data_1-Sm
_publ_contact_author_name        'Rong Cao'
_publ_contact_author_address     
;
State Key Laboratory of Structural Chemistry,
Fujian Institute of Research on the Structure of Matter,
Chinese Academy of Sciences, Fujian, Fuzhou 350002, PR China
;
_publ_contact_author_email       rcao@fjirsm.ac.cn
_publ_contact_author_phone       +86-591-83796710
_publ_contact_author_fax         +86-591-83796710
loop_
_publ_author_name
_publ_author_address
'Cao, Rong'
;
State Key Laboratory of Structural Chemistry,
Fujian Institute of Research on the Structure of Matter,
Chinese Academy of Sciences, Fujian, Fuzhou 350002, PR China
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H20 N12 O42 Sm2'
_chemical_formula_weight         1641.38

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'
Sm Sm -0.1638 3.4418 '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                   14.1523(7)
_cell_length_b                   15.1344(7)
_cell_length_c                   18.0022(9)
_cell_angle_alpha                66.294(4)
_cell_angle_beta                 71.031(4)
_cell_angle_gamma                64.522(5)
_cell_volume                     3132.7(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    8395
_cell_measurement_theta_min      2.2852
_cell_measurement_theta_max      29.1374

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1608
_exptl_absorpt_coefficient_mu    1.971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7978
_exptl_absorpt_correction_T_max  0.8583
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(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  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.2083
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26860
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0553
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.29
_diffrn_reflns_theta_max         25.50
_reflns_number_total             11643
_reflns_number_gt                7593
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;

_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0443P)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    constr 
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11643
_refine_ls_number_parameters     865
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0352
_refine_ls_wR_factor_ref         0.1021
_refine_ls_wR_factor_gt          0.0885
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_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
Sm1 Sm 0.454339(18) 0.568240(19) 0.096749(14) 0.01778(8) Uani 1 1 d . . .
Sm2 Sm 0.551108(18) 0.431075(19) 0.403431(14) 0.01749(8) Uani 1 1 d . . .
C1 C 0.3141(4) 0.5954(4) 0.4879(3) 0.0202(11) Uani 1 1 d . . .
C2 C 0.3526(4) 0.5805(3) 0.2930(3) 0.0173(11) Uani 1 1 d . . .
C3 C 0.2450(3) 0.6012(4) 0.4380(3) 0.0170(11) Uani 1 1 d . . .
C4 C 0.2583(3) 0.5891(4) 0.3619(3) 0.0177(11) Uani 1 1 d . . .
C5 C 0.0938(4) 0.6118(4) 0.4190(3) 0.0181(11) Uani 1 1 d . . .
C6 C -0.0182(4) 0.6215(4) 0.4346(3) 0.0207(11) Uani 1 1 d . . .
C7 C -0.0541(4) 0.6021(4) 0.3816(3) 0.0280(13) Uani 1 1 d . . .
H7 H -0.0075 0.5834 0.3359 0.034 Uiso 1 1 calc R . .
C8 C -0.1583(4) 0.6108(4) 0.3968(3) 0.0298(13) Uani 1 1 d . . .
H8 H -0.1811 0.5984 0.3602 0.036 Uiso 1 1 calc R . .
C9 C -0.1944(4) 0.6537(4) 0.5128(3) 0.0305(13) Uani 1 1 d . . .
H9 H -0.2423 0.6706 0.5587 0.037 Uiso 1 1 calc R . .
C10 C -0.0912(4) 0.6482(4) 0.5012(3) 0.0280(13) Uani 1 1 d . . .
H10 H -0.0709 0.6625 0.5382 0.034 Uiso 1 1 calc R . .
C11 C 0.6498(4) 0.4121(4) 0.2068(3) 0.0185(11) Uani 1 1 d . . .
C12 C 0.6840(4) 0.3948(4) 0.0127(3) 0.0193(11) Uani 1 1 d . . .
C13 C 0.7431(3) 0.3982(4) 0.1389(3) 0.0170(11) Uani 1 1 d . . .
C14 C 0.7536(4) 0.3886(4) 0.0625(3) 0.0194(11) Uani 1 1 d . . .
C15 C 0.9073(4) 0.3734(4) 0.0803(3) 0.0224(12) Uani 1 1 d . . .
C16 C 1.0204(4) 0.3635(4) 0.0624(3) 0.0226(12) Uani 1 1 d . . .
C17 C 1.0871(4) 0.3469(5) -0.0092(3) 0.0399(16) Uani 1 1 d . . .
H17 H 1.0631 0.3388 -0.0475 0.048 Uiso 1 1 calc R . .
C18 C 1.1904(4) 0.3426(5) -0.0233(4) 0.0477(18) Uani 1 1 d . . .
H18 H 1.2341 0.3343 -0.0731 0.057 Uiso 1 1 calc R . .
C19 C 1.1658(4) 0.3634(5) 0.0990(4) 0.0476(17) Uani 1 1 d . . .
H19 H 1.1923 0.3686 0.1375 0.057 Uiso 1 1 calc R . .
C20 C 1.0622(4) 0.3709(5) 0.1177(4) 0.0376(15) Uani 1 1 d . . .
H20 H 1.0200 0.3809 0.1674 0.045 Uiso 1 1 calc R . .
C21 C 1.1825(5) 0.1241(5) 0.2566(4) 0.0455(16) Uani 1 1 d . . .
C22 C 1.2334(5) 0.0705(5) 0.0804(4) 0.0475(17) Uani 1 1 d . . .
C23 C 1.1156(4) 0.1126(4) 0.2149(3) 0.0306(13) Uani 1 1 d . . .
C24 C 1.1350(4) 0.0917(4) 0.1419(3) 0.0310(13) Uani 1 1 d . . .
C25 C 0.9706(4) 0.1136(4) 0.1935(3) 0.0298(13) Uani 1 1 d . . .
C26 C 0.8608(4) 0.1216(4) 0.2061(3) 0.0290(13) Uani 1 1 d . . .
C27 C 0.8312(5) 0.0994(5) 0.1521(4) 0.0446(17) Uani 1 1 d . . .
H27 H 0.8813 0.0776 0.1088 0.054 Uiso 1 1 calc R . .
C28 C 0.7257(5) 0.1101(5) 0.1627(4) 0.0533(19) Uani 1 1 d . . .
H28 H 0.7067 0.0957 0.1252 0.064 Uiso 1 1 calc R . .
C29 C 0.6807(5) 0.1572(5) 0.2769(4) 0.0511(18) Uani 1 1 d . . .
H29 H 0.6300 0.1750 0.3215 0.061 Uiso 1 1 calc R . .
C30 C 0.7839(5) 0.1505(4) 0.2699(4) 0.0424(16) Uani 1 1 d . . .
H30 H 0.8007 0.1655 0.3082 0.051 Uiso 1 1 calc R . .
C31 C -0.2681(5) 0.9074(5) 0.4126(4) 0.0471(17) Uani 1 1 d . . .
C32 C -0.1907(5) 0.8347(5) 0.2430(4) 0.0409(15) Uani 1 1 d . . .
C33 C -0.1659(4) 0.8856(4) 0.3566(3) 0.0321(13) Uani 1 1 d . . .
C34 C -0.1340(4) 0.8542(4) 0.2877(3) 0.0306(13) Uani 1 1 d . . .
C35 C 0.0005(4) 0.8651(4) 0.3143(3) 0.0288(13) Uani 1 1 d . . .
C36 C 0.1081(4) 0.8592(4) 0.3089(3) 0.0262(12) Uani 1 1 d . . .
C37 C 0.1886(4) 0.8401(4) 0.2425(4) 0.0394(15) Uani 1 1 d . . .
H37 H 0.1744 0.8334 0.1984 0.047 Uiso 1 1 calc R . .
C38 C 0.2904(5) 0.8312(4) 0.2422(4) 0.0409(15) Uani 1 1 d . . .
H38 H 0.3437 0.8176 0.1975 0.049 Uiso 1 1 calc R . .
C39 C 0.2371(5) 0.8621(5) 0.3660(4) 0.0485(17) Uani 1 1 d . . .
H39 H 0.2523 0.8707 0.4087 0.058 Uiso 1 1 calc R . .
C40 C 0.1346(5) 0.8716(5) 0.3701(4) 0.0433(16) Uani 1 1 d . . .
H40 H 0.0825 0.8867 0.4150 0.052 Uiso 1 1 calc R . .
N1 N 0.1399(3) 0.6173(3) 0.4710(2) 0.0194(9) Uani 1 1 d . . .
H1 H 0.1081 0.6291 0.5175 0.023 Uiso 1 1 calc R . .
N2 N 0.1638(3) 0.5945(3) 0.3519(2) 0.0179(9) Uani 1 1 d . . .
N3 N -0.2291(3) 0.6362(3) 0.4615(3) 0.0329(11) Uani 1 1 d . . .
N4 N 0.8395(3) 0.3898(3) 0.1484(2) 0.0203(9) Uani 1 1 d . . .
N5 N 0.8588(3) 0.3722(3) 0.0278(2) 0.0241(10) Uani 1 1 d . . .
H5 H 0.8889 0.3626 -0.0196 0.029 Uiso 1 1 calc R . .
N6 N 1.2315(3) 0.3494(4) 0.0300(3) 0.0450(14) Uani 1 1 d . . .
N7 N 1.0449(3) 0.0931(3) 0.1295(3) 0.0332(11) Uani 1 1 d . . .
N8 N 1.0108(3) 0.1262(3) 0.2463(3) 0.0329(11) Uani 1 1 d . . .
H8A H 0.9760 0.1403 0.2915 0.039 Uiso 1 1 calc R . .
N9 N 0.6506(4) 0.1396(4) 0.2235(3) 0.0510(15) Uani 1 1 d . . .
N10 N -0.0816(4) 0.8924(3) 0.3732(3) 0.0328(11) Uani 1 1 d . . .
N11 N -0.0288(3) 0.8416(3) 0.2624(3) 0.0299(11) Uani 1 1 d . . .
H11 H 0.0120 0.8221 0.2206 0.036 Uiso 1 1 calc R . .
N12 N 0.3157(4) 0.8411(4) 0.3033(3) 0.0471(14) Uani 1 1 d . . .
O1 O 0.2697(3) 0.6188(3) 0.5525(2) 0.0318(9) Uani 1 1 d . . .
O2 O 0.4155(2) 0.5674(2) 0.46483(19) 0.0219(8) Uani 1 1 d . . .
O3 O 0.4408(2) 0.5652(3) 0.30612(19) 0.0227(8) Uani 1 1 d . . .
O4 O 0.3350(2) 0.5923(2) 0.22447(18) 0.0215(8) Uani 1 1 d . . .
O5 O 0.6660(2) 0.4027(2) 0.27466(18) 0.0223(8) Uani 1 1 d . . .
O6 O 0.5598(2) 0.4304(2) 0.19309(19) 0.0219(8) Uani 1 1 d . . .
O7 O 0.5829(2) 0.4254(3) 0.03490(19) 0.0242(8) Uani 1 1 d . . .
O8 O 0.7274(2) 0.3730(3) -0.0525(2) 0.0272(9) Uani 1 1 d . . .
O9W O 0.5434(3) 0.6370(3) 0.1475(2) 0.0295(9) Uani 1 1 d . . .
O10W O 0.5835(3) 0.6314(3) -0.0127(2) 0.0371(10) Uani 1 1 d . . .
O11W O 0.3722(3) 0.7558(3) 0.0478(2) 0.0402(10) Uani 1 1 d . . .
O12W O 0.3770(3) 0.4310(3) 0.1543(2) 0.0325(9) Uani 1 1 d . . .
O13W O 0.6279(3) 0.5673(3) 0.3316(2) 0.0391(10) Uani 1 1 d . . .
O14W O 0.4582(3) 0.3626(3) 0.3538(2) 0.0300(9) Uani 1 1 d . . .
O15W O 0.4392(3) 0.3447(3) 0.5174(2) 0.0304(9) Uani 1 1 d . . .
O16W O 0.6528(3) 0.2462(3) 0.4413(2) 0.0396(10) Uani 1 1 d . . .
O17 O 1.1391(4) 0.1523(4) 0.3196(3) 0.0602(13) Uani 1 1 d . . .
O18 O 1.2799(3) 0.1058(4) 0.2239(3) 0.0589(13) Uani 1 1 d . . .
O19 O 1.3191(3) 0.0673(4) 0.0949(3) 0.0686(15) Uani 1 1 d . . .
O20 O 1.2324(3) 0.0548(4) 0.0192(3) 0.0683(15) Uani 1 1 d . . .
O21 O -0.2771(3) 0.9234(4) 0.4759(3) 0.0687(15) Uani 1 1 d . . .
O22 O -0.3491(3) 0.9069(4) 0.3929(3) 0.0620(14) Uani 1 1 d . . .
O23 O -0.2902(3) 0.8535(3) 0.2683(3) 0.0556(13) Uani 1 1 d . . .
O24 O -0.1384(3) 0.8018(4) 0.1833(3) 0.0576(13) Uani 1 1 d . . .
O25W O 0.0008(4) 0.4147(4) 0.8234(3) 0.0775(16) Uani 1 1 d . . .
O26W O 0.3747(4) 0.0717(4) 0.8759(3) 0.0735(15) Uani 1 1 d . . .
O27W O 0.0992(4) 0.0375(4) 0.4919(3) 0.0728(15) Uani 1 1 d . . .
O28W O 0.5343(4) 0.0058(4) 0.7008(4) 0.0912(18) Uani 1 1 d . . .
O29W O 0.5934(4) 0.0855(4) 0.5323(3) 0.0862(18) Uani 1 1 d . . .
O30W O 0.4506(4) 0.1674(4) 0.4169(3) 0.0766(16) Uani 1 1 d . . .
O31W O 0.4754(3) 0.2312(3) 0.6795(3) 0.0552(12) Uani 1 1 d . . .
O32W O 0.2582(4) 0.2467(4) 0.3332(3) 0.0746(15) Uani 1 1 d . . .
O33W O 0.4455(3) 0.2267(3) 0.2027(3) 0.0662(14) Uani 1 1 d . . .
O34W O 0.1837(3) 0.4567(3) 0.2606(2) 0.0461(11) Uani 1 1 d . . .
O35W O 0.5044(4) 0.1306(4) 0.0797(3) 0.0865(17) Uani 1 1 d . . .
O36W O 0.8853(3) 0.1589(3) 0.4068(3) 0.0589(13) Uani 1 1 d . . .
O37W O 0.8419(3) 0.4887(3) 0.2561(2) 0.0490(12) Uani 1 1 d . . .
O38W O 0.5211(4) 0.8413(4) 0.0852(3) 0.0809(16) Uani 1 1 d . . .
O39W O 0.1172(3) 0.7004(3) 0.1816(2) 0.0440(11) Uani 1 1 d . . .
O40W O 0.1686(3) 0.8880(3) 0.0400(3) 0.0621(14) Uani 1 1 d . . .
O41W O 0.0364(3) 0.6708(4) 0.6231(2) 0.0576(13) Uani 1 1 d . . .
O42W O 0.0016(4) 0.8370(5) 0.0347(3) 0.0888(19) 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
Sm1 O6 2.384(3) . ?
Sm1 O10W 2.405(4) . ?
Sm1 O4 2.427(3) . ?
Sm1 O11W 2.450(4) . ?
Sm1 O12W 2.464(4) . ?
Sm1 O9W 2.480(3) . ?
Sm1 O7 2.541(3) . ?
Sm1 O7 2.547(3) 2_665 ?
Sm1 O8 2.615(3) 2_665 ?
Sm1 C12 2.951(4) 2_665 ?
Sm2 O3 2.412(3) . ?
Sm2 O15W 2.437(3) . ?
Sm2 O5 2.439(3) . ?
Sm2 O13W 2.445(4) . ?
Sm2 O16W 2.450(3) . ?
Sm2 O2 2.492(3) . ?
Sm2 O14W 2.507(3) . ?
Sm2 O2 2.575(3) 2_666 ?
Sm2 O1 2.610(3) 2_666 ?
Sm2 C1 2.960(4) 2_666 ?
C1 O1 1.239(5) . ?
C1 O2 1.281(5) . ?
C1 C3 1.486(6) . ?
C1 Sm2 2.960(4) 2_666 ?
C2 O3 1.252(5) . ?
C2 O4 1.265(5) . ?
C2 C4 1.497(6) . ?
C3 N1 1.362(6) . ?
C3 C4 1.395(6) . ?
C4 N2 1.371(5) . ?
C5 N2 1.327(5) . ?
C5 N1 1.348(5) . ?
C5 C6 1.469(6) . ?
C6 C10 1.376(6) . ?
C6 C7 1.385(6) . ?
C7 C8 1.367(7) . ?
C7 H7 0.9300 . ?
C8 N3 1.333(6) . ?
C8 H8 0.9300 . ?
C9 N3 1.329(6) . ?
C9 C10 1.377(7) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 O5 1.256(5) . ?
C11 O6 1.268(5) . ?
C11 C13 1.483(6) . ?
C12 O8 1.238(5) . ?
C12 O7 1.276(5) . ?
C12 C14 1.487(6) . ?
C12 Sm1 2.951(4) 2_665 ?
C13 N4 1.376(5) . ?
C13 C14 1.393(6) . ?
C14 N5 1.368(6) . ?
C15 N4 1.325(6) . ?
C15 N5 1.346(6) . ?
C15 C16 1.479(6) . ?
C16 C17 1.371(6) . ?
C16 C20 1.372(6) . ?
C17 C18 1.376(7) . ?
C17 H17 0.9300 . ?
C18 N6 1.326(7) . ?
C18 H18 0.9300 . ?
C19 N6 1.322(7) . ?
C19 C20 1.357(7) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 O17 1.246(7) . ?
C21 O18 1.264(7) . ?
C21 C23 1.484(7) . ?
C22 O20 1.222(7) . ?
C22 O19 1.298(7) . ?
C22 C24 1.472(8) . ?
C23 N8 1.359(7) . ?
C23 C24 1.387(7) . ?
C24 N7 1.355(6) . ?
C25 N7 1.323(6) . ?
C25 N8 1.361(6) . ?
C25 C26 1.453(7) . ?
C26 C30 1.369(7) . ?
C26 C27 1.372(7) . ?
C27 C28 1.387(8) . ?
C27 H27 0.9300 . ?
C28 N9 1.325(7) . ?
C28 H28 0.9300 . ?
C29 N9 1.321(7) . ?
C29 C30 1.386(8) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
C31 O21 1.214(7) . ?
C31 O22 1.310(7) . ?
C31 C33 1.458(7) . ?
C32 O24 1.244(7) . ?
C32 O23 1.270(7) . ?
C32 C34 1.482(8) . ?
C33 N10 1.372(7) . ?
C33 C34 1.376(7) . ?
C34 N11 1.358(6) . ?
C35 N10 1.336(6) . ?
C35 N11 1.347(6) . ?
C35 C36 1.460(7) . ?
C36 C40 1.374(7) . ?
C36 C37 1.385(7) . ?
C37 C38 1.387(8) . ?
C37 H37 0.9300 . ?
C38 N12 1.339(7) . ?
C38 H38 0.9300 . ?
C39 N12 1.335(7) . ?
C39 C40 1.374(8) . ?
C39 H39 0.9300 . ?
C40 H40 0.9300 . ?
N1 H1 0.8600 . ?
N5 H5 0.8600 . ?
N8 H8A 0.8600 . ?
N11 H11 0.8600 . ?
O1 Sm2 2.610(3) 2_666 ?
O2 Sm2 2.575(3) 2_666 ?
O7 Sm1 2.547(3) 2_665 ?
O8 Sm1 2.615(3) 2_665 ?

