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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 1523869'
_audit_update_record             
;
2017-03-20 deposited with the CCDC.
2017-03-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H36 Dy2 O24, 3.5(H2 O)'
_chemical_formula_sum            'C30 H43 Dy2 O27.50'
_chemical_formula_weight         1168.64

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'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

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

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

_cell_length_a                   16.3718(5)
_cell_length_b                   7.9713(3)
_cell_length_c                   30.9027(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4032.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(1)
_cell_measurement_reflns_used    5807
_cell_measurement_theta_min      3.6230
_cell_measurement_theta_max      29.3620

_exptl_crystal_description       needle
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.925
_exptl_crystal_F_000             2300
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.267
_exptl_crystal_size_mid          0.039
_exptl_crystal_size_min          0.013
_exptl_absorpt_coefficient_mu    3.775
_shelx_estimated_absorpt_T_min   0.432
_shelx_estimated_absorpt_T_max   0.953
_exptl_absorpt_correction_T_min  0.90267
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Multi-scan absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   
; 
 The following created by CrysAlis:  
  oxdiff_exptl_absorpt_empirical_full_min           0.917
  oxdiff_exptl_absorpt_empirical_full_max           1.095
  oxdiff_exptl_absorpt_empirical_details
  Multi-scan correction (ABSPACK) includes:
  - Absorption correction using spherical harmonics
  - Frame scaling
;
_diffrn_ambient_temperature      173(1)
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3
_diffrn_detector_area_resol_mean 16.0655
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            19610
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         3.463
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_full        27.497
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4632
_reflns_number_gt                3520
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_solution    'SIR 92'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2007)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_refine_special_details          
', Bridging ligand disordered about inversion center.'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0241P)²+3.6121P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4632
_refine_ls_number_parameters     349
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0387
_refine_ls_wR_factor_ref         0.0822
_refine_ls_wR_factor_gt          0.0762
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_restrained_S_all      1.132
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.05254(2) 0.12792(3) 0.67375(2) 0.02136(8) Uani 1 1 d . . . . .
O1 O -0.0354(2) 0.3426(4) 0.69667(11) 0.0267(8) Uani 1 1 d . . . . .
O2 O -0.1532(2) 0.4837(4) 0.69502(12) 0.0325(9) Uani 1 1 d . . . . .
O3 O -0.0943(2) 0.0921(4) 0.65153(11) 0.0234(8) Uani 1 1 d . . . . .
O4 O 0.0008(2) -0.1627(4) 0.64983(12) 0.0285(8) Uani 1 1 d . . . . .
O5 O 0.1411(2) -0.0945(4) 0.68487(12) 0.0343(9) Uani 1 1 d . . . . .
O6 O 0.1879(2) -0.3532(5) 0.67658(15) 0.0458(11) Uani 1 1 d . . . . .
C1 C -0.1087(3) 0.3636(6) 0.68420(15) 0.0245(11) Uani 1 1 d . . . . .
C2 C -0.1449(3) 0.2396(6) 0.65310(16) 0.0250(11) Uani 1 1 d . . . . .
H2A H -0.200718 0.208722 0.662569 0.030 Uiso 1 1 calc R U . . .
H2B H -0.148714 0.290298 0.623922 0.030 Uiso 1 1 calc R U . . .
C3 C -0.1156(3) -0.0329(6) 0.62200(15) 0.0214(10) Uani 1 1 d . . . . .
C4 C -0.1821(3) -0.0239(6) 0.59471(16) 0.0269(11) Uani 1 1 d . . . . .
H4 H -0.217697 0.070171 0.595536 0.032 Uiso 1 1 calc R U . . .
C5 C -0.1961(3) -0.1545(6) 0.56605(17) 0.0326(13) Uani 1 1 d . . . . .
H5 H -0.240886 -0.148729 0.546535 0.039 Uiso 1 1 calc R U . . .
C6 C -0.1458(3) -0.2921(6) 0.56569(17) 0.0306(12) Uani 1 1 d . . . . .
H6 H -0.156368 -0.380973 0.545997 0.037 Uiso 1 1 calc R U . . .
C7 C -0.0802(3) -0.3034(6) 0.59344(17) 0.0293(12) Uani 1 1 d . . . . .
