.5(3) 5_767 5_767 ?
O25 Pr2 Ti2 154.8(3) 3_675 5_767 ?
O25 Pr2 Ti2 109.4(3) 6_677 5_767 ?
O25 Pr2 Ti2 77.2(3) 2_765 5_767 ?
O25 Pr2 Ti2 66.6(3) 4_557 5_767 ?
Ti2 Pr2 Ti2 125.89(3) . 5_767 ?
O21 Pr2 Ti2 131.6(5) 3_675 4_557 ?
O21 Pr2 Ti2 101.9(5) 2_765 4_557 ?
O21 Pr2 Ti2 29.5(3) . 4_557 ?
O25 Pr2 Ti2 77.2(3) . 4_557 ?
O25 Pr2 Ti2 109.4(3) 5_767 4_557 ?
O25 Pr2 Ti2 100.1(3) 3_675 4_557 ?
O25 Pr2 Ti2 66.6(3) 6_677 4_557 ?
O25 Pr2 Ti2 154.8(3) 2_765 4_557 ?
O25 Pr2 Ti2 37.5(3) 4_557 4_557 ?
Ti2 Pr2 Ti2 49.07(12) . 4_557 ?
Ti2 Pr2 Ti2 103.96(7) 5_767 4_557 ?
O3 Ti1 O4 95.2(7) . . ?
O3 Ti1 O1 103.8(8) . . ?
O4 Ti1 O1 160.4(8) . . ?
O3 Ti1 O2 97.6(8) . . ?
O4 Ti1 O2 97.5(7) . . ?
O1 Ti1 O2 75.3(7) . . ?
O3 Ti1 O5 91.8(7) . . ?
O4 Ti1 O5 95.0(7) . . ?
O1 Ti1 O5 89.5(6) . . ?
O2 Ti1 O5 163.6(6) . . ?
O3 Ti1 O6 171.0(7) . . ?
O4 Ti1 O6 81.9(6) . . ?
O1 Ti1 O6 80.1(7) . . ?
O2 Ti1 O6 91.3(7) . . ?
O5 Ti1 O6 80.0(6) . . ?
O3 Ti1 Ti1 90.9(5) . 4_556 ?
O4 Ti1 Ti1 138.5(5) . 4_556 ?
O1 Ti1 Ti1 37.9(5) . 4_556 ?
O2 Ti1 Ti1 41.0(4) . 4_556 ?
O5 Ti1 Ti1 125.9(4) . 4_556 ?
O6 Ti1 Ti1 96.9(4) . 4_556 ?
O3 Ti1 Pr1 137.2(6) . . ?
O4 Ti1 Pr1 126.5(5) . . ?
O1 Ti1 Pr1 36.4(6) . . ?
O2 Ti1 Pr1 87.1(5) . . ?
O5 Ti1 Pr1 76.9(4) . . ?
O6 Ti1 Pr1 44.7(4) . . ?
Ti1 Ti1 Pr1 65.32(6) 4_556 . ?
O23 Ti2 O24 93.4(7) . . ?
O23 Ti2 O21 103.5(8) . . ?
O24 Ti2 O21 163.0(8) . . ?
O23 Ti2 O22 97.0(8) . . ?
O24 Ti2 O22 98.4(7) . . ?
O21 Ti2 O22 77.4(7) . . ?
O23 Ti2 O26 91.9(7) . . ?
O24 Ti2 O26 93.1(7) . . ?
O21 Ti2 O26 88.8(8) . . ?
O22 Ti2 O26 165.0(7) . . ?
O23 Ti2 O25 170.4(6) . . ?
O24 Ti2 O25 80.7(6) . . ?
O21 Ti2 O25 82.9(7) . . ?
O22 Ti2 O25 91.4(7) . . ?
O26 Ti2 O25 80.9(7) . . ?
O23 Ti2 Ti2 91.9(5) . 4_557 ?
O24 Ti2 Ti2 139.7(5) . 4_557 ?
O21 Ti2 Ti2 38.8(5) . 4_557 ?
O22 Ti2 Ti2 41.4(4) . 4_557 ?
O26 Ti2 Ti2 126.6(5) . 4_557 ?
O25 Ti2 Ti2 97.5(4) . 4_557 ?
O23 Ti2 Pr2 139.1(5) . . ?
O24 Ti2 Pr2 126.2(5) . . ?
O21 Ti2 Pr2 38.0(6) . . ?
O22 Ti2 Pr2 87.7(5) . . ?
O26 Ti2 Pr2 77.8(5) . . ?
O25 Ti2 Pr2 45.6(3) . . ?
Ti2 Ti2 Pr2 65.46(6) 4_557 . ?
Ti1 O1 Ti1 104.2(9) 4_556 . ?
Ti1 O1 Pr1 114.9(7) 4_556 . ?
Ti1 O1 Pr1 114.9(7) . . ?
C2 O2 Ti1 129.8(5) . 4_556 ?
C2 O2 Ti1 129.8(5) . . ?
Ti1 O2 Ti1 98.1(8) 4_556 . ?
C3' O3 Ti1 159(2) . . ?
C3 O3 Ti1 137.8(19) . . ?
C11 O4 Ti1 140.9(15) . . ?
C17 O5 Ti1 140.6(17) . . ?
C17 O6 Ti1 129.6(15) 3_665 . ?
C17 O6 Pr1 131.7(15) 3_665 . ?
Ti1 O6 Pr1 98.4(5) . . ?
Ti2 O21 Ti2 102.3(11) . 4_557 ?
Ti2 O21 Pr2 112.5(7) . . ?
Ti2 O21 Pr2 112.5(7) 4_557 . ?
C22 O22 Ti2 130.3(6) . . ?
C22 O22 Ti2 130.3(6) . 4_557 ?
Ti2 O22 Ti2 97.3(8) . 4_557 ?
C23' O23 Ti2 171(2) . . ?
C23 O23 Ti2 131(2) . . ?
C31 O24 Ti2 141.3(14) . . ?
C37 O25 Ti2 133.7(15) 2_765 . ?
C37 O25 Pr2 129.0(15) 2_765 . ?
Ti2 O25 Pr2 97.0(5) . . ?
C37 O26 Ti2 136.2(19) . . ?
C2A C2 O2 108(3) . . ?
C2A C2 C2B 144(4) . . ?
O2 C2 C2B 107(3) . . ?
C2A C2 H2A 92.7 . . ?
O2 C2 H2A 92.7 . . ?
C2B C2 H2A 92.7 . . ?
C2 C2A H2AA 109.5 . . ?
C2 C2A H2AB 109.5 . . ?
H2AA C2A H2AB 109.5 . . ?
C2 C2A H2AC 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
C2 C2B H2BA 109.5 . . ?
C2 C2B H2BB 109.5 . . ?
