# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2016

####################################################################### 
# 
# 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_2-Eu
_database_code_depnum_ccdc_archive 'CCDC 1442620'
_audit_update_record             
;
2016-10-24 deposited with the CCDC.
2016-10-31 downloaded from the CCDC.
;
_audit_creation_date             2016-10-22
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C45 H31 O23 Eu3, 12(H2 O)'
_chemical_formula_sum            'C45 H55 Eu3 O35'
_chemical_formula_weight         1611.77
_chemical_absolute_configuration .
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_H-M_alt        'I -4 2 d'
_space_group_name_Hall           'I -4 2bw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y, -z+3/4'
'x+1/2, -y, -z+3/4'
'-y+1/2, -x, z+3/4'
'y+1/2, x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1, y+1/2, -z+5/4'
'x+1, -y+1/2, -z+5/4'
'-y+1, -x+1/2, z+5/4'
'y+1, x+1/2, z+5/4'

_cell_length_a                   14.2118(5)
_cell_length_b                   14.2118(5)
_cell_length_c                   63.501(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     12825.7(13)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9663
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.678
_cell_measurement_theta_min      3.141
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.987
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6110
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0973 before and 0.0846 after correction.
The Ratio of minimum to maximum transmission is 0.8195.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             6352
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.205
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.104
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1110
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       75
_diffrn_reflns_limit_l_min       -75
_diffrn_reflns_number            71877
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         3.141
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.824
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                4776
_reflns_number_total             5652
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2015)'
_refine_diff_density_max         0.815
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.139
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.09(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         5652
_refine_ls_number_restraints     23
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0618
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0415P)²+250.8724P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1278
_refine_ls_wR_factor_ref         0.1327
_refine_special_details          
;
 Refined as a 2-component inversion twin.
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.

 The refinement was performed by a routine procedure with 
 SHELXL 2014. All the  hydrogens on carbon atoms were placed
 on calculated positions.  All the hydrogens on water 
 molecules were placed on proper positions and fixed by AFIX 3.

 The highly disordered crystallisation water molecules couldn't 
 located from Q-maps, so the SQUEEZE function in PLATON program
 was performed. And TG experiment was used to 
 
 The TGA curve displays a weight loss of 19.7% below 448 K, 
 consistent with the loss of 12 molecules of crystallisation 
 water (disordered, treated using PLATON SQUEEZE solvent mask)
 and 5 molecules of coordinated water per formula unit
 (calculated loss 19.0%).

 Some alerts caused by SQUEEZE were explained by _vrf_PLAT
 in CIF files.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.91(4) 0.09(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
3. Restrained distances
 O6-O5_$2
 3 with sigma of 0.02
 C1-C19
 1.5 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 Eu2, O3W, O9, C23
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Riding coordinates:
 O1W(H1W), O2W(H2WA,H2WB), O3W(H3WA,H3WB)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C8(H8), C9(H9), C10(H10), C12(H12), C14(H14),
 C15(H15), C17(H17), C23(H23)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu1 Eu 0.5000 1.0000 0.45980(2) 0.0315(3) Uani 1 2 d S T P . .
Eu2 Eu 0.22204(7) 0.98080(8) 0.43826(2) 0.0546(3) Uani 1 1 d . U . . .
O1 O 0.3741(10) 0.9090(12) 0.4656(2) 0.067(4) Uani 1 1 d . . . . .
O1W O 0.5000 1.0000 0.4976(2) 0.083(6) Uani 1 2 d S T P . .
H1W H 0.5447 1.0276 0.5060 0.124 Uiso 1 1 d R . . . .
O2 O 0.2189(12) 0.8834(13) 0.4668(2) 0.086(6) Uani 1 1 d . . . . .
O2W O 0.3067(10) 0.8556(9) 0.4220(2) 0.062(4) Uani 1 1 d . . . . .
H2WA H 0.3147 0.8545 0.4087 0.092 Uiso 1 1 d R . . . .
H2WB H 0.3618 0.8464 0.4283 0.092 Uiso 1 1 d R . . . .
O3 O 0.0950(10) 0.7445(9) 0.5352(2) 0.061(4) Uani 1 1 d . . . . .
O3W O 0.1169(14) 0.8433(18) 0.4295(3) 0.135(8) Uani 1 1 d . U . . .
H3WA H 0.0486 0.8437 0.4298 0.202 Uiso 1 1 d R . . . .
H3WB H 0.1382 0.7815 0.4251 0.202 Uiso 1 1 d R . . . .
O4 O 0.1226(10) 0.5951(10) 0.5292(2) 0.055(4) Uani 1 1 d . . . . .
O5 O 0.0448(7) 0.6315(8) 0.57108(17) 0.037(3) Uani 1 1 d D . . . .
O6 O 0.1136(8) 0.4977(9) 0.56961(15) 0.048(3) Uani 1 1 d D . . . .
O7 O 0.1363(10) 0.6786(12) 0.6711(2) 0.067(4) Uani 1 1 d . . . . .
O8 O 0.0018(16) 0.6768(10) 0.65194(18) 0.076(4) Uani 1 1 d . . . . .
O9 O 0.0755(13) 1.0118(19) 0.4513(3) 0.119(6) Uani 1 1 d . U . . .
C1 C 0.3163(16) 0.7922(16) 0.4916(3) 0.067(7) Uani 1 1 d D . . . .
C2 C 0.3962(14) 0.7627(15) 0.4969(3) 0.055(5) Uani 1 1 d . . . . .
H2 H 0.4495 0.7848 0.4900 0.066 Uiso 1 1 calc R . . . .
C3 C 0.4054(15) 0.6964(16) 0.5133(3) 0.064(6) Uani 1 1 d . . . . .
H3 H 0.4639 0.6710 0.5166 0.077 Uiso 1 1 calc R . . . .
C4 C 0.3210(16) 0.6679(19) 0.5250(3) 0.070(7) Uani 1 1 d . . . . .
C5 C 0.2363(14) 0.7075(14) 0.5188(3) 0.053(5) Uani 1 1 d . . . . .
C6 C 0.2328(15) 0.7721(17) 0.5036(3) 0.066(6) Uani 1 1 d . . . . .
H6 H 0.1770 0.8038 0.5007 0.079 Uiso 1 1 calc R . . . .
C7 C 0.3357(13) 0.6036(14) 0.5429(3) 0.046(4) Uani 1 1 d . . . . .
C8 C 0.3784(13) 0.5201(15) 0.5410(3) 0.060(6) Uani 1 1 d . . . . .
H8 H 0.4008 0.5015 0.5278 0.072 Uiso 1 1 calc R . . . .
C9 C 0.3900(17) 0.4615(18) 0.5579(3) 0.078(7) Uani 1 1 d . . . . .
H9 H 0.4253 0.4068 0.5565 0.094 Uiso 1 1 calc R . . . .
C10 C 0.3505(17) 0.483(2) 0.5764(3) 0.093(10) Uani 1 1 d . . . . .
H10 H 0.3581 0.4414 0.5876 0.111 Uiso 1 1 calc R . . . .
C11 C 0.2984(13) 0.5642(16) 0.5795(3) 0.055(5) Uani 1 1 d . . . . .
C12 C 0.2917(11) 0.6178(15) 0.5625(3) 0.055(5) Uani 1 1 d . . . . .
H12 H 0.2536 0.6708 0.5636 0.066 Uiso 1 1 calc R . . . .
C13 C 0.2476(14) 0.5845(16) 0.5984(3) 0.057(5) Uani 1 1 d . . . . .
C14 C 0.2939(15) 0.5997(17) 0.6189(3) 0.067(6) Uani 1 1 d . . . . .
H14 H 0.3587 0.5936 0.6204 0.080 Uiso 1 1 calc R . . . .
C15 C 0.2390(16) 0.6227(16) 0.6352(3) 0.064(6) Uani 1 1 d . . . . .
H15 H 0.2690 0.6305 0.6481 0.077 Uiso 1 1 calc R . . . .
C16 C 0.1457(16) 0.6357(16) 0.6350(3) 0.059(6) Uani 1 1 d . . . . .
C17 C 0.0992(13) 0.6222(12) 0.6161(3) 0.043(4) Uani 1 1 d . . . . .
H17 H 0.0347 0.6322 0.6150 0.052 Uiso 1 1 calc R . . . .
C18 C 0.1527(14) 0.5928(14) 0.5985(3) 0.048(5) Uani 1 1 d . . . . .
C19 C 0.3026(17) 0.8683(16) 0.4746(3) 0.063(6) Uani 1 1 d D . . . .
C20 C 0.1420(17) 0.6813(16) 0.5290(3) 0.052(6) Uani 1 1 d . . . . .
C21 C 0.0990(13) 0.5719(16) 0.5777(3) 0.053(5) Uani 1 1 d . . . . .
C22 C 0.0940(19) 0.6591(16) 0.6540(3) 0.064(6) Uani 1 1 d . . . . .
C23 C 0.0000 1.0000 0.4430(6) 0.102(10) Uani 1 2 d S TU P . .
H23 H 0.0000 1.0000 0.4283 0.122 Uiso 1 2 calc RS T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 Eu2 4.1892(10) 2_675 ?
Eu1 O1 2.238(14) . ?
Eu1 O1 2.238(14) 2_675 ?
Eu1 O1W 2.402(15) . ?
Eu1 O4 2.313(13) 3_566 ?
Eu1 O4 2.313(13) 4_666 ?
Eu1 O5 2.783(11) 3_566 ?
Eu1 O5 2.783(11) 4_666 ?
Eu1 O6 2.469(10) 4_666 ?
Eu1 O6 2.469(10) 3_566 ?
Eu1 C21 2.95(2) 3_566 ?
Eu1 C21 2.95(2) 4_666 ?
Eu2 O1 2.954(16) . ?
Eu2 O2 2.282(15) . ?
Eu2 O2W 2.384(14) . ?
Eu2 O3 2.386(15) 4_666 ?
Eu2 O3W 2.52(2) . ?
Eu2 O5 2.348(11) 4_666 ?
Eu2 O7 2.541(14) 8_464 ?
Eu2 O8 2.413(11) 8_464 ?
Eu2 O9 2.284(19) . ?
Eu2 C19 3.03(2) . ?
Eu2 C22 2.85(2) 8_464 ?
O1 C19 1.30(2) . ?
O1W H1W 0.9176 . ?
O2 C19 1.31(3) . ?
O2W H2WA 0.8498 . ?
O2W H2WB 0.8893 . ?
O3 Eu2 2.386(14) 3_466 ?
O3 C20 1.19(2) . ?
O3W H3WA 0.9712 . ?
O3W H3WB 0.9712 . ?
O4 Eu1 2.313(13) 3_466 ?
O4 C20 1.26(2) . ?
O5 Eu1 2.783(11) 3_466 ?
O5 Eu2 2.348(11) 3_466 ?
O5 C21 1.22(2) . ?
O6 Eu1 2.469(10) 3_466 ?
O6 C21 1.19(2) . ?
O7 Eu2 2.541(14) 16_354 ?
O7 C22 1.27(2) . ?
O8 Eu2 2.413(11) 16_354 ?
O8 C22 1.34(3) . ?
O9 C23 1.21(2) . ?
C1 C2 1.26(3) . ?
C1 C6 1.44(3) . ?
C1 C19 1.54(2) . ?
C2 H2 0.9300 . ?
C2 C3 1.41(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.47(3) . ?
C4 C5 1.39(3) . ?
C4 C7 1.47(3) . ?
C5 C6 1.33(3) . ?
C5 C20 1.53(3) . ?
C6 H6 0.9300 . ?
C7 C8 1.34(3) . ?
C7 C12 1.41(2) . ?
C8 H8 0.9300 . ?
C8 C9 1.37(3) . ?
C9 H9 0.9300 . ?
C9 C10 1.34(3) . ?
C10 H10 0.9300 . ?
C10 C11 1.39(3) . ?
C11 C12 1.33(3) . ?
C11 C13 1.43(2) . ?
C12 H12 0.9300 . ?
C13 C14 1.47(2) . ?
C13 C18 1.35(3) . ?
C14 H14 0.9300 . ?
C14 C15 1.34(3) . ?
C15 H15 0.9300 . ?
C15 C16 1.34(3) . ?
C16 C17 1.38(2) . ?
C16 C22 1.45(3) . ?
C17 H17 0.9300 . ?
C17 C18 1.42(3) . ?
C18 C21 1.55(3) . ?
C21 Eu1 2.95(2) 3_466 ?
C22 Eu2 2.85(2) 16_354 ?
C23 Eu2 3.181(4) 2_575 ?
C23 O9 1.21(2) 2_575 ?
C23 H23 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Eu1 Eu2 147.7(4) . 2_675 ?
O1 Eu1 Eu2 42.5(4) 2_675 2_675 ?
O1 Eu1 O1 161.0(7) . 2_675 ?
O1 Eu1 O1W 80.5(4) 2_675 . ?
O1 Eu1 O1W 80.5(4) . . ?
O1 Eu1 O4 85.3(6) . 4_666 ?
O1 Eu1 O4 89.0(6) . 3_566 ?
O1 Eu1 O4 89.0(6) 2_675 4_666 ?
O1 Eu1 O4 85.3(6) 2_675 3_566 ?
O1 Eu1 O5 73.2(5) 2_675 3_566 ?
O1 Eu1 O5 73.2(5) . 4_666 ?
O1 Eu1 O5 121.4(4) . 3_566 ?
O1 Eu1 O5 121.4(4) 2_675 4_666 ?
O1 Eu1 O6 74.7(5) . 3_566 ?
O1 Eu1 O6 120.9(5) . 4_666 ?
O1 Eu1 O6 120.9(5) 2_675 3_566 ?
O1 Eu1 O6 74.7(5) 2_675 4_666 ?
O1 Eu1 C21 97.7(5) 2_675 4_666 ?
O1 Eu1 C21 97.7(5) . 3_566 ?
O1 Eu1 C21 97.6(6) . 4_666 ?
O1 Eu1 C21 97.6(6) 2_675 3_566 ?
O1W Eu1 Eu2 109.052(17) . 2_675 ?
O1W Eu1 O5 134.8(2) . 3_566 ?
O1W Eu1 O5 134.8(2) . 4_666 ?
O1W Eu1 O6 139.1(3) . 4_666 ?
O1W Eu1 O6 139.1(3) . 3_566 ?
O1W Eu1 C21 143.9(4) . 3_566 ?
O1W Eu1 C21 143.9(4) . 4_666 ?
O4 Eu1 Eu2 66.2(3) 3_566 2_675 ?
O4 Eu1 Eu2 126.9(4) 4_666 2_675 ?
O4 Eu1 O1W 72.5(3) 3_566 . ?
O4 Eu1 O1W 72.5(3) 4_666 . ?
O4 Eu1 O4 145.0(7) 4_666 3_566 ?
O4 Eu1 O5 141.0(4) 4_666 3_566 ?
O4 Eu1 O5 141.0(4) 3_566 4_666 ?
O4 Eu1 O5 69.3(4) 3_566 3_566 ?
O4 Eu1 O5 69.3(4) 4_666 4_666 ?
O4 Eu1 O6 135.4(5) 4_666 3_566 ?
O4 Eu1 O6 75.1(5) 3_566 3_566 ?
O4 Eu1 O6 135.4(5) 3_566 4_666 ?
O4 Eu1 O6 75.1(5) 4_666 4_666 ?
O4 Eu1 C21 71.4(5) 3_566 3_566 ?
O4 Eu1 C21 143.6(5) 4_666 3_566 ?
O4 Eu1 C21 143.6(5) 3_566 4_666 ?
O4 Eu1 C21 71.4(5) 4_666 4_666 ?
O5 Eu1 Eu2 32.0(2) 3_566 2_675 ?
O5 Eu1 Eu2 112.8(2) 4_666 2_675 ?
O5 Eu1 O5 90.4(4) 4_666 3_566 ?
O5 Eu1 C21 24.3(4) 3_566 3_566 ?
O5 Eu1 C21 76.9(4) 4_666 3_566 ?
O5 Eu1 C21 24.3(4) 4_666 4_666 ?
O5 Eu1 C21 76.9(4) 3_566 4_666 ?
O6 Eu1 Eu2 79.0(3) 3_566 2_675 ?
O6 Eu1 Eu2 72.4(3) 4_666 2_675 ?
O6 Eu1 O5 47.7(4) 3_566 3_566 ?
O6 Eu1 O5 66.9(3) 4_666 3_566 ?
O6 Eu1 O5 47.7(4) 4_666 4_666 ?
O6 Eu1 O5 66.9(3) 3_566 4_666 ?
O6 Eu1 O6 81.7(5) 3_566 4_666 ?
O6 Eu1 C21 72.3(4) 3_566 4_666 ?
O6 Eu1 C21 72.3(4) 4_666 3_566 ?
O6 Eu1 C21 23.3(4) 4_666 4_666 ?
O6 Eu1 C21 23.3(4) 3_566 3_566 ?
C21 Eu1 Eu2 56.0(4) 3_566 2_675 ?
C21 Eu1 Eu2 91.8(4) 4_666 2_675 ?
C21 Eu1 C21 72.3(7) 3_566 4_666 ?
O1 Eu2 Eu1 30.8(3) . . ?
O1 Eu2 C19 25.1(5) . . ?
O2 Eu2 Eu1 78.4(4) . . ?
O2 Eu2 O1 48.5(5) . . ?
O2 Eu2 O2W 84.4(6) . . ?
O2 Eu2 O3 81.7(5) . 4_666 ?
O2 Eu2 O3W 72.1(7) . . ?
O2 Eu2 O5 117.0(5) . 4_666 ?
O2 Eu2 O7 149.8(6) . 8_464 ?
O2 Eu2 O8 146.0(7) . 8_464 ?
O2 Eu2 O9 79.1(7) . . ?
O2 Eu2 C19 23.4(5) . . ?
O2 Eu2 C22 160.6(6) . 8_464 ?
O2W Eu2 Eu1 73.4(3) . . ?
O2W Eu2 O1 68.2(4) . . ?
O2W Eu2 O3 135.5(5) . 4_666 ?
O2W Eu2 O3W 68.0(7) . . ?
O2W Eu2 O7 125.9(4) . 8_464 ?
O2W Eu2 O8 79.2(6) . 8_464 ?
O2W Eu2 C19 75.3(6) . . ?
O2W Eu2 C22 104.4(6) . 8_464 ?
O3 Eu2 Eu1 62.5(3) 4_666 . ?
O3 Eu2 O1 71.0(4) 4_666 . ?
O3 Eu2 O3W 143.1(6) 4_666 . ?
O3 Eu2 O7 76.1(5) 4_666 8_464 ?
O3 Eu2 O8 130.0(7) 4_666 8_464 ?
O3 Eu2 C19 75.3(6) 4_666 . ?
O3 Eu2 C22 102.5(6) 4_666 8_464 ?
O3W Eu2 Eu1 132.9(6) . . ?
O3W Eu2 O1 107.1(7) . . ?
O3W Eu2 O7 115.9(6) . 8_464 ?
O3W Eu2 C19 89.0(7) . . ?
O3W Eu2 C22 94.8(7) . 8_464 ?
O5 Eu2 Eu1 38.9(3) 4_666 . ?
O5 Eu2 O1 68.5(4) 4_666 . ?
O5 Eu2 O2W 74.5(4) 4_666 . ?
O5 Eu2 O3 74.8(4) 4_666 4_666 ?
O5 Eu2 O3W 140.4(6) 4_666 . ?
O5 Eu2 O7 76.7(5) 4_666 8_464 ?
O5 Eu2 O8 87.0(5) 4_666 8_464 ?
O5 Eu2 C19 93.6(5) 4_666 . ?
O5 Eu2 C22 82.3(5) 4_666 8_464 ?
O7 Eu2 Eu1 108.2(4) 8_464 . ?
O7 Eu2 O1 136.9(5) 8_464 . ?
O7 Eu2 C19 151.3(6) 8_464 . ?
O7 Eu2 C22 26.5(5) 8_464 8_464 ?
O8 Eu2 Eu1 123.7(4) 8_464 . ?
O8 Eu2 O1 143.1(5) 8_464 . ?
O8 Eu2 O3W 74.2(7) 8_464 . ?
O8 Eu2 O7 54.4(6) 8_464 8_464 ?
O8 Eu2 C19 153.3(7) 8_464 . ?
O8 Eu2 C22 28.0(6) 8_464 8_464 ?
O9 Eu2 Eu1 136.8(5) . . ?
O9 Eu2 O1 121.4(6) . . ?
O9 Eu2 O2W 139.6(7) . . ?
O9 Eu2 O3 78.2(7) . 4_666 ?
O9 Eu2 O3W 71.9(9) . . ?
O9 Eu2 O5 145.6(7) . 4_666 ?
O9 Eu2 O7 76.5(7) . 8_464 ?
O9 Eu2 O8 94.6(6) . 8_464 ?
O9 Eu2 C19 99.8(7) . . ?
O9 Eu2 C22 83.2(7) . 8_464 ?
C19 Eu2 Eu1 55.2(4) . . ?
C22 Eu2 Eu1 120.6(4) 8_464 . ?
C22 Eu2 O1 150.8(5) 8_464 . ?
C22 Eu2 C19 175.8(6) 8_464 . ?
Eu1 O1 Eu2 106.8(6) . . ?
C19 O1 Eu1 162.4(15) . . ?
C19 O1 Eu2 80.8(12) . . ?
Eu1 O1W H1W 125.5 . . ?
C19 O2 Eu2 112.5(11) . . ?
Eu2 O2W H2WA 120.7 . . ?
Eu2 O2W H2WB 111.1 . . ?
H2WA O2W H2WB 109.0 . . ?
C20 O3 Eu2 140.3(13) . 3_466 ?
Eu2 O3W H3WA 125.8 . . ?
Eu2 O3W H3WB 125.5 . . ?
H3WA O3W H3WB 108.7 . . ?
C20 O4 Eu1 137.7(14) . 3_466 ?
Eu2 O5 Eu1 109.2(4) 3_466 3_466 ?
C21 O5 Eu1 85.5(12) . 3_466 ?
C21 O5 Eu2 161.3(13) . 3_466 ?
C21 O6 Eu1 101.6(11) . 3_466 ?
C22 O7 Eu2 90.5(14) . 16_354 ?
C22 O8 Eu2 94.5(11) . 16_354 ?
C23 O9 Eu2 129(2) . . ?
C2 C1 C6 122.7(18) . . ?
C2 C1 C19 122(2) . . ?
C6 C1 C19 113.9(19) . . ?
C1 C2 H2 119.9 . . ?
C1 C2 C3 120.3(18) . . ?
C3 C2 H2 119.9 . . ?
C2 C3 H3 120.6 . . ?
C2 C3 C4 119(2) . . ?
C4 C3 H3 120.6 . . ?
C3 C4 C7 116(2) . . ?
C5 C4 C3 117(2) . . ?
C5 C4 C7 126.4(18) . . ?
C4 C5 C20 122.8(17) . . ?
C6 C5 C4 121(2) . . ?
C6 C5 C20 116.1(19) . . ?
C1 C6 H6 120.4 . . ?
C5 C6 C1 119(2) . . ?
C5 C6 H6 120.4 . . ?
C8 C7 C4 123.0(19) . . ?
C8 C7 C12 114.1(18) . . ?
C12 C7 C4 122.0(18) . . ?
C7 C8 H8 119.2 . . ?
C7 C8 C9 122(2) . . ?
C9 C8 H8 119.2 . . ?
C8 C9 H9 119.9 . . ?
C10 C9 C8 120(2) . . ?
C10 C9 H9 119.9 . . ?
C9 C10 H10 118.8 . . ?
C9 C10 C11 122(2) . . ?
C11 C10 H10 118.8 . . ?
C10 C11 C13 124(2) . . ?
C12 C11 C10 113.7(18) . . ?
C12 C11 C13 122.2(18) . . ?
C7 C12 H12 116.3 . . ?
C11 C12 C7 127.4(18) . . ?
C11 C12 H12 116.3 . . ?
C11 C13 C14 123.0(18) . . ?
C18 C13 C11 121.5(16) . . ?
C18 C13 C14 115.5(17) . . ?
C13 C14 H14 121.4 . . ?
C15 C14 C13 117.2(19) . . ?
C15 C14 H14 121.4 . . ?
C14 C15 H15 116.4 . . ?
C14 C15 C16 127.2(19) . . ?
C16 C15 H15 116.4 . . ?
C15 C16 C17 117.5(19) . . ?
C15 C16 C22 121.7(18) . . ?
C17 C16 C22 120.7(19) . . ?
C16 C17 H17 121.0 . . ?
C16 C17 C18 118.0(17) . . ?
C18 C17 H17 121.0 . . ?
C13 C18 C17 124.3(16) . . ?
C13 C18 C21 118.0(17) . . ?
C17 C18 C21 117.6(17) . . ?
O1 C19 Eu2 74.1(11) . . ?
O1 C19 O2 118.1(17) . . ?
O1 C19 C1 121(2) . . ?
O2 C19 Eu2 44.0(8) . . ?
O2 C19 C1 119.8(18) . . ?
C1 C19 Eu2 162.1(16) . . ?
O3 C20 O4 128(2) . . ?
O3 C20 C5 116.7(19) . . ?
O4 C20 C5 116(2) . . ?
O5 C21 Eu1 70.1(11) . 3_466 ?
O5 C21 C18 118.1(19) . . ?
O6 C21 Eu1 55.1(10) . 3_466 ?
O6 C21 O5 125.1(19) . . ?
O6 C21 C18 116.8(16) . . ?
C18 C21 Eu1 170.7(14) . 3_466 ?
O7 C22 Eu2 63.0(11) . 16_354 ?
O7 C22 O8 120(2) . . ?
O7 C22 C16 121(2) . . ?
O8 C22 Eu2 57.5(10) . 16_354 ?
O8 C22 C16 117.2(17) . . ?
C16 C22 Eu2 173.0(17) . 16_354 ?
Eu2 C23 H23 84.6 2_575 . ?
O9 C23 Eu2 34.1(14) 2_575 2_575 ?
O9 C23 Eu2 156(2) . 2_575 ?
O9 C23 O9 128(4) . 2_575 ?
O9 C23 H23 115.9 . . ?
O9 C23 H23 115.9 2_575 . ?