H7 H -0.046136 -0.399920 0.593282 0.035 Uiso 1 1 calc R U . . .
C8 C -0.0644(3) -0.1712(6) 0.62174(16) 0.0242(11) Uani 1 1 d . . . . .
C9 C 0.0597(3) -0.2948(7) 0.6475(2) 0.0365(14) Uani 1 1 d . . . . .
H9A H 0.074108 -0.317091 0.616931 0.044 Uiso 1 1 calc R U . . .
H9B H 0.036667 -0.398868 0.660039 0.044 Uiso 1 1 calc R U . . .
C10 C 0.1346(3) -0.2439(6) 0.67219(19) 0.0336(13) Uani 1 1 d . . . . .
O7 O 0.0870(3) 0.0664(4) 0.59991(12) 0.0398(10) Uani 1 1 d . . . . .
O8 O 0.0181(2) 0.3004(4) 0.60883(11) 0.0300(8) Uani 1 1 d . . . . .
C11A C 0.0545(4) 0.1983(7) 0.58552(17) 0.0325(13) Uani 0.5 1 d . . P . .
C12 C 0.0424(10) 0.208(2) 0.5362(5) 0.037(4) Uani 0.5 1 d . . P A -1
H12A H 0.096008 0.190475 0.522187 0.044 Uiso 0.5 1 calc R U P A -1
H12B H 0.006367 0.114714 0.527365 0.044 Uiso 0.5 1 calc R U P A -1
O9 O 0.0083(8) 0.361(2) 0.5197(6) 0.032(3) Uani 0.5 1 d . . P A -1
C13 C 0.0596(7) 0.4977(18) 0.5210(3) 0.029(3) Uani 0.5 1 d . . P A -1
C14 C 0.1339(7) 0.5107(15) 0.5424(4) 0.037(3) Uani 0.5 1 d . . P A -1
H14 H 0.153054 0.418342 0.559019 0.045 Uiso 0.5 1 calc R U P A -1
C15 C 0.1795(13) 0.651(3) 0.5402(5) 0.046(4) Uani 0.5 1 d . . P A -1
H15 H 0.230632 0.655778 0.554687 0.055 Uiso 0.5 1 calc R U P A -1
C16 C 0.1516(10) 0.7926(17) 0.5164(5) 0.051(4) Uani 0.5 1 d . . P A -1
H16 H 0.181976 0.894171 0.516235 0.061 Uiso 0.5 1 calc R U P A -1
C17 C 0.0801(9) 0.7793(14) 0.4937(4) 0.041(3) Uani 0.5 1 d . . P A -1
H17 H 0.062731 0.870275 0.476056 0.049 Uiso 0.5 1 calc R U P A -1
C18 C 0.0320(9) 0.6335(17) 0.4959(4) 0.032(3) Uani 0.5 1 d . . P A -1
O10 O -0.0406(9) 0.612(3) 0.4759(6) 0.037(3) Uani 0.5 1 d . . P A -1
C19 C -0.0853(10) 0.752(2) 0.4602(6) 0.042(4) Uani 0.5 1 d . . P A -1
H19A H -0.078235 0.848351 0.480190 0.050 Uiso 0.5 1 calc R U P A -1
H19B H -0.144144 0.724610 0.458878 0.050 Uiso 0.5 1 calc R U P A -1
C11B C 0.0545(4) 0.1983(7) 0.58552(17) 0.0325(13) Uani 0.5 1 d . . P . .
O11W O 0.1664(3) 0.3029(5) 0.65931(14) 0.0360(10) Uani 1 1 d D . . . .
H11A H 0.169(4) 0.407(5) 0.666(2) 0.054 Uiso 1 1 d D U . . .
H11B H 0.209(3) 0.254(7) 0.6699(19) 0.054 Uiso 1 1 d D U . . .
O12W O -0.0208(2) 0.0101(6) 0.73220(14) 0.0364(11) Uani 1 1 d . . . . .
H12C H -0.007(4) -0.037(8) 0.755(2) 0.055 Uiso 1 1 d . U . . .
H12D H -0.061(4) 0.001(9) 0.732(2) 0.055 Uiso 1 1 d . U . . .
O13W O 0.1184(3) 0.1976(5) 0.73970(14) 0.0378(11) Uani 1 1 d . . . . .
H13A H 0.137(4) 0.278(8) 0.743(2) 0.057 Uiso 1 1 d . U . . .
H13B H 0.119(5) 0.139(8) 0.756(2) 0.057 Uiso 1 1 d . U . . .
O14W O 0.1977(3) 0.4911(6) 0.75974(15) 0.0426(11) Uani 1 1 d . . . . .
H14A H 0.243(5) 0.488(8) 0.771(2) 0.064 Uiso 1 1 d . U . . .
H14B H 0.212(5) 0.524(8) 0.736(2) 0.064 Uiso 1 1 d . U . . .
O15W O -0.1643(11) 0.344(3) 0.4796(5) 0.098(6) Uani 0.5 1 d . . P . .
O16W O -0.2309(12) 0.064(2) 0.4410(8) 0.080(6) Uani 0.25 1 d . U 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 O5 2.316(3) . ?
Dy1 O1 2.345(3) . ?
Dy1 O12W 2.364(4) . ?
Dy1 O11W 2.370(4) . ?
Dy1 O13W 2.372(4) . ?
Dy1 O7 2.401(4) . ?
Dy1 O8 2.497(3) . ?
Dy1 O3 2.516(3) . ?
Dy1 O4 2.575(3) . ?
O1 C1 1.272(6) . ?
O2 C1 1.248(6) . ?
O3 C3 1.396(5) . ?
O3 C2 1.440(5) . ?
O4 C8 1.377(6) . ?
O4 C9 1.431(6) . ?
O5 C10 1.258(6) . ?
O6 C10 1.241(6) . ?
C1 C2 1.501(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.379(7) . ?
C3 C8 1.386(7) . ?
C4 C5 1.386(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.372(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.378(7) . ?
C6 H6 0.9500 . ?
C7 C8 1.393(7) . ?
C7 H7 0.9500 . ?
C9 C10 1.499(8) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
O7 C11A 1.260(6) . ?
O8 C11A 1.240(6) . ?
C11A C12 1.538(15) . ?
C11A C19 1.549(17) 5_566 ?
C12 O9 1.43(2) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
O9 C13 1.375(18) . ?
C13 C14 1.388(16) . ?
C13 C18 1.407(18) . ?
C14 C15 1.35(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.42(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.369(19) . ?
C16 H16 0.9500 . ?
C17 C18 1.406(19) . ?
C17 H17 0.9500 . ?
C18 O10 1.352(17) . ?
O10 C19 1.42(3) . ?
C19 C11B 1.549(17) 5_566 ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
O11W H11A 0.85(4) . ?
O11W H11B 0.86(4) . ?
O12W H12C 0.82(7) . ?
O12W H12D 0.66(7) . ?
O13W H13A 0.72(6) . ?
O13W H13B 0.69(6) . ?
O14W H14A 0.82(8) . ?
O14W H14B 0.82(7) . ?