H2BA C2B H2BB 109.5 . . ?
C2 C2B H2BC 109.5 . . ?
H2BA C2B H2BC 109.5 . . ?
H2BB C2B H2BC 109.5 . . ?
C3B C3 O3 107(3) . . ?
C3B C3 C3A 111(3) . . ?
O3 C3 C3A 115(4) . . ?
C3B C3 H3 107.7 . . ?
O3 C3 H3 107.7 . . ?
C3A C3 H3 107.7 . . ?
C3 C3A H3AA 109.5 . . ?
C3 C3A H3AB 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
C3 C3A H3AC 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
C3 C3B H3BA 109.5 . . ?
C3 C3B H3BB 109.5 . . ?
H3BA C3B H3BB 109.5 . . ?
C3 C3B H3BC 109.5 . . ?
H3BA C3B H3BC 109.5 . . ?
H3BB C3B H3BC 109.5 . . ?
C3B' C3' O3 141(4) . . ?
C3B' C3' C3A' 111(3) . . ?
O3 C3' C3A' 107(4) . . ?
C3B' C3' H3A' 91.8 . . ?
O3 C3' H3A' 91.8 . . ?
C3A' C3' H3A' 91.8 . . ?
C3' C3A' H3AD 109.5 . . ?
C3' C3A' H3AE 109.5 . . ?
H3AD C3A' H3AE 109.5 . . ?
C3' C3A' H3AF 109.5 . . ?
H3AD C3A' H3AF 109.5 . . ?
H3AE C3A' H3AF 109.5 . . ?
C3' C3B' H3BD 109.5 . . ?
C3' C3B' H3BE 109.5 . . ?
H3BD C3B' H3BE 109.5 . . ?
C3' C3B' H3BF 109.5 . . ?
H3BD C3B' H3BF 109.5 . . ?
H3BE C3B' H3BF 109.5 . . ?
O4 C11 C16 122(2) . . ?
O4 C11 C12 118(2) . . ?
C16 C11 C12 120(3) . . ?
C13 C12 C11 117(3) . . ?
C13 C12 H12A 121.3 . . ?
C11 C12 H12A 121.3 . . ?
C14 C13 C12 126(3) . . ?
C14 C13 H13A 116.9 . . ?
C12 C13 H13A 116.9 . . ?
C13 C14 C15 118(3) . . ?
C13 C14 H14A 120.8 . . ?
C15 C14 H14A 120.8 . . ?
C16 C15 C14 117(3) . . ?
C16 C15 H15A 121.3 . . ?
C14 C15 H15A 121.3 . . ?
C11 C16 C15 121(2) . . ?
C11 C16 C17 123(2) . 3_665 ?
C15 C16 C17 116(2) . 3_665 ?
O5 C17 O6 119(2) . 2_655 ?
O5 C17 C16 119(2) . 2_655 ?
O6 C17 C16 122(2) 2_655 2_655 ?
C22B C22 O22 113(5) . . ?
C22B C22 C22A 147(7) . . ?
O22 C22 C22A 95(6) . . ?
C22B C22 H22' 96.9 . . ?
O22 C22 H22' 96.9 . . ?
C22A C22 H22' 96.9 . . ?
C22 C22A H22A 109.5 . . ?
C22 C22A H22B 109.5 . . ?
H22A C22A H22B 109.5 . . ?
C22 C22A H22C 109.5 . . ?
H22A C22A H22C 109.5 . . ?
H22B C22A H22C 109.5 . . ?
C22 C22B H22D 109.5 . . ?
C22 C22B H22E 109.5 . . ?
H22D C22B H22E 109.5 . . ?
C22 C22B H22F 109.5 . . ?
H22D C22B H22F 109.5 . . ?
H22E C22B H22F 109.5 . . ?
C23B C23 C23A 108(3) . . ?
C23B C23 O23 113(5) . . ?
C23A C23 O23 110(4) . . ?
C23B C23 H23A 108.5 . . ?
C23A C23 H23A 108.5 . . ?
O23 C23 H23A 108.5 . . ?
C23 C23A H23B 109.5 . . ?
C23 C23A H23C 109.5 . . ?
H23B C23A H23C 109.5 . . ?
C23 C23A H23D 109.5 . . ?
H23B C23A H23D 109.5 . . ?
H23C C23A H23D 109.5 . . ?
C23 C23B H23E 109.5 . . ?
C23 C23B H23F 109.5 . . ?
H23E C23B H23F 109.5 . . ?
C23 C23B H23G 109.5 . . ?
H23E C23B H23G 109.5 . . ?
H23F C23B H23G 109.5 . . ?
C23C C23' O23 91(4) . . ?
C23C C23' C23D 109(3) . . ?
O23 C23' C23D 120(4) . . ?
C23C C23' H23H 111.7 . . ?
O23 C23' H23H 111.7 . . ?
C23D C23' H23H 111.7 . . ?
C23' C23C H23I 109.5 . . ?
C23' C23C H23J 109.5 . . ?
H23I C23C H23J 109.5 . . ?
C23' C23C H23K 109.5 . . ?
H23I C23C H23K 109.5 . . ?
H23J C23C H23K 109.5 . . ?
C23' C23D H23L 109.5 . . ?
C23' C23D H23M 109.5 . . ?
H23L C23D H23M 109.5 . . ?
C23' C23D H23N 109.5 . . ?
H23L C23D H23N 109.5 . . ?
H23M C23D H23N 109.5 . . ?
O24 C31 C32 119(2) . . ?
O24 C31 C36 120(2) . . ?
C32 C31 C36 121(2) . . ?
C31 C32 C33 122(3) . . ?
C31 C32 H32A 119.2 . . ?
C33 C32 H32A 119.2 . . ?
C32 C33 C34 118(3) . . ?
C32 C33 H33A 121.1 . . ?
C34 C33 H33A 121.1 . . ?
C35 C34 C33 120(3) . . ?
C35 C34 H34A 120.1 . . ?
C33 C34 H34A 120.1 . . ?
C34 C35 C36 123(3) . . ?
C34 C35 H35A 118.7 . . ?
C36 C35 H35A 118.7 . . ?
C31 C36 C35 117(2) . . ?
C31 C36 C37 125(2) . 2_765 ?
C35 C36 C37 118(2) . 2_765 ?
O26 C37 O25 126(2) . 3_675 ?
O26 C37 C36 115(2) . 3_675 ?
O25 C37 C36 119(2) 3_675 3_675 ?

_refine_diff_density_max         8.674
_refine_diff_density_min         -1.144
_refine_diff_density_rms         0.256

####################################################################### 
# 
# 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_la_b
_database_code_depnum_ccdc_archive 'CCDC 1504171'
_audit_update_record             
;
2017-02-27 deposited with the CCDC.
