# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_cp80
_database_code_depnum_ccdc_archive 'CCDC 1021088'
_audit_update_record             
;
2014-08-25 deposited with the CCDC.
2015-01-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C36.64 H49.28 Dy4 Fe2 N10 O32, 0.36(H2 O), 3(C H4 O)'
_chemical_formula_sum            'C39.64 H62 Dy4 Fe2 N10 O35.36'
_chemical_formula_weight         2006.13

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0043 0.0021 http://skuld.bmsc.washington.edu/scatter/AS_periodic.html
H H 0.0000 0.0000 http://skuld.bmsc.washington.edu/scatter/AS_periodic.html
N N 0.0082 0.0043 http://skuld.bmsc.washington.edu/scatter/AS_periodic.html
O O 0.0142 0.0079 http://skuld.bmsc.washington.edu/scatter/AS_periodic.html
Fe Fe 0.3536 1.0498 http://skuld.bmsc.washington.edu/scatter/AS_periodic.html
Dy Dy -0.1899 5.4020 http://skuld.bmsc.washington.edu/scatter/AS_periodic.html

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.226(2)
_cell_length_b                   12.250(3)
_cell_length_c                   13.744(3)
_cell_angle_alpha                102.500(3)
_cell_angle_beta                 97.563(3)
_cell_angle_gamma                104.646(3)
_cell_volume                     1594.3(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9955
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      32.62

_exptl_crystal_description       needle
_exptl_crystal_colour            'pale orange'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.090
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             969
_exptl_absorpt_coefficient_mu    7.134
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.582
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   'SADABS 2.10 (Bruker AXS Inc., 2005)'

_exptl_special_details           
; 
 Data were measured on the SCD beamline at the ANKA synchrotron,
 Karlsruhe Institute of Technology 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.80000
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_radiation_monochromator  silicon
_diffrn_measurement_device_type  'Bruker SMART Apex'
_diffrn_measurement_method       'CCD area detector, ω-scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20261
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.29
_diffrn_reflns_theta_max         32.68
_reflns_number_total             7495
_reflns_number_gt                7000
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2 (Bruker AXS Inc., 2005)'
_computing_cell_refinement       'Apex2 (Bruker AXS Inc., 2005)'
_computing_data_reduction        'Apex2 (Bruker AXS Inc., 2005)'
_computing_structure_solution    'Apex2 (Bruker AXS Inc., 2005)'
_computing_structure_refinement  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_molecular_graphics    'Diamond 2.1 (Crystal Impact, 1998)'

_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.
 The triply-bridging ligand based on O(3) was modelled as a disordered
 superposition of methoxo (with methyl carbon C3A, 82% occupancy) and
 hydroxo (forming a hydrogen bond to lattice water O33B, 18% occupancy). 
 Over the molecule as a whole this comes to 1.64 (OMe) and 0.36 (OH..OH2).
 The neutral monodentate ligands on Dy1 and Dy2 were also disordered. Those
 based on O15 and O16 were methanol, with their respective carbons 55:45
 disordered. That on O14 was a 50:50 mixture of MeOH and water (i.e. 50%
 occupancy for the carbon); it was not possible to model the second H-atom
 of the water component. Similarity restraints were applied to the C-O
 distances. The molecule thus has a total of 5 MeOH and 1 H2O.
 A lattice MeOH on a general site was 72:28 disordered. The major component
 could be refined anisotropically with torsion angles of all H-atoms
 refined, the minor component only as isotropic part atoms without
 hydrogens. Another MeOH was badly disordered over an inversion centre, and
 was refined with partial occupancy isotropic C and O atoms. Similarity
 restraints were applied to the C-O bond distances of the lattice MeOH.
 There are thuis three lattice MeOH per cluster, in addition to the
 0.36 water.
 One of the cyanoacetate ligands has its CN group 55:45 disordered. These
 partial atoms were refined anisotropically, with geometrical similarity
 restraints. 