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
O5 Dy1 O1 153.87(13) . . ?
O5 Dy1 O12W 84.27(15) . . ?
O1 Dy1 O12W 75.37(14) . . ?
O5 Dy1 O11W 89.21(13) . . ?
O1 Dy1 O11W 96.32(13) . . ?
O12W Dy1 O11W 141.00(15) . . ?
O5 Dy1 O13W 76.54(14) . . ?
O1 Dy1 O13W 81.29(14) . . ?
O12W Dy1 O13W 70.57(15) . . ?
O11W Dy1 O13W 70.51(15) . . ?
O5 Dy1 O7 80.65(13) . . ?
O1 Dy1 O7 125.47(12) . . ?
O12W Dy1 O7 139.86(15) . . ?
O11W Dy1 O7 75.90(14) . . ?
O13W Dy1 O7 139.25(16) . . ?
O5 Dy1 O8 133.04(13) . . ?
O1 Dy1 O8 72.67(12) . . ?
O12W Dy1 O8 135.89(14) . . ?
O11W Dy1 O8 72.69(13) . . ?
O13W Dy1 O8 131.62(13) . . ?
O7 Dy1 O8 53.28(12) . . ?
O5 Dy1 O3 123.48(11) . . ?
O1 Dy1 O3 65.10(11) . . ?
O12W Dy1 O3 71.23(13) . . ?
O11W Dy1 O3 140.05(12) . . ?
O13W Dy1 O3 134.06(14) . . ?
O7 Dy1 O3 86.68(13) . . ?
O8 Dy1 O3 68.11(12) . . ?
O5 Dy1 O4 63.89(12) . . ?
O1 Dy1 O4 122.75(12) . . ?
O12W Dy1 O4 72.22(14) . . ?
O11W Dy1 O4 137.23(13) . . ?
O13W Dy1 O4 127.38(12) . . ?
O7 Dy1 O4 67.72(12) . . ?
O8 Dy1 O4 100.97(12) . . ?
O3 Dy1 O4 60.34(10) . . ?
C1 O1 Dy1 125.7(3) . . ?
C3 O3 C2 117.4(4) . . ?
C3 O3 Dy1 119.9(3) . . ?
C2 O3 Dy1 116.7(3) . . ?
C8 O4 C9 117.0(4) . . ?
C8 O4 Dy1 118.7(3) . . ?
C9 O4 Dy1 117.0(3) . . ?
C10 O5 Dy1 128.7(3) . . ?
O2 C1 O1 124.8(5) . . ?
O2 C1 C2 116.5(4) . . ?
O1 C1 C2 118.7(4) . . ?
O3 C2 C1 109.4(4) . . ?
O3 C2 H2A 109.8 . . ?
C1 C2 H2A 109.8 . . ?
O3 C2 H2B 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.2 . . ?
C4 C3 C8 121.0(4) . . ?
C4 C3 O3 124.1(4) . . ?
C8 C3 O3 114.9(4) . . ?
C3 C4 C5 118.9(5) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
C6 C5 C4 120.4(5) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C5 C6 C7 121.1(5) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C6 C7 C8 119.1(5) . . ?
C6 C7 H7 120.5 . . ?
C8 C7 H7 120.5 . . ?
O4 C8 C3 115.2(4) . . ?
O4 C8 C7 125.2(4) . . ?
C3 C8 C7 119.5(5) . . ?
O4 C9 C10 109.1(4) . . ?
O4 C9 H9A 109.9 . . ?
C10 C9 H9A 109.9 . . ?
O4 C9 H9B 109.9 . . ?
C10 C9 H9B 109.9 . . ?
H9A C9 H9B 108.3 . . ?
O6 C10 O5 124.8(5) . . ?
O6 C10 C9 116.1(5) . . ?
O5 C10 C9 118.9(5) . . ?
C11A O7 Dy1 93.8(3) . . ?
C11A O8 Dy1 89.8(3) . . ?
O8 C11A O7 123.1(5) . . ?
O8 C11A C12 118.6(8) . . ?
O7 C11A C12 116.6(7) . . ?
O8 C11A C19 121.3(8) . 5_566 ?
O7 C11A C19 113.3(7) . 5_566 ?
O9 C12 C11A 116.5(13) . . ?
O9 C12 H12A 108.2 . . ?
C11A C12 H12A 108.2 . . ?
O9 C12 H12B 108.2 . . ?
C11A C12 H12B 108.2 . . ?
H12A C12 H12B 107.3 . . ?
C13 O9 C12 115.1(13) . . ?
O9 C13 C14 127.4(13) . . ?
O9 C13 C18 113.3(12) . . ?
C14 C13 C18 119.2(14) . . ?
C15 C14 C13 121.5(14) . . ?
C15 C14 H14 119.2 . . ?
C13 C14 H14 119.2 . . ?
C14 C15 C16 120.5(17) . . ?
C14 C15 H15 119.7 . . ?
C16 C15 H15 119.7 . . ?
C17 C16 C15 118.6(14) . . ?
C17 C16 H16 120.7 . . ?
C15 C16 H16 120.7 . . ?
C16 C17 C18 121.2(12) . . ?
C16 C17 H17 119.4 . . ?
C18 C17 H17 119.4 . . ?
O10 C18 C17 125.2(14) . . ?
O10 C18 C13 115.9(15) . . ?
C17 C18 C13 118.9(14) . . ?
C18 O10 C19 120.3(17) . . ?
O10 C19 C11B 110.1(13) . 5_566 ?
O10 C19 H19A 109.6 . . ?
C11B C19 H19A 109.6 5_566 . ?
O10 C19 H19B 109.6 . . ?
C11B C19 H19B 109.6 5_566 . ?
H19A C19 H19B 108.2 . . ?
Dy1 O11W H11A 125(5) . . ?
Dy1 O11W H11B 107(4) . . ?
H11A O11W H11B 108(6) . . ?
Dy1 O12W H12C 133(5) . . ?
Dy1 O12W H12D 122(7) . . ?
H12C O12W H12D 104(8) . . ?
Dy1 O13W H13A 123(6) . . ?
Dy1 O13W H13B 119(6) . . ?
H13A O13W H13B 118(8) . . ?
H14A O14W H14B 99(7) . . ?