2017-03-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT094_la_b                
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       9.51 Report
RESPONSE: There is a large amount of residual electron density that did not resolve into anything meaningful. It is presumably disordered solvent, as the NMR and elemental analysis of the complex is in excellent agreement with the crystallographic formula.
;
# Added during the CSD deposition process: Monday 27 February 2017 10:24 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C69 H87 La O30 Ti6'
_chemical_formula_sum            'C69 H87 La O30 Ti6'
_chemical_formula_weight         1822.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -1.4094 9.0376 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           174
_space_group_name_H-M_alt        'P -6'
_space_group_name_Hall           'P -6'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'

_cell_length_a                   15.0084(4)
_cell_length_b                   15.0084(4)
_cell_length_c                   23.5238(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4588.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9163
_cell_measurement_theta_min      3.885
_cell_measurement_theta_max      66.7

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_F_000             1860
_exptl_transmission_factor_min   0.741
_exptl_transmission_factor_max   1.00
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.240
_exptl_absorpt_coefficient_mu    8.328
_shelx_estimated_absorpt_T_min   0.196
_shelx_estimated_absorpt_T_max   0.240
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.196
_exptl_absorpt_correction_T_max  0.240
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements (SADABS) 
;
_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         '30W microfocus sealed tube, Quazar optics'
_diffrn_measurement_device_type  'Bruker QUEST D8 CCD'
_diffrn_measurement_method       'Thin slice ω and φ scans'
_diffrn_reflns_number            61633
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.400
_diffrn_reflns_theta_max         66.713
_diffrn_reflns_theta_full        66.713
_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             5571
_reflns_number_gt                5436
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.990
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    1.000

_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 software package, narrow-frames'
_computing_cell_refinement       'refinement of XYZ centroids > 20sigma(I)'
_computing_data_reduction        
;
 Bruker SAINT software package, narrow frame algorithm
;
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_refine_special_details          
;Refined as a 2-component twin. Residual electron density between
molecules would not resolve into anything meaningful but are presumably
disordered solvent. Disordered iPr ligands refined satisfactorily by 
restraining and treating isotropically., Twin
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1289P)²+16.1168P] 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_abs_structure_details 
;
 Flack x determined using 2638 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.286(6)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5571
_refine_ls_number_parameters     331
_refine_ls_number_restraints     142
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0667
_refine_ls_wR_factor_ref         0.1900
_refine_ls_wR_factor_gt          0.1886
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_restrained_S_all      1.152
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
La1 La 0.666667 0.333333 0.500000 0.0154(5) Uani 1 6 d S T P . .
La2 La 1.000000 1.000000 1.000000 0.0153(5) Uani 1 6 d S T P . .
Ti1 Ti 0.4649(2) 0.3650(2) 0.56389(12) 0.0249(7) Uani 1 1 d . . . . .
Ti2 Ti 0.8081(2) 0.7603(2) 0.93619(11) 0.0238(6) Uani 1 1 d . . . . .
O1 O 0.4970(12) 0.3082(13) 0.500000 0.023(3) Uani 1 2 d S T P . .
O2 O 0.4850(12) 0.4602(13) 0.500000 0.032(4) Uani 1 2 d S T P C .
O3 O 0.3286(9) 0.2973(10) 0.5662(5) 0.039(3) Uani 1 1 d D . . . .
O4 O 0.4809(10) 0.4547(11) 0.6237(6) 0.038(3) Uani 1 1 d . . . . .
O5 O 0.4709(10) 0.2588(9) 0.6139(5) 0.030(3) Uani 1 1 d . . . . .
O6 O 0.6305(9) 0.4365(9) 0.5759(5) 0.027(3) Uani 1 1 d . . . . .
O21 O 0.8294(14) 0.8464(12) 1.000000 0.029(4) Uani 1 2 d S T P . .
O22 O 0.8305(15) 0.6848(11) 1.000000 0.031(4) Uani 1 2 d S T P G .
O23 O 0.6725(10) 0.6817(9) 0.9342(5) 0.035(3) Uani 1 1 d D . . . .
O24 O 0.8304(10) 0.6928(9) 0.8756(5) 0.035(3) Uani 1 1 d . . . . .
O25 O 0.9753(10) 0.8642(9) 0.9248(4) 0.023(2) Uani 1 1 d . . . . .
O26 O 0.8045(11) 0.8703(11) 0.8856(6) 0.036(3) Uani 1 1 d . . . . .
C2 C 0.482(2) 0.560(2) 0.500000 0.050(8) Uani 1 2 d DS TU P . .
H2A H 0.473987 0.560406 0.542163 0.059 Uiso 0.5 1 calc R U P A -1
C2A C 0.588(2) 0.647(2) 0.500000 0.061(9) Uani 1 2 d DS TU P C .
H2AA H 0.635350 0.623162 0.511584 0.092 Uiso 0.5 1 calc R U P B -1
H2AB H 0.606016 0.676413 0.461706 0.092 Uiso 0.5 1 calc R U P B -1
H2AC H 0.593295 0.699506 0.526710 0.092 Uiso 0.5 1 calc R U P B -1
C2B C 0.378(3) 0.541(4) 0.488(3) 0.09(2) Uani 0.5 1 d D U P C -1
H2BA H 0.327959 0.467585 0.493566 0.130 Uiso 0.5 1 calc R U P C -1
H2BB H 0.361716 0.582313 0.513134 0.130 Uiso 0.5 1 calc R U P C -1
H2BC H 0.374437 0.559219 0.448129 0.130 Uiso 0.5 1 calc R U P C -1
C3 C 0.249(2) 0.254(3) 0.6075(15) 0.055(8) Uiso 0.53(3) 1 d D U P D 1
H3 H 0.281147 0.257390 0.645165 0.066 Uiso 0.53(3) 1 calc R U P D 1
C3A C 0.195(4) 0.312(4) 0.612(2) 0.086(9) Uiso 0.53(3) 1 d D U P D 1
H3AA H 0.140911 0.279628 0.640791 0.128 Uiso 0.53(3) 1 calc R U P D 1
H3AB H 0.244117 0.382533 0.623327 0.128 Uiso 0.53(3) 1 calc R U P D 1
H3AC H 0.164738 0.311625 0.575288 0.128 Uiso 0.53(3) 1 calc R U P D 1
C3B C 0.178(3) 0.148(3) 0.596(2) 0.086(9) Uiso 0.53(3) 1 d D U P D 1
H3BA H 0.124269 0.120478 0.624606 0.128 Uiso 0.53(3) 1 calc R U P D 1
H3BB H 0.147400 0.142313 0.558108 0.128 Uiso 0.53(3) 1 calc R U P D 1
H3BC H 0.215145 0.109744 0.595925 0.128 Uiso 0.53(3) 1 calc R U P D 1
C3' C 0.225(2) 0.221(3) 0.5637(19) 0.055(8) Uiso 0.47(3) 1 d D U P D 2
H3A' H 0.207253 0.234632 0.524882 0.066 Uiso 0.47(3) 1 calc R U P D 2
C3A' C 0.160(3) 0.244(4) 0.597(3) 0.086(9) Uiso 0.47(3) 1 d D U P D 2
H3AD H 0.188308 0.318596 0.598182 0.128 Uiso 0.47(3) 1 calc R U P D 2
H3AE H 0.090910 0.211046 0.580231 0.128 Uiso 0.47(3) 1 calc R U P D 2
H3AF H 0.155598 0.218046 0.635812 0.128 Uiso 0.47(3) 1 calc R U P D 2
C3B' C 0.196(4) 0.119(3) 0.558(3) 0.086(9) Uiso 0.47(3) 1 d D U P D 2
H3BD H 0.120316 0.077358 0.556866 0.128 Uiso 0.47(3) 1 calc R U P D 2
H3BE H 0.223840 0.108836 0.522387 0.128 Uiso 0.47(3) 1 calc R U P D 2
H3BF H 0.221696 0.097183 0.590071 0.128 Uiso 0.47(3) 1 calc R U P D 2
C11 C 0.5557(16) 0.5311(14) 0.6554(8) 0.038(4) Uani 1 1 d . U . . .