;

_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)+(0.0207P)²+1.8636P] 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         7495
_refine_ls_number_parameters     481
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0257
_refine_ls_wR_factor_ref         0.0657
_refine_ls_wR_factor_gt          0.0648
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.033
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.329228(13) 0.256384(12) 0.467331(9) 0.01755(5) Uani 1 1 d . . .
Dy2 Dy 0.485492(13) 0.432706(12) 0.275663(9) 0.01679(5) Uani 1 1 d . . .
Fe1 Fe 0.37194(4) 0.53818(4) 0.48379(3) 0.01553(9) Uani 1 1 d . . .
O1 O 0.4484(2) 0.44233(18) 0.56318(15) 0.0159(4) Uani 1 1 d . . .
O2 O 0.3026(2) 0.39203(19) 0.37158(15) 0.0187(4) Uani 1 1 d D . .
H2 H 0.233(3) 0.384(3) 0.332(3) 0.022 Uiso 1 1 d D . .
O3 O 0.4653(2) 0.67871(18) 0.60083(15) 0.0181(4) Uani 1 1 d . . .
H3 H 0.4129 0.7362 0.6199 0.022 Uiso 0.18 1 calc PR A 2
C3A C 0.4002(4) 0.7677(3) 0.6329(3) 0.0211(7) Uani 0.82 1 d P B 1
H3A H 0.4620 0.8285 0.6908 0.032 Uiso 0.82 1 calc PR B 1
H3B H 0.3140 0.7331 0.6531 0.032 Uiso 0.82 1 calc PR B 1
H3C H 0.3803 0.8021 0.5766 0.032 Uiso 0.82 1 calc PR B 1
O33B O 0.356(4) 0.821(3) 0.705(3) 0.136(12) Uiso 0.18 1 d P C 2
O4 O 0.3606(2) 0.2371(2) 0.19356(16) 0.0244(5) Uani 1 1 d . . .
O5 O 0.2730(2) 0.1390(2) 0.30085(16) 0.0273(5) Uani 1 1 d . . .
C4 C 0.2837(3) 0.1526(3) 0.2146(2) 0.0231(6) Uani 1 1 d . . .
C5 C 0.1928(4) 0.0511(3) 0.1267(3) 0.0366(9) Uani 1 1 d . . .
H5A H 0.2398 -0.0104 0.1127 0.044 Uiso 1 1 calc R . .
H5B H 0.1050 0.0169 0.1465 0.044 Uiso 1 1 calc R . .
C6 C 0.1635(4) 0.0893(4) 0.0344(3) 0.0428(10) Uani 1 1 d . . .
N1 N 0.1397(5) 0.1201(4) -0.0362(3) 0.0675(14) Uani 1 1 d . . .
O6 O 0.3049(2) 0.6318(2) 0.39112(17) 0.0231(5) Uani 1 1 d . . .
O7 O 0.4970(2) 0.7830(2) 0.42352(17) 0.0237(5) Uani 1 1 d . . .
C7 C 0.3833(3) 0.7195(3) 0.3712(2) 0.0227(6) Uani 1 1 d . B .
C8 C 0.3280(4) 0.7440(3) 0.2719(3) 0.0373(9) Uani 1 1 d . . .
H8A H 0.3107 0.6731 0.2156 0.045 Uiso 1 1 calc R B .
H8B H 0.2387 0.7604 0.2762 0.045 Uiso 1 1 calc R . .
C9 C 0.4219(4) 0.8428(4) 0.2482(3) 0.0377(9) Uani 1 1 d . B .
N2 N 0.4951(5) 0.9188(4) 0.2292(3) 0.0598(11) Uani 1 1 d . . .
O8 O 0.1907(2) 0.5097(2) 0.53443(16) 0.0229(5) Uani 1 1 d . . .
O9 O 0.2750(2) 0.5408(2) 0.70050(17) 0.0249(5) Uani 1 1 d . . .
C10 C 0.1791(3) 0.5097(3) 0.6248(2) 0.0233(6) Uani 1 1 d . B .
