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

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

data_x
_database_code_depnum_ccdc_archive 'CCDC 1044883'
_audit_update_record             
;
2015-11-09 deposited with the CCDC.
2015-11-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C122 H116 La2 N16 O21'
_chemical_formula_weight         2420.13

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   13.729(3)
_cell_length_b                   14.267(3)
_cell_length_c                   16.791(3)
_cell_angle_alpha                79.44(3)
_cell_angle_beta                 71.27(3)
_cell_angle_gamma                64.18(3)
_cell_volume                     2800.1(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    12640
_cell_measurement_theta_min      3.09
_cell_measurement_theta_max      27.46

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1242
_exptl_absorpt_coefficient_mu    0.831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7216
_exptl_absorpt_correction_T_max  0.8925
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            22275
_diffrn_reflns_av_R_equivalents  0.1024
_diffrn_reflns_av_sigmaI/netI    0.1256
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.09
_diffrn_reflns_theta_max         25.02
_reflns_number_total             9856
_reflns_number_gt                6605
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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)+(0.0000P)²+13.3259P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0042(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         9856
_refine_ls_number_parameters     737
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.1198
_refine_ls_R_factor_gt           0.0726
_refine_ls_wR_factor_ref         0.1525
_refine_ls_wR_factor_gt          0.1265
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.15471(3) 0.49775(3) 0.43744(3) 0.03321(16) Uani 1 1 d . . .
O1 O 0.2374(4) 0.3942(4) 0.3031(3) 0.0473(13) Uani 1 1 d . . .
O2 O 0.2247(4) 0.5552(4) 0.2809(3) 0.0482(14) Uani 1 1 d . . .
O3 O 0.1786(5) 0.4862(5) 0.5846(3) 0.0706(19) Uani 1 1 d . . .
O4 O 0.0091(4) 0.5078(4) 0.5889(3) 0.0407(12) Uani 1 1 d . . .
O5 O 0.1590(4) 0.3255(4) 0.4890(3) 0.0476(14) Uani 1 1 d . . .
O6 O -0.0099(4) 0.3205(4) 0.5483(3) 0.0450(13) Uani 1 1 d . . .
O7 O 0.7013(8) 0.8764(7) -0.1225(7) 0.134(4) Uani 1 1 d . . .
O8 O 0.7913(8) 0.7165(7) -0.0902(6) 0.127(3) Uani 1 1 d . . .
O9 O 0.7579(3) 0.8326(3) -0.0113(2) 0.138(4) Uani 1 1 d . . .
N1 N 0.3798(3) 0.3889(3) 0.4090(2) 0.0391(15) Uani 1 1 d R . .
N2 N 0.2862(3) 0.5987(3) 0.4315(2) 0.0388(15) Uani 1 1 d R . .
N3 N 0.6613(3) 0.0681(3) -0.0123(2) 0.068(2) Uani 1 1 d R . .
H3A H 0.6796 0.0033 -0.0176 0.082 Uiso 1 1 calc R . .
N4 N 0.2993(9) 0.0427(8) 0.8321(6) 0.088(3) Uani 1 1 d . . .
H4A H 0.3093 -0.0003 0.8749 0.106 Uiso 1 1 calc R . .
N5 N -0.0056(6) -0.1754(6) 0.6804(5) 0.068(2) Uani 1 1 d . . .
H5A H -0.0477 -0.2071 0.6837 0.081 Uiso 1 1 calc R . .
N6 N 0.4932(6) 0.5486(5) 0.1864(4) 0.0501(17) Uani 1 1 d . . .
N7 N 0.2917(5) 0.7141(5) 0.2320(4) 0.0471(17) Uani 1 1 d . . .
H7A H 0.2961 0.6520 0.2329 0.057 Uiso 1 1 calc R . .
N8 N 0.7491(8) 0.8090(9) -0.0740(7) 0.087(3) Uani 1 1 d . . .
C1 C 0.4254(7) 0.2890(6) 0.3980(6) 0.059(2) Uani 1 1 d . . .
H1 H 0.3780 0.2557 0.4049 0.071 Uiso 1 1 calc R . .
C2 C 0.5418(8) 0.2290(8) 0.3765(6) 0.072(3) Uani 1 1 d . . .
H2 H 0.5700 0.1580 0.3690 0.087 Uiso 1 1 calc R . .
C3 C 0.6127(7) 0.2759(7) 0.3666(6) 0.067(3) Uani 1 1 d . . .
H3B H 0.6900 0.2372 0.3520 0.080 Uiso 1 1 calc R . .
C4 C 0.5688(6) 0.3823(7) 0.3784(5) 0.053(2) Uani 1 1 d . . .
C5 C 0.6358(7) 0.4388(9) 0.3710(5) 0.066(3) Uani 1 1 d . . .
H5B H 0.7135 0.4029 0.3589 0.080 Uiso 1 1 calc R . .
C6 C 0.5911(7) 0.5405(8) 0.3806(5) 0.060(3) Uani 1 1 d . . .
H6B H 0.6379 0.5746 0.3735 0.072 Uiso 1 1 calc R . .
C7 C 0.4720(6) 0.5988(7) 0.4017(5) 0.046(2) Uani 1 1 d . . .
C8 C 0.4202(8) 0.7061(8) 0.4123(5) 0.063(3) Uani 1 1 d . . .
H8A H 0.4638 0.7436 0.4045 0.076 Uiso 1 1 calc R . .
C9 C 0.3064(8) 0.7556(7) 0.4338(6) 0.067(3) Uani 1 1 d . . .
H9A H 0.2721 0.8267 0.4426 0.081 Uiso 1 1 calc R . .
C10 C 0.2411(7) 0.7004(6) 0.4429(5) 0.055(2) Uani 1 1 d . . .
H10A H 0.1632 0.7358 0.4575 0.066 Uiso 1 1 calc R . .
C11 C 0.4016(6) 0.5477(6) 0.4098(4) 0.0386(18) Uani 1 1 d . . .
C12 C 0.4504(6) 0.4379(6) 0.3984(5) 0.0388(18) Uani 1 1 d . . .
C13 C 0.2531(6) 0.4668(6) 0.2530(5) 0.0413(18) Uani 1 1 d . . .
C14 C 0.3058(7) 0.4506(6) 0.1604(5) 0.054(2) Uani 1 1 d . . .
H14A H 0.3320 0.5053 0.1354 0.064 Uiso 1 1 calc R . .
H14B H 0.2482 0.4583 0.1351 0.064 Uiso 1 1 calc R . .
C15 C 0.4038(7) 0.3454(6) 0.1383(5) 0.051(2) Uani 1 1 d . . .
H15A H 0.4614 0.3365 0.1641 0.062 Uiso 1 1 calc R . .
H15B H 0.3778 0.2903 0.1614 0.062 Uiso 1 1 calc R . .
C16 C 0.4548(8) 0.3352(7) 0.0441(5) 0.068(3) Uani 1 1 d . . .
H16A H 0.3970 0.3427 0.0192 0.081 Uiso 1 1 calc R . .
H16B H 0.4774 0.3925 0.0213 0.081 Uiso 1 1 calc R . .
C17 C 0.5535(7) 0.2359(7) 0.0174(5) 0.055(2) Uani 1 1 d . . .
C18 C 0.5529(7) 0.1424(8) 0.0164(5) 0.065(3) Uani 1 1 d . . .
H18A H 0.4884 0.1292 0.0327 0.077 Uiso 1 1 calc R . .
C19 C 0.7346(8) 0.1164(8) -0.0309(5) 0.062(2) Uani 1 1 d . . .
C20 C 0.8503(9) 0.0753(9) -0.0643(6) 0.083(3) Uani 1 1 d . . .
H20A H 0.8911 0.0049 -0.0748 0.100 Uiso 1 1 calc R . .
C21 C 0.9022(11) 0.1427(12) -0.0813(7) 0.100(4) Uani 1 1 d . . .
H21A H 0.9795 0.1184 -0.1054 0.120 Uiso 1 1 calc R . .
C22 C 0.8412(11) 0.2455(12) -0.0629(8) 0.096(4) Uani 1 1 d . . .
H22A H 0.8791 0.2887 -0.0726 0.116 Uiso 1 1 calc R . .
C23 C 0.7252(10) 0.2879(8) -0.0306(6) 0.071(3) Uani 1 1 d . . .
H23A H 0.6856 0.3586 -0.0208 0.086 Uiso 1 1 calc R . .
C24 C 0.6685(8) 0.2206(7) -0.0128(5) 0.057(2) Uani 1 1 d . . .
C25 C 0.0825(7) 0.4923(7) 0.6264(5) 0.051(2) Uani 1 1 d . . .
C26 C 0.0541(7) 0.4775(8) 0.7209(5) 0.070(3) Uani 1 1 d . . .
H26A H -0.0217 0.4805 0.7423 0.084 Uiso 1 1 calc R . .
H26B H 0.0559 0.5341 0.7439 0.084 Uiso 1 1 calc R . .
C27 C 0.1355(8) 0.3736(8) 0.7509(6) 0.074(3) Uani 1 1 d . . .
H27A H 0.2116 0.3690 0.7260 0.089 Uiso 1 1 calc R . .
H27B H 0.1201 0.3731 0.8115 0.089 Uiso 1 1 calc R . .
C28 C 0.1292(9) 0.2795(9) 0.7298(7) 0.090(4) Uani 1 1 d . . .
H28A H 0.1385 0.2825 0.6698 0.108 Uiso 1 1 calc R . .
H28B H 0.0551 0.2806 0.7587 0.108 Uiso 1 1 calc R . .
C29 C 0.2169(9) 0.1784(8) 0.7539(6) 0.069(3) Uani 1 1 d . . .
C30 C 0.2038(10) 0.1293(11) 0.8317(7) 0.097(4) Uani 1 1 d . . .
H30A H 0.1399 0.1514 0.8770 0.117 Uiso 1 1 calc R . .
C31 C 0.3777(10) 0.0325(9) 0.7560(7) 0.073(3) Uani 1 1 d . . .
C32 C 0.4873(12) -0.0394(9) 0.7278(9) 0.094(4) Uani 1 1 d . . .
H32A H 0.5209 -0.0954 0.7621 0.113 Uiso 1 1 calc R . .
C33 C 0.5438(13) -0.0231(12) 0.6456(12) 0.120(5) Uani 1 1 d . . .
H33A H 0.6172 -0.0704 0.6241 0.144 Uiso 1 1 calc R . .
C34 C 0.4961(14) 0.0600(14) 0.5946(9) 0.117(5) Uani 1 1 d . . .
H34A H 0.5378 0.0678 0.5399 0.140 Uiso 1 1 calc R . .
C35 C 0.3887(12) 0.1310(10) 0.6227(7) 0.088(3) Uani 1 1 d . . .
H35A H 0.3571 0.1870 0.5875 0.105 Uiso 1 1 calc R . .
C36 C 0.3266(9) 0.1189(8) 0.7046(6) 0.065(3) Uani 1 1 d . . .
C37 C 0.0958(6) 0.2773(5) 0.5190(4) 0.0369(17) Uani 1 1 d . . .
C38 C 0.1526(6) 0.1604(6) 0.5176(5) 0.049(2) Uani 1 1 d . . .
H38A H 0.2269 0.1385 0.5249 0.058 Uiso 1 1 calc R . .
H38B H 0.1628 0.1407 0.4622 0.058 Uiso 1 1 calc R . .
C39 C 0.0935(7) 0.1006(6) 0.5822(5) 0.049(2) Uani 1 1 d . . .
H39A H 0.0162 0.1269 0.5800 0.058 Uiso 1 1 calc R . .
H39B H 0.0925 0.1111 0.6379 0.058 Uiso 1 1 calc R . .
C40 C 0.1515(7) -0.0151(6) 0.5667(6) 0.064(3) Uani 1 1 d . . .
H40A H 0.1538 -0.0244 0.5103 0.076 Uiso 1 1 calc R . .
H40B H 0.2286 -0.0405 0.5692 0.076 Uiso 1 1 calc R . .
C41 C 0.0966(7) -0.0803(6) 0.6277(6) 0.051(2) Uani 1 1 d . . .
C42 C 0.0318(8) -0.1207(7) 0.6113(6) 0.063(3) Uani 1 1 d . . .
H42A H 0.0156 -0.1121 0.5601 0.076 Uiso 1 1 calc R . .
C43 C 0.0352(7) -0.1715(6) 0.7438(6) 0.057(2) Uani 1 1 d . . .
C44 C 0.0211(9) -0.2160(7) 0.8253(7) 0.074(3) Uani 1 1 d . . .
H44A H -0.0218 -0.2554 0.8447 0.089 Uiso 1 1 calc R . .
C45 C 0.0724(9) -0.1999(8) 0.8753(7) 0.084(3) Uani 1 1 d . . .
H45A H 0.0651 -0.2295 0.9299 0.101 Uiso 1 1 calc R . .
C46 C 0.1358(9) -0.1397(8) 0.8465(7) 0.080(3) Uani 1 1 d . . .
H46A H 0.1695 -0.1301 0.8825 0.096 Uiso 1 1 calc R . .
C47 C 0.1496(7) -0.0945(7) 0.7664(6) 0.065(3) Uani 1 1 d . . .
H47A H 0.1913 -0.0541 0.7480 0.078 Uiso 1 1 calc R . .
C48 C 0.0986(6) -0.1111(6) 0.7131(5) 0.047(2) Uani 1 1 d . . .
C49 C 0.5933(8) 0.4691(7) 0.1656(6) 0.068(3) Uani 1 1 d . . .
H49A H 0.5957 0.4023 0.1693 0.081 Uiso 1 1 calc R . .
C50 C 0.6958(8) 0.4813(10) 0.1384(7) 0.083(3) Uani 1 1 d . . .
H50A H 0.7637 0.4241 0.1221 0.099 Uiso 1 1 calc R . .
C51 C 0.6944(8) 0.5766(10) 0.1361(6) 0.080(3) Uani 1 1 d . . .
H51A H 0.7615 0.5853 0.1193 0.096 Uiso 1 1 calc R . .
C52 C 0.5927(7) 0.6618(8) 0.1587(5) 0.055(2) Uani 1 1 d . . .
C53 C 0.5812(10) 0.7657(10) 0.1588(6) 0.077(3) Uani 1 1 d . . .
H53A H 0.6463 0.7780 0.1429 0.092 Uiso 1 1 calc R . .
C54 C 0.4817(10) 0.8473(8) 0.1806(6) 0.072(3) Uani 1 1 d . . .
H54A H 0.4784 0.9140 0.1794 0.087 Uiso 1 1 calc R . .
C55 C 0.3814(8) 0.8297(7) 0.2055(5) 0.056(2) Uani 1 1 d . . .
C56 C 0.2751(9) 0.9123(7) 0.2299(6) 0.074(3) Uani 1 1 d . . .
H56A H 0.2690 0.9800 0.2290 0.089 Uiso 1 1 calc R . .
C57 C 0.1800(8) 0.8919(7) 0.2551(6) 0.070(3) Uani 1 1 d . . .
H57A H 0.1091 0.9453 0.2719 0.084 Uiso 1 1 calc R . .
C58 C 0.1918(7) 0.7923(7) 0.2548(5) 0.062(3) Uani 1 1 d . . .
H58A H 0.1277 0.7785 0.2711 0.075 Uiso 1 1 calc R . .
C59 C 0.3874(7) 0.7312(6) 0.2074(5) 0.046(2) Uani 1 1 d . . .
C60 C 0.4946(7) 0.6421(7) 0.1837(4) 0.045(2) Uani 1 1 d . . .
O1W O 0.8061(8) 0.7764(7) -0.2882(5) 0.101(3) Uani 1 1 d D . .
H1A H 0.798(11) 0.730(7) -0.304(5) 0.152 Uiso 1 1 d D . .
H1B H 0.799(5) 0.774(9) -0.2374(7) 0.152 Uiso 1 1 d D . .
O10 O 1.062(2) 0.3685(16) -0.0299(14) 0.182(9) Uani 0.50 1 d PDU A -1
H10B H 1.0858 0.3626 0.0106 0.274 Uiso 0.50 1 calc PR A -1
C61 C 0.970(3) 0.463(2) -0.028(3) 0.19(2) Uani 0.50 1 d PDU A -1
H61A H 0.9066 0.4623 0.0188 0.234 Uiso 0.50 1 calc PR A -1
H61B H 0.9472 0.4755 -0.0800 0.234 Uiso 0.50 1 calc PR A -1
C62 C 1.005(4) 0.5480(16) -0.020(2) 0.149(15) Uani 0.50 1 d PDU A -1
H62A H 0.9434 0.6149 -0.0205 0.224 Uiso 0.50 1 calc PR A -1
H62B H 1.0684 0.5465 -0.0663 0.224 Uiso 0.50 1 calc PR A -1
H62C H 1.0244 0.5360 0.0320 0.224 Uiso 0.50 1 calc PR A -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
La1 O5 2.433(5) . ?
La1 O4 2.463(5) 2_566 ?
La1 O6 2.483(5) 2_566 ?
La1 O3 2.562(5) . ?
La1 O1 2.584(5) . ?
La1 O2 2.603(5) . ?
La1 O4 2.665(5) . ?
La1 N1 2.708(4) . ?
La1 N2 2.728(4) . ?
La1 La1 4.0673(16) 2_566 ?
O1 C13 1.259(8) . ?
O2 C13 1.277(8) . ?
O3 C25 1.252(9) . ?
O4 C25 1.275(8) . ?
O4 La1 2.463(5) 2_566 ?
O5 C37 1.261(8) . ?
O6 C37 1.266(8) . ?
O6 La1 2.483(5) 2_566 ?
O7 N8 1.235(11) . ?
O8 N8 1.231(11) . ?
O9 N8 1.218(11) . ?
N1 C1 1.304(9) . ?
N1 C12 1.375(8) . ?
N2 C10 1.330(8) . ?
N2 C11 1.377(7) . ?
N3 C19 1.381(10) . ?
N3 C18 1.387(9) . ?
N4 C30 1.355(13) . ?
N4 C31 1.365(13) . ?
N5 C42 1.361(10) . ?
N5 C43 1.374(11) . ?
N6 C49 1.333(10) . ?
N6 C60 1.334(10) . ?
N7 C58 1.326(9) . ?
N7 C59 1.359(9) . ?
C1 C2 1.402(11) . ?
C2 C3 1.359(13) . ?
C3 C4 1.395(12) . ?
C4 C12 1.417(9) . ?
C4 C5 1.431(12) . ?
C5 C6 1.325(12) . ?
C6 C7 1.429(11) . ?
C7 C8 1.397(11) . ?
C7 C11 1.405(10) . ?
C8 C9 1.356(12) . ?
C9 C10 1.390(11) . ?
C11 C12 1.434(10) . ?
C13 C14 1.502(10) . ?
C14 C15 1.526(10) . ?
C15 C16 1.515(10) . ?
C16 C17 1.488(11) . ?
C17 C18 1.341(12) . ?
C17 C24 1.423(12) . ?
C19 C20 1.385(13) . ?
C19 C24 1.393(12) . ?
C20 C21 1.371(15) . ?
C21 C22 1.371(16) . ?
C22 C23 1.387(14) . ?
C23 C24 1.419(12) . ?
C25 C26 1.505(11) . ?
C26 C27 1.530(12) . ?
C27 C28 1.494(13) . ?
C28 C29 1.509(13) . ?
C29 C30 1.362(13) . ?
C29 C36 1.421(13) . ?
C31 C32 1.384(15) . ?
C31 C36 1.415(13) . ?
C32 C33 1.383(17) . ?
C33 C34 1.370(18) . ?
C34 C35 1.360(16) . ?
C35 C36 1.391(13) . ?
C37 C38 1.503(9) . ?
C38 C39 1.504(10) . ?
C39 C40 1.519(10) . ?
C40 C41 1.499(11) . ?
C41 C42 1.365(12) . ?
C41 C48 1.425(11) . ?
C43 C44 1.389(12) . ?
C43 C48 1.402(11) . ?
C44 C45 1.359(14) . ?
C45 C46 1.399(14) . ?
C46 C47 1.374(12) . ?
C47 C48 1.405(12) . ?
C49 C50 1.412(13) . ?
C50 C51 1.344(14) . ?
C51 C52 1.386(13) . ?
C52 C60 1.412(11) . ?
C52 C53 1.420(13) . ?
C53 C54 1.344(13) . ?
C54 C55 1.423(12) . ?
C55 C59 1.367(11) . ?
C55 C56 1.407(12) . ?
C56 C57 1.378(13) . ?
C57 C58 1.359(11) . ?
C59 C60 1.456(11) . ?
O10 C61 1.391(10) . ?
C61 C62 1.530(10) . ?

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
O5 La1 O4 74.14(17) . 2_566 ?
O5 La1 O6 135.82(16) . 2_566 ?
O4 La1 O6 74.98(17) 2_566 2_566 ?
O5 La1 O3 78.8(2) . . ?
O4 La1 O3 123.91(17) 2_566 . ?
O6 La1 O3 93.3(2) 2_566 . ?
O5 La1 O1 75.77(17) . . ?
O4 La1 O1 75.53(16) 2_566 . ?
O6 La1 O1 124.93(17) 2_566 . ?
O3 La1 O1 141.62(19) . . ?
O5 La1 O2 125.85(17) . . ?
O4 La1 O2 91.49(16) 2_566 . ?
O6 La1 O2 85.56(16) 2_566 . ?
O3 La1 O2 143.05(18) . . ?
O1 La1 O2 50.09(16) . . ?
O5 La1 O4 69.75(16) . . ?
O4 La1 O4 75.11(17) 2_566 . ?
O6 La1 O4 72.31(16) 2_566 . ?
O3 La1 O4 49.46(16) . . ?
O1 La1 O4 139.47(16) . . ?
O2 La1 O4 156.36(15) . . ?
O5 La1 N1 80.77(14) . . ?
O4 La1 N1 140.70(14) 2_566 . ?
O6 La1 N1 140.71(14) 2_566 . ?
O3 La1 N1 78.72(16) . . ?
O1 La1 N1 69.22(14) . . ?
O2 La1 N1 79.15(14) . . ?
O4 La1 N1 123.43(12) . . ?
O5 La1 N2 134.38(14) . . ?
O4 La1 N2 151.47(13) 2_566 . ?
O6 La1 N2 80.39(14) 2_566 . ?
O3 La1 N2 71.12(16) . . ?
O1 La1 N2 108.32(14) . . ?
O2 La1 N2 72.28(14) . . ?
O4 La1 N2 110.87(13) . . ?
N1 La1 N2 60.54(8) . . ?
O5 La1 La1 66.90(12) . 2_566 ?
O4 La1 La1 39.29(11) 2_566 2_566 ?
O6 La1 La1 69.14(11) 2_566 2_566 ?
O3 La1 La1 84.94(13) . 2_566 ?
O1 La1 La1 110.29(12) . 2_566 ?
O2 La1 La1 128.03(12) . 2_566 ?
O4 La1 La1 35.81(10) . 2_566 ?
N1 La1 La1 146.06(8) . 2_566 ?
N2 La1 La1 139.95(8) . 2_566 ?
C13 O1 La1 95.6(5) . . ?
C13 O2 La1 94.3(4) . . ?
C25 O3 La1 97.9(5) . . ?
C25 O4 La1 159.2(5) . 2_566 ?
C25 O4 La1 92.4(5) . . ?
La1 O4 La1 104.89(17) 2_566 . ?
C37 O5 La1 142.0(5) . . ?
C37 O6 La1 136.1(5) . 2_566 ?
C1 N1 C12 117.8(6) . . ?
C1 N1 La1 120.5(4) . . ?
C12 N1 La1 121.4(4) . . ?
C10 N2 C11 118.1(5) . . ?
C10 N2 La1 120.9(4) . . ?
C11 N2 La1 120.9(4) . . ?
C19 N3 C18 108.1(6) . . ?
C30 N4 C31 111.4(10) . . ?
C42 N5 C43 108.5(8) . . ?
C49 N6 C60 116.0(8) . . ?
C58 N7 C59 120.7(7) . . ?
O9 N8 O8 119.2(11) . . ?
O9 N8 O7 121.2(11) . . ?
O8 N8 O7 119.6(12) . . ?
N1 C1 C2 123.8(9) . . ?
C3 C2 C1 119.1(9) . . ?
C2 C3 C4 119.7(8) . . ?
C3 C4 C12 117.7(8) . . ?
C3 C4 C5 124.1(8) . . ?
C12 C4 C5 118.2(9) . . ?
C6 C5 C4 122.3(8) . . ?
C5 C6 C7 121.0(8) . . ?
C8 C7 C11 117.1(7) . . ?
C8 C7 C6 123.5(8) . . ?
C11 C7 C6 119.3(8) . . ?
C9 C8 C7 120.1(8) . . ?
C8 C9 C10 120.1(9) . . ?
N2 C10 C9 122.2(8) . . ?
N2 C11 C7 122.3(7) . . ?
N2 C11 C12 118.2(6) . . ?
C7 C11 C12 119.5(7) . . ?
N1 C12 C4 121.8(7) . . ?
N1 C12 C11 118.5(6) . . ?
C4 C12 C11 119.6(7) . . ?
O1 C13 O2 120.0(7) . . ?
O1 C13 C14 120.7(7) . . ?
O2 C13 C14 119.4(7) . . ?
C13 C14 C15 115.2(7) . . ?
C16 C15 C14 112.5(7) . . ?
C17 C16 C15 115.7(7) . . ?
C18 C17 C24 105.6(8) . . ?
C18 C17 C16 127.4(9) . . ?
C24 C17 C16 127.0(9) . . ?
C17 C18 N3 110.9(8) . . ?
N3 C19 C20 129.3(10) . . ?
N3 C19 C24 106.2(8) . . ?
C20 C19 C24 124.4(10) . . ?
C21 C20 C19 117.2(11) . . ?
C22 C21 C20 120.6(12) . . ?
C21 C22 C23 122.7(12) . . ?
C22 C23 C24 118.3(10) . . ?
C19 C24 C23 116.8(9) . . ?
C19 C24 C17 109.2(9) . . ?
C23 C24 C17 134.0(9) . . ?
O3 C25 O4 120.0(7) . . ?
O3 C25 C26 120.4(7) . . ?
O4 C25 C26 119.5(7) . . ?
C25 C26 C27 112.5(8) . . ?
C28 C27 C26 114.5(8) . . ?
C27 C28 C29 113.1(8) . . ?
C30 C29 C36 107.1(10) . . ?
C30 C29 C28 124.1(11) . . ?
C36 C29 C28 128.8(9) . . ?
N4 C30 C29 108.6(11) . . ?
N4 C31 C32 132.2(12) . . ?
N4 C31 C36 105.5(10) . . ?
C32 C31 C36 122.3(11) . . ?
C33 C32 C31 116.1(13) . . ?
C34 C33 C32 122.7(15) . . ?
C35 C34 C33 121.1(15) . . ?
C34 C35 C36 119.3(12) . . ?
C35 C36 C31 118.6(11) . . ?
C35 C36 C29 133.9(10) . . ?
C31 C36 C29 107.5(9) . . ?
O5 C37 O6 124.7(7) . . ?
O5 C37 C38 116.2(6) . . ?
O6 C37 C38 119.1(6) . . ?
C37 C38 C39 116.6(6) . . ?
C38 C39 C40 111.2(6) . . ?
C41 C40 C39 114.6(7) . . ?
C42 C41 C48 106.2(8) . . ?
C42 C41 C40 125.4(9) . . ?
C48 C41 C40 128.4(8) . . ?
N5 C42 C41 110.5(9) . . ?
N5 C43 C44 129.8(9) . . ?
N5 C43 C48 107.7(8) . . ?
C44 C43 C48 122.5(10) . . ?
C45 C44 C43 117.4(10) . . ?
C44 C45 C46 121.4(10) . . ?
C47 C46 C45 121.7(10) . . ?
C46 C47 C48 117.9(9) . . ?
C43 C48 C47 119.0(9) . . ?
C43 C48 C41 107.2(8) . . ?
C47 C48 C41 133.8(8) . . ?
N6 C49 C50 123.2(9) . . ?
C51 C50 C49 119.3(10) . . ?
C50 C51 C52 120.0(10) . . ?
C51 C52 C60 116.5(9) . . ?
C51 C52 C53 124.8(10) . . ?
C60 C52 C53 118.7(9) . . ?
C54 C53 C52 123.7(9) . . ?
C53 C54 C55 118.8(9) . . ?
C59 C55 C56 118.9(9) . . ?
C59 C55 C54 120.0(9) . . ?
C56 C55 C54 121.1(9) . . ?
C57 C56 C55 119.3(9) . . ?
C58 C57 C56 118.8(9) . . ?
N7 C58 C57 122.2(9) . . ?
N7 C59 C55 120.1(8) . . ?
N7 C59 C60 118.1(7) . . ?
C55 C59 C60 121.8(8) . . ?
N6 C60 C52 124.9(8) . . ?
N6 C60 C59 118.1(7) . . ?
C52 C60 C59 117.0(8) . . ?
O10 C61 C62 107.0(8) . . ?