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
Eu1 O1 C19 Eu2 117(5) . . . . ?
Eu1 O1 C19 O2 117(5) . . . . ?
Eu1 O1 C19 C1 -73(6) . . . . ?
Eu1 O4 C20 O3 0(3) 3_466 . . . ?
Eu1 O4 C20 C5 -178.1(12) 3_466 . . . ?
Eu1 O5 C21 O6 3.7(19) 3_466 . . . ?
Eu1 O5 C21 C18 -175.3(16) 3_466 . . . ?
Eu1 O6 C21 O5 -4(2) 3_466 . . . ?
Eu1 O6 C21 C18 174.8(13) 3_466 . . . ?
Eu2 O1 C19 O2 0(2) . . . . ?
Eu2 O1 C19 C1 170(2) . . . . ?
Eu2 O2 C19 O1 0(3) . . . . ?
Eu2 O2 C19 C1 -170.2(16) . . . . ?
Eu2 O3 C20 O4 31(4) 3_466 . . . ?
Eu2 O3 C20 C5 -150.8(15) 3_466 . . . ?
Eu2 O5 C21 Eu1 -143(4) 3_466 . . 3_466 ?
Eu2 O5 C21 O6 -139(3) 3_466 . . . ?
Eu2 O5 C21 C18 42(4) 3_466 . . . ?
Eu2 O7 C22 O8 6(2) 16_354 . . . ?
Eu2 O7 C22 C16 174(2) 16_354 . . . ?
Eu2 O8 C22 O7 -7(2) 16_354 . . . ?
Eu2 O8 C22 C16 -174.6(17) 16_354 . . . ?
Eu2 O9 C23 Eu2 -170(3) . . . 2_575 ?
Eu2 O9 C23 O9 155(3) . . . 2_575 ?
C1 C2 C3 C4 -5(3) . . . . ?
C2 C1 C6 C5 -11(3) . . . . ?
C2 C1 C19 Eu2 144(4) . . . . ?
C2 C1 C19 O1 -3(4) . . . . ?
C2 C1 C19 O2 167(2) . . . . ?
C2 C3 C4 C5 1(3) . . . . ?
C2 C3 C4 C7 -175.7(19) . . . . ?
C3 C4 C5 C6 -3(3) . . . . ?
C3 C4 C5 C20 177.5(19) . . . . ?
C3 C4 C7 C8 -56(3) . . . . ?
C3 C4 C7 C12 135(2) . . . . ?
C4 C5 C6 C1 8(3) . . . . ?
C4 C5 C20 O3 127(2) . . . . ?
C4 C5 C20 O4 -54(3) . . . . ?
C4 C7 C8 C9 -179(2) . . . . ?
C4 C7 C12 C11 179(2) . . . . ?
C5 C4 C7 C8 127(2) . . . . ?
C5 C4 C7 C12 -42(3) . . . . ?
C6 C1 C2 C3 10(3) . . . . ?
C6 C1 C19 Eu2 -47(6) . . . . ?
C6 C1 C19 O1 165(2) . . . . ?
C6 C1 C19 O2 -25(3) . . . . ?
C6 C5 C20 O3 -52(3) . . . . ?
C6 C5 C20 O4 127(2) . . . . ?
C7 C4 C5 C6 173(2) . . . . ?
C7 C4 C5 C20 -6(3) . . . . ?
C7 C8 C9 C10 6(4) . . . . ?
C8 C7 C12 C11 9(3) . . . . ?
C8 C9 C10 C11 -1(4) . . . . ?
C9 C10 C11 C12 0(4) . . . . ?
C9 C10 C11 C13 174(2) . . . . ?
C10 C11 C12 C7 -5(3) . . . . ?
C10 C11 C13 C14 65(3) . . . . ?
C10 C11 C13 C18 -116(3) . . . . ?
C11 C13 C14 C15 177(2) . . . . ?
C11 C13 C18 C17 -173(2) . . . . ?
C11 C13 C18 C21 5(3) . . . . ?
C12 C7 C8 C9 -10(3) . . . . ?
C12 C11 C13 C14 -122(2) . . . . ?
C12 C11 C13 C18 56(3) . . . . ?
C13 C11 C12 C7 -177.9(19) . . . . ?
C13 C14 C15 C16 -2(4) . . . . ?
C13 C18 C21 O5 -127(2) . . . . ?
C13 C18 C21 O6 54(3) . . . . ?
C14 C13 C18 C17 6(3) . . . . ?
C14 C13 C18 C21 -176.6(18) . . . . ?
C14 C15 C16 C17 2(4) . . . . ?
C14 C15 C16 C22 179(2) . . . . ?
C15 C16 C17 C18 2(3) . . . . ?
C15 C16 C22 O7 8(4) . . . . ?
C15 C16 C22 O8 176(2) . . . . ?
C16 C17 C18 C13 -6(3) . . . . ?
C16 C17 C18 C21 176.3(18) . . . . ?
C17 C16 C22 O7 -175(2) . . . . ?
C17 C16 C22 O8 -7(3) . . . . ?
C17 C18 C21 O5 51(2) . . . . ?
C17 C18 C21 O6 -128(2) . . . . ?
C18 C13 C14 C15 -2(3) . . . . ?
C19 C1 C2 C3 177(2) . . . . ?
C19 C1 C6 C5 -180(2) . . . . ?
C20 C5 C6 C1 -172.8(18) . . . . ?
C22 C16 C17 C18 -175.5(19) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.91(4)
2 0.09(4)
_vrf_CHEMW03_2-Eu                
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as  
RESPONSE: Some water molecules were squeezed, which gave inconsitent formula
from _atom_site_*.
;

