# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 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_1
_audit_block_doi                 10.5517/cc1jqk71
_database_code_depnum_ccdc_archive 'CCDC 1421853'
_audit_update_record             
;
2016-01-23 deposited with the CCDC.
2016-01-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H18 K O11 Tb, 4H2O'
_chemical_formula_sum            'C28 H26 K O15 Tb'
_chemical_formula_weight         800.53

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           126
_space_group_name_H-M_alt        'P 4/n n c'
_space_group_name_Hall           '-P 4a 2bc'

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

_cell_length_a                   15.513(2)
_cell_length_b                   15.513(2)
_cell_length_c                   26.445(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6364.1(19)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4165
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      27.19

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3056
_exptl_absorpt_coefficient_mu    2.418
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.608
_exptl_absorpt_correction_T_max  0.679
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            31247
_diffrn_reflns_av_R_equivalents  0.1285
_diffrn_reflns_av_sigmaI/netI    0.0594
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.41
_diffrn_reflns_theta_max         27.47
_reflns_number_total             3669
_reflns_number_gt                1847
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1477P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3613
_refine_ls_number_parameters     203
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.1178
_refine_ls_R_factor_gt           0.0719
_refine_ls_wR_factor_ref         0.2427
_refine_ls_wR_factor_gt          0.2050
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_restrained_S_all      0.983
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4521(7) 0.5590(7) 0.6820(3) 0.066(2) Uani 1 1 d . . .
C2 C 0.4576(6) 0.6246(6) 0.6401(3) 0.072(3) Uani 1 1 d . . .
C3 C 0.5249(7) 0.6228(7) 0.6069(3) 0.088(3) Uani 1 1 d . . .
H3 H 0.5678 0.5813 0.6096 0.105 Uiso 1 1 calc R . .
C4 C 0.5278(9) 0.6856(7) 0.5680(3) 0.101(4) Uani 1 1 d . . .
H4 H 0.5739 0.6864 0.5455 0.121 Uiso 1 1 calc R . .
C5 C 0.4616(10) 0.7467(6) 0.5631(3) 0.092(4) Uani 1 1 d . . .
C6 C 0.3911(10) 0.7461(6) 0.5946(4) 0.099(4) Uani 1 1 d . . .
H6 H 0.3465 0.7857 0.5909 0.119 Uiso 1 1 calc R . .
C7 C 0.3895(8) 0.6819(8) 0.6332(3) 0.114(4) Uani 1 1 d . . .
H7 H 0.3418 0.6783 0.6544 0.137 Uiso 1 1 calc R . .
C8 C 0.4892(6) 0.7940(7) 0.4790(3) 0.077(3) Uani 1 1 d . . .
C9 C 0.4594(7) 0.7214(7) 0.4551(3) 0.073(2) Uani 1 1 d . . .
H9 H 0.4257 0.6817 0.4725 0.087 Uiso 1 1 calc R . .
C10 C 0.4805(6) 0.7075(7) 0.4039(2) 0.069(2) Uani 1 1 d . . .
H10 H 0.4604 0.6588 0.3871 0.083 Uiso 1 1 calc R . .
C11 C 0.5319(7) 0.7679(6) 0.3785(2) 0.062(2) Uani 1 1 d . . .
C12 C 0.5587(6) 0.8390(6) 0.4034(2) 0.074(3) Uani 1 1 d . . .
H12 H 0.5924 0.8794 0.3865 0.089 Uiso 1 1 calc R . .
C13 C 0.5370(7) 0.8533(6) 0.4540(2) 0.083(3) Uani 1 1 d . . .
H13 H 0.5553 0.9031 0.4703 0.099 Uiso 1 1 calc R . .
C14 C 0.5557(6) 0.7511(6) 0.3241(3) 0.061(3) Uani 1 1 d . . .
Tb1 Tb 0.42446(3) 0.42446(3) 0.7500 0.0620(3) Uani 1 2 d S . .
K1 K 0.7500 0.7500 0.2500 0.0557(17) Uani 0.80 8 d SP . .
O1 O 0.3886(4) 0.5640(4) 0.71310(19) 0.0811(19) Uani 1 1 d . . .
O2 O 0.5078(5) 0.5017(5) 0.6850(2) 0.091(2) Uani 1 1 d . . .
O3 O 0.4657(5) 0.8135(4) 0.52827(18) 0.102(2) Uani 1 1 d . . .
O4 O 0.5270(4) 0.6870(4) 0.30232(16) 0.0679(17) Uani 1 1 d . . .
O5 O 0.6057(4) 0.8070(4) 0.30351(15) 0.0682(16) Uani 1 1 d . . .
K2 K 0.2500 0.6295(5) 0.7500 0.137(2) Uani 0.80 2 d SP . .
O2W O 0.948(3) 0.787(4) 0.7635(15) 0.54(3) Uani 1 1 d DU . .
O1W O 0.101(5) 0.7500 0.7500 0.54(4) Uani 1 2 d S . .
O3W O 0.7500 0.7500 0.395(13) 1.0(2) Uani 1 4 d S . .
H4W H 0.903(3) 0.7500 0.7500 1.565 Uiso 1 2 d SD . .
H3W H 0.992(3) 0.7500 0.7500 1.565 Uiso 1 2 d SD . .
O4W O 0.7500 0.7500 0.688(3) 1.4(4) Uani 1 4 d S . .


_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
C1 O2 1.243(10) . ?
C1 O1 1.286(11) . ?
C1 C2 1.506(10) . ?
C2 C3 1.364(11) . ?
C2 C7 1.393(14) . ?
C3 C4 1.417(11) . ?
C3 H3 0.9300 . ?
C4 C5 1.403(16) . ?
C4 H4 0.9300 . ?
C5 C6 1.373(18) . ?
C5 O3 1.389(9) . ?
C6 C7 1.427(11) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C13 1.355(12) . ?
C8 C9 1.371(14) . ?
C8 O3 1.387(8) . ?
C9 C10 1.411(9) . ?
C9 H9 0.9300 . ?
C10 C11 1.401(12) . ?
C10 H10 0.9300 . ?
C11 C12 1.352(11) . ?
C11 C14 1.508(10) . ?
C12 C13 1.395(9) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 O4 1.233(9) . ?
C14 O5 1.284(10) . ?
C14 K2 3.477(11) 12_666 ?
Tb1 O4 2.339(6) 9_666 ?
Tb1 O4 2.339(6) 15_666 ?
Tb1 O5 2.354(5) 11_566 ?
Tb1 O5 2.354(5) 14_656 ?
Tb1 O1 2.439(6) 7_556 ?
Tb1 O1 2.439(6) . ?
Tb1 O2 2.461(7) 7_556 ?
Tb1 O2 2.461(7) . ?
Tb1 C1 2.789(8) 7_556 ?
Tb1 K1 3.8274(9) 9_666 ?
Tb1 K2 4.176(6) 4 ?
K1 O5 2.793(6) 4_565 ?
K1 O5 2.793(6) 6_565 ?
K1 O5 2.793(6) 8_665 ?
K1 O5 2.793(6) 5_655 ?
K1 O5 2.793(6) 2_665 ?
K1 O5 2.793(6) . ?
K1 O5 2.793(6) 7 ?
K1 O5 2.793(6) 3_655 ?
K1 Tb1 3.8274(9) 10_666 ?
K1 Tb1 3.8274(9) 9_666 ?
K1 Tb1 3.8274(9) 12_666 ?
K1 Tb1 3.8274(9) 11_666 ?
O1 K2 2.570(7) . ?
O4 Tb1 2.339(6) 9_666 ?
O4 K2 2.960(9) 12_666 ?
O5 Tb1 2.354(5) 12_666 ?
K2 O1 2.570(7) 5_556 ?
K2 O1W 2.98(6) 2_565 ?
K2 O1W 2.98(6) . ?
K2 O4 2.960(9) 11_566 ?
K2 O4 2.960(9) 15_666 ?
K2 C14 3.477(11) 11_566 ?
K2 C14 3.477(11) 15_666 ?
K2 K2 3.739(16) 2_565 ?
K2 Tb1 4.176(6) 3 ?
O2W H4W 0.96(2) . ?
O2W H3W 0.96(2) . ?
O2W O2W 1.35(6) 6_566 ?
O2W H4W 0.96(2) . ?
O2W H3W 0.96(2) . ?
O1W K2 2.98(6) 2_565 ?

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 C1 O1 122.2(7) . . ?
O2 C1 C2 119.5(8) . . ?
O1 C1 C2 118.3(9) . . ?
C3 C2 C7 120.6(8) . . ?
C3 C2 C1 120.3(9) . . ?
C7 C2 C1 118.9(8) . . ?
C2 C3 C4 118.5(10) . . ?
C2 C3 H3 120.7 . . ?
C4 C3 H3 120.7 . . ?
C3 C4 C5 120.5(10) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.8 . . ?
C6 C5 O3 116.3(11) . . ?
C6 C5 C4 121.5(8) . . ?
O3 C5 C4 122.0(10) . . ?
C5 C6 C7 116.8(11) . . ?
C5 C6 H6 121.5 . . ?
C7 C6 H6 121.6 . . ?
C2 C7 C6 121.8(10) . . ?
C2 C7 H7 119.2 . . ?
C6 C7 H7 119.0 . . ?
C13 C8 C9 121.2(7) . . ?
C13 C8 O3 117.0(8) . . ?
C9 C8 O3 121.6(8) . . ?
C8 C9 C10 119.3(8) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.4 . . ?
C11 C10 C9 119.3(9) . . ?
C11 C10 H10 120.4 . . ?
C9 C10 H10 120.3 . . ?
C12 C11 C10 119.2(7) . . ?
C12 C11 C14 122.0(7) . . ?
C10 C11 C14 118.7(8) . . ?
C11 C12 C13 121.5(8) . . ?
C11 C12 H12 119.2 . . ?
C13 C12 H12 119.3 . . ?
C8 C13 C12 119.4(9) . . ?
C8 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
O4 C14 O5 124.4(7) . . ?
O4 C14 C11 119.7(7) . . ?
O5 C14 C11 115.9(8) . . ?
O4 C14 K2 55.6(4) . 12_666 ?
O5 C14 K2 105.3(5) . 12_666 ?
C11 C14 K2 109.7(6) . 12_666 ?
O4 Tb1 O4 145.7(3) 9_666 15_666 ?
O4 Tb1 O5 75.34(19) 9_666 11_566 ?
O4 Tb1 O5 81.2(2) 15_666 11_566 ?
O4 Tb1 O5 81.2(2) 9_666 14_656 ?
O4 Tb1 O5 75.34(19) 15_666 14_656 ?
O5 Tb1 O5 93.1(3) 11_566 14_656 ?
O4 Tb1 O1 77.4(2) 9_666 7_556 ?
O4 Tb1 O1 119.54(18) 15_666 7_556 ?
O5 Tb1 O1 151.9(2) 11_566 7_556 ?
O5 Tb1 O1 76.1(2) 14_656 7_556 ?
O4 Tb1 O1 119.54(18) 9_666 . ?
O4 Tb1 O1 77.4(2) 15_666 . ?
O5 Tb1 O1 76.1(2) 11_566 . ?
O5 Tb1 O1 151.9(2) 14_656 . ?
O1 Tb1 O1 124.4(3) 7_556 . ?
O4 Tb1 O2 130.1(2) 9_666 7_556 ?
O4 Tb1 O2 77.2(2) 15_666 7_556 ?
O5 Tb1 O2 154.2(2) 11_566 7_556 ?
O5 Tb1 O2 94.8(2) 14_656 7_556 ?
O1 Tb1 O2 53.8(2) 7_556 7_556 ?
O1 Tb1 O2 85.6(2) . 7_556 ?
O4 Tb1 O2 77.2(2) 9_666 . ?
O4 Tb1 O2 130.1(2) 15_666 . ?
O5 Tb1 O2 94.8(2) 11_566 . ?
O5 Tb1 O2 154.2(2) 14_656 . ?
O1 Tb1 O2 85.6(2) 7_556 . ?
O1 Tb1 O2 53.8(2) . . ?
O2 Tb1 O2 88.6(4) 7_556 . ?
O4 Tb1 C1 104.7(3) 9_666 7_556 ?
O4 Tb1 C1 97.0(3) 15_666 7_556 ?
O5 Tb1 C1 176.1(2) 11_566 7_556 ?
O5 Tb1 C1 83.1(2) 14_656 7_556 ?
O1 Tb1 C1 27.4(3) 7_556 7_556 ?
O1 Tb1 C1 107.0(3) . 7_556 ?
O2 Tb1 C1 26.5(2) 7_556 7_556 ?
O2 Tb1 C1 89.0(3) . 7_556 ?
O4 Tb1 K1 72.85(16) 9_666 9_666 ?
O4 Tb1 K1 72.85(16) 15_666 9_666 ?
O5 Tb1 K1 46.55(14) 11_566 9_666 ?
O5 Tb1 K1 46.55(14) 14_656 9_666 ?
O1 Tb1 K1 117.80(16) 7_556 9_666 ?
O1 Tb1 K1 117.80(16) . 9_666 ?
O2 Tb1 K1 135.69(19) 7_556 9_666 ?
O2 Tb1 K1 135.69(19) . 9_666 ?
C1 Tb1 K1 129.64(19) 7_556 9_666 ?
O4 Tb1 K2 43.59(14) 9_666 4 ?
O4 Tb1 K2 140.51(13) 15_666 4 ?
O5 Tb1 K2 117.44(17) 11_566 4 ?
O5 Tb1 K2 69.49(17) 14_656 4 ?
O1 Tb1 K2 34.53(15) 7_556 4 ?
O1 Tb1 K2 138.50(17) . 4 ?
O2 Tb1 K2 88.27(18) 7_556 4 ?
O2 Tb1 K2 85.13(18) . 4 ?
C1 Tb1 K2 61.9(2) 7_556 4 ?
K1 Tb1 K2 94.61(7) 9_666 4 ?
O5 K1 O5 139.9(3) 4_565 6_565 ?
O5 K1 O5 73.4(2) 4_565 8_665 ?
O5 K1 O5 75.12(9) 6_565 8_665 ?
O5 K1 O5 75.4(2) 4_565 5_655 ?
O5 K1 O5 119.1(2) 6_565 5_655 ?
O5 K1 O5 75.12(9) 8_665 5_655 ?
O5 K1 O5 75.12(9) 4_565 2_665 ?
O5 K1 O5 143.1(3) 6_565 2_665 ?
O5 K1 O5 139.9(3) 8_665 2_665 ?
O5 K1 O5 73.4(2) 5_655 2_665 ?
O5 K1 O5 75.12(9) 4_565 . ?
O5 K1 O5 73.4(2) 6_565 . ?
O5 K1 O5 75.4(2) 8_665 . ?
O5 K1 O5 143.1(3) 5_655 . ?
O5 K1 O5 119.1(2) 2_665 . ?
O5 K1 O5 143.1(3) 4_565 7 ?
O5 K1 O5 75.12(9) 6_565 7 ?
O5 K1 O5 119.1(2) 8_665 7 ?
O5 K1 O5 75.12(9) 5_655 7 ?
O5 K1 O5 75.4(2) 2_665 7 ?
O5 K1 O5 139.9(3) . 7 ?
O5 K1 O5 119.1(2) 4_565 3_655 ?
O5 K1 O5 75.4(2) 6_565 3_655 ?
O5 K1 O5 143.1(3) 8_665 3_655 ?
O5 K1 O5 139.9(3) 5_655 3_655 ?
O5 K1 O5 75.12(9) 2_665 3_655 ?
O5 K1 O5 75.12(9) . 3_655 ?
O5 K1 O5 73.4(2) 7 3_655 ?
O5 K1 Tb1 37.72(10) 4_565 10_666 ?
O5 K1 Tb1 142.28(10) 6_565 10_666 ?
O5 K1 Tb1 69.94(13) 8_665 10_666 ?
O5 K1 Tb1 37.72(10) 5_655 10_666 ?
O5 K1 Tb1 69.94(13) 2_665 10_666 ?
O5 K1 Tb1 110.06(13) . 10_666 ?
O5 K1 Tb1 110.06(13) 7 10_666 ?
O5 K1 Tb1 142.28(10) 3_655 10_666 ?
O5 K1 Tb1 142.28(10) 4_565 9_666 ?
O5 K1 Tb1 37.72(10) 6_565 9_666 ?
O5 K1 Tb1 110.06(13) 8_665 9_666 ?
O5 K1 Tb1 142.28(10) 5_655 9_666 ?
O5 K1 Tb1 110.06(13) 2_665 9_666 ?
O5 K1 Tb1 69.94(13) . 9_666 ?
O5 K1 Tb1 69.94(13) 7 9_666 ?
O5 K1 Tb1 37.72(10) 3_655 9_666 ?
Tb1 K1 Tb1 180.0 10_666 9_666 ?
O5 K1 Tb1 69.94(13) 4_565 12_666 ?
O5 K1 Tb1 69.94(13) 6_565 12_666 ?
O5 K1 Tb1 37.72(10) 8_665 12_666 ?
O5 K1 Tb1 110.06(13) 5_655 12_666 ?
O5 K1 Tb1 142.28(10) 2_665 12_666 ?
O5 K1 Tb1 37.72(10) . 12_666 ?
O5 K1 Tb1 142.28(10) 7 12_666 ?
O5 K1 Tb1 110.06(13) 3_655 12_666 ?
Tb1 K1 Tb1 90.0 10_666 12_666 ?
Tb1 K1 Tb1 90.0 9_666 12_666 ?
O5 K1 Tb1 110.06(13) 4_565 11_666 ?
O5 K1 Tb1 110.06(13) 6_565 11_666 ?
O5 K1 Tb1 142.28(10) 8_665 11_666 ?
O5 K1 Tb1 69.94(13) 5_655 11_666 ?
O5 K1 Tb1 37.72(10) 2_665 11_666 ?
O5 K1 Tb1 142.28(10) . 11_666 ?
O5 K1 Tb1 37.72(10) 7 11_666 ?
O5 K1 Tb1 69.94(13) 3_655 11_666 ?
Tb1 K1 Tb1 90.0 10_666 11_666 ?
Tb1 K1 Tb1 90.0 9_666 11_666 ?
Tb1 K1 Tb1 180.0 12_666 11_666 ?
C1 O1 Tb1 91.6(6) . . ?
C1 O1 K2 155.2(6) . . ?
Tb1 O1 K2 112.9(3) . . ?
C1 O2 Tb1 91.6(5) . . ?
C8 O3 C5 118.2(7) . . ?
C14 O4 Tb1 139.2(6) . 9_666 ?
C14 O4 K2 104.4(5) . 12_666 ?
Tb1 O4 K2 103.39(18) 9_666 12_666 ?
C14 O5 Tb1 131.1(6) . 12_666 ?
C14 O5 K1 119.0(5) . . ?
Tb1 O5 K1 95.72(16) 12_666 . ?
O1 K2 O1 133.4(4) . 5_556 ?
O1 K2 O1W 66.2(8) . 2_565 ?
O1 K2 O1W 154.0(5) 5_556 2_565 ?
O1 K2 O1W 154.0(5) . . ?
O1 K2 O1W 66.2(8) 5_556 . ?
O1W K2 O1W 102.2(17) 2_565 . ?
O1 K2 O4 77.0(2) . 11_566 ?
O1 K2 O4 65.0(2) 5_556 11_566 ?
O1W K2 O4 140.5(6) 2_565 11_566 ?
O1W K2 O4 105.0(8) . 11_566 ?
O1 K2 O4 65.0(2) . 15_666 ?
O1 K2 O4 77.0(2) 5_556 15_666 ?
O1W K2 O4 105.0(8) 2_565 15_666 ?
O1W K2 O4 140.5(6) . 15_666 ?
O4 K2 O4 69.8(3) 11_566 15_666 ?
O1 K2 C14 57.0(2) . 11_566 ?
O1 K2 C14 83.8(3) 5_556 11_566 ?
O1W K2 C14 121.0(7) 2_565 11_566 ?
O1W K2 C14 121.5(7) . 11_566 ?
O4 K2 C14 20.09(17) 11_566 11_566 ?
O4 K2 C14 65.4(2) 15_666 11_566 ?
O1 K2 C14 83.8(3) . 15_666 ?
O1 K2 C14 57.0(2) 5_556 15_666 ?
O1W K2 C14 121.5(7) 2_565 15_666 ?
O1W K2 C14 121.0(7) . 15_666 ?
O4 K2 C14 65.4(2) 11_566 15_666 ?
O4 K2 C14 20.09(17) 15_666 15_666 ?
C14 K2 C14 68.6(3) 11_566 15_666 ?
O1 K2 K2 113.3(2) . 2_565 ?
O1 K2 K2 113.3(2) 5_556 2_565 ?
O1W K2 K2 51.1(9) 2_565 2_565 ?
O1W K2 K2 51.1(9) . 2_565 ?
O4 K2 K2 145.09(14) 11_566 2_565 ?
O4 K2 K2 145.09(14) 15_666 2_565 ?
C14 K2 K2 145.70(15) 11_566 2_565 ?
C14 K2 K2 145.70(15) 15_666 2_565 ?
O1 K2 Tb1 104.0(3) . 3 ?
O1 K2 Tb1 32.54(15) 5_556 3 ?
O1W K2 Tb1 169.3(9) 2_565 3 ?
O1W K2 Tb1 88.5(9) . 3 ?
O4 K2 Tb1 33.02(12) 11_566 3 ?
O4 K2 Tb1 65.75(18) 15_666 3 ?
C14 K2 Tb1 51.26(17) 11_566 3 ?
C14 K2 Tb1 50.77(16) 15_666 3 ?
K2 K2 Tb1 139.61(7) 2_565 3 ?
H4W O2W H3W 91(3) . . ?
H4W O2W O2W 45.6(14) . 6_566 ?
H3W O2W O2W 45.6(14) . 6_566 ?
H4W O2W H4W 0(4) . . ?
H3W O2W H4W 91(3) . . ?
O2W O2W H4W 45.6(14) 6_566 . ?
H4W O2W H3W 91(3) . . ?
H3W O2W H3W 0.000(10) . . ?
O2W O2W H3W 45.6(14) 6_566 . ?
H4W O2W H3W 91(3) . . ?
K2 O1W K2 77.8(17) 2_565 . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         2.047
_refine_diff_density_min         -4.281
_refine_diff_density_rms         0.167

