# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2014

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#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
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#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
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data_a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '[Y(3,5-Dnbz)3(H2O)2]H2O,12oct27d'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H15 N6 O21 Y'
_chemical_formula_weight         776.30

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'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.2897(10)
_cell_length_b                   11.5182(13)
_cell_length_c                   13.7146(15)
_cell_angle_alpha                107.747(2)
_cell_angle_beta                 90.548(2)
_cell_angle_gamma                93.464(2)
_cell_volume                     1394.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2800
_cell_measurement_theta_min      2.66
_cell_measurement_theta_max      24.57

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.849
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             780
_exptl_absorpt_coefficient_mu    2.202
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.6430
_exptl_absorpt_correction_T_max  0.6672
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_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 P4'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10156
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0539
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.56
_diffrn_reflns_theta_max         27.78
_reflns_number_total             6544
_reflns_number_gt                5275
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker XSCANS'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0356P)²+0.1125P] 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     SHELXL
_refine_ls_extinction_coef       0.0008(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         6544
_refine_ls_number_parameters     467
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0380
_refine_ls_wR_factor_ref         0.0821
_refine_ls_wR_factor_gt          0.0755
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.030
_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
Y1 Y 0.26945(2) -0.01146(2) 0.008392(18) 0.02050(8) Uani 1 1 d . . .
C1 C 0.0307(2) 0.1622(2) 0.14773(18) 0.0223(5) Uani 1 1 d . . .
C3 C -0.1416(3) 0.3014(2) 0.25719(19) 0.0279(6) Uani 1 1 d . . .
H3A H -0.2177 0.2460 0.2260 0.033 Uiso 1 1 calc R . .
C8 C 0.5360(2) 0.2325(2) 0.04928(19) 0.0242(5) Uani 1 1 d . . .
C2 C 0.0000(2) 0.2761(2) 0.23137(19) 0.0238(5) Uani 1 1 d . . .
C9 C 0.4892(3) 0.3611(2) 0.08403(18) 0.0239(5) Uani 1 1 d . . .
C10 C 0.3433(3) 0.3823(2) 0.0825(2) 0.0278(6) Uani 1 1 d . . .
H10A H 0.2737 0.3176 0.0611 0.033 Uiso 1 1 calc R . .
C4 C -0.1669(3) 0.4100(2) 0.3297(2) 0.0316(6) Uani 1 1 d . . .
C6 C 0.0799(3) 0.4692(2) 0.3487(2) 0.0301(6) Uani 1 1 d . . .
C7 C 0.1122(3) 0.3597(2) 0.27902(19) 0.0274(6) Uani 1 1 d . . .
H7A H 0.2075 0.3424 0.2644 0.033 Uiso 1 1 calc R . .
C5 C -0.0586(3) 0.4971(2) 0.3760(2) 0.0347(6) Uani 1 1 d . . .
H5A H -0.0783 0.5711 0.4233 0.042 Uiso 1 1 calc R . .
C14 C 0.5917(3) 0.4586(2) 0.11701(19) 0.0271(6) Uani 1 1 d . . .
H14A H 0.6894 0.4452 0.1176 0.033 Uiso 1 1 calc R . .
C13 C 0.5458(3) 0.5759(2) 0.14900(19) 0.0284(6) Uani 1 1 d . . .
C11 C 0.3044(3) 0.5019(2) 0.1137(2) 0.0294(6) Uani 1 1 d . . .
C12 C 0.4028(3) 0.6006(2) 0.1484(2) 0.0321(6) Uani 1 1 d . . .
H12A H 0.3741 0.6802 0.1703 0.039 Uiso 1 1 calc R . .
C15 C 0.4781(3) -0.0337(2) -0.19717(19) 0.0244(5) Uani 1 1 d . . .
C16 C 0.4855(3) -0.0792(2) -0.31185(19) 0.0268(6) Uani 1 1 d . . .
C21 C 0.6157(3) -0.1206(2) -0.3543(2) 0.0311(6) Uani 1 1 d . . .
H21A H 0.6954 -0.1187 -0.3122 0.037 Uiso 1 1 calc R . .
C17 C 0.3683(3) -0.0812(2) -0.3756(2) 0.0297(6) Uani 1 1 d . . .
H17A H 0.2807 -0.0538 -0.3486 0.036 Uiso 1 1 calc R . .
C18 C 0.3841(3) -0.1247(2) -0.4805(2) 0.0316(6) Uani 1 1 d . . .
C20 C 0.6250(3) -0.1644(2) -0.4593(2) 0.0344(6) Uani 1 1 d . . .
C19 C 0.5104(3) -0.1676(2) -0.5252(2) 0.0357(6) Uani 1 1 d . . .