C11 C 0.0307(3) 0.4691(4) 0.6407(3) 0.0392(10) Uani 1 1 d . . .
H11A H -0.0123 0.5330 0.6403 0.047 Uiso 1 1 calc R B .
H11B H -0.0228 0.4016 0.5833 0.047 Uiso 1 1 calc R . .
C12 C 0.0228(3) 0.4356(4) 0.7351(3) 0.0346(8) Uani 1 1 d . B .
N3 N 0.0167(3) 0.4079(4) 0.8084(3) 0.0471(9) Uani 1 1 d . . .
O10 O 0.2501(2) 0.2685(2) 0.62080(16) 0.0276(5) Uani 1 1 d . . .
O11 O 0.4185(2) 0.3796(2) 0.75418(16) 0.0238(5) Uani 1 1 d . . .
C13 C 0.3076(3) 0.3015(3) 0.7129(2) 0.0226(6) Uani 1 1 d . . .
C14 C 0.2349(4) 0.2366(3) 0.7836(3) 0.0323(8) Uani 1 1 d . . .
H14A H 0.2907 0.1883 0.8065 0.039 Uiso 1 1 calc R . .
H14B H 0.2298 0.2946 0.8445 0.039 Uiso 1 1 calc R . .
C15 C 0.0945(4) 0.1609(3) 0.7350(3) 0.0363(9) Uani 1 1 d . . .
N4 N -0.0134(4) 0.1036(4) 0.6961(3) 0.0584(12) Uani 1 1 d . . .
O12 O 0.3002(2) 0.4560(2) 0.17039(17) 0.0274(5) Uani 1 1 d . . .
O13 O 0.1082(2) 0.3524(2) 0.20798(18) 0.0336(6) Uani 1 1 d . . .
C16 C 0.1741(3) 0.3998(3) 0.1503(2) 0.0268(7) Uani 1 1 d . E .
C17 C 0.0971(4) 0.3908(4) 0.0442(3) 0.0434(11) Uani 1 1 d D . .
H17A H 0.0894 0.4692 0.0419 0.052 Uiso 0.55 1 calc PR D 1
H17B H 0.1535 0.3687 -0.0058 0.052 Uiso 0.55 1 calc PR D 1
H17C H 0.1174 0.3301 -0.0070 0.052 Uiso 0.45 1 d PR D 2
H17D H 0.1278 0.4664 0.0269 0.052 Uiso 0.45 1 d PR D 2
C18A C -0.0400(9) 0.3084(8) 0.0123(7) 0.039(2) Uani 0.55 1 d PD E 1
N5A N -0.1493(7) 0.2520(7) -0.0091(6) 0.0544(19) Uani 0.55 1 d PD E 1
C18B C -0.0584(8) 0.3578(10) 0.0419(8) 0.037(2) Uani 0.45 1 d PD E 2
N5B N -0.1765(8) 0.3249(10) 0.0374(8) 0.060(3) Uani 0.45 1 d PD E 2
O14 O 0.0842(2) 0.2133(3) 0.4269(2) 0.0366(6) Uani 1 1 d D . .
H14 H 0.029(4) 0.206(4) 0.366(3) 0.044 Uiso 1 1 d D . .
C19A C -0.0240(7) 0.1621(8) 0.4649(6) 0.041(2) Uani 0.50 1 d PD F 1
H19A H -0.1101 0.1624 0.4241 0.062 Uiso 0.50 1 calc PR F 1
H19B H -0.0152 0.2054 0.5354 0.062 Uiso 0.50 1 calc PR F 1
H19C H -0.0253 0.0813 0.4626 0.062 Uiso 0.50 1 calc PR F 1
O15 O 0.2476(3) 0.0498(2) 0.46063(19) 0.0340(6) Uani 1 1 d D . .
H15 H 0.188(4) 0.017(4) 0.407(3) 0.041 Uiso 1 1 d D . .
