# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

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

data_1
_database_code_depnum_ccdc_archive 'CCDC 1404026'
_audit_update_record             
;
2015-06-01 deposited with the CCDC.
2015-12-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C32 H24 Eu N8 O12), 2(C6 H16 N), 3(C H4 O)'
_chemical_formula_sum            'C79 H92 Eu2 N18 O27'
_chemical_formula_weight         2029.62

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'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.5131(6)
_cell_length_b                   12.5800(6)
_cell_length_c                   15.4397(7)
_cell_angle_alpha                70.3150(10)
_cell_angle_beta                 74.862(2)
_cell_angle_gamma                71.875(2)
_cell_volume                     2141.39(18)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5812
_cell_measurement_theta_min      3.31
_cell_measurement_theta_max      25.04

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_F_000             1034
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.541
_shelx_estimated_absorpt_T_min   0.655
_shelx_estimated_absorpt_T_max   0.748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.670
_exptl_absorpt_correction_T_max  0.738
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19072
_diffrn_reflns_av_unetI/netI     0.0881
_diffrn_reflns_av_R_equivalents  0.0677
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.066
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measured_fraction_theta_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_point_group_measured_fraction_full 0.982
_reflns_number_total             8089
_reflns_number_gt                6086
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0569P)²+0.9878P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8089
_refine_ls_number_parameters     574
_refine_ls_number_restraints     95
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0490
_refine_ls_wR_factor_ref         0.1179
_refine_ls_wR_factor_gt          0.1046
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.027
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu1 Eu 0.23077(2) 0.81212(2) 0.26980(2) 0.02403(6) Uani 1 1 d . . . . .
C1 C -0.0093(4) 0.7449(4) 0.2595(3) 0.0316(11) Uani 1 1 d . . . . .
C2 C -0.1132(4) 0.7146(4) 0.3133(3) 0.0392(11) Uani 1 1 d . U . . .
C3 C -0.2020(4) 0.7203(4) 0.2729(4) 0.0415(13) Uani 1 1 d . . . . .
H3A H -0.2692 0.6995 0.3119 0.050 Uiso 1 1 calc R U . . .
C4 C -0.1952(5) 0.7554(4) 0.1779(4) 0.0457(13) Uani 1 1 d . . . . .
H4A H -0.2546 0.7547 0.1505 0.055 Uiso 1 1 calc R U . . .
C5 C -0.0995(4) 0.7918(4) 0.1229(3) 0.0402(13) Uani 1 1 d . . . . .
H5A H -0.0956 0.8195 0.0571 0.048 Uiso 1 1 calc R U . . .
C6 C -0.0085(4) 0.7895(4) 0.1604(3) 0.0312(11) Uani 1 1 d . . . . .
C7 C 0.0839(4) 0.8370(4) 0.0953(3) 0.0312(11) Uani 1 1 d . . . . .
H7A H 0.0787 0.8599 0.0310 0.037 Uiso 1 1 calc R U . . .
C8 C 0.2479(4) 0.9059(4) 0.0343(3) 0.0300(11) Uani 1 1 d . . . . .
H8A H 0.2124 0.9365 -0.0223 0.036 Uiso 1 1 calc R U . . .
H8B H 0.3199 0.8473 0.0225 0.036 Uiso 1 1 calc R U . . .
C9 C 0.2731(4) 1.0046(4) 0.0550(3) 0.0311(11) Uani 1 1 d . . . . .
H9A H 0.3244 1.0424 0.0008 0.037 Uiso 1 1 calc R U . . .
H9B H 0.2012 1.0637 0.0657 0.037 Uiso 1 1 calc R U . . .
C10 C 0.4112(4) 0.9986(4) 0.1345(3) 0.0294(11) Uani 1 1 d . . . . .
H10A H 0.4342 1.0515 0.0770 0.035 Uiso 1 1 calc R U . . .
C11 C 0.4762(4) 0.9723(3) 0.2075(3) 0.0254(10) Uani 1 1 d . . . . .
C12 C 0.5627(4) 1.0289(4) 0.1862(3) 0.0348(12) Uani 1 1 d . . . . .
H12A H 0.5776 1.0789 0.1250 0.042 Uiso 1 1 calc R U . . .
C13 C 0.6283(4) 1.0150(4) 0.2508(3) 0.0414(13) Uani 1 1 d . . . . .
H13A H 0.6869 1.0551 0.2345 0.050 Uiso 1 1 calc R U . . .
C14 C 0.6067(4) 0.9421(4) 0.3390(3) 0.0355(12) Uani 1 1 d . . . . .
H14A H 0.6489 0.9336 0.3849 0.043 Uiso 1 1 calc R U . . .
C15 C 0.5246(4) 0.8816(4) 0.3610(3) 0.0288(11) Uani 1 1 d . . . . .
C16 C 0.4512(4) 0.8947(4) 0.2980(3) 0.0246(10) Uani 1 1 d . . . . .
C17 C 0.4747(4) 0.6220(3) 0.2181(3) 0.0255(10) Uani 1 1 d . . . . .
C18 C 0.5796(4) 0.6124(4) 0.1524(3) 0.0285(11) Uani 1 1 d . . . . .
C19 C 0.6849(4) 0.5454(4) 0.1749(3) 0.0347(12) Uani 1 1 d . . . . .
H19A H 0.7515 0.5457 0.1280 0.042 Uiso 1 1 calc R U . . .
C20 C 0.6931(4) 0.4788(4) 0.2645(3) 0.0394(13) Uani 1 1 d . . . . .
H20A H 0.7644 0.4305 0.2803 0.047 Uiso 1 1 calc R U . . .
C21 C 0.5950(4) 0.4833(4) 0.3320(3) 0.0345(12) Uani 1 1 d . . . . .
H21A H 0.6006 0.4360 0.3941 0.041 Uiso 1 1 calc R U . . .
C22 C 0.4892(4) 0.5538(4) 0.3127(3) 0.0274(10) Uani 1 1 d . . . . .
C23 C 0.3924(4) 0.5524(4) 0.3905(3) 0.0295(11) Uani 1 1 d . . . . .
H23A H 0.4056 0.4940 0.4473 0.035 Uiso 1 1 calc R U . . .
C24 C 0.2123(4) 0.6035(4) 0.4793(3) 0.0357(12) Uani 1 1 d . . . . .
H24A H 0.2476 0.5369 0.5279 0.043 Uiso 1 1 calc R U . . .
H24B H 0.1437 0.5874 0.4708 0.043 Uiso 1 1 calc R U . . .
C25 C 0.1793(4) 0.7142(4) 0.5088(3) 0.0364(12) Uani 1 1 d . . . . .
H25A H 0.1249 0.7056 0.5687 0.044 Uiso 1 1 calc R U . . .
H25B H 0.2479 0.7295 0.5179 0.044 Uiso 1 1 calc R U . . .
C26 C 0.0259(4) 0.8707(4) 0.4600(3) 0.0378(12) Uani 1 1 d . . . . .
H26A H -0.0068 0.8475 0.5242 0.045 Uiso 1 1 calc R U . . .
C27 C -0.0443(4) 0.9686(4) 0.4015(3) 0.0378(12) Uani 1 1 d . . . . .
C28 C -0.1578(5) 1.0083(5) 0.4397(4) 0.0551(15) Uani 1 1 d . . . . .
H28A H -0.1850 0.9693 0.5022 0.066 Uiso 1 1 calc R U . . .
C29 C -0.2332(5) 1.1018(5) 0.3911(4) 0.0620(17) Uani 1 1 d . . . . .
H29A H -0.3104 1.1258 0.4195 0.074 Uiso 1 1 calc R U . . .
C30 C -0.1939(5) 1.1584(5) 0.3017(4) 0.0563(15) Uani 1 1 d . . . . .
H30A H -0.2441 1.2223 0.2667 0.068 Uiso 1 1 calc R U . . .
C31 C -0.0810(5) 1.1226(4) 0.2618(3) 0.0444(13) Uani 1 1 d . . . . .
C32 C -0.0013(4) 1.0235(4) 0.3081(3) 0.0335(11) Uani 1 1 d . . . . .
C33 C 0.2551(5) 0.2732(4) 0.2186(4) 0.0554(14) Uani 1 1 d . U . . .
H33A H 0.3290 0.2504 0.1783 0.067 Uiso 1 1 calc R U . . .
H33B H 0.1943 0.2974 0.1808 0.067 Uiso 1 1 calc R U . . .
C34 C 0.2362(7) 0.1698(5) 0.2979(6) 0.099(3) Uani 1 1 d . . . . .
H34A H 0.2373 0.1067 0.2737 0.119 Uiso 1 1 calc R U . . .
H34B H 0.1620 0.1906 0.3372 0.119 Uiso 1 1 calc R U . . .
H34C H 0.2968 0.1439 0.3352 0.119 Uiso 1 1 calc R U . . .
C35 C 0.1434(6) 0.4214(5) 0.3054(4) 0.0600(16) Uani 1 1 d . U . . .
H35A H 0.1340 0.3642 0.3675 0.072 Uiso 1 1 calc R U . . .
H35B H 0.1467 0.4941 0.3150 0.072 Uiso 1 1 calc R U . . .
C36 C 0.0415(6) 0.4458(6) 0.2620(6) 0.091(3) Uani 1 1 d . . . . .
H36A H -0.0278 0.4751 0.3030 0.109 Uiso 1 1 calc R U . . .
H36B H 0.0368 0.3740 0.2531 0.109 Uiso 1 1 calc R U . . .
H36C H 0.0488 0.5045 0.2014 0.109 Uiso 1 1 calc R U . . .
C37 C 0.3506(6) 0.3543(6) 0.2948(4) 0.0679(16) Uani 1 1 d . U . . .
H37A H 0.3448 0.2900 0.3530 0.081 Uiso 1 1 calc R U . . .
H37B H 0.3434 0.4252 0.3125 0.081 Uiso 1 1 calc R U . . .
C38 C 0.4661(6) 0.3247(5) 0.2363(5) 0.0792(19) Uani 1 1 d . . . . .
H38A H 0.5254 0.3118 0.2720 0.095 Uiso 1 1 calc R U . . .
H38B H 0.4737 0.3891 0.1795 0.095 Uiso 1 1 calc R U . . .
H38C H 0.4746 0.2539 0.2192 0.095 Uiso 1 1 calc R U . . .
N1 N 0.1706(3) 0.8517(3) 0.1138(2) 0.0265(9) Uani 1 1 d . . . . .
N2 N 0.3273(3) 0.9596(3) 0.1377(2) 0.0285(9) Uani 1 1 d . . . . .
N3 N 0.2940(3) 0.6194(3) 0.3909(2) 0.0272(9) Uani 1 1 d . . . . .
N4 N 0.1263(3) 0.8117(3) 0.4361(2) 0.0326(9) Uani 1 1 d . . . . .
N5 N -0.1313(4) 0.6808(4) 0.4135(3) 0.0521(11) Uani 1 1 d . U . . .
O5 O -0.0494(4) 0.6286(5) 0.4530(3) 0.0987(16) Uani 1 1 d . U . . .
O6 O -0.2269(4) 0.6935(4) 0.4591(3) 0.0837(16) Uani 1 1 d . U . . .
N6 N 0.5105(3) 0.8029(4) 0.4534(3) 0.0382(10) Uani 1 1 d . . . . .
N7 N 0.5785(4) 0.6818(3) 0.0550(3) 0.0394(11) Uani 1 1 d . . . . .
O9 O 0.6607(4) 0.7231(4) 0.0137(3) 0.0661(12) Uani 1 1 d . . . . .
O10 O 0.4983(3) 0.6957(4) 0.0183(2) 0.0563(11) Uani 1 1 d . . . . .
N8 N -0.0453(5) 1.1885(5) 0.1675(3) 0.0703(14) Uani 1 1 d . U . . .
O11 O 0.0507(4) 1.2084(4) 0.1434(3) 0.0851(15) Uani 1 1 d . U . . .
O12 O -0.1102(5) 1.2248(5) 0.1125(4) 0.1105(16) Uani 1 1 d . U . . .
N9 N 0.2557(4) 0.3742(3) 0.2474(3) 0.0410(10) Uani 1 1 d . U . . .
H9C H 0.2651 0.4317 0.1944 0.049 Uiso 1 1 d R U . . .
O1 O 0.0760(3) 0.7352(3) 0.2954(2) 0.0360(8) Uani 1 1 d . . . . .
O2 O 0.3687(3) 0.8458(3) 0.32330(19) 0.0302(7) Uani 1 1 d . . . . .
O3 O 0.3781(3) 0.6846(3) 0.19592(19) 0.0310(8) Uani 1 1 d . . . . .
O4 O 0.1000(3) 0.9886(3) 0.2663(2) 0.0369(8) Uani 1 1 d . . . . .
O7 O 0.4873(4) 0.7111(3) 0.4638(3) 0.0645(11) Uani 1 1 d . . . . .
O8 O 0.5226(3) 0.8289(4) 0.5194(2) 0.0587(11) Uani 1 1 d . . . . .
O13 O 0.2893(4) 0.5714(3) 0.1106(3) 0.0702(12) Uani 1 1 d . . . . .
H13B H 0.3221 0.6135 0.1212 0.084 Uiso 1 1 calc R U . . .
C39 C 0.3018(6) 0.5912(5) 0.0154(4) 0.0678(18) Uani 1 1 d . . . . .
H39A H 0.3742 0.5448 -0.0066 0.081 Uiso 1 1 d R U . . .
H39B H 0.2415 0.5706 0.0017 0.081 Uiso 1 1 d R U . . .
H39C H 0.2987 0.6721 -0.0152 0.081 Uiso 1 1 d R U . . .
C40 C 0.0000 0.5000 0.0000 0.1510(19) Uani 1 2 d DS U P . .
H40A H -0.0309 0.4816 -0.0424 0.181 Uiso 0.5 1 d R U P . .
H40B H -0.0469 0.4852 0.0608 0.181 Uiso 0.5 1 d R U P . .
H40C H 0.0015 0.5807 -0.0221 0.181 Uiso 0.5 1 d R U P . .
O14 O 0.1103(5) 0.4318(10) 0.0065(10) 0.172(4) Uani 0.5 1 d D U P . .
H14D H 0.1101 0.3921 0.0632 0.207 Uiso 0.5 1 d R U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 O2 2.297(3) . ?
Eu1 O4 2.306(3) . ?
Eu1 O1 2.313(3) . ?
Eu1 O3 2.360(3) . ?
Eu1 N3 2.554(3) . ?
Eu1 N1 2.554(3) . ?
Eu1 N4 2.558(3) . ?
Eu1 N2 2.572(3) . ?
C1 O1 1.282(5) . ?
C1 C2 1.434(7) . ?
C1 C6 1.440(6) . ?
C2 C3 1.384(7) . ?
C2 N5 1.434(6) . ?
C3 C4 1.370(7) . ?
C3 H3A 0.9500 . ?
C4 C5 1.384(7) . ?
C4 H4A 0.9500 . ?
C5 C6 1.394(7) . ?
C5 H5A 0.9500 . ?
C6 C7 1.457(6) . ?
C7 N1 1.271(6) . ?
C7 H7A 0.9500 . ?
C8 N1 1.460(5) . ?
C8 C9 1.519(7) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 N2 1.462(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 N2 1.274(6) . ?
C10 C11 1.449(6) . ?
C10 H10A 0.9500 . ?
C11 C12 1.387(6) . ?
C11 C16 1.430(5) . ?
C12 C13 1.386(7) . ?
C12 H12A 0.9500 . ?
C13 C14 1.374(6) . ?
C13 H13A 0.9500 . ?
C14 C15 1.372(7) . ?
C14 H14A 0.9500 . ?
C15 N6 1.439(5) . ?
C15 C16 1.443(6) . ?
C16 O2 1.272(5) . ?
C17 O3 1.281(5) . ?
C17 C18 1.434(6) . ?
C17 C22 1.449(5) . ?
C18 C19 1.386(6) . ?
C18 N7 1.463(5) . ?
C19 C20 1.366(6) . ?
C19 H19A 0.9500 . ?
C20 C21 1.387(7) . ?
C20 H20A 0.9500 . ?
C21 C22 1.388(6) . ?
C21 H21A 0.9500 . ?
C22 C23 1.466(6) . ?
C23 N3 1.257(6) . ?
C23 H23A 0.9500 . ?
C24 N3 1.471(5) . ?
C24 C25 1.511(7) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 N4 1.469(5) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 N4 1.276(6) . ?
C26 C27 1.448(7) . ?
C26 H26A 0.9500 . ?
C27 C28 1.390(7) . ?
C27 C32 1.415(6) . ?
C28 C29 1.386(8) . ?
C28 H28A 0.9500 . ?
C29 C30 1.362(8) . ?
C29 H29A 0.9500 . ?
C30 C31 1.384(7) . ?
C30 H30A 0.9500 . ?
C31 C32 1.434(7) . ?
C31 N8 1.444(7) . ?
C32 O4 1.278(5) . ?
C33 N9 1.485(6) . ?
C33 C34 1.488(8) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C36 1.494(10) . ?
C35 N9 1.520(7) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 N9 1.468(7) . ?
C37 C38 1.500(9) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
N5 O6 1.213(6) . ?
N5 O5 1.221(6) . ?
N6 O7 1.227(5) . ?
N6 O8 1.227(5) . ?
N7 O10 1.216(5) . ?
N7 O9 1.226(6) . ?
N8 O12 1.208(7) . ?
N8 O11 1.238(7) . ?
N9 H9C 0.9001 . ?
O13 C39 1.380(6) . ?
O13 H13B 0.8400 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9601 . ?
C40 O14 1.389(4) . ?
C40 O14 1.389(4) 2_565 ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9601 . ?
O14 H14D 0.8502 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Eu1 O4 97.78(11) . . ?
O2 Eu1 O1 151.14(10) . . ?
O4 Eu1 O1 86.50(12) . . ?
O2 Eu1 O3 87.74(11) . . ?
O4 Eu1 O3 151.69(10) . . ?
O1 Eu1 O3 101.96(11) . . ?
O2 Eu1 N3 77.31(11) . . ?
O4 Eu1 N3 137.85(11) . . ?
O1 Eu1 N3 80.46(11) . . ?
O3 Eu1 N3 70.46(10) . . ?
O2 Eu1 N1 138.05(11) . . ?
O4 Eu1 N1 80.99(11) . . ?
O1 Eu1 N1 70.80(11) . . ?
O3 Eu1 N1 76.57(10) . . ?
N3 Eu1 N1 130.06(11) . . ?
O2 Eu1 N4 80.90(11) . . ?
O4 Eu1 N4 70.90(11) . . ?
O1 Eu1 N4 73.55(12) . . ?
O3 Eu1 N4 137.37(10) . . ?
N3 Eu1 N4 66.98(11) . . ?
N1 Eu1 N4 135.43(12) . . ?
O2 Eu1 N2 71.16(11) . . ?
O4 Eu1 N2 75.96(11) . . ?
O1 Eu1 N2 137.01(11) . . ?
O3 Eu1 N2 79.71(11) . . ?
N3 Eu1 N2 137.02(12) . . ?
N1 Eu1 N2 67.89(12) . . ?
N4 Eu1 N2 132.74(12) . . ?
O1 C1 C2 123.7(4) . . ?
O1 C1 C6 121.9(4) . . ?
C2 C1 C6 114.4(4) . . ?
C3 C2 C1 122.8(4) . . ?
C3 C2 N5 116.6(4) . . ?
C1 C2 N5 120.7(4) . . ?
C4 C3 C2 121.3(5) . . ?
C4 C3 H3A 119.3 . . ?
C2 C3 H3A 119.3 . . ?
C3 C4 C5 118.3(5) . . ?
C3 C4 H4A 120.9 . . ?
C5 C4 H4A 120.9 . . ?
C4 C5 C6 122.5(5) . . ?
C4 C5 H5A 118.8 . . ?
C6 C5 H5A 118.8 . . ?
C5 C6 C1 120.6(4) . . ?
C5 C6 C7 116.9(4) . . ?
C1 C6 C7 122.5(4) . . ?
N1 C7 C6 128.1(4) . . ?
N1 C7 H7A 115.9 . . ?
C6 C7 H7A 115.9 . . ?
N1 C8 C9 109.5(3) . . ?
N1 C8 H8A 109.8 . . ?
C9 C8 H8A 109.8 . . ?
N1 C8 H8B 109.8 . . ?
C9 C8 H8B 109.8 . . ?
H8A C8 H8B 108.2 . . ?
N2 C9 C8 110.0(3) . . ?
N2 C9 H9A 109.7 . . ?
C8 C9 H9A 109.7 . . ?
N2 C9 H9B 109.7 . . ?
C8 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
N2 C10 C11 128.2(4) . . ?
N2 C10 H10A 115.9 . . ?
C11 C10 H10A 115.9 . . ?
C12 C11 C16 121.2(4) . . ?
C12 C11 C10 116.5(4) . . ?
C16 C11 C10 122.2(4) . . ?
C13 C12 C11 122.3(4) . . ?
C13 C12 H12A 118.8 . . ?
C11 C12 H12A 118.8 . . ?
C14 C13 C12 118.6(5) . . ?
C14 C13 H13A 120.7 . . ?
C12 C13 H13A 120.7 . . ?
C15 C14 C13 120.3(4) . . ?
C15 C14 H14A 119.8 . . ?
C13 C14 H14A 119.8 . . ?
C14 C15 N6 117.1(4) . . ?
C14 C15 C16 123.8(4) . . ?
N6 C15 C16 119.1(4) . . ?
O2 C16 C11 124.0(4) . . ?
O2 C16 C15 122.3(4) . . ?
C11 C16 C15 113.6(4) . . ?
O3 C17 C18 123.7(4) . . ?
O3 C17 C22 123.3(4) . . ?
C18 C17 C22 113.0(4) . . ?
C19 C18 C17 124.7(4) . . ?
C19 C18 N7 116.5(4) . . ?
C17 C18 N7 118.8(4) . . ?
C20 C19 C18 120.0(4) . . ?
C20 C19 H19A 120.0 . . ?
C18 C19 H19A 120.0 . . ?
C19 C20 C21 118.7(4) . . ?
C19 C20 H20A 120.7 . . ?
C21 C20 H20A 120.7 . . ?
C20 C21 C22 122.8(4) . . ?
C20 C21 H21A 118.6 . . ?
C22 C21 H21A 118.6 . . ?
C21 C22 C17 120.8(4) . . ?
C21 C22 C23 117.6(4) . . ?
C17 C22 C23 121.5(4) . . ?
N3 C23 C22 127.7(4) . . ?
N3 C23 H23A 116.2 . . ?
C22 C23 H23A 116.2 . . ?
N3 C24 C25 108.0(4) . . ?
N3 C24 H24A 110.1 . . ?
C25 C24 H24A 110.1 . . ?
N3 C24 H24B 110.1 . . ?
C25 C24 H24B 110.1 . . ?
H24A C24 H24B 108.4 . . ?
N4 C25 C24 109.3(4) . . ?
N4 C25 H25A 109.8 . . ?
C24 C25 H25A 109.8 . . ?
N4 C25 H25B 109.8 . . ?
C24 C25 H25B 109.8 . . ?
H25A C25 H25B 108.3 . . ?
N4 C26 C27 128.1(4) . . ?
N4 C26 H26A 116.0 . . ?
C27 C26 H26A 116.0 . . ?
C28 C27 C32 119.9(5) . . ?
C28 C27 C26 117.9(4) . . ?
C32 C27 C26 122.3(4) . . ?
C29 C28 C27 123.3(5) . . ?
C29 C28 H28A 118.3 . . ?
C27 C28 H28A 118.3 . . ?
C30 C29 C28 118.4(5) . . ?
C30 C29 H29A 120.8 . . ?
C28 C29 H29A 120.8 . . ?
C29 C30 C31 120.0(5) . . ?
C29 C30 H30A 120.0 . . ?
C31 C30 H30A 120.0 . . ?
C30 C31 C32 123.5(5) . . ?
C30 C31 N8 116.7(5) . . ?
C32 C31 N8 119.8(5) . . ?
O4 C32 C27 123.7(4) . . ?
O4 C32 C31 121.5(4) . . ?
C27 C32 C31 114.8(4) . . ?
N9 C33 C34 114.1(5) . . ?
N9 C33 H33A 108.7 . . ?
C34 C33 H33A 108.7 . . ?
N9 C33 H33B 108.7 . . ?
C34 C33 H33B 108.7 . . ?
H33A C33 H33B 107.6 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36 C35 N9 113.6(5) . . ?
C36 C35 H35A 108.8 . . ?
N9 C35 H35A 108.8 . . ?
C36 C35 H35B 108.8 . . ?
N9 C35 H35B 108.8 . . ?
H35A C35 H35B 107.7 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N9 C37 C38 113.6(5) . . ?
N9 C37 H37A 108.9 . . ?
C38 C37 H37A 108.9 . . ?
N9 C37 H37B 108.9 . . ?
C38 C37 H37B 108.9 . . ?
H37A C37 H37B 107.7 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C7 N1 C8 116.4(3) . . ?
C7 N1 Eu1 131.0(3) . . ?
C8 N1 Eu1 112.6(3) . . ?
C10 N2 C9 117.2(3) . . ?
C10 N2 Eu1 130.5(3) . . ?
C9 N2 Eu1 112.3(3) . . ?
C23 N3 C24 117.5(3) . . ?
C23 N3 Eu1 127.3(3) . . ?
C24 N3 Eu1 113.4(3) . . ?
C26 N4 C25 117.8(4) . . ?
C26 N4 Eu1 126.9(3) . . ?
C25 N4 Eu1 113.8(3) . . ?
O6 N5 O5 119.6(5) . . ?
O6 N5 C2 121.0(5) . . ?
O5 N5 C2 119.0(5) . . ?
O7 N6 O8 121.7(4) . . ?
O7 N6 C15 118.9(4) . . ?
O8 N6 C15 119.4(4) . . ?
O10 N7 O9 122.8(4) . . ?
O10 N7 C18 119.8(4) . . ?
O9 N7 C18 117.3(4) . . ?
O12 N8 O11 120.3(6) . . ?
O12 N8 C31 119.4(6) . . ?
O11 N8 C31 120.3(5) . . ?
C37 N9 C33 114.4(4) . . ?
C37 N9 C35 109.8(4) . . ?
C33 N9 C35 113.5(4) . . ?
C37 N9 H9C 106.0 . . ?
C33 N9 H9C 106.3 . . ?
C35 N9 H9C 106.2 . . ?
C1 O1 Eu1 142.3(3) . . ?
C16 O2 Eu1 143.4(3) . . ?
C17 O3 Eu1 130.6(3) . . ?
C32 O4 Eu1 136.3(3) . . ?
C39 O13 H13B 109.5 . . ?
O13 C39 H39A 109.2 . . ?
O13 C39 H39B 109.8 . . ?
H39A C39 H39B 109.5 . . ?
O13 C39 H39C 109.4 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O14 C40 O14 180.0 . 2_565 ?
O14 C40 H40A 110.2 . . ?
O14 C40 H40A 69.8 2_565 . ?
O14 C40 H40B 109.0 . . ?
O14 C40 H40B 71.0 2_565 . ?
H40A C40 H40B 109.5 . . ?
O14 C40 H40C 109.2 . . ?
O14 C40 H40C 70.8 2_565 . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C40 O14 H14D 107.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 -176.7(4) . . . . ?
C6 C1 C2 C3 4.1(7) . . . . ?
O1 C1 C2 N5 5.8(7) . . . . ?
C6 C1 C2 N5 -173.4(4) . . . . ?
C1 C2 C3 C4 0.2(8) . . . . ?
N5 C2 C3 C4 177.8(5) . . . . ?
C2 C3 C4 C5 -3.8(7) . . . . ?
C3 C4 C5 C6 2.8(7) . . . . ?
C4 C5 C6 C1 1.9(7) . . . . ?
C4 C5 C6 C7 -176.3(4) . . . . ?
O1 C1 C6 C5 175.8(4) . . . . ?
C2 C1 C6 C5 -5.1(6) . . . . ?
O1 C1 C6 C7 -6.2(7) . . . . ?
C2 C1 C6 C7 173.0(4) . . . . ?
C5 C6 C7 N1 174.5(5) . . . . ?
C1 C6 C7 N1 -3.6(7) . . . . ?
N1 C8 C9 N2 60.3(5) . . . . ?
N2 C10 C11 C12 -178.8(4) . . . . ?
N2 C10 C11 C16 -0.4(7) . . . . ?
C16 C11 C12 C13 -1.0(7) . . . . ?
C10 C11 C12 C13 177.5(4) . . . . ?
C11 C12 C13 C14 0.3(7) . . . . ?
C12 C13 C14 C15 2.2(7) . . . . ?
C13 C14 C15 N6 177.2(4) . . . . ?
C13 C14 C15 C16 -4.2(7) . . . . ?
C12 C11 C16 O2 175.6(4) . . . . ?
C10 C11 C16 O2 -2.7(7) . . . . ?
C12 C11 C16 C15 -0.8(6) . . . . ?
C10 C11 C16 C15 -179.1(4) . . . . ?
C14 C15 C16 O2 -173.1(4) . . . . ?
N6 C15 C16 O2 5.5(6) . . . . ?
C14 C15 C16 C11 3.4(6) . . . . ?
N6 C15 C16 C11 -178.0(4) . . . . ?
O3 C17 C18 C19 179.9(4) . . . . ?
C22 C17 C18 C19 0.1(7) . . . . ?
O3 C17 C18 N7 3.2(7) . . . . ?
C22 C17 C18 N7 -176.7(4) . . . . ?
C17 C18 C19 C20 2.7(8) . . . . ?
N7 C18 C19 C20 179.5(4) . . . . ?
C18 C19 C20 C21 -2.2(8) . . . . ?
C19 C20 C21 C22 -1.0(8) . . . . ?
C20 C21 C22 C17 3.9(7) . . . . ?
C20 C21 C22 C23 -178.8(4) . . . . ?
O3 C17 C22 C21 176.9(4) . . . . ?
C18 C17 C22 C21 -3.2(6) . . . . ?
O3 C17 C22 C23 -0.3(7) . . . . ?
C18 C17 C22 C23 179.6(4) . . . . ?
C21 C22 C23 N3 170.2(5) . . . . ?
C17 C22 C23 N3 -12.5(7) . . . . ?
N3 C24 C25 N4 60.1(5) . . . . ?
N4 C26 C27 C28 170.3(5) . . . . ?
N4 C26 C27 C32 -9.4(8) . . . . ?
C32 C27 C28 C29 -0.9(9) . . . . ?
C26 C27 C28 C29 179.4(5) . . . . ?
C27 C28 C29 C30 -0.6(9) . . . . ?
C28 C29 C30 C31 -0.5(9) . . . . ?
C29 C30 C31 C32 3.2(9) . . . . ?
C29 C30 C31 N8 -178.8(5) . . . . ?
C28 C27 C32 O4 -176.2(5) . . . . ?
C26 C27 C32 O4 3.5(8) . . . . ?
C28 C27 C32 C31 3.2(7) . . . . ?
C26 C27 C32 C31 -177.1(5) . . . . ?
C30 C31 C32 O4 174.9(5) . . . . ?
N8 C31 C32 O4 -3.1(8) . . . . ?
C30 C31 C32 C27 -4.4(8) . . . . ?
N8 C31 C32 C27 177.5(5) . . . . ?
C6 C7 N1 C8 -177.6(4) . . . . ?
C6 C7 N1 Eu1 -1.3(7) . . . . ?
C9 C8 N1 C7 130.9(4) . . . . ?
C9 C8 N1 Eu1 -46.0(4) . . . . ?
C11 C10 N2 C9 177.2(4) . . . . ?
C11 C10 N2 Eu1 -1.8(7) . . . . ?
C8 C9 N2 C10 137.5(4) . . . . ?
C8 C9 N2 Eu1 -43.4(4) . . . . ?
C22 C23 N3 C24 -177.5(4) . . . . ?
C22 C23 N3 Eu1 -14.1(7) . . . . ?
C25 C24 N3 C23 118.2(4) . . . . ?
C25 C24 N3 Eu1 -47.5(4) . . . . ?
C27 C26 N4 C25 -178.9(5) . . . . ?
C27 C26 N4 Eu1 -14.1(8) . . . . ?
C24 C25 N4 C26 123.2(5) . . . . ?
C24 C25 N4 Eu1 -43.6(4) . . . . ?
C3 C2 N5 O6 -23.3(8) . . . . ?
C1 C2 N5 O6 154.4(5) . . . . ?
C3 C2 N5 O5 149.8(6) . . . . ?
C1 C2 N5 O5 -32.6(8) . . . . ?
C14 C15 N6 O7 -143.8(5) . . . . ?
C16 C15 N6 O7 37.5(6) . . . . ?
C14 C15 N6 O8 35.9(6) . . . . ?
C16 C15 N6 O8 -142.8(4) . . . . ?
C19 C18 N7 O10 144.3(5) . . . . ?
C17 C18 N7 O10 -38.6(6) . . . . ?
C19 C18 N7 O9 -35.1(6) . . . . ?
C17 C18 N7 O9 141.9(5) . . . . ?
C30 C31 N8 O12 -37.4(8) . . . . ?
C32 C31 N8 O12 140.7(6) . . . . ?
C30 C31 N8 O11 142.0(6) . . . . ?
C32 C31 N8 O11 -39.9(8) . . . . ?
C38 C37 N9 C33 59.7(6) . . . . ?
C38 C37 N9 C35 -171.4(5) . . . . ?
C34 C33 N9 C37 65.3(7) . . . . ?
C34 C33 N9 C35 -61.7(7) . . . . ?
C36 C35 N9 C37 179.3(5) . . . . ?
C36 C35 N9 C33 -51.3(6) . . . . ?
C2 C1 O1 Eu1 -152.9(4) . . . . ?
C6 C1 O1 Eu1 26.2(7) . . . . ?
C11 C16 O2 Eu1 10.2(7) . . . . ?
C15 C16 O2 Eu1 -173.7(3) . . . . ?
C18 C17 O3 Eu1 -136.2(4) . . . . ?
C22 C17 O3 Eu1 43.7(6) . . . . ?
C27 C32 O4 Eu1 32.6(7) . . . . ?
C31 C32 O4 Eu1 -146.8(4) . . . . ?