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 O1 C1 O2 -176.0(3) . . . . ?
Dy1 O1 C1 C2 2.0(6) . . . . ?
C3 O3 C2 C1 -175.8(4) . . . . ?
Dy1 O3 C2 C1 -23.0(5) . . . . ?
O2 C1 C2 O3 -167.2(4) . . . . ?
O1 C1 C2 O3 14.6(6) . . . . ?
C2 O3 C3 C4 -0.5(7) . . . . ?
Dy1 O3 C3 C4 -152.3(4) . . . . ?
C2 O3 C3 C8 179.6(4) . . . . ?
Dy1 O3 C3 C8 27.7(5) . . . . ?
C8 C3 C4 C5 -1.5(7) . . . . ?
O3 C3 C4 C5 178.6(4) . . . . ?
C3 C4 C5 C6 1.6(8) . . . . ?
C4 C5 C6 C7 -0.4(8) . . . . ?
C5 C6 C7 C8 -1.0(8) . . . . ?
C9 O4 C8 C3 -173.9(4) . . . . ?
Dy1 O4 C8 C3 -24.3(5) . . . . ?
C9 O4 C8 C7 4.5(7) . . . . ?
Dy1 O4 C8 C7 154.1(4) . . . . ?
C4 C3 C8 O4 178.6(4) . . . . ?
O3 C3 C8 O4 -1.5(6) . . . . ?
C4 C3 C8 C7 0.1(7) . . . . ?
O3 C3 C8 C7 -180.0(4) . . . . ?
C6 C7 C8 O4 -177.2(5) . . . . ?
C6 C7 C8 C3 1.2(7) . . . . ?
C8 O4 C9 C10 166.5(4) . . . . ?
Dy1 O4 C9 C10 16.5(6) . . . . ?
Dy1 O5 C10 O6 174.0(4) . . . . ?
Dy1 O5 C10 C9 -2.1(7) . . . . ?
O4 C9 C10 O6 173.1(5) . . . . ?
O4 C9 C10 O5 -10.4(7) . . . . ?
Dy1 O8 C11A O7 2.3(6) . . . . ?
Dy1 O8 C11A C12 166.9(8) . . . . ?
Dy1 O8 C11A C19 -159.4(9) . . . 5_566 ?
Dy1 O7 C11A O8 -2.4(6) . . . . ?
Dy1 O7 C11A C12 -167.3(8) . . . . ?
Dy1 O7 C11A C19 160.7(8) . . . 5_566 ?
O8 C11A C12 O9 16.7(16) . . . . ?
O7 C11A C12 O9 -177.6(10) . . . . ?
C19 C11A C12 O9 -87(2) 5_566 . . . ?
C11A C12 O9 C13 71.6(18) . . . . ?
C12 O9 C13 C14 -11(2) . . . . ?
C12 O9 C13 C18 166.1(12) . . . . ?
O9 C13 C14 C15 178.3(16) . . . . ?
C18 C13 C14 C15 1.0(18) . . . . ?
C13 C14 C15 C16 1(2) . . . . ?
C14 C15 C16 C17 -4(2) . . . . ?
C15 C16 C17 C18 4(2) . . . . ?
C16 C17 C18 O10 177.6(16) . . . . ?
C16 C17 C18 C13 -2.0(17) . . . . ?
O9 C13 C18 O10 2.0(15) . . . . ?
C14 C13 C18 O10 179.7(14) . . . . ?
O9 C13 C18 C17 -178.4(13) . . . . ?
C14 C13 C18 C17 -0.7(16) . . . . ?
C17 C18 O10 C19 -17(3) . . . . ?
C13 C18 O10 C19 162.1(14) . . . . ?
C18 O10 C19 C11B 85(2) . . . 5_566 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C7 H7 O8 0.95 2.65 3.576(6) 163.8 1_545
C9 H9B O1 0.99 2.63 3.618(7) 174.6 1_545
O11W H11A O6 0.85(4) 1.96(4) 2.815(5) 173(7) 1_565
O11W H11B O6 0.86(4) 1.90(5) 2.743(6) 164(6) 7_665
O12W H12C O1 0.82(7) 1.91(7) 2.731(5) 174(7) 4_546
O12W H12D O14W 0.66(7) 2.26(7) 2.911(6) 171(9) 4_546
O13W H13A O14W 0.72(6) 2.03(6) 2.746(6) 173(8) .
O13W H13B O2 0.69(6) 2.03(7) 2.702(5) 165(9) 4_546
O14W H14A O2 0.82(8) 1.99(8) 2.814(6) 174(7) 6_657
O14W H14B O6 0.82(7) 2.10(7) 2.858(6) 152(7) 1_565
C19 H19B O16W 0.99 2.47 3.41(2) 158.4 7_565