# start Validation Reply Form
_vrf_PLAT972_1                   
;
PROBLEM: Check Calcd Residual Density  0.79A From     Tb1      -4.41 eA-3  
RESPONSE: It should be due to the not perfect crystal quality. 
The Tb content has been proved by elemental analysis.
;
_vrf_PLAT973_1                   
;
PROBLEM: Check Calcd Positive Residual Density on      K1       2.55 eA-3  
RESPONSE: It should be due to the not perfect crystal quality. 
The K content has been proved by elemental analysis.
;
####################################################################### 
# 
# 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
_audit_block_doi                 10.5517/cc1jqk82
_database_code_depnum_ccdc_archive 'CCDC 1421854'
_audit_update_record             
;
2016-01-23 deposited with the CCDC.
2016-01-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H18 Dy K O11, 4H2O'
_chemical_formula_sum            'C28 H26 Dy K O15'
_chemical_formula_weight         804.11

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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      tetragonal
_space_group_IT_number           126
_space_group_name_H-M_alt        'P 4/n n c'
_space_group_name_Hall           '-P 4a 2bc'

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

_cell_length_a                   15.322(2)
_cell_length_b                   15.322(2)
_cell_length_c                   26.327(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6180.6(19)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6831
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      27.32

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3050.4
_exptl_absorpt_coefficient_mu    2.593
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.633
_exptl_absorpt_correction_T_max  0.714
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29264
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_sigmaI/netI    0.0219
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.54
_diffrn_reflns_theta_max         25.25
_reflns_number_total             2816
_reflns_number_gt                1893
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1650P)²+97.6540P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2815
_refine_ls_number_parameters     212
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1078
_refine_ls_R_factor_gt           0.0822
_refine_ls_wR_factor_ref         0.3021
_refine_ls_wR_factor_gt          0.2537
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.369
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0481(14) 0.9379(14) 0.6825(7) 0.063(5) Uani 1 1 d . . .
C2 C 0.0431(13) 0.8739(13) 0.6405(6) 0.063(5) Uani 1 1 d . . .
C3 C -0.0249(14) 0.8730(14) 0.6070(7) 0.070(5) Uani 1 1 d . . .
H3 H -0.0691 0.9143 0.6101 0.084 Uiso 1 1 calc R . .
C4 C -0.0289(16) 0.8118(16) 0.5687(7) 0.080(6) Uani 1 1 d . . .
H4 H -0.0759 0.8114 0.5464 0.096 Uiso 1 1 calc R . .
C5 C 0.0362(17) 0.7521(12) 0.5638(7) 0.068(6) Uani 1 1 d . . .
C6 C 0.108(2) 0.7536(16) 0.5952(9) 0.100(9) Uani 1 1 d . . .
H6 H 0.1533 0.7140 0.5909 0.120 Uiso 1 1 calc R . .
C7 C 0.1107(17) 0.8158(16) 0.6334(8) 0.092(8) Uani 1 1 d . . .
H7 H 0.1591 0.8183 0.6547 0.110 Uiso 1 1 calc R . .
C8 C 0.0115(14) 0.7059(12) 0.4786(6) 0.062(5) Uani 1 1 d . . .
C9 C 0.0402(13) 0.7792(13) 0.4549(6) 0.061(5) Uani 1 1 d . . .
H9 H 0.0733 0.8202 0.4724 0.073 Uiso 1 1 calc R . .
C10 C 0.0194(11) 0.7921(12) 0.4043(6) 0.053(4) Uani 1 1 d . . .
H10 H 0.0396 0.8415 0.3875 0.063 Uiso 1 1 calc R . .
C11 C -0.0311(12) 0.7320(11) 0.3785(6) 0.050(4) Uani 1 1 d . . .
C12 C -0.0583(13) 0.6590(12) 0.4032(6) 0.060(5) Uani 1 1 d . . .
H12 H -0.0915 0.6180 0.3857 0.072 Uiso 1 1 calc R . .
C13 C -0.0381(15) 0.6442(13) 0.4535(6) 0.069(5) Uani 1 1 d . . .
H13 H -0.0573 0.5941 0.4700 0.083 Uiso 1 1 calc R . .
C14 C -0.0552(12) 0.7467(11) 0.3239(6) 0.051(4) Uani 1 1 d . . .
Dy1 Dy 0.07484(5) 1.07484(5) 0.7500 0.0488(6) Uani 1 2 d S . .
K1 K 0.2500 1.2500 0.7500 0.057(3) Uani 0.26 8 d SP . .
K2 K 0.2500 0.8700(11) 0.7500 0.115(4) Uani 0.74 2 d SP . .
O1 O 0.1093(10) 0.9344(9) 0.7138(5) 0.071(4) Uani 1 1 d . . .
O2 O -0.0076(9) 0.9984(10) 0.6858(5) 0.069(4) Uani 1 1 d . . .
O3 O 0.0336(12) 0.6847(9) 0.5285(5) 0.087(5) Uani 1 1 d . . .
O4 O -0.0255(8) 0.8135(8) 0.3024(4) 0.055(3) Uani 1 1 d . . .
O5 O -0.1054(8) 0.6918(8) 0.3027(4) 0.054(3) Uani 1 1 d . . .
O1W O 0.118(3) 0.7500 0.7500 0.47(8) Uani 1 2 d S . .
O2W O 0.9502(18) 0.707(4) 0.719(3) 0.30(3) Uani 1 1 d D . .
O3W O 0.7500 0.7500 0.6677(9) 0.050(5) Uani 1 4 d S . .
O4W O 0.7500 0.7500 0.5305(9) 0.050(5) Uani 1 4 d S . .
H3W H 0.90(5) 0.69(9) 0.74(4) 0.5(8) Uiso 1 1 d D . .
H4W H 0.89(3) 0.70(11) 0.70(4) 0.5(7) Uiso 1 1 d 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
C1 O1 1.25(2) . ?
C1 O2 1.26(2) . ?
C1 C2 1.48(2) . ?
C2 C3 1.36(3) . ?
C2 C7 1.38(3) . ?
C3 C4 1.38(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.36(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.38(4) . ?
C5 O3 1.39(2) . ?
C6 C7 1.38(3) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.36(3) . ?
C8 C13 1.38(3) . ?
C8 O3 1.39(2) . ?
C9 C10 1.38(2) . ?
C9 H9 0.9300 . ?
C10 C11 1.38(2) . ?
C10 H10 0.9300 . ?
C11 C12 1.36(2) . ?
C11 C14 1.50(2) . ?
C12 C13 1.38(2) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 O4 1.25(2) . ?
C14 O5 1.27(2) . ?
C14 K2 3.44(2) 12_666 ?
Dy1 O5 2.314(11) 11_566 ?
Dy1 O5 2.314(11) 14_566 ?
Dy1 O4 2.324(12) 9_576 ?
Dy1 O4 2.324(12) 15_666 ?
Dy1 O1 2.412(13) . ?
Dy1 O1 2.412(13) 7_466 ?
Dy1 O2 2.414(13) . ?
Dy1 O2 2.414(13) 7_466 ?
Dy1 C1 2.779(18) 7_466 ?
Dy1 K2 4.130(13) 4_465 ?
K1 O5 2.763(12) 10_666 ?
K1 O5 2.763(12) 11_566 ?
K1 O5 2.763(12) 12_676 ?
K1 O5 2.763(12) 16_576 ?
K1 O5 2.763(12) 13_676 ?
K1 O5 2.763(12) 14_566 ?
K1 O5 2.763(12) 9_576 ?
K1 O5 2.763(12) 15_666 ?
K1 Dy1 3.7956(13) 3_665 ?
K1 Dy1 3.7956(13) 4_465 ?
K1 Dy1 3.7957(13) 2_575 ?
K2 O1 2.555(16) 5_556 ?
K2 O1W 2.74(4) 2_565 ?
K2 O4 2.920(19) 15_666 ?
K2 O4 2.920(19) 11_566 ?
K2 C14 3.44(2) 11_566 ?
K2 C14 3.44(2) 15_666 ?
K2 K2 3.68(4) 2_565 ?
K2 Dy1 4.130(13) 3_665 ?
O4 Dy1 2.324(12) 9_576 ?
O4 K2 2.920(19) 12_666 ?
O5 Dy1 2.314(11) 12_666 ?
O5 K1 2.763(12) 9_576 ?
O1W K2 2.74(4) 2_565 ?
O2W H3W 1.056(15) . ?
O2W H4W 1.056(15) . ?