C20A C 0.3206(8) -0.0247(6) 0.4721(7) 0.0463(19) Uani 0.55 1 d PD F 1
H20A H 0.2577 -0.1023 0.4647 0.069 Uiso 0.55 1 calc PR F 1
H20B H 0.3801 0.0029 0.5398 0.069 Uiso 0.55 1 calc PR F 1
H20C H 0.3776 -0.0292 0.4202 0.069 Uiso 0.55 1 calc PR F 1
C20B C 0.2445(10) -0.0144(8) 0.5335(6) 0.040(2) Uani 0.45 1 d PD F 2
H20D H 0.2018 -0.0976 0.4999 0.060 Uiso 0.45 1 calc PR F 2
H20E H 0.1908 0.0119 0.5829 0.060 Uiso 0.45 1 calc PR F 2
H20F H 0.3388 -0.0026 0.5686 0.060 Uiso 0.45 1 calc PR F 2
O16 O 0.5498(4) 0.3774(3) 0.1131(2) 0.0492(8) Uani 1 1 d D . .
H16A H 0.6475 0.3997 0.1223 0.059 Uiso 0.55 1 calc PR G 1
H16B H 0.5138 0.2956 0.0833 0.059 Uiso 0.45 1 calc PR G 2
C21A C 0.4964(9) 0.3267(10) 0.0155(5) 0.064(3) Uani 0.55 1 d PD H 1
H21A H 0.5709 0.3255 -0.0225 0.095 Uiso 0.55 1 calc PR H 1
H21B H 0.4386 0.3707 -0.0108 0.095 Uiso 0.55 1 calc PR H 1
H21C H 0.4402 0.2465 0.0077 0.095 Uiso 0.55 1 calc PR H 1
C21B C 0.6228(12) 0.4309(10) 0.0532(7) 0.056(3) Uani 0.45 1 d PD H 2
H21D H 0.6226 0.3728 -0.0084 0.083 Uiso 0.45 1 calc PR H 2
H21E H 0.7179 0.4698 0.0900 0.083 Uiso 0.45 1 calc PR H 2
H21F H 0.5810 0.4890 0.0343 0.083 Uiso 0.45 1 calc PR H 2
O31A O -0.0925(4) 0.2238(5) 0.2751(4) 0.0618(14) Uani 0.72 1 d PD I 1
H31A H -0.0391 0.2593 0.2432 0.093 Uiso 0.72 1 calc PR I 1
C31A C -0.1831(16) 0.1200(13) 0.2078(14) 0.125(7) Uani 0.72 1 d PD I 1
H31B H -0.2364 0.0732 0.2466 0.188 Uiso 0.72 1 calc PR I 1
H31C H -0.1296 0.0750 0.1712 0.188 Uiso 0.72 1 calc PR I 1
H31D H -0.2461 0.1399 0.1590 0.188 Uiso 0.72 1 calc PR I 1
O31B O -0.0460(11) 0.1504(9) 0.2222(8) 0.042(2) Uiso 0.28 1 d PD J 2
C31B C -0.1893(15) 0.1128(17) 0.2073(14) 0.030(4) Uiso 0.28 1 d PD J 2
O32A O 0.449(3) 0.122(2) -0.0101(19) 0.068(6) Uiso 0.16 1 d PD K -1
C32A C 0.492(10) 0.035(6) 0.025(6) 0.14(4) Uiso 0.16 1 d PD K -1
O32B O 0.5681(15) 0.1708(11) 0.0293(11) 0.085(4) Uiso 0.34 1 d PD L -2
C32B C 0.5109(18) 0.0500(13) 0.0083(16) 0.049(4) Uiso 0.34 1 d PD L -2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O1 2.299(2) . ?
Dy1 O5 2.333(2) . ?
Dy1 O10 2.345(2) . ?
Dy1 O2 2.376(2) . ?
Dy1 O7 2.384(2) 2_666 ?
Dy1 O14 2.388(2) . ?
Dy1 O3 2.433(2) 2_666 ?
Dy1 O15 2.434(3) . ?
