# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_Ti4Dy2
_database_code_depnum_ccdc_archive 'CCDC 2283715'
loop_
_audit_author_name
_audit_author_address
'Andrew Bond'
;University of Cambridge
United Kingdom
;
_audit_update_record             
;
2023-07-22 deposited with the CCDC.	2023-09-15 downloaded from the CCDC.
;
#===============================================================================
_audit_creation_method           SHELXL-2019/2

#-------------------------------------------------------------------------------
# Inserted by local software: cifUpdate ver. 3.1  (Andrew D. Bond, March 2019)
#-------------------------------------------------------------------------------
_cambridge_user_name             'Rosa Mueller'
_cambridge_user_crsid            rm2055
_cambridge_supervisor_name       'Dominic Wright'
_cambridge_supervisor_crsid      dsw1000
_cambridge_crystallographer_name 'Andrew Bond'
_cambridge_crystallographer_crsid adb29
_cambridge_sample_id             RM93C(Dy)
_cambridge_data_id               DW_B2_0375
#-------------------------------------------------------------------------------

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H92 Cl2 Dy2 O20 Ti4'
_chemical_formula_sum            'C36 H92 Cl2 Dy2 O20 Ti4'
_chemical_formula_weight         1432.59

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'
Cl Cl 0.3639 0.7018 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   11.9219(5)
_cell_length_b                   18.7644(8)
_cell_length_c                   12.7482(6)
_cell_angle_alpha                90
_cell_angle_beta                 92.549(2)
_cell_angle_gamma                90
_cell_volume                     2849.0(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9907
_cell_measurement_theta_min      5.50
_cell_measurement_theta_max      66.45

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_F_000             1444
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    19.716
_shelx_estimated_absorpt_T_min   0.301
_shelx_estimated_absorpt_T_max   0.506
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4677
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Incoatec I\mS Cu microsource'
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-III'
_diffrn_measurement_method       'ω and φ-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28283
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         5.502
_diffrn_reflns_theta_max         66.529
_diffrn_reflns_theta_full        66.529
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             5003
_reflns_number_gt                4631
_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.

#===============================================================================
INTENSITY STATISTICS FOR DATASET # 1  DW_B2_0375_0m.hkl
#===============================================================================
 Resolution   #Data #Theory %Complete Redundancy Mean I Mean I/s Rmerge  Rsigma
#-------------------------------------------------------------------------------
  Inf - 3.51      78     84     92.9     3.45     69.38   29.33  0.0339  0.0279
 3.51 - 2.31     181    182     99.5     3.81    131.39   29.25  0.0309  0.0311
 2.31 - 1.83     263    263    100.0     5.39    101.32   33.37  0.0334  0.0231
 1.83 - 1.59     261    264     98.9     6.77     85.62   35.97  0.0363  0.0211
 1.59 - 1.44     266    266    100.0     8.32     69.62   38.77  0.0367  0.0188
 1.44 - 1.34     254    254    100.0     8.30     53.12   35.63  0.0395  0.0207
 1.34 - 1.26     257    258     99.6     7.90     46.34   28.99  0.0427  0.0224
 1.26 - 1.19     286    287     99.7     7.57     45.14   29.46  0.0441  0.0240
 1.19 - 1.14     260    260    100.0     7.50     35.65   27.19  0.0493  0.0257
 1.14 - 1.10     228    228    100.0     7.01     42.21   27.73  0.0487  0.0254
 1.10 - 1.06     264    264    100.0     6.53     34.39   23.11  0.0636  0.0302
 1.06 - 1.03     255    255    100.0     6.61     33.11   25.23  0.0581  0.0282
 1.03 - 0.99     328    328    100.0     5.69     30.29   22.38  0.0620  0.0306
 0.99 - 0.97     216    218     99.1     4.25     28.47   20.47  0.0510  0.0343
 0.97 - 0.94     328    330     99.4     4.08     21.93   19.45  0.0469  0.0362
 0.94 - 0.92     230    231     99.6     3.95     22.52   18.82  0.0490  0.0358
 0.92 - 0.90     278    278    100.0     3.58     21.21   17.78  0.0532  0.0383
 0.90 - 0.88     298    298    100.0     3.60     19.27   18.18  0.0566  0.0390
 0.88 - 0.87     164    164    100.0     3.53     16.85   17.84  0.0546  0.0406
 0.87 - 0.85     310    310    100.0     3.08     18.64   17.45  0.0480  0.0400
 0.85 - 0.84     177    186     95.2     2.58     15.46   14.39  0.0489  0.0466
#-------------------------------------------------------------------------------
 0.94 - 0.84    1457   1467     99.3     3.40     19.28   17.55  0.0519  0.0394
  Inf - 0.84    5182   5208     99.5     5.53     43.00   25.21  0.0434  0.0272
#===============================================================================
;

_computing_data_collection       'APEX4 (Bruker, 2021)'
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL

_refine_special_details          ?

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0159P)²+2.2898P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5003
_refine_ls_number_parameters     329
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0210
_refine_ls_wR_factor_ref         0.0490
_refine_ls_wR_factor_gt          0.0477
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.068

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 0.38196(2) 0.54088(2) 0.42014(2) 0.01307(5) Uani 1 1 d . . . . .
Ti2 Ti 0.39086(3) 0.54409(2) 0.67612(3) 0.01361(9) Uani 1 1 d . . . . .
Ti1 Ti 0.49474(3) 0.66502(2) 0.57324(3) 0.01400(10) Uani 1 1 d . . . . .
Cl1 Cl 0.22872(5) 0.61130(3) 0.30550(6) 0.02799(15) Uani 1 1 d . . . . .
C11 C 0.4561(2) 0.71267(14) 0.3509(2) 0.0255(6) Uani 1 1 d . . . . .
H11A H 0.393984 0.742377 0.375769 0.031 Uiso 1 1 calc R U . . .
H11B H 0.432598 0.693293 0.281158 0.031 Uiso 1 1 calc R U . . .
C12 C 0.5592(3) 0.75847(17) 0.3407(3) 0.0393(8) Uani 1 1 d . . . . .
H12A H 0.578229 0.781533 0.408147 0.059 Uiso 1 1 calc R U . . .
H12B H 0.544081 0.794967 0.286936 0.059 Uiso 1 1 calc R U . . .
H12C H 0.622113 0.728647 0.320428 0.059 Uiso 1 1 calc R U . . .
C21 C 0.5253(8) 0.6474(4) 0.8187(6) 0.031(3) Uani 0.347(9) 1 d D . P A 1
H21A H 0.601056 0.626192 0.815034 0.037 Uiso 0.347(9) 1 calc R U P A 1
H21B H 0.486382 0.621401 0.874086 0.037 Uiso 0.347(9) 1 calc R U P A 1
C22 C 0.5396(4) 0.72270(19) 0.8539(3) 0.0562(11) Uani 0.347(9) 1 d D . P A 1
H22A H 0.584660 0.748604 0.804047 0.084 Uiso 0.347(9) 1 calc R U P A 1
H22B H 0.577678 0.723698 0.923642 0.084 Uiso 0.347(9) 1 calc R U P A 1
H22C H 0.465721 0.745331 0.857306 0.084 Uiso 0.347(9) 1 calc R U P A 1
C21A C 0.4478(4) 0.6766(2) 0.8148(3) 0.0257(14) Uani 0.653(9) 1 d D . P A 2
H21C H 0.427451 0.644460 0.872487 0.031 Uiso 0.653(9) 1 calc R U P A 2
H21D H 0.381705 0.707025 0.797481 0.031 Uiso 0.653(9) 1 calc R U P A 2
C22A C 0.5396(4) 0.72270(19) 0.8539(3) 0.0562(11) Uani 0.653(9) 1 d D . P A 2
H22D H 0.605798 0.693565 0.872211 0.084 Uiso 0.653(9) 1 calc R U P A 2
H22E H 0.516421 0.748300 0.916407 0.084 Uiso 0.653(9) 1 calc R U P A 2
H22F H 0.557855 0.757078 0.799415 0.084 Uiso 0.653(9) 1 calc R U P A 2
C31 C 0.2580(2) 0.41963(14) 0.6021(2) 0.0229(6) Uani 1 1 d . . . . .
H31A H 0.286295 0.404018 0.672632 0.028 Uiso 1 1 calc R U . . .
H31B H 0.276445 0.382041 0.551196 0.028 Uiso 1 1 calc R U . . .
C32 C 0.1327(3) 0.42866(19) 0.6023(3) 0.0460(9) Uani 1 1 d . . . . .
H32A H 0.113828 0.462411 0.657444 0.069 Uiso 1 1 calc R U . . .
H32B H 0.097528 0.382517 0.615565 0.069 Uiso 1 1 calc R U . . .
H32C H 0.105035 0.446932 0.533903 0.069 Uiso 1 1 calc R U . . .
C41 C 0.2312(2) 0.66688(14) 0.5798(2) 0.0241(6) Uani 1 1 d . . . . .
H41A H 0.229703 0.703287 0.523528 0.029 Uiso 1 1 calc R U . . .
H41B H 0.238315 0.691969 0.648059 0.029 Uiso 1 1 calc R U . . .
C42 C 0.1227(2) 0.62598(16) 0.5738(2) 0.0304(7) Uani 1 1 d . . . . .
H42A H 0.116444 0.599658 0.507357 0.046 Uiso 1 1 calc R U . . .
H42B H 0.059564 0.659228 0.577425 0.046 Uiso 1 1 calc R U . . .
H42C H 0.121242 0.592402 0.632556 0.046 Uiso 1 1 calc R U . . .
C51 C 0.3857(3) 0.81753(16) 0.6052(3) 0.0480(9) Uani 1 1 d . . . . .
H51A H 0.348789 0.812757 0.672875 0.058 Uiso 1 1 calc R U . . .
H51B H 0.326307 0.823240 0.549095 0.058 Uiso 1 1 calc R U . . .
C52 C 0.4579(3) 0.88177(17) 0.6086(4) 0.0623(12) Uani 1 1 d . . . . .
H52A H 0.514349 0.877468 0.666495 0.093 Uiso 1 1 calc R U . . .
H52B H 0.411633 0.924076 0.619289 0.093 Uiso 1 1 calc R U . . .
H52C H 0.495582 0.886271 0.542089 0.093 Uiso 1 1 calc R U . . .
C61 C 0.7131(2) 0.74128(14) 0.6272(2) 0.0282(6) Uani 1 1 d . . . . .
H61A H 0.740586 0.736233 0.701254 0.034 Uiso 1 1 calc R U . . .
H61B H 0.665175 0.784310 0.621919 0.034 Uiso 1 1 calc R U . . .
C62 C 0.8114(2) 0.75053(16) 0.5591(3) 0.0354(7) Uani 1 1 d . . . . .
H62A H 0.860310 0.708659 0.565841 0.053 Uiso 1 1 calc R U . . .
H62B H 0.853618 0.793186 0.581063 0.053 Uiso 1 1 calc R U . . .
H62C H 0.784462 0.755782 0.485703 0.053 Uiso 1 1 calc R U . . .
C71 C 0.2186(3) 0.5754(2) 0.8491(3) 0.0432(8) Uani 1 1 d . . . . .
H71A H 0.141208 0.559792 0.829166 0.052 Uiso 1 1 calc R U . . .
H71B H 0.220630 0.628079 0.844627 0.052 Uiso 1 1 calc R U . . .
C72 C 0.2466(3) 0.5533(2) 0.9596(3) 0.0489(9) Uani 1 1 d . . . . .
H72A H 0.242829 0.501255 0.964893 0.073 Uiso 1 1 calc R U . . .
H72B H 0.192813 0.574708 1.006240 0.073 Uiso 1 1 calc R U . . .
H72C H 0.322632 0.569383 0.980215 0.073 Uiso 1 1 calc R U . . .
C81 C 0.5211(3) 0.45350(16) 0.8335(2) 0.0317(7) Uani 1 1 d . . . . .
H81A H 0.521312 0.496213 0.879090 0.038 Uiso 1 1 calc R U . . .
H81B H 0.596768 0.431796 0.839789 0.038 Uiso 1 1 calc R U . . .
C82 C 0.4363(3) 0.40100(18) 0.8710(3) 0.0467(9) Uani 1 1 d . . . . .
H82A H 0.361121 0.422105 0.864556 0.070 Uiso 1 1 calc R U . . .
H82B H 0.454260 0.389063 0.944729 0.070 Uiso 1 1 calc R U . . .
H82C H 0.438305 0.357643 0.828317 0.070 Uiso 1 1 calc R U . . .
C91 C 0.1566(3) 0.43950(19) 0.3012(3) 0.0319(12) Uani 0.815(9) 1 d D . P B 1
H91A H 0.112885 0.482866 0.316283 0.038 Uiso 0.815(9) 1 calc R U P B 1
H91B H 0.119396 0.398364 0.333623 0.038 Uiso 0.815(9) 1 calc R U P B 1
C92 C 0.1581(6) 0.4287(4) 0.1847(4) 0.071(2) Uani 0.815(9) 1 d D . P B 1
H92A H 0.194288 0.469606 0.152514 0.107 Uiso 0.815(9) 1 calc R U P B 1
H92B H 0.080888 0.424174 0.155704 0.107 Uiso 0.815(9) 1 calc R U P B 1
H92C H 0.199994 0.385188 0.169794 0.107 Uiso 0.815(9) 1 calc R U P B 1
C91A C 0.2294(12) 0.4397(8) 0.2368(8) 0.037(6) Uani 0.185(9) 1 d D . P B 2
H91C H 0.264650 0.397295 0.205877 0.044 Uiso 0.185(9) 1 calc R U P B 2
H91D H 0.252774 0.482122 0.197143 0.044 Uiso 0.185(9) 1 calc R U P B 2
C92A C 0.1006(14) 0.4322(19) 0.2262(17) 0.070(9) Uani 0.185(9) 1 d D . P B 2
H92D H 0.079649 0.382486 0.238409 0.105 Uiso 0.185(9) 1 calc R U P B 2
H92E H 0.074280 0.446499 0.155387 0.105 Uiso 0.185(9) 1 calc R U P B 2
H92F H 0.066148 0.462830 0.278025 0.105 Uiso 0.185(9) 1 calc R U P B 2
O1 O 0.47656(14) 0.65517(8) 0.42252(14) 0.0175(4) Uani 1 1 d . . . . .
O2 O 0.46882(15) 0.63428(9) 0.72568(14) 0.0221(4) Uani 1 1 d D . . . .
O3 O 0.31290(13) 0.48452(9) 0.57499(14) 0.0174(4) Uani 1 1 d . . . . .
O4 O 0.32693(13) 0.62164(8) 0.56903(14) 0.0162(4) Uani 1 1 d . . . . .
O5 O 0.44761(15) 0.75491(9) 0.58632(16) 0.0251(4) Uani 1 1 d . . . . .
O6 O 0.64776(14) 0.68012(8) 0.59734(14) 0.0190(4) Uani 1 1 d . . . . .
O7 O 0.29259(14) 0.54683(9) 0.77803(15) 0.0208(4) Uani 1 1 d . . . . .
O8 O 0.49791(14) 0.47472(9) 0.72679(14) 0.0182(4) Uani 1 1 d . . . . .
O9 O 0.26846(14) 0.44672(9) 0.34605(16) 0.0247(4) Uani 1 1 d D . . . .
H9 H 0.312246 0.413911 0.374554 0.037 Uiso 1 1 d R U . B .
O10 O 0.50342(13) 0.55958(8) 0.56628(13) 0.0132(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O10 2.3302(15) 3_666 ?
Dy1 O10 2.3348(15) . ?
Dy1 O9 2.3939(16) . ?
Dy1 O3 2.4162(17) . ?
Dy1 O1 2.4226(16) . ?
Dy1 O8 2.4256(18) 3_666 ?
Dy1 O4 2.5378(17) . ?
Dy1 Cl1 2.6423(6) . ?
Dy1 Ti2 3.2609(5) . ?
Dy1 Ti1 3.2879(4) . ?
Dy1 Ti2 3.4175(4) 3_666 ?
Dy1 Dy1 3.7299(3) 3_666 ?
Ti2 O7 1.7884(18) . ?
Ti2 O8 1.9150(17) . ?
Ti2 O3 1.9155(17) . ?
Ti2 O10 2.0033(17) . ?
Ti2 O2 2.0185(17) . ?
Ti2 O4 2.1141(17) . ?
Ti2 Ti1 2.9236(6) . ?
Ti1 O5 1.7880(17) . ?
Ti1 O6 1.8582(16) . ?
Ti1 O1 1.9328(18) . ?
Ti1 O10 1.9833(16) . ?
Ti1 O2 2.0635(18) . ?
Ti1 O4 2.1583(16) . ?
C11 O1 1.427(3) . ?
C11 C12 1.510(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C21 O2 1.360(6) . ?
C21 C22 1.490(7) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C21A O2 1.418(4) . ?
C21A C22A 1.464(5) . ?
C21A H21C 0.9900 . ?
C21A H21D 0.9900 . ?
C22A H22D 0.9800 . ?
C22A H22E 0.9800 . ?
C22A H22F 0.9800 . ?
C31 O3 1.432(3) . ?
C31 C32 1.504(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C41 O4 1.434(3) . ?
C41 C42 1.503(4) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C51 O5 1.414(3) . ?
C51 C52 1.481(5) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C61 O6 1.429(3) . ?
C61 C62 1.499(4) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C71 O7 1.400(4) . ?
C71 C72 1.492(5) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C81 O8 1.433(3) . ?
C81 C82 1.505(5) . ?
C81 H81A 0.9900 . ?
C81 H81B 0.9900 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C91 O9 1.434(3) . ?
C91 C92 1.499(6) . ?
C91 H91A 0.9900 . ?
C91 H91B 0.9900 . ?
C92 H92A 0.9800 . ?
C92 H92B 0.9800 . ?
C92 H92C 0.9800 . ?
C91A O9 1.455(9) . ?
C91A C92A 1.541(10) . ?
C91A H91C 0.9900 . ?
C91A H91D 0.9900 . ?
C92A H92D 0.9800 . ?
C92A H92E 0.9800 . ?
C92A H92F 0.9800 . ?
O9 H9 0.8756 . ?

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
O10 Dy1 O10 73.83(6) 3_666 . ?
O10 Dy1 O9 75.62(6) 3_666 . ?
O10 Dy1 O9 138.19(6) . . ?
O10 Dy1 O3 78.77(6) 3_666 . ?
O10 Dy1 O3 68.63(5) . . ?
O9 Dy1 O3 78.00(6) . . ?
O10 Dy1 O1 116.36(5) 3_666 . ?
O10 Dy1 O1 65.48(6) . . ?
O9 Dy1 O1 155.92(6) . . ?
O3 Dy1 O1 123.54(6) . . ?
O10 Dy1 O8 66.13(6) 3_666 3_666 ?
O10 Dy1 O8 105.53(6) . 3_666 ?
O9 Dy1 O8 87.08(6) . 3_666 ?
O3 Dy1 O8 144.34(5) . 3_666 ?
O1 Dy1 O8 79.98(6) . 3_666 ?
O10 Dy1 O4 126.71(5) 3_666 . ?
O10 Dy1 O4 59.01(5) . . ?
O9 Dy1 O4 125.13(6) . . ?
O3 Dy1 O4 62.71(5) . . ?
O1 Dy1 O4 66.28(6) . . ?
O8 Dy1 O4 146.17(5) 3_666 . ?
O10 Dy1 Cl1 146.55(4) 3_666 . ?
O10 Dy1 Cl1 139.04(4) . . ?
O9 Dy1 Cl1 77.65(4) . . ?
O3 Dy1 Cl1 114.73(4) . . ?
O1 Dy1 Cl1 82.78(4) . . ?
O8 Dy1 Cl1 92.91(4) 3_666 . ?
O4 Dy1 Cl1 85.39(4) . . ?
O10 Dy1 Ti2 87.00(4) 3_666 . ?
O10 Dy1 Ti2 37.55(4) . . ?
O9 Dy1 Ti2 113.65(5) . . ?
O3 Dy1 Ti2 35.66(4) . . ?
O1 Dy1 Ti2 88.66(4) . . ?
O8 Dy1 Ti2 141.35(4) 3_666 . ?
O4 Dy1 Ti2 40.40(4) . . ?
Cl1 Dy1 Ti2 122.354(18) . . ?
O10 Dy1 Ti1 107.82(4) 3_666 . ?
O10 Dy1 Ti1 36.59(4) . . ?
O9 Dy1 Ti1 165.05(5) . . ?
O3 Dy1 Ti1 88.30(4) . . ?
O1 Dy1 Ti1 35.66(4) . . ?
O8 Dy1 Ti1 107.70(4) 3_666 . ?
O4 Dy1 Ti1 41.01(4) . . ?
Cl1 Dy1 Ti1 103.206(16) . . ?
Ti2 Dy1 Ti1 53.027(11) . . ?
O10 Dy1 Ti2 34.69(4) 3_666 3_666 ?
O10 Dy1 Ti2 83.30(4) . 3_666 ?
O9 Dy1 Ti2 87.54(5) . 3_666 ?
O3 Dy1 Ti2 113.17(4) . 3_666 ?
O1 Dy1 Ti2 92.38(4) . 3_666 ?
O8 Dy1 Ti2 33.06(4) 3_666 3_666 ?
O4 Dy1 Ti2 141.49(4) . 3_666 ?
Cl1 Dy1 Ti2 125.045(19) . 3_666 ?
Ti2 Dy1 Ti2 112.145(9) . 3_666 ?
Ti1 Dy1 Ti2 103.532(11) . 3_666 ?
O10 Dy1 Dy1 36.96(4) 3_666 3_666 ?
O10 Dy1 Dy1 36.87(4) . 3_666 ?
O9 Dy1 Dy1 108.14(4) . 3_666 ?
O3 Dy1 Dy1 69.53(4) . 3_666 ?
O1 Dy1 Dy1 91.01(4) . 3_666 ?
O8 Dy1 Dy1 85.11(4) 3_666 3_666 ?
O4 Dy1 Dy1 92.93(4) . 3_666 ?
Cl1 Dy1 Dy1 173.729(15) . 3_666 ?
Ti2 Dy1 Dy1 58.068(8) . 3_666 ?
Ti1 Dy1 Dy1 71.855(8) . 3_666 ?
Ti2 Dy1 Dy1 54.076(8) 3_666 3_666 ?
O7 Ti2 O8 102.87(8) . . ?
O7 Ti2 O3 101.06(8) . . ?
O8 Ti2 O3 97.26(7) . . ?
O7 Ti2 O10 169.88(7) . . ?
O8 Ti2 O10 82.95(7) . . ?
O3 Ti2 O10 86.23(7) . . ?
O7 Ti2 O2 93.21(8) . . ?
O8 Ti2 O2 100.00(7) . . ?
O3 Ti2 O2 154.53(8) . . ?
O10 Ti2 O2 77.51(7) . . ?
O7 Ti2 O4 102.73(7) . . ?
O8 Ti2 O4 154.34(7) . . ?
O3 Ti2 O4 79.45(7) . . ?
O10 Ti2 O4 71.47(6) . . ?
O2 Ti2 O4 76.87(7) . . ?
O7 Ti2 Ti1 127.44(6) . . ?
O8 Ti2 Ti1 112.93(5) . . ?
O3 Ti2 Ti1 110.70(5) . . ?
O10 Ti2 Ti1 42.57(5) . . ?
O2 Ti2 Ti1 44.88(5) . . ?
O4 Ti2 Ti1 47.46(4) . . ?
O7 Ti2 Dy1 137.25(6) . . ?
O8 Ti2 Dy1 108.45(6) . . ?
O3 Ti2 Dy1 47.34(5) . . ?
O10 Ti2 Dy1 45.27(4) . . ?
O2 Ti2 Dy1 108.83(5) . . ?
O4 Ti2 Dy1 51.08(5) . . ?
Ti1 Ti2 Dy1 63.959(12) . . ?
O7 Ti2 Dy1 146.04(6) . 3_666 ?
O8 Ti2 Dy1 43.70(5) . 3_666 ?
O3 Ti2 Dy1 81.64(5) . 3_666 ?
O10 Ti2 Dy1 41.45(4) . 3_666 ?
O2 Ti2 Dy1 98.18(5) . 3_666 ?
O4 Ti2 Dy1 110.97(5) . 3_666 ?
Ti1 Ti2 Dy1 80.951(13) . 3_666 ?
Dy1 Ti2 Dy1 67.856(9) . 3_666 ?
O5 Ti1 O6 98.68(8) . . ?
O5 Ti1 O1 99.27(8) . . ?
O6 Ti1 O1 104.17(8) . . ?
O5 Ti1 O10 164.25(8) . . ?
O6 Ti1 O10 96.12(7) . . ?
O1 Ti1 O10 82.18(7) . . ?
O5 Ti1 O2 96.61(8) . . ?
O6 Ti1 O2 94.24(8) . . ?
O1 Ti1 O2 153.45(7) . . ?
O10 Ti1 O2 76.91(7) . . ?
O5 Ti1 O4 93.63(7) . . ?
O6 Ti1 O4 164.52(7) . . ?
O1 Ti1 O4 82.90(7) . . ?
O10 Ti1 O4 70.90(6) . . ?
O2 Ti1 O4 74.96(7) . . ?
O5 Ti1 Ti2 123.31(7) . . ?
O6 Ti1 Ti2 118.46(6) . . ?
O1 Ti1 Ti2 109.92(5) . . ?
O10 Ti1 Ti2 43.10(5) . . ?
O2 Ti1 Ti2 43.65(5) . . ?
O4 Ti1 Ti2 46.19(4) . . ?
O5 Ti1 Dy1 127.00(6) . . ?
O6 Ti1 Dy1 125.36(5) . . ?
O1 Ti1 Dy1 46.94(5) . . ?
O10 Ti1 Dy1 44.56(5) . . ?
O2 Ti1 Dy1 106.65(5) . . ?
O4 Ti1 Dy1 50.50(5) . . ?
Ti2 Ti1 Dy1 63.014(12) . . ?
O1 C11 C12 111.7(2) . . ?
O1 C11 H11A 109.3 . . ?
C12 C11 H11A 109.3 . . ?
O1 C11 H11B 109.3 . . ?
C12 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O2 C21 C22 118.7(6) . . ?
O2 C21 H21A 107.6 . . ?
C22 C21 H21A 107.6 . . ?
O2 C21 H21B 107.6 . . ?
C22 C21 H21B 107.6 . . ?
H21A C21 H21B 107.1 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O2 C21A C22A 116.6(3) . . ?
O2 C21A H21C 108.1 . . ?
C22A C21A H21C 108.1 . . ?
O2 C21A H21D 108.1 . . ?
C22A C21A H21D 108.1 . . ?
H21C C21A H21D 107.3 . . ?
C21A C22A H22D 109.5 . . ?
C21A C22A H22E 109.5 . . ?
H22D C22A H22E 109.5 . . ?
C21A C22A H22F 109.5 . . ?
H22D C22A H22F 109.5 . . ?
H22E C22A H22F 109.5 . . ?
O3 C31 C32 111.7(2) . . ?
O3 C31 H31A 109.3 . . ?
C32 C31 H31A 109.3 . . ?
O3 C31 H31B 109.3 . . ?
C32 C31 H31B 109.3 . . ?
H31A C31 H31B 107.9 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O4 C41 C42 112.3(2) . . ?
O4 C41 H41A 109.1 . . ?
C42 C41 H41A 109.1 . . ?
O4 C41 H41B 109.1 . . ?
C42 C41 H41B 109.1 . . ?
H41A C41 H41B 107.9 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O5 C51 C52 112.0(3) . . ?
O5 C51 H51A 109.2 . . ?
C52 C51 H51A 109.2 . . ?
O5 C51 H51B 109.2 . . ?
C52 C51 H51B 109.2 . . ?
H51A C51 H51B 107.9 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
O6 C61 C62 111.7(2) . . ?
O6 C61 H61A 109.3 . . ?
C62 C61 H61A 109.3 . . ?
O6 C61 H61B 109.3 . . ?
C62 C61 H61B 109.3 . . ?
H61A C61 H61B 107.9 . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
O7 C71 C72 112.5(3) . . ?
O7 C71 H71A 109.1 . . ?
C72 C71 H71A 109.1 . . ?
O7 C71 H71B 109.1 . . ?
C72 C71 H71B 109.1 . . ?
H71A C71 H71B 107.8 . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
O8 C81 C82 112.3(3) . . ?
O8 C81 H81A 109.1 . . ?
C82 C81 H81A 109.1 . . ?
O8 C81 H81B 109.1 . . ?
C82 C81 H81B 109.1 . . ?
H81A C81 H81B 107.9 . . ?
C81 C82 H82A 109.5 . . ?
C81 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
C81 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
O9 C91 C92 110.9(4) . . ?
O9 C91 H91A 109.5 . . ?
C92 C91 H91A 109.5 . . ?
O9 C91 H91B 109.5 . . ?
C92 C91 H91B 109.5 . . ?
H91A C91 H91B 108.1 . . ?
C91 C92 H92A 109.5 . . ?
C91 C92 H92B 109.5 . . ?
H92A C92 H92B 109.5 . . ?
C91 C92 H92C 109.5 . . ?
H92A C92 H92C 109.5 . . ?
H92B C92 H92C 109.5 . . ?
O9 C91A C92A 111.6(9) . . ?
O9 C91A H91C 109.3 . . ?
C92A C91A H91C 109.3 . . ?
O9 C91A H91D 109.3 . . ?
C92A C91A H91D 109.3 . . ?
H91C C91A H91D 108.0 . . ?
C91A C92A H92D 109.5 . . ?
C91A C92A H92E 109.5 . . ?
H92D C92A H92E 109.5 . . ?
C91A C92A H92F 109.5 . . ?
H92D C92A H92F 109.5 . . ?
H92E C92A H92F 109.5 . . ?
C11 O1 Ti1 124.87(16) . . ?
C11 O1 Dy1 126.52(14) . . ?
Ti1 O1 Dy1 97.40(7) . . ?
C21 O2 Ti2 128.9(3) . . ?
C21A O2 Ti2 128.7(2) . . ?
C21 O2 Ti1 133.0(4) . . ?
C21A O2 Ti1 129.6(2) . . ?
Ti2 O2 Ti1 91.48(7) . . ?
C31 O3 Ti2 123.15(16) . . ?
C31 O3 Dy1 138.21(15) . . ?
Ti2 O3 Dy1 96.99(6) . . ?
C41 O4 Ti2 127.69(16) . . ?
C41 O4 Ti1 121.02(14) . . ?
Ti2 O4 Ti1 86.35(6) . . ?
C41 O4 Dy1 131.17(15) . . ?
Ti2 O4 Dy1 88.52(6) . . ?
Ti1 O4 Dy1 88.49(6) . . ?
C51 O5 Ti1 165.6(2) . . ?
C61 O6 Ti1 133.33(16) . . ?
C71 O7 Ti2 159.0(2) . . ?
C81 O8 Ti2 127.35(17) . . ?
C81 O8 Dy1 127.17(16) . 3_666 ?
Ti2 O8 Dy1 103.24(7) . 3_666 ?
C91 O9 Dy1 136.59(18) . . ?
C91A O9 Dy1 126.6(6) . . ?
C91 O9 H9 128.7 . . ?
C91A O9 H9 119.5 . . ?
Dy1 O9 H9 92.2 . . ?
Ti1 O10 Ti2 94.33(7) . . ?
Ti1 O10 Dy1 146.64(8) . 3_666 ?
Ti2 O10 Dy1 103.86(7) . 3_666 ?
Ti1 O10 Dy1 98.85(6) . . ?
Ti2 O10 Dy1 97.18(6) . . ?
Dy1 O10 Dy1 106.17(6) 3_666 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C12 C11 O1 Ti1 72.0(3) . . . . ?
C12 C11 O1 Dy1 -152.6(2) . . . . ?
C22 C21 O2 Ti2 -157.9(4) . . . . ?
C22 C21 O2 Ti1 59.2(10) . . . . ?
C22A C21A O2 Ti2 158.3(3) . . . . ?
C22A C21A O2 Ti1 -66.9(5) . . . . ?
C32 C31 O3 Ti2 103.7(3) . . . . ?
C32 C31 O3 Dy1 -94.7(3) . . . . ?
C42 C41 O4 Ti2 -68.7(3) . . . . ?
C42 C41 O4 Ti1 179.54(18) . . . . ?
C42 C41 O4 Dy1 60.5(3) . . . . ?
C52 C51 O5 Ti1 165.2(7) . . . . ?
O6 Ti1 O5 C51 -150.7(9) . . . . ?
O1 Ti1 O5 C51 103.3(9) . . . . ?
O10 Ti1 O5 C51 9.2(11) . . . . ?
O2 Ti1 O5 C51 -55.4(9) . . . . ?
O4 Ti1 O5 C51 19.9(9) . . . . ?
Ti2 Ti1 O5 C51 -18.1(9) . . . . ?
Dy1 Ti1 O5 C51 61.3(9) . . . . ?
C62 C61 O6 Ti1 -132.3(2) . . . . ?
O5 Ti1 O6 C61 5.3(3) . . . . ?
O1 Ti1 O6 C61 107.3(2) . . . . ?
O10 Ti1 O6 C61 -169.3(2) . . . . ?
O2 Ti1 O6 C61 -92.0(2) . . . . ?
O4 Ti1 O6 C61 -137.0(3) . . . . ?
Ti2 Ti1 O6 C61 -130.3(2) . . . . ?
Dy1 Ti1 O6 C61 154.1(2) . . . . ?
C72 C71 O7 Ti2 -125.8(5) . . . . ?
O8 Ti2 O7 C71 139.2(5) . . . . ?
O3 Ti2 O7 C71 -120.7(5) . . . . ?
O10 Ti2 O7 C71 14.9(8) . . . . ?
O2 Ti2 O7 C71 38.1(6) . . . . ?
O4 Ti2 O7 C71 -39.1(6) . . . . ?
Ti1 Ti2 O7 C71 6.5(6) . . . . ?
Dy1 Ti2 O7 C71 -84.3(6) . . . . ?
Dy1 Ti2 O7 C71 147.9(5) 3_666 . . . ?
C82 C81 O8 Ti2 80.2(3) . . . . ?
C82 C81 O8 Dy1 -119.7(2) . . . 3_666 ?
C92 C91 O9 Dy1 108.2(4) . . . . ?
C92A C91A O9 Dy1 -124.8(16) . . . . ?