H19A H 0.5181 -0.1972 -0.5959 0.043 Uiso 1 1 calc R . .
N1 N -0.3181(3) 0.4350(2) 0.3592(2) 0.0462(7) Uani 1 1 d . . .
N2 N 0.1982(3) 0.5610(2) 0.39462(19) 0.0407(6) Uani 1 1 d . . .
N3 N 0.1497(2) 0.5243(2) 0.1099(2) 0.0403(6) Uani 1 1 d . . .
N4 N 0.6558(3) 0.6792(2) 0.18125(19) 0.0381(6) Uani 1 1 d . . .
N5 N 0.2628(3) -0.1209(2) -0.54961(19) 0.0414(6) Uani 1 1 d . . .
N6 N 0.7641(3) -0.2063(2) -0.5034(2) 0.0474(7) Uani 1 1 d . . .
O2 O -0.07172(17) 0.10738(16) 0.08914(14) 0.0315(4) Uani 1 1 d . . .
O1 O 0.15858(17) 0.13140(16) 0.14006(14) 0.0313(4) Uani 1 1 d . . .
O13 O 0.3162(2) 0.5480(2) 0.35556(19) 0.0602(7) Uani 1 1 d . . .
O10 O -0.4133(2) 0.3595(2) 0.31567(19) 0.0589(6) Uani 1 1 d . . .
O12 O 0.1711(2) 0.6467(2) 0.46931(17) 0.0567(6) Uani 1 1 d . . .
O7 O 0.17128(19) 0.13434(17) -0.06625(15) 0.0329(4) Uani 1 1 d D . .
O4 O 0.66838(17) 0.21805(15) 0.03791(14) 0.0310(4) Uani 1 1 d . . .
O3 O 0.44131(18) 0.14639(16) 0.03488(14) 0.0304(4) Uani 1 1 d . . .
O8 O 0.12591(19) -0.12707(18) 0.10561(16) 0.0337(4) Uani 1 1 d D . .
O11 O -0.3371(3) 0.5286(2) 0.4270(2) 0.0910(10) Uani 1 1 d . . .
O9 O -0.0193(4) -0.0661(5) 0.2890(3) 0.1145(14) Uani 1 1 d D . .
O5 O 0.35810(17) -0.04434(16) -0.15861(13) 0.0286(4) Uani 1 1 d . . .
O14 O 0.0630(2) 0.4370(2) 0.0800(2) 0.0546(6) Uani 1 1 d . . .
O17 O 0.7815(2) 0.6565(2) 0.17977(19) 0.0578(6) Uani 1 1 d . . .
O16 O 0.6144(2) 0.78262(18) 0.20659(19) 0.0561(6) Uani 1 1 d . . .
O15 O 0.1182(2) 0.6305(2) 0.1381(2) 0.0759(8) Uani 1 1 d . . .
O18 O 0.1564(2) -0.0703(2) -0.51155(18) 0.0583(6) Uani 1 1 d . . .
O21 O 0.8587(3) -0.2175(3) -0.44586(19) 0.0679(7) Uani 1 1 d . . .
O19 O 0.2766(3) -0.1657(2) -0.64136(17) 0.0644(7) Uani 1 1 d . . .
O20 O 0.7771(3) -0.2284(3) -0.59474(18) 0.0735(8) Uani 1 1 d . . .
O6 O 0.59503(17) 0.00985(17) -0.14977(13) 0.0300(4) Uani 1 1 d . . .
H72 H 0.075(2) 0.144(3) -0.070(3) 0.087(13) Uiso 1 1 d D . .
H81 H 0.157(4) -0.2034(19) 0.095(3) 0.076(12) Uiso 1 1 d D . .
H71 H 0.212(3) 0.131(4) -0.1283(19) 0.093(15) Uiso 1 1 d D . .
H82 H 0.109(5) -0.094(3) 0.1765(16) 0.122(18) Uiso 1 1 d D . .
H91 H 0.034(3) 0.006(2) 0.309(2) 0.034(10) Uiso 1 1 d D . .
H92 H -0.024(11) -0.097(7) 0.347(4) 0.45(8) 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
Y1 O2 2.2784(16) 2 ?
Y1 O3 2.2852(16) . ?
Y1 O6 2.2964(17) 2_655 ?
Y1 O1 2.3363(17) . ?
Y1 O5 2.3690(17) . ?
Y1 O4 2.3772(17) 2_655 ?
Y1 O7 2.4321(18) . ?
Y1 O8 2.4962(19) . ?
C1 O2 1.246(3) . ?
C1 O1 1.256(3) . ?
C1 C2 1.501(3) . ?
C3 C4 1.375(4) . ?
C3 C2 1.390(3) . ?
C3 H3A 0.9300 . ?
C8 O3 1.253(3) . ?