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
N3 H3A O9 0.86 2.19 3.027 164.3 1_545
N4 H4A N3 0.86 2.42 3.241(9) 159.3 2_656
N5 H5A O1W 0.86 2.02 2.824(10) 155.9 1_446
N7 H7A O2 0.86 1.94 2.704(8) 146.6 .
O1W H1A O1 0.822(10) 2.02(3) 2.815(8) 162(9) 2_665
O1W H1B O7 0.822(10) 2.30(7) 2.990(14) 141(11) .
O10 H10B O8 0.82 2.27 3.03(3) 154.4 2_765

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.224
_refine_diff_density_min         -1.396
_refine_diff_density_rms         0.127
####################################################################### 
# 
# 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_k
_database_code_depnum_ccdc_archive 'CCDC 1044884'
_audit_update_record             
;
2015-11-09 deposited with the CCDC.
2015-11-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C120 H114 N16 O22 Pr2'
_chemical_formula_weight         2414.09

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   13.642(3)
_cell_length_b                   14.294(3)
_cell_length_c                   16.721(3)
_cell_angle_alpha                79.49(3)
_cell_angle_beta                 71.27(3)
_cell_angle_gamma                64.01(3)
_cell_volume                     2772.3(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    12540
_cell_measurement_theta_min      3.00
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1240
_exptl_absorpt_coefficient_mu    0.948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7772
_exptl_absorpt_correction_T_max  0.8631
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            27020
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_sigmaI/netI    0.0684
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.00
_diffrn_reflns_theta_max         27.48
_reflns_number_total             12540
_reflns_number_gt                10574
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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)+(0.0719P)²+4.5992P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12540
_refine_ls_number_parameters     721
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0534
_refine_ls_wR_factor_ref         0.1458
_refine_ls_wR_factor_gt          0.1363
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O2W O 0.1930(3) 0.7194(3) 0.2891(2) 0.0500(9) Uani 1 1 d . . .
H2WA H 0.2146 0.7197 0.2354 0.075 Uiso 1 1 d R . .
H2WC H 0.1878 0.7749 0.3052 0.075 Uiso 1 1 d R . .
O1W O 0.9784(11) 0.0706(15) -0.0013(10) 0.337(14) Uani 1 1 d . . .
H1WA H 0.9174 0.0994 -0.0165 0.505 Uiso 1 1 d R . .
H1WC H 1.0159 0.0095 -0.0194 0.505 Uiso 1 1 d R . .
Pr1 Pr 0.846390(18) 0.002740(17) 0.562460(14) 0.02461(8) Uani 1 1 d . . .
O1 O 0.7776(3) -0.0542(3) 0.7168(2) 0.0416(8) Uani 1 1 d . . .
O2 O 0.7670(3) 0.1057(3) 0.6947(2) 0.0389(8) Uani 1 1 d . . .
O3 O 0.8207(3) 0.0126(4) 0.4180(2) 0.0567(11) Uani 1 1 d . . .
O4 O 0.9908(3) -0.0077(3) 0.41242(19) 0.0342(7) Uani 1 1 d . . .
O5 O 0.8408(3) 0.1718(3) 0.5116(2) 0.0383(7) Uani 1 1 d . . .
O7 O 0.2057(6) 0.7819(5) 0.0926(5) 0.113(2) Uani 1 1 d . . .
O8 O 0.2990(7) 0.6197(6) 0.1225(6) 0.130(3) Uani 1 1 d . . .
O9 O 0.2426(8) 0.6642(7) 0.0100(4) 0.133(3) Uani 1 1 d . . .
N1 N 0.6247(3) 0.1101(3) 0.5910(3) 0.0366(8) Uani 1 1 d . . .
N2 N 0.7176(3) -0.0981(3) 0.5687(2) 0.0350(8) Uani 1 1 d . . .
N3 N 0.3395(5) 0.4314(4) 1.0118(3) 0.0604(13) Uani 1 1 d . . .
H3A H 0.3203 0.4964 1.0167 0.072 Uiso 1 1 calc R . .
N4 N 0.7000(6) 0.4563(6) 0.1659(4) 0.0771(18) Uani 1 1 d . . .
H4A H 0.6896 0.4992 0.1231 0.093 Uiso 1 1 calc R . .
N5 N 1.0040(5) 0.6723(4) 0.3214(3) 0.0572(12) Uani 1 1 d . . .
H5 H 1.0455 0.7046 0.3185 0.069 Uiso 1 1 calc R . .
N6 N 0.4939(4) 0.0462(4) 0.1874(3) 0.0504(11) Uani 1 1 d . . .
N7 N 0.2913(4) 0.2124(3) 0.2334(3) 0.0414(9) Uani 1 1 d . . .
H7 H 0.2954 0.1505 0.2341 0.050 Uiso 1 1 calc R . .
N8 N 0.2511(6) 0.6881(6) 0.0740(5) 0.0746(17) Uani 1 1 d . . .
C1 C 0.5767(5) 0.2111(4) 0.6031(4) 0.0485(13) Uani 1 1 d . . .
H1A H 0.6241 0.2444 0.5971 0.058 Uiso 1 1 calc R . .
C2 C 0.4607(5) 0.2710(5) 0.6241(4) 0.0607(16) Uani 1 1 d . . .
H2A H 0.4318 0.3420 0.6317 0.073 Uiso 1 1 calc R . .
C3 C 0.3902(5) 0.2234(5) 0.6333(4) 0.0625(17) Uani 1 1 d . . .
H3B H 0.3122 0.2619 0.6477 0.075 Uiso 1 1 calc R . .
C4 C 0.4348(4) 0.1167(5) 0.6211(3) 0.0474(13) Uani 1 1 d . . .
C5 C 0.3643(4) 0.0643(6) 0.6301(4) 0.0574(16) Uani 1 1 d . . .
H5B H 0.2860 0.1010 0.6442 0.069 Uiso 1 1 calc R . .
C6 C 0.4114(5) -0.0400(6) 0.6179(4) 0.0557(16) Uani 1 1 d . . .
H6C H 0.3645 -0.0733 0.6223 0.067 Uiso 1 1 calc R . .
C7 C 0.5314(5) -0.0992(5) 0.5984(3) 0.0429(12) Uani 1 1 d . . .
C8 C 0.5839(5) -0.2066(5) 0.5853(4) 0.0517(14) Uani 1 1 d . . .
H8A H 0.5401 -0.2436 0.5915 0.062 Uiso 1 1 calc R . .
C9 C 0.6965(6) -0.2554(5) 0.5641(4) 0.0591(16) Uani 1 1 d . . .
H9A H 0.7317 -0.3264 0.5552 0.071 Uiso 1 1 calc R . .
C10 C 0.7617(5) -0.1986(4) 0.5552(4) 0.0463(12) Uani 1 1 d . . .
H10A H 0.8402 -0.2336 0.5390 0.056 Uiso 1 1 calc R . .
C11 C 0.6033(4) -0.0475(4) 0.5885(3) 0.0318(9) Uani 1 1 d . . .
C12 C 0.5536(4) 0.0621(4) 0.5997(3) 0.0348(10) Uani 1 1 d . . .
C13 C 0.7502(4) 0.0325(4) 0.7451(3) 0.0325(9) Uani 1 1 d . . .
C14 C 0.6974(5) 0.0502(4) 0.8380(3) 0.0463(12) Uani 1 1 d . . .
H14A H 0.7556 0.0429 0.8630 0.056 Uiso 1 1 calc R . .
H14B H 0.6710 -0.0040 0.8639 0.056 Uiso 1 1 calc R . .
C15 C 0.6001(4) 0.1543(4) 0.8594(3) 0.0429(11) Uani 1 1 d . . .
H15A H 0.5419 0.1631 0.8338 0.051 Uiso 1 1 calc R . .
H15B H 0.6263 0.2091 0.8360 0.051 Uiso 1 1 calc R . .
C16 C 0.5490(6) 0.1645(5) 0.9546(3) 0.0635(18) Uani 1 1 d . . .
H16A H 0.5283 0.1064 0.9777 0.076 Uiso 1 1 calc R . .
H16B H 0.6072 0.1585 0.9791 0.076 Uiso 1 1 calc R . .
C17 C 0.4476(5) 0.2630(5) 0.9824(3) 0.0520(14) Uani 1 1 d . . .
C18 C 0.4495(6) 0.3583(5) 0.9834(4) 0.0586(16) Uani 1 1 d . . .
H18A H 0.5143 0.3715 0.9675 0.070 Uiso 1 1 calc R . .
C19 C 0.2659(5) 0.3836(5) 1.0312(3) 0.0525(14) Uani 1 1 d . . .
C20 C 0.1507(6) 0.4236(7) 1.0652(4) 0.075(2) Uani 1 1 d . . .
H20A H 0.1090 0.4937 1.0767 0.090 Uiso 1 1 calc R . .
C21 C 0.0999(7) 0.3556(9) 1.0814(6) 0.094(3) Uani 1 1 d . . .
H21A H 0.0218 0.3803 1.1043 0.113 Uiso 1 1 calc R . .
C22 C 0.1611(8) 0.2512(9) 1.0648(5) 0.090(3) Uani 1 1 d . . .
H22A H 0.1235 0.2073 1.0777 0.108 Uiso 1 1 calc R . .
C23 C 0.2776(7) 0.2106(6) 1.0293(4) 0.0670(18) Uani 1 1 d . . .
H23A H 0.3180 0.1407 1.0170 0.080 Uiso 1 1 calc R . .
C24 C 0.3318(5) 0.2767(5) 1.0127(3) 0.0495(13) Uani 1 1 d . . .
C25 C 0.9164(4) 0.0082(4) 0.3763(3) 0.0391(11) Uani 1 1 d . . .
C26 C 0.9454(5) 0.0193(6) 0.2795(3) 0.0588(16) Uani 1 1 d . . .
H26A H 1.0221 0.0152 0.2568 0.071 Uiso 1 1 calc R . .
H26B H 0.9420 -0.0376 0.2582 0.071 Uiso 1 1 calc R . .
C27 C 0.8629(5) 0.1232(6) 0.2497(4) 0.0613(17) Uani 1 1 d . . .
H27A H 0.8772 0.1235 0.1890 0.074 Uiso 1 1 calc R . .
H27B H 0.7862 0.1286 0.2758 0.074 Uiso 1 1 calc R . .
C28 C 0.8717(7) 0.2162(7) 0.2701(5) 0.076(2) Uani 1 1 d . . .
H28A H 0.9470 0.2130 0.2410 0.091 Uiso 1 1 calc R . .
H28B H 0.8624 0.2134 0.3304 0.091 Uiso 1 1 calc R . .
C29 C 0.7848(6) 0.3192(6) 0.2456(4) 0.0658(18) Uani 1 1 d . . .
C30 C 0.7938(8) 0.3701(8) 0.1673(5) 0.083(2) Uani 1 1 d . . .
H30A H 0.8571 0.3475 0.1212 0.100 Uiso 1 1 calc R . .
C31 C 0.6236(7) 0.4652(6) 0.2431(5) 0.0664(18) Uani 1 1 d . . .
C32 C 0.5103(9) 0.5371(7) 0.2736(7) 0.091(3) Uani 1 1 d . . .
H32A H 0.4769 0.5943 0.2399 0.109 Uiso 1 1 calc R . .
C33 C 0.4518(9) 0.5204(10) 0.3529(8) 0.109(4) Uani 1 1 d . . .
H33A H 0.3763 0.5659 0.3723 0.131 Uiso 1 1 calc R . .
C34 C 0.4984(10) 0.4405(10) 0.4053(6) 0.102(3) Uani 1 1 d . . .
H34A H 0.4558 0.4341 0.4604 0.122 Uiso 1 1 calc R . .
C35 C 0.6110(9) 0.3669(8) 0.3771(5) 0.083(3) Uani 1 1 d . . .
H35A H 0.6429 0.3115 0.4128 0.100 Uiso 1 1 calc R . .
C36 C 0.6734(6) 0.3788(5) 0.2952(4) 0.0580(16) Uani 1 1 d . . .
C37 C 0.9049(4) 0.2190(3) 0.4815(3) 0.0320(9) Uani 1 1 d . . .
C38 C 0.8463(4) 0.3369(4) 0.4833(3) 0.0397(11) Uani 1 1 d . . .
H38A H 0.7716 0.3588 0.4758 0.048 Uiso 1 1 calc R . .
H38B H 0.8359 0.3568 0.5389 0.048 Uiso 1 1 calc R . .
C39 C 0.9070(4) 0.3959(3) 0.4177(3) 0.0396(11) Uani 1 1 d . . .
H39A H 0.9087 0.3849 0.3617 0.048 Uiso 1 1 calc R . .
H39B H 0.9846 0.3702 0.4205 0.048 Uiso 1 1 calc R . .
C40 C 0.8459(5) 0.5120(4) 0.4340(4) 0.0512(14) Uani 1 1 d . . .
H40A H 0.7690 0.5368 0.4300 0.061 Uiso 1 1 calc R . .
H40B H 0.8414 0.5214 0.4912 0.061 Uiso 1 1 calc R . .
C41 C 0.9014(4) 0.5776(4) 0.3742(4) 0.0436(12) Uani 1 1 d . . .
C42 C 0.9672(5) 0.6161(5) 0.3907(4) 0.0548(14) Uani 1 1 d . . .
H42A H 0.9849 0.6059 0.4417 0.066 Uiso 1 1 calc R . .
C43 C 0.9633(5) 0.6686(4) 0.2576(4) 0.0481(13) Uani 1 1 d . . .
C44 C 0.9778(6) 0.7136(5) 0.1757(4) 0.0661(18) Uani 1 1 d . . .
H44A H 1.0208 0.7529 0.1559 0.079 Uiso 1 1 calc R . .
C45 C 0.9251(7) 0.6965(6) 0.1260(5) 0.078(2) Uani 1 1 d . . .
H45A H 0.9323 0.7260 0.0712 0.094 Uiso 1 1 calc R . .
C46 C 0.8619(6) 0.6376(6) 0.1534(5) 0.0723(19) Uani 1 1 d . . .
H46A H 0.8278 0.6283 0.1172 0.087 Uiso 1 1 calc R . .
C47 C 0.8488(5) 0.5919(5) 0.2351(4) 0.0569(15) Uani 1 1 d . . .
H47A H 0.8073 0.5512 0.2535 0.068 Uiso 1 1 calc R . .
C48 C 0.8992(4) 0.6084(4) 0.2886(4) 0.0437(12) Uani 1 1 d . . .
C49 C 0.5945(6) -0.0333(6) 0.1650(4) 0.0645(17) Uani 1 1 d . . .
H49A H 0.5966 -0.0997 0.1674 0.077 Uiso 1 1 calc R . .
C50 C 0.6983(6) -0.0220(7) 0.1376(5) 0.075(2) Uani 1 1 d . . .
H50A H 0.7668 -0.0793 0.1216 0.091 Uiso 1 1 calc R . .
C51 C 0.6958(6) 0.0740(7) 0.1352(4) 0.0674(18) Uani 1 1 d . . .
H51A H 0.7631 0.0831 0.1168 0.081 Uiso 1 1 calc R . .
C52 C 0.5939(5) 0.1587(6) 0.1601(4) 0.0543(14) Uani 1 1 d . . .
C53 C 0.5866(6) 0.2620(7) 0.1579(4) 0.0664(19) Uani 1 1 d . . .
H53A H 0.6526 0.2733 0.1414 0.080 Uiso 1 1 calc R . .
C54 C 0.4863(7) 0.3421(6) 0.1794(5) 0.0686(19) Uani 1 1 d . . .
H54A H 0.4837 0.4086 0.1771 0.082 Uiso 1 1 calc R . .
C55 C 0.3820(6) 0.3287(5) 0.2058(3) 0.0507(13) Uani 1 1 d . . .
C56 C 0.2756(6) 0.4098(5) 0.2310(4) 0.0622(17) Uani 1 1 d . . .
H56A H 0.2699 0.4771 0.2306 0.075 Uiso 1 1 calc R . .
C57 C 0.1789(6) 0.3916(5) 0.2565(4) 0.0616(17) Uani 1 1 d . . .
H57A H 0.1078 0.4459 0.2728 0.074 Uiso 1 1 calc R . .
C58 C 0.1900(5) 0.2900(5) 0.2574(4) 0.0553(15) Uani 1 1 d . . .
H58A H 0.1255 0.2762 0.2752 0.066 Uiso 1 1 calc R . .
C59 C 0.3886(5) 0.2276(4) 0.2077(3) 0.0400(11) Uani 1 1 d . . .
C60 C 0.4944(5) 0.1409(4) 0.1836(3) 0.0426(11) Uani 1 1 d . . .
O6 O 1.0108(3) 0.1767(2) 0.4517(2) 0.0376(7) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O2W H2WA 0.8500 . ?
O2W H2WC 0.8500 . ?
O1W O1W 1.83(4) 2_755 ?
O1W H1WA 0.8499 . ?
O1W H1WC 0.8500 . ?
Pr1 O5 2.388(3) . ?
Pr1 O4 2.422(3) 2_756 ?
Pr1 O6 2.445(3) 2_756 ?
Pr1 O3 2.521(4) . ?
Pr1 O2 2.546(3) . ?
Pr1 O1 2.559(3) . ?
Pr1 O4 2.627(3) . ?
Pr1 N1 2.646(4) . ?
Pr1 N2 2.687(4) . ?
Pr1 Pr1 4.0106(14) 2_756 ?
O1 C13 1.262(6) . ?
O2 C13 1.274(6) . ?
O3 C25 1.247(6) . ?
O4 C25 1.259(6) . ?
O4 Pr1 2.422(3) 2_756 ?
O5 C37 1.258(5) . ?
O7 N8 1.257(9) . ?
O8 N8 1.238(10) . ?
O9 N8 1.234(9) . ?
N1 C1 1.322(7) . ?
N1 C12 1.375(6) . ?
N2 C10 1.323(6) . ?
N2 C11 1.354(6) . ?
N3 C19 1.376(8) . ?
N3 C18 1.385(8) . ?
N3 H3A 0.8600 . ?
N4 C30 1.335(11) . ?
N4 C31 1.360(10) . ?
N4 H4A 0.8600 . ?
N5 C43 1.369(8) . ?
N5 C42 1.371(8) . ?
N5 H5 0.8600 . ?
N6 C49 1.333(8) . ?
N6 C60 1.346(7) . ?
N7 C58 1.328(7) . ?
N7 C59 1.359(7) . ?
N7 H7 0.8600 . ?
C1 C2 1.388(7) . ?
C1 H1A 0.9300 . ?
C2 C3 1.361(10) . ?
C2 H2A 0.9300 . ?
C3 C4 1.399(9) . ?
C3 H3B 0.9300 . ?
C4 C12 1.409(6) . ?
C4 C5 1.415(8) . ?
C5 C6 1.366(10) . ?
C5 H5B 0.9300 . ?
C6 C7 1.431(8) . ?
C6 H6C 0.9300 . ?
C7 C8 1.406(8) . ?
C7 C11 1.420(6) . ?
C8 C9 1.331(9) . ?
C8 H8A 0.9300 . ?
C9 C10 1.406(7) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
C11 C12 1.430(7) . ?
C13 C14 1.504(6) . ?
C14 C15 1.504(7) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.524(7) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.493(8) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.378(9) . ?
C17 C24 1.429(8) . ?
C18 H18A 0.9300 . ?
C19 C20 1.370(9) . ?
C19 C24 1.424(9) . ?
C20 C21 1.368(13) . ?
C20 H20A 0.9300 . ?
C21 C22 1.382(14) . ?
C21 H21A 0.9300 . ?
C22 C23 1.387(12) . ?
C22 H22A 0.9300 . ?
C23 C24 1.378(9) . ?
C23 H23A 0.9300 . ?
C25 C26 1.533(7) . ?
C26 C27 1.531(9) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.492(10) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C29 1.518(11) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.373(10) . ?
C29 C36 1.427(10) . ?
C30 H30A 0.9300 . ?
C31 C36 1.413(10) . ?
C31 C32 1.413(12) . ?
C32 C33 1.350(14) . ?
C32 H32A 0.9300 . ?
C33 C34 1.354(15) . ?
C33 H33A 0.9300 . ?
C34 C35 1.411(14) . ?
C34 H34A 0.9300 . ?
C35 C36 1.386(9) . ?
C35 H35A 0.9300 . ?
C37 O6 1.258(5) . ?
C37 C38 1.517(6) . ?
C38 C39 1.514(6) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 C40 1.527(7) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 C41 1.499(7) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 C42 1.352(8) . ?
C41 C48 1.425(8) . ?
C42 H42A 0.9300 . ?
C43 C44 1.395(9) . ?
C43 C48 1.407(7) . ?
C44 C45 1.370(12) . ?
C44 H44A 0.9300 . ?
C45 C46 1.381(11) . ?
C45 H45A 0.9300 . ?
C46 C47 1.395(10) . ?
C46 H46A 0.9300 . ?
C47 C48 1.394(8) . ?
C47 H47A 0.9300 . ?
C49 C50 1.413(10) . ?
C49 H49A 0.9300 . ?
C50 C51 1.350(11) . ?
C50 H50A 0.9300 . ?
C51 C52 1.382(10) . ?
C51 H51A 0.9300 . ?
C52 C60 1.409(8) . ?
C52 C53 1.430(10) . ?
C53 C54 1.333(11) . ?
C53 H53A 0.9300 . ?
C54 C55 1.435(9) . ?
C54 H54A 0.9300 . ?
C55 C56 1.393(9) . ?
C55 C59 1.402(7) . ?
C56 C57 1.373(10) . ?
C56 H56A 0.9300 . ?
C57 C58 1.390(8) . ?
C57 H57A 0.9300 . ?
C58 H58A 0.9300 . ?
C59 C60 1.422(8) . ?
O6 Pr1 2.445(3) 2_756 ?