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 C1 O2 119.6(16) . . ?
O1 C1 C2 120.2(18) . . ?
O2 C1 C2 120.1(18) . . ?
C3 C2 C7 118.7(17) . . ?
C3 C2 C1 121.9(19) . . ?
C7 C2 C1 119.3(17) . . ?
C2 C3 C4 121(2) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C5 C4 C3 120(2) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 121.1(18) . . ?
C4 C5 O3 123(2) . . ?
C6 C5 O3 116(2) . . ?
C5 C6 C7 118(2) . . ?
C5 C6 H6 120.9 . . ?
C7 C6 H6 120.9 . . ?
C2 C7 C6 121(2) . . ?
C2 C7 H7 119.4 . . ?
C6 C7 H7 119.4 . . ?
C9 C8 C13 121.5(16) . . ?
C9 C8 O3 123.2(16) . . ?
C13 C8 O3 115.2(17) . . ?
C8 C9 C10 119.1(16) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 H9 120.5 . . ?
C11 C10 C9 120.5(17) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C12 C11 C10 119.1(15) . . ?
C12 C11 C14 120.4(15) . . ?
C10 C11 C14 120.6(16) . . ?
C11 C12 C13 121.7(16) . . ?
C11 C12 H12 119.1 . . ?
C13 C12 H12 119.1 . . ?
C12 C13 C8 118.1(18) . . ?
C12 C13 H13 121.0 . . ?
C8 C13 H13 121.0 . . ?
O4 C14 O5 124.2(16) . . ?
O4 C14 C11 117.7(15) . . ?
O5 C14 C11 118.1(16) . . ?
O4 C14 K2 55.5(9) . 12_666 ?
O5 C14 K2 105.1(10) . 12_666 ?
C11 C14 K2 109.9(11) . 12_666 ?
O5 Dy1 O5 92.7(6) 11_566 14_566 ?
O5 Dy1 O4 75.4(4) 11_566 9_576 ?
O5 Dy1 O4 81.5(4) 14_566 9_576 ?
O5 Dy1 O4 81.5(4) 11_566 15_666 ?
O5 Dy1 O4 75.4(4) 14_566 15_666 ?
O4 Dy1 O4 146.2(6) 9_576 15_666 ?
O5 Dy1 O1 76.9(5) 11_566 . ?
O5 Dy1 O1 152.1(5) 14_566 . ?
O4 Dy1 O1 119.5(4) 9_576 . ?
O4 Dy1 O1 77.5(4) 15_666 . ?
O5 Dy1 O1 152.1(5) 11_566 7_466 ?
O5 Dy1 O1 76.9(5) 14_566 7_466 ?
O4 Dy1 O1 77.5(4) 9_576 7_466 ?
O4 Dy1 O1 119.5(4) 15_666 7_466 ?
O1 Dy1 O1 123.2(7) . 7_466 ?
O5 Dy1 O2 94.8(4) 11_566 . ?
O5 Dy1 O2 154.4(5) 14_566 . ?
O4 Dy1 O2 76.8(5) 9_576 . ?
O4 Dy1 O2 130.0(4) 15_666 . ?
O1 Dy1 O2 53.5(5) . . ?
O1 Dy1 O2 85.2(5) 7_466 . ?
O5 Dy1 O2 154.4(5) 11_566 7_466 ?
O5 Dy1 O2 94.8(4) 14_566 7_466 ?
O4 Dy1 O2 130.0(5) 9_576 7_466 ?
O4 Dy1 O2 76.8(5) 15_666 7_466 ?
O1 Dy1 O2 85.2(5) . 7_466 ?
O1 Dy1 O2 53.5(5) 7_466 7_466 ?
O2 Dy1 O2 89.0(7) . 7_466 ?
O5 Dy1 C1 176.0(5) 11_566 7_466 ?
O5 Dy1 C1 83.3(5) 14_566 7_466 ?
O4 Dy1 C1 104.0(5) 9_576 7_466 ?
O4 Dy1 C1 97.4(5) 15_666 7_466 ?
O1 Dy1 C1 106.6(6) . 7_466 ?
O1 Dy1 C1 26.7(5) 7_466 7_466 ?
O2 Dy1 C1 88.9(5) . 7_466 ?
O2 Dy1 C1 27.0(5) 7_466 7_466 ?
O5 Dy1 K2 117.2(3) 11_566 4_465 ?
O5 Dy1 K2 69.5(3) 14_566 4_465 ?
O4 Dy1 K2 43.5(3) 9_576 4_465 ?
O4 Dy1 K2 140.4(3) 15_666 4_465 ?
O1 Dy1 K2 138.3(4) . 4_465 ?
O1 Dy1 K2 34.9(3) 7_466 4_465 ?
O2 Dy1 K2 85.3(3) . 4_465 ?
O2 Dy1 K2 88.4(3) 7_466 4_465 ?
C1 Dy1 K2 61.5(5) 7_466 4_465 ?
O5 K1 O5 75.4(2) 10_666 11_566 ?
O5 K1 O5 75.4(2) 10_666 12_676 ?
O5 K1 O5 119.7(4) 11_566 12_676 ?
O5 K1 O5 140.4(5) 10_666 16_576 ?
O5 K1 O5 142.3(5) 11_566 16_576 ?
O5 K1 O5 73.3(5) 12_676 16_576 ?
O5 K1 O5 73.3(5) 10_666 13_676 ?
O5 K1 O5 140.4(5) 11_566 13_676 ?
O5 K1 O5 74.6(4) 12_676 13_676 ?
O5 K1 O5 75.4(2) 16_576 13_676 ?
O5 K1 O5 142.3(5) 10_666 14_566 ?
O5 K1 O5 74.6(4) 11_566 14_566 ?
O5 K1 O5 140.4(5) 12_676 14_566 ?
O5 K1 O5 75.4(2) 16_576 14_566 ?
O5 K1 O5 119.7(4) 13_676 14_566 ?
O5 K1 O5 119.7(4) 10_666 9_576 ?
O5 K1 O5 75.4(2) 11_566 9_576 ?
O5 K1 O5 75.4(2) 12_676 9_576 ?
O5 K1 O5 74.6(4) 16_576 9_576 ?
O5 K1 O5 142.3(5) 13_676 9_576 ?
O5 K1 O5 73.3(5) 14_566 9_576 ?
O5 K1 O5 74.6(4) 10_666 15_666 ?
O5 K1 O5 73.3(5) 11_566 15_666 ?
O5 K1 O5 142.3(5) 12_676 15_666 ?
O5 K1 O5 119.7(4) 16_576 15_666 ?
O5 K1 O5 75.4(2) 13_676 15_666 ?
O5 K1 O5 75.4(2) 14_566 15_666 ?
O5 K1 O5 140.4(5) 9_576 15_666 ?
O5 K1 Dy1 37.3(2) 10_666 3_665 ?
O5 K1 Dy1 70.2(3) 11_566 3_665 ?
O5 K1 Dy1 109.8(3) 12_676 3_665 ?
O5 K1 Dy1 142.7(2) 16_576 3_665 ?
O5 K1 Dy1 70.2(3) 13_676 3_665 ?
O5 K1 Dy1 109.8(3) 14_566 3_665 ?
O5 K1 Dy1 142.7(2) 9_576 3_665 ?
O5 K1 Dy1 37.3(2) 15_666 3_665 ?
O5 K1 Dy1 142.7(2) 10_666 4_465 ?
O5 K1 Dy1 109.8(3) 11_566 4_465 ?
O5 K1 Dy1 70.2(3) 12_676 4_465 ?
O5 K1 Dy1 37.3(2) 16_576 4_465 ?
O5 K1 Dy1 109.8(3) 13_676 4_465 ?
O5 K1 Dy1 70.2(3) 14_566 4_465 ?
O5 K1 Dy1 37.3(2) 9_576 4_465 ?
O5 K1 Dy1 142.7(2) 15_666 4_465 ?
Dy1 K1 Dy1 180.0 3_665 4_465 ?
O5 K1 Dy1 70.2(3) 10_666 2_575 ?
O5 K1 Dy1 142.7(2) 11_566 2_575 ?
O5 K1 Dy1 37.3(2) 12_676 2_575 ?
O5 K1 Dy1 70.2(3) 16_576 2_575 ?
O5 K1 Dy1 37.3(2) 13_676 2_575 ?
O5 K1 Dy1 142.7(2) 14_566 2_575 ?
O5 K1 Dy1 109.8(3) 9_576 2_575 ?
O5 K1 Dy1 109.8(3) 15_666 2_575 ?
Dy1 K1 Dy1 90.0 3_665 2_575 ?
Dy1 K1 Dy1 89.999(1) 4_465 2_575 ?
O1 K2 O1W 68.5(7) 5_556 2_565 ?
O1 K2 O4 77.9(6) 5_556 15_666 ?
O1W K2 O4 142.6(5) 2_565 15_666 ?
O1 K2 O4 65.2(5) 5_556 11_566 ?
O1W K2 O4 107.5(7) 2_565 11_566 ?
O4 K2 O4 70.6(6) 15_666 11_566 ?
O1 K2 C14 84.5(6) 5_556 11_566 ?
O1W K2 C14 124.4(6) 2_565 11_566 ?
O4 K2 C14 65.8(5) 15_666 11_566 ?
O4 K2 C14 20.7(4) 11_566 11_566 ?
O1 K2 C14 57.2(5) 5_556 15_666 ?
O1W K2 C14 122.9(6) 2_565 15_666 ?
O4 K2 C14 20.7(4) 15_666 15_666 ?
O4 K2 C14 65.8(5) 11_566 15_666 ?
C14 K2 C14 68.9(7) 11_566 15_666 ?
O1 K2 K2 112.7(5) 5_556 2_565 ?
O1W K2 K2 47.8(8) 2_565 2_565 ?
O4 K2 K2 144.7(3) 15_666 2_565 ?
O4 K2 K2 144.7(3) 11_566 2_565 ?
C14 K2 K2 145.6(3) 11_566 2_565 ?
C14 K2 K2 145.6(3) 15_666 2_565 ?
O1 K2 Dy1 32.7(3) 5_556 3_665 ?
O1W K2 Dy1 91.6(7) 2_565 3_665 ?
O4 K2 Dy1 66.2(4) 15_666 3_665 ?
O4 K2 Dy1 33.2(3) 11_566 3_665 ?
C14 K2 Dy1 51.9(4) 11_566 3_665 ?
C14 K2 Dy1 50.5(3) 15_666 3_665 ?
K2 K2 Dy1 139.46(16) 2_565 3_665 ?
C1 O1 Dy1 93.3(12) . . ?
C1 O2 Dy1 92.9(11) . . ?
C5 O3 C8 117.6(14) . . ?
C14 O4 Dy1 138.6(12) . 9_576 ?
C14 O4 K2 103.7(10) . 12_666 ?
Dy1 O4 K2 103.3(4) 9_576 12_666 ?
C14 O5 Dy1 130.9(11) . 12_666 ?
C14 O5 K1 119.5(11) . 9_576 ?
Dy1 O5 K1 96.4(3) 12_666 9_576 ?
H3W O2W H4W 64(14) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.758
_refine_diff_density_min         -8.555
_refine_diff_density_rms         0.241
####################################################################### 
# 
# 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
_audit_block_doi                 10.5517/cc1jqk93
_database_code_depnum_ccdc_archive 'CCDC 1421855'
_audit_update_record             
;
2016-01-23 deposited with the CCDC.
2016-01-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C59 H35 K O26 Tb3, 2H2O'
_chemical_formula_sum            'C59 H39 K O28 Tb3'
_chemical_formula_weight         1712.91

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'

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

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

_cell_length_a                   20.15(5)
_cell_length_b                   30.14(7)
_cell_length_c                   11.69(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7100(30)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1365
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      17.13