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
O6 Sm1 O10W 103.27(11) . . ?
O6 Sm1 O4 80.59(10) . . ?
O10W Sm1 O4 142.57(12) . . ?
O6 Sm1 O11W 143.35(12) . . ?
O10W Sm1 O11W 73.13(13) . . ?
O4 Sm1 O11W 81.91(12) . . ?
O6 Sm1 O12W 73.02(11) . . ?
O10W Sm1 O12W 143.28(12) . . ?
O4 Sm1 O12W 73.89(11) . . ?
O11W Sm1 O12W 131.41(12) . . ?
O6 Sm1 O9W 70.80(11) . . ?
O10W Sm1 O9W 69.43(11) . . ?
O4 Sm1 O9W 77.23(11) . . ?
O11W Sm1 O9W 74.05(12) . . ?
O12W Sm1 O9W 136.58(11) . . ?
O6 Sm1 O7 68.84(10) . . ?
O10W Sm1 O7 71.29(12) . . ?
O4 Sm1 O7 140.43(11) . . ?
O11W Sm1 O7 137.27(12) . . ?
O12W Sm1 O7 73.55(11) . . ?
O9W Sm1 O7 113.46(10) . . ?
O6 Sm1 O7 130.63(10) . 2_665 ?
O10W Sm1 O7 74.86(11) . 2_665 ?
O4 Sm1 O7 130.65(10) . 2_665 ?
O11W Sm1 O7 84.57(11) . 2_665 ?
O12W Sm1 O7 80.56(11) . 2_665 ?
O9W Sm1 O7 142.30(11) . 2_665 ?
O7 Sm1 O7 63.95(11) . 2_665 ?
O6 Sm1 O8 139.57(12) . 2_665 ?
O10W Sm1 O8 113.20(11) . 2_665 ?
O4 Sm1 O8 80.87(10) . 2_665 ?
O11W Sm1 O8 67.55(12) . 2_665 ?
O12W Sm1 O8 67.43(11) . 2_665 ?
O9W Sm1 O8 137.89(11) . 2_665 ?
O7 Sm1 O8 106.38(10) . 2_665 ?
O7 Sm1 O8 50.23(9) 2_665 2_665 ?
O6 Sm1 C12 140.22(12) . 2_665 ?
O10W Sm1 C12 95.20(12) . 2_665 ?
O4 Sm1 C12 105.28(11) . 2_665 ?
O11W Sm1 C12 75.67(13) . 2_665 ?
O12W Sm1 C12 71.21(13) . 2_665 ?
O9W Sm1 C12 148.92(12) . 2_665 ?
O7 Sm1 C12 84.75(11) . 2_665 ?
O7 Sm1 C12 25.50(11) 2_665 2_665 ?
O8 Sm1 C12 24.77(10) 2_665 2_665 ?
O3 Sm2 O15W 108.09(11) . . ?
O3 Sm2 O5 80.01(10) . . ?
O15W Sm2 O5 135.65(11) . . ?
O3 Sm2 O13W 71.73(12) . . ?
O15W Sm2 O13W 153.12(12) . . ?
O5 Sm2 O13W 71.23(12) . . ?
O3 Sm2 O16W 141.49(12) . . ?
O15W Sm2 O16W 72.29(12) . . ?
O5 Sm2 O16W 75.44(12) . . ?
O13W Sm2 O16W 125.31(12) . . ?
O3 Sm2 O2 68.85(10) . . ?
O15W Sm2 O2 75.13(11) . . ?
O5 Sm2 O2 142.99(11) . . ?
O13W Sm2 O2 80.15(11) . . ?
O16W Sm2 O2 141.51(12) . . ?
O3 Sm2 O14W 68.02(11) . . ?
O15W Sm2 O14W 68.41(11) . . ?
O5 Sm2 O14W 75.47(11) . . ?
O13W Sm2 O14W 131.11(12) . . ?
O16W Sm2 O14W 77.29(12) . . ?
O2 Sm2 O14W 108.96(10) . . ?
O3 Sm2 O2 130.10(10) . 2_666 ?
O15W Sm2 O2 74.53(11) . 2_666 ?
O5 Sm2 O2 133.76(10) . 2_666 ?
O13W Sm2 O2 85.27(12) . 2_666 ?
O16W Sm2 O2 87.90(11) . 2_666 ?
O2 Sm2 O2 63.83(11) . 2_666 ?
O14W Sm2 O2 142.71(11) . 2_666 ?
O3 Sm2 O1 140.07(12) . 2_666 ?
O15W Sm2 O1 108.98(11) . 2_666 ?
O5 Sm2 O1 83.83(10) . 2_666 ?
O13W Sm2 O1 68.53(12) . 2_666 ?
O16W Sm2 O1 65.84(12) . 2_666 ?
O2 Sm2 O1 107.31(10) . 2_666 ?
O14W Sm2 O1 141.24(11) . 2_666 ?
O2 Sm2 O1 50.21(9) 2_666 2_666 ?
O3 Sm2 C1 140.15(12) . 2_666 ?
O15W Sm2 C1 92.98(13) . 2_666 ?
O5 Sm2 C1 108.26(12) . 2_666 ?
O13W Sm2 C1 74.43(13) . 2_666 ?
O16W Sm2 C1 76.58(13) . 2_666 ?
O2 Sm2 C1 85.28(12) . 2_666 ?
O14W Sm2 C1 151.57(12) . 2_666 ?
O2 Sm2 C1 25.57(11) 2_666 2_666 ?
O1 Sm2 C1 24.69(11) 2_666 2_666 ?
O1 C1 O2 121.7(4) . . ?
O1 C1 C3 117.3(4) . . ?
O2 C1 C3 121.1(4) . . ?
O1 C1 Sm2 61.7(2) . 2_666 ?
O2 C1 Sm2 60.2(2) . 2_666 ?
C3 C1 Sm2 175.5(4) . 2_666 ?
O3 C2 O4 125.1(4) . . ?
O3 C2 C4 118.7(4) . . ?
O4 C2 C4 116.1(4) . . ?
N1 C3 C4 104.7(4) . . ?
N1 C3 C1 118.4(4) . . ?
C4 C3 C1 136.8(4) . . ?
N2 C4 C3 109.7(4) . . ?
N2 C4 C2 119.8(4) . . ?
C3 C4 C2 130.4(4) . . ?
N2 C5 N1 110.9(4) . . ?
N2 C5 C6 124.2(4) . . ?
N1 C5 C6 124.9(4) . . ?
C10 C6 C7 117.2(5) . . ?
C10 C6 C5 122.8(4) . . ?
C7 C6 C5 120.0(4) . . ?
C8 C7 C6 119.6(5) . . ?
C8 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
N3 C8 C7 123.5(5) . . ?
N3 C8 H8 118.3 . . ?
C7 C8 H8 118.3 . . ?
N3 C9 C10 123.3(5) . . ?
N3 C9 H9 118.4 . . ?
C10 C9 H9 118.4 . . ?
C6 C10 C9 119.6(5) . . ?
C6 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
O5 C11 O6 124.4(4) . . ?
O5 C11 C13 117.6(4) . . ?
O6 C11 C13 117.9(4) . . ?
O8 C12 O7 121.4(4) . . ?
O8 C12 C14 117.6(4) . . ?
O7 C12 C14 121.0(4) . . ?
O8 C12 Sm1 62.3(2) . 2_665 ?
O7 C12 Sm1 59.3(2) . 2_665 ?
C14 C12 Sm1 173.3(3) . 2_665 ?
N4 C13 C14 109.7(4) . . ?
N4 C13 C11 119.4(4) . . ?
C14 C13 C11 130.8(4) . . ?
N5 C14 C13 104.8(4) . . ?
N5 C14 C12 117.3(4) . . ?
C13 C14 C12 137.9(4) . . ?
N4 C15 N5 111.5(4) . . ?
N4 C15 C16 124.3(4) . . ?
N5 C15 C16 124.2(4) . . ?
C17 C16 C20 117.5(5) . . ?
C17 C16 C15 122.0(4) . . ?
C20 C16 C15 120.5(5) . . ?
C16 C17 C18 118.8(5) . . ?
C16 C17 H17 120.6 . . ?
C18 C17 H17 120.6 . . ?
N6 C18 C17 123.9(5) . . ?
N6 C18 H18 118.0 . . ?
C17 C18 H18 118.0 . . ?
N6 C19 C20 124.5(6) . . ?
N6 C19 H19 117.7 . . ?
C20 C19 H19 117.7 . . ?
C19 C20 C16 119.3(5) . . ?
C19 C20 H20 120.3 . . ?
C16 C20 H20 120.3 . . ?
O17 C21 O18 125.3(6) . . ?
O17 C21 C23 118.3(6) . . ?
O18 C21 C23 116.4(6) . . ?
O20 C22 O19 122.6(6) . . ?
O20 C22 C24 119.7(6) . . ?
O19 C22 C24 117.7(6) . . ?
N8 C23 C24 104.9(5) . . ?
N8 C23 C21 121.7(5) . . ?
C24 C23 C21 133.3(5) . . ?
N7 C24 C23 110.3(5) . . ?
N7 C24 C22 119.0(5) . . ?
C23 C24 C22 130.6(5) . . ?
N7 C25 N8 110.8(5) . . ?
N7 C25 C26 124.8(5) . . ?
N8 C25 C26 124.4(5) . . ?
C30 C26 C27 117.5(5) . . ?
C30 C26 C25 123.3(5) . . ?
C27 C26 C25 119.2(5) . . ?
C26 C27 C28 119.2(6) . . ?
C26 C27 H27 120.4 . . ?
C28 C27 H27 120.4 . . ?
N9 C28 C27 123.6(6) . . ?
N9 C28 H28 118.2 . . ?
C27 C28 H28 118.2 . . ?
N9 C29 C30 123.4(6) . . ?
N9 C29 H29 118.3 . . ?
C30 C29 H29 118.3 . . ?
C26 C30 C29 119.5(6) . . ?
C26 C30 H30 120.2 . . ?
C29 C30 H30 120.2 . . ?
O21 C31 O22 121.3(6) . . ?
O21 C31 C33 121.2(6) . . ?
O22 C31 C33 117.5(6) . . ?
O24 C32 O23 124.5(6) . . ?
O24 C32 C34 118.2(5) . . ?
O23 C32 C34 117.2(5) . . ?
N10 C33 C34 110.1(5) . . ?
N10 C33 C31 118.4(5) . . ?
C34 C33 C31 131.4(6) . . ?
N11 C34 C33 105.6(5) . . ?
N11 C34 C32 121.5(5) . . ?
C33 C34 C32 133.0(5) . . ?
N10 C35 N11 111.1(5) . . ?
N10 C35 C36 123.9(5) . . ?
N11 C35 C36 125.0(5) . . ?
C40 C36 C37 116.7(5) . . ?
C40 C36 C35 121.3(5) . . ?
C37 C36 C35 121.9(5) . . ?
C36 C37 C38 119.4(5) . . ?
C36 C37 H37 120.3 . . ?
C38 C37 H37 120.3 . . ?
N12 C38 C37 123.2(6) . . ?
N12 C38 H38 118.4 . . ?
C37 C38 H38 118.4 . . ?
N12 C39 C40 122.7(6) . . ?
N12 C39 H39 118.7 . . ?
C40 C39 H39 118.7 . . ?
C36 C40 C39 121.0(6) . . ?
C36 C40 H40 119.5 . . ?
C39 C40 H40 119.5 . . ?
C5 N1 C3 108.8(4) . . ?
C5 N1 H1 125.6 . . ?
C3 N1 H1 125.6 . . ?
C5 N2 C4 105.9(4) . . ?
C9 N3 C8 116.9(4) . . ?
C15 N4 C13 105.6(4) . . ?
C15 N5 C14 108.4(4) . . ?
C15 N5 H5 125.8 . . ?
C14 N5 H5 125.8 . . ?
C19 N6 C18 115.8(5) . . ?
C25 N7 C24 105.9(4) . . ?
C23 N8 C25 108.0(5) . . ?
C23 N8 H8A 126.0 . . ?
C25 N8 H8A 126.0 . . ?
C29 N9 C28 116.7(6) . . ?
C35 N10 C33 105.0(4) . . ?
C35 N11 C34 108.2(5) . . ?
C35 N11 H11 125.9 . . ?
C34 N11 H11 125.9 . . ?
C39 N12 C38 117.0(5) . . ?
C1 O1 Sm2 93.6(3) . 2_666 ?
C1 O2 Sm2 134.1(3) . . ?
C1 O2 Sm2 94.2(3) . 2_666 ?
Sm2 O2 Sm2 116.17(11) . 2_666 ?
C2 O3 Sm2 133.0(3) . . ?
C2 O4 Sm1 131.8(3) . . ?
C11 O5 Sm2 134.5(3) . . ?
C11 O6 Sm1 132.0(3) . . ?
C12 O7 Sm1 131.7(3) . . ?
C12 O7 Sm1 95.2(3) . 2_665 ?
Sm1 O7 Sm1 116.05(11) . 2_665 ?
C12 O8 Sm1 93.0(3) . 2_665 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.800
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.107


# Start Validation Reply Form

_vrf_PLAT306_1-Sm
;
PROBLEM:
 Isolated Oxygen Atom (H-atoms Missing ?) ....... O25W
 Isolated Oxygen Atom (H-atoms Missing ?) ....... O26W
 Isolated Oxygen Atom (H-atoms Missing ?) ....... O27W
 Isolated Oxygen Atom (H-atoms Missing ?) ....... O28W
 Isolated Oxygen Atom (H-atoms Missing ?) ....... O29W
 Isolated Oxygen Atom (H-atoms Missing ?) ....... O30W
 Isolated Oxygen Atom (H-atoms Missing ?) ....... O31W
 Isolated Oxygen Atom (H-atoms Missing ?) ....... O32W
 Isolated Oxygen Atom (H-atoms Missing ?) ....... O33W
 Isolated Oxygen Atom (H-atoms Missing ?) ....... O34W
 Isolated Oxygen Atom (H-atoms Missing ?) ....... O35W
 Isolated Oxygen Atom (H-atoms Missing ?) ....... O36W
 Isolated Oxygen Atom (H-atoms Missing ?) ....... O37W
 Isolated Oxygen Atom (H-atoms Missing ?) ....... O38W
 Isolated Oxygen Atom (H-atoms Missing ?) ....... O39W
 Isolated Oxygen Atom (H-atoms Missing ?) ....... O40W
 Isolated Oxygen Atom (H-atoms Missing ?) ....... O41W
 Isolated Oxygen Atom (H-atoms Missing ?) ....... O42W

RESPONSE:
This is because the hydrogen atoms attaching to free water molecules have not been added.
; 


 
data_2-Eu
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C20 H25 Eu N6 O21' 
_chemical_formula_weight          837.42 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Eu'  'Eu'  -0.1578   3.6682 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 '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' 
 
_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                    8.9815(3) 
_cell_length_b                    14.0907(4) 
_cell_length_c                    14.1747(5) 
_cell_angle_alpha                 67.246(3) 
_cell_angle_beta                  78.097(3) 
_cell_angle_gamma                 71.811(3) 
_cell_volume                      1564.11(9) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     298(2) 
_cell_measurement_reflns_used     6100
_cell_measurement_theta_min       2.3936
_cell_measurement_theta_max       29.1729
 
_exptl_crystal_description        block 
_exptl_crystal_colour             colorless
_exptl_crystal_size_max           0.20
_exptl_crystal_size_mid           0.18 
_exptl_crystal_size_min           0.10 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.778 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              836 
_exptl_absorpt_coefficient_mu     2.103 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.93068
_exptl_absorpt_correction_T_max   1.00000
_exptl_absorpt_process_details    

;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
; 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       298(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   'Xcalibur, Eos' 
_diffrn_measurement_method        'ω scans' 
_diffrn_detector_area_resol_mean  16.2083 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             14952 
_diffrn_reflns_av_R_equivalents   0.0399 
_diffrn_reflns_av_sigmaI/netI     0.0591 
_diffrn_reflns_limit_h_min        -11 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        -17 
_diffrn_reflns_limit_k_max        17 
_diffrn_reflns_limit_l_min        -17 
_diffrn_reflns_limit_l_max        17 
_diffrn_reflns_theta_min          2.40 
_diffrn_reflns_theta_max          27.10 
_reflns_number_total              6775 
_reflns_number_gt                 5842 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        

;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
 
_computing_cell_refinement        

;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;

_computing_data_reduction         

;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;