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
H2WA O2W H2WC 109.5 . . ?
O1W O1W H1WA 106.9 2_755 . ?
O1W O1W H1WC 23.6 2_755 . ?
H1WA O1W H1WC 109.5 . . ?
O5 Pr1 O4 74.44(12) . 2_756 ?
O5 Pr1 O6 136.43(11) . 2_756 ?
O4 Pr1 O6 75.25(11) 2_756 2_756 ?
O5 Pr1 O3 79.33(14) . . ?
O4 Pr1 O3 124.38(11) 2_756 . ?
O6 Pr1 O3 92.96(14) 2_756 . ?
O5 Pr1 O2 75.21(11) . . ?
O4 Pr1 O2 74.99(11) 2_756 . ?
O6 Pr1 O2 124.99(12) 2_756 . ?
O3 Pr1 O2 141.86(14) . . ?
O5 Pr1 O1 126.09(12) . . ?
O4 Pr1 O1 91.79(11) 2_756 . ?
O6 Pr1 O1 85.23(12) 2_756 . ?
O3 Pr1 O1 142.11(12) . . ?
O2 Pr1 O1 50.93(11) . . ?
O5 Pr1 O4 69.90(11) . . ?
O4 Pr1 O4 74.88(11) 2_756 . ?
O6 Pr1 O4 72.47(11) 2_756 . ?
O3 Pr1 O4 50.07(10) . . ?
O2 Pr1 O4 138.66(10) . . ?
O1 Pr1 O4 156.21(11) . . ?
O5 Pr1 N1 80.30(12) . . ?
O4 Pr1 N1 140.64(12) 2_756 . ?
O6 Pr1 N1 140.52(12) 2_756 . ?
O3 Pr1 N1 78.51(13) . . ?
O2 Pr1 N1 69.63(13) . . ?
O1 Pr1 N1 79.20(13) . . ?
O4 Pr1 N1 123.50(12) . . ?
O5 Pr1 N2 134.58(12) . . ?
O4 Pr1 N2 150.97(12) 2_756 . ?
O6 Pr1 N2 79.44(12) 2_756 . ?
O3 Pr1 N2 70.49(13) . . ?
O2 Pr1 N2 109.42(11) . . ?
O1 Pr1 N2 71.99(12) . . ?
O4 Pr1 N2 110.73(11) . . ?
N1 Pr1 N2 61.30(12) . . ?
O5 Pr1 Pr1 67.22(8) . 2_756 ?
O4 Pr1 Pr1 39.22(7) 2_756 2_756 ?
O6 Pr1 Pr1 69.45(8) 2_756 2_756 ?
O3 Pr1 Pr1 85.44(8) . 2_756 ?
O2 Pr1 Pr1 109.59(8) . 2_756 ?
O1 Pr1 Pr1 128.19(9) . 2_756 ?
O4 Pr1 Pr1 35.65(7) . 2_756 ?
N1 Pr1 Pr1 145.94(9) . 2_756 ?
N2 Pr1 Pr1 139.44(8) . 2_756 ?
C13 O1 Pr1 94.4(3) . . ?
C13 O2 Pr1 94.7(3) . . ?
C25 O3 Pr1 97.0(3) . . ?
C25 O4 Pr1 159.6(3) . 2_756 ?
C25 O4 Pr1 91.6(3) . . ?
Pr1 O4 Pr1 105.12(11) 2_756 . ?
C37 O5 Pr1 141.2(3) . . ?
C1 N1 C12 116.9(4) . . ?
C1 N1 Pr1 121.4(3) . . ?
C12 N1 Pr1 121.5(3) . . ?
C10 N2 C11 117.2(4) . . ?
C10 N2 Pr1 122.2(3) . . ?
C11 N2 Pr1 120.6(3) . . ?
C19 N3 C18 109.3(6) . . ?
C19 N3 H3A 125.4 . . ?
C18 N3 H3A 125.4 . . ?
C30 N4 C31 109.1(6) . . ?
C30 N4 H4A 125.5 . . ?
C31 N4 H4A 125.5 . . ?
C43 N5 C42 108.5(5) . . ?
C43 N5 H5 125.7 . . ?
C42 N5 H5 125.7 . . ?
C49 N6 C60 116.6(5) . . ?
C58 N7 C59 122.1(5) . . ?
C58 N7 H7 118.9 . . ?
C59 N7 H7 118.9 . . ?
O9 N8 O8 120.4(9) . . ?
O9 N8 O7 120.0(9) . . ?
O8 N8 O7 119.6(9) . . ?
N1 C1 C2 124.7(6) . . ?
N1 C1 H1A 117.6 . . ?
C2 C1 H1A 117.6 . . ?
C3 C2 C1 118.4(6) . . ?
C3 C2 H2A 120.8 . . ?
C1 C2 H2A 120.8 . . ?
C2 C3 C4 120.3(5) . . ?
C2 C3 H3B 119.9 . . ?
C4 C3 H3B 119.9 . . ?
C3 C4 C12 117.5(5) . . ?
C3 C4 C5 122.0(5) . . ?
C12 C4 C5 120.6(6) . . ?
C6 C5 C4 120.0(5) . . ?
C6 C5 H5B 120.0 . . ?
C4 C5 H5B 120.0 . . ?
C5 C6 C7 121.3(5) . . ?
C5 C6 H6C 119.3 . . ?
C7 C6 H6C 119.3 . . ?
C8 C7 C11 117.2(5) . . ?
C8 C7 C6 123.5(5) . . ?
C11 C7 C6 119.3(5) . . ?
C9 C8 C7 119.9(5) . . ?
C9 C8 H8A 120.1 . . ?
C7 C8 H8A 120.1 . . ?
C8 C9 C10 119.4(6) . . ?
C8 C9 H9A 120.3 . . ?
C10 C9 H9A 120.3 . . ?
N2 C10 C9 123.7(5) . . ?
N2 C10 H10A 118.2 . . ?
C9 C10 H10A 118.2 . . ?
N2 C11 C7 122.6(5) . . ?
N2 C11 C12 118.3(4) . . ?
C7 C11 C12 119.1(4) . . ?
N1 C12 C4 122.2(5) . . ?
N1 C12 C11 118.0(4) . . ?
C4 C12 C11 119.7(4) . . ?
O1 C13 O2 119.9(4) . . ?
O1 C13 C14 120.5(4) . . ?
O2 C13 C14 119.6(4) . . ?
C13 C14 C15 115.3(4) . . ?
C13 C14 H14A 108.5 . . ?
C15 C14 H14A 108.5 . . ?
C13 C14 H14B 108.5 . . ?
C15 C14 H14B 108.5 . . ?
H14A C14 H14B 107.5 . . ?
C14 C15 C16 112.0(4) . . ?
C14 C15 H15A 109.2 . . ?
C16 C15 H15A 109.2 . . ?
C14 C15 H15B 109.2 . . ?
C16 C15 H15B 109.2 . . ?
H15A C15 H15B 107.9 . . ?
C17 C16 C15 116.1(5) . . ?
C17 C16 H16A 108.3 . . ?
C15 C16 H16A 108.3 . . ?
C17 C16 H16B 108.3 . . ?
C15 C16 H16B 108.3 . . ?
H16A C16 H16B 107.4 . . ?
C18 C17 C24 107.3(5) . . ?
C18 C17 C16 125.5(6) . . ?
C24 C17 C16 127.2(6) . . ?
C17 C18 N3 109.2(6) . . ?
C17 C18 H18A 125.4 . . ?
N3 C18 H18A 125.4 . . ?
C20 C19 N3 129.8(7) . . ?
C20 C19 C24 122.7(7) . . ?
N3 C19 C24 107.4(5) . . ?
C21 C20 C19 116.8(8) . . ?
C21 C20 H20A 121.6 . . ?
C19 C20 H20A 121.6 . . ?
C20 C21 C22 122.1(8) . . ?
C20 C21 H21A 119.0 . . ?
C22 C21 H21A 119.0 . . ?
C21 C22 C23 121.3(8) . . ?
C21 C22 H22A 119.4 . . ?
C23 C22 H22A 119.4 . . ?
C24 C23 C22 118.3(8) . . ?
C24 C23 H23A 120.9 . . ?
C22 C23 H23A 120.9 . . ?
C23 C24 C19 118.8(6) . . ?
C23 C24 C17 134.3(6) . . ?
C19 C24 C17 106.9(5) . . ?
O3 C25 O4 120.9(4) . . ?
O3 C25 C26 119.7(4) . . ?
O4 C25 C26 119.4(4) . . ?
C27 C26 C25 111.1(5) . . ?
C27 C26 H26A 109.4 . . ?
C25 C26 H26A 109.4 . . ?
C27 C26 H26B 109.4 . . ?
C25 C26 H26B 109.4 . . ?
H26A C26 H26B 108.0 . . ?
C28 C27 C26 113.8(5) . . ?
C28 C27 H27A 108.8 . . ?
C26 C27 H27A 108.8 . . ?
C28 C27 H27B 108.8 . . ?
C26 C27 H27B 108.8 . . ?
H27A C27 H27B 107.7 . . ?
C27 C28 C29 113.7(6) . . ?
C27 C28 H28A 108.8 . . ?
C29 C28 H28A 108.8 . . ?
C27 C28 H28B 108.8 . . ?
C29 C28 H28B 108.8 . . ?
H28A C28 H28B 107.7 . . ?
C30 C29 C36 105.2(7) . . ?
C30 C29 C28 126.5(8) . . ?
C36 C29 C28 128.0(6) . . ?
N4 C30 C29 111.4(7) . . ?
N4 C30 H30A 124.3 . . ?
C29 C30 H30A 124.3 . . ?
N4 C31 C36 107.6(7) . . ?
N4 C31 C32 132.0(8) . . ?
C36 C31 C32 120.2(8) . . ?
C33 C32 C31 118.3(10) . . ?
C33 C32 H32A 120.9 . . ?
C31 C32 H32A 120.9 . . ?
C32 C33 C34 122.9(11) . . ?
C32 C33 H33A 118.6 . . ?
C34 C33 H33A 118.6 . . ?
C33 C34 C35 120.4(9) . . ?
C33 C34 H34A 119.8 . . ?
C35 C34 H34A 119.8 . . ?
C36 C35 C34 118.8(9) . . ?
C36 C35 H35A 120.6 . . ?
C34 C35 H35A 120.6 . . ?
C35 C36 C31 119.3(8) . . ?
C35 C36 C29 134.0(7) . . ?
C31 C36 C29 106.7(6) . . ?
O6 C37 O5 125.6(4) . . ?
O6 C37 C38 119.0(4) . . ?
O5 C37 C38 115.4(4) . . ?
C39 C38 C37 115.8(4) . . ?
C39 C38 H38A 108.3 . . ?
C37 C38 H38A 108.3 . . ?
C39 C38 H38B 108.3 . . ?
C37 C38 H38B 108.3 . . ?
H38A C38 H38B 107.4 . . ?
C38 C39 C40 109.8(4) . . ?
C38 C39 H39A 109.7 . . ?
C40 C39 H39A 109.7 . . ?
C38 C39 H39B 109.7 . . ?
C40 C39 H39B 109.7 . . ?
H39A C39 H39B 108.2 . . ?
C41 C40 C39 114.3(4) . . ?
C41 C40 H40A 108.7 . . ?
C39 C40 H40A 108.7 . . ?
C41 C40 H40B 108.7 . . ?
C39 C40 H40B 108.7 . . ?
H40A C40 H40B 107.6 . . ?
C42 C41 C48 106.6(5) . . ?
C42 C41 C40 126.2(6) . . ?
C48 C41 C40 127.1(5) . . ?
C41 C42 N5 110.4(6) . . ?
C41 C42 H42A 124.8 . . ?
N5 C42 H42A 124.8 . . ?
N5 C43 C44 129.7(6) . . ?
N5 C43 C48 107.4(5) . . ?
C44 C43 C48 122.9(6) . . ?
C45 C44 C43 116.1(7) . . ?
C45 C44 H44A 121.9 . . ?
C43 C44 H44A 121.9 . . ?
C44 C45 C46 123.2(7) . . ?
C44 C45 H45A 118.4 . . ?
C46 C45 H45A 118.4 . . ?
C45 C46 C47 120.4(7) . . ?
C45 C46 H46A 119.8 . . ?
C47 C46 H46A 119.8 . . ?
C48 C47 C46 118.6(6) . . ?
C48 C47 H47A 120.7 . . ?
C46 C47 H47A 120.7 . . ?
C47 C48 C43 118.8(5) . . ?
C47 C48 C41 134.1(5) . . ?
C43 C48 C41 107.0(5) . . ?
N6 C49 C50 123.3(7) . . ?
N6 C49 H49A 118.3 . . ?
C50 C49 H49A 118.3 . . ?
C51 C50 C49 118.5(7) . . ?
C51 C50 H50A 120.7 . . ?
C49 C50 H50A 120.7 . . ?
C50 C51 C52 120.5(6) . . ?
C50 C51 H51A 119.8 . . ?
C52 C51 H51A 119.8 . . ?
C51 C52 C60 117.2(6) . . ?
C51 C52 C53 122.6(6) . . ?
C60 C52 C53 120.1(6) . . ?
C54 C53 C52 120.7(6) . . ?
C54 C53 H53A 119.7 . . ?
C52 C53 H53A 119.7 . . ?
C53 C54 C55 121.8(6) . . ?
C53 C54 H54A 119.1 . . ?
C55 C54 H54A 119.1 . . ?
C56 C55 C59 118.6(6) . . ?
C56 C55 C54 123.7(6) . . ?
C59 C55 C54 117.8(6) . . ?
C57 C56 C55 120.9(5) . . ?
C57 C56 H56A 119.6 . . ?
C55 C56 H56A 119.6 . . ?
C56 C57 C58 118.3(6) . . ?
C56 C57 H57A 120.8 . . ?
C58 C57 H57A 120.8 . . ?
N7 C58 C57 121.1(6) . . ?
N7 C58 H58A 119.5 . . ?
C57 C58 H58A 119.5 . . ?
N7 C59 C55 119.0(5) . . ?
N7 C59 C60 119.3(5) . . ?
C55 C59 C60 121.7(5) . . ?
N6 C60 C52 123.8(5) . . ?
N6 C60 C59 118.2(5) . . ?
C52 C60 C59 117.9(5) . . ?
C37 O6 Pr1 135.2(3) . 2_756 ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         1.232
_refine_diff_density_min         -2.995
_refine_diff_density_rms         0.124
####################################################################### 
# 
# 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_x
_database_code_depnum_ccdc_archive 'CCDC 1044885'
_audit_update_record             
;
2015-11-09 deposited with the CCDC.
2015-11-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C120 H114 Eu2 N16 O22'
_chemical_formula_weight         2436.19

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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   13.549(4)
_cell_length_b                   14.302(4)
_cell_length_c                   16.740(5)
_cell_angle_alpha                79.802(4)
_cell_angle_beta                 71.163(4)
_cell_angle_gamma                64.190(4)
_cell_volume                     2761.3(13)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    11015
_cell_measurement_theta_min      1.85
_cell_measurement_theta_max      26.37

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1248
_exptl_absorpt_coefficient_mu    1.205
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6990
_exptl_absorpt_correction_T_max  0.8399
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker AXS SMART APEX II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            15532
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_sigmaI/netI    0.0996
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.85
_diffrn_reflns_theta_max         26.37
_reflns_number_total             11015
_reflns_number_gt                7949
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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)+(0.0486P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11015
_refine_ls_number_parameters     731
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0562
_refine_ls_wR_factor_ref         0.1232
_refine_ls_wR_factor_gt          0.1080
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_restrained_S_all      0.997
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O2W O -0.0245(8) 0.5746(12) -0.0006(9) 0.379(14) Uani 1 1 d . . .
H2WB H -0.0360 0.6289 -0.0330 0.569 Uiso 1 1 d R . .
H2WC H 0.0066 0.5212 -0.0301 0.569 Uiso 1 1 d R . .
Eu1 Eu 0.84792(2) 0.50291(2) 0.562584(18) 0.03132(10) Uani 1 1 d . . .
O1 O 0.7822(3) 0.4458(3) 0.7133(2) 0.0461(10) Uani 1 1 d . . .
O2 O 0.7704(3) 0.6049(3) 0.6927(2) 0.0420(9) Uani 1 1 d . . .
O3 O 0.9919(3) 0.4916(3) 0.4148(2) 0.0373(9) Uani 1 1 d . . .
O4 O 0.8200(3) 0.5122(4) 0.4226(3) 0.0576(12) Uani 1 1 d . . .
O5 O 1.0117(3) 0.6724(3) 0.4511(2) 0.0400(9) Uani 1 1 d . . .
O6 O 0.8409(3) 0.6683(3) 0.5122(2) 0.0393(9) Uani 1 1 d . . .
N1 N 0.7242(4) 0.4009(3) 0.5691(3) 0.0379(11) Uani 1 1 d . . .
N2 N 0.6291(4) 0.6083(3) 0.5912(3) 0.0406(11) Uani 1 1 d . . .
N3 N 0.3403(5) 0.9288(4) 1.0108(3) 0.0657(16) Uani 1 1 d . . .
H3 H 0.3206 0.9938 1.0159 0.079 Uiso 1 1 calc R . .
N4 N 0.7037(7) 0.9497(6) 0.1664(4) 0.087(2) Uani 1 1 d . . .
H4 H 0.6947 0.9925 0.1236 0.104 Uiso 1 1 calc R . .
N5 N 1.0016(5) 1.1691(4) 0.3235(4) 0.0654(16) Uani 1 1 d . . .
H5 H 1.0433 1.2016 0.3208 0.079 Uiso 1 1 calc R . .
C1 C 0.7689(5) 0.2999(4) 0.5559(4) 0.0511(16) Uani 1 1 d . . .
H1 H 0.8480 0.2651 0.5406 0.061 Uiso 1 1 calc R . .
C2 C 0.7053(6) 0.2431(5) 0.5633(4) 0.0639(19) Uani 1 1 d . . .
H2A H 0.7405 0.1723 0.5539 0.077 Uiso 1 1 calc R . .
C3 C 0.5894(6) 0.2944(6) 0.5847(4) 0.0597(18) Uani 1 1 d . . .
H3B H 0.5446 0.2579 0.5914 0.072 Uiso 1 1 calc R . .
C4 C 0.5377(5) 0.4006(5) 0.5965(4) 0.0460(15) Uani 1 1 d . . .
C5 C 0.4159(6) 0.4591(7) 0.6162(4) 0.064(2) Uani 1 1 d . . .
H5B H 0.3686 0.4257 0.6212 0.076 Uiso 1 1 calc R . .
C6 C 0.3710(6) 0.5608(7) 0.6273(4) 0.068(2) Uani 1 1 d . . .
H6C H 0.2921 0.5969 0.6401 0.082 Uiso 1 1 calc R . .
C7 C 0.4388(5) 0.6166(5) 0.6203(4) 0.0492(16) Uani 1 1 d . . .
C8 C 0.3940(5) 0.7232(6) 0.6318(5) 0.068(2) Uani 1 1 d . . .
H8A H 0.3155 0.7620 0.6452 0.081 Uiso 1 1 calc R . .
C9 C 0.4641(5) 0.7691(6) 0.6236(5) 0.067(2) Uani 1 1 d . . .
H9A H 0.4350 0.8399 0.6314 0.080 Uiso 1 1 calc R . .
C10 C 0.5818(5) 0.7097(5) 0.6032(4) 0.0537(17) Uani 1 1 d . . .
H10 H 0.6295 0.7429 0.5977 0.064 Uiso 1 1 calc R . .
C11 C 0.5580(4) 0.5614(4) 0.6005(3) 0.0373(13) Uani 1 1 d . . .
C12 C 0.6089(4) 0.4507(4) 0.5885(3) 0.0371(13) Uani 1 1 d . . .
C13 C 0.7545(4) 0.5332(5) 0.7416(4) 0.0390(14) Uani 1 1 d . . .
C14 C 0.7022(5) 0.5491(5) 0.8359(4) 0.0505(16) Uani 1 1 d . . .
H14A H 0.6765 0.4943 0.8614 0.061 Uiso 1 1 calc R . .
H14B H 0.7609 0.5423 0.8605 0.061 Uiso 1 1 calc R . .
C15 C 0.6032(5) 0.6527(5) 0.8582(4) 0.0482(15) Uani 1 1 d . . .
H15A H 0.5453 0.6613 0.8320 0.058 Uiso 1 1 calc R . .
H15B H 0.6292 0.7079 0.8357 0.058 Uiso 1 1 calc R . .
C16 C 0.5510(6) 0.6620(6) 0.9530(4) 0.072(2) Uani 1 1 d . . .
H16A H 0.5283 0.6047 0.9751 0.087 Uiso 1 1 calc R . .
H16B H 0.6093 0.6545 0.9783 0.087 Uiso 1 1 calc R . .
C17 C 0.4495(6) 0.7619(5) 0.9805(4) 0.0577(18) Uani 1 1 d . . .
C18 C 0.4488(6) 0.8568(6) 0.9819(4) 0.0647(19) Uani 1 1 d . . .
H18A H 0.5137 0.8707 0.9654 0.078 Uiso 1 1 calc R . .
C19 C 0.2693(6) 0.8804(6) 1.0297(4) 0.0614(19) Uani 1 1 d . . .
C20 C 0.1499(7) 0.9218(7) 1.0636(5) 0.086(3) Uani 1 1 d . . .
H20A H 0.1082 0.9921 1.0742 0.104 Uiso 1 1 calc R . .
C21 C 0.0983(8) 0.8554(10) 1.0802(6) 0.108(3) Uani 1 1 d . . .
H21A H 0.0197 0.8805 1.1034 0.130 Uiso 1 1 calc R . .
C22 C 0.1603(9) 0.7496(9) 1.0632(6) 0.101(3) Uani 1 1 d . . .
H22A H 0.1227 0.7057 1.0754 0.121 Uiso 1 1 calc R . .
C23 C 0.2776(7) 0.7104(7) 1.0282(4) 0.075(2) Uani 1 1 d . . .
H23A H 0.3186 0.6404 1.0164 0.090 Uiso 1 1 calc R . .
C24 C 0.3333(6) 0.7761(6) 1.0110(4) 0.0583(18) Uani 1 1 d . . .
C25 C 0.9159(5) 0.5052(5) 0.3796(4) 0.0439(15) Uani 1 1 d . . .
C26 C 0.9433(5) 0.5162(6) 0.2843(4) 0.064(2) Uani 1 1 d . . .
H26A H 0.9384 0.4597 0.2635 0.077 Uiso 1 1 calc R . .
H26B H 1.0210 0.5106 0.2611 0.077 Uiso 1 1 calc R . .
C27 C 0.8627(6) 0.6197(6) 0.2533(4) 0.071(2) Uani 1 1 d . . .
H27A H 0.8783 0.6183 0.1926 0.085 Uiso 1 1 calc R . .
H27B H 0.7849 0.6259 0.2787 0.085 Uiso 1 1 calc R . .
C28 C 0.8707(7) 0.7136(7) 0.2722(5) 0.086(3) Uani 1 1 d . . .
H28A H 0.9466 0.7105 0.2431 0.103 Uiso 1 1 calc R . .
H28B H 0.8606 0.7127 0.3324 0.103 Uiso 1 1 calc R . .
C29 C 0.7842(7) 0.8146(7) 0.2467(5) 0.071(2) Uani 1 1 d . . .
C30 C 0.7978(8) 0.8613(8) 0.1680(5) 0.089(3) Uani 1 1 d . . .
H30A H 0.8619 0.8363 0.1223 0.107 Uiso 1 1 calc R . .
C31 C 0.6257(8) 0.9599(7) 0.2432(5) 0.070(2) Uani 1 1 d . . .
C32 C 0.5143(10) 1.0343(7) 0.2703(8) 0.099(3) Uani 1 1 d . . .
H32A H 0.4826 1.0897 0.2349 0.119 Uiso 1 1 calc R . .
C33 C 0.4545(10) 1.0219(10) 0.3510(10) 0.124(5) Uani 1 1 d . . .
H33A H 0.3799 1.0699 0.3712 0.149 Uiso 1 1 calc R . .
C34 C 0.5015(11) 0.9398(11) 0.4039(7) 0.121(4) Uani 1 1 d . . .
H34A H 0.4582 0.9339 0.4589 0.145 Uiso 1 1 calc R . .
C35 C 0.6091(9) 0.8681(8) 0.3772(5) 0.089(3) Uani 1 1 d . . .
H35A H 0.6392 0.8137 0.4139 0.107 Uiso 1 1 calc R . .
C36 C 0.6746(7) 0.8748(6) 0.2963(5) 0.0628(19) Uani 1 1 d . . .
C37 C 0.9056(5) 0.7146(4) 0.4816(3) 0.0354(13) Uani 1 1 d . . .
C38 C 0.8473(5) 0.8319(4) 0.4839(4) 0.0461(15) Uani 1 1 d . . .
H38A H 0.7713 0.8535 0.4782 0.055 Uiso 1 1 calc R . .
H38B H 0.8385 0.8514 0.5393 0.055 Uiso 1 1 calc R . .
C39 C 0.9055(5) 0.8926(4) 0.4182(4) 0.0479(15) Uani 1 1 d . . .
H39A H 0.9067 0.8811 0.3625 0.057 Uiso 1 1 calc R . .
H39B H 0.9838 0.8683 0.4198 0.057 Uiso 1 1 calc R . .
C40 C 0.8432(6) 1.0087(4) 0.4344(4) 0.0614(19) Uani 1 1 d . . .
H40A H 0.7663 1.0328 0.4297 0.074 Uiso 1 1 calc R . .
H40B H 0.8374 1.0186 0.4918 0.074 Uiso 1 1 calc R . .
C41 C 0.8991(5) 1.0735(4) 0.3759(4) 0.0507(16) Uani 1 1 d . . .
C42 C 0.9653(6) 1.1124(5) 0.3921(5) 0.0616(18) Uani 1 1 d . . .
H42A H 0.9835 1.1019 0.4429 0.074 Uiso 1 1 calc R . .
C43 C 0.9606(6) 1.1655(5) 0.2601(5) 0.0574(18) Uani 1 1 d . . .
C44 C 0.9744(7) 1.2115(5) 0.1791(5) 0.076(2) Uani 1 1 d . . .
H44A H 1.0165 1.2519 0.1601 0.092 Uiso 1 1 calc R . .
C45 C 0.9221(8) 1.1937(7) 0.1288(6) 0.093(3) Uani 1 1 d . . .
H45A H 0.9309 1.2217 0.0737 0.111 Uiso 1 1 calc R . .
C46 C 0.8575(7) 1.1361(7) 0.1568(6) 0.084(2) Uani 1 1 d . . .
H46A H 0.8216 1.1286 0.1210 0.100 Uiso 1 1 calc R . .
C47 C 0.8445(6) 1.0893(5) 0.2367(5) 0.067(2) Uani 1 1 d . . .
H47A H 0.8027 1.0486 0.2545 0.080 Uiso 1 1 calc R . .
C48 C 0.8970(5) 1.1051(4) 0.2906(4) 0.0494(16) Uani 1 1 d . . .
N6 N 0.4922(4) 0.5436(4) 0.1883(3) 0.0559(14) Uani 1 1 d . . .
N7 N 0.2890(5) 0.7114(4) 0.2336(3) 0.0487(13) Uani 1 1 d . . .
H7 H 0.294(5) 0.643(5) 0.242(4) 0.073 Uiso 1 1 d . . .
C49 C 0.5929(6) 0.4649(6) 0.1666(5) 0.072(2) Uani 1 1 d . . .
H49A H 0.5943 0.3988 0.1698 0.087 Uiso 1 1 calc R . .
C50 C 0.6959(6) 0.4743(7) 0.1396(5) 0.082(3) Uani 1 1 d . . .
H50A H 0.7639 0.4159 0.1243 0.098 Uiso 1 1 calc R . .
C51 C 0.6972(7) 0.5712(8) 0.1353(5) 0.083(3) Uani 1 1 d . . .
H51A H 0.7658 0.5791 0.1174 0.100 Uiso 1 1 calc R . .
C52 C 0.5928(6) 0.6571(6) 0.1587(4) 0.0578(18) Uani 1 1 d . . .
C53 C 0.5852(7) 0.7604(7) 0.1570(5) 0.076(2) Uani 1 1 d . . .
H53A H 0.6516 0.7719 0.1405 0.091 Uiso 1 1 calc R . .
C54 C 0.4839(7) 0.8405(6) 0.1789(5) 0.071(2) Uani 1 1 d . . .
H54A H 0.4811 0.9070 0.1768 0.085 Uiso 1 1 calc R . .
C55 C 0.3814(6) 0.8264(5) 0.2050(4) 0.0538(17) Uani 1 1 d . . .
C56 C 0.2725(7) 0.9071(6) 0.2297(4) 0.072(2) Uani 1 1 d . . .
H56A H 0.2658 0.9748 0.2285 0.087 Uiso 1 1 calc R . .
C57 C 0.1777(6) 0.8883(6) 0.2551(5) 0.071(2) Uani 1 1 d . . .
H57A H 0.1062 0.9426 0.2710 0.085 Uiso 1 1 calc R . .
C58 C 0.1871(6) 0.7881(5) 0.2572(4) 0.0610(18) Uani 1 1 d . . .
H58A H 0.1220 0.7745 0.2753 0.073 Uiso 1 1 calc R . .
C59 C 0.3869(5) 0.7255(5) 0.2072(4) 0.0469(15) Uani 1 1 d . . .
C60 C 0.4942(5) 0.6385(5) 0.1837(4) 0.0490(16) Uani 1 1 d . . .
N8 N 0.7515(6) 0.8139(6) 0.9244(6) 0.084(2) Uani 1 1 d . . .
O7 O 0.7033(6) 0.8811(6) 0.8762(5) 0.131(3) Uani 1 1 d . . .
O8 O 0.7932(6) 0.7224(5) 0.9056(5) 0.124(2) Uani 1 1 d . . .
O9 O 0.7587(7) 0.8365(6) 0.9880(4) 0.136(3) Uani 1 1 d . . .
O1W O 0.8115(6) 0.7766(5) 0.7078(4) 0.0968(18) Uani 1 1 d D . .
H1A H 0.780(8) 0.804(6) 0.754(3) 0.145 Uiso 1 1 d D . .
H1B H 0.801(8) 0.725(5) 0.705(5) 0.145 Uiso 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O2W H2WB 0.8500 . ?
O2W H2WC 0.8501 . ?
Eu1 O6 2.337(4) . ?
Eu1 O3 2.356(3) 2_766 ?
Eu1 O5 2.393(3) 2_766 ?
Eu1 O4 2.464(4) . ?
Eu1 O1 2.506(4) . ?
Eu1 O2 2.507(4) . ?
Eu1 O3 2.589(4) . ?
Eu1 N2 2.596(4) . ?
Eu1 N1 2.628(4) . ?
Eu1 Eu1 3.9454(11) 2_766 ?
O1 C13 1.270(6) . ?
O2 C13 1.245(6) . ?
O3 C25 1.274(6) . ?
O3 Eu1 2.356(3) 2_766 ?
O4 C25 1.233(7) . ?
O5 C37 1.254(6) . ?
O5 Eu1 2.393(3) 2_766 ?
O6 C37 1.250(6) . ?
N1 C1 1.330(7) . ?
N1 C12 1.355(6) . ?
N2 C10 1.329(7) . ?
N2 C11 1.353(7) . ?
N3 C19 1.345(8) . ?
N3 C18 1.362(8) . ?
N3 H3 0.8600 . ?
N4 C30 1.352(10) . ?
N4 C31 1.359(10) . ?
N4 H4 0.8600 . ?
N5 C43 1.365(8) . ?
N5 C42 1.369(8) . ?
N5 H5 0.8600 . ?
C1 C2 1.387(8) . ?
C1 H1 0.9300 . ?
C2 C3 1.362(8) . ?
C2 H2A 0.9300 . ?
C3 C4 1.389(9) . ?
C3 H3B 0.9300 . ?
C4 C12 1.395(7) . ?
C4 C5 1.441(8) . ?
C5 C6 1.331(10) . ?
C5 H5B 0.9300 . ?
C6 C7 1.425(9) . ?
C6 H6C 0.9300 . ?
C7 C8 1.398(9) . ?
C7 C11 1.406(7) . ?
C8 C9 1.334(9) . ?
C8 H8A 0.9300 . ?
C9 C10 1.397(8) . ?
C9 H9A 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.447(8) . ?
C13 C14 1.520(8) . ?
C14 C15 1.508(7) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.518(8) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.503(9) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.357(9) . ?
C17 C24 1.422(9) . ?
C18 H18A 0.9300 . ?
C19 C24 1.393(9) . ?
C19 C20 1.408(10) . ?
C20 C21 1.353(12) . ?
C20 H20A 0.9300 . ?
C21 C22 1.402(13) . ?
C21 H21A 0.9300 . ?
C22 C23 1.386(11) . ?
C22 H22A 0.9300 . ?
C23 C24 1.383(10) . ?
C23 H23A 0.9300 . ?
C25 C26 1.512(8) . ?
C26 C27 1.529(9) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.490(10) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C29 1.506(10) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.363(10) . ?
C29 C36 1.407(10) . ?
C30 H30A 0.9300 . ?
C31 C32 1.395(11) . ?
C31 C36 1.416(10) . ?
C32 C33 1.359(14) . ?
C32 H32A 0.9300 . ?
C33 C34 1.384(14) . ?
C33 H33A 0.9300 . ?
C34 C35 1.347(13) . ?
C34 H34A 0.9300 . ?
C35 C36 1.372(10) . ?
C35 H35A 0.9300 . ?
C37 C38 1.514(7) . ?
C38 C39 1.512(8) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 C40 1.527(7) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 C41 1.484(9) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 C42 1.354(9) . ?
C41 C48 1.424(8) . ?
C42 H42A 0.9300 . ?
C43 C44 1.390(10) . ?
C43 C48 1.399(9) . ?
C44 C45 1.377(11) . ?
C44 H44A 0.9300 . ?
C45 C46 1.375(11) . ?
C45 H45A 0.9300 . ?
C46 C47 1.379(10) . ?
C46 H46A 0.9300 . ?
C47 C48 1.413(9) . ?
C47 H47A 0.9300 . ?
N6 C49 1.321(8) . ?
N6 C60 1.357(8) . ?
N7 C58 1.323(7) . ?
N7 C59 1.348(8) . ?
N7 H7 0.94(6) . ?
C49 C50 1.380(10) . ?
C49 H49A 0.9300 . ?
C50 C51 1.383(11) . ?
C50 H50A 0.9300 . ?
C51 C52 1.402(10) . ?
C51 H51A 0.9300 . ?
C52 C60 1.392(9) . ?
C52 C53 1.431(10) . ?
C53 C54 1.336(10) . ?
C53 H53A 0.9300 . ?
C54 C55 1.408(9) . ?
C54 H54A 0.9300 . ?
C55 C56 1.404(9) . ?
C55 C59 1.406(8) . ?
C56 C57 1.346(10) . ?
C56 H56A 0.9300 . ?
C57 C58 1.376(9) . ?
C57 H57A 0.9300 . ?
C58 H58A 0.9300 . ?
C59 C60 1.430(8) . ?
N8 O9 1.210(9) . ?
N8 O8 1.232(8) . ?
N8 O7 1.233(9) . ?
O1W H1A 0.822(10) . ?
O1W H1B 0.824(10) . ?