C12 C 0.527(2) 0.5812(17) 0.6940(9) 0.049(5) Uani 1 1 d . U . . .
H12A H 0.457962 0.566069 0.696692 0.059 Uiso 1 1 calc R U . . .
C13 C 0.601(2) 0.653(2) 0.7281(10) 0.067(7) Uani 1 1 d . U . . .
H13A H 0.579928 0.684451 0.755753 0.081 Uiso 1 1 calc R U . . .
C14 C 0.697(2) 0.681(2) 0.7264(11) 0.062(6) Uani 1 1 d . U . . .
H14A H 0.744781 0.735525 0.750153 0.074 Uiso 1 1 calc R U . . .
C15 C 0.7301(18) 0.6309(17) 0.6886(9) 0.049(5) Uani 1 1 d . U . . .
H15A H 0.800100 0.647968 0.687435 0.059 Uiso 1 1 calc R U . . .
C16 C 0.6558(15) 0.5538(15) 0.6521(8) 0.034(4) Uani 1 1 d . U . . .
C17 C 0.4951(15) 0.1888(16) 0.6124(8) 0.032(4) Uani 1 1 d . U . . .
C22 C 0.836(3) 0.592(3) 1.000000 0.057(8) Uani 1 2 d S TU P . .
H22' H 0.822327 0.573806 0.958861 0.068 Uiso 0.5 1 calc R U P E -1
C22A C 0.950(6) 0.637(7) 1.000000 0.17(3) Uani 1 2 d S TU P G .
H22A H 0.982152 0.700030 0.976808 0.256 Uiso 0.5 1 calc R U P F -1
H22B H 0.976205 0.654321 1.039048 0.256 Uiso 0.5 1 calc R U P F -1
H22C H 0.967506 0.587461 0.984144 0.256 Uiso 0.5 1 calc R U P F -1
C22B C 0.749(6) 0.506(3) 1.0241(19) 0.072(13) Uani 0.5 1 d . U P G -1
H22D H 0.758996 0.445893 1.022640 0.109 Uiso 0.5 1 calc R U P G -1
H22E H 0.741394 0.520613 1.063798 0.109 Uiso 0.5 1 calc R U P G -1
H22F H 0.687552 0.491157 1.002638 0.109 Uiso 0.5 1 calc R U P G -1
C23 C 0.602(3) 0.638(3) 0.8863(15) 0.059(8) Uiso 0.54(2) 1 d D U P H 1
H23A H 0.638319 0.671483 0.850268 0.071 Uiso 0.54(2) 1 calc R U P H 1
C23A C 0.513(4) 0.653(4) 0.894(2) 0.083(9) Uiso 0.54(2) 1 d D U P H 1
H23B H 0.466659 0.622888 0.861337 0.124 Uiso 0.54(2) 1 calc R U P H 1
H23C H 0.477080 0.618920 0.928870 0.124 Uiso 0.54(2) 1 calc R U P H 1
H23D H 0.537295 0.726519 0.896055 0.124 Uiso 0.54(2) 1 calc R U P H 1
C23B C 0.562(4) 0.527(3) 0.883(2) 0.083(9) Uiso 0.54(2) 1 d D U P H 1
H23E H 0.514330 0.498765 0.850175 0.124 Uiso 0.54(2) 1 calc R U P H 1
H23F H 0.618750 0.513621 0.877220 0.124 Uiso 0.54(2) 1 calc R U P H 1
H23G H 0.524738 0.493594 0.917638 0.124 Uiso 0.54(2) 1 calc R U P H 1
C23' C 0.566(2) 0.635(3) 0.941(2) 0.059(8) Uiso 0.46(2) 1 d D U P H 2
H23H H 0.542064 0.597126 0.977487 0.071 Uiso 0.46(2) 1 calc R U P H 2
C23C C 0.559(6) 0.726(4) 0.941(3) 0.083(9) Uiso 0.46(2) 1 d D U P H 2
H23I H 0.486812 0.707894 0.945010 0.124 Uiso 0.46(2) 1 calc R U P H 2
H23J H 0.599212 0.769945 0.972528 0.124 Uiso 0.46(2) 1 calc R U P H 2
H23K H 0.586042 0.762993 0.904888 0.124 Uiso 0.46(2) 1 calc R U P H 2
C23D C 0.511(6) 0.570(5) 0.893(3) 0.083(9) Uiso 0.46(2) 1 d D U P H 2
H23L H 0.436587 0.538784 0.899387 0.124 Uiso 0.46(2) 1 calc R U P H 2
H23M H 0.530131 0.610869 0.858205 0.124 Uiso 0.46(2) 1 calc R U P H 2
H23N H 0.528361 0.515303 0.889480 0.124 Uiso 0.46(2) 1 calc R U P H 2
C31 C 0.9063(16) 0.6992(14) 0.8423(8) 0.037(4) Uani 1 1 d . U . . .
C32 C 0.8807(17) 0.6216(17) 0.8027(9) 0.046(5) Uani 1 1 d . U . . .
H32A H 0.812051 0.565695 0.801068 0.056 Uiso 1 1 calc R U . . .
C33 C 0.955(2) 0.625(2) 0.7650(10) 0.060(6) Uani 1 1 d . U . . .
H33A H 0.936141 0.572686 0.736924 0.072 Uiso 1 1 calc R U . . .