####################################################################### 
# 
# 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_Ti4Ho2
_database_code_depnum_ccdc_archive 'CCDC 2283717'
loop_
_audit_author_name
_audit_author_address
'Andrew Bond'
;University of Cambridge
United Kingdom
;
_audit_update_record             
;
2023-07-22 deposited with the CCDC.	2023-09-15 downloaded from the CCDC.
;
#===============================================================================
_audit_creation_method           SHELXL-2019/1

#-------------------------------------------------------------------------------
# Inserted by local software: cifUpdate ver. 3.1  (Andrew D. Bond, March 2019)
#-------------------------------------------------------------------------------
_cambridge_user_name             'Rosa Mueller'
_cambridge_user_crsid            rm2055
_cambridge_supervisor_name       'Dominic Wright'
_cambridge_supervisor_crsid      dsw1000
_cambridge_crystallographer_name 'Andrew Bond'
_cambridge_crystallographer_crsid adb29
_cambridge_sample_id             RM93D
_cambridge_data_id               DW_B1_0431
#-------------------------------------------------------------------------------

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H92 Cl2 Ho2 O20 Ti4'
_chemical_formula_sum            'C36 H92 Cl2 Ho2 O20 Ti4'
_chemical_formula_weight         1437.45

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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   11.9118(4)
_cell_length_b                   18.7283(6)
_cell_length_c                   12.7532(4)
_cell_angle_alpha                90
_cell_angle_beta                 92.6111(12)
_cell_angle_gamma                90
_cell_volume                     2842.13(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9866
_cell_measurement_theta_min      5.50
_cell_measurement_theta_max      66.64

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_F_000             1448
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    10.897
_shelx_estimated_absorpt_T_min   0.409
_shelx_estimated_absorpt_T_max   0.476
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5379
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Incoatec I\mS Cu microsource'
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-III'
_diffrn_measurement_method       'ω and φ-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31868
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         4.722
_diffrn_reflns_theta_max         66.598
_diffrn_reflns_theta_full        66.598
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             4981
_reflns_number_gt                4839
_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.

#===============================================================================
INTENSITY STATISTICS FOR DATASET # 1  DW_B1_0431_0m.hkl
#===============================================================================
 Resolution   #Data #Theory %Complete Redundancy Mean I Mean I/s Rmerge  Rsigma
#-------------------------------------------------------------------------------
  Inf - 3.43      78     88     88.6     1.78     87.30   26.69  0.0340  0.0317
 3.43 - 2.30     182    185     98.4     3.11    117.41   33.51  0.0252  0.0338
 2.30 - 1.82     259    263     98.5     3.46     94.41   33.64  0.0329  0.0306
 1.82 - 1.58     267    271     98.5     5.72     74.76   43.72  0.0328  0.0248
 1.58 - 1.44     249    252     98.8     8.37     62.17   55.87  0.0278  0.0157
 1.44 - 1.33     269    271     99.3     9.16     45.84   55.36  0.0290  0.0139
 1.33 - 1.25     276    277     99.6     8.53     41.95   45.71  0.0294  0.0148
 1.25 - 1.19     246    246    100.0     8.70     38.32   48.78  0.0273  0.0150
 1.19 - 1.14     262    262    100.0     8.58     29.14   44.35  0.0313  0.0157
 1.14 - 1.09     290    290    100.0     7.97     34.75   44.24  0.0309  0.0164
 1.09 - 1.05     283    285     99.3     6.82     30.15   38.29  0.0362  0.0193
 1.05 - 1.02     241    241    100.0     7.84     28.07   42.59  0.0353  0.0169
 1.02 - 0.99     255    255    100.0     7.24     24.81   38.63  0.0347  0.0175
 0.99 - 0.97     216    217     99.5     6.22     24.12   37.84  0.0292  0.0185
 0.97 - 0.94     331    331    100.0     5.64     17.67   33.63  0.0339  0.0207
 0.94 - 0.92     233    233    100.0     5.57     18.71   33.30  0.0329  0.0200
 0.92 - 0.90     265    266     99.6     4.84     16.65   29.67  0.0360  0.0224
 0.90 - 0.88     308    308    100.0     5.04     15.14   32.23  0.0347  0.0220
 0.88 - 0.87     158    158    100.0     4.57     12.37   29.78  0.0336  0.0234
 0.87 - 0.85     301    301    100.0     4.16     14.13   29.57  0.0380  0.0236
 0.85 - 0.84     199    203     98.0     3.13     11.87   23.81  0.0392  0.0281
#-------------------------------------------------------------------------------
 0.94 - 0.84    1464   1469     99.7     4.59     15.03   29.98  0.0353  0.0228
  Inf - 0.84    5168   5203     99.3     6.25     37.50   38.81  0.0313  0.0222
#===============================================================================
;

_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL

_refine_special_details          ?

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0182P)²+2.5003P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4981
_refine_ls_number_parameters     329
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_gt           0.0206
_refine_ls_wR_factor_ref         0.0505
_refine_ls_wR_factor_gt          0.0502
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.127
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.066

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 0.38243(2) 0.54106(2) 0.42056(2) 0.01365(6) Uani 1 1 d . . . . .
Ti2 Ti 0.39135(3) 0.54405(2) 0.67572(2) 0.01384(8) Uani 1 1 d . . . . .
Ti1 Ti 0.49529(3) 0.66492(2) 0.57302(2) 0.01420(8) Uani 1 1 d . . . . .
Cl1 Cl 0.22949(4) 0.61163(3) 0.30682(4) 0.02795(11) Uani 1 1 d . . . . .
C11 C 0.45666(19) 0.71246(11) 0.35054(16) 0.0265(4) Uani 1 1 d . . . . .
H11A H 0.394478 0.742242 0.375240 0.032 Uiso 1 1 calc R U . . .
H11B H 0.433155 0.693015 0.280771 0.032 Uiso 1 1 calc R U . . .
C12 C 0.5595(2) 0.75818(13) 0.3404(2) 0.0412(6) Uani 1 1 d . . . . .
H12A H 0.579131 0.780793 0.408097 0.062 Uiso 1 1 calc R U . . .
H12B H 0.544033 0.795135 0.287313 0.062 Uiso 1 1 calc R U . . .
H12C H 0.622191 0.728394 0.319314 0.062 Uiso 1 1 calc R U . . .
C21 C 0.5261(6) 0.6479(3) 0.8175(4) 0.028(2) Uani 0.330(8) 1 d D U P A 1
H21A H 0.602104 0.627046 0.813296 0.034 Uiso 0.330(8) 1 calc R U P A 1
H21B H 0.488019 0.621524 0.872966 0.034 Uiso 0.330(8) 1 calc R U P A 1
C22 C 0.5402(3) 0.72209(16) 0.8535(2) 0.0568(8) Uani 0.330(8) 1 d D U P A 1
H22A H 0.587140 0.748081 0.805182 0.085 Uiso 0.330(8) 1 calc R U P A 1
H22B H 0.576395 0.722504 0.924036 0.085 Uiso 0.330(8) 1 calc R U P A 1
H22C H 0.466433 0.745137 0.855210 0.085 Uiso 0.330(8) 1 calc R U P A 1
C21A C 0.4487(3) 0.67683(18) 0.8147(2) 0.0275(10) Uani 0.670(8) 1 d D U P A 2
H21C H 0.427869 0.644754 0.872340 0.033 Uiso 0.670(8) 1 calc R U P A 2
H21D H 0.382952 0.707593 0.797150 0.033 Uiso 0.670(8) 1 calc R U P A 2
C22A C 0.5402(3) 0.72209(16) 0.8535(2) 0.0568(8) Uani 0.670(8) 1 d D U P A 2
H22D H 0.605728 0.692506 0.872929 0.085 Uiso 0.670(8) 1 calc R U P A 2
H22E H 0.516905 0.748491 0.915179 0.085 Uiso 0.670(8) 1 calc R U P A 2
H22F H 0.559766 0.755888 0.798559 0.085 Uiso 0.670(8) 1 calc R U P A 2
C31 C 0.25777(17) 0.41993(11) 0.60091(16) 0.0234(4) Uani 1 1 d . . . . .
H31A H 0.286511 0.403994 0.671122 0.028 Uiso 1 1 calc R U . . .
H31B H 0.275768 0.382423 0.549612 0.028 Uiso 1 1 calc R U . . .
C32 C 0.1328(2) 0.42881(15) 0.6018(2) 0.0464(7) Uani 1 1 d . . . . .
H32A H 0.114342 0.462972 0.656655 0.070 Uiso 1 1 calc R U . . .
H32B H 0.097903 0.382636 0.616042 0.070 Uiso 1 1 calc R U . . .
H32C H 0.104421 0.446643 0.533408 0.070 Uiso 1 1 calc R U . . .
C41 C 0.23200(16) 0.66702(11) 0.57906(17) 0.0235(4) Uani 1 1 d . . . . .
H41A H 0.230296 0.703054 0.522212 0.028 Uiso 1 1 calc R U . . .
H41B H 0.239626 0.692708 0.646862 0.028 Uiso 1 1 calc R U . . .
C42 C 0.12283(17) 0.62613(13) 0.57421(18) 0.0321(5) Uani 1 1 d . . . . .
H42A H 0.115369 0.599977 0.507700 0.048 Uiso 1 1 calc R U . . .
H42B H 0.059943 0.659534 0.578978 0.048 Uiso 1 1 calc R U . . .
H42C H 0.122226 0.592294 0.632804 0.048 Uiso 1 1 calc R U . . .
C51 C 0.3867(2) 0.81761(13) 0.6049(3) 0.0484(7) Uani 1 1 d . . . . .
H51A H 0.349757 0.812851 0.672559 0.058 Uiso 1 1 calc R U . . .
H51B H 0.327188 0.823444 0.548816 0.058 Uiso 1 1 calc R U . . .
C52 C 0.4594(3) 0.88190(14) 0.6083(3) 0.0637(9) Uani 1 1 d . . . . .
H52A H 0.517405 0.876756 0.664818 0.096 Uiso 1 1 calc R U . . .
H52B H 0.413659 0.924204 0.621402 0.096 Uiso 1 1 calc R U . . .
H52C H 0.495115 0.887222 0.541079 0.096 Uiso 1 1 calc R U . . .
C61 C 0.71378(18) 0.74100(11) 0.62748(17) 0.0278(5) Uani 1 1 d . . . . .
H61A H 0.741128 0.735732 0.701544 0.033 Uiso 1 1 calc R U . . .
H61B H 0.665855 0.784161 0.622302 0.033 Uiso 1 1 calc R U . . .
C62 C 0.8125(2) 0.75024(13) 0.5593(2) 0.0369(5) Uani 1 1 d . . . . .
H62A H 0.861078 0.708068 0.565619 0.055 Uiso 1 1 calc R U . . .
H62B H 0.855251 0.792708 0.581723 0.055 Uiso 1 1 calc R U . . .
H62C H 0.785599 0.755951 0.485974 0.055 Uiso 1 1 calc R U . . .
C71 C 0.2189(2) 0.57477(16) 0.84922(19) 0.0449(6) Uani 1 1 d . . . . .
H71A H 0.141732 0.558631 0.829386 0.054 Uiso 1 1 calc R U . . .
H71B H 0.220200 0.627529 0.844644 0.054 Uiso 1 1 calc R U . . .
C72 C 0.2475(3) 0.55286(17) 0.9599(2) 0.0504(7) Uani 1 1 d . . . . .
H72A H 0.241196 0.500868 0.966022 0.076 Uiso 1 1 calc R U . . .
H72B H 0.195445 0.575769 1.006802 0.076 Uiso 1 1 calc R U . . .
H72C H 0.324593 0.567569 0.979423 0.076 Uiso 1 1 calc R U . . .
C81 C 0.5217(2) 0.45309(13) 0.83224(16) 0.0309(5) Uani 1 1 d . . . . .
H81A H 0.522394 0.495959 0.877687 0.037 Uiso 1 1 calc R U . . .
H81B H 0.597335 0.431136 0.838511 0.037 Uiso 1 1 calc R U . . .
C82 C 0.4365(2) 0.40072(15) 0.8702(2) 0.0465(7) Uani 1 1 d . . . . .
H82A H 0.361522 0.422330 0.864693 0.070 Uiso 1 1 calc R U . . .
H82B H 0.455238 0.388296 0.943530 0.070 Uiso 1 1 calc R U . . .
H82C H 0.437280 0.357477 0.826932 0.070 Uiso 1 1 calc R U . . .
C91 C 0.1569(2) 0.44052(16) 0.3020(2) 0.0325(9) Uani 0.812(7) 1 d D U P B 1
H91A H 0.113486 0.484092 0.317336 0.039 Uiso 0.812(7) 1 calc R U P B 1
H91B H 0.119576 0.399404 0.334659 0.039 Uiso 0.812(7) 1 calc R U P B 1
C92 C 0.1576(5) 0.4297(3) 0.1859(3) 0.0742(16) Uani 0.812(7) 1 d D U P B 1
H92A H 0.190477 0.471660 0.153149 0.111 Uiso 0.812(7) 1 calc R U P B 1
H92B H 0.080413 0.422956 0.157652 0.111 Uiso 0.812(7) 1 calc R U P B 1
H92C H 0.202371 0.387338 0.170677 0.111 Uiso 0.812(7) 1 calc R U P B 1
C91A C 0.2315(9) 0.4410(6) 0.2352(6) 0.029(4) Uani 0.188(7) 1 d D U P B 2
H91C H 0.267881 0.399106 0.203830 0.035 Uiso 0.188(7) 1 calc R U P B 2
H91D H 0.254095 0.484120 0.196557 0.035 Uiso 0.188(7) 1 calc R U P B 2
C92A C 0.1032(11) 0.4324(12) 0.2249(14) 0.060(6) Uani 0.188(7) 1 d D U P B 2
H92D H 0.082288 0.385031 0.250059 0.091 Uiso 0.188(7) 1 calc R U P B 2
H92E H 0.077903 0.437655 0.151093 0.091 Uiso 0.188(7) 1 calc R U P B 2
H92F H 0.067593 0.469131 0.266919 0.091 Uiso 0.188(7) 1 calc R U P B 2
O1 O 0.47712(11) 0.65485(7) 0.42221(10) 0.0181(3) Uani 1 1 d . . . . .
O2 O 0.46953(12) 0.63411(7) 0.72546(10) 0.0224(3) Uani 1 1 d D . . . .
O3 O 0.31286(11) 0.48480(7) 0.57407(10) 0.0179(3) Uani 1 1 d . . . . .
O4 O 0.32748(10) 0.62165(7) 0.56874(10) 0.0168(3) Uani 1 1 d . . . . .
O5 O 0.44838(12) 0.75496(7) 0.58602(12) 0.0263(3) Uani 1 1 d . . . . .
O6 O 0.64864(11) 0.68000(7) 0.59705(10) 0.0198(3) Uani 1 1 d . . . . .
O7 O 0.29324(11) 0.54658(7) 0.77800(10) 0.0206(3) Uani 1 1 d . . . . .
O8 O 0.49858(11) 0.47427(7) 0.72572(10) 0.0182(3) Uani 1 1 d . . . . .
O9 O 0.26918(12) 0.44746(7) 0.34622(11) 0.0245(3) Uani 1 1 d D . . . .
H9 H 0.312971 0.414652 0.374725 0.037 Uiso 1 1 d R U . B .
O10 O 0.50389(10) 0.55932(6) 0.56581(9) 0.0126(2) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho1 O10 2.3187(12) 3_666 ?
Ho1 O10 2.3233(12) . ?
Ho1 O9 2.3822(13) . ?
Ho1 O3 2.4037(12) . ?
Ho1 O1 2.4109(13) . ?
Ho1 O8 2.4109(13) 3_666 ?
Ho1 O4 2.5279(12) . ?
Ho1 Cl1 2.6324(5) . ?
Ho1 Ti2 3.2515(3) . ?
Ho1 Ti1 3.2758(3) . ?
Ho1 Ti2 3.4075(3) 3_666 ?
Ho1 Ho1 3.7147(3) 3_666 ?
Ti2 O7 1.7912(13) . ?
Ti2 O8 1.9162(13) . ?
Ti2 O3 1.9173(13) . ?
Ti2 O10 2.0037(12) . ?
Ti2 O2 2.0150(13) . ?
Ti2 O4 2.1113(13) . ?
Ti2 Ti1 2.9189(4) . ?
Ti1 O5 1.7866(14) . ?
Ti1 O6 1.8600(13) . ?
Ti1 O1 1.9348(13) . ?
Ti1 O10 1.9827(12) . ?
Ti1 O2 2.0643(13) . ?
Ti1 O4 2.1554(13) . ?
C11 O1 1.428(2) . ?
C11 C12 1.505(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C21 O2 1.351(5) . ?
C21 C22 1.470(6) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C21A O2 1.422(3) . ?
C21A C22A 1.449(4) . ?
C21A H21C 0.9900 . ?
C21A H21D 0.9900 . ?
C22A H22D 0.9800 . ?
C22A H22E 0.9800 . ?
C22A H22F 0.9800 . ?
C31 O3 1.430(2) . ?
C31 C32 1.498(3) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C41 O4 1.431(2) . ?
C41 C42 1.508(3) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C51 O5 1.411(3) . ?
C51 C52 1.482(4) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C61 O6 1.425(2) . ?
C61 C62 1.505(3) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C71 O7 1.400(3) . ?
C71 C72 1.494(4) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C81 O8 1.430(2) . ?
C81 C82 1.507(4) . ?
C81 H81A 0.9900 . ?
C81 H81B 0.9900 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C91 O9 1.434(3) . ?
C91 C92 1.496(5) . ?
C91 H91A 0.9900 . ?
C91 H91B 0.9900 . ?
C92 H92A 0.9800 . ?
C92 H92B 0.9800 . ?
C92 H92C 0.9800 . ?
C91A O9 1.470(8) . ?
C91A C92A 1.536(9) . ?
C91A H91C 0.9900 . ?
C91A H91D 0.9900 . ?
C92A H92D 0.9800 . ?
C92A H92E 0.9800 . ?
C92A H92F 0.9800 . ?
O9 H9 0.8744 . ?

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
O10 Ho1 O10 73.69(5) 3_666 . ?
O10 Ho1 O9 75.61(4) 3_666 . ?
O10 Ho1 O9 138.28(4) . . ?
O10 Ho1 O3 78.78(4) 3_666 . ?
O10 Ho1 O3 68.92(4) . . ?
O9 Ho1 O3 77.97(5) . . ?
O10 Ho1 O1 116.40(4) 3_666 . ?
O10 Ho1 O1 65.72(4) . . ?
O9 Ho1 O1 155.53(5) . . ?
O3 Ho1 O1 123.98(4) . . ?
O10 Ho1 O8 66.39(4) 3_666 3_666 ?
O10 Ho1 O8 105.53(4) . 3_666 ?
O9 Ho1 O8 86.94(5) . 3_666 ?
O3 Ho1 O8 144.56(4) . 3_666 ?
O1 Ho1 O8 79.67(4) . 3_666 ?
O10 Ho1 O4 126.74(4) 3_666 . ?
O10 Ho1 O4 59.28(4) . . ?
O9 Ho1 O4 125.14(5) . . ?
O3 Ho1 O4 62.76(4) . . ?
O1 Ho1 O4 66.59(4) . . ?
O8 Ho1 O4 146.20(4) 3_666 . ?
O10 Ho1 Cl1 146.67(3) 3_666 . ?
O10 Ho1 Cl1 139.09(3) . . ?
O9 Ho1 Cl1 77.58(3) . . ?
O3 Ho1 Cl1 114.41(3) . . ?
O1 Ho1 Cl1 82.69(3) . . ?
O8 Ho1 Cl1 92.86(3) 3_666 . ?
O4 Ho1 Cl1 85.18(3) . . ?
O10 Ho1 Ti2 86.94(3) 3_666 . ?
O10 Ho1 Ti2 37.69(3) . . ?
O9 Ho1 Ti2 113.77(4) . . ?
O3 Ho1 Ti2 35.82(3) . . ?
O1 Ho1 Ti2 88.97(3) . . ?
O8 Ho1 Ti2 141.53(3) 3_666 . ?
O4 Ho1 Ti2 40.47(3) . . ?
Cl1 Ho1 Ti2 122.214(14) . . ?
O10 Ho1 Ti1 107.89(3) 3_666 . ?
O10 Ho1 Ti1 36.74(3) . . ?
O9 Ho1 Ti1 165.23(4) . . ?
O3 Ho1 Ti1 88.53(3) . . ?
O1 Ho1 Ti1 35.87(3) . . ?
O8 Ho1 Ti1 107.69(3) 3_666 . ?
O4 Ho1 Ti1 41.13(3) . . ?
Cl1 Ho1 Ti1 103.095(13) . . ?
Ti2 Ho1 Ti1 53.125(8) . . ?
O10 Ho1 Ti2 34.82(3) 3_666 3_666 ?
O10 Ho1 Ti2 83.23(3) . 3_666 ?
O9 Ho1 Ti2 87.43(4) . 3_666 ?
O3 Ho1 Ti2 113.33(3) . 3_666 ?
O1 Ho1 Ti2 92.25(3) . 3_666 ?
O8 Ho1 Ti2 33.18(3) 3_666 3_666 ?
O4 Ho1 Ti2 141.69(3) . 3_666 ?
Cl1 Ho1 Ti2 125.108(14) . 3_666 ?
Ti2 Ho1 Ti2 112.233(7) . 3_666 ?
Ti1 Ho1 Ti2 103.605(9) . 3_666 ?
O10 Ho1 Ho1 36.89(3) 3_666 3_666 ?
O10 Ho1 Ho1 36.81(3) . 3_666 ?
O9 Ho1 Ho1 108.16(3) . 3_666 ?
O3 Ho1 Ho1 69.73(3) . 3_666 ?
O1 Ho1 Ho1 91.17(3) . 3_666 ?
O8 Ho1 Ho1 85.27(3) 3_666 3_666 ?
O4 Ho1 Ho1 93.09(3) . 3_666 ?
Cl1 Ho1 Ho1 173.812(13) . 3_666 ?
Ti2 Ho1 Ho1 58.116(7) . 3_666 ?
Ti1 Ho1 Ho1 71.974(7) . 3_666 ?
Ti2 Ho1 Ho1 54.117(7) 3_666 3_666 ?
O7 Ti2 O8 102.87(6) . . ?
O7 Ti2 O3 101.15(6) . . ?
O8 Ti2 O3 97.32(6) . . ?
O7 Ti2 O10 170.12(6) . . ?
O8 Ti2 O10 82.71(5) . . ?
O3 Ti2 O10 86.03(5) . . ?
O7 Ti2 O2 93.22(6) . . ?
O8 Ti2 O2 100.06(6) . . ?
O3 Ti2 O2 154.36(6) . . ?
O10 Ti2 O2 77.67(5) . . ?
O7 Ti2 O4 102.98(6) . . ?
O8 Ti2 O4 154.11(5) . . ?
O3 Ti2 O4 79.12(5) . . ?
O10 Ti2 O4 71.50(5) . . ?
O2 Ti2 O4 77.01(5) . . ?
O7 Ti2 Ti1 127.62(4) . . ?
O8 Ti2 Ti1 112.85(4) . . ?
O3 Ti2 Ti1 110.44(4) . . ?
O10 Ti2 Ti1 42.65(4) . . ?
O2 Ti2 Ti1 44.99(4) . . ?
O4 Ti2 Ti1 47.47(4) . . ?
O7 Ti2 Ho1 137.44(5) . . ?
O8 Ti2 Ho1 108.19(4) . . ?
O3 Ti2 Ho1 47.20(4) . . ?
O10 Ti2 Ho1 45.15(3) . . ?
O2 Ti2 Ho1 108.85(4) . . ?
O4 Ti2 Ho1 51.00(3) . . ?
Ti1 Ti2 Ho1 63.863(9) . . ?
O7 Ti2 Ho1 145.86(5) . 3_666 ?
O8 Ti2 Ho1 43.51(4) . 3_666 ?
O3 Ti2 Ho1 81.65(4) . 3_666 ?
O10 Ti2 Ho1 41.36(3) . 3_666 ?
O2 Ti2 Ho1 98.24(4) . 3_666 ?
O4 Ti2 Ho1 110.90(4) . 3_666 ?
Ti1 Ti2 Ho1 80.939(10) . 3_666 ?
Ho1 Ti2 Ho1 67.766(7) . 3_666 ?
O5 Ti1 O6 98.65(6) . . ?
O5 Ti1 O1 99.38(6) . . ?
O6 Ti1 O1 104.07(6) . . ?
O5 Ti1 O10 164.33(6) . . ?
O6 Ti1 O10 96.12(5) . . ?
O1 Ti1 O10 81.98(5) . . ?
O5 Ti1 O2 96.66(6) . . ?
O6 Ti1 O2 94.26(6) . . ?
O1 Ti1 O2 153.42(5) . . ?
O10 Ti1 O2 77.00(5) . . ?
O5 Ti1 O4 93.65(6) . . ?
O6 Ti1 O4 164.58(6) . . ?
O1 Ti1 O4 82.91(5) . . ?
O10 Ti1 O4 70.95(5) . . ?
O2 Ti1 O4 75.01(5) . . ?
O5 Ti1 Ti2 123.33(5) . . ?
O6 Ti1 Ti2 118.51(4) . . ?
O1 Ti1 Ti2 109.88(4) . . ?
O10 Ti1 Ti2 43.21(4) . . ?
O2 Ti1 Ti2 43.64(4) . . ?
O4 Ti1 Ti2 46.21(3) . . ?
O5 Ti1 Ho1 127.00(5) . . ?
O6 Ti1 Ho1 125.36(4) . . ?
O1 Ti1 Ho1 46.90(4) . . ?
O10 Ti1 Ho1 44.51(3) . . ?
O2 Ti1 Ho1 106.65(4) . . ?
O4 Ti1 Ho1 50.48(3) . . ?
Ti2 Ti1 Ho1 63.012(9) . . ?
O1 C11 C12 111.65(18) . . ?
O1 C11 H11A 109.3 . . ?
C12 C11 H11A 109.3 . . ?
O1 C11 H11B 109.3 . . ?
C12 C11 H11B 109.3 . . ?
H11A C11 H11B 108.0 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O2 C21 C22 119.8(5) . . ?
O2 C21 H21A 107.4 . . ?
C22 C21 H21A 107.4 . . ?
O2 C21 H21B 107.4 . . ?
C22 C21 H21B 107.4 . . ?
H21A C21 H21B 106.9 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O2 C21A C22A 116.5(3) . . ?
O2 C21A H21C 108.2 . . ?
C22A C21A H21C 108.2 . . ?
O2 C21A H21D 108.2 . . ?
C22A C21A H21D 108.2 . . ?
H21C C21A H21D 107.3 . . ?
C21A C22A H22D 109.5 . . ?
C21A C22A H22E 109.5 . . ?
H22D C22A H22E 109.5 . . ?
C21A C22A H22F 109.5 . . ?
H22D C22A H22F 109.5 . . ?
H22E C22A H22F 109.5 . . ?
O3 C31 C32 111.99(18) . . ?
O3 C31 H31A 109.2 . . ?
C32 C31 H31A 109.2 . . ?
O3 C31 H31B 109.2 . . ?
C32 C31 H31B 109.2 . . ?
H31A C31 H31B 107.9 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O4 C41 C42 112.47(17) . . ?
O4 C41 H41A 109.1 . . ?
C42 C41 H41A 109.1 . . ?
O4 C41 H41B 109.1 . . ?
C42 C41 H41B 109.1 . . ?
H41A C41 H41B 107.8 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O5 C51 C52 111.9(2) . . ?
O5 C51 H51A 109.2 . . ?
C52 C51 H51A 109.2 . . ?
O5 C51 H51B 109.2 . . ?
C52 C51 H51B 109.2 . . ?
H51A C51 H51B 107.9 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
O6 C61 C62 111.41(17) . . ?
O6 C61 H61A 109.3 . . ?
C62 C61 H61A 109.3 . . ?
O6 C61 H61B 109.3 . . ?
C62 C61 H61B 109.3 . . ?
H61A C61 H61B 108.0 . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
O7 C71 C72 112.7(2) . . ?
O7 C71 H71A 109.1 . . ?
C72 C71 H71A 109.1 . . ?
O7 C71 H71B 109.1 . . ?
C72 C71 H71B 109.1 . . ?
H71A C71 H71B 107.8 . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
O8 C81 C82 112.4(2) . . ?
O8 C81 H81A 109.1 . . ?
C82 C81 H81A 109.1 . . ?
O8 C81 H81B 109.1 . . ?
C82 C81 H81B 109.1 . . ?
H81A C81 H81B 107.8 . . ?
C81 C82 H82A 109.5 . . ?
C81 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
C81 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
O9 C91 C92 110.7(3) . . ?
O9 C91 H91A 109.5 . . ?
C92 C91 H91A 109.5 . . ?
O9 C91 H91B 109.5 . . ?
C92 C91 H91B 109.5 . . ?
H91A C91 H91B 108.1 . . ?
C91 C92 H92A 109.5 . . ?
C91 C92 H92B 109.5 . . ?
H92A C92 H92B 109.5 . . ?
C91 C92 H92C 109.5 . . ?
H92A C92 H92C 109.5 . . ?
H92B C92 H92C 109.5 . . ?
O9 C91A C92A 110.5(8) . . ?
O9 C91A H91C 109.5 . . ?
C92A C91A H91C 109.5 . . ?
O9 C91A H91D 109.5 . . ?
C92A C91A H91D 109.5 . . ?
H91C C91A H91D 108.1 . . ?
C91A C92A H92D 109.5 . . ?
C91A C92A H92E 109.5 . . ?
H92D C92A H92E 109.5 . . ?
C91A C92A H92F 109.5 . . ?
H92D C92A H92F 109.5 . . ?
H92E C92A H92F 109.5 . . ?
C11 O1 Ti1 124.81(12) . . ?
C11 O1 Ho1 126.60(11) . . ?
Ti1 O1 Ho1 97.23(5) . . ?
C21 O2 Ti2 129.7(3) . . ?
C21A O2 Ti2 128.91(15) . . ?
C21 O2 Ti1 132.4(3) . . ?
C21A O2 Ti1 129.43(16) . . ?
Ti2 O2 Ti1 91.37(5) . . ?
C31 O3 Ti2 123.02(11) . . ?
C31 O3 Ho1 138.29(11) . . ?
Ti2 O3 Ho1 96.97(5) . . ?
C41 O4 Ti2 127.88(11) . . ?
C41 O4 Ti1 120.97(11) . . ?
Ti2 O4 Ti1 86.33(5) . . ?
C41 O4 Ho1 131.11(11) . . ?
Ti2 O4 Ho1 88.52(4) . . ?
Ti1 O4 Ho1 88.39(4) . . ?
C51 O5 Ti1 165.52(16) . . ?
C61 O6 Ti1 133.25(13) . . ?
C71 O7 Ti2 159.24(16) . . ?
C81 O8 Ti2 127.02(13) . . ?
C81 O8 Ho1 127.40(12) . 3_666 ?
Ti2 O8 Ho1 103.31(5) . 3_666 ?
C91 O9 Ho1 136.43(15) . . ?
C91A O9 Ho1 125.9(5) . . ?
C91 O9 H9 128.9 . . ?
C91A O9 H9 119.5 . . ?
Ho1 O9 H9 92.0 . . ?
Ti1 O10 Ti2 94.14(5) . . ?
Ti1 O10 Ho1 146.77(6) . 3_666 ?
Ti2 O10 Ho1 103.83(5) . 3_666 ?
Ti1 O10 Ho1 98.75(5) . . ?
Ti2 O10 Ho1 97.16(5) . . ?
Ho1 O10 Ho1 106.30(5) 3_666 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C12 C11 O1 Ti1 72.0(2) . . . . ?
C12 C11 O1 Ho1 -152.96(15) . . . . ?
C22 C21 O2 Ti2 -157.3(3) . . . . ?
C22 C21 O2 Ti1 59.4(8) . . . . ?
C22A C21A O2 Ti2 158.1(2) . . . . ?
C22A C21A O2 Ti1 -67.2(4) . . . . ?
C32 C31 O3 Ti2 103.41(19) . . . . ?
C32 C31 O3 Ho1 -95.4(2) . . . . ?
C42 C41 O4 Ti2 -68.0(2) . . . . ?
C42 C41 O4 Ti1 -179.87(13) . . . . ?
C42 C41 O4 Ho1 61.4(2) . . . . ?
C52 C51 O5 Ti1 165.0(6) . . . . ?
O6 Ti1 O5 C51 -150.6(7) . . . . ?
O1 Ti1 O5 C51 103.5(7) . . . . ?
O10 Ti1 O5 C51 9.8(8) . . . . ?
O2 Ti1 O5 C51 -55.2(7) . . . . ?
O4 Ti1 O5 C51 20.1(7) . . . . ?
Ti2 Ti1 O5 C51 -17.9(7) . . . . ?
Ho1 Ti1 O5 C51 61.5(7) . . . . ?
C62 C61 O6 Ti1 -132.70(17) . . . . ?
O5 Ti1 O6 C61 5.89(18) . . . . ?
O1 Ti1 O6 C61 107.89(17) . . . . ?
O10 Ti1 O6 C61 -168.87(17) . . . . ?
O2 Ti1 O6 C61 -91.52(17) . . . . ?
O4 Ti1 O6 C61 -136.6(2) . . . . ?
Ti2 Ti1 O6 C61 -129.76(16) . . . . ?
Ho1 Ti1 O6 C61 154.58(15) . . . . ?
C72 C71 O7 Ti2 -125.9(4) . . . . ?
O8 Ti2 O7 C71 139.9(4) . . . . ?
O3 Ti2 O7 C71 -119.8(4) . . . . ?
O2 Ti2 O7 C71 38.8(4) . . . . ?
O4 Ti2 O7 C71 -38.6(4) . . . . ?
Ti1 Ti2 O7 C71 7.2(5) . . . . ?
Ho1 Ti2 O7 C71 -83.8(4) . . . . ?
Ho1 Ti2 O7 C71 148.6(4) 3_666 . . . ?
C82 C81 O8 Ti2 80.0(2) . . . . ?
C82 C81 O8 Ho1 -120.01(18) . . . 3_666 ?
C92 C91 O9 Ho1 108.9(3) . . . . ?
C92A C91A O9 Ho1 -126.3(11) . . . . ?