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
O14 H14D O11 0.85 2.47 3.067(13) 128.2 1_545
O13 H13B O3 0.84 2.03 2.830(5) 158.6 .
N9 H9C O13 0.90 1.86 2.729(5) 162.4 .
C24 H24B O5 0.99 2.38 3.310(7) 156.5 .
C23 H23A O7 0.95 2.60 3.458(5) 150.3 2_666
C19 H19A O14 0.95 2.33 3.264(12) 168.9 2_665
C9 H9B O11 0.99 2.54 3.481(7) 158.6 .
C8 H8B O10 0.99 2.45 3.428(6) 171.4 .

_refine_diff_density_max         1.221
_refine_diff_density_min         -1.499
_refine_diff_density_rms         0.130

_shelxl_version_number           2013-4

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

data_1
_database_code_depnum_ccdc_archive 'CCDC 1404027'
_audit_update_record             
;
2015-06-01 deposited with the CCDC.
2015-12-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'2(C32 H24 N8 O12 Tb), 2(C6 H16 N),  0.25(H8 O4), 2(C H4 O'
_chemical_formula_sum            'C39 H45 N9 O13.50 Tb'
_chemical_formula_weight         1014.76

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'
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'
H H 0.0000 0.0000 '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                   12.427(8)
_cell_length_b                   12.703(8)
_cell_length_c                   15.553(10)
_cell_angle_alpha                70.024(11)
_cell_angle_beta                 75.363(11)
_cell_angle_gamma                72.030(11)
_cell_volume                     2165(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    3518
_cell_measurement_theta_min      2.421
_cell_measurement_theta_max      21.877