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3336
_exptl_absorpt_coefficient_mu    3.091
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.411
_exptl_absorpt_correction_T_max  0.462
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            33152
_diffrn_reflns_av_R_equivalents  0.1180
_diffrn_reflns_av_sigmaI/netI    0.0944
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.87
_diffrn_reflns_theta_max         25.25
_reflns_number_total             6541
_reflns_number_gt                3822
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0794P)²+0.4620P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6541
_refine_ls_number_parameters     426
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1133
_refine_ls_R_factor_gt           0.0609
_refine_ls_wR_factor_ref         0.1690
_refine_ls_wR_factor_gt          0.1437
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.004
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4501(9) 0.2500 1.5222(16) 0.125(11) Uani 1 2 d S . .
H1 H 0.4152 0.2500 1.5742 0.149 Uiso 1 2 calc SR . .
C2 C 0.2729(7) 0.2500 1.0241(12) 0.052(4) Uani 1 2 d S . .
H2 H 0.2311 0.2500 0.9904 0.063 Uiso 1 2 calc SR . .
C3 C 0.6174(9) 0.2500 1.0051(15) 0.082(6) Uani 1 2 d S . .
H3 H 0.6485 0.2500 1.0639 0.098 Uiso 1 2 calc SR . .
C4 C 0.4620(6) 0.3231(4) 0.7754(9) 0.055(3) Uani 1 1 d . . .
C5 C 0.4619(5) 0.3717(3) 0.7332(9) 0.048(3) Uani 1 1 d . . .
C6 C 0.4032(6) 0.3901(4) 0.6756(10) 0.067(3) Uani 1 1 d . . .
H6 H 0.3682 0.3715 0.6565 0.080 Uiso 1 1 calc R . .
C7 C 0.3992(7) 0.4372(4) 0.6479(12) 0.090(5) Uani 1 1 d . . .
H7 H 0.3617 0.4484 0.6118 0.108 Uiso 1 1 calc R . .
C8 C 0.4531(9) 0.4664(5) 0.6764(13) 0.105(6) Uani 1 1 d . . .
C9 C 0.5123(8) 0.4491(4) 0.7334(13) 0.101(5) Uani 1 1 d . . .
H9 H 0.5471 0.4679 0.7533 0.122 Uiso 1 1 calc R . .
C10 C 0.5158(7) 0.4021(4) 0.7583(11) 0.074(4) Uani 1 1 d . . .
H10 H 0.5542 0.3909 0.7918 0.089 Uiso 1 1 calc R . .
C11 C 0.4800(10) 0.5487(5) 0.7026(18) 0.113(7) Uani 1 1 d . . .
C12 C 0.4756(11) 0.5559(6) 0.8188(16) 0.155(10) Uani 1 1 d . . .
H12 H 0.4542 0.5351 0.8645 0.186 Uiso 1 1 calc R . .
C13 C 0.5031(8) 0.5947(4) 0.8708(14) 0.099(5) Uani 1 1 d . . .
H13 H 0.4978 0.5991 0.9491 0.119 Uiso 1 1 calc R . .
C14 C 0.5390(6) 0.6272(4) 0.8042(9) 0.056(3) Uani 1 1 d . . .
C15 C 0.5437(7) 0.6181(6) 0.6857(10) 0.104(6) Uani 1 1 d . . .
H15 H 0.5667 0.6381 0.6398 0.124 Uiso 1 1 calc R . .
C16 C 0.5149(8) 0.5797(7) 0.6324(15) 0.116(6) Uani 1 1 d . . .
H16 H 0.5189 0.5751 0.5540 0.140 Uiso 1 1 calc R . .
C17 C 0.5665(6) 0.6713(4) 0.8553(14) 0.069(4) Uani 1 1 d . . .
C18 C 0.1702(5) 0.3282(4) 0.8768(9) 0.054(3) Uani 1 1 d . . .
C19 C 0.2060(6) 0.3694(3) 0.9246(9) 0.053(3) Uani 1 1 d . . .
C20 C 0.1710(7) 0.4042(5) 0.9821(14) 0.101(5) Uani 1 1 d . . .
H20 H 0.1256 0.4016 0.9947 0.121 Uiso 1 1 calc R . .
C21 C 0.2066(7) 0.4439(4) 1.0213(14) 0.109(6) Uani 1 1 d . . .
H21 H 0.1830 0.4668 1.0557 0.131 Uiso 1 1 calc R . .
C22 C 0.2754(7) 0.4479(4) 1.0080(12) 0.076(4) Uani 1 1 d . . .
C23 C 0.3128(7) 0.4135(4) 0.9547(11) 0.072(4) Uani 1 1 d . . .
H23 H 0.3586 0.4160 0.9472 0.087 Uiso 1 1 calc R . .
C24 C 0.2783(6) 0.3742(4) 0.9119(10) 0.066(3) Uani 1 1 d . . .
H24 H 0.3024 0.3518 0.8761 0.079 Uiso 1 1 calc R . .
C25 C 0.2898(7) 0.5317(4) 1.0153(12) 0.075(4) Uani 1 1 d . . .
C26 C 0.2659(8) 0.5400(5) 0.9007(13) 0.099(5) Uani 1 1 d . . .
H26 H 0.2622 0.5167 0.8491 0.119 Uiso 1 1 calc R . .
C27 C 0.2480(8) 0.5835(5) 0.8663(12) 0.105(6) Uani 1 1 d . . .
H27 H 0.2333 0.5883 0.7919 0.127 Uiso 1 1 calc R . .
C28 C 0.2522(6) 0.6211(4) 0.9459(10) 0.065(3) Uani 1 1 d . . .
C29 C 0.2755(6) 0.6129(4) 1.0579(10) 0.075(4) Uani 1 1 d . . .
H29 H 0.2780 0.6363 1.1097 0.090 Uiso 1 1 calc R . .
C30 C 0.2961(6) 0.5677(4) 1.0951(11) 0.067(3) Uani 1 1 d . . .
H30 H 0.3126 0.5629 1.1683 0.081 Uiso 1 1 calc R . .
C31 C 0.2298(6) 0.6688(5) 0.9053(12) 0.075(4) Uani 1 1 d . . .
K1 K 0.29117(16) 0.2500 0.6827(3) 0.0505(8) Uani 1 2 d S . .
O1 O 0.5036(6) 0.2500 1.5764(10) 0.073(3) Uani 1 2 d S . .
O2 O 0.4292(7) 0.2500 1.4327(11) 0.108(5) Uani 1 2 d S . .
O3 O 0.2738(5) 0.2500 1.1321(10) 0.083(4) Uani 1 2 d S . .
O4 O 0.3230(5) 0.2500 0.9541(9) 0.070(3) Uani 1 2 d S . .
O5 O 0.5537(5) 0.2500 1.0341(8) 0.065(3) Uani 1 2 d S . .
O6 O 0.6394(6) 0.2500 0.9014(9) 0.085(4) Uani 1 2 d S . .
O7 O 0.4046(4) 0.3005(3) 0.7830(6) 0.061(2) Uani 1 1 d . . .
O8 O 0.5182(3) 0.3024(2) 0.8093(5) 0.0501(18) Uani 1 1 d . . .
O9 O 0.4458(8) 0.5127(3) 0.6418(13) 0.193(8) Uani 1 1 d . . .
O10 O 0.5612(5) 0.6769(3) 0.9667(10) 0.103(3) Uani 1 1 d . . .
O11 O 0.5910(7) 0.6998(4) 0.7897(12) 0.191(8) Uani 1 1 d . . .
O12 O 0.1121(7) 0.3149(4) 0.9222(10) 0.138(3) Uani 1 1 d . . .
O13 O 0.1953(4) 0.3034(3) 0.7920(7) 0.071(2) Uani 1 1 d . . .
O14 O 0.3113(5) 0.4874(3) 1.0540(9) 0.097(3) Uani 1 1 d . . .
O15 O 0.2072(7) 0.6987(3) 0.9736(8) 0.120(4) Uani 1 1 d . . .
O16 O 0.2271(11) 0.6793(5) 0.8029(10) 0.272(13) Uani 1 1 d . . .
O1W O 0.0768(6) 0.2785(3) 0.1800(9) 0.138(3) Uani 1 1 d D . .
Tb1 Tb 0.33360(3) 0.2500 1.30708(6) 0.0454(2) Uani 1 2 d S . .
Tb2 Tb 0.44326(3) 0.2500 0.94581(6) 0.0431(2) Uani 1 2 d S . .
Tb3 Tb 0.09447(3) 0.2500 0.78886(6) 0.0454(2) Uani 1 2 d S . .
H1W H 0.1120 0.2953 0.2021 0.06(3) Uiso 1 1 d RD . .
H2W H 0.0966 0.2500 0.1683 0.00(2) Uiso 1 2 d SRD . .


_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
C1 O2 1.128(19) . ?
C1 O1 1.25(2) . ?
C1 H1 0.9300 . ?
C2 O3 1.262(16) . ?
C2 O4 1.299(16) . ?
C2 H2 0.9300 . ?
C3 O6 1.290(19) . ?
C3 O5 1.327(19) . ?
C3 H3 0.9300 . ?
C4 O7 1.346(13) . ?
C4 O8 1.353(13) . ?
C4 C5 1.547(14) . ?
C5 C10 1.450(16) . ?
C5 C6 1.469(15) . ?
C6 C7 1.459(16) . ?
C6 H6 0.9300 . ?
C7 C8 1.436(19) . ?
C7 H7 0.9300 . ?
C8 C9 1.461(18) . ?
C8 O9 1.463(16) . ?
C9 C10 1.448(16) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.38(2) . ?
C11 C16 1.43(2) . ?
C11 O9 1.468(17) . ?
C12 C13 1.43(2) . ?
C12 H12 0.9300 . ?
C13 C14 1.446(16) . ?
C13 H13 0.9300 . ?
C14 C15 1.415(15) . ?
C14 C17 1.561(17) . ?
C15 C16 1.44(2) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 O11 1.254(15) . ?
C17 O10 1.317(16) . ?
C18 O13 1.342(12) . ?
C18 O12 1.347(15) . ?
C18 C19 1.539(15) . ?
C19 C20 1.431(16) . ?
C19 C24 1.471(15) . ?
C20 C21 1.468(18) . ?
C20 H20 0.9300 . ?
C21 C22 1.400(18) . ?
C21 H21 0.9300 . ?
C22 C23 1.426(16) . ?
C22 O14 1.494(14) . ?
C23 C24 1.461(15) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C30 1.436(15) . ?
C25 C26 1.446(18) . ?
C25 O14 1.474(14) . ?
C26 C27 1.418(18) . ?
C26 H26 0.9300 . ?
C27 C28 1.469(17) . ?
C27 H27 0.9300 . ?
C28 C29 1.412(15) . ?
C28 C31 1.580(17) . ?
C29 C30 1.491(15) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C31 O16 1.239(15) . ?
C31 O15 1.287(14) . ?
C31 Tb1 2.990(14) 2_564 ?
K1 O13 2.819(9) . ?
K1 O13 2.819(9) 7_565 ?
K1 O15 2.891(11) 8_655 ?
K1 O15 2.891(11) 2_564 ?
K1 O7 2.985(9) . ?
K1 O7 2.985(9) 7_565 ?
K1 O6 3.212(15) 6_557 ?
K1 O4 3.236(14) . ?
K1 Tb1 4.472(11) 1_554 ?
O1 Tb3 2.415(13) 6_658 ?
O2 Tb1 2.421(13) . ?
O3 Tb1 2.373(12) . ?
O4 Tb2 2.425(13) . ?
O5 Tb2 2.453(11) . ?
O6 Tb3 2.400(12) 6_657 ?
O6 K1 3.212(15) 6_657 ?
O7 Tb2 2.558(8) . ?
O8 Tb3 2.484(8) 6_657 ?
O8 Tb2 2.705(8) . ?
O10 Tb2 2.431(10) 5_667 ?
O11 Tb1 2.423(11) 5_667 ?
O12 Tb3 2.527(12) . ?
O13 Tb3 2.592(9) . ?
O15 Tb1 2.617(10) 2_564 ?
O15 K1 2.891(11) 2_565 ?
O16 Tb1 2.458(12) 2_564 ?
O1W O1W 1.72(2) 7_565 ?
O1W H1W 0.9091 . ?
O1W H2W 0.9571 . ?
Tb1 O11 2.423(11) 5_667 ?
Tb1 O11 2.423(11) 3_647 ?
Tb1 O16 2.458(12) 8_656 ?
Tb1 O16 2.458(12) 2_565 ?
Tb1 O15 2.617(10) 2_565 ?
Tb1 O15 2.617(10) 8_656 ?
Tb1 C31 2.990(14) 8_656 ?
Tb1 C31 2.990(14) 2_565 ?
Tb1 K1 4.472(11) 1_556 ?
Tb2 O10 2.431(10) 5_667 ?
Tb2 O10 2.431(10) 3_647 ?
Tb2 O7 2.558(8) 7_565 ?
Tb2 O8 2.705(8) 7_565 ?
Tb2 C4 2.993(12) 7_565 ?
Tb3 O6 2.400(12) 6_557 ?
Tb3 O1 2.415(13) 6_558 ?
Tb3 O8 2.484(8) 4_456 ?
Tb3 O8 2.484(8) 6_557 ?
Tb3 O12 2.527(12) 7_565 ?
Tb3 O13 2.592(9) 7_565 ?
Tb3 C18 2.992(13) 7_565 ?