####################################################################### 
# 
# 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_Ti4Yb2
_database_code_depnum_ccdc_archive 'CCDC 2283716'
loop_
_audit_author_name
_audit_author_address
'Andrew Bond'
;University of Cambridge
United Kingdom
;
_audit_update_record             
;
2023-07-22 deposited with the CCDC.	2023-09-15 downloaded from the CCDC.
;
#===============================================================================
_audit_creation_method           SHELXL-2018/3

#-------------------------------------------------------------------------------
# Inserted by local software: cifUpdate ver. 3.1  (Andrew D. Bond, March 2019)
#-------------------------------------------------------------------------------
_cambridge_user_name             'Victor Riesgo Gonzalez'
_cambridge_user_crsid            vrg25
_cambridge_supervisor_name       'Dominic wright'
_cambridge_supervisor_crsid      dsw1000
_cambridge_crystallographer_name 'Andrew Bond'
_cambridge_crystallographer_crsid adb29
_cambridge_sample_id             VR076
_cambridge_data_id               DW_B1_0396
#-------------------------------------------------------------------------------

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H92 Cl2 O20 Ti4 Yb2'
_chemical_formula_sum            'C36 H92 Cl2 O20 Ti4 Yb2'
_chemical_formula_weight         1453.67

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'
Yb Yb -7.2108 4.4329 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   11.9050(3)
_cell_length_b                   18.6786(5)
_cell_length_c                   12.7568(4)
_cell_angle_alpha                90
_cell_angle_beta                 92.6397(11)
_cell_angle_gamma                90
_cell_volume                     2833.70(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9830
_cell_measurement_theta_min      4.41
_cell_measurement_theta_max      66.71

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_F_000             1460
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    11.819
_shelx_estimated_absorpt_T_min   0.288
_shelx_estimated_absorpt_T_max   0.331
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5524
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Incoatec I\mS Cu microsource'
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-III'
_diffrn_measurement_method       'ω and φ-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            46776
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         4.200
_diffrn_reflns_theta_max         66.815
_diffrn_reflns_theta_full        66.815
_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             5020
_reflns_number_gt                4530
_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.

#===============================================================================
INTENSITY STATISTICS FOR DATASET # 1  DW_B1_0396_0m.hkl
#===============================================================================
 Resolution   #Data #Theory %Complete Redundancy Mean I Mean I/s Rmerge  Rsigma
#-------------------------------------------------------------------------------
  Inf - 3.56      78     78    100.0     3.90     93.36   27.39  0.0310  0.0293
 3.56 - 2.33     182    182    100.0     4.14    100.56   28.81  0.0326  0.0261
 2.33 - 1.83     264    264    100.0     5.47     71.36   30.07  0.0363  0.0246
 1.83 - 1.59     267    267    100.0     8.87     62.87   38.09  0.0391  0.0212
 1.59 - 1.44     264    264    100.0    13.09     48.25   43.30  0.0405  0.0163
 1.44 - 1.34     251    251    100.0    13.61     36.70   41.40  0.0431  0.0169
 1.34 - 1.26     257    257    100.0    12.63     33.10   33.79  0.0456  0.0185
 1.26 - 1.19     286    286    100.0    12.64     29.59   34.71  0.0476  0.0200
 1.19 - 1.14     258    258    100.0    12.07     23.09   30.70  0.0563  0.0217
 1.14 - 1.09     295    295    100.0    11.84     27.24   32.07  0.0542  0.0213
 1.09 - 1.06     199    199    100.0     9.54     23.26   25.77  0.0742  0.0279
 1.06 - 1.03     255    255    100.0    11.13     22.64   29.30  0.0671  0.0230
 1.03 - 0.99     319    319    100.0    10.10     20.24   26.68  0.0696  0.0246
 0.99 - 0.97     217    217    100.0     8.33     18.80   25.42  0.0512  0.0265
 0.97 - 0.94     325    325    100.0     8.16     14.50   23.77  0.0597  0.0294
 0.94 - 0.92     238    238    100.0     7.74     14.33   21.60  0.0609  0.0294
 0.92 - 0.90     268    268    100.0     7.11     13.30   20.28  0.0787  0.0328
 0.90 - 0.88     304    304    100.0     7.08     11.80   20.51  0.0711  0.0330
 0.88 - 0.87     154    154    100.0     6.91      9.59   19.01  0.0798  0.0349
 0.87 - 0.85     306    306    100.0     6.06     11.52   20.16  0.0751  0.0336
 0.85 - 0.84     215    219     98.2     5.37      8.60   15.40  0.0861  0.0415
#-------------------------------------------------------------------------------
 0.94 - 0.84    1485   1489     99.7     6.71     11.73   19.68  0.0729  0.0334
  Inf - 0.84    5202   5206     99.9     9.15     30.22   28.23  0.0495  0.0239
#===============================================================================
;

_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL

_refine_special_details          ?

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0168P)²+6.3564P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5020
_refine_ls_number_parameters     338
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0244
_refine_ls_wR_factor_ref         0.0591
_refine_ls_wR_factor_gt          0.0562
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.356
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.089

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
Yb1 Yb 0.38436(2) 0.54133(2) 0.42192(2) 0.01776(6) Uani 1 1 d . . . . .
Ti2 Ti 0.39169(5) 0.54343(3) 0.67475(4) 0.01856(12) Uani 1 1 d . . . . .
Ti1 Ti 0.49622(5) 0.66476(3) 0.57307(4) 0.01922(12) Uani 1 1 d . . . . .
Cl1 Cl 0.23296(7) 0.61253(4) 0.31156(7) 0.03207(19) Uani 1 1 d . . . . .
C11 C 0.4588(3) 0.71185(19) 0.3513(3) 0.0324(8) Uani 1 1 d . . . . .
H11A H 0.396291 0.741657 0.375546 0.039 Uiso 1 1 calc R U . . .
H11B H 0.435764 0.692429 0.281348 0.039 Uiso 1 1 calc R U . . .
C12 C 0.5617(4) 0.7581(2) 0.3417(3) 0.0461(10) Uani 1 1 d . . . . .
H12A H 0.582800 0.779145 0.410144 0.069 Uiso 1 1 calc R U . . .
H12B H 0.545343 0.796312 0.290694 0.069 Uiso 1 1 calc R U . . .
H12C H 0.623922 0.728711 0.318026 0.069 Uiso 1 1 calc R U . . .
C21 C 0.5252(10) 0.6498(5) 0.8193(6) 0.040(3) Uani 0.433(13) 1 d D U P A 1
H21A H 0.605181 0.636102 0.815145 0.048 Uiso 0.433(13) 1 calc R U P A 1
H21B H 0.492810 0.620192 0.874874 0.048 Uiso 0.433(13) 1 calc R U P A 1
C22 C 0.5191(16) 0.7291(7) 0.8518(15) 0.039(4) Uani 0.433(13) 1 d D U P A 1
H22A H 0.552786 0.758883 0.798342 0.059 Uiso 0.433(13) 1 calc R U P A 1
H22B H 0.560216 0.735933 0.919328 0.059 Uiso 0.433(13) 1 calc R U P A 1
H22C H 0.440269 0.742936 0.858236 0.059 Uiso 0.433(13) 1 calc R U P A 1
C21A C 0.4508(6) 0.6764(3) 0.8152(4) 0.030(2) Uani 0.567(13) 1 d D U P A 2
H21C H 0.423237 0.644977 0.871057 0.036 Uiso 0.567(13) 1 calc R U P A 2
H21D H 0.391096 0.711793 0.797314 0.036 Uiso 0.567(13) 1 calc R U P A 2
C22A C 0.5545(10) 0.7157(9) 0.8575(14) 0.050(4) Uani 0.567(13) 1 d D U P A 2
H22D H 0.614989 0.681193 0.873274 0.075 Uiso 0.567(13) 1 calc R U P A 2
H22E H 0.536987 0.741405 0.921664 0.075 Uiso 0.567(13) 1 calc R U P A 2
H22F H 0.578753 0.749920 0.804859 0.075 Uiso 0.567(13) 1 calc R U P A 2
C31 C 0.2572(3) 0.42054(18) 0.5992(3) 0.0278(7) Uani 1 1 d . . . . .
H31A H 0.287275 0.403971 0.668643 0.033 Uiso 1 1 calc R U . . .
H31B H 0.273839 0.383271 0.546958 0.033 Uiso 1 1 calc R U . . .
C32 C 0.1314(3) 0.4296(3) 0.6026(4) 0.0539(12) Uani 1 1 d . . . . .
H32A H 0.114244 0.463250 0.658612 0.081 Uiso 1 1 calc R U . . .
H32B H 0.096616 0.383214 0.616213 0.081 Uiso 1 1 calc R U . . .
H32C H 0.101693 0.448358 0.535088 0.081 Uiso 1 1 calc R U . . .
C41 C 0.2338(3) 0.66763(19) 0.5798(3) 0.0306(8) Uani 1 1 d . . . . .
H41A H 0.231662 0.703670 0.522799 0.037 Uiso 1 1 calc R U . . .
H41B H 0.242289 0.693479 0.647401 0.037 Uiso 1 1 calc R U . . .
C42 C 0.1245(3) 0.6271(2) 0.5761(3) 0.0371(9) Uani 1 1 d . . . . .
H42A H 0.115089 0.601907 0.508847 0.056 Uiso 1 1 calc R U . . .
H42B H 0.062107 0.660688 0.583319 0.056 Uiso 1 1 calc R U . . .
H42C H 0.125163 0.592322 0.633587 0.056 Uiso 1 1 calc R U . . .
C51 C 0.3897(4) 0.8188(2) 0.6031(5) 0.0579(13) Uani 1 1 d . . . . .
H51A H 0.351925 0.814604 0.670313 0.069 Uiso 1 1 calc R U . . .
H51B H 0.330853 0.824891 0.546383 0.069 Uiso 1 1 calc R U . . .
C52 C 0.4632(5) 0.8825(2) 0.6067(5) 0.0750(17) Uani 1 1 d . . . . .
H52A H 0.518179 0.878287 0.665966 0.112 Uiso 1 1 calc R U . . .
H52B H 0.417503 0.925542 0.615361 0.112 Uiso 1 1 calc R U . . .
H52C H 0.502750 0.885938 0.541185 0.112 Uiso 1 1 calc R U . . .
C61 C 0.7151(3) 0.7402(2) 0.6292(3) 0.0345(8) Uani 1 1 d . . . . .
H61A H 0.742584 0.734325 0.703164 0.041 Uiso 1 1 calc R U . . .
H61B H 0.667247 0.783559 0.624910 0.041 Uiso 1 1 calc R U . . .
C62 C 0.8135(3) 0.7500(2) 0.5614(3) 0.0413(9) Uani 1 1 d . . . . .
H62A H 0.863835 0.708686 0.569422 0.062 Uiso 1 1 calc R U . . .
H62B H 0.854326 0.793645 0.582578 0.062 Uiso 1 1 calc R U . . .
H62C H 0.786693 0.754213 0.487863 0.062 Uiso 1 1 calc R U . . .
C71 C 0.2227(4) 0.5751(3) 0.8499(3) 0.0529(12) Uani 1 1 d . . . . .
H71A H 0.144400 0.560706 0.830602 0.063 Uiso 1 1 calc R U . . .
H71B H 0.226721 0.627964 0.846036 0.063 Uiso 1 1 calc R U . . .
C72 C 0.2512(5) 0.5520(3) 0.9598(3) 0.0611(13) Uani 1 1 d . . . . .
H72A H 0.242371 0.499987 0.965228 0.092 Uiso 1 1 calc R U . . .
H72B H 0.200707 0.575706 1.007449 0.092 Uiso 1 1 calc R U . . .
H72C H 0.329139 0.565125 0.978873 0.092 Uiso 1 1 calc R U . . .
C81 C 0.5218(3) 0.4512(2) 0.8297(3) 0.0370(9) Uani 1 1 d . . . . .
H81A H 0.524382 0.494018 0.875560 0.044 Uiso 1 1 calc R U . . .
H81B H 0.596630 0.428097 0.835450 0.044 Uiso 1 1 calc R U . . .
C82 C 0.4358(4) 0.4002(3) 0.8678(4) 0.0550(12) Uani 1 1 d . . . . .
H82A H 0.361397 0.422753 0.862378 0.082 Uiso 1 1 calc R U . . .
H82B H 0.454405 0.387825 0.941237 0.082 Uiso 1 1 calc R U . . .
H82C H 0.435233 0.356726 0.824894 0.082 Uiso 1 1 calc R U . . .
C91 C 0.1579(4) 0.4436(3) 0.3052(4) 0.0349(15) Uani 0.772(11) 1 d D U P B 1
H91A H 0.115607 0.487495 0.321961 0.042 Uiso 0.772(11) 1 calc R U P B 1
H91B H 0.121302 0.402528 0.338754 0.042 Uiso 0.772(11) 1 calc R U P B 1
C92 C 0.1543(7) 0.4329(6) 0.1877(5) 0.074(3) Uani 0.772(11) 1 d D U P B 1
H92A H 0.194027 0.472284 0.154733 0.111 Uiso 0.772(11) 1 calc R U P B 1
H92B H 0.075869 0.431984 0.160714 0.111 Uiso 0.772(11) 1 calc R U P B 1
H92C H 0.190622 0.387404 0.171359 0.111 Uiso 0.772(11) 1 calc R U P B 1
C91A C 0.2325(12) 0.4432(10) 0.2376(8) 0.046(6) Uani 0.228(11) 1 d D U P B 2
H91C H 0.270562 0.402126 0.205453 0.055 Uiso 0.228(11) 1 calc R U P B 2
H91D H 0.252698 0.486949 0.198899 0.055 Uiso 0.228(11) 1 calc R U P B 2
C92A C 0.1041(14) 0.4321(18) 0.2265(18) 0.073(9) Uani 0.228(11) 1 d D U P B 2
H92D H 0.082691 0.391910 0.270737 0.109 Uiso 0.228(11) 1 calc R U P B 2
H92E H 0.082302 0.421618 0.153055 0.109 Uiso 0.228(11) 1 calc R U P B 2
H92F H 0.065860 0.475636 0.248508 0.109 Uiso 0.228(11) 1 calc R U P B 2
O1 O 0.47822(18) 0.65410(11) 0.42265(17) 0.0227(5) Uani 1 1 d . . . . .
O2 O 0.4696(2) 0.63383(12) 0.72456(17) 0.0275(5) Uani 1 1 d D . . . .
O3 O 0.31219(18) 0.48538(12) 0.57249(16) 0.0224(5) Uani 1 1 d . . . . .
O4 O 0.32893(17) 0.62194(11) 0.56872(17) 0.0217(4) Uani 1 1 d . . . . .
O5 O 0.4504(2) 0.75531(12) 0.5853(2) 0.0322(5) Uani 1 1 d . . . . .
O6 O 0.64935(18) 0.67927(11) 0.59804(18) 0.0240(5) Uani 1 1 d . . . . .
O7 O 0.29435(19) 0.54574(12) 0.77779(18) 0.0259(5) Uani 1 1 d . . . . .
O8 O 0.49932(18) 0.47350(12) 0.72329(16) 0.0232(5) Uani 1 1 d . . . . .
O9 O 0.27284(19) 0.45007(12) 0.34651(19) 0.0286(5) Uani 1 1 d D . . . .
H9 H 0.316634 0.417261 0.375013 0.043 Uiso 1 1 d R U . B .
O10 O 0.50450(16) 0.55841(11) 0.56483(15) 0.0173(4) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Yb1 O10 2.287(2) 3_666 ?
Yb1 O10 2.2871(19) . ?
Yb1 O9 2.340(2) . ?
Yb1 O8 2.380(2) 3_666 ?
Yb1 O3 2.382(2) . ?
Yb1 O1 2.384(2) . ?
Yb1 O4 2.515(2) . ?
Yb1 Cl1 2.6011(8) . ?
Yb1 Ti2 3.2227(6) . ?
Yb1 Ti1 3.2513(6) . ?
Yb1 Ti2 3.3821(6) 3_666 ?
Yb1 Yb1 3.6645(3) 3_666 ?
Yb1 H9 2.5167 . ?
Ti2 O7 1.792(2) . ?
Ti2 O8 1.913(2) . ?
Ti2 O3 1.913(2) . ?
Ti2 O10 2.005(2) . ?
Ti2 O2 2.015(2) . ?
Ti2 O4 2.108(2) . ?
Ti2 Ti1 2.9184(8) . ?
Ti1 O5 1.786(2) . ?
Ti1 O6 1.856(2) . ?
Ti1 O1 1.931(2) . ?
Ti1 O10 1.992(2) . ?
Ti1 O2 2.056(2) . ?
Ti1 O4 2.145(2) . ?
C11 O1 1.424(4) . ?
C11 C12 1.509(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C21 O2 1.383(7) . ?
C21 C22 1.541(9) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C21A O2 1.429(5) . ?
C21A C22A 1.515(8) . ?
C21A H21C 0.9900 . ?
C21A H21D 0.9900 . ?
C22A H22D 0.9800 . ?
C22A H22E 0.9800 . ?
C22A H22F 0.9800 . ?
C31 O3 1.425(4) . ?
C31 C32 1.510(5) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C41 O4 1.431(4) . ?
C41 C42 1.503(5) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C51 O5 1.412(5) . ?
C51 C52 1.476(7) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C61 O6 1.427(4) . ?
C61 C62 1.500(5) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C71 O7 1.396(5) . ?
C71 C72 1.490(6) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C81 O8 1.433(4) . ?
C81 C82 1.496(6) . ?
C81 H81A 0.9900 . ?
C81 H81B 0.9900 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C91 O9 1.449(4) . ?
C91 C92 1.511(7) . ?
C91 H91A 0.9900 . ?
C91 H91B 0.9900 . ?
C92 H92A 0.9800 . ?
C92 H92B 0.9800 . ?
C92 H92C 0.9800 . ?
C91A O9 1.454(9) . ?
C91A C92A 1.543(10) . ?
C91A H91C 0.9900 . ?
C91A H91D 0.9900 . ?
C92A H92D 0.9800 . ?
C92A H92E 0.9800 . ?
C92A H92F 0.9800 . ?
O9 H9 0.8730 . ?

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
O10 Yb1 O10 73.52(8) 3_666 . ?
O10 Yb1 O9 75.66(7) 3_666 . ?
O10 Yb1 O9 138.72(8) . . ?
O10 Yb1 O8 66.87(7) 3_666 3_666 ?
O10 Yb1 O8 105.77(7) . 3_666 ?
O9 Yb1 O8 86.25(8) . 3_666 ?
O10 Yb1 O3 79.16(7) 3_666 . ?
O10 Yb1 O3 69.75(7) . . ?
O9 Yb1 O3 78.05(8) . . ?
O8 Yb1 O3 145.21(7) 3_666 . ?
O10 Yb1 O1 116.74(7) 3_666 . ?
O10 Yb1 O1 66.29(7) . . ?
O9 Yb1 O1 154.43(8) . . ?
O8 Yb1 O1 79.42(8) 3_666 . ?
O3 Yb1 O1 124.82(7) . . ?
O10 Yb1 O4 127.12(7) 3_666 . ?
O10 Yb1 O4 59.92(7) . . ?
O9 Yb1 O4 125.38(8) . . ?
O8 Yb1 O4 146.26(7) 3_666 . ?
O3 Yb1 O4 62.96(7) . . ?
O1 Yb1 O4 66.87(7) . . ?
O10 Yb1 Cl1 147.22(5) 3_666 . ?
O10 Yb1 Cl1 138.80(5) . . ?
O9 Yb1 Cl1 77.53(6) . . ?
O8 Yb1 Cl1 92.97(6) 3_666 . ?
O3 Yb1 Cl1 113.22(6) . . ?
O1 Yb1 Cl1 82.14(5) . . ?
O4 Yb1 Cl1 84.14(5) . . ?
O10 Yb1 Ti2 86.96(5) 3_666 . ?
O10 Yb1 Ti2 38.14(5) . . ?
O9 Yb1 Ti2 114.14(6) . . ?
O8 Yb1 Ti2 142.24(5) 3_666 . ?
O3 Yb1 Ti2 36.13(5) . . ?
O1 Yb1 Ti2 89.67(5) . . ?
O4 Yb1 Ti2 40.83(5) . . ?
Cl1 Yb1 Ti2 121.44(2) . . ?
O10 Yb1 Ti1 108.30(5) 3_666 . ?
O10 Yb1 Ti1 37.28(5) . . ?
O9 Yb1 Ti1 165.81(6) . . ?
O8 Yb1 Ti1 107.88(5) 3_666 . ?
O3 Yb1 Ti1 89.20(5) . . ?
O1 Yb1 Ti1 36.11(5) . . ?
O4 Yb1 Ti1 41.25(5) . . ?
Cl1 Yb1 Ti1 102.30(2) . . ?
Ti2 Yb1 Ti1 53.586(14) . . ?
O10 Yb1 Ti2 35.16(5) 3_666 3_666 ?
O10 Yb1 Ti2 83.19(5) . 3_666 ?
O9 Yb1 Ti2 87.19(6) . 3_666 ?
O8 Yb1 Ti2 33.37(5) 3_666 3_666 ?
O3 Yb1 Ti2 114.11(5) . 3_666 ?
O1 Yb1 Ti2 92.16(5) . 3_666 ?
O4 Yb1 Ti2 142.20(5) . 3_666 ?
Cl1 Yb1 Ti2 125.46(2) . 3_666 ?
Ti2 Yb1 Ti2 112.653(11) . 3_666 ?
Ti1 Yb1 Ti2 103.881(14) . 3_666 ?
O10 Yb1 Yb1 36.76(5) 3_666 3_666 ?
O10 Yb1 Yb1 36.76(5) . 3_666 ?
O9 Yb1 Yb1 108.33(5) . 3_666 ?
O8 Yb1 Yb1 85.67(5) 3_666 3_666 ?
O3 Yb1 Yb1 70.53(5) . 3_666 ?
O1 Yb1 Yb1 91.71(5) . 3_666 ?
O4 Yb1 Yb1 93.66(5) . 3_666 ?
Cl1 Yb1 Yb1 173.85(2) . 3_666 ?
Ti2 Yb1 Yb1 58.401(10) . 3_666 ?
Ti1 Yb1 Yb1 72.505(11) . 3_666 ?
Ti2 Yb1 Yb1 54.252(10) 3_666 3_666 ?
O10 Yb1 H9 56.3 3_666 . ?
O10 Yb1 H9 120.0 . . ?
O9 Yb1 H9 20.3 . . ?
O8 Yb1 H9 84.2 3_666 . ?
O3 Yb1 H9 70.4 . . ?
O1 Yb1 H9 163.6 . . ?
O4 Yb1 H9 129.5 . . ?
Cl1 Yb1 H9 97.8 . . ?
Ti2 Yb1 H9 104.0 . . ?
Ti1 Yb1 H9 155.8 . . ?
Ti2 Yb1 H9 74.4 3_666 . ?
Yb1 Yb1 H9 88.0 3_666 . ?
O7 Ti2 O8 103.01(10) . . ?
O7 Ti2 O3 101.39(10) . . ?
O8 Ti2 O3 97.86(10) . . ?
O7 Ti2 O10 170.33(10) . . ?
O8 Ti2 O10 82.04(9) . . ?
O3 Ti2 O10 85.90(9) . . ?
O7 Ti2 O2 93.01(10) . . ?
O8 Ti2 O2 100.27(10) . . ?
O3 Ti2 O2 153.64(10) . . ?
O10 Ti2 O2 77.88(9) . . ?
O7 Ti2 O4 103.40(10) . . ?
O8 Ti2 O4 153.51(9) . . ?
O3 Ti2 O4 78.88(9) . . ?
O10 Ti2 O4 71.54(8) . . ?
O2 Ti2 O4 76.34(9) . . ?
O7 Ti2 Ti1 127.63(8) . . ?
O8 Ti2 Ti1 112.41(7) . . ?
O3 Ti2 Ti1 110.17(7) . . ?
O10 Ti2 Ti1 42.93(6) . . ?
O2 Ti2 Ti1 44.75(6) . . ?
O4 Ti2 Ti1 47.19(6) . . ?
O7 Ti2 Yb1 138.21(8) . . ?
O8 Ti2 Yb1 107.61(7) . . ?
O3 Ti2 Yb1 47.22(6) . . ?
O10 Ti2 Yb1 44.77(6) . . ?
O2 Ti2 Yb1 108.45(7) . . ?
O4 Ti2 Yb1 51.24(6) . . ?
Ti1 Ti2 Yb1 63.708(15) . . ?
O7 Ti2 Yb1 145.67(8) . 3_666 ?
O8 Ti2 Yb1 43.18(6) . 3_666 ?
O3 Ti2 Yb1 81.93(7) . 3_666 ?
O10 Ti2 Yb1 41.05(6) . 3_666 ?
O2 Ti2 Yb1 98.50(7) . 3_666 ?
O4 Ti2 Yb1 110.71(6) . 3_666 ?
Ti1 Ti2 Yb1 80.907(17) . 3_666 ?
Yb1 Ti2 Yb1 67.347(11) . 3_666 ?
O5 Ti1 O6 98.54(11) . . ?
O5 Ti1 O1 99.43(11) . . ?
O6 Ti1 O1 104.41(10) . . ?
O5 Ti1 O10 164.78(10) . . ?
O6 Ti1 O10 95.97(9) . . ?
O1 Ti1 O10 81.27(9) . . ?
O5 Ti1 O2 97.09(11) . . ?
O6 Ti1 O2 94.14(10) . . ?
O1 Ti1 O2 152.91(9) . . ?
O10 Ti1 O2 77.26(9) . . ?
O5 Ti1 O4 93.91(10) . . ?
O6 Ti1 O4 164.26(9) . . ?
O1 Ti1 O4 82.84(9) . . ?
O10 Ti1 O4 71.02(8) . . ?
O2 Ti1 O4 74.72(9) . . ?
O5 Ti1 Ti2 123.94(9) . . ?
O6 Ti1 Ti2 118.21(7) . . ?
O1 Ti1 Ti2 109.36(7) . . ?
O10 Ti1 Ti2 43.29(6) . . ?
O2 Ti1 Ti2 43.66(6) . . ?
O4 Ti1 Ti2 46.15(6) . . ?
O5 Ti1 Yb1 127.20(8) . . ?
O6 Ti1 Yb1 125.28(7) . . ?
O1 Ti1 Yb1 46.68(6) . . ?
O10 Ti1 Yb1 44.06(6) . . ?
O2 Ti1 Yb1 106.36(6) . . ?
O4 Ti1 Yb1 50.63(6) . . ?
Ti2 Ti1 Yb1 62.706(15) . . ?
O1 C11 C12 112.1(3) . . ?
O1 C11 H11A 109.2 . . ?
C12 C11 H11A 109.2 . . ?
O1 C11 H11B 109.2 . . ?
C12 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O2 C21 C22 114.5(8) . . ?
O2 C21 H21A 108.6 . . ?
C22 C21 H21A 108.6 . . ?
O2 C21 H21B 108.6 . . ?
C22 C21 H21B 108.6 . . ?
H21A C21 H21B 107.6 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O2 C21A C22A 113.7(7) . . ?
O2 C21A H21C 108.8 . . ?
C22A C21A H21C 108.8 . . ?
O2 C21A H21D 108.8 . . ?
C22A C21A H21D 108.8 . . ?
H21C C21A H21D 107.7 . . ?
C21A C22A H22D 109.5 . . ?
C21A C22A H22E 109.5 . . ?
H22D C22A H22E 109.5 . . ?
C21A C22A H22F 109.5 . . ?
H22D C22A H22F 109.5 . . ?
H22E C22A H22F 109.5 . . ?
O3 C31 C32 112.2(3) . . ?
O3 C31 H31A 109.2 . . ?
C32 C31 H31A 109.2 . . ?
O3 C31 H31B 109.2 . . ?
C32 C31 H31B 109.2 . . ?
H31A C31 H31B 107.9 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O4 C41 C42 112.6(3) . . ?
O4 C41 H41A 109.1 . . ?
C42 C41 H41A 109.1 . . ?
O4 C41 H41B 109.1 . . ?
C42 C41 H41B 109.1 . . ?
H41A C41 H41B 107.8 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O5 C51 C52 112.0(4) . . ?
O5 C51 H51A 109.2 . . ?
C52 C51 H51A 109.2 . . ?
O5 C51 H51B 109.2 . . ?
C52 C51 H51B 109.2 . . ?
H51A C51 H51B 107.9 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
O6 C61 C62 111.7(3) . . ?
O6 C61 H61A 109.3 . . ?
C62 C61 H61A 109.3 . . ?
O6 C61 H61B 109.3 . . ?
C62 C61 H61B 109.3 . . ?
H61A C61 H61B 107.9 . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
O7 C71 C72 112.7(4) . . ?
O7 C71 H71A 109.0 . . ?
C72 C71 H71A 109.0 . . ?
O7 C71 H71B 109.0 . . ?
C72 C71 H71B 109.0 . . ?
H71A C71 H71B 107.8 . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
O8 C81 C82 113.1(3) . . ?
O8 C81 H81A 109.0 . . ?
C82 C81 H81A 109.0 . . ?
O8 C81 H81B 109.0 . . ?
C82 C81 H81B 109.0 . . ?
H81A C81 H81B 107.8 . . ?
C81 C82 H82A 109.5 . . ?
C81 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
C81 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
O9 C91 C92 110.8(4) . . ?
O9 C91 H91A 109.5 . . ?
C92 C91 H91A 109.5 . . ?
O9 C91 H91B 109.5 . . ?
C92 C91 H91B 109.5 . . ?
H91A C91 H91B 108.1 . . ?
C91 C92 H92A 109.5 . . ?
C91 C92 H92B 109.5 . . ?
H92A C92 H92B 109.5 . . ?
C91 C92 H92C 109.5 . . ?
H92A C92 H92C 109.5 . . ?
H92B C92 H92C 109.5 . . ?
O9 C91A C92A 112.5(9) . . ?
O9 C91A H91C 109.1 . . ?
C92A C91A H91C 109.1 . . ?
O9 C91A H91D 109.1 . . ?
C92A C91A H91D 109.1 . . ?
H91C C91A H91D 107.8 . . ?
C91A C92A H92D 109.5 . . ?
C91A C92A H92E 109.5 . . ?
H92D C92A H92E 109.5 . . ?
C91A C92A H92F 109.5 . . ?
H92D C92A H92F 109.5 . . ?
H92E C92A H92F 109.5 . . ?
C11 O1 Ti1 124.4(2) . . ?
C11 O1 Yb1 127.20(19) . . ?
Ti1 O1 Yb1 97.21(9) . . ?
C21 O2 Ti2 130.6(4) . . ?
C21A O2 Ti2 129.3(3) . . ?
C21 O2 Ti1 132.3(4) . . ?
C21A O2 Ti1 129.9(3) . . ?
Ti2 O2 Ti1 91.59(9) . . ?
C31 O3 Ti2 122.47(19) . . ?
C31 O3 Yb1 138.79(19) . . ?
Ti2 O3 Yb1 96.65(9) . . ?
C41 O4 Ti2 127.6(2) . . ?
C41 O4 Ti1 120.91(19) . . ?
Ti2 O4 Ti1 86.65(8) . . ?
C41 O4 Yb1 131.81(19) . . ?
Ti2 O4 Yb1 87.93(7) . . ?
Ti1 O4 Yb1 88.13(7) . . ?
C51 O5 Ti1 165.9(3) . . ?
C61 O6 Ti1 133.3(2) . . ?
C71 O7 Ti2 158.2(3) . . ?
C81 O8 Ti2 126.7(2) . . ?
C81 O8 Yb1 127.9(2) . 3_666 ?
Ti2 O8 Yb1 103.46(9) . 3_666 ?
C91 O9 Yb1 135.9(2) . . ?
C91A O9 Yb1 127.8(7) . . ?
C91 O9 H9 129.0 . . ?
C91A O9 H9 120.0 . . ?
Yb1 O9 H9 91.4 . . ?
Ti1 O10 Ti2 93.78(9) . . ?
Ti1 O10 Yb1 146.97(10) . 3_666 ?
Ti2 O10 Yb1 103.79(8) . 3_666 ?
Ti1 O10 Yb1 98.66(8) . . ?
Ti2 O10 Yb1 97.10(8) . . ?
Yb1 O10 Yb1 106.48(8) 3_666 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C12 C11 O1 Ti1 71.4(4) . . . . ?
C12 C11 O1 Yb1 -153.4(3) . . . . ?
C22 C21 O2 Ti2 -149.2(10) . . . . ?
C22 C21 O2 Ti1 64.8(15) . . . . ?
C22A C21A O2 Ti2 151.1(9) . . . . ?
C22A C21A O2 Ti1 -72.0(11) . . . . ?
C32 C31 O3 Ti2 102.9(3) . . . . ?
C32 C31 O3 Yb1 -97.9(4) . . . . ?
C42 C41 O4 Ti2 -67.1(4) . . . . ?
C42 C41 O4 Ti1 -179.2(2) . . . . ?
C42 C41 O4 Yb1 61.8(4) . . . . ?
C52 C51 O5 Ti1 165.2(10) . . . . ?
O6 Ti1 O5 C51 -150.9(12) . . . . ?
O1 Ti1 O5 C51 102.8(12) . . . . ?
O10 Ti1 O5 C51 11.4(15) . . . . ?
O2 Ti1 O5 C51 -55.7(12) . . . . ?
O4 Ti1 O5 C51 19.4(12) . . . . ?
Ti2 Ti1 O5 C51 -18.3(13) . . . . ?
Yb1 Ti1 O5 C51 61.1(13) . . . . ?
C62 C61 O6 Ti1 -132.0(3) . . . . ?
O5 Ti1 O6 C61 6.3(3) . . . . ?
O1 Ti1 O6 C61 108.4(3) . . . . ?
O10 Ti1 O6 C61 -169.1(3) . . . . ?
O2 Ti1 O6 C61 -91.5(3) . . . . ?
O4 Ti1 O6 C61 -135.6(4) . . . . ?
Ti2 Ti1 O6 C61 -129.8(3) . . . . ?
Yb1 Ti1 O6 C61 155.1(3) . . . . ?
C72 C71 O7 Ti2 -125.1(6) . . . . ?
O8 Ti2 O7 C71 137.5(7) . . . . ?
O3 Ti2 O7 C71 -121.6(7) . . . . ?
O2 Ti2 O7 C71 36.2(7) . . . . ?
O4 Ti2 O7 C71 -40.5(7) . . . . ?
Ti1 Ti2 O7 C71 5.2(7) . . . . ?
Yb1 Ti2 O7 C71 -86.1(7) . . . . ?
Yb1 Ti2 O7 C71 146.1(7) 3_666 . . . ?
C82 C81 O8 Ti2 78.1(4) . . . . ?
C82 C81 O8 Yb1 -120.6(3) . . . 3_666 ?
C92 C91 O9 Yb1 111.6(5) . . . . ?
C92A C91A O9 Yb1 -127.3(17) . . . . ?

