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

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

data_69-1
_database_code_depnum_ccdc_archive 'CCDC 1000758'
_audit_update_record             
;
2014-10-08 deposited with the CCDC.
2015-01-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
' C88 H100 Dy4 N10 O24, 2(N O3), 0.66(O4), 0.66(O2)  '
_chemical_formula_sum            ' C88 H100 Dy4 N12 O33.96  '
_chemical_formula_weight         2519.17

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 '
_symmetry_space_group_name_Hall  ' -P 1 '

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

_cell_length_a                   14.4293(7)
_cell_length_b                   14.5421(9)
_cell_length_c                   14.7018(8)
_cell_angle_alpha                111.061(5)
_cell_angle_beta                 104.181(4)
_cell_angle_gamma                107.967(5)
_cell_volume                     2508.8(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1247.7
_exptl_absorpt_coefficient_mu    3.030
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.503
_exptl_absorpt_correction_T_max  0.580
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'

_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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19128
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0537
_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       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.86
_diffrn_reflns_theta_max         25.00
_reflns_number_total             8834
_reflns_number_gt                6938
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_cell_refinement       'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXL-97

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
The water molecules in complex are highly disordered, and H-atoms can not be added. But the H-atoms located on the water molecules are took into consideration in the formular of complex.
;

_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)+(0.0343P)²+3.6472P] 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         8834
_refine_ls_number_parameters     632
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0351
_refine_ls_wR_factor_ref         0.0930
_refine_ls_wR_factor_gt          0.0819
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.074
_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
C1 C 0.1052(5) 0.1087(5) 0.2712(5) 0.0351(14) Uani 1 1 d . . .
C2 C 0.0114(5) 0.0837(5) 0.1877(5) 0.0346(14) Uani 1 1 d . . .
C3 C -0.0366(5) -0.0145(5) 0.0952(5) 0.0438(16) Uani 1 1 d . . .
H3 H -0.0996 -0.0316 0.0427 0.053 Uiso 1 1 calc R . .
C4 C 0.0078(6) -0.0885(6) 0.0792(5) 0.0478(17) Uani 1 1 d . . .
H4 H -0.0242 -0.1533 0.0155 0.057 Uiso 1 1 calc R . .
C5 C 0.0979(5) -0.0656(5) 0.1570(6) 0.0438(17) Uani 1 1 d . . .
H5 H 0.1275 -0.1150 0.1462 0.053 Uiso 1 1 calc R . .
C6 C 0.1471(5) 0.0324(5) 0.2544(5) 0.0370(15) Uani 1 1 d . . .
C7 C 0.2396(5) 0.0510(5) 0.3360(6) 0.0418(16) Uani 1 1 d . . .
H7 H 0.2635 -0.0030 0.3235 0.050 Uiso 1 1 calc R . .
C8 C 0.3856(5) 0.1643(5) 0.5145(5) 0.0401(16) Uani 1 1 d . . .
H8 H 0.3707 0.1026 0.5303 0.048 Uiso 1 1 calc R . .
C9 C 0.4818(5) 0.1812(7) 0.4850(6) 0.060(2) Uani 1 1 d . . .
H9A H 0.4676 0.1145 0.4247 0.072 Uiso 1 1 calc R . .
H9B H 0.4949 0.2392 0.4650 0.072 Uiso 1 1 calc R . .
C10 C 0.5782(6) 0.2113(8) 0.5784(7) 0.071(2) Uani 1 1 d . . .
H10A H 0.5670 0.1504 0.5941 0.085 Uiso 1 1 calc R . .
H10B H 0.6395 0.2247 0.5600 0.085 Uiso 1 1 calc R . .
C11 C 0.6001(6) 0.3117(8) 0.6755(7) 0.073(2) Uani 1 1 d . . .
H11A H 0.6180 0.3741 0.6619 0.087 Uiso 1 1 calc R . .
H11B H 0.6608 0.3269 0.7346 0.087 Uiso 1 1 calc R . .
C12 C 0.5053(5) 0.2971(7) 0.7051(6) 0.0564(19) Uani 1 1 d . . .
H12A H 0.5208 0.3648 0.7651 0.068 Uiso 1 1 calc R . .
H12B H 0.4923 0.2402 0.7265 0.068 Uiso 1 1 calc R . .
C13 C 0.4062(5) 0.2664(6) 0.6125(5) 0.0421(16) Uani 1 1 d . . .
H13 H 0.4160 0.3275 0.5960 0.050 Uiso 1 1 calc R . .
C14 C 0.2605(5) 0.2968(5) 0.6338(5) 0.0365(15) Uani 1 1 d . . .
H14 H 0.2813 0.3486 0.6108 0.044 Uiso 1 1 calc R . .
C15 C 0.1685(5) 0.2813(5) 0.6633(5) 0.0346(14) Uani 1 1 d . . .
C16 C 0.1510(5) 0.2221(5) 0.7198(5) 0.0440(17) Uani 1 1 d . . .
H16 H 0.1972 0.1928 0.7376 0.053 Uiso 1 1 calc R . .
C17 C 0.0665(5) 0.2073(6) 0.7489(6) 0.0483(18) Uani 1 1 d . . .
H17 H 0.0550 0.1667 0.7849 0.058 Uiso 1 1 calc R . .
C18 C -0.0028(5) 0.2525(5) 0.7250(5) 0.0429(16) Uani 1 1 d . . .
H18 H -0.0595 0.2432 0.7457 0.051 Uiso 1 1 calc R . .
C19 C 0.0148(5) 0.3110(5) 0.6704(5) 0.0337(14) Uani 1 1 d . . .
C20 C 0.0987(5) 0.3242(5) 0.6358(5) 0.0307(13) Uani 1 1 d . . .
C21 C -0.1229(5) 0.1402(6) 0.1360(5) 0.0456(17) Uani 1 1 d . . .
H21A H -0.1193 0.1247 0.0681 0.068 Uiso 1 1 calc R . .
H21B H -0.1381 0.2024 0.1604 0.068 Uiso 1 1 calc R . .
H21C H -0.1783 0.0778 0.1293 0.068 Uiso 1 1 calc R . .
C22 C -0.1451(5) 0.3358(6) 0.6566(7) 0.056(2) Uani 1 1 d . . .
H22A H -0.1859 0.2576 0.6172 0.084 Uiso 1 1 calc R . .
H22B H -0.1832 0.3699 0.6287 0.084 Uiso 1 1 calc R . .
H22C H -0.1335 0.3600 0.7302 0.084 Uiso 1 1 calc R . .
C23 C 0.0519(5) 0.3885(5) 0.1939(5) 0.0326(14) Uani 1 1 d . . .
C24 C -0.0098(5) 0.3940(5) 0.1081(5) 0.0386(15) Uani 1 1 d . . .
C25 C 0.0243(5) 0.3903(5) 0.0259(5) 0.0448(17) Uani 1 1 d . . .
H25 H -0.0177 0.3912 -0.0326 0.054 Uiso 1 1 calc R . .
C26 C 0.1169(6) 0.3854(6) 0.0302(6) 0.0513(19) Uani 1 1 d . . .
H26 H 0.1403 0.3881 -0.0228 0.062 Uiso 1 1 calc R . .
C27 C 0.1779(5) 0.3764(6) 0.1128(5) 0.0470(17) Uani 1 1 d . . .
H27 H 0.2408 0.3711 0.1142 0.056 Uiso 1 1 calc R . .
C28 C 0.1444(5) 0.3754(5) 0.1930(5) 0.0372(15) Uani 1 1 d . . .
C29 C -0.1144(5) 0.3917(5) 0.0937(5) 0.0412(16) Uani 1 1 d . . .
H29 H -0.1584 0.3725 0.0254 0.049 Uiso 1 1 calc R . .
C30 C -0.2669(5) 0.3881(6) 0.1248(5) 0.0428(16) Uani 1 1 d . . .
H30 H -0.3049 0.3103 0.0723 0.051 Uiso 1 1 calc R . .
C31 C -0.2972(5) 0.4489(6) 0.0675(6) 0.0545(19) Uani 1 1 d . . .
H31A H -0.2780 0.4321 0.0067 0.065 Uiso 1 1 calc R . .
H31B H -0.2573 0.5271 0.1149 0.065 Uiso 1 1 calc R . .
C32 C -0.4149(6) 0.4189(7) 0.0299(6) 0.069(2) Uani 1 1 d . . .
H32A H -0.4281 0.4689 0.0049 0.083 Uiso 1 1 calc R . .
H32B H -0.4536 0.3456 -0.0299 0.083 Uiso 1 1 calc R . .
C33 C -0.4570(6) 0.4229(7) 0.1142(7) 0.066(2) Uani 1 1 d . . .
H33A H -0.5340 0.3906 0.0815 0.079 Uiso 1 1 calc R . .
H33B H -0.4320 0.4990 0.1652 0.079 Uiso 1 1 calc R . .
C34 C -0.4241(5) 0.3633(6) 0.1739(6) 0.0533(19) Uani 1 1 d . . .
H34A H -0.4440 0.3789 0.2342 0.064 Uiso 1 1 calc R . .
H34B H -0.4610 0.2848 0.1271 0.064 Uiso 1 1 calc R . .
C35 C -0.3058(5) 0.3997(6) 0.2121(6) 0.0435(16) Uani 1 1 d . . .
H35 H -0.2736 0.4787 0.2600 0.052 Uiso 1 1 calc R . .
C36 C -0.3131(5) 0.2699(5) 0.2791(5) 0.0418(16) Uani 1 1 d . . .
H36 H -0.3865 0.2439 0.2479 0.050 Uiso 1 1 calc R . .
C37 C -0.2746(5) 0.2103(5) 0.3278(5) 0.0385(15) Uani 1 1 d . . .
C38 C -0.3510(5) 0.1244(6) 0.3299(6) 0.057(2) Uani 1 1 d . . .
H38 H -0.4211 0.1145 0.3089 0.068 Uiso 1 1 calc R . .
C39 C -0.3260(6) 0.0559(7) 0.3612(7) 0.065(2) Uani 1 1 d . . .
H39 H -0.3781 0.0015 0.3640 0.079 Uiso 1 1 calc R . .
C40 C -0.2234(5) 0.0659(6) 0.3894(6) 0.0538(19) Uani 1 1 d . . .
H40 H -0.2068 0.0173 0.4095 0.065 Uiso 1 1 calc R . .
C41 C -0.1463(5) 0.1476(5) 0.3875(5) 0.0378(15) Uani 1 1 d . . .
C42 C -0.1690(5) 0.2248(5) 0.3605(5) 0.0325(14) Uani 1 1 d . . .
C43 C 0.2914(6) 0.3513(7) 0.2850(7) 0.064(2) Uani 1 1 d . . .
H43A H 0.2786 0.2898 0.2213 0.097 Uiso 1 1 calc R . .
H43B H 0.3165 0.3403 0.3452 0.097 Uiso 1 1 calc R . .
H43C H 0.3439 0.4169 0.2936 0.097 Uiso 1 1 calc R . .
C44 C -0.0181(5) 0.0820(5) 0.4302(6) 0.0488(18) Uani 1 1 d . . .
H44A H -0.0296 0.0823 0.4919 0.073 Uiso 1 1 calc R . .
H44B H 0.0548 0.0982 0.4422 0.073 Uiso 1 1 calc R . .
H44C H -0.0634 0.0111 0.3698 0.073 Uiso 1 1 calc R . .
Dy1 Dy 0.08547(2) 0.32984(2) 0.39760(2) 0.02950(9) Uani 1 1 d . . .
Dy2 Dy -0.06759(2) 0.46914(2) 0.35867(2) 0.02580(9) Uani 1 1 d . . .
N1 N 0.3124(4) 0.2406(4) 0.6393(4) 0.0422(13) Uani 1 1 d . . .
N2 N 0.2909(4) 0.1392(4) 0.4258(4) 0.0391(13) Uani 1 1 d D . .
H21 H 0.2548 0.1810 0.4309 0.047 Uiso 1 1 d RD . .
N3 N -0.1522(4) 0.4133(4) 0.1652(4) 0.0374(12) Uani 1 1 d . . .
N4 N -0.2574(4) 0.3536(4) 0.2745(4) 0.0341(12) Uani 1 1 d . . .
N5 N 0.3366(4) 0.5326(5) 0.5223(5) 0.0471(14) Uani 1 1 d . . .
N6 N 0.6811(9) 0.1561(10) 0.8116(10) 0.128(4) Uani 1 1 d . . .
O1 O 0.1477(3) 0.2012(3) 0.3602(3) 0.0384(10) Uani 1 1 d . . .
O2 O -0.0232(3) 0.1637(3) 0.2111(3) 0.0424(11) Uani 1 1 d . . .
O3 O 0.1085(3) 0.3815(3) 0.5812(3) 0.0303(9) Uani 1 1 d . . .
O4 O -0.0444(3) 0.3656(3) 0.6474(3) 0.0355(10) Uani 1 1 d . . .
O5 O 0.0270(3) 0.3926(3) 0.2764(3) 0.0333(9) Uani 1 1 d . . .
O6 O 0.1935(3) 0.3617(4) 0.2771(4) 0.0477(12) Uani 1 1 d . . .
O7 O -0.0897(3) 0.3044(3) 0.3633(3) 0.0289(9) Uani 1 1 d . . .
O8 O -0.0422(3) 0.1634(3) 0.4105(4) 0.0393(10) Uani 1 1 d . . .
O9 O 0.2719(3) 0.4372(4) 0.5017(4) 0.0421(11) Uani 1 1 d . . .
O10 O 0.3004(4) 0.5896(4) 0.4948(5) 0.0626(15) Uani 1 1 d . . .
O11 O 0.4313(4) 0.5647(5) 0.5700(5) 0.089(2) Uani 1 1 d . . .
O12 O 0.0908(3) 0.5049(3) 0.4848(3) 0.0265(8) Uani 1 1 d D . .
H121 H 0.1531 0.5483 0.4988 0.032 Uiso 1 1 d RD . .
O13 O 0.7564(8) 0.2031(9) 0.7995(9) 0.155(4) Uani 1 1 d . . .
O14 O 0.6581(12) 0.1959(13) 0.8748(11) 0.311(11) Uani 1 1 d . . .
O15 O 0.6193(8) 0.0657(8) 0.7465(9) 0.192(6) Uani 1 1 d . . .
O16A O 0.3936(16) 0.0543(18) 0.0776(18) 0.103(6) Uiso 0.33 1 d P . .
O17A O 0.364(2) 0.095(2) -0.062(2) 0.153(10) Uiso 0.33 1 d P . .
O16B O 0.314(2) 0.154(2) -0.105(2) 0.149(10) Uiso 0.33 1 d P . .
O17B O 0.322(3) 0.120(3) 0.094(3) 0.202(14) Uiso 0.33 1 d P . .
O17C O 0.306(2) 0.164(2) 0.022(3) 0.157(10) Uiso 0.33 1 d P . .
O16C O 0.364(2) 0.094(2) 0.154(2) 0.135(9) Uiso 0.33 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
C1 O1 1.316(7) . ?
C1 C6 1.396(8) . ?
C1 C2 1.425(8) . ?
C2 O2 1.370(7) . ?
C2 C3 1.378(9) . ?
C3 C4 1.393(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.357(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.413(9) . ?
C5 H5 0.9300 . ?
C6 C7 1.432(9) . ?
C7 N2 1.286(8) . ?
C7 H7 0.9300 . ?
C8 N2 1.476(8) . ?
C8 C9 1.528(8) . ?
C8 C13 1.533(9) . ?
C8 H8 0.9800 . ?
C9 C10 1.506(10) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.506(11) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.512(9) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.521(9) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N1 1.478(7) . ?
C13 H13 0.9800 . ?
C14 N1 1.276(7) . ?
C14 C15 1.472(8) . ?
C14 H14 0.9300 . ?
C15 C20 1.391(8) . ?
C15 C16 1.406(8) . ?
C16 C17 1.370(8) . ?
C16 H16 0.9300 . ?
C17 C18 1.396(9) . ?
C17 H17 0.9300 . ?
C18 C19 1.376(8) . ?
C18 H18 0.9300 . ?
C19 O4 1.395(7) . ?
C19 C20 1.411(7) . ?
C20 O3 1.350(6) . ?
C21 O2 1.433(7) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 O4 1.438(6) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 O5 1.333(6) . ?
C23 C24 1.398(8) . ?
C23 C28 1.408(8) . ?