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
H2WB O2W H2WC 109.5 . . ?
O6 Eu1 O3 74.92(12) . 2_766 ?
O6 Eu1 O5 136.97(12) . 2_766 ?
O3 Eu1 O5 75.20(12) 2_766 2_766 ?
O6 Eu1 O4 78.90(14) . . ?
O3 Eu1 O4 124.61(13) 2_766 . ?
O5 Eu1 O4 93.58(14) 2_766 . ?
O6 Eu1 O1 126.88(12) . . ?
O3 Eu1 O1 91.95(13) 2_766 . ?
O5 Eu1 O1 84.26(12) 2_766 . ?
O4 Eu1 O1 141.62(14) . . ?
O6 Eu1 O2 75.36(13) . . ?
O3 Eu1 O2 75.01(12) 2_766 . ?
O5 Eu1 O2 124.64(12) 2_766 . ?
O4 Eu1 O2 141.56(14) . . ?
O1 Eu1 O2 51.59(12) . . ?
O6 Eu1 O3 70.01(12) . . ?
O3 Eu1 O3 74.24(13) 2_766 . ?
O5 Eu1 O3 72.53(12) 2_766 . ?
O4 Eu1 O3 51.00(12) . . ?
O1 Eu1 O3 155.27(12) . . ?
O2 Eu1 O3 138.35(12) . . ?
O6 Eu1 N2 79.60(13) . . ?
O3 Eu1 N2 140.69(13) 2_766 . ?
O5 Eu1 N2 140.63(13) 2_766 . ?
O4 Eu1 N2 77.83(14) . . ?
O1 Eu1 N2 79.92(14) . . ?
O2 Eu1 N2 69.86(13) . . ?
O3 Eu1 N2 123.68(13) . . ?
O6 Eu1 N1 134.84(13) . . ?
O3 Eu1 N1 150.19(13) 2_766 . ?
O5 Eu1 N1 78.35(13) 2_766 . ?
O4 Eu1 N1 70.25(14) . . ?
O1 Eu1 N1 71.81(13) . . ?
O2 Eu1 N1 110.21(13) . . ?
O3 Eu1 N1 110.50(12) . . ?
N2 Eu1 N1 62.51(14) . . ?
O6 Eu1 Eu1 67.68(8) . 2_766 ?
O3 Eu1 Eu1 39.17(9) 2_766 2_766 ?
O5 Eu1 Eu1 69.54(9) 2_766 2_766 ?
O4 Eu1 Eu1 85.76(9) . 2_766 ?
O1 Eu1 Eu1 128.06(9) . 2_766 ?
O2 Eu1 Eu1 109.63(9) . 2_766 ?
O3 Eu1 Eu1 35.07(7) . 2_766 ?
N2 Eu1 Eu1 145.68(10) . 2_766 ?
N1 Eu1 Eu1 138.40(10) . 2_766 ?
C13 O1 Eu1 93.7(3) . . ?
C13 O2 Eu1 94.3(3) . . ?
C25 O3 Eu1 160.5(4) . 2_766 ?
C25 O3 Eu1 90.6(3) . . ?
Eu1 O3 Eu1 105.76(13) 2_766 . ?
C25 O4 Eu1 97.6(3) . . ?
C37 O5 Eu1 135.1(3) . 2_766 ?
C37 O6 Eu1 140.4(3) . . ?
C1 N1 C12 116.8(5) . . ?
C1 N1 Eu1 123.1(4) . . ?
C12 N1 Eu1 120.1(3) . . ?
C10 N2 C11 117.2(5) . . ?
C10 N2 Eu1 121.0(4) . . ?
C11 N2 Eu1 121.6(3) . . ?
C19 N3 C18 107.9(6) . . ?
C19 N3 H3 126.0 . . ?
C18 N3 H3 126.0 . . ?
C30 N4 C31 109.1(7) . . ?
C30 N4 H4 125.5 . . ?
C31 N4 H4 125.5 . . ?
C43 N5 C42 108.4(6) . . ?
C43 N5 H5 125.8 . . ?
C42 N5 H5 125.8 . . ?
N1 C1 C2 124.2(6) . . ?
N1 C1 H1 117.9 . . ?
C2 C1 H1 117.9 . . ?
C3 C2 C1 117.9(6) . . ?
C3 C2 H2A 121.1 . . ?
C1 C2 H2A 121.1 . . ?
C2 C3 C4 120.6(6) . . ?
C2 C3 H3B 119.7 . . ?
C4 C3 H3B 119.7 . . ?
C3 C4 C12 117.2(6) . . ?
C3 C4 C5 122.8(6) . . ?
C12 C4 C5 120.0(6) . . ?
C6 C5 C4 120.2(6) . . ?
C6 C5 H5B 119.9 . . ?
C4 C5 H5B 119.9 . . ?
C5 C6 C7 122.6(7) . . ?
C5 C6 H6C 118.7 . . ?
C7 C6 H6C 118.7 . . ?
C8 C7 C11 117.9(6) . . ?
C8 C7 C6 123.9(6) . . ?
C11 C7 C6 118.3(6) . . ?
C9 C8 C7 119.7(6) . . ?
C9 C8 H8A 120.1 . . ?
C7 C8 H8A 120.1 . . ?
C8 C9 C10 119.4(7) . . ?
C8 C9 H9A 120.3 . . ?
C10 C9 H9A 120.3 . . ?
N2 C10 C9 123.4(6) . . ?
N2 C10 H10 118.3 . . ?
C9 C10 H10 118.3 . . ?
N2 C11 C7 122.3(5) . . ?
N2 C11 C12 117.5(5) . . ?
C7 C11 C12 120.2(5) . . ?
N1 C12 C4 123.1(5) . . ?
N1 C12 C11 118.1(5) . . ?
C4 C12 C11 118.7(5) . . ?
O2 C13 O1 120.3(5) . . ?
O2 C13 C14 120.4(5) . . ?
O1 C13 C14 119.3(5) . . ?
C15 C14 C13 114.4(5) . . ?
C15 C14 H14A 108.7 . . ?
C13 C14 H14A 108.7 . . ?
C15 C14 H14B 108.7 . . ?
C13 C14 H14B 108.7 . . ?
H14A C14 H14B 107.6 . . ?
C14 C15 C16 112.0(5) . . ?
C14 C15 H15A 109.2 . . ?
C16 C15 H15A 109.2 . . ?
C14 C15 H15B 109.2 . . ?
C16 C15 H15B 109.2 . . ?
H15A C15 H15B 107.9 . . ?
C17 C16 C15 115.3(5) . . ?
C17 C16 H16A 108.4 . . ?
C15 C16 H16A 108.4 . . ?
C17 C16 H16B 108.4 . . ?
C15 C16 H16B 108.4 . . ?
H16A C16 H16B 107.5 . . ?
C18 C17 C24 105.6(6) . . ?
C18 C17 C16 127.8(7) . . ?
C24 C17 C16 126.6(7) . . ?
C17 C18 N3 110.9(7) . . ?
C17 C18 H18A 124.6 . . ?
N3 C18 H18A 124.6 . . ?
N3 C19 C24 108.8(6) . . ?
N3 C19 C20 128.8(8) . . ?
C24 C19 C20 122.3(8) . . ?
C21 C20 C19 117.4(9) . . ?
C21 C20 H20A 121.3 . . ?
C19 C20 H20A 121.3 . . ?
C20 C21 C22 121.7(9) . . ?
C20 C21 H21A 119.1 . . ?
C22 C21 H21A 119.1 . . ?
C23 C22 C21 120.2(10) . . ?
C23 C22 H22A 119.9 . . ?
C21 C22 H22A 119.9 . . ?
C24 C23 C22 119.6(8) . . ?
C24 C23 H23A 120.2 . . ?
C22 C23 H23A 120.2 . . ?
C23 C24 C19 118.7(7) . . ?
C23 C24 C17 134.4(7) . . ?
C19 C24 C17 106.7(7) . . ?
O4 C25 O3 120.6(5) . . ?
O4 C25 C26 120.3(5) . . ?
O3 C25 C26 119.1(5) . . ?
C25 C26 C27 112.6(5) . . ?
C25 C26 H26A 109.1 . . ?
C27 C26 H26A 109.1 . . ?
C25 C26 H26B 109.1 . . ?
C27 C26 H26B 109.1 . . ?
H26A C26 H26B 107.8 . . ?
C28 C27 C26 115.1(6) . . ?
C28 C27 H27A 108.5 . . ?
C26 C27 H27A 108.5 . . ?
C28 C27 H27B 108.5 . . ?
C26 C27 H27B 108.5 . . ?
H27A C27 H27B 107.5 . . ?
C27 C28 C29 113.8(6) . . ?
C27 C28 H28A 108.8 . . ?
C29 C28 H28A 108.8 . . ?
C27 C28 H28B 108.8 . . ?
C29 C28 H28B 108.8 . . ?
H28A C28 H28B 107.7 . . ?
C30 C29 C36 107.4(7) . . ?
C30 C29 C28 124.8(8) . . ?
C36 C29 C28 127.7(8) . . ?
N4 C30 C29 109.7(8) . . ?
N4 C30 H30A 125.2 . . ?
C29 C30 H30A 125.2 . . ?
N4 C31 C32 130.1(9) . . ?
N4 C31 C36 107.7(8) . . ?
C32 C31 C36 122.2(8) . . ?
C33 C32 C31 116.7(10) . . ?
C33 C32 H32A 121.6 . . ?
C31 C32 H32A 121.6 . . ?
C32 C33 C34 121.8(12) . . ?
C32 C33 H33A 119.1 . . ?
C34 C33 H33A 119.1 . . ?
C35 C34 C33 121.1(12) . . ?
C35 C34 H34A 119.4 . . ?
C33 C34 H34A 119.4 . . ?
C34 C35 C36 120.6(10) . . ?
C34 C35 H35A 119.7 . . ?
C36 C35 H35A 119.7 . . ?
C35 C36 C29 136.2(8) . . ?
C35 C36 C31 117.7(8) . . ?
C29 C36 C31 106.1(7) . . ?
O6 C37 O5 125.9(5) . . ?
O6 C37 C38 115.2(5) . . ?
O5 C37 C38 118.9(5) . . ?
C39 C38 C37 117.0(5) . . ?
C39 C38 H38A 108.0 . . ?
C37 C38 H38A 108.0 . . ?
C39 C38 H38B 108.0 . . ?
C37 C38 H38B 108.0 . . ?
H38A C38 H38B 107.3 . . ?
C38 C39 C40 110.7(5) . . ?
C38 C39 H39A 109.5 . . ?
C40 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C40 C39 H39B 109.5 . . ?
H39A C39 H39B 108.1 . . ?
C41 C40 C39 114.2(5) . . ?
C41 C40 H40A 108.7 . . ?
C39 C40 H40A 108.7 . . ?
C41 C40 H40B 108.7 . . ?
C39 C40 H40B 108.7 . . ?
H40A C40 H40B 107.6 . . ?
C42 C41 C48 105.8(6) . . ?
C42 C41 C40 126.8(7) . . ?
C48 C41 C40 127.3(6) . . ?
C41 C42 N5 110.7(6) . . ?
C41 C42 H42A 124.7 . . ?
N5 C42 H42A 124.7 . . ?
N5 C43 C44 129.4(7) . . ?
N5 C43 C48 107.4(6) . . ?
C44 C43 C48 123.2(7) . . ?
C45 C44 C43 116.0(8) . . ?
C45 C44 H44A 122.0 . . ?
C43 C44 H44A 122.0 . . ?
C46 C45 C44 122.6(9) . . ?
C46 C45 H45A 118.7 . . ?
C44 C45 H45A 118.7 . . ?
C45 C46 C47 121.7(8) . . ?
C45 C46 H46A 119.2 . . ?
C47 C46 H46A 119.2 . . ?
C46 C47 C48 117.8(8) . . ?
C46 C47 H47A 121.1 . . ?
C48 C47 H47A 121.1 . . ?
C43 C48 C47 118.7(7) . . ?
C43 C48 C41 107.6(6) . . ?
C47 C48 C41 133.6(7) . . ?
C49 N6 C60 115.7(6) . . ?
C58 N7 C59 123.3(6) . . ?
C58 N7 H7 118(4) . . ?
C59 N7 H7 118(4) . . ?
N6 C49 C50 124.4(8) . . ?
N6 C49 H49A 117.8 . . ?
C50 C49 H49A 117.8 . . ?
C49 C50 C51 119.5(8) . . ?
C49 C50 H50A 120.3 . . ?
C51 C50 H50A 120.3 . . ?
C50 C51 C52 118.4(7) . . ?
C50 C51 H51A 120.8 . . ?
C52 C51 H51A 120.8 . . ?
C60 C52 C51 117.1(7) . . ?
C60 C52 C53 120.3(7) . . ?
C51 C52 C53 122.6(7) . . ?
C54 C53 C52 120.8(7) . . ?
C54 C53 H53A 119.6 . . ?
C52 C53 H53A 119.6 . . ?
C53 C54 C55 121.5(7) . . ?
C53 C54 H54A 119.3 . . ?
C55 C54 H54A 119.3 . . ?
C56 C55 C59 117.2(6) . . ?
C56 C55 C54 124.1(7) . . ?
C59 C55 C54 118.6(7) . . ?
C57 C56 C55 121.2(7) . . ?
C57 C56 H56A 119.4 . . ?
C55 C56 H56A 119.4 . . ?
C56 C57 C58 119.6(7) . . ?
C56 C57 H57A 120.2 . . ?
C58 C57 H57A 120.2 . . ?
N7 C58 C57 119.8(7) . . ?
N7 C58 H58A 120.1 . . ?
C57 C58 H58A 120.1 . . ?
N7 C59 C55 118.8(6) . . ?
N7 C59 C60 120.1(6) . . ?
C55 C59 C60 121.0(6) . . ?
N6 C60 C52 124.9(6) . . ?
N6 C60 C59 117.4(6) . . ?
C52 C60 C59 117.8(6) . . ?
O9 N8 O8 120.7(9) . . ?
O9 N8 O7 121.4(9) . . ?
O8 N8 O7 117.9(9) . . ?
H1A O1W H1B 115(2) . . ?

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
O6 Eu1 O1 C13 -2.4(4) . . . . ?
O3 Eu1 O1 C13 70.1(3) 2_766 . . . ?
O5 Eu1 O1 C13 145.1(3) 2_766 . . . ?
O4 Eu1 O1 C13 -126.4(3) . . . . ?
O2 Eu1 O1 C13 1.1(3) . . . . ?
O3 Eu1 O1 C13 125.0(3) . . . . ?
N2 Eu1 O1 C13 -71.1(3) . . . . ?
N1 Eu1 O1 C13 -135.3(3) . . . . ?
Eu1 Eu1 O1 C13 86.7(3) 2_766 . . . ?
O6 Eu1 O2 C13 176.0(3) . . . . ?
O3 Eu1 O2 C13 -106.0(3) 2_766 . . . ?
O5 Eu1 O2 C13 -46.5(4) 2_766 . . . ?
O4 Eu1 O2 C13 126.5(3) . . . . ?
O1 Eu1 O2 C13 -1.1(3) . . . . ?
O3 Eu1 O2 C13 -149.6(3) . . . . ?
N2 Eu1 O2 C13 91.9(3) . . . . ?
N1 Eu1 O2 C13 43.1(3) . . . . ?
Eu1 Eu1 O2 C13 -124.6(3) 2_766 . . . ?
O6 Eu1 O3 C25 -90.1(3) . . . . ?
O3 Eu1 O3 C25 -169.4(4) 2_766 . . . ?
O5 Eu1 O3 C25 111.5(3) 2_766 . . . ?
O4 Eu1 O3 C25 1.7(3) . . . . ?
O1 Eu1 O3 C25 132.5(4) . . . . ?
O2 Eu1 O3 C25 -125.6(3) . . . . ?
N2 Eu1 O3 C25 -28.3(4) . . . . ?
N1 Eu1 O3 C25 41.6(3) . . . . ?
Eu1 Eu1 O3 C25 -169.4(4) 2_766 . . . ?
O6 Eu1 O3 Eu1 79.33(14) . . . 2_766 ?
O3 Eu1 O3 Eu1 0.0 2_766 . . 2_766 ?
O5 Eu1 O3 Eu1 -79.08(14) 2_766 . . 2_766 ?
O4 Eu1 O3 Eu1 171.1(2) . . . 2_766 ?
O1 Eu1 O3 Eu1 -58.1(3) . . . 2_766 ?
O2 Eu1 O3 Eu1 43.8(2) . . . 2_766 ?
N2 Eu1 O3 Eu1 141.08(14) . . . 2_766 ?
N1 Eu1 O3 Eu1 -148.98(14) . . . 2_766 ?
O6 Eu1 O4 C25 71.4(4) . . . . ?
O3 Eu1 O4 C25 8.7(5) 2_766 . . . ?
O5 Eu1 O4 C25 -65.8(4) 2_766 . . . ?
O1 Eu1 O4 C25 -151.1(3) . . . . ?
O2 Eu1 O4 C25 120.0(4) . . . . ?
O3 Eu1 O4 C25 -1.8(3) . . . . ?
N2 Eu1 O4 C25 153.0(4) . . . . ?
N1 Eu1 O4 C25 -142.1(4) . . . . ?
Eu1 Eu1 O4 C25 3.4(4) 2_766 . . . ?
O3 Eu1 O6 C37 27.3(5) 2_766 . . . ?
O5 Eu1 O6 C37 -20.1(6) 2_766 . . . ?
O4 Eu1 O6 C37 -103.4(6) . . . . ?
O1 Eu1 O6 C37 108.2(5) . . . . ?
O2 Eu1 O6 C37 105.4(6) . . . . ?
O3 Eu1 O6 C37 -51.1(5) . . . . ?
N2 Eu1 O6 C37 177.1(6) . . . . ?
N1 Eu1 O6 C37 -150.5(5) . . . . ?
Eu1 Eu1 O6 C37 -13.5(5) 2_766 . . . ?
O6 Eu1 N1 C1 141.4(4) . . . . ?
O3 Eu1 N1 C1 -34.4(6) 2_766 . . . ?
O5 Eu1 N1 C1 -6.6(4) 2_766 . . . ?
O4 Eu1 N1 C1 91.6(5) . . . . ?
O1 Eu1 N1 C1 -94.3(5) . . . . ?
O2 Eu1 N1 C1 -129.4(4) . . . . ?
O3 Eu1 N1 C1 59.6(5) . . . . ?
N2 Eu1 N1 C1 177.8(5) . . . . ?
Eu1 Eu1 N1 C1 33.1(5) 2_766 . . . ?
O6 Eu1 N1 C12 -40.1(4) . . . . ?
O3 Eu1 N1 C12 144.1(3) 2_766 . . . ?
O5 Eu1 N1 C12 171.9(4) 2_766 . . . ?
O4 Eu1 N1 C12 -89.9(4) . . . . ?
O1 Eu1 N1 C12 84.2(4) . . . . ?
O2 Eu1 N1 C12 49.1(4) . . . . ?
O3 Eu1 N1 C12 -121.9(4) . . . . ?
N2 Eu1 N1 C12 -3.7(4) . . . . ?
Eu1 Eu1 N1 C12 -148.4(3) 2_766 . . . ?
O6 Eu1 N2 C10 -26.2(4) . . . . ?
O3 Eu1 N2 C10 23.8(6) 2_766 . . . ?
O5 Eu1 N2 C10 172.3(4) 2_766 . . . ?
O4 Eu1 N2 C10 -107.0(5) . . . . ?
O1 Eu1 N2 C10 104.5(5) . . . . ?
O2 Eu1 N2 C10 51.8(4) . . . . ?
O3 Eu1 N2 C10 -83.6(5) . . . . ?
N1 Eu1 N2 C10 179.1(5) . . . . ?
Eu1 Eu1 N2 C10 -43.7(5) 2_766 . . . ?
O6 Eu1 N2 C11 158.5(4) . . . . ?
O3 Eu1 N2 C11 -151.4(4) 2_766 . . . ?
O5 Eu1 N2 C11 -2.9(5) 2_766 . . . ?
O4 Eu1 N2 C11 77.8(4) . . . . ?
O1 Eu1 N2 C11 -70.7(4) . . . . ?
O2 Eu1 N2 C11 -123.4(4) . . . . ?
O3 Eu1 N2 C11 101.2(4) . . . . ?
N1 Eu1 N2 C11 3.9(4) . . . . ?
Eu1 Eu1 N2 C11 141.0(3) 2_766 . . . ?
C12 N1 C1 C2 -2.1(9) . . . . ?
Eu1 N1 C1 C2 176.5(5) . . . . ?
N1 C1 C2 C3 0.7(10) . . . . ?
C1 C2 C3 C4 1.6(10) . . . . ?
C2 C3 C4 C12 -2.3(9) . . . . ?
C2 C3 C4 C5 177.8(6) . . . . ?
C3 C4 C5 C6 179.7(7) . . . . ?
C12 C4 C5 C6 -0.3(9) . . . . ?
C4 C5 C6 C7 0.1(11) . . . . ?
C5 C6 C7 C8 -179.8(7) . . . . ?
C5 C6 C7 C11 0.3(10) . . . . ?
C11 C7 C8 C9 0.2(10) . . . . ?
C6 C7 C8 C9 -179.6(7) . . . . ?
C7 C8 C9 C10 0.3(11) . . . . ?
C11 N2 C10 C9 -0.8(9) . . . . ?
Eu1 N2 C10 C9 -176.2(5) . . . . ?
C8 C9 C10 N2 0.0(11) . . . . ?
C10 N2 C11 C7 1.3(8) . . . . ?
Eu1 N2 C11 C7 176.7(4) . . . . ?
C10 N2 C11 C12 -179.3(5) . . . . ?
Eu1 N2 C11 C12 -3.9(6) . . . . ?
C8 C7 C11 N2 -1.0(9) . . . . ?
C6 C7 C11 N2 178.8(5) . . . . ?
C8 C7 C11 C12 179.6(6) . . . . ?
C6 C7 C11 C12 -0.6(8) . . . . ?
C1 N1 C12 C4 1.3(8) . . . . ?
Eu1 N1 C12 C4 -177.3(4) . . . . ?
C1 N1 C12 C11 -178.0(5) . . . . ?
Eu1 N1 C12 C11 3.4(6) . . . . ?
C3 C4 C12 N1 0.8(8) . . . . ?
C5 C4 C12 N1 -179.2(5) . . . . ?
C3 C4 C12 C11 -179.9(5) . . . . ?
C5 C4 C12 C11 0.1(8) . . . . ?
N2 C11 C12 N1 0.3(7) . . . . ?
C7 C11 C12 N1 179.7(5) . . . . ?
N2 C11 C12 C4 -179.0(5) . . . . ?
C7 C11 C12 C4 0.4(8) . . . . ?
Eu1 O2 C13 O1 2.0(5) . . . . ?
Eu1 O2 C13 C14 -178.3(4) . . . . ?
Eu1 O1 C13 O2 -2.0(5) . . . . ?
Eu1 O1 C13 C14 178.3(4) . . . . ?
O2 C13 C14 C15 42.3(8) . . . . ?
O1 C13 C14 C15 -137.9(6) . . . . ?
C13 C14 C15 C16 177.3(6) . . . . ?
C14 C15 C16 C17 -178.3(6) . . . . ?
C15 C16 C17 C18 -75.8(9) . . . . ?
C15 C16 C17 C24 104.5(8) . . . . ?
C24 C17 C18 N3 -0.3(8) . . . . ?
C16 C17 C18 N3 179.9(6) . . . . ?
C19 N3 C18 C17 1.0(8) . . . . ?
C18 N3 C19 C24 -1.3(8) . . . . ?
C18 N3 C19 C20 178.2(7) . . . . ?
N3 C19 C20 C21 -177.5(8) . . . . ?
C24 C19 C20 C21 2.0(12) . . . . ?
C19 C20 C21 C22 -1.0(14) . . . . ?
C20 C21 C22 C23 -0.2(15) . . . . ?
C21 C22 C23 C24 0.6(12) . . . . ?
C22 C23 C24 C19 0.3(10) . . . . ?
C22 C23 C24 C17 176.0(7) . . . . ?
N3 C19 C24 C23 177.9(6) . . . . ?
C20 C19 C24 C23 -1.6(10) . . . . ?
N3 C19 C24 C17 1.1(8) . . . . ?
C20 C19 C24 C17 -178.4(6) . . . . ?
C18 C17 C24 C23 -176.6(8) . . . . ?
C16 C17 C24 C23 3.2(12) . . . . ?
C18 C17 C24 C19 -0.5(7) . . . . ?
C16 C17 C24 C19 179.3(6) . . . . ?
Eu1 O4 C25 O3 3.2(6) . . . . ?
Eu1 O4 C25 C26 -174.6(5) . . . . ?
Eu1 O3 C25 O4 -151.0(8) 2_766 . . . ?
Eu1 O3 C25 O4 -3.0(6) . . . . ?
Eu1 O3 C25 C26 26.9(14) 2_766 . . . ?
Eu1 O3 C25 C26 174.8(5) . . . . ?
O4 C25 C26 C27 57.0(9) . . . . ?
O3 C25 C26 C27 -120.8(6) . . . . ?
C25 C26 C27 C28 65.4(9) . . . . ?
C26 C27 C28 C29 -175.6(7) . . . . ?
C27 C28 C29 C30 -85.1(10) . . . . ?
C27 C28 C29 C36 91.4(9) . . . . ?
C31 N4 C30 C29 -2.1(9) . . . . ?
C36 C29 C30 N4 2.0(9) . . . . ?
C28 C29 C30 N4 179.1(7) . . . . ?
C30 N4 C31 C32 -175.8(8) . . . . ?
C30 N4 C31 C36 1.4(9) . . . . ?
N4 C31 C32 C33 177.3(9) . . . . ?
C36 C31 C32 C33 0.5(12) . . . . ?
C31 C32 C33 C34 0.2(15) . . . . ?
C32 C33 C34 C35 -0.3(17) . . . . ?
C33 C34 C35 C36 -0.3(15) . . . . ?
C34 C35 C36 C29 -176.7(8) . . . . ?
C34 C35 C36 C31 1.0(12) . . . . ?
C30 C29 C36 C35 176.8(9) . . . . ?
C28 C29 C36 C35 -0.2(14) . . . . ?
C30 C29 C36 C31 -1.1(8) . . . . ?
C28 C29 C36 C31 -178.1(7) . . . . ?
N4 C31 C36 C35 -178.6(7) . . . . ?
C32 C31 C36 C35 -1.1(11) . . . . ?
N4 C31 C36 C29 -0.2(8) . . . . ?
C32 C31 C36 C29 177.2(7) . . . . ?
Eu1 O6 C37 O5 16.4(9) . . . . ?
Eu1 O6 C37 C38 -162.7(4) . . . . ?
Eu1 O5 C37 O6 -3.8(9) 2_766 . . . ?
Eu1 O5 C37 C38 175.3(4) 2_766 . . . ?
O6 C37 C38 C39 -154.3(5) . . . . ?
O5 C37 C38 C39 26.5(8) . . . . ?
C37 C38 C39 C40 -174.2(5) . . . . ?
C38 C39 C40 C41 176.3(6) . . . . ?
C39 C40 C41 C42 -100.9(8) . . . . ?
C39 C40 C41 C48 77.2(8) . . . . ?
C48 C41 C42 N5 2.0(7) . . . . ?
C40 C41 C42 N5 -179.6(6) . . . . ?
C43 N5 C42 C41 -1.4(8) . . . . ?
C42 N5 C43 C44 179.7(7) . . . . ?
C42 N5 C43 C48 0.1(7) . . . . ?
N5 C43 C44 C45 -180.0(7) . . . . ?
C48 C43 C44 C45 -0.5(10) . . . . ?
C43 C44 C45 C46 1.5(12) . . . . ?
C44 C45 C46 C47 -2.4(13) . . . . ?
C45 C46 C47 C48 2.1(11) . . . . ?
N5 C43 C48 C47 179.9(5) . . . . ?
C44 C43 C48 C47 0.3(9) . . . . ?
N5 C43 C48 C41 1.1(7) . . . . ?
C44 C43 C48 C41 -178.5(6) . . . . ?
C46 C47 C48 C43 -1.1(9) . . . . ?
C46 C47 C48 C41 177.4(6) . . . . ?
C42 C41 C48 C43 -1.9(7) . . . . ?
C40 C41 C48 C43 179.7(6) . . . . ?
C42 C41 C48 C47 179.6(7) . . . . ?
C40 C41 C48 C47 1.2(11) . . . . ?
C60 N6 C49 C50 -0.8(10) . . . . ?
N6 C49 C50 C51 1.0(12) . . . . ?
C49 C50 C51 C52 -0.2(12) . . . . ?
C50 C51 C52 C60 -0.8(10) . . . . ?
C50 C51 C52 C53 179.6(7) . . . . ?
C60 C52 C53 C54 -0.3(11) . . . . ?
C51 C52 C53 C54 179.3(7) . . . . ?
C52 C53 C54 C55 0.6(11) . . . . ?
C53 C54 C55 C56 179.2(7) . . . . ?
C53 C54 C55 C59 -0.5(10) . . . . ?
C59 C55 C56 C57 0.5(10) . . . . ?
C54 C55 C56 C57 -179.2(7) . . . . ?
C55 C56 C57 C58 0.2(11) . . . . ?
C59 N7 C58 C57 0.4(10) . . . . ?
C56 C57 C58 N7 -0.7(11) . . . . ?
C58 N7 C59 C55 0.3(9) . . . . ?
C58 N7 C59 C60 179.2(6) . . . . ?
C56 C55 C59 N7 -0.8(9) . . . . ?
C54 C55 C59 N7 178.9(6) . . . . ?
C56 C55 C59 C60 -179.6(5) . . . . ?
C54 C55 C59 C60 0.1(9) . . . . ?
C49 N6 C60 C52 -0.4(9) . . . . ?
C49 N6 C60 C59 -179.6(5) . . . . ?
C51 C52 C60 N6 1.1(9) . . . . ?
C53 C52 C60 N6 -179.3(6) . . . . ?
C51 C52 C60 C59 -179.6(6) . . . . ?
C53 C52 C60 C59 -0.1(9) . . . . ?
N7 C59 C60 N6 0.6(8) . . . . ?
C55 C59 C60 N6 179.4(5) . . . . ?
N7 C59 C60 C52 -178.7(6) . . . . ?
C55 C59 C60 C52 0.2(9) . . . . ?