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 C1 O1 142.4(19) . . ?
O2 C1 H1 108.8 . . ?
O1 C1 H1 108.8 . . ?
O3 C2 O4 128.2(14) . . ?
O3 C2 H2 115.9 . . ?
O4 C2 H2 115.9 . . ?
O6 C3 O5 124.8(16) . . ?
O6 C3 H3 117.6 . . ?
O5 C3 H3 117.6 . . ?
O7 C4 O8 117.8(9) . . ?
O7 C4 C5 120.0(10) . . ?
O8 C4 C5 122.1(10) . . ?
C10 C5 C6 117.2(10) . . ?
C10 C5 C4 122.2(10) . . ?
C6 C5 C4 120.3(10) . . ?
C7 C6 C5 120.9(11) . . ?
C7 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
C8 C7 C6 120.1(12) . . ?
C8 C7 H7 119.9 . . ?
C6 C7 H7 119.9 . . ?
C7 C8 C9 120.4(12) . . ?
C7 C8 O9 116.3(12) . . ?
C9 C8 O9 123.3(13) . . ?
C10 C9 C8 118.6(12) . . ?
C10 C9 H9 120.7 . . ?
C8 C9 H9 120.7 . . ?
C9 C10 C5 122.8(12) . . ?
C9 C10 H10 118.6 . . ?
C5 C10 H10 118.6 . . ?
C12 C11 C16 119.6(15) . . ?
C12 C11 O9 124(2) . . ?
C16 C11 O9 115.8(18) . . ?
C11 C12 C13 121.6(15) . . ?
C11 C12 H12 119.2 . . ?
C13 C12 H12 119.2 . . ?
C12 C13 C14 121.3(14) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 H13 119.4 . . ?
C15 C14 C13 115.5(12) . . ?
C15 C14 C17 121.1(12) . . ?
C13 C14 C17 123.3(11) . . ?
C14 C15 C16 123.6(14) . . ?
C14 C15 H15 118.2 . . ?
C16 C15 H15 118.2 . . ?
C11 C16 C15 118.4(15) . . ?
C11 C16 H16 120.8 . . ?
C15 C16 H16 120.8 . . ?
O11 C17 O10 123.4(14) . . ?
O11 C17 C14 119.3(14) . . ?
O10 C17 C14 117.3(11) . . ?
O13 C18 O12 116.8(11) . . ?
O13 C18 C19 122.8(9) . . ?
O12 C18 C19 120.3(10) . . ?
C20 C19 C24 117.5(11) . . ?
C20 C19 C18 122.1(11) . . ?
C24 C19 C18 120.4(9) . . ?
C19 C20 C21 120.3(13) . . ?
C19 C20 H20 119.9 . . ?
C21 C20 H20 119.9 . . ?
C22 C21 C20 121.2(12) . . ?
C22 C21 H21 119.4 . . ?
C20 C21 H21 119.4 . . ?
C21 C22 C23 120.6(12) . . ?
C21 C22 O14 120.5(11) . . ?
C23 C22 O14 118.8(12) . . ?
C22 C23 C24 119.2(12) . . ?
C22 C23 H23 120.4 . . ?
C24 C23 H23 120.4 . . ?
C23 C24 C19 121.1(10) . . ?
C23 C24 H24 119.5 . . ?
C19 C24 H24 119.5 . . ?
C30 C25 C26 119.9(11) . . ?
C30 C25 O14 117.4(11) . . ?
C26 C25 O14 122.7(11) . . ?
C27 C26 C25 120.6(13) . . ?
C27 C26 H26 119.7 . . ?
C25 C26 H26 119.7 . . ?
C26 C27 C28 121.3(13) . . ?
C26 C27 H27 119.4 . . ?
C28 C27 H27 119.4 . . ?
C29 C28 C27 118.1(12) . . ?
C29 C28 C31 122.2(11) . . ?
C27 C28 C31 119.7(11) . . ?
C28 C29 C30 121.5(11) . . ?
C28 C29 H29 119.3 . . ?
C30 C29 H29 119.3 . . ?
C25 C30 C29 118.6(11) . . ?
C25 C30 H30 120.7 . . ?
C29 C30 H30 120.7 . . ?
O16 C31 O15 113.9(13) . . ?
O16 C31 C28 122.3(13) . . ?
O15 C31 C28 123.6(11) . . ?
O16 C31 Tb1 53.3(7) . 2_564 ?
O15 C31 Tb1 60.9(7) . 2_564 ?
C28 C31 Tb1 169.2(9) . 2_564 ?
O13 K1 O13 69.6(4) . 7_565 ?
O13 K1 O15 134.1(3) . 8_655 ?
O13 K1 O15 94.9(3) 7_565 8_655 ?
O13 K1 O15 94.9(3) . 2_564 ?
O13 K1 O15 134.1(3) 7_565 2_564 ?
O15 K1 O15 64.6(4) 8_655 2_564 ?
O13 K1 O7 93.2(3) . . ?
O13 K1 O7 129.6(3) 7_565 . ?
O15 K1 O7 126.5(3) 8_655 . ?
O15 K1 O7 92.9(3) 2_564 . ?
O13 K1 O7 129.6(3) . 7_565 ?
O13 K1 O7 93.2(3) 7_565 7_565 ?
O15 K1 O7 92.9(3) 8_655 7_565 ?
O15 K1 O7 126.5(3) 2_564 7_565 ?
O7 K1 O7 61.3(3) . 7_565 ?
O13 K1 O6 59.1(2) . 6_557 ?
O13 K1 O6 59.1(2) 7_565 6_557 ?
O15 K1 O6 75.7(3) 8_655 6_557 ?
O15 K1 O6 75.7(3) 2_564 6_557 ?
O7 K1 O6 148.11(18) . 6_557 ?
O7 K1 O6 148.11(18) 7_565 6_557 ?
O13 K1 O4 72.0(3) . . ?
O13 K1 O4 72.0(3) 7_565 . ?
O15 K1 O4 145.7(2) 8_655 . ?
O15 K1 O4 145.7(2) 2_564 . ?
O7 K1 O4 57.5(2) . . ?
O7 K1 O4 57.5(2) 7_565 . ?
O6 K1 O4 119.2(3) 6_557 . ?
O13 K1 Tb1 125.1(2) . 1_554 ?
O13 K1 Tb1 125.1(2) 7_565 1_554 ?
O15 K1 Tb1 33.7(2) 8_655 1_554 ?
O15 K1 Tb1 33.7(2) 2_564 1_554 ?
O7 K1 Tb1 103.83(19) . 1_554 ?
O7 K1 Tb1 103.83(19) 7_565 1_554 ?
O6 K1 Tb1 83.2(2) 6_557 1_554 ?
O4 K1 Tb1 157.5(2) . 1_554 ?
C1 O1 Tb3 169.8(11) . 6_658 ?
C1 O2 Tb1 149.3(14) . . ?
C2 O3 Tb1 150.4(10) . . ?
C2 O4 Tb2 143.3(10) . . ?
C2 O4 K1 117.6(9) . . ?
Tb2 O4 K1 99.1(4) . . ?
C3 O5 Tb2 140.4(10) . . ?
C3 O6 Tb3 137.8(12) . 6_657 ?
C3 O6 K1 127.8(11) . 6_657 ?
Tb3 O6 K1 94.3(4) 6_657 6_657 ?
C4 O7 Tb2 95.1(6) . . ?
C4 O7 K1 153.0(7) . . ?
Tb2 O7 K1 102.9(3) . . ?
C4 O8 Tb3 132.5(6) . 6_657 ?
C4 O8 Tb2 88.5(6) . . ?
Tb3 O8 Tb2 104.3(3) 6_657 . ?
C8 O9 C11 121.6(10) . . ?
C17 O10 Tb2 122.3(9) . 5_667 ?
C17 O11 Tb1 163.9(10) . 5_667 ?
C18 O12 Tb3 96.4(8) . . ?
C18 O13 Tb3 93.6(6) . . ?
C18 O13 K1 155.7(7) . . ?
Tb3 O13 K1 100.2(3) . . ?
C25 O14 C22 118.0(9) . . ?
C31 O15 Tb1 93.7(7) . 2_564 ?
C31 O15 K1 153.4(9) . 2_565 ?
Tb1 O15 K1 108.5(4) 2_564 2_565 ?
C31 O16 Tb1 102.9(9) . 2_564 ?
O1W O1W H1W 123.8 7_565 . ?
O1W O1W H2W 26.2 7_565 . ?
H1W O1W H2W 102.4 . . ?
O3 Tb1 O2 157.8(4) . . ?
O3 Tb1 O11 85.2(4) . 5_667 ?
O2 Tb1 O11 77.6(4) . 5_667 ?
O3 Tb1 O11 85.2(4) . 3_647 ?
O2 Tb1 O11 77.6(4) . 3_647 ?
O11 Tb1 O11 77.2(9) 5_667 3_647 ?
O3 Tb1 O16 74.4(3) . 8_656 ?
O2 Tb1 O16 114.1(4) . 8_656 ?
O11 Tb1 O16 147.5(6) 5_667 8_656 ?
O11 Tb1 O16 76.2(7) 3_647 8_656 ?
O3 Tb1 O16 74.4(3) . 2_565 ?
O2 Tb1 O16 114.1(4) . 2_565 ?
O11 Tb1 O16 76.2(7) 5_667 2_565 ?
O11 Tb1 O16 147.5(6) 3_647 2_565 ?
O16 Tb1 O16 120.3(12) 8_656 2_565 ?
O3 Tb1 O15 118.8(4) . 2_565 ?
O2 Tb1 O15 78.4(4) . 2_565 ?
O11 Tb1 O15 100.1(5) 5_667 2_565 ?
O11 Tb1 O15 155.8(4) 3_647 2_565 ?
O16 Tb1 O15 111.8(5) 8_656 2_565 ?
O16 Tb1 O15 49.2(3) 2_565 2_565 ?
O3 Tb1 O15 118.8(4) . 8_656 ?
O2 Tb1 O15 78.4(4) . 8_656 ?
O11 Tb1 O15 155.8(4) 5_667 8_656 ?
O11 Tb1 O15 100.1(5) 3_647 8_656 ?
O16 Tb1 O15 49.2(3) 8_656 8_656 ?
O16 Tb1 O15 111.8(5) 2_565 8_656 ?
O15 Tb1 O15 72.4(4) 2_565 8_656 ?
O3 Tb1 C31 96.6(3) . 8_656 ?
O2 Tb1 C31 96.1(3) . 8_656 ?
O11 Tb1 C31 163.3(5) 5_667 8_656 ?
O11 Tb1 C31 86.3(5) 3_647 8_656 ?
O16 Tb1 C31 23.8(3) 8_656 8_656 ?
O16 Tb1 C31 120.3(6) 2_565 8_656 ?
O15 Tb1 C31 93.6(4) 2_565 8_656 ?
O15 Tb1 C31 25.5(3) 8_656 8_656 ?
O3 Tb1 C31 96.6(3) . 2_565 ?
O2 Tb1 C31 96.1(3) . 2_565 ?
O11 Tb1 C31 86.3(5) 5_667 2_565 ?
O11 Tb1 C31 163.3(5) 3_647 2_565 ?
O16 Tb1 C31 120.3(6) 8_656 2_565 ?
O16 Tb1 C31 23.8(3) 2_565 2_565 ?
O15 Tb1 C31 25.5(3) 2_565 2_565 ?
O15 Tb1 C31 93.6(4) 8_656 2_565 ?
C31 Tb1 C31 109.9(6) 8_656 2_565 ?
O3 Tb1 K1 138.5(3) . 1_556 ?
O2 Tb1 K1 63.7(4) . 1_556 ?
O11 Tb1 K1 125.3(3) 5_667 1_556 ?
O11 Tb1 K1 125.3(3) 3_647 1_556 ?
O16 Tb1 K1 85.7(3) 8_656 1_556 ?
O16 Tb1 K1 85.7(3) 2_565 1_556 ?
O15 Tb1 K1 37.8(2) 2_565 1_556 ?
O15 Tb1 K1 37.8(2) 8_656 1_556 ?
C31 Tb1 K1 62.7(3) 8_656 1_556 ?
C31 Tb1 K1 62.7(3) 2_565 1_556 ?
O4 Tb2 O10 86.9(2) . 5_667 ?
O4 Tb2 O10 86.9(2) . 3_647 ?
O10 Tb2 O10 130.1(6) 5_667 3_647 ?
O4 Tb2 O5 152.8(4) . . ?
O10 Tb2 O5 81.8(2) 5_667 . ?
O10 Tb2 O5 81.8(2) 3_647 . ?
O4 Tb2 O7 74.1(3) . 7_565 ?
O10 Tb2 O7 147.2(3) 5_667 7_565 ?
O10 Tb2 O7 76.3(4) 3_647 7_565 ?
O5 Tb2 O7 126.1(2) . 7_565 ?
O4 Tb2 O7 74.1(3) . . ?
O10 Tb2 O7 76.3(4) 5_667 . ?
O10 Tb2 O7 147.2(3) 3_647 . ?
O5 Tb2 O7 126.1(2) . . ?
O7 Tb2 O7 73.0(4) 7_565 . ?
O4 Tb2 O8 125.6(2) . 7_565 ?
O10 Tb2 O8 142.9(3) 5_667 7_565 ?
O10 Tb2 O8 74.9(3) 3_647 7_565 ?
O5 Tb2 O8 75.0(3) . 7_565 ?
O7 Tb2 O8 52.0(3) 7_565 7_565 ?
O7 Tb2 O8 94.5(3) . 7_565 ?
O4 Tb2 O8 125.6(2) . . ?
O10 Tb2 O8 74.9(3) 5_667 . ?
O10 Tb2 O8 142.9(3) 3_647 . ?
O5 Tb2 O8 75.0(3) . . ?
O7 Tb2 O8 94.5(3) 7_565 . ?
O7 Tb2 O8 52.0(3) . . ?
O8 Tb2 O8 71.4(3) 7_565 . ?
O4 Tb2 C4 98.8(3) . 7_565 ?
O10 Tb2 C4 162.1(4) 5_667 7_565 ?
O10 Tb2 C4 67.5(4) 3_647 7_565 ?
O5 Tb2 C4 99.5(3) . 7_565 ?
O7 Tb2 C4 26.6(3) 7_565 7_565 ?
O7 Tb2 C4 88.9(3) . 7_565 ?
O8 Tb2 C4 26.9(3) 7_565 7_565 ?
O8 Tb2 C4 88.1(3) . 7_565 ?
O6 Tb3 O1 152.8(4) 6_557 6_558 ?
O6 Tb3 O8 78.8(3) 6_557 4_456 ?
O1 Tb3 O8 80.3(3) 6_558 4_456 ?
O6 Tb3 O8 78.8(3) 6_557 6_557 ?
O1 Tb3 O8 80.3(3) 6_558 6_557 ?
O8 Tb3 O8 78.9(4) 4_456 6_557 ?
O6 Tb3 O12 121.2(3) 6_557 . ?
O1 Tb3 O12 72.8(3) 6_558 . ?
O8 Tb3 O12 149.8(3) 4_456 . ?
O8 Tb3 O12 83.1(4) 6_557 . ?
O6 Tb3 O12 121.2(3) 6_557 7_565 ?
O1 Tb3 O12 72.8(3) 6_558 7_565 ?
O8 Tb3 O12 83.1(4) 4_456 7_565 ?
O8 Tb3 O12 149.8(3) 6_557 7_565 ?
O12 Tb3 O12 101.5(6) . 7_565 ?
O6 Tb3 O13 73.6(3) 6_557 . ?
O1 Tb3 O13 125.8(3) 6_558 . ?
O8 Tb3 O13 152.4(2) 4_456 . ?
O8 Tb3 O13 95.6(3) 6_557 . ?
O12 Tb3 O13 53.2(3) . . ?
O12 Tb3 O13 111.2(4) 7_565 . ?
O6 Tb3 O13 73.6(3) 6_557 7_565 ?
O1 Tb3 O13 125.8(3) 6_558 7_565 ?
O8 Tb3 O13 95.6(3) 4_456 7_565 ?
O8 Tb3 O13 152.4(2) 6_557 7_565 ?
O12 Tb3 O13 111.2(4) . 7_565 ?
O12 Tb3 O13 53.2(3) 7_565 7_565 ?
O13 Tb3 O13 76.7(4) . 7_565 ?
O6 Tb3 C18 97.2(3) 6_557 7_565 ?
O1 Tb3 C18 99.4(3) 6_558 7_565 ?
O8 Tb3 C18 88.5(3) 4_456 7_565 ?
O8 Tb3 C18 167.3(3) 6_557 7_565 ?
O12 Tb3 C18 109.1(4) . 7_565 ?
O12 Tb3 C18 26.6(3) 7_565 7_565 ?
O13 Tb3 C18 94.8(3) . 7_565 ?
O13 Tb3 C18 26.6(2) 7_565 7_565 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.670
_refine_diff_density_min         -1.049
_refine_diff_density_rms         0.165
####################################################################### 
# 
# 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
_audit_block_doi                 10.5517/cc1jqkb4
_database_code_depnum_ccdc_archive 'CCDC 1421856'
_audit_update_record             
;
2016-01-23 deposited with the CCDC.
2016-01-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C59 H35 Dy3 K O26, 2H2O'
_chemical_formula_sum            'C59 H39 Dy3 K O28'
_chemical_formula_weight         1720.91

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

_cell_length_a                   19.100(3)
_cell_length_b                   28.260(4)
_cell_length_c                   11.1446(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6015.5(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2988
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      22.89