####################################################################### 
# 
# 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_Ti4Tm2
_database_code_depnum_ccdc_archive 'CCDC 2283718'
loop_
_audit_author_name
_audit_author_address
'Andrew Bond'
;University of Cambridge
United Kingdom
;
_audit_update_record             
;
2023-07-22 deposited with the CCDC.	2023-09-15 downloaded from the CCDC.
;
#===============================================================================
_audit_creation_method           SHELXL-2019/2

#-------------------------------------------------------------------------------
# Inserted by local software: cifUpdate ver. 3.1  (Andrew D. Bond, March 2019)
#-------------------------------------------------------------------------------
_cambridge_user_name             'Olivia Georghiades'
_cambridge_user_crsid            omg24
_cambridge_supervisor_name       'Dominic Wright'
_cambridge_supervisor_crsid      dsw1000
_cambridge_crystallographer_name 'Andrew Bond'
_cambridge_crystallographer_crsid adb29
_cambridge_sample_id             'OG03 Tm'
_cambridge_data_id               DW_B1_0479
#-------------------------------------------------------------------------------

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H92 Cl2 O20 Ti4 Tm2'
_chemical_formula_sum            'C36 H92 Cl2 O20 Ti4 Tm2'
_chemical_formula_weight         1445.45

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'
Cl Cl 0.3639 0.7018 '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'
Tm Tm -8.0393 4.1821 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   11.9196(4)
_cell_length_b                   18.7621(6)
_cell_length_c                   12.7550(4)
_cell_angle_alpha                90
_cell_angle_beta                 92.8718(13)
_cell_angle_gamma                90
_cell_volume                     2848.90(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9805
_cell_measurement_theta_min      5.21
_cell_measurement_theta_max      66.55

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_F_000             1456
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    11.517
_shelx_estimated_absorpt_T_min   0.277
_shelx_estimated_absorpt_T_max   0.392
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5184
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Incoatec I\mS Cu microsource'
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-III'
_diffrn_measurement_method       'ω and φ-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            47040
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         5.489
_diffrn_reflns_theta_max         66.648
_diffrn_reflns_theta_full        66.648
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             5004
_reflns_number_gt                4736
_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.

#===============================================================================
INTENSITY STATISTICS FOR DATASET # 1  DW_B1_0479_0m.hkl
#===============================================================================
 Resolution   #Data #Theory %Complete Redundancy Mean I Mean I/s Rmerge  Rsigma
#-------------------------------------------------------------------------------
  Inf - 3.40      78     90     86.7     5.20     64.09   39.12  0.0317  0.0271
 3.40 - 2.29     183    188     97.3     6.18    109.44   40.04  0.0318  0.0289
 2.29 - 1.82     259    260     99.6     8.25     97.93   46.73  0.0325  0.0209
 1.82 - 1.58     273    273    100.0    11.23     80.30   51.84  0.0363  0.0175
 1.58 - 1.44     250    250    100.0    13.82     65.44   54.61  0.0351  0.0132
 1.44 - 1.34     252    252    100.0    14.08     50.11   52.10  0.0384  0.0137
 1.34 - 1.25     294    294    100.0    13.31     42.03   42.33  0.0390  0.0150
 1.25 - 1.19     251    251    100.0    12.97     40.17   43.52  0.0405  0.0157
 1.19 - 1.14     258    258    100.0    12.22     31.74   39.49  0.0444  0.0173
 1.14 - 1.09     293    293    100.0    12.18     35.23   40.65  0.0451  0.0169
 1.09 - 1.06     203    203    100.0     9.90     31.14   32.95  0.0514  0.0210
 1.06 - 1.03     255    255    100.0    11.27     29.44   36.88  0.0534  0.0187
 1.03 - 0.99     328    328    100.0    10.01     25.97   32.22  0.0555  0.0204
 0.99 - 0.97     222    222    100.0     7.33     25.21   30.80  0.0429  0.0228
 0.97 - 0.94     322    322    100.0     6.72     18.62   27.03  0.0473  0.0255
 0.94 - 0.92     237    237    100.0     6.52     19.06   26.19  0.0476  0.0252
 0.92 - 0.90     267    267    100.0     5.76     17.21   23.79  0.0515  0.0276
 0.90 - 0.88     304    306     99.3     5.96     14.63   24.93  0.0525  0.0275
 0.88 - 0.87     160    160    100.0     5.65     13.81   24.30  0.0524  0.0276
 0.87 - 0.85     308    308    100.0     5.14     15.33   24.64  0.0487  0.0273
 0.85 - 0.84     190    196     96.9     4.56     11.98   20.58  0.0503  0.0308
#-------------------------------------------------------------------------------
 0.94 - 0.84    1466   1474     99.5     5.62     15.53   24.23  0.0503  0.0274
  Inf - 0.84    5187   5213     99.5     9.20     38.36   35.98  0.0410  0.0202
#===============================================================================
;

_computing_data_collection       'APEX4 (Bruker, 2021)'
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL

_refine_special_details          ?

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0237P)²+2.5468P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5004
_refine_ls_number_parameters     318
_refine_ls_number_restraints     143
_refine_ls_R_factor_all          0.0214
_refine_ls_R_factor_gt           0.0200
_refine_ls_wR_factor_ref         0.0511
_refine_ls_wR_factor_gt          0.0504
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.107
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.917
_refine_diff_density_rms         0.073

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
Tm1 Tm 0.38412(2) 0.54138(2) 0.42131(2) 0.01731(5) Uani 1 1 d . . . . .
Ti2 Ti 0.39252(3) 0.54387(2) 0.67492(3) 0.01833(9) Uani 1 1 d . . . . .
Ti1 Ti 0.49694(3) 0.66448(2) 0.57278(3) 0.01878(9) Uani 1 1 d . . . . .
Cl1 Cl 0.23342(5) 0.61241(3) 0.30825(5) 0.03274(14) Uani 1 1 d . . . . .
O1 O 0.47877(13) 0.65401(8) 0.42227(12) 0.0228(3) Uani 1 1 d . . . . .
O2 O 0.47114(14) 0.63374(9) 0.72490(12) 0.0267(4) Uani 1 1 d D . . . .
O3 O 0.31340(13) 0.48554(8) 0.57255(12) 0.0227(3) Uani 1 1 d . . . . .
O4 O 0.32956(12) 0.62175(8) 0.56775(12) 0.0213(3) Uani 1 1 d . . . . .
O5 O 0.45105(15) 0.75470(9) 0.58520(15) 0.0318(4) Uani 1 1 d . . . . .
O6 O 0.64995(13) 0.67942(8) 0.59733(13) 0.0246(3) Uani 1 1 d . . . . .
H6 H 0.675147 0.638598 0.615217 0.037 Uiso 1 1 d R U . . .
O7 O 0.29488(14) 0.54642(9) 0.77714(13) 0.0259(4) Uani 1 1 d . . . . .
O8 O 0.49963(14) 0.47391(9) 0.72429(12) 0.0228(3) Uani 1 1 d . . . . .
O9 O 0.27186(14) 0.44933(9) 0.34631(14) 0.0287(4) Uani 1 1 d D . . . .
O10 O 0.50467(12) 0.55872(8) 0.56530(11) 0.0170(3) Uani 1 1 d . . . . .
C11 C 0.4597(2) 0.71166(14) 0.3501(2) 0.0320(6) Uani 1 1 d . U . . .
H11A H 0.397975 0.741900 0.374227 0.038 Uiso 1 1 calc R U . . .
H11B H 0.435910 0.692236 0.280266 0.038 Uiso 1 1 calc R U . . .
C12 C 0.5629(3) 0.75650(17) 0.3402(3) 0.0487(8) Uani 1 1 d . U . . .
H12A H 0.546531 0.795274 0.290263 0.073 Uiso 1 1 calc R U . . .
H12B H 0.585800 0.776571 0.408900 0.073 Uiso 1 1 calc R U . . .
H12C H 0.623718 0.726930 0.314981 0.073 Uiso 1 1 calc R U . . .
C21 C 0.4504(4) 0.6762(2) 0.8145(3) 0.0322(13) Uani 0.655(9) 1 d D U P A 1
H21A H 0.429405 0.643963 0.871819 0.039 Uiso 0.655(9) 1 calc R U P A 1
H21B H 0.384715 0.706996 0.796925 0.039 Uiso 0.655(9) 1 calc R U P A 1
C22 C 0.5422(3) 0.7213(2) 0.8543(3) 0.0646(11) Uani 0.655(9) 1 d D U P A 1
H22A H 0.518596 0.747855 0.915542 0.097 Uiso 0.655(9) 1 calc R U P A 1
H22B H 0.607301 0.691578 0.874585 0.097 Uiso 0.655(9) 1 calc R U P A 1
H22C H 0.562461 0.754823 0.799440 0.097 Uiso 0.655(9) 1 calc R U P A 1
C21A C 0.5276(8) 0.6476(4) 0.8148(6) 0.034(3) Uani 0.345(9) 1 d D U P A 2
H21C H 0.603795 0.627282 0.809302 0.040 Uiso 0.345(9) 1 calc R U P A 2
H21D H 0.491158 0.620171 0.870008 0.040 Uiso 0.345(9) 1 calc R U P A 2
C22A C 0.5422(3) 0.7213(2) 0.8543(3) 0.0646(11) Uani 0.345(9) 1 d D U P A 2
H22D H 0.586002 0.720609 0.921342 0.097 Uiso 0.345(9) 1 calc R U P A 2
H22E H 0.581794 0.749624 0.803226 0.097 Uiso 0.345(9) 1 calc R U P A 2
H22F H 0.468335 0.742462 0.864375 0.097 Uiso 0.345(9) 1 calc R U P A 2
C31 C 0.2582(2) 0.42090(13) 0.5993(2) 0.0282(5) Uani 1 1 d . U . . .
H31A H 0.286784 0.404987 0.669631 0.034 Uiso 1 1 calc R U . . .
H31B H 0.275845 0.383378 0.548094 0.034 Uiso 1 1 calc R U . . .
C32 C 0.1330(2) 0.43040(19) 0.5996(3) 0.0537(9) Uani 1 1 d . U . . .
H32A H 0.097974 0.385181 0.618191 0.081 Uiso 1 1 calc R U . . .
H32B H 0.115198 0.466902 0.651147 0.081 Uiso 1 1 calc R U . . .
H32C H 0.104266 0.445307 0.529685 0.081 Uiso 1 1 calc R U . . .
C41 C 0.2343(2) 0.66737(14) 0.5780(2) 0.0293(5) Uani 1 1 d . U . . .
H41A H 0.232614 0.703353 0.521120 0.035 Uiso 1 1 calc R U . . .
H41B H 0.242208 0.692974 0.645785 0.035 Uiso 1 1 calc R U . . .
C42 C 0.1251(2) 0.62678(17) 0.5728(2) 0.0374(6) Uani 1 1 d . U . . .
H42A H 0.062575 0.660039 0.580136 0.056 Uiso 1 1 calc R U . . .
H42B H 0.116050 0.602134 0.505207 0.056 Uiso 1 1 calc R U . . .
H42C H 0.125643 0.591756 0.629869 0.056 Uiso 1 1 calc R U . . .
C51 C 0.3906(3) 0.81783(17) 0.6027(3) 0.0606(10) Uani 1 1 d . U . . .
H51A H 0.352203 0.813420 0.669419 0.073 Uiso 1 1 calc R U . . .
H51B H 0.332231 0.824014 0.545386 0.073 Uiso 1 1 calc R U . . .
C52 C 0.4634(4) 0.88124(19) 0.6076(4) 0.0881(15) Uani 1 1 d . U . . .
H52A H 0.417889 0.923658 0.619792 0.132 Uiso 1 1 calc R U . . .
H52B H 0.520369 0.875833 0.665145 0.132 Uiso 1 1 calc R U . . .
H52C H 0.500398 0.886426 0.541118 0.132 Uiso 1 1 calc R U . . .
C61 C 0.7160(2) 0.73971(14) 0.6285(2) 0.0328(6) Uani 1 1 d . U . . .
H61A H 0.743569 0.733839 0.702537 0.039 Uiso 1 1 calc R U . . .
H61B H 0.668609 0.783056 0.623998 0.039 Uiso 1 1 calc R U . . .
C62 C 0.8142(2) 0.74893(17) 0.5607(2) 0.0424(7) Uani 1 1 d . U . . .
H62A H 0.857789 0.790775 0.584230 0.064 Uiso 1 1 calc R U . . .
H62B H 0.861942 0.706436 0.566088 0.064 Uiso 1 1 calc R U . . .
H62C H 0.787038 0.755616 0.487607 0.064 Uiso 1 1 calc R U . . .
C71 C 0.2205(3) 0.5742(2) 0.8483(2) 0.0537(9) Uani 1 1 d . U . . .
H71A H 0.143516 0.557664 0.828520 0.064 Uiso 1 1 calc R U . . .
H71B H 0.221046 0.626883 0.843619 0.064 Uiso 1 1 calc R U . . .
C72 C 0.2497(4) 0.5527(2) 0.9585(3) 0.0645(11) Uani 1 1 d . U . . .
H72A H 0.195402 0.573471 1.004962 0.097 Uiso 1 1 calc R U . . .
H72B H 0.247746 0.500646 0.964057 0.097 Uiso 1 1 calc R U . . .
H72C H 0.325295 0.569881 0.979160 0.097 Uiso 1 1 calc R U . . .
C81 C 0.5230(3) 0.45271(16) 0.8313(2) 0.0375(7) Uani 1 1 d . U . . .
H81A H 0.525024 0.495622 0.876500 0.045 Uiso 1 1 calc R U . . .
H81B H 0.598022 0.430076 0.837518 0.045 Uiso 1 1 calc R U . . .
C82 C 0.4373(3) 0.40157(18) 0.8698(3) 0.0552(9) Uani 1 1 d . U . . .
H82A H 0.456914 0.388799 0.942920 0.083 Uiso 1 1 calc R U . . .
H82B H 0.362954 0.424051 0.865290 0.083 Uiso 1 1 calc R U . . .
H82C H 0.435966 0.358491 0.826300 0.083 Uiso 1 1 calc R U . . .
C91 C 0.1576(3) 0.4431(2) 0.3039(3) 0.0382(12) Uani 0.756(8) 1 d D U P B 1
H91A H 0.115366 0.486884 0.319827 0.046 Uiso 0.756(8) 1 calc R U P B 1
H91B H 0.120464 0.402313 0.337260 0.046 Uiso 0.756(8) 1 calc R U P B 1
C92 C 0.1557(6) 0.4321(4) 0.1873(4) 0.081(2) Uani 0.756(8) 1 d D U P B 1
H92A H 0.077722 0.427937 0.159731 0.121 Uiso 0.756(8) 1 calc R U P B 1
H92B H 0.191501 0.472773 0.154307 0.121 Uiso 0.756(8) 1 calc R U P B 1
H92C H 0.196590 0.388340 0.171712 0.121 Uiso 0.756(8) 1 calc R U P B 1
C91A C 0.2297(8) 0.4436(6) 0.2367(7) 0.034(3) Uani 0.244(8) 1 d D U P B 2
H91C H 0.264613 0.401976 0.203531 0.041 Uiso 0.244(8) 1 calc R U P B 2
H91D H 0.250710 0.486871 0.197853 0.041 Uiso 0.244(8) 1 calc R U P B 2
C92A C 0.1015(10) 0.4351(13) 0.2302(14) 0.075(6) Uani 0.244(8) 1 d D U P B 2
H92D H 0.074874 0.431395 0.156429 0.112 Uiso 0.244(8) 1 calc R U P B 2
H92E H 0.080811 0.391914 0.267786 0.112 Uiso 0.244(8) 1 calc R U P B 2
H92F H 0.066928 0.476685 0.262117 0.112 Uiso 0.244(8) 1 calc R U P B 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
Tm1 O10 2.2976(14) . ?
Tm1 O10 2.3002(15) 3_666 ?
Tm1 O9 2.3581(16) . ?
Tm1 O3 2.3859(16) . ?
Tm1 O8 2.3894(16) 3_666 ?
Tm1 O1 2.3951(16) . ?
Tm1 O4 2.5114(16) . ?
Tm1 Cl1 2.6120(6) . ?
Tm1 Ti2 3.2316(4) . ?
Tm1 Ti1 3.2580(4) . ?
Tm1 Ti2 3.3884(4) 3_666 ?
Tm1 Tm1 3.6764(2) 3_666 ?
Ti2 O7 1.7913(17) . ?
Ti2 O3 1.9155(16) . ?
Ti2 O8 1.9155(16) . ?
Ti2 O10 2.0017(16) . ?
Ti2 O2 2.0168(16) . ?
Ti2 O4 2.1128(16) . ?
Ti2 Ti1 2.9205(6) . ?
Ti1 O5 1.7884(17) . ?
Ti1 O6 1.8562(16) . ?
Ti1 O1 1.9312(16) . ?
Ti1 O10 1.9890(15) . ?
Ti1 O2 2.0620(16) . ?
Ti1 O4 2.1482(16) . ?
Ti1 H6 2.2193 . ?
O1 C11 1.431(3) . ?
O2 C21A 1.326(7) . ?
O2 C21 1.425(4) . ?
O3 C31 1.429(3) . ?
O4 C41 1.433(3) . ?
O5 C51 1.410(3) . ?
O6 C61 1.423(3) . ?
O6 H6 0.8497 . ?
O7 C71 1.401(3) . ?
O8 C81 1.435(3) . ?
O9 C91 1.445(4) . ?
O9 C91A 1.466(8) . ?
C11 C12 1.501(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C21 C22 1.454(5) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C21A C22A 1.479(7) . ?
C21A H21C 0.9900 . ?
C21A H21D 0.9900 . ?
C22A H22D 0.9800 . ?
C22A H22E 0.9800 . ?
C22A H22F 0.9800 . ?
C31 C32 1.503(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C41 C42 1.506(4) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C51 C52 1.472(5) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C61 C62 1.500(4) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C71 C72 1.486(5) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C81 C82 1.502(4) . ?
C81 H81A 0.9900 . ?
C81 H81B 0.9900 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C91 C92 1.501(6) . ?
C91 H91A 0.9900 . ?
C91 H91B 0.9900 . ?
C92 H92A 0.9800 . ?
C92 H92B 0.9800 . ?
C92 H92C 0.9800 . ?
C91A C92A 1.534(9) . ?
C91A H91C 0.9900 . ?
C91A H91D 0.9900 . ?
C92A H92D 0.9800 . ?
C92A H92E 0.9800 . ?
C92A H92F 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
O10 Tm1 O10 73.81(6) . 3_666 ?
O10 Tm1 O9 138.37(6) . . ?
O10 Tm1 O9 75.24(6) 3_666 . ?
O10 Tm1 O3 69.39(5) . . ?
O10 Tm1 O3 78.88(5) 3_666 . ?
O9 Tm1 O3 77.88(6) . . ?
O10 Tm1 O8 105.93(5) . 3_666 ?
O10 Tm1 O8 66.74(5) 3_666 3_666 ?
O9 Tm1 O8 86.34(6) . 3_666 ?
O3 Tm1 O8 144.87(5) . 3_666 ?
O10 Tm1 O1 66.14(5) . . ?
O10 Tm1 O1 116.77(5) 3_666 . ?
O9 Tm1 O1 154.93(6) . . ?
O3 Tm1 O1 124.66(5) . . ?
O8 Tm1 O1 79.54(6) 3_666 . ?
O10 Tm1 O4 59.70(5) . . ?
O10 Tm1 O4 127.21(5) 3_666 . ?
O9 Tm1 O4 125.36(6) . . ?
O3 Tm1 O4 63.08(5) . . ?
O8 Tm1 O4 146.31(5) 3_666 . ?
O1 Tm1 O4 66.80(5) . . ?
O10 Tm1 Cl1 138.97(4) . . ?
O10 Tm1 Cl1 146.65(4) 3_666 . ?
O9 Tm1 Cl1 77.83(4) . . ?
O3 Tm1 Cl1 114.17(4) . . ?
O8 Tm1 Cl1 92.39(4) 3_666 . ?
O1 Tm1 Cl1 82.15(4) . . ?
O4 Tm1 Cl1 84.71(4) . . ?
O10 Tm1 Ti2 37.91(4) . . ?
O10 Tm1 Ti2 87.06(4) 3_666 . ?
O9 Tm1 Ti2 113.90(5) . . ?
O3 Tm1 Ti2 36.06(4) . . ?
O8 Tm1 Ti2 142.15(4) 3_666 . ?
O1 Tm1 Ti2 89.50(4) . . ?
O4 Tm1 Ti2 40.80(4) . . ?
Cl1 Tm1 Ti2 122.087(17) . . ?
O10 Tm1 Ti1 37.12(4) . . ?
O10 Tm1 Ti1 108.39(4) 3_666 . ?
O9 Tm1 Ti1 165.64(5) . . ?
O3 Tm1 Ti1 89.08(4) . . ?
O8 Tm1 Ti1 107.93(4) 3_666 . ?
O1 Tm1 Ti1 36.03(4) . . ?
O4 Tm1 Ti1 41.23(4) . . ?
Cl1 Tm1 Ti1 102.575(16) . . ?
Ti2 Tm1 Ti1 53.488(10) . . ?
O10 Tm1 Ti2 83.40(4) . 3_666 ?
O10 Tm1 Ti2 35.02(4) 3_666 3_666 ?
O9 Tm1 Ti2 86.99(5) . 3_666 ?
O3 Tm1 Ti2 113.67(4) . 3_666 ?
O8 Tm1 Ti2 33.38(4) 3_666 3_666 ?
O1 Tm1 Ti2 92.28(4) . 3_666 ?
O4 Tm1 Ti2 142.22(3) . 3_666 ?
Cl1 Tm1 Ti2 124.887(17) . 3_666 ?
Ti2 Tm1 Ti2 112.578(9) . 3_666 ?
Ti1 Tm1 Ti2 103.945(10) . 3_666 ?
O10 Tm1 Tm1 36.93(4) . 3_666 ?
O10 Tm1 Tm1 36.88(4) 3_666 3_666 ?
O9 Tm1 Tm1 107.92(4) . 3_666 ?
O3 Tm1 Tm1 70.08(4) . 3_666 ?
O8 Tm1 Tm1 85.67(4) 3_666 3_666 ?
O1 Tm1 Tm1 91.66(4) . 3_666 ?
O4 Tm1 Tm1 93.61(3) . 3_666 ?
Cl1 Tm1 Tm1 173.760(15) . 3_666 ?
Ti2 Tm1 Tm1 58.323(8) . 3_666 ?
Ti1 Tm1 Tm1 72.489(8) . 3_666 ?
Ti2 Tm1 Tm1 54.255(8) 3_666 3_666 ?
O7 Ti2 O3 101.29(7) . . ?
O7 Ti2 O8 103.04(7) . . ?
O3 Ti2 O8 97.46(7) . . ?
O7 Ti2 O10 170.30(7) . . ?
O3 Ti2 O10 85.79(6) . . ?
O8 Ti2 O10 82.39(6) . . ?
O7 Ti2 O2 93.22(7) . . ?
O3 Ti2 O2 153.94(7) . . ?
O8 Ti2 O2 100.22(7) . . ?
O10 Ti2 O2 77.79(6) . . ?
O7 Ti2 O4 103.29(7) . . ?
O3 Ti2 O4 78.89(7) . . ?
O8 Ti2 O4 153.63(7) . . ?
O10 Ti2 O4 71.33(6) . . ?
O2 Ti2 O4 76.75(6) . . ?
O7 Ti2 Ti1 127.66(6) . . ?
O3 Ti2 Ti1 110.18(5) . . ?
O8 Ti2 Ti1 112.69(5) . . ?
O10 Ti2 Ti1 42.79(4) . . ?
O2 Ti2 Ti1 44.90(5) . . ?
O4 Ti2 Ti1 47.24(4) . . ?
O7 Ti2 Tm1 137.75(6) . . ?
O3 Ti2 Tm1 47.15(5) . . ?
O8 Ti2 Tm1 107.81(5) . . ?
O10 Ti2 Tm1 44.86(4) . . ?
O2 Ti2 Tm1 108.61(5) . . ?
O4 Ti2 Tm1 50.97(4) . . ?
Ti1 Ti2 Tm1 63.719(11) . . ?
O7 Ti2 Tm1 145.81(6) . 3_666 ?
O3 Ti2 Tm1 81.50(5) . 3_666 ?
O8 Ti2 Tm1 43.34(5) . 3_666 ?
O10 Ti2 Tm1 41.26(4) . 3_666 ?
O2 Ti2 Tm1 98.51(5) . 3_666 ?
O4 Ti2 Tm1 110.62(4) . 3_666 ?
Ti1 Ti2 Tm1 81.025(13) . 3_666 ?
Tm1 Ti2 Tm1 67.422(9) . 3_666 ?
O5 Ti1 O6 98.30(8) . . ?
O5 Ti1 O1 99.48(8) . . ?
O6 Ti1 O1 104.09(7) . . ?
O5 Ti1 O10 164.51(8) . . ?
O6 Ti1 O10 96.39(7) . . ?
O1 Ti1 O10 81.60(6) . . ?
O5 Ti1 O2 96.93(8) . . ?
O6 Ti1 O2 94.31(7) . . ?
O1 Ti1 O2 153.18(7) . . ?
O10 Ti1 O2 77.03(6) . . ?
O5 Ti1 O4 93.91(7) . . ?
O6 Ti1 O4 164.71(7) . . ?
O1 Ti1 O4 82.80(6) . . ?
O10 Ti1 O4 70.82(6) . . ?
O2 Ti1 O4 75.03(6) . . ?
O5 Ti1 Ti2 123.70(6) . . ?
O6 Ti1 Ti2 118.61(5) . . ?
O1 Ti1 Ti2 109.60(5) . . ?
O10 Ti1 Ti2 43.13(4) . . ?
O2 Ti1 Ti2 43.66(4) . . ?
O4 Ti1 Ti2 46.23(4) . . ?
O5 Ti1 Tm1 127.19(6) . . ?
O6 Ti1 Tm1 125.45(5) . . ?
O1 Ti1 Tm1 46.84(5) . . ?
O10 Ti1 Tm1 44.20(4) . . ?
O2 Ti1 Tm1 106.45(5) . . ?
O4 Ti1 Tm1 50.40(4) . . ?
Ti2 Ti1 Tm1 62.793(11) . . ?
O5 Ti1 H6 118.6 . . ?
O6 Ti1 H6 21.8 . . ?
O1 Ti1 H6 106.2 . . ?
O10 Ti1 H6 75.4 . . ?
O2 Ti1 H6 84.0 . . ?
O4 Ti1 H6 143.3 . . ?
Ti2 Ti1 H6 98.4 . . ?
Tm1 Ti1 H6 110.6 . . ?
C11 O1 Ti1 124.68(15) . . ?
C11 O1 Tm1 127.13(14) . . ?
Ti1 O1 Tm1 97.13(6) . . ?
C21A O2 Ti2 130.2(3) . . ?
C21 O2 Ti2 128.62(19) . . ?
C21A O2 Ti1 131.7(4) . . ?
C21 O2 Ti1 129.7(2) . . ?
Ti2 O2 Ti1 91.44(6) . . ?
C31 O3 Ti2 122.63(14) . . ?
C31 O3 Tm1 138.69(14) . . ?
Ti2 O3 Tm1 96.80(6) . . ?
C41 O4 Ti2 127.71(14) . . ?
C41 O4 Ti1 120.89(14) . . ?
Ti2 O4 Ti1 86.53(6) . . ?
C41 O4 Tm1 131.45(14) . . ?
Ti2 O4 Tm1 88.23(5) . . ?
Ti1 O4 Tm1 88.37(5) . . ?
C51 O5 Ti1 166.0(2) . . ?
C61 O6 Ti1 133.79(16) . . ?
C61 O6 H6 117.3 . . ?
Ti1 O6 H6 103.9 . . ?
C71 O7 Ti2 159.5(2) . . ?
C81 O8 Ti2 126.64(16) . . ?
C81 O8 Tm1 127.84(15) . 3_666 ?
Ti2 O8 Tm1 103.28(7) . 3_666 ?
C91 O9 Tm1 135.76(19) . . ?
C91A O9 Tm1 127.0(4) . . ?
Ti1 O10 Ti2 94.08(6) . . ?
Ti1 O10 Tm1 98.68(6) . . ?
Ti2 O10 Tm1 97.23(6) . . ?
Ti1 O10 Tm1 147.03(8) . 3_666 ?
Ti2 O10 Tm1 103.72(6) . 3_666 ?
Tm1 O10 Tm1 106.19(6) . 3_666 ?
O1 C11 C12 111.9(2) . . ?
O1 C11 H11A 109.2 . . ?
C12 C11 H11A 109.2 . . ?
O1 C11 H11B 109.2 . . ?
C12 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O2 C21 C22 116.6(3) . . ?
O2 C21 H21A 108.2 . . ?
C22 C21 H21A 108.2 . . ?
O2 C21 H21B 108.2 . . ?
C22 C21 H21B 108.2 . . ?
H21A C21 H21B 107.3 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O2 C21A C22A 121.5(6) . . ?
O2 C21A H21C 106.9 . . ?
C22A C21A H21C 106.9 . . ?
O2 C21A H21D 106.9 . . ?
C22A C21A H21D 106.9 . . ?
H21C C21A H21D 106.7 . . ?
C21A C22A H22D 109.5 . . ?
C21A C22A H22E 109.5 . . ?
H22D C22A H22E 109.5 . . ?
C21A C22A H22F 109.5 . . ?
H22D C22A H22F 109.5 . . ?
H22E C22A H22F 109.5 . . ?
O3 C31 C32 111.7(2) . . ?
O3 C31 H31A 109.3 . . ?
C32 C31 H31A 109.3 . . ?
O3 C31 H31B 109.3 . . ?
C32 C31 H31B 109.3 . . ?
H31A C31 H31B 107.9 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O4 C41 C42 112.4(2) . . ?
O4 C41 H41A 109.1 . . ?
C42 C41 H41A 109.1 . . ?
O4 C41 H41B 109.1 . . ?
C42 C41 H41B 109.1 . . ?
H41A C41 H41B 107.9 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O5 C51 C52 112.4(3) . . ?
O5 C51 H51A 109.1 . . ?
C52 C51 H51A 109.1 . . ?
O5 C51 H51B 109.1 . . ?
C52 C51 H51B 109.1 . . ?
H51A C51 H51B 107.9 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
O6 C61 C62 111.5(2) . . ?
O6 C61 H61A 109.3 . . ?
C62 C61 H61A 109.3 . . ?
O6 C61 H61B 109.3 . . ?
C62 C61 H61B 109.3 . . ?
H61A C61 H61B 108.0 . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
O7 C71 C72 112.7(3) . . ?
O7 C71 H71A 109.0 . . ?
C72 C71 H71A 109.0 . . ?
O7 C71 H71B 109.0 . . ?
C72 C71 H71B 109.0 . . ?
H71A C71 H71B 107.8 . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
O8 C81 C82 112.7(3) . . ?
O8 C81 H81A 109.1 . . ?
C82 C81 H81A 109.1 . . ?
O8 C81 H81B 109.1 . . ?
C82 C81 H81B 109.1 . . ?
H81A C81 H81B 107.8 . . ?
C81 C82 H82A 109.5 . . ?
C81 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
C81 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
O9 C91 C92 110.4(4) . . ?
O9 C91 H91A 109.6 . . ?
C92 C91 H91A 109.6 . . ?
O9 C91 H91B 109.6 . . ?
C92 C91 H91B 109.6 . . ?
H91A C91 H91B 108.1 . . ?
C91 C92 H92A 109.5 . . ?
C91 C92 H92B 109.5 . . ?
H92A C92 H92B 109.5 . . ?
C91 C92 H92C 109.5 . . ?
H92A C92 H92C 109.5 . . ?
H92B C92 H92C 109.5 . . ?
O9 C91A C92A 110.6(8) . . ?
O9 C91A H91C 109.5 . . ?
C92A C91A H91C 109.5 . . ?
O9 C91A H91D 109.5 . . ?
C92A C91A H91D 109.5 . . ?
H91C C91A H91D 108.1 . . ?
C91A C92A H92D 109.5 . . ?
C91A C92A H92E 109.5 . . ?
H92D C92A H92E 109.5 . . ?
C91A C92A H92F 109.5 . . ?
H92D C92A H92F 109.5 . . ?
H92E C92A H92F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O6 Ti1 O5 C51 -152.1(9) . . . . ?
O1 Ti1 O5 C51 102.1(9) . . . . ?
O10 Ti1 O5 C51 9.3(11) . . . . ?
O2 Ti1 O5 C51 -56.7(9) . . . . ?
O4 Ti1 O5 C51 18.7(9) . . . . ?
Ti2 Ti1 O5 C51 -19.3(9) . . . . ?
Tm1 Ti1 O5 C51 60.1(9) . . . . ?
O5 Ti1 O6 C61 6.6(2) . . . . ?
O1 Ti1 O6 C61 108.6(2) . . . . ?
O10 Ti1 O6 C61 -168.5(2) . . . . ?
O2 Ti1 O6 C61 -91.1(2) . . . . ?
O4 Ti1 O6 C61 -136.1(3) . . . . ?
Ti2 Ti1 O6 C61 -129.3(2) . . . . ?
Tm1 Ti1 O6 C61 155.20(19) . . . . ?
O3 Ti2 O7 C71 -118.9(6) . . . . ?
O8 Ti2 O7 C71 140.7(6) . . . . ?
O2 Ti2 O7 C71 39.4(6) . . . . ?
O4 Ti2 O7 C71 -37.8(6) . . . . ?
Ti1 Ti2 O7 C71 7.9(6) . . . . ?
Tm1 Ti2 O7 C71 -83.1(6) . . . . ?
Tm1 Ti2 O7 C71 149.7(5) 3_666 . . . ?
Ti1 O1 C11 C12 71.9(3) . . . . ?
Tm1 O1 C11 C12 -152.62(19) . . . . ?
Ti2 O2 C21 C22 157.9(3) . . . . ?
Ti1 O2 C21 C22 -67.3(5) . . . . ?
Ti2 O2 C21A C22A -156.3(4) . . . . ?
Ti1 O2 C21A C22A 60.8(10) . . . . ?
Ti2 O3 C31 C32 103.8(2) . . . . ?
Tm1 O3 C31 C32 -96.0(3) . . . . ?
Ti2 O4 C41 C42 -67.8(3) . . . . ?
Ti1 O4 C41 C42 -179.71(16) . . . . ?
Tm1 O4 C41 C42 61.3(3) . . . . ?
Ti1 O5 C51 C52 165.4(7) . . . . ?
Ti1 O6 C61 C62 -132.6(2) . . . . ?
Ti2 O7 C71 C72 -125.9(5) . . . . ?
Ti2 O8 C81 C82 79.3(3) . . . . ?
Tm1 O8 C81 C82 -120.6(2) 3_666 . . . ?
Tm1 O9 C91 C92 110.9(4) . . . . ?
Tm1 O9 C91A C92A -125.0(11) . . . . ?