_vrf_PLAT420_2-Eu                
;
PROBLEM: D-H Without Acceptor       O1W    --  H1WA   ...     Please Check   
RESPONSE: Some accepters for these hydrogens couldn??t located because the 
water molecules which can be the acceptors were squeezed.
;

_vrf_PLAT342_2-Eu                
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.03 Ang.   
RESPONSE: The low bond precision was caused by the inversion twin.
;

####################################################################### 
# 
# 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_3-Tb
_database_code_depnum_ccdc_archive 'CCDC 1442621'
_audit_update_record             
;
2016-10-24 deposited with the CCDC.
2016-10-31 downloaded from the CCDC.
;
_audit_creation_date             2016-10-22
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C45 H31 O23 Tb3, 12(H2 O)'
_chemical_formula_sum            'C45 H55 O35 Tb3'
_chemical_formula_weight         1632.65
_chemical_absolute_configuration .
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_H-M_alt        'I -4 2 d'
_space_group_name_Hall           'I -4 2bw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y, -z+3/4'
'x+1/2, -y, -z+3/4'
'-y+1/2, -x, z+3/4'
'y+1/2, x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1, y+1/2, -z+5/4'
'x+1, -y+1/2, -z+5/4'
'-y+1, -x+1/2, z+5/4'
'y+1, x+1/2, z+5/4'

_cell_length_a                   14.1842(14)
_cell_length_b                   14.1842(14)
_cell_length_c                   63.709(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     12818(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9846
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      26.726
_cell_measurement_theta_min      3.124
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.363
_exptl_absorpt_correction_T_max  0.7395
_exptl_absorpt_correction_T_min  0.5229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1331 before and 0.1100 after correction.
The Ratio of minimum to maximum transmission is 0.7071.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             6400
_exptl_crystal_size_max          0.291
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.093
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2025
_diffrn_reflns_av_unetI/netI     0.0789
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       79
_diffrn_reflns_limit_l_min       -79
_diffrn_reflns_number            84991
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         2.943
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.831
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                5611
_reflns_number_total             6562
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2015)'
_refine_diff_density_max         1.821
_refine_diff_density_min         -2.192
_refine_diff_density_rms         0.237
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.20(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         6562
_refine_ls_number_restraints     344
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0815
_refine_ls_restrained_S_all      1.087
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0433P)²+667.8850P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1772
_refine_ls_wR_factor_ref         0.1842
_refine_special_details          
;
 Refined as a 2-component inversion twin.
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.

 The refinement was performed by a routine procedure with 
 SHELXL 2014. All the  hydrogens on carbon atoms were placed
 on calculated positions.  All the hydrogens on water 
 molecules were placed on proper positions and fixed by AFIX 3.

 The highly disordered crystallisation water molecules couldn't 
 located from Q-maps, so the SQUEEZE function in PLATON program
 was performed. And TG experiment was used to 
 
 The TGA curve displays a weight loss of 18.7% below 448 K, 
 consistent with the loss of 12 molecules of crystallisation 
 water (disordered, treated using PLATON SQUEEZE solvent mask)
 and 5 molecules of coordinated water per formula unit
 (calculated loss 18.8%).