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.27
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.901
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3332
_exptl_absorpt_coefficient_mu    3.848
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.316
_exptl_absorpt_correction_T_max  0.354
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            33497
_diffrn_reflns_av_R_equivalents  0.0955
_diffrn_reflns_av_sigmaI/netI    0.0855
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.44
_diffrn_reflns_theta_max         27.53
_reflns_number_total             7072
_reflns_number_gt                4536
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0682P)²+7.6832P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7072
_refine_ls_number_parameters     424
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.1007
_refine_ls_R_factor_gt           0.0587
_refine_ls_wR_factor_ref         0.1544
_refine_ls_wR_factor_gt          0.1349
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.095
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4511(9) 0.2500 1.0227(18) 0.077(5) Uani 1 2 d SU . .
H1 H 0.4143 0.2500 1.0772 0.093 Uiso 1 2 calc SR . .
C2 C 0.2726(7) 0.2500 0.5265(13) 0.042(3) Uani 1 2 d S . .
H2 H 0.2285 0.2500 0.4914 0.050 Uiso 1 2 calc SR . .
C3 C 0.6183(7) 0.2500 0.5032(14) 0.060(4) Uani 1 2 d S . .
H3 H 0.6520 0.2500 0.5636 0.072 Uiso 1 2 calc SR . .
C4 C 0.2694(5) 0.1718(5) 0.9128(11) 0.072(4) Uani 1 1 d . . .
C5 C 0.2472(5) 0.1211(3) 0.9449(10) 0.051(3) Uani 1 1 d . . .
C6 C 0.2522(7) 0.0836(5) 0.8666(12) 0.084(4) Uani 1 1 d . . .
H6 H 0.2689 0.0885 0.7892 0.101 Uiso 1 1 calc R . .
C7 C 0.2328(7) 0.0393(5) 0.9022(13) 0.084(4) Uani 1 1 d . . .
H7 H 0.2356 0.0143 0.8479 0.101 Uiso 1 1 calc R . .
C8 C 0.2096(5) 0.0310(3) 1.0145(11) 0.056(3) Uani 1 1 d . . .
C9 C 0.2042(6) 0.0684(3) 1.0945(11) 0.058(3) Uani 1 1 d . . .
H9 H 0.1877 0.0633 1.1719 0.070 Uiso 1 1 calc R . .
C10 C 0.2237(5) 0.1134(4) 1.0580(11) 0.059(3) Uani 1 1 d . . .
H10 H 0.2207 0.1386 1.1117 0.071 Uiso 1 1 calc R . .
C11 C 0.2250(6) -0.0520(4) 1.0082(11) 0.060(3) Uani 1 1 d . . .
C12 C 0.2951(7) -0.0560(5) 1.0247(15) 0.099(5) Uani 1 1 d . . .
H12 H 0.3201 -0.0321 1.0628 0.119 Uiso 1 1 calc R . .
C13 C 0.3289(6) -0.0962(4) 0.9840(13) 0.076(4) Uani 1 1 d . . .
H13 H 0.3767 -0.0998 0.9967 0.092 Uiso 1 1 calc R . .
C14 C 0.2926(5) -0.1305(3) 0.9254(9) 0.045(2) Uani 1 1 d . . .
C15 C 0.2221(5) -0.1265(3) 0.9121(11) 0.054(3) Uani 1 1 d . . .
H15 H 0.1968 -0.1503 0.8743 0.065 Uiso 1 1 calc R . .
C16 C 0.1884(5) -0.0869(4) 0.9549(11) 0.058(3) Uani 1 1 d . . .
H16 H 0.1401 -0.0842 0.9469 0.069 Uiso 1 1 calc R . .
C17 C 0.3300(4) -0.1724(3) 0.8780(9) 0.039(2) Uani 1 1 d . . .
C18 C 0.4335(5) 0.1710(4) 0.6448(13) 0.057(3) Uani 1 1 d . . .
C19 C 0.4609(5) 0.1269(3) 0.6957(9) 0.043(2) Uani 1 1 d . . .
C20 C 0.4964(7) 0.0958(4) 0.6275(11) 0.078(4) Uani 1 1 d . . .
H20 H 0.5004 0.1007 0.5453 0.094 Uiso 1 1 calc R . .
C21 C 0.5267(9) 0.0564(5) 0.6796(15) 0.113(6) Uani 1 1 d . . .
H21 H 0.5519 0.0351 0.6327 0.136 Uiso 1 1 calc R . .
C22 C 0.5198(9) 0.0490(4) 0.7976(16) 0.092(6) Uani 1 1 d . . .
C23 C 0.4852(8) 0.0794(6) 0.8674(15) 0.099(5) Uani 1 1 d . . .
H23 H 0.4817 0.0746 0.9497 0.119 Uiso 1 1 calc R . .
C24 C 0.4552(6) 0.1178(5) 0.8140(12) 0.084(4) Uani 1 1 d . . .
H24 H 0.4296 0.1386 0.8613 0.101 Uiso 1 1 calc R . .
C25 C 0.5465(9) -0.0330(4) 0.8206(13) 0.094(5) Uani 1 1 d . . .
C26 C 0.6011(6) -0.0637(4) 0.8538(12) 0.073(4) Uani 1 1 d . . .
H26 H 0.6397 -0.0522 0.8954 0.088 Uiso 1 1 calc R . .
C27 C 0.5968(5) -0.1103(4) 0.8246(10) 0.056(3) Uani 1 1 d . . .
H27 H 0.6339 -0.1303 0.8432 0.067 Uiso 1 1 calc R . .
C28 C 0.5374(5) -0.1288(3) 0.7670(9) 0.040(2) Uani 1 1 d . . .
C29 C 0.4839(6) -0.0979(3) 0.7402(10) 0.056(3) Uani 1 1 d . . .
H29 H 0.4439 -0.1098 0.7034 0.068 Uiso 1 1 calc R . .
C30 C 0.4868(8) -0.0510(4) 0.7649(13) 0.088(5) Uani 1 1 d . . .
H30 H 0.4496 -0.0312 0.7452 0.106 Uiso 1 1 calc R . .
C31 C 0.5380(5) -0.1775(3) 0.7254(9) 0.041(2) Uani 1 1 d . . .
Dy1 Dy 0.33362(3) 0.2500 0.80822(6) 0.03569(18) Uani 1 2 d S . .
Dy2 Dy 0.44357(3) 0.2500 0.44511(6) 0.03311(17) Uani 1 2 d S . .
Dy3 Dy 0.40555(3) -0.2500 0.78878(6) 0.03638(18) Uani 1 2 d S . .
K1 K 0.29094(14) 0.2500 1.1831(3) 0.0415(7) Uani 1 2 d S . .
O1 O 0.5031(4) 0.2500 1.0775(9) 0.053(3) Uani 1 2 d S . .
O2 O 0.4287(5) 0.2500 0.9328(11) 0.084(4) Uani 1 2 d S . .
O3 O 0.2744(4) 0.2500 0.6345(9) 0.060(3) Uani 1 2 d S . .
O4 O 0.3252(4) 0.2500 0.4546(9) 0.053(3) Uani 1 2 d S . .
O5 O 0.5537(4) 0.2500 0.5347(9) 0.055(3) Uani 1 2 d S . .
O6 O 0.6387(5) 0.2500 0.3985(9) 0.065(3) Uani 1 2 d S . .
O7 O 0.2951(9) 0.1981(4) 0.9760(10) 0.154(4) Uani 1 1 d . . .
O8 O 0.2693(8) 0.1807(4) 0.8066(9) 0.154(4) Uani 1 1 d . . .
O9 O 0.1898(4) -0.0126(2) 1.0541(8) 0.078(3) Uani 1 1 d . . .
O10 O 0.3051(3) -0.1966(2) 0.7938(7) 0.0541(19) Uani 1 1 d . . .
O11 O 0.3882(4) -0.1855(3) 0.9230(7) 0.068(2) Uani 1 1 d . . .
O12 O 0.4102(7) 0.2008(4) 0.7099(13) 0.180(8) Uani 1 1 d . . .
O13 O 0.4383(4) 0.1782(3) 0.5356(10) 0.079(3) Uani 1 1 d . . .
O14 O 0.5552(7) 0.0125(3) 0.8553(13) 0.170(7) Uani 1 1 d . . .
O15 O 0.4818(3) -0.1973(2) 0.6900(5) 0.0370(14) Uani 1 1 d . . .
O16 O 0.5946(3) -0.1998(2) 0.7163(6) 0.0502(17) Uani 1 1 d . . .
O1W O 0.4132(9) 0.7840(7) 0.1872(13) 0.265(14) Uani 1 1 d D . .
H1W H 0.4073 0.7500 0.1855 0.398 Uiso 1 2 d SRD . .
H2W H 0.3770 0.7979 0.2376 0.398 Uiso 1 1 d RD . .


_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
C1 O2 1.09(2) . ?
C1 O1 1.17(2) . ?
C1 H1 0.9300 . ?
C2 O3 1.204(15) . ?
C2 O4 1.284(14) . ?
C2 H2 0.9300 . ?
C3 O6 1.231(18) . ?
C3 O5 1.283(15) . ?
C3 H3 0.9300 . ?
C4 O7 1.136(15) . ?
C4 O8 1.210(14) . ?
C4 C5 1.535(15) . ?
C5 C10 1.355(14) . ?
C5 C6 1.376(16) . ?
C6 C7 1.366(16) . ?
C6 H6 0.9300 . ?
C7 C8 1.348(17) . ?
C7 H7 0.9300 . ?
C8 O9 1.361(12) . ?
C8 C9 1.386(14) . ?
C9 C10 1.388(13) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C16 1.346(14) . ?
C11 C12 1.356(16) . ?
C11 O9 1.399(12) . ?
C12 C13 1.383(16) . ?
C12 H12 0.9300 . ?
C13 C14 1.359(14) . ?
C13 H13 0.9300 . ?
C14 C15 1.359(13) . ?
C14 C17 1.480(12) . ?
C15 C16 1.376(13) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C17 O10 1.255(11) . ?
C17 O11 1.274(10) . ?
C18 O12 1.196(14) . ?
C18 O13 1.237(15) . ?
C18 C19 1.467(15) . ?
C19 C20 1.345(14) . ?
C19 C24 1.348(15) . ?
C20 C21 1.382(17) . ?
C20 H20 0.9300 . ?
C21 C22 1.34(2) . ?
C21 H21 0.9300 . ?
C22 C23 1.34(2) . ?
C22 O14 1.390(15) . ?
C23 C24 1.363(18) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 O14 1.353(14) . ?
C25 C30 1.396(17) . ?
C25 C26 1.406(17) . ?
C26 C27 1.358(14) . ?
C26 H26 0.9300 . ?
C27 C28 1.406(13) . ?
C27 H27 0.9300 . ?
C28 C29 1.375(13) . ?
C28 C31 1.453(12) . ?
C29 C30 1.355(14) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C31 O16 1.255(10) . ?
C31 O15 1.273(10) . ?
C31 Dy2 2.816(9) 5_656 ?
Dy1 O3 2.242(10) . ?
Dy1 O2 2.285(11) . ?
Dy1 O12 2.297(11) 8_565 ?
Dy1 O12 2.297(11) . ?
Dy1 O8 2.311(9) . ?
Dy1 O8 2.311(9) 8_565 ?
Dy1 O7 2.489(10) 8_565 ?
Dy1 O7 2.489(10) . ?
Dy1 C4 2.784(11) 8_565 ?
Dy2 O4 2.264(8) . ?
Dy2 O13 2.268(7) 8_565 ?
Dy2 O13 2.268(7) . ?
Dy2 O5 2.329(9) . ?
Dy2 O16 2.404(6) 5_656 ?
Dy2 O16 2.404(6) 4_656 ?
Dy2 O15 2.552(6) 4_656 ?
Dy2 O15 2.552(6) 5_656 ?
Dy2 C31 2.816(9) 5_656 ?
Dy2 C31 2.816(9) 4_656 ?
Dy2 Dy3 3.8859(9) 5_656 ?
Dy2 K1 4.126(3) 1_554 ?
Dy3 O6 2.252(10) 5_656 ?
Dy3 O1 2.295(9) 5_657 ?
Dy3 O15 2.356(6) . ?
Dy3 O15 2.356(6) 8 ?
Dy3 O11 2.380(7) . ?
Dy3 O11 2.380(7) 8 ?
Dy3 O10 2.440(6) 8 ?
Dy3 O10 2.440(6) . ?
Dy3 C17 2.806(9) 8 ?
Dy3 Dy2 3.8859(9) 5_656 ?
Dy3 K1 3.933(3) 2_554 ?
K1 O10 2.677(7) 2 ?
K1 O10 2.677(7) 7_666 ?
K1 O7 2.736(12) . ?
K1 O7 2.736(12) 8_565 ?
K1 O16 2.837(7) 4_657 ?
K1 O16 2.837(7) 5_657 ?
K1 O6 3.046(10) 6_557 ?
K1 O4 3.096(11) 1_556 ?
K1 Dy3 3.933(3) 2 ?
K1 Dy2 4.126(3) 1_556 ?
O1 Dy3 2.295(9) 5_657 ?
O4 K1 3.096(11) 1_554 ?
O6 Dy3 2.252(10) 5_656 ?
O6 K1 3.046(10) 6_657 ?
O10 K1 2.677(7) 2_554 ?
O15 Dy2 2.552(6) 5_656 ?
O16 Dy2 2.404(6) 5_656 ?
O16 K1 2.837(7) 5_657 ?
O1W H1W 0.9695 . ?
O1W H2W 0.9730 . ?