Dy2 O1 2.307(2) 2_666 ?
Dy2 O12 2.345(2) . ?
Dy2 O4 2.355(2) . ?
Dy2 O9 2.356(2) 2_666 ?
Dy2 O11 2.406(2) 2_666 ?
Dy2 O16 2.417(3) . ?
Dy2 O2 2.439(2) . ?
Dy2 O3 2.474(2) 2_666 ?
Fe1 O2 1.990(2) . ?
Fe1 O1 1.994(2) . ?
Fe1 O1 2.001(2) 2_666 ?
Fe1 O3 2.007(2) . ?
Fe1 O8 2.039(2) . ?
Fe1 O6 2.051(2) . ?
O1 Fe1 2.001(2) 2_666 ?
O1 Dy2 2.307(2) 2_666 ?
O2 H2 0.81(3) . ?
O3 C3A 1.435(4) . ?
O3 Dy1 2.433(2) 2_666 ?
O3 Dy2 2.474(2) 2_666 ?
O3 H3 1.0000 . ?
C3A H3A 0.9800 . ?
C3A H3B 0.9800 . ?
C3A H3C 0.9800 . ?
O4 C4 1.247(4) . ?
O5 C4 1.246(4) . ?
C4 C5 1.529(4) . ?
C5 C6 1.466(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 N1 1.134(5) . ?
O6 C7 1.273(4) . ?
O7 C7 1.247(4) . ?
O7 Dy1 2.384(2) 2_666 ?
C7 C8 1.527(4) . ?
C8 C9 1.470(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 N2 1.139(5) . ?
O8 C10 1.263(4) . ?
O9 C10 1.249(4) . ?
O9 Dy2 2.356(2) 2_666 ?
C10 C11 1.534(4) . ?
C11 C12 1.449(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 N3 1.135(5) . ?
O10 C13 1.255(4) . ?
O11 C13 1.253(4) . ?
O11 Dy2 2.406(2) 2_666 ?
C13 C14 1.534(4) . ?
C14 C15 1.475(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 N4 1.133(5) . ?
O12 C16 1.260(4) . ?
O13 C16 1.250(4) . ?
C16 C17 1.531(4) . ?
C17 C18A 1.452(8) . ?
C17 C18B 1.533(9) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 H17C 0.9901 . ?
C17 H17D 0.9900 . ?
C18A N5A 1.118(9) . ?
C18B N5B 1.161(10) . ?
O14 C19A 1.355(7) . ?
O14 H14 0.91(3) . ?
C19A H19A 0.9800 . ?
C19A H19B 0.9800 . ?
C19A H19C 0.9800 . ?
O15 C20A 1.339(7) . ?
O15 C20B 1.399(7) . ?
O15 H15 0.84(3) . ?
C20A H20A 0.9800 . ?
C20A H20B 0.9800 . ?
C20A H20C 0.9800 . ?
C20B H20D 0.9800 . ?
C20B H20E 0.9800 . ?
C20B H20F 0.9800 . ?
O16 C21A 1.325(7) . ?
O16 C21B 1.346(8) . ?
O16 H16A 0.9500 . ?
O16 H16B 0.9500 . ?
C21A H21A 0.9800 . ?
C21A H21B 0.9800 . ?
C21A H21C 0.9800 . ?
C21B H21D 0.9800 . ?
C21B H21E 0.9800 . ?
C21B H21F 0.9800 . ?
O31A C31A 1.414(12) . ?
O31A H31A 0.8400 . ?
C31A H31B 0.9800 . ?
C31A H31C 0.9800 . ?
C31A H31D 0.9800 . ?
O31B C31B 1.393(14) . ?
O32A C32A 1.406(19) . ?
O32B C32B 1.395(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 Dy1 O5 141.73(8) . . ?
O1 Dy1 O10 76.36(8) . . ?
O5 Dy1 O10 140.15(8) . . ?
O1 Dy1 O2 70.79(7) . . ?
O5 Dy1 O2 77.99(8) . . ?