C8 O4 1.256(3) . ?
C8 C9 1.504(3) . ?
C2 C7 1.386(3) . ?
C9 C14 1.387(3) . ?
C9 C10 1.392(3) . ?
C10 C11 1.384(4) . ?
C10 H10A 0.9300 . ?
C4 C5 1.378(4) . ?
C4 N1 1.486(3) . ?
C6 C5 1.373(4) . ?
C6 C7 1.382(3) . ?
C6 N2 1.471(3) . ?
C7 H7A 0.9300 . ?
C5 H5A 0.9300 . ?
C14 C13 1.383(3) . ?
C14 H14A 0.9300 . ?
C13 C12 1.375(4) . ?
C13 N4 1.476(3) . ?
C11 C12 1.375(4) . ?
C11 N3 1.478(3) . ?
C12 H12A 0.9300 . ?
C15 O5 1.254(3) . ?
C15 O6 1.255(3) . ?
C15 C16 1.502(3) . ?
C16 C17 1.385(3) . ?
C16 C21 1.393(3) . ?
C21 C20 1.378(4) . ?
C21 H21A 0.9300 . ?
C17 C18 1.384(4) . ?
C17 H17A 0.9300 . ?
C18 C19 1.377(4) . ?
C18 N5 1.477(4) . ?
C20 C19 1.382(4) . ?
C20 N6 1.477(4) . ?
C19 H19A 0.9300 . ?
N1 O11 1.213(3) . ?
N1 O10 1.214(3) . ?
N2 O13 1.222(3) . ?
N2 O12 1.227(3) . ?
N3 O14 1.214(3) . ?
N3 O15 1.219(3) . ?
N4 O17 1.211(3) . ?
N4 O16 1.222(3) . ?
N5 O19 1.217(3) . ?
N5 O18 1.218(3) . ?
N6 O20 1.209(3) . ?
N6 O21 1.213(3) . ?
O2 Y1 2.2783(16) 2 ?
O7 H72 0.912(17) . ?
O7 H71 0.924(18) . ?
O4 Y1 2.3772(17) 2_655 ?
O8 H81 0.913(17) . ?
O8 H82 0.949(18) . ?
O9 H91 0.902(16) . ?
O9 H92 0.97(2) . ?
O6 Y1 2.2964(17) 2_655 ?

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 Y1 O3 144.31(7) 2 . ?
O2 Y1 O6 142.12(6) 2 2_655 ?
O3 Y1 O6 73.42(6) . 2_655 ?
O2 Y1 O1 100.06(6) 2 . ?
O3 Y1 O1 81.91(6) . . ?
O6 Y1 O1 77.89(6) 2_655 . ?
O2 Y1 O5 79.03(6) 2 . ?
O3 Y1 O5 78.45(6) . . ?
O6 Y1 O5 125.18(6) 2_655 . ?
O1 Y1 O5 142.52(6) . . ?
O2 Y1 O4 79.31(6) 2 2_655 ?
O3 Y1 O4 121.59(6) . 2_655 ?
O6 Y1 O4 79.03(6) 2_655 2_655 ?
O1 Y1 O4 139.94(6) . 2_655 ?
O5 Y1 O4 77.22(6) . 2_655 ?
O2 Y1 O7 72.95(6) 2 . ?
O3 Y1 O7 73.66(6) . . ?
O6 Y1 O7 138.55(6) 2_655 . ?
O1 Y1 O7 73.18(7) . . ?
O5 Y1 O7 70.79(6) . . ?
O4 Y1 O7 140.79(7) 2_655 . ?
O2 Y1 O8 71.41(7) 2 . ?
O3 Y1 O8 140.44(7) . . ?
O6 Y1 O8 71.98(6) 2_655 . ?
O1 Y1 O8 72.64(7) . . ?
O5 Y1 O8 138.48(6) . . ?
O4 Y1 O8 69.27(6) 2_655 . ?
O7 Y1 O8 124.32(6) . . ?
O2 C1 O1 124.9(2) . . ?
O2 C1 C2 117.5(2) . . ?
O1 C1 C2 117.6(2) . . ?
C4 C3 C2 118.7(2) . . ?
C4 C3 H3A 120.6 . . ?
C2 C3 H3A 120.6 . . ?
O3 C8 O4 123.9(2) . . ?
O3 C8 C9 118.3(2) . . ?
O4 C8 C9 117.9(2) . . ?
C7 C2 C3 119.8(2) . . ?
C7 C2 C1 120.0(2) . . ?
C3 C2 C1 120.1(2) . . ?
C14 C9 C10 120.1(2) . . ?
C14 C9 C8 119.8(2) . . ?
C10 C9 C8 120.1(2) . . ?
C11 C10 C9 118.4(2) . . ?