C34 C 1.060(2) 0.707(2) 0.7696(12) 0.070(7) Uani 1 1 d . U . . .
H34A H 1.112328 0.708552 0.746430 0.084 Uiso 1 1 calc R U . . .
C35 C 1.0808(18) 0.7845(18) 0.8098(9) 0.048(5) Uani 1 1 d . U . . .
H35A H 1.147986 0.843003 0.811109 0.057 Uiso 1 1 calc R U . . .
C36 C 1.0073(14) 0.7785(14) 0.8474(8) 0.030(4) Uani 1 1 d . U . . .
C37 C 0.8260(15) 0.9614(15) 0.8886(8) 0.026(4) Uani 1 1 d . 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
La1 O1 2.381(15) 2_655 ?
La1 O1 2.381(15) . ?
La1 O1 2.381(15) 3_665 ?
La1 O6 2.593(11) 3_665 ?
La1 O6 2.593(11) . ?
La1 O6 2.593(11) 6_666 ?
La1 O6 2.593(11) 5_656 ?
La1 O6 2.593(11) 2_655 ?
La1 O6 2.593(11) 4_556 ?
La1 Ti1 3.619(3) 5_656 ?
La1 Ti1 3.619(3) 2_655 ?
La1 Ti1 3.619(3) 3_665 ?
La2 O21 2.442(17) 3_675 ?
La2 O21 2.442(17) 2_765 ?
La2 O21 2.442(18) . ?
La2 O25 2.582(10) . ?
La2 O25 2.582(11) 5_767 ?
La2 O25 2.582(10) 3_675 ?
La2 O25 2.582(10) 6_677 ?
La2 O25 2.582(11) 2_765 ?
La2 O25 2.582(10) 4_557 ?
La2 Ti2 3.623(3) 5_767 ?
La2 Ti2 3.623(3) 6_677 ?
La2 Ti2 3.623(3) 4_557 ?
Ti1 O3 1.772(12) . ?
Ti1 O4 1.878(13) . ?
Ti1 O1 1.905(10) . ?
Ti1 O2 1.990(11) . ?
Ti1 O5 2.019(11) . ?
Ti1 O6 2.179(13) . ?
Ti1 Ti1 3.006(6) 4_556 ?
Ti2 O23 1.771(14) . ?
Ti2 O24 1.874(12) . ?
Ti2 O21 1.900(11) . ?
Ti2 O22 2.008(11) . ?
Ti2 O26 2.058(14) . ?
Ti2 O25 2.210(13) . ?
Ti2 Ti2 3.002(5) 4_557 ?
O2 C2 1.52(3) . ?
O3 C3' 1.40(3) . ?
O3 C3 1.42(3) . ?
O4 C11 1.36(2) . ?
O5 C17 1.27(2) . ?
O6 C17 1.31(2) 3_665 ?
O22 C22 1.43(4) . ?
O23 C23' 1.40(3) . ?
O23 C23 1.46(3) . ?
O24 C31 1.35(2) . ?
O25 C37 1.27(2) 2_765 ?
O26 C37 1.24(2) . ?
C2 C2A 1.47(3) . ?
C2 C2B 1.47(3) . ?
C2 H2A 1.0000 . ?
C2A H2AA 0.9800 . ?
C2A H2AB 0.9800 . ?
C2A H2AC 0.9800 . ?
C2B H2BA 0.9800 . ?
C2B H2BB 0.9800 . ?
C2B H2BC 0.9800 . ?
C3 C3B 1.42(3) . ?
C3 C3A 1.45(3) . ?
C3 H3 1.0000 . ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?
C3A H3AC 0.9800 . ?
C3B H3BA 0.9800 . ?
C3B H3BB 0.9800 . ?
C3B H3BC 0.9800 . ?
C3' C3B' 1.37(3) . ?
C3' C3A' 1.42(3) . ?
C3' H3A' 1.0000 . ?
C3A' H3AD 0.9800 . ?
C3A' H3AE 0.9800 . ?
C3A' H3AF 0.9800 . ?
C3B' H3BD 0.9800 . ?
C3B' H3BE 0.9800 . ?
C3B' H3BF 0.9800 . ?
C11 C16 1.37(3) . ?
C11 C12 1.38(3) . ?
C12 C13 1.36(4) . ?
C12 H12A 0.9500 . ?
C13 C14 1.28(4) . ?
C13 H13A 0.9500 . ?
C14 C15 1.41(3) . ?
C14 H14A 0.9500 . ?
C15 C16 1.42(3) . ?
C15 H15A 0.9500 . ?
C16 C17 1.47(3) 3_665 ?
C22 C22B 1.42(6) . ?
C22 C22A 1.49(9) . ?
C22 H22' 1.0000 . ?
C22A H22A 0.9800 . ?
C22A H22B 0.9800 . ?
C22A H22C 0.9800 . ?
C22B H22D 0.9800 . ?
C22B H22E 0.9800 . ?
C22B H22F 0.9800 . ?
C23 C23A 1.46(3) . ?
C23 C23B 1.46(3) . ?
C23 H23A 1.0000 . ?
C23A H23B 0.9800 . ?
C23A H23C 0.9800 . ?
C23A H23D 0.9800 . ?
C23B H23E 0.9800 . ?
C23B H23F 0.9800 . ?
C23B H23G 0.9800 . ?
C23' C23C 1.42(3) . ?
C23' C23D 1.44(3) . ?
C23' H23H 1.0000 . ?
C23C H23I 0.9800 . ?
C23C H23J 0.9800 . ?
C23C H23K 0.9800 . ?
C23D H23L 0.9800 . ?
C23D H23M 0.9800 . ?
C23D H23N 0.9800 . ?
C31 C32 1.39(3) . ?
C31 C36 1.39(3) . ?
C32 C33 1.41(3) . ?
C32 H32A 0.9500 . ?
C33 C34 1.43(4) . ?
C33 H33A 0.9500 . ?
C34 C35 1.41(3) . ?
C34 H34A 0.9500 . ?
C35 C36 1.38(3) . ?
C35 H35A 0.9500 . ?
C36 C37 1.49(3) 2_765 ?

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 La1 O1 119.999(2) 2_655 . ?
O1 La1 O1 120.002(3) 2_655 3_665 ?
O1 La1 O1 119.999(2) . 3_665 ?
O1 La1 O6 73.3(4) 2_655 3_665 ?
O1 La1 O6 136.0(2) . 3_665 ?
O1 La1 O6 64.4(4) 3_665 3_665 ?
O1 La1 O6 136.0(2) 2_655 . ?
O1 La1 O6 64.4(4) . . ?
O1 La1 O6 73.3(4) 3_665 . ?
O6 La1 O6 77.7(4) 3_665 . ?