####################################################################### 
# 
# 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_Ti4Sm2
_database_code_depnum_ccdc_archive 'CCDC 2283720'
loop_
_audit_author_name
_audit_author_address
'Andrew Bond'
;University of Cambridge
United Kingdom
;
_audit_update_record             
;
2023-07-22 deposited with the CCDC.	2023-09-15 downloaded from the CCDC.
;
#===============================================================================
_audit_creation_method           SHELXL-2018/3

#-------------------------------------------------------------------------------
# Inserted by local software: cifUpdate ver. 3.1  (Andrew D. Bond, March 2019)
#-------------------------------------------------------------------------------
_cambridge_user_name             'Rosa Mueller'
_cambridge_user_crsid            rm2055
_cambridge_supervisor_name       'Dominic Wright'
_cambridge_supervisor_crsid      dsw1000
_cambridge_crystallographer_name 'Andrew Bond'
_cambridge_crystallographer_crsid adb29
_cambridge_sample_id             RM55B
_cambridge_data_id               DW_B1_0414
#-------------------------------------------------------------------------------

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H92 Cl2 O20 Sm2 Ti4'
_chemical_formula_sum            'C36 H92 Cl2 O20 Sm2 Ti4'
_chemical_formula_weight         1408.29

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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   11.9374(4)
_cell_length_b                   18.9359(6)
_cell_length_c                   12.7346(4)
_cell_angle_alpha                90
_cell_angle_beta                 92.3995(12)
_cell_angle_gamma                90
_cell_volume                     2876.07(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9258
_cell_measurement_theta_min      5.83
_cell_measurement_theta_max      66.61

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_F_000             1428
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    20.963
_shelx_estimated_absorpt_T_min   0.134
_shelx_estimated_absorpt_T_max   0.285
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5249
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Incoatec I\mS Cu microsource'
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-III'
_diffrn_measurement_method       'ω and φ-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28827
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         5.497
_diffrn_reflns_theta_max         66.630
_diffrn_reflns_theta_full        66.630
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             5059
_reflns_number_gt                4831
_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.

#===============================================================================
INTENSITY STATISTICS FOR DATASET # 1  DW_B1_0414_0m.hkl
#===============================================================================
 Resolution   #Data #Theory %Complete Redundancy Mean I Mean I/s Rmerge  Rsigma
#-------------------------------------------------------------------------------
  Inf - 3.52      80     84     95.2     2.01     84.93   25.23  0.0297  0.0304
 3.52 - 2.32     182    182    100.0     3.64    142.59   34.61  0.0316  0.0231
 2.32 - 1.83     267    267    100.0     5.26    109.30   37.98  0.0286  0.0203
 1.83 - 1.59     268    268    100.0     6.69     97.36   41.46  0.0308  0.0184
 1.59 - 1.44     270    270    100.0     7.84     78.74   43.01  0.0317  0.0173
 1.44 - 1.34     250    250    100.0     7.99     59.06   40.09  0.0346  0.0187
 1.34 - 1.26     264    264    100.0     7.56     57.87   35.23  0.0336  0.0193
 1.26 - 1.19     288    289     99.7     7.38     51.60   35.59  0.0366  0.0204
 1.19 - 1.14     261    261    100.0     7.20     48.60   33.22  0.0364  0.0213
 1.14 - 1.10     234    234    100.0     6.64     50.17   31.09  0.0369  0.0221
 1.10 - 1.06     267    267    100.0     6.36     44.92   29.59  0.0414  0.0239
 1.06 - 1.03     255    255    100.0     6.63     39.27   29.81  0.0412  0.0238
 1.03 - 0.99     329    330     99.7     5.85     37.01   27.06  0.0448  0.0256
 0.99 - 0.97     227    230     98.7     5.16     35.74   27.01  0.0432  0.0266
 0.97 - 0.94     332    332    100.0     4.80     28.25   23.81  0.0441  0.0290
 0.94 - 0.92     227    228     99.6     4.69     31.10   24.27  0.0454  0.0282
 0.92 - 0.90     274    274    100.0     4.39     28.50   23.08  0.0514  0.0306
 0.90 - 0.88     302    303     99.7     4.17     25.41   23.42  0.0526  0.0312
 0.88 - 0.87     154    154    100.0     3.75     25.10   22.11  0.0529  0.0322
 0.87 - 0.85     326    327     99.7     3.19     24.63   20.43  0.0493  0.0351
 0.85 - 0.84     187    199     94.0     2.33     21.87   17.76  0.0482  0.0396
#-------------------------------------------------------------------------------
 0.94 - 0.84    1470   1485     99.0     3.79     26.21   21.97  0.0499  0.0323
  Inf - 0.84    5244   5268     99.5     5.59     51.26   30.02  0.0364  0.0231
#===============================================================================
;

_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL

_refine_special_details          ?

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0263P)²+2.4309P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5059
_refine_ls_number_parameters     329
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0227
_refine_ls_R_factor_gt           0.0212
_refine_ls_wR_factor_ref         0.0531
_refine_ls_wR_factor_gt          0.0521
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.083

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 0.37995(2) 0.54052(2) 0.41769(2) 0.01029(6) Uani 1 1 d . . . . .
Ti2 Ti 0.38973(4) 0.54505(2) 0.67792(3) 0.01167(10) Uani 1 1 d . . . . .
Ti1 Ti 0.49333(3) 0.66465(2) 0.57407(3) 0.01201(10) Uani 1 1 d . . . . .
Cl1 Cl 0.22566(6) 0.60988(4) 0.29678(6) 0.02977(16) Uani 1 1 d . . . . .
C11 C 0.4543(2) 0.71255(15) 0.3510(2) 0.0243(6) Uani 1 1 d . . . . .
H11A H 0.393277 0.742497 0.376764 0.029 Uiso 1 1 calc R U . . .
H11B H 0.429183 0.693172 0.281744 0.029 Uiso 1 1 calc R U . . .
C12 C 0.5571(3) 0.75708(18) 0.3382(3) 0.0416(8) Uani 1 1 d . . . . .
H12A H 0.579121 0.779021 0.405683 0.062 Uiso 1 1 calc R U . . .
H12B H 0.540792 0.793948 0.285811 0.062 Uiso 1 1 calc R U . . .
H12C H 0.618428 0.727285 0.314927 0.062 Uiso 1 1 calc R U . . .
C21 C 0.5262(11) 0.6467(5) 0.8213(8) 0.020(4) Uani 0.197(9) 1 d D U P A 1
H21A H 0.601770 0.625553 0.817504 0.024 Uiso 0.197(9) 1 calc R U P A 1
H21B H 0.487188 0.621614 0.877286 0.024 Uiso 0.197(9) 1 calc R U P A 1
C22 C 0.5401(3) 0.7224(2) 0.8537(3) 0.0498(10) Uani 0.197(9) 1 d D U P A 1
H22A H 0.594766 0.745323 0.809617 0.075 Uiso 0.197(9) 1 calc R U P A 1
H22B H 0.566684 0.724678 0.927504 0.075 Uiso 0.197(9) 1 calc R U P A 1
H22C H 0.467820 0.746786 0.845278 0.075 Uiso 0.197(9) 1 calc R U P A 1
C21A C 0.4462(3) 0.6771(2) 0.8151(3) 0.0279(12) Uani 0.803(9) 1 d D U P A 2
H21C H 0.424309 0.646040 0.873265 0.033 Uiso 0.803(9) 1 calc R U P A 2
H21D H 0.381198 0.707740 0.796307 0.033 Uiso 0.803(9) 1 calc R U P A 2
C22A C 0.5401(3) 0.7224(2) 0.8537(3) 0.0498(10) Uani 0.803(9) 1 d D U P A 2
H22D H 0.605026 0.692868 0.873272 0.075 Uiso 0.803(9) 1 calc R U P A 2
H22E H 0.517328 0.749047 0.915304 0.075 Uiso 0.803(9) 1 calc R U P A 2
H22F H 0.560048 0.755408 0.798227 0.075 Uiso 0.803(9) 1 calc R U P A 2
C31 C 0.2601(2) 0.41963(15) 0.6056(2) 0.0223(6) Uani 1 1 d . . . . .
H31A H 0.286411 0.405412 0.677262 0.027 Uiso 1 1 calc R U . . .
H31B H 0.280968 0.381833 0.556370 0.027 Uiso 1 1 calc R U . . .
C32 C 0.1347(3) 0.4277(2) 0.6021(3) 0.0423(8) Uani 1 1 d . . . . .
H32A H 0.113438 0.461719 0.655767 0.063 Uiso 1 1 calc R U . . .
H32B H 0.099969 0.381913 0.615855 0.063 Uiso 1 1 calc R U . . .
H32C H 0.109031 0.444725 0.532562 0.063 Uiso 1 1 calc R U . . .
C41 C 0.2291(2) 0.66576(15) 0.5797(2) 0.0222(6) Uani 1 1 d . . . . .
H41A H 0.228798 0.702300 0.524081 0.027 Uiso 1 1 calc R U . . .
H41B H 0.234202 0.690035 0.648578 0.027 Uiso 1 1 calc R U . . .
C42 C 0.1207(2) 0.62437(18) 0.5705(2) 0.0307(7) Uani 1 1 d . . . . .
H42A H 0.115399 0.600210 0.502464 0.046 Uiso 1 1 calc R U . . .
H42B H 0.057126 0.656710 0.576042 0.046 Uiso 1 1 calc R U . . .
H42C H 0.119392 0.589397 0.627200 0.046 Uiso 1 1 calc R U . . .
C51 C 0.3823(3) 0.81489(17) 0.6071(3) 0.0452(9) Uani 1 1 d . . . . .
H51A H 0.345085 0.809828 0.674750 0.054 Uiso 1 1 calc R U . . .
H51B H 0.323128 0.820292 0.550835 0.054 Uiso 1 1 calc R U . . .
C52 C 0.4536(4) 0.87899(19) 0.6108(4) 0.0598(12) Uani 1 1 d . . . . .
H52A H 0.509359 0.875090 0.669202 0.090 Uiso 1 1 calc R U . . .
H52B H 0.406669 0.920692 0.621077 0.090 Uiso 1 1 calc R U . . .
H52C H 0.491884 0.883581 0.544560 0.090 Uiso 1 1 calc R U . . .
C61 C 0.7105(2) 0.74156(15) 0.6244(2) 0.0264(6) Uani 1 1 d . . . . .
H61A H 0.736544 0.737968 0.699048 0.032 Uiso 1 1 calc R U . . .
H61B H 0.662242 0.783927 0.616697 0.032 Uiso 1 1 calc R U . . .
C62 C 0.8101(3) 0.74960(18) 0.5569(3) 0.0350(7) Uani 1 1 d . . . . .
H62A H 0.858529 0.708026 0.565255 0.052 Uiso 1 1 calc R U . . .
H62B H 0.852303 0.791974 0.578286 0.052 Uiso 1 1 calc R U . . .
H62C H 0.784355 0.754053 0.483083 0.052 Uiso 1 1 calc R U . . .
C71 C 0.2118(3) 0.5739(2) 0.8483(2) 0.0406(8) Uani 1 1 d . . . . .
H71A H 0.136850 0.554868 0.827422 0.049 Uiso 1 1 calc R U . . .
H71B H 0.208107 0.625963 0.842879 0.049 Uiso 1 1 calc R U . . .
C72 C 0.2398(4) 0.5538(2) 0.9596(3) 0.0483(9) Uani 1 1 d . . . . .
H72A H 0.239113 0.502268 0.966319 0.072 Uiso 1 1 calc R U . . .
H72B H 0.184284 0.574265 1.005330 0.072 Uiso 1 1 calc R U . . .
H72C H 0.314507 0.571779 0.980378 0.072 Uiso 1 1 calc R U . . .
C81 C 0.5185(3) 0.45745(17) 0.8381(2) 0.0303(7) Uani 1 1 d . . . . .
H81A H 0.513948 0.500086 0.882755 0.036 Uiso 1 1 calc R U . . .
H81B H 0.595825 0.438739 0.845997 0.036 Uiso 1 1 calc R U . . .
C82 C 0.4377(3) 0.4027(2) 0.8755(3) 0.0463(9) Uani 1 1 d . . . . .
H82A H 0.361222 0.421551 0.869913 0.070 Uiso 1 1 calc R U . . .
H82B H 0.456878 0.390793 0.948995 0.070 Uiso 1 1 calc R U . . .
H82C H 0.442464 0.360216 0.832055 0.070 Uiso 1 1 calc R U . . .
C91 C 0.1562(3) 0.4362(2) 0.2962(3) 0.0329(12) Uani 0.841(9) 1 d D U P B 1
H91A H 0.112452 0.479891 0.306806 0.040 Uiso 0.841(9) 1 calc R U P B 1
H91B H 0.116255 0.396628 0.328861 0.040 Uiso 0.841(9) 1 calc R U P B 1
C92 C 0.1638(6) 0.4226(4) 0.1804(4) 0.080(2) Uani 0.841(9) 1 d D U P B 1
H92A H 0.198829 0.463160 0.147095 0.120 Uiso 0.841(9) 1 calc R U P B 1
H92B H 0.088318 0.415405 0.148881 0.120 Uiso 0.841(9) 1 calc R U P B 1
H92C H 0.209108 0.380227 0.169689 0.120 Uiso 0.841(9) 1 calc R U P B 1
C91A C 0.2258(14) 0.4371(11) 0.2361(8) 0.033(6) Uani 0.159(9) 1 d D U P B 2
H91C H 0.255557 0.392671 0.207124 0.040 Uiso 0.159(9) 1 calc R U P B 2
H91D H 0.256416 0.476767 0.195617 0.040 Uiso 0.159(9) 1 calc R U P B 2
C92A C 0.0974(16) 0.437(2) 0.221(2) 0.079(11) Uani 0.159(9) 1 d D U P B 2
H92D H 0.067150 0.393873 0.251634 0.119 Uiso 0.159(9) 1 calc R U P B 2
H92E H 0.076548 0.438616 0.145755 0.119 Uiso 0.159(9) 1 calc R U P B 2
H92F H 0.066594 0.478337 0.255896 0.119 Uiso 0.159(9) 1 calc R U P B 2
O1 O 0.47506(14) 0.65579(9) 0.42278(13) 0.0162(4) Uani 1 1 d . . . . .
O2 O 0.46844(15) 0.63418(9) 0.72695(13) 0.0190(4) Uani 1 1 d D . . . .
O3 O 0.31411(14) 0.48390(9) 0.57780(13) 0.0160(4) Uani 1 1 d . . . . .
O4 O 0.32501(13) 0.62133(9) 0.57010(13) 0.0144(3) Uani 1 1 d . . . . .
O5 O 0.44506(16) 0.75344(10) 0.58819(15) 0.0238(4) Uani 1 1 d . . . . .
O6 O 0.64678(14) 0.68033(9) 0.59584(14) 0.0178(4) Uani 1 1 d . . . . .
O7 O 0.29029(15) 0.54847(9) 0.77893(14) 0.0191(4) Uani 1 1 d . . . . .
O8 O 0.49554(15) 0.47660(10) 0.73103(13) 0.0166(4) Uani 1 1 d . . . . .
O9 O 0.26467(16) 0.44365(10) 0.34612(15) 0.0238(4) Uani 1 1 d D . . . .
H9 H 0.308457 0.410836 0.374617 0.036 Uiso 1 1 d R U . B .
O10 O 0.50230(13) 0.56047(9) 0.56801(12) 0.0102(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 O10 2.3758(16) 3_666 ?
Sm1 O10 2.3887(15) . ?
Sm1 O9 2.4464(18) . ?
Sm1 O1 2.4599(17) . ?
Sm1 O3 2.4614(16) . ?
Sm1 O8 2.4772(17) 3_666 ?
Sm1 O4 2.5778(17) . ?
Sm1 Cl1 2.6927(6) . ?
Sm1 Ti2 3.3121(4) . ?
Sm1 Ti1 3.3312(4) . ?
Sm1 Ti2 3.4565(4) 3_666 ?
Sm1 Sm1 3.8027(2) 3_666 ?
Ti2 O7 1.7877(18) . ?
Ti2 O8 1.9135(18) . ?
Ti2 O3 1.9195(17) . ?
Ti2 O10 2.0018(16) . ?
Ti2 O2 2.0180(17) . ?
Ti2 O4 2.1165(17) . ?
Ti2 Ti1 2.9231(6) . ?
Ti1 O5 1.7888(18) . ?
Ti1 O6 1.8649(18) . ?
Ti1 O1 1.9371(17) . ?
Ti1 O10 1.9774(17) . ?
Ti1 O2 2.0639(17) . ?
Ti1 O4 2.1690(17) . ?
C11 O1 1.426(3) . ?
C11 C12 1.503(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C21 O2 1.381(8) . ?
C21 C22 1.499(8) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C21A O2 1.420(3) . ?
C21A C22A 1.479(4) . ?
C21A H21C 0.9900 . ?
C21A H21D 0.9900 . ?
C22A H22D 0.9800 . ?
C22A H22E 0.9800 . ?
C22A H22F 0.9800 . ?
C31 O3 1.429(3) . ?
C31 C32 1.504(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C41 O4 1.430(3) . ?
C41 C42 1.513(4) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C51 O5 1.410(4) . ?
C51 C52 1.482(5) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C61 O6 1.426(3) . ?
C61 C62 1.504(4) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C71 O7 1.400(3) . ?
C71 C72 1.492(5) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C81 O8 1.427(3) . ?
C81 C82 1.506(5) . ?
C81 H81A 0.9900 . ?
C81 H81B 0.9900 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C91 O9 1.425(4) . ?
C91 C92 1.504(6) . ?
C91 H91A 0.9900 . ?
C91 H91B 0.9900 . ?
C92 H92A 0.9800 . ?
C92 H92B 0.9800 . ?
C92 H92C 0.9800 . ?
C91A O9 1.463(9) . ?
C91A C92A 1.536(10) . ?
C91A H91C 0.9900 . ?
C91A H91D 0.9900 . ?
C92A H92D 0.9800 . ?
C92A H92E 0.9800 . ?
C92A H92F 0.9800 . ?
O9 H9 0.8804 . ?

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
O10 Sm1 O10 74.09(6) 3_666 . ?
O10 Sm1 O9 75.33(6) 3_666 . ?
O10 Sm1 O9 137.11(6) . . ?
O10 Sm1 O1 116.19(6) 3_666 . ?
O10 Sm1 O1 64.70(6) . . ?
O9 Sm1 O1 157.97(6) . . ?
O10 Sm1 O3 78.13(6) 3_666 . ?
O10 Sm1 O3 67.09(5) . . ?
O9 Sm1 O3 77.75(6) . . ?
O1 Sm1 O3 121.85(6) . . ?
O10 Sm1 O8 65.25(6) 3_666 3_666 ?
O10 Sm1 O8 105.49(6) . 3_666 ?
O9 Sm1 O8 87.89(6) . 3_666 ?
O1 Sm1 O8 81.10(6) . 3_666 ?
O3 Sm1 O8 143.03(6) . 3_666 ?
O10 Sm1 O4 126.05(5) 3_666 . ?
O10 Sm1 O4 57.93(5) . . ?
O9 Sm1 O4 124.66(6) . . ?
O1 Sm1 O4 65.49(5) . . ?
O3 Sm1 O4 62.27(6) . . ?
O8 Sm1 O4 146.41(6) 3_666 . ?
O10 Sm1 Cl1 145.56(4) 3_666 . ?
O10 Sm1 Cl1 139.62(4) . . ?
O9 Sm1 Cl1 77.99(5) . . ?
O1 Sm1 Cl1 83.47(4) . . ?
O3 Sm1 Cl1 116.85(4) . . ?
O8 Sm1 Cl1 92.55(4) 3_666 . ?
O4 Sm1 Cl1 87.22(4) . . ?
O10 Sm1 Ti2 87.03(4) 3_666 . ?
O10 Sm1 Ti2 36.81(4) . . ?
O9 Sm1 Ti2 112.82(5) . . ?
O1 Sm1 Ti2 87.35(4) . . ?
O3 Sm1 Ti2 35.07(4) . . ?
O8 Sm1 Ti2 140.46(4) 3_666 . ?
O4 Sm1 Ti2 39.71(4) . . ?
Cl1 Sm1 Ti2 123.650(19) . . ?
O10 Sm1 Ti1 107.33(4) 3_666 . ?
O10 Sm1 Ti1 35.89(4) . . ?
O9 Sm1 Ti1 163.74(5) . . ?
O1 Sm1 Ti1 35.18(4) . . ?
O3 Sm1 Ti1 87.02(4) . . ?
O8 Sm1 Ti1 107.92(4) 3_666 . ?
O4 Sm1 Ti1 40.61(4) . . ?
Cl1 Sm1 Ti1 104.406(17) . . ?
Ti2 Sm1 Ti1 52.207(10) . . ?
O10 Sm1 Ti2 34.20(4) 3_666 3_666 ?
O10 Sm1 Ti2 83.56(4) . 3_666 ?
O9 Sm1 Ti2 87.74(5) . 3_666 ?
O1 Sm1 Ti2 92.99(4) . 3_666 ?
O3 Sm1 Ti2 111.96(4) . 3_666 ?
O8 Sm1 Ti2 32.63(4) 3_666 3_666 ?
O4 Sm1 Ti2 140.78(4) . 3_666 ?
Cl1 Sm1 Ti2 124.217(18) . 3_666 ?
Ti2 Sm1 Ti2 111.675(9) . 3_666 ?
Ti1 Sm1 Ti2 103.421(11) . 3_666 ?
O10 Sm1 Sm1 37.16(4) 3_666 3_666 ?
O10 Sm1 Sm1 36.93(4) . 3_666 ?
O9 Sm1 Sm1 107.58(4) . 3_666 ?
O1 Sm1 Sm1 90.41(4) . 3_666 ?
O3 Sm1 Sm1 68.10(4) . 3_666 ?
O8 Sm1 Sm1 84.62(4) 3_666 3_666 ?
O4 Sm1 Sm1 91.96(4) . 3_666 ?
Cl1 Sm1 Sm1 173.596(16) . 3_666 ?
Ti2 Sm1 Sm1 57.638(8) . 3_666 ?
Ti1 Sm1 Sm1 71.169(8) . 3_666 ?
Ti2 Sm1 Sm1 54.037(8) 3_666 3_666 ?
O7 Ti2 O8 102.63(8) . . ?
O7 Ti2 O3 101.06(8) . . ?
O8 Ti2 O3 96.39(8) . . ?
O7 Ti2 O10 169.48(8) . . ?
O8 Ti2 O10 83.88(7) . . ?
O3 Ti2 O10 86.24(7) . . ?
O7 Ti2 O2 93.53(8) . . ?
O8 Ti2 O2 99.51(8) . . ?
O3 Ti2 O2 155.50(7) . . ?
O10 Ti2 O2 77.11(7) . . ?
O7 Ti2 O4 101.93(8) . . ?
O8 Ti2 O4 155.40(7) . . ?
O3 Ti2 O4 80.33(7) . . ?
O10 Ti2 O4 71.60(6) . . ?
O2 Ti2 O4 77.44(7) . . ?
O7 Ti2 Ti1 127.14(6) . . ?
O8 Ti2 Ti1 113.53(6) . . ?
O3 Ti2 Ti1 111.28(5) . . ?
O10 Ti2 Ti1 42.40(5) . . ?
O2 Ti2 Ti1 44.90(5) . . ?
O4 Ti2 Ti1 47.75(5) . . ?
O7 Ti2 Sm1 136.40(6) . . ?
O8 Ti2 Sm1 109.34(5) . . ?
O3 Ti2 Sm1 47.46(5) . . ?
O10 Ti2 Sm1 45.64(4) . . ?
O2 Ti2 Sm1 109.13(5) . . ?
O4 Ti2 Sm1 51.10(5) . . ?
Ti1 Ti2 Sm1 64.232(11) . . ?
O7 Ti2 Sm1 146.34(6) . 3_666 ?
O8 Ti2 Sm1 44.27(5) . 3_666 ?
O3 Ti2 Sm1 80.92(5) . 3_666 ?
O10 Ti2 Sm1 41.84(5) . 3_666 ?
O2 Ti2 Sm1 97.71(5) . 3_666 ?
O4 Ti2 Sm1 111.44(5) . 3_666 ?
Ti1 Ti2 Sm1 81.141(13) . 3_666 ?
Sm1 Ti2 Sm1 68.325(9) . 3_666 ?
O5 Ti1 O6 98.86(8) . . ?
O5 Ti1 O1 99.09(8) . . ?
O6 Ti1 O1 103.34(8) . . ?
O5 Ti1 O10 163.70(8) . . ?
O6 Ti1 O10 96.33(7) . . ?
O1 Ti1 O10 83.04(7) . . ?
O5 Ti1 O2 96.21(8) . . ?
O6 Ti1 O2 94.79(8) . . ?
O1 Ti1 O2 154.06(7) . . ?
O10 Ti1 O2 76.59(7) . . ?
O5 Ti1 O4 93.20(8) . . ?
O6 Ti1 O4 165.21(7) . . ?
O1 Ti1 O4 83.02(7) . . ?
O10 Ti1 O4 70.93(6) . . ?
O2 Ti1 O4 75.31(7) . . ?
O5 Ti1 Ti2 122.58(6) . . ?
O6 Ti1 Ti2 119.18(6) . . ?
O1 Ti1 Ti2 110.53(5) . . ?
O10 Ti1 Ti2 43.05(5) . . ?
O2 Ti1 Ti2 43.64(5) . . ?
O4 Ti1 Ti2 46.24(5) . . ?
O5 Ti1 Sm1 126.78(6) . . ?
O6 Ti1 Sm1 124.97(6) . . ?
O1 Ti1 Sm1 47.02(5) . . ?
O10 Ti1 Sm1 45.09(4) . . ?
O2 Ti1 Sm1 107.20(5) . . ?
O4 Ti1 Sm1 50.68(4) . . ?
Ti2 Ti1 Sm1 63.561(11) . . ?
O1 C11 C12 111.8(2) . . ?
O1 C11 H11A 109.3 . . ?
C12 C11 H11A 109.3 . . ?
O1 C11 H11B 109.3 . . ?
C12 C11 H11B 109.3 . . ?
H11A C11 H11B 107.9 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O2 C21 C22 116.7(7) . . ?
O2 C21 H21A 108.1 . . ?
C22 C21 H21A 108.1 . . ?
O2 C21 H21B 108.1 . . ?
C22 C21 H21B 108.1 . . ?
H21A C21 H21B 107.3 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O2 C21A C22A 115.5(3) . . ?
O2 C21A H21C 108.4 . . ?
C22A C21A H21C 108.4 . . ?
O2 C21A H21D 108.4 . . ?
C22A C21A H21D 108.4 . . ?
H21C C21A H21D 107.5 . . ?
C21A C22A H22D 109.5 . . ?
C21A C22A H22E 109.5 . . ?
H22D C22A H22E 109.5 . . ?
C21A C22A H22F 109.5 . . ?
H22D C22A H22F 109.5 . . ?
H22E C22A H22F 109.5 . . ?
O3 C31 C32 111.4(2) . . ?
O3 C31 H31A 109.3 . . ?
C32 C31 H31A 109.3 . . ?
O3 C31 H31B 109.3 . . ?
C32 C31 H31B 109.3 . . ?
H31A C31 H31B 108.0 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O4 C41 C42 112.0(2) . . ?
O4 C41 H41A 109.2 . . ?
C42 C41 H41A 109.2 . . ?
O4 C41 H41B 109.2 . . ?
C42 C41 H41B 109.2 . . ?
H41A C41 H41B 107.9 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O5 C51 C52 111.9(3) . . ?
O5 C51 H51A 109.2 . . ?
C52 C51 H51A 109.2 . . ?
O5 C51 H51B 109.2 . . ?
C52 C51 H51B 109.2 . . ?
H51A C51 H51B 107.9 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
O6 C61 C62 111.3(2) . . ?
O6 C61 H61A 109.4 . . ?
C62 C61 H61A 109.4 . . ?
O6 C61 H61B 109.4 . . ?
C62 C61 H61B 109.4 . . ?
H61A C61 H61B 108.0 . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
O7 C71 C72 112.5(3) . . ?
O7 C71 H71A 109.1 . . ?
C72 C71 H71A 109.1 . . ?
O7 C71 H71B 109.1 . . ?
C72 C71 H71B 109.1 . . ?
H71A C71 H71B 107.8 . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
O8 C81 C82 112.2(3) . . ?
O8 C81 H81A 109.2 . . ?
C82 C81 H81A 109.2 . . ?
O8 C81 H81B 109.2 . . ?
C82 C81 H81B 109.2 . . ?
H81A C81 H81B 107.9 . . ?
C81 C82 H82A 109.5 . . ?
C81 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
C81 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
O9 C91 C92 111.3(4) . . ?
O9 C91 H91A 109.4 . . ?
C92 C91 H91A 109.4 . . ?
O9 C91 H91B 109.4 . . ?
C92 C91 H91B 109.4 . . ?
H91A C91 H91B 108.0 . . ?
C91 C92 H92A 109.5 . . ?
C91 C92 H92B 109.5 . . ?
H92A C92 H92B 109.5 . . ?
C91 C92 H92C 109.5 . . ?
H92A C92 H92C 109.5 . . ?
H92B C92 H92C 109.5 . . ?
O9 C91A C92A 113.3(10) . . ?
O9 C91A H91C 108.9 . . ?
C92A C91A H91C 108.9 . . ?
O9 C91A H91D 108.9 . . ?
C92A C91A H91D 108.9 . . ?
H91C C91A H91D 107.7 . . ?
C91A C92A H92D 109.5 . . ?
C91A C92A H92E 109.5 . . ?
H92D C92A H92E 109.5 . . ?
C91A C92A H92F 109.5 . . ?
H92D C92A H92F 109.5 . . ?
H92E C92A H92F 109.5 . . ?
C11 O1 Ti1 125.57(16) . . ?
C11 O1 Sm1 125.75(15) . . ?
Ti1 O1 Sm1 97.80(7) . . ?
C21 O2 Ti2 128.5(4) . . ?
C21A O2 Ti2 128.57(18) . . ?
C21 O2 Ti1 133.3(5) . . ?
C21A O2 Ti1 128.6(2) . . ?
Ti2 O2 Ti1 91.46(7) . . ?
C31 O3 Ti2 123.63(15) . . ?
C31 O3 Sm1 137.67(15) . . ?
Ti2 O3 Sm1 97.46(7) . . ?
C41 O4 Ti2 128.16(15) . . ?
C41 O4 Ti1 121.31(15) . . ?
Ti2 O4 Ti1 86.01(6) . . ?
C41 O4 Sm1 130.04(15) . . ?
Ti2 O4 Sm1 89.19(6) . . ?
Ti1 O4 Sm1 88.70(6) . . ?
C51 O5 Ti1 165.6(2) . . ?
C61 O6 Ti1 132.66(17) . . ?
C71 O7 Ti2 161.6(2) . . ?
C81 O8 Ti2 127.41(17) . . ?
C81 O8 Sm1 126.89(17) . 3_666 ?
Ti2 O8 Sm1 103.10(7) . 3_666 ?
C91 O9 Sm1 136.6(2) . . ?
C91A O9 Sm1 124.9(8) . . ?
C91 O9 H9 128.8 . . ?
C91A O9 H9 119.6 . . ?
Sm1 O9 H9 93.5 . . ?
Ti1 O10 Ti2 94.54(7) . . ?
Ti1 O10 Sm1 146.39(8) . 3_666 ?
Ti2 O10 Sm1 103.97(7) . 3_666 ?
Ti1 O10 Sm1 99.02(6) . . ?
Ti2 O10 Sm1 97.55(6) . . ?
Sm1 O10 Sm1 105.91(6) 3_666 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C12 C11 O1 Ti1 73.4(3) . . . . ?
C12 C11 O1 Sm1 -150.5(2) . . . . ?
C22 C21 O2 Ti2 -158.3(5) . . . . ?
C22 C21 O2 Ti1 59.0(13) . . . . ?
C22A C21A O2 Ti2 158.4(3) . . . . ?
C22A C21A O2 Ti1 -68.8(4) . . . . ?
C32 C31 O3 Ti2 104.6(2) . . . . ?
C32 C31 O3 Sm1 -91.3(3) . . . . ?
C42 C41 O4 Ti2 -70.2(3) . . . . ?
C42 C41 O4 Ti1 177.79(17) . . . . ?
C42 C41 O4 Sm1 59.3(3) . . . . ?
C52 C51 O5 Ti1 166.7(7) . . . . ?
O6 Ti1 O5 C51 -153.2(9) . . . . ?
O1 Ti1 O5 C51 101.7(9) . . . . ?
O10 Ti1 O5 C51 5.3(11) . . . . ?
O2 Ti1 O5 C51 -57.3(9) . . . . ?
O4 Ti1 O5 C51 18.2(9) . . . . ?
Ti2 Ti1 O5 C51 -19.9(9) . . . . ?
Sm1 Ti1 O5 C51 59.6(9) . . . . ?
C62 C61 O6 Ti1 -134.5(2) . . . . ?
O5 Ti1 O6 C61 5.0(2) . . . . ?
O1 Ti1 O6 C61 106.6(2) . . . . ?
O10 Ti1 O6 C61 -169.1(2) . . . . ?
O2 Ti1 O6 C61 -92.1(2) . . . . ?
O4 Ti1 O6 C61 -139.3(3) . . . . ?
Ti2 Ti1 O6 C61 -130.3(2) . . . . ?
Sm1 Ti1 O6 C61 153.1(2) . . . . ?
C72 C71 O7 Ti2 -128.6(6) . . . . ?
O8 Ti2 O7 C71 144.8(6) . . . . ?
O3 Ti2 O7 C71 -116.0(6) . . . . ?
O10 Ti2 O7 C71 17.4(9) . . . . ?
O2 Ti2 O7 C71 44.2(7) . . . . ?
O4 Ti2 O7 C71 -33.7(7) . . . . ?
Ti1 Ti2 O7 C71 11.8(7) . . . . ?
Sm1 Ti2 O7 C71 -78.5(7) . . . . ?
Sm1 Ti2 O7 C71 153.8(6) 3_666 . . . ?
C82 C81 O8 Ti2 84.3(3) . . . . ?
C82 C81 O8 Sm1 -117.1(3) . . . 3_666 ?
C92 C91 O9 Sm1 105.8(4) . . . . ?
C92A C91A O9 Sm1 -119(2) . . . . ?