C11 C10 H10A 120.8 . . ?
C9 C10 H10A 120.8 . . ?
C3 C4 C5 123.0(2) . . ?
C3 C4 N1 118.5(2) . . ?
C5 C4 N1 118.5(2) . . ?
C5 C6 C7 122.8(2) . . ?
C5 C6 N2 118.2(2) . . ?
C7 C6 N2 118.9(2) . . ?
C6 C7 C2 118.8(2) . . ?
C6 C7 H7A 120.6 . . ?
C2 C7 H7A 120.6 . . ?
C6 C5 C4 116.6(2) . . ?
C6 C5 H5A 121.7 . . ?
C4 C5 H5A 121.7 . . ?
C13 C14 C9 118.7(2) . . ?
C13 C14 H14A 120.6 . . ?
C9 C14 H14A 120.6 . . ?
C12 C13 C14 122.9(2) . . ?
C12 C13 N4 118.7(2) . . ?
C14 C13 N4 118.3(2) . . ?
C12 C11 C10 123.0(2) . . ?
C12 C11 N3 118.6(2) . . ?
C10 C11 N3 118.4(2) . . ?
C13 C12 C11 116.8(2) . . ?
C13 C12 H12A 121.6 . . ?
C11 C12 H12A 121.6 . . ?
O5 C15 O6 126.8(2) . . ?
O5 C15 C16 117.5(2) . . ?
O6 C15 C16 115.7(2) . . ?
C17 C16 C21 119.6(2) . . ?
C17 C16 C15 122.3(2) . . ?
C21 C16 C15 118.1(2) . . ?
C20 C21 C16 119.3(2) . . ?
C20 C21 H21A 120.3 . . ?
C16 C21 H21A 120.3 . . ?
C18 C17 C16 118.6(2) . . ?
C18 C17 H17A 120.7 . . ?
C16 C17 H17A 120.7 . . ?
C19 C18 C17 123.4(2) . . ?
C19 C18 N5 117.2(2) . . ?
C17 C18 N5 119.3(2) . . ?
C21 C20 C19 122.6(3) . . ?
C21 C20 N6 118.8(3) . . ?
C19 C20 N6 118.5(3) . . ?
C18 C19 C20 116.4(3) . . ?
C18 C19 H19A 121.8 . . ?
C20 C19 H19A 121.8 . . ?
O11 N1 O10 124.7(3) . . ?
O11 N1 C4 117.3(3) . . ?
O10 N1 C4 118.0(2) . . ?
O13 N2 O12 124.3(2) . . ?
O13 N2 C6 118.2(2) . . ?
O12 N2 C6 117.5(2) . . ?
O14 N3 O15 124.5(2) . . ?
O14 N3 C11 118.4(2) . . ?
O15 N3 C11 117.1(3) . . ?
O17 N4 O16 123.9(2) . . ?
O17 N4 C13 118.2(2) . . ?
O16 N4 C13 117.9(2) . . ?
O19 N5 O18 123.9(3) . . ?
O19 N5 C18 118.0(3) . . ?
O18 N5 C18 118.0(2) . . ?
O20 N6 O21 123.7(3) . . ?
O20 N6 C20 118.2(3) . . ?
O21 N6 C20 118.1(3) . . ?
C1 O2 Y1 175.95(16) . 2 ?
C1 O1 Y1 130.62(15) . . ?
Y1 O7 H72 123(2) . . ?
Y1 O7 H71 112(2) . . ?
H72 O7 H71 110(2) . . ?
C8 O4 Y1 114.79(15) . 2_655 ?
C8 O3 Y1 179.70(19) . . ?
Y1 O8 H81 112(2) . . ?
Y1 O8 H82 122(3) . . ?
H81 O8 H82 108(2) . . ?
H91 O9 H92 107(3) . . ?
C15 O5 Y1 136.53(16) . . ?
C15 O6 Y1 141.95(16) . 2_655 ?

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
O7 H72 O8 0.912(17) 1.91(2) 2.799(3) 165(3) 2
O7 H71 O16 0.924(18) 2.29(3) 3.090(3) 145(3) 2_665
O8 H82 O9 0.949(18) 1.92(3) 2.782(4) 150(4) .