O1 La1 O6 73.3(4) 2_655 6_666 ?
O1 La1 O6 136.0(2) . 6_666 ?
O1 La1 O6 64.4(4) 3_665 6_666 ?
O6 La1 O6 87.1(5) 3_665 6_666 ?
O6 La1 O6 137.52(19) . 6_666 ?
O1 La1 O6 64.4(4) 2_655 5_656 ?
O1 La1 O6 73.3(4) . 5_656 ?
O1 La1 O6 136.0(3) 3_665 5_656 ?
O6 La1 O6 137.52(18) 3_665 5_656 ?
O6 La1 O6 137.51(18) . 5_656 ?
O6 La1 O6 77.7(4) 6_666 5_656 ?
O1 La1 O6 64.4(4) 2_655 2_655 ?
O1 La1 O6 73.3(4) . 2_655 ?
O1 La1 O6 136.0(2) 3_665 2_655 ?
O6 La1 O6 77.7(4) 3_665 2_655 ?
O6 La1 O6 77.7(4) . 2_655 ?
O6 La1 O6 137.52(18) 6_666 2_655 ?
O6 La1 O6 87.1(5) 5_656 2_655 ?
O1 La1 O6 136.0(2) 2_655 4_556 ?
O1 La1 O6 64.4(4) . 4_556 ?
O1 La1 O6 73.3(4) 3_665 4_556 ?
O6 La1 O6 137.51(18) 3_665 4_556 ?
O6 La1 O6 87.1(5) . 4_556 ?
O6 La1 O6 77.7(4) 6_666 4_556 ?
O6 La1 O6 77.7(4) 5_656 4_556 ?
O6 La1 O6 137.51(18) 2_655 4_556 ?
O1 La1 Ti1 28.5(2) 2_655 5_656 ?
O1 La1 Ti1 103.6(4) . 5_656 ?
O1 La1 Ti1 130.1(3) 3_665 5_656 ?
O6 La1 Ti1 101.0(3) 3_665 5_656 ?
O6 La1 Ti1 154.0(3) . 5_656 ?
O6 La1 Ti1 67.6(3) 6_666 5_656 ?
O6 La1 Ti1 36.6(3) 5_656 5_656 ?
O6 La1 Ti1 76.7(3) 2_655 5_656 ?
O6 La1 Ti1 109.1(2) 4_556 5_656 ?
O1 La1 Ti1 28.5(2) 2_655 2_655 ?
O1 La1 Ti1 103.6(4) . 2_655 ?
O1 La1 Ti1 130.1(3) 3_665 2_655 ?
O6 La1 Ti1 67.6(3) 3_665 2_655 ?
O6 La1 Ti1 109.1(2) . 2_655 ?
O6 La1 Ti1 101.0(3) 6_666 2_655 ?
O6 La1 Ti1 76.7(3) 5_656 2_655 ?
O6 La1 Ti1 36.6(3) 2_655 2_655 ?
O6 La1 Ti1 154.0(3) 4_556 2_655 ?
Ti1 La1 Ti1 49.07(9) 5_656 2_655 ?
O1 La1 Ti1 103.6(4) 2_655 3_665 ?
O1 La1 Ti1 130.1(3) . 3_665 ?
O1 La1 Ti1 28.5(2) 3_665 3_665 ?
O6 La1 Ti1 36.6(3) 3_665 3_665 ?
O6 La1 Ti1 67.6(3) . 3_665 ?
O6 La1 Ti1 76.7(3) 6_666 3_665 ?
O6 La1 Ti1 154.0(3) 5_656 3_665 ?
O6 La1 Ti1 109.1(2) 2_655 3_665 ?
O6 La1 Ti1 101.0(3) 4_556 3_665 ?
Ti1 La1 Ti1 125.89(2) 5_656 3_665 ?
Ti1 La1 Ti1 103.97(5) 2_655 3_665 ?
O21 La2 O21 120.000(15) 3_675 2_765 ?
O21 La2 O21 120.001(8) 3_675 . ?
O21 La2 O21 119.999(5) 2_765 . ?
O21 La2 O25 136.5(2) 3_675 . ?
O21 La2 O25 71.8(4) 2_765 . ?
O21 La2 O25 65.5(4) . . ?
O21 La2 O25 71.8(4) 3_675 5_767 ?
O21 La2 O25 65.5(4) 2_765 5_767 ?
O21 La2 O25 136.5(2) . 5_767 ?
O25 La2 O25 137.29(18) . 5_767 ?
O21 La2 O25 65.5(4) 3_675 3_675 ?
O21 La2 O25 136.5(2) 2_765 3_675 ?
O21 La2 O25 71.8(4) . 3_675 ?
O25 La2 O25 78.2(4) . 3_675 ?
O25 La2 O25 137.29(18) 5_767 3_675 ?
O21 La2 O25 65.5(4) 3_675 6_677 ?
O21 La2 O25 136.5(2) 2_765 6_677 ?
O21 La2 O25 71.8(4) . 6_677 ?
O25 La2 O25 137.29(18) . 6_677 ?
O25 La2 O25 78.2(4) 5_767 6_677 ?
O25 La2 O25 86.5(5) 3_675 6_677 ?
O21 La2 O25 71.8(4) 3_675 2_765 ?
O21 La2 O25 65.5(4) 2_765 2_765 ?
O21 La2 O25 136.5(2) . 2_765 ?
O25 La2 O25 78.2(4) . 2_765 ?
O25 La2 O25 86.5(5) 5_767 2_765 ?
O25 La2 O25 78.2(4) 3_675 2_765 ?
O25 La2 O25 137.29(18) 6_677 2_765 ?
O21 La2 O25 136.5(2) 3_675 4_557 ?
O21 La2 O25 71.8(4) 2_765 4_557 ?
O21 La2 O25 65.5(4) . 4_557 ?
O25 La2 O25 86.5(5) . 4_557 ?
O25 La2 O25 78.2(4) 5_767 4_557 ?
O25 La2 O25 137.29(18) 3_675 4_557 ?
O25 La2 O25 78.2(4) 6_677 4_557 ?
O25 La2 O25 137.29(18) 2_765 4_557 ?
O21 La2 Ti2 102.7(4) 3_675 5_767 ?
O21 La2 Ti2 29.0(2) 2_765 5_767 ?
O21 La2 Ti2 130.9(4) . 5_767 ?
O25 La2 Ti2 100.2(3) . 5_767 ?
O25 La2 Ti2 37.2(3) 5_767 5_767 ?
O25 La2 Ti2 154.7(3) 3_675 5_767 ?
O25 La2 Ti2 109.6(2) 6_677 5_767 ?
O25 La2 Ti2 76.8(3) 2_765 5_767 ?
O25 La2 Ti2 67.0(3) 4_557 5_767 ?