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 C1 O1 144.8(18) . . ?
O2 C1 H1 107.6 . . ?
O1 C1 H1 107.6 . . ?
O3 C2 O4 127.0(13) . . ?
O3 C2 H2 116.5 . . ?
O4 C2 H2 116.5 . . ?
O6 C3 O5 124.3(13) . . ?
O6 C3 H3 117.8 . . ?
O5 C3 H3 117.8 . . ?
O7 C4 O8 118.1(12) . . ?
O7 C4 C5 125.7(11) . . ?
O8 C4 C5 115.0(13) . . ?
C10 C5 C6 119.3(10) . . ?
C10 C5 C4 117.3(10) . . ?
C6 C5 C4 123.4(11) . . ?
C7 C6 C5 120.3(12) . . ?
C7 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
C8 C7 C6 121.2(11) . . ?
C8 C7 H7 119.4 . . ?
C6 C7 H7 119.4 . . ?
C7 C8 O9 123.3(10) . . ?
C7 C8 C9 119.3(10) . . ?
O9 C8 C9 117.4(10) . . ?
C8 C9 C10 119.4(11) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
C5 C10 C9 120.5(10) . . ?
C5 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C16 C11 C12 120.8(10) . . ?
C16 C11 O9 119.7(10) . . ?
C12 C11 O9 119.4(10) . . ?
C11 C12 C13 119.0(11) . . ?
C11 C12 H12 120.5 . . ?
C13 C12 H12 120.5 . . ?
C14 C13 C12 120.4(11) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C13 C14 C15 119.8(9) . . ?
C13 C14 C17 119.7(9) . . ?
C15 C14 C17 120.4(8) . . ?
C14 C15 C16 119.6(9) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
C11 C16 C15 120.4(10) . . ?
C11 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
O10 C17 O11 117.8(8) . . ?
O10 C17 C14 121.4(8) . . ?
O11 C17 C14 120.9(9) . . ?
O12 C18 O13 120.6(14) . . ?
O12 C18 C19 119.7(14) . . ?
O13 C18 C19 119.5(9) . . ?
C20 C19 C24 118.0(11) . . ?
C20 C19 C18 121.1(11) . . ?
C24 C19 C18 120.7(10) . . ?
C19 C20 C21 120.0(13) . . ?
C19 C20 H20 120.0 . . ?
C21 C20 H20 120.0 . . ?
C22 C21 C20 119.9(13) . . ?
C22 C21 H21 120.1 . . ?
C20 C21 H21 120.1 . . ?
C23 C22 C21 121.3(13) . . ?
C23 C22 O14 116.7(17) . . ?
C21 C22 O14 121.5(17) . . ?
C22 C23 C24 117.8(15) . . ?
C22 C23 H23 121.1 . . ?
C24 C23 H23 121.1 . . ?
C19 C24 C23 123.0(13) . . ?
C19 C24 H24 118.5 . . ?
C23 C24 H24 118.5 . . ?
O14 C25 C30 125.1(13) . . ?
O14 C25 C26 114.9(11) . . ?
C30 C25 C26 119.8(11) . . ?
C27 C26 C25 119.4(10) . . ?
C27 C26 H26 120.3 . . ?
C25 C26 H26 120.3 . . ?
C26 C27 C28 121.2(10) . . ?
C26 C27 H27 119.4 . . ?
C28 C27 H27 119.4 . . ?
C29 C28 C27 117.6(9) . . ?
C29 C28 C31 122.5(9) . . ?
C27 C28 C31 119.5(9) . . ?
C30 C29 C28 123.1(11) . . ?
C30 C29 H29 118.4 . . ?
C28 C29 H29 118.4 . . ?
C29 C30 C25 118.7(12) . . ?
C29 C30 H30 120.6 . . ?
C25 C30 H30 120.6 . . ?
O16 C31 O15 118.7(8) . . ?
O16 C31 C28 120.6(8) . . ?
O15 C31 C28 120.6(8) . . ?
O16 C31 Dy2 58.2(5) . 5_656 ?
O15 C31 Dy2 64.9(5) . 5_656 ?
C28 C31 Dy2 154.9(7) . 5_656 ?
O3 Dy1 O2 157.7(4) . . ?
O3 Dy1 O12 84.8(3) . 8_565 ?
O2 Dy1 O12 77.5(4) . 8_565 ?
O3 Dy1 O12 84.8(3) . . ?
O2 Dy1 O12 77.5(4) . . ?
O12 Dy1 O12 74.5(9) 8_565 . ?
O3 Dy1 O8 74.0(3) . . ?
O2 Dy1 O8 115.3(4) . . ?
O12 Dy1 O8 148.0(5) 8_565 . ?
O12 Dy1 O8 79.7(6) . . ?
O3 Dy1 O8 74.0(3) . 8_565 ?
O2 Dy1 O8 115.3(4) . 8_565 ?
O12 Dy1 O8 79.7(6) 8_565 8_565 ?
O12 Dy1 O8 148.0(5) . 8_565 ?
O8 Dy1 O8 115.8(9) . 8_565 ?
O3 Dy1 O7 120.0(3) . 8_565 ?
O2 Dy1 O7 77.2(4) . 8_565 ?
O12 Dy1 O7 100.9(6) 8_565 8_565 ?
O12 Dy1 O7 154.7(4) . 8_565 ?
O8 Dy1 O7 110.4(5) . 8_565 ?
O8 Dy1 O7 49.4(3) 8_565 8_565 ?
O3 Dy1 O7 120.0(3) . . ?
O2 Dy1 O7 77.2(4) . . ?
O12 Dy1 O7 154.7(4) 8_565 . ?
O12 Dy1 O7 100.9(6) . . ?
O8 Dy1 O7 49.4(3) . . ?
O8 Dy1 O7 110.4(5) 8_565 . ?
O7 Dy1 O7 72.3(6) 8_565 . ?
O3 Dy1 C4 98.0(3) . 8_565 ?
O2 Dy1 C4 95.5(3) . 8_565 ?
O12 Dy1 C4 90.0(5) 8_565 8_565 ?
O12 Dy1 C4 164.0(5) . 8_565 ?
O8 Dy1 C4 116.2(5) . 8_565 ?
O8 Dy1 C4 25.4(4) 8_565 8_565 ?
O7 Dy1 C4 24.0(3) 8_565 8_565 ?
O7 Dy1 C4 91.4(5) . 8_565 ?
O4 Dy2 O13 86.3(2) . 8_565 ?
O4 Dy2 O13 86.3(2) . . ?
O13 Dy2 O13 126.9(6) 8_565 . ?
O4 Dy2 O5 151.9(4) . . ?
O13 Dy2 O5 81.3(2) 8_565 . ?
O13 Dy2 O5 81.3(2) . . ?
O4 Dy2 O16 74.5(3) . 5_656 ?
O13 Dy2 O16 147.9(3) 8_565 5_656 ?
O13 Dy2 O16 78.0(3) . 5_656 ?
O5 Dy2 O16 126.5(2) . 5_656 ?
O4 Dy2 O16 74.5(3) . 4_656 ?
O13 Dy2 O16 78.0(3) 8_565 4_656 ?
O13 Dy2 O16 147.9(3) . 4_656 ?
O5 Dy2 O16 126.5(2) . 4_656 ?
O16 Dy2 O16 72.3(3) 5_656 4_656 ?
O4 Dy2 O15 125.8(2) . 4_656 ?
O13 Dy2 O15 76.4(3) 8_565 4_656 ?
O13 Dy2 O15 144.0(3) . 4_656 ?
O5 Dy2 O15 75.4(2) . 4_656 ?
O16 Dy2 O15 94.1(2) 5_656 4_656 ?
O16 Dy2 O15 51.96(19) 4_656 4_656 ?
O4 Dy2 O15 125.8(2) . 5_656 ?
O13 Dy2 O15 144.0(3) 8_565 5_656 ?
O13 Dy2 O15 76.4(3) . 5_656 ?
O5 Dy2 O15 75.4(2) . 5_656 ?
O16 Dy2 O15 51.96(19) 5_656 5_656 ?
O16 Dy2 O15 94.1(2) 4_656 5_656 ?
O15 Dy2 O15 71.3(3) 4_656 5_656 ?
O4 Dy2 C31 99.0(3) . 5_656 ?
O13 Dy2 C31 163.0(4) 8_565 5_656 ?
O13 Dy2 C31 69.8(4) . 5_656 ?
O5 Dy2 C31 100.2(2) . 5_656 ?
O16 Dy2 C31 26.3(2) 5_656 5_656 ?
O16 Dy2 C31 87.8(3) 4_656 5_656 ?
O15 Dy2 C31 87.5(2) 4_656 5_656 ?
O15 Dy2 C31 26.9(2) 5_656 5_656 ?
O4 Dy2 C31 99.0(3) . 4_656 ?
O13 Dy2 C31 69.8(4) 8_565 4_656 ?
O13 Dy2 C31 163.0(4) . 4_656 ?
O5 Dy2 C31 100.2(2) . 4_656 ?
O16 Dy2 C31 87.8(3) 5_656 4_656 ?
O16 Dy2 C31 26.3(2) 4_656 4_656 ?
O15 Dy2 C31 26.9(2) 4_656 4_656 ?
O15 Dy2 C31 87.5(2) 5_656 4_656 ?
C31 Dy2 C31 93.3(4) 5_656 4_656 ?
O4 Dy2 Dy3 140.5(3) . 5_656 ?
O13 Dy2 Dy3 109.3(2) 8_565 5_656 ?
O13 Dy2 Dy3 109.3(2) . 5_656 ?
O5 Dy2 Dy3 67.5(2) . 5_656 ?
O16 Dy2 Dy3 73.91(16) 5_656 5_656 ?
O16 Dy2 Dy3 73.91(16) 4_656 5_656 ?
O15 Dy2 Dy3 35.91(12) 4_656 5_656 ?
O15 Dy2 Dy3 35.91(12) 5_656 5_656 ?
C31 Dy2 Dy3 56.94(19) 5_656 5_656 ?
C31 Dy2 Dy3 56.94(19) 4_656 5_656 ?
O4 Dy2 K1 47.7(3) . 1_554 ?
O13 Dy2 K1 106.5(2) 8_565 1_554 ?
O13 Dy2 K1 106.5(2) . 1_554 ?
O5 Dy2 K1 160.3(2) . 1_554 ?
O16 Dy2 K1 41.94(15) 5_656 1_554 ?
O16 Dy2 K1 41.94(16) 4_656 1_554 ?
O15 Dy2 K1 88.69(13) 4_656 1_554 ?
O15 Dy2 K1 88.69(13) 5_656 1_554 ?
C31 Dy2 K1 67.09(19) 5_656 1_554 ?
C31 Dy2 K1 67.09(19) 4_656 1_554 ?
Dy3 Dy2 K1 92.82(4) 5_656 1_554 ?
O6 Dy3 O1 152.6(3) 5_656 5_657 ?
O6 Dy3 O15 78.4(2) 5_656 . ?
O1 Dy3 O15 80.4(2) 5_657 . ?
O6 Dy3 O15 78.4(2) 5_656 8 ?
O1 Dy3 O15 80.4(2) 5_657 8 ?
O15 Dy3 O15 78.4(3) . 8 ?
O6 Dy3 O11 122.0(2) 5_656 . ?
O1 Dy3 O11 72.4(2) 5_657 . ?
O15 Dy3 O11 84.0(3) . . ?
O15 Dy3 O11 149.7(2) 8 . ?
O6 Dy3 O11 122.0(2) 5_656 8 ?
O1 Dy3 O11 72.4(2) 5_657 8 ?
O15 Dy3 O11 149.7(2) . 8 ?
O15 Dy3 O11 84.0(3) 8 8 ?
O11 Dy3 O11 99.9(4) . 8 ?
O6 Dy3 O10 74.1(3) 5_656 8 ?
O1 Dy3 O10 125.6(2) 5_657 8 ?
O15 Dy3 O10 152.5(2) . 8 ?
O15 Dy3 O10 96.1(2) 8 8 ?
O11 Dy3 O10 110.4(3) . 8 ?
O11 Dy3 O10 53.4(2) 8 8 ?
O6 Dy3 O10 74.1(3) 5_656 . ?
O1 Dy3 O10 125.6(2) 5_657 . ?
O15 Dy3 O10 96.1(2) . . ?
O15 Dy3 O10 152.5(2) 8 . ?
O11 Dy3 O10 53.4(2) . . ?
O11 Dy3 O10 110.4(3) 8 . ?
O10 Dy3 O10 76.3(3) 8 . ?
O6 Dy3 C17 97.8(3) 5_656 8 ?
O1 Dy3 C17 99.3(2) 5_657 8 ?
O15 Dy3 C17 167.7(2) . 8 ?
O15 Dy3 C17 89.4(2) 8 8 ?
O11 Dy3 C17 107.7(3) . 8 ?
O11 Dy3 C17 26.9(2) 8 8 ?
O10 Dy3 C17 26.5(2) 8 8 ?
O10 Dy3 C17 94.0(2) . 8 ?
O6 Dy3 Dy2 69.9(2) 5_656 5_656 ?
O1 Dy3 Dy2 82.6(2) 5_657 5_656 ?
O15 Dy3 Dy2 39.46(14) . 5_656 ?
O15 Dy3 Dy2 39.46(14) 8 5_656 ?
O11 Dy3 Dy2 121.6(2) . 5_656 ?
O11 Dy3 Dy2 121.6(2) 8 5_656 ?
O10 Dy3 Dy2 126.75(18) 8 5_656 ?
O10 Dy3 Dy2 126.75(18) . 5_656 ?
C17 Dy3 Dy2 128.25(18) 8 5_656 ?
O6 Dy3 K1 50.5(3) 5_656 2_554 ?
O1 Dy3 K1 156.9(2) 5_657 2_554 ?
O15 Dy3 K1 116.74(14) . 2_554 ?
O15 Dy3 K1 116.74(14) 8 2_554 ?
O11 Dy3 K1 93.18(16) . 2_554 ?
O11 Dy3 K1 93.18(16) 8 2_554 ?
O10 Dy3 K1 42.02(15) 8 2_554 ?
O10 Dy3 K1 42.02(15) . 2_554 ?
C17 Dy3 K1 67.40(18) 8 2_554 ?
Dy2 Dy3 K1 120.44(5) 5_656 2_554 ?
O10 K1 O10 68.6(3) 2 7_666 ?
O10 K1 O7 96.1(3) 2 . ?
O10 K1 O7 135.3(4) 7_666 . ?
O10 K1 O7 135.3(4) 2 8_565 ?
O10 K1 O7 96.1(3) 7_666 8_565 ?
O7 K1 O7 64.9(5) . 8_565 ?
O10 K1 O16 128.9(2) 2 4_657 ?
O10 K1 O16 93.7(2) 7_666 4_657 ?
O7 K1 O16 125.4(4) . 4_657 ?
O7 K1 O16 92.4(4) 8_565 4_657 ?
O10 K1 O16 93.7(2) 2 5_657 ?
O10 K1 O16 128.9(2) 7_666 5_657 ?
O7 K1 O16 92.4(4) . 5_657 ?
O7 K1 O16 125.4(4) 8_565 5_657 ?
O16 K1 O16 60.0(3) 4_657 5_657 ?
O10 K1 O6 58.9(2) 2 6_557 ?
O10 K1 O6 58.9(2) 7_666 6_557 ?
O7 K1 O6 77.1(4) . 6_557 ?
O7 K1 O6 77.1(4) 8_565 6_557 ?
O16 K1 O6 148.60(15) 4_657 6_557 ?
O16 K1 O6 148.60(15) 5_657 6_557 ?
O10 K1 O4 72.2(2) 2 1_556 ?
O10 K1 O4 72.2(2) 7_666 1_556 ?
O7 K1 O4 144.9(3) . 1_556 ?
O7 K1 O4 144.9(3) 8_565 1_556 ?
O16 K1 O4 56.69(19) 4_657 1_556 ?
O16 K1 O4 56.69(19) 5_657 1_556 ?
O6 K1 O4 119.6(3) 6_557 1_556 ?
O10 K1 Dy3 37.60(14) 2 2 ?
O10 K1 Dy3 37.60(14) 7_666 2 ?
O7 K1 Dy3 106.3(3) . 2 ?
O7 K1 Dy3 106.3(3) 8_565 2 ?
O16 K1 Dy3 128.09(16) 4_657 2 ?
O16 K1 Dy3 128.09(16) 5_657 2 ?
O6 K1 Dy3 34.8(2) 6_557 2 ?
O4 K1 Dy3 84.77(17) 1_556 2 ?
O10 K1 Dy2 99.09(18) 2 1_556 ?
O10 K1 Dy2 99.09(18) 7_666 1_556 ?
O7 K1 Dy2 125.2(4) . 1_556 ?
O7 K1 Dy2 125.2(4) 8_565 1_556 ?
O16 K1 Dy2 34.49(14) 4_657 1_556 ?
O16 K1 Dy2 34.49(14) 5_657 1_556 ?
O6 K1 Dy2 152.3(2) 6_557 1_556 ?
O4 K1 Dy2 32.75(16) 1_556 1_556 ?
Dy3 K1 Dy2 117.52(8) 2 1_556 ?
C1 O1 Dy3 171.1(12) . 5_657 ?
C1 O2 Dy1 150.6(13) . . ?
C2 O3 Dy1 151.3(9) . . ?
C2 O4 Dy2 144.1(10) . . ?
C2 O4 K1 116.4(8) . 1_554 ?
Dy2 O4 K1 99.5(3) . 1_554 ?
C3 O5 Dy2 138.7(10) . . ?
C3 O6 Dy3 139.5(9) . 5_656 ?
C3 O6 K1 125.8(9) . 6_657 ?
Dy3 O6 K1 94.7(4) 5_656 6_657 ?
C4 O7 Dy1 92.7(8) . . ?
C4 O7 K1 149.5(12) . . ?
Dy1 O7 K1 109.0(4) . . ?
C4 O8 Dy1 99.7(8) . . ?
C8 O9 C11 117.9(8) . . ?
C17 O10 Dy3 93.3(5) . . ?
C17 O10 K1 155.7(6) . 2_554 ?
Dy3 O10 K1 100.4(2) . 2_554 ?
C17 O11 Dy3 95.6(6) . . ?
C18 O12 Dy1 162.1(10) . . ?
C18 O13 Dy2 125.9(9) . . ?
C25 O14 C22 120.8(10) . . ?
C31 O15 Dy3 130.8(6) . . ?
C31 O15 Dy2 88.2(5) . 5_656 ?
Dy3 O15 Dy2 104.6(2) . 5_656 ?
C31 O16 Dy2 95.5(5) . 5_656 ?
C31 O16 K1 151.9(6) . 5_657 ?
Dy2 O16 K1 103.6(2) 5_656 5_657 ?
H1W O1W H2W 109.1 . . ?