 Some alerts caused by SQUEEZE were explained by _vrf_PLAT
 in CIF files.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.80(5) 0.20(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
3. Restrained distances
 C5-C20
 1.4 with sigma of 0.02
 C19-C1
 1.4 with sigma of 0.02
 O9-O2WA
 2.6 with sigma of 0.02
 O1W-O2W
 2.6 with sigma of 0.02
 O2W-Tb2 \\sim Tb2-O2WA
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O4) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O2WA)=Sof(H2WC)=Sof(H2WD)=1-FVAR(1)
 Sof(O2W)=Sof(H2WA)=Sof(H2WB)=FVAR(1)
7.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O2WA(H2WC,H2WD), O3W(H3W)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C8(H8), C9(H9), C10(H10), C12(H12), C14(H14),
 C15(H15), C17(H17), C23(H23)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 1.0000 0.0000 0.29020(2) 0.0209(3) Uani 1 2 d S TU P . .
Tb2 Tb 1.51608(10) 0.27873(8) 0.06209(2) 0.0447(4) Uani 1 1 d D U . . .
O1 O 1.1278(13) 0.0921(13) 0.2843(3) 0.043(4) Uani 1 1 d . U . . .
O1W O 1.6415(15) 0.1946(14) 0.0777(3) 0.060(5) Uani 1 1 d D U . . .
H1WA H 1.6954 0.2229 0.0752 0.090 Uiso 1 1 d R . . . .
H1WB H 1.6452 0.1370 0.0727 0.090 Uiso 1 1 d R . . . .
O2 O 1.2843(13) 0.1150(16) 0.2828(3) 0.055(5) Uani 1 1 d . U . . .
O2W O 1.657(3) 0.366(3) 0.0658(10) 0.088(11) Uani 0.47(6) 1 d D U . A 1
H2WA H 1.6925 0.3845 0.0567 0.131 Uiso 0.47(6) 1 d R . . A 1
H2WB H 1.6640 0.4027 0.0769 0.131 Uiso 0.47(6) 1 d R . . A 1
O2WA O 1.616(3) 0.400(3) 0.0736(7) 0.085(10) Uani 0.53(6) 1 d D U . A 2
H2WC H 1.6335 0.4235 0.0859 0.128 Uiso 0.53(6) 1 d R . . A 2
H2WD H 1.6553 0.4180 0.0651 0.128 Uiso 0.53(6) 1 d R . . A 2
O3 O 1.4032(12) 0.2550(12) 0.2148(3) 0.040(4) Uani 1 1 d . U . . .
O3W O 1.0000 0.0000 0.2524(3) 0.068(7) Uani 1 2 d S TU P . .
H3W H 1.0361 0.0292 0.2443 0.102 Uiso 1 1 d R . . . .
O4 O 1.3751(12) 0.4039(12) 0.2204(2) 0.032(3) Uani 1 1 d . U . . .
O5 O 1.3901(10) 0.5055(13) 0.18059(18) 0.030(3) Uani 1 1 d . U . . .
O6 O 1.4598(9) 0.3677(9) 0.1791(2) 0.020(3) Uani 1 1 d . U . . .
O7 O 1.498(2) 0.3227(12) 0.0983(2) 0.054(4) Uani 1 1 d . U . . .
O8 O 1.3582(13) 0.3178(13) 0.0791(2) 0.043(4) Uani 1 1 d . U . . .
O9 O 1.4686(18) 0.4322(15) 0.0515(3) 0.083(6) Uani 1 1 d D U . . .
C1 C 1.1923(18) 0.2058(17) 0.2588(3) 0.038(5) Uani 1 1 d D U . . .
C2 C 1.1099(18) 0.234(2) 0.2540(3) 0.044(6) Uani 1 1 d . U . . .
H2 H 1.0584 0.2107 0.2614 0.053 Uiso 1 1 calc R . . . .
C3 C 1.095(2) 0.302(2) 0.2368(4) 0.051(7) Uani 1 1 d . U . . .
H3 H 1.0357 0.3257 0.2334 0.061 Uiso 1 1 calc R . . . .
C4 C 1.1829(19) 0.329(2) 0.2255(3) 0.041(5) Uani 1 1 d . U . . .
C5 C 1.2631(16) 0.2910(17) 0.2310(3) 0.034(4) Uani 1 1 d D U . . .
C6 C 1.274(2) 0.227(2) 0.2477(5) 0.057(7) Uani 1 1 d . U . . .
H6 H 1.3320 0.2000 0.2511 0.068 Uiso 1 1 calc R . . . .
C7 C 1.1665(17) 0.3991(19) 0.2079(3) 0.037(5) Uani 1 1 d . U . . .
C8 C 1.1191(15) 0.4822(19) 0.2092(3) 0.039(5) Uani 1 1 d . U . . .
H8 H 1.0959 0.5007 0.2222 0.047 Uiso 1 1 calc R . . . .
C9 C 1.104(2) 0.540(2) 0.1925(4) 0.069(9) Uani 1 1 d . U . . .
H9 H 1.0661 0.5931 0.1933 0.082 Uiso 1 1 calc R . . . .
C10 C 1.149(2) 0.512(3) 0.1739(4) 0.084(11) Uani 1 1 d . U . . .
H10 H 1.1424 0.5512 0.1624 0.101 Uiso 1 1 calc R . . . .
C11 C 1.2005(19) 0.436(2) 0.1713(4) 0.051(6) Uani 1 1 d . U . . .
C12 C 1.2052(17) 0.379(2) 0.1880(4) 0.051(6) Uani 1 1 d . U . . .
H12 H 1.2364 0.3217 0.1864 0.061 Uiso 1 1 calc R . . . .
C13 C 1.2526(18) 0.415(2) 0.1516(3) 0.042(5) Uani 1 1 d . U . . .
C14 C 1.1992(19) 0.403(2) 0.1321(3) 0.043(6) Uani 1 1 d . U . . .
H14 H 1.1343 0.4108 0.1309 0.052 Uiso 1 1 calc R . . . .
C15 C 1.260(2) 0.378(2) 0.1152(4) 0.048(6) Uani 1 1 d . U . . .
H15 H 1.2311 0.3692 0.1022 0.057 Uiso 1 1 calc R . . . .
C16 C 1.3497(19) 0.3650(17) 0.1159(3) 0.034(4) Uani 1 1 d . U . . .
C17 C 1.3981(18) 0.3799(15) 0.1343(3) 0.030(4) Uani 1 1 d . U . . .
H17 H 1.4631 0.3720 0.1351 0.036 Uiso 1 1 calc R . . . .
C18 C 1.3439(17) 0.4084(17) 0.1523(3) 0.034(5) Uani 1 1 d . U . . .
C19 C 1.1990(18) 0.1344(18) 0.2753(3) 0.036(5) Uani 1 1 d D U . . .
C20 C 1.3533(16) 0.3207(18) 0.2209(3) 0.034(4) Uani 1 1 d D U . . .
C21 C 1.4029(15) 0.4258(15) 0.1720(3) 0.023(4) Uani 1 1 d . U . . .
C22 C 1.402(2) 0.3383(19) 0.0964(4) 0.043(5) Uani 1 1 d . U . . .
C23 C 1.5000 0.5000 0.0586(8) 0.094(14) Uani 1 2 d S TU P . .
H23 H 1.5000 0.5000 0.0732 0.113 Uiso 1 2 calc RS T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O1 2.266(17) . ?
Tb1 O1 2.266(17) 2_755 ?
Tb1 O3W 2.41(2) . ?
Tb1 O4 2.333(16) 12_635 ?
Tb1 O4 2.333(16) 11_565 ?
Tb1 O5 2.429(12) 11_565 ?
Tb1 O5 2.429(12) 12_635 ?
Tb1 O6 2.769(13) 12_635 ?
Tb1 O6 2.769(13) 11_565 ?
Tb1 C21 2.97(2) 11_565 ?
Tb1 C21 2.97(2) 12_635 ?
Tb2 O1W 2.36(2) . ?
Tb2 O2 2.334(16) 8_644 ?
Tb2 O2W 2.36(3) . ?
Tb2 O2WA 2.35(3) . ?
Tb2 O3 2.393(16) 14_454 ?
Tb2 O6 2.294(13) 14_454 ?
Tb2 O7 2.405(13) . ?
Tb2 O8 2.549(18) . ?
Tb2 O9 2.38(2) . ?
Tb2 C22 2.85(3) . ?
O1 C19 1.31(3) . ?
O1W H1WA 0.8768 . ?
O1W H1WB 0.8777 . ?
O2 Tb2 2.334(16) 16_534 ?
O2 C19 1.33(3) . ?
O2W H2WA 0.8134 . ?
O2W H2WB 0.8830 . ?
O2WA H2WC 0.8819 . ?
O2WA H2WD 0.8216 . ?
O3 Tb2 2.393(16) 14_454 ?
O3 C20 1.23(3) . ?
O3W H3W 0.8351 . ?
O4 Tb1 2.333(16) 11_665 ?
O4 C20 1.22(3) . ?
O5 Tb1 2.429(12) 11_665 ?
O5 C21 1.27(3) . ?
O6 Tb1 2.769(13) 11_665 ?
O6 Tb2 2.294(13) 14_454 ?
O6 C21 1.24(2) . ?
O7 C22 1.40(4) . ?
O8 C22 1.30(3) . ?
O9 C23 1.15(3) . ?
C1 C2 1.27(4) . ?
C1 C6 1.39(4) . ?
C1 C19 1.46(2) . ?
C2 H2 0.9300 . ?
C2 C3 1.47(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.50(4) . ?
C4 C5 1.30(4) . ?
C4 C7 1.52(3) . ?
C5 C6 1.41(3) . ?
C5 C20 1.49(2) . ?
C6 H6 0.9300 . ?
C7 C8 1.36(4) . ?
C7 C12 1.41(3) . ?
C8 H8 0.9300 . ?
C8 C9 1.36(3) . ?
C9 H9 0.9300 . ?
C9 C10 1.41(3) . ?
C10 H10 0.9300 . ?
C10 C11 1.31(4) . ?
C11 C12 1.34(3) . ?
C11 C13 1.48(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.47(3) . ?
C13 C18 1.30(3) . ?
C14 H14 0.9300 . ?
C14 C15 1.42(3) . ?
C15 H15 0.9300 . ?
C15 C16 1.29(4) . ?
C16 C17 1.38(3) . ?
C16 C22 1.49(3) . ?
C17 H17 0.9300 . ?
C17 C18 1.44(3) . ?
C18 C21 1.53(3) . ?
C21 Tb1 2.97(2) 11_665 ?
C23 O9 1.15(3) 2_865 ?
C23 H23 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Tb1 O1 160.9(9) . 2_755 ?
O1 Tb1 O3W 80.4(4) 2_755 . ?
O1 Tb1 O3W 80.4(4) . . ?
O1 Tb1 O4 89.0(7) . 11_565 ?
O1 Tb1 O4 85.6(7) . 12_635 ?
O1 Tb1 O4 89.0(7) 2_755 12_635 ?
O1 Tb1 O4 85.6(7) 2_755 11_565 ?
O1 Tb1 O5 74.4(6) . 11_565 ?
O1 Tb1 O5 74.4(6) 2_755 12_635 ?
O1 Tb1 O5 121.5(6) . 12_635 ?
O1 Tb1 O5 121.5(6) 2_755 11_565 ?
O1 Tb1 O6 72.2(5) . 12_635 ?
O1 Tb1 O6 122.7(5) . 11_565 ?
O1 Tb1 O6 122.7(5) 2_755 12_635 ?
O1 Tb1 O6 72.2(5) 2_755 11_565 ?
O1 Tb1 C21 98.7(6) . 11_565 ?
O1 Tb1 C21 96.8(6) . 12_635 ?
O1 Tb1 C21 96.8(6) 2_755 11_565 ?
O1 Tb1 C21 98.7(6) 2_755 12_635 ?
O3W Tb1 O5 140.0(3) . 12_635 ?
O3W Tb1 O5 140.0(3) . 11_565 ?
O3W Tb1 O6 134.9(3) . 12_635 ?
O3W Tb1 O6 134.9(3) . 11_565 ?
O3W Tb1 C21 144.2(4) . 11_565 ?
O3W Tb1 C21 144.2(4) . 12_635 ?
O4 Tb1 O3W 73.3(4) 12_635 . ?
O4 Tb1 O3W 73.3(4) 11_565 . ?
O4 Tb1 O4 146.5(7) 12_635 11_565 ?
O4 Tb1 O5 75.7(5) 11_565 11_565 ?
O4 Tb1 O5 133.5(6) 11_565 12_635 ?
O4 Tb1 O5 133.5(6) 12_635 11_565 ?
O4 Tb1 O5 75.7(5) 12_635 12_635 ?
O4 Tb1 O6 69.6(5) 12_635 12_635 ?
O4 Tb1 O6 139.1(5) 12_635 11_565 ?
O4 Tb1 O6 69.6(5) 11_565 11_565 ?
O4 Tb1 O6 139.1(5) 11_565 12_635 ?
O4 Tb1 C21 142.5(5) 11_565 12_635 ?
O4 Tb1 C21 71.0(6) 11_565 11_565 ?
O4 Tb1 C21 71.0(6) 12_635 12_635 ?
O4 Tb1 C21 142.5(5) 12_635 11_565 ?
O5 Tb1 O5 80.0(7) 11_565 12_635 ?
O5 Tb1 O6 64.5(5) 11_565 12_635 ?
O5 Tb1 O6 64.5(5) 12_635 11_565 ?
O5 Tb1 O6 49.4(5) 11_565 11_565 ?
O5 Tb1 O6 49.4(5) 12_635 12_635 ?
O5 Tb1 C21 70.4(5) 12_635 11_565 ?
O5 Tb1 C21 24.7(5) 11_565 11_565 ?
O5 Tb1 C21 70.4(5) 11_565 12_635 ?
O5 Tb1 C21 24.7(5) 12_635 12_635 ?
O6 Tb1 O6 90.2(5) 12_635 11_565 ?
O6 Tb1 C21 24.6(5) 12_635 12_635 ?
O6 Tb1 C21 76.3(5) 12_635 11_565 ?
O6 Tb1 C21 76.3(5) 11_565 12_635 ?
O6 Tb1 C21 24.6(5) 11_565 11_565 ?
C21 Tb1 C21 71.5(8) 11_565 12_635 ?
O1W Tb2 O2W 65.3(9) . . ?
O1W Tb2 O3 134.8(6) . 14_454 ?
O1W Tb2 O7 78.8(7) . . ?
O1W Tb2 O8 126.3(6) . . ?
O1W Tb2 O9 142.8(8) . . ?
O1W Tb2 C22 104.8(7) . . ?
O2 Tb2 O1W 84.3(7) 8_644 . ?
O2 Tb2 O2W 63.5(17) 8_644 . ?
O2 Tb2 O2WA 82.1(14) 8_644 . ?
O2 Tb2 O3 80.7(6) 8_644 14_454 ?
O2 Tb2 O7 145.1(8) 8_644 . ?
O2 Tb2 O8 149.4(7) 8_644 . ?
O2 Tb2 O9 84.9(8) 8_644 . ?
O2 Tb2 C22 160.8(7) 8_644 . ?
O2W Tb2 O3 138.0(14) . 14_454 ?
O2W Tb2 O7 81.7(17) . . ?
O2W Tb2 O8 126.0(16) . . ?
O2W Tb2 O9 78.0(11) . . ?
O2W Tb2 C22 104.5(17) . . ?
O2WA Tb2 O1W 77.6(11) . . ?
O2WA Tb2 O3 140.7(10) . 14_454 ?
O2WA Tb2 O7 64.6(14) . . ?
O2WA Tb2 O8 103.7(14) . . ?
O2WA Tb2 O9 65.6(9) . . ?
O2WA Tb2 C22 83.4(14) . . ?
O3 Tb2 O7 132.0(8) 14_454 . ?
O3 Tb2 O8 76.1(6) 14_454 . ?
O3 Tb2 C22 103.1(7) 14_454 . ?
O6 Tb2 O1W 72.7(6) 14_454 . ?
O6 Tb2 O2 115.8(6) 14_454 8_644 ?
O6 Tb2 O2W 137.9(10) 14_454 . ?
O6 Tb2 O2WA 142.9(10) 14_454 . ?
O6 Tb2 O3 76.1(5) 14_454 14_454 ?
O6 Tb2 O7 88.0(6) 14_454 . ?
O6 Tb2 O8 77.7(5) 14_454 . ?
O6 Tb2 O9 143.1(7) 14_454 . ?
O6 Tb2 C22 83.3(6) 14_454 . ?
O7 Tb2 O8 56.2(7) . . ?
O7 Tb2 C22 29.3(8) . . ?
O8 Tb2 C22 27.0(7) . . ?
O9 Tb2 O3 77.8(7) . 14_454 ?
O9 Tb2 O7 90.4(7) . . ?
O9 Tb2 O8 70.9(7) . . ?
O9 Tb2 C22 77.6(8) . . ?
C19 O1 Tb1 162.9(16) . . ?
Tb2 O1W H1WA 110.4 . . ?
Tb2 O1W H1WB 111.3 . . ?
H1WA O1W H1WB 108.0 . . ?
C19 O2 Tb2 112.4(13) . 16_534 ?
Tb2 O2W H2WA 128.3 . . ?
Tb2 O2W H2WB 118.8 . . ?
H2WA O2W H2WB 107.9 . . ?
Tb2 O2WA H2WC 136.1 . . ?
Tb2 O2WA H2WD 115.1 . . ?
H2WC O2WA H2WD 106.5 . . ?
C20 O3 Tb2 139.5(14) . 14_454 ?
Tb1 O3W H3W 127.9 . . ?
C20 O4 Tb1 139.9(15) . 11_665 ?
C21 O5 Tb1 102.1(12) . 11_665 ?
Tb2 O6 Tb1 111.7(5) 14_454 11_665 ?
C21 O6 Tb1 86.6(12) . 11_665 ?
C21 O6 Tb2 156.6(14) . 14_454 ?
C22 O7 Tb2 93.4(13) . . ?
C22 O8 Tb2 89.6(16) . . ?
C23 O9 Tb2 123(2) . . ?
C2 C1 C6 125(2) . . ?
C2 C1 C19 117(2) . . ?
C6 C1 C19 117(2) . . ?
C1 C2 H2 119.5 . . ?
C1 C2 C3 121(2) . . ?
C3 C2 H2 119.5 . . ?
C2 C3 H3 123.1 . . ?
C2 C3 C4 114(2) . . ?
C4 C3 H3 123.1 . . ?
C3 C4 C7 113(2) . . ?
C5 C4 C3 120(2) . . ?
C5 C4 C7 127(2) . . ?
C4 C5 C6 124(2) . . ?
C4 C5 C20 121(2) . . ?
C6 C5 C20 114(2) . . ?
C1 C6 C5 115(2) . . ?
C1 C6 H6 122.3 . . ?
C5 C6 H6 122.3 . . ?
C8 C7 C4 127(2) . . ?
C8 C7 C12 115(2) . . ?
C12 C7 C4 118(2) . . ?
C7 C8 H8 118.2 . . ?
C9 C8 C7 124(2) . . ?
C9 C8 H8 118.2 . . ?
C8 C9 H9 122.6 . . ?
C8 C9 C10 115(3) . . ?
C10 C9 H9 122.6 . . ?
C9 C10 H10 116.8 . . ?
C11 C10 C9 126(3) . . ?
C11 C10 H10 116.8 . . ?
C10 C11 C12 115(2) . . ?
C10 C11 C13 124(2) . . ?
C12 C11 C13 122(3) . . ?
C7 C12 H12 117.5 . . ?
C11 C12 C7 125(3) . . ?
C11 C12 H12 117.5 . . ?
C14 C13 C11 119(2) . . ?
C18 C13 C11 119(2) . . ?
C18 C13 C14 122(2) . . ?
C13 C14 H14 124.5 . . ?
C15 C14 C13 111(2) . . ?
C15 C14 H14 124.5 . . ?
C14 C15 H15 116.4 . . ?
C16 C15 C14 127(2) . . ?
C16 C15 H15 116.4 . . ?
C15 C16 C17 120(2) . . ?
C15 C16 C22 120(2) . . ?
C17 C16 C22 120(2) . . ?
C16 C17 H17 121.4 . . ?
C16 C17 C18 117(2) . . ?
C18 C17 H17 121.4 . . ?
C13 C18 C17 122(2) . . ?
C13 C18 C21 124(2) . . ?
C17 C18 C21 114(2) . . ?
O1 C19 O2 116.8(19) . . ?
O1 C19 C1 126(2) . . ?
O2 C19 C1 117(2) . . ?
O3 C20 C5 115(2) . . ?
O4 C20 O3 125(2) . . ?
O4 C20 C5 120(2) . . ?
O5 C21 Tb1 53.2(9) . 11_665 ?
O5 C21 C18 114.8(18) . . ?
O6 C21 Tb1 68.7(11) . 11_665 ?
O6 C21 O5 121.9(18) . . ?
O6 C21 C18 123.3(18) . . ?
C18 C21 Tb1 167.9(14) . 11_665 ?
O7 C22 Tb2 57.3(11) . . ?
O7 C22 C16 117(2) . . ?
O8 C22 Tb2 63.4(13) . . ?
O8 C22 O7 120(2) . . ?
O8 C22 C16 122(2) . . ?
C16 C22 Tb2 173.8(19) . . ?
O9 C23 O9 133(5) . 2_865 ?
O9 C23 H23 113.3 2_865 . ?
O9 C23 H23 113.3 . . ?

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
Tb1 O1 C19 O2 -117(5) . . . . ?
Tb1 O1 C19 C1 68(7) . . . . ?
Tb1 O4 C20 O3 1(4) 11_665 . . . ?
Tb1 O4 C20 C5 175.6(14) 11_665 . . . ?
Tb1 O5 C21 O6 1(2) 11_665 . . . ?
Tb1 O5 C21 C18 -178.6(15) 11_665 . . . ?
Tb1 O6 C21 O5 -1(2) 11_665 . . . ?
Tb1 O6 C21 C18 179(2) 11_665 . . . ?
Tb2 O2 C19 O1 -4(3) 16_534 . . . ?
Tb2 O2 C19 C1 171.9(17) 16_534 . . . ?
Tb2 O3 C20 O4 -35(4) 14_454 . . . ?
Tb2 O3 C20 C5 149.8(18) 14_454 . . . ?
Tb2 O6 C21 Tb1 143(3) 14_454 . . 11_665 ?
Tb2 O6 C21 O5 142(3) 14_454 . . . ?
Tb2 O6 C21 C18 -39(4) 14_454 . . . ?
Tb2 O7 C22 O8 6(2) . . . . ?
Tb2 O7 C22 C16 177.2(19) . . . . ?
Tb2 O8 C22 O7 -6(2) . . . . ?
Tb2 O8 C22 C16 -176(2) . . . . ?
Tb2 O9 C23 O9 130(2) . . . 2_865 ?
C1 C2 C3 C4 3(4) . . . . ?
C2 C1 C6 C5 6(5) . . . . ?
C2 C1 C19 O1 6(4) . . . . ?
C2 C1 C19 O2 -170(2) . . . . ?
C2 C3 C4 C5 1(4) . . . . ?
C2 C3 C4 C7 -180(2) . . . . ?
C3 C4 C5 C6 -2(4) . . . . ?
C3 C4 C5 C20 -176(2) . . . . ?
C3 C4 C7 C8 51(4) . . . . ?
C3 C4 C7 C12 -130(3) . . . . ?
C4 C5 C6 C1 -1(4) . . . . ?
C4 C5 C20 O3 -131(3) . . . . ?
C4 C5 C20 O4 54(3) . . . . ?
C4 C7 C8 C9 -177(3) . . . . ?
C4 C7 C12 C11 -177(3) . . . . ?
C5 C4 C7 C8 -130(3) . . . . ?
C5 C4 C7 C12 49(4) . . . . ?
C6 C1 C2 C3 -7(5) . . . . ?
C6 C1 C19 O1 -165(3) . . . . ?
C6 C1 C19 O2 19(4) . . . . ?
C6 C5 C20 O3 54(3) . . . . ?
C6 C5 C20 O4 -122(3) . . . . ?
C7 C4 C5 C6 179(3) . . . . ?
C7 C4 C5 C20 5(4) . . . . ?
C7 C8 C9 C10 -6(5) . . . . ?
C8 C7 C12 C11 2(4) . . . . ?
C8 C9 C10 C11 3(6) . . . . ?
C9 C10 C11 C12 3(6) . . . . ?
C9 C10 C11 C13 -175(4) . . . . ?
C10 C11 C12 C7 -5(5) . . . . ?
C10 C11 C13 C14 -61(5) . . . . ?
C10 C11 C13 C18 118(4) . . . . ?
C11 C13 C14 C15 -177(3) . . . . ?
C11 C13 C18 C17 175(2) . . . . ?
C11 C13 C18 C21 -3(4) . . . . ?
C12 C7 C8 C9 4(4) . . . . ?
C12 C11 C13 C14 121(3) . . . . ?
C12 C11 C13 C18 -60(4) . . . . ?
C13 C11 C12 C7 173(3) . . . . ?
C13 C14 C15 C16 0(4) . . . . ?
C13 C18 C21 Tb1 -61(8) . . . 11_665 ?
C13 C18 C21 O5 -56(3) . . . . ?
C13 C18 C21 O6 125(3) . . . . ?
C14 C13 C18 C17 -7(4) . . . . ?
C14 C13 C18 C21 176(2) . . . . ?
C14 C15 C16 C17 -3(4) . . . . ?
C14 C15 C16 C22 180(3) . . . . ?
C15 C16 C17 C18 1(3) . . . . ?
C15 C16 C22 O7 -178(2) . . . . ?
C15 C16 C22 O8 -7(4) . . . . ?
C16 C17 C18 C13 4(4) . . . . ?
C16 C17 C18 C21 -179(2) . . . . ?
C17 C16 C22 O7 5(3) . . . . ?
C17 C16 C22 O8 175(2) . . . . ?
C17 C18 C21 Tb1 121(7) . . . 11_665 ?
C17 C18 C21 O5 127(2) . . . . ?
C17 C18 C21 O6 -52(3) . . . . ?
C18 C13 C14 C15 4(4) . . . . ?
C19 C1 C2 C3 -177(2) . . . . ?
C19 C1 C6 C5 176(3) . . . . ?
C20 C5 C6 C1 173(2) . . . . ?
C22 C16 C17 C18 178(2) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.80(5)
2 0.20(5)
_vrf_CHEMW03_3-Tb                
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as  
RESPONSE: Some water molecules were squeezed, which gave inconsitent formula
from _atom_site_*.
;