 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_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)+(0.0513P)²+1.8172P] 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          6775 
_refine_ls_number_parameters      529 
_refine_ls_number_restraints      22 
_refine_ls_R_factor_all           0.0520 
_refine_ls_R_factor_gt            0.0411 
_refine_ls_wR_factor_ref          0.1037 
_refine_ls_wR_factor_gt           0.0962 
_refine_ls_goodness_of_fit_ref    1.049 
_refine_ls_restrained_S_all       1.047 
_refine_ls_shift/su_max           0.002 
_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 
Eu1 Eu 0.28636(2) 0.952015(16) 0.568310(17) 0.01979(8) Uani 1 1 d D . . 
O1 O 0.4991(4) 0.7718(2) 0.6232(3) 0.0330(8) Uani 1 1 d . . . 
O2 O 0.5819(4) 0.9169(2) 0.5705(3) 0.0255(7) Uani 1 1 d . . . 
O3 O 0.8789(4) 0.9410(2) 0.5675(2) 0.0229(7) Uani 1 1 d . . . 
O4 O 1.1210(4) 0.8352(2) 0.5943(3) 0.0253(7) Uani 1 1 d . . . 
O5 O 0.3713(5) 0.8755(3) 0.4336(3) 0.0408(10) Uani 1 1 d D . . 
H5A H 0.397(8) 0.911(3) 0.375(2) 0.061 Uiso 1 1 d D . . 
H5B H 0.390(8) 0.8114(12) 0.446(4) 0.061 Uiso 1 1 d D . . 
O6 O 0.3143(4) 1.0719(3) 0.6417(4) 0.0485(11) Uani 1 1 d D . . 
H6A H 0.243(3) 1.124(3) 0.644(5) 0.073 Uiso 1 1 d D . . 
H6B H 0.400(2) 1.070(4) 0.654(5) 0.073 Uiso 1 1 d D . . 
O7 O 0.0285(4) 1.0429(3) 0.6362(3) 0.0300(8) Uani 1 1 d D . . 
H7A H 0.016(6) 1.042(5) 0.6957(17) 0.045 Uiso 1 1 d D . . 
H7B H -0.041(5) 1.027(5) 0.620(4) 0.045 Uiso 1 1 d D . . 
O8 O 0.2788(6) 0.8614(4) 0.7524(3) 0.0534(12) Uani 1 1 d D . . 
H8A H 0.282(10) 0.899(4) 0.784(5) 0.080 Uiso 1 1 d D . . 
H8B H 0.305(9) 0.7969(10) 0.782(5) 0.080 Uiso 1 1 d D . . 
O9 O 0.5481(7) 0.6388(5) 0.1764(7) 0.110(3) Uani 1 1 d . . . 
O10 O 0.6294(9) 0.7852(4) 0.1283(6) 0.128(3) Uani 1 1 d . . . 
H10A H 0.7134 0.8017 0.1120 0.192 Uiso 1 1 calc R . . 
O11 O 0.8841(13) 0.8346(6) 0.0786(7) 0.153(4) Uani 1 1 d . . . 
O12 O 1.1375(12) 0.7545(7) 0.0658(6) 0.157(4) Uani 1 1 d . . . 
N1 N 0.7931(4) 0.6407(3) 0.6223(3) 0.0247(8) Uani 1 1 d . . . 
H1A H 0.7194 0.6097 0.6334 0.030 Uiso 1 1 calc R . . 
N2 N 1.0316(4) 0.6628(3) 0.6017(3) 0.0260(9) Uani 1 1 d . . . 
N5 N 1.1553(6) 0.2698(3) 0.6425(4) 0.0464(13) Uani 1 1 d . . . 
N6 N 0.8537(7) 0.5190(5) 0.1431(5) 0.073(2) Uani 1 1 d . . . 
H6 H 0.7874 0.4810 0.1599 0.088 Uiso 1 1 calc R . . 
N7 N 1.0808(9) 0.5627(6) 0.1010(5) 0.081(2) Uani 1 1 d . . . 
N8 N 1.2622(8) 0.1679(6) 0.1485(5) 0.098(3) Uani 1 1 d . . . 
C1 C 0.6087(5) 0.8159(3) 0.6008(3) 0.0227(9) Uani 1 1 d . . . 
C2 C 0.7724(5) 0.7468(3) 0.6059(4) 0.0227(9) Uani 1 1 d . . . 
C3 C 0.9487(5) 0.5941(3) 0.6180(4) 0.0251(10) Uani 1 1 d . . . 
C4 C 1.0174(6) 0.4811(4) 0.6287(4) 0.0289(11) Uani 1 1 d . . . 
C5 C 0.9269(7) 0.4114(4) 0.6506(5) 0.0407(14) Uani 1 1 d . . . 
H5 H 0.8178 0.4336 0.6615 0.049 Uiso 1 1 calc R . . 
C6 C 1.0008(7) 0.3072(4) 0.6562(5) 0.0453(15) Uani 1 1 d . . . 
H6E H 0.9381 0.2609 0.6705 0.054 Uiso 1 1 calc R . . 
C7 C 1.2419(8) 0.3382(5) 0.6220(6) 0.0540(18) Uani 1 1 d . . . 
H7 H 1.3507 0.3140 0.6117 0.065 Uiso 1 1 calc R . . 
C8 C 1.1787(7) 0.4433(4) 0.6151(5) 0.0487(16) Uani 1 1 d . . . 
H8 H 1.2440 0.4879 0.6014 0.058 Uiso 1 1 calc R . . 
C9 C 0.9232(5) 0.7582(3) 0.5940(3) 0.0214(9) Uani 1 1 d . . . 
C10 C 0.9779(5) 0.8521(3) 0.5834(3) 0.0205(9) Uani 1 1 d . . . 
C11 C 0.6551(12) 0.6847(6) 0.1454(9) 0.097(4) Uani 1 1 d . . . 
C12 C 0.8186(10) 0.6241(6) 0.1300(7) 0.080(3) Uani 1 1 d . . . 
C13 C 1.0120(8) 0.4847(6) 0.1248(5) 0.068(2) Uani 1 1 d . . . 
C14 C 1.0951(8) 0.3751(7) 0.1309(5) 0.068(2) Uani 1 1 d . . . 
C15 C 1.0183(8) 0.2973(6) 0.1562(5) 0.0583(19) Uani 1 1 d . . . 
H15 H 0.9091 0.3127 0.1684 0.070 Uiso 1 1 calc R . . 
C16 C 1.1062(9) 0.1954(7) 0.1631(6) 0.075(3) Uani 1 1 d . . . 
H16 H 1.0531 0.1432 0.1789 0.090 Uiso 1 1 calc R . . 
C17 C 1.3346(9) 0.2433(9) 0.1243(8) 0.115(5) Uani 1 1 d . . . 
H17 H 1.4440 0.2247 0.1139 0.138 Uiso 1 1 calc R . . 
C18 C 1.2599(9) 0.3475(8) 0.1133(7) 0.107(4) Uani 1 1 d . . . 
H18 H 1.3166 0.3982 0.0948 0.129 Uiso 1 1 calc R . . 
C19 C 0.9625(12) 0.6494(8) 0.1018(6) 0.091(4) Uani 1 1 d . . . 
C20 C 0.9971(18) 0.7526(10) 0.0829(8) 0.129(6) Uani 1 1 d . . . 
O13 O 0.3424(6) 0.6713(5) 0.4849(8) 0.109(3) Uani 1 1 d D . . 
H13A H 0.259(8) 0.672(9) 0.522(7) 0.163 Uiso 1 1 d D . . 
H13B H 0.354(13) 0.645(10) 0.441(7) 0.163 Uiso 1 1 d D . . 
O14 O 0.4263(8) 0.9595(5) 0.2308(4) 0.089(2) Uani 1 1 d D . . 
H14A H 0.507(8) 0.938(7) 0.198(6) 0.134 Uiso 1 1 d D . . 
H14B H 0.377(10) 1.021(3) 0.204(7) 0.134 Uiso 1 1 d D . . 
O15 O 0.0388(8) 0.9633(6) 0.1661(5) 0.0913(19) Uani 1 1 d D . . 
H15A H 0.109(9) 0.922(7) 0.143(7) 0.137 Uiso 1 1 d D . . 
H15B H -0.031(9) 1.002(8) 0.128(6) 0.137 Uiso 1 1 d D . . 
O16 O 0.3563(11) 0.6180(8) 0.8425(8) 0.059(3) Uani 0.50 1 d P . . 
O16B O 0.3641(11) 0.6689(8) 0.8863(8) 0.060(3) Uani 0.50 1 d P . . 
O17 O 0.3806(12) 0.5962(10) 0.0388(9) 0.077(3) Uani 0.50 1 d P . . 
O17B O 0.4098(13) 0.4981(8) 0.1626(11) 0.091(4) Uani 0.50 1 d P . . 
O18 O 0.3023(11) 0.8755(8) 0.0700(9) 0.067(3) Uani 0.50 1 d P . . 
O18B O 0.4407(15) 0.9684(9) -0.0071(9) 0.085(4) Uani 0.50 1 d P . . 
O19 O 0.2934(13) 0.9964(9) 0.8675(9) 0.072(3) Uani 0.50 1 d P . . 
O19B O 0.2417(15) 0.9087(9) 0.9155(8) 0.078(3) Uani 0.50 1 d P . . 
O20 O 0.3263(12) 0.7603(9) 0.2474(9) 0.072(3) Uani 0.50 1 d P . . 
O21 O 0.3195(9) 0.6174(6) 0.6998(6) 0.045(2) Uani 0.50 1 d P . . 
O21B O 0.5475(10) 0.5360(7) 0.6700(8) 0.058(3) Uani 0.50 1 d P . . 
O22 O 0.5632(11) 0.5004(10) 0.5859(8) 0.081(4) Uani 0.50 1 d P . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Eu1 O3 2.391(3) 2_676 ? 
Eu1 O6 2.393(4) . ? 
Eu1 O8 2.419(4) . ? 
Eu1 O5 2.423(4) . ? 
Eu1 O4 2.425(3) 1_455 ? 
Eu1 O7 2.472(3) . ? 
Eu1 O2 2.505(3) 2_676 ? 
Eu1 O2 2.548(3) . ? 
Eu1 O1 2.600(3) . ? 
Eu1 C1 2.945(4) . ? 
Eu1 Eu1 4.2958(5) 2_676 ? 
O1 C1 1.248(5) . ? 
O2 C1 1.274(5) . ? 
O2 Eu1 2.505(3) 2_676 ? 
O3 C10 1.257(5) . ? 
O3 Eu1 2.391(3) 2_676 ? 
O4 C10 1.263(5) . ? 
O4 Eu1 2.425(3) 1_655 ? 
O5 H5A 0.818(10) . ? 
O5 H5B 0.818(10) . ? 
O6 H6A 0.818(10) . ? 
O6 H6B 0.819(10) . ? 
O7 H7A 0.823(10) . ? 
O7 H7B 0.822(10) . ? 
O8 H8A 0.818(10) . ? 
O8 H8B 0.819(10) . ? 
O9 C11 1.237(11) . ? 
O10 C11 1.292(9) . ? 
O10 H10A 0.8200 . ? 
O11 C20 1.268(18) . ? 
O12 C20 1.241(15) . ? 
N1 C3 1.346(6) . ? 
N1 C2 1.377(5) . ? 
N1 H1A 0.8600 . ? 
N2 C3 1.323(6) . ? 
N2 C9 1.371(5) . ? 
N5 C6 1.324(8) . ? 
N5 C7 1.333(8) . ? 
N6 C13 1.355(9) . ? 
N6 C12 1.360(10) . ? 
N6 H6 0.8600 . ? 
N7 C13 1.325(9) . ? 
N7 C19 1.348(13) . ? 
N8 C17 1.314(13) . ? 
N8 C16 1.327(10) . ? 
C1 C2 1.487(6) . ? 
C2 C9 1.382(6) . ? 
C3 C4 1.475(6) . ? 
C4 C5 1.372(7) . ? 
C4 C8 1.379(8) . ? 
C5 C6 1.388(7) . ? 
C5 H5 0.9300 . ? 
C6 H6E 0.9300 . ? 
C7 C8 1.382(7) . ? 
C7 H7 0.9300 . ? 
C8 H8 0.9300 . ? 
C9 C10 1.496(6) . ? 
C11 C12 1.471(14) . ? 
C12 C19 1.386(11) . ? 
C13 C14 1.467(12) . ? 
C14 C15 1.369(10) . ? 
C14 C18 1.402(10) . ? 
C15 C16 1.383(11) . ? 
C15 H15 0.9300 . ? 
C16 H16 0.9300 . ? 
C17 C18 1.372(15) . ? 
C17 H17 0.9300 . ? 
C18 H18 0.9300 . ? 
C19 C20 1.494(13) . ? 
O13 H13A 0.820(10) . ? 
O13 H13B 0.819(10) . ? 
O14 H14A 0.818(10) . ? 
O14 H14B 0.819(10) . ? 
O15 H15A 0.820(10) . ? 
O15 H15B 0.822(10) . ? 
O16 O16B 1.139(14) . ? 
O17 O17B 1.774(18) . ? 
O18B O18B 1.67(3) 2_675 ? 
O19 O19B 1.336(14) . ? 
O21B O22 1.429(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 
O3 Eu1 O6 105.84(14) 2_676 . ? 
O3 Eu1 O8 142.49(14) 2_676 . ? 
O6 Eu1 O8 72.76(18) . . ? 
O3 Eu1 O5 72.43(12) 2_676 . ? 
O6 Eu1 O5 147.95(15) . . ? 
O8 Eu1 O5 128.50(15) . . ? 
O3 Eu1 O4 80.11(10) 2_676 1_455 ? 
O6 Eu1 O4 139.32(13) . 1_455 ? 
O8 Eu1 O4 78.75(15) . 1_455 ? 
O5 Eu1 O4 72.66(13) . 1_455 ? 
O3 Eu1 O7 69.55(11) 2_676 . ? 
O6 Eu1 O7 68.61(12) . . ? 
O8 Eu1 O7 75.60(14) . . ? 
O5 Eu1 O7 134.30(14) . . ? 
O4 Eu1 O7 76.66(11) 1_455 . ? 
O3 Eu1 O2 69.21(10) 2_676 2_676 ? 
O6 Eu1 O2 73.05(14) . 2_676 ? 
O8 Eu1 O2 139.18(16) . 2_676 ? 
O5 Eu1 O2 76.75(12) . 2_676 ? 
O4 Eu1 O2 141.85(11) 1_455 2_676 ? 
O7 Eu1 O2 111.25(11) . 2_676 ? 
O3 Eu1 O2 130.34(10) 2_676 . ? 
O6 Eu1 O2 74.64(12) . . ? 
O8 Eu1 O2 86.29(14) . . ? 
O5 Eu1 O2 82.57(14) . . ? 
O4 Eu1 O2 132.18(10) 1_455 . ? 
O7 Eu1 O2 142.37(12) . . ? 
O2 Eu1 O2 63.56(11) 2_676 . ? 
O3 Eu1 O1 139.63(12) 2_676 . ? 
O6 Eu1 O1 111.26(13) . . ? 
O8 Eu1 O1 66.53(14) . . ? 
O5 Eu1 O1 67.76(13) . . ? 
O4 Eu1 O1 82.03(10) 1_455 . ? 
O7 Eu1 O1 139.41(11) . . ? 
O2 Eu1 O1 106.89(10) 2_676 . ? 
O2 Eu1 O1 50.53(10) . . ? 
O3 Eu1 C1 140.29(12) 2_676 . ? 
O6 Eu1 C1 93.94(13) . . ? 
O8 Eu1 C1 75.96(15) . . ? 
O5 Eu1 C1 72.69(14) . . ? 
O4 Eu1 C1 106.77(11) 1_455 . ? 
O7 Eu1 C1 150.01(13) . . ? 
O2 Eu1 C1 84.82(11) 2_676 . ? 
O2 Eu1 C1 25.53(11) . . ? 
O1 Eu1 C1 25.03(11) . . ? 
O3 Eu1 Eu1 100.20(8) 2_676 2_676 ? 
O6 Eu1 Eu1 70.91(10) . 2_676 ? 
O8 Eu1 Eu1 113.77(13) . 2_676 ? 
O5 Eu1 Eu1 77.85(11) . 2_676 ? 
O4 Eu1 Eu1 148.97(8) 1_455 2_676 ? 
O7 Eu1 Eu1 132.93(8) . 2_676 ? 
O2 Eu1 Eu1 32.08(7) 2_676 2_676 ? 
O2 Eu1 Eu1 31.48(7) . 2_676 ? 
O1 Eu1 Eu1 78.02(7) . 2_676 ? 
C1 Eu1 Eu1 54.00(8) . 2_676 ? 
C1 O1 Eu1 93.1(3) . . ? 
C1 O2 Eu1 133.0(3) . 2_676 ? 
C1 O2 Eu1 94.9(3) . . ? 
Eu1 O2 Eu1 116.44(11) 2_676 . ? 
C10 O3 Eu1 131.7(3) . 2_676 ? 
C10 O4 Eu1 133.1(3) . 1_655 ? 
Eu1 O5 H5A 121(4) . . ? 
Eu1 O5 H5B 122(4) . . ? 
H5A O5 H5B 117(2) . . ? 
Eu1 O6 H6A 121.5(15) . . ? 
Eu1 O6 H6B 121.2(15) . . ? 
H6A O6 H6B 116(2) . . ? 
Eu1 O7 H7A 120(4) . . ? 
Eu1 O7 H7B 109(4) . . ? 
H7A O7 H7B 115(2) . . ? 
Eu1 O8 H8A 113(5) . . ? 
Eu1 O8 H8B 126(5) . . ? 
H8A O8 H8B 116(2) . . ? 
C11 O10 H10A 109.5 . . ? 
C3 N1 C2 108.2(4) . . ? 
C3 N1 H1A 125.9 . . ? 
C2 N1 H1A 125.9 . . ? 
C3 N2 C9 105.6(4) . . ? 
C6 N5 C7 116.6(5) . . ? 
C13 N6 C12 107.8(6) . . ? 
C13 N6 H6 126.1 . . ? 
C12 N6 H6 126.1 . . ? 
C13 N7 C19 105.4(7) . . ? 
C17 N8 C16 117.2(9) . . ? 
O1 C1 O2 121.3(4) . . ? 
O1 C1 C2 117.6(4) . . ? 
O2 C1 C2 121.1(4) . . ? 
O1 C1 Eu1 61.8(2) . . ? 
O2 C1 Eu1 59.6(2) . . ? 
C2 C1 Eu1 173.8(3) . . ? 
N1 C2 C9 104.6(4) . . ? 
N1 C2 C1 117.6(4) . . ? 
C9 C2 C1 137.7(4) . . ? 
N2 C3 N1 111.4(4) . . ? 
N2 C3 C4 124.6(4) . . ? 
N1 C3 C4 124.1(4) . . ? 
C5 C4 C8 118.0(5) . . ? 
C5 C4 C3 122.6(5) . . ? 
C8 C4 C3 119.4(5) . . ? 
C4 C5 C6 118.9(5) . . ? 
C4 C5 H5 120.6 . . ? 
C6 C5 H5 120.6 . . ? 
N5 C6 C5 123.9(6) . . ? 
N5 C6 H6E 118.0 . . ? 
C5 C6 H6E 118.0 . . ? 
N5 C7 C8 123.6(6) . . ? 
N5 C7 H7 118.2 . . ? 
C8 C7 H7 118.2 . . ? 
C4 C8 C7 119.0(6) . . ? 
C4 C8 H8 120.5 . . ? 
C7 C8 H8 120.5 . . ? 
N2 C9 C2 110.3(4) . . ? 
N2 C9 C10 119.3(4) . . ? 
C2 C9 C10 130.2(4) . . ? 
O3 C10 O4 124.5(4) . . ? 
O3 C10 C9 118.5(4) . . ? 
O4 C10 C9 117.0(4) . . ? 
O9 C11 O10 122.2(10) . . ? 
O9 C11 C12 119.9(7) . . ? 
O10 C11 C12 117.8(9) . . ? 
N6 C12 C19 104.7(8) . . ? 
N6 C12 C11 121.0(7) . . ? 
C19 C12 C11 134.2(9) . . ? 
N7 C13 N6 111.3(8) . . ? 
N7 C13 C14 124.8(7) . . ? 
N6 C13 C14 124.0(6) . . ? 
C15 C14 C18 118.3(9) . . ? 
C15 C14 C13 122.4(6) . . ? 
C18 C14 C13 119.2(8) . . ? 
C14 C15 C16 118.7(7) . . ? 
C14 C15 H15 120.7 . . ? 
C16 C15 H15 120.7 . . ? 
N8 C16 C15 123.5(9) . . ? 
N8 C16 H16 118.2 . . ? 
C15 C16 H16 118.2 . . ? 
N8 C17 C18 124.5(8) . . ? 
N8 C17 H17 117.8 . . ? 
C18 C17 H17 117.8 . . ? 
C17 C18 C14 117.8(9) . . ? 
C17 C18 H18 121.1 . . ? 
C14 C18 H18 121.1 . . ? 
N7 C19 C12 110.9(7) . . ? 
N7 C19 C20 120.4(10) . . ? 
C12 C19 C20 128.5(12) . . ? 
O12 C20 O11 123.2(11) . . ? 
O12 C20 C19 117.2(15) . . ? 
O11 C20 C19 119.5(11) . . ? 
H13A O13 H13B 116(2) . . ? 
H14A O14 H14B 116(2) . . ? 
H15A O15 H15B 116(2) . . ? 
 
_diffrn_measured_fraction_theta_max    0.981 
_diffrn_reflns_theta_full              27.10 
_diffrn_measured_fraction_theta_full   0.981 
_refine_diff_density_max    1.307 
_refine_diff_density_min   -1.000 
_refine_diff_density_rms    0.142 

####





 
 
data_3-Dy 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C40 H46 Dy2 N12 O42' 
_chemical_formula_weight          1691.89 
 
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                    13.7707(5) 
_cell_length_b                    13.8802(3) 
_cell_length_c                    17.8970(5) 
_cell_angle_alpha                 82.980(2) 
_cell_angle_beta                  81.471(3) 
_cell_angle_gamma                 70.077(2) 
_cell_volume                      3171.07(16) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     13126
_cell_measurement_theta_min       2.3036
_cell_measurement_theta_max       29.2172
 
_exptl_crystal_description        block 
_exptl_crystal_colour             yellow 
_exptl_crystal_size_max           0.14 
_exptl_crystal_size_mid           0.11 
_exptl_crystal_size_min           0.09 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.772 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1676 
_exptl_absorpt_coefficient_mu     2.453 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.7252 
_exptl_absorpt_correction_T_max   0.8094 
_exptl_absorpt_process_details    

;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
; 
 
_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   'Xcalibur, Eos' 
_diffrn_measurement_method        'ω scans'
_diffrn_detector_area_resol_mean  16.2083
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             34276 
_diffrn_reflns_av_R_equivalents   0.0427 
_diffrn_reflns_av_sigmaI/netI     0.0542 
_diffrn_reflns_limit_h_min        -17 
_diffrn_reflns_limit_h_max        17 
_diffrn_reflns_limit_k_min        -17 
_diffrn_reflns_limit_k_max        17 
_diffrn_reflns_limit_l_min        -22 
_diffrn_reflns_limit_l_max        22 
_diffrn_reflns_theta_min          2.31 
_diffrn_reflns_theta_max          27.10 
_reflns_number_total              13794 
_reflns_number_gt                 11134 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        

;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
 
_computing_cell_refinement        

;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;