O8 H81 O15 0.913(17) 2.18(3) 2.956(3) 143(3) 1_545
O9 H92 O18 0.97(2) 2.48(6) 3.187(4) 129(6) 1_556
O9 H92 O20 0.97(2) 2.60(6) 3.326(5) 132(6) 1_456

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.072
_exptl_crystal_recrystallization_method 'Hydrothermal method'
_database_code_depnum_ccdc_archive 'CCDC 1015887'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            '[Dy(3,5-Dnbz)3(H2O)2]H2O,12jul26c'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H15 Dy N6 O21'
_chemical_formula_weight         849.89

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.2791(11)
_cell_length_b                   11.4893(14)
_cell_length_c                   13.7207(16)
_cell_angle_alpha                107.5990(10)
_cell_angle_beta                 90.4890(10)
_cell_angle_gamma                93.625(2)
_cell_volume                     1390.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5542
_cell_measurement_theta_min      2.66
_cell_measurement_theta_max      29.76

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.029
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             834
_exptl_absorpt_coefficient_mu    2.797
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.5415
_exptl_absorpt_correction_T_max  0.8072
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_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 P4'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9789
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0545
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.03
_diffrn_reflns_theta_max         30.11
_reflns_number_total             7107
_reflns_number_gt                6421
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker XSCANS'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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)+(0.0461P)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     SHELXL
_refine_ls_extinction_coef       0.0010(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         7107
_refine_ls_number_parameters     467
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0315
_refine_ls_wR_factor_ref         0.0855
_refine_ls_wR_factor_gt          0.0825
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.009
_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 0.270092(14) -0.012101(11) 0.008576(10) 0.02006(6) Uani 1 1 d . . .
C1 C 0.0318(3) 0.1627(3) 0.1479(2) 0.0217(6) Uani 1 1 d . . .
C3 C -0.1406(4) 0.3010(3) 0.2573(3) 0.0280(7) Uani 1 1 d . . .
H3A H -0.2166 0.2449 0.2264 0.034 Uiso 1 1 calc R . .
C8 C 0.5379(4) 0.2334(3) 0.0497(2) 0.0236(6) Uani 1 1 d . . .
C2 C 0.0001(4) 0.2762(3) 0.2315(2) 0.0223(6) Uani 1 1 d . . .
C9 C 0.4896(4) 0.3614(3) 0.0843(2) 0.0231(6) Uani 1 1 d . . .
C10 C 0.3440(4) 0.3821(3) 0.0819(2) 0.0265(7) Uani 1 1 d . . .
H10A H 0.2747 0.3170 0.0593 0.032 Uiso 1 1 calc R . .
C4 C -0.1672(4) 0.4102(3) 0.3295(3) 0.0312(7) Uani 1 1 d . . .
C6 C 0.0803(4) 0.4689(3) 0.3489(3) 0.0294(7) Uani 1 1 d . . .
C7 C 0.1142(4) 0.3595(3) 0.2794(2) 0.0264(7) Uani 1 1 d . . .
H7A H 0.2096 0.3422 0.2651 0.032 Uiso 1 1 calc R . .
C5 C -0.0589(4) 0.4974(3) 0.3760(3) 0.0342(8) Uani 1 1 d . . .
H5A H -0.0785 0.5714 0.4232 0.041 Uiso 1 1 calc R . .
C14 C 0.5922(4) 0.4598(3) 0.1174(3) 0.0258(7) Uani 1 1 d . . .
H14A H 0.6902 0.4472 0.1183 0.031 Uiso 1 1 calc R . .
C13 C 0.5448(4) 0.5766(3) 0.1490(3) 0.0288(7) Uani 1 1 d . . .
C11 C 0.3041(4) 0.5011(3) 0.1137(3) 0.0284(7) Uani 1 1 d . . .
C12 C 0.4024(4) 0.6013(3) 0.1490(3) 0.0305(7) Uani 1 1 d . . .
H12A H 0.3734 0.6809 0.1714 0.037 Uiso 1 1 calc R . .
C15 C 0.4776(4) -0.0336(3) -0.1976(2) 0.0237(6) Uani 1 1 d . . .
C16 C 0.4860(4) -0.0794(3) -0.3128(2) 0.0246(6) Uani 1 1 d . . .
C21 C 0.6158(4) -0.1210(3) -0.3547(3) 0.0297(7) Uani 1 1 d . . .
H21A H 0.6955 -0.1195 -0.3126 0.036 Uiso 1 1 calc R . .
C17 C 0.3679(4) -0.0820(3) -0.3758(3) 0.0287(7) Uani 1 1 d . . .
H17A H 0.2800 -0.0557 -0.3485 0.034 Uiso 1 1 calc R . .
C18 C 0.3841(4) -0.1251(3) -0.4813(3) 0.0307(7) Uani 1 1 d . . .
C20 C 0.6247(4) -0.1646(3) -0.4592(3) 0.0329(8) Uani 1 1 d . . .
C19 C 0.5107(5) -0.1682(3) -0.5249(3) 0.0356(8) Uani 1 1 d . . .
H19A H 0.5188 -0.1984 -0.5955 0.043 Uiso 1 1 calc R . .
H71 H 0.201(5) 0.134(5) -0.132(2) 0.062(16) Uiso 1 1 d D . .