_refine_diff_density_max         0.873
_refine_diff_density_min         -1.284
_refine_diff_density_rms         0.125


_exptl_crystal_recrystallization_method 'from hydrothermal reaction mixture'
_exptl_crystal_preparation       ', Magnetic properties'
####################################################################### 
# 
# 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
_database_code_depnum_ccdc_archive 'CCDC 1523868'
_audit_update_record             
;
2017-02-17 deposited with the CCDC.
2017-03-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        '{[Dy2(PDOA)3(H2O)6]?2H2O}n '
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H18 Dy O12, H2 O'
_chemical_formula_sum            'C15 H20 Dy O13'
_chemical_formula_weight         570.81

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'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'

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

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

_cell_length_a                   34.0219(7)
_cell_length_b                   12.6029(3)
_cell_length_c                   8.29345(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3556.01(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(1)
_cell_measurement_reflns_used    19423
_cell_measurement_theta_min      4.6690
_cell_measurement_theta_max      30.3620

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.132
_exptl_crystal_F_000             2240
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    4.276
_shelx_estimated_absorpt_T_min   0.369
_shelx_estimated_absorpt_T_max   0.868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.53570
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Multi-scan absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_detector_area_resol_mean 16.0655
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            42072
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         4.198
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_full        27.500
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             4078
_reflns_number_gt                3768
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SIR 92'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2007)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0174P)²+6.5144P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4078
_refine_ls_number_parameters     294
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0218
_refine_ls_R_factor_gt           0.0194
_refine_ls_wR_factor_ref         0.0438
_refine_ls_wR_factor_gt          0.0427
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.67857(2) 0.67913(2) 0.65962(2) 0.00916(4) Uani 1 1 d . . . . .
C1 C 0.64896(7) 0.55381(18) 0.9879(3) 0.0139(5) Uani 1 1 d . . . . .
C2 C 0.61389(7) 0.62622(19) 0.9684(3) 0.0158(5) Uani 1 1 d . . . . .
H2A H 0.592207 0.588254 0.913571 0.019 Uiso 1 1 calc R U . . .
H2B H 0.604440 0.650237 1.075287 0.019 Uiso 1 1 calc R U . . .
C3 C 0.60111(7) 0.80166(18) 0.8618(3) 0.0122(4) Uani 1 1 d . . . . .
C4 C 0.56389(7) 0.80657(19) 0.9284(3) 0.0152(5) Uani 1 1 d . . . . .
H4 H 0.554109 0.749237 0.991034 0.018 Uiso 1 1 calc R U . . .
C5 C 0.54087(7) 0.8965(2) 0.9028(3) 0.0179(5) Uani 1 1 d . . . . .
H5 H 0.515181 0.900119 0.947345 0.022 Uiso 1 1 calc R U . . .
C6 C 0.55513(8) 0.9804(2) 0.8129(3) 0.0180(5) Uani 1 1 d . . . . .
H6 H 0.539063 1.040876 0.794512 0.022 Uiso 1 1 calc R U . . .
C7 C 0.59300(7) 0.97674(18) 0.7493(3) 0.0156(5) Uani 1 1 d . . . . .
H7 H 0.602985 1.035165 0.689597 0.019 Uiso 1 1 calc R U . . .