_vrf_PLAT420_3-Tb                
;
PROBLEM: D-H Without Acceptor       O1W    --  H1WA   ...     Please Check   
RESPONSE: Some accepters for these hydrogens couldn??t located because the 
water molecules which can be the acceptors were squeezed.
;

_vrf_PLAT342_3-Tb                
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.03 Ang.   
RESPONSE: The low bond precision was caused by the inversion twin and the
bad data quality.
;

_vrf_PLAT020_3-Tb                
;
PROBLEM: The value of Rint is greater than 0.12   
RESPONSE:  The high Rint was caused by the bad quality of crystals.
;

_vrf_RINTA01_3-Tb                
;
PROBLEM: The value of Rint is greater than 0.18   
RESPONSE:  The high Rint was caused by the bad quality of crystals.
;


####################################################################### 
# 
# 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_4-Dy
_database_code_depnum_ccdc_archive 'CCDC 1442622'
_audit_update_record             
;
2016-10-24 deposited with the CCDC.
2016-10-31 downloaded from the CCDC.
;
_audit_creation_date             2016-10-22
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C45 H31 O23 Dy3, 12(H2 O)'
_chemical_formula_sum            'C45 H55 Dy3 O35'
_chemical_formula_weight         1643.39
_chemical_absolute_configuration .
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_H-M_alt        'I -4 2 d'
_space_group_name_Hall           'I -4 2bw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y, -z+3/4'
'x+1/2, -y, -z+3/4'
'-y+1/2, -x, z+3/4'
'y+1/2, x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1, y+1/2, -z+5/4'
'x+1, -y+1/2, -z+5/4'
'-y+1, -x+1/2, z+5/4'
'y+1, x+1/2, z+5/4'

_cell_length_a                   14.1545(3)
_cell_length_b                   14.1545(3)
_cell_length_c                   62.938(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     12609.6(7)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.878
_cell_measurement_theta_min      2.950
_shelx_estimated_absorpt_T_max   0.532
_shelx_estimated_absorpt_T_min   0.504
_exptl_absorpt_coefficient_mu    3.609
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5401
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0947 before and 0.0585 after correction.
The Ratio of minimum to maximum transmission is 0.7244.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             6424
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       77
_diffrn_reflns_limit_l_min       -78
_diffrn_reflns_number            89662
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         2.950
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.829
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                5620
_reflns_number_total             6440
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2015)'
_refine_diff_density_max         0.637
_refine_diff_density_min         -1.292
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details 
;
 Flack x determined using 2289 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.012(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         6440
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0281
_refine_ls_restrained_S_all      1.114
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0366P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0590
_refine_ls_wR_factor_ref         0.0613
_refine_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.

 The refinement was performed by a routine procedure with 
 SHELXL 2014. All the  hydrogens on carbon atoms were placed
 on calculated positions.  All the hydrogens on water 
 molecules were placed on proper positions and fixed by AFIX 3.

 The highly disordered crystallisation water molecules couldn't 
 located from Q-maps, so the SQUEEZE function in PLATON program
 was performed. And TG experiment was used to 
 
 The TGA curve displays a weight loss of 18.2% below 448 K, 
 consistent with the loss of 12 molecules of crystallisation 
 water (disordered, treated using PLATON SQUEEZE solvent mask)
 and 5 molecules of coordinated water per formula unit
 (calculated loss 18.6%).

 Some alerts caused by SQUEEZE were explained by _vrf_PLAT
 in CIF files.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O9-C23
 1.2 with sigma of 0.02
 C23-O9_$2
 1.2 with sigma of 0.02
 O9-O9_$2
 2.1 with sigma of 0.001
 O2W-C23
 2.1 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C23) \\sim Ueq, Uanis(O9) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 Dy2, O9, C23
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O8, C22, O7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed X: C23(0.5)
 Fixed Y: C23(0.5)
6.a Riding coordinates:
 O2W(H2WA,H2WB), O3W(H3WA,H3WB), O1W(H1W)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C14(H14), C16(H16),
 C17(H17), C19(H19), C23(H23)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 1.0000 0.5000 0.45908(2) 0.02245(9) Uani 1 2 d S T P . .
Dy2 Dy 0.72283(2) 0.48884(2) 0.43889(2) 0.03735(10) Uani 1 1 d . U . . .
O1 O 0.7586(3) 0.5960(3) 0.46489(7) 0.0415(12) Uani 1 1 d . . . . .
O2 O 0.9108(3) 0.6274(3) 0.47057(7) 0.0359(11) Uani 1 1 d . . . . .
O3 O 0.6138(4) 0.7176(4) 0.53226(8) 0.0624(16) Uani 1 1 d . . . . .
O4 O 0.5918(4) 0.8702(4) 0.53473(8) 0.0442(12) Uani 1 1 d . . . . .
O5 O 0.8242(5) 0.6376(4) 0.32775(8) 0.0657(17) Uani 1 1 d . . . . .
O6 O 0.8214(3) 0.5102(4) 0.34732(6) 0.0511(12) Uani 1 1 d . . . . .
O7 O 0.8689(3) 0.5447(3) 0.42870(6) 0.0330(10) Uani 1 1 d . U . . .
O8 O 1.0081(4) 0.6104(3) 0.42981(5) 0.0333(9) Uani 1 1 d . U . . .
O9 O 0.5698(2) 0.5255(6) 0.45600(14) 0.135(3) Uani 1 1 d D U . . .
O2W O 0.5988(6) 0.3770(7) 0.43113(15) 0.157(5) Uani 1 1 d D . . . .
H2WA H 0.6083 0.3120 0.4365 0.236 Uiso 1 1 d R . . . .
H2WB H 0.5845 0.3646 0.4158 0.236 Uiso 1 1 d R . . . .
O3W O 0.8025(4) 0.3594(4) 0.42153(8) 0.0573(14) Uani 1 1 d . . . . .
H3WA H 0.7678 0.3099 0.4220 0.086 Uiso 1 1 d R . . . .
H3WB H 0.8547 0.3482 0.4279 0.086 Uiso 1 1 d R . . . .
O1W O 1.0000 0.5000 0.49750(8) 0.069(2) Uani 1 2 d S T P . .
H1W H 0.9810 0.5435 0.5056 0.104 Uiso 1 1 d R . . . .
C1 C 0.8242(5) 0.6472(5) 0.47128(11) 0.0325(16) Uani 1 1 d . . . . .
C2 C 0.7959(4) 0.7390(5) 0.48166(9) 0.0332(15) Uani 1 1 d . . . . .
C3 C 0.7297(5) 0.7341(5) 0.49748(12) 0.0371(15) Uani 1 1 d . . . . .
H3 H 0.7035 0.6758 0.5009 0.045 Uiso 1 1 calc R . . . .
C4 C 0.7006(5) 0.8134(5) 0.50862(11) 0.0422(17) Uani 1 1 d . . . . .
C5 C 0.7390(5) 0.9006(5) 0.50324(11) 0.0433(17) Uani 1 1 d . . . . .
H5 H 0.7210 0.9545 0.5107 0.052 Uiso 1 1 calc R . . . .
C6 C 0.8028(5) 0.9074(5) 0.48716(11) 0.0472(19) Uani 1 1 d . . . . .
H6 H 0.8265 0.9664 0.4835 0.057 Uiso 1 1 calc R . . . .
C7 C 0.8343(5) 0.8255(5) 0.47579(10) 0.0374(16) Uani 1 1 d . . . . .
C8 C 0.6300(6) 0.8001(6) 0.52625(12) 0.0413(19) Uani 1 1 d . . . . .
C9 C 0.9018(5) 0.8358(5) 0.45761(11) 0.0402(17) Uani 1 1 d . . . . .
C10 C 0.9861(6) 0.8826(5) 0.45990(10) 0.0479(18) Uani 1 1 d . . . . .
H10 H 1.0019 0.9092 0.4729 0.057 Uiso 1 1 calc R . . . .
C11 C 1.0475(6) 0.8904(6) 0.44292(12) 0.056(2) Uani 1 1 d . . . . .
H11 H 1.1044 0.9224 0.4447 0.067 Uiso 1 1 calc R . . . .
C12 C 1.0255(6) 0.8514(5) 0.42336(11) 0.050(2) Uani 1 1 d . . . . .
H12 H 1.0675 0.8565 0.4121 0.060 Uiso 1 1 calc R . . . .
C13 C 0.9407(5) 0.8048(5) 0.42086(10) 0.0377(16) Uani 1 1 d . . . . .
C14 C 0.8779(5) 0.7981(4) 0.43776(10) 0.0383(16) Uani 1 1 d . . . . .
H14 H 0.8198 0.7685 0.4359 0.046 Uiso 1 1 calc R . . . .
C15 C 0.9171(5) 0.7538(5) 0.40070(9) 0.0370(16) Uani 1 1 d . . . . .
C16 C 0.9036(6) 0.7978(6) 0.38148(11) 0.052(2) Uani 1 1 d . . . . .
H16 H 0.9127 0.8628 0.3805 0.062 Uiso 1 1 calc R . . . .
C17 C 0.8775(5) 0.7495(6) 0.36382(10) 0.0506(19) Uani 1 1 d . . . . .
H17 H 0.8661 0.7817 0.3512 0.061 Uiso 1 1 calc R . . . .
C18 C 0.8677(5) 0.6527(5) 0.36460(10) 0.0420(18) Uani 1 1 d . . . . .
C19 C 0.8799(5) 0.6065(5) 0.38337(9) 0.0372(16) Uani 1 1 d . . . . .
H19 H 0.8701 0.5416 0.3841 0.045 Uiso 1 1 calc R . . . .
C20 C 0.9067(4) 0.6557(5) 0.40136(9) 0.0318(15) Uani 1 1 d . . . . .
C21 C 0.8363(5) 0.5974(6) 0.34544(11) 0.0437(18) Uani 1 1 d . . . . .
C22 C 0.9298(5) 0.6017(4) 0.42147(9) 0.0306(14) Uani 1 1 d . U . . .
C23 C 0.5000 0.5000 0.4439(3) 0.153(5) Uani 1 2 d DS TU P . .
H23 H 0.5000 0.5000 0.4292 0.183 Uiso 1 2 calc RS T P . .