H72 H 0.071(2) 0.136(5) -0.066(3) 0.071(17) Uiso 1 1 d D . .
H82 H 0.091(7) -0.104(5) 0.175(2) 0.10(2) Uiso 1 1 d D . .
H81 H 0.160(5) -0.206(2) 0.096(3) 0.052(14) Uiso 1 1 d D . .
H92 H -0.024(10) -0.094(6) 0.347(4) 0.19(5) Uiso 1 1 d D . .
H91 H 0.039(5) 0.008(3) 0.309(3) 0.034(14) Uiso 1 1 d D . .
N1 N -0.3176(4) 0.4334(3) 0.3587(3) 0.0450(9) Uani 1 1 d . . .
N2 N 0.1993(4) 0.5611(3) 0.3947(3) 0.0399(8) Uani 1 1 d . . .
N3 N 0.1501(4) 0.5229(3) 0.1097(3) 0.0397(8) Uani 1 1 d . . .
N4 N 0.6548(4) 0.6800(3) 0.1820(2) 0.0362(7) Uani 1 1 d . . .
N5 N 0.2629(4) -0.1211(3) -0.5495(3) 0.0399(8) Uani 1 1 d . . .
N6 N 0.7641(4) -0.2069(3) -0.5032(3) 0.0462(9) Uani 1 1 d . . .
O2 O -0.0702(3) 0.1075(2) 0.08923(19) 0.0315(5) Uani 1 1 d . . .
O1 O 0.1594(3) 0.1329(2) 0.14030(19) 0.0295(5) Uani 1 1 d . . .
O13 O 0.3170(4) 0.5481(3) 0.3559(3) 0.0582(9) Uani 1 1 d . . .
O10 O -0.4138(3) 0.3593(3) 0.3140(3) 0.0569(9) Uani 1 1 d . . .
O12 O 0.1711(4) 0.6463(3) 0.4690(2) 0.0554(9) Uani 1 1 d . . .
O7 O 0.1725(3) 0.1348(2) -0.0661(2) 0.0309(5) Uani 1 1 d D . .
O4 O 0.6711(3) 0.2208(2) 0.03733(19) 0.0290(5) Uani 1 1 d . . .
O3 O 0.4450(3) 0.1461(2) 0.03431(19) 0.0300(5) Uani 1 1 d . . .
O8 O 0.1242(3) -0.1282(2) 0.1067(2) 0.0328(6) Uani 1 1 d D . .
O11 O -0.3382(4) 0.5274(4) 0.4265(4) 0.0879(16) Uani 1 1 d . . .
O9 O -0.0196(6) -0.0655(7) 0.2885(4) 0.112(2) Uani 1 1 d D . .
O5 O 0.3582(3) -0.0447(2) -0.15944(18) 0.0282(5) Uani 1 1 d . . .
O14 O 0.0636(3) 0.4355(3) 0.0789(3) 0.0538(8) Uani 1 1 d . . .
O17 O 0.7815(4) 0.6583(3) 0.1807(3) 0.0555(9) Uani 1 1 d . . .
O16 O 0.6129(4) 0.7834(2) 0.2077(3) 0.0539(9) Uani 1 1 d . . .
O15 O 0.1171(4) 0.6287(3) 0.1394(4) 0.0730(12) Uani 1 1 d . . .
O18 O 0.1568(4) -0.0710(3) -0.5121(2) 0.0567(9) Uani 1 1 d . . .
O21 O 0.8579(4) -0.2176(4) -0.4460(3) 0.0679(11) Uani 1 1 d . . .
O19 O 0.2770(4) -0.1659(4) -0.6413(2) 0.0627(10) Uani 1 1 d . . .
O20 O 0.7783(5) -0.2280(4) -0.5939(3) 0.0714(12) Uani 1 1 d . . .
O6 O 0.5947(3) 0.0103(2) -0.15134(18) 0.0289(5) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O2 2.292(2) 2 ?
Dy1 O3 2.301(2) . ?
Dy1 O6 2.311(2) 2_655 ?
Dy1 O1 2.350(2) . ?
Dy1 O5 2.382(2) . ?
Dy1 O4 2.387(2) 2_655 ?
Dy1 O7 2.438(3) . ?
Dy1 O8 2.512(3) . ?
C1 O2 1.244(4) . ?
C1 O1 1.250(4) . ?
C1 C2 1.501(4) . ?
C3 C2 1.380(5) . ?
C3 C4 1.382(4) . ?
C3 H3A 0.9300 . ?
C8 O3 1.246(4) . ?
C8 O4 1.260(4) . ?
C8 C9 1.501(4) . ?
C2 C7 1.396(4) . ?
C9 C10 1.389(5) . ?
C9 C14 1.391(5) . ?
C10 C11 1.379(5) . ?