C24 C25 1.402(8) . ?
C24 C29 1.459(9) . ?
C25 C26 1.347(9) . ?
C25 H25 0.9300 . ?
C26 C27 1.388(9) . ?
C26 H26 0.9300 . ?
C27 C28 1.383(8) . ?
C27 H27 0.9300 . ?
C28 O6 1.381(7) . ?
C29 N3 1.286(7) . ?
C29 H29 0.9300 . ?
C30 N3 1.488(7) . ?
C30 C35 1.499(9) . ?
C30 C31 1.507(9) . ?
C30 H30 0.9800 . ?
C31 C32 1.514(9) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C33 1.500(10) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 C34 1.530(9) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 C35 1.506(8) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 N4 1.482(7) . ?
C35 H35 0.9800 . ?
C36 N4 1.271(7) . ?
C36 C37 1.456(9) . ?
C36 H36 0.9300 . ?
C37 C42 1.402(8) . ?
C37 C38 1.404(8) . ?
C38 C39 1.342(10) . ?
C38 H38 0.9300 . ?
C39 C40 1.382(9) . ?
C39 H39 0.9300 . ?
C40 C41 1.369(8) . ?
C40 H40 0.9300 . ?
C41 O8 1.380(7) . ?
C41 C42 1.418(8) . ?
C42 O7 1.333(6) . ?
C43 O6 1.448(7) . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 O8 1.433(7) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
Dy1 O1 2.268(4) . ?
Dy1 O7 2.333(4) . ?
Dy1 O12 2.370(4) . ?
Dy1 O5 2.373(4) . ?
Dy1 O9 2.386(4) . ?
Dy1 O3 2.431(4) . ?
Dy1 O2 2.571(4) . ?
Dy1 O8 2.654(4) . ?
Dy1 O6 2.698(4) . ?
Dy1 Dy2 3.5046(4) . ?
Dy1 Dy2 3.8525(5) 2_566 ?
Dy2 O5 2.312(4) . ?
Dy2 O12 2.321(3) 2_566 ?
Dy2 O12 2.330(4) . ?
Dy2 O7 2.346(4) . ?
Dy2 O3 2.348(4) 2_566 ?
Dy2 N4 2.421(5) . ?
Dy2 O4 2.495(4) 2_566 ?
Dy2 N3 2.503(5) . ?
Dy2 Dy2 3.7611(6) 2_566 ?
Dy2 Dy1 3.8525(5) 2_566 ?
N2 H21 0.9096 . ?
N5 O11 1.217(7) . ?
N5 O10 1.236(7) . ?
N5 O9 1.284(7) . ?
N6 O14 1.092(12) . ?
N6 O15 1.181(12) . ?
N6 O13 1.186(12) . ?
O3 Dy2 2.348(4) 2_566 ?
O4 Dy2 2.495(4) 2_566 ?
O12 Dy2 2.321(3) 2_566 ?
O12 H121 0.8450 . ?
O16A O16C 1.30(3) . ?
O16A O17B 1.61(4) . ?
O17A O16B 1.48(3) . ?
O17B O16C 1.18(4) . ?
O17B O17C 1.43(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C6 123.1(6) . . ?
O1 C1 C2 119.1(5) . . ?
C6 C1 C2 117.8(6) . . ?
O2 C2 C3 126.3(6) . . ?
O2 C2 C1 113.6(5) . . ?
C3 C2 C1 120.1(6) . . ?
C2 C3 C4 121.1(6) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
C5 C4 C3 119.7(6) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 120.7(6) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C1 C6 C5 120.5(6) . . ?
C1 C6 C7 120.7(6) . . ?
C5 C6 C7 118.8(6) . . ?
N2 C7 C6 122.8(6) . . ?
N2 C7 H7 118.6 . . ?
C6 C7 H7 118.6 . . ?
N2 C8 C9 110.9(5) . . ?
N2 C8 C13 108.2(5) . . ?
C9 C8 C13 111.5(6) . . ?
N2 C8 H8 108.7 . . ?
C9 C8 H8 108.7 . . ?
C13 C8 H8 108.7 . . ?
C10 C9 C8 109.8(6) . . ?
C10 C9 H9A 109.7 . . ?
C8 C9 H9A 109.7 . . ?
C10 C9 H9B 109.7 . . ?
C8 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
C11 C10 C9 111.5(7) . . ?
C11 C10 H10A 109.3 . . ?
C9 C10 H10A 109.3 . . ?
C11 C10 H10B 109.3 . . ?
C9 C10 H10B 109.3 . . ?
H10A C10 H10B 108.0 . . ?
C10 C11 C12 111.7(7) . . ?
C10 C11 H11A 109.3 . . ?
C12 C11 H11A 109.3 . . ?
C10 C11 H11B 109.3 . . ?
C12 C11 H11B 109.3 . . ?
H11A C11 H11B 107.9 . . ?
C11 C12 C13 111.4(6) . . ?
C11 C12 H12A 109.3 . . ?
C13 C12 H12A 109.3 . . ?
C11 C12 H12B 109.3 . . ?
C13 C12 H12B 109.3 . . ?
H12A C12 H12B 108.0 . . ?
N1 C13 C12 110.3(5) . . ?
N1 C13 C8 107.9(5) . . ?
C12 C13 C8 109.8(5) . . ?
N1 C13 H13 109.6 . . ?
C12 C13 H13 109.6 . . ?
C8 C13 H13 109.6 . . ?
N1 C14 C15 121.3(5) . . ?
N1 C14 H14 119.4 . . ?
C15 C14 H14 119.4 . . ?
C20 C15 C16 119.7(5) . . ?
C20 C15 C14 120.9(5) . . ?
C16 C15 C14 119.4(5) . . ?
C17 C16 C15 120.5(6) . . ?
C17 C16 H16 119.7 . . ?
C15 C16 H16 119.7 . . ?
C16 C17 C18 120.8(6) . . ?
C16 C17 H17 119.6 . . ?
C18 C17 H17 119.6 . . ?
C19 C18 C17 118.6(5) . . ?
C19 C18 H18 120.7 . . ?
C17 C18 H18 120.7 . . ?
C18 C19 O4 124.2(5) . . ?
C18 C19 C20 121.9(6) . . ?
O4 C19 C20 113.8(5) . . ?
O3 C20 C15 124.1(5) . . ?
O3 C20 C19 117.6(5) . . ?
C15 C20 C19 118.3(5) . . ?
O2 C21 H21A 109.5 . . ?
O2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O4 C22 H22A 109.5 . . ?
O4 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
O4 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O5 C23 C24 123.7(5) . . ?
O5 C23 C28 117.4(5) . . ?
C24 C23 C28 118.8(5) . . ?
C23 C24 C25 119.1(6) . . ?
C23 C24 C29 123.1(5) . . ?
C25 C24 C29 117.5(6) . . ?
C26 C25 C24 121.2(6) . . ?
C26 C25 H25 119.4 . . ?
C24 C25 H25 119.4 . . ?
C25 C26 C27 120.8(6) . . ?
C25 C26 H26 119.6 . . ?
C27 C26 H26 119.6 . . ?
C28 C27 C26 119.5(6) . . ?
C28 C27 H27 120.3 . . ?
C26 C27 H27 120.3 . . ?
O6 C28 C27 126.1(6) . . ?
O6 C28 C23 113.5(5) . . ?
C27 C28 C23 120.4(6) . . ?
N3 C29 C24 127.0(6) . . ?
N3 C29 H29 116.5 . . ?
C24 C29 H29 116.5 . . ?
N3 C30 C35 110.2(5) . . ?
N3 C30 C31 115.7(5) . . ?
C35 C30 C31 112.0(6) . . ?
N3 C30 H30 106.1 . . ?
C35 C30 H30 106.1 . . ?
C31 C30 H30 106.1 . . ?
C30 C31 C32 112.2(6) . . ?
C30 C31 H31A 109.2 . . ?
C32 C31 H31A 109.2 . . ?
C30 C31 H31B 109.2 . . ?
C32 C31 H31B 109.2 . . ?
H31A C31 H31B 107.9 . . ?
C33 C32 C31 113.6(6) . . ?
C33 C32 H32A 108.9 . . ?
C31 C32 H32A 108.9 . . ?
C33 C32 H32B 108.9 . . ?
C31 C32 H32B 108.9 . . ?
H32A C32 H32B 107.7 . . ?
C32 C33 C34 114.0(6) . . ?
C32 C33 H33A 108.7 . . ?
C34 C33 H33A 108.7 . . ?
C32 C33 H33B 108.7 . . ?
C34 C33 H33B 108.7 . . ?
H33A C33 H33B 107.6 . . ?
C35 C34 C33 110.2(6) . . ?
C35 C34 H34A 109.6 . . ?
C33 C34 H34A 109.6 . . ?
C35 C34 H34B 109.6 . . ?
C33 C34 H34B 109.6 . . ?
H34A C34 H34B 108.1 . . ?
N4 C35 C30 107.8(5) . . ?
N4 C35 C34 118.7(5) . . ?
C30 C35 C34 113.0(6) . . ?
N4 C35 H35 105.4 . . ?
C30 C35 H35 105.4 . . ?
C34 C35 H35 105.4 . . ?
N4 C36 C37 127.1(6) . . ?
N4 C36 H36 116.5 . . ?
C37 C36 H36 116.5 . . ?
C42 C37 C38 118.4(6) . . ?
C42 C37 C36 124.0(5) . . ?
C38 C37 C36 117.1(6) . . ?
C39 C38 C37 122.1(6) . . ?
C39 C38 H38 119.0 . . ?
C37 C38 H38 119.0 . . ?
C38 C39 C40 120.4(6) . . ?
C38 C39 H39 119.8 . . ?
C40 C39 H39 119.8 . . ?
C41 C40 C39 119.7(6) . . ?
C41 C40 H40 120.1 . . ?
C39 C40 H40 120.1 . . ?
C40 C41 O8 124.8(6) . . ?
C40 C41 C42 121.1(6) . . ?
O8 C41 C42 114.1(5) . . ?
O7 C42 C37 123.7(5) . . ?
O7 C42 C41 118.1(5) . . ?
C37 C42 C41 118.1(5) . . ?
O6 C43 H43A 109.5 . . ?
O6 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
O6 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
O8 C44 H44A 109.5 . . ?
O8 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
O8 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O1 Dy1 O7 128.53(14) . . ?
O1 Dy1 O12 157.46(14) . . ?
O7 Dy1 O12 72.70(12) . . ?
O1 Dy1 O5 123.41(14) . . ?
O7 Dy1 O5 68.51(12) . . ?
O12 Dy1 O5 67.80(13) . . ?
O1 Dy1 O9 77.88(15) . . ?
O7 Dy1 O9 150.79(14) . . ?
O12 Dy1 O9 79.79(14) . . ?
O5 Dy1 O9 109.97(14) . . ?
O1 Dy1 O3 102.48(14) . . ?
O7 Dy1 O3 86.46(13) . . ?
O12 Dy1 O3 68.12(12) . . ?
O5 Dy1 O3 133.99(12) . . ?
O9 Dy1 O3 74.14(13) . . ?
O1 Dy1 O2 65.12(14) . . ?
O7 Dy1 O2 75.67(13) . . ?
O12 Dy1 O2 135.31(13) . . ?
O5 Dy1 O2 71.67(14) . . ?
O9 Dy1 O2 132.77(14) . . ?
O3 Dy1 O2 139.94(13) . . ?
O1 Dy1 O8 73.23(13) . . ?
O7 Dy1 O8 62.74(12) . . ?
O12 Dy1 O8 118.93(12) . . ?
O5 Dy1 O8 123.61(13) . . ?
O9 Dy1 O8 126.42(13) . . ?
O3 Dy1 O8 69.53(13) . . ?
O2 Dy1 O8 70.42(14) . . ?
O1 Dy1 O6 73.11(14) . . ?
O7 Dy1 O6 126.39(13) . . ?
O12 Dy1 O6 101.31(13) . . ?
O5 Dy1 O6 60.63(12) . . ?
O9 Dy1 O6 68.18(14) . . ?
O3 Dy1 O6 142.17(13) . . ?
O2 Dy1 O6 73.54(14) . . ?
O8 Dy1 O6 138.32(14) . . ?
O1 Dy1 Dy2 159.55(11) . . ?
O7 Dy1 Dy2 41.64(9) . . ?
O12 Dy1 Dy2 41.35(9) . . ?
O5 Dy1 Dy2 40.92(9) . . ?
O9 Dy1 Dy2 117.49(11) . . ?
O3 Dy1 Dy2 95.10(9) . . ?
O2 Dy1 Dy2 94.66(9) . . ?
O8 Dy1 Dy2 103.90(8) . . ?
O6 Dy1 Dy2 99.16(9) . . ?
O1 Dy1 Dy2 137.70(11) . 2_566 ?
O7 Dy1 Dy2 69.11(10) . 2_566 ?
O12 Dy1 Dy2 34.36(8) . 2_566 ?
O5 Dy1 Dy2 98.45(9) . 2_566 ?
O9 Dy1 Dy2 82.68(11) . 2_566 ?
O3 Dy1 Dy2 35.57(9) . 2_566 ?
O2 Dy1 Dy2 144.54(9) . 2_566 ?
O8 Dy1 Dy2 89.47(9) . 2_566 ?
O6 Dy1 Dy2 132.19(10) . 2_566 ?
Dy2 Dy1 Dy2 61.275(9) . 2_566 ?
O5 Dy2 O12 133.93(13) . 2_566 ?
O5 Dy2 O12 69.47(13) . . ?
O12 Dy2 O12 72.05(13) 2_566 . ?
O5 Dy2 O7 69.31(13) . . ?
O12 Dy2 O7 76.12(12) 2_566 . ?
O12 Dy2 O7 73.19(13) . . ?
O5 Dy2 O3 147.58(12) . 2_566 ?
O12 Dy2 O3 70.32(12) 2_566 2_566 ?
O12 Dy2 O3 109.84(13) . 2_566 ?
O7 Dy2 O3 142.86(12) . 2_566 ?
O5 Dy2 N4 113.45(16) . . ?
O12 Dy2 N4 84.07(15) 2_566 . ?
O12 Dy2 N4 143.21(14) . . ?
O7 Dy2 N4 74.17(15) . . ?
O3 Dy2 N4 86.80(15) 2_566 . ?
O5 Dy2 O4 83.00(13) . 2_566 ?
O12 Dy2 O4 117.52(13) 2_566 2_566 ?
O12 Dy2 O4 84.50(12) . 2_566 ?
O7 Dy2 O4 149.02(12) . 2_566 ?
O3 Dy2 O4 64.92(12) 2_566 2_566 ?
N4 Dy2 O4 131.99(14) . 2_566 ?
O5 Dy2 N3 72.92(14) . . ?
O12 Dy2 N3 147.02(14) 2_566 . ?
O12 Dy2 N3 140.45(14) . . ?
O7 Dy2 N3 104.51(15) . . ?
O3 Dy2 N3 95.42(15) 2_566 . ?
N4 Dy2 N3 65.08(15) . . ?
O4 Dy2 N3 79.20(15) 2_566 . ?
O5 Dy2 Dy1 42.24(9) . . ?
O12 Dy2 Dy1 91.79(9) 2_566 . ?
O12 Dy2 Dy1 42.21(9) . . ?
O7 Dy2 Dy1 41.35(9) . . ?
O3 Dy2 Dy1 151.69(10) 2_566 . ?
N4 Dy2 Dy1 113.78(12) . . ?
O4 Dy2 Dy1 108.08(9) 2_566 . ?
N3 Dy2 Dy1 110.58(11) . . ?
O5 Dy2 Dy2 102.17(10) . 2_566 ?
O12 Dy2 Dy2 36.11(9) 2_566 2_566 ?
O12 Dy2 Dy2 35.94(8) . 2_566 ?
O7 Dy2 Dy2 70.90(10) . 2_566 ?
O3 Dy2 Dy2 90.14(9) 2_566 2_566 ?
N4 Dy2 Dy2 115.62(11) . 2_566 ?
O4 Dy2 Dy2 103.05(10) 2_566 2_566 ?
N3 Dy2 Dy2 174.44(12) . 2_566 ?
Dy1 Dy2 Dy2 63.927(9) . 2_566 ?
O5 Dy2 Dy1 151.56(10) . 2_566 ?
O12 Dy2 Dy1 35.20(9) 2_566 2_566 ?
O12 Dy2 Dy1 83.30(9) . 2_566 ?
O7 Dy2 Dy1 111.31(9) . 2_566 ?
O3 Dy2 Dy1 37.02(9) 2_566 2_566 ?
N4 Dy2 Dy1 93.17(12) . 2_566 ?
O4 Dy2 Dy1 86.45(9) 2_566 2_566 ?
N3 Dy2 Dy1 130.69(11) . 2_566 ?
Dy1 Dy2 Dy1 118.725(9) . 2_566 ?
Dy2 Dy2 Dy1 54.798(9) 2_566 2_566 ?
C14 N1 C13 116.7(5) . . ?
C7 N2 C8 126.4(6) . . ?
C7 N2 H21 109.6 . . ?
C8 N2 H21 123.6 . . ?
C29 N3 C30 115.2(5) . . ?
C29 N3 Dy2 129.2(4) . . ?
C30 N3 Dy2 115.0(3) . . ?
C36 N4 C35 122.0(5) . . ?
C36 N4 Dy2 131.0(4) . . ?
C35 N4 Dy2 106.9(4) . . ?
O11 N5 O10 122.2(6) . . ?
O11 N5 O9 118.8(6) . . ?
O10 N5 O9 118.9(5) . . ?
O14 N6 O15 116.1(15) . . ?
O14 N6 O13 123.2(16) . . ?
O15 N6 O13 120.1(13) . . ?
C1 O1 Dy1 126.2(4) . . ?
C2 O2 C21 117.2(5) . . ?
C2 O2 Dy1 115.9(3) . . ?
C21 O2 Dy1 126.4(4) . . ?
C20 O3 Dy2 114.0(3) . 2_566 ?
C20 O3 Dy1 132.8(3) . . ?
Dy2 O3 Dy1 107.42(14) 2_566 . ?
C19 O4 C22 117.0(4) . . ?
C19 O4 Dy2 110.6(3) . 2_566 ?
C22 O4 Dy2 130.4(4) . 2_566 ?
C23 O5 Dy2 134.8(4) . . ?
C23 O5 Dy1 128.2(3) . . ?
Dy2 O5 Dy1 96.84(13) . . ?
C28 O6 C43 117.4(5) . . ?
C28 O6 Dy1 116.8(3) . . ?
C43 O6 Dy1 125.2(4) . . ?
C42 O7 Dy1 128.3(3) . . ?
C42 O7 Dy2 134.3(3) . . ?
Dy1 O7 Dy2 97.01(13) . . ?
C41 O8 C44 115.7(5) . . ?
C41 O8 Dy1 116.6(3) . . ?
C44 O8 Dy1 127.4(3) . . ?
N5 O9 Dy1 132.2(4) . . ?
Dy2 O12 Dy2 107.95(13) 2_566 . ?
Dy2 O12 Dy1 110.44(13) 2_566 . ?
Dy2 O12 Dy1 96.44(14) . . ?
Dy2 O12 H121 109.9 2_566 . ?
Dy2 O12 H121 127.3 . . ?
Dy1 O12 H121 103.1 . . ?
O16C O16A O17B 46.4(17) . . ?
O16C O17B O17C 160(4) . . ?
O16C O17B O16A 53(2) . . ?
O17C O17B O16A 113(3) . . ?
O17B O16C O16A 81(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H21 O1 0.91 1.81 2.610(6) 145.6 .
O12 H121 O10 0.85 2.04 2.834(6) 155.4 .
O12 H121 N5 0.85 2.68 3.323(6) 134.4 .