O10 Dy1 O2 119.43(8) . . ?
O1 Dy1 O7 79.30(7) . 2_666 ?
O5 Dy1 O7 114.53(9) . 2_666 ?
O10 Dy1 O7 76.26(8) . 2_666 ?
O2 Dy1 O7 140.22(7) . 2_666 ?
O1 Dy1 O14 116.34(9) . . ?
O5 Dy1 O14 76.98(9) . . ?
O10 Dy1 O14 72.79(9) . . ?
O2 Dy1 O14 78.32(8) . . ?
O7 Dy1 O14 139.99(9) 2_666 . ?
O1 Dy1 O3 72.26(7) . 2_666 ?
O5 Dy1 O3 76.40(7) . 2_666 ?
O10 Dy1 O3 141.89(7) . 2_666 ?
O2 Dy1 O3 69.26(7) . 2_666 ?
O7 Dy1 O3 77.14(7) 2_666 2_666 ?
O14 Dy1 O3 141.47(8) . 2_666 ?
O1 Dy1 O15 147.48(8) . . ?
O5 Dy1 O15 68.11(8) . . ?
O10 Dy1 O15 79.92(9) . . ?
O2 Dy1 O15 141.34(8) . . ?
O7 Dy1 O15 73.65(8) 2_666 . ?
O14 Dy1 O15 76.48(9) . . ?
O3 Dy1 O15 117.60(9) 2_666 . ?
O1 Dy2 O12 115.64(8) 2_666 . ?
O1 Dy2 O4 139.50(8) 2_666 . ?
O12 Dy2 O4 78.42(9) . . ?
O1 Dy2 O9 80.82(7) 2_666 2_666 ?
O12 Dy2 O9 143.05(8) . 2_666 ?
O4 Dy2 O9 111.33(8) . 2_666 ?
O1 Dy2 O11 76.61(7) 2_666 2_666 ?
O12 Dy2 O11 77.21(8) . 2_666 ?
O4 Dy2 O11 143.17(7) . 2_666 ?
O9 Dy2 O11 74.99(8) 2_666 2_666 ?
O1 Dy2 O16 145.76(9) 2_666 . ?
O12 Dy2 O16 80.71(11) . . ?
O4 Dy2 O16 70.68(9) . . ?
O9 Dy2 O16 70.28(10) 2_666 . ?
O11 Dy2 O16 78.44(9) 2_666 . ?
O1 Dy2 O2 69.91(7) 2_666 . ?
O12 Dy2 O2 78.64(8) . . ?
O4 Dy2 O2 76.85(7) . . ?
O9 Dy2 O2 137.70(7) 2_666 . ?
O11 Dy2 O2 124.03(8) 2_666 . ?
O16 Dy2 O2 144.32(9) . . ?
O1 Dy2 O3 71.16(7) 2_666 2_666 ?
O12 Dy2 O3 140.90(7) . 2_666 ?
O4 Dy2 O3 75.26(7) . 2_666 ?
O9 Dy2 O3 74.50(7) 2_666 2_666 ?
O11 Dy2 O3 138.38(7) 2_666 2_666 ?
O16 Dy2 O3 116.13(9) . 2_666 ?
O2 Dy2 O3 67.61(7) . 2_666 ?
O2 Fe1 O1 85.67(9) . . ?
O2 Fe1 O1 85.94(9) . 2_666 ?
O1 Fe1 O1 82.33(9) . 2_666 ?
O2 Fe1 O3 172.12(9) . . ?
O1 Fe1 O3 88.23(9) . . ?
O1 Fe1 O3 88.31(8) 2_666 . ?
O2 Fe1 O8 92.73(9) . . ?
O1 Fe1 O8 94.33(9) . . ?
O1 Fe1 O8 176.48(9) 2_666 . ?
O3 Fe1 O8 92.70(9) . . ?
O2 Fe1 O6 91.08(9) . . ?
O1 Fe1 O6 174.06(9) . . ?