 
_computing_data_reduction         

;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_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)+(0.0600P)²+5.0000P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          13794 
_refine_ls_number_parameters      928 
_refine_ls_number_restraints      252 
_refine_ls_R_factor_all           0.0527 
_refine_ls_R_factor_gt            0.0387 
_refine_ls_wR_factor_ref          0.1153 
_refine_ls_wR_factor_gt           0.1050 
_refine_ls_goodness_of_fit_ref    1.007 
_refine_ls_restrained_S_all       1.011 
_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 0.908255(16) 0.467726(15) 0.142204(11) 0.02247(7) Uani 1 1 d . . . 
Dy2 Dy 0.529930(16) 0.600489(17) 0.367049(12) 0.02603(7) Uani 1 1 d . . . 
O1 O 0.6991(2) 0.5153(3) 0.31562(19) 0.0339(8) Uani 1 1 d . . . 
O2 O 0.8677(3) 0.4534(3) 0.27807(18) 0.0305(7) Uani 1 1 d . . . 
O3 O 0.5948(2) 0.4514(3) 0.44630(19) 0.0312(8) Uani 1 1 d . . . 
O4 O 0.6266(2) 0.4105(3) 0.56588(19) 0.0332(8) Uani 1 1 d . . . 
O5 O 0.9083(3) 0.6242(2) 0.06824(17) 0.0276(7) Uani 1 1 d . . . 
O6 O 0.9429(3) 0.5869(2) -0.05287(18) 0.0265(7) Uani 1 1 d . . . 
O7 O 0.9833(3) 0.6873(3) -0.1893(2) 0.0470(11) Uani 1 1 d . . . 
O8 O 0.8927(4) 0.8477(3) -0.2221(2) 0.0632(14) Uani 1 1 d . . . 
O9 O 1.3258(4) 0.0357(6) 0.4851(4) 0.112(3) Uani 1 1 d . . . 
O10 O 1.3179(4) 0.0424(5) 0.6076(3) 0.0792(16) Uani 1 1 d . . . 
O11 O 1.1856(4) 0.0911(4) 0.7155(3) 0.0681(14) Uani 1 1 d . . . 
O12 O 1.0147(4) 0.1371(4) 0.7394(3) 0.0627(13) Uani 1 1 d . . . 
O13 O 0.5998(6) 1.2759(5) -0.0674(5) 0.111(3) Uani 1 1 d . . . 
O14 O 0.5709(5) 1.3068(4) 0.0536(5) 0.108(3) Uani 1 1 d . . . 
O15 O 0.5603(5) 1.2169(5) 0.1766(4) 0.105(2) Uani 1 1 d . . . 
O16 O 0.5756(7) 1.0579(6) 0.2237(4) 0.114(3) Uani 1 1 d . . . 
O17W O 1.0216(3) 0.5332(3) 0.1902(2) 0.0447(10) Uani 1 1 d . . . 
O18W O 0.8531(3) 0.4517(3) 0.0253(2) 0.0343(8) Uani 1 1 d . . . 
O19W O 0.7509(3) 0.6038(3) 0.1713(2) 0.0418(10) Uani 1 1 d . . . 
O20W O 0.7901(3) 0.3724(3) 0.1632(2) 0.0435(10) Uani 1 1 d . . . 
O21W O 0.4910(3) 0.4713(3) 0.3158(3) 0.0517(11) Uani 1 1 d . . . 
O22W O 0.5405(3) 0.6545(3) 0.4865(2) 0.0398(9) Uani 1 1 d . . . 
O23W O 0.3951(3) 0.7657(3) 0.3626(3) 0.0531(11) Uani 1 1 d . . . 
O24W O 0.6157(3) 0.7267(3) 0.3402(2) 0.0484(11) Uani 1 1 d . . . 
O25W O 0.5144(4) 0.6508(4) 0.2367(2) 0.0586(12) Uani 1 1 d . . . 
N1 N 0.9188(3) 0.4159(3) 0.4218(2) 0.0233(8) Uani 1 1 d . . . 
H1 H 0.9709 0.4152 0.3884 0.028 Uiso 1 1 calc R . . 
N2 N 0.8293(3) 0.4002(3) 0.5323(2) 0.0249(8) Uani 1 1 d . . . 
N3 N 1.1949(3) 0.3214(3) 0.6078(3) 0.0382(11) Uani 1 1 d . . . 
N4 N 0.8988(3) 0.8244(3) 0.0304(2) 0.0260(8) Uani 1 1 d . . . 
N5 N 0.8989(3) 0.9078(3) -0.0829(2) 0.0284(9) Uani 1 1 d . . . 
H5 H 0.8934 0.9578 -0.1173 0.034 Uiso 1 1 calc R . . 
N6 N 0.8334(4) 1.1931(3) 0.0955(3) 0.0455(12) Uani 1 1 d . . . 
N7 N 1.1117(4) 0.0969(4) 0.4909(3) 0.0432(11) Uani 1 1 d . . . 
H7A H 1.1405 0.0883 0.4451 0.052 Uiso 1 1 calc R . . 
N8 N 0.9925(4) 0.1292(3) 0.5894(3) 0.0375(10) Uani 1 1 d . . . 
N9 N 0.7727(4) 0.2021(4) 0.3686(3) 0.0518(13) Uani 1 1 d . . . 
N10 N 0.6199(4) 1.0704(4) -0.0296(3) 0.0516(13) Uani 1 1 d . . . 
H10A H 0.6260 1.0840 -0.0779 0.062 Uiso 1 1 calc R . . 
N11 N 0.6140(4) 0.9861(4) 0.0808(3) 0.0481(12) Uani 1 1 d . . . 
N12 N 0.6795(5) 0.7052(6) -0.0986(5) 0.079(2) Uani 1 1 d . . . 
C1 C 0.7926(3) 0.4707(3) 0.3280(3) 0.0234(9) Uani 1 1 d . . . 
C2 C 0.6527(4) 0.4310(3) 0.4982(3) 0.0272(10) Uani 1 1 d . . . 
C3 C 0.7635(3) 0.4265(3) 0.4771(2) 0.0225(9) Uani 1 1 d . . . 
C4 C 0.8183(3) 0.4390(3) 0.4074(3) 0.0239(9) Uani 1 1 d . . . 
C5 C 0.9224(4) 0.3943(3) 0.4968(3) 0.0240(9) Uani 1 1 d . . . 
C6 C 1.0167(4) 0.3691(4) 0.5347(3) 0.0271(10) Uani 1 1 d . . . 
C7 C 1.1134(4) 0.3509(4) 0.4935(3) 0.0367(12) Uani 1 1 d . . . 
H7 H 1.1205 0.3549 0.4408 0.044 Uiso 1 1 calc R . . 
C8 C 1.2003(4) 0.3262(5) 0.5327(4) 0.0429(13) Uani 1 1 d . . . 
H8 H 1.2654 0.3125 0.5048 0.051 Uiso 1 1 calc R . . 
C9 C 1.1013(4) 0.3401(4) 0.6464(3) 0.0381(12) Uani 1 1 d . . . 
H9 H 1.0960 0.3371 0.6990 0.046 Uiso 1 1 calc R . . 
C10 C 1.0116(4) 0.3637(4) 0.6128(3) 0.0320(11) Uani 1 1 d . . . 
H10 H 0.9478 0.3760 0.6425 0.038 Uiso 1 1 calc R . . 
C11 C 0.9239(3) 0.6480(3) -0.0008(3) 0.0240(9) Uani 1 1 d . . . 
C12 C 0.9322(4) 0.7790(4) -0.1744(3) 0.0352(12) Uani 1 1 d . . . 
C13 C 0.9193(3) 0.8081(3) -0.0948(3) 0.0261(10) Uani 1 1 d . . . 
C14 C 0.9175(4) 0.7567(3) -0.0241(3) 0.0238(9) Uani 1 1 d . . . 
C15 C 0.8890(4) 0.9152(4) -0.0074(3) 0.0269(10) Uani 1 1 d . . . 
C16 C 0.8696(4) 1.0114(4) 0.0278(3) 0.0309(11) Uani 1 1 d . . . 
C17 C 0.8586(5) 1.0138(4) 0.1051(3) 0.0410(13) Uani 1 1 d . . . 
H17 H 0.8630 0.9540 0.1362 0.049 Uiso 1 1 calc R . . 
C18 C 0.8408(5) 1.1056(4) 0.1367(4) 0.0449(14) Uani 1 1 d . . . 
H18 H 0.8337 1.1056 0.1892 0.054 Uiso 1 1 calc R . . 
C19 C 0.8448(5) 1.1903(4) 0.0214(4) 0.0462(15) Uani 1 1 d . . . 
H19 H 0.8406 1.2513 -0.0080 0.055 Uiso 1 1 calc R . . 
C20 C 0.8625(4) 1.1035(4) -0.0159(3) 0.0382(12) Uani 1 1 d . . . 
H20 H 0.8694 1.1063 -0.0686 0.046 Uiso 1 1 calc R . . 
C21 C 1.2761(5) 0.0524(6) 0.5471(5) 0.0638(19) Uani 1 1 d . . . 
C22 C 1.0958(6) 0.1111(5) 0.6954(4) 0.0512(16) Uani 1 1 d . . . 
C23 C 1.0890(4) 0.1036(4) 0.6150(3) 0.0379(12) Uani 1 1 d . . . 
C24 C 1.1607(5) 0.0850(4) 0.5534(4) 0.0432(14) Uani 1 1 d . . . 
C25 C 1.0105(4) 0.1242(4) 0.5143(3) 0.0334(11) Uani 1 1 d . . . 
C26 C 0.9290(4) 0.1486(4) 0.4642(3) 0.0361(12) Uani 1 1 d . . . 
C27 C 0.8282(5) 0.1556(4) 0.4917(4) 0.0435(13) Uani 1 1 d . . . 
H27 H 0.8106 0.1419 0.5431 0.052 Uiso 1 1 calc R . . 
C28 C 0.7533(5) 0.1830(5) 0.4423(4) 0.0513(16) Uani 1 1 d . . . 
H28 H 0.6854 0.1884 0.4622 0.062 Uiso 1 1 calc R . . 
C29 C 0.8701(6) 0.1945(5) 0.3421(4) 0.0557(17) Uani 1 1 d . . . 
H29 H 0.8855 0.2074 0.2903 0.067 Uiso 1 1 calc R . . 
C30 C 0.9494(5) 0.1685(5) 0.3869(4) 0.0489(15) Uani 1 1 d . . . 
H30 H 1.0163 0.1644 0.3654 0.059 Uiso 1 1 calc R . . 
C31 C 0.5899(6) 1.2474(6) 0.0008(7) 0.077(3) Uani 1 1 d . . . 
C32 C 0.5743(7) 1.1213(7) 0.1714(6) 0.078(3) Uani 1 1 d . . . 
C33 C 0.5967(5) 1.0876(5) 0.0926(4) 0.0533(17) Uani 1 1 d . . . 
C34 C 0.6013(5) 1.1375(5) 0.0231(4) 0.0530(17) Uani 1 1 d . . . 
C35 C 0.6271(4) 0.9801(4) 0.0063(4) 0.0411(13) Uani 1 1 d . . . 
C36 C 0.6465(4) 0.8859(5) -0.0293(4) 0.0454(14) Uani 1 1 d . . . 
C37 C 0.6609(5) 0.8850(6) -0.1073(4) 0.0610(18) Uani 1 1 d . . . 
H37 H 0.6594 0.9442 -0.1384 0.073 Uiso 1 1 calc R . . 
C38 C 0.6777(6) 0.7926(8) -0.1373(5) 0.081(3) Uani 1 1 d . . . 
H38 H 0.6888 0.7923 -0.1898 0.098 Uiso 1 1 calc R . . 
C39 C 0.6659(5) 0.7082(6) -0.0247(6) 0.070(2) Uani 1 1 d . . . 
H39 H 0.6674 0.6476 0.0044 0.084 Uiso 1 1 calc R . . 
C40 C 0.6495(5) 0.7944(5) 0.0132(4) 0.0545(17) Uani 1 1 d . . . 
H40 H 0.6407 0.7912 0.0659 0.065 Uiso 1 1 calc R . . 
O26W O 0.8546(5) 0.0611(4) 0.7944(4) 0.0911(19) Uani 1 1 d . . . 
O27W O 0.9645(4) 0.2749(4) 0.8471(3) 0.0674(13) Uani 1 1 d . . . 
O28W O 0.5131(5) 0.8543(5) 0.5026(5) 0.121(3) Uani 1 1 d . . . 
O29W O 0.2064(3) 0.7428(3) 0.3406(2) 0.0533(11) Uani 1 1 d . . . 
O30W O 0.7585(4) 0.8021(4) 0.1712(3) 0.0678(14) Uani 1 1 d . . . 
O31W O 0.0954(4) 0.3712(5) 0.3072(3) 0.092(2) Uani 1 1 d . . . 
O32W O 0.6424(4) 0.3105(4) 0.2652(3) 0.0604(12) Uani 1 1 d . . . 
O33W O 0.6640(5) 0.4597(4) 0.9949(4) 0.093(2) Uani 1 1 d . . . 
O34W O 0.2430(6) 0.6806(7) 0.1908(4) 0.127(3) Uani 1 1 d . . . 
O35W O 0.5202(7) 0.5269(6) 0.1287(4) 0.126(3) Uani 1 1 d . . . 
O36A O 0.3143(19) 0.3874(19) 0.3281(14) 0.174(8) Uani 0.50 1 d PU . . 
O36B O 0.2910(12) 0.4586(13) 0.3367(9) 0.108(4) Uani 0.50 1 d PU . . 
O37A O 0.7611(18) 0.5395(17) 0.8091(13) 0.078(6) Uani 0.25 1 d PU . . 
O37B O 0.6507(9) 0.5442(7) 0.8357(6) 0.116(3) Uani 0.75 1 d PU . . 
O38A O 0.214(3) 1.025(3) 0.3425(19) 0.121(7) Uani 0.25 1 d PU . . 
O39A O 0.3085(19) 0.2507(18) 0.3454(13) 0.180(7) Uani 0.50 1 d PU . . 
O40A O 0.4141(17) 0.9548(14) 0.3094(12) 0.149(5) Uani 0.50 1 d PU . . 
O41A O 0.5385(19) 0.8878(18) 0.2325(14) 0.186(7) Uani 0.50 1 d PU . . 
O42A O 0.3816(13) 0.8471(11) 0.1870(8) 0.113(4) Uani 0.50 1 d PU . . 
O38B O 0.2310(9) 1.1195(10) 0.3458(6) 0.141(4) Uani 0.75 1 d PU . . 
O39B O 0.4292(15) 0.1790(14) 0.3452(10) 0.135(5) Uani 0.50 1 d PU . . 
O40B O 0.2940(17) 0.9578(15) 0.2773(13) 0.164(5) Uani 0.50 1 d PU . . 
O41B O 0.4800(11) 0.8498(9) 0.1759(7) 0.089(3) Uani 0.50 1 d PU . . 
O42B O 0.4883(17) 0.9326(14) 0.3444(12) 0.147(5) Uani 0.50 1 d PU . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Dy1 O7 2.305(4) 2_765 ? 
Dy1 O17W 2.357(4) . ? 
Dy1 O6 2.366(3) 2_765 ? 
Dy1 O19W 2.377(3) . ? 
Dy1 O18W 2.388(4) . ? 
Dy1 O20W 2.388(4) . ? 
Dy1 O5 2.401(3) . ? 
Dy1 O2 2.412(3) . ? 
Dy2 O1 2.329(3) . ? 
Dy2 O3 2.344(3) . ? 
Dy2 O4 2.351(3) 2_666 ? 
Dy2 O21W 2.355(4) . ? 
Dy2 O25W 2.371(4) . ? 
Dy2 O22W 2.391(4) . ? 
Dy2 O24W 2.394(4) . ? 
Dy2 O23W 2.411(4) . ? 
O1 C1 1.264(5) . ? 
O2 C1 1.239(5) . ? 
O3 C2 1.258(6) . ? 
O4 C2 1.237(6) . ? 
O4 Dy2 2.351(3) 2_666 ? 
O5 C11 1.247(5) . ? 
O6 C11 1.275(6) . ? 
O6 Dy1 2.366(3) 2_765 ? 
O7 C12 1.266(6) . ? 
O7 Dy1 2.305(4) 2_765 ? 
O8 C12 1.233(6) . ? 
O9 C21 1.217(9) . ? 
O10 C21 1.272(9) . ? 
O11 C22 1.269(8) . ? 
O12 C22 1.237(8) . ? 
O13 C31 1.239(12) . ? 
O14 C31 1.269(12) . ? 
O15 C32 1.288(10) . ? 
O16 C32 1.202(11) . ? 
N1 C5 1.344(6) . ? 
N1 C4 1.366(6) . ? 
N2 C5 1.324(6) . ? 
N2 C3 1.371(6) . ? 
N3 C9 1.326(7) . ? 
N3 C8 1.329(7) . ? 
N4 C15 1.330(6) . ? 
N4 C14 1.374(6) . ? 
N5 C15 1.350(6) . ? 
N5 C13 1.354(6) . ? 
N6 C19 1.315(8) . ? 
N6 C18 1.322(8) . ? 
N7 C25 1.329(7) . ? 
N7 C24 1.354(7) . ? 
N8 C25 1.336(7) . ? 
N8 C23 1.385(7) . ? 
N9 C28 1.319(9) . ? 
N9 C29 1.328(9) . ? 
N10 C35 1.315(7) . ? 
N10 C34 1.341(9) . ? 
N11 C35 1.328(8) . ? 
N11 C33 1.383(8) . ? 
N12 C39 1.312(11) . ? 
N12 C38 1.316(12) . ? 
C1 C4 1.493(6) . ? 
C2 C3 1.498(6) . ? 
C3 C4 1.383(6) . ? 
C5 C6 1.471(6) . ? 
C6 C7 1.381(7) . ? 
C6 C10 1.382(7) . ? 
C7 C8 1.398(7) . ? 
C9 C10 1.375(7) . ? 
C11 C14 1.492(6) . ? 
C12 C13 1.497(7) . ? 
C13 C14 1.374(6) . ? 
C15 C16 1.470(7) . ? 
C16 C17 1.372(8) . ? 
C16 C20 1.397(7) . ? 
C17 C18 1.388(8) . ? 
C19 C20 1.380(8) . ? 
C21 C24 1.487(9) . ? 
C22 C23 1.475(8) . ? 
C23 C24 1.353(8) . ? 
C25 C26 1.465(7) . ? 
C26 C27 1.376(8) . ? 
C26 C30 1.383(8) . ? 
C27 C28 1.382(8) . ? 
C29 C30 1.373(9) . ? 
C31 C34 1.490(10) . ? 
C32 C33 1.495(11) . ? 
C33 C34 1.352(10) . ? 
C35 C36 1.449(9) . ? 
C36 C37 1.382(10) . ? 
C36 C40 1.389(9) . ? 
C37 C38 1.384(11) . ? 
C39 C40 1.383(10) . ? 
O36A O36B 0.95(2) . ? 
O37A O37B 1.51(2) . ? 
O38A O38B 1.42(3) . ? 
O38A O40B 1.62(4) . ? 
O39A O39B 1.62(3) . ? 
O40A O42B 1.21(2) . ? 
O40A O40B 1.82(3) . ? 
O41A O41B 1.62(3) . ? 
O42A O41B 1.353(19) . ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
O7 Dy1 O17W 82.90(16) 2_765 . ? 
O7 Dy1 O6 71.84(12) 2_765 2_765 ? 
O17W Dy1 O6 79.63(13) . 2_765 ? 
O7 Dy1 O19W 143.57(12) 2_765 . ? 
O17W Dy1 O19W 98.06(15) . . ? 
O6 Dy1 O19W 144.40(11) 2_765 . ? 
O7 Dy1 O18W 111.39(13) 2_765 . ? 
O17W Dy1 O18W 141.01(13) . . ? 
O6 Dy1 O18W 71.66(12) 2_765 . ? 
O19W Dy1 O18W 90.73(14) . . ? 
O7 Dy1 O20W 80.61(16) 2_765 . ? 
O17W Dy1 O20W 149.41(14) . . ? 
O6 Dy1 O20W 118.69(12) 2_765 . ? 
O19W Dy1 O20W 80.78(14) . . ? 
O18W Dy1 O20W 69.44(12) . . ? 
O7 Dy1 O5 142.74(14) 2_765 . ? 
O17W Dy1 O5 71.81(13) . . ? 
O6 Dy1 O5 76.93(10) 2_765 . ? 
O19W Dy1 O5 68.80(11) . . ? 
O18W Dy1 O5 76.36(11) . . ? 
O20W Dy1 O5 133.42(13) . . ? 
O7 Dy1 O2 71.53(12) 2_765 . ? 
O17W Dy1 O2 74.73(13) . . ? 
O6 Dy1 O2 137.26(11) 2_765 . ? 
O19W Dy1 O2 73.65(12) . . ? 
O18W Dy1 O2 143.65(12) . . ? 
O20W Dy1 O2 75.67(13) . . ? 
O5 Dy1 O2 124.45(11) . . ? 
O1 Dy2 O3 72.78(11) . . ? 
O1 Dy2 O4 148.08(12) . 2_666 ? 
O3 Dy2 O4 80.14(11) . 2_666 ? 
O1 Dy2 O21W 83.73(14) . . ? 
O3 Dy2 O21W 74.76(14) . . ? 
O4 Dy2 O21W 72.92(14) 2_666 . ? 
O1 Dy2 O25W 80.14(15) . . ? 
O3 Dy2 O25W 139.49(15) . . ? 
O4 Dy2 O25W 112.07(15) 2_666 . ? 
O21W Dy2 O25W 72.80(16) . . ? 
O1 Dy2 O22W 107.27(13) . . ? 
O3 Dy2 O22W 72.97(13) . . ? 
O4 Dy2 O22W 79.83(13) 2_666 . ? 
O21W Dy2 O22W 140.62(14) . . ? 
O25W Dy2 O22W 145.39(15) . . ? 
O1 Dy2 O24W 73.53(14) . . ? 
O3 Dy2 O24W 121.64(12) . . ? 
O4 Dy2 O24W 136.90(14) 2_666 . ? 
O21W Dy2 O24W 144.49(16) . . ? 
O25W Dy2 O24W 76.64(16) . . ? 
O22W Dy2 O24W 73.50(14) . . ? 
O1 Dy2 O23W 141.85(13) . . ? 
O3 Dy2 O23W 142.72(13) . . ? 
O4 Dy2 O23W 69.32(13) 2_666 . ? 
O21W Dy2 O23W 114.00(16) . . ? 
O25W Dy2 O23W 74.15(16) . . ? 
O22W Dy2 O23W 80.83(15) . . ? 
O24W Dy2 O23W 73.43(14) . . ? 
C1 O1 Dy2 146.5(3) . . ? 
C1 O2 Dy1 141.2(3) . . ? 
C2 O3 Dy2 132.1(3) . . ? 
C2 O4 Dy2 133.0(3) . 2_666 ? 
C11 O5 Dy1 134.3(3) . . ? 
C11 O6 Dy1 129.4(3) . 2_765 ? 
C12 O7 Dy1 144.2(4) . 2_765 ? 
C5 N1 C4 108.3(4) . . ? 
C5 N2 C3 106.0(4) . . ? 
C9 N3 C8 117.1(5) . . ? 
C15 N4 C14 105.3(4) . . ? 
C15 N5 C13 108.0(4) . . ? 
C19 N6 C18 117.0(5) . . ? 
C25 N7 C24 106.7(5) . . ? 
C25 N8 C23 106.2(5) . . ? 
C28 N9 C29 116.7(6) . . ? 
C35 N10 C34 107.5(6) . . ? 
C35 N11 C33 106.7(5) . . ? 
C39 N12 C38 115.1(7) . . ? 
O2 C1 O1 124.3(4) . . ? 
O2 C1 C4 115.8(4) . . ? 
O1 C1 C4 119.8(4) . . ? 
O4 C2 O3 125.2(4) . . ? 
O4 C2 C3 116.6(4) . . ? 
O3 C2 C3 118.2(4) . . ? 
N2 C3 C4 109.5(4) . . ? 
N2 C3 C2 119.3(4) . . ? 
C4 C3 C2 131.1(4) . . ? 
N1 C4 C3 105.2(4) . . ? 
N1 C4 C1 118.9(4) . . ? 
C3 C4 C1 135.9(4) . . ? 
N2 C5 N1 111.0(4) . . ? 
N2 C5 C6 124.3(4) . . ? 
N1 C5 C6 124.7(4) . . ? 
C7 C6 C10 117.7(5) . . ? 
C7 C6 C5 121.1(5) . . ? 
C10 C6 C5 121.3(4) . . ? 
C6 C7 C8 118.5(5) . . ? 
N3 C8 C7 123.6(5) . . ? 
N3 C9 C10 123.4(5) . . ? 
C9 C10 C6 119.8(5) . . ? 
O5 C11 O6 124.8(4) . . ? 
O5 C11 C14 117.3(4) . . ? 
O6 C11 C14 117.8(4) . . ? 
O8 C12 O7 123.8(5) . . ? 
O8 C12 C13 116.9(5) . . ? 
O7 C12 C13 119.3(4) . . ? 
N5 C13 C14 106.0(4) . . ? 
N5 C13 C12 118.8(4) . . ? 
C14 C13 C12 135.1(4) . . ? 
N4 C14 C13 109.6(4) . . ? 
N4 C14 C11 119.5(4) . . ? 
C13 C14 C11 130.7(4) . . ? 
N4 C15 N5 111.0(4) . . ? 
N4 C15 C16 124.8(5) . . ? 
N5 C15 C16 124.1(4) . . ? 
C17 C16 C20 117.4(5) . . ? 
C17 C16 C15 121.2(4) . . ? 
C20 C16 C15 121.5(5) . . ? 
C16 C17 C18 119.9(5) . . ? 
N6 C18 C17 122.9(6) . . ? 
N6 C19 C20 124.9(5) . . ? 
C19 C20 C16 117.9(6) . . ? 
O9 C21 O10 123.3(7) . . ? 
O9 C21 C24 119.0(7) . . ? 
O10 C21 C24 117.7(7) . . ? 
O12 C22 O11 123.5(6) . . ? 
O12 C22 C23 119.0(6) . . ? 
O11 C22 C23 117.5(6) . . ? 
C24 C23 N8 106.9(5) . . ? 
C24 C23 C22 132.9(6) . . ? 
N8 C23 C22 119.8(5) . . ? 
C23 C24 N7 109.0(5) . . ? 
C23 C24 C21 130.5(6) . . ? 
N7 C24 C21 120.4(6) . . ? 
N7 C25 N8 111.2(5) . . ? 
N7 C25 C26 124.6(5) . . ? 
N8 C25 C26 124.2(5) . . ? 
C27 C26 C30 116.9(5) . . ? 
C27 C26 C25 121.9(5) . . ? 
C30 C26 C25 121.2(5) . . ? 
C26 C27 C28 119.6(6) . . ? 
N9 C28 C27 123.6(6) . . ? 
N9 C29 C30 123.7(6) . . ? 
C29 C30 C26 119.5(6) . . ? 
O13 C31 O14 123.6(8) . . ? 
O13 C31 C34 118.9(9) . . ? 
O14 C31 C34 117.5(9) . . ? 
O16 C32 O15 125.6(9) . . ? 
O16 C32 C33 118.7(8) . . ? 
O15 C32 C33 115.6(9) . . ? 
C34 C33 N11 106.1(6) . . ? 
C34 C33 C32 133.6(7) . . ? 
N11 C33 C32 120.2(7) . . ? 
N10 C34 C33 109.0(6) . . ? 
N10 C34 C31 120.9(7) . . ? 
C33 C34 C31 130.1(8) . . ? 
N10 C35 N11 110.7(6) . . ? 
N10 C35 C36 125.6(6) . . ? 
N11 C35 C36 123.7(5) . . ? 
C37 C36 C40 117.7(6) . . ? 
C37 C36 C35 120.5(6) . . ? 
C40 C36 C35 121.7(6) . . ? 
C36 C37 C38 117.4(8) . . ? 
N12 C38 C37 126.2(9) . . ? 
N12 C39 C40 125.2(8) . . ? 
C39 C40 C36 118.4(8) . . ? 
O38B O38A O40B 111(2) . . ? 
O42B O40A O40B 162(2) . . ? 
O38A O40B O40A 97.8(19) . . ? 
O42A O41B O41A 127.6(15) . . ? 
 
_diffrn_measured_fraction_theta_max    0.986 
_diffrn_reflns_theta_full              27.10 
_diffrn_measured_fraction_theta_full   0.986 
_refine_diff_density_max    0.953 
_refine_diff_density_min   -1.026 
_refine_diff_density_rms    0.124 


# Start Validation Reply Form

_vrf_PLAT306_3-Dy
;
PROBLEM:
  Isolated Oxygen Atom (H-atoms Missing ?) .......       O26W     
 Isolated Oxygen Atom (H-atoms Missing ?) .......       O27W     
 Isolated Oxygen Atom (H-atoms Missing ?) .......       O28W     
 Isolated Oxygen Atom (H-atoms Missing ?) .......       O29W     
 Isolated Oxygen Atom (H-atoms Missing ?) .......       O30W     
 Isolated Oxygen Atom (H-atoms Missing ?) .......       O31W     
 Isolated Oxygen Atom (H-atoms Missing ?) .......       O32W     
 Isolated Oxygen Atom (H-atoms Missing ?) .......       O33W     
 Isolated Oxygen Atom (H-atoms Missing ?) .......       O34W     
 Isolated Oxygen Atom (H-atoms Missing ?) .......       O35W     
 

RESPONSE: This is because the hydrogen atoms attaching to free water molecules have not been added.
; 





data_4-Dy
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C40 H46 Dy3 N13 O33' 
_chemical_formula_weight          1724.40 
 
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           monoclinic 
_symmetry_space_group_name_H-M    C2/c 

loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y, -z+1/2' 
 'x+1/2, y+1/2, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y, z-1/2' 
 '-x+1/2, -y+1/2, -z' 
 'x+1/2, -y+1/2, z-1/2' 
 
_cell_length_a                    20.836(4) 
_cell_length_b                    9.4722(16) 
_cell_length_c                    28.136(5) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  106.372(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      5327.8(17) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     298(2) 
_cell_measurement_reflns_used     7041
_cell_measurement_theta_min       2.1667
_cell_measurement_theta_max       27.4835
 
_exptl_crystal_description        Prism 
_exptl_crystal_colour             colorless 
_exptl_crystal_size_max           0.20 
_exptl_crystal_size_mid           0.18 
_exptl_crystal_size_min           0.16 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     2.150 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              3356 
_exptl_absorpt_coefficient_mu     4.281 
_exptl_absorpt_correction_type    Multi-scan 
_exptl_absorpt_correction_T_min   0.4814 
_exptl_absorpt_correction_T_max   0.5475 
_exptl_absorpt_process_details    

;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;  
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       298(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   ? 
_diffrn_measurement_method        'CCD_Profile_fitting' 
_diffrn_detector_area_resol_mean  13.6612  
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             20224 
_diffrn_reflns_av_R_equivalents   0.0509 
_diffrn_reflns_av_sigmaI/netI     0.0501 
_diffrn_reflns_limit_h_min        -26 
_diffrn_reflns_limit_h_max        26 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -36 
_diffrn_reflns_limit_l_max        33 
_diffrn_reflns_theta_min          2.04 
_diffrn_reflns_theta_max          27.49 
_reflns_number_total              6034 
_reflns_number_gt                 5670 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement        'CrystalClear (Rigaku Inc., 2007)'