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.169
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.118
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_72-1
_database_code_depnum_ccdc_archive 'CCDC 1000759'
_audit_update_record             
;
2014-10-08 deposited with the CCDC.
2015-01-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ' C88 H100 N10 O24 Tb4, 0.66(O6), 2(N O3)  '
_chemical_formula_sum            ' C88 H100 N12 O33.96 Tb4  '
_chemical_formula_weight         2504.89

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'
Tb Tb -0.1723 4.1537 '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 '
_symmetry_space_group_name_Hall  ' -P 1 '

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

_cell_length_a                   14.4379(7)
_cell_length_b                   14.5620(5)
_cell_length_c                   14.7018(7)
_cell_angle_alpha                110.979(4)
_cell_angle_beta                 104.156(4)
_cell_angle_gamma                107.975(4)
_cell_volume                     2516.3(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1243.7
_exptl_absorpt_coefficient_mu    2.862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.494
_exptl_absorpt_correction_T_max  0.581
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'

_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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19577
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0474
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.94
_diffrn_reflns_theta_max         25.00
_reflns_number_total             8861
_reflns_number_gt                7060
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_cell_refinement       'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXL-97

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
The water molecules in complex are highly disordered, and H-atoms can not be added. But the H-atoms located on the water molecules are took into consideration in the formular of complex.
;