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1030
_exptl_absorpt_coefficient_mu    1.708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5136
_exptl_absorpt_correction_T_max  0.6747
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker AFEX II'
_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            12267
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.76
_diffrn_reflns_theta_max         25.00
_reflns_number_total             7605
_reflns_number_gt                6297
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0496P)²+0.7074P] 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         7605
_refine_ls_number_parameters     636
_refine_ls_number_restraints     254
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0378
_refine_ls_wR_factor_ref         0.0926
_refine_ls_wR_factor_gt          0.0860
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_restrained_S_all      1.003
_refine_ls_shift/su_max          0.003
_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
Tb1 Tb 0.231604(19) 0.814047(18) 0.268439(15) 0.04191(9) Uani 1 1 d . A .
C1 C -0.0075(4) 0.7487(4) 0.2591(4) 0.0537(12) Uani 1 1 d . A .
C2 C -0.1109(5) 0.7162(5) 0.3126(4) 0.0603(13) Uani 1 1 d . . .
C3 C -0.2006(5) 0.7200(5) 0.2733(5) 0.0747(17) Uani 1 1 d . A .
H3 H -0.2654 0.6975 0.3113 0.090 Uiso 1 1 calc R . .
C4 C -0.1952(6) 0.7563(5) 0.1800(5) 0.0803(18) Uani 1 1 d . . .
H4 H -0.2539 0.7557 0.1533 0.096 Uiso 1 1 calc R A .
C5 C -0.1008(5) 0.7940(5) 0.1260(4) 0.0713(16) Uani 1 1 d . A .
H5 H -0.0982 0.8218 0.0620 0.086 Uiso 1 1 calc R . .
C6 C -0.0094(5) 0.7927(4) 0.1620(4) 0.0579(13) Uani 1 1 d . . .
C7 C 0.0820(5) 0.8405(4) 0.0974(4) 0.0586(13) Uani 1 1 d . A .
H7 H 0.0749 0.8647 0.0351 0.070 Uiso 1 1 calc R . .
C8 C 0.2481(5) 0.9074(4) 0.0365(3) 0.0585(13) Uani 1 1 d . A .
H8A H 0.2126 0.9374 -0.0186 0.070 Uiso 1 1 calc R . .
H8B H 0.3189 0.8507 0.0253 0.070 Uiso 1 1 calc R . .
C9 C 0.2731(5) 1.0039(4) 0.0571(3) 0.0585(13) Uani 1 1 d . A .
H9A H 0.3237 1.0409 0.0048 0.070 Uiso 1 1 calc R . .
H9B H 0.2024 1.0613 0.0669 0.070 Uiso 1 1 calc R . .
C10 C 0.4109(4) 0.9965(4) 0.1380(3) 0.0518(12) Uani 1 1 d . A .
H10 H 0.4329 1.0488 0.0823 0.062 Uiso 1 1 calc R . .
C11 C 0.4765(4) 0.9700(4) 0.2100(3) 0.0487(11) Uani 1 1 d . . .
C12 C 0.5633(5) 1.0254(4) 0.1906(4) 0.0637(14) Uani 1 1 d . . .
H12 H 0.5784 1.0744 0.1313 0.076 Uiso 1 1 calc R . .
C13 C 0.6282(5) 1.0113(5) 0.2552(4) 0.0736(16) Uani 1 1 d . . .
H13 H 0.6853 1.0507 0.2404 0.088 Uiso 1 1 calc R . .
C14 C 0.6069(5) 0.9383(5) 0.3410(4) 0.0656(14) Uani 1 1 d . . .
H14 H 0.6489 0.9285 0.3861 0.079 Uiso 1 1 calc R . .
C15 C 0.5246(4) 0.8793(4) 0.3618(3) 0.0508(11) Uani 1 1 d . . .
C16 C 0.4517(4) 0.8937(4) 0.2994(3) 0.0443(11) Uani 1 1 d . A .
C17 C 0.4753(4) 0.6269(4) 0.2166(3) 0.0445(11) Uani 1 1 d . A .
C18 C 0.5775(4) 0.6163(4) 0.1514(4) 0.0530(12) Uani 1 1 d . . .
C19 C 0.6836(5) 0.5466(5) 0.1732(4) 0.0646(14) Uani 1 1 d . B .
H19 H 0.7483 0.5457 0.1274 0.077 Uiso 1 1 calc R . .
C20 C 0.6922(5) 0.4796(5) 0.2618(4) 0.0697(16) Uani 1 1 d . . .
H20 H 0.7620 0.4311 0.2773 0.084 Uiso 1 1 calc R B .
C21 C 0.5955(5) 0.4857(4) 0.3274(4) 0.0632(14) Uani 1 1 d . B .
H21 H 0.6015 0.4391 0.3878 0.076 Uiso 1 1 calc R . .
C22 C 0.4887(4) 0.5573(4) 0.3094(3) 0.0505(12) Uani 1 1 d . . .
C23 C 0.3939(5) 0.5566(4) 0.3859(3) 0.0542(13) Uani 1 1 d . A .
H23 H 0.4071 0.4993 0.4412 0.065 Uiso 1 1 calc R . .
C24 C 0.2153(5) 0.6092(5) 0.4737(3) 0.0623(14) Uani 1 1 d . A .
H24A H 0.2505 0.5439 0.5210 0.075 Uiso 1 1 calc R . .
H24B H 0.1470 0.5942 0.4658 0.075 Uiso 1 1 calc R . .
C25 C 0.1840(5) 0.7175(5) 0.5030(3) 0.0654(15) Uani 1 1 d . A .
H25A H 0.1311 0.7089 0.5613 0.078 Uiso 1 1 calc R . .
H25B H 0.2522 0.7317 0.5119 0.078 Uiso 1 1 calc R . .
C26 C 0.0313(5) 0.8715(5) 0.4557(4) 0.0680(16) Uani 1 1 d . A .
H26 H 0.0007 0.8481 0.5183 0.082 Uiso 1 1 calc R . .
C27 C -0.0405(5) 0.9691(5) 0.3983(4) 0.0630(14) Uani 1 1 d . . .
C28 C -0.1539(6) 1.0127(7) 0.4364(5) 0.089(2) Uani 1 1 d . . .
H28 H -0.1796 0.9765 0.4979 0.107 Uiso 1 1 calc R . .
C29 C -0.2288(6) 1.1041(7) 0.3896(7) 0.099(3) Uani 1 1 d . . .
H29 H -0.3037 1.1286 0.4181 0.119 Uiso 1 1 calc R . .
C30 C -0.1918(6) 1.1588(6) 0.3005(7) 0.093(2) Uani 1 1 d . C .
H30 H -0.2415 1.2214 0.2668 0.111 Uiso 1 1 calc R . .
C31 C -0.0797(5) 1.1214(5) 0.2595(5) 0.0738(18) Uani 1 1 d D . .
C32 C 0.0003(5) 1.0233(4) 0.3042(4) 0.0589(14) Uani 1 1 d . A .
C33 C 0.2537(6) 0.2718(6) 0.2238(5) 0.095(2) Uani 1 1 d . . .
H33A H 0.1935 0.2960 0.1868 0.114 Uiso 1 1 calc R . .
H33B H 0.3260 0.2494 0.1847 0.114 Uiso 1 1 calc R . .
C34 C 0.2350(8) 0.1707(7) 0.3003(8) 0.158(5) Uani 1 1 d . . .
H34A H 0.2463 0.1070 0.2764 0.237 Uiso 1 1 calc R . .
H34B H 0.1581 0.1873 0.3331 0.237 Uiso 1 1 calc R . .
H34C H 0.2884 0.1510 0.3418 0.237 Uiso 1 1 calc R . .
C35 C 0.1461(8) 0.4181(7) 0.3093(6) 0.111(3) Uani 1 1 d . . .
H35A H 0.1388 0.3628 0.3703 0.134 Uiso 1 1 calc R . .
H35B H 0.1514 0.4888 0.3172 0.134 Uiso 1 1 calc R . .
C36 C 0.0406(8) 0.4429(9) 0.2690(8) 0.155(4) Uani 1 1 d . . .
H36A H 0.0499 0.4921 0.2064 0.233 Uiso 1 1 calc R . .
H36B H -0.0244 0.4808 0.3055 0.233 Uiso 1 1 calc R . .
H36C H 0.0285 0.3718 0.2691 0.233 Uiso 1 1 calc R . .
C37 C 0.3532(8) 0.3526(8) 0.2953(7) 0.122(3) Uani 1 1 d . . .
H37A H 0.3505 0.2894 0.3521 0.147 Uiso 1 1 calc R . .
H37B H 0.3468 0.4216 0.3118 0.147 Uiso 1 1 calc R . .
C38 C 0.4692(7) 0.3246(7) 0.2318(8) 0.144(4) Uani 1 1 d . . .
H38A H 0.4788 0.2526 0.2199 0.215 Uiso 1 1 calc R . .
H38B H 0.5304 0.3187 0.2618 0.215 Uiso 1 1 calc R . .
H38C H 0.4705 0.3850 0.1743 0.215 Uiso 1 1 calc R . .
N1 N 0.1713(3) 0.8537(3) 0.1155(3) 0.0510(10) Uani 1 1 d . . .
N2 N 0.3273(3) 0.9582(3) 0.1401(3) 0.0487(9) Uani 1 1 d . . .
N3 N 0.2956(4) 0.6245(3) 0.3863(3) 0.0492(9) Uani 1 1 d . . .
N4 N 0.1307(4) 0.8142(4) 0.4310(3) 0.0549(10) Uani 1 1 d . . .
N5 N -0.1257(5) 0.6809(5) 0.4122(4) 0.0824(14) Uani 0.661(12) 1 d PDU A 1
O5 O -0.0438(6) 0.6166(11) 0.4505(5) 0.121(4) Uani 0.661(12) 1 d PDU A 1
O6 O -0.2201(8) 0.7015(10) 0.4583(8) 0.118(4) Uani 0.661(12) 1 d PDU A 1
N5' N -0.1257(5) 0.6809(5) 0.4122(4) 0.0824(14) Uani 0.339(12) 1 d PDU A 2
O5' O -0.0774(15) 0.7158(17) 0.4513(9) 0.094(4) Uani 0.339(12) 1 d PDU A 2
O6' O -0.2086(14) 0.644(2) 0.4543(17) 0.110(5) Uani 0.339(12) 1 d PDU A 2
N6 N 0.5102(4) 0.7982(5) 0.4537(3) 0.0695(13) Uani 1 1 d . . .
N7 N 0.5769(5) 0.6850(4) 0.0565(3) 0.0696(12) Uani 0.865(7) 1 d PDU B 1
O9 O 0.6588(5) 0.7233(6) 0.0130(4) 0.107(2) Uani 0.865(7) 1 d PDU B 1
O10 O 0.4977(4) 0.6984(5) 0.0183(3) 0.0904(17) Uani 0.865(7) 1 d PDU B 1
N7' N 0.5769(5) 0.6850(4) 0.0565(3) 0.0696(12) Uani 0.135(7) 1 d PDU B 2
O9' O 0.512(3) 0.7800(18) 0.0400(18) 0.088(7) Uani 0.135(7) 1 d PDU B 2
O10' O 0.636(3) 0.647(3) -0.0062(15) 0.098(6) Uani 0.135(7) 1 d PDU B 2
N8 N -0.0447(7) 1.1831(6) 0.1660(6) 0.113(2) Uani 0.768(7) 1 d PDU C 1
O11 O 0.0494(7) 1.2062(6) 0.1413(6) 0.132(3) Uani 0.768(7) 1 d PDU C 1
O12 O -0.1107(8) 1.2214(9) 0.1113(6) 0.161(3) Uani 0.768(7) 1 d PDU C 1
N8' N -0.0447(7) 1.1831(6) 0.1660(6) 0.113(2) Uani 0.232(7) 1 d PDU C 2
O11' O -0.011(2) 1.1239(19) 0.1127(15) 0.122(5) Uani 0.232(7) 1 d PDU C 2
O12' O -0.078(3) 1.2861(12) 0.151(2) 0.141(6) Uani 0.232(7) 1 d PDU C 2
N9 N 0.2562(4) 0.3706(4) 0.2503(3) 0.0723(13) Uani 1 1 d . . .
H9C H 0.2641 0.4281 0.1965 0.087 Uiso 1 1 calc R . .
O1 O 0.0786(3) 0.7372(3) 0.2949(2) 0.0603(9) Uani 1 1 d . . .
O2 O 0.3688(3) 0.8441(3) 0.3227(2) 0.0524(8) Uani 1 1 d . . .
O3 O 0.3772(3) 0.6916(3) 0.1951(2) 0.0516(8) Uani 1 1 d . . .
O4 O 0.1014(3) 0.9878(3) 0.2628(2) 0.0614(9) Uani 1 1 d . . .
O7 O 0.4885(5) 0.7094(4) 0.4638(3) 0.1059(17) Uani 1 1 d . . .
O8 O 0.5208(4) 0.8244(5) 0.5199(3) 0.1059(16) Uani 1 1 d . . .
O13 O 0.2893(5) 0.5692(4) 0.1148(4) 0.1203(18) Uani 1 1 d . . .
H13A H 0.3183 0.6128 0.1247 0.180 Uiso 1 1 calc R . .
C39 C 0.2934(9) 0.5943(8) 0.0210(6) 0.132(3) Uani 1 1 d . . .
H39A H 0.3536 0.5375 -0.0024 0.198 Uiso 1 1 calc R . .
H39B H 0.3081 0.6694 -0.0095 0.198 Uiso 1 1 calc R . .
H39C H 0.2213 0.5938 0.0093 0.198 Uiso 1 1 calc R . .
O1W O 1.0000 0.5000 1.0000 0.205(12) Uani 0.50 2 d SPU D 1
H1WA H 0.9393 0.4758 1.0212 0.307 Uiso 0.25 1 d PR D 1
H1WB H 0.9932 0.5502 0.9482 0.307 Uiso 0.25 1 d PR D 1
O2W O 1.069(2) 0.449(2) 1.001(2) 0.163(12) Uani 0.25 1 d PU . 2
H2WB H 1.0255 0.4127 1.0446 0.244 Uiso 0.25 1 d PR . 2
H2WA H 1.0282 0.5027 0.9640 0.244 Uiso 0.25 1 d PR . 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O2 2.261(3) . ?
Tb1 O1 2.283(3) . ?
Tb1 O4 2.287(3) . ?
Tb1 O3 2.330(3) . ?
Tb1 N1 2.515(4) . ?
Tb1 N3 2.516(4) . ?
Tb1 N4 2.523(4) . ?
Tb1 N2 2.530(4) . ?
C1 O1 1.275(6) . ?
C1 C6 1.423(7) . ?
C1 C2 1.438(7) . ?
C2 C3 1.383(8) . ?
C2 N5 1.437(8) . ?
C3 C4 1.354(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.374(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.382(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.448(8) . ?
C7 N1 1.282(6) . ?
C7 H7 0.9300 . ?
C8 N1 1.457(6) . ?
C8 C9 1.501(7) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N2 1.464(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.265(6) . ?
C10 C11 1.438(7) . ?
C10 H10 0.9300 . ?
C11 C12 1.381(7) . ?
C11 C16 1.419(6) . ?
C12 C13 1.374(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.356(8) . ?
C13 H13 0.9300 . ?
C14 C15 1.361(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.421(6) . ?
C15 N6 1.455(7) . ?
C16 O2 1.283(5) . ?
C17 O3 1.294(5) . ?
C17 C18 1.413(7) . ?
C17 C22 1.433(6) . ?
C18 C19 1.392(7) . ?
C18 N7 1.436(7) . ?
C19 C20 1.360(8) . ?
C19 H19 0.9300 . ?
C20 C21 1.367(8) . ?
C20 H20 0.9300 . ?
C21 C22 1.392(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.447(7) . ?
C23 N3 1.260(6) . ?
C23 H23 0.9300 . ?
C24 N3 1.462(6) . ?
C24 C25 1.503(7) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 N4 1.461(6) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 N4 1.265(7) . ?
C26 C27 1.448(8) . ?
C26 H26 0.9300 . ?
C27 C28 1.401(8) . ?
C27 C32 1.423(8) . ?
C28 C29 1.358(10) . ?
C28 H28 0.9300 . ?
C29 C30 1.354(11) . ?
C29 H29 0.9300 . ?
C30 C31 1.387(9) . ?
C30 H30 0.9300 . ?
C31 C32 1.420(8) . ?
C31 N8 1.425(10) . ?
C32 O4 1.280(6) . ?
C33 C34 1.456(11) . ?
C33 N9 1.460(7) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 C36 1.496(12) . ?
C35 N9 1.521(9) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 N9 1.463(9) . ?
C37 C38 1.544(12) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
N5 O6 1.213(8) . ?
N5 O5 1.232(8) . ?
N6 O7 1.189(6) . ?
N6 O8 1.231(6) . ?
N7 O9 1.209(7) . ?
N7 O10 1.214(6) . ?
N8 O12 1.207(9) . ?
N8 O11 1.228(9) . ?
N9 H9C 0.9100 . ?
O13 C39 1.373(9) . ?
O13 H13A 0.8200 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
O1W H1WA 0.8489 . ?
O1W H1WB 0.8444 . ?
O2W O2W 1.80(5) 2_767 ?
O2W H2WB 0.8461 . ?
O2W H2WA 0.8479 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Tb1 O1 149.73(12) . . ?
O2 Tb1 O4 98.65(13) . . ?
O1 Tb1 O4 86.80(14) . . ?
O2 Tb1 O3 87.61(13) . . ?
O1 Tb1 O3 102.21(13) . . ?
O4 Tb1 O3 150.53(12) . . ?
O2 Tb1 N1 138.63(12) . . ?
O1 Tb1 N1 71.59(13) . . ?
O4 Tb1 N1 80.49(13) . . ?
O3 Tb1 N1 76.06(12) . . ?
O2 Tb1 N3 76.62(12) . . ?
O1 Tb1 N3 79.78(13) . . ?
O4 Tb1 N3 138.81(13) . . ?
O3 Tb1 N3 70.65(13) . . ?
N1 Tb1 N3 129.70(13) . . ?
O2 Tb1 N4 79.86(13) . . ?
O1 Tb1 N4 73.76(13) . . ?
O4 Tb1 N4 71.23(13) . . ?
O3 Tb1 N4 138.17(12) . . ?
N1 Tb1 N4 135.98(14) . . ?
N3 Tb1 N4 67.65(14) . . ?
O2 Tb1 N2 71.61(12) . . ?
O1 Tb1 N2 138.08(12) . . ?
O4 Tb1 N2 75.83(13) . . ?
O3 Tb1 N2 79.00(12) . . ?
N1 Tb1 N2 68.10(13) . . ?
N3 Tb1 N2 136.52(13) . . ?
N4 Tb1 N2 132.01(13) . . ?
O1 C1 C6 123.2(5) . . ?
O1 C1 C2 123.2(5) . . ?
C6 C1 C2 113.6(5) . . ?
C3 C2 N5 117.0(5) . . ?
C3 C2 C1 123.3(6) . . ?
N5 C2 C1 119.7(5) . . ?
C4 C3 C2 120.7(6) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C3 C4 C5 118.3(5) . . ?
C3 C4 H4 120.8 . . ?
C5 C4 H4 120.8 . . ?
C4 C5 C6 123.1(6) . . ?
C4 C5 H5 118.4 . . ?
C6 C5 H5 118.4 . . ?
C5 C6 C1 120.8(5) . . ?
C5 C6 C7 117.3(5) . . ?
C1 C6 C7 121.9(5) . . ?
N1 C7 C6 128.1(5) . . ?
N1 C7 H7 115.9 . . ?
C6 C7 H7 115.9 . . ?
N1 C8 C9 108.9(4) . . ?
N1 C8 H8A 109.9 . . ?
C9 C8 H8A 109.9 . . ?
N1 C8 H8B 109.9 . . ?
C9 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
N2 C9 C8 109.7(4) . . ?
N2 C9 H9A 109.7 . . ?
C8 C9 H9A 109.7 . . ?
N2 C9 H9B 109.7 . . ?
C8 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
N2 C10 C11 128.7(4) . . ?
N2 C10 H10 115.6 . . ?
C11 C10 H10 115.6 . . ?
C12 C11 C16 120.2(5) . . ?
C12 C11 C10 117.5(4) . . ?
C16 C11 C10 122.2(4) . . ?
C13 C12 C11 122.8(5) . . ?
C13 C12 H12 118.6 . . ?
C11 C12 H12 118.6 . . ?
C14 C13 C12 118.3(5) . . ?
C14 C13 H13 120.9 . . ?
C12 C13 H13 120.9 . . ?
C13 C14 C15 120.6(5) . . ?
C13 C14 H14 119.7 . . ?
C15 C14 H14 119.7 . . ?
C14 C15 C16 123.7(5) . . ?
C14 C15 N6 117.7(5) . . ?
C16 C15 N6 118.5(4) . . ?
O2 C16 C11 123.0(4) . . ?
O2 C16 C15 122.8(4) . . ?
C11 C16 C15 114.2(4) . . ?
O3 C17 C18 123.6(4) . . ?
O3 C17 C22 122.3(4) . . ?
C18 C17 C22 114.1(4) . . ?
C19 C18 C17 124.3(5) . . ?
C19 C18 N7 115.9(5) . . ?
C17 C18 N7 119.7(4) . . ?
C20 C19 C18 119.8(5) . . ?
C20 C19 H19 120.1 . . ?
C18 C19 H19 120.1 . . ?
C19 C20 C21 118.2(5) . . ?
C19 C20 H20 120.9 . . ?
C21 C20 H20 120.9 . . ?
C20 C21 C22 124.0(5) . . ?
C20 C21 H21 118.0 . . ?
C22 C21 H21 118.0 . . ?
C21 C22 C17 119.6(5) . . ?
C21 C22 C23 118.2(5) . . ?
C17 C22 C23 122.3(4) . . ?
N3 C23 C22 127.5(4) . . ?
N3 C23 H23 116.2 . . ?
C22 C23 H23 116.2 . . ?
N3 C24 C25 108.6(4) . . ?
N3 C24 H24A 110.0 . . ?
C25 C24 H24A 110.0 . . ?
N3 C24 H24B 110.0 . . ?
C25 C24 H24B 110.0 . . ?
H24A C24 H24B 108.4 . . ?
N4 C25 C24 108.8(4) . . ?
N4 C25 H25A 109.9 . . ?
C24 C25 H25A 109.9 . . ?
N4 C25 H25B 109.9 . . ?
C24 C25 H25B 109.9 . . ?
H25A C25 H25B 108.3 . . ?
N4 C26 C27 127.8(5) . . ?
N4 C26 H26 116.1 . . ?
C27 C26 H26 116.1 . . ?
C28 C27 C32 118.5(6) . . ?
C28 C27 C26 119.2(6) . . ?
C32 C27 C26 122.2(5) . . ?
C29 C28 C27 124.5(8) . . ?
C29 C28 H28 117.7 . . ?
C27 C28 H28 117.7 . . ?
C30 C29 C28 118.3(7) . . ?
C30 C29 H29 120.9 . . ?
C28 C29 H29 120.9 . . ?
C29 C30 C31 120.0(7) . . ?
C29 C30 H30 120.0 . . ?
C31 C30 H30 120.0 . . ?
C30 C31 C32 123.8(7) . . ?
C30 C31 N8 117.6(7) . . ?
C32 C31 N8 118.5(6) . . ?
O4 C32 C31 122.2(6) . . ?
O4 C32 C27 123.0(5) . . ?
C31 C32 C27 114.8(5) . . ?
C34 C33 N9 115.6(7) . . ?
C34 C33 H33A 108.4 . . ?
N9 C33 H33A 108.4 . . ?
C34 C33 H33B 108.4 . . ?
N9 C33 H33B 108.4 . . ?
H33A C33 H33B 107.4 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36 C35 N9 113.7(7) . . ?
C36 C35 H35A 108.8 . . ?
N9 C35 H35A 108.8 . . ?
C36 C35 H35B 108.8 . . ?
N9 C35 H35B 108.8 . . ?
H35A C35 H35B 107.7 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N9 C37 C38 111.8(7) . . ?
N9 C37 H37A 109.3 . . ?
C38 C37 H37A 109.3 . . ?
N9 C37 H37B 109.3 . . ?
C38 C37 H37B 109.3 . . ?
H37A C37 H37B 107.9 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C7 N1 C8 116.4(4) . . ?
C7 N1 Tb1 130.4(3) . . ?
C8 N1 Tb1 113.0(3) . . ?
C10 N2 C9 117.1(4) . . ?
C10 N2 Tb1 130.3(3) . . ?
C9 N2 Tb1 112.5(3) . . ?
C23 N3 C24 117.3(4) . . ?
C23 N3 Tb1 127.9(3) . . ?
C24 N3 Tb1 112.9(3) . . ?
C26 N4 C25 116.8(5) . . ?
C26 N4 Tb1 127.8(4) . . ?
C25 N4 Tb1 113.7(3) . . ?
O6 N5 O5 119.7(9) . . ?
O6 N5 C2 120.7(8) . . ?
O5 N5 C2 118.9(7) . . ?
O7 N6 O8 121.6(5) . . ?
O7 N6 C15 120.3(5) . . ?
O8 N6 C15 118.2(5) . . ?
O9 N7 O10 120.0(6) . . ?
O9 N7 C18 119.8(5) . . ?
O10 N7 C18 120.0(5) . . ?
O12 N8 O11 118.6(10) . . ?
O12 N8 C31 120.3(9) . . ?
O11 N8 C31 120.9(7) . . ?
C33 N9 C37 114.9(6) . . ?
C33 N9 C35 114.3(5) . . ?
C37 N9 C35 108.7(6) . . ?
C33 N9 H9C 106.1 . . ?
C37 N9 H9C 106.1 . . ?
C35 N9 H9C 106.1 . . ?
C1 O1 Tb1 140.9(3) . . ?
C16 O2 Tb1 143.8(3) . . ?
C17 O3 Tb1 131.6(3) . . ?
C32 O4 Tb1 136.7(3) . . ?
C39 O13 H13A 109.5 . . ?
O13 C39 H39A 109.5 . . ?
O13 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
O13 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
H1WA O1W H1WB 109.2 . . ?
H1WA O1W H2WB 74.0 . . ?
H1WB O1W H2WB 154.0 . . ?
H1WA O1W H2WA 128.1 . . ?
H1WB O1W H2WA 48.8 . . ?
H2WB O1W H2WA 108.2 . . ?
O2W O2W H1WB 31.9 2_767 . ?
O2W O2W H2WB 76.9 2_767 . ?
H1WB O2W H2WB 106.3 . . ?
O2W O2W H2WA 38.4 2_767 . ?
H1WB O2W H2WA 8.7 . . ?
H2WB O2W H2WA 109.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 -174.6(5) . . . . ?
C6 C1 C2 C3 4.1(7) . . . . ?
O1 C1 C2 N5 7.3(8) . . . . ?
C6 C1 C2 N5 -174.0(5) . . . . ?
N5 C2 C3 C4 177.7(6) . . . . ?
C1 C2 C3 C4 -0.4(9) . . . . ?
C2 C3 C4 C5 -2.9(9) . . . . ?
C3 C4 C5 C6 2.5(9) . . . . ?
C4 C5 C6 C1 1.5(9) . . . . ?
C4 C5 C6 C7 -176.9(5) . . . . ?
O1 C1 C6 C5 174.2(5) . . . . ?
C2 C1 C6 C5 -4.5(7) . . . . ?
O1 C1 C6 C7 -7.4(8) . . . . ?
C2 C1 C6 C7 173.9(5) . . . . ?
C5 C6 C7 N1 176.2(5) . . . . ?
C1 C6 C7 N1 -2.2(8) . . . . ?
N1 C8 C9 N2 59.8(5) . . . . ?
N2 C10 C11 C12 -178.9(5) . . . . ?
N2 C10 C11 C16 -1.5(8) . . . . ?
C16 C11 C12 C13 -0.6(8) . . . . ?
C10 C11 C12 C13 176.9(5) . . . . ?
C11 C12 C13 C14 1.0(9) . . . . ?
C12 C13 C14 C15 1.1(9) . . . . ?
C13 C14 C15 C16 -3.8(9) . . . . ?
C13 C14 C15 N6 177.0(5) . . . . ?
C12 C11 C16 O2 176.6(4) . . . . ?
C10 C11 C16 O2 -0.8(7) . . . . ?
C12 C11 C16 C15 -1.7(7) . . . . ?
C10 C11 C16 C15 -179.1(4) . . . . ?
C14 C15 C16 O2 -174.4(5) . . . . ?
N6 C15 C16 O2 4.8(7) . . . . ?
C14 C15 C16 C11 4.0(7) . . . . ?
N6 C15 C16 C11 -176.8(4) . . . . ?
O3 C17 C18 C19 -179.5(5) . . . . ?
C22 C17 C18 C19 -1.0(7) . . . . ?
O3 C17 C18 N7 4.0(7) . . . . ?
C22 C17 C18 N7 -177.4(4) . . . . ?
C17 C18 C19 C20 2.6(8) . . . . ?
N7 C18 C19 C20 179.2(5) . . . . ?
C18 C19 C20 C21 -1.6(8) . . . . ?
C19 C20 C21 C22 -0.8(9) . . . . ?
C20 C21 C22 C17 2.4(8) . . . . ?
C20 C21 C22 C23 -178.9(5) . . . . ?
O3 C17 C22 C21 177.2(4) . . . . ?
C18 C17 C22 C21 -1.5(6) . . . . ?
O3 C17 C22 C23 -1.4(7) . . . . ?
C18 C17 C22 C23 179.9(4) . . . . ?
C21 C22 C23 N3 170.5(5) . . . . ?
C17 C22 C23 N3 -10.9(8) . . . . ?
N3 C24 C25 N4 59.9(6) . . . . ?
N4 C26 C27 C28 172.4(5) . . . . ?
N4 C26 C27 C32 -8.0(9) . . . . ?
C32 C27 C28 C29 -0.1(9) . . . . ?
C26 C27 C28 C29 179.5(6) . . . . ?
C27 C28 C29 C30 -1.1(11) . . . . ?
C28 C29 C30 C31 -0.4(10) . . . . ?
C29 C30 C31 C32 3.2(9) . . . . ?
C29 C30 C31 N8 -179.1(7) . . . . ?
C30 C31 C32 O4 176.5(5) . . . . ?
N8 C31 C32 O4 -1.3(8) . . . . ?
C30 C31 C32 C27 -4.2(8) . . . . ?
N8 C31 C32 C27 178.1(6) . . . . ?
C28 C27 C32 O4 -178.1(5) . . . . ?
C26 C27 C32 O4 2.4(8) . . . . ?
C28 C27 C32 C31 2.6(7) . . . . ?
C26 C27 C32 C31 -177.0(5) . . . . ?
C6 C7 N1 C8 -178.4(5) . . . . ?
C6 C7 N1 Tb1 -3.2(8) . . . . ?
C9 C8 N1 C7 129.9(5) . . . . ?
C9 C8 N1 Tb1 -46.1(4) . . . . ?
O2 Tb1 N1 C7 -171.9(4) . . . . ?
O1 Tb1 N1 C7 10.2(4) . . . . ?
O4 Tb1 N1 C7 -79.6(4) . . . . ?
O3 Tb1 N1 C7 118.4(4) . . . . ?
N3 Tb1 N1 C7 68.9(5) . . . . ?
N4 Tb1 N1 C7 -29.6(5) . . . . ?
N2 Tb1 N1 C7 -158.0(5) . . . . ?
O2 Tb1 N1 C8 3.4(4) . . . . ?
O1 Tb1 N1 C8 -174.5(3) . . . . ?
O4 Tb1 N1 C8 95.7(3) . . . . ?
O3 Tb1 N1 C8 -66.3(3) . . . . ?
N3 Tb1 N1 C8 -115.8(3) . . . . ?
N4 Tb1 N1 C8 145.7(3) . . . . ?
N2 Tb1 N1 C8 17.3(3) . . . . ?
C11 C10 N2 C9 177.6(5) . . . . ?
C11 C10 N2 Tb1 -1.0(8) . . . . ?
C8 C9 N2 C10 137.7(5) . . . . ?
C8 C9 N2 Tb1 -43.5(5) . . . . ?
O2 Tb1 N2 C10 3.3(4) . . . . ?
O1 Tb1 N2 C10 176.1(4) . . . . ?
O4 Tb1 N2 C10 107.6(4) . . . . ?
O3 Tb1 N2 C10 -87.8(4) . . . . ?
N1 Tb1 N2 C10 -167.1(4) . . . . ?
N3 Tb1 N2 C10 -41.9(5) . . . . ?
N4 Tb1 N2 C10 60.0(5) . . . . ?
O2 Tb1 N2 C9 -175.4(3) . . . . ?
O1 Tb1 N2 C9 -2.6(4) . . . . ?
O4 Tb1 N2 C9 -71.1(3) . . . . ?
O3 Tb1 N2 C9 93.5(3) . . . . ?
N1 Tb1 N2 C9 14.2(3) . . . . ?
N3 Tb1 N2 C9 139.4(3) . . . . ?
N4 Tb1 N2 C9 -118.7(3) . . . . ?
C22 C23 N3 C24 -177.5(4) . . . . ?
C22 C23 N3 Tb1 -13.9(7) . . . . ?
C25 C24 N3 C23 118.5(5) . . . . ?
C25 C24 N3 Tb1 -47.4(5) . . . . ?
O2 Tb1 N3 C23 -61.5(4) . . . . ?
O1 Tb1 N3 C23 137.6(4) . . . . ?
O4 Tb1 N3 C23 -149.4(4) . . . . ?
O3 Tb1 N3 C23 30.7(4) . . . . ?
N1 Tb1 N3 C23 82.1(4) . . . . ?
N4 Tb1 N3 C23 -145.9(4) . . . . ?
N2 Tb1 N3 C23 -17.7(5) . . . . ?
O2 Tb1 N3 C24 102.7(3) . . . . ?
O1 Tb1 N3 C24 -58.2(3) . . . . ?
O4 Tb1 N3 C24 14.8(4) . . . . ?
O3 Tb1 N3 C24 -165.2(3) . . . . ?
N1 Tb1 N3 C24 -113.7(3) . . . . ?
N4 Tb1 N3 C24 18.3(3) . . . . ?
N2 Tb1 N3 C24 146.4(3) . . . . ?
C27 C26 N4 C25 -178.9(5) . . . . ?
C27 C26 N4 Tb1 -14.5(8) . . . . ?
C24 C25 N4 C26 123.3(5) . . . . ?
C24 C25 N4 Tb1 -43.2(5) . . . . ?
O2 Tb1 N4 C26 129.4(5) . . . . ?
O1 Tb1 N4 C26 -65.5(4) . . . . ?
O4 Tb1 N4 C26 26.6(4) . . . . ?
O3 Tb1 N4 C26 -155.8(4) . . . . ?
N1 Tb1 N4 C26 -26.3(5) . . . . ?
N3 Tb1 N4 C26 -151.0(5) . . . . ?
N2 Tb1 N4 C26 75.8(5) . . . . ?
O2 Tb1 N4 C25 -65.8(3) . . . . ?
O1 Tb1 N4 C25 99.2(3) . . . . ?
O4 Tb1 N4 C25 -168.7(4) . . . . ?
O3 Tb1 N4 C25 8.9(4) . . . . ?
N1 Tb1 N4 C25 138.4(3) . . . . ?
N3 Tb1 N4 C25 13.8(3) . . . . ?
N2 Tb1 N4 C25 -119.5(3) . . . . ?
C3 C2 N5 O6 -31.1(11) . . . . ?
C1 C2 N5 O6 147.1(9) . . . . ?
C3 C2 N5 O5 139.7(9) . . . . ?
C1 C2 N5 O5 -42.1(10) . . . . ?
C14 C15 N6 O7 -142.5(6) . . . . ?
C16 C15 N6 O7 38.2(8) . . . . ?
C14 C15 N6 O8 37.6(7) . . . . ?
C16 C15 N6 O8 -141.7(5) . . . . ?
C19 C18 N7 O9 -34.1(8) . . . . ?
C17 C18 N7 O9 142.7(6) . . . . ?
C19 C18 N7 O10 141.2(6) . . . . ?
C17 C18 N7 O10 -42.0(8) . . . . ?
C30 C31 N8 O12 -36.5(11) . . . . ?
C32 C31 N8 O12 141.3(9) . . . . ?
C30 C31 N8 O11 137.8(8) . . . . ?
C32 C31 N8 O11 -44.4(11) . . . . ?
C34 C33 N9 C37 66.5(9) . . . . ?
C34 C33 N9 C35 -60.2(10) . . . . ?
C38 C37 N9 C33 60.3(9) . . . . ?
C38 C37 N9 C35 -170.1(7) . . . . ?
C36 C35 N9 C33 -51.5(9) . . . . ?
C36 C35 N9 C37 178.6(7) . . . . ?
C6 C1 O1 Tb1 27.6(8) . . . . ?
C2 C1 O1 Tb1 -153.8(4) . . . . ?
O2 Tb1 O1 C1 158.6(5) . . . . ?
O4 Tb1 O1 C1 56.9(5) . . . . ?
O3 Tb1 O1 C1 -94.8(5) . . . . ?
N1 Tb1 O1 C1 -24.2(5) . . . . ?
N3 Tb1 O1 C1 -162.2(5) . . . . ?
N4 Tb1 O1 C1 128.2(5) . . . . ?
N2 Tb1 O1 C1 -7.7(6) . . . . ?
C11 C16 O2 Tb1 7.2(8) . . . . ?
C15 C16 O2 Tb1 -174.6(3) . . . . ?
O1 Tb1 O2 C16 -177.4(4) . . . . ?
O4 Tb1 O2 C16 -78.9(5) . . . . ?
O3 Tb1 O2 C16 72.2(5) . . . . ?
N1 Tb1 O2 C16 6.5(6) . . . . ?
N3 Tb1 O2 C16 142.9(5) . . . . ?
N4 Tb1 O2 C16 -147.9(5) . . . . ?
N2 Tb1 O2 C16 -7.0(5) . . . . ?
C18 C17 O3 Tb1 -138.4(4) . . . . ?
C22 C17 O3 Tb1 43.1(6) . . . . ?
O2 Tb1 O3 C17 30.1(4) . . . . ?
O1 Tb1 O3 C17 -121.0(4) . . . . ?
O4 Tb1 O3 C17 133.6(4) . . . . ?
N1 Tb1 O3 C17 171.8(4) . . . . ?
N3 Tb1 O3 C17 -46.5(4) . . . . ?
N4 Tb1 O3 C17 -41.8(5) . . . . ?
N2 Tb1 O3 C17 101.9(4) . . . . ?
C31 C32 O4 Tb1 -148.3(4) . . . . ?
C27 C32 O4 Tb1 32.4(7) . . . . ?
O2 Tb1 O4 C32 -113.9(5) . . . . ?
O1 Tb1 O4 C32 36.1(5) . . . . ?
O3 Tb1 O4 C32 145.5(4) . . . . ?
N1 Tb1 O4 C32 108.0(5) . . . . ?
N3 Tb1 O4 C32 -34.4(5) . . . . ?
N4 Tb1 O4 C32 -37.8(5) . . . . ?
N2 Tb1 O4 C32 177.6(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.745
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.079
####################################################################### 
# 
# 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_20130225b_0m
_database_code_depnum_ccdc_archive 'CCDC 1404028'
_audit_update_record             
;
2015-06-01 deposited with the CCDC.
2015-12-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H24 Dy N8 O12, C6 H16 N, H2 O'
_chemical_formula_sum            'C38 H42 Dy N9 O13'
_chemical_formula_weight         995.31