_computing_data_reduction         'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_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)+(0.0628P)²+42.0000P] 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        0.00049(5) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          6034 
_refine_ls_number_parameters      460 
_refine_ls_number_restraints      61 
_refine_ls_R_factor_all           0.0444 
_refine_ls_R_factor_gt            0.0419 
_refine_ls_wR_factor_ref          0.1205 
_refine_ls_wR_factor_gt           0.1169 
_refine_ls_goodness_of_fit_ref    1.023 
_refine_ls_restrained_S_all       1.022 
_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 
Dy1 Dy 0.186955(11) 0.18781(2) 0.215964(9) 0.02016(11) Uani 1 1 d . . . 
Dy2 Dy 0.0000 0.75515(3) 0.2500 0.02344(12) Uani 1 2 d S . . 
O1 O 0.3288(2) 0.4646(4) 0.32618(16) 0.0306(9) Uani 1 1 d . . . 
O2 O 0.2488(2) 0.3302(4) 0.27991(16) 0.0276(9) Uani 1 1 d . . . 
O3 O 0.2673(2) -0.1349(4) 0.32454(16) 0.0273(8) Uani 1 1 d . . . 
O4 O 0.21435(19) 0.0561(4) 0.28874(15) 0.0267(8) Uani 1 1 d . . . 
O5 O -0.0034(2) -0.0368(4) 0.19909(19) 0.0370(11) Uani 1 1 d . . . 
O6 O 0.09004(19) 0.0887(4) 0.22616(17) 0.0319(9) Uani 1 1 d . . . 
O7 O 0.11852(18) 0.3733(4) 0.22665(16) 0.0269(8) Uani 1 1 d . . . 
O8 O 0.0546(2) 0.5587(4) 0.22664(17) 0.0315(9) Uani 1 1 d . . . 
O9W O 0.2964(2) 0.1031(4) 0.21830(17) 0.0318(9) Uani 1 1 d D . . 
H9A H 0.3061 0.0162 0.2232 0.048 Uiso 1 1 d RD . . 
H9B H 0.3276 0.1530 0.2367 0.048 Uiso 1 1 d RD . . 
O10W O 0.1195(3) 0.2159(5) 0.13353(18) 0.0406(12) Uani 1 1 d D . . 
H10A H 0.100(4) 0.160(6) 0.110(2) 0.061 Uiso 1 1 d D . . 
H10B H 0.100(4) 0.296(4) 0.128(3) 0.061 Uiso 1 1 d D . . 
O11W O 0.0534(3) 0.7033(5) 0.33240(19) 0.0466(13) Uani 1 1 d D . . 
H11A H 0.070(4) 0.622(4) 0.339(3) 0.070 Uiso 1 1 d D . . 
H11B H 0.072(4) 0.761(6) 0.355(2) 0.070 Uiso 1 1 d D . . 
O12W O -0.1130(2) 0.8322(4) 0.23533(19) 0.0347(10) Uani 1 1 d D . . 
H12A H -0.1228 0.9052 0.2495 0.052 Uiso 1 1 d RD . . 
H12B H -0.1317 0.8382 0.2044 0.052 Uiso 1 1 d RD . . 
O13W O 0.1300(3) 0.9125(7) 0.3915(3) 0.0637(17) Uani 1 1 d D . . 
H13A H 0.169(2) 0.878(12) 0.397(3) 0.096 Uiso 1 1 d D . . 
H13B H 0.126(5) 0.947(12) 0.418(2) 0.096 Uiso 1 1 d D . . 
O14W O 0.7349(3) 0.1267(8) 0.5712(2) 0.0607(16) Uani 1 1 d D . . 
H14A H 0.705(3) 0.085(11) 0.549(3) 0.091 Uiso 1 1 d D . . 
H14B H 0.720(4) 0.145(12) 0.596(2) 0.091 Uiso 1 1 d D . . 
N1 N 0.4004(2) 0.2409(5) 0.3733(2) 0.0274(10) Uani 1 1 d . . . 
H1 H 0.423(4) 0.309(8) 0.376(3) 0.033 Uiso 1 1 d . . . 
N2 N 0.3775(2) 0.0143(5) 0.37554(18) 0.0239(9) Uani 1 1 d . . . 
N3 N 0.6158(3) 0.0427(7) 0.4939(2) 0.0440(14) Uani 1 1 d . . . 
N4 N -0.0745(2) 0.1911(5) 0.1561(2) 0.0273(11) Uani 1 1 d D . . 
H4 H -0.095(3) 0.113(4) 0.146(2) 0.033 Uiso 1 1 d D . . 
N5 N -0.0562(2) 0.4196(5) 0.16375(19) 0.0267(10) Uani 1 1 d . . . 
N6 N -0.2974(4) 0.3954(9) 0.0505(3) 0.073(3) Uani 1 1 d . . . 
C1 C 0.3023(3) 0.3470(5) 0.3134(2) 0.0238(11) Uani 1 1 d . . . 
C2 C 0.3374(3) 0.2228(6) 0.3410(2) 0.0234(11) Uani 1 1 d . . . 
C3 C 0.4225(3) 0.1138(5) 0.3927(2) 0.0247(11) Uani 1 1 d . . . 
C4 C 0.4887(3) 0.0893(6) 0.4277(2) 0.0285(12) Uani 1 1 d . . . 
C5 C 0.5311(4) 0.1990(8) 0.4487(3) 0.051(2) Uani 1 1 d . . . 
H5 H 0.5180 0.2919 0.4406 0.061 Uiso 1 1 calc R . . 
C6 C 0.5925(4) 0.1709(8) 0.4813(3) 0.054(2) Uani 1 1 d . . . 
H6 H 0.6193 0.2471 0.4955 0.065 Uiso 1 1 calc R . . 
C7 C 0.5754(3) -0.0640(8) 0.4736(3) 0.0413(16) Uani 1 1 d . . . 
H7 H 0.5903 -0.1557 0.4820 0.050 Uiso 1 1 calc R . . 
C8 C 0.5121(3) -0.0452(7) 0.4405(3) 0.0355(14) Uani 1 1 d . . . 
H8 H 0.4860 -0.1230 0.4272 0.043 Uiso 1 1 calc R . . 
C9 C 0.3244(3) 0.0810(5) 0.3430(2) 0.0213(10) Uani 1 1 d . . . 
C10 C 0.2642(3) -0.0032(5) 0.3164(2) 0.0236(11) Uani 1 1 d . . . 
C11 C 0.0283(3) 0.0767(6) 0.2037(2) 0.0270(11) Uani 1 1 d . . . 
C12 C -0.0098(3) 0.2054(6) 0.1841(2) 0.0247(11) Uani 1 1 d . . . 
C13 C -0.1004(3) 0.3208(6) 0.1445(2) 0.0269(12) Uani 1 1 d . . . 
C14 C -0.1690(3) 0.3454(7) 0.1122(2) 0.0316(13) Uani 1 1 d . . . 
C15 C -0.2093(4) 0.2388(8) 0.0897(4) 0.053(2) Uani 1 1 d . . . 
H15 H -0.1940 0.1462 0.0941 0.064 Uiso 1 1 calc R . . 
C16 C -0.2734(5) 0.2667(11) 0.0600(4) 0.073(3) Uani 1 1 d . . . 
H16 H -0.3006 0.1910 0.0461 0.088 Uiso 1 1 calc R . . 
C17 C -0.2589(5) 0.4998(10) 0.0748(4) 0.076(3) Uani 1 1 d . . . 
H17 H -0.2761 0.5910 0.0707 0.091 Uiso 1 1 calc R . . 
C18 C -0.1958(4) 0.4811(8) 0.1054(4) 0.058(2) Uani 1 1 d . . . 
H18 H -0.1712 0.5577 0.1215 0.070 Uiso 1 1 calc R . . 
C19 C 0.0016(3) 0.3506(6) 0.1888(2) 0.0232(11) Uani 1 1 d . . . 
C20 C 0.0621(3) 0.4330(5) 0.2160(2) 0.0212(10) Uani 1 1 d . . . 
N7 N 0.5141(6) 0.5572(17) 0.4421(5) 0.076(5) Uani 0.50 1 d PDU A 1 
O16 O 0.4817(9) 0.610(3) 0.4704(7) 0.140(7) Uani 0.50 1 d PDU A 1 
O17 O 0.5779(9) 0.544(3) 0.4583(7) 0.082(6) Uani 0.50 1 d PDU A 1 
O18 O 0.4819(8) 0.5118(15) 0.3991(5) 0.086(4) Uani 0.50 1 d PDU A 1 
O15W O 0.4363(7) 0.5112(12) 0.4337(4) 0.062(3) Uani 0.50 1 d P B 2 
O19W O 0.5910(9) 0.534(3) 0.4784(7) 0.070(6) Uani 0.50 1 d P C 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 O6 2.317(4) . ? 
Dy1 O2 2.326(4) . ? 
Dy1 O4 2.327(4) . ? 
Dy1 O7 2.335(4) . ? 
Dy1 O10W 2.364(5) . ? 
Dy1 O3 2.374(4) 4 ? 
Dy1 O9W 2.401(4) . ? 
Dy1 O1 2.401(4) 4_545 ? 
Dy2 O11W 2.324(5) . ? 
Dy2 O11W 2.324(5) 2 ? 
Dy2 O8 2.368(4) 2 ? 
Dy2 O8 2.368(4) . ? 
Dy2 O12W 2.388(4) 2 ? 
Dy2 O12W 2.388(4) . ? 
Dy2 O5 2.426(4) 2_565 ? 
Dy2 O5 2.426(4) 1_565 ? 
O1 C1 1.250(6) . ? 
O1 Dy1 2.401(4) 4 ? 
O2 C1 1.251(7) . ? 
O3 C10 1.267(6) . ? 
O3 Dy1 2.374(4) 4_545 ? 
O4 C10 1.243(7) . ? 
O5 C11 1.249(7) . ? 
O5 Dy2 2.426(4) 1_545 ? 
O6 C11 1.268(7) . ? 
O7 C20 1.262(6) . ? 
O8 C20 1.249(6) . ? 
O9W H9A 0.8500 . ? 
O9W H9B 0.8501 . ? 
O10W H10A 0.851(10) . ? 
O10W H10B 0.851(10) . ? 
O11W H11A 0.847(10) . ? 
O11W H11B 0.847(10) . ? 
O12W H12A 0.8500 . ? 
O12W H12B 0.8501 . ? 
O13W H13A 0.855(10) . ? 
O13W H13B 0.853(10) . ? 
O14W H14A 0.850(10) . ? 
O14W H14B 0.851(10) . ? 
N1 C3 1.349(7) . ? 
N1 C2 1.380(7) . ? 
N1 H1 0.79(7) . ? 
N2 C3 1.321(7) . ? 
N2 C9 1.375(7) . ? 
N3 C6 1.318(10) . ? 
N3 C7 1.336(10) . ? 
N4 C13 1.345(7) . ? 
N4 C12 1.362(7) . ? 
N4 H4 0.860(10) . ? 
N5 C13 1.319(7) . ? 
N5 C19 1.375(7) . ? 
N6 C16 1.317(12) . ? 
N6 C17 1.335(13) . ? 
C1 C2 1.484(7) . ? 
C2 C9 1.375(7) . ? 
C3 C4 1.470(8) . ? 
C4 C8 1.376(8) . ? 
C4 C5 1.384(9) . ? 
C5 C6 1.375(10) . ? 
C5 H5 0.9300 . ? 
C6 H6 0.9300 . ? 
C7 C8 1.394(9) . ? 
C7 H7 0.9300 . ? 
C8 H8 0.9300 . ? 
C9 C10 1.496(7) . ? 
C11 C12 1.475(8) . ? 
C12 C19 1.396(7) . ? 
C13 C14 1.480(8) . ? 
C14 C15 1.352(10) . ? 
C14 C18 1.393(9) . ? 
C15 C16 1.385(11) . ? 
C15 H15 0.9300 . ? 
C16 H16 0.9300 . ? 
C17 C18 1.364(12) . ? 
C17 H17 0.9300 . ? 
C18 H18 0.9300 . ? 
C19 C20 1.497(7) . ? 
N7 O18 1.280(12) . ? 
N7 O16 1.283(12) . ? 
N7 O17 1.285(12) . ? 
 
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 
O6 Dy1 O2 116.82(16) . . ? 
O6 Dy1 O4 71.34(14) . . ? 
O2 Dy1 O4 71.64(14) . . ? 
O6 Dy1 O7 72.78(14) . . ? 
O2 Dy1 O7 71.89(14) . . ? 
O4 Dy1 O7 107.30(15) . . ? 
O6 Dy1 O10W 82.48(18) . . ? 
O2 Dy1 O10W 137.76(15) . . ? 
O4 Dy1 O10W 148.67(16) . . ? 
O7 Dy1 O10W 79.97(17) . . ? 
O6 Dy1 O3 145.84(14) . 4 ? 
O2 Dy1 O3 75.62(15) . 4 ? 
O4 Dy1 O3 140.30(14) . 4 ? 
O7 Dy1 O3 82.62(14) . 4 ? 
O10W Dy1 O3 69.97(17) . 4 ? 
O6 Dy1 O9W 135.68(15) . . ? 
O2 Dy1 O9W 81.83(15) . . ? 
O4 Dy1 O9W 78.54(14) . . ? 
O7 Dy1 O9W 149.05(14) . . ? 
O10W Dy1 O9W 111.22(18) . . ? 
O3 Dy1 O9W 75.12(14) 4 . ? 
O6 Dy1 O1 72.63(16) . 4_545 ? 
O2 Dy1 O1 149.49(13) . 4_545 ? 
O4 Dy1 O1 85.87(14) . 4_545 ? 
O7 Dy1 O1 136.28(14) . 4_545 ? 
O10W Dy1 O1 69.74(15) . 4_545 ? 
O3 Dy1 O1 113.80(14) 4 4_545 ? 
O9W Dy1 O1 73.50(14) . 4_545 ? 
O11W Dy2 O11W 155.6(2) . 2 ? 
O11W Dy2 O8 71.89(17) . 2 ? 
O11W Dy2 O8 88.78(18) 2 2 ? 
O11W Dy2 O8 88.78(18) . . ? 
O11W Dy2 O8 71.89(17) 2 . ? 
O8 Dy2 O8 76.4(2) 2 . ? 
O11W Dy2 O12W 73.8(2) . 2 ? 
O11W Dy2 O12W 114.1(2) 2 2 ? 
O8 Dy2 O12W 136.02(14) 2 2 ? 
O8 Dy2 O12W 76.16(14) . 2 ? 
O11W Dy2 O12W 114.1(2) . . ? 
O11W Dy2 O12W 73.8(2) 2 . ? 
O8 Dy2 O12W 76.16(14) 2 . ? 
O8 Dy2 O12W 136.02(14) . . ? 
O12W Dy2 O12W 144.39(19) 2 . ? 
O11W Dy2 O5 69.91(17) . 2_565 ? 
O11W Dy2 O5 133.40(16) 2 2_565 ? 
O8 Dy2 O5 114.25(16) 2 2_565 ? 
O8 Dy2 O5 149.99(14) . 2_565 ? 
O12W Dy2 O5 77.67(15) 2 2_565 ? 
O12W Dy2 O5 73.54(14) . 2_565 ? 
O11W Dy2 O5 133.40(16) . 1_565 ? 
O11W Dy2 O5 69.91(17) 2 1_565 ? 
O8 Dy2 O5 149.99(14) 2 1_565 ? 
O8 Dy2 O5 114.25(16) . 1_565 ? 
O12W Dy2 O5 73.54(14) 2 1_565 ? 
O12W Dy2 O5 77.67(15) . 1_565 ? 
O5 Dy2 O5 71.3(2) 2_565 1_565 ? 
C1 O1 Dy1 130.9(4) . 4 ? 
C1 O2 Dy1 147.0(4) . . ? 
C10 O3 Dy1 128.0(4) . 4_545 ? 
C10 O4 Dy1 138.3(4) . . ? 
C11 O5 Dy2 135.3(4) . 1_545 ? 
C11 O6 Dy1 140.5(4) . . ? 
C20 O7 Dy1 150.2(4) . . ? 
C20 O8 Dy2 156.7(4) . . ? 
Dy1 O9W H9A 120.6 . . ? 
Dy1 O9W H9B 112.9 . . ? 
H9A O9W H9B 109.5 . . ? 
Dy1 O10W H10A 135(5) . . ? 
Dy1 O10W H10B 113(5) . . ? 
H10A O10W H10B 109.4(18) . . ? 
Dy2 O11W H11A 117(5) . . ? 
Dy2 O11W H11B 127(5) . . ? 
H11A O11W H11B 110.5(19) . . ? 
Dy2 O12W H12A 121.4 . . ? 
Dy2 O12W H12B 110.0 . . ? 
H12A O12W H12B 109.0 . . ? 
H13A O13W H13B 108.6(18) . . ? 
H14A O14W H14B 109.6(18) . . ? 
C3 N1 C2 107.9(5) . . ? 
C3 N1 H1 124(5) . . ? 
C2 N1 H1 127(5) . . ? 
C3 N2 C9 105.7(4) . . ? 
C6 N3 C7 116.3(6) . . ? 
C13 N4 C12 108.2(5) . . ? 
C13 N4 H4 125(5) . . ? 
C12 N4 H4 126(5) . . ? 
C13 N5 C19 106.4(5) . . ? 
C16 N6 C17 116.3(7) . . ? 
O1 C1 O2 123.9(5) . . ? 
O1 C1 C2 116.3(5) . . ? 
O2 C1 C2 119.8(5) . . ? 
C9 C2 N1 104.9(5) . . ? 
C9 C2 C1 136.2(5) . . ? 
N1 C2 C1 118.9(5) . . ? 
N2 C3 N1 111.3(5) . . ? 
N2 C3 C4 124.6(5) . . ? 
N1 C3 C4 124.1(5) . . ? 
C8 C4 C5 116.6(6) . . ? 
C8 C4 C3 121.2(5) . . ? 
C5 C4 C3 122.2(6) . . ? 
C6 C5 C4 120.2(7) . . ? 
C6 C5 H5 119.9 . . ? 
C4 C5 H5 119.9 . . ? 
N3 C6 C5 124.0(7) . . ? 
N3 C6 H6 118.0 . . ? 
C5 C6 H6 118.0 . . ? 
N3 C7 C8 123.5(6) . . ? 
N3 C7 H7 118.2 . . ? 
C8 C7 H7 118.2 . . ? 
C4 C8 C7 119.5(6) . . ? 
C4 C8 H8 120.3 . . ? 
C7 C8 H8 120.3 . . ? 
C2 C9 N2 110.2(5) . . ? 
C2 C9 C10 130.4(5) . . ? 
N2 C9 C10 119.5(5) . . ? 
O4 C10 O3 123.3(5) . . ? 
O4 C10 C9 120.5(5) . . ? 
O3 C10 C9 116.2(5) . . ? 
O5 C11 O6 124.1(5) . . ? 
O5 C11 C12 117.4(5) . . ? 
O6 C11 C12 118.4(5) . . ? 
N4 C12 C19 105.5(5) . . ? 
N4 C12 C11 118.3(5) . . ? 
C19 C12 C11 136.0(5) . . ? 
N5 C13 N4 111.3(5) . . ? 
N5 C13 C14 125.6(5) . . ? 
N4 C13 C14 123.0(5) . . ? 
C15 C14 C18 116.9(6) . . ? 
C15 C14 C13 122.4(6) . . ? 
C18 C14 C13 120.7(6) . . ? 
C14 C15 C16 120.4(8) . . ? 
C14 C15 H15 119.8 . . ? 
C16 C15 H15 119.8 . . ? 
N6 C16 C15 123.1(9) . . ? 
N6 C16 H16 118.5 . . ? 
C15 C16 H16 118.5 . . ? 
N6 C17 C18 124.1(8) . . ? 
N6 C17 H17 117.9 . . ? 
C18 C17 H17 117.9 . . ? 
C17 C18 C14 118.9(8) . . ? 
C17 C18 H18 120.5 . . ? 
C14 C18 H18 120.5 . . ? 
N5 C19 C12 108.6(5) . . ? 
N5 C19 C20 120.2(5) . . ? 
C12 C19 C20 131.2(5) . . ? 
O8 C20 O7 122.7(5) . . ? 
O8 C20 C19 118.4(5) . . ? 
O7 C20 C19 118.9(5) . . ? 
O18 N7 O16 119.4(7) . . ? 
O18 N7 O17 121.1(7) . . ? 
O16 N7 O17 119.4(7) . . ? 
 