_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)+(0.0377P)²+3.7434P] 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         8861
_refine_ls_number_parameters     632
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0328
_refine_ls_wR_factor_ref         0.0918
_refine_ls_wR_factor_gt          0.0820
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_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
C1 C 0.1050(4) 0.1076(4) 0.2697(4) 0.0334(13) Uani 1 1 d . . .
C2 C 0.0122(5) 0.0822(4) 0.1879(4) 0.0366(13) Uani 1 1 d . . .
C3 C -0.0367(5) -0.0152(4) 0.0944(4) 0.0397(14) Uani 1 1 d . . .
H3 H -0.0990 -0.0311 0.0417 0.048 Uiso 1 1 calc R . .
C4 C 0.0072(6) -0.0895(5) 0.0791(5) 0.0471(16) Uani 1 1 d . . .
H4 H -0.0253 -0.1546 0.0158 0.057 Uiso 1 1 calc R . .
C5 C 0.0979(5) -0.0667(5) 0.1570(5) 0.0420(15) Uani 1 1 d . . .
H5 H 0.1273 -0.1163 0.1459 0.050 Uiso 1 1 calc R . .
C6 C 0.1478(5) 0.0308(4) 0.2539(5) 0.0369(13) Uani 1 1 d . . .
C7 C 0.2392(5) 0.0495(5) 0.3356(5) 0.0408(14) Uani 1 1 d . . .
H7 H 0.2629 -0.0046 0.3236 0.049 Uiso 1 1 calc R . .
C8 C 0.3852(5) 0.1630(5) 0.5135(5) 0.0427(15) Uani 1 1 d . . .
H8 H 0.3706 0.1014 0.5294 0.051 Uiso 1 1 calc R . .
C9 C 0.4817(5) 0.1808(6) 0.4848(6) 0.0561(18) Uani 1 1 d . . .
H9A H 0.4680 0.1145 0.4245 0.067 Uiso 1 1 calc R . .
H9B H 0.4946 0.2389 0.4650 0.067 Uiso 1 1 calc R . .
C10 C 0.5776(5) 0.2107(7) 0.5776(6) 0.069(2) Uani 1 1 d . . .
H10A H 0.6387 0.2237 0.5591 0.083 Uiso 1 1 calc R . .
H10B H 0.5663 0.1502 0.5938 0.083 Uiso 1 1 calc R . .
C11 C 0.5998(6) 0.3116(6) 0.6745(6) 0.067(2) Uani 1 1 d . . .
H11A H 0.6173 0.3736 0.6604 0.080 Uiso 1 1 calc R . .
H11B H 0.6606 0.3270 0.7336 0.080 Uiso 1 1 calc R . .
C12 C 0.5052(5) 0.2967(6) 0.7043(5) 0.0533(17) Uani 1 1 d . . .
H12A H 0.5203 0.3644 0.7639 0.064 Uiso 1 1 calc R . .
H12B H 0.4929 0.2403 0.7263 0.064 Uiso 1 1 calc R . .
C13 C 0.4059(5) 0.2650(5) 0.6116(5) 0.0399(14) Uani 1 1 d . . .
H13 H 0.4154 0.3257 0.5947 0.048 Uiso 1 1 calc R . .
C14 C 0.2605(4) 0.2962(5) 0.6337(4) 0.0357(13) Uani 1 1 d . . .
H14 H 0.2816 0.3486 0.6115 0.043 Uiso 1 1 calc R . .
C15 C 0.1689(5) 0.2805(4) 0.6622(4) 0.0336(13) Uani 1 1 d . . .
C16 C 0.1515(5) 0.2222(5) 0.7204(5) 0.0429(15) Uani 1 1 d . . .
H16 H 0.1987 0.1944 0.7395 0.052 Uiso 1 1 calc R . .
C17 C 0.0665(5) 0.2060(5) 0.7490(5) 0.0478(16) Uani 1 1 d . . .
H17 H 0.0546 0.1650 0.7846 0.057 Uiso 1 1 calc R . .
C18 C -0.0018(5) 0.2514(5) 0.7244(5) 0.0430(15) Uani 1 1 d . . .
H18 H -0.0590 0.2416 0.7444 0.052 Uiso 1 1 calc R . .
C19 C 0.0154(4) 0.3103(4) 0.6709(4) 0.0334(13) Uani 1 1 d . . .
C20 C 0.0991(4) 0.3237(4) 0.6357(4) 0.0299(12) Uani 1 1 d . . .
C21 C -0.1224(5) 0.1386(5) 0.1343(5) 0.0464(16) Uani 1 1 d . . .
H21A H -0.1169 0.1256 0.0675 0.070 Uiso 1 1 calc R . .
H21B H -0.1391 0.1995 0.1590 0.070 Uiso 1 1 calc R . .
H21C H -0.1775 0.0747 0.1255 0.070 Uiso 1 1 calc R . .
C22 C -0.1447(5) 0.3349(5) 0.6572(6) 0.0545(18) Uani 1 1 d . . .
H22A H -0.1867 0.2572 0.6157 0.082 Uiso 1 1 calc R . .
H22B H -0.1815 0.3714 0.6320 0.082 Uiso 1 1 calc R . .
H22C H -0.1329 0.3564 0.7304 0.082 Uiso 1 1 calc R . .
C23 C 0.0521(4) 0.3884(4) 0.1934(4) 0.0314(12) Uani 1 1 d . . .
C24 C -0.0101(5) 0.3933(4) 0.1074(4) 0.0375(14) Uani 1 1 d . . .
C25 C 0.0247(6) 0.3901(5) 0.0252(5) 0.0477(16) Uani 1 1 d . . .
H25 H -0.0165 0.3920 -0.0330 0.057 Uiso 1 1 calc R . .
C26 C 0.1173(6) 0.3842(5) 0.0298(5) 0.0535(18) Uani 1 1 d . . .
H26 H 0.1401 0.3847 -0.0240 0.064 Uiso 1 1 calc R . .
C27 C 0.1784(5) 0.3774(5) 0.1130(5) 0.0478(16) Uani 1 1 d . . .
H27 H 0.2422 0.3739 0.1155 0.057 Uiso 1 1 calc R . .
C28 C 0.1445(5) 0.3758(4) 0.1929(4) 0.0368(13) Uani 1 1 d . . .
C29 C -0.1144(5) 0.3906(5) 0.0930(4) 0.0414(14) Uani 1 1 d . . .
H29 H -0.1585 0.3703 0.0245 0.050 Uiso 1 1 calc R . .
C30 C -0.2673(5) 0.3873(5) 0.1234(5) 0.0440(15) Uani 1 1 d . . .
H30 H -0.3051 0.3097 0.0709 0.053 Uiso 1 1 calc R . .
C31 C -0.2962(5) 0.4489(6) 0.0668(5) 0.0537(17) Uani 1 1 d . . .
H31A H -0.2770 0.4323 0.0061 0.064 Uiso 1 1 calc R . .
H31B H -0.2563 0.5268 0.1144 0.064 Uiso 1 1 calc R . .
C32 C -0.4148(6) 0.4186(7) 0.0293(6) 0.067(2) Uani 1 1 d . . .
H32A H -0.4285 0.4680 0.0039 0.080 Uiso 1 1 calc R . .
H32B H -0.4535 0.3451 -0.0299 0.080 Uiso 1 1 calc R . .
C33 C -0.4555(6) 0.4235(6) 0.1144(6) 0.067(2) Uani 1 1 d . . .
H33A H -0.5324 0.3930 0.0828 0.081 Uiso 1 1 calc R . .
H33B H -0.4289 0.4996 0.1658 0.081 Uiso 1 1 calc R . .
C34 C -0.4242(5) 0.3625(5) 0.1724(5) 0.0496(16) Uani 1 1 d . . .
H34A H -0.4456 0.3763 0.2317 0.060 Uiso 1 1 calc R . .
H34B H -0.4605 0.2845 0.1245 0.060 Uiso 1 1 calc R . .
C35 C -0.3059(5) 0.3994(5) 0.2126(5) 0.0420(14) Uani 1 1 d . . .
H35 H -0.2738 0.4782 0.2607 0.050 Uiso 1 1 calc R . .
C36 C -0.3144(5) 0.2700(5) 0.2785(4) 0.0384(13) Uani 1 1 d . . .
H36 H -0.3876 0.2457 0.2491 0.046 Uiso 1 1 calc R . .
C37 C -0.2756(5) 0.2088(5) 0.3265(5) 0.0377(13) Uani 1 1 d . . .
C38 C -0.3513(5) 0.1253(5) 0.3295(6) 0.0553(18) Uani 1 1 d . . .
H38 H -0.4209 0.1168 0.3096 0.066 Uiso 1 1 calc R . .
C39 C -0.3268(6) 0.0554(6) 0.3606(7) 0.070(2) Uani 1 1 d . . .
H39 H -0.3792 0.0007 0.3628 0.083 Uiso 1 1 calc R . .
C40 C -0.2238(5) 0.0656(5) 0.3892(6) 0.0556(18) Uani 1 1 d . . .
H40 H -0.2069 0.0172 0.4093 0.067 Uiso 1 1 calc R . .
C41 C -0.1471(5) 0.1479(4) 0.3876(5) 0.0374(13) Uani 1 1 d . . .
C42 C -0.1700(4) 0.2245(4) 0.3595(4) 0.0317(12) Uani 1 1 d . . .
C43 C 0.2922(6) 0.3521(7) 0.2845(6) 0.064(2) Uani 1 1 d . . .
H43A H 0.2785 0.2879 0.2231 0.096 Uiso 1 1 calc R . .
H43B H 0.3205 0.3463 0.3474 0.096 Uiso 1 1 calc R . .
H43C H 0.3427 0.4156 0.2878 0.096 Uiso 1 1 calc R . .
C44 C -0.0185(5) 0.0817(5) 0.4305(5) 0.0515(17) Uani 1 1 d . . .
H44A H -0.0326 0.0802 0.4906 0.077 Uiso 1 1 calc R . .
H44B H 0.0551 0.0993 0.4452 0.077 Uiso 1 1 calc R . .
H44C H -0.0618 0.0112 0.3693 0.077 Uiso 1 1 calc R . .
Tb1 Tb 0.08599(2) 0.32940(2) 0.397201(19) 0.02914(9) Uani 1 1 d . . .
Tb2 Tb -0.06760(2) 0.469533(19) 0.358375(19) 0.02528(8) Uani 1 1 d . . .
N1 N 0.3124(4) 0.2398(4) 0.6383(4) 0.0430(12) Uani 1 1 d . . .
N2 N 0.2909(4) 0.1382(4) 0.4259(4) 0.0384(12) Uani 1 1 d D . .
H21 H 0.2531 0.1778 0.4310 0.058 Uiso 1 1 d RD . .
N3 N -0.1529(4) 0.4132(4) 0.1643(3) 0.0358(11) Uani 1 1 d . . .
N4 N -0.2578(4) 0.3525(4) 0.2734(4) 0.0338(10) Uani 1 1 d . . .
N5 N 0.3379(4) 0.5335(4) 0.5231(4) 0.0479(13) Uani 1 1 d . . .
N6 N 0.6794(9) 0.1558(9) 0.8121(9) 0.122(4) Uani 1 1 d . . .
O1 O 0.1485(3) 0.1999(3) 0.3592(3) 0.0389(9) Uani 1 1 d . . .
O2 O -0.0226(3) 0.1626(3) 0.2109(3) 0.0427(10) Uani 1 1 d . . .
O3 O 0.1086(3) 0.3804(3) 0.5805(3) 0.0297(8) Uani 1 1 d . . .
O4 O -0.0442(3) 0.3644(3) 0.6475(3) 0.0353(9) Uani 1 1 d . . .
O5 O 0.0268(3) 0.3919(3) 0.2756(3) 0.0341(9) Uani 1 1 d . . .
O6 O 0.1940(3) 0.3619(3) 0.2771(3) 0.0459(10) Uani 1 1 d . . .
O7 O -0.0908(3) 0.3033(3) 0.3624(3) 0.0295(8) Uani 1 1 d . . .
O8 O -0.0428(3) 0.1635(3) 0.4102(3) 0.0380(9) Uani 1 1 d . . .
O9 O 0.2739(3) 0.4384(3) 0.5024(3) 0.0441(10) Uani 1 1 d . . .
O10 O 0.3005(4) 0.5894(4) 0.4949(4) 0.0624(13) Uani 1 1 d . . .
O11 O 0.4323(4) 0.5655(5) 0.5713(5) 0.0900(18) Uani 1 1 d . . .
O12 O 0.0913(3) 0.5049(3) 0.4848(3) 0.0273(8) Uani 1 1 d D . .
H121 H 0.1551 0.5464 0.5012 0.033 Uiso 1 1 d RD . .
O13 O 0.7563(8) 0.2042(8) 0.8007(9) 0.150(4) Uani 1 1 d . . .
O14 O 0.6569(11) 0.1970(12) 0.8755(9) 0.315(10) Uani 1 1 d . . .
O15 O 0.6193(7) 0.0680(7) 0.7458(8) 0.188(5) Uani 1 1 d . . .
O16A O 0.3933(16) 0.0547(16) 0.0840(16) 0.104(6) Uiso 0.33 1 d P . .
O17A O 0.314(2) 0.152(2) -0.107(2) 0.148(9) Uiso 0.33 1 d P . .
O17B O 0.301(2) 0.165(2) 0.038(2) 0.154(9) Uiso 0.33 1 d P . .
O16B O 0.351(2) 0.104(2) 0.145(2) 0.141(8) Uiso 0.33 1 d P . .
O16C O 0.355(3) 0.101(3) 0.019(3) 0.195(13) Uiso 0.33 1 d P . .
O17C O 0.375(2) 0.097(2) -0.081(2) 0.151(9) Uiso 0.33 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
C1 O1 1.319(6) . ?
C1 C2 1.403(8) . ?
C1 C6 1.412(7) . ?
C2 O2 1.379(6) . ?
C2 C3 1.382(8) . ?
C3 C4 1.394(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.365(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.409(8) . ?
C5 H5 0.9300 . ?
C6 C7 1.424(8) . ?
C7 N2 1.296(7) . ?
C7 H7 0.9300 . ?
C8 N2 1.466(7) . ?
C8 C9 1.526(8) . ?
C8 C13 1.535(8) . ?
C8 H8 0.9800 . ?
C9 C10 1.498(9) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.509(10) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.511(9) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.521(8) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N1 1.473(7) . ?
C13 H13 0.9800 . ?
C14 N1 1.279(7) . ?
C14 C15 1.459(7) . ?
C14 H14 0.9300 . ?
C15 C20 1.392(7) . ?
C15 C16 1.417(7) . ?
C16 C17 1.373(8) . ?
C16 H16 0.9300 . ?
C17 C18 1.391(8) . ?
C17 H17 0.9300 . ?
C18 C19 1.366(7) . ?
C18 H18 0.9300 . ?
C19 O4 1.396(6) . ?
C19 C20 1.414(7) . ?
C20 O3 1.350(6) . ?
C21 O2 1.442(7) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 O4 1.438(6) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 O5 1.333(6) . ?
C23 C24 1.400(8) . ?
C23 C28 1.403(8) . ?
C24 C25 1.410(8) . ?
C24 C29 1.454(8) . ?
C25 C26 1.353(9) . ?
C25 H25 0.9300 . ?
C26 C27 1.377(9) . ?
C26 H26 0.9300 . ?
C27 C28 1.384(8) . ?
C27 H27 0.9300 . ?
C28 O6 1.386(7) . ?
C29 N3 1.290(7) . ?
C29 H29 0.9300 . ?
C30 N3 1.484(7) . ?
C30 C31 1.504(8) . ?
C30 C35 1.521(8) . ?
C30 H30 0.9800 . ?
C31 C32 1.525(9) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C33 1.496(9) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 C34 1.524(8) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 C35 1.506(8) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 N4 1.474(7) . ?
C35 H35 0.9800 . ?
C36 N4 1.268(7) . ?
C36 C37 1.474(8) . ?
C36 H36 0.9300 . ?
C37 C38 1.384(8) . ?
C37 C42 1.399(8) . ?
C38 C39 1.360(9) . ?
C38 H38 0.9300 . ?
C39 C40 1.387(9) . ?
C39 H39 0.9300 . ?
C40 C41 1.370(8) . ?
C40 H40 0.9300 . ?
C41 O8 1.386(7) . ?
C41 C42 1.419(7) . ?
C42 O7 1.326(6) . ?
C43 O6 1.451(7) . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 O8 1.447(6) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
Tb1 O1 2.287(3) . ?
Tb1 O7 2.354(3) . ?
Tb1 O5 2.378(3) . ?
Tb1 O12 2.381(3) . ?
Tb1 O9 2.408(4) . ?
Tb1 O3 2.431(3) . ?
Tb1 O2 2.578(4) . ?
Tb1 O8 2.658(4) . ?
Tb1 O6 2.695(4) . ?
Tb1 Tb2 3.5236(3) . ?
Tb1 Tb2 3.8690(4) 2_566 ?
Tb2 O5 2.323(3) . ?
Tb2 O12 2.329(3) 2_566 ?
Tb2 O12 2.341(3) . ?
Tb2 O3 2.363(3) 2_566 ?
Tb2 O7 2.363(3) . ?
Tb2 N4 2.432(5) . ?
Tb2 O4 2.504(4) 2_566 ?
Tb2 N3 2.512(4) . ?
Tb2 Tb2 3.7747(5) 2_566 ?
Tb2 Tb1 3.8690(4) 2_566 ?
N2 H21 0.9048 . ?
N5 O11 1.214(7) . ?
N5 O10 1.236(7) . ?
N5 O9 1.279(6) . ?
N6 O14 1.096(12) . ?
N6 O15 1.161(11) . ?
N6 O13 1.204(12) . ?
O3 Tb2 2.363(3) 2_566 ?
O4 Tb2 2.504(4) 2_566 ?
O12 Tb2 2.329(3) 2_566 ?
O12 H121 0.8463 . ?
O16A O16B 1.34(3) . ?
O16A O16C 1.45(4) . ?
O17A O17C 1.44(3) . ?
O17B O16C 1.39(4) . ?
O16C O17C 1.55(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 120.0(5) . . ?
O1 C1 C6 121.9(5) . . ?
C2 C1 C6 118.1(5) . . ?
O2 C2 C3 125.2(5) . . ?
O2 C2 C1 113.6(5) . . ?
C3 C2 C1 121.3(5) . . ?
C2 C3 C4 120.0(6) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 120.0(5) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 120.9(5) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C5 C6 C1 119.6(6) . . ?
C5 C6 C7 119.5(5) . . ?
C1 C6 C7 120.9(5) . . ?
N2 C7 C6 123.2(5) . . ?
N2 C7 H7 118.4 . . ?
C6 C7 H7 118.4 . . ?
N2 C8 C9 111.5(5) . . ?
N2 C8 C13 108.0(4) . . ?
C9 C8 C13 111.0(5) . . ?
N2 C8 H8 108.8 . . ?
C9 C8 H8 108.8 . . ?
C13 C8 H8 108.8 . . ?
C10 C9 C8 110.1(6) . . ?
C10 C9 H9A 109.6 . . ?
C8 C9 H9A 109.6 . . ?
C10 C9 H9B 109.6 . . ?
C8 C9 H9B 109.6 . . ?
H9A C9 H9B 108.2 . . ?
C9 C10 C11 111.5(6) . . ?
C9 C10 H10A 109.3 . . ?
C11 C10 H10A 109.3 . . ?
C9 C10 H10B 109.3 . . ?
C11 C10 H10B 109.3 . . ?
H10A C10 H10B 108.0 . . ?
C10 C11 C12 111.3(6) . . ?
C10 C11 H11A 109.4 . . ?
C12 C11 H11A 109.4 . . ?
C10 C11 H11B 109.4 . . ?
C12 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
C11 C12 C13 111.4(6) . . ?
C11 C12 H12A 109.3 . . ?
C13 C12 H12A 109.3 . . ?
C11 C12 H12B 109.3 . . ?
C13 C12 H12B 109.3 . . ?
H12A C12 H12B 108.0 . . ?
N1 C13 C12 110.6(5) . . ?
N1 C13 C8 108.0(5) . . ?
C12 C13 C8 110.3(5) . . ?
N1 C13 H13 109.3 . . ?
C12 C13 H13 109.3 . . ?
C8 C13 H13 109.3 . . ?
N1 C14 C15 121.8(5) . . ?
N1 C14 H14 119.1 . . ?
C15 C14 H14 119.1 . . ?
C20 C15 C16 119.0(5) . . ?
C20 C15 C14 121.5(5) . . ?
C16 C15 C14 119.5(5) . . ?
C17 C16 C15 121.3(5) . . ?
C17 C16 H16 119.4 . . ?
C15 C16 H16 119.4 . . ?
C16 C17 C18 119.6(5) . . ?
C16 C17 H17 120.2 . . ?
C18 C17 H17 120.2 . . ?
C19 C18 C17 119.8(5) . . ?
C19 C18 H18 120.1 . . ?
C17 C18 H18 120.1 . . ?
C18 C19 O4 124.6(5) . . ?
C18 C19 C20 121.8(5) . . ?
O4 C19 C20 113.6(4) . . ?
O3 C20 C15 123.6(5) . . ?
O3 C20 C19 118.0(5) . . ?
C15 C20 C19 118.4(5) . . ?
O2 C21 H21A 109.5 . . ?
O2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O4 C22 H22A 109.5 . . ?
O4 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
O4 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O5 C23 C24 123.5(5) . . ?
O5 C23 C28 117.4(5) . . ?
C24 C23 C28 119.1(5) . . ?
C23 C24 C25 118.7(6) . . ?
C23 C24 C29 123.2(5) . . ?
C25 C24 C29 117.8(5) . . ?
C26 C25 C24 120.8(6) . . ?
C26 C25 H25 119.6 . . ?
C24 C25 H25 119.6 . . ?
C25 C26 C27 121.1(6) . . ?
C25 C26 H26 119.5 . . ?
C27 C26 H26 119.5 . . ?
C26 C27 C28 119.6(6) . . ?
C26 C27 H27 120.2 . . ?
C28 C27 H27 120.2 . . ?
C27 C28 O6 125.8(5) . . ?
C27 C28 C23 120.5(6) . . ?
O6 C28 C23 113.8(5) . . ?
N3 C29 C24 127.6(5) . . ?
N3 C29 H29 116.2 . . ?
C24 C29 H29 116.2 . . ?
N3 C30 C31 115.0(5) . . ?
N3 C30 C35 109.5(5) . . ?
C31 C30 C35 112.4(5) . . ?
N3 C30 H30 106.5 . . ?
C31 C30 H30 106.5 . . ?
C35 C30 H30 106.5 . . ?
C30 C31 C32 111.3(6) . . ?
C30 C31 H31A 109.4 . . ?
C32 C31 H31A 109.4 . . ?
C30 C31 H31B 109.4 . . ?
C32 C31 H31B 109.4 . . ?
H31A C31 H31B 108.0 . . ?
C33 C32 C31 113.2(6) . . ?
C33 C32 H32A 108.9 . . ?
C31 C32 H32A 108.9 . . ?
C33 C32 H32B 108.9 . . ?
C31 C32 H32B 108.9 . . ?
H32A C32 H32B 107.7 . . ?
C32 C33 C34 114.0(6) . . ?
C32 C33 H33A 108.8 . . ?
C34 C33 H33A 108.8 . . ?
C32 C33 H33B 108.8 . . ?
C34 C33 H33B 108.8 . . ?
H33A C33 H33B 107.7 . . ?
C35 C34 C33 110.3(6) . . ?
C35 C34 H34A 109.6 . . ?
C33 C34 H34A 109.6 . . ?
C35 C34 H34B 109.6 . . ?
C33 C34 H34B 109.6 . . ?
H34A C34 H34B 108.1 . . ?
N4 C35 C34 119.4(5) . . ?
N4 C35 C30 107.5(5) . . ?
C34 C35 C30 111.5(5) . . ?
N4 C35 H35 105.8 . . ?
C34 C35 H35 105.8 . . ?
C30 C35 H35 105.8 . . ?
N4 C36 C37 126.3(5) . . ?
N4 C36 H36 116.8 . . ?
C37 C36 H36 116.8 . . ?
C38 C37 C42 119.5(5) . . ?
C38 C37 C36 116.6(6) . . ?
C42 C37 C36 123.6(5) . . ?
C39 C38 C37 121.9(6) . . ?
C39 C38 H38 119.1 . . ?
C37 C38 H38 119.1 . . ?
C38 C39 C40 120.0(6) . . ?
C38 C39 H39 120.0 . . ?
C40 C39 H39 120.0 . . ?
C41 C40 C39 119.3(6) . . ?
C41 C40 H40 120.3 . . ?
C39 C40 H40 120.3 . . ?
C40 C41 O8 124.5(5) . . ?
C40 C41 C42 121.6(6) . . ?
O8 C41 C42 113.9(5) . . ?
O7 C42 C37 124.5(5) . . ?
O7 C42 C41 117.9(5) . . ?
C37 C42 C41 117.5(5) . . ?
O6 C43 H43A 109.5 . . ?
O6 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
O6 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
O8 C44 H44A 109.5 . . ?
O8 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
O8 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O1 Tb1 O7 128.34(13) . . ?
O1 Tb1 O5 123.32(12) . . ?
O7 Tb1 O5 68.33(12) . . ?
O1 Tb1 O12 157.53(13) . . ?
O7 Tb1 O12 72.85(11) . . ?
O5 Tb1 O12 67.91(11) . . ?
O1 Tb1 O9 78.26(14) . . ?
O7 Tb1 O9 150.67(12) . . ?
O5 Tb1 O9 110.02(13) . . ?
O12 Tb1 O9 79.48(12) . . ?
O1 Tb1 O3 102.58(12) . . ?
O7 Tb1 O3 86.46(12) . . ?
O5 Tb1 O3 134.01(11) . . ?
O12 Tb1 O3 68.13(11) . . ?
O9 Tb1 O3 74.18(13) . . ?
O1 Tb1 O2 64.76(13) . . ?
O7 Tb1 O2 75.61(12) . . ?
O5 Tb1 O2 71.87(12) . . ?
O12 Tb1 O2 135.64(11) . . ?
O9 Tb1 O2 132.97(13) . . ?
O3 Tb1 O2 139.55(12) . . ?
O1 Tb1 O8 73.64(13) . . ?
O7 Tb1 O8 62.25(11) . . ?
O5 Tb1 O8 123.08(13) . . ?
O12 Tb1 O8 118.57(11) . . ?
O9 Tb1 O8 126.90(13) . . ?
O3 Tb1 O8 69.38(12) . . ?
O2 Tb1 O8 70.17(13) . . ?
O1 Tb1 O6 73.20(13) . . ?
O7 Tb1 O6 126.33(12) . . ?
O5 Tb1 O6 60.70(12) . . ?
O12 Tb1 O6 101.18(12) . . ?
O9 Tb1 O6 68.18(13) . . ?
O3 Tb1 O6 142.22(13) . . ?
O2 Tb1 O6 73.85(13) . . ?
O8 Tb1 O6 138.73(12) . . ?
O1 Tb1 Tb2 159.50(10) . . ?
O7 Tb1 Tb2 41.78(8) . . ?
O5 Tb1 Tb2 40.87(8) . . ?
O12 Tb1 Tb2 41.31(8) . . ?
O9 Tb1 Tb2 117.13(9) . . ?
O3 Tb1 Tb2 95.05(8) . . ?
O2 Tb1 Tb2 94.99(8) . . ?
O8 Tb1 Tb2 103.51(8) . . ?
O6 Tb1 Tb2 99.05(8) . . ?
O1 Tb1 Tb2 137.83(10) . 2_566 ?
O7 Tb1 Tb2 69.20(8) . 2_566 ?
O5 Tb1 Tb2 98.45(8) . 2_566 ?
O12 Tb1 Tb2 34.33(8) . 2_566 ?
O9 Tb1 Tb2 82.51(9) . 2_566 ?
O3 Tb1 Tb2 35.61(8) . 2_566 ?
O2 Tb1 Tb2 144.53(9) . 2_566 ?
O8 Tb1 Tb2 89.20(8) . 2_566 ?
O6 Tb1 Tb2 132.06(9) . 2_566 ?
Tb2 Tb1 Tb2 61.197(8) . 2_566 ?
O5 Tb2 O12 133.81(12) . 2_566 ?
O5 Tb2 O12 69.47(12) . . ?
O12 Tb2 O12 72.14(13) 2_566 . ?
O5 Tb2 O3 148.02(12) . 2_566 ?
O12 Tb2 O3 70.12(11) 2_566 2_566 ?
O12 Tb2 O3 109.76(12) . 2_566 ?
O5 Tb2 O7 69.07(12) . . ?
O12 Tb2 O7 76.18(11) 2_566 . ?
O12 Tb2 O7 73.39(12) . . ?
O3 Tb2 O7 142.67(12) 2_566 . ?
O5 Tb2 N4 112.77(14) . . ?
O12 Tb2 N4 84.17(14) 2_566 . ?
O12 Tb2 N4 142.93(13) . . ?
O3 Tb2 N4 87.33(13) 2_566 . ?
O7 Tb2 N4 73.51(13) . . ?
O5 Tb2 O4 83.61(12) . 2_566 ?
O12 Tb2 O4 117.42(12) 2_566 2_566 ?
O12 Tb2 O4 84.70(12) . 2_566 ?
O3 Tb2 O4 64.74(11) 2_566 2_566 ?
O7 Tb2 O4 149.47(11) . 2_566 ?
N4 Tb2 O4 132.11(13) . 2_566 ?
O5 Tb2 N3 72.95(13) . . ?
O12 Tb2 N3 146.82(14) 2_566 . ?
O12 Tb2 N3 140.51(13) . . ?
O3 Tb2 N3 95.75(13) 2_566 . ?
O7 Tb2 N3 104.08(13) . . ?
N4 Tb2 N3 64.80(15) . . ?
O4 Tb2 N3 79.48(14) 2_566 . ?
O5 Tb2 Tb1 42.03(8) . . ?
O12 Tb2 Tb1 91.86(8) 2_566 . ?
O12 Tb2 Tb1 42.17(8) . . ?
O3 Tb2 Tb1 151.55(9) 2_566 . ?
O7 Tb2 Tb1 41.57(9) . . ?
N4 Tb2 Tb1 113.33(10) . . ?
O4 Tb2 Tb1 108.34(8) 2_566 . ?
N3 Tb2 Tb1 110.46(10) . . ?
O5 Tb2 Tb2 102.10(9) . 2_566 ?
O12 Tb2 Tb2 36.18(8) 2_566 2_566 ?
O12 Tb2 Tb2 35.96(8) . 2_566 ?
O3 Tb2 Tb2 89.99(8) 2_566 2_566 ?
O7 Tb2 Tb2 71.06(9) . 2_566 ?
N4 Tb2 Tb2 115.61(11) . 2_566 ?
O4 Tb2 Tb2 103.11(9) 2_566 2_566 ?
N3 Tb2 Tb2 174.26(10) . 2_566 ?
Tb1 Tb2 Tb2 63.919(8) . 2_566 ?
O5 Tb2 Tb1 151.76(9) . 2_566 ?
O12 Tb2 Tb1 35.21(8) 2_566 2_566 ?
O12 Tb2 Tb1 83.41(8) . 2_566 ?
O3 Tb2 Tb1 36.79(8) 2_566 2_566 ?
O7 Tb2 Tb1 111.38(8) . 2_566 ?
N4 Tb2 Tb1 93.50(10) . 2_566 ?
O4 Tb2 Tb1 86.26(8) 2_566 2_566 ?
N3 Tb2 Tb1 130.72(10) . 2_566 ?
Tb1 Tb2 Tb1 118.803(8) . 2_566 ?
Tb2 Tb2 Tb1 54.884(8) 2_566 2_566 ?
C14 N1 C13 117.3(5) . . ?
C7 N2 C8 126.2(5) . . ?
C7 N2 H21 108.7 . . ?
C8 N2 H21 124.3 . . ?
C29 N3 C30 115.4(5) . . ?
C29 N3 Tb2 128.6(4) . . ?
C30 N3 Tb2 115.4(3) . . ?
C36 N4 C35 121.4(5) . . ?
C36 N4 Tb2 131.9(4) . . ?
C35 N4 Tb2 106.6(3) . . ?
O11 N5 O10 123.1(6) . . ?
O11 N5 O9 118.5(6) . . ?
O10 N5 O9 118.4(5) . . ?
O14 N6 O15 118.4(14) . . ?
O14 N6 O13 121.7(14) . . ?
O15 N6 O13 118.9(12) . . ?
C1 O1 Tb1 125.7(3) . . ?
C2 O2 C21 116.7(4) . . ?
C2 O2 Tb1 116.0(3) . . ?
C21 O2 Tb1 126.8(3) . . ?
C20 O3 Tb2 113.5(3) . 2_566 ?
C20 O3 Tb1 133.3(3) . . ?
Tb2 O3 Tb1 107.61(13) 2_566 . ?
C19 O4 C22 117.1(4) . . ?
C19 O4 Tb2 110.7(3) . 2_566 ?
C22 O4 Tb2 130.1(3) . 2_566 ?
C23 O5 Tb2 134.6(3) . . ?
C23 O5 Tb1 128.1(3) . . ?
Tb2 O5 Tb1 97.10(12) . . ?
C28 O6 C43 117.2(5) . . ?
C28 O6 Tb1 116.7(3) . . ?
C43 O6 Tb1 125.6(4) . . ?
C42 O7 Tb1 128.7(3) . . ?
C42 O7 Tb2 134.2(3) . . ?
Tb1 O7 Tb2 96.65(12) . . ?
C41 O8 C44 115.6(4) . . ?
C41 O8 Tb1 117.1(3) . . ?
C44 O8 Tb1 127.1(4) . . ?
N5 O9 Tb1 132.3(4) . . ?
Tb2 O12 Tb2 107.86(13) 2_566 . ?
Tb2 O12 Tb1 110.46(13) 2_566 . ?
Tb2 O12 Tb1 96.52(12) . . ?
Tb2 O12 H121 107.9 2_566 . ?
Tb2 O12 H121 131.0 . . ?
Tb1 O12 H121 101.2 . . ?
O16B O16A O16C 84(2) . . ?
O17B O16C O16A 127(3) . . ?
O17B O16C O17C 106(3) . . ?
O16A O16C O17C 127(3) . . ?
O17A O17C O16C 98(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
N2 H21 O1 0.90 1.81 2.603(6) 145.7 .
O12 H121 O10 0.85 2.03 2.832(6) 157.0 .
O12 H121 N5 0.85 2.65 3.332(6) 138.3 .