####################################################################### 
# 
# 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_Ti4Er2
_database_code_depnum_ccdc_archive 'CCDC 2283719'
loop_
_audit_author_name
_audit_author_address
'Andrew Bond'
;University of Cambridge
United Kingdom
;
_audit_update_record             
;
2023-07-22 deposited with the CCDC.	2023-09-15 downloaded from the CCDC.
;
#===============================================================================
_audit_creation_method           SHELXL-2019/1

#-------------------------------------------------------------------------------
# Inserted by local software: cifUpdate ver. 3.1  (Andrew D. Bond, March 2019)
#-------------------------------------------------------------------------------
_cambridge_user_name             'Rosa Mueller'
_cambridge_user_crsid            rm2055
_cambridge_supervisor_name       'Dominic Wright'
_cambridge_supervisor_crsid      dsw1000
_cambridge_crystallographer_name 'Andrew Bond'
_cambridge_crystallographer_crsid adb29
_cambridge_sample_id             RM130
_cambridge_data_id               DW_B1_0463
#-------------------------------------------------------------------------------

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H92 Cl2 Er2 O20 Ti4'
_chemical_formula_sum            'C36 H92 Cl2 Er2 O20 Ti4'
_chemical_formula_weight         1442.11

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'
Cl Cl 0.3639 0.7018 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   11.9203(6)
_cell_length_b                   18.7662(10)
_cell_length_c                   12.7290(7)
_cell_angle_alpha                90
_cell_angle_beta                 92.705(3)
_cell_angle_gamma                90
_cell_volume                     2844.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    4389
_cell_measurement_theta_min      4.97
_cell_measurement_theta_max      66.32

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_F_000             1452
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    11.170
_shelx_estimated_absorpt_T_min   0.268
_shelx_estimated_absorpt_T_max   0.554
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4494
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Incoatec I\mS Cu microsource'
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-III'
_diffrn_measurement_method       'ω and φ-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            40698
_diffrn_reflns_av_unetI/netI     0.0709
_diffrn_reflns_av_R_equivalents  0.1390
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         4.200
_diffrn_reflns_theta_max         66.704
_diffrn_reflns_theta_full        66.704
_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 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5024
_reflns_number_gt                3493
_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.

#===============================================================================
INTENSITY STATISTICS FOR DATASET # 1  DW_B1_0463_0m.hkl
#===============================================================================
 Resolution   #Data #Theory %Complete Redundancy Mean I Mean I/s Rmerge  Rsigma
#-------------------------------------------------------------------------------
  Inf - 3.55      78     80     97.5     4.81     71.20   15.07  0.0482  0.0638
 3.55 - 2.32     183    183    100.0     5.27     89.71   15.79  0.0476  0.0445
 2.32 - 1.83     266    266    100.0     6.52     60.37   15.73  0.0590  0.0463
 1.83 - 1.59     263    263    100.0     8.84     46.28   16.42  0.0751  0.0432
 1.59 - 1.44     267    267    100.0    11.27     36.57   16.97  0.0947  0.0429
 1.44 - 1.34     253    253    100.0    11.72     25.54   14.75  0.1131  0.0485
 1.34 - 1.26     253    253    100.0    11.19     21.52   11.67  0.1324  0.0562
 1.26 - 1.19     288    288    100.0    10.79     19.29   11.00  0.1463  0.0628
 1.19 - 1.14     260    260    100.0    10.42     14.23    9.25  0.1835  0.0780
 1.14 - 1.10     230    230    100.0    10.28     16.52    9.95  0.1698  0.0723
 1.10 - 1.06     259    259    100.0     9.51     12.19    7.57  0.2380  0.0982
 1.06 - 1.03     260    260    100.0     9.23     12.45    7.92  0.2399  0.0942
 1.03 - 0.99     324    325     99.7     8.21     10.34    6.74  0.2474  0.1092
 0.99 - 0.97     219    220     99.5     6.63     10.11    6.45  0.2117  0.1192
 0.97 - 0.94     324    325     99.7     6.54      6.99    5.20  0.2647  0.1509
 0.94 - 0.92     236    237     99.6     6.22      6.73    5.03  0.2657  0.1529
 0.92 - 0.90     264    265     99.6     5.83      6.10    4.79  0.2744  0.1656
 0.90 - 0.88     306    306    100.0     5.64      5.21    4.38  0.2991  0.1795
 0.88 - 0.87     162    163     99.4     5.31      4.61    4.30  0.3288  0.2001
 0.87 - 0.85     301    302     99.7     4.92      4.85    4.47  0.2941  0.1850
 0.85 - 0.84     206    209     98.6     3.95      3.82    3.23  0.3320  0.2652
#-------------------------------------------------------------------------------
 0.94 - 0.84    1475   1482     99.5     5.35      5.28    4.41  0.2905  0.1829
  Inf - 0.84    5202   5214     99.8     7.95     20.56    9.12  0.1281  0.0684
#===============================================================================
;

_computing_data_collection       'APEX4 (Bruker, 2021)'
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL

_refine_special_details          ?

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0729P)²+7.0551P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5024
_refine_ls_number_parameters     309
_refine_ls_number_restraints     144
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0532
_refine_ls_wR_factor_ref         0.1478
_refine_ls_wR_factor_gt          0.1252
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         2.495
_refine_diff_density_min         -1.245
_refine_diff_density_rms         0.168

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 0.38328(4) 0.54168(2) 0.42100(3) 0.03143(16) Uani 1 1 d . . . . .
Ti2 Ti 0.39245(11) 0.54427(7) 0.67529(10) 0.0314(3) Uani 1 1 d . . . . .
Ti1 Ti 0.49749(12) 0.66435(7) 0.57323(11) 0.0328(3) Uani 1 1 d . . . . .
Cl1 Cl 0.23168(17) 0.61277(11) 0.30777(18) 0.0482(5) Uani 1 1 d . . . . .
O1 O 0.4785(4) 0.6546(3) 0.4231(4) 0.0348(12) Uani 1 1 d . . . . .
O2 O 0.4719(5) 0.6332(3) 0.7246(4) 0.0400(13) Uani 1 1 d D . . . .
O3 O 0.3136(4) 0.4858(3) 0.5732(4) 0.0374(12) Uani 1 1 d . . . . .
O4 O 0.3291(4) 0.6218(3) 0.5689(4) 0.0351(12) Uani 1 1 d . . . . .
O5 O 0.4518(5) 0.7550(3) 0.5859(5) 0.0472(14) Uani 1 1 d . . . . .
O6 O 0.6495(5) 0.6798(3) 0.5963(4) 0.0383(13) Uani 1 1 d . . . . .
H6 H 0.674712 0.638943 0.614221 0.057 Uiso 1 1 d R U . . .
O7 O 0.2950(5) 0.5466(3) 0.7780(4) 0.0402(13) Uani 1 1 d . . . . .
O8 O 0.4983(4) 0.4735(3) 0.7234(4) 0.0372(12) Uani 1 1 d . . . . .
O9 O 0.2711(4) 0.4493(3) 0.3467(4) 0.0415(13) Uani 1 1 d D . . . .
O10 O 0.5043(4) 0.5589(2) 0.5661(4) 0.0301(11) Uani 1 1 d . . . . .
C11 C 0.4593(7) 0.7117(4) 0.3506(7) 0.045(2) Uani 1 1 d . U . . .
H11A H 0.398107 0.742258 0.375012 0.054 Uiso 1 1 calc R U . . .
H11B H 0.434910 0.691961 0.281038 0.054 Uiso 1 1 calc R U . . .
C12 C 0.5650(9) 0.7570(5) 0.3390(8) 0.065(3) Uani 1 1 d . U . . .
H12A H 0.548652 0.795524 0.288709 0.097 Uiso 1 1 calc R U . . .
H12B H 0.588548 0.777286 0.407479 0.097 Uiso 1 1 calc R U . . .
H12C H 0.625331 0.727016 0.313555 0.097 Uiso 1 1 calc R U . . .
C21 C 0.4488(9) 0.6752(6) 0.8148(8) 0.053(4) Uani 0.74(2) 1 d D U P A 1
H21A H 0.426457 0.642672 0.871448 0.064 Uiso 0.74(2) 1 calc R U P A 1
H21B H 0.383620 0.706198 0.796490 0.064 Uiso 0.74(2) 1 calc R U P A 1
C22 C 0.5441(10) 0.7216(6) 0.8578(8) 0.079(3) Uani 0.74(2) 1 d D U P A 1
H22A H 0.519676 0.747953 0.919157 0.118 Uiso 0.74(2) 1 calc R U P A 1
H22B H 0.608591 0.691532 0.878706 0.118 Uiso 0.74(2) 1 calc R U P A 1
H22C H 0.565631 0.755241 0.803532 0.118 Uiso 0.74(2) 1 calc R U P A 1
C21A C 0.535(3) 0.6440(7) 0.8213(16) 0.045(10) Uani 0.26(2) 1 d D U P A 2
H21C H 0.612221 0.625303 0.813434 0.054 Uiso 0.26(2) 1 calc R U P A 2
H21D H 0.500787 0.615661 0.876869 0.054 Uiso 0.26(2) 1 calc R U P A 2
C22A C 0.5441(10) 0.7216(6) 0.8578(8) 0.079(3) Uani 0.26(2) 1 d D U P A 2
H22D H 0.588779 0.724007 0.924353 0.118 Uiso 0.26(2) 1 calc R U P A 2
H22E H 0.580313 0.750004 0.804502 0.118 Uiso 0.26(2) 1 calc R U P A 2
H22F H 0.468647 0.740341 0.868070 0.118 Uiso 0.26(2) 1 calc R U P A 2
C31 C 0.2565(7) 0.4217(4) 0.5990(7) 0.044(2) Uani 1 1 d . U . . .
H31A H 0.285165 0.405254 0.669094 0.053 Uiso 1 1 calc R U . . .
H31B H 0.274462 0.384496 0.547246 0.053 Uiso 1 1 calc R U . . .
C32 C 0.1315(8) 0.4295(6) 0.6002(10) 0.067(3) Uani 1 1 d . U . . .
H32A H 0.098016 0.383745 0.618301 0.101 Uiso 1 1 calc R U . . .
H32B H 0.112782 0.465396 0.652499 0.101 Uiso 1 1 calc R U . . .
H32C H 0.102066 0.444613 0.530505 0.101 Uiso 1 1 calc R U . . .
C41 C 0.2335(7) 0.6678(5) 0.5797(8) 0.048(2) Uani 1 1 d . U . . .
H41A H 0.231883 0.703935 0.522960 0.058 Uiso 1 1 calc R U . . .
H41B H 0.241458 0.693230 0.647829 0.058 Uiso 1 1 calc R U . . .
C42 C 0.1252(7) 0.6273(5) 0.5746(8) 0.054(2) Uani 1 1 d . U . . .
H42A H 0.062520 0.660394 0.582282 0.081 Uiso 1 1 calc R U . . .
H42B H 0.116283 0.602811 0.506745 0.081 Uiso 1 1 calc R U . . .
H42C H 0.125855 0.592109 0.631576 0.081 Uiso 1 1 calc R U . . .
C51 C 0.3920(10) 0.8174(6) 0.6037(10) 0.077(3) Uani 1 1 d . U . . .
H51A H 0.355268 0.813347 0.671566 0.093 Uiso 1 1 calc R U . . .
H51B H 0.332365 0.823035 0.547483 0.093 Uiso 1 1 calc R U . . .
C52 C 0.4640(12) 0.8805(5) 0.6059(12) 0.098(4) Uani 1 1 d . U . . .
H52A H 0.418684 0.922945 0.618565 0.147 Uiso 1 1 calc R U . . .
H52B H 0.522313 0.875615 0.662395 0.147 Uiso 1 1 calc R U . . .
H52C H 0.499412 0.885302 0.538324 0.147 Uiso 1 1 calc R U . . .
C61 C 0.7164(8) 0.7394(5) 0.6276(8) 0.050(2) Uani 1 1 d . U . . .
H61A H 0.744041 0.733063 0.701615 0.060 Uiso 1 1 calc R U . . .
H61B H 0.669573 0.782978 0.623816 0.060 Uiso 1 1 calc R U . . .
C62 C 0.8140(8) 0.7487(5) 0.5601(8) 0.056(2) Uani 1 1 d . U . . .
H62A H 0.857940 0.790206 0.584087 0.083 Uiso 1 1 calc R U . . .
H62B H 0.861366 0.705990 0.564729 0.083 Uiso 1 1 calc R U . . .
H62C H 0.786928 0.755885 0.486962 0.083 Uiso 1 1 calc R U . . .
C71 C 0.2203(10) 0.5726(6) 0.8486(8) 0.070(3) Uani 1 1 d . U . . .
H71A H 0.144157 0.554734 0.828409 0.084 Uiso 1 1 calc R U . . .
H71B H 0.218482 0.625205 0.843682 0.084 Uiso 1 1 calc R U . . .
C72 C 0.2481(12) 0.5523(6) 0.9584(9) 0.081(4) Uani 1 1 d . U . . .
H72A H 0.192065 0.572300 1.003985 0.121 Uiso 1 1 calc R U . . .
H72B H 0.248186 0.500209 0.964579 0.121 Uiso 1 1 calc R U . . .
H72C H 0.322593 0.570758 0.979868 0.121 Uiso 1 1 calc R U . . .
C81 C 0.5210(9) 0.4518(5) 0.8301(8) 0.057(2) Uani 1 1 d . U . . .
H81A H 0.524052 0.494592 0.875602 0.069 Uiso 1 1 calc R U . . .
H81B H 0.595775 0.428708 0.835847 0.069 Uiso 1 1 calc R U . . .
C82 C 0.4359(10) 0.4015(6) 0.8696(9) 0.073(3) Uani 1 1 d . U . . .
H82A H 0.456201 0.388752 0.942700 0.110 Uiso 1 1 calc R U . . .
H82B H 0.361889 0.424326 0.865918 0.110 Uiso 1 1 calc R U . . .
H82C H 0.433676 0.358383 0.826128 0.110 Uiso 1 1 calc R U . . .
C91 C 0.1576(8) 0.4431(6) 0.3024(9) 0.061(4) Uani 0.79(2) 1 d D U P B 1
H91A H 0.116639 0.487393 0.318244 0.073 Uiso 0.79(2) 1 calc R U P B 1
H91B H 0.120210 0.403471 0.338367 0.073 Uiso 0.79(2) 1 calc R U P B 1
C92 C 0.1463(13) 0.4301(9) 0.1851(9) 0.133(6) Uani 0.79(2) 1 d D U P B 1
H92A H 0.066596 0.426701 0.163005 0.199 Uiso 0.79(2) 1 calc R U P B 1
H92B H 0.180697 0.469666 0.147995 0.199 Uiso 0.79(2) 1 calc R U P B 1
H92C H 0.184278 0.385508 0.168176 0.199 Uiso 0.79(2) 1 calc R U P B 1
C91A C 0.2642(15) 0.441(3) 0.2348(10) 0.069(17) Uani 0.21(2) 1 d D U P B 2
H91C H 0.310504 0.398993 0.216713 0.082 Uiso 0.21(2) 1 calc R U P B 2
H91D H 0.297699 0.483144 0.202575 0.082 Uiso 0.21(2) 1 calc R U P B 2
C92A C 0.1463(13) 0.4301(9) 0.1851(9) 0.133(6) Uani 0.21(2) 1 d D U P B 2
H92D H 0.150662 0.424688 0.108784 0.199 Uiso 0.21(2) 1 calc R U P B 2
H92E H 0.112702 0.387228 0.214324 0.199 Uiso 0.21(2) 1 calc R U P B 2
H92F H 0.099862 0.471612 0.200147 0.199 Uiso 0.21(2) 1 calc R U P B 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
Er1 O10 2.312(5) . ?
Er1 O10 2.316(5) 3_666 ?
Er1 O9 2.360(5) . ?
Er1 O3 2.386(5) . ?
Er1 O8 2.386(6) 3_666 ?
Er1 O1 2.403(5) . ?
Er1 O4 2.518(5) . ?
Er1 Cl1 2.6225(18) . ?
Er1 Ti2 3.2339(14) . ?
Er1 Ti1 3.2648(14) . ?
Er1 Ti2 3.4000(14) 3_666 ?
Er1 Er1 3.7021(8) 3_666 ?
Ti2 O7 1.790(6) . ?
Ti2 O3 1.912(5) . ?
Ti2 O8 1.912(5) . ?
Ti2 O10 1.990(5) . ?
Ti2 O2 2.005(5) . ?
Ti2 O4 2.104(5) . ?
Ti2 Ti1 2.9133(19) . ?
Ti1 O5 1.795(5) . ?
Ti1 O6 1.845(5) . ?
Ti1 O1 1.922(5) . ?
Ti1 O10 1.982(5) . ?
Ti1 O2 2.051(5) . ?
Ti1 O4 2.158(5) . ?
Ti1 H6 2.2042 . ?
O1 C11 1.426(9) . ?
O2 C21A 1.428(10) . ?
O2 C21 1.430(8) . ?
O3 C31 1.428(9) . ?
O4 C41 1.441(9) . ?
O5 C51 1.395(11) . ?
O6 C61 1.420(9) . ?
O6 H6 0.8500 . ?
O7 C71 1.384(11) . ?
O8 C81 1.432(10) . ?
O9 C91A 1.433(10) . ?
O9 C91 1.445(8) . ?
C11 C12 1.532(13) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C21 C22 1.513(8) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C21A C22A 1.531(10) . ?
C21A H21C 0.9900 . ?
C21A H21D 0.9900 . ?
C22A H22D 0.9800 . ?
C22A H22E 0.9800 . ?
C22A H22F 0.9800 . ?
C31 C32 1.498(12) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C41 C42 1.498(12) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C51 C52 1.463(16) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C61 C62 1.489(13) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C71 C72 1.471(15) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C81 C82 1.490(14) . ?
C81 H81A 0.9900 . ?
C81 H81B 0.9900 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C91 C92 1.513(9) . ?
C91 H91A 0.9900 . ?
C91 H91B 0.9900 . ?
C92 H92A 0.9800 . ?
C92 H92B 0.9800 . ?
C92 H92C 0.9800 . ?
C91A C92A 1.526(10) . ?
C91A H91C 0.9900 . ?
C91A H91D 0.9900 . ?
C92A H92D 0.9800 . ?
C92A H92E 0.9800 . ?
C92A H92F 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
O10 Er1 O10 73.77(19) . 3_666 ?
O10 Er1 O9 138.04(17) . . ?
O10 Er1 O9 75.22(17) 3_666 . ?
O10 Er1 O3 68.95(17) . . ?
O10 Er1 O3 78.84(18) 3_666 . ?
O9 Er1 O3 77.90(18) . . ?
O10 Er1 O8 105.21(18) . 3_666 ?
O10 Er1 O8 66.19(17) 3_666 3_666 ?
O9 Er1 O8 87.04(19) . 3_666 ?
O3 Er1 O8 144.48(17) . 3_666 ?
O10 Er1 O1 65.85(16) . . ?
O10 Er1 O1 116.52(17) 3_666 . ?
O9 Er1 O1 155.59(18) . . ?
O3 Er1 O1 124.07(18) . . ?
O8 Er1 O1 79.50(18) 3_666 . ?
O10 Er1 O4 59.44(16) . . ?
O10 Er1 O4 127.00(16) 3_666 . ?
O9 Er1 O4 125.30(19) . . ?
O3 Er1 O4 62.86(18) . . ?
O8 Er1 O4 146.00(17) 3_666 . ?
O1 Er1 O4 66.58(17) . . ?
O10 Er1 Cl1 139.08(12) . . ?
O10 Er1 Cl1 146.61(13) 3_666 . ?
O9 Er1 Cl1 77.91(13) . . ?
O3 Er1 Cl1 114.37(14) . . ?
O8 Er1 Cl1 93.14(13) 3_666 . ?
O1 Er1 Cl1 82.56(12) . . ?
O4 Er1 Cl1 84.98(12) . . ?
O10 Er1 Ti2 37.64(13) . . ?
O10 Er1 Ti2 87.08(13) 3_666 . ?
O9 Er1 Ti2 113.82(14) . . ?
O3 Er1 Ti2 35.95(12) . . ?
O8 Er1 Ti2 141.20(12) 3_666 . ?
O1 Er1 Ti2 88.95(13) . . ?
O4 Er1 Ti2 40.57(11) . . ?
Cl1 Er1 Ti2 122.16(6) . . ?
O10 Er1 Ti1 36.88(11) . . ?
O10 Er1 Ti1 108.00(12) 3_666 . ?
O9 Er1 Ti1 165.55(15) . . ?
O3 Er1 Ti1 88.80(12) . . ?
O8 Er1 Ti1 107.22(13) 3_666 . ?
O1 Er1 Ti1 35.72(13) . . ?
O4 Er1 Ti1 41.36(12) . . ?
Cl1 Er1 Ti1 102.98(5) . . ?
Ti2 Er1 Ti1 53.26(3) . . ?
O10 Er1 Ti2 83.27(13) . 3_666 ?
O10 Er1 Ti2 34.61(13) 3_666 3_666 ?
O9 Er1 Ti2 87.00(14) . 3_666 ?
O3 Er1 Ti2 113.20(13) . 3_666 ?
O8 Er1 Ti2 33.08(12) 3_666 3_666 ?
O1 Er1 Ti2 92.49(13) . 3_666 ?
O4 Er1 Ti2 141.89(11) . 3_666 ?
Cl1 Er1 Ti2 125.20(6) . 3_666 ?
Ti2 Er1 Ti2 112.21(3) . 3_666 ?
Ti1 Er1 Ti2 103.62(4) . 3_666 ?
O10 Er1 Er1 36.92(11) . 3_666 ?
O10 Er1 Er1 36.84(12) 3_666 3_666 ?
O9 Er1 Er1 107.74(12) . 3_666 ?
O3 Er1 Er1 69.80(12) . 3_666 ?
O8 Er1 Er1 84.91(12) 3_666 3_666 ?
O1 Er1 Er1 91.37(12) . 3_666 ?
O4 Er1 Er1 93.38(11) . 3_666 ?
Cl1 Er1 Er1 173.87(5) . 3_666 ?
Ti2 Er1 Er1 58.24(3) . 3_666 ?
Ti1 Er1 Er1 72.17(3) . 3_666 ?
Ti2 Er1 Er1 53.97(2) 3_666 3_666 ?
O7 Ti2 O3 101.3(2) . . ?
O7 Ti2 O8 103.0(2) . . ?
O3 Ti2 O8 96.6(2) . . ?
O7 Ti2 O10 170.4(2) . . ?
O3 Ti2 O10 85.9(2) . . ?
O8 Ti2 O10 82.3(2) . . ?
O7 Ti2 O2 93.7(2) . . ?
O3 Ti2 O2 154.1(2) . . ?
O8 Ti2 O2 100.5(2) . . ?
O10 Ti2 O2 77.4(2) . . ?
O7 Ti2 O4 103.1(2) . . ?
O3 Ti2 O4 79.0(2) . . ?
O8 Ti2 O4 153.9(2) . . ?
O10 Ti2 O4 71.7(2) . . ?
O2 Ti2 O4 77.0(2) . . ?
O7 Ti2 Ti1 127.88(18) . . ?
O3 Ti2 Ti1 110.39(17) . . ?
O8 Ti2 Ti1 112.88(17) . . ?
O10 Ti2 Ti1 42.72(14) . . ?
O2 Ti2 Ti1 44.71(15) . . ?
O4 Ti2 Ti1 47.67(14) . . ?
O7 Ti2 Er1 137.66(18) . . ?
O3 Ti2 Er1 47.10(16) . . ?
O8 Ti2 Er1 107.49(17) . . ?
O10 Ti2 Er1 45.18(14) . . ?
O2 Ti2 Er1 108.62(15) . . ?
O4 Ti2 Er1 51.10(15) . . ?
Ti1 Ti2 Er1 63.91(4) . . ?
O7 Ti2 Er1 145.43(18) . 3_666 ?
O3 Ti2 Er1 81.52(17) . 3_666 ?
O8 Ti2 Er1 42.93(17) . 3_666 ?
O10 Ti2 Er1 41.38(13) . 3_666 ?
O2 Ti2 Er1 98.04(16) . 3_666 ?
O4 Ti2 Er1 111.14(15) . 3_666 ?
Ti1 Ti2 Er1 81.05(4) . 3_666 ?
Er1 Ti2 Er1 67.79(3) . 3_666 ?
O5 Ti1 O6 97.9(2) . . ?
O5 Ti1 O1 99.1(3) . . ?
O6 Ti1 O1 104.0(2) . . ?
O5 Ti1 O10 164.3(3) . . ?
O6 Ti1 O10 97.0(2) . . ?
O1 Ti1 O10 82.1(2) . . ?
O5 Ti1 O2 97.3(3) . . ?
O6 Ti1 O2 94.8(2) . . ?
O1 Ti1 O2 153.0(2) . . ?
O10 Ti1 O2 76.5(2) . . ?
O5 Ti1 O4 93.8(2) . . ?
O6 Ti1 O4 165.3(2) . . ?
O1 Ti1 O4 82.7(2) . . ?
O10 Ti1 O4 70.7(2) . . ?
O2 Ti1 O4 74.9(2) . . ?
O5 Ti1 Ti2 123.6(2) . . ?
O6 Ti1 Ti2 119.33(17) . . ?
O1 Ti1 Ti2 109.68(16) . . ?
O10 Ti1 Ti2 42.94(15) . . ?
O2 Ti1 Ti2 43.45(14) . . ?
O4 Ti1 Ti2 46.11(14) . . ?
O5 Ti1 Er1 126.96(19) . . ?
O6 Ti1 Er1 125.74(17) . . ?
O1 Ti1 Er1 46.89(15) . . ?
O10 Ti1 Er1 44.43(14) . . ?
O2 Ti1 Er1 106.27(15) . . ?
O4 Ti1 Er1 50.43(14) . . ?
Ti2 Ti1 Er1 62.83(4) . . ?
O5 Ti1 H6 118.4 . . ?
O6 Ti1 H6 22.0 . . ?
O1 Ti1 H6 106.3 . . ?
O10 Ti1 H6 75.8 . . ?
O2 Ti1 H6 84.2 . . ?
O4 Ti1 H6 143.7 . . ?
Ti2 Ti1 H6 98.9 . . ?
Er1 Ti1 H6 110.9 . . ?
C11 O1 Ti1 125.5(5) . . ?
C11 O1 Er1 126.4(4) . . ?
Ti1 O1 Er1 97.4(2) . . ?
C21A O2 Ti2 127.7(8) . . ?
C21 O2 Ti2 127.2(5) . . ?
C21A O2 Ti1 132.3(13) . . ?
C21 O2 Ti1 129.8(6) . . ?
Ti2 O2 Ti1 91.84(19) . . ?
C31 O3 Ti2 123.5(5) . . ?
C31 O3 Er1 138.1(5) . . ?
Ti2 O3 Er1 97.0(2) . . ?
C41 O4 Ti2 127.9(5) . . ?
C41 O4 Ti1 121.0(5) . . ?
Ti2 O4 Ti1 86.22(18) . . ?
C41 O4 Er1 131.4(5) . . ?
Ti2 O4 Er1 88.33(18) . . ?
Ti1 O4 Er1 88.21(18) . . ?
C51 O5 Ti1 165.8(7) . . ?
C61 O6 Ti1 134.6(5) . . ?
C61 O6 H6 116.6 . . ?
Ti1 O6 H6 103.5 . . ?
C71 O7 Ti2 160.6(6) . . ?
C81 O8 Ti2 126.4(5) . . ?
C81 O8 Er1 127.2(5) . 3_666 ?
Ti2 O8 Er1 104.0(2) . 3_666 ?
C91A O9 Er1 119.2(17) . . ?
C91 O9 Er1 135.9(6) . . ?
Ti1 O10 Ti2 94.3(2) . . ?
Ti1 O10 Er1 98.69(19) . . ?
Ti2 O10 Er1 97.2(2) . . ?
Ti1 O10 Er1 146.6(3) . 3_666 ?
Ti2 O10 Er1 104.0(2) . 3_666 ?
Er1 O10 Er1 106.23(19) . 3_666 ?
O1 C11 C12 111.8(7) . . ?
O1 C11 H11A 109.3 . . ?
C12 C11 H11A 109.3 . . ?
O1 C11 H11B 109.3 . . ?
C12 C11 H11B 109.3 . . ?
H11A C11 H11B 107.9 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O2 C21 C22 116.0(7) . . ?
O2 C21 H21A 108.3 . . ?
C22 C21 H21A 108.3 . . ?
O2 C21 H21B 108.3 . . ?
C22 C21 H21B 108.3 . . ?
H21A C21 H21B 107.4 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O2 C21A C22A 115.0(9) . . ?
O2 C21A H21C 108.5 . . ?
C22A C21A H21C 108.5 . . ?
O2 C21A H21D 108.5 . . ?
C22A C21A H21D 108.5 . . ?
H21C C21A H21D 107.5 . . ?
C21A C22A H22D 109.5 . . ?
C21A C22A H22E 109.5 . . ?
H22D C22A H22E 109.5 . . ?
C21A C22A H22F 109.5 . . ?
H22D C22A H22F 109.5 . . ?
H22E C22A H22F 109.5 . . ?
O3 C31 C32 113.9(7) . . ?
O3 C31 H31A 108.8 . . ?
C32 C31 H31A 108.8 . . ?
O3 C31 H31B 108.8 . . ?
C32 C31 H31B 108.8 . . ?
H31A C31 H31B 107.7 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O4 C41 C42 112.1(7) . . ?
O4 C41 H41A 109.2 . . ?
C42 C41 H41A 109.2 . . ?
O4 C41 H41B 109.2 . . ?
C42 C41 H41B 109.2 . . ?
H41A C41 H41B 107.9 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O5 C51 C52 112.3(10) . . ?
O5 C51 H51A 109.1 . . ?
C52 C51 H51A 109.1 . . ?
O5 C51 H51B 109.1 . . ?
C52 C51 H51B 109.1 . . ?
H51A C51 H51B 107.9 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
O6 C61 C62 111.9(8) . . ?
O6 C61 H61A 109.2 . . ?
C62 C61 H61A 109.2 . . ?
O6 C61 H61B 109.2 . . ?
C62 C61 H61B 109.2 . . ?
H61A C61 H61B 107.9 . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
O7 C71 C72 113.8(9) . . ?
O7 C71 H71A 108.8 . . ?
C72 C71 H71A 108.8 . . ?
O7 C71 H71B 108.8 . . ?
C72 C71 H71B 108.8 . . ?
H71A C71 H71B 107.7 . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
O8 C81 C82 113.5(9) . . ?
O8 C81 H81A 108.9 . . ?
C82 C81 H81A 108.9 . . ?
O8 C81 H81B 108.9 . . ?
C82 C81 H81B 108.9 . . ?
H81A C81 H81B 107.7 . . ?
C81 C82 H82A 109.5 . . ?
C81 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
C81 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
O9 C91 C92 115.9(8) . . ?
O9 C91 H91A 108.3 . . ?
C92 C91 H91A 108.3 . . ?
O9 C91 H91B 108.3 . . ?
C92 C91 H91B 108.3 . . ?
H91A C91 H91B 107.4 . . ?
C91 C92 H92A 109.5 . . ?
C91 C92 H92B 109.5 . . ?
H92A C92 H92B 109.5 . . ?
C91 C92 H92C 109.5 . . ?
H92A C92 H92C 109.5 . . ?
H92B C92 H92C 109.5 . . ?
O9 C91A C92A 115.8(10) . . ?
O9 C91A H91C 108.3 . . ?
C92A C91A H91C 108.3 . . ?
O9 C91A H91D 108.3 . . ?
C92A C91A H91D 108.3 . . ?
H91C C91A H91D 107.4 . . ?
C91A C92A H92D 109.5 . . ?
C91A C92A H92E 109.5 . . ?
H92D C92A H92E 109.5 . . ?
C91A C92A H92F 109.5 . . ?
H92D C92A H92F 109.5 . . ?
H92E C92A H92F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O6 Ti1 O5 C51 -152(3) . . . . ?
O1 Ti1 O5 C51 102(3) . . . . ?
O10 Ti1 O5 C51 9(3) . . . . ?
O2 Ti1 O5 C51 -56(3) . . . . ?
O4 Ti1 O5 C51 19(3) . . . . ?
Ti2 Ti1 O5 C51 -19(3) . . . . ?
Er1 Ti1 O5 C51 61(3) . . . . ?
O5 Ti1 O6 C61 7.3(8) . . . . ?
O1 Ti1 O6 C61 108.8(8) . . . . ?
O10 Ti1 O6 C61 -167.7(7) . . . . ?
O2 Ti1 O6 C61 -90.7(8) . . . . ?
O4 Ti1 O6 C61 -135.2(9) . . . . ?
Ti2 Ti1 O6 C61 -128.7(7) . . . . ?
Er1 Ti1 O6 C61 155.3(7) . . . . ?
O3 Ti2 O7 C71 -117.0(19) . . . . ?
O8 Ti2 O7 C71 143.4(19) . . . . ?
O2 Ti2 O7 C71 41.7(19) . . . . ?
O4 Ti2 O7 C71 -35.8(19) . . . . ?
Ti1 Ti2 O7 C71 10(2) . . . . ?
Er1 Ti2 O7 C71 -81.3(19) . . . . ?
Er1 Ti2 O7 C71 151.6(18) 3_666 . . . ?
Ti1 O1 C11 C12 72.2(9) . . . . ?
Er1 O1 C11 C12 -151.6(6) . . . . ?
Ti2 O2 C21 C22 157.8(8) . . . . ?
Ti1 O2 C21 C22 -69.1(13) . . . . ?
Ti2 O2 C21A C22A -155.5(12) . . . . ?
Ti1 O2 C21A C22A 65(3) . . . . ?
Ti2 O3 C31 C32 102.9(8) . . . . ?
Er1 O3 C31 C32 -94.5(9) . . . . ?
Ti2 O4 C41 C42 -68.2(9) . . . . ?
Ti1 O4 C41 C42 -179.9(6) . . . . ?
Er1 O4 C41 C42 61.4(10) . . . . ?
Ti1 O5 C51 C52 166(2) . . . . ?
Ti1 O6 C61 C62 -133.2(7) . . . . ?
Ti2 O7 C71 C72 -126.9(17) . . . . ?
Ti2 O8 C81 C82 79.1(10) . . . . ?
Er1 O8 C81 C82 -121.3(8) 3_666 . . . ?
Er1 O9 C91 C92 110.8(11) . . . . ?
Er1 O9 C91A C92A -134(3) . . . . ?