C10 H10A 0.9300 . ?
C4 C5 1.376(5) . ?
C4 N1 1.474(5) . ?
C6 C5 1.379(5) . ?
C6 C7 1.385(5) . ?
C6 N2 1.474(5) . ?
C7 H7A 0.9300 . ?
C5 H5A 0.9300 . ?
C14 C13 1.381(5) . ?
C14 H14A 0.9300 . ?
C13 C12 1.369(5) . ?
C13 N4 1.473(5) . ?
C11 C12 1.384(5) . ?
C11 N3 1.470(5) . ?
C12 H12A 0.9300 . ?
C15 O5 1.245(4) . ?
C15 O6 1.251(4) . ?
C15 C16 1.512(4) . ?
C16 C17 1.383(5) . ?
C16 C21 1.388(5) . ?
C21 C20 1.374(5) . ?
C21 H21A 0.9300 . ?
C17 C18 1.394(5) . ?
C17 H17A 0.9300 . ?
C18 C19 1.374(6) . ?
C18 N5 1.469(5) . ?
C20 C19 1.375(6) . ?
C20 N6 1.480(5) . ?
C19 H19A 0.9300 . ?
N1 O10 1.215(5) . ?
N1 O11 1.220(5) . ?
N2 O13 1.216(5) . ?
N2 O12 1.225(4) . ?
N3 O14 1.211(5) . ?
N3 O15 1.220(4) . ?
N4 O17 1.217(5) . ?
N4 O16 1.222(4) . ?
N5 O18 1.210(5) . ?
N5 O19 1.220(5) . ?
N6 O20 1.203(5) . ?
N6 O21 1.204(5) . ?
O2 Dy1 2.292(2) 2 ?
O7 H71 0.941(19) . ?
O7 H72 0.940(19) . ?
O4 Dy1 2.387(2) 2_655 ?
O8 H82 0.950(19) . ?
O8 H81 0.942(19) . ?
O9 H92 0.96(2) . ?
O9 H91 0.942(18) . ?
O6 Dy1 2.311(2) 2_655 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Dy1 O3 144.12(9) 2 . ?
O2 Dy1 O6 142.20(9) 2 2_655 ?
O3 Dy1 O6 73.52(9) . 2_655 ?
O2 Dy1 O1 99.95(9) 2 . ?
O3 Dy1 O1 81.98(9) . . ?
O6 Dy1 O1 77.73(9) 2_655 . ?
O2 Dy1 O5 78.83(9) 2 . ?
O3 Dy1 O5 78.28(8) . . ?
O6 Dy1 O5 125.82(8) 2_655 . ?
O1 Dy1 O5 141.95(9) . . ?
O2 Dy1 O4 79.12(9) 2 2_655 ?
O3 Dy1 O4 121.90(8) . 2_655 ?
O6 Dy1 O4 79.42(9) 2_655 2_655 ?
O1 Dy1 O4 139.92(9) . 2_655 ?
O5 Dy1 O4 77.74(9) . 2_655 ?
O2 Dy1 O7 72.72(9) 2 . ?
O3 Dy1 O7 73.78(9) . . ?
O6 Dy1 O7 138.35(8) 2_655 . ?
O1 Dy1 O7 72.81(9) . . ?
O5 Dy1 O7 70.58(9) . . ?
O4 Dy1 O7 140.82(9) 2_655 . ?
O2 Dy1 O8 71.50(9) 2 . ?
O3 Dy1 O8 140.60(9) . . ?
O6 Dy1 O8 71.85(9) 2_655 . ?
O1 Dy1 O8 72.86(9) . . ?
O5 Dy1 O8 138.57(8) . . ?
O4 Dy1 O8 68.90(8) 2_655 . ?
O7 Dy1 O8 124.15(9) . . ?
O2 C1 O1 124.9(3) . . ?
O2 C1 C2 117.5(3) . . ?
O1 C1 C2 117.6(3) . . ?
C2 C3 C4 119.2(3) . . ?
C2 C3 H3A 120.4 . . ?
C4 C3 H3A 120.4 . . ?
O3 C8 O4 123.8(3) . . ?
O3 C8 C9 118.6(3) . . ?
O4 C8 C9 117.6(3) . . ?
C3 C2 C7 120.3(3) . . ?
C3 C2 C1 120.4(3) . . ?
C7 C2 C1 119.2(3) . . ?
C10 C9 C14 120.0(3) . . ?
C10 C9 C8 120.5(3) . . ?
C14 C9 C8 119.5(3) . . ?
C11 C10 C9 118.7(3) . . ?
C11 C10 H10A 120.6 . . ?
C9 C10 H10A 120.6 . . ?
C5 C4 C3 122.7(3) . . ?