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'
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'
H H 0.0000 0.0000 '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                   12.400(4)
_cell_length_b                   12.692(4)
_cell_length_c                   15.776(5)
_cell_angle_alpha                69.934(5)
_cell_angle_beta                 75.538(5)
_cell_angle_gamma                72.017(5)
_cell_volume                     2189.3(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2034
_cell_measurement_theta_min      2.771
_cell_measurement_theta_max      19.817

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1006
_exptl_absorpt_coefficient_mu    1.778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.495
_exptl_absorpt_correction_T_max  0.700
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12160
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_av_sigmaI/netI    0.0945
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.76
_diffrn_reflns_theta_max         25.00
_reflns_number_total             7667
_reflns_number_gt                5292
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1039P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7667
_refine_ls_number_parameters     629
_refine_ls_number_restraints     236
_refine_ls_R_factor_all          0.1047
_refine_ls_R_factor_gt           0.0679
_refine_ls_wR_factor_ref         0.1803
_refine_ls_wR_factor_gt          0.1573
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_restrained_S_all      0.987
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.23068(3) 0.81545(4) 0.26774(3) 0.05251(18) Uani 1 1 d . A .
C1 C -0.0096(8) 0.7482(8) 0.2612(7) 0.065(2) Uani 1 1 d . A .
C2 C -0.1126(9) 0.7168(9) 0.3145(8) 0.069(3) Uani 1 1 d . . .
C3 C -0.2029(10) 0.7196(10) 0.2763(11) 0.091(4) Uani 1 1 d . A .
H3 H -0.2674 0.6968 0.3140 0.109 Uiso 1 1 calc R . .
C4 C -0.1979(11) 0.7556(11) 0.1837(11) 0.099(4) Uani 1 1 d . . .
H4 H -0.2579 0.7559 0.1581 0.119 Uiso 1 1 calc R A .
C5 C -0.1022(11) 0.7919(10) 0.1280(9) 0.087(3) Uani 1 1 d . A .
H5 H -0.0986 0.8161 0.0649 0.104 Uiso 1 1 calc R . .
C6 C -0.0116(8) 0.7928(9) 0.1650(7) 0.066(3) Uani 1 1 d . . .
C7 C 0.0796(9) 0.8398(9) 0.1003(7) 0.074(3) Uani 1 1 d . A .
H7 H 0.0721 0.8632 0.0389 0.088 Uiso 1 1 calc R . .
C8 C 0.2475(9) 0.9053(9) 0.0380(6) 0.071(3) Uani 1 1 d . A .
H8A H 0.2131 0.9330 -0.0169 0.086 Uiso 1 1 calc R . .
H8B H 0.3188 0.8480 0.0291 0.086 Uiso 1 1 calc R . .
C9 C 0.2708(10) 1.0048(9) 0.0567(7) 0.076(3) Uani 1 1 d . A .
H9A H 0.3214 1.0417 0.0051 0.091 Uiso 1 1 calc R . .
H9B H 0.1994 1.0619 0.0657 0.091 Uiso 1 1 calc R . .
C10 C 0.4108(8) 0.9975(8) 0.1366(6) 0.061(2) Uani 1 1 d . A .
H10 H 0.4340 1.0478 0.0809 0.073 Uiso 1 1 calc R . .
C11 C 0.4757(8) 0.9720(8) 0.2094(6) 0.059(2) Uani 1 1 d . . .
C12 C 0.5637(9) 1.0252(9) 0.1886(8) 0.077(3) Uani 1 1 d . . .
H12 H 0.5797 1.0721 0.1294 0.092 Uiso 1 1 calc R . .
C13 C 0.6297(10) 1.0116(11) 0.2527(9) 0.088(3) Uani 1 1 d . . .
H13 H 0.6876 1.0504 0.2372 0.105 Uiso 1 1 calc R . .
C14 C 0.6080(8) 0.9399(10) 0.3391(8) 0.074(3) Uani 1 1 d . . .
H14 H 0.6503 0.9304 0.3834 0.089 Uiso 1 1 calc R . .
C15 C 0.5238(8) 0.8822(8) 0.3598(7) 0.063(2) Uani 1 1 d . . .
C16 C 0.4507(7) 0.8947(7) 0.2977(6) 0.056(2) Uani 1 1 d . A .
C17 C 0.4735(8) 0.6269(7) 0.2183(7) 0.057(2) Uani 1 1 d . A .
C18 C 0.5760(8) 0.6157(8) 0.1534(7) 0.066(3) Uani 1 1 d . . .
C19 C 0.6814(9) 0.5435(10) 0.1743(9) 0.082(3) Uani 1 1 d . B .
H19 H 0.7456 0.5397 0.1289 0.098 Uiso 1 1 calc R . .
C20 C 0.6893(10) 0.4776(9) 0.2632(9) 0.083(3) Uani 1 1 d . . .
H20 H 0.7594 0.4292 0.2788 0.100 Uiso 1 1 calc R B .
C21 C 0.5936(10) 0.4837(9) 0.3284(8) 0.079(3) Uani 1 1 d . B .
H21 H 0.5995 0.4374 0.3880 0.095 Uiso 1 1 calc R . .
C22 C 0.4874(8) 0.5567(8) 0.3088(7) 0.059(2) Uani 1 1 d . . .
C23 C 0.3938(9) 0.5574(8) 0.3849(6) 0.066(3) Uani 1 1 d . A .
H23 H 0.4075 0.5006 0.4396 0.079 Uiso 1 1 calc R . .
C24 C 0.2145(9) 0.6118(10) 0.4727(7) 0.078(3) Uani 1 1 d . A .
H24A H 0.2505 0.5471 0.5195 0.093 Uiso 1 1 calc R . .
H24B H 0.1460 0.5960 0.4657 0.093 Uiso 1 1 calc R . .
C25 C 0.1832(10) 0.7231(11) 0.4999(7) 0.084(3) Uani 1 1 d . A .
H25A H 0.1298 0.7161 0.5570 0.100 Uiso 1 1 calc R . .
H25B H 0.2515 0.7376 0.5084 0.100 Uiso 1 1 calc R . .
C26 C 0.0304(11) 0.8767(12) 0.4505(8) 0.091(4) Uani 1 1 d . A .
H26 H -0.0005 0.8543 0.5122 0.109 Uiso 1 1 calc R . .
C27 C -0.0415(9) 0.9725(10) 0.3942(9) 0.075(3) Uani 1 1 d . . .
C28 C -0.1535(10) 1.0164(14) 0.4315(12) 0.108(5) Uani 1 1 d . . .
H28 H -0.1780 0.9810 0.4926 0.130 Uiso 1 1 calc R . .
C29 C -0.2275(13) 1.1038(17) 0.3874(15) 0.128(6) Uani 1 1 d . . .
H29 H -0.3021 1.1269 0.4165 0.153 Uiso 1 1 calc R . .
C30 C -0.1928(11) 1.1631(13) 0.2945(14) 0.116(6) Uani 1 1 d . C .
H30 H -0.2441 1.2248 0.2617 0.139 Uiso 1 1 calc R . .
C31 C -0.0783(10) 1.1256(10) 0.2534(10) 0.086(3) Uani 1 1 d D . .
C32 C 0.0006(9) 1.0261(10) 0.3009(9) 0.077(3) Uani 1 1 d . A .
C33 C 0.2501(15) 0.2697(14) 0.2268(11) 0.126(5) Uani 1 1 d . . .
H33A H 0.3229 0.2469 0.1892 0.151 Uiso 1 1 calc R . .
H33B H 0.1907 0.2930 0.1894 0.151 Uiso 1 1 calc R . .
C34 C 0.2309(17) 0.1669(15) 0.3023(15) 0.180(9) Uani 1 1 d . . .
H34A H 0.2836 0.1470 0.3440 0.270 Uiso 1 1 calc R . .
H34B H 0.2430 0.1035 0.2783 0.270 Uiso 1 1 calc R . .
H34C H 0.1535 0.1833 0.3340 0.270 Uiso 1 1 calc R . .
C35 C 0.1398(16) 0.4218(14) 0.3081(12) 0.132(6) Uani 1 1 d . . .
H35A H 0.1318 0.3689 0.3693 0.159 Uiso 1 1 calc R . .
H35B H 0.1451 0.4942 0.3130 0.159 Uiso 1 1 calc R . .
C36 C 0.0404(16) 0.4421(17) 0.2680(16) 0.176(9) Uani 1 1 d . . .
H36A H 0.0549 0.4808 0.2038 0.264 Uiso 1 1 calc R . .
H36B H -0.0244 0.4896 0.2969 0.264 Uiso 1 1 calc R . .
H36C H 0.0243 0.3695 0.2766 0.264 Uiso 1 1 calc R . .
C37 C 0.3517(18) 0.3538(19) 0.2975(15) 0.171(8) Uani 1 1 d . . .
H37A H 0.3487 0.2925 0.3548 0.205 Uiso 1 1 calc R . .
H37B H 0.3462 0.4247 0.3108 0.205 Uiso 1 1 calc R . .
C38 C 0.4668(15) 0.3221(16) 0.2334(17) 0.176(9) Uani 1 1 d . . .
H38A H 0.4774 0.2461 0.2284 0.265 Uiso 1 1 calc R . .
H38B H 0.5294 0.3233 0.2583 0.265 Uiso 1 1 calc R . .
H38C H 0.4645 0.3773 0.1739 0.265 Uiso 1 1 calc R . .
N1 N 0.1682(6) 0.8528(7) 0.1175(5) 0.062(2) Uani 1 1 d . . .
N2 N 0.3257(7) 0.9586(6) 0.1403(5) 0.0613(19) Uani 1 1 d . . .
N3 N 0.2948(7) 0.6274(7) 0.3852(5) 0.0615(19) Uani 1 1 d . . .
N4 N 0.1310(7) 0.8177(8) 0.4279(5) 0.069(2) Uani 1 1 d . . .
N5 N -0.1260(9) 0.6809(10) 0.4126(8) 0.097(2) Uani 0.602(17) 1 d PDU A 1
O5 O -0.0439(12) 0.6161(17) 0.4529(10) 0.120(5) Uani 0.602(17) 1 d PDU A 1
O6 O -0.2192(14) 0.6998(19) 0.4616(14) 0.123(6) Uani 0.602(17) 1 d PDU A 1
N5' N -0.1260(9) 0.6809(10) 0.4126(8) 0.097(2) Uani 0.398(17) 1 d PDU A 2
O5' O -0.081(2) 0.722(2) 0.4517(15) 0.106(5) Uani 0.398(17) 1 d PDU A 2
O6' O -0.213(2) 0.646(3) 0.449(2) 0.115(6) Uani 0.398(17) 1 d PDU A 2
N6 N 0.5073(8) 0.7981(10) 0.4525(7) 0.084(3) Uani 1 1 d . . .
N7 N 0.5746(9) 0.6848(10) 0.0573(7) 0.094(3) Uani 0.863(12) 1 d PDU B 1
O9 O 0.6570(10) 0.7219(12) 0.0134(8) 0.119(4) Uani 0.863(12) 1 d PDU B 1
O10 O 0.4940(9) 0.6967(11) 0.0211(6) 0.113(4) Uani 0.863(12) 1 d PDU B 1
N7' N 0.5746(9) 0.6848(10) 0.0573(7) 0.094(3) Uani 0.137(12) 1 d PDU B 2
O9' O 0.527(5) 0.787(2) 0.042(4) 0.108(8) Uani 0.137(12) 1 d PDU B 2
O10' O 0.644(5) 0.649(4) -0.003(3) 0.109(9) Uani 0.137(12) 1 d PDU B 2
N8 N -0.044(4) 1.184(2) 0.1597(16) 0.136(5) Uani 0.735(14) 1 d PDU C 1
O11 O 0.0500(16) 1.2089(14) 0.1361(12) 0.146(5) Uani 0.735(14) 1 d PDU C 1
O12 O -0.1116(16) 1.2192(17) 0.1080(12) 0.161(5) Uani 0.735(14) 1 d PDU C 1
N8' N -0.042(12) 1.188(4) 0.161(4) 0.141(6) Uani 0.265(14) 1 d PDU C 2
O11' O -0.019(4) 1.125(4) 0.111(3) 0.147(7) Uani 0.265(14) 1 d PDU C 2
O12' O -0.080(4) 1.290(4) 0.139(3) 0.153(8) Uani 0.265(14) 1 d PDU C 2
N9 N 0.2516(9) 0.3700(9) 0.2495(8) 0.094(3) Uani 1 1 d . . .
H9C H 0.2603 0.4259 0.1955 0.113 Uiso 1 1 calc R . .
O1 O 0.0793(6) 0.7364(6) 0.2962(4) 0.0681(17) Uani 1 1 d . . .
O2 O 0.3675(5) 0.8469(5) 0.3211(4) 0.0610(16) Uani 1 1 d . . .
O3 O 0.3752(5) 0.6927(5) 0.1963(4) 0.0607(15) Uani 1 1 d . . .
O4 O 0.1020(5) 0.9896(6) 0.2601(5) 0.0734(18) Uani 1 1 d . . .
O7 O 0.4852(9) 0.7113(9) 0.4632(6) 0.120(4) Uani 1 1 d . . .
O8 O 0.5176(9) 0.8280(10) 0.5182(6) 0.125(3) Uani 1 1 d . . .
O1W O 0.2844(12) 0.5678(10) 0.1176(10) 0.089(5) Uani 0.595(19) 1 d P D 1
H1WA H 0.2555 0.6378 0.1178 0.107 Uiso 0.595(19) 1 d PR D 1
H1WB H 0.3562 0.5507 0.1182 0.133 Uiso 0.595(19) 1 d PR D 1
O1W' O 0.294(2) 0.590(2) 0.0285(17) 0.114(10) Uani 0.405(19) 1 d P D 2
H1WC H 0.2989 0.6451 0.0452 0.137 Uiso 0.405(19) 1 d PR D 2
H1WD H 0.2234 0.5899 0.0360 0.171 Uiso 0.405(19) 1 d PR D 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O2 2.260(6) . ?
Dy1 O1 2.272(6) . ?
Dy1 O4 2.277(6) . ?
Dy1 O3 2.319(6) . ?
Dy1 N3 2.508(8) . ?
Dy1 N1 2.522(7) . ?
Dy1 N2 2.522(7) . ?
Dy1 N4 2.527(8) . ?
C1 O1 1.300(11) . ?
C1 C6 1.429(14) . ?
C1 C2 1.430(14) . ?
C2 C3 1.383(15) . ?
C2 N5 1.437(15) . ?
C3 C4 1.365(18) . ?
C3 H3 0.9300 . ?
C4 C5 1.389(17) . ?
C4 H4 0.9300 . ?
C5 C6 1.395(14) . ?
C5 H5 0.9300 . ?
C6 C7 1.449(14) . ?
C7 N1 1.265(12) . ?
C7 H7 0.9300 . ?
C8 N1 1.483(12) . ?
C8 C9 1.512(15) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N2 1.490(12) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.278(12) . ?
C10 C11 1.454(13) . ?
C10 H10 0.9300 . ?
C11 C12 1.371(13) . ?
C11 C16 1.426(13) . ?
C12 C13 1.389(16) . ?
C12 H12 0.9300 . ?
C13 C14 1.370(15) . ?
C13 H13 0.9300 . ?
C14 C15 1.368(13) . ?
C14 H14 0.9300 . ?
C15 C16 1.432(13) . ?
C15 N6 1.496(13) . ?
C16 O2 1.271(10) . ?
C17 O3 1.299(10) . ?
C17 C22 1.421(13) . ?
C17 C18 1.422(13) . ?
C18 C19 1.387(14) . ?
C18 N7 1.469(14) . ?
C19 C20 1.375(15) . ?
C19 H19 0.9300 . ?
C20 C21 1.364(15) . ?
C20 H20 0.9300 . ?
C21 C22 1.394(13) . ?
C21 H21 0.9300 . ?
C22 C23 1.446(13) . ?
C23 N3 1.274(12) . ?
C23 H23 0.9300 . ?
C24 N3 1.478(12) . ?
C24 C25 1.526(15) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 N4 1.449(13) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 N4 1.276(14) . ?
C26 C27 1.431(17) . ?
C26 H26 0.9300 . ?
C27 C28 1.387(16) . ?
C27 C32 1.432(16) . ?
C28 C29 1.31(2) . ?
C28 H28 0.9300 . ?
C29 C30 1.42(2) . ?
C29 H29 0.9300 . ?
C30 C31 1.413(17) . ?
C30 H30 0.9300 . ?
C31 N8' 1.43(2) . ?
C31 N8 1.43(2) . ?
C31 C32 1.438(15) . ?
C32 O4 1.285(12) . ?
C33 N9 1.441(16) . ?
C33 C34 1.47(2) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 C36 1.44(2) . ?
C35 N9 1.557(18) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 N9 1.537(19) . ?
C37 C38 1.56(2) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
N5 O6 1.225(14) . ?
N5 O5 1.252(14) . ?
N6 O7 1.164(12) . ?
N6 O8 1.264(13) . ?
N7 O9 1.211(13) . ?
N7 O10 1.216(14) . ?
N8 O12 1.19(5) . ?
N8 O11 1.23(6) . ?
N8' O12' 1.19(5) . ?
N8' O11' 1.23(6) . ?
N9 H9C 0.9100 . ?
O1W H1WA 0.8499 . ?
O1W H1WB 0.8501 . ?
O1W H1WC 1.2391 . ?
O1W' H1WC 0.8500 . ?
O1W' H1WD 0.8501 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Dy1 O1 148.9(2) . . ?
O2 Dy1 O4 98.1(2) . . ?
O1 Dy1 O4 87.8(2) . . ?
O2 Dy1 O3 88.1(2) . . ?
O1 Dy1 O3 101.9(2) . . ?
O4 Dy1 O3 150.0(2) . . ?
O2 Dy1 N3 76.5(2) . . ?
O1 Dy1 N3 79.0(2) . . ?
O4 Dy1 N3 139.0(3) . . ?
O3 Dy1 N3 71.0(2) . . ?
O2 Dy1 N1 139.3(2) . . ?
O1 Dy1 N1 71.8(2) . . ?
O4 Dy1 N1 80.4(3) . . ?
O3 Dy1 N1 76.0(2) . . ?
N3 Dy1 N1 129.7(3) . . ?
O2 Dy1 N2 71.9(2) . . ?
O1 Dy1 N2 138.7(2) . . ?
O4 Dy1 N2 75.3(2) . . ?
O3 Dy1 N2 78.9(2) . . ?
N3 Dy1 N2 136.6(3) . . ?
N1 Dy1 N2 68.4(3) . . ?
O2 Dy1 N4 79.2(2) . . ?
O1 Dy1 N4 73.8(3) . . ?
O4 Dy1 N4 71.5(3) . . ?
O3 Dy1 N4 138.4(2) . . ?
N3 Dy1 N4 67.5(3) . . ?
N1 Dy1 N4 135.9(3) . . ?
N2 Dy1 N4 131.8(3) . . ?
O1 C1 C6 122.2(9) . . ?
O1 C1 C2 123.5(10) . . ?
C6 C1 C2 114.3(9) . . ?
C3 C2 C1 123.2(11) . . ?
C3 C2 N5 116.9(11) . . ?
C1 C2 N5 119.8(9) . . ?