####################################################################### 
# 
# 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_Ti4Tb2
_database_code_depnum_ccdc_archive 'CCDC 2283722'
loop_
_audit_author_name
_audit_author_address
'Andrew Bond'
;University of Cambridge
United Kingdom
;
_audit_update_record             
;
2023-07-22 deposited with the CCDC.	2023-09-15 downloaded from the CCDC.
;
#===============================================================================
_audit_creation_method           SHELXL-2019/1

#-------------------------------------------------------------------------------
# Inserted by local software: cifUpdate ver. 3.1  (Andrew D. Bond, March 2019)
#-------------------------------------------------------------------------------
_cambridge_user_name             'Rosa Mueller'
_cambridge_user_crsid            rm2055
_cambridge_supervisor_name       'Dominic Wright'
_cambridge_supervisor_crsid      dsw1000
_cambridge_crystallographer_name 'Andrew Bond'
_cambridge_crystallographer_crsid adb29
_cambridge_sample_id             RM93B
_cambridge_data_id               DW_B1_0430
#-------------------------------------------------------------------------------

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H92 Cl2 O20 Tb2 Ti4'
_chemical_formula_sum            'C36 H92 Cl2 O20 Tb2 Ti4'
_chemical_formula_weight         1425.43

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'
Cl Cl 0.3639 0.7018 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   11.9091(5)
_cell_length_b                   18.8221(8)
_cell_length_c                   12.7415(6)
_cell_angle_alpha                90
_cell_angle_beta                 92.592(2)
_cell_angle_gamma                90
_cell_volume                     2853.1(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9757
_cell_measurement_theta_min      5.50
_cell_measurement_theta_max      66.57

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_F_000             1440
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    17.865
_shelx_estimated_absorpt_T_min   0.223
_shelx_estimated_absorpt_T_max   0.268
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5315
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Incoatec I\mS Cu microsource'
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-III'
_diffrn_measurement_method       'ω and φ-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            41828
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         5.501
_diffrn_reflns_theta_max         66.640
_diffrn_reflns_theta_full        66.640
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             5005
_reflns_number_gt                4830
_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.

#===============================================================================
INTENSITY STATISTICS FOR DATASET # 1  DW_B1_0430_0m.hkl
#===============================================================================
 Resolution   #Data #Theory %Complete Redundancy Mean I Mean I/s Rmerge  Rsigma
#-------------------------------------------------------------------------------
  Inf - 3.47      78     85     91.8     4.28     58.39   31.17  0.0470  0.0332
 3.47 - 2.30     183    191     95.8     5.05    104.53   32.28  0.0381  0.0337
 2.30 - 1.81     267    271     98.5     5.53     92.30   31.95  0.0365  0.0286
 1.81 - 1.58     259    261     99.2     8.52     79.48   39.09  0.0391  0.0224
 1.58 - 1.44     250    250    100.0    11.82     70.08   47.94  0.0390  0.0168
 1.44 - 1.33     278    282     98.6    12.19     48.98   45.39  0.0425  0.0173
 1.33 - 1.25     272    274     99.3    11.69     48.43   39.27  0.0411  0.0175
 1.25 - 1.19     241    243     99.2    11.51     46.49   41.87  0.0437  0.0179
 1.19 - 1.14     262    263     99.6    11.25     37.18   38.12  0.0463  0.0188
 1.14 - 1.09     299    299    100.0    10.93     41.66   38.73  0.0439  0.0185
 1.09 - 1.05     280    283     98.9     9.04     34.96   31.63  0.0539  0.0239
 1.05 - 1.02     238    238    100.0     9.71     36.14   35.68  0.0485  0.0203
 1.02 - 0.99     255    255    100.0     8.57     29.84   31.57  0.0476  0.0222
 0.99 - 0.97     221    221    100.0     7.05     28.67   30.04  0.0431  0.0243
 0.97 - 0.94     325    325    100.0     6.66     24.80   28.95  0.0423  0.0247
 0.94 - 0.92     241    241    100.0     6.38     22.51   26.78  0.0460  0.0258
 0.92 - 0.90     271    271    100.0     5.72     22.51   25.35  0.0532  0.0277
 0.90 - 0.88     296    296    100.0     5.89     20.12   27.38  0.0456  0.0268
 0.88 - 0.87     166    166    100.0     5.86     17.73   26.86  0.0481  0.0266
 0.87 - 0.85     312    312    100.0     5.42     19.60   26.45  0.0492  0.0271
 0.85 - 0.84     195    200     97.5     4.32     16.39   21.77  0.0496  0.0317
#-------------------------------------------------------------------------------
 0.94 - 0.84    1481   1486     99.7     5.63     20.08   25.92  0.0486  0.0274
  Inf - 0.84    5189   5227     99.3     8.19     41.77   33.49  0.0433  0.0234
#===============================================================================
;

_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL

_refine_special_details          ?

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0255P)²+2.2973P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5005
_refine_ls_number_parameters     329
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_gt           0.0212
_refine_ls_wR_factor_ref         0.0526
_refine_ls_wR_factor_gt          0.0520
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.107
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.082

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 0.38139(2) 0.54080(2) 0.41960(2) 0.01073(6) Uani 1 1 d . . . . .
Ti2 Ti 0.39093(3) 0.54436(2) 0.67672(3) 0.01162(9) Uani 1 1 d . . . . .
Ti1 Ti 0.49450(3) 0.66486(2) 0.57340(3) 0.01185(9) Uani 1 1 d . . . . .
Cl1 Cl 0.22806(5) 0.61096(3) 0.30305(5) 0.02680(13) Uani 1 1 d . . . . .
C11 C 0.4556(2) 0.71240(13) 0.35085(19) 0.0236(5) Uani 1 1 d . . . . .
H11A H 0.393759 0.742191 0.375851 0.028 Uiso 1 1 calc R U . . .
H11B H 0.431562 0.693002 0.281192 0.028 Uiso 1 1 calc R U . . .
C12 C 0.5585(3) 0.75774(16) 0.3399(2) 0.0394(7) Uani 1 1 d . . . . .
H12A H 0.577532 0.781385 0.406862 0.059 Uiso 1 1 calc R U . . .
H12B H 0.543528 0.793598 0.285251 0.059 Uiso 1 1 calc R U . . .
H12C H 0.621561 0.727769 0.320336 0.059 Uiso 1 1 calc R U . . .
C21 C 0.5263(8) 0.6476(4) 0.8185(6) 0.025(3) Uani 0.285(9) 1 d D U P A 1
H21A H 0.602054 0.626437 0.814299 0.030 Uiso 0.285(9) 1 calc R U P A 1
H21B H 0.487866 0.621739 0.874193 0.030 Uiso 0.285(9) 1 calc R U P A 1
C22 C 0.5412(3) 0.72214(18) 0.8539(2) 0.0520(9) Uani 0.285(9) 1 d D U P A 1
H22A H 0.595488 0.745951 0.810216 0.078 Uiso 0.285(9) 1 calc R U P A 1
H22B H 0.569124 0.722780 0.927414 0.078 Uiso 0.285(9) 1 calc R U P A 1
H22C H 0.468926 0.746985 0.847390 0.078 Uiso 0.285(9) 1 calc R U P A 1
C21A C 0.4478(3) 0.67714(19) 0.8148(3) 0.0250(11) Uani 0.715(9) 1 d D U P A 2
H21C H 0.426027 0.645560 0.872584 0.030 Uiso 0.715(9) 1 calc R U P A 2
H21D H 0.382587 0.708134 0.796618 0.030 Uiso 0.715(9) 1 calc R U P A 2
C22A C 0.5412(3) 0.72214(18) 0.8539(2) 0.0520(9) Uani 0.715(9) 1 d D U P A 2
H22D H 0.606626 0.692325 0.872346 0.078 Uiso 0.715(9) 1 calc R U P A 2
H22E H 0.518854 0.748126 0.916220 0.078 Uiso 0.715(9) 1 calc R U P A 2
H22F H 0.560596 0.756017 0.799155 0.078 Uiso 0.715(9) 1 calc R U P A 2
C31 C 0.2590(2) 0.41953(12) 0.60326(19) 0.0215(5) Uani 1 1 d . . . . .
H31A H 0.286495 0.404571 0.674347 0.026 Uiso 1 1 calc R U . . .
H31B H 0.278367 0.381750 0.553134 0.026 Uiso 1 1 calc R U . . .
C32 C 0.1335(2) 0.42841(18) 0.6017(3) 0.0428(7) Uani 1 1 d . . . . .
H32A H 0.113763 0.462434 0.656045 0.064 Uiso 1 1 calc R U . . .
H32B H 0.098243 0.382478 0.615207 0.064 Uiso 1 1 calc R U . . .
H32C H 0.106712 0.446121 0.532657 0.064 Uiso 1 1 calc R U . . .
C41 C 0.23072(18) 0.66661(13) 0.5793(2) 0.0212(5) Uani 1 1 d . . . . .
H41A H 0.229467 0.702841 0.522945 0.025 Uiso 1 1 calc R U . . .
H41B H 0.237359 0.691676 0.647626 0.025 Uiso 1 1 calc R U . . .
C42 C 0.12205(18) 0.62528(16) 0.5726(2) 0.0290(6) Uani 1 1 d . . . . .
H42A H 0.116388 0.599101 0.506127 0.043 Uiso 1 1 calc R U . . .
H42B H 0.058548 0.658183 0.576079 0.043 Uiso 1 1 calc R U . . .
H42C H 0.120658 0.591724 0.631370 0.043 Uiso 1 1 calc R U . . .
C51 C 0.3847(3) 0.81643(15) 0.6056(3) 0.0451(8) Uani 1 1 d . . . . .
H51A H 0.347726 0.811514 0.673316 0.054 Uiso 1 1 calc R U . . .
H51B H 0.325153 0.821988 0.549457 0.054 Uiso 1 1 calc R U . . .
C52 C 0.4569(3) 0.88091(16) 0.6091(4) 0.0595(11) Uani 1 1 d . . . . .
H52A H 0.514916 0.876039 0.665681 0.089 Uiso 1 1 calc R U . . .
H52B H 0.410661 0.922794 0.622168 0.089 Uiso 1 1 calc R U . . .
H52C H 0.492632 0.886385 0.541821 0.089 Uiso 1 1 calc R U . . .
C61 C 0.7125(2) 0.74145(13) 0.6261(2) 0.0254(5) Uani 1 1 d . . . . .
H61A H 0.739498 0.737030 0.700449 0.030 Uiso 1 1 calc R U . . .
H61B H 0.664302 0.784237 0.619738 0.030 Uiso 1 1 calc R U . . .
C62 C 0.8112(2) 0.75005(15) 0.5582(2) 0.0343(6) Uani 1 1 d . . . . .
H62A H 0.859479 0.707980 0.565081 0.051 Uiso 1 1 calc R U . . .
H62B H 0.854156 0.792280 0.580440 0.051 Uiso 1 1 calc R U . . .
H62C H 0.784540 0.755503 0.484769 0.051 Uiso 1 1 calc R U . . .
C71 C 0.2163(3) 0.57458(18) 0.8488(2) 0.0412(7) Uani 1 1 d . . . . .
H71A H 0.139716 0.557406 0.828665 0.049 Uiso 1 1 calc R U . . .
H71B H 0.215725 0.627065 0.843843 0.049 Uiso 1 1 calc R U . . .
C72 C 0.2447(3) 0.55354(19) 0.9596(2) 0.0474(8) Uani 1 1 d . . . . .
H72A H 0.240285 0.501749 0.966074 0.071 Uiso 1 1 calc R U . . .
H72B H 0.191454 0.575686 1.006047 0.071 Uiso 1 1 calc R U . . .
H72C H 0.321139 0.569361 0.979502 0.071 Uiso 1 1 calc R U . . .
C81 C 0.5211(2) 0.45479(14) 0.8350(2) 0.0289(6) Uani 1 1 d . . . . .
H81A H 0.519991 0.497578 0.880157 0.035 Uiso 1 1 calc R U . . .
H81B H 0.597361 0.433929 0.841915 0.035 Uiso 1 1 calc R U . . .
C82 C 0.4370(3) 0.40163(17) 0.8727(2) 0.0447(8) Uani 1 1 d . . . . .
H82A H 0.361264 0.421994 0.865779 0.067 Uiso 1 1 calc R U . . .
H82B H 0.454955 0.390049 0.946522 0.067 Uiso 1 1 calc R U . . .
H82C H 0.440096 0.358340 0.830184 0.067 Uiso 1 1 calc R U . . .
C91 C 0.1566(2) 0.43873(18) 0.2995(3) 0.0307(10) Uani 0.837(8) 1 d D U P B 1
H91A H 0.112940 0.482285 0.312931 0.037 Uiso 0.837(8) 1 calc R U P B 1
H91B H 0.118190 0.398195 0.331970 0.037 Uiso 0.837(8) 1 calc R U P B 1
C92 C 0.1602(5) 0.4270(4) 0.1841(3) 0.0724(18) Uani 0.837(8) 1 d D U P B 1
H92A H 0.195750 0.467871 0.151514 0.109 Uiso 0.837(8) 1 calc R U P B 1
H92B H 0.083434 0.421346 0.154114 0.109 Uiso 0.837(8) 1 calc R U P B 1
H92C H 0.203617 0.383956 0.170694 0.109 Uiso 0.837(8) 1 calc R U P B 1
C91A C 0.2300(11) 0.4393(8) 0.2358(7) 0.025(5) Uani 0.163(8) 1 d D U P B 2
H91C H 0.263510 0.396136 0.205765 0.030 Uiso 0.163(8) 1 calc R U P B 2
H91D H 0.256682 0.480891 0.196440 0.030 Uiso 0.163(8) 1 calc R U P B 2
C92A C 0.1011(13) 0.4348(15) 0.2228(17) 0.059(8) Uani 0.163(8) 1 d D U P B 2
H92D H 0.076825 0.386002 0.236281 0.088 Uiso 0.163(8) 1 calc R U P B 2
H92E H 0.077090 0.448433 0.151028 0.088 Uiso 0.163(8) 1 calc R U P B 2
H92F H 0.067225 0.467038 0.272820 0.088 Uiso 0.163(8) 1 calc R U P B 2
O1 O 0.47607(12) 0.65519(8) 0.42250(12) 0.0155(3) Uani 1 1 d . . . . .
O2 O 0.46904(13) 0.63429(8) 0.72587(12) 0.0193(3) Uani 1 1 d D . . . .
O3 O 0.31355(12) 0.48424(8) 0.57570(12) 0.0154(3) Uani 1 1 d . . . . .
O4 O 0.32654(12) 0.62143(8) 0.56921(12) 0.0145(3) Uani 1 1 d . . . . .
O5 O 0.44697(14) 0.75443(8) 0.58677(14) 0.0232(4) Uani 1 1 d . . . . .
O6 O 0.64773(13) 0.68013(8) 0.59665(12) 0.0175(3) Uani 1 1 d . . . . .
O7 O 0.29202(13) 0.54735(8) 0.77826(13) 0.0186(3) Uani 1 1 d . . . . .
O8 O 0.49769(13) 0.47515(8) 0.72793(12) 0.0165(3) Uani 1 1 d . . . . .
O9 O 0.26747(13) 0.44584(9) 0.34655(14) 0.0226(4) Uani 1 1 d D . . . .
H9 H 0.311265 0.413031 0.375054 0.034 Uiso 1 1 d R U . B .
O10 O 0.50346(11) 0.55982(8) 0.56690(11) 0.0103(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O10 2.3401(14) 3_666 ?
Tb1 O10 2.3489(13) . ?
Tb1 O9 2.4056(15) . ?
Tb1 O3 2.4265(15) . ?
Tb1 O1 2.4299(15) . ?
Tb1 O8 2.4377(15) 3_666 ?
Tb1 O4 2.5448(15) . ?
Tb1 Cl1 2.6529(5) . ?
Tb1 Ti2 3.2736(4) . ?
Tb1 Ti1 3.2968(4) . ?
Tb1 Ti2 3.4247(4) 3_666 ?
Tb1 Tb1 3.7437(2) 3_666 ?
Ti2 O7 1.7895(16) . ?
Ti2 O8 1.9143(16) . ?
Ti2 O3 1.9181(15) . ?
Ti2 O10 2.0020(15) . ?
Ti2 O2 2.0173(15) . ?
Ti2 O4 2.1150(15) . ?
Ti2 Ti1 2.9232(5) . ?
Ti1 O5 1.7890(16) . ?
Ti1 O6 1.8578(15) . ?
Ti1 O1 1.9338(15) . ?
Ti1 O10 1.9819(15) . ?
Ti1 O2 2.0617(16) . ?
Ti1 O4 2.1593(15) . ?
C11 O1 1.426(3) . ?
C11 C12 1.505(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C21 O2 1.360(6) . ?
C21 C22 1.481(7) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C21A O2 1.423(3) . ?
C21A C22A 1.468(4) . ?
C21A H21C 0.9900 . ?
C21A H21D 0.9900 . ?
C22A H22D 0.9800 . ?
C22A H22E 0.9800 . ?
C22A H22F 0.9800 . ?
C31 O3 1.432(3) . ?
C31 C32 1.503(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C41 O4 1.434(3) . ?
C41 C42 1.509(3) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C51 O5 1.409(3) . ?
C51 C52 1.487(4) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C61 O6 1.429(3) . ?
C61 C62 1.500(4) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C71 O7 1.400(3) . ?
C71 C72 1.490(4) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C81 O8 1.433(3) . ?
C81 C82 1.509(4) . ?
C81 H81A 0.9900 . ?
C81 H81B 0.9900 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C91 O9 1.431(3) . ?
C91 C92 1.490(5) . ?
C91 H91A 0.9900 . ?
C91 H91B 0.9900 . ?
C92 H92A 0.9800 . ?
C92 H92B 0.9800 . ?
C92 H92C 0.9800 . ?
C91A O9 1.466(9) . ?
C91A C92A 1.539(10) . ?
C91A H91C 0.9900 . ?
C91A H91D 0.9900 . ?
C92A H92D 0.9800 . ?
C92A H92E 0.9800 . ?
C92A H92F 0.9800 . ?
O9 H9 0.8764 . ?

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
O10 Tb1 O10 74.05(6) 3_666 . ?
O10 Tb1 O9 75.25(5) 3_666 . ?
O10 Tb1 O9 137.75(5) . . ?
O10 Tb1 O3 78.48(5) 3_666 . ?
O10 Tb1 O3 68.22(5) . . ?
O9 Tb1 O3 77.78(6) . . ?
O10 Tb1 O1 116.49(5) 3_666 . ?
O10 Tb1 O1 65.34(5) . . ?
O9 Tb1 O1 156.55(5) . . ?
O3 Tb1 O1 123.21(5) . . ?
O10 Tb1 O8 65.95(5) 3_666 3_666 ?
O10 Tb1 O8 105.61(5) . 3_666 ?
O9 Tb1 O8 87.29(6) . 3_666 ?
O3 Tb1 O8 143.93(5) . 3_666 ?
O1 Tb1 O8 80.27(5) . 3_666 ?
O10 Tb1 O4 126.65(5) 3_666 . ?
O10 Tb1 O4 58.74(5) . . ?
O9 Tb1 O4 125.00(5) . . ?
O3 Tb1 O4 62.70(5) . . ?
O1 Tb1 O4 66.10(5) . . ?
O8 Tb1 O4 146.27(5) 3_666 . ?
O10 Tb1 Cl1 146.13(4) 3_666 . ?
O10 Tb1 Cl1 139.19(4) . . ?
O9 Tb1 Cl1 77.96(4) . . ?
O3 Tb1 Cl1 115.53(4) . . ?
O1 Tb1 Cl1 82.80(4) . . ?
O8 Tb1 Cl1 92.59(4) 3_666 . ?
O4 Tb1 Cl1 85.93(3) . . ?
O10 Tb1 Ti2 87.09(3) 3_666 . ?
O10 Tb1 Ti2 37.35(4) . . ?
O9 Tb1 Ti2 113.32(4) . . ?
O3 Tb1 Ti2 35.55(3) . . ?
O1 Tb1 Ti2 88.37(4) . . ?
O8 Tb1 Ti2 141.19(4) 3_666 . ?
O4 Tb1 Ti2 40.24(3) . . ?
Cl1 Tb1 Ti2 122.811(16) . . ?
O10 Tb1 Ti1 107.89(3) 3_666 . ?
O10 Tb1 Ti1 36.45(4) . . ?
O9 Tb1 Ti1 164.65(5) . . ?
O3 Tb1 Ti1 88.04(4) . . ?
O1 Tb1 Ti1 35.56(4) . . ?
O8 Tb1 Ti1 107.81(4) 3_666 . ?
O4 Tb1 Ti1 40.90(3) . . ?
Cl1 Tb1 Ti1 103.447(15) . . ?
Ti2 Tb1 Ti1 52.833(9) . . ?
O10 Tb1 Ti2 34.58(4) 3_666 3_666 ?
O10 Tb1 Ti2 83.47(4) . 3_666 ?
O9 Tb1 Ti2 87.44(4) . 3_666 ?
O3 Tb1 Ti2 112.75(4) . 3_666 ?
O1 Tb1 Ti2 92.63(4) . 3_666 ?
O8 Tb1 Ti2 32.98(4) 3_666 3_666 ?
O4 Tb1 Ti2 141.42(3) . 3_666 ?
Cl1 Tb1 Ti2 124.645(16) . 3_666 ?
Ti2 Tb1 Ti2 112.083(8) . 3_666 ?
Ti1 Tb1 Ti2 103.632(10) . 3_666 ?
O10 Tb1 Tb1 37.10(3) 3_666 3_666 ?
O10 Tb1 Tb1 36.94(3) . 3_666 ?
O9 Tb1 Tb1 107.78(4) . 3_666 ?
O3 Tb1 Tb1 69.04(4) . 3_666 ?
O1 Tb1 Tb1 90.97(3) . 3_666 ?
O8 Tb1 Tb1 85.07(4) 3_666 3_666 ?
O4 Tb1 Tb1 92.73(3) . 3_666 ?
Cl1 Tb1 Tb1 173.646(14) . 3_666 ?
Ti2 Tb1 Tb1 57.960(7) . 3_666 ?
Ti1 Tb1 Tb1 71.780(7) . 3_666 ?
Ti2 Tb1 Tb1 54.123(7) 3_666 3_666 ?
O7 Ti2 O8 102.93(7) . . ?
O7 Ti2 O3 101.05(7) . . ?
O8 Ti2 O3 96.82(7) . . ?
O7 Ti2 O10 169.75(7) . . ?
O8 Ti2 O10 83.22(6) . . ?
O3 Ti2 O10 86.17(6) . . ?
O7 Ti2 O2 93.35(7) . . ?
O8 Ti2 O2 100.10(7) . . ?
O3 Ti2 O2 154.71(7) . . ?
O10 Ti2 O2 77.36(6) . . ?
O7 Ti2 O4 102.44(7) . . ?
O8 Ti2 O4 154.59(6) . . ?
O3 Ti2 O4 79.68(6) . . ?
O10 Ti2 O4 71.47(6) . . ?
O2 Ti2 O4 76.95(6) . . ?
O7 Ti2 Ti1 127.31(5) . . ?
O8 Ti2 Ti1 113.22(5) . . ?
O3 Ti2 Ti1 110.81(5) . . ?
O10 Ti2 Ti1 42.53(4) . . ?
O2 Ti2 Ti1 44.83(4) . . ?
O4 Ti2 Ti1 47.49(4) . . ?
O7 Ti2 Tb1 136.88(5) . . ?
O8 Ti2 Tb1 108.64(5) . . ?
O3 Ti2 Tb1 47.35(5) . . ?
O10 Ti2 Tb1 45.38(4) . . ?
O2 Ti2 Tb1 108.82(5) . . ?
O4 Ti2 Tb1 51.01(4) . . ?
Ti1 Ti2 Tb1 63.991(11) . . ?
O7 Ti2 Tb1 146.25(5) . 3_666 ?
O8 Ti2 Tb1 43.88(5) . 3_666 ?
O3 Ti2 Tb1 81.23(5) . 3_666 ?
O10 Ti2 Tb1 41.56(4) . 3_666 ?
O2 Ti2 Tb1 98.20(5) . 3_666 ?
O4 Ti2 Tb1 111.02(4) . 3_666 ?
Ti1 Ti2 Tb1 81.071(12) . 3_666 ?
Tb1 Ti2 Tb1 67.917(8) . 3_666 ?
O5 Ti1 O6 98.73(7) . . ?
O5 Ti1 O1 99.28(7) . . ?
O6 Ti1 O1 103.86(7) . . ?
O5 Ti1 O10 164.14(7) . . ?
O6 Ti1 O10 96.12(6) . . ?
O1 Ti1 O10 82.44(6) . . ?
O5 Ti1 O2 96.47(7) . . ?
O6 Ti1 O2 94.48(7) . . ?
O1 Ti1 O2 153.59(6) . . ?
O10 Ti1 O2 76.79(6) . . ?
O5 Ti1 O4 93.58(7) . . ?
O6 Ti1 O4 164.72(6) . . ?
O1 Ti1 O4 82.90(6) . . ?
O10 Ti1 O4 70.90(6) . . ?
O2 Ti1 O4 75.05(6) . . ?
O5 Ti1 Ti2 123.13(6) . . ?
O6 Ti1 Ti2 118.66(5) . . ?
O1 Ti1 Ti2 110.09(5) . . ?
O10 Ti1 Ti2 43.07(4) . . ?
O2 Ti1 Ti2 43.62(4) . . ?
O4 Ti1 Ti2 46.22(4) . . ?
O5 Ti1 Tb1 126.98(6) . . ?
O6 Ti1 Tb1 125.19(5) . . ?
O1 Ti1 Tb1 46.95(4) . . ?
O10 Ti1 Tb1 44.76(4) . . ?
O2 Ti1 Tb1 106.79(4) . . ?
O4 Ti1 Tb1 50.51(4) . . ?
Ti2 Ti1 Tb1 63.177(10) . . ?
O1 C11 C12 111.8(2) . . ?
O1 C11 H11A 109.3 . . ?
C12 C11 H11A 109.3 . . ?
O1 C11 H11B 109.3 . . ?
C12 C11 H11B 109.3 . . ?
H11A C11 H11B 107.9 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O2 C21 C22 119.2(6) . . ?
O2 C21 H21A 107.5 . . ?
C22 C21 H21A 107.5 . . ?
O2 C21 H21B 107.5 . . ?
C22 C21 H21B 107.5 . . ?
H21A C21 H21B 107.0 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O2 C21A C22A 116.0(3) . . ?
O2 C21A H21C 108.3 . . ?
C22A C21A H21C 108.3 . . ?
O2 C21A H21D 108.3 . . ?
C22A C21A H21D 108.3 . . ?
H21C C21A H21D 107.4 . . ?
C21A C22A H22D 109.5 . . ?
C21A C22A H22E 109.5 . . ?
H22D C22A H22E 109.5 . . ?
C21A C22A H22F 109.5 . . ?
H22D C22A H22F 109.5 . . ?
H22E C22A H22F 109.5 . . ?
O3 C31 C32 111.3(2) . . ?
O3 C31 H31A 109.4 . . ?
C32 C31 H31A 109.4 . . ?
O3 C31 H31B 109.4 . . ?
C32 C31 H31B 109.4 . . ?
H31A C31 H31B 108.0 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O4 C41 C42 111.9(2) . . ?
O4 C41 H41A 109.2 . . ?
C42 C41 H41A 109.2 . . ?
O4 C41 H41B 109.2 . . ?
C42 C41 H41B 109.2 . . ?
H41A C41 H41B 107.9 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O5 C51 C52 111.9(3) . . ?
O5 C51 H51A 109.2 . . ?
C52 C51 H51A 109.2 . . ?
O5 C51 H51B 109.2 . . ?
C52 C51 H51B 109.2 . . ?
H51A C51 H51B 107.9 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
O6 C61 C62 111.3(2) . . ?
O6 C61 H61A 109.4 . . ?
C62 C61 H61A 109.4 . . ?
O6 C61 H61B 109.4 . . ?
C62 C61 H61B 109.4 . . ?
H61A C61 H61B 108.0 . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
O7 C71 C72 112.7(2) . . ?
O7 C71 H71A 109.1 . . ?
C72 C71 H71A 109.1 . . ?
O7 C71 H71B 109.1 . . ?
C72 C71 H71B 109.1 . . ?
H71A C71 H71B 107.8 . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
O8 C81 C82 112.1(2) . . ?
O8 C81 H81A 109.2 . . ?
C82 C81 H81A 109.2 . . ?
O8 C81 H81B 109.2 . . ?
C82 C81 H81B 109.2 . . ?
H81A C81 H81B 107.9 . . ?
C81 C82 H82A 109.5 . . ?
C81 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
C81 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
O9 C91 C92 111.2(3) . . ?
O9 C91 H91A 109.4 . . ?
C92 C91 H91A 109.4 . . ?
O9 C91 H91B 109.4 . . ?
C92 C91 H91B 109.4 . . ?
H91A C91 H91B 108.0 . . ?
C91 C92 H92A 109.5 . . ?
C91 C92 H92B 109.5 . . ?
H92A C92 H92B 109.5 . . ?
C91 C92 H92C 109.5 . . ?
H92A C92 H92C 109.5 . . ?
H92B C92 H92C 109.5 . . ?
O9 C91A C92A 111.6(9) . . ?
O9 C91A H91C 109.3 . . ?
C92A C91A H91C 109.3 . . ?
O9 C91A H91D 109.3 . . ?
C92A C91A H91D 109.3 . . ?
H91C C91A H91D 108.0 . . ?
C91A C92A H92D 109.5 . . ?
C91A C92A H92E 109.5 . . ?
H92D C92A H92E 109.5 . . ?
C91A C92A H92F 109.5 . . ?
H92D C92A H92F 109.5 . . ?
H92E C92A H92F 109.5 . . ?
C11 O1 Ti1 125.03(14) . . ?
C11 O1 Tb1 126.43(13) . . ?
Ti1 O1 Tb1 97.49(6) . . ?
C21 O2 Ti2 129.1(3) . . ?
C21A O2 Ti2 128.81(17) . . ?
C21 O2 Ti1 132.6(4) . . ?
C21A O2 Ti1 129.13(18) . . ?
Ti2 O2 Ti1 91.55(6) . . ?
C31 O3 Ti2 123.16(13) . . ?
C31 O3 Tb1 138.24(13) . . ?
Ti2 O3 Tb1 97.10(6) . . ?
C41 O4 Ti2 127.98(14) . . ?
C41 O4 Ti1 120.89(13) . . ?
Ti2 O4 Ti1 86.29(5) . . ?
C41 O4 Tb1 130.79(13) . . ?
Ti2 O4 Tb1 88.76(5) . . ?
Ti1 O4 Tb1 88.59(5) . . ?
C51 O5 Ti1 165.43(18) . . ?
C61 O6 Ti1 132.96(14) . . ?
C71 O7 Ti2 160.16(18) . . ?
C81 O8 Ti2 127.18(15) . . ?
C81 O8 Tb1 127.26(14) . 3_666 ?
Ti2 O8 Tb1 103.14(6) . 3_666 ?
C91 O9 Tb1 136.46(17) . . ?
C91A O9 Tb1 125.2(6) . . ?
C91 O9 H9 128.9 . . ?
C91A O9 H9 119.3 . . ?
Tb1 O9 H9 92.8 . . ?
Ti1 O10 Ti2 94.40(6) . . ?
Ti1 O10 Tb1 146.80(7) . 3_666 ?
Ti2 O10 Tb1 103.86(6) . 3_666 ?
Ti1 O10 Tb1 98.80(6) . . ?
Ti2 O10 Tb1 97.28(5) . . ?
Tb1 O10 Tb1 105.96(6) 3_666 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C12 C11 O1 Ti1 72.3(3) . . . . ?
C12 C11 O1 Tb1 -152.00(18) . . . . ?
C22 C21 O2 Ti2 -158.1(4) . . . . ?
C22 C21 O2 Ti1 59.3(10) . . . . ?
C22A C21A O2 Ti2 157.5(2) . . . . ?
C22A C21A O2 Ti1 -68.2(4) . . . . ?
C32 C31 O3 Ti2 104.2(2) . . . . ?
C32 C31 O3 Tb1 -93.4(3) . . . . ?
C42 C41 O4 Ti2 -69.0(2) . . . . ?
C42 C41 O4 Ti1 179.17(15) . . . . ?
C42 C41 O4 Tb1 60.6(3) . . . . ?
C52 C51 O5 Ti1 165.7(6) . . . . ?
O6 Ti1 O5 C51 -151.6(8) . . . . ?
O1 Ti1 O5 C51 102.7(8) . . . . ?
O10 Ti1 O5 C51 7.7(9) . . . . ?
O2 Ti1 O5 C51 -56.0(8) . . . . ?
O4 Ti1 O5 C51 19.3(8) . . . . ?
Ti2 Ti1 O5 C51 -18.8(8) . . . . ?
Tb1 Ti1 O5 C51 60.7(8) . . . . ?
C62 C61 O6 Ti1 -133.2(2) . . . . ?
O5 Ti1 O6 C61 5.3(2) . . . . ?
O1 Ti1 O6 C61 107.2(2) . . . . ?
O10 Ti1 O6 C61 -169.2(2) . . . . ?
O2 Ti1 O6 C61 -92.0(2) . . . . ?
O4 Ti1 O6 C61 -138.0(3) . . . . ?
Ti2 Ti1 O6 C61 -130.30(19) . . . . ?
Tb1 Ti1 O6 C61 153.81(18) . . . . ?
C72 C71 O7 Ti2 -126.1(5) . . . . ?
O8 Ti2 O7 C71 141.0(5) . . . . ?
O3 Ti2 O7 C71 -119.2(5) . . . . ?
O10 Ti2 O7 C71 15.0(8) . . . . ?
O2 Ti2 O7 C71 39.9(5) . . . . ?
O4 Ti2 O7 C71 -37.5(5) . . . . ?
Ti1 Ti2 O7 C71 7.9(6) . . . . ?
Tb1 Ti2 O7 C71 -82.5(5) . . . . ?
Tb1 Ti2 O7 C71 150.0(5) 3_666 . . . ?
C82 C81 O8 Ti2 81.6(3) . . . . ?
C82 C81 O8 Tb1 -119.1(2) . . . 3_666 ?
C92 C91 O9 Tb1 107.2(4) . . . . ?
C92A C91A O9 Tb1 -122.9(14) . . . . ?