_diffrn_measured_fraction_theta_max    0.988 
_diffrn_reflns_theta_full              27.49 
_diffrn_measured_fraction_theta_full   0.988 
_refine_diff_density_max    2.076 
_refine_diff_density_min   -1.916 
_refine_diff_density_rms    0.177 

####

 
 
data_5-Dy
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C28 H38 Dy2 N6 O24' 
_chemical_formula_weight          1167.64 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 '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' 
 
_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                    8.3855(2) 
_cell_length_b                    9.4526(3) 
_cell_length_c                    13.2169(3) 
_cell_angle_alpha                 88.674(2) 
_cell_angle_beta                  79.772(2) 
_cell_angle_gamma                 66.784(3) 
_cell_volume                      946.23(4) 
_cell_formula_units_Z             1 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     4798
_cell_measurement_theta_min       2.6832
_cell_measurement_theta_max       29.1523 
 
_exptl_crystal_description        block
_exptl_crystal_colour             colorless
_exptl_crystal_size_max           0.12 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.07 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     2.049 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              572 
_exptl_absorpt_coefficient_mu     4.021 
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.57671
_exptl_absorpt_correction_T_max   1.00000 
_exptl_absorpt_process_details   

;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;  
 
_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   'Xcalibur, Eos' 
_diffrn_measurement_method        'ω scans'
_diffrn_detector_area_resol_mean  16.2083
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             9035 
_diffrn_reflns_av_R_equivalents   0.0317 
_diffrn_reflns_av_sigmaI/netI     0.0351 
_diffrn_reflns_limit_h_min        -10 
_diffrn_reflns_limit_h_max        10 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -16 
_diffrn_reflns_limit_l_max        16 
_diffrn_reflns_theta_min          2.69 
_diffrn_reflns_theta_max          27.10 
_reflns_number_total              4109 
_reflns_number_gt                 3869 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        

;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
 
_computing_cell_refinement        

;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
 
_computing_data_reduction         

;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;

_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_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)+(0.0300P)²+1.4000P] 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          4109 
_refine_ls_number_parameters      292 
_refine_ls_number_restraints      18 
_refine_ls_R_factor_all           0.0267 
_refine_ls_R_factor_gt            0.0244 
_refine_ls_wR_factor_ref          0.0608 
_refine_ls_wR_factor_gt           0.0588 
_refine_ls_goodness_of_fit_ref    1.007 
_refine_ls_restrained_S_all       1.005 
_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 0.024679(19) 0.254398(16) 0.380613(10) 0.01688(6) Uani 1 1 d . . . 
O1 O 0.0459(3) 0.4873(3) 0.33251(18) 0.0241(5) Uani 1 1 d . . . 
O2 O -0.0429(3) 0.6649(3) 0.46160(17) 0.0214(5) Uani 1 1 d . . . 
O3 O 0.1800(4) 0.8063(3) 0.50628(18) 0.0277(6) Uani 1 1 d . . . 
O4 O 0.2002(3) 1.0045(3) 0.4210(2) 0.0273(5) Uani 1 1 d . . . 
O5 O 0.0726(4) 0.2307(3) 0.19439(18) 0.0282(6) Uani 1 1 d . . . 
O6 O -0.0771(3) 0.1046(3) 0.27656(17) 0.0253(5) Uani 1 1 d . . . 
O7 O -0.2582(4) 0.4374(3) 0.3594(3) 0.0401(7) Uani 1 1 d D . . 
H7A H -0.279(6) 0.527(2) 0.346(4) 0.060 Uiso 1 1 d D . . 
H7B H -0.343(4) 0.414(5) 0.374(4) 0.060 Uiso 1 1 d D . . 
O8 O 0.3323(3) 0.2119(3) 0.3388(2) 0.0311(6) Uani 1 1 d D . . 
H8A H 0.364(5) 0.241(5) 0.2825(19) 0.047 Uiso 1 1 d D . . 
H8B H 0.410(4) 0.140(4) 0.360(3) 0.047 Uiso 1 1 d D . . 
N1 N 0.3028(4) 0.8178(3) 0.2363(2) 0.0208(6) Uani 1 1 d . . . 
N2 N 0.1894(4) 0.6519(3) 0.2041(2) 0.0196(6) Uani 1 1 d . . . 
H2 H 0.146(5) 0.609(5) 0.173(3) 0.029 Uiso 1 1 d . . . 
N3 N 0.5156(4) 0.7223(4) -0.1526(3) 0.0370(8) Uani 1 1 d . . . 
C1 C 0.0392(4) 0.6087(4) 0.3729(2) 0.0171(6) Uani 1 1 d . . . 
C2 C 0.1387(4) 0.6882(3) 0.3073(2) 0.0174(6) Uani 1 1 d . . . 
C3 C 0.2096(4) 0.7926(3) 0.3260(2) 0.0173(6) Uani 1 1 d . . . 
C4 C 0.2871(4) 0.7314(4) 0.1642(3) 0.0201(6) Uani 1 1 d . . . 
C5 C 0.3657(4) 0.7253(4) 0.0545(3) 0.0220(7) Uani 1 1 d . . . 
C6 C 0.4771(5) 0.8001(5) 0.0251(3) 0.0343(9) Uani 1 1 d . . . 
H6 H 0.5040 0.8525 0.0738 0.041 Uiso 1 1 calc R . . 
C7 C 0.5483(6) 0.7955(6) -0.0786(3) 0.0419(10) Uani 1 1 d . . . 
H7 H 0.6231 0.8463 -0.0977 0.050 Uiso 1 1 calc R . . 
C8 C 0.4092(5) 0.6505(4) -0.1231(3) 0.0323(8) Uani 1 1 d . . . 
H8 H 0.3853 0.5984 -0.1734 0.039 Uiso 1 1 calc R . . 
C9 C 0.3313(5) 0.6483(4) -0.0216(3) 0.0259(7) Uani 1 1 d . . . 
H9 H 0.2573 0.5961 -0.0048 0.031 Uiso 1 1 calc R . . 
C10 C 0.1934(4) 0.8739(4) 0.4246(2) 0.0171(6) Uani 1 1 d . . . 
C11 C -0.0031(4) 0.1372(4) 0.1938(2) 0.0187(6) Uani 1 1 d . . . 
C12 C -0.0027(4) 0.0663(4) 0.0923(2) 0.0187(6) Uani 1 1 d . . . 
C13 C -0.0860(4) -0.0339(4) 0.0912(3) 0.0215(7) Uani 1 1 d . . . 
H13 H -0.1433 -0.0564 0.1523 0.026 Uiso 1 1 calc R . . 
C14 C 0.0836(5) 0.1006(4) 0.0019(3) 0.0220(7) Uani 1 1 d . . . 
H14 H 0.1395 0.1679 0.0035 0.026 Uiso 1 1 calc R . . 
O1W O 0.3296(5) 0.0103(4) 0.6235(3) 0.0483(8) Uani 1 1 d D . . 
H1A H 0.316(7) 0.023(7) 0.5637(15) 0.072 Uiso 1 1 d D . . 
H1B H 0.268(6) -0.027(6) 0.660(3) 0.072 Uiso 1 1 d D . . 
O2W O -0.0025(7) 0.5186(5) 0.1057(3) 0.0838(16) Uani 1 1 d D . . 
H2A H -0.0198 0.4499 0.1383 0.126 Uiso 1 1 d RD . . 
H2B H 0.0637 0.4917 0.0498 0.126 Uiso 0.50 1 d PRD . . 
H2C H 0.0001 0.5069 0.0418 0.126 Uiso 0.50 1 d PR . . 
O3W O 0.3321(5) 0.2694(4) 0.7272(4) 0.0770(13) Uani 1 1 d D . . 
H3A H 0.4303 0.2376 0.7440 0.116 Uiso 1 1 d RD . . 
H3B H 0.3266 0.2171 0.6798 0.116 Uiso 1 1 d RD . . 
O4W O 0.5632(7) 0.5820(7) 0.5687(5) 0.133(3) Uani 1 1 d D . . 
H4A H 0.6000 0.6425 0.5892 0.199 Uiso 1 1 d RD . . 
H4B H 0.6369 0.5110 0.5298 0.199 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 
Dy1 O2 2.287(2) 2_566 ? 
Dy1 O3 2.310(2) 2_566 ? 
Dy1 O1 2.343(2) . ? 
Dy1 O4 2.347(2) 1_545 ? 
Dy1 O7 2.383(3) . ? 
Dy1 O8 2.410(3) . ? 
Dy1 O5 2.423(2) . ? 
Dy1 O6 2.467(2) . ? 
Dy1 C11 2.813(3) . ? 
O1 C1 1.253(4) . ? 
O2 C1 1.259(4) . ? 
O2 Dy1 2.287(2) 2_566 ? 
O3 C10 1.252(4) . ? 
O3 Dy1 2.310(2) 2_566 ? 
O4 C10 1.257(4) . ? 
O4 Dy1 2.347(2) 1_565 ? 
O5 C11 1.276(4) . ? 
O6 C11 1.253(4) . ? 
O7 H7A 0.816(10) . ? 
O7 H7B 0.815(10) . ? 
O8 H8A 0.823(10) . ? 
O8 H8B 0.821(10) . ? 
N1 C4 1.326(4) . ? 
N1 C3 1.371(4) . ? 
N2 C4 1.351(4) . ? 
N2 C2 1.364(4) . ? 
N2 H2 0.81(4) . ? 
N3 C8 1.323(6) . ? 
N3 C7 1.336(6) . ? 
C1 C2 1.490(4) . ? 
C2 C3 1.383(4) . ? 
C3 C10 1.487(4) . ? 
C4 C5 1.475(4) . ? 
C5 C6 1.379(5) . ? 
C5 C9 1.388(5) . ? 
C6 C7 1.389(5) . ? 
C6 H6 0.9300 . ? 
C7 H7 0.9300 . ? 
C8 C9 1.388(5) . ? 
C8 H8 0.9300 . ? 
C9 H9 0.9300 . ? 
C11 C12 1.513(4) . ? 
C12 C13 1.382(5) . ? 
C12 C14 1.384(5) . ? 
C13 C14 1.388(4) 2 ? 
C13 H13 0.9300 . ? 
C14 C13 1.388(4) 2 ? 
C14 H14 0.9300 . ? 
O1W H1A 0.817(10) . ? 
O1W H1B 0.816(10) . ? 
O2W H2A 0.8168 . ? 
O2W H2B 0.8196 . ? 
O2W H2C 0.8495 . ? 
O3W H3A 0.8278 . ? 
O3W H3B 0.8255 . ? 
O4W H4A 0.8200 . ? 
O4W H4B 0.8200 . ? 
 
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 76.08(8) 2_566 2_566 ? 
O2 Dy1 O1 82.39(8) 2_566 . ? 
O3 Dy1 O1 133.49(9) 2_566 . ? 
O2 Dy1 O4 86.88(8) 2_566 1_545 ? 
O3 Dy1 O4 79.02(9) 2_566 1_545 ? 
O1 Dy1 O4 140.67(9) . 1_545 ? 
O2 Dy1 O7 101.04(10) 2_566 . ? 
O3 Dy1 O7 73.69(10) 2_566 . ? 
O1 Dy1 O7 70.68(10) . . ? 
O4 Dy1 O7 148.64(9) 1_545 . ? 
O2 Dy1 O8 83.79(9) 2_566 . ? 
O3 Dy1 O8 143.73(9) 2_566 . ? 
O1 Dy1 O8 71.34(9) . . ? 
O4 Dy1 O8 69.94(9) 1_545 . ? 
O7 Dy1 O8 140.64(10) . . ? 
O2 Dy1 O5 157.14(8) 2_566 . ? 
O3 Dy1 O5 126.08(8) 2_566 . ? 
O1 Dy1 O5 77.49(8) . . ? 
O4 Dy1 O5 101.88(9) 1_545 . ? 
O7 Dy1 O5 82.51(11) . . ? 
O8 Dy1 O5 79.61(9) . . ? 
O2 Dy1 O6 149.58(8) 2_566 . ? 
O3 Dy1 O6 74.37(8) 2_566 . ? 
O1 Dy1 O6 124.01(8) . . ? 
O4 Dy1 O6 80.60(8) 1_545 . ? 
O7 Dy1 O6 77.45(10) . . ? 
O8 Dy1 O6 116.93(9) . . ? 
O5 Dy1 O6 53.28(8) . . ? 
O2 Dy1 C11 175.72(9) 2_566 . ? 
O3 Dy1 C11 100.35(9) 2_566 . ? 
O1 Dy1 C11 101.85(9) . . ? 
O4 Dy1 C11 90.14(9) 1_545 . ? 
O7 Dy1 C11 80.00(11) . . ? 
O8 Dy1 C11 98.07(10) . . ? 
O5 Dy1 C11 26.90(9) . . ? 
O6 Dy1 C11 26.43(9) . . ? 
C1 O1 Dy1 139.8(2) . . ? 
C1 O2 Dy1 146.3(2) . 2_566 ? 
C10 O3 Dy1 140.6(2) . 2_566 ? 
C10 O4 Dy1 137.7(2) . 1_565 ? 
C11 O5 Dy1 93.81(19) . . ? 
C11 O6 Dy1 92.38(19) . . ? 
Dy1 O7 H7A 124(3) . . ? 
Dy1 O7 H7B 119(3) . . ? 
H7A O7 H7B 117(2) . . ? 
Dy1 O8 H8A 116(3) . . ? 
Dy1 O8 H8B 123(3) . . ? 
H8A O8 H8B 114.8(19) . . ? 
C4 N1 C3 105.3(3) . . ? 
C4 N2 C2 107.9(3) . . ? 
C4 N2 H2 127(3) . . ? 
C2 N2 H2 124(3) . . ? 
C8 N3 C7 116.7(4) . . ? 
O1 C1 O2 125.3(3) . . ? 
O1 C1 C2 115.0(3) . . ? 
O2 C1 C2 119.7(3) . . ? 
N2 C2 C3 105.3(3) . . ? 
N2 C2 C1 119.7(3) . . ? 
C3 C2 C1 134.9(3) . . ? 
N1 C3 C2 110.1(3) . . ? 
N1 C3 C10 120.9(3) . . ? 
C2 C3 C10 129.0(3) . . ? 
N1 C4 N2 111.5(3) . . ? 
N1 C4 C5 123.6(3) . . ? 
N2 C4 C5 124.9(3) . . ? 
C6 C5 C9 118.0(3) . . ? 
C6 C5 C4 119.2(3) . . ? 
C9 C5 C4 122.8(3) . . ? 
C5 C6 C7 118.7(4) . . ? 
C5 C6 H6 120.7 . . ? 
C7 C6 H6 120.7 . . ? 
N3 C7 C6 123.9(4) . . ? 
N3 C7 H7 118.1 . . ? 
C6 C7 H7 118.1 . . ? 
N3 C8 C9 123.9(4) . . ? 
N3 C8 H8 118.1 . . ? 
C9 C8 H8 118.1 . . ? 
C8 C9 C5 118.8(4) . . ? 
C8 C9 H9 120.6 . . ? 
C5 C9 H9 120.6 . . ? 
O3 C10 O4 123.7(3) . . ? 
O3 C10 C3 118.2(3) . . ? 
O4 C10 C3 118.1(3) . . ? 
O6 C11 O5 120.3(3) . . ? 
O6 C11 C12 120.4(3) . . ? 
O5 C11 C12 119.3(3) . . ? 
O6 C11 Dy1 61.19(17) . . ? 
O5 C11 Dy1 59.28(16) . . ? 
C12 C11 Dy1 175.5(2) . . ? 
C13 C12 C14 120.9(3) . . ? 
C13 C12 C11 119.6(3) . . ? 
C14 C12 C11 119.6(3) . . ? 
C12 C13 C14 119.6(3) . 2 ? 
C12 C13 H13 120.2 . . ? 
C14 C13 H13 120.2 2 . ? 
C12 C14 C13 119.6(3) . 2 ? 
C12 C14 H14 120.2 . . ? 
C13 C14 H14 120.2 2 . ? 
H1A O1W H1B 117(2) . . ? 
H2A O2W H2B 115.8 . . ? 
H2A O2W H2C 111.9 . . ? 
H2B O2W H2C 36.6 . . ? 
H3A O3W H3B 113.8 . . ? 
H4A O4W H4B 114.9 . . ? 
 
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
O2 Dy1 O1 C1 -11.3(3) 2_566 . . . ? 
O3 Dy1 O1 C1 51.2(4) 2_566 . . . ? 
O4 Dy1 O1 C1 -86.8(4) 1_545 . . . ? 
O7 Dy1 O1 C1 93.3(4) . . . . ? 
O8 Dy1 O1 C1 -97.3(4) . . . . ? 
O5 Dy1 O1 C1 179.6(4) . . . . ? 
O6 Dy1 O1 C1 152.3(3) . . . . ? 
C11 Dy1 O1 C1 168.1(3) . . . . ? 
O2 Dy1 O5 C11 176.7(2) 2_566 . . . ? 
O3 Dy1 O5 C11 -19.1(2) 2_566 . . . ? 
O1 Dy1 O5 C11 -154.4(2) . . . . ? 
O4 Dy1 O5 C11 65.9(2) 1_545 . . . ? 
O7 Dy1 O5 C11 -82.6(2) . . . . ? 
O8 Dy1 O5 C11 132.6(2) . . . . ? 
O6 Dy1 O5 C11 -2.74(19) . . . . ? 
O2 Dy1 O6 C11 -176.77(19) 2_566 . . . ? 
O3 Dy1 O6 C11 169.1(2) 2_566 . . . ? 
O1 Dy1 O6 C11 36.8(2) . . . . ? 
O4 Dy1 O6 C11 -109.8(2) 1_545 . . . ? 
O7 Dy1 O6 C11 92.8(2) . . . . ? 
O8 Dy1 O6 C11 -48.1(2) . . . . ? 
O5 Dy1 O6 C11 2.78(19) . . . . ? 
Dy1 O1 C1 O2 -26.3(6) . . . . ? 
Dy1 O1 C1 C2 153.6(3) . . . . ? 
Dy1 O2 C1 O1 123.2(4) 2_566 . . . ? 
Dy1 O2 C1 C2 -56.8(5) 2_566 . . . ? 
C4 N2 C2 C3 0.4(4) . . . . ? 
C4 N2 C2 C1 -175.8(3) . . . . ? 
O1 C1 C2 N2 16.6(5) . . . . ? 
O2 C1 C2 N2 -163.4(3) . . . . ? 
O1 C1 C2 C3 -158.1(4) . . . . ? 
O2 C1 C2 C3 21.8(6) . . . . ? 
C4 N1 C3 C2 0.6(4) . . . . ? 
C4 N1 C3 C10 -178.6(3) . . . . ? 
N2 C2 C3 N1 -0.6(4) . . . . ? 
C1 C2 C3 N1 174.6(3) . . . . ? 
N2 C2 C3 C10 178.5(3) . . . . ? 
C1 C2 C3 C10 -6.3(6) . . . . ? 
C3 N1 C4 N2 -0.4(4) . . . . ? 
C3 N1 C4 C5 179.0(3) . . . . ? 
C2 N2 C4 N1 0.0(4) . . . . ? 
C2 N2 C4 C5 -179.4(3) . . . . ? 
N1 C4 C5 C6 7.1(5) . . . . ? 
N2 C4 C5 C6 -173.6(3) . . . . ? 
N1 C4 C5 C9 -172.4(3) . . . . ? 
N2 C4 C5 C9 6.9(5) . . . . ? 
C9 C5 C6 C7 0.4(6) . . . . ? 
C4 C5 C6 C7 -179.1(4) . . . . ? 
C8 N3 C7 C6 -0.3(7) . . . . ? 
C5 C6 C7 N3 -0.1(7) . . . . ? 
C7 N3 C8 C9 0.3(6) . . . . ? 
N3 C8 C9 C5 -0.1(6) . . . . ? 
C6 C5 C9 C8 -0.3(5) . . . . ? 
C4 C5 C9 C8 179.1(3) . . . . ? 
Dy1 O3 C10 O4 105.4(4) 2_566 . . . ? 
Dy1 O3 C10 C3 -77.1(4) 2_566 . . . ? 
Dy1 O4 C10 O3 -113.4(4) 1_565 . . . ? 
Dy1 O4 C10 C3 69.1(4) 1_565 . . . ? 
N1 C3 C10 O3 -149.2(3) . . . . ? 
C2 C3 C10 O3 31.8(5) . . . . ? 
N1 C3 C10 O4 28.4(5) . . . . ? 
C2 C3 C10 O4 -150.6(3) . . . . ? 
Dy1 O6 C11 O5 -4.9(3) . . . . ? 
Dy1 O6 C11 C12 175.2(3) . . . . ? 
Dy1 O5 C11 O6 5.0(3) . . . . ? 
Dy1 O5 C11 C12 -175.1(3) . . . . ? 
O2 Dy1 C11 O6 22.5(13) 2_566 . . . ? 
O3 Dy1 C11 O6 -10.7(2) 2_566 . . . ? 
O1 Dy1 C11 O6 -149.5(2) . . . . ? 
O4 Dy1 C11 O6 68.2(2) 1_545 . . . ? 
O7 Dy1 C11 O6 -81.9(2) . . . . ? 
O8 Dy1 C11 O6 137.9(2) . . . . ? 
O5 Dy1 C11 O6 -175.1(3) . . . . ? 
O2 Dy1 C11 O5 -162.4(11) 2_566 . . . ? 
O3 Dy1 C11 O5 164.4(2) 2_566 . . . ? 
O1 Dy1 C11 O5 25.5(2) . . . . ? 
O4 Dy1 C11 O5 -116.8(2) 1_545 . . . ? 
O7 Dy1 C11 O5 93.2(2) . . . . ? 
O8 Dy1 C11 O5 -47.0(2) . . . . ? 
O6 Dy1 C11 O5 175.1(3) . . . . ? 
O2 Dy1 C11 C12 -89(3) 2_566 . . . ? 
O3 Dy1 C11 C12 -122(3) 2_566 . . . ? 
O1 Dy1 C11 C12 99(3) . . . . ? 
O4 Dy1 C11 C12 -43(3) 1_545 . . . ? 
O7 Dy1 C11 C12 166(3) . . . . ? 
O8 Dy1 C11 C12 26(3) . . . . ? 
O5 Dy1 C11 C12 73(3) . . . . ? 
O6 Dy1 C11 C12 -112(3) . . . . ? 
O6 C11 C12 C13 0.6(5) . . . . ? 
O5 C11 C12 C13 -179.4(3) . . . . ? 
Dy1 C11 C12 C13 110(3) . . . . ? 
O6 C11 C12 C14 -178.4(3) . . . . ? 
O5 C11 C12 C14 1.7(5) . . . . ? 
Dy1 C11 C12 C14 -69(3) . . . . ? 
C14 C12 C13 C14 -0.2(6) . . . 2 ? 
C11 C12 C13 C14 -179.1(3) . . . 2 ? 
C13 C12 C14 C13 0.2(6) . . . 2 ? 
C11 C12 C14 C13 179.1(3) . . . 2 ? 
 