C4 C3 C2 120.4(12) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 119.3(11) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C4 C5 C6 121.2(12) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C5 C6 C1 121.2(11) . . ?
C5 C6 C7 116.0(10) . . ?
C1 C6 C7 122.8(9) . . ?
N1 C7 C6 127.5(9) . . ?
N1 C7 H7 116.2 . . ?
C6 C7 H7 116.2 . . ?
N1 C8 C9 108.3(8) . . ?
N1 C8 H8A 110.0 . . ?
C9 C8 H8A 110.0 . . ?
N1 C8 H8B 110.0 . . ?
C9 C8 H8B 110.0 . . ?
H8A C8 H8B 108.4 . . ?
N2 C9 C8 108.5(8) . . ?
N2 C9 H9A 110.0 . . ?
C8 C9 H9A 110.0 . . ?
N2 C9 H9B 110.0 . . ?
C8 C9 H9B 110.0 . . ?
H9A C9 H9B 108.4 . . ?
N2 C10 C11 127.5(8) . . ?
N2 C10 H10 116.3 . . ?
C11 C10 H10 116.3 . . ?
C12 C11 C16 121.2(9) . . ?
C12 C11 C10 116.5(9) . . ?
C16 C11 C10 122.2(9) . . ?
C11 C12 C13 122.4(10) . . ?
C11 C12 H12 118.8 . . ?
C13 C12 H12 118.8 . . ?
C14 C13 C12 118.7(10) . . ?
C14 C13 H13 120.7 . . ?
C12 C13 H13 120.7 . . ?
C15 C14 C13 119.6(10) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C14 C15 C16 124.5(9) . . ?
C14 C15 N6 118.5(9) . . ?
C16 C15 N6 117.0(9) . . ?
O2 C16 C11 123.4(8) . . ?
O2 C16 C15 122.9(8) . . ?
C11 C16 C15 113.5(8) . . ?
O3 C17 C22 122.9(8) . . ?
O3 C17 C18 123.1(8) . . ?
C22 C17 C18 114.0(8) . . ?
C19 C18 C17 124.4(10) . . ?
C19 C18 N7 115.8(10) . . ?
C17 C18 N7 119.8(9) . . ?
C20 C19 C18 118.9(10) . . ?
C20 C19 H19 120.5 . . ?
C18 C19 H19 120.5 . . ?
C21 C20 C19 119.4(9) . . ?
C21 C20 H20 120.3 . . ?
C19 C20 H20 120.3 . . ?
C20 C21 C22 122.4(10) . . ?
C20 C21 H21 118.8 . . ?
C22 C21 H21 118.8 . . ?
C21 C22 C17 120.8(9) . . ?
C21 C22 C23 116.7(9) . . ?
C17 C22 C23 122.4(8) . . ?
N3 C23 C22 127.2(8) . . ?
N3 C23 H23 116.4 . . ?
C22 C23 H23 116.4 . . ?
N3 C24 C25 107.8(8) . . ?
N3 C24 H24A 110.1 . . ?
C25 C24 H24A 110.1 . . ?
N3 C24 H24B 110.1 . . ?
C25 C24 H24B 110.1 . . ?
H24A C24 H24B 108.5 . . ?
N4 C25 C24 108.5(9) . . ?
N4 C25 H25A 110.0 . . ?
C24 C25 H25A 110.0 . . ?
N4 C25 H25B 110.0 . . ?
C24 C25 H25B 110.0 . . ?
H25A C25 H25B 108.4 . . ?
N4 C26 C27 129.0(11) . . ?
N4 C26 H26 115.5 . . ?
C27 C26 H26 115.5 . . ?
C28 C27 C26 119.3(13) . . ?
C28 C27 C32 119.2(13) . . ?
C26 C27 C32 121.4(10) . . ?
C29 C28 C27 125.2(17) . . ?
C29 C28 H28 117.4 . . ?
C27 C28 H28 117.4 . . ?
C28 C29 C30 119.4(15) . . ?
C28 C29 H29 120.3 . . ?
C30 C29 H29 120.3 . . ?
C31 C30 C29 118.3(14) . . ?
C31 C30 H30 120.9 . . ?
C29 C30 H30 120.9 . . ?
C30 C31 N8' 118(4) . . ?
C30 C31 N8 118.2(19) . . ?
N8' C31 N8 3(9) . . ?
C30 C31 C32 121.9(14) . . ?
N8' C31 C32 120(4) . . ?
N8 C31 C32 119.8(17) . . ?
O4 C32 C27 123.5(10) . . ?
O4 C32 C31 120.6(12) . . ?
C27 C32 C31 115.9(10) . . ?
N9 C33 C34 118.0(14) . . ?
N9 C33 H33A 107.8 . . ?
C34 C33 H33A 107.8 . . ?
N9 C33 H33B 107.8 . . ?
C34 C33 H33B 107.8 . . ?
H33A C33 H33B 107.1 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36 C35 N9 111.1(15) . . ?
C36 C35 H35A 109.4 . . ?
N9 C35 H35A 109.4 . . ?
C36 C35 H35B 109.4 . . ?
N9 C35 H35B 109.4 . . ?
H35A C35 H35B 108.0 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N9 C37 C38 108.6(15) . . ?
N9 C37 H37A 110.0 . . ?
C38 C37 H37A 110.0 . . ?
N9 C37 H37B 110.0 . . ?
C38 C37 H37B 110.0 . . ?
H37A C37 H37B 108.3 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C7 N1 C8 116.6(8) . . ?
C7 N1 Dy1 130.9(7) . . ?
C8 N1 Dy1 112.4(6) . . ?
C10 N2 C9 116.1(8) . . ?
C10 N2 Dy1 130.8(6) . . ?
C9 N2 Dy1 113.1(6) . . ?
C23 N3 C24 116.9(8) . . ?
C23 N3 Dy1 128.1(6) . . ?
C24 N3 Dy1 113.5(6) . . ?
C26 N4 C25 117.0(9) . . ?
C26 N4 Dy1 126.6(8) . . ?
C25 N4 Dy1 114.6(6) . . ?
O6 N5 O5 115.8(16) . . ?
O6 N5 C2 122.9(15) . . ?
O5 N5 C2 120.8(12) . . ?
O7 N6 O8 122.5(11) . . ?
O7 N6 C15 121.7(10) . . ?
O8 N6 C15 115.8(11) . . ?
O9 N7 O10 120.7(12) . . ?
O9 N7 C18 119.7(11) . . ?
O10 N7 C18 119.3(11) . . ?
O12 N8 O11 121(2) . . ?
O12 N8 C31 119(4) . . ?
O11 N8 C31 119(4) . . ?
O12' N8' O11' 125(9) . . ?
O12' N8' C31 117(4) . . ?
O11' N8' C31 110(6) . . ?
C33 N9 C37 115.1(13) . . ?
C33 N9 C35 115.5(12) . . ?
C37 N9 C35 106.7(13) . . ?
C33 N9 H9C 106.3 . . ?
C37 N9 H9C 106.3 . . ?
C35 N9 H9C 106.3 . . ?
C1 O1 Dy1 140.4(6) . . ?
C16 O2 Dy1 143.7(6) . . ?
C17 O3 Dy1 131.6(6) . . ?
C32 O4 Dy1 136.4(7) . . ?
H1WA O1W H1WB 109.5 . . ?
H1WA O1W H1WC 61.7 . . ?
H1WB O1W H1WC 88.5 . . ?
H1WC O1W' H1WD 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 -173.9(10) . . . . ?
C6 C1 C2 C3 5.3(15) . . . . ?
O1 C1 C2 N5 6.5(15) . . . . ?
C6 C1 C2 N5 -174.3(10) . . . . ?
C1 C2 C3 C4 -1.3(18) . . . . ?
N5 C2 C3 C4 178.4(11) . . . . ?
C2 C3 C4 C5 -1.4(19) . . . . ?
C3 C4 C5 C6 -0.3(18) . . . . ?
C4 C5 C6 C1 4.8(16) . . . . ?
C4 C5 C6 C7 -175.9(10) . . . . ?
O1 C1 C6 C5 172.3(9) . . . . ?
C2 C1 C6 C5 -6.9(14) . . . . ?
O1 C1 C6 C7 -6.9(15) . . . . ?
C2 C1 C6 C7 173.9(9) . . . . ?
C5 C6 C7 N1 177.7(10) . . . . ?
C1 C6 C7 N1 -3.0(17) . . . . ?
N1 C8 C9 N2 60.8(11) . . . . ?
N2 C10 C11 C12 -179.7(9) . . . . ?
N2 C10 C11 C16 1.1(15) . . . . ?
C16 C11 C12 C13 -3.1(16) . . . . ?
C10 C11 C12 C13 177.7(10) . . . . ?
C11 C12 C13 C14 1.8(18) . . . . ?
C12 C13 C14 C15 1.1(17) . . . . ?
C13 C14 C15 C16 -2.8(16) . . . . ?
C13 C14 C15 N6 175.7(10) . . . . ?
C12 C11 C16 O2 177.3(9) . . . . ?
C10 C11 C16 O2 -3.6(14) . . . . ?
C12 C11 C16 C15 1.3(13) . . . . ?
C10 C11 C16 C15 -179.5(8) . . . . ?
C14 C15 C16 O2 -174.4(9) . . . . ?
N6 C15 C16 O2 7.0(13) . . . . ?
C14 C15 C16 C11 1.6(13) . . . . ?
N6 C15 C16 C11 -177.0(8) . . . . ?
O3 C17 C18 C19 -178.0(9) . . . . ?
C22 C17 C18 C19 0.2(14) . . . . ?
O3 C17 C18 N7 2.9(15) . . . . ?
C22 C17 C18 N7 -178.9(9) . . . . ?
C17 C18 C19 C20 -0.1(17) . . . . ?
N7 C18 C19 C20 179.1(11) . . . . ?
C18 C19 C20 C21 0.7(18) . . . . ?
C19 C20 C21 C22 -1.5(18) . . . . ?
C20 C21 C22 C17 1.6(17) . . . . ?
C20 C21 C22 C23 -178.1(10) . . . . ?
O3 C17 C22 C21 177.2(9) . . . . ?
C18 C17 C22 C21 -0.9(13) . . . . ?
O3 C17 C22 C23 -3.1(14) . . . . ?
C18 C17 C22 C23 178.8(9) . . . . ?
C21 C22 C23 N3 170.1(10) . . . . ?
C17 C22 C23 N3 -9.5(16) . . . . ?
N3 C24 C25 N4 59.1(11) . . . . ?
N4 C26 C27 C28 173.2(12) . . . . ?
N4 C26 C27 C32 -8.7(19) . . . . ?
C26 C27 C28 C29 179.7(14) . . . . ?
C32 C27 C28 C29 1(2) . . . . ?
C27 C28 C29 C30 -2(2) . . . . ?
C28 C29 C30 C31 -1(2) . . . . ?
C29 C30 C31 N8' -178(7) . . . . ?
C29 C30 C31 N8 179(3) . . . . ?
C29 C30 C31 C32 3.7(18) . . . . ?
C28 C27 C32 O4 -178.2(10) . . . . ?
C26 C27 C32 O4 3.7(16) . . . . ?
C28 C27 C32 C31 1.5(15) . . . . ?
C26 C27 C32 C31 -176.6(10) . . . . ?
C30 C31 C32 O4 175.7(10) . . . . ?
N8' C31 C32 O4 -3(8) . . . . ?
N8 C31 C32 O4 0(3) . . . . ?
C30 C31 C32 C27 -4.1(15) . . . . ?
N8' C31 C32 C27 177(8) . . . . ?
N8 C31 C32 C27 -179(3) . . . . ?
C6 C7 N1 C8 -179.0(9) . . . . ?
C6 C7 N1 Dy1 -3.2(16) . . . . ?
C9 C8 N1 C7 128.7(10) . . . . ?
C9 C8 N1 Dy1 -47.9(9) . . . . ?
O2 Dy1 N1 C7 -171.2(8) . . . . ?
O1 Dy1 N1 C7 11.1(9) . . . . ?
O4 Dy1 N1 C7 -79.8(9) . . . . ?
O3 Dy1 N1 C7 118.8(9) . . . . ?
N3 Dy1 N1 C7 68.8(10) . . . . ?
N2 Dy1 N1 C7 -157.8(10) . . . . ?
N4 Dy1 N1 C7 -29.3(11) . . . . ?
O2 Dy1 N1 C8 4.8(8) . . . . ?
O1 Dy1 N1 C8 -173.0(7) . . . . ?
O4 Dy1 N1 C8 96.1(6) . . . . ?
O3 Dy1 N1 C8 -65.2(6) . . . . ?
N3 Dy1 N1 C8 -115.3(6) . . . . ?
N2 Dy1 N1 C8 18.2(6) . . . . ?
N4 Dy1 N1 C8 146.6(6) . . . . ?
C11 C10 N2 C9 176.5(9) . . . . ?
C11 C10 N2 Dy1 -2.9(14) . . . . ?
C8 C9 N2 C10 136.5(9) . . . . ?
C8 C9 N2 Dy1 -44.0(10) . . . . ?
O2 Dy1 N2 C10 4.3(8) . . . . ?
O1 Dy1 N2 C10 177.2(7) . . . . ?
O4 Dy1 N2 C10 108.1(8) . . . . ?
O3 Dy1 N2 C10 -87.4(8) . . . . ?
N3 Dy1 N2 C10 -41.0(10) . . . . ?
N1 Dy1 N2 C10 -166.6(9) . . . . ?
N4 Dy1 N2 C10 60.4(9) . . . . ?
O2 Dy1 N2 C9 -175.1(7) . . . . ?
O1 Dy1 N2 C9 -2.1(8) . . . . ?
O4 Dy1 N2 C9 -71.2(6) . . . . ?
O3 Dy1 N2 C9 93.2(7) . . . . ?
N3 Dy1 N2 C9 139.6(6) . . . . ?
N1 Dy1 N2 C9 14.1(6) . . . . ?
N4 Dy1 N2 C9 -118.9(7) . . . . ?
C22 C23 N3 C24 -178.6(9) . . . . ?
C22 C23 N3 Dy1 -13.6(15) . . . . ?
C25 C24 N3 C23 119.9(10) . . . . ?
C25 C24 N3 Dy1 -47.2(10) . . . . ?
O2 Dy1 N3 C23 -63.1(8) . . . . ?
O1 Dy1 N3 C23 136.3(8) . . . . ?
O4 Dy1 N3 C23 -150.0(8) . . . . ?
O3 Dy1 N3 C23 29.6(8) . . . . ?
N1 Dy1 N3 C23 81.4(9) . . . . ?
N2 Dy1 N3 C23 -19.1(10) . . . . ?
N4 Dy1 N3 C23 -146.8(9) . . . . ?
O2 Dy1 N3 C24 102.3(7) . . . . ?
O1 Dy1 N3 C24 -58.3(6) . . . . ?
O4 Dy1 N3 C24 15.4(8) . . . . ?
O3 Dy1 N3 C24 -165.0(7) . . . . ?
N1 Dy1 N3 C24 -113.2(7) . . . . ?
N2 Dy1 N3 C24 146.3(6) . . . . ?
N4 Dy1 N3 C24 18.6(6) . . . . ?
C27 C26 N4 C25 -179.0(11) . . . . ?
C27 C26 N4 Dy1 -14.7(17) . . . . ?
C24 C25 N4 C26 123.0(10) . . . . ?
C24 C25 N4 Dy1 -43.1(10) . . . . ?
O2 Dy1 N4 C26 129.6(9) . . . . ?
O1 Dy1 N4 C26 -66.1(9) . . . . ?
O4 Dy1 N4 C26 27.1(9) . . . . ?
O3 Dy1 N4 C26 -155.8(8) . . . . ?
N3 Dy1 N4 C26 -150.7(10) . . . . ?
N1 Dy1 N4 C26 -26.2(11) . . . . ?
N2 Dy1 N4 C26 76.1(10) . . . . ?
O2 Dy1 N4 C25 -65.9(7) . . . . ?
O1 Dy1 N4 C25 98.5(7) . . . . ?
O4 Dy1 N4 C25 -168.3(8) . . . . ?
O3 Dy1 N4 C25 8.8(9) . . . . ?
N3 Dy1 N4 C25 13.9(7) . . . . ?
N1 Dy1 N4 C25 138.3(7) . . . . ?
N2 Dy1 N4 C25 -119.3(7) . . . . ?
C3 C2 N5 O6 -32(2) . . . . ?
C1 C2 N5 O6 147.7(17) . . . . ?
C3 C2 N5 O5 139.6(16) . . . . ?
C1 C2 N5 O5 -40.8(19) . . . . ?
C14 C15 N6 O7 -141.7(12) . . . . ?
C16 C15 N6 O7 37.0(15) . . . . ?
C14 C15 N6 O8 39.1(14) . . . . ?
C16 C15 N6 O8 -142.2(10) . . . . ?
C19 C18 N7 O9 -35.6(17) . . . . ?
C17 C18 N7 O9 143.6(13) . . . . ?
C19 C18 N7 O10 139.1(13) . . . . ?
C17 C18 N7 O10 -41.7(17) . . . . ?
C30 C31 N8 O12 -35(4) . . . . ?
N8' C31 N8 O12 -128(100) . . . . ?
C32 C31 N8 O12 140(2) . . . . ?
C30 C31 N8 O11 136.9(19) . . . . ?
N8' C31 N8 O11 44(100) . . . . ?
C32 C31 N8 O11 -48(4) . . . . ?
C30 C31 N8' O12' 36(18) . . . . ?
N8 C31 N8' O12' 125(100) . . . . ?
C32 C31 N8' O12' -145(11) . . . . ?
C30 C31 N8' O11' -115(7) . . . . ?
N8 C31 N8' O11' -26(100) . . . . ?
C32 C31 N8' O11' 64(14) . . . . ?
C34 C33 N9 C37 66(2) . . . . ?
C34 C33 N9 C35 -59(2) . . . . ?
C38 C37 N9 C33 60.0(19) . . . . ?
C38 C37 N9 C35 -170.5(14) . . . . ?
C36 C35 N9 C33 -52(2) . . . . ?
C36 C35 N9 C37 179.1(16) . . . . ?
C6 C1 O1 Dy1 28.4(15) . . . . ?
C2 C1 O1 Dy1 -152.4(8) . . . . ?
O2 Dy1 O1 C1 157.5(9) . . . . ?
O4 Dy1 O1 C1 55.3(10) . . . . ?
O3 Dy1 O1 C1 -96.1(10) . . . . ?
N3 Dy1 O1 C1 -163.8(10) . . . . ?
N1 Dy1 O1 C1 -25.3(10) . . . . ?
N2 Dy1 O1 C1 -9.4(12) . . . . ?
N4 Dy1 O1 C1 126.7(10) . . . . ?
C11 C16 O2 Dy1 10.1(15) . . . . ?
C15 C16 O2 Dy1 -174.3(7) . . . . ?
O1 Dy1 O2 C16 -179.7(8) . . . . ?
O4 Dy1 O2 C16 -80.3(9) . . . . ?
O3 Dy1 O2 C16 70.3(9) . . . . ?
N3 Dy1 O2 C16 141.2(10) . . . . ?
N1 Dy1 O2 C16 4.4(11) . . . . ?
N2 Dy1 O2 C16 -8.7(9) . . . . ?
N4 Dy1 O2 C16 -149.6(10) . . . . ?
C22 C17 O3 Dy1 43.3(12) . . . . ?
C18 C17 O3 Dy1 -138.7(8) . . . . ?
O2 Dy1 O3 C17 31.0(7) . . . . ?
O1 Dy1 O3 C17 -119.3(7) . . . . ?
O4 Dy1 O3 C17 134.0(7) . . . . ?
N3 Dy1 O3 C17 -45.4(7) . . . . ?
N1 Dy1 O3 C17 173.2(8) . . . . ?
N2 Dy1 O3 C17 102.9(7) . . . . ?
N4 Dy1 O3 C17 -40.4(9) . . . . ?
C27 C32 O4 Dy1 31.5(15) . . . . ?
C31 C32 O4 Dy1 -148.2(8) . . . . ?
O2 Dy1 O4 C32 -113.5(10) . . . . ?
O1 Dy1 O4 C32 35.8(10) . . . . ?
O3 Dy1 O4 C32 146.1(9) . . . . ?
N3 Dy1 O4 C32 -34.7(11) . . . . ?
N1 Dy1 O4 C32 107.7(10) . . . . ?
N2 Dy1 O4 C32 177.7(10) . . . . ?
N4 Dy1 O4 C32 -37.8(9) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         2.424
_refine_diff_density_min         -1.248
_refine_diff_density_rms         0.138
####################################################################### 
# 
# 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. 
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#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1404029'
_audit_update_record             
;
2015-06-01 deposited with the CCDC.
2015-12-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'2(C32 H24 Ho N8 O12), 2(C6 H16 N),  0.25(H8 O4), 2(C H4 O)'
_chemical_formula_sum            'C39 H45 Ho N9 O13.50'
_chemical_formula_weight         1020.77