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.182
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.111
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_73-2
_database_code_depnum_ccdc_archive 'CCDC 1000760'
_audit_update_record             
;
2014-10-08 deposited with the CCDC.
2015-01-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C88 H100 Ho4 N10 O24, 0.66(O6), 2(N O3) '
_chemical_formula_sum            ' C88 H100 Ho4 N12 O33.96  '
_chemical_formula_weight         2528.89

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'
Ho Ho -0.2175 4.6783 '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 '
_symmetry_space_group_name_Hall  ' -P 1 '

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

_cell_length_a                   14.4145(6)
_cell_length_b                   14.5348(8)
_cell_length_c                   14.6776(8)
_cell_angle_alpha                111.197(5)
_cell_angle_beta                 104.067(4)
_cell_angle_gamma                107.837(4)
_cell_volume                     2503.0(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1251.7
_exptl_absorpt_coefficient_mu    3.213
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.549
_exptl_absorpt_correction_T_max  0.659
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'

_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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19711
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_sigmaI/netI    0.0623
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.94
_diffrn_reflns_theta_max         25.00
_reflns_number_total             8810
_reflns_number_gt                6831
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_cell_refinement       'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXL-97

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
The water molecules in complex are highly disordered, and H-atoms can not be added. But the H-atoms located on the water molecules are took into consideration in the formular of complex.
;