_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 O2 2.317(4) . ?
Dy1 O2 2.317(4) 2_765 ?
Dy1 O4 2.283(5) 4_756 ?
Dy1 O4 2.283(5) 3_566 ?
Dy1 O7 2.738(4) 2_765 ?
Dy1 O7 2.738(4) . ?
Dy1 O8 2.418(4) 2_765 ?
Dy1 O8 2.418(4) . ?
Dy1 O1W 2.418(5) . ?
Dy1 C22 2.943(6) 2_765 ?
Dy1 C22 2.943(6) . ?
Dy2 O1 2.288(5) . ?
Dy2 O3 2.327(5) 3_566 ?
Dy2 O4 2.901(6) 3_566 ?
Dy2 O5 2.443(6) 5_655 ?
Dy2 O6 2.382(4) 5_655 ?
Dy2 O7 2.305(4) . ?
Dy2 O9 2.475(6) . ?
Dy2 O2W 2.413(8) . ?
Dy2 O3W 2.413(5) . ?
Dy2 C8 2.973(8) 3_566 ?
Dy2 C21 2.780(7) 5_655 ?
O1 C1 1.244(8) . ?
O2 C1 1.258(8) . ?
O3 Dy2 2.327(5) 4_656 ?
O3 C8 1.249(9) . ?
O4 Dy1 2.283(5) 3_576 ?
O4 Dy2 2.900(6) 4_656 ?
O4 C8 1.250(8) . ?
O5 Dy2 2.443(5) 5_655 ?
O5 C21 1.262(8) . ?
O6 Dy2 2.382(4) 5_655 ?
O6 C21 1.258(10) . ?
O7 C22 1.265(7) . ?
O8 C22 1.232(8) . ?
O9 C23 1.297(11) . ?
O2W H2WA 0.9900 . ?
O2W H2WB 1.0028 . ?
O3W H3WA 0.8553 . ?
O3W H3WB 0.8554 . ?
O1W H1W 0.8446 . ?
C1 C2 1.508(9) . ?
C2 C3 1.369(9) . ?
C2 C7 1.391(9) . ?
C3 H3 0.9300 . ?
C3 C4 1.387(9) . ?
C4 C5 1.390(10) . ?
C4 C8 1.505(10) . ?
C5 H5 0.9300 . ?
C5 C6 1.360(9) . ?
C6 H6 0.9300 . ?
C6 C7 1.433(9) . ?
C7 C9 1.497(9) . ?
C8 Dy2 2.974(8) 4_656 ?
C9 C10 1.372(10) . ?
C9 C14 1.400(9) . ?
C10 H10 0.9300 . ?
C10 C11 1.382(10) . ?
C11 H11 0.9300 . ?
C11 C12 1.385(9) . ?
C12 H12 0.9300 . ?
C12 C13 1.380(10) . ?
C13 C14 1.389(9) . ?
C13 C15 1.497(9) . ?
C14 H14 0.9300 . ?
C15 C16 1.374(9) . ?
C15 C20 1.396(10) . ?
C16 H16 0.9300 . ?
C16 C17 1.356(10) . ?
C17 H17 0.9300 . ?
C17 C18 1.379(10) . ?
C18 C19 1.361(9) . ?
C18 C21 1.504(9) . ?
C19 H19 0.9300 . ?
C19 C20 1.383(9) . ?
C20 C22 1.515(8) . ?
C21 Dy2 2.780(7) 5_655 ?
C23 O9 1.297(11) 2_665 ?
C23 H23 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Dy1 O2 143.6(2) . 2_765 ?
O2 Dy1 O7 140.09(15) . 2_765 ?
O2 Dy1 O7 70.67(14) 2_765 2_765 ?
O2 Dy1 O7 70.67(14) . . ?
O2 Dy1 O7 140.09(15) 2_765 . ?
O2 Dy1 O8 76.15(16) . . ?
O2 Dy1 O8 135.64(16) 2_765 . ?
O2 Dy1 O8 76.15(16) 2_765 2_765 ?
O2 Dy1 O8 135.64(16) . 2_765 ?
O2 Dy1 O1W 71.80(11) 2_765 . ?
O2 Dy1 O1W 71.81(11) . . ?
O2 Dy1 C22 144.65(16) . 2_765 ?
O2 Dy1 C22 144.65(16) 2_765 . ?
O2 Dy1 C22 71.74(16) 2_765 2_765 ?
O2 Dy1 C22 71.73(16) . . ?
O4 Dy1 O2 86.7(2) 4_756 . ?
O4 Dy1 O2 86.7(2) 3_566 2_765 ?
O4 Dy1 O2 87.19(19) 3_566 . ?
O4 Dy1 O2 87.18(19) 4_756 2_765 ?
O4 Dy1 O4 160.3(3) 4_756 3_566 ?
O4 Dy1 O7 122.20(15) 4_756 . ?
O4 Dy1 O7 72.87(16) 4_756 2_765 ?
O4 Dy1 O7 72.87(16) 3_566 . ?
O4 Dy1 O7 122.20(15) 3_566 2_765 ?
O4 Dy1 O8 122.39(18) 4_756 2_765 ?
O4 Dy1 O8 122.39(18) 3_566 . ?
O4 Dy1 O8 74.00(16) 3_566 2_765 ?
O4 Dy1 O8 74.00(16) 4_756 . ?
O4 Dy1 O1W 80.17(13) 3_566 . ?
O4 Dy1 O1W 80.17(13) 4_756 . ?
O4 Dy1 C22 97.51(18) 3_566 2_765 ?
O4 Dy1 C22 98.27(19) 3_566 . ?
O4 Dy1 C22 97.51(18) 4_756 . ?
O4 Dy1 C22 98.27(19) 4_756 2_765 ?
O7 Dy1 O7 91.44(17) 2_765 . ?
O7 Dy1 C22 25.41(15) 2_765 2_765 ?
O7 Dy1 C22 77.31(15) 2_765 . ?
O7 Dy1 C22 77.30(15) . 2_765 ?
O7 Dy1 C22 25.40(15) . . ?
O8 Dy1 O7 49.53(14) 2_765 2_765 ?
O8 Dy1 O7 65.51(14) 2_765 . ?
O8 Dy1 O7 49.53(14) . . ?
O8 Dy1 O7 65.51(14) . 2_765 ?
O8 Dy1 O8 80.79(18) . 2_765 ?
O8 Dy1 C22 24.13(16) . . ?
O8 Dy1 C22 24.13(16) 2_765 2_765 ?
O8 Dy1 C22 71.79(15) 2_765 . ?
O8 Dy1 C22 71.79(15) . 2_765 ?
O1W Dy1 O7 134.28(9) . . ?
O1W Dy1 O7 134.28(9) . 2_765 ?
O1W Dy1 O8 139.61(9) . 2_765 ?
O1W Dy1 O8 139.61(9) . . ?
O1W Dy1 C22 143.54(11) . . ?
O1W Dy1 C22 143.54(11) . 2_765 ?
C22 Dy1 C22 72.9(2) 2_765 . ?
O1 Dy2 O3 82.11(19) . 3_566 ?
O1 Dy2 O4 72.06(15) . 3_566 ?
O1 Dy2 O5 78.21(17) . 5_655 ?
O1 Dy2 O6 131.2(2) . 5_655 ?
O1 Dy2 O7 76.87(16) . . ?
O1 Dy2 O9 75.1(2) . . ?
O1 Dy2 O2W 137.8(3) . . ?
O1 Dy2 O3W 136.35(17) . . ?
O1 Dy2 C8 76.45(19) . 3_566 ?
O1 Dy2 C21 104.9(2) . 5_655 ?
O3 Dy2 O4 47.96(17) 3_566 3_566 ?
O3 Dy2 O5 149.7(2) 3_566 5_655 ?
O3 Dy2 O6 144.8(2) 3_566 5_655 ?
O3 Dy2 O9 76.3(3) 3_566 . ?
O3 Dy2 O2W 74.1(3) 3_566 . ?
O3 Dy2 O3W 83.9(2) 3_566 . ?
O3 Dy2 C8 23.44(18) 3_566 3_566 ?
O3 Dy2 C21 160.4(2) 3_566 5_655 ?
O4 Dy2 C8 24.53(16) 3_566 3_566 ?
O5 Dy2 O4 141.28(18) 5_655 3_566 ?
O5 Dy2 O9 76.6(3) 5_655 . ?
O5 Dy2 C8 154.66(19) 5_655 3_566 ?
O5 Dy2 C21 27.0(2) 5_655 5_655 ?
O6 Dy2 O4 141.86(16) 5_655 3_566 ?
O6 Dy2 O5 53.80(19) 5_655 5_655 ?
O6 Dy2 O9 99.2(2) 5_655 . ?
O6 Dy2 O2W 72.5(3) 5_655 . ?
O6 Dy2 O3W 77.66(19) 5_655 . ?
O6 Dy2 C8 151.0(2) 5_655 3_566 ?
O6 Dy2 C21 26.8(2) 5_655 5_655 ?
O7 Dy2 O3 117.37(18) . 3_566 ?
O7 Dy2 O4 69.44(13) . 3_566 ?
O7 Dy2 O5 80.19(19) . 5_655 ?
O7 Dy2 O6 85.77(16) . 5_655 ?
O7 Dy2 O9 146.6(2) . . ?
O7 Dy2 O2W 145.2(3) . . ?
O7 Dy2 O3W 73.46(16) . . ?
O7 Dy2 C8 93.97(18) . 3_566 ?
O7 Dy2 C21 82.22(19) . 5_655 ?
O9 Dy2 O4 117.6(2) . 3_566 ?
O9 Dy2 C8 96.9(3) . 3_566 ?
O9 Dy2 C21 87.6(3) . 5_655 ?
O2W Dy2 O4 112.4(3) . 3_566 ?
O2W Dy2 O5 106.3(3) . 5_655 ?
O2W Dy2 O9 65.7(3) . . ?
O2W Dy2 C8 92.6(3) . 3_566 ?
O2W Dy2 C21 89.2(3) . 5_655 ?
O3W Dy2 O4 67.93(16) . 3_566 ?
O3W Dy2 O5 125.99(17) . 5_655 ?
O3W Dy2 O9 139.9(2) . . ?
O3W Dy2 O2W 75.5(3) . . ?
O3W Dy2 C8 74.5(2) . 3_566 ?
O3W Dy2 C21 102.1(2) . 5_655 ?
C21 Dy2 O4 151.53(18) 5_655 3_566 ?
C21 Dy2 C8 175.5(2) 5_655 3_566 ?
C1 O1 Dy2 141.5(4) . . ?
C1 O2 Dy1 135.7(5) . . ?
C8 O3 Dy2 108.7(4) . 4_656 ?
Dy1 O4 Dy2 104.90(18) 3_576 4_656 ?
C8 O4 Dy1 163.3(5) . 3_576 ?
C8 O4 Dy2 81.0(5) . 4_656 ?
C21 O5 Dy2 91.5(5) . 5_655 ?
C21 O6 Dy2 94.5(4) . 5_655 ?
Dy2 O7 Dy1 109.55(15) . . ?
C22 O7 Dy1 86.4(4) . . ?
C22 O7 Dy2 158.4(4) . . ?
C22 O8 Dy1 102.5(4) . . ?
C23 O9 Dy2 110.7(7) . . ?
Dy2 O2W H2WA 116.2 . . ?
Dy2 O2W H2WB 117.2 . . ?
H2WA O2W H2WB 101.3 . . ?
Dy2 O3W H3WA 109.7 . . ?
Dy2 O3W H3WB 109.4 . . ?
H3WA O3W H3WB 109.2 . . ?
Dy1 O1W H1W 127.3 . . ?
O1 C1 O2 125.8(7) . . ?
O1 C1 C2 116.3(6) . . ?
O2 C1 C2 117.8(6) . . ?
C3 C2 C1 117.0(6) . . ?
C3 C2 C7 120.4(6) . . ?
C7 C2 C1 122.7(5) . . ?
C2 C3 H3 119.0 . . ?
C2 C3 C4 122.0(6) . . ?
C4 C3 H3 119.0 . . ?
C3 C4 C5 118.7(6) . . ?
C3 C4 C8 117.9(7) . . ?
C5 C4 C8 123.4(6) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 C4 120.2(6) . . ?
C6 C5 H5 119.9 . . ?
C5 C6 H6 119.3 . . ?
C5 C6 C7 121.4(7) . . ?
C7 C6 H6 119.3 . . ?
C2 C7 C6 117.3(6) . . ?
C2 C7 C9 122.6(6) . . ?
C6 C7 C9 120.1(6) . . ?
O3 C8 Dy2 47.8(3) . 4_656 ?
O3 C8 O4 122.3(7) . . ?
O3 C8 C4 117.5(6) . . ?
O4 C8 Dy2 74.5(4) . 4_656 ?
O4 C8 C4 120.2(7) . . ?
C4 C8 Dy2 165.0(5) . 4_656 ?
C10 C9 C7 121.4(6) . . ?
C10 C9 C14 119.2(6) . . ?
C14 C9 C7 119.4(6) . . ?
C9 C10 H10 119.9 . . ?
C9 C10 C11 120.3(6) . . ?
C11 C10 H10 119.9 . . ?
C10 C11 H11 119.5 . . ?
C10 C11 C12 121.0(7) . . ?
C12 C11 H11 119.5 . . ?
C11 C12 H12 120.4 . . ?
C13 C12 C11 119.2(7) . . ?
C13 C12 H12 120.4 . . ?
C12 C13 C14 120.2(6) . . ?
C12 C13 C15 121.4(6) . . ?
C14 C13 C15 118.3(6) . . ?
C9 C14 H14 119.9 . . ?
C13 C14 C9 120.2(6) . . ?
C13 C14 H14 119.9 . . ?
C16 C15 C13 124.0(7) . . ?
C16 C15 C20 117.5(6) . . ?
C20 C15 C13 118.5(5) . . ?
C15 C16 H16 119.0 . . ?
C17 C16 C15 122.0(7) . . ?
C17 C16 H16 119.0 . . ?
C16 C17 H17 120.0 . . ?
C16 C17 C18 120.0(7) . . ?
C18 C17 H17 120.0 . . ?
C17 C18 C21 121.2(6) . . ?
C19 C18 C17 119.7(6) . . ?
C19 C18 C21 118.9(6) . . ?
C18 C19 H19 119.9 . . ?
C18 C19 C20 120.2(7) . . ?
C20 C19 H19 119.9 . . ?
C15 C20 C22 120.3(6) . . ?
C19 C20 C15 120.4(6) . . ?
C19 C20 C22 119.3(6) . . ?
O5 C21 Dy2 61.5(4) . 5_655 ?
O5 C21 C18 120.9(7) . . ?
O6 C21 Dy2 58.7(3) . 5_655 ?
O6 C21 O5 120.1(7) . . ?
O6 C21 C18 119.0(6) . . ?
C18 C21 Dy2 177.6(5) . 5_655 ?
O7 C22 Dy1 68.2(3) . . ?
O7 C22 C20 118.4(6) . . ?
O8 C22 Dy1 53.3(3) . . ?
O8 C22 O7 121.5(6) . . ?
O8 C22 C20 119.9(6) . . ?
C20 C22 Dy1 172.7(4) . . ?
O9 C23 O9 108.3(14) . 2_665 ?
O9 C23 H23 125.8 . . ?
O9 C23 H23 125.8 2_665 . ?

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
Dy1 O2 C1 O1 -0.9(11) . . . . ?
Dy1 O2 C1 C2 176.2(4) . . . . ?
Dy1 O4 C8 Dy2 -112.2(19) 3_576 . . 4_656 ?
Dy1 O4 C8 O3 -110.5(18) 3_576 . . . ?
Dy1 O4 C8 C4 72(2) 3_576 . . . ?
Dy1 O7 C22 O8 0.1(6) . . . . ?
Dy1 O7 C22 C20 176.7(5) . . . . ?
Dy1 O8 C22 O7 -0.2(6) . . . . ?
Dy1 O8 C22 C20 -176.6(4) . . . . ?
Dy2 O1 C1 O2 -34.6(12) . . . . ?
Dy2 O1 C1 C2 148.3(5) . . . . ?
Dy2 O3 C8 O4 -2.3(10) 4_656 . . . ?
Dy2 O3 C8 C4 175.7(5) 4_656 . . . ?
Dy2 O4 C8 O3 1.7(8) 4_656 . . . ?
Dy2 O4 C8 C4 -176.2(7) 4_656 . . . ?
Dy2 O5 C21 O6 -0.3(8) 5_655 . . . ?
Dy2 O5 C21 C18 -179.6(6) 5_655 . . . ?
Dy2 O6 C21 O5 0.3(8) 5_655 . . . ?
Dy2 O6 C21 C18 179.6(6) 5_655 . . . ?
Dy2 O7 C22 Dy1 138.7(10) . . . . ?
Dy2 O7 C22 O8 138.9(9) . . . . ?
Dy2 O7 C22 C20 -44.6(13) . . . . ?
Dy2 O9 C23 O9 147.9(7) . . . 2_665 ?
O1 C1 C2 C3 50.8(9) . . . . ?
O1 C1 C2 C7 -129.5(7) . . . . ?
O2 C1 C2 C3 -126.5(7) . . . . ?
O2 C1 C2 C7 53.2(9) . . . . ?
C1 C2 C3 C4 177.8(7) . . . . ?
C1 C2 C7 C6 -178.8(7) . . . . ?
C1 C2 C7 C9 4.6(10) . . . . ?
C2 C3 C4 C5 1.0(11) . . . . ?
C2 C3 C4 C8 -177.9(7) . . . . ?
C2 C7 C9 C10 -129.5(8) . . . . ?
C2 C7 C9 C14 51.4(10) . . . . ?
C3 C2 C7 C6 0.9(10) . . . . ?
C3 C2 C7 C9 -175.6(6) . . . . ?
C3 C4 C5 C6 0.9(11) . . . . ?
C3 C4 C8 Dy2 24(2) . . . 4_656 ?
C3 C4 C8 O3 12.0(11) . . . . ?
C3 C4 C8 O4 -170.0(7) . . . . ?
C4 C5 C6 C7 -1.8(11) . . . . ?
C5 C4 C8 Dy2 -154.7(17) . . . 4_656 ?
C5 C4 C8 O3 -166.9(8) . . . . ?
C5 C4 C8 O4 11.1(12) . . . . ?
C5 C6 C7 C2 0.9(11) . . . . ?
C5 C6 C7 C9 177.6(7) . . . . ?
C6 C7 C9 C10 54.1(10) . . . . ?
C6 C7 C9 C14 -125.0(7) . . . . ?
C7 C2 C3 C4 -1.9(10) . . . . ?
C7 C9 C10 C11 179.4(7) . . . . ?
C7 C9 C14 C13 -178.3(6) . . . . ?
C8 C4 C5 C6 179.8(7) . . . . ?
C9 C10 C11 C12 -0.1(13) . . . . ?
C10 C9 C14 C13 2.6(10) . . . . ?
C10 C11 C12 C13 0.6(12) . . . . ?
C11 C12 C13 C14 0.6(11) . . . . ?
C11 C12 C13 C15 -174.4(7) . . . . ?
C12 C13 C14 C9 -2.2(10) . . . . ?
C12 C13 C15 C16 -66.2(10) . . . . ?
C12 C13 C15 C20 114.8(7) . . . . ?
C13 C15 C16 C17 -176.4(7) . . . . ?
C13 C15 C20 C19 176.4(6) . . . . ?
C13 C15 C20 C22 -6.9(9) . . . . ?
C14 C9 C10 C11 -1.5(11) . . . . ?
C14 C13 C15 C16 118.7(8) . . . . ?
C14 C13 C15 C20 -60.3(9) . . . . ?
C15 C13 C14 C9 173.0(6) . . . . ?
C15 C16 C17 C18 -2.9(12) . . . . ?
C15 C20 C22 O7 128.8(6) . . . . ?
C15 C20 C22 O8 -54.6(8) . . . . ?
C16 C15 C20 C19 -2.7(10) . . . . ?
C16 C15 C20 C22 174.1(6) . . . . ?
C16 C17 C18 C19 3.2(11) . . . . ?
C16 C17 C18 C21 178.4(7) . . . . ?
C17 C18 C19 C20 -3.3(10) . . . . ?
C17 C18 C21 O5 4.7(11) . . . . ?
C17 C18 C21 O6 -174.6(7) . . . . ?
C18 C19 C20 C15 3.1(10) . . . . ?
C18 C19 C20 C22 -173.7(6) . . . . ?
C19 C18 C21 O5 180.0(7) . . . . ?
C19 C18 C21 O6 0.7(11) . . . . ?
C19 C20 C22 O7 -54.4(8) . . . . ?
C19 C20 C22 O8 122.2(7) . . . . ?
C20 C15 C16 C17 2.6(11) . . . . ?
C21 C18 C19 C20 -178.7(6) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_vrf_CHEMW03_4-Dy                
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as  
RESPONSE: Some water molecules were squeezed, which gave inconsitent formula
from _atom_site_*.
;