_diffrn_measured_fraction_theta_max 0.975
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.975
_refine_diff_density_max         0.857
_refine_diff_density_min         -1.114
_refine_diff_density_rms         0.111
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_k
_database_code_depnum_ccdc_archive 'CCDC 1044886'
_audit_update_record             
;
2015-11-09 deposited with the CCDC.
2015-11-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C120 H114 Gd2 N16 O22'
_chemical_formula_weight         2446.77

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'
Gd Gd -0.1653 3.9035 '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

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

_cell_length_a                   13.556(3)
_cell_length_b                   14.326(3)
_cell_length_c                   16.725(3)
_cell_angle_alpha                79.75(3)
_cell_angle_beta                 71.18(3)
_cell_angle_gamma                64.16(3)
_cell_volume                     2764.3(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    10885
_cell_measurement_theta_min      3.02
_cell_measurement_theta_max      26.37

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1250
_exptl_absorpt_coefficient_mu    1.269
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6650
_exptl_absorpt_correction_T_max  0.8132
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            20994
_diffrn_reflns_av_R_equivalents  0.0927
_diffrn_reflns_av_sigmaI/netI    0.1368
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         26.37
_reflns_number_total             10885
_reflns_number_gt                8051
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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)+(0.0985P)²+1.9157P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10885
_refine_ls_number_parameters     721
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.1055
_refine_ls_R_factor_gt           0.0760
_refine_ls_wR_factor_ref         0.1965
_refine_ls_wR_factor_gt          0.1748
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.769
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O2W O 0.4812(16) 0.0693(18) 0.5089(18) 0.2650(14) Uani 1 1 d DU . .
H2WA H 0.5031 0.0749 0.4553 0.397 Uiso 1 1 d RD . .
H2WB H 0.5210 0.0089 0.5257 0.397 Uiso 1 1 d RD . .
Gd1 Gd 0.65193(3) 0.99681(3) 0.93761(3) 0.02712(11) Uani 1 1 d . . .
O1 O 0.7164(5) 1.0539(5) 0.7877(4) 0.0430(18) Uani 1 1 d . . .
O2 O 0.7281(5) 0.8947(5) 0.8084(4) 0.0380(17) Uani 1 1 d . . .
O3 O 0.6812(5) 0.9860(6) 1.0775(4) 0.054(2) Uani 1 1 d . . .
O4 O 0.5079(4) 1.0084(5) 1.0847(4) 0.0330(16) Uani 1 1 d . . .
O5 O 0.6593(4) 0.8311(5) 0.9870(4) 0.0396(17) Uani 1 1 d . . .
O7 O 0.2025(10) 0.3812(11) 0.3757(9) 0.134(6) Uani 1 1 d . . .
O8 O 0.2944(10) 0.2213(10) 0.4067(9) 0.121(5) Uani 1 1 d . . .
O9 O 0.2563(11) 0.3402(11) 0.4873(7) 0.128(5) Uani 1 1 d . . .
O1W O 0.6869(7) 0.7266(8) 0.7926(6) 0.090(3) Uani 1 1 d . . .
H1WA H 0.7075 0.7392 0.7396 0.136 Uiso 1 1 d R . .
H1WB H 0.7366 0.6699 0.8061 0.136 Uiso 1 1 d R . .
N1 N 0.7748(5) 1.0994(6) 0.9330(5) 0.037(2) Uani 1 1 d . . .
N2 N 0.8694(5) 0.8901(6) 0.9089(5) 0.0359(19) Uani 1 1 d . . .
N3 N 1.1584(7) 0.5722(8) 0.4888(6) 0.062(3) Uani 1 1 d . . .
H3A H 1.1767 0.5077 0.4833 0.074 Uiso 1 1 calc R . .
N4 N 0.7980(8) 0.5491(9) 1.3330(7) 0.077(3) Uani 1 1 d . . .
H4A H 0.8071 0.5069 1.3761 0.092 Uiso 1 1 calc R . .
N5 N 0.4977(7) 0.3310(8) 1.1773(6) 0.060(3) Uani 1 1 d . . .
H5A H 0.4559 0.2988 1.1798 0.072 Uiso 1 1 calc R . .
N6 N 0.2101(6) 0.7892(6) 0.2654(5) 0.042(2) Uani 1 1 d . . .
H6 H 0.2065 0.8509 0.2636 0.050 Uiso 1 1 calc R . .
N7 N 0.0069(6) 0.9578(7) 0.3115(5) 0.049(2) Uani 1 1 d . . .
N8 N 0.2505(8) 0.3125(9) 0.4233(8) 0.072(3) Uani 1 1 d . . .
C1 C 0.7306(8) 1.1978(7) 0.9436(7) 0.046(3) Uani 1 1 d . . .
H1A H 0.6517 1.2328 0.9554 0.055 Uiso 1 1 calc R . .
C2 C 0.7943(9) 1.2560(8) 0.9383(7) 0.059(3) Uani 1 1 d . . .
H2A H 0.7581 1.3263 0.9490 0.070 Uiso 1 1 calc R . .
C3 C 0.9095(8) 1.2063(9) 0.9171(7) 0.054(3) Uani 1 1 d . . .
H3B H 0.9539 1.2429 0.9116 0.065 Uiso 1 1 calc R . .
C4 C 0.9620(7) 1.0991(8) 0.9032(6) 0.044(3) Uani 1 1 d . . .
C5 C 1.0834(8) 1.0398(10) 0.8845(7) 0.060(3) Uani 1 1 d . . .
H5B H 1.1303 1.0733 0.8804 0.073 Uiso 1 1 calc R . .
C7 C 1.0609(6) 0.8857(9) 0.8795(6) 0.046(3) Uani 1 1 d . . .
C8 C 1.1054(8) 0.7764(11) 0.8670(8) 0.067(4) Uani 1 1 d . . .
H8A H 1.1839 0.7376 0.8527 0.080 Uiso 1 1 calc R . .
C9 C 1.0353(9) 0.7297(10) 0.8758(8) 0.066(4) Uani 1 1 d . . .
H9A H 1.0649 0.6591 0.8673 0.079 Uiso 1 1 calc R . .
C10 C 0.9154(7) 0.7892(9) 0.8982(7) 0.052(3) Uani 1 1 d . . .
H10A H 0.8675 0.7558 0.9057 0.062 Uiso 1 1 calc R . .
C11 C 0.9411(6) 0.9392(8) 0.8993(6) 0.038(2) Uani 1 1 d . . .
C12 C 0.8911(6) 1.0490(8) 0.9130(5) 0.037(2) Uani 1 1 d . . .
C6 C 1.1302(8) 0.9382(11) 0.8729(8) 0.062(4) Uani 1 1 d . . .
H6C H 1.2090 0.9019 0.8604 0.075 Uiso 1 1 calc R . .
C13 C 0.7433(7) 0.9684(7) 0.7589(6) 0.036(2) Uani 1 1 d . . .
C14 C 0.7966(9) 0.9512(9) 0.6645(6) 0.052(3) Uani 1 1 d . . .
H14A H 0.7380 0.9581 0.6397 0.062 Uiso 1 1 calc R . .
H14B H 0.8229 1.0055 0.6388 0.062 Uiso 1 1 calc R . .
C15 C 0.8956(8) 0.8468(8) 0.6428(6) 0.044(3) Uani 1 1 d . . .
H15A H 0.8688 0.7919 0.6633 0.053 Uiso 1 1 calc R . .
H15B H 0.9525 0.8368 0.6705 0.053 Uiso 1 1 calc R . .
C16 C 0.9495(10) 0.8407(10) 0.5471(7) 0.065(4) Uani 1 1 d . . .
H16A H 0.8917 0.8511 0.5202 0.077 Uiso 1 1 calc R . .
H16B H 0.9741 0.8971 0.5272 0.077 Uiso 1 1 calc R . .
C17 C 1.0503(9) 0.7395(9) 0.5192(7) 0.053(3) Uani 1 1 d U . .
C18 C 1.0510(9) 0.6451(11) 0.5178(7) 0.062(4) Uani 1 1 d U . .
H18A H 0.9858 0.6317 0.5347 0.074 Uiso 1 1 calc R . .
C19 C 1.2326(9) 0.6198(10) 0.4697(7) 0.056(3) Uani 1 1 d . . .
C20 C 1.3494(10) 0.5808(11) 0.4372(8) 0.072(5) Uani 1 1 d . . .
H20A H 1.3914 0.5104 0.4279 0.086 Uiso 1 1 calc R . .
C21 C 1.4007(11) 0.6446(17) 0.4195(11) 0.108(7) Uani 1 1 d . . .
H21A H 1.4793 0.6191 0.3960 0.129 Uiso 1 1 calc R . .
C22 C 1.3380(11) 0.7510(14) 0.4357(10) 0.092(5) Uani 1 1 d . . .
H22A H 1.3759 0.7948 0.4225 0.110 Uiso 1 1 calc R . .
C23 C 1.2204(10) 0.7914(11) 0.4711(7) 0.068(4) Uani 1 1 d . . .
H23A H 1.1792 0.8613 0.4827 0.082 Uiso 1 1 calc R . .
C24 C 1.1664(9) 0.7237(9) 0.4887(6) 0.050(3) Uani 1 1 d . . .
C25 C 0.5834(6) 0.9940(8) 1.1198(5) 0.036(2) Uani 1 1 d . . .
C26 C 0.5567(8) 0.9836(10) 1.2149(6) 0.056(3) Uani 1 1 d . . .
H26A H 0.4791 0.9888 1.2384 0.067 Uiso 1 1 calc R . .
H26B H 0.5611 1.0407 1.2351 0.067 Uiso 1 1 calc R . .
C27 C 0.6380(9) 0.8809(12) 1.2466(7) 0.071(4) Uani 1 1 d . . .
H27A H 0.7156 0.8748 1.2209 0.085 Uiso 1 1 calc R . .
H27B H 0.6224 0.8827 1.3072 0.085 Uiso 1 1 calc R . .
C28 C 0.6296(9) 0.7859(12) 1.2279(9) 0.080(4) Uani 1 1 d . . .
H28A H 0.5531 0.7901 1.2563 0.096 Uiso 1 1 calc R . .
H28B H 0.6409 0.7861 1.1676 0.096 Uiso 1 1 calc R . .
C29 C 0.7136(9) 0.6853(12) 1.2547(7) 0.068(4) Uani 1 1 d . . .
C30 C 0.7037(10) 0.6349(13) 1.3305(8) 0.081(5) Uani 1 1 d . . .
H30A H 0.6388 0.6569 1.3760 0.097 Uiso 1 1 calc R . .
C31 C 0.8765(9) 0.5395(10) 1.2572(8) 0.065(3) Uani 1 1 d . . .
C32 C 0.9874(13) 0.4670(13) 1.2299(11) 0.098(5) Uani 1 1 d . . .
H32A H 1.0207 0.4115 1.2646 0.117 Uiso 1 1 calc R . .
C33 C 1.0437(15) 0.4821(15) 1.1498(12) 0.119(7) Uani 1 1 d . . .
H33A H 1.1188 0.4349 1.1299 0.143 Uiso 1 1 calc R . .
C34 C 0.9991(14) 0.5623(14) 1.0943(11) 0.107(6) Uani 1 1 d . . .
H34A H 1.0426 0.5677 1.0393 0.128 Uiso 1 1 calc R . .
C35 C 0.8905(11) 0.6326(12) 1.1226(9) 0.081(4) Uani 1 1 d . . .
H35A H 0.8587 0.6875 1.0869 0.097 Uiso 1 1 calc R . .
C36 C 0.8260(8) 0.6229(9) 1.2055(7) 0.054(3) Uani 1 1 d . . .
C37 C 0.5939(6) 0.7858(7) 1.0191(5) 0.032(2) Uani 1 1 d . . .
C38 C 0.6521(7) 0.6677(7) 1.0158(7) 0.044(3) Uani 1 1 d . . .
H38A H 0.6592 0.6490 0.9606 0.053 Uiso 1 1 calc R . .
H38B H 0.7286 0.6454 1.0205 0.053 Uiso 1 1 calc R . .
C39 C 0.5947(7) 0.6080(7) 1.0815(6) 0.039(3) Uani 1 1 d . . .
H39A H 0.5165 0.6318 1.0800 0.047 Uiso 1 1 calc R . .
H39B H 0.5936 0.6201 1.1371 0.047 Uiso 1 1 calc R . .
C40 C 0.6573(8) 0.4932(8) 1.0657(8) 0.053(3) Uani 1 1 d . . .
H40A H 0.7340 0.4697 1.0705 0.064 Uiso 1 1 calc R . .
H40B H 0.6636 0.4829 1.0081 0.064 Uiso 1 1 calc R . .
C41 C 0.6004(8) 0.4258(8) 1.1260(7) 0.050(3) Uani 1 1 d . . .
C42 C 0.5353(8) 0.3876(9) 1.1082(7) 0.051(3) Uani 1 1 d . . .
H42A H 0.5183 0.3980 1.0569 0.061 Uiso 1 1 calc R . .
C43 C 0.5381(8) 0.3350(8) 1.2406(7) 0.049(3) Uani 1 1 d . . .
C44 C 0.5246(10) 0.2901(10) 1.3222(8) 0.067(4) Uani 1 1 d . . .
H44A H 0.4804 0.2517 1.3411 0.080 Uiso 1 1 calc R . .
C45 C 0.5759(11) 0.3027(11) 1.3731(9) 0.076(5) Uani 1 1 d . . .
H45A H 0.5700 0.2706 1.4268 0.091 Uiso 1 1 calc R . .
C46 C 0.6404(10) 0.3659(11) 1.3446(8) 0.075(4) Uani 1 1 d . . .
H46A H 0.6729 0.3767 1.3814 0.090 Uiso 1 1 calc R . .
C47 C 0.6547(8) 0.4102(9) 1.2650(8) 0.056(3) Uani 1 1 d . . .
H47A H 0.6974 0.4500 1.2470 0.068 Uiso 1 1 calc R . .
C48 C 0.6038(7) 0.3945(8) 1.2105(7) 0.046(3) Uani 1 1 d . . .
C49 C 0.3124(9) 0.7121(9) 0.2416(7) 0.055(3) Uani 1 1 d . . .
H49A H 0.3775 0.7257 0.2225 0.065 Uiso 1 1 calc R . .
C50 C 0.3214(10) 0.6122(10) 0.2455(8) 0.065(4) Uani 1 1 d . . .
H50A H 0.3929 0.5577 0.2312 0.078 Uiso 1 1 calc R . .
C51 C 0.2265(11) 0.5932(10) 0.2699(8) 0.067(4) Uani 1 1 d . . .
H51A H 0.2326 0.5258 0.2709 0.080 Uiso 1 1 calc R . .
C52 C 0.1182(9) 0.6754(9) 0.2940(7) 0.053(3) Uani 1 1 d . . .
C53 C 0.0129(10) 0.6616(11) 0.3220(8) 0.071(4) Uani 1 1 d . . .
H53A H 0.0147 0.5954 0.3255 0.085 Uiso 1 1 calc R . .
C54 C -0.0870(9) 0.7429(10) 0.3428(8) 0.065(3) Uani 1 1 d . . .
H54A H -0.1537 0.7321 0.3587 0.078 Uiso 1 1 calc R . .
C55 C -0.0948(8) 0.8447(10) 0.3414(7) 0.055(3) Uani 1 1 d . . .
C56 C -0.1973(9) 0.9291(12) 0.3643(8) 0.071(4) Uani 1 1 d . . .
H56A H -0.2656 0.9208 0.3820 0.085 Uiso 1 1 calc R . .
C57 C -0.1975(10) 1.0274(13) 0.3606(9) 0.078(5) Uani 1 1 d . . .
H57A H -0.2657 1.0853 0.3760 0.094 Uiso 1 1 calc R . .
C58 C -0.0937(9) 1.0371(10) 0.3333(8) 0.061(4) Uani 1 1 d . . .
H58A H -0.0950 1.1031 0.3302 0.073 Uiso 1 1 calc R . .
C59 C 0.0058(8) 0.8622(8) 0.3153(6) 0.043(3) Uani 1 1 d . . .
C60 C 0.1116(8) 0.7760(8) 0.2922(6) 0.043(3) Uani 1 1 d . . .
O6 O 0.4875(4) 0.8288(5) 1.0489(4) 0.0372(16) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O2W H2WB 0.8501 . ?
O2W H2WA 0.8500 . ?
O2W H2WB 0.8501 . ?
Gd1 O5 2.340(7) . ?
Gd1 O4 2.347(6) 2_677 ?
Gd1 O6 2.382(5) 2_677 ?
Gd1 O3 2.465(7) . ?
Gd1 O1 2.490(6) . ?
Gd1 O2 2.499(6) . ?
Gd1 O4 2.581(5) . ?
Gd1 N2 2.584(6) . ?
Gd1 N1 2.636(9) . ?
Gd1 Gd1 3.9401(15) 2_677 ?
O1 C13 1.254(12) . ?
O2 C13 1.269(12) . ?
O3 C25 1.250(10) . ?
O4 C25 1.263(11) . ?
O4 Gd1 2.347(6) 2_677 ?
O5 C37 1.253(12) . ?
O7 N8 1.233(17) . ?
O8 N8 1.219(16) . ?
O9 N8 1.241(17) . ?
O1W H1WA 0.8499 . ?
O1W H1WB 0.8500 . ?
N1 C1 1.289(12) . ?
N1 C12 1.368(10) . ?
N2 C10 1.320(13) . ?
N2 C11 1.386(13) . ?
N3 C18 1.358(13) . ?
N3 C19 1.376(17) . ?
N3 H3A 0.8600 . ?
N4 C30 1.339(16) . ?
N4 C31 1.351(15) . ?
N4 H4A 0.8600 . ?
N5 C43 1.360(16) . ?
N5 C42 1.379(15) . ?
N5 H5A 0.8600 . ?
N6 C49 1.329(12) . ?
N6 C60 1.350(13) . ?
N6 H6 0.8600 . ?
N7 C58 1.327(12) . ?
N7 C59 1.365(15) . ?
C1 C2 1.414(16) . ?
C1 H1A 0.9300 . ?
C2 C3 1.355(14) . ?
C2 H2A 0.9300 . ?
C3 C4 1.410(15) . ?
C3 H3B 0.9300 . ?
C4 C12 1.386(15) . ?
C4 C5 1.440(12) . ?
C5 C6 1.332(19) . ?
C5 H5B 0.9300 . ?
C7 C6 1.408(18) . ?
C7 C11 1.412(10) . ?
C7 C8 1.438(18) . ?
C8 C9 1.34(2) . ?
C8 H8A 0.9300 . ?
C9 C10 1.422(13) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
C11 C12 1.444(14) . ?
C6 H6C 0.9300 . ?
C13 C14 1.524(13) . ?
C14 C15 1.516(13) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.531(14) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.513(14) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.352(19) . ?
C17 C24 1.415(16) . ?
C18 H18A 0.9300 . ?
C19 C20 1.376(15) . ?
C19 C24 1.393(16) . ?
C20 C21 1.32(3) . ?
C20 H20A 0.9300 . ?
C21 C22 1.41(3) . ?
C21 H21A 0.9300 . ?
C22 C23 1.392(17) . ?
C22 H22A 0.9300 . ?
C23 C24 1.393(19) . ?
C23 H23A 0.9300 . ?
C25 C26 1.508(13) . ?
C26 C27 1.532(17) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.51(2) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C29 1.498(18) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.339(18) . ?
C29 C36 1.437(14) . ?
C30 H30A 0.9300 . ?
C31 C32 1.382(17) . ?
C31 C36 1.394(17) . ?
C32 C33 1.34(2) . ?
C32 H32A 0.9300 . ?
C33 C34 1.39(3) . ?
C33 H33A 0.9300 . ?
C34 C35 1.354(19) . ?
C34 H34A 0.9300 . ?
C35 C36 1.401(17) . ?
C35 H35A 0.9300 . ?
C37 O6 1.257(9) . ?
C37 C38 1.526(13) . ?
C38 C39 1.496(14) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 C40 1.513(13) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 C41 1.531(16) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 C42 1.347(18) . ?
C41 C48 1.414(16) . ?
C42 H42A 0.9300 . ?
C43 C44 1.393(17) . ?
C43 C48 1.412(16) . ?
C44 C45 1.34(2) . ?
C44 H44A 0.9300 . ?
C45 C46 1.44(2) . ?
C45 H45A 0.9300 . ?
C46 C47 1.361(18) . ?
C46 H46A 0.9300 . ?
C47 C48 1.404(17) . ?
C47 H47A 0.9300 . ?
C49 C50 1.373(18) . ?
C49 H49A 0.9300 . ?
C50 C51 1.350(19) . ?
C50 H50A 0.9300 . ?
C51 C52 1.408(15) . ?
C51 H51A 0.9300 . ?
C52 C60 1.401(16) . ?
C52 C53 1.441(17) . ?
C53 C54 1.333(16) . ?
C53 H53A 0.9300 . ?
C54 C55 1.413(19) . ?
C54 H54A 0.9300 . ?
C55 C56 1.377(15) . ?
C55 C59 1.411(15) . ?
C56 C57 1.40(2) . ?
C56 H56A 0.9300 . ?
C57 C58 1.393(19) . ?
C57 H57A 0.9300 . ?
C58 H58A 0.9300 . ?
C59 C60 1.413(12) . ?
O6 Gd1 2.382(5) 2_677 ?