C8 C 0.61598(7) 0.88767(18) 0.7733(3) 0.0115(4) Uani 1 1 d . . . . .
C9 C 0.66640(8) 0.95180(19) 0.5992(3) 0.0159(5) Uani 1 1 d . . . . .
H9A H 0.671130 1.020687 0.653166 0.019 Uiso 1 1 calc R U . . .
H9B H 0.645598 0.962087 0.517176 0.019 Uiso 1 1 calc R U . . .
C10 C 0.70365(7) 0.91455(18) 0.5186(3) 0.0127(4) Uani 1 1 d . . . . .
C11 C 0.59855(7) 0.74854(19) 0.4136(3) 0.0161(5) Uani 1 1 d . . . . .
C12 C 0.55715(7) 0.7606(2) 0.4810(3) 0.0186(5) Uani 1 1 d . . . . .
H12A H 0.552081 0.702193 0.558013 0.022 Uiso 1 1 calc R U . . .
H12B H 0.555537 0.828250 0.541463 0.022 Uiso 1 1 calc R U . . .
C13 C 0.51574(7) 0.6621(2) 0.3053(3) 0.0175(5) Uani 1 1 d . . . . .
C14 C 0.53212(9) 0.5665(2) 0.3522(3) 0.0253(6) Uani 1 1 d . . . . .
H14 H 0.554399 0.566037 0.421279 0.030 Uiso 1 1 calc R U . . .
C15 C 0.51624(9) 0.4709(2) 0.2992(4) 0.0315(7) Uani 1 1 d . . . . .
H15 H 0.527864 0.405684 0.331028 0.038 Uiso 1 1 calc R U . . .
O1 O 0.67759(5) 0.56875(13) 0.8948(2) 0.0149(3) Uani 1 1 d . . . . .
O2 O 0.64632(5) 0.48317(13) 1.0931(2) 0.0189(4) Uani 1 1 d . . . . .
O3 O 0.62630(5) 0.71577(13) 0.8734(2) 0.0139(3) Uani 1 1 d . . . . .
O4 O 0.65378(5) 0.87482(13) 0.7157(2) 0.0128(3) Uani 1 1 d . . . . .
O5 O 0.71515(5) 0.82090(12) 0.5438(2) 0.0144(3) Uani 1 1 d . . . . .
O6 O 0.72072(5) 0.98143(13) 0.43128(19) 0.0159(4) Uani 1 1 d . . . . .
O7 O 0.62467(5) 0.72606(15) 0.5160(2) 0.0210(4) Uani 1 1 d . . . . .
O8 O 0.60390(6) 0.76579(17) 0.2690(2) 0.0286(5) Uani 1 1 d . . . . .
O9 O 0.52733(5) 0.75973(14) 0.3602(2) 0.0205(4) Uani 1 1 d . . . . .
O10W O 0.73655(6) 0.58295(16) 0.6763(2) 0.0207(4) Uani 1 1 d . . . . .
H10C H 0.7495(11) 0.560(3) 0.593(5) 0.042(10) Uiso 1 1 d . . . . .
H10D H 0.7484(11) 0.569(3) 0.749(5) 0.042(12) Uiso 1 1 d . . . . .
O11W O 0.70350(6) 0.63536(16) 0.3953(2) 0.0158(4) Uani 1 1 d . . . . .
H11C H 0.6967(11) 0.677(3) 0.321(4) 0.032(10) Uiso 1 1 d . . . . .
H11D H 0.6975(11) 0.578(3) 0.369(4) 0.034(10) Uiso 1 1 d . . . . .
O12W O 0.71670(6) 0.76390(17) 0.8804(2) 0.0172(4) Uani 1 1 d . . . . .
H12C H 0.7213(11) 0.822(3) 0.863(4) 0.034(11) Uiso 1 1 d . . . . .
H12D H 0.7354(12) 0.737(3) 0.918(4) 0.039(11) Uiso 1 1 d . . . . .
O13W O 0.67993(6) 0.78375(17) 0.1906(3) 0.0227(4) Uani 1 1 d . . . . .
H13C H 0.6859(12) 0.778(3) 0.112(5) 0.045(13) Uiso 1 1 d . . . . .
H13D H 0.6526(11) 0.776(3) 0.209(4) 0.031(9) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O7 2.2652(17) . ?
Dy1 O10W 2.3195(19) . ?
Dy1 O5 2.3799(16) . ?
Dy1 O2 2.3856(17) 8_565 ?
Dy1 O1 2.3958(17) . ?
Dy1 O11W 2.4143(18) . ?
Dy1 O12W 2.4852(18) . ?
Dy1 O3 2.5530(17) . ?
Dy1 O4 2.6477(16) . ?
C1 O2 1.250(3) . ?
C1 O1 1.257(3) . ?
C1 C2 1.511(3) . ?
C2 O3 1.440(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.383(3) . ?
C3 O3 1.384(3) . ?
C3 C8 1.403(3) . ?
C4 C5 1.394(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.382(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.393(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.382(3) . ?
C7 H7 0.9500 . ?
C8 O4 1.381(3) . ?
C9 O4 1.435(3) . ?
C9 C10 1.508(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 O6 1.254(3) . ?
C10 O5 1.261(3) . ?
C11 O8 1.232(3) . ?
C11 O7 1.262(3) . ?
C11 C12 1.523(4) . ?
C12 O9 1.426(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 O9 1.370(3) . ?
C13 C14 1.384(4) . ?
C13 C13 1.410(5) 4_655 ?
C14 C15 1.391(4) . ?
C14 H14 0.9500 . ?
C15 C15 1.374(6) 4_655 ?
C15 H15 0.9500 . ?
O10W H10C 0.87(4) . ?
O10W H10D 0.75(4) . ?
O11W H11C 0.84(4) . ?
O11W H11D 0.78(4) . ?
O12W H12C 0.76(4) . ?
O12W H12D 0.78(4) . ?
O13W H13C 0.68(4) . ?
O13W H13D 0.95(4) . ?