O21 La2 Ti2 29.0(2) 3_675 6_677 ?
O21 La2 Ti2 130.9(4) 2_765 6_677 ?
O21 La2 Ti2 102.7(4) . 6_677 ?
O25 La2 Ti2 154.7(3) . 6_677 ?
O25 La2 Ti2 67.0(3) 5_767 6_677 ?
O25 La2 Ti2 76.8(3) 3_675 6_677 ?
O25 La2 Ti2 37.2(3) 6_677 6_677 ?
O25 La2 Ti2 100.2(3) 2_765 6_677 ?
O25 La2 Ti2 109.6(2) 4_557 6_677 ?
Ti2 La2 Ti2 104.03(5) 5_767 6_677 ?
O21 La2 Ti2 130.9(4) 3_675 4_557 ?
O21 La2 Ti2 102.7(4) 2_765 4_557 ?
O21 La2 Ti2 29.0(2) . 4_557 ?
O25 La2 Ti2 76.8(3) . 4_557 ?
O25 La2 Ti2 109.6(2) 5_767 4_557 ?
O25 La2 Ti2 100.2(3) 3_675 4_557 ?
O25 La2 Ti2 67.0(3) 6_677 4_557 ?
O25 La2 Ti2 154.7(3) 2_765 4_557 ?
O25 La2 Ti2 37.2(3) 4_557 4_557 ?
Ti2 La2 Ti2 104.03(5) 5_767 4_557 ?
Ti2 La2 Ti2 104.03(5) 6_677 4_557 ?
O3 Ti1 O4 94.9(6) . . ?
O3 Ti1 O1 104.2(6) . . ?
O4 Ti1 O1 160.3(6) . . ?
O3 Ti1 O2 98.8(6) . . ?
O4 Ti1 O2 97.6(6) . . ?
O1 Ti1 O2 75.2(6) . . ?
O3 Ti1 O5 91.4(6) . . ?
O4 Ti1 O5 95.1(6) . . ?
O1 Ti1 O5 89.1(5) . . ?
O2 Ti1 O5 162.9(5) . . ?
O3 Ti1 O6 169.8(5) . . ?
O4 Ti1 O6 81.0(5) . . ?
O1 Ti1 O6 80.8(6) . . ?
O2 Ti1 O6 91.1(6) . . ?
O5 Ti1 O6 79.7(5) . . ?
O3 Ti1 Ti1 91.8(4) . 4_556 ?
O4 Ti1 Ti1 138.6(4) . 4_556 ?
O1 Ti1 Ti1 37.9(4) . 4_556 ?
O2 Ti1 Ti1 40.9(4) . 4_556 ?
O5 Ti1 Ti1 125.6(3) . 4_556 ?
O6 Ti1 Ti1 97.5(3) . 4_556 ?
O3 Ti1 La1 137.7(4) . . ?
O4 Ti1 La1 126.1(4) . . ?
O1 Ti1 La1 36.7(4) . . ?
O2 Ti1 La1 86.8(4) . . ?
O5 Ti1 La1 76.5(3) . . ?
O6 Ti1 La1 45.1(3) . . ?
Ti1 Ti1 La1 65.47(5) 4_556 . ?
O23 Ti2 O24 94.4(6) . . ?
O23 Ti2 O21 102.7(7) . . ?
O24 Ti2 O21 162.5(7) . . ?
O23 Ti2 O22 96.0(7) . . ?
O24 Ti2 O22 97.9(6) . . ?
O21 Ti2 O22 77.0(5) . . ?
O23 Ti2 O26 92.1(6) . . ?
O24 Ti2 O26 94.4(6) . . ?
O21 Ti2 O26 88.5(6) . . ?
O22 Ti2 O26 164.6(6) . . ?
O23 Ti2 O25 171.1(5) . . ?
O24 Ti2 O25 80.9(5) . . ?
O21 Ti2 O25 82.6(6) . . ?
O22 Ti2 O25 92.2(6) . . ?
O26 Ti2 O25 80.8(5) . . ?
O23 Ti2 Ti2 91.5(4) . 4_557 ?
O24 Ti2 Ti2 139.5(4) . 4_557 ?
O21 Ti2 Ti2 37.8(4) . 4_557 ?
O22 Ti2 Ti2 41.6(4) . 4_557 ?
O26 Ti2 Ti2 125.3(4) . 4_557 ?
O25 Ti2 Ti2 97.0(3) . 4_557 ?
O23 Ti2 La2 138.6(4) . . ?
O24 Ti2 La2 125.7(4) . . ?
O21 Ti2 La2 38.5(5) . . ?
O22 Ti2 La2 88.7(4) . . ?
O26 Ti2 La2 76.7(4) . . ?
O25 Ti2 La2 44.9(3) . . ?
Ti2 Ti2 La2 65.52(4) 4_557 . ?
Ti1 O1 Ti1 104.2(7) 4_556 . ?
Ti1 O1 La1 114.8(5) 4_556 . ?
Ti1 O1 La1 114.8(5) . . ?
C2 O2 Ti1 129.7(4) . . ?
C2 O2 Ti1 129.7(4) . 4_556 ?
Ti1 O2 Ti1 98.1(7) . 4_556 ?
C3' O3 Ti1 163.9(18) . . ?
C3 O3 Ti1 138.7(18) . . ?
C11 O4 Ti1 140.6(12) . . ?
C17 O5 Ti1 141.2(14) . . ?
C17 O6 Ti1 132.2(12) 3_665 . ?
C17 O6 La1 129.3(12) 3_665 . ?
Ti1 O6 La1 98.3(4) . . ?
Ti2 O21 Ti2 104.4(8) . 4_557 ?
Ti2 O21 La2 112.5(6) . . ?
Ti2 O21 La2 112.5(6) 4_557 . ?
C22 O22 Ti2 130.9(4) . . ?
C22 O22 Ti2 130.9(4) . 4_557 ?
Ti2 O22 Ti2 96.7(7) . 4_557 ?
C23' O23 Ti2 168(2) . . ?
C23 O23 Ti2 130.9(17) . . ?
C31 O24 Ti2 141.1(11) . . ?
C37 O25 Ti2 131.8(12) 2_765 . ?
C37 O25 La2 129.9(12) 2_765 . ?
Ti2 O25 La2 97.9(4) . . ?
C37 O26 Ti2 139.0(15) . . ?
C2A C2 C2B 138(3) . . ?
C2A C2 O2 109(2) . . ?
C2B C2 O2 111(3) . . ?
C2A C2 H2A 94.2 . . ?
C2B C2 H2A 94.2 . . ?
O2 C2 H2A 94.2 . . ?
C2 C2A H2AA 109.5 . . ?
C2 C2A H2AB 109.5 . . ?