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
O7 C4 C5 C10 34(2) . . . . ?
O8 C4 C5 C10 -158.4(14) . . . . ?
O7 C4 C5 C6 -143.6(18) . . . . ?
O8 C4 C5 C6 23.8(18) . . . . ?
C10 C5 C6 C7 1(2) . . . . ?
C4 C5 C6 C7 178.7(12) . . . . ?
C5 C6 C7 C8 -1(2) . . . . ?
C6 C7 C8 O9 -179.9(12) . . . . ?
C6 C7 C8 C9 1(2) . . . . ?
C7 C8 C9 C10 -0.9(19) . . . . ?
O9 C8 C9 C10 -179.9(10) . . . . ?
C6 C5 C10 C9 -0.7(18) . . . . ?
C4 C5 C10 C9 -178.6(10) . . . . ?
C8 C9 C10 C5 0.7(18) . . . . ?
C16 C11 C12 C13 1(2) . . . . ?
O9 C11 C12 C13 177.0(13) . . . . ?
C11 C12 C13 C14 2(2) . . . . ?
C12 C13 C14 C15 -3(2) . . . . ?
C12 C13 C14 C17 177.5(13) . . . . ?
C13 C14 C15 C16 2.0(18) . . . . ?
C17 C14 C15 C16 -178.8(10) . . . . ?
C12 C11 C16 C15 -2(2) . . . . ?
O9 C11 C16 C15 -178.3(11) . . . . ?
C14 C15 C16 C11 0.8(18) . . . . ?
C13 C14 C17 O10 -157.1(11) . . . . ?
C15 C14 C17 O10 23.7(15) . . . . ?
C13 C14 C17 O11 24.0(16) . . . . ?
C15 C14 C17 O11 -155.2(10) . . . . ?
O12 C18 C19 C20 -170.4(13) . . . . ?
O13 C18 C19 C20 5.6(16) . . . . ?
O12 C18 C19 C24 5.2(18) . . . . ?
O13 C18 C19 C24 -178.8(11) . . . . ?
C24 C19 C20 C21 -1(2) . . . . ?
C18 C19 C20 C21 174.5(13) . . . . ?
C19 C20 C21 C22 1(2) . . . . ?
C20 C21 C22 C23 -1(3) . . . . ?
C20 C21 C22 O14 -173.5(14) . . . . ?
C21 C22 C23 C24 2(2) . . . . ?
O14 C22 C23 C24 174.4(13) . . . . ?
C20 C19 C24 C23 2(2) . . . . ?
C18 C19 C24 C23 -173.9(13) . . . . ?
C22 C23 C24 C19 -2(2) . . . . ?
O14 C25 C26 C27 179.1(14) . . . . ?
C30 C25 C26 C27 4(2) . . . . ?
C25 C26 C27 C28 -3(2) . . . . ?
C26 C27 C28 C29 0.6(17) . . . . ?
C26 C27 C28 C31 173.2(11) . . . . ?
C27 C28 C29 C30 1.2(18) . . . . ?
C31 C28 C29 C30 -171.3(12) . . . . ?
C28 C29 C30 C25 0(2) . . . . ?
O14 C25 C30 C29 -176.9(15) . . . . ?
C26 C25 C30 C29 -2(2) . . . . ?
C29 C28 C31 O16 156.6(10) . . . . ?
C27 C28 C31 O16 -15.7(15) . . . . ?
C29 C28 C31 O15 -18.6(15) . . . . ?
C27 C28 C31 O15 169.1(9) . . . . ?
C29 C28 C31 Dy2 77.2(18) . . . 5_656 ?
C27 C28 C31 Dy2 -95.1(17) . . . 5_656 ?
O2 C1 O1 Dy3 180.000(12) . . . 5_657 ?
O1 C1 O2 Dy1 180.000(8) . . . . ?
O3 Dy1 O2 C1 180.000(8) . . . . ?
O12 Dy1 O2 C1 141.7(5) 8_565 . . . ?
O12 Dy1 O2 C1 -141.7(5) . . . . ?
O8 Dy1 O2 C1 -69.5(4) . . . . ?
O8 Dy1 O2 C1 69.5(4) 8_565 . . . ?
O7 Dy1 O2 C1 37.2(3) 8_565 . . . ?
O7 Dy1 O2 C1 -37.2(3) . . . . ?
C4 Dy1 O2 C1 52.9(3) 8_565 . . . ?
O4 C2 O3 Dy1 0.000(3) . . . . ?
O2 Dy1 O3 C2 0.000(4) . . . . ?
O12 Dy1 O3 C2 37.4(4) 8_565 . . . ?
O12 Dy1 O3 C2 -37.4(4) . . . . ?
O8 Dy1 O3 C2 -118.2(4) . . . . ?
O8 Dy1 O3 C2 118.2(4) 8_565 . . . ?
O7 Dy1 O3 C2 137.1(4) 8_565 . . . ?
O7 Dy1 O3 C2 -137.1(4) . . . . ?
C4 Dy1 O3 C2 126.7(3) 8_565 . . . ?
O3 C2 O4 Dy2 0.000(3) . . . . ?
O3 C2 O4 K1 180.000(2) . . . 1_554 ?
O13 Dy2 O4 C2 -63.7(3) 8_565 . . . ?
O13 Dy2 O4 C2 63.7(3) . . . . ?
O5 Dy2 O4 C2 0.000(3) . . . . ?
O16 Dy2 O4 C2 142.24(18) 5_656 . . . ?
O16 Dy2 O4 C2 -142.24(18) 4_656 . . . ?
O15 Dy2 O4 C2 -134.0(2) 4_656 . . . ?
O15 Dy2 O4 C2 134.0(2) 5_656 . . . ?
C31 Dy2 O4 C2 132.6(2) 5_656 . . . ?
C31 Dy2 O4 C2 -132.6(2) 4_656 . . . ?
Dy3 Dy2 O4 C2 180.000(2) 5_656 . . . ?
K1 Dy2 O4 C2 180.000(2) 1_554 . . . ?
O13 Dy2 O4 K1 116.3(3) 8_565 . . 1_554 ?
O13 Dy2 O4 K1 -116.3(3) . . . 1_554 ?
O5 Dy2 O4 K1 180.0 . . . 1_554 ?
O16 Dy2 O4 K1 -37.76(18) 5_656 . . 1_554 ?
O16 Dy2 O4 K1 37.76(18) 4_656 . . 1_554 ?
O15 Dy2 O4 K1 46.0(2) 4_656 . . 1_554 ?
O15 Dy2 O4 K1 -46.0(2) 5_656 . . 1_554 ?
C31 Dy2 O4 K1 -47.4(2) 5_656 . . 1_554 ?
C31 Dy2 O4 K1 47.4(2) 4_656 . . 1_554 ?
Dy3 Dy2 O4 K1 0.0 5_656 . . 1_554 ?
O6 C3 O5 Dy2 0.000(2) . . . . ?
O4 Dy2 O5 C3 180.000(2) . . . . ?
O13 Dy2 O5 C3 -115.2(3) 8_565 . . . ?
O13 Dy2 O5 C3 115.2(3) . . . . ?
O16 Dy2 O5 C3 47.2(3) 5_656 . . . ?
O16 Dy2 O5 C3 -47.2(3) 4_656 . . . ?
O15 Dy2 O5 C3 -37.05(14) 4_656 . . . ?
O15 Dy2 O5 C3 37.05(14) 5_656 . . . ?
C31 Dy2 O5 C3 47.6(2) 5_656 . . . ?
C31 Dy2 O5 C3 -47.6(2) 4_656 . . . ?
Dy3 Dy2 O5 C3 0.000(2) 5_656 . . . ?
K1 Dy2 O5 C3 0.000(3) 1_554 . . . ?
O5 C3 O6 Dy3 0.000(3) . . . 5_656 ?
O5 C3 O6 K1 180.000(2) . . . 6_657 ?
O8 C4 O7 Dy1 -3.1(18) . . . . ?
C5 C4 O7 Dy1 164.1(11) . . . . ?
O8 C4 O7 K1 133.2(19) . . . . ?
C5 C4 O7 K1 -60(3) . . . . ?
O3 Dy1 O7 C4 26.0(14) . . . . ?
O2 Dy1 O7 C4 -138.6(13) . . . . ?
O12 Dy1 O7 C4 -141.2(13) 8_565 . . . ?
O12 Dy1 O7 C4 -64.3(13) . . . . ?
O8 Dy1 O7 C4 1.9(11) . . . . ?
O8 Dy1 O7 C4 108.9(12) 8_565 . . . ?
O7 Dy1 O7 C4 140.9(10) 8_565 . . . ?
C4 Dy1 O7 C4 126.0(13) 8_565 . . . ?
O3 Dy1 O7 K1 -132.2(4) . . . . ?
O2 Dy1 O7 K1 63.1(5) . . . . ?
O12 Dy1 O7 K1 60.6(16) 8_565 . . . ?
O12 Dy1 O7 K1 137.5(5) . . . . ?
O8 Dy1 O7 K1 -156.4(10) . . . . ?
O8 Dy1 O7 K1 -49.4(7) 8_565 . . . ?
O7 Dy1 O7 K1 -17.3(8) 8_565 . . . ?
C4 Dy1 O7 K1 -32.2(6) 8_565 . . . ?
O10 K1 O7 C4 21(2) 2 . . . ?
O10 K1 O7 C4 -44(3) 7_666 . . . ?
O7 K1 O7 C4 -117(2) 8_565 . . . ?
O16 K1 O7 C4 169(2) 4_657 . . . ?
O16 K1 O7 C4 115(2) 5_657 . . . ?
O6 K1 O7 C4 -35(2) 6_557 . . . ?
O4 K1 O7 C4 89(3) 1_556 . . . ?
Dy3 K1 O7 C4 -16(2) 2 . . . ?
Dy2 K1 O7 C4 127(2) 1_556 . . . ?
O10 K1 O7 Dy1 154.2(5) 2 . . . ?
O10 K1 O7 Dy1 88.7(6) 7_666 . . . ?
O7 K1 O7 Dy1 16.6(8) 8_565 . . . ?
O16 K1 O7 Dy1 -57.5(7) 4_657 . . . ?
O16 K1 O7 Dy1 -111.8(6) 5_657 . . . ?
O6 K1 O7 Dy1 98.2(6) 6_557 . . . ?
O4 K1 O7 Dy1 -138.2(4) 1_556 . . . ?
Dy3 K1 O7 Dy1 117.3(5) 2 . . . ?
Dy2 K1 O7 Dy1 -100.1(5) 1_556 . . . ?
O7 C4 O8 Dy1 3(2) . . . . ?
C5 C4 O8 Dy1 -165.1(7) . . . . ?
O3 Dy1 O8 C4 -160.1(12) . . . . ?
O2 Dy1 O8 C4 41.5(13) . . . . ?
O12 Dy1 O8 C4 149.2(9) 8_565 . . . ?
O12 Dy1 O8 C4 112.4(12) . . . . ?
O8 Dy1 O8 C4 -97.3(12) 8_565 . . . ?
O7 Dy1 O8 C4 -43.5(13) 8_565 . . . ?
O7 Dy1 O8 C4 -1.8(10) . . . . ?
C4 Dy1 O8 C4 -69.0(13) 8_565 . . . ?
C7 C8 O9 C11 33.5(18) . . . . ?
C9 C8 O9 C11 -147.6(11) . . . . ?
C16 C11 O9 C8 -124.2(12) . . . . ?
C12 C11 O9 C8 59.8(17) . . . . ?
O11 C17 O10 Dy3 -2.7(9) . . . . ?
C14 C17 O10 Dy3 178.4(8) . . . . ?
O11 C17 O10 K1 121.7(13) . . . 2_554 ?
C14 C17 O10 K1 -57(2) . . . 2_554 ?
O6 Dy3 O10 C17 -152.4(6) 5_656 . . . ?
O1 Dy3 O10 C17 6.3(7) 5_657 . . . ?
O15 Dy3 O10 C17 -76.3(6) . . . . ?
O15 Dy3 O10 C17 -152.8(5) 8 . . . ?
O11 Dy3 O10 C17 1.6(6) . . . . ?
O11 Dy3 O10 C17 88.8(6) 8 . . . ?
O10 Dy3 O10 C17 130.5(5) 8 . . . ?
C17 Dy3 O10 C17 110.7(7) 8 . . . ?
Dy2 Dy3 O10 C17 -103.5(6) 5_656 . . . ?
K1 Dy3 O10 C17 159.8(7) 2_554 . . . ?
O6 Dy3 O10 K1 47.8(2) 5_656 . . 2_554 ?
O1 Dy3 O10 K1 -153.6(3) 5_657 . . 2_554 ?
O15 Dy3 O10 K1 123.9(2) . . . 2_554 ?
O15 Dy3 O10 K1 47.4(6) 8 . . 2_554 ?
O11 Dy3 O10 K1 -158.2(4) . . . 2_554 ?
O11 Dy3 O10 K1 -71.0(3) 8 . . 2_554 ?
O10 Dy3 O10 K1 -29.3(3) 8 . . 2_554 ?
C17 Dy3 O10 K1 -49.2(3) 8 . . 2_554 ?
Dy2 Dy3 O10 K1 96.7(2) 5_656 . . 2_554 ?
O10 C17 O11 Dy3 2.8(10) . . . . ?
C14 C17 O11 Dy3 -178.3(7) . . . . ?
O6 Dy3 O11 C17 28.3(7) 5_656 . . . ?
O1 Dy3 O11 C17 -177.6(7) 5_657 . . . ?
O15 Dy3 O11 C17 100.6(6) . . . . ?
O15 Dy3 O11 C17 155.1(5) 8 . . . ?
O11 Dy3 O11 C17 -109.7(6) 8 . . . ?
O10 Dy3 O11 C17 -55.3(7) 8 . . . ?
O10 Dy3 O11 C17 -1.6(5) . . . . ?
C17 Dy3 O11 C17 -83.2(6) 8 . . . ?
Dy2 Dy3 O11 C17 113.1(6) 5_656 . . . ?
K1 Dy3 O11 C17 -16.0(6) 2_554 . . . ?
O13 C18 O12 Dy1 75(5) . . . . ?
C19 C18 O12 Dy1 -109(4) . . . . ?
O3 Dy1 O12 C18 -35(5) . . . . ?
O2 Dy1 O12 C18 158(5) . . . . ?
O12 Dy1 O12 C18 -121(5) 8_565 . . . ?
O8 Dy1 O12 C18 40(5) . . . . ?
O8 Dy1 O12 C18 -83(5) 8_565 . . . ?
O7 Dy1 O12 C18 156(4) 8_565 . . . ?
O7 Dy1 O12 C18 84(5) . . . . ?
C4 Dy1 O12 C18 -136(4) 8_565 . . . ?
O12 C18 O13 Dy2 22.9(16) . . . . ?
C19 C18 O13 Dy2 -153.0(7) . . . . ?
O4 Dy2 O13 C18 -84.2(9) . . . . ?
O13 Dy2 O13 C18 -1.6(12) 8_565 . . . ?
O5 Dy2 O13 C18 70.6(9) . . . . ?
O16 Dy2 O13 C18 -159.0(9) 5_656 . . . ?
O16 Dy2 O13 C18 -136.7(8) 4_656 . . . ?
O15 Dy2 O13 C18 120.6(9) 4_656 . . . ?
O15 Dy2 O13 C18 147.6(9) 5_656 . . . ?
C31 Dy2 O13 C18 174.8(9) 5_656 . . . ?
C31 Dy2 O13 C18 167.0(9) 4_656 . . . ?
Dy3 Dy2 O13 C18 133.0(8) 5_656 . . . ?
K1 Dy2 O13 C18 -127.9(8) 1_554 . . . ?
C30 C25 O14 C22 -27(3) . . . . ?
C26 C25 O14 C22 158.5(17) . . . . ?
C23 C22 O14 C25 129.5(17) . . . . ?
C21 C22 O14 C25 -58(2) . . . . ?
O16 C31 O15 Dy3 84.8(11) . . . . ?
C28 C31 O15 Dy3 -100.0(10) . . . . ?
Dy2 C31 O15 Dy3 107.9(6) 5_656 . . . ?
O16 C31 O15 Dy2 -23.1(9) . . . 5_656 ?
C28 C31 O15 Dy2 152.2(9) . . . 5_656 ?
O6 Dy3 O15 C31 -172.9(8) 5_656 . . . ?
O1 Dy3 O15 C31 -10.5(7) 5_657 . . . ?
O15 Dy3 O15 C31 -92.6(7) 8 . . . ?
O11 Dy3 O15 C31 62.6(7) . . . . ?
O11 Dy3 O15 C31 -36.8(10) 8 . . . ?
O10 Dy3 O15 C31 -173.3(7) 8 . . . ?
O10 Dy3 O15 C31 114.7(7) . . . . ?
C17 Dy3 O15 C31 -99.9(13) 8 . . . ?
Dy2 Dy3 O15 C31 -100.5(8) 5_656 . . . ?
K1 Dy3 O15 C31 153.2(7) 2_554 . . . ?
O6 Dy3 O15 Dy2 -72.4(2) 5_656 . . 5_656 ?
O1 Dy3 O15 Dy2 90.0(2) 5_657 . . 5_656 ?
O15 Dy3 O15 Dy2 7.9(3) 8 . . 5_656 ?
O11 Dy3 O15 Dy2 163.1(2) . . . 5_656 ?
O11 Dy3 O15 Dy2 63.7(6) 8 . . 5_656 ?
O10 Dy3 O15 Dy2 -72.8(5) 8 . . 5_656 ?
O10 Dy3 O15 Dy2 -144.8(2) . . . 5_656 ?
C17 Dy3 O15 Dy2 0.6(12) 8 . . 5_656 ?
K1 Dy3 O15 Dy2 -106.30(16) 2_554 . . 5_656 ?
O15 C31 O16 Dy2 24.7(10) . . . 5_656 ?
C28 C31 O16 Dy2 -150.6(8) . . . 5_656 ?
O15 C31 O16 K1 -108.2(12) . . . 5_657 ?
C28 C31 O16 K1 76.5(16) . . . 5_657 ?
Dy2 C31 O16 K1 -133.0(13) 5_656 . . 5_657 ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        27.53
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         1.942
_refine_diff_density_min         -1.934
_refine_diff_density_rms         0.189