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
O7 Dy1 O10W 148.91(7) . . ?
O7 Dy1 O5 90.87(6) . . ?
O10W Dy1 O5 88.38(7) . . ?
O7 Dy1 O2 74.34(7) . 8_565 ?
O10W Dy1 O2 87.53(7) . 8_565 ?
O5 Dy1 O2 142.27(6) . 8_565 ?
O7 Dy1 O1 124.64(6) . . ?
O10W Dy1 O1 70.11(6) . . ?
O5 Dy1 O1 140.51(6) . . ?
O2 Dy1 O1 71.58(6) 8_565 . ?
O7 Dy1 O11W 82.34(6) . . ?
O10W Dy1 O11W 68.66(7) . . ?
O5 Dy1 O11W 67.75(6) . . ?
O2 Dy1 O11W 75.86(6) 8_565 . ?
O1 Dy1 O11W 127.69(6) . . ?
O7 Dy1 O12W 134.24(7) . . ?
O10W Dy1 O12W 74.73(7) . . ?
O5 Dy1 O12W 72.64(6) . . ?
O2 Dy1 O12W 141.17(6) 8_565 . ?
O1 Dy1 O12W 69.95(6) . . ?
O11W Dy1 O12W 125.71(6) . . ?
O7 Dy1 O3 75.76(6) . . ?
O10W Dy1 O3 130.20(6) . . ?
O5 Dy1 O3 120.57(5) . . ?
O2 Dy1 O3 89.74(6) 8_565 . ?
O1 Dy1 O3 61.97(5) . . ?
O11W Dy1 O3 156.42(6) . . ?
O12W Dy1 O3 76.95(6) . . ?
O7 Dy1 O4 65.87(6) . . ?
O10W Dy1 O4 138.35(6) . . ?
O5 Dy1 O4 62.49(5) . . ?
O2 Dy1 O4 133.85(6) 8_565 . ?
O1 Dy1 O4 113.17(5) . . ?
O11W Dy1 O4 118.96(6) . . ?
O12W Dy1 O4 68.68(6) . . ?
O3 Dy1 O4 59.18(5) . . ?
O2 C1 O1 126.2(2) . . ?
O2 C1 C2 116.6(2) . . ?
O1 C1 C2 117.1(2) . . ?
O3 C2 C1 107.46(19) . . ?
O3 C2 H2A 110.2 . . ?
C1 C2 H2A 110.2 . . ?
O3 C2 H2B 110.2 . . ?
C1 C2 H2B 110.2 . . ?
H2A C2 H2B 108.5 . . ?
C4 C3 O3 125.0(2) . . ?
C4 C3 C8 120.3(2) . . ?
O3 C3 C8 114.7(2) . . ?
C3 C4 C5 119.3(2) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C6 C5 C4 120.5(2) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C5 C6 C7 120.2(2) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 H6 119.9 . . ?
C8 C7 C6 119.7(2) . . ?
C8 C7 H7 120.1 . . ?
C6 C7 H7 120.1 . . ?
O4 C8 C7 124.9(2) . . ?
O4 C8 C3 115.2(2) . . ?
C7 C8 C3 119.9(2) . . ?
O4 C9 C10 109.85(19) . . ?
O4 C9 H9A 109.7 . . ?
C10 C9 H9A 109.7 . . ?
O4 C9 H9B 109.7 . . ?
C10 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
O6 C10 O5 125.6(2) . . ?
O6 C10 C9 115.8(2) . . ?
O5 C10 C9 118.6(2) . . ?
O8 C11 O7 126.2(2) . . ?
O8 C11 C12 118.4(2) . . ?
O7 C11 C12 115.2(2) . . ?
O9 C12 C11 113.5(2) . . ?
O9 C12 H12A 108.9 . . ?
C11 C12 H12A 108.9 . . ?
O9 C12 H12B 108.9 . . ?
C11 C12 H12B 108.9 . . ?
H12A C12 H12B 107.7 . . ?
O9 C13 C14 125.0(2) . . ?
O9 C13 C13 115.76(13) . 4_655 ?
C14 C13 C13 119.27(16) . 4_655 ?
C13 C14 C15 120.6(3) . . ?
C13 C14 H14 119.7 . . ?
C15 C14 H14 119.7 . . ?
C15 C15 C14 120.02(16) 4_655 . ?
C15 C15 H15 120.0 4_655 . ?
C14 C15 H15 120.0 . . ?
C1 O1 Dy1 126.70(15) . . ?
C1 O2 Dy1 137.66(16) . 8_566 ?
C3 O3 C2 117.99(18) . . ?
C3 O3 Dy1 121.63(13) . . ?
C2 O3 Dy1 116.28(13) . . ?
C8 O4 C9 115.61(18) . . ?
C8 O4 Dy1 117.81(13) . . ?
C9 O4 Dy1 114.60(13) . . ?
C10 O5 Dy1 127.41(15) . . ?
C11 O7 Dy1 169.38(18) . . ?
C13 O9 C12 116.45(19) . . ?
Dy1 O10W H10C 124(2) . . ?
Dy1 O10W H10D 129(3) . . ?
H10C O10W H10D 107(4) . . ?
Dy1 O11W H11C 115(2) . . ?
Dy1 O11W H11D 112(3) . . ?
H11C O11W H11D 108(3) . . ?
Dy1 O12W H12C 112(3) . . ?
Dy1 O12W H12D 122(3) . . ?
H12C O12W H12D 109(4) . . ?
H13C O13W H13D 116(4) . . ?