####################################################################### 
# 
# 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_Ti4Gd2
_database_code_depnum_ccdc_archive 'CCDC 2283721'
loop_
_audit_author_name
_audit_author_address
'Andrew Bond'
;University of Cambridge
United Kingdom
;
_audit_update_record             
;
2023-07-22 deposited with the CCDC.	2023-09-15 downloaded from the CCDC.
;
#===============================================================================
_audit_creation_method           SHELXL-2019/2

#-------------------------------------------------------------------------------
# Inserted by local software: cifUpdate ver. 3.1  (Andrew D. Bond, March 2019)
#-------------------------------------------------------------------------------
_cambridge_user_name             'Rosa Mueller'
_cambridge_user_crsid            rm2055
_cambridge_supervisor_name       'Dominic Wright'
_cambridge_supervisor_crsid      dsw1000
_cambridge_crystallographer_name 'Andrew Bond'
_cambridge_crystallographer_crsid adb29
_cambridge_sample_id             RM93A
_cambridge_data_id               DW_B2_0373
#-------------------------------------------------------------------------------

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H92 Cl2 Gd2 O20 Ti4'
_chemical_formula_sum            'C36 H92 Cl2 Gd2 O20 Ti4'
_chemical_formula_weight         1422.09

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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   11.9414(5)
_cell_length_b                   18.8718(8)
_cell_length_c                   12.7327(5)
_cell_angle_alpha                90
_cell_angle_beta                 92.454(2)
_cell_angle_gamma                90
_cell_volume                     2866.8(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9000
_cell_measurement_theta_min      4.69
_cell_measurement_theta_max      66.46

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_F_000             1436
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    20.613
_shelx_estimated_absorpt_T_min   0.232
_shelx_estimated_absorpt_T_max   0.289
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5403
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Incoatec I\mS Cu microsource'
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-III'
_diffrn_measurement_method       'ω and φ-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            49395
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         4.686
_diffrn_reflns_theta_max         66.797
_diffrn_reflns_theta_full        66.797
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             5049
_reflns_number_gt                4807
_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.

#===============================================================================
INTENSITY STATISTICS FOR DATASET # 1  DW_B2_0373_0m.hkl
#===============================================================================
 Resolution   #Data #Theory %Complete Redundancy Mean I Mean I/s Rmerge  Rsigma
#-------------------------------------------------------------------------------
  Inf - 3.52      81     83     97.6     6.93     93.35   44.94  0.0312  0.0189
 3.52 - 2.32     181    181    100.0     7.23    128.92   44.87  0.0317  0.0165
 2.32 - 1.83     268    268    100.0     8.40     97.23   42.94  0.0344  0.0166
 1.83 - 1.59     267    267    100.0    10.82     85.14   48.01  0.0399  0.0155
 1.59 - 1.44     267    267    100.0    14.05     68.71   54.19  0.0370  0.0135
 1.44 - 1.34     250    250    100.0    14.66     51.05   51.04  0.0392  0.0142
 1.34 - 1.26     265    265    100.0    13.36     48.62   42.23  0.0434  0.0156
 1.26 - 1.19     289    289    100.0    13.36     45.56   43.09  0.0433  0.0165
 1.19 - 1.14     255    255    100.0    12.71     37.51   38.68  0.0477  0.0178
 1.14 - 1.10     237    237    100.0    12.59     43.62   40.36  0.0479  0.0173
 1.10 - 1.06     269    269    100.0    11.01     34.93   32.88  0.0619  0.0220
 1.06 - 1.03     246    246    100.0    11.05     32.82   34.86  0.0581  0.0202
 1.03 - 0.99     332    332    100.0     9.79     31.39   32.95  0.0568  0.0208
 0.99 - 0.97     222    222    100.0     7.76     29.08   30.74  0.0480  0.0232
 0.97 - 0.94     329    329    100.0     7.75     23.66   28.48  0.0477  0.0241
 0.94 - 0.92     237    237    100.0     7.26     23.91   27.48  0.0473  0.0246
 0.92 - 0.90     269    270     99.6     6.43     23.20   26.93  0.0502  0.0257
 0.90 - 0.88     304    304    100.0     6.41     20.04   26.89  0.0520  0.0266
 0.88 - 0.87     161    161    100.0     6.17     19.73   27.51  0.0487  0.0262
 0.87 - 0.85     322    322    100.0     5.75     19.32   25.98  0.0528  0.0268
 0.85 - 0.84     181    214     84.6     3.75     16.92   20.95  0.0556  0.0346
#-------------------------------------------------------------------------------
 0.94 - 0.84    1474   1508     97.7     6.00     20.66   26.13  0.0506  0.0269
  Inf - 0.84    5232   5268     99.3     9.55     43.83   36.21  0.0432  0.0185
#===============================================================================
;

_computing_data_collection       'APEX4 (Bruker, 2021)'
_computing_cell_refinement       'SAINT (Bruker, 2016)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL

_refine_special_details          ?

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0215P)²+1.8308P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5049
_refine_ls_number_parameters     329
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0198
_refine_ls_R_factor_gt           0.0183
_refine_ls_wR_factor_ref         0.0448
_refine_ls_wR_factor_gt          0.0440
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.088
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.060

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 0.38073(2) 0.54072(2) 0.41869(2) 0.01161(5) Uani 1 1 d . . . . .
Ti2 Ti 0.39031(3) 0.54474(2) 0.67704(3) 0.01283(8) Uani 1 1 d . . . . .
Ti1 Ti 0.49421(3) 0.66467(2) 0.57349(3) 0.01308(8) Uani 1 1 d . . . . .
Cl1 Cl 0.22661(5) 0.61054(3) 0.30079(5) 0.02920(13) Uani 1 1 d . . . . .
C11 C 0.4553(2) 0.71267(12) 0.35065(19) 0.0254(5) Uani 1 1 d . . . . .
H11A H 0.393966 0.742558 0.376206 0.030 Uiso 1 1 calc R U . . .
H11B H 0.430646 0.693400 0.281124 0.030 Uiso 1 1 calc R U . . .
C12 C 0.5578(3) 0.75751(15) 0.3388(2) 0.0423(7) Uani 1 1 d . . . . .
H12A H 0.577875 0.780627 0.405950 0.063 Uiso 1 1 calc R U . . .
H12B H 0.542462 0.793641 0.284844 0.063 Uiso 1 1 calc R U . . .
H12C H 0.620096 0.727522 0.317996 0.063 Uiso 1 1 calc R U . . .
C21 C 0.5260(9) 0.6470(4) 0.8193(6) 0.025(3) Uani 0.246(8) 1 d D U P A 1
H21A H 0.601419 0.625717 0.815186 0.030 Uiso 0.246(8) 1 calc R U P A 1
H21B H 0.487205 0.621350 0.875037 0.030 Uiso 0.246(8) 1 calc R U P A 1
C22 C 0.5407(3) 0.72177(17) 0.8539(2) 0.0524(9) Uani 0.246(8) 1 d D U P A 1
H22A H 0.592934 0.745752 0.808471 0.079 Uiso 0.246(8) 1 calc R U P A 1
H22B H 0.570736 0.722792 0.926771 0.079 Uiso 0.246(8) 1 calc R U P A 1
H22C H 0.468095 0.746047 0.849438 0.079 Uiso 0.246(8) 1 calc R U P A 1
C21A C 0.4467(3) 0.67717(17) 0.8149(2) 0.0273(10) Uani 0.754(8) 1 d D U P A 2
H21C H 0.424291 0.645914 0.872844 0.033 Uiso 0.754(8) 1 calc R U P A 2
H21D H 0.382212 0.708292 0.796189 0.033 Uiso 0.754(8) 1 calc R U P A 2
C22A C 0.5407(3) 0.72177(17) 0.8539(2) 0.0524(9) Uani 0.754(8) 1 d D U P A 2
H22D H 0.605840 0.691801 0.871539 0.079 Uiso 0.754(8) 1 calc R U P A 2
H22E H 0.518959 0.747391 0.916850 0.079 Uiso 0.754(8) 1 calc R U P A 2
H22F H 0.559815 0.755809 0.799427 0.079 Uiso 0.754(8) 1 calc R U P A 2
C31 C 0.25902(19) 0.41996(12) 0.60367(19) 0.0230(5) Uani 1 1 d . . . . .
H31A H 0.286294 0.405064 0.674795 0.028 Uiso 1 1 calc R U . . .
H31B H 0.278751 0.382321 0.553550 0.028 Uiso 1 1 calc R U . . .
C32 C 0.1333(2) 0.42822(17) 0.6021(3) 0.0452(7) Uani 1 1 d . . . . .
H32A H 0.113093 0.462721 0.655611 0.068 Uiso 1 1 calc R U . . .
H32B H 0.098698 0.382410 0.617005 0.068 Uiso 1 1 calc R U . . .
H32C H 0.106301 0.444888 0.532627 0.068 Uiso 1 1 calc R U . . .
C41 C 0.23015(18) 0.66616(12) 0.57963(19) 0.0228(5) Uani 1 1 d . . . . .
H41A H 0.229184 0.702544 0.523583 0.027 Uiso 1 1 calc R U . . .
H41B H 0.236486 0.690896 0.648188 0.027 Uiso 1 1 calc R U . . .
C42 C 0.12169(19) 0.62534(15) 0.5725(2) 0.0308(6) Uani 1 1 d . . . . .
H42A H 0.114673 0.601059 0.504463 0.046 Uiso 1 1 calc R U . . .
H42B H 0.058695 0.658101 0.579016 0.046 Uiso 1 1 calc R U . . .
H42C H 0.121129 0.590304 0.629247 0.046 Uiso 1 1 calc R U . . .
C51 C 0.3843(3) 0.81598(14) 0.6057(3) 0.0470(8) Uani 1 1 d . . . . .
H51A H 0.346736 0.811065 0.673167 0.056 Uiso 1 1 calc R U . . .
H51B H 0.325469 0.821620 0.549179 0.056 Uiso 1 1 calc R U . . .
C52 C 0.4558(3) 0.87996(15) 0.6098(3) 0.0627(11) Uani 1 1 d . . . . .
H52A H 0.511755 0.875677 0.668012 0.094 Uiso 1 1 calc R U . . .
H52B H 0.409138 0.921851 0.620664 0.094 Uiso 1 1 calc R U . . .
H52C H 0.493744 0.884784 0.543473 0.094 Uiso 1 1 calc R U . . .
C61 C 0.7116(2) 0.74127(13) 0.6253(2) 0.0273(5) Uani 1 1 d . . . . .
H61A H 0.737994 0.737144 0.699841 0.033 Uiso 1 1 calc R U . . .
H61B H 0.663665 0.783938 0.618350 0.033 Uiso 1 1 calc R U . . .
C62 C 0.8108(2) 0.74959(15) 0.5578(2) 0.0358(6) Uani 1 1 d . . . . .
H62A H 0.859034 0.707739 0.565446 0.054 Uiso 1 1 calc R U . . .
H62B H 0.853256 0.791896 0.579679 0.054 Uiso 1 1 calc R U . . .
H62C H 0.784802 0.754559 0.484083 0.054 Uiso 1 1 calc R U . . .
C71 C 0.2146(3) 0.57419(18) 0.8486(2) 0.0429(7) Uani 1 1 d . . . . .
H71A H 0.138827 0.556256 0.828116 0.051 Uiso 1 1 calc R U . . .
H71B H 0.212751 0.626526 0.843412 0.051 Uiso 1 1 calc R U . . .
C72 C 0.2430(3) 0.55346(18) 0.9597(2) 0.0499(8) Uani 1 1 d . . . . .
H72A H 0.241480 0.501715 0.965902 0.075 Uiso 1 1 calc R U . . .
H72B H 0.188060 0.574133 1.005843 0.075 Uiso 1 1 calc R U . . .
H72C H 0.318015 0.570939 0.980278 0.075 Uiso 1 1 calc R U . . .
C81 C 0.5197(2) 0.45560(14) 0.83588(19) 0.0314(6) Uani 1 1 d . . . . .
H81A H 0.517652 0.498323 0.880878 0.038 Uiso 1 1 calc R U . . .
H81B H 0.596109 0.435332 0.842981 0.038 Uiso 1 1 calc R U . . .
C82 C 0.4366(3) 0.40209(16) 0.8735(2) 0.0471(8) Uani 1 1 d . . . . .
H82A H 0.360885 0.422103 0.867196 0.071 Uiso 1 1 calc R U . . .
H82B H 0.454930 0.390289 0.947187 0.071 Uiso 1 1 calc R U . . .
H82C H 0.440007 0.359121 0.830537 0.071 Uiso 1 1 calc R U . . .
C91 C 0.1562(3) 0.43757(18) 0.2979(3) 0.0327(10) Uani 0.816(8) 1 d D U P B 1
H91A H 0.112314 0.481092 0.309932 0.039 Uiso 0.816(8) 1 calc R U P B 1
H91B H 0.117460 0.397389 0.330685 0.039 Uiso 0.816(8) 1 calc R U P B 1
C92 C 0.1620(5) 0.4247(4) 0.1821(3) 0.0779(19) Uani 0.816(8) 1 d D U P B 1
H92A H 0.198938 0.464998 0.149417 0.117 Uiso 0.816(8) 1 calc R U P B 1
H92B H 0.086000 0.419430 0.151004 0.117 Uiso 0.816(8) 1 calc R U P B 1
H92C H 0.204920 0.381425 0.170209 0.117 Uiso 0.816(8) 1 calc R U P B 1
C91A C 0.2279(11) 0.4377(8) 0.2358(7) 0.033(5) Uani 0.184(8) 1 d D U P B 2
H91C H 0.262213 0.394862 0.205870 0.039 Uiso 0.184(8) 1 calc R U P B 2
H91D H 0.253165 0.479256 0.195618 0.039 Uiso 0.184(8) 1 calc R U P B 2
C92A C 0.0997(12) 0.4319(15) 0.2240(16) 0.072(8) Uani 0.184(8) 1 d D U P B 2
H92D H 0.076610 0.383707 0.241981 0.108 Uiso 0.184(8) 1 calc R U P B 2
H92E H 0.075315 0.442347 0.151145 0.108 Uiso 0.184(8) 1 calc R U P B 2
H92F H 0.065471 0.465814 0.271175 0.108 Uiso 0.184(8) 1 calc R U P B 2
O1 O 0.47576(13) 0.65543(7) 0.42234(11) 0.0172(3) Uani 1 1 d . . . . .
O2 O 0.46892(13) 0.63419(8) 0.72635(11) 0.0201(3) Uani 1 1 d D . . . .
O3 O 0.31333(12) 0.48426(8) 0.57631(11) 0.0172(3) Uani 1 1 d . . . . .
O4 O 0.32594(12) 0.62141(7) 0.56932(11) 0.0154(3) Uani 1 1 d . . . . .
O5 O 0.44633(14) 0.75396(8) 0.58714(13) 0.0248(4) Uani 1 1 d . . . . .
O6 O 0.64735(13) 0.68018(8) 0.59618(12) 0.0192(3) Uani 1 1 d . . . . .
O7 O 0.29128(13) 0.54776(8) 0.77870(12) 0.0198(3) Uani 1 1 d . . . . .
O8 O 0.49652(13) 0.47557(8) 0.72875(11) 0.0183(3) Uani 1 1 d . . . . .
O9 O 0.26622(13) 0.44516(8) 0.34606(13) 0.0244(4) Uani 1 1 d D . . . .
H9 H 0.310012 0.412348 0.374564 0.037 Uiso 1 1 d R U . B .
O10 O 0.50279(11) 0.56013(7) 0.56715(10) 0.0111(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O10 2.3598(13) 3_666 ?
Gd1 O10 2.3656(13) . ?
Gd1 O9 2.4226(15) . ?
Gd1 O3 2.4391(14) . ?
Gd1 O1 2.4436(14) . ?
Gd1 O8 2.4501(15) 3_666 ?
Gd1 O4 2.5559(14) . ?
Gd1 Cl1 2.6721(5) . ?
Gd1 Ti2 3.2874(4) . ?
Gd1 Ti1 3.3112(4) . ?
Gd1 Ti2 3.4421(4) 3_666 ?
Gd1 Gd1 3.7760(2) 3_666 ?
Ti2 O7 1.7911(16) . ?
Ti2 O8 1.9169(15) . ?
Ti2 O3 1.9214(15) . ?
Ti2 O10 2.0018(14) . ?
Ti2 O2 2.0187(15) . ?
Ti2 O4 2.1155(14) . ?
Ti2 Ti1 2.9224(5) . ?
Ti1 O5 1.7902(15) . ?
Ti1 O6 1.8622(15) . ?
Ti1 O1 1.9357(15) . ?
Ti1 O10 1.9773(14) . ?
Ti1 O2 2.0642(15) . ?
Ti1 O4 2.1674(15) . ?
C11 O1 1.429(3) . ?
C11 C12 1.502(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C21 O2 1.362(7) . ?
C21 C22 1.487(7) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C21A O2 1.423(3) . ?
C21A C22A 1.472(4) . ?
C21A H21C 0.9900 . ?
C21A H21D 0.9900 . ?
C22A H22D 0.9800 . ?
C22A H22E 0.9800 . ?
C22A H22F 0.9800 . ?
C31 O3 1.426(3) . ?
C31 C32 1.509(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C41 O4 1.432(3) . ?
C41 C42 1.506(3) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C51 O5 1.411(3) . ?
C51 C52 1.478(4) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C61 O6 1.425(3) . ?
C61 C62 1.501(4) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C71 O7 1.396(3) . ?
C71 C72 1.493(4) . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C81 O8 1.431(3) . ?
C81 C82 1.508(4) . ?
C81 H81A 0.9900 . ?
C81 H81B 0.9900 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C91 O9 1.433(3) . ?
C91 C92 1.499(5) . ?
C91 H91A 0.9900 . ?
C91 H91B 0.9900 . ?
C92 H92A 0.9800 . ?
C92 H92B 0.9800 . ?
C92 H92C 0.9800 . ?
C91A O9 1.465(8) . ?
C91A C92A 1.536(10) . ?
C91A H91C 0.9900 . ?
C91A H91D 0.9900 . ?
C92A H92D 0.9800 . ?
C92A H92E 0.9800 . ?
C92A H92F 0.9800 . ?
O9 H9 0.8788 . ?

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
O10 Gd1 O10 73.91(5) 3_666 . ?
O10 Gd1 O9 75.52(5) 3_666 . ?
O10 Gd1 O9 137.62(5) . . ?
O10 Gd1 O3 78.41(5) 3_666 . ?
O10 Gd1 O3 67.91(5) . . ?
O9 Gd1 O3 77.77(5) . . ?
O10 Gd1 O1 116.19(5) 3_666 . ?
O10 Gd1 O1 65.03(5) . . ?
O9 Gd1 O1 157.04(5) . . ?
O3 Gd1 O1 122.73(5) . . ?
O10 Gd1 O8 65.62(5) 3_666 3_666 ?
O10 Gd1 O8 105.27(5) . 3_666 ?
O9 Gd1 O8 87.74(6) . 3_666 ?
O3 Gd1 O8 143.61(5) . 3_666 ?
O1 Gd1 O8 80.39(5) . 3_666 ?
O10 Gd1 O4 126.32(5) 3_666 . ?
O10 Gd1 O4 58.46(4) . . ?
O9 Gd1 O4 124.86(5) . . ?
O3 Gd1 O4 62.53(5) . . ?
O1 Gd1 O4 65.89(5) . . ?
O8 Gd1 O4 146.15(5) 3_666 . ?
O10 Gd1 Cl1 146.11(3) 3_666 . ?
O10 Gd1 Cl1 139.34(4) . . ?
O9 Gd1 Cl1 77.80(4) . . ?
O3 Gd1 Cl1 115.73(4) . . ?
O1 Gd1 Cl1 83.22(4) . . ?
O8 Gd1 Cl1 92.96(4) 3_666 . ?
O4 Gd1 Cl1 86.30(3) . . ?
O10 Gd1 Ti2 86.96(3) 3_666 . ?
O10 Gd1 Ti2 37.16(3) . . ?
O9 Gd1 Ti2 113.20(4) . . ?
O3 Gd1 Ti2 35.45(3) . . ?
O1 Gd1 Ti2 87.96(3) . . ?
O8 Gd1 Ti2 140.65(4) 3_666 . ?
O4 Gd1 Ti2 40.05(3) . . ?
Cl1 Gd1 Ti2 122.985(16) . . ?
O10 Gd1 Ti1 107.43(3) 3_666 . ?
O10 Gd1 Ti1 36.15(3) . . ?
O9 Gd1 Ti1 164.37(4) . . ?
O3 Gd1 Ti1 87.70(3) . . ?
O1 Gd1 Ti1 35.41(3) . . ?
O8 Gd1 Ti1 107.56(4) 3_666 . ?
O4 Gd1 Ti1 40.87(3) . . ?
Cl1 Gd1 Ti1 103.920(14) . . ?
Ti2 Gd1 Ti1 52.575(9) . . ?
O10 Gd1 Ti2 34.37(3) 3_666 3_666 ?
O10 Gd1 Ti2 83.34(3) . 3_666 ?
O9 Gd1 Ti2 87.70(4) . 3_666 ?
O3 Gd1 Ti2 112.45(4) . 3_666 ?
O1 Gd1 Ti2 92.67(4) . 3_666 ?
O8 Gd1 Ti2 32.81(3) 3_666 3_666 ?
O4 Gd1 Ti2 141.04(3) . 3_666 ?
Cl1 Gd1 Ti2 124.785(16) . 3_666 ?
Ti2 Gd1 Ti2 111.779(8) . 3_666 ?
Ti1 Gd1 Ti2 103.342(9) . 3_666 ?
O10 Gd1 Gd1 37.01(3) 3_666 3_666 ?
O10 Gd1 Gd1 36.90(3) . 3_666 ?
O9 Gd1 Gd1 107.85(4) . 3_666 ?
O3 Gd1 Gd1 68.83(4) . 3_666 ?
O1 Gd1 Gd1 90.65(3) . 3_666 ?
O8 Gd1 Gd1 84.67(3) 3_666 3_666 ?
O4 Gd1 Gd1 92.43(3) . 3_666 ?
Cl1 Gd1 Gd1 173.730(14) . 3_666 ?
Ti2 Gd1 Gd1 57.833(7) . 3_666 ?
Ti1 Gd1 Gd1 71.415(7) . 3_666 ?
Ti2 Gd1 Gd1 53.945(7) 3_666 3_666 ?
O7 Ti2 O8 102.77(7) . . ?
O7 Ti2 O3 100.92(7) . . ?
O8 Ti2 O3 96.63(7) . . ?
O7 Ti2 O10 169.74(6) . . ?
O8 Ti2 O10 83.40(6) . . ?
O3 Ti2 O10 86.32(6) . . ?
O7 Ti2 O2 93.51(7) . . ?
O8 Ti2 O2 99.82(7) . . ?
O3 Ti2 O2 155.13(6) . . ?
O10 Ti2 O2 77.23(6) . . ?
O7 Ti2 O4 102.36(6) . . ?
O8 Ti2 O4 154.84(6) . . ?
O3 Ti2 O4 79.83(6) . . ?
O10 Ti2 O4 71.56(5) . . ?
O2 Ti2 O4 77.34(6) . . ?
O7 Ti2 Ti1 127.41(5) . . ?
O8 Ti2 Ti1 113.26(5) . . ?
O3 Ti2 Ti1 111.05(5) . . ?
O10 Ti2 Ti1 42.41(4) . . ?
O2 Ti2 Ti1 44.92(4) . . ?
O4 Ti2 Ti1 47.72(4) . . ?
O7 Ti2 Gd1 136.73(5) . . ?
O8 Ti2 Gd1 108.79(5) . . ?
O3 Ti2 Gd1 47.41(4) . . ?
O10 Ti2 Gd1 45.54(4) . . ?
O2 Ti2 Gd1 109.05(4) . . ?
O4 Ti2 Gd1 51.02(4) . . ?
Ti1 Ti2 Gd1 64.131(10) . . ?
O7 Ti2 Gd1 146.08(5) . 3_666 ?
O8 Ti2 Gd1 43.83(5) . 3_666 ?
O3 Ti2 Gd1 81.37(5) . 3_666 ?
O10 Ti2 Gd1 41.72(4) . 3_666 ?
O2 Ti2 Gd1 97.82(5) . 3_666 ?
O4 Ti2 Gd1 111.28(4) . 3_666 ?
Ti1 Ti2 Gd1 81.032(11) . 3_666 ?
Gd1 Ti2 Gd1 68.222(8) . 3_666 ?
O5 Ti1 O6 98.78(7) . . ?
O5 Ti1 O1 99.10(7) . . ?
O6 Ti1 O1 103.75(7) . . ?
O5 Ti1 O10 163.82(7) . . ?
O6 Ti1 O10 96.37(6) . . ?
O1 Ti1 O10 82.73(6) . . ?
O5 Ti1 O2 96.35(7) . . ?
O6 Ti1 O2 94.58(7) . . ?
O1 Ti1 O2 153.82(6) . . ?
O10 Ti1 O2 76.72(6) . . ?
O5 Ti1 O4 93.29(7) . . ?
O6 Ti1 O4 165.06(6) . . ?
O1 Ti1 O4 82.86(6) . . ?
O10 Ti1 O4 70.90(5) . . ?
O2 Ti1 O4 75.24(6) . . ?
O5 Ti1 Ti2 122.80(6) . . ?
O6 Ti1 Ti2 119.00(5) . . ?
O1 Ti1 Ti2 110.26(4) . . ?
O10 Ti1 Ti2 43.07(4) . . ?
O2 Ti1 Ti2 43.67(4) . . ?
O4 Ti1 Ti2 46.23(4) . . ?
O5 Ti1 Gd1 126.76(5) . . ?
O6 Ti1 Gd1 125.28(5) . . ?
O1 Ti1 Gd1 47.02(4) . . ?
O10 Ti1 Gd1 44.89(4) . . ?
O2 Ti1 Gd1 106.96(4) . . ?
O4 Ti1 Gd1 50.50(4) . . ?
Ti2 Ti1 Gd1 63.294(10) . . ?
O1 C11 C12 111.8(2) . . ?
O1 C11 H11A 109.2 . . ?
C12 C11 H11A 109.2 . . ?
O1 C11 H11B 109.2 . . ?
C12 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O2 C21 C22 118.3(6) . . ?
O2 C21 H21A 107.7 . . ?
C22 C21 H21A 107.7 . . ?
O2 C21 H21B 107.7 . . ?
C22 C21 H21B 107.7 . . ?
H21A C21 H21B 107.1 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O2 C21A C22A 115.4(3) . . ?
O2 C21A H21C 108.4 . . ?
C22A C21A H21C 108.4 . . ?
O2 C21A H21D 108.4 . . ?
C22A C21A H21D 108.4 . . ?
H21C C21A H21D 107.5 . . ?
C21A C22A H22D 109.5 . . ?
C21A C22A H22E 109.5 . . ?
H22D C22A H22E 109.5 . . ?
C21A C22A H22F 109.5 . . ?
H22D C22A H22F 109.5 . . ?
H22E C22A H22F 109.5 . . ?
O3 C31 C32 111.8(2) . . ?
O3 C31 H31A 109.3 . . ?
C32 C31 H31A 109.3 . . ?
O3 C31 H31B 109.3 . . ?
C32 C31 H31B 109.3 . . ?
H31A C31 H31B 107.9 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O4 C41 C42 112.39(19) . . ?
O4 C41 H41A 109.1 . . ?
C42 C41 H41A 109.1 . . ?
O4 C41 H41B 109.1 . . ?
C42 C41 H41B 109.1 . . ?
H41A C41 H41B 107.9 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O5 C51 C52 112.2(3) . . ?
O5 C51 H51A 109.2 . . ?
C52 C51 H51A 109.2 . . ?
O5 C51 H51B 109.2 . . ?
C52 C51 H51B 109.2 . . ?
H51A C51 H51B 107.9 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
O6 C61 C62 111.4(2) . . ?
O6 C61 H61A 109.3 . . ?
C62 C61 H61A 109.3 . . ?
O6 C61 H61B 109.3 . . ?
C62 C61 H61B 109.3 . . ?
H61A C61 H61B 108.0 . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
O7 C71 C72 112.4(2) . . ?
O7 C71 H71A 109.1 . . ?
C72 C71 H71A 109.1 . . ?
O7 C71 H71B 109.1 . . ?
C72 C71 H71B 109.1 . . ?
H71A C71 H71B 107.8 . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
O8 C81 C82 112.1(2) . . ?
O8 C81 H81A 109.2 . . ?
C82 C81 H81A 109.2 . . ?
O8 C81 H81B 109.2 . . ?
C82 C81 H81B 109.2 . . ?
H81A C81 H81B 107.9 . . ?
C81 C82 H82A 109.5 . . ?
C81 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
C81 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
O9 C91 C92 110.9(3) . . ?
O9 C91 H91A 109.5 . . ?
C92 C91 H91A 109.5 . . ?
O9 C91 H91B 109.5 . . ?
C92 C91 H91B 109.5 . . ?
H91A C91 H91B 108.0 . . ?
C91 C92 H92A 109.5 . . ?
C91 C92 H92B 109.5 . . ?
H92A C92 H92B 109.5 . . ?
C91 C92 H92C 109.5 . . ?
H92A C92 H92C 109.5 . . ?
H92B C92 H92C 109.5 . . ?
O9 C91A C92A 111.7(9) . . ?
O9 C91A H91C 109.3 . . ?
C92A C91A H91C 109.3 . . ?
O9 C91A H91D 109.3 . . ?
C92A C91A H91D 109.3 . . ?
H91C C91A H91D 107.9 . . ?
C91A C92A H92D 109.5 . . ?
C91A C92A H92E 109.5 . . ?
H92D C92A H92E 109.5 . . ?
C91A C92A H92F 109.5 . . ?
H92D C92A H92F 109.5 . . ?
H92E C92A H92F 109.5 . . ?
C11 O1 Ti1 125.18(14) . . ?
C11 O1 Gd1 126.23(13) . . ?
Ti1 O1 Gd1 97.57(6) . . ?
C21 O2 Ti2 128.9(4) . . ?
C21A O2 Ti2 128.55(16) . . ?
C21 O2 Ti1 133.0(4) . . ?
C21A O2 Ti1 128.92(17) . . ?
Ti2 O2 Ti1 91.41(6) . . ?
C31 O3 Ti2 123.50(13) . . ?
C31 O3 Gd1 137.92(13) . . ?
Ti2 O3 Gd1 97.15(6) . . ?
C41 O4 Ti2 127.83(13) . . ?
C41 O4 Ti1 121.25(13) . . ?
Ti2 O4 Ti1 86.05(5) . . ?
C41 O4 Gd1 130.62(13) . . ?
Ti2 O4 Gd1 88.94(5) . . ?
Ti1 O4 Gd1 88.62(5) . . ?
C51 O5 Ti1 165.81(18) . . ?
C61 O6 Ti1 132.99(14) . . ?
C71 O7 Ti2 160.62(17) . . ?
C81 O8 Ti2 127.22(15) . . ?
C81 O8 Gd1 126.86(14) . 3_666 ?
Ti2 O8 Gd1 103.36(6) . 3_666 ?
C91 O9 Gd1 136.88(17) . . ?
C91A O9 Gd1 125.8(6) . . ?
C91 O9 H9 128.7 . . ?
C91A O9 H9 119.0 . . ?
Gd1 O9 H9 92.9 . . ?
Ti1 O10 Ti2 94.52(6) . . ?
Ti1 O10 Gd1 146.41(7) . 3_666 ?
Ti2 O10 Gd1 103.92(6) . 3_666 ?
Ti1 O10 Gd1 98.97(5) . . ?
Ti2 O10 Gd1 97.30(5) . . ?
Gd1 O10 Gd1 106.09(5) 3_666 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C12 C11 O1 Ti1 72.8(3) . . . . ?
C12 C11 O1 Gd1 -151.43(18) . . . . ?
C22 C21 O2 Ti2 -158.1(4) . . . . ?
C22 C21 O2 Ti1 59.3(11) . . . . ?
C22A C21A O2 Ti2 157.7(2) . . . . ?
C22A C21A O2 Ti1 -69.1(4) . . . . ?
C32 C31 O3 Ti2 104.2(2) . . . . ?
C32 C31 O3 Gd1 -92.9(3) . . . . ?
C42 C41 O4 Ti2 -69.4(2) . . . . ?
C42 C41 O4 Ti1 178.90(15) . . . . ?
C42 C41 O4 Gd1 60.0(2) . . . . ?
C52 C51 O5 Ti1 166.0(6) . . . . ?
O6 Ti1 O5 C51 -152.5(8) . . . . ?
O1 Ti1 O5 C51 102.0(8) . . . . ?
O10 Ti1 O5 C51 6.7(9) . . . . ?
O2 Ti1 O5 C51 -56.8(8) . . . . ?
O4 Ti1 O5 C51 18.7(8) . . . . ?
Ti2 Ti1 O5 C51 -19.4(8) . . . . ?
Gd1 Ti1 O5 C51 59.9(8) . . . . ?
C62 C61 O6 Ti1 -133.89(19) . . . . ?
O5 Ti1 O6 C61 5.2(2) . . . . ?
O1 Ti1 O6 C61 106.9(2) . . . . ?
O10 Ti1 O6 C61 -169.1(2) . . . . ?
O2 Ti1 O6 C61 -91.9(2) . . . . ?
O4 Ti1 O6 C61 -138.2(2) . . . . ?
Ti2 Ti1 O6 C61 -130.19(19) . . . . ?
Gd1 Ti1 O6 C61 153.54(18) . . . . ?
C72 C71 O7 Ti2 -127.4(5) . . . . ?
O8 Ti2 O7 C71 143.0(5) . . . . ?
O3 Ti2 O7 C71 -117.5(5) . . . . ?
O10 Ti2 O7 C71 16.9(8) . . . . ?
O2 Ti2 O7 C71 42.1(5) . . . . ?
O4 Ti2 O7 C71 -35.7(5) . . . . ?
Ti1 Ti2 O7 C71 9.9(6) . . . . ?
Gd1 Ti2 O7 C71 -80.7(5) . . . . ?
Gd1 Ti2 O7 C71 151.7(5) 3_666 . . . ?
C82 C81 O8 Ti2 82.4(3) . . . . ?
C82 C81 O8 Gd1 -118.8(2) . . . 3_666 ?
C92 C91 O9 Gd1 106.9(4) . . . . ?
C92A C91A O9 Gd1 -123.7(14) . . . . ?