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'
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'
H H 0.0000 0.0000 '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                   12.4153(7)
_cell_length_b                   12.7506(7)
_cell_length_c                   15.6649(9)
_cell_angle_alpha                70.0850(9)
_cell_angle_beta                 75.2677(10)
_cell_angle_gamma                71.7208(10)
_cell_volume                     2183.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    3472
_cell_measurement_theta_min      2.418
_cell_measurement_theta_max      21.463

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1034
_exptl_absorpt_coefficient_mu    1.886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.640
_exptl_absorpt_correction_T_max  0.684
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker AFEX II'
_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            12287
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.91
_diffrn_reflns_theta_max         25.00
_reflns_number_total             7663
_reflns_number_gt                6281
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0499P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7663
_refine_ls_number_parameters     636
_refine_ls_number_restraints     248
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0382
_refine_ls_wR_factor_ref         0.0925
_refine_ls_wR_factor_gt          0.0854
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.010
_refine_ls_shift/su_max          0.005
_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
Ho1 Ho 0.232327(18) 0.814274(18) 0.267694(15) 0.04292(9) Uani 1 1 d . A .
C1 C -0.0074(5) 0.7484(4) 0.2611(4) 0.0567(13) Uani 1 1 d . A .
C2 C -0.1101(5) 0.7160(5) 0.3143(4) 0.0607(14) Uani 1 1 d . . .
C3 C -0.2000(5) 0.7201(5) 0.2752(5) 0.0778(19) Uani 1 1 d . A .
H3 H -0.2647 0.6978 0.3131 0.093 Uiso 1 1 calc R . .
C4 C -0.1952(6) 0.7567(5) 0.1815(5) 0.0825(19) Uani 1 1 d . . .
H4 H -0.2541 0.7556 0.1552 0.099 Uiso 1 1 calc R A .
C5 C -0.1016(5) 0.7947(5) 0.1276(5) 0.0729(17) Uani 1 1 d . A .
H5 H -0.0996 0.8227 0.0643 0.087 Uiso 1 1 calc R . .
C6 C -0.0093(5) 0.7934(4) 0.1635(4) 0.0582(14) Uani 1 1 d . . .
C7 C 0.0826(5) 0.8389(4) 0.0988(4) 0.0597(14) Uani 1 1 d . A .
H7 H 0.0762 0.8611 0.0369 0.072 Uiso 1 1 calc R . .
C8 C 0.2489(5) 0.9057(5) 0.0377(3) 0.0605(14) Uani 1 1 d . A .
H8A H 0.2132 0.9353 -0.0170 0.073 Uiso 1 1 calc R . .
H8B H 0.3199 0.8487 0.0267 0.073 Uiso 1 1 calc R . .
C9 C 0.2744(5) 1.0022(5) 0.0573(4) 0.0616(14) Uani 1 1 d . A .
H9A H 0.3259 1.0376 0.0053 0.074 Uiso 1 1 calc R . .
H9B H 0.2037 1.0604 0.0661 0.074 Uiso 1 1 calc R . .
C10 C 0.4117(4) 0.9949(4) 0.1386(3) 0.0528(12) Uani 1 1 d . A .
H10 H 0.4344 1.0462 0.0832 0.063 Uiso 1 1 calc R . .
C11 C 0.4770(4) 0.9685(4) 0.2116(3) 0.0478(11) Uani 1 1 d . . .
C12 C 0.5638(5) 1.0250(5) 0.1925(4) 0.0637(14) Uani 1 1 d . . .
H12 H 0.5788 1.0745 0.1340 0.076 Uiso 1 1 calc R . .
C13 C 0.6276(5) 1.0097(5) 0.2576(5) 0.0753(17) Uani 1 1 d . . .
H13 H 0.6850 1.0484 0.2430 0.090 Uiso 1 1 calc R . .
C14 C 0.6064(5) 0.9381(5) 0.3431(4) 0.0673(15) Uani 1 1 d . . .
H14 H 0.6475 0.9293 0.3882 0.081 Uiso 1 1 calc R . .
C15 C 0.5236(4) 0.8781(4) 0.3629(4) 0.0524(12) Uani 1 1 d . . .
C16 C 0.4508(4) 0.8924(4) 0.3003(3) 0.0453(11) Uani 1 1 d . A .
C17 C 0.4753(4) 0.6285(4) 0.2156(3) 0.0481(12) Uani 1 1 d . A .
C18 C 0.5786(5) 0.6178(4) 0.1501(4) 0.0528(12) Uani 1 1 d . . .
C19 C 0.6841(5) 0.5475(5) 0.1718(4) 0.0646(15) Uani 1 1 d . B .
H19 H 0.7491 0.5453 0.1264 0.077 Uiso 1 1 calc R . .
C20 C 0.6921(5) 0.4809(5) 0.2610(5) 0.0732(17) Uani 1 1 d . . .
H20 H 0.7621 0.4323 0.2765 0.088 Uiso 1 1 calc R B .
C21 C 0.5962(5) 0.4872(5) 0.3258(4) 0.0654(15) Uani 1 1 d . B .
H21 H 0.6022 0.4412 0.3858 0.078 Uiso 1 1 calc R . .
C22 C 0.4894(4) 0.5588(4) 0.3075(4) 0.0517(12) Uani 1 1 d . . .
C23 C 0.3958(5) 0.5578(4) 0.3839(4) 0.0552(13) Uani 1 1 d . A .
H23 H 0.4099 0.5012 0.4388 0.066 Uiso 1 1 calc R . .
C24 C 0.2157(5) 0.6109(5) 0.4722(3) 0.0626(14) Uani 1 1 d . A .
H24A H 0.2514 0.5457 0.5188 0.075 Uiso 1 1 calc R . .
H24B H 0.1469 0.5963 0.4649 0.075 Uiso 1 1 calc R . .
C25 C 0.1851(5) 0.7199(5) 0.5008(4) 0.0687(16) Uani 1 1 d . A .
H25A H 0.1320 0.7124 0.5587 0.082 Uiso 1 1 calc R . .
H25B H 0.2538 0.7335 0.5093 0.082 Uiso 1 1 calc R . .
C26 C 0.0321(5) 0.8744(5) 0.4534(4) 0.0680(16) Uani 1 1 d . A .
H26 H 0.0015 0.8523 0.5156 0.082 Uiso 1 1 calc R . .
C27 C -0.0397(5) 0.9717(5) 0.3952(4) 0.0677(16) Uani 1 1 d . . .
C28 C -0.1523(6) 1.0152(7) 0.4340(6) 0.090(2) Uani 1 1 d . . .
H28 H -0.1775 0.9802 0.4954 0.108 Uiso 1 1 calc R . .
C29 C -0.2273(6) 1.1064(8) 0.3866(7) 0.104(3) Uani 1 1 d . . .
H29 H -0.3024 1.1315 0.4146 0.125 Uiso 1 1 calc R . .
C30 C -0.1897(6) 1.1606(6) 0.2964(7) 0.093(3) Uani 1 1 d . C .
H30 H -0.2394 1.2230 0.2626 0.111 Uiso 1 1 calc R . .
C31 C -0.0779(5) 1.1220(5) 0.2564(5) 0.0733(18) Uani 1 1 d D . .
C32 C 0.0027(5) 1.0239(5) 0.3021(4) 0.0639(15) Uani 1 1 d . A .
C33 C 0.2535(7) 0.2688(6) 0.2263(5) 0.097(2) Uani 1 1 d . . .
H33A H 0.3250 0.2461 0.1864 0.116 Uiso 1 1 calc R . .
H33B H 0.1916 0.2916 0.1913 0.116 Uiso 1 1 calc R . .
C34 C 0.2372(8) 0.1674(7) 0.3055(8) 0.160(5) Uani 1 1 d . . .
H34A H 0.2366 0.1060 0.2835 0.240 Uiso 1 1 calc R . .
H34B H 0.1654 0.1879 0.3445 0.240 Uiso 1 1 calc R . .
H34C H 0.2990 0.1427 0.3399 0.240 Uiso 1 1 calc R . .
C35 C 0.1452(8) 0.4197(7) 0.3085(6) 0.109(3) Uani 1 1 d . . .
H35A H 0.1365 0.3660 0.3695 0.131 Uiso 1 1 calc R . .
H35B H 0.1506 0.4906 0.3153 0.131 Uiso 1 1 calc R . .
C36 C 0.0412(8) 0.4439(9) 0.2667(9) 0.155(4) Uani 1 1 d . . .
H36A H 0.0488 0.4977 0.2066 0.233 Uiso 1 1 calc R . .
H36B H -0.0260 0.4761 0.3050 0.233 Uiso 1 1 calc R . .
H36C H 0.0338 0.3736 0.2618 0.233 Uiso 1 1 calc R . .
C37 C 0.3556(9) 0.3528(8) 0.2941(7) 0.127(3) Uani 1 1 d . . .
H37A H 0.3537 0.2909 0.3511 0.153 Uiso 1 1 calc R . .
H37B H 0.3490 0.4225 0.3092 0.153 Uiso 1 1 calc R . .
C38 C 0.4703(7) 0.3241(8) 0.2324(8) 0.137(4) Uani 1 1 d . . .
H38A H 0.4769 0.2559 0.2163 0.205 Uiso 1 1 calc R . .
H38B H 0.5318 0.3113 0.2644 0.205 Uiso 1 1 calc R . .
H38C H 0.4746 0.3871 0.1774 0.205 Uiso 1 1 calc R . .
N1 N 0.1715(4) 0.8524(3) 0.1166(3) 0.0528(10) Uani 1 1 d . . .
N2 N 0.3282(4) 0.9570(3) 0.1410(3) 0.0489(10) Uani 1 1 d . . .
N3 N 0.2960(4) 0.6261(3) 0.3843(3) 0.0511(10) Uani 1 1 d . . .
N4 N 0.1318(4) 0.8163(4) 0.4286(3) 0.0569(11) Uani 1 1 d . . .
N5 N -0.1244(5) 0.6815(6) 0.4131(4) 0.0889(15) Uani 0.611(12) 1 d PDU A 1
O5 O -0.0430(7) 0.6141(11) 0.4521(6) 0.122(4) Uani 0.611(12) 1 d PDU A 1
O6 O -0.2179(9) 0.7017(12) 0.4601(10) 0.128(5) Uani 0.611(12) 1 d PDU A 1
N5' N -0.1244(5) 0.6815(6) 0.4131(4) 0.0889(15) Uani 0.389(12) 1 d PDU A 2
O5' O -0.0768(13) 0.7179(15) 0.4518(9) 0.099(4) Uani 0.389(12) 1 d PDU A 2
O6' O -0.2064(14) 0.6446(18) 0.4559(15) 0.115(5) Uani 0.389(12) 1 d PDU A 2
N6 N 0.5085(4) 0.7968(5) 0.4547(3) 0.0724(14) Uani 1 1 d . . .
N7 N 0.5770(4) 0.6859(4) 0.0553(4) 0.0709(12) Uani 0.849(8) 1 d PDU B 1
O9 O 0.6597(6) 0.7251(7) 0.0115(4) 0.108(2) Uani 0.849(8) 1 d PDU B 1
O10 O 0.4977(5) 0.7005(6) 0.0171(3) 0.094(2) Uani 0.849(8) 1 d PDU B 1
N7' N 0.5770(4) 0.6859(4) 0.0553(4) 0.0709(12) Uani 0.151(8) 1 d PDU B 2
O9' O 0.519(3) 0.7866(14) 0.0381(18) 0.091(7) Uani 0.151(8) 1 d PDU B 2
O10' O 0.651(3) 0.655(2) -0.0044(17) 0.104(8) Uani 0.151(8) 1 d PDU B 2
N8 N -0.0412(7) 1.1847(7) 0.1621(6) 0.115(2) Uani 0.770(7) 1 d PDU C 1
O11 O 0.0537(7) 1.2087(6) 0.1368(6) 0.129(3) Uani 0.770(7) 1 d PDU C 1
O12 O -0.1072(8) 1.2195(9) 0.1070(6) 0.160(3) Uani 0.770(7) 1 d PDU C 1
N8' N -0.0412(7) 1.1847(7) 0.1621(6) 0.115(2) Uani 0.230(7) 1 d PDU C 2
O11' O -0.011(2) 1.122(2) 0.1103(17) 0.133(6) Uani 0.230(7) 1 d PDU C 2
O12' O -0.079(3) 1.2886(12) 0.137(2) 0.138(6) Uani 0.230(7) 1 d PDU C 2
N9 N 0.2564(4) 0.3694(4) 0.2509(3) 0.0712(13) Uani 1 1 d . . .
H9C H 0.2640 0.4253 0.1967 0.085 Uiso 1 1 calc R . .
O1 O 0.0802(3) 0.7377(3) 0.2953(2) 0.0617(9) Uani 1 1 d . . .
O2 O 0.3684(3) 0.8435(3) 0.3232(2) 0.0532(8) Uani 1 1 d . . .
O3 O 0.3769(3) 0.6937(3) 0.1945(2) 0.0527(8) Uani 1 1 d . . .
O4 O 0.1039(3) 0.9873(3) 0.2602(3) 0.0622(9) Uani 1 1 d . . .
O7 O 0.4871(5) 0.7076(5) 0.4645(4) 0.1092(18) Uani 1 1 d . . .
O8 O 0.5197(5) 0.8233(5) 0.5202(3) 0.1115(17) Uani 1 1 d . . .
O13 O 0.2877(5) 0.5697(5) 0.1148(5) 0.131(2) Uani 1 1 d . . .
H13A H 0.3167 0.6133 0.1245 0.196 Uiso 1 1 calc R . .
C39 C 0.2923(9) 0.5944(9) 0.0202(6) 0.140(4) Uani 1 1 d . . .
H39A H 0.3527 0.5372 -0.0027 0.211 Uiso 1 1 calc R . .
H39B H 0.3072 0.6690 -0.0104 0.211 Uiso 1 1 calc R . .
H39C H 0.2201 0.5942 0.0085 0.211 Uiso 1 1 calc R . .
O1W O 1.0000 0.5000 0.0000 0.206(13) Uani 0.50 2 d SPU D 1
H1WA H 0.9393 0.4758 0.0212 0.309 Uiso 0.25 1 d PR D 1
H1WB H 0.9932 0.5502 -0.0518 0.309 Uiso 0.25 1 d PR D 1
O2W O 1.069(2) 0.449(2) 0.002(2) 0.158(11) Uani 0.25 1 d PU . 2
H2WB H 1.0260 0.4128 0.0457 0.237 Uiso 0.25 1 d PR . 2
H2WA H 1.0287 0.5028 -0.0349 0.237 Uiso 0.25 1 d PR . 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho1 O2 2.260(3) . ?
Ho1 O4 2.266(3) . ?
Ho1 O1 2.272(3) . ?
Ho1 O3 2.307(3) . ?
Ho1 N3 2.506(4) . ?
Ho1 N1 2.511(4) . ?
Ho1 N4 2.518(4) . ?
Ho1 N2 2.524(4) . ?
C1 O1 1.281(6) . ?
C1 C2 1.431(8) . ?
C1 C6 1.443(8) . ?
C2 C3 1.382(8) . ?
C2 N5 1.438(8) . ?
C3 C4 1.373(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.369(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.392(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.446(8) . ?
C7 N1 1.278(6) . ?
C7 H7 0.9300 . ?
C8 N1 1.465(6) . ?
C8 C9 1.503(7) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N2 1.479(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.261(6) . ?
C10 C11 1.454(7) . ?
C10 H10 0.9300 . ?
C11 C12 1.395(7) . ?
C11 C16 1.424(7) . ?
C12 C13 1.372(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.355(8) . ?
C13 H13 0.9300 . ?
C14 C15 1.381(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.427(6) . ?
C15 N6 1.465(7) . ?
C16 O2 1.275(5) . ?
C17 O3 1.294(5) . ?
C17 C18 1.426(7) . ?
C17 C22 1.432(7) . ?
C18 C19 1.386(7) . ?
C18 N7 1.443(7) . ?
C19 C20 1.375(8) . ?
C19 H19 0.9300 . ?
C20 C21 1.355(8) . ?
C20 H20 0.9300 . ?
C21 C22 1.389(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.441(7) . ?
C23 N3 1.272(6) . ?
C23 H23 0.9300 . ?
C24 N3 1.472(6) . ?
C24 C25 1.512(8) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 N4 1.467(7) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 N4 1.268(7) . ?
C26 C27 1.453(8) . ?
C26 H26 0.9300 . ?
C27 C28 1.394(8) . ?
C27 C32 1.420(9) . ?
C28 C29 1.362(10) . ?
C28 H28 0.9300 . ?
C29 C30 1.377(11) . ?
C29 H29 0.9300 . ?
C30 C31 1.378(9) . ?
C30 H30 0.9300 . ?
C31 C32 1.431(8) . ?
C31 N8 1.452(10) . ?
C32 O4 1.284(6) . ?
C33 N9 1.472(8) . ?
C33 C34 1.482(12) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 C36 1.494(11) . ?
C35 N9 1.528(9) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 N9 1.478(9) . ?
C37 C38 1.520(12) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
N5 O6 1.209(9) . ?
N5 O5 1.244(8) . ?
N6 O7 1.200(6) . ?
N6 O8 1.234(7) . ?
N7 O10 1.213(7) . ?
N7 O9 1.227(7) . ?
N8 O12 1.217(8) . ?
N8 O11 1.243(9) . ?
N9 H9C 0.9100 . ?
O13 C39 1.397(9) . ?
O13 H13A 0.8200 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8500 . ?
O2W O2W 1.80(5) 2_765 ?
O2W H2WB 0.8500 . ?
O2W H2WA 0.8499 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ho1 O4 98.49(13) . . ?
O2 Ho1 O1 148.56(12) . . ?
O4 Ho1 O1 87.41(14) . . ?
O2 Ho1 O3 88.21(12) . . ?
O4 Ho1 O3 149.34(13) . . ?
O1 Ho1 O3 102.36(13) . . ?
O2 Ho1 N3 76.41(12) . . ?
O4 Ho1 N3 139.49(14) . . ?
O1 Ho1 N3 79.18(13) . . ?
O3 Ho1 N3 71.17(12) . . ?
O2 Ho1 N1 139.61(13) . . ?
O4 Ho1 N1 80.18(13) . . ?
O1 Ho1 N1 71.78(13) . . ?
O3 Ho1 N1 75.62(12) . . ?
N3 Ho1 N1 129.32(13) . . ?
O2 Ho1 N4 78.91(13) . . ?
O4 Ho1 N4 71.77(14) . . ?
O1 Ho1 N4 73.68(13) . . ?
O3 Ho1 N4 138.80(13) . . ?
N3 Ho1 N4 67.80(14) . . ?
N1 Ho1 N4 135.98(14) . . ?
O2 Ho1 N2 71.98(12) . . ?
O4 Ho1 N2 75.12(13) . . ?
O1 Ho1 N2 138.83(13) . . ?
O3 Ho1 N2 78.70(12) . . ?
N3 Ho1 N2 136.53(13) . . ?
N1 Ho1 N2 68.69(13) . . ?
N4 Ho1 N2 131.46(14) . . ?
O1 C1 C2 124.1(5) . . ?
O1 C1 C6 121.9(5) . . ?
C2 C1 C6 114.0(5) . . ?
C3 C2 C1 123.1(6) . . ?
C3 C2 N5 117.4(6) . . ?
C1 C2 N5 119.5(5) . . ?
C4 C3 C2 121.1(6) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C5 C4 C3 118.2(6) . . ?
C5 C4 H4 120.9 . . ?
C3 C4 H4 120.9 . . ?
C4 C5 C6 122.9(6) . . ?
C4 C5 H5 118.5 . . ?
C6 C5 H5 118.5 . . ?
C5 C6 C1 120.5(6) . . ?
C5 C6 C7 117.1(6) . . ?
C1 C6 C7 122.4(5) . . ?
N1 C7 C6 127.7(5) . . ?
N1 C7 H7 116.1 . . ?
C6 C7 H7 116.1 . . ?
N1 C8 C9 109.3(4) . . ?
N1 C8 H8A 109.8 . . ?
C9 C8 H8A 109.8 . . ?
N1 C8 H8B 109.8 . . ?
C9 C8 H8B 109.8 . . ?
H8A C8 H8B 108.3 . . ?
N2 C9 C8 109.8(4) . . ?
N2 C9 H9A 109.7 . . ?
C8 C9 H9A 109.7 . . ?
N2 C9 H9B 109.7 . . ?
C8 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
N2 C10 C11 128.2(5) . . ?
N2 C10 H10 115.9 . . ?
C11 C10 H10 115.9 . . ?
C12 C11 C16 121.0(5) . . ?
C12 C11 C10 117.1(5) . . ?
C16 C11 C10 121.9(4) . . ?
C13 C12 C11 121.8(5) . . ?
C13 C12 H12 119.1 . . ?
C11 C12 H12 119.1 . . ?
C14 C13 C12 119.7(5) . . ?
C14 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
C13 C14 C15 119.6(5) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
C14 C15 C16 124.0(5) . . ?
C14 C15 N6 117.5(5) . . ?
C16 C15 N6 118.4(4) . . ?
O2 C16 C11 123.7(4) . . ?
O2 C16 C15 122.6(5) . . ?
C11 C16 C15 113.7(4) . . ?
O3 C17 C18 123.5(5) . . ?
O3 C17 C22 122.6(5) . . ?
C18 C17 C22 114.0(4) . . ?
C19 C18 C17 124.0(5) . . ?
C19 C18 N7 116.4(5) . . ?
C17 C18 N7 119.6(5) . . ?
C20 C19 C18 119.5(6) . . ?
C20 C19 H19 120.3 . . ?
C18 C19 H19 120.3 . . ?
C21 C20 C19 118.8(5) . . ?
C21 C20 H20 120.6 . . ?
C19 C20 H20 120.6 . . ?
C20 C21 C22 123.5(6) . . ?
C20 C21 H21 118.2 . . ?
C22 C21 H21 118.2 . . ?
C21 C22 C17 120.2(5) . . ?
C21 C22 C23 117.1(5) . . ?
C17 C22 C23 122.7(5) . . ?
N3 C23 C22 126.9(5) . . ?
N3 C23 H23 116.6 . . ?
C22 C23 H23 116.6 . . ?
N3 C24 C25 108.1(4) . . ?
N3 C24 H24A 110.1 . . ?
C25 C24 H24A 110.1 . . ?
N3 C24 H24B 110.1 . . ?
C25 C24 H24B 110.1 . . ?
H24A C24 H24B 108.4 . . ?
N4 C25 C24 108.5(4) . . ?
N4 C25 H25A 110.0 . . ?
C24 C25 H25A 110.0 . . ?
N4 C25 H25B 110.0 . . ?
C24 C25 H25B 110.0 . . ?
H25A C25 H25B 108.4 . . ?
N4 C26 C27 127.1(5) . . ?
N4 C26 H26 116.4 . . ?
C27 C26 H26 116.4 . . ?
C28 C27 C32 120.0(6) . . ?
C28 C27 C26 118.0(6) . . ?
C32 C27 C26 121.9(5) . . ?
C29 C28 C27 123.4(8) . . ?
C29 C28 H28 118.3 . . ?
C27 C28 H28 118.3 . . ?
C28 C29 C30 118.7(7) . . ?
C28 C29 H29 120.7 . . ?
C30 C29 H29 120.7 . . ?
C29 C30 C31 119.6(7) . . ?
C29 C30 H30 120.2 . . ?
C31 C30 H30 120.2 . . ?
C30 C31 C32 123.8(7) . . ?
C30 C31 N8 117.5(7) . . ?
C32 C31 N8 118.7(6) . . ?
O4 C32 C27 124.0(5) . . ?
O4 C32 C31 121.5(6) . . ?
C27 C32 C31 114.5(6) . . ?
N9 C33 C34 114.8(7) . . ?
N9 C33 H33A 108.6 . . ?
C34 C33 H33A 108.6 . . ?
N9 C33 H33B 108.6 . . ?
C34 C33 H33B 108.6 . . ?
H33A C33 H33B 107.5 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36 C35 N9 112.8(7) . . ?
C36 C35 H35A 109.0 . . ?
N9 C35 H35A 109.0 . . ?
C36 C35 H35B 109.0 . . ?
N9 C35 H35B 109.0 . . ?
H35A C35 H35B 107.8 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N9 C37 C38 112.8(7) . . ?
N9 C37 H37A 109.0 . . ?
C38 C37 H37A 109.0 . . ?
N9 C37 H37B 109.0 . . ?
C38 C37 H37B 109.0 . . ?
H37A C37 H37B 107.8 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C7 N1 C8 116.4(4) . . ?
C7 N1 Ho1 130.7(4) . . ?
C8 N1 Ho1 112.7(3) . . ?
C10 N2 C9 116.9(4) . . ?
C10 N2 Ho1 130.7(3) . . ?
C9 N2 Ho1 112.5(3) . . ?
C23 N3 C24 117.0(4) . . ?
C23 N3 Ho1 127.7(3) . . ?
C24 N3 Ho1 113.4(3) . . ?
C26 N4 C25 116.4(5) . . ?
C26 N4 Ho1 128.0(4) . . ?
C25 N4 Ho1 113.9(3) . . ?
O6 N5 O5 117.9(10) . . ?
O6 N5 C2 121.7(10) . . ?
O5 N5 C2 119.5(7) . . ?
O7 N6 O8 122.0(6) . . ?
O7 N6 C15 120.3(5) . . ?
O8 N6 C15 117.7(6) . . ?
O10 N7 O9 119.4(6) . . ?
O10 N7 C18 121.1(5) . . ?
O9 N7 C18 119.4(6) . . ?
O12 N8 O11 118.8(11) . . ?
O12 N8 C31 119.2(10) . . ?
O11 N8 C31 121.9(7) . . ?
C33 N9 C37 115.1(6) . . ?
C33 N9 C35 114.3(5) . . ?
C37 N9 C35 109.6(6) . . ?
C33 N9 H9C 105.7 . . ?
C37 N9 H9C 105.7 . . ?
C35 N9 H9C 105.7 . . ?
C1 O1 Ho1 141.4(3) . . ?
C16 O2 Ho1 143.3(3) . . ?
C17 O3 Ho1 131.6(3) . . ?
C32 O4 Ho1 136.2(4) . . ?
C39 O13 H13A 109.5 . . ?
O13 C39 H39A 109.5 . . ?
O13 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
O13 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
H1WA O1W H1WB 109.5 . . ?
H1WA O1W H2WB 73.9 . . ?
H1WB O1W H2WB 154.9 . . ?
H1WA O1W H2WA 129.5 . . ?
H1WB O1W H2WA 49.1 . . ?
H2WB O1W H2WA 108.8 . . ?
O2W O2W H1WB 31.7 2_765 . ?
O2W O2W H2WB 77.6 2_765 . ?
H1WB O2W H2WB 106.8 . . ?
O2W O2W H2WA 37.7 2_765 . ?
H1WB O2W H2WA 8.1 . . ?
H2WB O2W H2WA 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 -174.9(5) . . . . ?
C6 C1 C2 C3 4.0(8) . . . . ?
O1 C1 C2 N5 7.7(8) . . . . ?
C6 C1 C2 N5 -173.4(5) . . . . ?
C1 C2 C3 C4 -0.2(9) . . . . ?
N5 C2 C3 C4 177.3(6) . . . . ?
C2 C3 C4 C5 -3.3(9) . . . . ?
C3 C4 C5 C6 2.8(10) . . . . ?
C4 C5 C6 C1 1.4(9) . . . . ?
C4 C5 C6 C7 -178.4(6) . . . . ?
O1 C1 C6 C5 174.4(5) . . . . ?
C2 C1 C6 C5 -4.5(7) . . . . ?
O1 C1 C6 C7 -5.8(8) . . . . ?
C2 C1 C6 C7 175.2(5) . . . . ?
C5 C6 C7 N1 175.6(5) . . . . ?
C1 C6 C7 N1 -4.2(9) . . . . ?
N1 C8 C9 N2 59.1(6) . . . . ?
N2 C10 C11 C12 -177.9(5) . . . . ?
N2 C10 C11 C16 -0.8(8) . . . . ?
C16 C11 C12 C13 0.3(8) . . . . ?
C10 C11 C12 C13 177.5(5) . . . . ?
C11 C12 C13 C14 -0.1(9) . . . . ?
C12 C13 C14 C15 2.2(9) . . . . ?
C13 C14 C15 C16 -4.7(9) . . . . ?
C13 C14 C15 N6 176.6(5) . . . . ?
C12 C11 C16 O2 175.9(5) . . . . ?
C10 C11 C16 O2 -1.1(7) . . . . ?
C12 C11 C16 C15 -2.3(7) . . . . ?
C10 C11 C16 C15 -179.4(4) . . . . ?
C14 C15 C16 O2 -173.7(5) . . . . ?
N6 C15 C16 O2 5.0(7) . . . . ?
C14 C15 C16 C11 4.6(7) . . . . ?
N6 C15 C16 C11 -176.7(4) . . . . ?
O3 C17 C18 C19 -179.4(5) . . . . ?
C22 C17 C18 C19 -0.3(7) . . . . ?
O3 C17 C18 N7 2.6(7) . . . . ?
C22 C17 C18 N7 -178.3(5) . . . . ?
C17 C18 C19 C20 1.5(8) . . . . ?
N7 C18 C19 C20 179.5(5) . . . . ?
C18 C19 C20 C21 -1.0(9) . . . . ?
C19 C20 C21 C22 -0.8(9) . . . . ?
C20 C21 C22 C17 2.0(8) . . . . ?
C20 C21 C22 C23 -178.9(5) . . . . ?
O3 C17 C22 C21 177.7(5) . . . . ?
C18 C17 C22 C21 -1.4(7) . . . . ?
O3 C17 C22 C23 -1.4(7) . . . . ?
C18 C17 C22 C23 179.5(4) . . . . ?
C21 C22 C23 N3 170.8(5) . . . . ?
C17 C22 C23 N3 -10.1(8) . . . . ?
N3 C24 C25 N4 59.5(6) . . . . ?
N4 C26 C27 C28 172.6(6) . . . . ?
N4 C26 C27 C32 -8.9(9) . . . . ?
C32 C27 C28 C29 1.0(10) . . . . ?
C26 C27 C28 C29 179.6(6) . . . . ?
C27 C28 C29 C30 -1.7(11) . . . . ?
C28 C29 C30 C31 -0.2(11) . . . . ?
C29 C30 C31 C32 2.8(10) . . . . ?
C29 C30 C31 N8 -177.9(7) . . . . ?
C28 C27 C32 O4 -177.8(5) . . . . ?
C26 C27 C32 O4 3.6(8) . . . . ?
C28 C27 C32 C31 1.4(8) . . . . ?
C26 C27 C32 C31 -177.1(5) . . . . ?
C30 C31 C32 O4 175.9(5) . . . . ?
N8 C31 C32 O4 -3.4(8) . . . . ?
C30 C31 C32 C27 -3.3(8) . . . . ?
N8 C31 C32 C27 177.3(6) . . . . ?
C6 C7 N1 C8 -177.3(5) . . . . ?
C6 C7 N1 Ho1 -1.9(8) . . . . ?
C9 C8 N1 C7 130.2(5) . . . . ?
C9 C8 N1 Ho1 -46.0(5) . . . . ?
O2 Ho1 N1 C7 -172.1(4) . . . . ?
O4 Ho1 N1 C7 -80.5(4) . . . . ?
O1 Ho1 N1 C7 10.0(4) . . . . ?
O3 Ho1 N1 C7 118.5(5) . . . . ?
N3 Ho1 N1 C7 68.3(5) . . . . ?
N4 Ho1 N1 C7 -30.0(5) . . . . ?
N2 Ho1 N1 C7 -158.2(5) . . . . ?
O2 Ho1 N1 C8 3.5(4) . . . . ?
O4 Ho1 N1 C8 95.0(3) . . . . ?
O1 Ho1 N1 C8 -174.5(4) . . . . ?
O3 Ho1 N1 C8 -66.0(3) . . . . ?
N3 Ho1 N1 C8 -116.1(3) . . . . ?
N4 Ho1 N1 C8 145.5(3) . . . . ?
N2 Ho1 N1 C8 17.3(3) . . . . ?
C11 C10 N2 C9 177.6(5) . . . . ?
C11 C10 N2 Ho1 -1.8(8) . . . . ?
C8 C9 N2 C10 137.9(5) . . . . ?
C8 C9 N2 Ho1 -42.5(5) . . . . ?
O2 Ho1 N2 C10 3.7(4) . . . . ?
O4 Ho1 N2 C10 108.0(4) . . . . ?
O1 Ho1 N2 C10 176.0(4) . . . . ?
O3 Ho1 N2 C10 -88.1(4) . . . . ?
N3 Ho1 N2 C10 -41.6(5) . . . . ?
N1 Ho1 N2 C10 -166.9(5) . . . . ?
N4 Ho1 N2 C10 59.8(5) . . . . ?
O2 Ho1 N2 C9 -175.7(3) . . . . ?
O4 Ho1 N2 C9 -71.4(3) . . . . ?
O1 Ho1 N2 C9 -3.5(4) . . . . ?
O3 Ho1 N2 C9 92.4(3) . . . . ?
N3 Ho1 N2 C9 138.9(3) . . . . ?
N1 Ho1 N2 C9 13.6(3) . . . . ?
N4 Ho1 N2 C9 -119.6(3) . . . . ?
C22 C23 N3 C24 -177.6(5) . . . . ?
C22 C23 N3 Ho1 -14.8(7) . . . . ?
C25 C24 N3 C23 117.9(5) . . . . ?
C25 C24 N3 Ho1 -47.3(5) . . . . ?
O2 Ho1 N3 C23 -61.7(4) . . . . ?
O4 Ho1 N3 C23 -148.9(4) . . . . ?
O1 Ho1 N3 C23 138.3(4) . . . . ?
O3 Ho1 N3 C23 31.1(4) . . . . ?
N1 Ho1 N3 C23 82.9(4) . . . . ?
N4 Ho1 N3 C23 -145.1(4) . . . . ?
N2 Ho1 N3 C23 -17.6(5) . . . . ?
O2 Ho1 N3 C24 101.7(3) . . . . ?
O4 Ho1 N3 C24 14.5(4) . . . . ?
O1 Ho1 N3 C24 -58.4(3) . . . . ?
O3 Ho1 N3 C24 -165.6(3) . . . . ?
N1 Ho1 N3 C24 -113.8(3) . . . . ?
N4 Ho1 N3 C24 18.3(3) . . . . ?
N2 Ho1 N3 C24 145.8(3) . . . . ?
C27 C26 N4 C25 -178.5(5) . . . . ?
C27 C26 N4 Ho1 -14.1(8) . . . . ?
C24 C25 N4 C26 123.3(5) . . . . ?
C24 C25 N4 Ho1 -43.4(5) . . . . ?
O2 Ho1 N4 C26 129.5(5) . . . . ?
O4 Ho1 N4 C26 26.6(5) . . . . ?
O1 Ho1 N4 C26 -66.1(5) . . . . ?
O3 Ho1 N4 C26 -156.3(4) . . . . ?
N3 Ho1 N4 C26 -150.8(5) . . . . ?
N1 Ho1 N4 C26 -26.6(6) . . . . ?
N2 Ho1 N4 C26 75.9(5) . . . . ?
O2 Ho1 N4 C25 -65.8(4) . . . . ?
O4 Ho1 N4 C25 -168.6(4) . . . . ?
O1 Ho1 N4 C25 98.7(4) . . . . ?
O3 Ho1 N4 C25 8.4(4) . . . . ?
N3 Ho1 N4 C25 14.0(3) . . . . ?
N1 Ho1 N4 C25 138.2(3) . . . . ?
N2 Ho1 N4 C25 -119.3(4) . . . . ?
C3 C2 N5 O6 -30.8(13) . . . . ?
C1 C2 N5 O6 146.7(11) . . . . ?
C3 C2 N5 O5 137.6(9) . . . . ?
C1 C2 N5 O5 -44.8(11) . . . . ?
C14 C15 N6 O7 -143.0(6) . . . . ?
C16 C15 N6 O7 38.2(8) . . . . ?
C14 C15 N6 O8 36.3(7) . . . . ?
C16 C15 N6 O8 -142.5(5) . . . . ?
C19 C18 N7 O10 141.0(6) . . . . ?
C17 C18 N7 O10 -40.9(8) . . . . ?
C19 C18 N7 O9 -35.6(8) . . . . ?
C17 C18 N7 O9 142.5(7) . . . . ?
C30 C31 N8 O12 -39.8(11) . . . . ?
C32 C31 N8 O12 139.6(8) . . . . ?
C30 C31 N8 O11 136.7(8) . . . . ?
C32 C31 N8 O11 -43.9(11) . . . . ?
C34 C33 N9 C37 65.9(9) . . . . ?
C34 C33 N9 C35 -62.3(9) . . . . ?
C38 C37 N9 C33 60.2(9) . . . . ?
C38 C37 N9 C35 -169.4(7) . . . . ?
C36 C35 N9 C33 -51.7(9) . . . . ?
C36 C35 N9 C37 177.4(7) . . . . ?
C2 C1 O1 Ho1 -153.8(4) . . . . ?
C6 C1 O1 Ho1 27.3(9) . . . . ?
O2 Ho1 O1 C1 157.9(5) . . . . ?
O4 Ho1 O1 C1 55.8(6) . . . . ?
O3 Ho1 O1 C1 -94.8(6) . . . . ?
N3 Ho1 O1 C1 -162.6(6) . . . . ?
N1 Ho1 O1 C1 -24.7(5) . . . . ?
N4 Ho1 O1 C1 127.6(6) . . . . ?
N2 Ho1 O1 C1 -7.9(7) . . . . ?
C11 C16 O2 Ho1 7.3(8) . . . . ?
C15 C16 O2 Ho1 -174.6(4) . . . . ?
O4 Ho1 O2 C16 -78.3(5) . . . . ?
O1 Ho1 O2 C16 -177.3(5) . . . . ?
O3 Ho1 O2 C16 71.6(5) . . . . ?
N3 Ho1 O2 C16 142.7(5) . . . . ?
N1 Ho1 O2 C16 6.5(6) . . . . ?
N4 Ho1 O2 C16 -147.7(5) . . . . ?
N2 Ho1 O2 C16 -7.1(5) . . . . ?
C18 C17 O3 Ho1 -138.5(4) . . . . ?
C22 C17 O3 Ho1 42.5(6) . . . . ?
O2 Ho1 O3 C17 30.2(4) . . . . ?
O4 Ho1 O3 C17 133.9(4) . . . . ?
O1 Ho1 O3 C17 -120.0(4) . . . . ?
N3 Ho1 O3 C17 -46.1(4) . . . . ?
N1 Ho1 O3 C17 172.8(4) . . . . ?
N4 Ho1 O3 C17 -40.7(5) . . . . ?
N2 Ho1 O3 C17 102.1(4) . . . . ?
C27 C32 O4 Ho1 30.8(8) . . . . ?
C31 C32 O4 Ho1 -148.4(4) . . . . ?
O2 Ho1 O4 C32 -112.0(5) . . . . ?
O1 Ho1 O4 C32 36.9(5) . . . . ?
O3 Ho1 O4 C32 147.0(4) . . . . ?
N3 Ho1 O4 C32 -33.0(6) . . . . ?
N1 Ho1 O4 C32 108.9(5) . . . . ?
N4 Ho1 O4 C32 -36.7(5) . . . . ?
N2 Ho1 O4 C32 179.3(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.082
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1404030'
_audit_update_record             
;
2015-06-01 deposited with the CCDC.
2015-12-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C32 H24 Er N8 O12), 2(C6 H16 N), 3(H2 O)'
_chemical_formula_sum            'C76 H86 Er2 N18 O27'
_chemical_formula_weight         2018.15