O1 Fe1 O6 92.49(9) 2_666 . ?
O3 Fe1 O6 94.55(9) . . ?
O8 Fe1 O6 90.79(9) . . ?
Fe1 O1 Fe1 97.67(9) . 2_666 ?
Fe1 O1 Dy1 101.15(8) . . ?
Fe1 O1 Dy1 100.47(9) 2_666 . ?
Fe1 O1 Dy2 101.57(9) . 2_666 ?
Fe1 O1 Dy2 101.92(8) 2_666 2_666 ?
Dy1 O1 Dy2 145.43(10) . 2_666 ?
Fe1 O2 Dy1 98.65(8) . . ?
Fe1 O2 Dy2 97.85(8) . . ?
Dy1 O2 Dy2 112.26(8) . . ?
Fe1 O2 H2 118(3) . . ?
Dy1 O2 H2 124(3) . . ?
Dy2 O2 H2 104(3) . . ?
C3A O3 Fe1 121.79(19) . . ?
C3A O3 Dy1 114.5(2) . 2_666 ?
Fe1 O3 Dy1 95.95(8) . 2_666 ?
C3A O3 Dy2 116.66(19) . 2_666 ?
Fe1 O3 Dy2 95.72(8) . 2_666 ?
Dy1 O3 Dy2 109.10(8) 2_666 2_666 ?
Fe1 O3 H3 117.4 . . ?
Dy1 O3 H3 117.4 2_666 . ?
Dy2 O3 H3 117.4 2_666 . ?
O3 C3A H3A 109.5 . . ?
O3 C3A H3B 109.5 . . ?
H3A C3A H3B 109.5 . . ?
O3 C3A H3C 109.5 . . ?
H3A C3A H3C 109.5 . . ?
H3B C3A H3C 109.5 . . ?
C4 O4 Dy2 137.9(2) . . ?
C4 O5 Dy1 137.1(2) . . ?
O5 C4 O4 127.3(3) . . ?
O5 C4 C5 114.6(3) . . ?
O4 C4 C5 118.0(3) . . ?
C6 C5 C4 111.6(3) . . ?
C6 C5 H5A 109.3 . . ?
C4 C5 H5A 109.3 . . ?
C6 C5 H5B 109.3 . . ?
C4 C5 H5B 109.3 . . ?
H5A C5 H5B 108.0 . . ?
N1 C6 C5 178.8(6) . . ?
C7 O6 Fe1 123.96(19) . . ?
C7 O7 Dy1 131.9(2) . 2_666 ?
O7 C7 O6 126.4(3) . . ?
O7 C7 C8 119.5(3) . . ?
O6 C7 C8 114.1(3) . . ?
C9 C8 C7 113.4(3) . . ?
C9 C8 H8A 108.9 . . ?
C7 C8 H8A 108.9 . . ?
C9 C8 H8B 108.9 . . ?
C7 C8 H8B 108.9 . . ?
H8A C8 H8B 107.7 . . ?
N2 C9 C8 179.5(5) . . ?
C10 O8 Fe1 125.12(19) . . ?
C10 O9 Dy2 134.7(2) . 2_666 ?
O9 C10 O8 126.6(3) . . ?
O9 C10 C11 118.2(3) . . ?
O8 C10 C11 115.1(3) . . ?
C12 C11 C10 112.8(3) . . ?
C12 C11 H11A 109.0 . . ?
C10 C11 H11A 109.0 . . ?
C12 C11 H11B 109.0 . . ?
C10 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
N3 C12 C11 179.1(5) . . ?
C13 O10 Dy1 134.5(2) . . ?
C13 O11 Dy2 130.9(2) . 2_666 ?
O11 C13 O10 128.1(3) . . ?
O11 C13 C14 115.8(3) . . ?
O10 C13 C14 116.1(3) . . ?
C15 C14 C13 113.2(3) . . ?
C15 C14 H14A 108.9 . . ?
C13 C14 H14A 108.9 . . ?
C15 C14 H14B 108.9 . . ?