C5 C4 N1 118.8(3) . . ?
C3 C4 N1 118.5(3) . . ?
C5 C6 C7 123.6(3) . . ?
C5 C6 N2 118.2(3) . . ?
C7 C6 N2 118.2(3) . . ?
C6 C7 C2 117.8(3) . . ?
C6 C7 H7A 121.1 . . ?
C2 C7 H7A 121.1 . . ?
C4 C5 C6 116.4(3) . . ?
C4 C5 H5A 121.8 . . ?
C6 C5 H5A 121.8 . . ?
C13 C14 C9 118.3(3) . . ?
C13 C14 H14A 120.9 . . ?
C9 C14 H14A 120.9 . . ?
C12 C13 C14 123.7(3) . . ?
C12 C13 N4 118.5(3) . . ?
C14 C13 N4 117.7(3) . . ?
C10 C11 C12 123.1(3) . . ?
C10 C11 N3 118.7(3) . . ?
C12 C11 N3 118.2(3) . . ?
C13 C12 C11 116.1(3) . . ?
C13 C12 H12A 121.9 . . ?
C11 C12 H12A 121.9 . . ?
O5 C15 O6 127.4(3) . . ?
O5 C15 C16 117.8(3) . . ?
O6 C15 C16 114.8(3) . . ?
C17 C16 C21 120.2(3) . . ?
C17 C16 C15 121.5(3) . . ?
C21 C16 C15 118.3(3) . . ?
C20 C21 C16 119.0(3) . . ?
C20 C21 H21A 120.5 . . ?
C16 C21 H21A 120.5 . . ?
C16 C17 C18 118.3(3) . . ?
C16 C17 H17A 120.9 . . ?
C18 C17 H17A 120.9 . . ?
C19 C18 C17 122.8(3) . . ?
C19 C18 N5 118.1(3) . . ?
C17 C18 N5 119.0(4) . . ?
C21 C20 C19 122.9(4) . . ?
C21 C20 N6 118.6(4) . . ?
C19 C20 N6 118.4(3) . . ?
C18 C19 C20 116.8(3) . . ?
C18 C19 H19A 121.6 . . ?
C20 C19 H19A 121.6 . . ?
O10 N1 O11 123.7(4) . . ?
O10 N1 C4 118.7(3) . . ?
O11 N1 C4 117.5(4) . . ?
O13 N2 O12 124.9(3) . . ?
O13 N2 C6 118.2(3) . . ?
O12 N2 C6 116.9(4) . . ?
O14 N3 O15 123.9(4) . . ?
O14 N3 C11 118.5(3) . . ?
O15 N3 C11 117.5(4) . . ?
O17 N4 O16 123.7(3) . . ?
O17 N4 C13 118.6(3) . . ?
O16 N4 C13 117.7(4) . . ?
O18 N5 O19 123.7(4) . . ?
O18 N5 C18 118.6(3) . . ?
O19 N5 C18 117.6(4) . . ?
O20 N6 O21 123.4(4) . . ?
O20 N6 C20 118.6(4) . . ?
O21 N6 C20 118.0(3) . . ?
C1 O2 Dy1 175.5(2) . 2 ?
C1 O1 Dy1 130.3(2) . . ?
Dy1 O7 H71 118(3) . . ?
Dy1 O7 H72 115(3) . . ?
H71 O7 H72 107(3) . . ?
C8 O4 Dy1 113.1(2) . 2_655 ?
C8 O3 Dy1 178.7(2) . . ?
Dy1 O8 H82 131(4) . . ?
Dy1 O8 H81 110(3) . . ?
H82 O8 H81 106(3) . . ?
H92 O9 H91 106(3) . . ?
C15 O5 Dy1 136.2(2) . . ?
C15 O6 Dy1 141.0(2) . 2_655 ?

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
O7 H72 O2 0.940(19) 2.60(4) 3.180(4) 120(3) .
O7 H71 O9 0.941(19) 2.61(4) 3.205(5) 121(3) 2
O7 H72 O8 0.940(19) 1.88(2) 2.796(4) 163(4) 2
O7 H71 O16 0.941(19) 2.32(3) 3.092(4) 139(4) 2_665
O8 H82 O9 0.950(19) 1.83(3) 2.760(6) 165(6) .
O8 H81 O15 0.942(19) 2.17(3) 2.956(4) 140(4) 1_545
O9 H92 O18 0.96(2) 2.49(6) 3.194(6) 131(6) 1_556
O9 H92 O20 0.96(2) 2.61(5) 3.321(8) 132(6) 1_456

_diffrn_measured_fraction_theta_max 0.868
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.325
_refine_diff_density_min         -1.431
_refine_diff_density_rms         0.126
_database_code_depnum_ccdc_archive 'CCDC 1015888'