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 H7A O3W  0.816(10) 2.056(19) 2.851(5) 164(6) 2_566 
O7 H7B O4W  0.815(10) 1.85(2) 2.641(6) 162(5) 2_566 
O8 H8A N3  0.823(10) 1.929(14) 2.740(4) 168(4) 2_665 
O8 H8B O1W  0.821(10) 2.13(2) 2.908(4) 158(4) 2_656 
N2 H2 O2W  0.81(4) 2.08(4) 2.878(5) 171(4) . 
O1W H1A O4  0.817(10) 2.31(2) 3.070(4) 155(5) 1_545 
O1W H1B O6  0.816(10) 2.058(17) 2.856(4) 166(5) 2_556 
O2W H2A O5  0.82 2.08 2.818(4) 150.8 . 
O2W H2C O2W  0.85 1.97 2.816(7) 179.2 2_565 
O3W H3A N1  0.83 2.15 2.967(5) 168.7 2_666 
O3W H3B O1W  0.83 2.10 2.843(5) 150.2 . 
O4W H4A O8  0.82 2.00 2.811(6) 170.8 2_666 
O4W H4B O7  0.82 2.28 2.975(6) 142.3 1_655 
 
_diffrn_measured_fraction_theta_max    0.985 
_diffrn_reflns_theta_full              27.10 
_diffrn_measured_fraction_theta_full   0.985 
_refine_diff_density_max    1.269 
_refine_diff_density_min   -1.240 
_refine_diff_density_rms    0.124 



####

 
data_6-Er
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C18 H9 Er N3 O10' 
_chemical_formula_weight          594.54 
 
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' 
 'Er'  'Er'  -0.2586   4.9576 
 '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                    8.4976(5) 
_cell_length_b                    10.4677(5) 
_cell_length_c                    12.1637(8) 
_cell_angle_alpha                 112.855(5) 
_cell_angle_beta                  96.677(5) 
_cell_angle_gamma                 103.448(5) 
_cell_volume                      943.57(9) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     298(2) 
_cell_measurement_reflns_used     6178
_cell_measurement_theta_min       2.5275
_cell_measurement_theta_max       29.1670
 
_exptl_crystal_description        block 
_exptl_crystal_colour             colorless 
_exptl_crystal_size_max           0.12 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.08 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     2.093 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              572 
_exptl_absorpt_coefficient_mu     4.514 
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.6134 
_exptl_absorpt_correction_T_max   0.7141 
_exptl_absorpt_process_details    

;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       298(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   'Xcalibur, Eos' 
_diffrn_measurement_method        'ω scans' 
_diffrn_detector_area_resol_mean  16.2083  
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             8912 
_diffrn_reflns_av_R_equivalents   0.0328 
_diffrn_reflns_av_sigmaI/netI     0.0327 
_diffrn_reflns_limit_h_min        -10 
_diffrn_reflns_limit_h_max        10 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -14 
_diffrn_reflns_limit_l_max        14 
_diffrn_reflns_theta_min          2.53 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              3328 
_reflns_number_gt                 3162 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        

;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;

_computing_cell_refinement        

;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;

_computing_data_reduction         

;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;

_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_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)+(0.0245P)²+0.9061P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          3328 
_refine_ls_number_parameters      298 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0206 
_refine_ls_R_factor_gt            0.0191 
_refine_ls_wR_factor_ref          0.0498 
_refine_ls_wR_factor_gt           0.0491 
_refine_ls_goodness_of_fit_ref    1.003 
_refine_ls_restrained_S_all       1.003 
_refine_ls_shift/su_max           0.002 
_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 
Er1 Er -0.252464(16) 0.074673(14) 0.546480(12) 0.01553(6) Uani 1 1 d . . . 
C1 C -0.1739(5) -0.1110(4) 0.7094(3) 0.0256(8) Uani 1 1 d . . . 
C2 C -0.2013(5) -0.2676(4) 0.6288(3) 0.0219(7) Uani 1 1 d . . . 
C3 C -0.1155(5) -0.3494(4) 0.6642(3) 0.0319(9) Uani 1 1 d . . . 
H3 H -0.0383 -0.3058 0.7389 0.038 Uiso 1 1 calc R . . 
C4 C -0.1453(5) -0.4952(4) 0.5883(3) 0.0304(9) Uani 1 1 d . . . 
H4 H -0.0892 -0.5496 0.6126 0.036 Uiso 1 1 calc R . . 
C5 C -0.2585(5) -0.5598(4) 0.4766(3) 0.0233(8) Uani 1 1 d . . . 
C6 C -0.2953(5) -0.7180(4) 0.3934(3) 0.0261(8) Uani 1 1 d . . . 
C7 C -0.3424(5) -0.4792(4) 0.4410(3) 0.0266(8) Uani 1 1 d . . . 
H7 H -0.4175 -0.5225 0.3653 0.032 Uiso 1 1 calc R . . 
C8 C -0.3153(5) -0.3342(4) 0.5175(3) 0.0252(8) Uani 1 1 d . . . 
H8 H -0.3744 -0.2812 0.4937 0.030 Uiso 1 1 calc R . . 
C9 C 0.1414(4) 0.1920(4) 0.6580(3) 0.0173(7) Uani 1 1 d . . . 
C10 C 0.2943(4) 0.3112(3) 0.7387(3) 0.0159(7) Uani 1 1 d . . . 
C11 C 0.4392(4) 0.5311(3) 0.8730(3) 0.0171(7) Uani 1 1 d . . . 
C12 C 0.4813(4) 0.6839(4) 0.9628(3) 0.0221(8) Uani 1 1 d . . . 
C13 C 0.3634(5) 0.7475(4) 1.0084(4) 0.0355(10) Uani 1 1 d . . . 
H13 H 0.2512 0.6943 0.9810 0.043 Uiso 1 1 calc R . . 
C14 C 0.4128(6) 0.8895(5) 1.0943(4) 0.0417(11) Uani 1 1 d . . . 
H14 H 0.3331 0.9315 1.1254 0.050 Uiso 1 1 calc R . . 
C15 C 0.6875(6) 0.9094(5) 1.0918(4) 0.0470(12) Uani 1 1 d . . . 
H15 H 0.7986 0.9655 1.1211 0.056 Uiso 1 1 calc R . . 
C16 C 0.6461(5) 0.7679(4) 1.0059(4) 0.0377(10) Uani 1 1 d . . . 
H16 H 0.7286 0.7286 0.9768 0.045 Uiso 1 1 calc R . . 
C17 C 0.4642(4) 0.3301(3) 0.7506(3) 0.0157(7) Uani 1 1 d . . . 
C18 C 0.5583(4) 0.2342(3) 0.6850(3) 0.0160(7) Uani 1 1 d . . . 
N1 N 0.2833(3) 0.4411(3) 0.8172(2) 0.0183(6) Uani 1 1 d . . . 
H1 H 0.1901 0.4619 0.8295 0.022 Uiso 1 1 d R . . 
N2 N 0.5527(3) 0.4684(3) 0.8351(2) 0.0198(6) Uani 1 1 d . . . 
N3 N 0.5706(5) 0.9675(3) 1.1337(3) 0.0350(8) Uani 1 1 d . . . 
O1 O -0.0969(4) -0.0574(3) 0.8179(2) 0.0449(8) Uani 1 1 d . . . 
O2 O -0.2369(3) -0.0389(3) 0.6622(2) 0.0288(6) Uani 1 1 d . . . 
O3 O -0.2640(4) -0.8007(3) 0.4401(2) 0.0318(6) Uani 1 1 d . . . 
O4 O -0.3550(4) -0.7609(3) 0.2823(2) 0.0458(8) Uani 1 1 d . . . 
O5 O 0.0098(3) 0.2233(3) 0.6531(2) 0.0276(6) Uani 1 1 d . . . 
O6 O 0.1537(3) 0.0670(2) 0.6006(2) 0.0262(6) Uani 1 1 d . . . 
O7 O 0.4862(3) 0.1134(2) 0.5905(2) 0.0225(5) Uani 1 1 d . . . 
O8 O 0.7126(3) 0.2730(3) 0.7191(2) 0.0252(6) Uani 1 1 d . . . 
O9W O 0.0096(4) 0.4884(3) 0.1274(3) 0.0467(8) Uani 1 1 d . . . 
O10W O 1.0143(8) 0.8159(6) 0.9657(5) 0.0434(15) Uani 0.50 1 d P . . 
O11W O 1.0099(11) 0.7514(10) 1.0815(8) 0.090(3) Uani 0.50 1 d P . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Er1 O2 2.177(3) . ? 
Er1 O3 2.175(3) 1_565 ? 
Er1 O6 2.230(2) 2_556 ? 
Er1 O5 2.284(2) . ? 
Er1 O7 2.337(2) 2_556 ? 
Er1 O8 2.419(2) 1_455 ? 
Er1 O7 2.431(2) 1_455 ? 
Er1 C18 2.812(3) 1_455 ? 
C1 O1 1.241(4) . ? 
C1 O2 1.280(4) . ? 
C1 C2 1.492(5) . ? 
C2 C8 1.381(5) . ? 
C2 C3 1.397(5) . ? 
C3 C4 1.384(5) . ? 
C3 H3 0.9300 . ? 
C4 C5 1.382(5) . ? 
C4 H4 0.9300 . ? 
C5 C7 1.378(5) . ? 
C5 C6 1.499(5) . ? 
C6 O4 1.245(4) . ? 
C6 O3 1.263(4) . ? 
C7 C8 1.383(5) . ? 
C7 H7 0.9300 . ? 
C8 H8 0.9300 . ? 
C9 O5 1.238(4) . ? 
C9 O6 1.257(4) . ? 
C9 C10 1.486(4) . ? 
C10 N1 1.357(4) . ? 
C10 C17 1.393(5) . ? 
C11 N2 1.318(4) . ? 
C11 N1 1.348(4) . ? 
C11 C12 1.472(4) . ? 
C12 C16 1.381(5) . ? 
C12 C13 1.381(5) . ? 
C13 C14 1.370(5) . ? 
C13 H13 0.9300 . ? 
C14 N3 1.316(6) . ? 
C14 H14 0.9300 . ? 
C15 N3 1.333(6) . ? 
C15 C16 1.371(6) . ? 
C15 H15 0.9300 . ? 
C16 H16 0.9300 . ? 
C17 N2 1.370(4) . ? 
C17 C18 1.477(4) . ? 
C18 O8 1.246(4) . ? 
C18 O7 1.281(4) . ? 
C18 Er1 2.812(3) 1_655 ? 
N1 H1 0.8827 . ? 
O3 Er1 2.175(3) 1_545 ? 
O6 Er1 2.230(2) 2_556 ? 
O7 Er1 2.337(2) 2_556 ? 
O7 Er1 2.431(2) 1_655 ? 
O8 Er1 2.419(2) 1_655 ? 
O10W O11W 1.784(12) . ? 
 
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 Er1 O3 176.84(8) . 1_565 ? 
O2 Er1 O6 95.83(10) . 2_556 ? 
O3 Er1 O6 86.70(10) 1_565 2_556 ? 
O2 Er1 O5 87.66(10) . . ? 
O3 Er1 O5 90.38(10) 1_565 . ? 
O6 Er1 O5 91.44(9) 2_556 . ? 
O2 Er1 O7 91.10(9) . 2_556 ? 
O3 Er1 O7 91.39(10) 1_565 2_556 ? 
O6 Er1 O7 74.93(8) 2_556 2_556 ? 
O5 Er1 O7 166.13(8) . 2_556 ? 
O2 Er1 O8 88.35(9) . 1_455 ? 
O3 Er1 O8 88.72(9) 1_565 1_455 ? 
O6 Er1 O8 164.84(8) 2_556 1_455 ? 
O5 Er1 O8 74.13(8) . 1_455 ? 
O7 Er1 O8 119.66(8) 2_556 1_455 ? 
O2 Er1 O7 92.91(9) . 1_455 ? 
O3 Er1 O7 86.29(10) 1_565 1_455 ? 
O6 Er1 O7 140.66(8) 2_556 1_455 ? 
O5 Er1 O7 127.25(8) . 1_455 ? 
O7 Er1 O7 66.60(9) 2_556 1_455 ? 
O8 Er1 O7 53.19(7) 1_455 1_455 ? 
O2 Er1 C18 92.06(9) . 1_455 ? 
O3 Er1 C18 85.84(10) 1_565 1_455 ? 
O6 Er1 C18 166.21(9) 2_556 1_455 ? 
O5 Er1 C18 100.19(9) . 1_455 ? 
O7 Er1 C18 93.66(9) 2_556 1_455 ? 
O8 Er1 C18 26.20(8) 1_455 1_455 ? 
O7 Er1 C18 27.06(8) 1_455 1_455 ? 
O1 C1 O2 123.1(3) . . ? 
O1 C1 C2 119.9(3) . . ? 
O2 C1 C2 117.0(3) . . ? 
C8 C2 C3 119.1(3) . . ? 
C8 C2 C1 119.5(3) . . ? 
C3 C2 C1 121.4(3) . . ? 
C4 C3 C2 120.2(3) . . ? 
C4 C3 H3 119.9 . . ? 
C2 C3 H3 119.9 . . ? 
C5 C4 C3 120.0(3) . . ? 
C5 C4 H4 120.0 . . ? 
C3 C4 H4 120.0 . . ? 
C7 C5 C4 120.0(3) . . ? 
C7 C5 C6 118.8(3) . . ? 
C4 C5 C6 121.2(3) . . ? 
O4 C6 O3 123.5(3) . . ? 
O4 C6 C5 118.4(3) . . ? 
O3 C6 C5 118.1(3) . . ? 
C5 C7 C8 120.2(3) . . ? 
C5 C7 H7 119.9 . . ? 
C8 C7 H7 119.9 . . ? 
C7 C8 C2 120.6(3) . . ? 
C7 C8 H8 119.7 . . ? 
C2 C8 H8 119.7 . . ? 
O5 C9 O6 124.6(3) . . ? 
O5 C9 C10 117.0(3) . . ? 
O6 C9 C10 118.3(3) . . ? 
N1 C10 C17 105.0(3) . . ? 
N1 C10 C9 120.2(3) . . ? 
C17 C10 C9 134.6(3) . . ? 
N2 C11 N1 112.3(3) . . ? 
N2 C11 C12 122.8(3) . . ? 
N1 C11 C12 124.9(3) . . ? 
C16 C12 C13 118.0(3) . . ? 
C16 C12 C11 119.1(3) . . ? 
C13 C12 C11 123.0(3) . . ? 
C14 C13 C12 119.5(4) . . ? 
C14 C13 H13 120.2 . . ? 
C12 C13 H13 120.2 . . ? 
N3 C14 C13 121.4(4) . . ? 
N3 C14 H14 119.3 . . ? 
C13 C14 H14 119.3 . . ? 
N3 C15 C16 120.8(4) . . ? 
N3 C15 H15 119.6 . . ? 
C16 C15 H15 119.6 . . ? 
C15 C16 C12 119.7(4) . . ? 
C15 C16 H16 120.1 . . ? 
C12 C16 H16 120.1 . . ? 
N2 C17 C10 110.0(3) . . ? 
N2 C17 C18 117.8(3) . . ? 
C10 C17 C18 132.1(3) . . ? 
O8 C18 O7 118.4(3) . . ? 
O8 C18 C17 119.7(3) . . ? 
O7 C18 C17 121.8(3) . . ? 
O8 C18 Er1 59.01(16) . 1_655 ? 
O7 C18 Er1 59.67(16) . 1_655 ? 
C17 C18 Er1 173.0(2) . 1_655 ? 
C11 N1 C10 107.8(3) . . ? 
C11 N1 H1 126.5 . . ? 
C10 N1 H1 125.7 . . ? 
C11 N2 C17 104.9(3) . . ? 
C14 N3 C15 120.5(4) . . ? 
C1 O2 Er1 155.1(3) . . ? 
C6 O3 Er1 166.1(3) . 1_545 ? 
C9 O5 Er1 128.7(2) . . ? 
C9 O6 Er1 146.8(2) . 2_556 ? 
C18 O7 Er1 153.3(2) . 2_556 ? 
C18 O7 Er1 93.27(19) . 1_655 ? 
Er1 O7 Er1 113.40(9) 2_556 1_655 ? 
C18 O8 Er1 94.80(18) . 1_655 ? 
 
_diffrn_measured_fraction_theta_max    0.999 
_diffrn_reflns_theta_full              25.00 
_diffrn_measured_fraction_theta_full   0.999 
_refine_diff_density_max    0.805 
_refine_diff_density_min   -0.564 
_refine_diff_density_rms    0.101 


# Start Validation Reply Form

_vrf_PLAT306_6-Er
;
PROBLEM:
  Isolated Oxygen Atom (H-atoms Missing ?) .......        O9W     
   
 

RESPONSE: This is because the hydrogen atoms attaching to free water molecules have not been added.
; 



 
data_7-Tm 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C18 H9 N3 O10 Tm' 
_chemical_formula_weight          596.21 
 
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' 
 'Tm'  'Tm'  -0.3139   5.2483 
 '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                    8.4828(5) 
_cell_length_b                    10.4482(5) 
_cell_length_c                    12.1414(8) 
_cell_angle_alpha                 112.753(5) 
_cell_angle_beta                  96.732(5) 
_cell_angle_gamma                 103.420(5) 
_cell_volume                      939.20(9) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     298(2) 
_cell_measurement_reflns_used     5671
_cell_measurement_theta_min       2.5318
_cell_measurement_theta_max       29.0498
 
_exptl_crystal_description        block
_exptl_crystal_colour             colorless 
_exptl_crystal_size_max           0.12 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.08 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     2.108 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              574 
_exptl_absorpt_coefficient_mu     4.791 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.5972 
_exptl_absorpt_correction_T_max   0.7005 
_exptl_absorpt_process_details    

;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
; 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       298(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   'Xcalibur, Eos'
_diffrn_measurement_method        'ω scans'
_diffrn_detector_area_resol_mean  16.2083 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             8825 
_diffrn_reflns_av_R_equivalents   0.0371 
_diffrn_reflns_av_sigmaI/netI     0.0355 
_diffrn_reflns_limit_h_min        -10 
_diffrn_reflns_limit_h_max        10 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -14 
_diffrn_reflns_limit_l_max        14 
_diffrn_reflns_theta_min          2.54 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              3308 
_reflns_number_gt                 3178 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        

;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;

_computing_cell_refinement        

;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction         

;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_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)+(0.0313P)²+0.9084P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr  
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          3308 
_refine_ls_number_parameters      298 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0239 
_refine_ls_R_factor_gt            0.0225 
_refine_ls_wR_factor_ref          0.0585 
_refine_ls_wR_factor_gt           0.0574 
_refine_ls_goodness_of_fit_ref    1.055 
_refine_ls_restrained_S_all       1.055 
_refine_ls_shift/su_max           0.002 
_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 
Tm1 Tm -0.252797(17) 0.074312(15) 0.546457(13) 0.01529(8) Uani 1 1 d . . . 
C1 C -0.1744(5) -0.1100(4) 0.7095(4) 0.0246(9) Uani 1 1 d . . . 
C2 C -0.2007(5) -0.2676(4) 0.6290(3) 0.0224(9) Uani 1 1 d . . . 
C3 C -0.1146(6) -0.3489(5) 0.6640(4) 0.0323(11) Uani 1 1 d . . . 
H3 H -0.0366 -0.3050 0.7386 0.039 Uiso 1 1 calc R . . 
C4 C -0.1444(6) -0.4951(5) 0.5886(4) 0.0302(10) Uani 1 1 d . . . 
H4 H -0.0877 -0.5493 0.6132 0.036 Uiso 1 1 calc R . . 
C5 C -0.2586(5) -0.5605(4) 0.4767(4) 0.0226(9) Uani 1 1 d . . . 
C6 C -0.2964(6) -0.7190(4) 0.3933(4) 0.0257(9) Uani 1 1 d . . . 
C7 C -0.3424(6) -0.4799(4) 0.4409(4) 0.0267(9) Uani 1 1 d . . . 
H7 H -0.4173 -0.5231 0.3650 0.032 Uiso 1 1 calc R . . 
C8 C -0.3159(6) -0.3346(4) 0.5174(4) 0.0255(9) Uani 1 1 d . . . 
H8 H -0.3757 -0.2817 0.4937 0.031 Uiso 1 1 calc R . . 
C9 C 0.1409(5) 0.1903(4) 0.6571(3) 0.0179(8) Uani 1 1 d . . . 
C10 C 0.2941(4) 0.3099(4) 0.7377(3) 0.0157(7) Uani 1 1 d . . . 
C11 C 0.4385(5) 0.5306(4) 0.8721(3) 0.0190(8) Uani 1 1 d . . . 
C12 C 0.4815(5) 0.6828(4) 0.9626(3) 0.0217(9) Uani 1 1 d . . . 
C13 C 0.3621(6) 0.7467(5) 1.0078(4) 0.0371(11) Uani 1 1 d . . . 
H13 H 0.2497 0.6938 0.9796 0.044 Uiso 1 1 calc R . . 
C14 C 0.4120(7) 0.8888(5) 1.0944(4) 0.0422(12) Uani 1 1 d . . . 
H14 H 0.3322 0.9308 1.1258 0.051 Uiso 1 1 calc R . . 
C15 C 0.6867(7) 0.9088(5) 1.0917(5) 0.0467(13) Uani 1 1 d . . . 
H15 H 0.7981 0.9649 1.1207 0.056 Uiso 1 1 calc R . . 
C16 C 0.6452(6) 0.7667(5) 1.0056(4) 0.0385(12) Uani 1 1 d . . . 
H16 H 0.7280 0.7275 0.9767 0.046 Uiso 1 1 calc R . . 
C17 C 0.4645(5) 0.3294(4) 0.7503(3) 0.0159(8) Uani 1 1 d . . . 
C18 C 0.5574(4) 0.2329(4) 0.6843(3) 0.0153(7) Uani 1 1 d . . . 
N1 N 0.2821(4) 0.4399(3) 0.8164(3) 0.0181(7) Uani 1 1 d . . . 
H1 H 0.1890 0.4607 0.8287 0.022 Uiso 1 1 d R . . 
N2 N 0.5524(4) 0.4676(3) 0.8349(3) 0.0193(7) Uani 1 1 d . . . 
N3 N 0.5705(5) 0.9673(4) 1.1341(3) 0.0363(9) Uani 1 1 d . . . 
O1 O -0.0970(5) -0.0569(3) 0.8177(3) 0.0442(9) Uani 1 1 d . . . 
O2 O -0.2368(4) -0.0383(3) 0.6617(3) 0.0277(7) Uani 1 1 d . . . 
O3 O -0.2645(4) -0.8018(3) 0.4403(3) 0.0317(7) Uani 1 1 d . . . 
O4 O -0.3558(5) -0.7613(3) 0.2829(3) 0.0461(10) Uani 1 1 d . . . 
O5 O 0.0084(3) 0.2216(3) 0.6532(3) 0.0269(7) Uani 1 1 d . . . 
O6 O 0.1541(3) 0.0654(3) 0.5994(2) 0.0256(6) Uani 1 1 d . . . 
O7 O 0.4854(3) 0.1125(3) 0.5900(2) 0.0218(6) Uani 1 1 d . . . 
O8 O 0.7119(3) 0.2710(3) 0.7179(2) 0.0251(7) Uani 1 1 d . . . 
O9W O 0.0099(4) 0.4893(4) 0.1265(3) 0.0472(10) Uani 1 1 d . . . 
O10W O 1.0131(9) 0.8152(7) 0.9651(6) 0.0440(17) Uani 0.50 1 d P . . 
O11W O 1.0117(14) 0.7539(12) 1.0816(9) 0.095(3) Uani 0.50 1 d P . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Tm1 O3 2.160(3) 1_565 ? 
Tm1 O2 2.160(3) . ? 
Tm1 O6 2.209(2) 2_556 ? 
Tm1 O5 2.271(3) . ? 
Tm1 O7 2.322(2) 2_556 ? 
Tm1 O8 2.401(3) 1_455 ? 
Tm1 O7 2.428(2) 1_455 ? 
Tm1 C18 2.804(3) 1_455 ? 
C1 O1 1.237(5) . ? 
C1 O2 1.275(5) . ? 
C1 C2 1.500(5) . ? 
C2 C8 1.385(6) . ? 
C2 C3 1.389(6) . ? 
C3 C4 1.385(6) . ? 
C3 H3 0.9300 . ? 
C4 C5 1.385(6) . ? 
C4 H4 0.9300 . ? 
C5 C7 1.375(6) . ? 
C5 C6 1.500(5) . ? 
C6 O4 1.235(5) . ? 
C6 O3 1.267(5) . ? 
C7 C8 1.386(6) . ? 
C7 H7 0.9300 . ? 
C8 H8 0.9300 . ? 
C9 O5 1.242(5) . ? 
C9 O6 1.260(4) . ? 
C9 C10 1.486(5) . ? 
C10 N1 1.360(4) . ? 
C10 C17 1.393(5) . ? 
C11 N2 1.318(5) . ? 
C11 N1 1.351(5) . ? 
C11 C12 1.467(5) . ? 
C12 C16 1.372(6) . ? 
C12 C13 1.390(6) . ? 
C13 C14 1.373(6) . ? 
C13 H13 0.9300 . ? 
C14 N3 1.320(7) . ? 
C14 H14 0.9300 . ? 
C15 N3 1.329(7) . ? 
C15 C16 1.375(6) . ? 
C15 H15 0.9300 . ? 
C16 H16 0.9300 . ? 
C17 N2 1.367(5) . ? 
C17 C18 1.474(5) . ? 
C18 O8 1.244(4) . ? 
C18 O7 1.278(4) . ? 
C18 Tm1 2.804(3) 1_655 ? 
N1 H1 0.8812 . ? 
O3 Tm1 2.160(3) 1_545 ? 
O6 Tm1 2.209(2) 2_556 ? 
O7 Tm1 2.322(2) 2_556 ? 
O7 Tm1 2.428(2) 1_655 ? 
O8 Tm1 2.401(3) 1_655 ? 
O10W O11W 1.764(14) . ? 
 