C13 C14 H14B 108.9 . . ?
H14A C14 H14B 107.7 . . ?
N4 C15 C14 178.7(4) . . ?
C16 O12 Dy2 129.9(2) . . ?
O13 C16 O12 126.6(3) . . ?
O13 C16 C17 118.3(3) . . ?
O12 C16 C17 115.1(3) . . ?
C18A C17 C16 115.9(5) . . ?
C16 C17 C18B 109.4(5) . . ?
C18A C17 H17A 108.3 . . ?
C16 C17 H17A 108.3 . . ?
C18A C17 H17B 108.3 . . ?
C16 C17 H17B 108.3 . . ?
H17A C17 H17B 107.4 . . ?
C16 C17 H17C 109.9 . . ?
C18B C17 H17C 109.1 . . ?
C16 C17 H17D 109.8 . . ?
C18B C17 H17D 110.3 . . ?
H17C C17 H17D 108.3 . . ?
N5A C18A C17 174.5(11) . . ?
N5B C18B C17 175.4(14) . . ?
C19A O14 Dy1 136.5(4) . . ?
C19A O14 H14 93(3) . . ?
Dy1 O14 H14 129(3) . . ?
O14 C19A H19A 109.5 . . ?
O14 C19A H19B 109.5 . . ?
H19A C19A H19B 109.5 . . ?
O14 C19A H19C 109.5 . . ?
H19A C19A H19C 109.5 . . ?
H19B C19A H19C 109.5 . . ?
C20A O15 Dy1 129.0(4) . . ?
C20B O15 Dy1 134.4(4) . . ?
C20A O15 H15 106(3) . . ?
C20B O15 H15 115(3) . . ?
Dy1 O15 H15 108(3) . . ?
O15 C20A H20A 109.5 . . ?
O15 C20A H20B 109.5 . . ?
H20A C20A H20B 109.5 . . ?
O15 C20A H20C 109.5 . . ?
H20A C20A H20C 109.5 . . ?
H20B C20A H20C 109.5 . . ?
O15 C20B H20D 109.5 . . ?
O15 C20B H20E 109.5 . . ?
H20D C20B H20E 109.5 . . ?
O15 C20B H20F 109.5 . . ?
H20D C20B H20F 109.5 . . ?
H20E C20B H20F 109.5 . . ?
C21A O16 Dy2 142.0(4) . . ?
C21B O16 Dy2 137.3(5) . . ?
C21A O16 H16A 109.0 . . ?
Dy2 O16 H16A 109.0 . . ?
C21B O16 H16B 111.3 . . ?
Dy2 O16 H16B 111.3 . . ?
O16 C21A H21A 109.5 . . ?
O16 C21A H21B 109.5 . . ?
H21A C21A H21B 109.5 . . ?
O16 C21A H21C 109.5 . . ?
H21A C21A H21C 109.5 . . ?
H21B C21A H21C 109.5 . . ?
O16 C21B H21D 109.5 . . ?
O16 C21B H21E 109.5 . . ?
H21D C21B H21E 109.5 . . ?
O16 C21B H21F 109.5 . . ?
H21D C21B H21F 109.5 . . ?
H21E C21B H21F 109.5 . . ?

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
O2 H2 O13 0.81(3) 1.89(3) 2.666(3) 161(4) .
O3 H3 O33B 1.00 1.66 2.58(4) 151.9 .
O14 H14 O31A 0.91(3) 1.74(3) 2.622(5) 162(4) .
O14 H14 O31B 0.91(3) 1.93(4) 2.800(11) 158(4) .
O15 H15 N4 0.84(3) 2.11(3) 2.919(4) 160(4) 2_556
O16 H16B O32B 0.95 1.80 2.607(14) 140.8 .
O31A H31A O13 0.84 1.83 2.653(5) 164.3 .

_diffrn_measured_fraction_theta_max 0.910
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.719
_refine_diff_density_min         -1.466
_refine_diff_density_rms         0.140