_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)+(0.0375P)²+2.9879P] 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         8810
_refine_ls_number_parameters     632
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0370
_refine_ls_wR_factor_ref         0.0995
_refine_ls_wR_factor_gt          0.0865
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_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
C1 C 0.1044(5) 0.1093(5) 0.2713(5) 0.0339(15) Uani 1 1 d . . .
C2 C 0.0131(5) 0.0841(5) 0.1894(5) 0.0350(15) Uani 1 1 d . . .
C3 C -0.0362(6) -0.0132(5) 0.0951(5) 0.0393(16) Uani 1 1 d . . .
H3 H -0.0984 -0.0288 0.0425 0.047 Uiso 1 1 calc R . .
C4 C 0.0082(6) -0.0886(5) 0.0792(5) 0.0467(19) Uani 1 1 d . . .
H4 H -0.0241 -0.1539 0.0156 0.056 Uiso 1 1 calc R . .
C5 C 0.0984(6) -0.0654(5) 0.1572(5) 0.0440(18) Uani 1 1 d . . .
H5 H 0.1280 -0.1150 0.1463 0.053 Uiso 1 1 calc R . .
C6 C 0.1482(5) 0.0327(5) 0.2545(5) 0.0358(16) Uani 1 1 d . . .
C7 C 0.2393(6) 0.0510(6) 0.3364(6) 0.0430(18) Uani 1 1 d . . .
H7 H 0.2627 -0.0035 0.3244 0.052 Uiso 1 1 calc R . .
C8 C 0.3859(5) 0.1649(6) 0.5149(5) 0.0408(17) Uani 1 1 d . . .
H8 H 0.3714 0.1032 0.5307 0.049 Uiso 1 1 calc R . .
C9 C 0.4824(6) 0.1824(7) 0.4857(6) 0.057(2) Uani 1 1 d . . .
H9A H 0.4685 0.1161 0.4247 0.068 Uiso 1 1 calc R . .
H9B H 0.4961 0.2412 0.4668 0.068 Uiso 1 1 calc R . .
C10 C 0.5778(6) 0.2109(8) 0.5788(7) 0.072(3) Uani 1 1 d . . .
H10A H 0.6392 0.2232 0.5606 0.086 Uiso 1 1 calc R . .
H10B H 0.5654 0.1501 0.5947 0.086 Uiso 1 1 calc R . .
C11 C 0.6000(6) 0.3126(7) 0.6760(7) 0.067(2) Uani 1 1 d . . .
H11A H 0.6610 0.3285 0.7353 0.080 Uiso 1 1 calc R . .
H11B H 0.6171 0.3745 0.6616 0.080 Uiso 1 1 calc R . .
C12 C 0.5053(6) 0.2975(6) 0.7057(6) 0.053(2) Uani 1 1 d . . .
H12A H 0.5207 0.3648 0.7664 0.064 Uiso 1 1 calc R . .
H12B H 0.4923 0.2400 0.7263 0.064 Uiso 1 1 calc R . .
C13 C 0.4066(6) 0.2678(6) 0.6140(5) 0.0430(17) Uani 1 1 d . . .
H13 H 0.4165 0.3291 0.5978 0.052 Uiso 1 1 calc R . .
C14 C 0.2605(5) 0.2967(5) 0.6345(5) 0.0367(16) Uani 1 1 d . . .
H14 H 0.2819 0.3492 0.6125 0.044 Uiso 1 1 calc R . .
C15 C 0.1683(5) 0.2812(5) 0.6628(5) 0.0337(15) Uani 1 1 d . . .
C16 C 0.1496(6) 0.2226(5) 0.7200(5) 0.0452(18) Uani 1 1 d . . .
H16 H 0.1955 0.1930 0.7380 0.054 Uiso 1 1 calc R . .
C17 C 0.0661(6) 0.2084(6) 0.7495(6) 0.050(2) Uani 1 1 d . . .
H17 H 0.0551 0.1685 0.7863 0.060 Uiso 1 1 calc R . .
C18 C -0.0038(6) 0.2534(5) 0.7249(5) 0.0436(18) Uani 1 1 d . . .
H18 H -0.0612 0.2437 0.7448 0.052 Uiso 1 1 calc R . .
C19 C 0.0146(5) 0.3123(5) 0.6707(5) 0.0328(15) Uani 1 1 d . . .
C20 C 0.0981(5) 0.3251(5) 0.6357(4) 0.0288(14) Uani 1 1 d . . .
C21 C -0.1221(5) 0.1403(6) 0.1361(5) 0.0457(18) Uani 1 1 d . . .
H21A H -0.1161 0.1286 0.0695 0.069 Uiso 1 1 calc R . .
H21B H -0.1398 0.2006 0.1615 0.069 Uiso 1 1 calc R . .
H21C H -0.1768 0.0753 0.1261 0.069 Uiso 1 1 calc R . .
C22 C -0.1455(6) 0.3382(6) 0.6565(6) 0.055(2) Uani 1 1 d . . .
H22A H -0.1880 0.2604 0.6147 0.082 Uiso 1 1 calc R . .
H22B H -0.1815 0.3753 0.6311 0.082 Uiso 1 1 calc R . .
H22C H -0.1344 0.3599 0.7298 0.082 Uiso 1 1 calc R . .
C23 C 0.0532(5) 0.3890(5) 0.1950(5) 0.0342(15) Uani 1 1 d . . .
C24 C -0.0083(6) 0.3941(5) 0.1094(5) 0.0359(16) Uani 1 1 d . . .
C25 C 0.0259(7) 0.3914(6) 0.0264(5) 0.0485(19) Uani 1 1 d . . .
H25 H -0.0151 0.3940 -0.0315 0.058 Uiso 1 1 calc R . .
C26 C 0.1183(7) 0.3850(6) 0.0312(6) 0.054(2) Uani 1 1 d . . .
H26 H 0.1419 0.3865 -0.0221 0.065 Uiso 1 1 calc R . .
C27 C 0.1785(6) 0.3761(6) 0.1139(6) 0.0494(19) Uani 1 1 d . . .
H27 H 0.2417 0.3712 0.1155 0.059 Uiso 1 1 calc R . .
C28 C 0.1450(5) 0.3743(5) 0.1935(5) 0.0373(16) Uani 1 1 d . . .
C29 C -0.1128(6) 0.3923(5) 0.0949(5) 0.0403(17) Uani 1 1 d . . .
H29 H -0.1566 0.3726 0.0264 0.048 Uiso 1 1 calc R . .
C30 C -0.2659(6) 0.3883(6) 0.1255(5) 0.0434(17) Uani 1 1 d . . .
H30 H -0.3036 0.3102 0.0733 0.052 Uiso 1 1 calc R . .
C31 C -0.2954(6) 0.4498(6) 0.0685(6) 0.052(2) Uani 1 1 d . . .
H31A H -0.2757 0.4336 0.0079 0.063 Uiso 1 1 calc R . .
H31B H -0.2562 0.5280 0.1164 0.063 Uiso 1 1 calc R . .
C32 C -0.4145(6) 0.4181(7) 0.0303(6) 0.066(2) Uani 1 1 d . . .
H32A H -0.4290 0.4663 0.0035 0.079 Uiso 1 1 calc R . .
H32B H -0.4524 0.3439 -0.0283 0.079 Uiso 1 1 calc R . .
C33 C -0.4557(7) 0.4241(7) 0.1152(7) 0.064(2) Uani 1 1 d . . .
H33A H -0.5327 0.3925 0.0832 0.077 Uiso 1 1 calc R . .
H33B H -0.4300 0.5005 0.1660 0.077 Uiso 1 1 calc R . .
C34 C -0.4225(6) 0.3645(6) 0.1743(6) 0.0520(19) Uani 1 1 d . . .
H34A H -0.4436 0.3789 0.2341 0.062 Uiso 1 1 calc R . .
H34B H -0.4584 0.2861 0.1269 0.062 Uiso 1 1 calc R . .
C35 C -0.3038(6) 0.4021(6) 0.2142(6) 0.0439(17) Uani 1 1 d . . .
H35 H -0.2717 0.4812 0.2619 0.053 Uiso 1 1 calc R . .
C36 C -0.3121(6) 0.2721(5) 0.2812(5) 0.0415(17) Uani 1 1 d . . .
H36 H -0.3854 0.2473 0.2515 0.050 Uiso 1 1 calc R . .
C37 C -0.2734(5) 0.2112(5) 0.3293(5) 0.0389(16) Uani 1 1 d . . .
C38 C -0.3490(6) 0.1269(6) 0.3321(6) 0.055(2) Uani 1 1 d . . .
H38 H -0.4188 0.1182 0.3116 0.066 Uiso 1 1 calc R . .
C39 C -0.3257(7) 0.0568(7) 0.3634(7) 0.067(2) Uani 1 1 d . . .
H39 H -0.3779 0.0027 0.3664 0.081 Uiso 1 1 calc R . .
C40 C -0.2222(6) 0.0669(6) 0.3910(6) 0.055(2) Uani 1 1 d . . .
H40 H -0.2052 0.0182 0.4107 0.066 Uiso 1 1 calc R . .
C41 C -0.1457(6) 0.1490(5) 0.3890(5) 0.0371(16) Uani 1 1 d . . .
C42 C -0.1677(5) 0.2262(5) 0.3615(5) 0.0333(15) Uani 1 1 d . . .
C43 C 0.2923(6) 0.3506(7) 0.2849(7) 0.064(2) Uani 1 1 d . . .
H43A H 0.2784 0.2862 0.2231 0.096 Uiso 1 1 calc R . .
H43B H 0.3209 0.3448 0.3478 0.096 Uiso 1 1 calc R . .
H43C H 0.3426 0.4141 0.2882 0.096 Uiso 1 1 calc R . .
C44 C -0.0175(6) 0.0819(5) 0.4306(6) 0.0494(19) Uani 1 1 d . . .
H44A H -0.0362 0.0769 0.4877 0.074 Uiso 1 1 calc R . .
H44B H 0.0571 0.1017 0.4498 0.074 Uiso 1 1 calc R . .
H44C H -0.0575 0.0122 0.3673 0.074 Uiso 1 1 calc R . .
Ho1 Ho 0.08512(2) 0.33010(2) 0.39788(2) 0.03013(10) Uani 1 1 d . . .
Ho2 Ho -0.06715(2) 0.46888(2) 0.35913(2) 0.02565(9) Uani 1 1 d . . .
N1 N 0.3117(5) 0.2410(4) 0.6393(4) 0.0409(14) Uani 1 1 d . . .
N2 N 0.2909(4) 0.1398(5) 0.4268(4) 0.0408(14) Uani 1 1 d D . .
H21 H 0.2549 0.1814 0.4375 0.049 Uiso 1 1 d RD . .
N3 N -0.1512(4) 0.4150(4) 0.1668(4) 0.0339(13) Uani 1 1 d . . .
N4 N -0.2564(4) 0.3546(4) 0.2760(4) 0.0360(13) Uani 1 1 d . . .
N5 N 0.3355(5) 0.5315(5) 0.5215(5) 0.0480(16) Uani 1 1 d . . .
N6 N 0.6793(11) 0.1557(11) 0.8135(11) 0.135(5) Uani 1 1 d . . .
O1 O 0.1474(3) 0.2014(3) 0.3607(3) 0.0389(11) Uani 1 1 d . . .
O2 O -0.0229(4) 0.1645(3) 0.2126(3) 0.0417(11) Uani 1 1 d . . .
O3 O 0.1081(3) 0.3818(3) 0.5805(3) 0.0291(10) Uani 1 1 d . . .
O4 O -0.0448(3) 0.3666(3) 0.6475(3) 0.0345(10) Uani 1 1 d . . .
O5 O 0.0275(3) 0.3922(3) 0.2774(3) 0.0333(10) Uani 1 1 d . . .
O6 O 0.1936(4) 0.3607(4) 0.2784(4) 0.0466(12) Uani 1 1 d . . .
O7 O -0.0899(3) 0.3045(3) 0.3629(3) 0.0304(10) Uani 1 1 d . . .
O8 O -0.0412(4) 0.1638(3) 0.4110(3) 0.0384(11) Uani 1 1 d . . .
O9 O 0.2708(4) 0.4369(4) 0.5015(3) 0.0425(11) Uani 1 1 d . . .
O10 O 0.2998(4) 0.5890(4) 0.4935(4) 0.0607(15) Uani 1 1 d . . .
O11 O 0.4298(5) 0.5623(5) 0.5695(5) 0.087(2) Uani 1 1 d . . .
O12 O 0.0906(3) 0.5049(3) 0.4845(3) 0.0267(9) Uani 1 1 d D . .
H121 H 0.1541 0.5477 0.5009 0.032 Uiso 1 1 d RD . .
O13 O 0.7551(9) 0.2039(9) 0.8019(10) 0.163(5) Uani 1 1 d . . .
O14 O 0.6575(12) 0.1949(13) 0.8777(10) 0.314(11) Uani 1 1 d . . .
O15 O 0.6192(8) 0.0683(8) 0.7450(9) 0.192(6) Uani 1 1 d . . .
O16A O 0.3892(18) 0.0541(18) 0.0817(18) 0.105(7) Uiso 0.33 1 d P . .
O17A O 0.378(2) 0.097(2) -0.082(2) 0.142(9) Uiso 0.33 1 d P . .
O17B O 0.355(2) 0.097(2) 0.006(2) 0.145(10) Uiso 0.33 1 d P . .
O17C O 0.316(2) 0.154(2) -0.106(2) 0.155(10) Uiso 0.33 1 d P . .
O16C O 0.304(2) 0.157(2) 0.045(2) 0.157(11) Uiso 0.33 1 d P . .
O16B O 0.356(2) 0.098(2) 0.143(2) 0.124(8) Uiso 0.33 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
C1 O1 1.314(7) . ?
C1 C2 1.388(9) . ?
C1 C6 1.416(8) . ?
C2 C3 1.382(8) . ?
C2 O2 1.386(7) . ?
C3 C4 1.408(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.358(10) . ?
C4 H4 0.9300 . ?
C5 C6 1.411(9) . ?
C5 H5 0.9300 . ?
C6 C7 1.424(9) . ?
C7 N2 1.293(8) . ?
C7 H7 0.9300 . ?
C8 N2 1.474(8) . ?
C8 C9 1.528(9) . ?
C8 C13 1.545(9) . ?
C8 H8 0.9800 . ?
C9 C10 1.502(10) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.511(11) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.509(10) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.515(9) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N1 1.478(8) . ?
C13 H13 0.9800 . ?
C14 N1 1.260(8) . ?
C14 C15 1.463(8) . ?
C14 H14 0.9300 . ?
C15 C20 1.404(8) . ?
C15 C16 1.411(9) . ?
C16 C17 1.357(9) . ?
C16 H16 0.9300 . ?
C17 C18 1.405(9) . ?
C17 H17 0.9300 . ?
C18 C19 1.376(9) . ?
C18 H18 0.9300 . ?
C19 O4 1.392(7) . ?
C19 C20 1.407(8) . ?
C20 O3 1.351(7) . ?
C21 O2 1.433(7) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 O4 1.436(7) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 O5 1.338(7) . ?
C23 C24 1.391(9) . ?
C23 C28 1.408(9) . ?
C24 C25 1.414(8) . ?
C24 C29 1.460(9) . ?
C25 C26 1.350(10) . ?
C25 H25 0.9300 . ?
C26 C27 1.383(10) . ?
C26 H26 0.9300 . ?
C27 C28 1.374(9) . ?
C27 H27 0.9300 . ?
C28 O6 1.385(8) . ?
C29 N3 1.293(7) . ?
C29 H29 0.9300 . ?
C30 N3 1.484(8) . ?
C30 C35 1.502(9) . ?
C30 C31 1.510(9) . ?
C30 H30 0.9800 . ?
C31 C32 1.527(10) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C33 1.492(10) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 C34 1.526(10) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 C35 1.509(9) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 N4 1.487(8) . ?
C35 H35 0.9800 . ?
C36 N4 1.263(8) . ?
C36 C37 1.468(9) . ?
C36 H36 0.9300 . ?
C37 C38 1.390(9) . ?
C37 C42 1.401(9) . ?
C38 C39 1.355(10) . ?
C38 H38 0.9300 . ?
C39 C40 1.392(11) . ?
C39 H39 0.9300 . ?
C40 C41 1.370(9) . ?
C40 H40 0.9300 . ?
C41 O8 1.392(8) . ?
C41 C42 1.415(9) . ?
C42 O7 1.321(7) . ?
C43 O6 1.459(8) . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 O8 1.437(7) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
Ho1 O1 2.265(4) . ?
Ho1 O7 2.329(4) . ?
Ho1 O5 2.352(4) . ?
Ho1 O12 2.361(3) . ?
Ho1 O9 2.378(5) . ?
Ho1 O3 2.412(4) . ?
Ho1 O2 2.555(4) . ?
Ho1 O8 2.647(4) . ?
Ho1 O6 2.681(4) . ?
Ho1 Ho2 3.4850(4) . ?
Ho1 Ho2 3.8342(4) 2_566 ?
Ho2 O5 2.303(4) . ?
Ho2 O12 2.314(4) 2_566 ?
Ho2 O12 2.317(4) . ?
Ho2 O7 2.333(4) . ?
Ho2 O3 2.343(4) 2_566 ?
Ho2 N4 2.414(5) . ?
Ho2 N3 2.492(5) . ?
Ho2 O4 2.492(4) 2_566 ?
Ho2 Ho2 3.7411(6) 2_566 ?
Ho2 Ho1 3.8342(4) 2_566 ?
N2 H21 0.9067 . ?
N5 O11 1.217(8) . ?
N5 O10 1.242(7) . ?
N5 O9 1.278(7) . ?
N6 O14 1.085(12) . ?
N6 O15 1.163(13) . ?
N6 O13 1.193(14) . ?
O3 Ho2 2.343(4) 2_566 ?
O4 Ho2 2.492(4) 2_566 ?
O12 Ho2 2.314(4) 2_566 ?
O12 H121 0.8477 . ?
O16A O16B 1.19(3) . ?
O16A O17B 1.51(3) . ?
O17A O17B 1.41(3) . ?
O17A O17C 1.46(3) . ?
O17B O16C 1.36(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 120.2(5) . . ?
O1 C1 C6 122.0(6) . . ?
C2 C1 C6 117.8(5) . . ?
C3 C2 O2 124.4(6) . . ?
C3 C2 C1 122.0(6) . . ?
O2 C2 C1 113.6(5) . . ?
C2 C3 C4 119.7(6) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C5 C4 C3 119.5(6) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 121.2(6) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C5 C6 C1 119.7(6) . . ?
C5 C6 C7 119.3(6) . . ?
C1 C6 C7 120.9(6) . . ?
N2 C7 C6 123.1(6) . . ?
N2 C7 H7 118.4 . . ?
C6 C7 H7 118.4 . . ?
N2 C8 C9 111.5(5) . . ?
N2 C8 C13 108.0(5) . . ?
C9 C8 C13 111.2(6) . . ?
N2 C8 H8 108.7 . . ?
C9 C8 H8 108.7 . . ?
C13 C8 H8 108.7 . . ?
C10 C9 C8 109.6(6) . . ?
C10 C9 H9A 109.8 . . ?
C8 C9 H9A 109.8 . . ?
C10 C9 H9B 109.8 . . ?
C8 C9 H9B 109.8 . . ?
H9A C9 H9B 108.2 . . ?
C9 C10 C11 111.0(7) . . ?
C9 C10 H10A 109.4 . . ?
C11 C10 H10A 109.4 . . ?
C9 C10 H10B 109.4 . . ?
C11 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
C12 C11 C10 111.0(7) . . ?
C12 C11 H11A 109.4 . . ?
C10 C11 H11A 109.4 . . ?
C12 C11 H11B 109.4 . . ?
C10 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
C11 C12 C13 111.6(6) . . ?
C11 C12 H12A 109.3 . . ?
C13 C12 H12A 109.3 . . ?
C11 C12 H12B 109.3 . . ?
C13 C12 H12B 109.3 . . ?
H12A C12 H12B 108.0 . . ?
N1 C13 C12 111.3(5) . . ?
N1 C13 C8 107.1(6) . . ?
C12 C13 C8 109.5(5) . . ?
N1 C13 H13 109.6 . . ?
C12 C13 H13 109.6 . . ?
C8 C13 H13 109.6 . . ?
N1 C14 C15 121.8(6) . . ?
N1 C14 H14 119.1 . . ?
C15 C14 H14 119.1 . . ?
C20 C15 C16 118.7(6) . . ?
C20 C15 C14 121.4(6) . . ?
C16 C15 C14 119.9(6) . . ?
C17 C16 C15 121.6(7) . . ?
C17 C16 H16 119.2 . . ?
C15 C16 H16 119.2 . . ?
C16 C17 C18 120.6(6) . . ?
C16 C17 H17 119.7 . . ?
C18 C17 H17 119.7 . . ?
C19 C18 C17 118.4(6) . . ?
C19 C18 H18 120.8 . . ?
C17 C18 H18 120.8 . . ?
C18 C19 O4 123.9(6) . . ?
C18 C19 C20 122.3(6) . . ?
O4 C19 C20 113.8(5) . . ?
O3 C20 C15 123.6(5) . . ?
O3 C20 C19 118.0(5) . . ?
C15 C20 C19 118.4(5) . . ?
O2 C21 H21A 109.5 . . ?
O2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O4 C22 H22A 109.5 . . ?
O4 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
O4 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O5 C23 C24 123.6(6) . . ?
O5 C23 C28 117.4(6) . . ?
C24 C23 C28 118.9(6) . . ?
C23 C24 C25 119.6(6) . . ?
C23 C24 C29 123.3(6) . . ?
C25 C24 C29 116.9(6) . . ?
C26 C25 C24 119.9(7) . . ?
C26 C25 H25 120.1 . . ?
C24 C25 H25 120.1 . . ?
C25 C26 C27 121.2(7) . . ?
C25 C26 H26 119.4 . . ?
C27 C26 H26 119.4 . . ?
C28 C27 C26 120.1(7) . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C27 C28 O6 126.9(6) . . ?
C27 C28 C23 120.0(7) . . ?
O6 C28 C23 113.1(5) . . ?
N3 C29 C24 127.2(6) . . ?
N3 C29 H29 116.4 . . ?
C24 C29 H29 116.4 . . ?
N3 C30 C35 109.5(5) . . ?
N3 C30 C31 114.9(6) . . ?
C35 C30 C31 111.7(6) . . ?
N3 C30 H30 106.8 . . ?
C35 C30 H30 106.8 . . ?
C31 C30 H30 106.8 . . ?
C30 C31 C32 111.1(6) . . ?
C30 C31 H31A 109.4 . . ?
C32 C31 H31A 109.4 . . ?
C30 C31 H31B 109.4 . . ?
C32 C31 H31B 109.4 . . ?
H31A C31 H31B 108.0 . . ?
C33 C32 C31 113.5(7) . . ?
C33 C32 H32A 108.9 . . ?
C31 C32 H32A 108.9 . . ?
C33 C32 H32B 108.9 . . ?
C31 C32 H32B 108.9 . . ?
H32A C32 H32B 107.7 . . ?
C32 C33 C34 113.1(7) . . ?
C32 C33 H33A 109.0 . . ?
C34 C33 H33A 109.0 . . ?
C32 C33 H33B 109.0 . . ?
C34 C33 H33B 109.0 . . ?
H33A C33 H33B 107.8 . . ?
C35 C34 C33 110.6(6) . . ?
C35 C34 H34A 109.5 . . ?
C33 C34 H34A 109.5 . . ?
C35 C34 H34B 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 108.1 . . ?
N4 C35 C30 107.6(5) . . ?
N4 C35 C34 118.3(6) . . ?
C30 C35 C34 111.8(6) . . ?
N4 C35 H35 106.2 . . ?
C30 C35 H35 106.2 . . ?
C34 C35 H35 106.2 . . ?
N4 C36 C37 126.9(6) . . ?
N4 C36 H36 116.6 . . ?
C37 C36 H36 116.6 . . ?
C38 C37 C42 119.1(6) . . ?
C38 C37 C36 117.0(6) . . ?
C42 C37 C36 123.5(6) . . ?
C39 C38 C37 122.9(7) . . ?
C39 C38 H38 118.6 . . ?
C37 C38 H38 118.6 . . ?
C38 C39 C40 119.0(7) . . ?
C38 C39 H39 120.5 . . ?
C40 C39 H39 120.5 . . ?
C41 C40 C39 119.6(7) . . ?
C41 C40 H40 120.2 . . ?
C39 C40 H40 120.2 . . ?
C40 C41 O8 124.2(6) . . ?
C40 C41 C42 122.1(7) . . ?
O8 C41 C42 113.7(6) . . ?
O7 C42 C37 123.7(6) . . ?
O7 C42 C41 119.0(6) . . ?
C37 C42 C41 117.2(6) . . ?
O6 C43 H43A 109.5 . . ?
O6 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
O6 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
O8 C44 H44A 109.5 . . ?
O8 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
O8 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O1 Ho1 O7 128.38(14) . . ?
O1 Ho1 O5 123.44(14) . . ?
O7 Ho1 O5 68.44(14) . . ?
O1 Ho1 O12 157.37(15) . . ?
O7 Ho1 O12 73.00(13) . . ?
O5 Ho1 O12 67.71(13) . . ?
O1 Ho1 O9 77.85(15) . . ?
O7 Ho1 O9 151.06(14) . . ?
O5 Ho1 O9 109.89(16) . . ?
O12 Ho1 O9 79.72(14) . . ?
O1 Ho1 O3 102.35(14) . . ?
O7 Ho1 O3 86.81(14) . . ?
O5 Ho1 O3 134.09(12) . . ?
O12 Ho1 O3 68.30(13) . . ?
O9 Ho1 O3 74.09(15) . . ?
O1 Ho1 O2 65.17(15) . . ?
O7 Ho1 O2 75.32(14) . . ?
O5 Ho1 O2 71.78(14) . . ?
O12 Ho1 O2 135.31(14) . . ?
O9 Ho1 O2 132.86(14) . . ?
O3 Ho1 O2 139.81(14) . . ?
O1 Ho1 O8 72.79(15) . . ?
O7 Ho1 O8 63.14(13) . . ?
O5 Ho1 O8 123.93(15) . . ?
O12 Ho1 O8 119.47(13) . . ?
O9 Ho1 O8 126.17(15) . . ?
O3 Ho1 O8 69.63(13) . . ?
O2 Ho1 O8 70.18(14) . . ?
O1 Ho1 O6 72.84(15) . . ?
O7 Ho1 O6 126.56(14) . . ?
O5 Ho1 O6 60.96(14) . . ?
O12 Ho1 O6 101.33(13) . . ?
O9 Ho1 O6 67.88(15) . . ?
O3 Ho1 O6 141.86(15) . . ?
O2 Ho1 O6 73.80(15) . . ?
O8 Ho1 O6 137.92(13) . . ?
O1 Ho1 Ho2 159.61(11) . . ?
O7 Ho1 Ho2 41.67(9) . . ?
O5 Ho1 Ho2 40.99(9) . . ?
O12 Ho1 Ho2 41.36(10) . . ?
O9 Ho1 Ho2 117.49(11) . . ?
O3 Ho1 Ho2 95.17(9) . . ?
O2 Ho1 Ho2 94.67(10) . . ?
O8 Ho1 Ho2 104.30(9) . . ?
O6 Ho1 Ho2 99.55(10) . . ?
O1 Ho1 Ho2 137.65(11) . 2_566 ?
O7 Ho1 Ho2 69.42(9) . 2_566 ?
O5 Ho1 Ho2 98.46(9) . 2_566 ?
O12 Ho1 Ho2 34.49(9) . 2_566 ?
O9 Ho1 Ho2 82.67(10) . 2_566 ?
O3 Ho1 Ho2 35.66(9) . 2_566 ?
O2 Ho1 Ho2 144.47(10) . 2_566 ?
O8 Ho1 Ho2 89.79(9) . 2_566 ?
O6 Ho1 Ho2 132.23(10) . 2_566 ?
Ho2 Ho1 Ho2 61.259(9) . 2_566 ?
O5 Ho2 O12 133.73(14) . 2_566 ?
O5 Ho2 O12 69.26(13) . . ?
O12 Ho2 O12 72.21(15) 2_566 . ?
O5 Ho2 O7 69.20(14) . . ?
O12 Ho2 O7 76.27(13) 2_566 . ?
O12 Ho2 O7 73.73(14) . . ?
O5 Ho2 O3 147.73(14) . 2_566 ?
O12 Ho2 O3 70.25(13) 2_566 2_566 ?
O12 Ho2 O3 109.67(13) . 2_566 ?
O7 Ho2 O3 142.82(13) . 2_566 ?
O5 Ho2 N4 113.81(16) . . ?
O12 Ho2 N4 83.82(16) 2_566 . ?
O12 Ho2 N4 143.43(16) . . ?
O7 Ho2 N4 74.00(16) . . ?
O3 Ho2 N4 86.59(15) 2_566 . ?
O5 Ho2 N3 73.56(15) . . ?
O12 Ho2 N3 146.84(16) 2_566 . ?
O12 Ho2 N3 140.62(15) . . ?
O7 Ho2 N3 104.80(15) . . ?
O3 Ho2 N3 94.91(15) 2_566 . ?
N4 Ho2 N3 65.35(17) . . ?
O5 Ho2 O4 82.94(14) . 2_566 ?
O12 Ho2 O4 117.68(13) 2_566 2_566 ?
O12 Ho2 O4 84.25(14) . 2_566 ?
O7 Ho2 O4 149.07(13) . 2_566 ?
O3 Ho2 O4 65.10(13) 2_566 2_566 ?
N4 Ho2 O4 131.99(16) . 2_566 ?
N3 Ho2 O4 78.73(16) . 2_566 ?
O5 Ho2 Ho1 42.06(10) . . ?
O12 Ho2 Ho1 91.78(9) 2_566 . ?
O12 Ho2 Ho1 42.32(9) . . ?
O7 Ho2 Ho1 41.58(10) . . ?
O3 Ho2 Ho1 151.59(10) 2_566 . ?
N4 Ho2 Ho1 113.96(12) . . ?
N3 Ho2 Ho1 111.16(11) . . ?
O4 Ho2 Ho1 107.98(9) 2_566 . ?
O5 Ho2 Ho2 102.02(10) . 2_566 ?
O12 Ho2 Ho2 36.13(10) 2_566 2_566 ?
O12 Ho2 Ho2 36.08(9) . 2_566 ?
O7 Ho2 Ho2 71.32(10) . 2_566 ?
O3 Ho2 Ho2 89.96(9) 2_566 2_566 ?
N4 Ho2 Ho2 115.51(13) . 2_566 ?
N3 Ho2 Ho2 175.11(11) . 2_566 ?
O4 Ho2 Ho2 103.02(10) 2_566 2_566 ?
Ho1 Ho2 Ho2 63.978(9) . 2_566 ?
O5 Ho2 Ho1 151.40(11) . 2_566 ?
O12 Ho2 Ho1 35.29(9) 2_566 2_566 ?
O12 Ho2 Ho1 83.31(8) . 2_566 ?
O7 Ho2 Ho1 111.55(9) . 2_566 ?
O3 Ho2 Ho1 36.87(9) 2_566 2_566 ?
N4 Ho2 Ho1 92.93(12) . 2_566 ?
N3 Ho2 Ho1 130.09(11) . 2_566 ?
O4 Ho2 Ho1 86.51(9) 2_566 2_566 ?
Ho1 Ho2 Ho1 118.741(9) . 2_566 ?
Ho2 Ho2 Ho1 54.763(9) 2_566 2_566 ?
C14 N1 C13 116.9(6) . . ?
C7 N2 C8 126.2(6) . . ?
C7 N2 H21 112.3 . . ?
C8 N2 H21 120.4 . . ?
C29 N3 C30 115.1(6) . . ?
C29 N3 Ho2 128.5(5) . . ?
C30 N3 Ho2 115.6(4) . . ?
C36 N4 C35 122.4(6) . . ?
C36 N4 Ho2 131.2(5) . . ?
C35 N4 Ho2 106.3(4) . . ?
O11 N5 O10 122.6(7) . . ?
O11 N5 O9 118.2(7) . . ?
O10 N5 O9 119.1(6) . . ?
O14 N6 O15 118.8(17) . . ?
O14 N6 O13 122.5(16) . . ?
O15 N6 O13 117.8(14) . . ?
C1 O1 Ho1 125.5(4) . . ?
C2 O2 C21 116.9(5) . . ?
C2 O2 Ho1 115.5(4) . . ?
C21 O2 Ho1 127.1(3) . . ?
C20 O3 Ho2 113.6(3) . 2_566 ?
C20 O3 Ho1 133.2(3) . . ?
Ho2 O3 Ho1 107.48(15) 2_566 . ?
C19 O4 C22 117.8(5) . . ?
C19 O4 Ho2 110.4(3) . 2_566 ?
C22 O4 Ho2 129.8(4) . 2_566 ?
C23 O5 Ho2 134.4(4) . . ?
C23 O5 Ho1 128.4(4) . . ?
Ho2 O5 Ho1 96.94(13) . . ?
C28 O6 C43 116.1(5) . . ?
C28 O6 Ho1 116.9(4) . . ?
C43 O6 Ho1 126.5(4) . . ?
C42 O7 Ho1 127.9(4) . . ?
C42 O7 Ho2 134.8(4) . . ?
Ho1 O7 Ho2 96.75(14) . . ?
C41 O8 C44 115.6(5) . . ?
C41 O8 Ho1 116.1(3) . . ?
C44 O8 Ho1 128.1(4) . . ?
N5 O9 Ho1 132.4(4) . . ?
Ho2 O12 Ho2 107.79(15) 2_566 . ?
Ho2 O12 Ho1 110.22(15) 2_566 . ?
Ho2 O12 Ho1 96.33(14) . . ?
Ho2 O12 H121 107.8 2_566 . ?
Ho2 O12 H121 130.4 . . ?
Ho1 O12 H121 102.5 . . ?
O16B O16A O17B 94(2) . . ?
O17B O17A O17C 96(2) . . ?
O16C O17B O17A 119(3) . . ?
O16C O17B O16A 108(3) . . ?
O17A O17B O16A 132(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H21 O1 0.91 1.85 2.610(7) 139.9 .
O12 H121 O10 0.85 2.04 2.835(6) 155.6 .
O12 H121 N5 0.85 2.65 3.315(7) 136.2 .