_vrf_PLAT420_4-Dy                
;
PROBLEM: D-H Without Acceptor       O1W    --  H1WA   ...     Please Check   
RESPONSE: Some accepters for these hydrogens couldn??t located because the 
water molecules which can be the acceptors were squeezed.
;
####################################################################### 
# 
# 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_1-Sm
_database_code_depnum_ccdc_archive 'CCDC 1442623'
_audit_update_record             
;
2016-10-24 deposited with the CCDC.
2016-10-31 downloaded from the CCDC.
;
_audit_creation_date             2016-10-21
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C45 H31 O23 Sm3, 12(H2 O)'
_chemical_formula_sum            'C45 H55 O35 Sm3'
_chemical_formula_weight         1606.97
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1640 3.4420 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_H-M_alt        'I -4 2 d'
_space_group_name_Hall           'I -4 2bw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'y, -x, -z'
'-x, -y, z'
'-y, x, -z'
'x, -y+1/2, -z+1/4'
'-y+1/2, -x, z+3/4'
'-x, y+1/2, -z+1/4'
'y+1/2, x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1, -z+3/4'
'-y+1, -x+1/2, z+5/4'
'-x+1/2, y+1, -z+3/4'
'y+1, x+1/2, z+5/4'

_cell_length_a                   14.3090(4)
_cell_length_b                   14.3090(4)
_cell_length_c                   63.900(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     13083.4(11)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9852
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      26.419
_cell_measurement_theta_min      3.120
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.745
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5645
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0928 before and 0.0756 after correction.
The Ratio of minimum to maximum transmission is 0.7571.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             6327
_exptl_crystal_size_max          0.444
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.078
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0973
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       79
_diffrn_reflns_limit_l_min       -79
_diffrn_reflns_number            92596
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         3.120
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.833
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                5872
_reflns_number_total             6688
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.

 The refinement was performed by a routine procedure with 
 SHELXL 2014. All the  hydrogens on carbon atoms were placed
 on calculated positions.  All the hydrogens on water 
 molecules were placed on proper positions and fixed by AFIX 3.

 The highly disordered crystallisation water molecules couldn't 
 located from Q-maps, so the SQUEEZE function in PLATON program
 was performed. And TG experiment was used to 
 
 The TGA curve displays a weight loss of 19.6% below 448 K, 
 consistent with the loss of 12 molecules of crystallisation 
 water (disordered, treated using PLATON SQUEEZE solvent mask)
 and 5 molecules of coordinated water per formula unit
 (calculated loss 19.0%).

 Some alerts caused by SQUEEZE were explained by _vrf_PLAT
 in CIF files.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2015)'
_refine_diff_density_max         1.064
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details 
;
 Flack x determined using 2368 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.010(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         6688
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0372
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0471P)²+30.2808P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0870
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3W)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C8(H8), C10(H10), C14(H14), C17(H17), C18(H18), C19(H19),
 C20(H20), C21(H21), C23(H23)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 1.0000 0.5000 0.45983(2) 0.02283(13) Uani 1 2 d S T P . .
Sm2 Sm 0.52019(3) 0.27694(3) 0.56202(2) 0.04364(15) Uani 1 1 d . . . . .
O1 O 0.8711(4) 0.4597(4) 0.42877(8) 0.0363(13) Uani 1 1 d . . . . .
O1W O 0.6468(5) 0.1882(6) 0.57901(11) 0.063(2) Uani 1 1 d . . . . .
H1WA H 0.6990 0.2102 0.5750 0.094 Uiso 1 1 d R . . . .
H1WB H 0.6430 0.1310 0.5755 0.094 Uiso 1 1 d R . . . .
O2 O 0.6161(6) 0.2818(5) 0.53172(11) 0.062(2) Uani 1 1 d . . . . .
O2W O 0.6538(10) 0.3806(9) 0.57169(17) 0.135(5) Uani 1 1 d . . . . .
H2WA H 0.6702 0.3931 0.5842 0.202 Uiso 1 1 d R . . . .
H2WB H 0.6902 0.4082 0.5632 0.202 Uiso 1 1 d R . . . .
O3 O 0.5944(5) 0.1315(4) 0.53439(10) 0.0446(16) Uani 1 1 d . . . . .
O3W O 1.0000 0.5000 0.49778(12) 0.067(3) Uani 1 2 d S T P . .
H3W H 1.0485 0.5000 0.5055 0.101 Uiso 1 1 d R . . . .
O4 O 0.9035(4) 0.3740(4) 0.47050(9) 0.0379(14) Uani 1 1 d . . . . .
O5 O 0.7544(4) 0.4050(5) 0.46395(9) 0.0451(15) Uani 1 1 d . . . . .
O6 O 0.8199(6) 0.3692(6) 0.32949(10) 0.064(2) Uani 1 1 d . . . . .
O7 O 0.8210(5) 0.4947(6) 0.34865(8) 0.0542(17) Uani 1 1 d . . . . .
O10 O 0.4914(9) 0.4266(5) 0.54916(16) 0.102(3) Uani 1 1 d . . . . .
O12 O 1.0051(4) 0.3861(4) 0.43044(7) 0.0348(12) Uani 1 1 d . . . . .
C1 C 0.6333(7) 0.2008(7) 0.52549(14) 0.042(2) Uani 1 1 d . . . . .
C2 C 0.7010(7) 0.1875(7) 0.50788(12) 0.042(2) Uani 1 1 d . . . . .
C3 C 0.7258(6) 0.2661(6) 0.49663(12) 0.0387(19) Uani 1 1 d . . . . .
H3 H 0.6977 0.3230 0.4998 0.046 Uiso 1 1 calc R . . . .
C4 C 0.7911(6) 0.2626(6) 0.48075(12) 0.0351(19) Uani 1 1 d . . . . .
C5 C 0.8186(6) 0.3547(6) 0.47056(12) 0.0316(19) Uani 1 1 d . . . . .
C6 C 0.8293(7) 0.1766(6) 0.47542(12) 0.039(2) Uani 1 1 d . . . . .
C7 C 0.8023(7) 0.0977(7) 0.48654(14) 0.049(2) Uani 1 1 d . . . . .
H7 H 0.8278 0.0399 0.4831 0.059 Uiso 1 1 calc R . . . .
C8 C 0.7371(7) 0.1039(6) 0.50294(13) 0.047(2) Uani 1 1 d . . . . .
H8 H 0.7192 0.0507 0.5103 0.056 Uiso 1 1 calc R . . . .
C9 C 0.8945(6) 0.1668(6) 0.45726(13) 0.0359(19) Uani 1 1 d . . . . .
C10 C 0.8732(6) 0.2079(6) 0.43752(13) 0.0380(19) Uani 1 1 d . . . . .
H10 H 0.8178 0.2410 0.4358 0.046 Uiso 1 1 calc R . . . .
C11 C 0.9339(7) 0.1991(6) 0.42086(12) 0.039(2) Uani 1 1 d . . . . .
C12 C 0.9139(7) 0.2514(6) 0.40144(12) 0.040(2) Uani 1 1 d . . . . .
C13 C 0.9062(6) 0.3472(6) 0.40210(12) 0.0298(18) Uani 1 1 d . . . . .
C14 C 0.8811(6) 0.3979(7) 0.38434(12) 0.037(2) Uani 1 1 d . . . . .
H14 H 0.8750 0.4625 0.3852 0.044 Uiso 1 1 calc R . . . .
C15 C 0.8651(7) 0.3532(7) 0.36565(13) 0.044(2) Uani 1 1 d . . . . .
C16 C 0.8352(7) 0.4105(8) 0.34680(14) 0.050(3) Uani 1 1 d . . . . .
C17 C 0.8729(8) 0.2571(7) 0.36502(14) 0.059(3) Uani 1 1 d . . . . .
H17 H 0.8621 0.2259 0.3525 0.071 Uiso 1 1 calc R . . . .
C18 C 0.8956(8) 0.2076(8) 0.38212(14) 0.060(3) Uani 1 1 d . . . . .
H18 H 0.8992 0.1428 0.3812 0.072 Uiso 1 1 calc R . . . .
C19 C 1.0156(8) 0.1495(7) 0.42326(14) 0.058(3) Uani 1 1 d . . . . .
H19 H 1.0557 0.1426 0.4119 0.070 Uiso 1 1 calc R . . . .
C20 C 1.0390(8) 0.1098(8) 0.44238(15) 0.063(3) Uani 1 1 d . . . . .
H20 H 1.0949 0.0775 0.4439 0.076 Uiso 1 1 calc R . . . .
C21 C 0.9790(8) 0.1186(7) 0.45905(15) 0.056(3) Uani 1 1 d . . . . .
H21 H 0.9950 0.0919 0.4718 0.067 Uiso 1 1 calc R . . . .
C22 C 0.9295(6) 0.4012(5) 0.42185(11) 0.0305(19) Uani 1 1 d . . . . .
C23 C 0.5000 0.5000 0.5581(3) 0.113(8) Uani 1 2 d S T P . .
H23 H 0.5000 0.5000 0.5727 0.135 Uiso 1 2 calc RS T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 O1 2.770(6) . ?
Sm1 O1 2.770(6) 3_765 ?
Sm1 O3 2.345(6) 4_656 ?
Sm1 O3 2.345(6) 2_666 ?
Sm1 O3W 2.425(8) . ?
Sm1 O4 2.371(6) 3_765 ?
Sm1 O4 2.371(6) . ?
Sm1 O12 2.488(5) 3_765 ?
Sm1 O12 2.488(5) . ?
Sm2 O1 2.363(6) 2_566 ?
Sm2 O1W 2.464(8) . ?
Sm2 O2 2.374(6) . ?
Sm2 O2W 2.498(10) . ?
Sm2 O3 2.928(7) . ?
Sm2 O5 2.382(6) 2_566 ?
Sm2 O6 2.508(8) 16_444 ?
Sm2 O7 2.451(5) 16_444 ?
Sm2 O10 2.331(8) . ?
Sm2 C16 2.845(9) 16_444 ?
O1 Sm2 2.363(6) 4_656 ?
O1 C22 1.263(10) . ?
O1W H1WA 0.8501 . ?
O1W H1WB 0.8501 . ?
O2 C1 1.250(12) . ?
O2W H2WA 0.8497 . ?
O2W H2WB 0.8500 . ?
O3 Sm1 2.345(6) 2_566 ?
O3 C1 1.272(10) . ?
O3W H3W 0.8507 . ?
O4 C5 1.247(10) . ?
O5 Sm2 2.382(6) 4_656 ?
O5 C5 1.240(11) . ?
O6 Sm2 2.508(8) 8_554 ?
O6 C16 1.273(12) . ?
O7 Sm2 2.451(5) 8_554 ?
O7 C16 1.227(13) . ?
O10 C23 1.202(13) . ?
O12 C22 1.231(10) . ?
C1 C2 1.497(12) . ?
C2 C3 1.382(12) . ?
C2 C8 1.340(13) . ?
C3 H3 0.9300 . ?
C3 C4 1.381(11) . ?
C4 C5 1.521(12) . ?
C4 C6 1.389(13) . ?
C6 C7 1.390(12) . ?
C6 C9 1.495(11) . ?
C7 H7 0.9300 . ?
C7 C8 1.407(12) . ?
C8 H8 0.9300 . ?
C9 C10 1.424(12) . ?
C9 C21 1.397(14) . ?
C10 H10 0.9300 . ?
C10 C11 1.379(12) . ?
C11 C12 1.478(12) . ?
C11 C19 1.376(14) . ?
C12 C13 1.375(13) . ?
C12 C18 1.409(12) . ?
C13 C14 1.394(11) . ?
C13 C22 1.517(10) . ?
C14 H14 0.9300 . ?
C14 C15 1.374(11) . ?
C15 C16 1.519(13) . ?
C15 C17 1.381(14) . ?
C16 Sm2 2.845(9) 8_554 ?
C17 H17 0.9300 . ?
C17 C18 1.342(13) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C19 C20 1.388(13) . ?
C20 H20 0.9300 . ?
C20 C21 1.374(13) . ?
C21 H21 0.9300 . ?
C23 O10 1.202(13) 3_665 ?
C23 H23 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Sm1 O1 88.5(2) 3_765 . ?
O3 Sm1 O1 72.4(2) 2_666 3_765 ?
O3 Sm1 O1 121.8(2) 2_666 . ?
O3 Sm1 O1 121.8(2) 4_656 3_765 ?
O3 Sm1 O1 72.4(2) 4_656 . ?
O3 Sm1 O3 161.9(3) 2_666 4_656 ?
O3 Sm1 O3W 80.94(16) 2_666 . ?
O3 Sm1 O3W 80.94(16) 4_656 . ?
O3 Sm1 O4 85.7(2) 4_656 . ?
O3 Sm1 O4 89.1(2) 2_666 . ?
O3 Sm1 O4 89.1(2) 4_656 3_765 ?
O3 Sm1 O4 85.7(2) 2_666 3_765 ?
O3 Sm1 O12 73.6(2) 4_656 3_765 ?
O3 Sm1 O12 121.3(2) 4_656 . ?
O3 Sm1 O12 121.3(2) 2_666 3_765 ?
O3 Sm1 O12 73.6(2) 2_666 . ?
O3W Sm1 O1 135.77(11) . . ?
O3W Sm1 O1 135.77(11) . 3_765 ?
O3W Sm1 O12 139.02(12) . . ?
O3W Sm1 O12 139.01(12) . 3_765 ?
O4 Sm1 O1 70.15(18) 3_765 3_765 ?
O4 Sm1 O1 138.75(19) 3_765 . ?
O4 Sm1 O1 70.15(18) . . ?
O4 Sm1 O1 138.75(19) . 3_765 ?
O4 Sm1 O3W 73.28(14) 3_765 . ?
O4 Sm1 O3W 73.28(14) . . ?
O4 Sm1 O4 146.6(3) . 3_765 ?
O4 Sm1 O12 134.3(2) . 3_765 ?
O4 Sm1 O12 134.3(2) 3_765 . ?
O4 Sm1 O12 74.7(2) 3_765 3_765 ?
O4 Sm1 O12 74.7(2) . . ?
O12 Sm1 O1 64.91(18) . 3_765 ?
O12 Sm1 O1 64.91(18) 3_765 . ?
O12 Sm1 O1 48.87(18) 3_765 3_765 ?
O12 Sm1 O1 48.86(18) . . ?
O12 Sm1 O12 82.0(2) 3_765 . ?
O1 Sm2 O1W 72.4(2) 2_566 . ?
O1 Sm2 O2 116.2(2) 2_566 . ?
O1 Sm2 O2W 138.7(3) 2_566 . ?
O1 Sm2 O3 69.25(18) 2_566 . ?
O1 Sm2 O5 75.6(2) 2_566 2_566 ?
O1 Sm2 O6 78.1(2) 2_566 16_444 ?
O1 Sm2 O7 86.5(2) 2_566 16_444 ?
O1 Sm2 C16 82.3(3) 2_566 16_444 ?
O1W Sm2 O2W 68.6(4) . . ?
O1W Sm2 O3 68.5(2) . . ?
O1W Sm2 O6 124.3(2) . 16_444 ?
O1W Sm2 C16 102.3(3) . 16_444 ?
O2 Sm2 O1W 87.1(3) . . ?
O2 Sm2 O2W 75.0(3) . . ?
O2 Sm2 O3 47.1(2) . . ?
O2 Sm2 O5 80.6(2) . 2_566 ?
O2 Sm2 O6 148.6(3) . 16_444 ?
O2 Sm2 O7 149.0(3) . 16_444 ?
O2 Sm2 C16 161.3(3) . 16_444 ?
O2W Sm2 O3 107.1(4) . . ?
O2W Sm2 O6 113.8(4) . 16_444 ?
O2W Sm2 C16 93.2(4) . 16_444 ?
O5 Sm2 O1W 136.0(2) 2_566 . ?
O5 Sm2 O2W 144.5(3) 2_566 . ?
O5 Sm2 O3 72.4(2) 2_566 . ?
O5 Sm2 O6 76.1(2) 2_566 16_444 ?
O5 Sm2 O7 127.6(3) 2_566 16_444 ?
O5 Sm2 C16 102.6(3) 2_566 16_444 ?
O6 Sm2 O3 139.0(2) 16_444 . ?
O6 Sm2 C16 26.6(3) 16_444 16_444 ?
O7 Sm2 O1W 79.7(2) 16_444 . ?
O7 Sm2 O2W 74.0(3) 16_444 . ?
O7 Sm2 O3 144.3(2) 16_444 . ?
O7 Sm2 O6 52.0(2) 16_444 16_444 ?
O7 Sm2 C16 25.4(3) 16_444 16_444 ?
O10 Sm2 O1 147.9(3) . 2_566 ?
O10 Sm2 O1W 139.4(4) . . ?
O10 Sm2 O2 77.7(3) . . ?
O10 Sm2 O2W 71.2(5) . . ?
O10 Sm2 O3 120.3(3) . . ?
O10 Sm2 O5 78.7(3) . 2_566 ?
O10 Sm2 O6 77.3(4) . 16_444 ?
O10 Sm2 O7 94.2(3) . 16_444 ?
O10 Sm2 C16 84.8(3) . 16_444 ?
C16 Sm2 O3 151.5(2) 16_444 . ?
Sm2 O1 Sm1 110.02(19) 4_656 . ?
C22 O1 Sm1 87.0(5) . . ?
C22 O1 Sm2 157.4(6) . 4_656 ?
Sm2 O1W H1WA 108.9 . . ?
Sm2 O1W H1WB 109.4 . . ?
H1WA O1W H1WB 109.5 . . ?
C1 O2 Sm2 110.2(5) . . ?
Sm2 O2W H2WA 124.6 . . ?
Sm2 O2W H2WB 125.9 . . ?
H2WA O2W H2WB 109.5 . . ?
Sm1 O3 Sm2 105.5(2) 2_566 . ?
C1 O3 Sm1 161.5(6) . 2_566 ?
C1 O3 Sm2 82.8(6) . . ?
Sm1 O3W H3W 125.3 . . ?
C5 O4 Sm1 137.4(6) . . ?
C5 O5 Sm2 141.1(5) . 4_656 ?
C16 O6 Sm2 91.7(6) . 8_554 ?
C16 O7 Sm2 95.6(5) . 8_554 ?
C23 O10 Sm2 128.1(11) . . ?
C22 O12 Sm1 101.3(5) . . ?
O2 C1 O3 119.7(8) . . ?
O2 C1 C2 119.0(8) . . ?
O3 C1 C2 121.3(9) . . ?
C3 C2 C1 117.0(9) . . ?
C8 C2 C1 122.7(8) . . ?
C8 C2 C3 120.4(8) . . ?
C2 C3 H3 119.1 . . ?
C4 C3 C2 121.8(8) . . ?
C4 C3 H3 119.1 . . ?
C3 C4 C5 117.3(8) . . ?
C3 C4 C6 118.6(8) . . ?
C6 C4 C5 124.1(7) . . ?
O4 C5 C4 116.4(8) . . ?
O5 C5 O4 126.4(8) . . ?
O5 C5 C4 117.2(8) . . ?
C4 C6 C7 119.1(8) . . ?
C4 C6 C9 121.3(7) . . ?
C7 C6 C9 119.6(8) . . ?
C6 C7 H7 119.5 . . ?
C6 C7 C8 120.9(9) . . ?
C8 C7 H7 119.5 . . ?
C2 C8 C7 119.2(8) . . ?
C2 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
C10 C9 C6 121.1(8) . . ?
C21 C9 C6 121.5(8) . . ?
C21 C9 C10 117.4(7) . . ?
C9 C10 H10 119.6 . . ?
C11 C10 C9 120.8(8) . . ?
C11 C10 H10 119.6 . . ?
C10 C11 C12 118.7(8) . . ?
C19 C11 C10 119.7(8) . . ?
C19 C11 C12 121.3(8) . . ?
C13 C12 C11 119.6(7) . . ?
C13 C12 C18 117.1(8) . . ?
C18 C12 C11 123.1(8) . . ?
C12 C13 C14 120.9(7) . . ?
C12 C13 C22 121.0(7) . . ?
C14 C13 C22 117.9(7) . . ?
C13 C14 H14 119.7 . . ?
C15 C14 C13 120.5(8) . . ?
C15 C14 H14 119.7 . . ?
C14 C15 C16 119.0(8) . . ?
C14 C15 C17 118.4(8) . . ?
C17 C15 C16 122.5(8) . . ?
O6 C16 Sm2 61.8(5) . 8_554 ?
O6 C16 C15 119.1(9) . . ?
O7 C16 Sm2 59.0(5) . 8_554 ?
O7 C16 O6 120.7(9) . . ?
O7 C16 C15 120.0(8) . . ?
C15 C16 Sm2 178.9(8) . 8_554 ?
C15 C17 H17 119.3 . . ?
C18 C17 C15 121.4(9) . . ?
C18 C17 H17 119.3 . . ?
C12 C18 H18 119.2 . . ?
C17 C18 C12 121.6(10) . . ?
C17 C18 H18 119.2 . . ?
C11 C19 H19 119.5 . . ?
C11 C19 C20 120.9(9) . . ?
C20 C19 H19 119.5 . . ?
C19 C20 H20 120.2 . . ?
C21 C20 C19 119.6(9) . . ?
C21 C20 H20 120.2 . . ?
C9 C21 H21 119.2 . . ?
C20 C21 C9 121.5(9) . . ?
C20 C21 H21 119.2 . . ?
O1 C22 C13 118.9(8) . . ?
O12 C22 O1 122.8(7) . . ?
O12 C22 C13 118.3(7) . . ?
O10 C23 O10 123(2) 3_665 . ?
O10 C23 H23 118.4 . . ?
O10 C23 H23 118.4 3_665 . ?