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
H2WB O2W H2WA 109.5 . . ?
H2WB O2W H2WB 0.0 . . ?
H2WA O2W H2WB 109.5 . . ?
O5 Gd1 O4 74.7(2) . 2_677 ?
O5 Gd1 O6 137.3(2) . 2_677 ?
O4 Gd1 O6 75.2(2) 2_677 2_677 ?
O5 Gd1 O3 79.1(3) . . ?
O4 Gd1 O3 124.7(2) 2_677 . ?
O6 Gd1 O3 94.0(2) 2_677 . ?
O5 Gd1 O1 126.5(2) . . ?
O4 Gd1 O1 91.9(2) 2_677 . ?
O6 Gd1 O1 84.1(2) 2_677 . ?
O3 Gd1 O1 141.7(3) . . ?
O5 Gd1 O2 74.5(2) . . ?
O4 Gd1 O2 74.8(2) 2_677 . ?
O6 Gd1 O2 124.7(2) 2_677 . ?
O3 Gd1 O2 141.1(2) . . ?
O1 Gd1 O2 52.0(2) . . ?
O5 Gd1 O4 70.5(2) . . ?
O4 Gd1 O4 73.9(2) 2_677 . ?
O6 Gd1 O4 72.4(2) 2_677 . ?
O3 Gd1 O4 51.49(19) . . ?
O1 Gd1 O4 154.87(18) . . ?
O2 Gd1 O4 137.8(2) . . ?
O5 Gd1 N2 78.9(2) . . ?
O4 Gd1 N2 140.1(2) 2_677 . ?
O6 Gd1 N2 141.2(3) 2_677 . ?
O3 Gd1 N2 77.7(2) . . ?
O1 Gd1 N2 80.2(2) . . ?
O2 Gd1 N2 69.6(2) . . ?
O4 Gd1 N2 123.9(2) . . ?
O5 Gd1 N1 134.9(2) . . ?
O4 Gd1 N1 150.3(2) 2_677 . ?
O6 Gd1 N1 78.0(2) 2_677 . ?
O3 Gd1 N1 69.7(3) . . ?
O1 Gd1 N1 72.5(2) . . ?
O2 Gd1 N1 111.3(2) . . ?
O4 Gd1 N1 109.9(2) . . ?
N2 Gd1 N1 63.5(2) . . ?
O5 Gd1 Gd1 67.95(13) . 2_677 ?
O4 Gd1 Gd1 39.00(13) 2_677 2_677 ?
O6 Gd1 Gd1 69.53(16) 2_677 2_677 ?
O3 Gd1 Gd1 86.07(15) . 2_677 ?
O1 Gd1 Gd1 127.78(15) . 2_677 ?
O2 Gd1 Gd1 109.20(15) . 2_677 ?
O4 Gd1 Gd1 34.93(14) . 2_677 ?
N2 Gd1 Gd1 145.36(18) . 2_677 ?
N1 Gd1 Gd1 137.77(15) . 2_677 ?
C13 O1 Gd1 94.3(6) . . ?
C13 O2 Gd1 93.5(6) . . ?
C25 O3 Gd1 96.3(6) . . ?
C25 O4 Gd1 160.1(6) . 2_677 ?
C25 O4 Gd1 90.5(4) . . ?
Gd1 O4 Gd1 106.1(2) 2_677 . ?
C37 O5 Gd1 140.0(5) . . ?
H1WA O1W H1WB 109.5 . . ?
C1 N1 C12 117.5(9) . . ?
C1 N1 Gd1 122.7(6) . . ?
C12 N1 Gd1 119.6(6) . . ?
C10 N2 C11 118.5(7) . . ?
C10 N2 Gd1 121.2(7) . . ?
C11 N2 Gd1 120.2(5) . . ?
C18 N3 C19 108.0(11) . . ?
C18 N3 H3A 126.0 . . ?
C19 N3 H3A 126.0 . . ?
C30 N4 C31 109.3(11) . . ?
C30 N4 H4A 125.4 . . ?
C31 N4 H4A 125.4 . . ?
C43 N5 C42 108.0(11) . . ?
C43 N5 H5A 126.0 . . ?
C42 N5 H5A 126.0 . . ?
C49 N6 C60 123.7(10) . . ?
C49 N6 H6 118.2 . . ?
C60 N6 H6 118.2 . . ?
C58 N7 C59 116.6(10) . . ?
O8 N8 O7 121.4(15) . . ?
O8 N8 O9 121.1(14) . . ?
O7 N8 O9 117.4(14) . . ?
N1 C1 C2 124.3(9) . . ?
N1 C1 H1A 117.9 . . ?
C2 C1 H1A 117.9 . . ?
C3 C2 C1 118.1(10) . . ?
C3 C2 H2A 121.0 . . ?
C1 C2 H2A 121.0 . . ?
C2 C3 C4 119.7(11) . . ?
C2 C3 H3B 120.1 . . ?
C4 C3 H3B 120.1 . . ?
C12 C4 C3 117.3(8) . . ?
C12 C4 C5 119.6(10) . . ?
C3 C4 C5 123.1(11) . . ?
C6 C5 C4 121.6(12) . . ?
C6 C5 H5B 119.2 . . ?
C4 C5 H5B 119.2 . . ?
C6 C7 C11 120.7(10) . . ?
C6 C7 C8 123.3(8) . . ?
C11 C7 C8 115.9(10) . . ?
C9 C8 C7 120.9(9) . . ?
C9 C8 H8A 119.5 . . ?
C7 C8 H8A 119.5 . . ?
C8 C9 C10 119.3(12) . . ?
C8 C9 H9A 120.3 . . ?
C10 C9 H9A 120.3 . . ?
N2 C10 C9 122.6(11) . . ?
N2 C10 H10A 118.7 . . ?
C9 C10 H10A 118.7 . . ?
N2 C11 C7 122.7(9) . . ?
N2 C11 C12 118.7(7) . . ?
C7 C11 C12 118.6(10) . . ?
N1 C12 C4 123.1(9) . . ?
N1 C12 C11 117.7(9) . . ?
C4 C12 C11 119.2(7) . . ?
C5 C6 C7 120.3(9) . . ?
C5 C6 H6C 119.9 . . ?
C7 C6 H6C 119.9 . . ?
O1 C13 O2 120.2(8) . . ?
O1 C13 C14 120.4(9) . . ?
O2 C13 C14 119.4(9) . . ?
C15 C14 C13 114.6(8) . . ?
C15 C14 H14A 108.6 . . ?
C13 C14 H14A 108.6 . . ?
C15 C14 H14B 108.6 . . ?
C13 C14 H14B 108.6 . . ?
H14A C14 H14B 107.6 . . ?
C14 C15 C16 110.6(8) . . ?
C14 C15 H15A 109.5 . . ?
C16 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C16 C15 H15B 109.5 . . ?
H15A C15 H15B 108.1 . . ?
C17 C16 C15 114.5(9) . . ?
C17 C16 H16A 108.6 . . ?
C15 C16 H16A 108.6 . . ?
C17 C16 H16B 108.6 . . ?
C15 C16 H16B 108.6 . . ?
H16A C16 H16B 107.6 . . ?
C18 C17 C24 104.7(9) . . ?
C18 C17 C16 128.7(11) . . ?
C24 C17 C16 126.6(12) . . ?
C17 C18 N3 111.9(11) . . ?
C17 C18 H18A 124.1 . . ?
N3 C18 H18A 124.1 . . ?
N3 C19 C20 130.8(12) . . ?
N3 C19 C24 106.5(9) . . ?
C20 C19 C24 122.7(14) . . ?
C21 C20 C19 119.1(14) . . ?
C21 C20 H20A 120.4 . . ?
C19 C20 H20A 120.4 . . ?
C20 C21 C22 120.8(13) . . ?
C20 C21 H21A 119.6 . . ?
C22 C21 H21A 119.6 . . ?
C23 C22 C21 120.9(16) . . ?
C23 C22 H22A 119.5 . . ?
C21 C22 H22A 119.5 . . ?
C22 C23 C24 117.9(13) . . ?
C22 C23 H23A 121.1 . . ?
C24 C23 H23A 121.1 . . ?
C19 C24 C23 118.5(10) . . ?
C19 C24 C17 109.0(12) . . ?
C23 C24 C17 132.4(11) . . ?
O3 C25 O4 121.7(8) . . ?
O3 C25 C26 118.7(8) . . ?
O4 C25 C26 119.6(8) . . ?
C25 C26 C27 112.8(8) . . ?
C25 C26 H26A 109.0 . . ?
C27 C26 H26A 109.0 . . ?
C25 C26 H26B 109.0 . . ?
C27 C26 H26B 109.0 . . ?
H26A C26 H26B 107.8 . . ?
C28 C27 C26 114.4(11) . . ?
C28 C27 H27A 108.7 . . ?
C26 C27 H27A 108.7 . . ?
C28 C27 H27B 108.7 . . ?
C26 C27 H27B 108.7 . . ?
H27A C27 H27B 107.6 . . ?
C29 C28 C27 114.3(11) . . ?
C29 C28 H28A 108.7 . . ?
C27 C28 H28A 108.7 . . ?
C29 C28 H28B 108.7 . . ?
C27 C28 H28B 108.7 . . ?
H28A C28 H28B 107.6 . . ?
C30 C29 C36 104.0(11) . . ?
C30 C29 C28 128.4(11) . . ?
C36 C29 C28 127.5(11) . . ?
N4 C30 C29 112.2(11) . . ?
N4 C30 H30A 123.9 . . ?
C29 C30 H30A 123.9 . . ?
N4 C31 C32 130.9(13) . . ?
N4 C31 C36 106.4(9) . . ?
C32 C31 C36 122.6(12) . . ?
C33 C32 C31 115.4(15) . . ?
C33 C32 H32A 122.3 . . ?
C31 C32 H32A 122.3 . . ?
C32 C33 C34 125.3(15) . . ?
C32 C33 H33A 117.3 . . ?
C34 C33 H33A 117.3 . . ?
C35 C34 C33 118.1(16) . . ?
C35 C34 H34A 120.9 . . ?
C33 C34 H34A 120.9 . . ?
C34 C35 C36 120.2(14) . . ?
C34 C35 H35A 119.9 . . ?
C36 C35 H35A 119.9 . . ?
C31 C36 C35 118.3(10) . . ?
C31 C36 C29 108.1(10) . . ?
C35 C36 C29 133.6(12) . . ?
O5 C37 O6 126.0(9) . . ?
O5 C37 C38 114.7(7) . . ?
O6 C37 C38 119.2(9) . . ?
C39 C38 C37 116.6(7) . . ?
C39 C38 H38A 108.1 . . ?
C37 C38 H38A 108.1 . . ?
C39 C38 H38B 108.1 . . ?
C37 C38 H38B 108.1 . . ?
H38A C38 H38B 107.3 . . ?
C38 C39 C40 110.3(7) . . ?
C38 C39 H39A 109.6 . . ?
C40 C39 H39A 109.6 . . ?
C38 C39 H39B 109.6 . . ?
C40 C39 H39B 109.6 . . ?
H39A C39 H39B 108.1 . . ?
C39 C40 C41 114.3(8) . . ?
C39 C40 H40A 108.7 . . ?
C41 C40 H40A 108.7 . . ?
C39 C40 H40B 108.7 . . ?
C41 C40 H40B 108.7 . . ?
H40A C40 H40B 107.6 . . ?
C42 C41 C48 107.6(10) . . ?
C42 C41 C40 125.6(11) . . ?
C48 C41 C40 126.8(12) . . ?
C41 C42 N5 110.0(11) . . ?
C41 C42 H42A 125.0 . . ?
N5 C42 H42A 125.0 . . ?
N5 C43 C44 130.2(12) . . ?
N5 C43 C48 108.3(10) . . ?
C44 C43 C48 121.5(12) . . ?
C45 C44 C43 119.3(14) . . ?
C45 C44 H44A 120.3 . . ?
C43 C44 H44A 120.3 . . ?
C44 C45 C46 120.0(13) . . ?
C44 C45 H45A 120.0 . . ?
C46 C45 H45A 120.0 . . ?
C47 C46 C45 121.4(14) . . ?
C47 C46 H46A 119.3 . . ?
C45 C46 H46A 119.3 . . ?
C46 C47 C48 118.6(13) . . ?
C46 C47 H47A 120.7 . . ?
C48 C47 H47A 120.7 . . ?
C47 C48 C43 119.0(10) . . ?
C47 C48 C41 134.8(12) . . ?
C43 C48 C41 106.2(11) . . ?
N6 C49 C50 119.6(11) . . ?
N6 C49 H49A 120.2 . . ?
C50 C49 H49A 120.2 . . ?
C51 C50 C49 120.1(10) . . ?
C51 C50 H50A 120.0 . . ?
C49 C50 H50A 120.0 . . ?
C50 C51 C52 120.1(12) . . ?
C50 C51 H51A 120.0 . . ?
C52 C51 H51A 120.0 . . ?
C60 C52 C51 118.7(11) . . ?
C60 C52 C53 117.7(10) . . ?
C51 C52 C53 123.6(12) . . ?
C54 C53 C52 120.6(13) . . ?
C54 C53 H53A 119.7 . . ?
C52 C53 H53A 119.7 . . ?
C53 C54 C55 122.2(12) . . ?
C53 C54 H54A 118.9 . . ?
C55 C54 H54A 118.9 . . ?
C56 C55 C59 117.8(12) . . ?
C56 C55 C54 122.9(11) . . ?
C59 C55 C54 119.3(9) . . ?
C55 C56 C57 119.2(12) . . ?
C55 C56 H56A 120.4 . . ?
C57 C56 H56A 120.4 . . ?
C58 C57 C56 118.9(11) . . ?
C58 C57 H57A 120.5 . . ?
C56 C57 H57A 120.5 . . ?
N7 C58 C57 123.9(14) . . ?
N7 C58 H58A 118.1 . . ?
C57 C58 H58A 118.1 . . ?
N7 C59 C55 123.6(9) . . ?
N7 C59 C60 118.1(9) . . ?
C55 C59 C60 118.3(11) . . ?
N6 C60 C52 117.8(8) . . ?
N6 C60 C59 120.4(10) . . ?
C52 C60 C59 121.8(10) . . ?
C37 O6 Gd1 135.6(6) . 2_677 ?

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
O5 Gd1 O1 C13 2.6(6) . . . . ?
O4 Gd1 O1 C13 -69.7(5) 2_677 . . . ?
O6 Gd1 O1 C13 -144.7(5) 2_677 . . . ?
O3 Gd1 O1 C13 126.4(6) . . . . ?
O2 Gd1 O1 C13 -0.8(5) . . . . ?
O4 Gd1 O1 C13 -124.1(6) . . . . ?
N2 Gd1 O1 C13 70.9(5) . . . . ?
N1 Gd1 O1 C13 136.0(5) . . . . ?
Gd1 Gd1 O1 C13 -86.4(5) 2_677 . . . ?
O5 Gd1 O2 C13 -176.4(5) . . . . ?
O4 Gd1 O2 C13 105.6(5) 2_677 . . . ?
O6 Gd1 O2 C13 46.3(6) 2_677 . . . ?
O3 Gd1 O2 C13 -127.4(5) . . . . ?
O1 Gd1 O2 C13 0.8(5) . . . . ?
O4 Gd1 O2 C13 148.9(5) . . . . ?
N2 Gd1 O2 C13 -92.7(5) . . . . ?
N1 Gd1 O2 C13 -43.7(5) . . . . ?
Gd1 Gd1 O2 C13 124.2(5) 2_677 . . . ?
O5 Gd1 O3 C25 -72.0(6) . . . . ?
O4 Gd1 O3 C25 -9.4(8) 2_677 . . . ?
O6 Gd1 O3 C25 65.4(7) 2_677 . . . ?
O1 Gd1 O3 C25 151.0(6) . . . . ?
O2 Gd1 O3 C25 -119.8(6) . . . . ?
O4 Gd1 O3 C25 1.7(6) . . . . ?
N2 Gd1 O3 C25 -152.9(7) . . . . ?
N1 Gd1 O3 C25 141.1(7) . . . . ?
Gd1 Gd1 O3 C25 -3.7(6) 2_677 . . . ?
O5 Gd1 O4 C25 89.7(6) . . . . ?
O4 Gd1 O4 C25 168.8(7) 2_677 . . . ?
O6 Gd1 O4 C25 -111.9(6) 2_677 . . . ?
O3 Gd1 O4 C25 -1.7(6) . . . . ?
O1 Gd1 O4 C25 -133.4(7) . . . . ?
O2 Gd1 O4 C25 125.3(6) . . . . ?
N2 Gd1 O4 C25 28.6(7) . . . . ?
N1 Gd1 O4 C25 -42.2(6) . . . . ?
Gd1 Gd1 O4 C25 168.8(7) 2_677 . . . ?
O5 Gd1 O4 Gd1 -79.1(3) . . . 2_677 ?
O4 Gd1 O4 Gd1 -0.001(2) 2_677 . . 2_677 ?
O6 Gd1 O4 Gd1 79.2(3) 2_677 . . 2_677 ?
O3 Gd1 O4 Gd1 -170.5(4) . . . 2_677 ?
O1 Gd1 O4 Gd1 57.8(6) . . . 2_677 ?
O2 Gd1 O4 Gd1 -43.5(4) . . . 2_677 ?
N2 Gd1 O4 Gd1 -140.2(3) . . . 2_677 ?
N1 Gd1 O4 Gd1 149.0(2) . . . 2_677 ?
O4 Gd1 O5 C37 -29.4(9) 2_677 . . . ?
O6 Gd1 O5 C37 17.4(11) 2_677 . . . ?
O3 Gd1 O5 C37 101.5(9) . . . . ?
O1 Gd1 O5 C37 -110.2(9) . . . . ?
O2 Gd1 O5 C37 -107.4(10) . . . . ?
O4 Gd1 O5 C37 48.6(9) . . . . ?
N2 Gd1 O5 C37 -179.1(10) . . . . ?
N1 Gd1 O5 C37 147.7(9) . . . . ?
Gd1 Gd1 O5 C37 11.3(9) 2_677 . . . ?
O5 Gd1 N1 C1 -143.7(7) . . . . ?
O4 Gd1 N1 C1 30.5(10) 2_677 . . . ?
O6 Gd1 N1 C1 4.3(8) 2_677 . . . ?
O3 Gd1 N1 C1 -94.6(8) . . . . ?
O1 Gd1 N1 C1 91.8(8) . . . . ?
O2 Gd1 N1 C1 127.1(8) . . . . ?
O4 Gd1 N1 C1 -61.8(8) . . . . ?
N2 Gd1 N1 C1 179.3(9) . . . . ?
Gd1 Gd1 N1 C1 -35.8(9) 2_677 . . . ?
O5 Gd1 N1 C12 40.9(7) . . . . ?
O4 Gd1 N1 C12 -144.8(6) 2_677 . . . ?
O6 Gd1 N1 C12 -171.1(7) 2_677 . . . ?
O3 Gd1 N1 C12 90.0(6) . . . . ?
O1 Gd1 N1 C12 -83.6(6) . . . . ?
O2 Gd1 N1 C12 -48.2(7) . . . . ?
O4 Gd1 N1 C12 122.8(6) . . . . ?
N2 Gd1 N1 C12 4.0(6) . . . . ?
Gd1 Gd1 N1 C12 148.9(5) 2_677 . . . ?
O5 Gd1 N2 C10 24.8(8) . . . . ?
O4 Gd1 N2 C10 -24.5(9) 2_677 . . . ?
O6 Gd1 N2 C10 -173.1(7) 2_677 . . . ?
O3 Gd1 N2 C10 105.9(8) . . . . ?
O1 Gd1 N2 C10 -105.6(8) . . . . ?
O2 Gd1 N2 C10 -52.6(8) . . . . ?
O4 Gd1 N2 C10 82.1(8) . . . . ?
N1 Gd1 N2 C10 179.1(8) . . . . ?
Gd1 Gd1 N2 C10 42.0(9) 2_677 . . . ?
O5 Gd1 N2 C11 -159.0(7) . . . . ?
O4 Gd1 N2 C11 151.7(6) 2_677 . . . ?
O6 Gd1 N2 C11 3.0(8) 2_677 . . . ?
O3 Gd1 N2 C11 -78.0(7) . . . . ?
O1 Gd1 N2 C11 70.6(7) . . . . ?
O2 Gd1 N2 C11 123.5(7) . . . . ?
O4 Gd1 N2 C11 -101.8(7) . . . . ?
N1 Gd1 N2 C11 -4.7(6) . . . . ?
Gd1 Gd1 N2 C11 -141.9(5) 2_677 . . . ?
C12 N1 C1 C2 -2.0(16) . . . . ?
Gd1 N1 C1 C2 -177.5(8) . . . . ?
N1 C1 C2 C3 3.1(18) . . . . ?
C1 C2 C3 C4 -1.7(17) . . . . ?
C2 C3 C4 C12 -0.5(15) . . . . ?
C2 C3 C4 C5 -176.9(11) . . . . ?
C12 C4 C5 C6 2.7(16) . . . . ?
C3 C4 C5 C6 179.1(11) . . . . ?
C6 C7 C8 C9 178.6(12) . . . . ?
C11 C7 C8 C9 -1.3(17) . . . . ?
C7 C8 C9 C10 -0.4(19) . . . . ?
C11 N2 C10 C9 -1.2(16) . . . . ?
Gd1 N2 C10 C9 175.0(9) . . . . ?
C8 C9 C10 N2 1.8(19) . . . . ?
C10 N2 C11 C7 -0.6(14) . . . . ?
Gd1 N2 C11 C7 -176.9(7) . . . . ?
C10 N2 C11 C12 -178.4(9) . . . . ?
Gd1 N2 C11 C12 5.3(11) . . . . ?
C6 C7 C11 N2 -178.0(10) . . . . ?
C8 C7 C11 N2 1.9(14) . . . . ?
C6 C7 C11 C12 -0.2(14) . . . . ?
C8 C7 C11 C12 179.7(9) . . . . ?
C1 N1 C12 C4 -0.4(14) . . . . ?
Gd1 N1 C12 C4 175.2(7) . . . . ?
C1 N1 C12 C11 -178.7(9) . . . . ?
Gd1 N1 C12 C11 -3.1(10) . . . . ?
C3 C4 C12 N1 1.6(14) . . . . ?
C5 C4 C12 N1 178.2(9) . . . . ?
C3 C4 C12 C11 179.9(9) . . . . ?
C5 C4 C12 C11 -3.5(14) . . . . ?
N2 C11 C12 N1 -1.4(13) . . . . ?
C7 C11 C12 N1 -179.3(8) . . . . ?
N2 C11 C12 C4 -179.8(8) . . . . ?
C7 C11 C12 C4 2.4(13) . . . . ?
C4 C5 C6 C7 -0.5(18) . . . . ?
C11 C7 C6 C5 -0.7(17) . . . . ?
C8 C7 C6 C5 179.4(11) . . . . ?
Gd1 O1 C13 O2 1.4(9) . . . . ?
Gd1 O1 C13 C14 -177.3(8) . . . . ?
Gd1 O2 C13 O1 -1.4(9) . . . . ?
Gd1 O2 C13 C14 177.4(8) . . . . ?
O1 C13 C14 C15 137.3(10) . . . . ?
O2 C13 C14 C15 -41.4(14) . . . . ?
C13 C14 C15 C16 -175.2(11) . . . . ?
C14 C15 C16 C17 179.3(12) . . . . ?
C15 C16 C17 C18 72.9(18) . . . . ?
C15 C16 C17 C24 -106.9(14) . . . . ?
C24 C17 C18 N3 0.0(13) . . . . ?
C16 C17 C18 N3 -179.8(11) . . . . ?
C19 N3 C18 C17 -0.2(13) . . . . ?
C18 N3 C19 C20 -178.8(13) . . . . ?
C18 N3 C19 C24 0.3(12) . . . . ?
N3 C19 C20 C21 175.8(14) . . . . ?
C24 C19 C20 C21 -3(2) . . . . ?
C19 C20 C21 C22 2(2) . . . . ?
C20 C21 C22 C23 0(3) . . . . ?
C21 C22 C23 C24 -1(2) . . . . ?
N3 C19 C24 C23 -176.9(10) . . . . ?
C20 C19 C24 C23 2.3(17) . . . . ?
N3 C19 C24 C17 -0.3(12) . . . . ?
C20 C19 C24 C17 178.9(11) . . . . ?
C22 C23 C24 C19 -0.2(17) . . . . ?
C22 C23 C24 C17 -175.7(13) . . . . ?
C18 C17 C24 C19 0.2(12) . . . . ?
C16 C17 C24 C19 -180.0(11) . . . . ?
C18 C17 C24 C23 176.1(12) . . . . ?
C16 C17 C24 C23 -4.1(19) . . . . ?
Gd1 O3 C25 O4 -3.3(11) . . . . ?
Gd1 O3 C25 C26 175.4(9) . . . . ?
Gd1 O4 C25 O3 149.9(12) 2_677 . . . ?
Gd1 O4 C25 O3 3.1(10) . . . . ?
Gd1 O4 C25 C26 -29(2) 2_677 . . . ?
Gd1 O4 C25 C26 -175.5(9) . . . . ?
O3 C25 C26 C27 -56.4(15) . . . . ?
O4 C25 C26 C27 122.2(11) . . . . ?
C25 C26 C27 C28 -65.4(13) . . . . ?
C26 C27 C28 C29 176.8(9) . . . . ?
C27 C28 C29 C30 86.1(19) . . . . ?
C27 C28 C29 C36 -90.8(17) . . . . ?
C31 N4 C30 C29 0.4(19) . . . . ?
C36 C29 C30 N4 0.5(18) . . . . ?
C28 C29 C30 N4 -177.0(15) . . . . ?
C30 N4 C31 C32 177.2(17) . . . . ?
C30 N4 C31 C36 -1.2(17) . . . . ?
N4 C31 C32 C33 -178.2(18) . . . . ?
C36 C31 C32 C33 0(3) . . . . ?
C31 C32 C33 C34 -1(3) . . . . ?
C32 C33 C34 C35 1(3) . . . . ?
C33 C34 C35 C36 -1(3) . . . . ?
N4 C31 C36 C35 179.0(13) . . . . ?
C32 C31 C36 C35 0(2) . . . . ?
N4 C31 C36 C29 1.4(16) . . . . ?
C32 C31 C36 C29 -177.1(14) . . . . ?
C34 C35 C36 C31 0(2) . . . . ?
C34 C35 C36 C29 176.6(16) . . . . ?
C30 C29 C36 C31 -1.2(16) . . . . ?
C28 C29 C36 C31 176.4(15) . . . . ?
C30 C29 C36 C35 -178.2(16) . . . . ?
C28 C29 C36 C35 -1(3) . . . . ?
Gd1 O5 C37 O6 -13.1(16) . . . . ?
Gd1 O5 C37 C38 163.5(7) . . . . ?
O5 C37 C38 C39 154.8(9) . . . . ?
O6 C37 C38 C39 -28.3(14) . . . . ?
C37 C38 C39 C40 175.6(9) . . . . ?
C38 C39 C40 C41 -175.9(10) . . . . ?
C39 C40 C41 C42 100.6(13) . . . . ?
C39 C40 C41 C48 -77.7(13) . . . . ?
C48 C41 C42 N5 -1.1(11) . . . . ?
C40 C41 C42 N5 -179.7(8) . . . . ?
C43 N5 C42 C41 1.1(11) . . . . ?
C42 N5 C43 C44 -179.5(10) . . . . ?
C42 N5 C43 C48 -0.7(11) . . . . ?
N5 C43 C44 C45 178.0(11) . . . . ?
C48 C43 C44 C45 -0.7(16) . . . . ?
C43 C44 C45 C46 2.6(18) . . . . ?
C44 C45 C46 C47 -2.9(18) . . . . ?
C45 C46 C47 C48 0.9(16) . . . . ?
C46 C47 C48 C43 1.0(14) . . . . ?
C46 C47 C48 C41 -179.3(11) . . . . ?
N5 C43 C48 C47 179.8(8) . . . . ?
C44 C43 C48 C47 -1.2(14) . . . . ?
N5 C43 C48 C41 0.0(10) . . . . ?
C44 C43 C48 C41 179.0(9) . . . . ?
C42 C41 C48 C47 -179.1(10) . . . . ?
C40 C41 C48 C47 -0.5(17) . . . . ?
C42 C41 C48 C43 0.6(10) . . . . ?
C40 C41 C48 C43 179.2(8) . . . . ?
C60 N6 C49 C50 -1.4(17) . . . . ?
N6 C49 C50 C51 2.8(19) . . . . ?
C49 C50 C51 C52 -2(2) . . . . ?
C50 C51 C52 C60 -0.2(18) . . . . ?
C50 C51 C52 C53 -179.1(12) . . . . ?
C60 C52 C53 C54 2.1(18) . . . . ?
C51 C52 C53 C54 -179.1(12) . . . . ?
C52 C53 C54 C55 -2(2) . . . . ?
C53 C54 C55 C56 -178.7(12) . . . . ?
C53 C54 C55 C59 1.6(18) . . . . ?
C59 C55 C56 C57 0.1(17) . . . . ?
C54 C55 C56 C57 -179.5(12) . . . . ?
C55 C56 C57 C58 0.4(19) . . . . ?
C59 N7 C58 C57 1.2(17) . . . . ?
C56 C57 C58 N7 -1(2) . . . . ?
C58 N7 C59 C55 -0.7(15) . . . . ?
C58 N7 C59 C60 179.8(10) . . . . ?
C56 C55 C59 N7 0.0(16) . . . . ?
C54 C55 C59 N7 179.7(10) . . . . ?
C56 C55 C59 C60 179.5(10) . . . . ?
C54 C55 C59 C60 -0.8(15) . . . . ?
C49 N6 C60 C52 -0.8(15) . . . . ?
C49 N6 C60 C59 -179.0(10) . . . . ?
C51 C52 C60 N6 1.6(15) . . . . ?
C53 C52 C60 N6 -179.5(10) . . . . ?
C51 C52 C60 C59 179.8(10) . . . . ?
C53 C52 C60 C59 -1.3(16) . . . . ?
N7 C59 C60 N6 -1.6(14) . . . . ?
C55 C59 C60 N6 178.9(9) . . . . ?
N7 C59 C60 C52 -179.8(9) . . . . ?
C55 C59 C60 C52 0.7(15) . . . . ?
O5 C37 O6 Gd1 1.8(15) . . . 2_677 ?
C38 C37 O6 Gd1 -174.7(7) . . . 2_677 ?