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'
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'
H H 0.0000 0.0000 '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                   12.349(8)
_cell_length_b                   12.659(8)
_cell_length_c                   15.668(10)
_cell_angle_alpha                69.829(9)
_cell_angle_beta                 75.214(10)
_cell_angle_gamma                71.612(10)
_cell_volume                     2152(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    3002
_cell_measurement_theta_min      2.426
_cell_measurement_theta_max      21.244

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1020
_exptl_absorpt_coefficient_mu    2.024
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.377
_exptl_absorpt_correction_T_max  0.546
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX DUO'
_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            15777
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_unetI/netI     0.0851
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.76
_diffrn_reflns_theta_max         25.00
_reflns_number_total             7460
_reflns_number_gt                5559
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0593P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7460
_refine_ls_number_parameters     638
_refine_ls_number_restraints     252
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0499
_refine_ls_wR_factor_ref         0.1277
_refine_ls_wR_factor_gt          0.1146
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.014
_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
Er1 Er 0.23206(2) 0.81560(3) 0.26682(2) 0.04962(13) Uani 1 1 d . A .
C1 C -0.0090(6) 0.7483(7) 0.2623(6) 0.068(2) Uani 1 1 d . A .
C2 C -0.1102(6) 0.7153(7) 0.3164(6) 0.068(2) Uani 1 1 d . . .
C3 C -0.2010(7) 0.7182(8) 0.2795(8) 0.087(3) Uani 1 1 d . A .
H3 H -0.2654 0.6948 0.3181 0.104 Uiso 1 1 calc R . .
C4 C -0.1970(8) 0.7551(8) 0.1866(9) 0.095(3) Uani 1 1 d . . .
H4 H -0.2577 0.7548 0.1617 0.113 Uiso 1 1 calc R A .
C5 C -0.1029(8) 0.7929(7) 0.1291(7) 0.084(3) Uani 1 1 d . A .
H5 H -0.1012 0.8192 0.0657 0.100 Uiso 1 1 calc R . .
C6 C -0.0096(6) 0.7921(6) 0.1658(6) 0.065(2) Uani 1 1 d . . .
C7 C 0.0819(7) 0.8397(7) 0.1003(5) 0.069(2) Uani 1 1 d . A .
H7 H 0.0743 0.8631 0.0385 0.082 Uiso 1 1 calc R . .
C8 C 0.2480(7) 0.9059(7) 0.0390(5) 0.068(2) Uani 1 1 d . A .
H8A H 0.2117 0.9350 -0.0155 0.081 Uiso 1 1 calc R . .
H8B H 0.3194 0.8483 0.0283 0.081 Uiso 1 1 calc R . .
C9 C 0.2739(7) 1.0042(7) 0.0565(5) 0.069(2) Uani 1 1 d . A .
H9A H 0.3261 1.0391 0.0043 0.083 Uiso 1 1 calc R . .
H9B H 0.2031 1.0634 0.0650 0.083 Uiso 1 1 calc R . .
C10 C 0.4122(7) 0.9956(6) 0.1382(5) 0.0615(18) Uani 1 1 d . A .
H10 H 0.4359 1.0468 0.0826 0.074 Uiso 1 1 calc R . .
C11 C 0.4760(6) 0.9694(6) 0.2114(5) 0.0535(16) Uani 1 1 d . . .
C12 C 0.5632(7) 1.0248(7) 0.1925(6) 0.073(2) Uani 1 1 d . . .
H12 H 0.5790 1.0736 0.1335 0.087 Uiso 1 1 calc R . .
C13 C 0.6285(8) 1.0106(8) 0.2580(7) 0.086(3) Uani 1 1 d . . .
H13 H 0.6857 1.0501 0.2436 0.104 Uiso 1 1 calc R . .
C14 C 0.6066(7) 0.9381(7) 0.3424(6) 0.072(2) Uani 1 1 d . . .
H14 H 0.6484 0.9275 0.3877 0.087 Uiso 1 1 calc R . .
C15 C 0.5228(6) 0.8796(6) 0.3619(5) 0.0585(17) Uani 1 1 d . . .
C16 C 0.4510(5) 0.8930(6) 0.2995(5) 0.0503(16) Uani 1 1 d . A .
C17 C 0.4741(6) 0.6280(6) 0.2170(5) 0.0522(16) Uani 1 1 d . A .
C18 C 0.5754(6) 0.6177(6) 0.1509(5) 0.0601(18) Uani 1 1 d . . .
C19 C 0.6832(7) 0.5451(7) 0.1730(7) 0.076(2) Uani 1 1 d . B .
H19 H 0.7484 0.5419 0.1274 0.091 Uiso 1 1 calc R . .
C20 C 0.6912(7) 0.4793(7) 0.2625(7) 0.082(3) Uani 1 1 d . . .
H20 H 0.7615 0.4300 0.2782 0.098 Uiso 1 1 calc R B .
C21 C 0.5948(7) 0.4873(7) 0.3279(6) 0.074(2) Uani 1 1 d . B .
H21 H 0.6004 0.4428 0.3886 0.089 Uiso 1 1 calc R . .
C22 C 0.4887(6) 0.5594(6) 0.3073(5) 0.0594(18) Uani 1 1 d . . .
C23 C 0.3942(7) 0.5589(6) 0.3826(5) 0.0621(19) Uani 1 1 d . A .
H23 H 0.4073 0.5008 0.4375 0.074 Uiso 1 1 calc R . .
C24 C 0.2153(7) 0.6135(8) 0.4717(5) 0.074(2) Uani 1 1 d . A .
H24A H 0.2525 0.5486 0.5184 0.089 Uiso 1 1 calc R . .
H24B H 0.1466 0.5970 0.4655 0.089 Uiso 1 1 calc R . .
C25 C 0.1828(8) 0.7223(8) 0.4994(5) 0.081(2) Uani 1 1 d . A .
H25A H 0.1288 0.7142 0.5570 0.097 Uiso 1 1 calc R . .
H25B H 0.2511 0.7364 0.5087 0.097 Uiso 1 1 calc R . .
C26 C 0.0308(7) 0.8808(9) 0.4484(6) 0.079(2) Uani 1 1 d . A .
H26 H -0.0008 0.8598 0.5106 0.095 Uiso 1 1 calc R . .
C27 C -0.0403(6) 0.9760(8) 0.3924(6) 0.073(2) Uani 1 1 d . . .
C28 C -0.1528(8) 1.0222(11) 0.4274(8) 0.102(3) Uani 1 1 d . . .
H28 H -0.1798 0.9887 0.4890 0.122 Uiso 1 1 calc R . .
C29 C -0.2265(8) 1.1123(12) 0.3790(11) 0.114(4) Uani 1 1 d . . .
H29 H -0.3026 1.1374 0.4059 0.137 Uiso 1 1 calc R . .
C30 C -0.1883(8) 1.1652(10) 0.2914(10) 0.101(4) Uani 1 1 d . C .
H30 H -0.2373 1.2292 0.2574 0.121 Uiso 1 1 calc R . .
C31 C -0.0777(7) 1.1249(8) 0.2524(8) 0.086(3) Uani 1 1 d D . .
C32 C 0.0019(6) 1.0270(8) 0.2989(6) 0.072(2) Uani 1 1 d . A .
C33 C 0.2537(9) 0.2684(11) 0.2266(9) 0.117(4) Uani 1 1 d . . .
H33A H 0.3269 0.2455 0.1882 0.141 Uiso 1 1 calc R . .
H33B H 0.1932 0.2900 0.1902 0.141 Uiso 1 1 calc R . .
C34 C 0.2362(13) 0.1645(11) 0.3073(11) 0.177(7) Uani 1 1 d . . .
H34A H 0.2874 0.1497 0.3494 0.266 Uiso 1 1 calc R . .
H34B H 0.2526 0.0979 0.2858 0.266 Uiso 1 1 calc R . .
H34C H 0.1576 0.1799 0.3383 0.266 Uiso 1 1 calc R . .
C35 C 0.1418(11) 0.4202(11) 0.3080(10) 0.126(4) Uani 1 1 d . . .
H35A H 0.1368 0.3677 0.3700 0.151 Uiso 1 1 calc R . .
H35B H 0.1459 0.4938 0.3116 0.151 Uiso 1 1 calc R . .
C36 C 0.0353(12) 0.4391(13) 0.2724(13) 0.179(7) Uani 1 1 d . . .
H36A H 0.0274 0.3659 0.2726 0.268 Uiso 1 1 calc R . .
H36B H 0.0398 0.4900 0.2105 0.268 Uiso 1 1 calc R . .
H36C H -0.0305 0.4736 0.3108 0.268 Uiso 1 1 calc R . .
C37 C 0.3535(11) 0.3530(12) 0.2934(10) 0.139(5) Uani 1 1 d . . .
H37A H 0.3511 0.2909 0.3508 0.166 Uiso 1 1 calc R . .
H37B H 0.3474 0.4235 0.3078 0.166 Uiso 1 1 calc R . .
C38 C 0.4662(9) 0.3235(12) 0.2327(11) 0.147(6) Uani 1 1 d . . .
H38A H 0.4802 0.2459 0.2291 0.220 Uiso 1 1 calc R . .
H38B H 0.5272 0.3282 0.2577 0.220 Uiso 1 1 calc R . .
H38C H 0.4636 0.3772 0.1721 0.220 Uiso 1 1 calc R . .
N1 N 0.1719(5) 0.8534(5) 0.1175(4) 0.0573(14) Uani 1 1 d . . .
N2 N 0.3277(5) 0.9575(5) 0.1401(4) 0.0526(13) Uani 1 1 d . . .
N3 N 0.2952(5) 0.6287(5) 0.3828(4) 0.0572(14) Uani 1 1 d . . .
N4 N 0.1296(5) 0.8202(6) 0.4275(4) 0.0685(17) Uani 1 1 d . . .
N5 N -0.1238(7) 0.6794(8) 0.4144(6) 0.097(2) Uani 0.584(14) 1 d PDU A 1
O5 O -0.0420(10) 0.6134(15) 0.4537(8) 0.125(5) Uani 0.584(14) 1 d PDU A 1
O6 O -0.2168(12) 0.7044(17) 0.4599(12) 0.133(6) Uani 0.584(14) 1 d PDU A 1
N5' N -0.1238(7) 0.6794(8) 0.4144(6) 0.097(2) Uani 0.416(14) 1 d PDU A 2
O5' O -0.0795(15) 0.7220(19) 0.4514(11) 0.104(4) Uani 0.416(14) 1 d PDU A 2
O6' O -0.2057(17) 0.641(2) 0.4537(17) 0.122(6) Uani 0.416(14) 1 d PDU A 2
N6 N 0.5069(6) 0.7996(7) 0.4533(5) 0.0768(19) Uani 1 1 d . . .
N7 N 0.5747(7) 0.6858(7) 0.0562(6) 0.0888(19) Uani 0.850(9) 1 d PDU B 1
O9 O 0.6598(8) 0.7224(9) 0.0121(6) 0.120(3) Uani 0.850(9) 1 d PDU B 1
O10 O 0.4965(7) 0.6989(8) 0.0189(5) 0.110(3) Uani 0.850(9) 1 d PDU B 1
N7' N 0.5747(7) 0.6858(7) 0.0562(6) 0.0888(19) Uani 0.150(9) 1 d PDU B 2
O9' O 0.530(4) 0.7913(16) 0.036(3) 0.110(7) Uani 0.150(9) 1 d PDU B 2
O10' O 0.636(4) 0.642(3) -0.002(2) 0.108(7) Uani 0.150(9) 1 d PDU B 2
N8 N -0.0396(11) 1.1882(14) 0.1587(9) 0.127(4) Uani 0.757(11) 1 d PDU C 1
O11 O 0.0550(10) 1.2100(10) 0.1344(9) 0.143(4) Uani 0.757(11) 1 d PDU C 1
O12 O -0.1064(11) 1.2257(14) 0.1037(9) 0.167(4) Uani 0.757(11) 1 d PDU C 1
N8' N -0.044(4) 1.186(3) 0.1572(13) 0.136(5) Uani 0.243(11) 1 d PDU C 2
O11' O -0.016(3) 1.131(3) 0.101(3) 0.147(7) Uani 0.243(11) 1 d PDU C 2
O12' O -0.065(4) 1.291(3) 0.134(3) 0.155(7) Uani 0.243(11) 1 d PDU C 2
N9 N 0.2537(6) 0.3700(6) 0.2493(5) 0.0802(19) Uani 1 1 d . . .
H9C H 0.2612 0.4263 0.1948 0.096 Uiso 1 1 calc R . .
O1 O 0.0798(4) 0.7388(5) 0.2954(3) 0.0673(13) Uani 1 1 d . . .
O2 O 0.3684(4) 0.8444(4) 0.3217(3) 0.0585(12) Uani 1 1 d . . .
O3 O 0.3770(4) 0.6954(4) 0.1945(3) 0.0598(12) Uani 1 1 d . . .
O4 O 0.1050(4) 0.9886(4) 0.2573(4) 0.0702(14) Uani 1 1 d . . .
O7 O 0.4866(7) 0.7097(6) 0.4633(5) 0.115(3) Uani 1 1 d . . .
O8 O 0.5175(6) 0.8258(8) 0.5187(5) 0.120(3) Uani 1 1 d . . .
O1W O 0.2872(9) 0.5696(8) 0.1167(8) 0.083(4) Uani 0.606(16) 1 d P D 1
O1W' O 0.2882(15) 0.5916(15) 0.0280(14) 0.100(7) Uani 0.394(16) 1 d P D 2
O2W O 0.964(3) 0.533(3) 0.009(3) 0.252(15) Uani 0.50 1 d PU . 1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 O4 2.238(5) . ?
Er1 O2 2.247(5) . ?
Er1 O1 2.260(5) . ?
Er1 O3 2.288(5) . ?
Er1 N3 2.470(6) . ?
Er1 N1 2.478(6) . ?
Er1 N2 2.500(5) . ?
Er1 N4 2.524(6) . ?
C1 O1 1.285(8) . ?
C1 C2 1.414(11) . ?
C1 C6 1.421(11) . ?
C2 C3 1.372(11) . ?
C2 N5 1.424(11) . ?
C3 C4 1.359(14) . ?
C3 H3 0.9300 . ?
C4 C5 1.383(13) . ?
C4 H4 0.9300 . ?
C5 C6 1.409(10) . ?
C5 H5 0.9300 . ?
C6 C7 1.450(11) . ?
C7 N1 1.283(9) . ?
C7 H7 0.9300 . ?
C8 N1 1.442(9) . ?
C8 C9 1.502(11) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N2 1.472(8) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.269(9) . ?
C10 C11 1.442(10) . ?
C10 H10 0.9300 . ?
C11 C12 1.382(10) . ?
C11 C16 1.410(9) . ?
C12 C13 1.393(12) . ?
C12 H12 0.9300 . ?
C13 C14 1.343(12) . ?
C13 H13 0.9300 . ?
C14 C15 1.371(10) . ?
C14 H14 0.9300 . ?
C15 C16 1.415(9) . ?
C15 N6 1.448(10) . ?
C16 O2 1.269(7) . ?
C17 O3 1.286(8) . ?
C17 C22 1.404(10) . ?
C17 C18 1.409(10) . ?
C18 C19 1.407(10) . ?
C18 N7 1.436(11) . ?
C19 C20 1.372(12) . ?
C19 H19 0.9300 . ?
C20 C21 1.361(12) . ?
C20 H20 0.9300 . ?
C21 C22 1.383(10) . ?
C21 H21 0.9300 . ?
C22 C23 1.432(10) . ?
C23 N3 1.262(9) . ?
C23 H23 0.9300 . ?
C24 N3 1.478(9) . ?
C24 C25 1.491(12) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 N4 1.462(11) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 N4 1.251(10) . ?
C26 C27 1.410(12) . ?
C26 H26 0.9300 . ?
C27 C28 1.376(12) . ?
C27 C32 1.417(12) . ?
C28 C29 1.343(16) . ?
C28 H28 0.9300 . ?
C29 C30 1.337(16) . ?
C29 H29 0.9300 . ?
C30 C31 1.360(13) . ?
C30 H30 0.9300 . ?
C31 C32 1.416(12) . ?
C31 N8' 1.444(17) . ?
C31 N8 1.447(15) . ?
C32 O4 1.299(9) . ?
C33 N9 1.447(12) . ?
C33 C34 1.506(18) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 C36 1.477(17) . ?
C35 N9 1.536(13) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 N9 1.486(13) . ?
C37 C38 1.491(16) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
N5 O6 1.198(11) . ?
N5 O5 1.237(11) . ?
N6 O7 1.191(9) . ?
N6 O8 1.228(9) . ?
N7 O10 1.193(10) . ?
N7 O9 1.230(10) . ?
N8 O12 1.217(10) . ?
N8 O11 1.221(10) . ?
N8' O11' 1.216(12) . ?
N8' O12' 1.216(12) . ?
N9 H9C 0.9100 . ?
O2W O2W 1.06(6) 2_765 ?