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
O2 C1 C2 O3 165.9(2) . . . . ?
O1 C1 C2 O3 -15.6(3) . . . . ?
O3 C3 C4 C5 -177.6(2) . . . . ?
C8 C3 C4 C5 1.9(4) . . . . ?
C3 C4 C5 C6 -0.6(4) . . . . ?
C4 C5 C6 C7 -1.1(4) . . . . ?
C5 C6 C7 C8 1.4(4) . . . . ?
C6 C7 C8 O4 179.8(2) . . . . ?
C6 C7 C8 C3 -0.1(3) . . . . ?
C4 C3 C8 O4 178.6(2) . . . . ?
O3 C3 C8 O4 -1.9(3) . . . . ?
C4 C3 C8 C7 -1.5(3) . . . . ?
O3 C3 C8 C7 178.0(2) . . . . ?
O4 C9 C10 O6 -170.1(2) . . . . ?
O4 C9 C10 O5 9.6(3) . . . . ?
O8 C11 C12 O9 17.9(3) . . . . ?
O7 C11 C12 O9 -165.3(2) . . . . ?
O9 C13 C14 C15 174.9(3) . . . . ?
C13 C13 C14 C15 -4.0(5) 4_655 . . . ?
C13 C14 C15 C15 -0.7(6) . . . 4_655 ?
O2 C1 O1 Dy1 166.82(18) . . . . ?
C2 C1 O1 Dy1 -11.5(3) . . . . ?
O1 C1 O2 Dy1 -15.8(4) . . . 8_566 ?
C2 C1 O2 Dy1 162.58(17) . . . 8_566 ?
C4 C3 O3 C2 -3.2(3) . . . . ?
C8 C3 O3 C2 177.2(2) . . . . ?
C4 C3 O3 Dy1 153.18(18) . . . . ?
C8 C3 O3 Dy1 -26.4(3) . . . . ?
C1 C2 O3 C3 -169.44(19) . . . . ?
C1 C2 O3 Dy1 32.9(2) . . . . ?
C7 C8 O4 C9 -11.9(3) . . . . ?
C3 C8 O4 C9 168.0(2) . . . . ?
C7 C8 O4 Dy1 -152.64(19) . . . . ?
C3 C8 O4 Dy1 27.2(2) . . . . ?
C10 C9 O4 C8 -166.74(19) . . . . ?
C10 C9 O4 Dy1 -24.7(2) . . . . ?
O6 C10 O5 Dy1 -165.92(17) . . . . ?
C9 C10 O5 Dy1 14.4(3) . . . . ?
O8 C11 O7 Dy1 -16.2(11) . . . . ?
C12 C11 O7 Dy1 167.3(8) . . . . ?
C14 C13 O9 C12 -3.4(4) . . . . ?
C13 C13 O9 C12 175.5(3) 4_655 . . . ?
C11 C12 O9 C13 81.3(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C2 H2B O8 0.99 2.17 3.069(3) 150.6 1_556
C7 H7 O8 0.95 2.59 3.270(3) 128.4 8_576
C9 H9A O13W 0.99 2.50 3.449(3) 159.9 8_576
O10W H10D O6 0.75(4) 1.95(4) 2.691(3) 174(4) 2_665
O10W H10C O6 0.87(4) 1.95(4) 2.807(3) 168(3) 7_755
O13W H13D O8 0.95(4) 1.74(4) 2.677(3) 173(3) .
O13W H13C O12W 0.68(4) 2.20(4) 2.872(3) 169(5) 1_554
O11W H11D O1 0.78(4) 1.98(4) 2.719(3) 157(3) 8_565
O12W H12C O6 0.76(4) 2.54(4) 3.240(3) 153(3) 8_576
O12W H12D O5 0.78(4) 2.11(4) 2.891(3) 173(4) 2_665
O11W H11C O13W 0.84(4) 1.82(4) 2.650(3) 169(3) .
C2 H2B O8 0.99 2.17 3.069(3) 150.6 1_556
C7 H7 O8 0.95 2.59 3.270(3) 128.4 8_576
C9 H9A O13W 0.99 2.50 3.449(3) 159.9 8_576
O10W H10D O6 0.75(4) 1.95(4) 2.691(3) 174(4) 2_665
O10W H10C O6 0.87(4) 1.95(4) 2.807(3) 168(3) 7_755
O13W H13D O8 0.95(4) 1.74(4) 2.677(3) 173(3) .
O13W H13C O12W 0.68(4) 2.20(4) 2.872(3) 169(5) 1_554
O12W H12C O6 0.76(4) 2.54(4) 3.240(3) 153(3) 8_576
O12W H12D O5 0.78(4) 2.11(4) 2.891(3) 173(4) 2_665

_refine_diff_density_max         0.895
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.091


_exptl_crystal_recrystallization_method 'crystallized from the reaction mixture'
_exptl_crystal_preparation       ', Magnetic properties'