_diffrn_measured_fraction_theta_max 0.963
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.963
_refine_diff_density_max         1.791
_refine_diff_density_min         -1.578
_refine_diff_density_rms         0.163
####################################################################### 
# 
# 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_bai-274
_database_code_depnum_ccdc_archive 'CCDC 1044887'
_audit_update_record             
;
2015-11-09 deposited with the CCDC.
2015-11-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C120 H112 N16 O21 Tb2'
_chemical_formula_weight         2432.12

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'
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'
Tb Tb -0.1723 4.1537 '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

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

_cell_length_a                   13.519(5)
_cell_length_b                   14.322(5)
_cell_length_c                   16.732(6)
_cell_angle_alpha                79.854(6)
_cell_angle_beta                 71.098(6)
_cell_angle_gamma                64.197(6)
_cell_volume                     2757.0(17)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5336
_cell_measurement_theta_min      1.74
_cell_measurement_theta_max      20.34

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      0.079
_exptl_crystal_density_diffrn    1.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1242
_exptl_absorpt_coefficient_mu    1.351
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6492
_exptl_absorpt_correction_T_max  0.8547
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            8882
_diffrn_reflns_av_R_equivalents  0.0742
_diffrn_reflns_av_sigmaI/netI    0.1401
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.74
_diffrn_reflns_theta_max         20.34
_reflns_number_total             5336
_reflns_number_gt                3737
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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)+(0.0964P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5336
_refine_ls_number_parameters     721
_refine_ls_number_restraints     39
_refine_ls_R_factor_all          0.1103
_refine_ls_R_factor_gt           0.0716
_refine_ls_wR_factor_ref         0.1818
_refine_ls_wR_factor_gt          0.1644
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      0.997
_refine_ls_shift/su_max          0.006
_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
O2W O 0.8140(7) 0.2748(7) 0.2093(6) 0.105(3) Uani 1 1 d . . .
H2WA H 0.8385 0.2428 0.1639 0.157 Uiso 1 1 d R . .
H2WC H 0.7452 0.2828 0.2334 0.157 Uiso 1 1 d R . .
O1W O 0.9837(19) 0.067(2) 0.4968(16) 0.251(17) Uani 0.50 1 d P . .
H1WA H 0.9567 0.0762 0.5497 0.377 Uiso 0.50 1 d PR . .
H1WB H 0.9482 0.0403 0.4814 0.377 Uiso 0.50 1 d PR . .
Tb1 Tb 0.84814(4) 1.00345(4) 0.06235(3) 0.03568(16) Uani 1 1 d . . .
O1 O 0.7844(6) 0.9467(5) 0.2093(4) 0.048(2) Uani 1 1 d . . .
O2 O 0.7733(6) 1.1051(5) 0.1913(4) 0.050(2) Uani 1 1 d . . .
O3 O 0.9933(5) 0.9917(5) -0.0860(4) 0.0360(19) Uani 1 1 d . . .
O4 O 0.8189(6) 1.0126(6) -0.0757(5) 0.062(2) Uani 1 1 d . . .
O5 O 0.9848(5) 0.8306(5) 0.0502(4) 0.043(2) Uani 1 1 d . . .
O7 O 0.7602(11) 0.3374(9) 0.4868(7) 0.149(5) Uani 1 1 d . . .
O8 O 0.7911(10) 0.2239(8) 0.4071(8) 0.136(5) Uani 1 1 d . . .
O9 O 0.7045(10) 0.3818(9) 0.3783(8) 0.130(5) Uani 1 1 d . . .
N1 N 0.7292(7) 0.9003(6) 0.0669(5) 0.047(3) Uani 1 1 d . . .
N2 N 0.6317(6) 1.1087(7) 0.0919(5) 0.044(2) Uani 1 1 d . . .
N3 N 0.3413(8) 1.4298(8) 0.5099(6) 0.068(3) Uani 1 1 d . . .
H3A H 0.3220 1.4947 0.5147 0.081 Uiso 1 1 calc R . .
N4 N 0.7071(10) 1.4467(9) -0.3348(7) 0.095(4) Uani 1 1 d . . .
H4A H 0.7008 1.4879 -0.3788 0.114 Uiso 1 1 calc R . .
N5 N 0.9974(8) 0.3340(7) 0.1772(6) 0.070(3) Uani 1 1 d . . .
H5A H 0.9528 0.3040 0.1817 0.084 Uiso 1 1 calc R . .
N6 N 0.5084(8) 0.9561(8) 0.3123(6) 0.063(3) Uani 1 1 d . . .
N7 N 0.7113(8) 0.7893(7) 0.2663(5) 0.051(3) Uani 1 1 d . . .
H7 H 0.7079 0.8509 0.2652 0.061 Uiso 1 1 calc R . .
N8 N 0.7514(11) 0.3128(10) 0.4240(9) 0.097(5) Uani 1 1 d . . .
C1 C 0.7722(9) 0.8010(8) 0.0541(7) 0.053(3) Uani 1 1 d . . .
H1A H 0.8514 0.7652 0.0385 0.063 Uiso 1 1 calc R . .
C2 C 0.7057(10) 0.7463(9) 0.0625(8) 0.068(4) Uani 1 1 d . . .
H2A H 0.7415 0.6755 0.0533 0.082 Uiso 1 1 calc R . .
C3 C 0.5901(9) 0.7937(9) 0.0836(7) 0.056(3) Uani 1 1 d . . .
H3B H 0.5462 0.7564 0.0893 0.067 Uiso 1 1 calc R . .
C4 C 0.5379(9) 0.9011(9) 0.0968(6) 0.046(3) Uani 1 1 d . . .
C5 C 0.4178(9) 0.9595(10) 0.1148(7) 0.061(4) Uani 1 1 d . . .
H5B H 0.3706 0.9264 0.1180 0.074 Uiso 1 1 calc R . .
C6 C 0.3713(9) 1.0622(10) 0.1272(7) 0.063(4) Uani 1 1 d . . .
H6C H 0.2922 1.0988 0.1407 0.076 Uiso 1 1 calc R . .
C7 C 0.4426(9) 1.1152(9) 0.1198(7) 0.050(3) Uani 1 1 d . . .
C8 C 0.3950(11) 1.2210(11) 0.1323(8) 0.073(5) Uani 1 1 d . . .
H8A H 0.3161 1.2584 0.1460 0.088 Uiso 1 1 calc R . .
C9 C 0.4658(10) 1.2696(10) 0.1241(7) 0.065(4) Uani 1 1 d . . .
H9A H 0.4359 1.3402 0.1327 0.079 Uiso 1 1 calc R . .
C10 C 0.5818(9) 1.2117(9) 0.1028(7) 0.051(4) Uani 1 1 d . . .
H10A H 0.6292 1.2459 0.0954 0.061 Uiso 1 1 calc R . .
C11 C 0.5604(8) 1.0621(9) 0.0985(6) 0.041(3) Uani 1 1 d . . .
C12 C 0.6109(9) 0.9509(8) 0.0881(6) 0.041(3) Uani 1 1 d . . .
C13 C 0.7575(9) 1.0345(9) 0.2392(6) 0.047(3) Uani 1 1 d . . .
C14 C 0.7050(10) 1.0501(8) 0.3346(6) 0.053(3) Uani 1 1 d . . .
H14A H 0.6800 0.9949 0.3601 0.064 Uiso 1 1 calc R . .
H14B H 0.7637 1.0441 0.3589 0.064 Uiso 1 1 calc R . .
C15 C 0.6035(10) 1.1546(8) 0.3571(6) 0.057(4) Uani 1 1 d . . .
H15A H 0.6286 1.2103 0.3344 0.069 Uiso 1 1 calc R . .
H15B H 0.5453 1.1623 0.3315 0.069 Uiso 1 1 calc R . .
C16 C 0.5526(12) 1.1631(10) 0.4521(7) 0.081(5) Uani 1 1 d . . .
H16A H 0.5293 1.1062 0.4742 0.098 Uiso 1 1 calc R . .
H16B H 0.6115 1.1552 0.4770 0.098 Uiso 1 1 calc R . .
C17 C 0.4520(10) 1.2629(9) 0.4790(7) 0.054(4) Uani 1 1 d . . .
C18 C 0.4525(12) 1.3550(11) 0.4802(7) 0.077(5) Uani 1 1 d . . .
H18A H 0.5181 1.3682 0.4634 0.092 Uiso 1 1 calc R . .
C19 C 0.2695(11) 1.3812(9) 0.5297(7) 0.0617(8) Uani 1 1 d U . .
C20 C 0.1493(12) 1.4228(13) 0.5607(9) 0.094(5) Uani 1 1 d . . .
H20A H 0.1069 1.4936 0.5686 0.113 Uiso 1 1 calc R . .
C21 C 0.0983(14) 1.3570(14) 0.5785(10) 0.109(6) Uani 1 1 d . . .
H21A H 0.0192 1.3835 0.6010 0.131 Uiso 1 1 calc R . .
C22 C 0.1573(13) 1.2503(13) 0.5649(9) 0.102(5) Uani 1 1 d . . .
H22A H 0.1179 1.2076 0.5791 0.122 Uiso 1 1 calc R . .
C23 C 0.2800(12) 1.2075(11) 0.5287(7) 0.083(5) Uani 1 1 d . . .
H23A H 0.3216 1.1373 0.5180 0.100 Uiso 1 1 calc R . .
C24 C 0.3330(10) 1.2761(9) 0.5106(7) 0.0608(8) Uani 1 1 d U . .
C25 C 0.9181(9) 1.0040(8) -0.1192(7) 0.042(3) Uani 1 1 d . . .
C26 C 0.9435(11) 1.0143(10) -0.2148(7) 0.075(5) Uani 1 1 d . . .
H26A H 0.9357 0.9586 -0.2344 0.090 Uiso 1 1 calc R . .
H26B H 1.0221 1.0065 -0.2393 0.090 Uiso 1 1 calc R . .
C27 C 0.8636(11) 1.1192(10) -0.2462(7) 0.070(4) Uani 1 1 d . . .
H27A H 0.8787 1.1169 -0.3068 0.085 Uiso 1 1 calc R . .
H27B H 0.7853 1.1267 -0.2203 0.085 Uiso 1 1 calc R . .
C28 C 0.8732(11) 1.2151(12) -0.2290(9) 0.089(4) Uani 1 1 d U . .
H28A H 0.8656 1.2149 -0.1693 0.107 Uiso 1 1 calc R . .
H28B H 0.9484 1.2127 -0.2604 0.107 Uiso 1 1 calc R . .
C29 C 0.7849(10) 1.3121(11) -0.2530(8) 0.075(4) Uani 1 1 d U . .
C30 C 0.7993(12) 1.3582(12) -0.3311(9) 0.093(6) Uani 1 1 d . . .
H30A H 0.8642 1.3322 -0.3763 0.111 Uiso 1 1 calc R . .
C31 C 0.6250(11) 1.4620(11) -0.2591(9) 0.082(4) Uani 1 1 d . . .
C32 C 0.5099(14) 1.5346(12) -0.2279(10) 0.1095(10) Uani 1 1 d U . .
H32A H 0.4752 1.5896 -0.2623 0.131 Uiso 1 1 calc R . .
C33 C 0.4528(14) 1.5214(13) -0.1473(11) 0.1151(9) Uani 1 1 d U . .
H33A H 0.3787 1.5702 -0.1261 0.138 Uiso 1 1 calc R . .
C34 C 0.4966(13) 1.4434(11) -0.0972(9) 0.097(4) Uani 1 1 d U . .
H34A H 0.4511 1.4395 -0.0425 0.117 Uiso 1 1 calc R . .
C35 C 0.6079(13) 1.3652(12) -0.1208(9) 0.103(5) Uani 1 1 d . . .
H35A H 0.6370 1.3103 -0.0842 0.124 Uiso 1 1 calc R . .
C36 C 0.6728(10) 1.3765(11) -0.2054(8) 0.069(4) Uani 1 1 d . . .
C37 C 1.0909(9) 0.7878(8) 0.0203(7) 0.053(3) Uani 1 1 d . . .
C38 C 1.1519(9) 0.6721(8) 0.0160(7) 0.049(3) Uani 1 1 d . . .
H38A H 1.2272 0.6515 0.0228 0.058 Uiso 1 1 calc R . .
H38B H 1.1624 0.6532 -0.0400 0.058 Uiso 1 1 calc R . .
C39 C 1.0932(9) 0.6105(7) 0.0804(7) 0.049(3) Uani 1 1 d . . .
H39A H 1.0152 0.6348 0.0777 0.059 Uiso 1 1 calc R . .
H39B H 1.0903 0.6224 0.1366 0.059 Uiso 1 1 calc R . .
C40 C 1.1554(10) 0.4942(8) 0.0652(8) 0.066(4) Uani 1 1 d . . .
H40A H 1.1596 0.4838 0.0082 0.079 Uiso 1 1 calc R . .
H40B H 1.2332 0.4712 0.0679 0.079 Uiso 1 1 calc R . .
C41 C 1.1032(9) 0.4264(9) 0.1251(7) 0.053(4) Uani 1 1 d . . .
C42 C 1.0353(10) 0.3885(10) 0.1054(8) 0.070(4) Uani 1 1 d . . .
H42A H 1.0184 0.3979 0.0542 0.084 Uiso 1 1 calc R . .
C43 C 1.0413(11) 0.3353(9) 0.2387(8) 0.067(4) Uani 1 1 d . . .
C44 C 1.0253(13) 0.2918(11) 0.3198(8) 0.089(6) Uani 1 1 d . . .
H44A H 0.9817 0.2526 0.3388 0.107 Uiso 1 1 calc R . .
C45 C 1.0768(13) 0.3090(12) 0.3717(9) 0.099(6) Uani 1 1 d . . .
H45A H 1.0674 0.2817 0.4270 0.119 Uiso 1 1 calc R . .
C46 C 1.1448(13) 0.3687(13) 0.3405(11) 0.107(6) Uani 1 1 d . . .
H46A H 1.1818 0.3763 0.3755 0.128 Uiso 1 1 calc R . .
C47 C 1.1570(11) 0.4144(10) 0.2617(9) 0.076(5) Uani 1 1 d . . .
H47A H 1.1988 0.4551 0.2431 0.092 Uiso 1 1 calc R . .
C48 C 1.1049(10) 0.3978(9) 0.2104(7) 0.053(4) Uani 1 1 d . . .
C49 C 0.4079(12) 1.0350(11) 0.3326(8) 0.076(4) Uani 1 1 d . . .
H49A H 0.4058 1.1013 0.3291 0.091 Uiso 1 1 calc R . .
C50 C 0.3023(13) 1.0233(12) 0.3595(8) 0.089(4) Uani 1 1 d U . .
H50A H 0.2334 1.0813 0.3728 0.106 Uiso 1 1 calc R . .
C51 C 0.3027(13) 0.9299(12) 0.3657(9) 0.095(5) Uani 1 1 d U . .
H51A H 0.2341 0.9218 0.3864 0.114 Uiso 1 1 calc R . .
C52 C 0.4056(10) 0.8435(10) 0.3411(7) 0.061(4) Uani 1 1 d . . .
C53 C 0.4126(12) 0.7421(11) 0.3424(8) 0.081(4) Uani 1 1 d . . .
H53A H 0.3456 0.7314 0.3580 0.097 Uiso 1 1 calc R . .
C54 C 0.5129(12) 0.6614(11) 0.3217(8) 0.081(4) Uani 1 1 d . . .
H54A H 0.5156 0.5950 0.3244 0.097 Uiso 1 1 calc R . .
C55 C 0.6167(10) 0.6765(9) 0.2953(7) 0.059(4) Uani 1 1 d . . .
C56 C 0.7231(12) 0.5958(10) 0.2713(8) 0.079(5) Uani 1 1 d . . .
H56A H 0.7283 0.5286 0.2731 0.094 Uiso 1 1 calc R . .
C57 C 0.8196(12) 0.6126(9) 0.2455(8) 0.076(5) Uani 1 1 d . . .
H57A H 0.8905 0.5574 0.2294 0.092 Uiso 1 1 calc R . .
C58 C 0.8124(11) 0.7131(10) 0.2429(7) 0.066(4) Uani 1 1 d . . .
H58A H 0.8783 0.7258 0.2249 0.080 Uiso 1 1 calc R . .
C59 C 0.6117(10) 0.7764(9) 0.2923(7) 0.049(3) Uani 1 1 d . . .
C60 C 0.5056(10) 0.8614(10) 0.3161(7) 0.055(4) Uani 1 1 d . . .
O6 O 1.1594(6) 0.8321(5) -0.0127(4) 0.044(2) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O2W H2WA 0.8500 . ?
O2W H2WC 0.8501 . ?
O1W O1W 1.77(6) 2_756 ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8499 . ?
Tb1 O6 2.324(7) 2_775 ?
Tb1 O3 2.333(7) 2_775 ?
Tb1 O5 2.353(6) . ?
Tb1 O4 2.439(8) . ?
Tb1 O1 2.446(6) . ?
Tb1 O2 2.491(7) . ?
Tb1 N2 2.562(8) . ?
Tb1 N1 2.594(9) . ?
Tb1 O3 2.596(6) . ?
Tb1 Tb1 3.9233(17) 2_775 ?
O1 C13 1.292(12) . ?
O2 C13 1.225(12) . ?
O3 C25 1.246(12) . ?
O3 Tb1 2.333(7) 2_775 ?
O4 C25 1.265(12) . ?
O5 C37 1.249(11) . ?
O7 N8 1.221(17) . ?
O8 N8 1.193(15) . ?
O9 N8 1.210(16) . ?
N1 C1 1.308(12) . ?
N1 C12 1.387(12) . ?
N2 C10 1.347(13) . ?
N2 C11 1.360(13) . ?
N3 C19 1.354(16) . ?
N3 C18 1.399(15) . ?
N3 H3A 0.8600 . ?
N4 C30 1.346(17) . ?
N4 C31 1.364(15) . ?
N4 H4A 0.8600 . ?
N5 C43 1.350(16) . ?
N5 C42 1.390(15) . ?
N5 H5A 0.8600 . ?
N6 C49 1.318(15) . ?
N6 C60 1.363(15) . ?
N7 C58 1.311(13) . ?
N7 C59 1.359(14) . ?
N7 H7 0.8600 . ?
C1 C2 1.391(16) . ?
C1 H1A 0.9300 . ?
C2 C3 1.354(15) . ?
C2 H2A 0.9300 . ?
C3 C4 1.410(15) . ?
C3 H3B 0.9300 . ?
C4 C12 1.409(15) . ?
C4 C5 1.420(14) . ?
C5 C6 1.349(16) . ?
C5 H5B 0.9300 . ?
C6 C7 1.432(17) . ?
C6 H6C 0.9300 . ?
C7 C11 1.384(13) . ?
C7 C8 1.388(16) . ?
C8 C9 1.371(18) . ?
C8 H8A 0.9300 . ?
C9 C10 1.372(15) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
C11 C12 1.451(14) . ?
C13 C14 1.535(14) . ?
C14 C15 1.530(14) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.516(15) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.495(15) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.326(18) . ?
C17 C24 1.457(16) . ?
C18 H18A 0.9300 . ?
C19 C24 1.405(16) . ?
C19 C20 1.409(17) . ?
C20 C21 1.34(2) . ?
C20 H20A 0.9300 . ?
C21 C22 1.40(2) . ?
C21 H21A 0.9300 . ?
C22 C23 1.445(19) . ?
C22 H22A 0.9300 . ?
C23 C24 1.392(18) . ?
C23 H23A 0.9300 . ?
C25 C26 1.517(15) . ?
C26 C27 1.542(16) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.518(19) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C29 1.479(18) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.351(17) . ?
C29 C36 1.429(16) . ?
C30 H30A 0.9300 . ?
C31 C36 1.422(18) . ?
C31 C32 1.425(19) . ?
C32 C33 1.35(2) . ?
C32 H32A 0.9300 . ?
C33 C34 1.31(2) . ?
C33 H33A 0.9300 . ?
C34 C35 1.407(19) . ?
C34 H34A 0.9300 . ?
C35 C36 1.428(17) . ?
C35 H35A 0.9300 . ?
C37 O6 1.274(12) . ?
C37 C38 1.499(14) . ?
C38 C39 1.512(14) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 C40 1.530(14) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 C41 1.497(16) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 C42 1.391(17) . ?
C41 C48 1.419(16) . ?
C42 H42A 0.9300 . ?
C43 C44 1.381(17) . ?
C43 C48 1.421(17) . ?
C44 C45 1.38(2) . ?
C44 H44A 0.9300 . ?
C45 C46 1.44(2) . ?
C45 H45A 0.9300 . ?
C46 C47 1.36(2) . ?
C46 H46A 0.9300 . ?
C47 C48 1.378(18) . ?
C47 H47A 0.9300 . ?
C49 C50 1.426(19) . ?
C49 H49A 0.9300 . ?
C50 C51 1.322(19) . ?
C50 H50A 0.9300 . ?
C51 C52 1.395(17) . ?
C51 H51A 0.9300 . ?
C52 C60 1.402(17) . ?
C52 C53 1.412(18) . ?
C53 C54 1.329(17) . ?
C53 H53A 0.9300 . ?
C54 C55 1.428(18) . ?
C54 H54A 0.9300 . ?
C55 C56 1.382(16) . ?
C55 C59 1.395(16) . ?
C56 C57 1.348(19) . ?
C56 H56A 0.9300 . ?
C57 C58 1.394(17) . ?
C57 H57A 0.9300 . ?
C58 H58A 0.9300 . ?
C59 C60 1.407(15) . ?
O6 Tb1 2.324(7) 2_775 ?

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
H2WA O2W H2WC 109.5 . . ?
O1W O1W H1WA 96.3 2_756 . ?
O1W O1W H1WB 55.2 2_756 . ?
H1WA O1W H1WB 109.5 . . ?
O6 Tb1 O3 75.3(2) 2_775 2_775 ?
O6 Tb1 O5 137.9(2) 2_775 . ?
O3 Tb1 O5 75.5(2) 2_775 . ?
O6 Tb1 O4 79.2(3) 2_775 . ?
O3 Tb1 O4 125.6(2) 2_775 . ?
O5 Tb1 O4 94.1(2) . . ?
O6 Tb1 O1 127.1(2) 2_775 . ?
O3 Tb1 O1 91.4(2) 2_775 . ?
O5 Tb1 O1 83.2(2) . . ?
O4 Tb1 O1 141.0(3) . . ?
O6 Tb1 O2 74.8(2) 2_775 . ?
O3 Tb1 O2 73.9(2) 2_775 . ?
O5 Tb1 O2 124.1(2) . . ?
O4 Tb1 O2 141.6(2) . . ?
O1 Tb1 O2 52.4(2) . . ?
O6 Tb1 N2 79.1(3) 2_775 . ?
O3 Tb1 N2 140.0(2) 2_775 . ?
O5 Tb1 N2 140.5(3) . . ?
O4 Tb1 N2 77.9(2) . . ?
O1 Tb1 N2 79.9(2) . . ?
O2 Tb1 N2 69.9(3) . . ?
O6 Tb1 N1 135.3(3) 2_775 . ?
O3 Tb1 N1 149.3(2) 2_775 . ?
O5 Tb1 N1 76.9(2) . . ?
O4 Tb1 N1 69.4(3) . . ?
O1 Tb1 N1 72.2(3) . . ?
O2 Tb1 N1 112.0(2) . . ?
N2 Tb1 N1 64.1(3) . . ?
O6 Tb1 O3 70.3(2) 2_775 . ?
O3 Tb1 O3 74.7(2) 2_775 . ?
O5 Tb1 O3 73.2(2) . . ?
O4 Tb1 O3 51.6(2) . . ?
O1 Tb1 O3 154.9(2) . . ?
O2 Tb1 O3 137.7(2) . . ?
N2 Tb1 O3 124.1(2) . . ?
N1 Tb1 O3 109.6(2) . . ?
O6 Tb1 Tb1 68.05(16) 2_775 2_775 ?
O3 Tb1 Tb1 39.66(14) 2_775 2_775 ?
O5 Tb1 Tb1 70.07(16) . 2_775 ?
O4 Tb1 Tb1 86.29(17) . 2_775 ?
O1 Tb1 Tb1 127.89(17) . 2_775 ?
O2 Tb1 Tb1 108.94(17) . 2_775 ?
N2 Tb1 Tb1 145.7(2) . 2_775 ?
N1 Tb1 Tb1 137.13(17) . 2_775 ?
O3 Tb1 Tb1 35.00(15) . 2_775 ?
C13 O1 Tb1 94.0(6) . . ?
C13 O2 Tb1 93.6(6) . . ?
C25 O3 Tb1 162.1(7) . 2_775 ?
C25 O3 Tb1 89.7(6) . . ?
Tb1 O3 Tb1 105.3(2) 2_775 . ?
C25 O4 Tb1 96.6(7) . . ?
C37 O5 Tb1 135.0(7) . . ?
C1 N1 C12 116.2(9) . . ?
C1 N1 Tb1 124.7(7) . . ?
C12 N1 Tb1 119.0(7) . . ?
C10 N2 C11 116.3(9) . . ?
C10 N2 Tb1 122.6(7) . . ?
C11 N2 Tb1 121.1(6) . . ?
C19 N3 C18 107.4(11) . . ?
C19 N3 H3A 126.3 . . ?
C18 N3 H3A 126.3 . . ?
C30 N4 C31 110.5(11) . . ?
C30 N4 H4A 124.8 . . ?
C31 N4 H4A 124.8 . . ?
C43 N5 C42 109.8(11) . . ?
C43 N5 H5A 125.1 . . ?
C42 N5 H5A 125.1 . . ?
C49 N6 C60 115.6(12) . . ?
C58 N7 C59 123.6(11) . . ?
C58 N7 H7 118.2 . . ?
C59 N7 H7 118.2 . . ?
O8 N8 O9 121.5(17) . . ?
O8 N8 O7 120.8(15) . . ?
O9 N8 O7 117.6(15) . . ?
N1 C1 C2 123.4(10) . . ?
N1 C1 H1A 118.3 . . ?
C2 C1 H1A 118.3 . . ?
C3 C2 C1 121.5(11) . . ?
C3 C2 H2A 119.2 . . ?
C1 C2 H2A 119.2 . . ?
C2 C3 C4 118.1(11) . . ?
C2 C3 H3B 120.9 . . ?
C4 C3 H3B 120.9 . . ?
C12 C4 C3 117.0(9) . . ?
C12 C4 C5 120.2(11) . . ?
C3 C4 C5 122.7(10) . . ?
C6 C5 C4 120.8(11) . . ?
C6 C5 H5B 119.6 . . ?
C4 C5 H5B 119.6 . . ?
C5 C6 C7 120.5(10) . . ?
C5 C6 H6C 119.7 . . ?
C7 C6 H6C 119.7 . . ?
C11 C7 C8 118.9(11) . . ?
C11 C7 C6 120.4(11) . . ?
C8 C7 C6 120.7(11) . . ?
C9 C8 C7 119.2(11) . . ?
C9 C8 H8A 120.4 . . ?
C7 C8 H8A 120.4 . . ?
C8 C9 C10 118.6(12) . . ?
C8 C9 H9A 120.7 . . ?
C10 C9 H9A 120.7 . . ?
N2 C10 C9 124.3(12) . . ?
N2 C10 H10A 117.8 . . ?
C9 C10 H10A 117.8 . . ?
N2 C11 C7 122.6(10) . . ?
N2 C11 C12 117.9(9) . . ?
C7 C11 C12 119.4(10) . . ?
N1 C12 C4 123.6(10) . . ?
N1 C12 C11 117.7(9) . . ?
C4 C12 C11 118.6(9) . . ?
O2 C13 O1 120.0(9) . . ?
O2 C13 C14 120.3(10) . . ?
O1 C13 C14 119.7(10) . . ?
C15 C14 C13 114.0(9) . . ?
C15 C14 H14A 108.8 . . ?
C13 C14 H14A 108.8 . . ?
C15 C14 H14B 108.8 . . ?
C13 C14 H14B 108.8 . . ?
H14A C14 H14B 107.7 . . ?
C16 C15 C14 111.3(9) . . ?
C16 C15 H15A 109.4 . . ?
C14 C15 H15A 109.4 . . ?
C16 C15 H15B 109.4 . . ?
C14 C15 H15B 109.4 . . ?
H15A C15 H15B 108.0 . . ?
C17 C16 C15 114.4(10) . . ?
C17 C16 H16A 108.7 . . ?
C15 C16 H16A 108.7 . . ?
C17 C16 H16B 108.7 . . ?
C15 C16 H16B 108.7 . . ?
H16A C16 H16B 107.6 . . ?
C18 C17 C24 106.9(11) . . ?
C18 C17 C16 127.7(13) . . ?
C24 C17 C16 125.4(12) . . ?
C17 C18 N3 110.9(13) . . ?
C17 C18 H18A 124.5 . . ?
N3 C18 H18A 124.5 . . ?
N3 C19 C24 109.3(11) . . ?
N3 C19 C20 129.3(13) . . ?
C24 C19 C20 121.3(13) . . ?
C21 C20 C19 117.7(15) . . ?
C21 C20 H20A 121.2 . . ?
C19 C20 H20A 121.2 . . ?
C20 C21 C22 123.7(16) . . ?
C20 C21 H21A 118.2 . . ?
C22 C21 H21A 118.2 . . ?
C21 C22 C23 119.3(15) . . ?
C21 C22 H22A 120.4 . . ?
C23 C22 H22A 120.4 . . ?
C24 C23 C22 117.0(13) . . ?
C24 C23 H23A 121.5 . . ?
C22 C23 H23A 121.5 . . ?
C23 C24 C19 120.9(12) . . ?
C23 C24 C17 133.5(12) . . ?
C19 C24 C17 105.5(11) . . ?
O3 C25 O4 122.0(10) . . ?
O3 C25 C26 119.4(10) . . ?
O4 C25 C26 118.5(10) . . ?
C25 C26 C27 112.9(9) . . ?
C25 C26 H26A 109.0 . . ?
C27 C26 H26A 109.0 . . ?
C25 C26 H26B 109.0 . . ?
C27 C26 H26B 109.0 . . ?
H26A C26 H26B 107.8 . . ?
C28 C27 C26 116.3(12) . . ?
C28 C27 H27A 108.2 . . ?
C26 C27 H27A 108.2 . . ?
C28 C27 H27B 108.2 . . ?
C26 C27 H27B 108.2 . . ?
H27A C27 H27B 107.4 . . ?
C29 C28 C27 112.1(12) . . ?
C29 C28 H28A 109.2 . . ?
C27 C28 H28A 109.2 . . ?
C29 C28 H28B 109.2 . . ?
C27 C28 H28B 109.2 . . ?
H28A C28 H28B 107.9 . . ?
C30 C29 C36 105.4(12) . . ?
C30 C29 C28 123.4(12) . . ?
C36 C29 C28 131.3(12) . . ?
N4 C30 C29 110.9(12) . . ?
N4 C30 H30A 124.5 . . ?
C29 C30 H30A 124.5 . . ?
N4 C31 C36 105.2(11) . . ?
N4 C31 C32 135.7(14) . . ?
C36 C31 C32 118.9(13) . . ?
C33 C32 C31 118.2(15) . . ?
C33 C32 H32A 120.9 . . ?
C31 C32 H32A 120.9 . . ?
C34 C33 C32 123.3(16) . . ?
C34 C33 H33A 118.4 . . ?
C32 C33 H33A 118.4 . . ?
C33 C34 C35 124.1(14) . . ?
C33 C34 H34A 117.9 . . ?
C35 C34 H34A 117.9 . . ?
C34 C35 C36 114.8(14) . . ?
C34 C35 H35A 122.6 . . ?
C36 C35 H35A 122.6 . . ?
C31 C36 C35 120.6(12) . . ?
C31 C36 C29 108.0(11) . . ?
C35 C36 C29 131.3(13) . . ?
O5 C37 O6 127.2(10) . . ?
O5 C37 C38 121.1(9) . . ?
O6 C37 C38 111.7(9) . . ?
C37 C38 C39 115.9(9) . . ?
C37 C38 H38A 108.3 . . ?
C39 C38 H38A 108.3 . . ?
C37 C38 H38B 108.3 . . ?
C39 C38 H38B 108.3 . . ?
H38A C38 H38B 107.4 . . ?
C38 C39 C40 111.9(8) . . ?
C38 C39 H39A 109.2 . . ?
C40 C39 H39A 109.2 . . ?
C38 C39 H39B 109.2 . . ?
C40 C39 H39B 109.2 . . ?
H39A C39 H39B 107.9 . . ?
C41 C40 C39 116.1(9) . . ?
C41 C40 H40A 108.3 . . ?
C39 C40 H40A 108.3 . . ?
C41 C40 H40B 108.3 . . ?
C39 C40 H40B 108.3 . . ?
H40A C40 H40B 107.4 . . ?
C42 C41 C48 109.2(11) . . ?
C42 C41 C40 123.1(12) . . ?
C48 C41 C40 127.4(12) . . ?
N5 C42 C41 106.8(11) . . ?
N5 C42 H42A 126.6 . . ?
C41 C42 H42A 126.6 . . ?
N5 C43 C44 129.0(14) . . ?
N5 C43 C48 109.3(11) . . ?
C44 C43 C48 121.6(14) . . ?
C43 C44 C45 117.0(16) . . ?
C43 C44 H44A 121.5 . . ?
C45 C44 H44A 121.5 . . ?
C44 C45 C46 120.3(15) . . ?
C44 C45 H45A 119.8 . . ?
C46 C45 H45A 119.8 . . ?
C47 C46 C45 122.4(16) . . ?
C47 C46 H46A 118.8 . . ?
C45 C46 H46A 118.8 . . ?
C46 C47 C48 117.1(15) . . ?
C46 C47 H47A 121.4 . . ?
C48 C47 H47A 121.4 . . ?
C47 C48 C41 133.8(13) . . ?
C47 C48 C43 121.4(12) . . ?
C41 C48 C43 104.7(11) . . ?
N6 C49 C50 123.0(13) . . ?
N6 C49 H49A 118.5 . . ?
C50 C49 H49A 118.5 . . ?
C51 C50 C49 119.8(14) . . ?
C51 C50 H50A 120.1 . . ?
C49 C50 H50A 120.1 . . ?
C50 C51 C52 120.2(15) . . ?
C50 C51 H51A 119.9 . . ?
C52 C51 H51A 119.9 . . ?
C51 C52 C60 116.3(13) . . ?
C51 C52 C53 123.5(13) . . ?
C60 C52 C53 120.1(12) . . ?
C54 C53 C52 121.3(14) . . ?
C54 C53 H53A 119.3 . . ?
C52 C53 H53A 119.3 . . ?
C53 C54 C55 120.2(14) . . ?
C53 C54 H54A 119.9 . . ?
C55 C54 H54A 119.9 . . ?
C56 C55 C59 118.1(12) . . ?
C56 C55 C54 122.5(12) . . ?
C59 C55 C54 119.4(11) . . ?
C57 C56 C55 121.2(13) . . ?
C57 C56 H56A 119.4 . . ?
C55 C56 H56A 119.4 . . ?
C56 C57 C58 119.7(12) . . ?
C56 C57 H57A 120.2 . . ?
C58 C57 H57A 120.2 . . ?
N7 C58 C57 118.9(13) . . ?
N7 C58 H58A 120.6 . . ?
C57 C58 H58A 120.6 . . ?
N7 C59 C55 118.5(10) . . ?
N7 C59 C60 121.1(11) . . ?
C55 C59 C60 120.4(11) . . ?
N6 C60 C52 124.8(11) . . ?
N6 C60 C59 116.7(11) . . ?
C52 C60 C59 118.5(12) . . ?
C37 O6 Tb1 138.8(7) . 2_775 ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        20.34
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         1.579
_refine_diff_density_min         -1.099
_refine_diff_density_rms         0.143
####################################################################### 
# 
# 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_bai-929
_database_code_depnum_ccdc_archive 'CCDC 1044888'
_audit_update_record             
;
2015-11-09 deposited with the CCDC.
2015-11-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C120 H114 N16 O22 Yb2'
_chemical_formula_weight         2478.35