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
O4 Er1 O2 98.79(19) . . ?
O4 Er1 O1 87.5(2) . . ?
O2 Er1 O1 148.29(17) . . ?
O4 Er1 O3 148.66(19) . . ?
O2 Er1 O3 87.82(18) . . ?
O1 Er1 O3 102.82(19) . . ?
O4 Er1 N3 139.9(2) . . ?
O2 Er1 N3 76.19(17) . . ?
O1 Er1 N3 79.09(18) . . ?
O3 Er1 N3 71.40(18) . . ?
O4 Er1 N1 79.74(19) . . ?
O2 Er1 N1 139.58(18) . . ?
O1 Er1 N1 72.08(18) . . ?
O3 Er1 N1 75.66(17) . . ?
N3 Er1 N1 129.45(19) . . ?
O4 Er1 N2 74.85(19) . . ?
O2 Er1 N2 72.22(17) . . ?
O1 Er1 N2 138.89(18) . . ?
O3 Er1 N2 78.20(18) . . ?
N3 Er1 N2 136.51(18) . . ?
N1 Er1 N2 68.42(19) . . ?
O4 Er1 N4 71.7(2) . . ?
O2 Er1 N4 79.02(18) . . ?
O1 Er1 N4 73.54(19) . . ?
O3 Er1 N4 139.5(2) . . ?
N3 Er1 N4 68.3(2) . . ?
N1 Er1 N4 135.7(2) . . ?
N2 Er1 N4 131.3(2) . . ?
O1 C1 C2 124.0(8) . . ?
O1 C1 C6 120.6(7) . . ?
C2 C1 C6 115.4(7) . . ?
C3 C2 C1 123.3(9) . . ?
C3 C2 N5 116.2(8) . . ?
C1 C2 N5 120.5(7) . . ?
C4 C3 C2 120.1(9) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 120.1(8) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 C6 120.6(9) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C5 C6 C1 120.3(8) . . ?
C5 C6 C7 116.4(8) . . ?
C1 C6 C7 123.3(7) . . ?
N1 C7 C6 127.7(7) . . ?
N1 C7 H7 116.2 . . ?
C6 C7 H7 116.2 . . ?
N1 C8 C9 109.6(6) . . ?
N1 C8 H8A 109.7 . . ?
C9 C8 H8A 109.7 . . ?
N1 C8 H8B 109.7 . . ?
C9 C8 H8B 109.7 . . ?
H8A C8 H8B 108.2 . . ?
N2 C9 C8 108.4(6) . . ?
N2 C9 H9A 110.0 . . ?
C8 C9 H9A 110.0 . . ?
N2 C9 H9B 110.0 . . ?
C8 C9 H9B 110.0 . . ?
H9A C9 H9B 108.4 . . ?
N2 C10 C11 128.2(7) . . ?
N2 C10 H10 115.9 . . ?
C11 C10 H10 115.9 . . ?
C12 C11 C16 120.2(7) . . ?
C12 C11 C10 117.0(7) . . ?
C16 C11 C10 122.7(6) . . ?
C11 C12 C13 122.8(8) . . ?
C11 C12 H12 118.6 . . ?
C13 C12 H12 118.6 . . ?
C14 C13 C12 118.1(8) . . ?
C14 C13 H13 120.9 . . ?
C12 C13 H13 120.9 . . ?
C13 C14 C15 120.0(8) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C14 C15 C16 124.6(7) . . ?
C14 C15 N6 117.0(7) . . ?
C16 C15 N6 118.4(6) . . ?
O2 C16 C11 122.7(6) . . ?
O2 C16 C15 123.1(6) . . ?
C11 C16 C15 114.1(6) . . ?
O3 C17 C22 123.9(7) . . ?
O3 C17 C18 121.4(6) . . ?
C22 C17 C18 114.7(6) . . ?
C19 C18 C17 123.0(7) . . ?
C19 C18 N7 116.0(8) . . ?
C17 C18 N7 121.0(7) . . ?
C20 C19 C18 119.3(8) . . ?
C20 C19 H19 120.3 . . ?
C18 C19 H19 120.3 . . ?
C21 C20 C19 119.0(7) . . ?
C21 C20 H20 120.5 . . ?
C19 C20 H20 120.5 . . ?
C20 C21 C22 122.2(8) . . ?
C20 C21 H21 118.9 . . ?
C22 C21 H21 118.9 . . ?
C21 C22 C17 121.7(8) . . ?
C21 C22 C23 116.4(7) . . ?
C17 C22 C23 121.9(6) . . ?
N3 C23 C22 127.1(7) . . ?
N3 C23 H23 116.4 . . ?
C22 C23 H23 116.4 . . ?
N3 C24 C25 108.9(6) . . ?
N3 C24 H24A 109.9 . . ?
C25 C24 H24A 109.9 . . ?
N3 C24 H24B 109.9 . . ?
C25 C24 H24B 109.9 . . ?
H24A C24 H24B 108.3 . . ?
N4 C25 C24 109.6(7) . . ?
N4 C25 H25A 109.7 . . ?
C24 C25 H25A 109.7 . . ?
N4 C25 H25B 109.7 . . ?
C24 C25 H25B 109.7 . . ?
H25A C25 H25B 108.2 . . ?
N4 C26 C27 130.1(8) . . ?
N4 C26 H26 115.0 . . ?
C27 C26 H26 115.0 . . ?
C28 C27 C26 120.8(10) . . ?
C28 C27 C32 118.0(9) . . ?
C26 C27 C32 121.2(7) . . ?
C29 C28 C27 124.7(11) . . ?
C29 C28 H28 117.7 . . ?
C27 C28 H28 117.7 . . ?
C30 C29 C28 118.8(10) . . ?
C30 C29 H29 120.6 . . ?
C28 C29 H29 120.6 . . ?
C29 C30 C31 119.8(11) . . ?
C29 C30 H30 120.1 . . ?
C31 C30 H30 120.1 . . ?
C30 C31 C32 123.8(11) . . ?
C30 C31 N8' 116(2) . . ?
C32 C31 N8' 120(2) . . ?
C30 C31 N8 117.4(11) . . ?
C32 C31 N8 118.8(9) . . ?
N8' C31 N8 3(2) . . ?
O4 C32 C27 123.7(8) . . ?
O4 C32 C31 121.5(9) . . ?
C27 C32 C31 114.8(8) . . ?
N9 C33 C34 115.8(10) . . ?
N9 C33 H33A 108.3 . . ?
C34 C33 H33A 108.3 . . ?
N9 C33 H33B 108.3 . . ?
C34 C33 H33B 108.3 . . ?
H33A C33 H33B 107.4 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36 C35 N9 114.2(11) . . ?
C36 C35 H35A 108.7 . . ?
N9 C35 H35A 108.7 . . ?
C36 C35 H35B 108.7 . . ?
N9 C35 H35B 108.7 . . ?
H35A C35 H35B 107.6 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N9 C37 C38 111.9(11) . . ?
N9 C37 H37A 109.2 . . ?
C38 C37 H37A 109.2 . . ?
N9 C37 H37B 109.2 . . ?
C38 C37 H37B 109.2 . . ?
H37A C37 H37B 107.9 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C7 N1 C8 116.2(6) . . ?
C7 N1 Er1 130.3(5) . . ?
C8 N1 Er1 113.3(4) . . ?
C10 N2 C9 116.8(6) . . ?
C10 N2 Er1 130.0(5) . . ?
C9 N2 Er1 113.1(4) . . ?
C23 N3 C24 116.3(6) . . ?
C23 N3 Er1 128.1(5) . . ?
C24 N3 Er1 113.7(5) . . ?
C26 N4 C25 118.9(7) . . ?
C26 N4 Er1 126.3(6) . . ?
C25 N4 Er1 113.1(5) . . ?
O6 N5 O5 118.9(14) . . ?
O6 N5 C2 120.6(12) . . ?
O5 N5 C2 120.2(10) . . ?
O7 N6 O8 121.7(8) . . ?
O7 N6 C15 120.0(8) . . ?
O8 N6 C15 118.3(8) . . ?
O10 N7 O9 120.3(9) . . ?
O10 N7 C18 120.3(9) . . ?
O9 N7 C18 119.2(9) . . ?
O12 N8 O11 119.1(16) . . ?
O12 N8 C31 118.7(13) . . ?
O11 N8 C31 122.0(11) . . ?
O11' N8' O12' 122(3) . . ?
O11' N8' C31 117(3) . . ?
O12' N8' C31 119(3) . . ?
C33 N9 C37 113.6(9) . . ?
C33 N9 C35 115.1(8) . . ?
C37 N9 C35 108.8(9) . . ?
C33 N9 H9C 106.2 . . ?
C37 N9 H9C 106.2 . . ?
C35 N9 H9C 106.2 . . ?
C1 O1 Er1 142.2(5) . . ?
C16 O2 Er1 143.8(4) . . ?
C17 O3 Er1 131.5(4) . . ?
C32 O4 Er1 136.3(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 -175.2(8) . . . . ?
C6 C1 C2 C3 3.6(11) . . . . ?
O1 C1 C2 N5 6.6(12) . . . . ?
C6 C1 C2 N5 -174.7(8) . . . . ?
C1 C2 C3 C4 -0.6(13) . . . . ?
N5 C2 C3 C4 177.8(9) . . . . ?
C2 C3 C4 C5 -1.8(14) . . . . ?
C3 C4 C5 C6 1.0(13) . . . . ?
C4 C5 C6 C1 2.3(12) . . . . ?
C4 C5 C6 C7 -176.6(7) . . . . ?
O1 C1 C6 C5 174.4(7) . . . . ?
C2 C1 C6 C5 -4.4(10) . . . . ?
O1 C1 C6 C7 -6.8(11) . . . . ?
C2 C1 C6 C7 174.4(7) . . . . ?
C5 C6 C7 N1 176.3(8) . . . . ?
C1 C6 C7 N1 -2.5(12) . . . . ?
N1 C8 C9 N2 58.8(8) . . . . ?
N2 C10 C11 C12 -178.4(7) . . . . ?
N2 C10 C11 C16 0.3(12) . . . . ?
C16 C11 C12 C13 -1.2(12) . . . . ?
C10 C11 C12 C13 177.6(8) . . . . ?
C11 C12 C13 C14 1.3(14) . . . . ?
C12 C13 C14 C15 0.6(13) . . . . ?
C13 C14 C15 C16 -2.8(13) . . . . ?
C13 C14 C15 N6 177.7(8) . . . . ?
C12 C11 C16 O2 176.6(7) . . . . ?
C10 C11 C16 O2 -2.2(10) . . . . ?
C12 C11 C16 C15 -0.7(10) . . . . ?
C10 C11 C16 C15 -179.5(6) . . . . ?
C14 C15 C16 O2 -174.6(7) . . . . ?
N6 C15 C16 O2 4.9(10) . . . . ?
C14 C15 C16 C11 2.7(10) . . . . ?
N6 C15 C16 C11 -177.8(6) . . . . ?
O3 C17 C18 C19 179.8(7) . . . . ?
C22 C17 C18 C19 -0.4(10) . . . . ?
O3 C17 C18 N7 2.5(11) . . . . ?
C22 C17 C18 N7 -177.7(7) . . . . ?
C17 C18 C19 C20 1.2(12) . . . . ?
N7 C18 C19 C20 178.6(8) . . . . ?
C18 C19 C20 C21 -1.0(13) . . . . ?
C19 C20 C21 C22 0.2(13) . . . . ?
C20 C21 C22 C17 0.6(12) . . . . ?
C20 C21 C22 C23 179.6(8) . . . . ?
O3 C17 C22 C21 179.4(7) . . . . ?
C18 C17 C22 C21 -0.5(10) . . . . ?
O3 C17 C22 C23 0.4(11) . . . . ?
C18 C17 C22 C23 -179.5(6) . . . . ?
C21 C22 C23 N3 169.0(7) . . . . ?
C17 C22 C23 N3 -11.9(12) . . . . ?
N3 C24 C25 N4 58.0(8) . . . . ?
N4 C26 C27 C28 172.0(9) . . . . ?
N4 C26 C27 C32 -8.2(14) . . . . ?
C26 C27 C28 C29 -179.7(10) . . . . ?
C32 C27 C28 C29 0.5(15) . . . . ?
C27 C28 C29 C30 -2.8(17) . . . . ?
C28 C29 C30 C31 2.0(16) . . . . ?
C29 C30 C31 C32 1.0(15) . . . . ?
C29 C30 C31 N8' 179(2) . . . . ?
C29 C30 C31 N8 -177.6(10) . . . . ?
C28 C27 C32 O4 -177.5(8) . . . . ?
C26 C27 C32 O4 2.7(12) . . . . ?
C28 C27 C32 C31 2.4(11) . . . . ?
C26 C27 C32 C31 -177.5(8) . . . . ?
C30 C31 C32 O4 176.7(8) . . . . ?
N8' C31 C32 O4 -1(2) . . . . ?
N8 C31 C32 O4 -4.7(13) . . . . ?
C30 C31 C32 C27 -3.2(12) . . . . ?
N8' C31 C32 C27 179(2) . . . . ?
N8 C31 C32 C27 175.4(9) . . . . ?
C6 C7 N1 C8 -178.5(7) . . . . ?
C6 C7 N1 Er1 -3.0(11) . . . . ?
C9 C8 N1 C7 129.9(7) . . . . ?
C9 C8 N1 Er1 -46.3(7) . . . . ?
O4 Er1 N1 C7 -80.7(6) . . . . ?
O2 Er1 N1 C7 -172.2(6) . . . . ?
O1 Er1 N1 C7 10.0(6) . . . . ?
O3 Er1 N1 C7 118.9(6) . . . . ?
N3 Er1 N1 C7 68.4(7) . . . . ?
N2 Er1 N1 C7 -158.3(7) . . . . ?
N4 Er1 N1 C7 -30.7(7) . . . . ?
O4 Er1 N1 C8 94.9(5) . . . . ?
O2 Er1 N1 C8 3.3(6) . . . . ?
O1 Er1 N1 C8 -174.4(5) . . . . ?
O3 Er1 N1 C8 -65.5(5) . . . . ?
N3 Er1 N1 C8 -116.0(5) . . . . ?
N2 Er1 N1 C8 17.3(4) . . . . ?
N4 Er1 N1 C8 144.9(5) . . . . ?
C11 C10 N2 C9 176.5(7) . . . . ?
C11 C10 N2 Er1 -2.0(11) . . . . ?
C8 C9 N2 C10 138.8(7) . . . . ?
C8 C9 N2 Er1 -42.4(7) . . . . ?
O4 Er1 N2 C10 108.0(6) . . . . ?
O2 Er1 N2 C10 3.3(6) . . . . ?
O1 Er1 N2 C10 175.8(5) . . . . ?
O3 Er1 N2 C10 -88.2(6) . . . . ?
N3 Er1 N2 C10 -42.1(7) . . . . ?
N1 Er1 N2 C10 -167.3(7) . . . . ?
N4 Er1 N2 C10 60.1(7) . . . . ?
O4 Er1 N2 C9 -70.6(5) . . . . ?
O2 Er1 N2 C9 -175.2(5) . . . . ?
O1 Er1 N2 C9 -2.8(6) . . . . ?
O3 Er1 N2 C9 93.3(5) . . . . ?
N3 Er1 N2 C9 139.4(5) . . . . ?
N1 Er1 N2 C9 14.2(5) . . . . ?
N4 Er1 N2 C9 -118.5(5) . . . . ?
C22 C23 N3 C24 -176.3(7) . . . . ?
C22 C23 N3 Er1 -12.9(11) . . . . ?
C25 C24 N3 C23 119.8(8) . . . . ?
C25 C24 N3 Er1 -46.0(7) . . . . ?
O4 Er1 N3 C23 -150.0(6) . . . . ?
O2 Er1 N3 C23 -62.7(6) . . . . ?
O1 Er1 N3 C23 137.3(6) . . . . ?
O3 Er1 N3 C23 29.7(6) . . . . ?
N1 Er1 N3 C23 81.7(6) . . . . ?
N2 Er1 N3 C23 -18.4(7) . . . . ?
N4 Er1 N3 C23 -146.2(7) . . . . ?
O4 Er1 N3 C24 13.8(6) . . . . ?
O2 Er1 N3 C24 101.1(5) . . . . ?
O1 Er1 N3 C24 -58.9(5) . . . . ?
O3 Er1 N3 C24 -166.5(5) . . . . ?
N1 Er1 N3 C24 -114.5(5) . . . . ?
N2 Er1 N3 C24 145.4(4) . . . . ?
N4 Er1 N3 C24 17.6(5) . . . . ?
C27 C26 N4 C25 -177.6(8) . . . . ?
C27 C26 N4 Er1 -13.6(13) . . . . ?
C24 C25 N4 C26 124.0(8) . . . . ?
C24 C25 N4 Er1 -41.9(7) . . . . ?
O4 Er1 N4 C26 25.9(7) . . . . ?
O2 Er1 N4 C26 129.1(7) . . . . ?
O1 Er1 N4 C26 -67.0(7) . . . . ?
O3 Er1 N4 C26 -157.6(6) . . . . ?
N3 Er1 N4 C26 -151.6(8) . . . . ?
N1 Er1 N4 C26 -26.7(8) . . . . ?
N2 Er1 N4 C26 74.8(7) . . . . ?
O4 Er1 N4 C25 -169.4(6) . . . . ?
O2 Er1 N4 C25 -66.2(5) . . . . ?
O1 Er1 N4 C25 97.7(5) . . . . ?
O3 Er1 N4 C25 7.2(7) . . . . ?
N3 Er1 N4 C25 13.2(5) . . . . ?
N1 Er1 N4 C25 138.1(5) . . . . ?
N2 Er1 N4 C25 -120.4(5) . . . . ?
C3 C2 N5 O6 -35.0(19) . . . . ?
C1 C2 N5 O6 143.4(16) . . . . ?
C3 C2 N5 O5 138.6(12) . . . . ?
C1 C2 N5 O5 -42.9(15) . . . . ?
C14 C15 N6 O7 -141.6(9) . . . . ?
C16 C15 N6 O7 38.8(11) . . . . ?
C14 C15 N6 O8 36.7(11) . . . . ?
C16 C15 N6 O8 -142.8(8) . . . . ?
C19 C18 N7 O10 140.1(9) . . . . ?
C17 C18 N7 O10 -42.4(12) . . . . ?
C19 C18 N7 O9 -34.0(12) . . . . ?
C17 C18 N7 O9 143.5(9) . . . . ?
C30 C31 N8 O12 -39.7(19) . . . . ?
C32 C31 N8 O12 141.6(15) . . . . ?
N8' C31 N8 O12 30(38) . . . . ?
C30 C31 N8 O11 136.6(14) . . . . ?
C32 C31 N8 O11 -42.0(18) . . . . ?
N8' C31 N8 O11 -153(40) . . . . ?
C30 C31 N8' O11' -117(4) . . . . ?
C32 C31 N8' O11' 61(5) . . . . ?
N8 C31 N8' O11' 131(42) . . . . ?
C30 C31 N8' O12' 49(6) . . . . ?
C32 C31 N8' O12' -133(5) . . . . ?
N8 C31 N8' O12' -63(36) . . . . ?
C34 C33 N9 C37 66.5(14) . . . . ?
C34 C33 N9 C35 -59.9(15) . . . . ?
C38 C37 N9 C33 60.0(14) . . . . ?
C38 C37 N9 C35 -170.4(11) . . . . ?
C36 C35 N9 C33 -50.0(15) . . . . ?
C36 C35 N9 C37 -178.8(12) . . . . ?
C2 C1 O1 Er1 -153.9(6) . . . . ?
C6 C1 O1 Er1 27.4(12) . . . . ?
O4 Er1 O1 C1 55.4(8) . . . . ?
O2 Er1 O1 C1 158.2(7) . . . . ?
O3 Er1 O1 C1 -94.7(8) . . . . ?
N3 Er1 O1 C1 -162.6(8) . . . . ?
N1 Er1 O1 C1 -24.6(8) . . . . ?
N2 Er1 O1 C1 -8.1(9) . . . . ?
N4 Er1 O1 C1 127.0(8) . . . . ?
C11 C16 O2 Er1 7.4(11) . . . . ?
C15 C16 O2 Er1 -175.5(5) . . . . ?
O4 Er1 O2 C16 -77.6(7) . . . . ?
O1 Er1 O2 C16 -177.2(6) . . . . ?
O3 Er1 O2 C16 71.6(7) . . . . ?
N3 Er1 O2 C16 143.0(7) . . . . ?
N1 Er1 O2 C16 6.9(8) . . . . ?
N2 Er1 O2 C16 -6.7(7) . . . . ?
N4 Er1 O2 C16 -146.9(7) . . . . ?
C22 C17 O3 Er1 39.9(10) . . . . ?
C18 C17 O3 Er1 -140.2(6) . . . . ?
O4 Er1 O3 C17 135.6(6) . . . . ?
O2 Er1 O3 C17 32.2(6) . . . . ?
O1 Er1 O3 C17 -117.6(6) . . . . ?
N3 Er1 O3 C17 -44.0(6) . . . . ?
N1 Er1 O3 C17 175.0(6) . . . . ?
N2 Er1 O3 C17 104.5(6) . . . . ?
N4 Er1 O3 C17 -38.0(7) . . . . ?
C27 C32 O4 Er1 31.4(11) . . . . ?
C31 C32 O4 Er1 -148.4(6) . . . . ?
O2 Er1 O4 C32 -111.9(7) . . . . ?
O1 Er1 O4 C32 36.8(7) . . . . ?
O3 Er1 O4 C32 147.7(6) . . . . ?
N3 Er1 O4 C32 -33.0(8) . . . . ?
N1 Er1 O4 C32 109.0(7) . . . . ?
N2 Er1 O4 C32 179.3(7) . . . . ?
N4 Er1 O4 C32 -36.7(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         1.037
_refine_diff_density_min         -0.997
_refine_diff_density_rms         0.105