H2AA C2A H2AB 109.5 . . ?
C2 C2A H2AC 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
C2 C2B H2BA 109.5 . . ?
C2 C2B H2BB 109.5 . . ?
H2BA C2B H2BB 109.5 . . ?
C2 C2B H2BC 109.5 . . ?
H2BA C2B H2BC 109.5 . . ?
H2BB C2B H2BC 109.5 . . ?
O3 C3 C3B 111(2) . . ?
O3 C3 C3A 112(2) . . ?
C3B C3 C3A 111(3) . . ?
O3 C3 H3 107.6 . . ?
C3B C3 H3 107.6 . . ?
C3A C3 H3 107.6 . . ?
C3 C3A H3AA 109.5 . . ?
C3 C3A H3AB 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
C3 C3A H3AC 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
C3 C3B H3BA 109.5 . . ?
C3 C3B H3BB 109.5 . . ?
H3BA C3B H3BB 109.5 . . ?
C3 C3B H3BC 109.5 . . ?
H3BA C3B H3BC 109.5 . . ?
H3BB C3B H3BC 109.5 . . ?
C3B' C3' O3 122(3) . . ?
C3B' C3' C3A' 117(3) . . ?
O3 C3' C3A' 113(2) . . ?
C3B' C3' H3A' 99.8 . . ?
O3 C3' H3A' 99.8 . . ?
C3A' C3' H3A' 99.8 . . ?
C3' C3A' H3AD 109.5 . . ?
C3' C3A' H3AE 109.5 . . ?
H3AD C3A' H3AE 109.5 . . ?
C3' C3A' H3AF 109.5 . . ?
H3AD C3A' H3AF 109.5 . . ?
H3AE C3A' H3AF 109.5 . . ?
C3' C3B' H3BD 109.5 . . ?
C3' C3B' H3BE 109.5 . . ?
H3BD C3B' H3BE 109.5 . . ?
C3' C3B' H3BF 109.5 . . ?
H3BD C3B' H3BF 109.5 . . ?
H3BE C3B' H3BF 109.5 . . ?
O4 C11 C16 121.4(18) . . ?
O4 C11 C12 118.3(19) . . ?
C16 C11 C12 120(2) . . ?
C13 C12 C11 118(2) . . ?
C13 C12 H12A 121.0 . . ?
C11 C12 H12A 121.0 . . ?
C14 C13 C12 126(2) . . ?
C14 C13 H13A 117.1 . . ?
C12 C13 H13A 117.1 . . ?
C13 C14 C15 118(3) . . ?
C13 C14 H14A 120.8 . . ?
C15 C14 H14A 120.8 . . ?
C14 C15 C16 118(2) . . ?
C14 C15 H15A 120.8 . . ?
C16 C15 H15A 120.8 . . ?
C11 C16 C15 119.0(19) . . ?
C11 C16 C17 124.3(19) . 3_665 ?
C15 C16 C17 116.7(18) . 3_665 ?
O5 C17 O6 120.5(19) . 2_655 ?
O5 C17 C16 119.5(18) . 2_655 ?
O6 C17 C16 120.0(18) 2_655 2_655 ?
C22B C22 O22 114(4) . . ?
C22B C22 C22A 137(5) . . ?
O22 C22 C22A 100(4) . . ?
C22B C22 H22' 99.3 . . ?
O22 C22 H22' 99.3 . . ?
C22A C22 H22' 99.3 . . ?
C22 C22A H22A 109.5 . . ?
C22 C22A H22B 109.5 . . ?
H22A C22A H22B 109.5 . . ?
C22 C22A H22C 109.5 . . ?
H22A C22A H22C 109.5 . . ?
H22B C22A H22C 109.5 . . ?
C22 C22B H22D 109.5 . . ?
C22 C22B H22E 109.5 . . ?
H22D C22B H22E 109.5 . . ?
C22 C22B H22F 109.5 . . ?
H22D C22B H22F 109.5 . . ?
H22E C22B H22F 109.5 . . ?
O23 C23 C23A 110(3) . . ?
O23 C23 C23B 111(3) . . ?
C23A C23 C23B 107(3) . . ?
O23 C23 H23A 109.5 . . ?
C23A C23 H23A 109.5 . . ?
C23B C23 H23A 109.5 . . ?
C23 C23A H23B 109.5 . . ?
C23 C23A H23C 109.5 . . ?
H23B C23A H23C 109.5 . . ?
C23 C23A H23D 109.5 . . ?
H23B C23A H23D 109.5 . . ?
H23C C23A H23D 109.5 . . ?
C23 C23B H23E 109.5 . . ?
C23 C23B H23F 109.5 . . ?
H23E C23B H23F 109.5 . . ?
C23 C23B H23G 109.5 . . ?
H23E C23B H23G 109.5 . . ?
H23F C23B H23G 109.5 . . ?
O23 C23' C23C 98(4) . . ?
O23 C23' C23D 112(4) . . ?
C23C C23' C23D 111(3) . . ?
O23 C23' H23H 111.6 . . ?
C23C C23' H23H 111.6 . . ?
C23D C23' H23H 111.6 . . ?
C23' C23C H23I 109.5 . . ?
C23' C23C H23J 109.5 . . ?
H23I C23C H23J 109.5 . . ?
C23' C23C H23K 109.5 . . ?
H23I C23C H23K 109.5 . . ?
H23J C23C H23K 109.5 . . ?
C23' C23D H23L 109.5 . . ?
C23' C23D H23M 109.5 . . ?
H23L C23D H23M 109.5 . . ?
C23' C23D H23N 109.5 . . ?
H23L C23D H23N 109.5 . . ?
H23M C23D H23N 109.5 . . ?
O24 C31 C32 117.4(18) . . ?
O24 C31 C36 122.3(16) . . ?
C32 C31 C36 120.3(19) . . ?
C31 C32 C33 121(2) . . ?
C31 C32 H32A 119.5 . . ?
C33 C32 H32A 119.5 . . ?
C32 C33 C34 119(2) . . ?
C32 C33 H33A 120.4 . . ?
C34 C33 H33A 120.4 . . ?
C35 C34 C33 117(2) . . ?
C35 C34 H34A 121.3 . . ?
C33 C34 H34A 121.3 . . ?
C36 C35 C34 122(2) . . ?
C36 C35 H35A 118.9 . . ?
C34 C35 H35A 118.9 . . ?
C35 C36 C31 119.7(19) . . ?
C35 C36 C37 117.6(18) . 2_765 ?
C31 C36 C37 122.4(17) . 2_765 ?
O26 C37 O25 123(2) . 3_675 ?
O26 C37 C36 115.5(18) . 3_675 ?
O25 C37 C36 121.2(17) 3_675 3_675 ?

_refine_diff_density_max         6.820
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.194