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.367
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.125
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_74-1
_database_code_depnum_ccdc_archive 'CCDC 1000761'
_audit_update_record             
;
2014-10-08 deposited with the CCDC.
2015-01-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C88 H100 Er4 N10 O24, 0.66(O6), 2(N O3) '
_chemical_formula_sum            'C88 H100 Er4 N12 O33.96 '
_chemical_formula_weight         2538.21

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'
Er Er -0.2586 4.9576 '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 '
_symmetry_space_group_name_Hall  ' -P 1 '

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

_cell_length_a                   14.4223(9)
_cell_length_b                   14.5202(9)
_cell_length_c                   14.6662(8)
_cell_angle_alpha                111.232(5)
_cell_angle_beta                 104.018(5)
_cell_angle_gamma                107.831(5)
_cell_volume                     2500.2(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1255.7
_exptl_absorpt_coefficient_mu    3.408
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.477
_exptl_absorpt_correction_T_max  0.600
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'

_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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18793
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0553
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.92
_diffrn_reflns_theta_max         25.00
_reflns_number_total             8805
_reflns_number_gt                6958
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_cell_refinement       'RAPID-AUTO (Rigaku 1998 RAPID-AUTO)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXL-97

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
The water molecules in complex are highly disordered, and H-atoms can not be added. But the H-atoms located on the water molecules are took into consideration in the formular of complex.
;