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 
O3 Tm1 O2 176.81(9) 1_565 . ? 
O3 Tm1 O6 86.51(11) 1_565 2_556 ? 
O2 Tm1 O6 96.00(11) . 2_556 ? 
O3 Tm1 O5 90.69(12) 1_565 . ? 
O2 Tm1 O5 87.29(12) . . ? 
O6 Tm1 O5 91.33(10) 2_556 . ? 
O3 Tm1 O7 91.26(11) 1_565 2_556 ? 
O2 Tm1 O7 91.29(11) . 2_556 ? 
O6 Tm1 O7 75.06(9) 2_556 2_556 ? 
O5 Tm1 O7 166.10(9) . 2_556 ? 
O3 Tm1 O8 88.83(11) 1_565 1_455 ? 
O2 Tm1 O8 88.24(10) . 1_455 ? 
O6 Tm1 O8 164.77(10) 2_556 1_455 ? 
O5 Tm1 O8 74.23(9) . 1_455 ? 
O7 Tm1 O8 119.57(9) 2_556 1_455 ? 
O3 Tm1 O7 86.31(11) 1_565 1_455 ? 
O2 Tm1 O7 92.95(10) . 1_455 ? 
O6 Tm1 O7 140.64(9) 2_556 1_455 ? 
O5 Tm1 O7 127.40(8) . 1_455 ? 
O7 Tm1 O7 66.48(9) 2_556 1_455 ? 
O8 Tm1 O7 53.23(8) 1_455 1_455 ? 
O3 Tm1 C18 85.91(11) 1_565 1_455 ? 
O2 Tm1 C18 92.03(11) . 1_455 ? 
O6 Tm1 C18 166.16(10) 2_556 1_455 ? 
O5 Tm1 C18 100.32(10) . 1_455 ? 
O7 Tm1 C18 93.54(9) 2_556 1_455 ? 
O8 Tm1 C18 26.23(10) 1_455 1_455 ? 
O7 Tm1 C18 27.07(9) 1_455 1_455 ? 
O1 C1 O2 123.5(4) . . ? 
O1 C1 C2 119.3(4) . . ? 
O2 C1 C2 117.2(3) . . ? 
C8 C2 C3 119.1(4) . . ? 
C8 C2 C1 119.1(4) . . ? 
C3 C2 C1 121.9(4) . . ? 
C4 C3 C2 120.4(4) . . ? 
C4 C3 H3 119.8 . . ? 
C2 C3 H3 119.8 . . ? 
C3 C4 C5 120.0(4) . . ? 
C3 C4 H4 120.0 . . ? 
C5 C4 H4 120.0 . . ? 
C7 C5 C4 119.8(4) . . ? 
C7 C5 C6 118.6(4) . . ? 
C4 C5 C6 121.7(4) . . ? 
O4 C6 O3 123.7(4) . . ? 
O4 C6 C5 118.4(4) . . ? 
O3 C6 C5 117.9(4) . . ? 
C5 C7 C8 120.4(4) . . ? 
C5 C7 H7 119.8 . . ? 
C8 C7 H7 119.8 . . ? 
C2 C8 C7 120.4(4) . . ? 
C2 C8 H8 119.8 . . ? 
C7 C8 H8 119.8 . . ? 
O5 C9 O6 124.9(4) . . ? 
O5 C9 C10 116.9(3) . . ? 
O6 C9 C10 118.1(3) . . ? 
N1 C10 C17 105.0(3) . . ? 
N1 C10 C9 120.0(3) . . ? 
C17 C10 C9 134.9(3) . . ? 
N2 C11 N1 112.2(3) . . ? 
N2 C11 C12 122.5(3) . . ? 
N1 C11 C12 125.3(3) . . ? 
C16 C12 C13 117.9(4) . . ? 
C16 C12 C11 119.5(4) . . ? 
C13 C12 C11 122.6(4) . . ? 
C14 C13 C12 119.3(4) . . ? 
C14 C13 H13 120.3 . . ? 
C12 C13 H13 120.3 . . ? 
N3 C14 C13 121.6(4) . . ? 
N3 C14 H14 119.2 . . ? 
C13 C14 H14 119.2 . . ? 
N3 C15 C16 121.1(5) . . ? 
N3 C15 H15 119.4 . . ? 
C16 C15 H15 119.4 . . ? 
C12 C16 C15 119.9(4) . . ? 
C12 C16 H16 120.0 . . ? 
C15 C16 H16 120.0 . . ? 
N2 C17 C10 110.2(3) . . ? 
N2 C17 C18 118.3(3) . . ? 
C10 C17 C18 131.4(3) . . ? 
O8 C18 O7 118.1(3) . . ? 
O8 C18 C17 119.7(3) . . ? 
O7 C18 C17 122.2(3) . . ? 
O8 C18 Tm1 58.51(18) . 1_655 ? 
O7 C18 Tm1 59.83(17) . 1_655 ? 
C17 C18 Tm1 172.8(3) . 1_655 ? 
C11 N1 C10 107.7(3) . . ? 
C11 N1 H1 126.4 . . ? 
C10 N1 H1 126.0 . . ? 
C11 N2 C17 105.0(3) . . ? 
C14 N3 C15 120.2(4) . . ? 
C1 O2 Tm1 155.5(3) . . ? 
C6 O3 Tm1 166.0(3) . 1_545 ? 
C9 O5 Tm1 128.8(2) . . ? 
C9 O6 Tm1 147.0(3) . 2_556 ? 
C18 O7 Tm1 153.4(2) . 2_556 ? 
C18 O7 Tm1 93.1(2) . 1_655 ? 
Tm1 O7 Tm1 113.52(9) 2_556 1_655 ? 
C18 O8 Tm1 95.3(2) . 1_655 ? 
 
_diffrn_measured_fraction_theta_max    0.999 
_diffrn_reflns_theta_full              25.00 
_diffrn_measured_fraction_theta_full   0.999 
_refine_diff_density_max    1.638 
_refine_diff_density_min   -0.961 
_refine_diff_density_rms    0.121 

# Start Validation Reply Form

_vrf_PLAT306_7-Tm
;
PROBLEM:
  Isolated Oxygen Atom (H-atoms Missing ?) .......        O9W     
   
 

RESPONSE: This is because the hydrogen atoms attaching to free water molecules have not been added.
; 

 
data_8-Yb 
 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C18 H9 N3 O10 Yb' 
_chemical_formula_weight          600.32 
 
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' 
 'Yb'  'Yb'  -0.3850   5.5486 
 '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                    8.4728(5) 
_cell_length_b                    10.4366(5) 
_cell_length_c                    12.1520(8) 
_cell_angle_alpha                 112.738(5) 
_cell_angle_beta                  96.828(5) 
_cell_angle_gamma                 103.269(5) 
_cell_volume                      938.44(9) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     298(2) 
_cell_measurement_reflns_used     4856
_cell_measurement_theta_min       2.5335
_cell_measurement_theta_max       29.1326
 
_exptl_crystal_description        block 
_exptl_crystal_colour             colorless  
_exptl_crystal_size_max           0.12 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.08 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     2.124 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              576 
_exptl_absorpt_coefficient_mu     5.050 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.5825 
_exptl_absorpt_correction_T_max   0.6881 
_exptl_absorpt_process_details   

;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
; 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       298(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   'Xcalibur, Eos'
_diffrn_measurement_method        'ω scans'
_diffrn_detector_area_resol_mean  16.2083
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             8830 
_diffrn_reflns_av_R_equivalents   0.0436 
_diffrn_reflns_av_sigmaI/netI     0.0523 
_diffrn_reflns_limit_h_min        -10 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -14 
_diffrn_reflns_limit_l_max        14 
_diffrn_reflns_theta_min          2.54 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              3305 
_reflns_number_gt                 3045 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        

;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;

_computing_cell_refinement        

;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;

_computing_data_reduction         

;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_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)+(0.0210P)²+0.4622P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          3305 
_refine_ls_number_parameters      298 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0305 
_refine_ls_R_factor_gt            0.0267 
_refine_ls_wR_factor_ref          0.0593 
_refine_ls_wR_factor_gt           0.0573 
_refine_ls_goodness_of_fit_ref    1.030 
_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 
Yb1 Yb -0.25332(2) 0.07425(2) 0.546522(18) 0.01539(8) Uani 1 1 d . . . 
C1 C -0.1738(6) -0.1098(5) 0.7088(5) 0.0231(12) Uani 1 1 d . . . 
C2 C -0.2012(6) -0.2679(5) 0.6286(4) 0.0207(11) Uani 1 1 d . . . 
C3 C -0.1146(6) -0.3483(5) 0.6643(5) 0.0309(13) Uani 1 1 d . . . 
H3 H -0.0365 -0.3040 0.7388 0.037 Uiso 1 1 calc R . . 
C4 C -0.1444(6) -0.4945(5) 0.5891(5) 0.0291(13) Uani 1 1 d . . . 
H4 H -0.0872 -0.5485 0.6139 0.035 Uiso 1 1 calc R . . 
C5 C -0.2588(6) -0.5611(5) 0.4769(4) 0.0225(11) Uani 1 1 d . . . 
C6 C -0.2958(6) -0.7194(5) 0.3935(5) 0.0256(12) Uani 1 1 d . . . 
C7 C -0.3428(6) -0.4802(5) 0.4403(5) 0.0241(12) Uani 1 1 d . . . 
H7 H -0.4176 -0.5233 0.3644 0.029 Uiso 1 1 calc R . . 
C8 C -0.3155(6) -0.3344(5) 0.5172(4) 0.0227(11) Uani 1 1 d . . . 
H8 H -0.3748 -0.2810 0.4933 0.027 Uiso 1 1 calc R . . 
C9 C 0.1397(6) 0.1883(5) 0.6561(4) 0.0181(11) Uani 1 1 d . . . 
C10 C 0.2937(5) 0.3092(5) 0.7379(4) 0.0126(10) Uani 1 1 d . . . 
C11 C 0.4386(5) 0.5298(5) 0.8720(4) 0.0174(10) Uani 1 1 d . . . 
C12 C 0.4792(6) 0.6826(5) 0.9624(4) 0.0199(11) Uani 1 1 d . . . 
C13 C 0.3625(7) 0.7460(5) 1.0073(5) 0.0350(14) Uani 1 1 d . . . 
H13 H 0.2501 0.6930 0.9797 0.042 Uiso 1 1 calc R . . 
C14 C 0.4116(8) 0.8887(6) 1.0937(6) 0.0422(15) Uani 1 1 d . . . 
H14 H 0.3311 0.9308 1.1239 0.051 Uiso 1 1 calc R . . 
C15 C 0.6848(8) 0.9093(6) 1.0919(6) 0.0485(18) Uani 1 1 d . . . 
H15 H 0.7959 0.9660 1.1204 0.058 Uiso 1 1 calc R . . 
C16 C 0.6454(6) 0.7661(5) 1.0053(6) 0.0380(15) Uani 1 1 d . . . 
H16 H 0.7285 0.7269 0.9767 0.046 Uiso 1 1 calc R . . 
C17 C 0.4643(5) 0.3278(5) 0.7499(4) 0.0152(10) Uani 1 1 d . . . 
C18 C 0.5574(5) 0.2327(5) 0.6843(4) 0.0145(10) Uani 1 1 d . . . 
N1 N 0.2812(4) 0.4385(4) 0.8163(3) 0.0161(9) Uani 1 1 d . . . 
H1 H 0.1881 0.4594 0.8286 0.019 Uiso 1 1 d R . . 
N2 N 0.5516(4) 0.4669(4) 0.8347(4) 0.0187(9) Uani 1 1 d . . . 
N3 N 0.5705(6) 0.9672(5) 1.1348(4) 0.0338(11) Uani 1 1 d . . . 
O1 O -0.0961(5) -0.0560(4) 0.8170(4) 0.0439(11) Uani 1 1 d . . . 
O2 O -0.2379(4) -0.0387(3) 0.6604(3) 0.0264(8) Uani 1 1 d . . . 
O3 O -0.2648(4) -0.8018(3) 0.4421(3) 0.0302(9) Uani 1 1 d . . . 
O4 O -0.3567(5) -0.7623(4) 0.2827(4) 0.0445(11) Uani 1 1 d . . . 
O5 O 0.0075(4) 0.2206(3) 0.6522(3) 0.0261(8) Uani 1 1 d . . . 
O6 O 0.1538(4) 0.0643(3) 0.5992(3) 0.0251(8) Uani 1 1 d . . . 
O7 O 0.4853(4) 0.1115(3) 0.5899(3) 0.0215(8) Uani 1 1 d . . . 
O8 O 0.7123(4) 0.2710(3) 0.7179(3) 0.0235(8) Uani 1 1 d . . . 
O9W O 0.0114(4) 0.4898(4) 0.1251(4) 0.0442(11) Uani 1 1 d . . . 
O10W O 1.0129(9) 0.8164(8) 0.9656(8) 0.042(2) Uani 0.50 1 d P . . 
O11W O 1.0107(15) 0.7510(14) 1.0839(14) 0.119(5) Uani 0.50 1 d P . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Yb1 O3 2.142(3) 1_565 ? 
Yb1 O2 2.147(3) . ? 
Yb1 O6 2.207(3) 2_556 ? 
Yb1 O5 2.264(3) . ? 
Yb1 O7 2.316(3) 2_556 ? 
Yb1 O8 2.398(3) 1_455 ? 
Yb1 O7 2.418(3) 1_455 ? 
Yb1 C18 2.797(5) 1_455 ? 
Yb1 Yb1 3.9625(5) 2_456 ? 
C1 O1 1.238(6) . ? 
C1 O2 1.279(6) . ? 
C1 C2 1.501(6) . ? 
C2 C8 1.380(6) . ? 
C2 C3 1.386(7) . ? 
C3 C4 1.386(7) . ? 
C3 H3 0.9300 . ? 
C4 C5 1.387(7) . ? 
C4 H4 0.9300 . ? 
C5 C7 1.382(7) . ? 
C5 C6 1.499(6) . ? 
C6 O4 1.242(6) . ? 
C6 O3 1.272(6) . ? 
C7 C8 1.389(6) . ? 
C7 H7 0.9300 . ? 
C8 H8 0.9300 . ? 
C9 O5 1.242(5) . ? 
C9 O6 1.252(5) . ? 
C9 C10 1.499(6) . ? 
C10 N1 1.355(5) . ? 
C10 C17 1.396(6) . ? 
C11 N2 1.309(6) . ? 
C11 N1 1.359(5) . ? 
C11 C12 1.474(6) . ? 
C12 C13 1.365(7) . ? 
C12 C16 1.387(7) . ? 
C13 C14 1.376(7) . ? 
C13 H13 0.9300 . ? 
C14 N3 1.323(7) . ? 
C14 H14 0.9300 . ? 
C15 N3 1.312(8) . ? 
C15 C16 1.387(8) . ? 
C15 H15 0.9300 . ? 
C16 H16 0.9300 . ? 
C17 N2 1.374(5) . ? 
C17 C18 1.463(6) . ? 
C18 O8 1.246(5) . ? 
C18 O7 1.283(5) . ? 
C18 Yb1 2.797(5) 1_655 ? 
N1 H1 0.8800 . ? 
O3 Yb1 2.142(3) 1_545 ? 
O6 Yb1 2.207(3) 2_556 ? 
O7 Yb1 2.316(3) 2_556 ? 
O7 Yb1 2.418(3) 1_655 ? 
O8 Yb1 2.398(3) 1_655 ? 
O10W O11W 1.814(16) . ? 
 
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 
O3 Yb1 O2 176.78(12) 1_565 . ? 
O3 Yb1 O6 86.40(13) 1_565 2_556 ? 
O2 Yb1 O6 96.18(13) . 2_556 ? 
O3 Yb1 O5 90.42(13) 1_565 . ? 
O2 Yb1 O5 87.62(13) . . ? 
O6 Yb1 O5 90.94(12) 2_556 . ? 
O3 Yb1 O7 91.25(12) 1_565 2_556 ? 
O2 Yb1 O7 91.27(12) . 2_556 ? 
O6 Yb1 O7 75.22(11) 2_556 2_556 ? 
O5 Yb1 O7 165.92(12) . 2_556 ? 
O3 Yb1 O8 88.67(13) 1_565 1_455 ? 
O2 Yb1 O8 88.34(12) . 1_455 ? 
O6 Yb1 O8 164.34(10) 2_556 1_455 ? 
O5 Yb1 O8 74.23(11) . 1_455 ? 
O7 Yb1 O8 119.78(10) 2_556 1_455 ? 
O3 Yb1 O7 86.54(13) 1_565 1_455 ? 
O2 Yb1 O7 92.63(12) . 1_455 ? 
O6 Yb1 O7 140.71(11) 2_556 1_455 ? 
O5 Yb1 O7 127.71(11) . 1_455 ? 
O7 Yb1 O7 66.35(13) 2_556 1_455 ? 
O8 Yb1 O7 53.53(10) 1_455 1_455 ? 
O3 Yb1 C18 85.84(13) 1_565 1_455 ? 
O2 Yb1 C18 91.99(13) . 1_455 ? 
O6 Yb1 C18 166.25(12) 2_556 1_455 ? 
O5 Yb1 C18 100.45(12) . 1_455 ? 
O7 Yb1 C18 93.61(12) 2_556 1_455 ? 
O8 Yb1 C18 26.35(11) 1_455 1_455 ? 
O7 Yb1 C18 27.26(11) 1_455 1_455 ? 
O3 Yb1 Yb1 88.62(9) 1_565 2_456 ? 
O2 Yb1 Yb1 92.35(9) . 2_456 ? 
O6 Yb1 Yb1 108.86(8) 2_556 2_456 ? 
O5 Yb1 Yb1 160.07(9) . 2_456 ? 
O7 Yb1 Yb1 33.99(8) 2_556 2_456 ? 
O8 Yb1 Yb1 85.84(7) 1_455 2_456 ? 
O7 Yb1 Yb1 32.37(7) 1_455 2_456 ? 
C18 Yb1 Yb1 59.62(8) 1_455 2_456 ? 
O1 C1 O2 123.6(5) . . ? 
O1 C1 C2 119.6(4) . . ? 
O2 C1 C2 116.8(4) . . ? 
C8 C2 C3 119.5(4) . . ? 
C8 C2 C1 119.2(4) . . ? 
C3 C2 C1 121.3(4) . . ? 
C4 C3 C2 120.0(5) . . ? 
C4 C3 H3 120.0 . . ? 
C2 C3 H3 120.0 . . ? 
C3 C4 C5 120.5(5) . . ? 
C3 C4 H4 119.8 . . ? 
C5 C4 H4 119.8 . . ? 
C7 C5 C4 119.5(4) . . ? 
C7 C5 C6 118.4(4) . . ? 
C4 C5 C6 122.1(5) . . ? 
O4 C6 O3 124.2(5) . . ? 
O4 C6 C5 118.6(5) . . ? 
O3 C6 C5 117.2(5) . . ? 
C5 C7 C8 119.9(5) . . ? 
C5 C7 H7 120.0 . . ? 
C8 C7 H7 120.0 . . ? 
C2 C8 C7 120.7(5) . . ? 
C2 C8 H8 119.7 . . ? 
C7 C8 H8 119.7 . . ? 
O5 C9 O6 125.6(4) . . ? 
O5 C9 C10 116.3(4) . . ? 
O6 C9 C10 118.1(4) . . ? 
N1 C10 C17 105.5(4) . . ? 
N1 C10 C9 120.2(4) . . ? 
C17 C10 C9 134.2(4) . . ? 
N2 C11 N1 112.1(4) . . ? 
N2 C11 C12 123.4(4) . . ? 
N1 C11 C12 124.5(4) . . ? 
C13 C12 C16 118.2(5) . . ? 
C13 C12 C11 123.6(4) . . ? 
C16 C12 C11 118.2(5) . . ? 
C12 C13 C14 119.9(5) . . ? 
C12 C13 H13 120.1 . . ? 
C14 C13 H13 120.1 . . ? 
N3 C14 C13 121.6(6) . . ? 
N3 C14 H14 119.2 . . ? 
C13 C14 H14 119.2 . . ? 
N3 C15 C16 122.1(5) . . ? 
N3 C15 H15 118.9 . . ? 
C16 C15 H15 118.9 . . ? 
C15 C16 C12 118.5(6) . . ? 
C15 C16 H16 120.7 . . ? 
C12 C16 H16 120.7 . . ? 
N2 C17 C10 109.4(4) . . ? 
N2 C17 C18 118.5(4) . . ? 
C10 C17 C18 132.0(4) . . ? 
O8 C18 O7 118.1(4) . . ? 
O8 C18 C17 119.8(4) . . ? 
O7 C18 C17 122.1(4) . . ? 
O8 C18 Yb1 58.7(2) . 1_655 ? 
O7 C18 Yb1 59.7(2) . 1_655 ? 
C17 C18 Yb1 173.2(3) . 1_655 ? 
C10 N1 C11 107.5(4) . . ? 
C10 N1 H1 126.1 . . ? 
C11 N1 H1 126.4 . . ? 
C11 N2 C17 105.5(4) . . ? 
C15 N3 C14 119.7(5) . . ? 
C1 O2 Yb1 155.2(3) . . ? 
C6 O3 Yb1 167.1(4) . 1_545 ? 
C9 O5 Yb1 128.6(3) . . ? 
C9 O6 Yb1 146.6(3) . 2_556 ? 
C18 O7 Yb1 153.3(3) . 2_556 ? 
C18 O7 Yb1 93.1(3) . 1_655 ? 
Yb1 O7 Yb1 113.65(13) 2_556 1_655 ? 
C18 O8 Yb1 95.0(3) . 1_655 ? 
 
_diffrn_measured_fraction_theta_max    0.999 
_diffrn_reflns_theta_full              25.00 
_diffrn_measured_fraction_theta_full   0.999 
_refine_diff_density_max    0.733 
_refine_diff_density_min   -0.786 
_refine_diff_density_rms    0.133 

# Start Validation Reply Form

_vrf_PLAT306_8-Yb
;
PROBLEM:
  Isolated Oxygen Atom (H-atoms Missing ?) .......        O9W     
   
 

RESPONSE: This is because the hydrogen atoms attaching to free water molecules have not been added.
; 