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
Sm1 O1 C22 O12 2.0(8) . . . . ?
Sm1 O1 C22 C13 -177.8(6) . . . . ?
Sm1 O3 C1 O2 114(2) 2_566 . . . ?
Sm1 O3 C1 C2 -67(2) 2_566 . . . ?
Sm1 O4 C5 O5 0.2(13) . . . . ?
Sm1 O4 C5 C4 -176.5(5) . . . . ?
Sm1 O12 C22 O1 -2.3(9) . . . . ?
Sm1 O12 C22 C13 177.6(6) . . . . ?
Sm2 O1 C22 O12 -138.1(11) 4_656 . . . ?
Sm2 O1 C22 C13 42.1(16) 4_656 . . . ?
Sm2 O2 C1 O3 5.2(12) . . . . ?
Sm2 O2 C1 C2 -173.6(7) . . . . ?
Sm2 O3 C1 O2 -4.0(9) . . . . ?
Sm2 O3 C1 C2 174.8(9) . . . . ?
Sm2 O5 C5 O4 31.3(14) 4_656 . . . ?
Sm2 O5 C5 C4 -152.1(6) 4_656 . . . ?
Sm2 O6 C16 O7 3.3(11) 8_554 . . . ?
Sm2 O6 C16 C15 179.2(9) 8_554 . . . ?
Sm2 O7 C16 O6 -3.4(11) 8_554 . . . ?
Sm2 O7 C16 C15 -179.3(8) 8_554 . . . ?
Sm2 O10 C23 O10 158.9(12) . . . 3_665 ?
O2 C1 C2 C3 -13.2(13) . . . . ?
O2 C1 C2 C8 166.7(10) . . . . ?
O3 C1 C2 C3 168.0(8) . . . . ?
O3 C1 C2 C8 -12.1(15) . . . . ?
C1 C2 C3 C4 176.8(8) . . . . ?
C1 C2 C8 C7 -178.2(9) . . . . ?
C2 C3 C4 C5 -175.4(8) . . . . ?
C2 C3 C4 C6 3.1(13) . . . . ?
C3 C2 C8 C7 1.7(15) . . . . ?
C3 C4 C5 O4 124.5(8) . . . . ?
C3 C4 C5 O5 -52.5(11) . . . . ?
C3 C4 C6 C7 -1.6(13) . . . . ?
C3 C4 C6 C9 175.0(8) . . . . ?
C4 C6 C7 C8 0.3(15) . . . . ?
C4 C6 C9 C10 -47.0(13) . . . . ?
C4 C6 C9 C21 131.9(10) . . . . ?
C5 C4 C6 C7 176.7(9) . . . . ?
C5 C4 C6 C9 -6.7(13) . . . . ?
C6 C4 C5 O4 -53.9(11) . . . . ?
C6 C4 C5 O5 129.2(9) . . . . ?
C6 C7 C8 C2 -0.3(15) . . . . ?
C6 C9 C10 C11 179.6(8) . . . . ?
C6 C9 C21 C20 -179.8(10) . . . . ?
C7 C6 C9 C10 129.6(10) . . . . ?
C7 C6 C9 C21 -51.5(13) . . . . ?
C8 C2 C3 C4 -3.2(14) . . . . ?
C9 C6 C7 C8 -176.4(9) . . . . ?
C9 C10 C11 C12 -173.4(8) . . . . ?
C9 C10 C11 C19 0.5(13) . . . . ?
C10 C9 C21 C20 -0.9(16) . . . . ?
C10 C11 C12 C13 58.1(12) . . . . ?
C10 C11 C12 C18 -117.3(11) . . . . ?
C10 C11 C19 C20 -1.4(16) . . . . ?
C11 C12 C13 C14 -175.5(8) . . . . ?
C11 C12 C13 C22 7.6(13) . . . . ?
C11 C12 C18 C17 176.5(10) . . . . ?
C11 C19 C20 C21 1.2(18) . . . . ?
C12 C11 C19 C20 172.3(10) . . . . ?
C12 C13 C14 C15 -1.3(13) . . . . ?
C12 C13 C22 O1 -129.3(9) . . . . ?
C12 C13 C22 O12 50.9(11) . . . . ?
C13 C12 C18 C17 0.9(16) . . . . ?
C13 C14 C15 C16 178.3(9) . . . . ?
C13 C14 C15 C17 1.3(15) . . . . ?
C14 C13 C22 O1 53.7(10) . . . . ?
C14 C13 C22 O12 -126.1(8) . . . . ?
C14 C15 C16 O6 -179.6(10) . . . . ?
C14 C15 C16 O7 -3.7(15) . . . . ?
C14 C15 C17 C18 -0.2(17) . . . . ?
C15 C17 C18 C12 -1.0(18) . . . . ?
C16 C15 C17 C18 -177.1(11) . . . . ?
C17 C15 C16 O6 -2.7(16) . . . . ?
C17 C15 C16 O7 173.2(11) . . . . ?
C18 C12 C13 C14 0.2(14) . . . . ?
C18 C12 C13 C22 -176.8(9) . . . . ?
C19 C11 C12 C13 -115.6(11) . . . . ?
C19 C11 C12 C18 69.0(14) . . . . ?
C19 C20 C21 C9 0.0(18) . . . . ?
C21 C9 C10 C11 0.7(13) . . . . ?
C22 C13 C14 C15 175.7(9) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_vrf_CHEMW03_1-Sm                
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as  
RESPONSE: Some water molecules were squeezed, which gave inconsitent formula
from _atom_site_*.
;

_vrf_PLAT420_1-Sm                
;
PROBLEM: D-H Without Acceptor       O1W    --  H1WA   ...     Please Check   
RESPONSE: Some accepters for these hydrogens couldn??t located because the 
water molecules which can be the acceptors were squeezed.
;