_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)+(0.0357P)²+4.3898P] 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         8805
_refine_ls_number_parameters     632
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0353
_refine_ls_wR_factor_ref         0.0938
_refine_ls_wR_factor_gt          0.0829
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1044(5) 0.1096(5) 0.2721(5) 0.0345(15) Uani 1 1 d . . .
C2 C 0.0119(5) 0.0836(5) 0.1888(5) 0.0373(15) Uani 1 1 d . . .
C3 C -0.0365(5) -0.0135(5) 0.0952(5) 0.0419(16) Uani 1 1 d . . .
H3 H -0.0988 -0.0296 0.0425 0.050 Uiso 1 1 calc R . .
C4 C 0.0078(6) -0.0880(5) 0.0790(5) 0.0447(17) Uani 1 1 d . . .
H4 H -0.0243 -0.1530 0.0152 0.054 Uiso 1 1 calc R . .
C5 C 0.0989(6) -0.0650(5) 0.1575(5) 0.0449(17) Uani 1 1 d . . .
H5 H 0.1286 -0.1145 0.1463 0.054 Uiso 1 1 calc R . .
C6 C 0.1480(5) 0.0330(5) 0.2550(5) 0.0378(15) Uani 1 1 d . . .
C7 C 0.2395(5) 0.0517(5) 0.3373(5) 0.0401(16) Uani 1 1 d . . .
H7 H 0.2633 -0.0026 0.3258 0.048 Uiso 1 1 calc R . .
C8 C 0.3852(5) 0.1652(6) 0.5152(5) 0.0414(16) Uani 1 1 d . . .
H8 H 0.3704 0.1032 0.5306 0.050 Uiso 1 1 calc R . .
C9 C 0.4811(5) 0.1828(7) 0.4857(6) 0.057(2) Uani 1 1 d . . .
H9A H 0.4669 0.1166 0.4242 0.069 Uiso 1 1 calc R . .
H9B H 0.4944 0.2419 0.4670 0.069 Uiso 1 1 calc R . .
C10 C 0.5768(6) 0.2111(8) 0.5777(7) 0.076(3) Uani 1 1 d . . .
H10A H 0.6378 0.2238 0.5589 0.091 Uiso 1 1 calc R . .
H10B H 0.5650 0.1499 0.5931 0.091 Uiso 1 1 calc R . .
C11 C 0.5996(6) 0.3133(7) 0.6768(6) 0.066(2) Uani 1 1 d . . .
H11A H 0.6602 0.3284 0.7359 0.080 Uiso 1 1 calc R . .
H11B H 0.6171 0.3759 0.6634 0.080 Uiso 1 1 calc R . .
C12 C 0.5041(6) 0.2975(7) 0.7061(6) 0.060(2) Uani 1 1 d . . .
H12A H 0.5187 0.3647 0.7666 0.072 Uiso 1 1 calc R . .
H12B H 0.4913 0.2399 0.7268 0.072 Uiso 1 1 calc R . .
C13 C 0.4057(5) 0.2669(5) 0.6130(5) 0.0401(16) Uani 1 1 d . . .
H13 H 0.4157 0.3282 0.5967 0.048 Uiso 1 1 calc R . .
C14 C 0.2576(5) 0.2962(5) 0.6332(5) 0.0360(15) Uani 1 1 d . . .
H14 H 0.2779 0.3474 0.6094 0.043 Uiso 1 1 calc R . .
C15 C 0.1658(5) 0.2810(5) 0.6617(5) 0.0322(14) Uani 1 1 d . . .
C16 C 0.1478(5) 0.2224(5) 0.7188(5) 0.0400(16) Uani 1 1 d . . .
H16 H 0.1937 0.1925 0.7363 0.048 Uiso 1 1 calc R . .
C17 C 0.0637(6) 0.2085(6) 0.7491(5) 0.0465(17) Uani 1 1 d . . .
H17 H 0.0522 0.1684 0.7856 0.056 Uiso 1 1 calc R . .
C18 C -0.0050(5) 0.2549(5) 0.7249(5) 0.0422(16) Uani 1 1 d . . .
H18 H -0.0618 0.2461 0.7456 0.051 Uiso 1 1 calc R . .
C19 C 0.0124(5) 0.3129(5) 0.6707(5) 0.0321(14) Uani 1 1 d . . .
C20 C 0.0970(5) 0.3250(5) 0.6344(4) 0.0299(13) Uani 1 1 d . . .
C21 C -0.1226(5) 0.1407(6) 0.1356(5) 0.0495(19) Uani 1 1 d . . .
H21A H -0.1167 0.1276 0.0687 0.074 Uiso 1 1 calc R . .
H21B H -0.1392 0.2021 0.1604 0.074 Uiso 1 1 calc R . .
H21C H -0.1781 0.0767 0.1262 0.074 Uiso 1 1 calc R . .
C22 C -0.1460(5) 0.3388(6) 0.6561(6) 0.0511(19) Uani 1 1 d . . .
H22A H -0.1881 0.2609 0.6138 0.077 Uiso 1 1 calc R . .
H22B H -0.1822 0.3760 0.6312 0.077 Uiso 1 1 calc R . .
H22C H -0.1348 0.3600 0.7294 0.077 Uiso 1 1 calc R . .
C23 C 0.0532(5) 0.3887(5) 0.1962(4) 0.0319(14) Uani 1 1 d . . .
C24 C -0.0083(5) 0.3944(5) 0.1098(5) 0.0388(16) Uani 1 1 d . . .
C25 C 0.0270(6) 0.3913(5) 0.0281(5) 0.0461(18) Uani 1 1 d . . .
H25 H -0.0137 0.3940 -0.0298 0.055 Uiso 1 1 calc R . .
C26 C 0.1199(6) 0.3844(6) 0.0323(6) 0.055(2) Uani 1 1 d . . .
H26 H 0.1430 0.3851 -0.0215 0.066 Uiso 1 1 calc R . .
C27 C 0.1797(6) 0.3764(6) 0.1148(5) 0.0479(18) Uani 1 1 d . . .
H27 H 0.2434 0.3727 0.1174 0.058 Uiso 1 1 calc R . .
C28 C 0.1451(5) 0.3738(5) 0.1937(5) 0.0385(15) Uani 1 1 d . . .
C29 C -0.1123(5) 0.3921(5) 0.0964(5) 0.0409(16) Uani 1 1 d . . .
H29 H -0.1566 0.3718 0.0278 0.049 Uiso 1 1 calc R . .
C30 C -0.2653(5) 0.3889(6) 0.1275(5) 0.0440(17) Uani 1 1 d . . .
H30 H -0.3029 0.3107 0.0755 0.053 Uiso 1 1 calc R . .
C31 C -0.2951(6) 0.4493(6) 0.0688(6) 0.0524(19) Uani 1 1 d . . .
H31A H -0.2760 0.4316 0.0077 0.063 Uiso 1 1 calc R . .
H31B H -0.2555 0.5278 0.1156 0.063 Uiso 1 1 calc R . .
C32 C -0.4139(6) 0.4184(7) 0.0312(6) 0.067(2) Uani 1 1 d . . .
H32A H -0.4282 0.4668 0.0044 0.081 Uiso 1 1 calc R . .
H32B H -0.4523 0.3440 -0.0273 0.081 Uiso 1 1 calc R . .
C33 C -0.4546(6) 0.4252(7) 0.1168(6) 0.063(2) Uani 1 1 d . . .
H33A H -0.5314 0.3949 0.0854 0.076 Uiso 1 1 calc R . .
H33B H -0.4275 0.5017 0.1682 0.076 Uiso 1 1 calc R . .
C34 C -0.4226(5) 0.3637(6) 0.1747(5) 0.0497(19) Uani 1 1 d . . .
H34A H -0.4450 0.3765 0.2336 0.060 Uiso 1 1 calc R . .
H34B H -0.4578 0.2855 0.1261 0.060 Uiso 1 1 calc R . .
C35 C -0.3041(5) 0.4023(6) 0.2161(5) 0.0413(16) Uani 1 1 d . . .
H35 H -0.2727 0.4814 0.2638 0.050 Uiso 1 1 calc R . .
C36 C -0.3113(5) 0.2729(5) 0.2822(5) 0.0397(16) Uani 1 1 d . . .
H36 H -0.3844 0.2485 0.2526 0.048 Uiso 1 1 calc R . .
C37 C -0.2737(5) 0.2116(5) 0.3296(5) 0.0339(14) Uani 1 1 d . . .
C38 C -0.3505(6) 0.1273(6) 0.3321(6) 0.0527(19) Uani 1 1 d . . .
H38 H -0.4202 0.1186 0.3115 0.063 Uiso 1 1 calc R . .
C39 C -0.3259(6) 0.0571(7) 0.3641(7) 0.065(2) Uani 1 1 d . . .
H39 H -0.3778 0.0031 0.3676 0.078 Uiso 1 1 calc R . .
C40 C -0.2229(6) 0.0673(6) 0.3915(6) 0.0538(19) Uani 1 1 d . . .
H40 H -0.2059 0.0187 0.4114 0.065 Uiso 1 1 calc R . .
C41 C -0.1455(5) 0.1494(5) 0.3891(5) 0.0374(15) Uani 1 1 d . . .
C42 C -0.1678(5) 0.2263(5) 0.3619(4) 0.0295(13) Uani 1 1 d . . .
C43 C 0.2919(6) 0.3492(7) 0.2853(6) 0.064(2) Uani 1 1 d . . .
H43A H 0.2777 0.2842 0.2238 0.096 Uiso 1 1 calc R . .
H43B H 0.3206 0.3441 0.3486 0.096 Uiso 1 1 calc R . .
H43C H 0.3422 0.4122 0.2877 0.096 Uiso 1 1 calc R . .
C44 C -0.0190(6) 0.0812(5) 0.4297(6) 0.0484(18) Uani 1 1 d . . .
H44A H -0.0330 0.0801 0.4902 0.073 Uiso 1 1 calc R . .
H44B H 0.0543 0.0973 0.4437 0.073 Uiso 1 1 calc R . .
H44C H -0.0633 0.0108 0.3680 0.073 Uiso 1 1 calc R . .
Er1 Er 0.08445(2) 0.33023(2) 0.39809(2) 0.02951(9) Uani 1 1 d . . .
Er2 Er -0.06677(2) 0.46855(2) 0.359585(19) 0.02487(9) Uani 1 1 d . . .
N1 N 0.3112(4) 0.2410(5) 0.6400(4) 0.0427(14) Uani 1 1 d . . .
N2 N 0.2903(4) 0.1412(4) 0.4270(4) 0.0385(13) Uani 1 1 d D . .
H21 H 0.2550 0.1836 0.4356 0.046 Uiso 1 1 d RD . .
N3 N -0.1502(4) 0.4150(4) 0.1682(4) 0.0339(12) Uani 1 1 d . . .
N4 N -0.2552(4) 0.3558(4) 0.2771(4) 0.0338(12) Uani 1 1 d . . .
N5 N 0.3338(5) 0.5302(5) 0.5202(4) 0.0460(14) Uani 1 1 d . . .
N6 N 0.6805(9) 0.1570(9) 0.8132(9) 0.119(4) Uani 1 1 d . . .
O1 O 0.1479(3) 0.2027(3) 0.3615(3) 0.0376(11) Uani 1 1 d . . .
O2 O -0.0238(3) 0.1641(3) 0.2124(3) 0.0407(11) Uani 1 1 d . . .
O3 O 0.1065(3) 0.3820(3) 0.5797(3) 0.0288(9) Uani 1 1 d . . .
O4 O -0.0458(3) 0.3679(3) 0.6471(3) 0.0344(10) Uani 1 1 d . . .
O5 O 0.0270(3) 0.3920(3) 0.2777(3) 0.0317(9) Uani 1 1 d . . .
O6 O 0.1940(4) 0.3600(4) 0.2786(3) 0.0455(12) Uani 1 1 d . . .
O7 O -0.0894(3) 0.3044(3) 0.3632(3) 0.0283(9) Uani 1 1 d . . .
O8 O -0.0414(3) 0.1643(3) 0.4107(3) 0.0355(10) Uani 1 1 d . . .
O9 O 0.2690(3) 0.4361(4) 0.5010(3) 0.0404(11) Uani 1 1 d . . .
O10 O 0.2996(4) 0.5886(4) 0.4931(4) 0.0586(14) Uani 1 1 d . . .
O11 O 0.4287(4) 0.5613(5) 0.5683(5) 0.0835(19) Uani 1 1 d . . .
O12 O 0.0902(3) 0.5049(3) 0.4847(3) 0.0254(9) Uani 1 1 d D . .
H121 H 0.1517 0.5441 0.4925 0.031 Uiso 1 1 d RD . .
O13 O 0.7574(9) 0.2065(9) 0.8013(9) 0.159(4) Uani 1 1 d . . .
O14 O 0.6618(12) 0.1968(13) 0.8801(10) 0.322(12) Uani 1 1 d . . .
O15 O 0.6191(8) 0.0681(8) 0.7454(9) 0.189(5) Uani 1 1 d . . .
O16A O 0.3896(18) 0.0510(19) 0.0808(18) 0.112(7) Uiso 0.33 1 d P . .
O17A O 0.313(2) 0.152(2) -0.111(2) 0.134(9) Uiso 0.33 1 d P . .
O17B O 0.305(2) 0.164(2) 0.038(2) 0.141(9) Uiso 0.33 1 d P . .
O16B O 0.355(2) 0.099(2) 0.015(2) 0.137(9) Uiso 0.33 1 d P . .
O17C O 0.373(2) 0.102(2) -0.079(2) 0.137(9) Uiso 0.33 1 d P . .
O16C O 0.357(2) 0.098(2) 0.146(2) 0.137(9) Uiso 0.33 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
C1 O1 1.319(7) . ?
C1 C2 1.407(8) . ?
C1 C6 1.413(8) . ?
C2 C3 1.376(8) . ?
C2 O2 1.383(7) . ?
C3 C4 1.394(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.372(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.411(8) . ?
C5 H5 0.9300 . ?
C6 C7 1.429(9) . ?
C7 N2 1.292(8) . ?
C7 H7 0.9300 . ?
C8 N2 1.480(8) . ?
C8 C13 1.523(9) . ?
C8 C9 1.523(9) . ?
C8 H8 0.9800 . ?
C9 C10 1.498(10) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.527(11) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.516(10) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.521(9) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N1 1.488(8) . ?
C13 H13 0.9800 . ?
C14 N1 1.284(7) . ?
C14 C15 1.461(8) . ?
C14 H14 0.9300 . ?
C15 C20 1.391(8) . ?
C15 C16 1.407(8) . ?
C16 C17 1.373(9) . ?
C16 H16 0.9300 . ?
C17 C18 1.405(9) . ?
C17 H17 0.9300 . ?
C18 C19 1.362(8) . ?
C18 H18 0.9300 . ?
C19 O4 1.389(7) . ?
C19 C20 1.433(8) . ?
C20 O3 1.345(7) . ?
C21 O2 1.437(7) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 O4 1.429(7) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 O5 1.328(6) . ?
C23 C24 1.405(8) . ?
C23 C28 1.412(8) . ?
C24 C25 1.402(8) . ?
C24 C29 1.453(9) . ?
C25 C26 1.362(10) . ?
C25 H25 0.9300 . ?
C26 C27 1.371(10) . ?
C26 H26 0.9300 . ?
C27 C28 1.374(9) . ?
C27 H27 0.9300 . ?
C28 O6 1.391(7) . ?
C29 N3 1.287(7) . ?
C29 H29 0.9300 . ?
C30 N3 1.492(8) . ?
C30 C35 1.508(9) . ?
C30 C31 1.514(9) . ?
C30 H30 0.9800 . ?
C31 C32 1.528(10) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C33 1.493(10) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 C34 1.530(10) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 C35 1.507(9) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 N4 1.476(8) . ?
C35 H35 0.9800 . ?
C36 N4 1.268(8) . ?
C36 C37 1.459(9) . ?
C36 H36 0.9300 . ?
C37 C38 1.397(9) . ?
C37 C42 1.406(8) . ?
C38 C39 1.367(10) . ?
C38 H38 0.9300 . ?
C39 C40 1.387(10) . ?
C39 H39 0.9300 . ?
C40 C41 1.378(9) . ?
C40 H40 0.9300 . ?
C41 O8 1.387(7) . ?
C41 C42 1.411(8) . ?
C42 O7 1.324(7) . ?
C43 O6 1.452(8) . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 O8 1.441(7) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
Er1 O1 2.260(4) . ?
Er1 O7 2.313(4) . ?
Er1 O5 2.346(4) . ?
Er1 O12 2.354(3) . ?
Er1 O9 2.364(4) . ?
Er1 O3 2.399(4) . ?
Er1 O2 2.559(4) . ?
Er1 O8 2.635(4) . ?
Er1 O6 2.687(4) . ?
Er1 Er2 3.4665(4) . ?
Er1 Er2 3.8220(4) 2_566 ?
Er2 O5 2.291(4) . ?
Er2 O12 2.301(3) 2_566 ?
Er2 O12 2.308(4) . ?
Er2 O7 2.327(4) . ?
Er2 O3 2.332(4) 2_566 ?
Er2 N4 2.403(5) . ?
Er2 N3 2.478(5) . ?
Er2 O4 2.484(4) 2_566 ?
Er2 Er2 3.7232(6) 2_566 ?
Er2 Er1 3.8220(4) 2_566 ?
N2 H21 0.9050 . ?
N5 O11 1.224(7) . ?
N5 O10 1.235(7) . ?
N5 O9 1.277(7) . ?
N6 O14 1.087(12) . ?
N6 O15 1.176(11) . ?
N6 O13 1.214(13) . ?
O3 Er2 2.332(4) 2_566 ?
O4 Er2 2.484(4) 2_566 ?
O12 Er2 2.301(3) 2_566 ?
O12 H121 0.8467 . ?
O16A O16C 1.24(3) . ?
O16A O16B 1.46(3) . ?
O17A O17C 1.40(3) . ?
O17B O16B 1.36(3) . ?
O16B O17C 1.47(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 120.4(5) . . ?
O1 C1 C6 122.2(6) . . ?
C2 C1 C6 117.4(5) . . ?
C3 C2 O2 125.0(6) . . ?
C3 C2 C1 121.9(6) . . ?
O2 C2 C1 113.1(5) . . ?
C2 C3 C4 120.1(6) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
C5 C4 C3 119.8(6) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 120.7(6) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C5 C6 C1 120.0(6) . . ?
C5 C6 C7 119.3(6) . . ?
C1 C6 C7 120.7(5) . . ?
N2 C7 C6 122.4(6) . . ?
N2 C7 H7 118.8 . . ?
C6 C7 H7 118.8 . . ?
N2 C8 C13 107.6(5) . . ?
N2 C8 C9 111.1(6) . . ?
C13 C8 C9 111.0(6) . . ?
N2 C8 H8 109.0 . . ?
C13 C8 H8 109.0 . . ?
C9 C8 H8 109.0 . . ?
C10 C9 C8 110.0(6) . . ?
C10 C9 H9A 109.7 . . ?
C8 C9 H9A 109.7 . . ?
C10 C9 H9B 109.7 . . ?
C8 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
C9 C10 C11 111.0(7) . . ?
C9 C10 H10A 109.4 . . ?
C11 C10 H10A 109.4 . . ?
C9 C10 H10B 109.4 . . ?
C11 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
C12 C11 C10 110.7(7) . . ?
C12 C11 H11A 109.5 . . ?
C10 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 108.1 . . ?
C11 C12 C13 111.1(6) . . ?
C11 C12 H12A 109.4 . . ?
C13 C12 H12A 109.4 . . ?
C11 C12 H12B 109.4 . . ?
C13 C12 H12B 109.4 . . ?
H12A C12 H12B 108.0 . . ?
N1 C13 C12 110.0(6) . . ?
N1 C13 C8 107.7(5) . . ?
C12 C13 C8 110.2(5) . . ?
N1 C13 H13 109.6 . . ?
C12 C13 H13 109.6 . . ?
C8 C13 H13 109.6 . . ?
N1 C14 C15 122.0(6) . . ?
N1 C14 H14 119.0 . . ?
C15 C14 H14 119.0 . . ?
C20 C15 C16 119.8(6) . . ?
C20 C15 C14 120.8(6) . . ?
C16 C15 C14 119.4(5) . . ?
C17 C16 C15 121.0(6) . . ?
C17 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
C16 C17 C18 120.1(6) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C19 C18 C17 119.3(6) . . ?
C19 C18 H18 120.4 . . ?
C17 C18 H18 120.4 . . ?
C18 C19 O4 125.0(5) . . ?
C18 C19 C20 121.9(6) . . ?
O4 C19 C20 113.1(5) . . ?
O3 C20 C15 124.6(5) . . ?
O3 C20 C19 117.5(5) . . ?
C15 C20 C19 117.8(5) . . ?
O2 C21 H21A 109.5 . . ?
O2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O4 C22 H22A 109.5 . . ?
O4 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
O4 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O5 C23 C24 123.3(5) . . ?
O5 C23 C28 118.4(5) . . ?
C24 C23 C28 118.2(5) . . ?
C25 C24 C23 118.8(6) . . ?
C25 C24 C29 118.4(6) . . ?
C23 C24 C29 122.4(6) . . ?
C26 C25 C24 121.1(6) . . ?
C26 C25 H25 119.4 . . ?
C24 C25 H25 119.4 . . ?
C25 C26 C27 120.8(7) . . ?
C25 C26 H26 119.6 . . ?
C27 C26 H26 119.6 . . ?
C26 C27 C28 119.8(7) . . ?
C26 C27 H27 120.1 . . ?
C28 C27 H27 120.1 . . ?
C27 C28 O6 126.2(6) . . ?
C27 C28 C23 121.0(6) . . ?
O6 C28 C23 112.8(5) . . ?
N3 C29 C24 127.6(6) . . ?
N3 C29 H29 116.2 . . ?
C24 C29 H29 116.2 . . ?
N3 C30 C35 110.1(5) . . ?
N3 C30 C31 115.0(6) . . ?
C35 C30 C31 112.3(6) . . ?
N3 C30 H30 106.3 . . ?
C35 C30 H30 106.3 . . ?
C31 C30 H30 106.3 . . ?
C30 C31 C32 111.2(6) . . ?
C30 C31 H31A 109.4 . . ?
C32 C31 H31A 109.4 . . ?
C30 C31 H31B 109.4 . . ?
C32 C31 H31B 109.4 . . ?
H31A C31 H31B 108.0 . . ?
C33 C32 C31 113.4(6) . . ?
C33 C32 H32A 108.9 . . ?
C31 C32 H32A 108.9 . . ?
C33 C32 H32B 108.9 . . ?
C31 C32 H32B 108.9 . . ?
H32A C32 H32B 107.7 . . ?
C32 C33 C34 112.9(6) . . ?
C32 C33 H33A 109.0 . . ?
C34 C33 H33A 109.0 . . ?
C32 C33 H33B 109.0 . . ?
C34 C33 H33B 109.0 . . ?
H33A C33 H33B 107.8 . . ?
C35 C34 C33 110.2(6) . . ?
C35 C34 H34A 109.6 . . ?
C33 C34 H34A 109.6 . . ?
C35 C34 H34B 109.6 . . ?
C33 C34 H34B 109.6 . . ?
H34A C34 H34B 108.1 . . ?
N4 C35 C34 119.5(6) . . ?
N4 C35 C30 106.5(5) . . ?
C34 C35 C30 111.3(5) . . ?
N4 C35 H35 106.2 . . ?
C34 C35 H35 106.2 . . ?
C30 C35 H35 106.2 . . ?
N4 C36 C37 127.2(6) . . ?
N4 C36 H36 116.4 . . ?
C37 C36 H36 116.4 . . ?
C38 C37 C42 119.6(6) . . ?
C38 C37 C36 116.8(6) . . ?
C42 C37 C36 123.3(6) . . ?
C39 C38 C37 121.7(7) . . ?
C39 C38 H38 119.1 . . ?
C37 C38 H38 119.1 . . ?
C38 C39 C40 119.4(7) . . ?
C38 C39 H39 120.3 . . ?
C40 C39 H39 120.3 . . ?
C41 C40 C39 120.2(7) . . ?
C41 C40 H40 119.9 . . ?
C39 C40 H40 119.9 . . ?
C40 C41 O8 124.9(6) . . ?
C40 C41 C42 121.4(6) . . ?
O8 C41 C42 113.7(6) . . ?
O7 C42 C37 124.0(5) . . ?
O7 C42 C41 118.3(5) . . ?
C37 C42 C41 117.6(6) . . ?
O6 C43 H43A 109.5 . . ?
O6 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
O6 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
O8 C44 H44A 109.5 . . ?
O8 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
O8 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O1 Er1 O7 128.68(14) . . ?
O1 Er1 O5 123.41(13) . . ?
O7 Er1 O5 68.52(14) . . ?
O1 Er1 O12 156.84(14) . . ?
O7 Er1 O12 73.24(13) . . ?
O5 Er1 O12 67.82(12) . . ?
O1 Er1 O9 77.28(15) . . ?
O7 Er1 O9 151.31(14) . . ?
O5 Er1 O9 109.98(15) . . ?
O12 Er1 O9 79.75(14) . . ?
O1 Er1 O3 102.53(14) . . ?
O7 Er1 O3 86.59(13) . . ?
O5 Er1 O3 133.91(12) . . ?
O12 Er1 O3 68.09(12) . . ?
O9 Er1 O3 74.33(14) . . ?
O1 Er1 O2 65.52(13) . . ?
O7 Er1 O2 75.16(13) . . ?
O5 Er1 O2 71.73(13) . . ?
O12 Er1 O2 135.39(12) . . ?
O9 Er1 O2 132.80(14) . . ?
O3 Er1 O2 139.74(14) . . ?
O1 Er1 O8 73.14(14) . . ?
O7 Er1 O8 62.99(13) . . ?
O5 Er1 O8 123.81(13) . . ?
O12 Er1 O8 119.60(12) . . ?
O9 Er1 O8 126.20(14) . . ?
O3 Er1 O8 69.74(13) . . ?
O2 Er1 O8 69.99(14) . . ?
O1 Er1 O6 72.15(15) . . ?
O7 Er1 O6 126.99(13) . . ?
O5 Er1 O6 61.41(13) . . ?
O12 Er1 O6 101.64(13) . . ?
O9 Er1 O6 67.61(14) . . ?
O3 Er1 O6 141.84(14) . . ?
O2 Er1 O6 73.87(14) . . ?
O8 Er1 O6 137.56(13) . . ?
O1 Er1 Er2 159.88(10) . . ?
O7 Er1 Er2 41.83(9) . . ?
O5 Er1 Er2 41.01(9) . . ?
O12 Er1 Er2 41.46(9) . . ?
O9 Er1 Er2 117.61(11) . . ?
O3 Er1 Er2 94.93(9) . . ?
O2 Er1 Er2 94.64(9) . . ?
O8 Er1 Er2 104.31(9) . . ?
O6 Er1 Er2 100.01(9) . . ?
O1 Er1 Er2 137.64(10) . 2_566 ?
O7 Er1 Er2 69.54(9) . 2_566 ?
O5 Er1 Er2 98.42(8) . 2_566 ?
O12 Er1 Er2 34.36(9) . 2_566 ?
O9 Er1 Er2 82.74(10) . 2_566 ?
O3 Er1 Er2 35.53(9) . 2_566 ?
O2 Er1 Er2 144.46(10) . 2_566 ?
O8 Er1 Er2 90.02(9) . 2_566 ?
O6 Er1 Er2 132.34(10) . 2_566 ?
Er2 Er1 Er2 61.209(9) . 2_566 ?
O5 Er2 O12 134.02(13) . 2_566 ?
O5 Er2 O12 69.52(13) . . ?
O12 Er2 O12 72.24(14) 2_566 . ?
O5 Er2 O7 69.20(13) . . ?
O12 Er2 O7 76.46(13) 2_566 . ?
O12 Er2 O7 73.83(13) . . ?
O5 Er2 O3 147.49(14) . 2_566 ?
O12 Er2 O3 70.11(13) 2_566 2_566 ?
O12 Er2 O3 109.27(13) . 2_566 ?
O7 Er2 O3 143.02(13) . 2_566 ?
O5 Er2 N4 114.05(15) . . ?
O12 Er2 N4 83.72(15) 2_566 . ?
O12 Er2 N4 143.73(16) . . ?
O7 Er2 N4 74.40(15) . . ?
O3 Er2 N4 86.49(15) 2_566 . ?
O5 Er2 N3 73.41(15) . . ?
O12 Er2 N3 146.77(15) 2_566 . ?
O12 Er2 N3 140.68(14) . . ?
O7 Er2 N3 104.80(15) . . ?
O3 Er2 N3 95.03(14) 2_566 . ?
N4 Er2 N3 65.35(17) . . ?
O5 Er2 O4 82.53(13) . 2_566 ?
O12 Er2 O4 117.73(13) 2_566 2_566 ?
O12 Er2 O4 83.87(13) . 2_566 ?
O7 Er2 O4 148.59(13) . 2_566 ?
O3 Er2 O4 65.27(13) 2_566 2_566 ?
N4 Er2 O4 132.03(15) . 2_566 ?
N3 Er2 O4 78.78(15) . 2_566 ?
O5 Er2 Er1 42.21(9) . . ?
O12 Er2 Er1 91.91(9) 2_566 . ?
O12 Er2 Er1 42.47(9) . . ?
O7 Er2 Er1 41.51(9) . . ?
O3 Er2 Er1 151.37(9) 2_566 . ?
N4 Er2 Er1 114.33(12) . . ?
N3 Er2 Er1 111.17(11) . . ?
O4 Er2 Er1 107.59(9) 2_566 . ?
O5 Er2 Er2 102.27(9) . 2_566 ?
O12 Er2 Er2 36.18(9) 2_566 2_566 ?
O12 Er2 Er2 36.05(9) . 2_566 ?
O7 Er2 Er2 71.50(9) . 2_566 ?
O3 Er2 Er2 89.68(9) 2_566 2_566 ?
N4 Er2 Er2 115.61(12) . 2_566 ?
N3 Er2 Er2 175.26(11) . 2_566 ?
O4 Er2 Er2 102.79(9) 2_566 2_566 ?
Er1 Er2 Er2 64.108(9) . 2_566 ?
O5 Er2 Er1 151.50(10) . 2_566 ?
O12 Er2 Er1 35.26(9) 2_566 2_566 ?
O12 Er2 Er1 83.19(8) . 2_566 ?
O7 Er2 Er1 111.71(9) . 2_566 ?
O3 Er2 Er1 36.72(9) 2_566 2_566 ?
N4 Er2 Er1 92.71(11) . 2_566 ?
N3 Er2 Er1 130.03(11) . 2_566 ?
O4 Er2 Er1 86.65(9) 2_566 2_566 ?
Er1 Er2 Er1 118.791(9) . 2_566 ?
Er2 Er2 Er1 54.682(8) 2_566 2_566 ?
C14 N1 C13 117.1(6) . . ?
C7 N2 C8 124.9(5) . . ?
C7 N2 H21 112.3 . . ?
C8 N2 H21 122.0 . . ?
C29 N3 C30 115.2(5) . . ?
C29 N3 Er2 128.7(4) . . ?
C30 N3 Er2 115.3(4) . . ?
C36 N4 C35 121.3(5) . . ?
C36 N4 Er2 131.0(4) . . ?
C35 N4 Er2 107.6(4) . . ?
O11 N5 O10 121.8(7) . . ?
O11 N5 O9 118.5(6) . . ?
O10 N5 O9 119.7(6) . . ?
O14 N6 O15 119.0(16) . . ?
O14 N6 O13 121.3(14) . . ?
O15 N6 O13 119.2(13) . . ?
C1 O1 Er1 125.3(4) . . ?
C2 O2 C21 117.0(5) . . ?
C2 O2 Er1 115.7(3) . . ?
C21 O2 Er1 127.0(3) . . ?
C20 O3 Er2 114.1(3) . 2_566 ?
C20 O3 Er1 132.7(3) . . ?
Er2 O3 Er1 107.75(15) 2_566 . ?
C19 O4 C22 116.6(5) . . ?
C19 O4 Er2 110.8(3) . 2_566 ?
C22 O4 Er2 130.7(4) . 2_566 ?
C23 O5 Er2 135.0(3) . . ?
C23 O5 Er1 128.0(3) . . ?
Er2 O5 Er1 96.78(13) . . ?
C28 O6 C43 116.6(5) . . ?
C28 O6 Er1 116.2(4) . . ?
C43 O6 Er1 126.7(4) . . ?
C42 O7 Er1 128.5(3) . . ?
C42 O7 Er2 134.2(3) . . ?
Er1 O7 Er2 96.66(14) . . ?
C41 O8 C44 114.7(5) . . ?
C41 O8 Er1 116.4(3) . . ?
C44 O8 Er1 128.7(4) . . ?
N5 O9 Er1 132.4(4) . . ?
Er2 O12 Er2 107.76(14) 2_566 . ?
Er2 O12 Er1 110.38(15) 2_566 . ?
Er2 O12 Er1 96.07(13) . . ?
Er2 O12 H121 115.3 2_566 . ?
Er2 O12 H121 125.1 . . ?
Er1 O12 H121 99.1 . . ?
O16C O16A O16B 90(2) . . ?
O17B O16B O16A 123(3) . . ?
O17B O16B O17C 105(3) . . ?
O16A O16B O17C 132(3) . . ?
O17A O17C O16B 104(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
N2 H21 O1 0.90 1.82 2.594(6) 141.9 .
O12 H121 O10 0.85 2.03 2.842(6) 161.0 .
O12 H121 N5 0.85 2.64 3.306(7) 136.5 .

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.290
_refine_diff_density_min         -0.838
_refine_diff_density_rms         0.122