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   13.414(3)
_cell_length_b                   14.310(3)
_cell_length_c                   16.704(3)
_cell_angle_alpha                80.06(3)
_cell_angle_beta                 71.24(3)
_cell_angle_gamma                64.17(3)
_cell_volume                     2730.7(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    12194
_cell_measurement_theta_min      3.05
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1262
_exptl_absorpt_coefficient_mu    1.783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5993
_exptl_absorpt_correction_T_max  0.8013
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            26539
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         27.48
_reflns_number_total             12194
_reflns_number_gt                11252
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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)+(0.0576P)²+1.7037P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12194
_refine_ls_number_parameters     721
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0264
_refine_ls_wR_factor_ref         0.0893
_refine_ls_wR_factor_gt          0.0808
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O2W O 0.4733(11) 0.5777(14) 0.9980(9) 0.431(16) Uani 1 1 d D . .
H2WA H 0.5318 0.5922 0.9845 0.646 Uiso 1 1 d RD . .
H2WB H 0.4149 0.6269 1.0258 0.646 Uiso 1 1 d RD . .
Yb Yb 0.348567(9) 0.504150(9) 0.561832(7) 0.02240(5) Uani 1 1 d . . .
O1 O 0.2744(2) 0.60620(18) 0.68840(14) 0.0350(5) Uani 1 1 d . . .
O2 O 0.2868(2) 0.44751(18) 0.70661(14) 0.0355(5) Uani 1 1 d . . .
O3 O 0.3220(2) 0.5111(2) 0.42713(15) 0.0435(6) Uani 1 1 d . . .
O4 O 0.49509(19) 0.49170(18) 0.41553(14) 0.0324(5) Uani 1 1 d . . .
O5 O 0.34177(18) 0.66302(17) 0.51249(14) 0.0312(5) Uani 1 1 d . . .
O6 O 0.51659(18) 0.66557(17) 0.45256(14) 0.0322(5) Uani 1 1 d . . .
O7 O 0.7957(5) 0.1167(5) 0.1257(4) 0.122(2) Uani 1 1 d . . .
O8 O 0.7039(5) 0.2738(4) 0.0969(4) 0.1097(16) Uani 1 1 d . . .
O9 O 0.7395(6) 0.1605(5) 0.0136(3) 0.119(2) Uani 1 1 d . . .
O1W O 0.6850(4) 0.2231(3) 0.2929(2) 0.0812(11) Uani 1 1 d . . .
H1WB H 0.6799 0.2779 0.2619 0.122 Uiso 1 1 d R . .
H1WC H 0.7406 0.2047 0.3143 0.122 Uiso 1 1 d R . .
N1 N 0.1356(2) 0.6097(2) 0.58973(17) 0.0315(5) Uani 1 1 d . . .
N2 N 0.2295(2) 0.4025(2) 0.56706(16) 0.0301(5) Uani 1 1 d . . .
N3 N -0.1579(3) 0.9266(3) 1.0093(2) 0.0567(9) Uani 1 1 d . . .
H3A H -0.1774 0.9915 1.0141 0.068 Uiso 1 1 calc R . .
N4 N 0.2028(4) 0.9459(4) 0.1659(3) 0.0718(12) Uani 1 1 d . . .
H4A H 0.1935 0.9878 0.1227 0.086 Uiso 1 1 calc R . .
N5 N 0.5007(3) 1.1651(3) 0.3238(2) 0.0559(9) Uani 1 1 d . . .
H5A H 0.5430 1.1973 0.3208 0.067 Uiso 1 1 calc R . .
N6 N 0.0052(3) 0.4609(3) 0.8103(2) 0.0479(8) Uani 1 1 d . . .
N7 N 0.2098(3) 0.2934(2) 0.76382(18) 0.0393(6) Uani 1 1 d . . .
H7 H 0.2061 0.3553 0.7613 0.047 Uiso 1 1 calc R . .
N8 N 0.7476(4) 0.1832(4) 0.0774(3) 0.0707(12) Uani 1 1 d . . .
C1 C 0.2748(3) 0.3024(3) 0.5521(2) 0.0427(8) Uani 1 1 d . . .
H1A H 0.3547 0.2677 0.5355 0.051 Uiso 1 1 calc R . .
C2 C 0.2090(4) 0.2457(3) 0.5598(3) 0.0534(10) Uani 1 1 d . . .
H2A H 0.2448 0.1752 0.5495 0.064 Uiso 1 1 calc R . .
C3 C 0.0925(4) 0.2956(4) 0.5825(3) 0.0500(10) Uani 1 1 d . . .
H3B H 0.0474 0.2590 0.5896 0.060 Uiso 1 1 calc R . .
C4 C 0.0404(3) 0.4022(3) 0.5953(2) 0.0398(8) Uani 1 1 d . . .
C5 C -0.0812(3) 0.4608(4) 0.6154(2) 0.0505(10) Uani 1 1 d . . .
H5B H -0.1290 0.4274 0.6204 0.061 Uiso 1 1 calc R . .
C6 C -0.1285(3) 0.5638(4) 0.6274(3) 0.0568(12) Uani 1 1 d . . .
H6B H -0.2082 0.6000 0.6405 0.068 Uiso 1 1 calc R . .
C7 C -0.0581(3) 0.6184(3) 0.6202(2) 0.0421(8) Uani 1 1 d . . .
C8 C -0.1024(3) 0.7234(4) 0.6306(3) 0.0562(11) Uani 1 1 d . . .
H8A H -0.1816 0.7625 0.6426 0.067 Uiso 1 1 calc R . .
C9 C -0.0306(3) 0.7704(3) 0.6233(3) 0.0537(10) Uani 1 1 d . . .
H9A H -0.0601 0.8410 0.6324 0.064 Uiso 1 1 calc R . .
C10 C 0.0884(3) 0.7107(3) 0.6019(3) 0.0426(8) Uani 1 1 d . . .
H10A H 0.1369 0.7436 0.5959 0.051 Uiso 1 1 calc R . .
C11 C 0.0631(3) 0.5627(3) 0.59924(19) 0.0301(6) Uani 1 1 d . . .
C12 C 0.1132(3) 0.4529(3) 0.58685(18) 0.0301(6) Uani 1 1 d . . .
C13 C 0.2583(3) 0.5339(3) 0.73688(19) 0.0308(6) Uani 1 1 d . . .
C14 C 0.2076(3) 0.5488(3) 0.8312(2) 0.0410(8) Uani 1 1 d . . .
H14A H 0.1833 0.4931 0.8566 0.049 Uiso 1 1 calc R . .
H14B H 0.2675 0.5428 0.8548 0.049 Uiso 1 1 calc R . .
C15 C 0.1061(3) 0.6516(3) 0.8551(2) 0.0398(8) Uani 1 1 d . . .
H15A H 0.0469 0.6592 0.8301 0.048 Uiso 1 1 calc R . .
H15B H 0.1307 0.7076 0.8322 0.048 Uiso 1 1 calc R . .
C16 C 0.0556(4) 0.6606(4) 0.9503(2) 0.0608(12) Uani 1 1 d . . .
H16A H 0.0345 0.6025 0.9728 0.073 Uiso 1 1 calc R . .
H16B H 0.1149 0.6545 0.9745 0.073 Uiso 1 1 calc R . .
C17 C -0.0475(4) 0.7587(3) 0.9787(2) 0.0490(10) Uani 1 1 d . . .
C18 C -0.0478(4) 0.8529(4) 0.9798(3) 0.0559(11) Uani 1 1 d . . .
H18A H 0.0180 0.8663 0.9628 0.067 Uiso 1 1 calc R . .
C19 C -0.2307(4) 0.8772(4) 1.0297(3) 0.0539(10) Uani 1 1 d . . .
C20 C -0.3502(4) 0.9190(5) 1.0651(3) 0.0767(16) Uani 1 1 d . . .
H20A H -0.3925 0.9893 1.0759 0.092 Uiso 1 1 calc R . .
C21 C -0.4014(5) 0.8508(7) 1.0829(4) 0.091(2) Uani 1 1 d . . .
H21A H -0.4805 0.8750 1.1077 0.109 Uiso 1 1 calc R . .
C22 C -0.3392(6) 0.7473(6) 1.0650(4) 0.0851(19) Uani 1 1 d . . .
H22A H -0.3775 0.7036 1.0771 0.102 Uiso 1 1 calc R . .
C23 C -0.2209(5) 0.7067(4) 1.0296(3) 0.0634(12) Uani 1 1 d . . .
H23A H -0.1798 0.6365 1.0181 0.076 Uiso 1 1 calc R . .
C24 C -0.1651(4) 0.7726(4) 1.0118(2) 0.0491(9) Uani 1 1 d . . .
C25 C 0.4179(3) 0.5054(3) 0.3817(2) 0.0326(7) Uani 1 1 d . . .
C26 C 0.4421(4) 0.5126(4) 0.2869(2) 0.0539(11) Uani 1 1 d . . .
H26A H 0.4338 0.4561 0.2687 0.065 Uiso 1 1 calc R . .
H26B H 0.5210 0.5051 0.2612 0.065 Uiso 1 1 calc R . .
C27 C 0.3596(4) 0.6172(4) 0.2559(2) 0.0533(10) Uani 1 1 d . . .
H27A H 0.3723 0.6148 0.1956 0.064 Uiso 1 1 calc R . .
H27B H 0.2808 0.6256 0.2838 0.064 Uiso 1 1 calc R . .
C28 C 0.3734(5) 0.7089(5) 0.2718(3) 0.0713(14) Uani 1 1 d . . .
H28A H 0.4505 0.7031 0.2407 0.086 Uiso 1 1 calc R . .
H28B H 0.3656 0.7090 0.3316 0.086 Uiso 1 1 calc R . .
C29 C 0.2860(4) 0.8115(4) 0.2462(3) 0.0575(11) Uani 1 1 d . . .
C30 C 0.2990(5) 0.8577(5) 0.1678(3) 0.0709(15) Uani 1 1 d . . .
H30A H 0.3640 0.8328 0.1221 0.085 Uiso 1 1 calc R . .
C31 C 0.1234(5) 0.9576(4) 0.2432(3) 0.0592(11) Uani 1 1 d . . .
C32 C 0.0109(6) 1.0307(5) 0.2713(5) 0.0850(18) Uani 1 1 d . . .
H32A H -0.0219 1.0859 0.2362 0.102 Uiso 1 1 calc R . .
C33 C -0.0496(7) 1.0182(7) 0.3527(6) 0.107(3) Uani 1 1 d . . .
H33A H -0.1253 1.0658 0.3729 0.129 Uiso 1 1 calc R . .
C34 C -0.0018(7) 0.9373(7) 0.4056(5) 0.105(3) Uani 1 1 d . . .
H34A H -0.0456 0.9316 0.4606 0.126 Uiso 1 1 calc R . .
C35 C 0.1084(6) 0.8654(5) 0.3787(3) 0.0759(16) Uani 1 1 d . . .
H35A H 0.1404 0.8117 0.4152 0.091 Uiso 1 1 calc R . .
C36 C 0.1729(4) 0.8734(4) 0.2954(3) 0.0568(11) Uani 1 1 d . . .
C37 C 0.4087(3) 0.7079(2) 0.48241(18) 0.0267(6) Uani 1 1 d . . .
C38 C 0.3497(3) 0.8261(2) 0.4863(2) 0.0368(7) Uani 1 1 d . . .
H38A H 0.2721 0.8482 0.4822 0.044 Uiso 1 1 calc R . .
H38B H 0.3430 0.8446 0.5415 0.044 Uiso 1 1 calc R . .
C39 C 0.4067(3) 0.8876(3) 0.4201(2) 0.0364(7) Uani 1 1 d . . .
H39A H 0.4087 0.8746 0.3644 0.044 Uiso 1 1 calc R . .
H39B H 0.4856 0.8650 0.4217 0.044 Uiso 1 1 calc R . .
C40 C 0.3417(3) 1.0031(3) 0.4355(3) 0.0444(9) Uani 1 1 d . . .
H40A H 0.2646 1.0258 0.4301 0.053 Uiso 1 1 calc R . .
H40B H 0.3345 1.0146 0.4930 0.053 Uiso 1 1 calc R . .
C41 C 0.3980(3) 1.0681(3) 0.3763(2) 0.0402(8) Uani 1 1 d . . .
C42 C 0.4639(4) 1.1088(3) 0.3927(3) 0.0494(9) Uani 1 1 d . . .
H42A H 0.4815 1.0997 0.4437 0.059 Uiso 1 1 calc R . .
C43 C 0.4589(3) 1.1612(3) 0.2609(3) 0.0467(9) Uani 1 1 d . . .
C44 C 0.4724(5) 1.2069(4) 0.1798(3) 0.0628(12) Uani 1 1 d . . .
H44A H 0.5144 1.2477 0.1610 0.075 Uiso 1 1 calc R . .
C45 C 0.4209(5) 1.1888(4) 0.1290(4) 0.0752(16) Uani 1 1 d . . .
H45A H 0.4294 1.2172 0.0741 0.090 Uiso 1 1 calc R . .
C46 C 0.3558(5) 1.1292(5) 0.1565(3) 0.0749(15) Uani 1 1 d . . .
H46A H 0.3216 1.1195 0.1201 0.090 Uiso 1 1 calc R . .
C47 C 0.3418(4) 1.0840(4) 0.2386(3) 0.0579(11) Uani 1 1 d . . .
H47A H 0.2987 1.0442 0.2572 0.070 Uiso 1 1 calc R . .
C48 C 0.3938(3) 1.1001(3) 0.2915(2) 0.0407(8) Uani 1 1 d . . .
C49 C -0.0952(4) 0.5408(4) 0.8333(3) 0.0593(11) Uani 1 1 d . . .
H49A H -0.0962 0.6065 0.8313 0.071 Uiso 1 1 calc R . .
C50 C -0.2014(5) 0.5303(5) 0.8610(4) 0.0770(16) Uani 1 1 d . . .
H50A H -0.2705 0.5885 0.8753 0.092 Uiso 1 1 calc R . .
C51 C -0.2015(4) 0.4351(5) 0.8666(3) 0.0722(15) Uani 1 1 d . . .
H51A H -0.2707 0.4272 0.8865 0.087 Uiso 1 1 calc R . .
C52 C -0.0973(4) 0.3487(4) 0.8425(3) 0.0571(11) Uani 1 1 d . . .
C53 C -0.0901(5) 0.2453(5) 0.8459(3) 0.0687(14) Uani 1 1 d . . .
H53A H -0.1574 0.2342 0.8639 0.082 Uiso 1 1 calc R . .
C54 C 0.0109(5) 0.1652(4) 0.8239(3) 0.0644(13) Uani 1 1 d . . .
H54A H 0.0130 0.0988 0.8272 0.077 Uiso 1 1 calc R . .
C55 C 0.1156(4) 0.1784(3) 0.7956(2) 0.0466(9) Uani 1 1 d . . .
C56 C 0.2241(5) 0.0972(3) 0.7708(3) 0.0611(12) Uani 1 1 d . . .
H56A H 0.2303 0.0296 0.7727 0.073 Uiso 1 1 calc R . .
C57 C 0.3201(4) 0.1157(4) 0.7443(3) 0.0644(13) Uani 1 1 d . . .
H57A H 0.3921 0.0608 0.7286 0.077 Uiso 1 1 calc R . .
C58 C 0.3123(4) 0.2152(3) 0.7404(3) 0.0545(10) Uani 1 1 d . . .
H58A H 0.3787 0.2277 0.7214 0.065 Uiso 1 1 calc R . .
C59 C 0.1105(3) 0.2789(3) 0.7915(2) 0.0373(7) Uani 1 1 d . . .
C60 C 0.0032(3) 0.3669(3) 0.8155(2) 0.0410(8) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O2W H2WA 0.8499 . ?
Yb O5 2.253(2) . ?
Yb O4 2.274(2) 2_666 ?
Yb O6 2.307(2) 2_666 ?
Yb O3 2.368(2) . ?
Yb O2 2.411(2) . ?
Yb O1 2.457(2) . ?
Yb N1 2.507(3) . ?
Yb N2 2.562(3) . ?
Yb O4 2.573(2) . ?
Yb Yb 3.8797(13) 2_666 ?
O1 C13 1.252(4) . ?
O2 C13 1.268(4) . ?
O3 C25 1.241(4) . ?
O4 C25 1.261(4) . ?
O4 Yb 2.274(2) 2_666 ?
O5 C37 1.253(4) . ?
O6 C37 1.260(4) . ?
O6 Yb 2.307(2) 2_666 ?
O7 N8 1.229(7) . ?
O8 N8 1.221(6) . ?
O9 N8 1.216(7) . ?
N1 C10 1.324(5) . ?
N1 C11 1.361(4) . ?
N2 C1 1.322(4) . ?
N2 C12 1.354(4) . ?
N3 C19 1.369(6) . ?
N3 C18 1.374(6) . ?
N4 C30 1.361(7) . ?
N4 C31 1.365(7) . ?
N5 C43 1.359(6) . ?
N5 C42 1.371(5) . ?
N6 C49 1.321(6) . ?
N6 C60 1.345(5) . ?
N7 C58 1.327(5) . ?
N7 C59 1.357(5) . ?
C1 C2 1.402(5) . ?
C2 C3 1.355(6) . ?
C3 C4 1.396(6) . ?
C4 C12 1.412(4) . ?
C4 C5 1.425(6) . ?
C5 C6 1.349(7) . ?
C6 C7 1.433(6) . ?
C7 C8 1.374(6) . ?
C7 C11 1.415(4) . ?
C8 C9 1.363(6) . ?
C9 C10 1.399(5) . ?
C11 C12 1.437(5) . ?
C13 C14 1.513(4) . ?
C14 C15 1.512(5) . ?
C15 C16 1.518(5) . ?
C16 C17 1.491(6) . ?
C17 C18 1.349(7) . ?
C17 C24 1.428(6) . ?
C19 C24 1.393(6) . ?
C19 C20 1.398(6) . ?
C20 C21 1.365(10) . ?
C21 C22 1.377(10) . ?
C22 C23 1.385(8) . ?
C23 C24 1.383(7) . ?
C25 C26 1.507(5) . ?
C26 C27 1.545(6) . ?
C27 C28 1.480(7) . ?
C28 C29 1.523(7) . ?
C29 C30 1.355(7) . ?
C29 C36 1.428(7) . ?
C31 C32 1.390(8) . ?
C31 C36 1.402(7) . ?
C32 C33 1.368(10) . ?
C33 C34 1.377(11) . ?
C34 C35 1.361(10) . ?
C35 C36 1.398(7) . ?
C37 C38 1.526(4) . ?
C38 C39 1.513(4) . ?
C39 C40 1.519(5) . ?
C40 C41 1.491(5) . ?
C41 C42 1.362(6) . ?
C41 C48 1.423(5) . ?
C43 C44 1.391(6) . ?
C43 C48 1.418(5) . ?
C44 C45 1.369(8) . ?
C45 C46 1.398(9) . ?
C46 C47 1.403(7) . ?
C47 C48 1.389(6) . ?
C49 C50 1.415(8) . ?
C50 C51 1.349(9) . ?
C51 C52 1.396(8) . ?
C52 C60 1.402(6) . ?
C52 C53 1.432(8) . ?
C53 C54 1.325(8) . ?
C54 C55 1.417(6) . ?
C55 C56 1.395(7) . ?
C55 C59 1.400(5) . ?
C56 C57 1.347(7) . ?
C57 C58 1.372(7) . ?
C59 C60 1.428(5) . ?

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
O5 Yb O4 75.53(9) . 2_666 ?
O5 Yb O6 137.32(8) . 2_666 ?
O4 Yb O6 75.85(8) 2_666 2_666 ?
O5 Yb O3 78.98(10) . . ?
O4 Yb O3 124.98(8) 2_666 . ?
O6 Yb O3 92.43(10) 2_666 . ?
O5 Yb O2 127.89(8) . . ?
O4 Yb O2 91.37(9) 2_666 . ?
O6 Yb O2 83.63(9) 2_666 . ?
O3 Yb O2 141.36(8) . . ?
O5 Yb O1 74.84(8) . . ?
O4 Yb O1 74.09(8) 2_666 . ?
O6 Yb O1 125.48(9) 2_666 . ?
O3 Yb O1 141.93(9) . . ?
O2 Yb O1 53.13(8) . . ?
O5 Yb N1 78.45(9) . . ?
O4 Yb N1 139.72(9) 2_666 . ?
O6 Yb N1 141.07(8) 2_666 . ?
O3 Yb N1 78.38(9) . . ?
O2 Yb N1 80.93(9) . . ?
O1 Yb N1 69.71(9) . . ?
O5 Yb N2 135.19(9) . . ?
O4 Yb N2 149.15(9) 2_666 . ?
O6 Yb N2 76.64(8) 2_666 . ?
O3 Yb N2 69.79(9) . . ?
O2 Yb N2 71.91(9) . . ?
O1 Yb N2 112.02(8) . . ?
N1 Yb N2 64.63(9) . . ?
O5 Yb O4 69.81(8) . . ?
O4 Yb O4 73.83(9) 2_666 . ?
O6 Yb O4 72.22(8) 2_666 . ?
O3 Yb O4 51.67(8) . . ?
O2 Yb O4 154.01(8) . . ?
O1 Yb O4 136.88(7) . . ?
N1 Yb O4 124.12(8) . . ?
N2 Yb O4 110.35(8) . . ?
O5 Yb Yb 67.96(6) . 2_666 ?
O4 Yb Yb 39.57(6) 2_666 2_666 ?
O6 Yb Yb 69.76(6) 2_666 2_666 ?
O3 Yb Yb 85.68(6) . 2_666 ?
O2 Yb Yb 127.61(7) . 2_666 ?
O1 Yb Yb 108.88(6) . 2_666 ?
N1 Yb Yb 145.01(6) . 2_666 ?
N2 Yb Yb 137.21(6) . 2_666 ?
O4 Yb Yb 34.26(5) . 2_666 ?
C13 O1 Yb 92.74(19) . . ?
C13 O2 Yb 94.50(19) . . ?
C25 O3 Yb 99.5(2) . . ?
C25 O4 Yb 161.6(2) . 2_666 ?
C25 O4 Yb 89.11(19) . . ?
Yb O4 Yb 106.17(9) 2_666 . ?
C37 O5 Yb 139.4(2) . . ?
C37 O6 Yb 134.37(19) . 2_666 ?
C10 N1 C11 117.4(3) . . ?
C10 N1 Yb 122.0(2) . . ?
C11 N1 Yb 120.4(2) . . ?
C1 N2 C12 117.3(3) . . ?
C1 N2 Yb 123.9(2) . . ?
C12 N2 Yb 118.8(2) . . ?
C19 N3 C18 107.2(4) . . ?
C30 N4 C31 109.5(4) . . ?
C43 N5 C42 108.3(3) . . ?
C49 N6 C60 117.0(4) . . ?
C58 N7 C59 122.2(3) . . ?
O9 N8 O8 120.4(6) . . ?
O9 N8 O7 121.8(6) . . ?
O8 N8 O7 117.8(6) . . ?
N2 C1 C2 123.7(4) . . ?
C3 C2 C1 118.8(4) . . ?
C2 C3 C4 119.8(3) . . ?
C3 C4 C12 117.5(3) . . ?
C3 C4 C5 123.0(3) . . ?
C12 C4 C5 119.5(4) . . ?
C6 C5 C4 121.3(3) . . ?
C5 C6 C7 121.2(4) . . ?
C8 C7 C11 117.9(3) . . ?
C8 C7 C6 123.1(4) . . ?
C11 C7 C6 118.9(4) . . ?
C9 C8 C7 120.1(4) . . ?
C8 C9 C10 118.8(4) . . ?
N1 C10 C9 123.4(4) . . ?
N1 C11 C7 122.2(3) . . ?
N1 C11 C12 118.0(3) . . ?
C7 C11 C12 119.8(3) . . ?
N2 C12 C4 122.7(3) . . ?
N2 C12 C11 117.9(3) . . ?
C4 C12 C11 119.3(3) . . ?
O1 C13 O2 119.6(3) . . ?
O1 C13 C14 120.1(3) . . ?
O2 C13 C14 120.3(3) . . ?
C15 C14 C13 114.4(3) . . ?
C14 C15 C16 112.2(3) . . ?
C17 C16 C15 115.2(3) . . ?
C18 C17 C24 105.8(4) . . ?
C18 C17 C16 126.6(4) . . ?
C24 C17 C16 127.6(4) . . ?
C17 C18 N3 111.4(4) . . ?
N3 C19 C24 108.4(4) . . ?
N3 C19 C20 128.2(5) . . ?
C24 C19 C20 123.3(5) . . ?
C21 C20 C19 116.2(6) . . ?
C20 C21 C22 121.9(6) . . ?
C21 C22 C23 121.5(6) . . ?
C24 C23 C22 118.6(5) . . ?
C23 C24 C19 118.5(4) . . ?
C23 C24 C17 134.3(5) . . ?
C19 C24 C17 107.2(4) . . ?
O3 C25 O4 119.6(3) . . ?
O3 C25 C26 119.8(3) . . ?
O4 C25 C26 120.6(3) . . ?
C25 C26 C27 111.9(3) . . ?
C28 C27 C26 114.2(4) . . ?
C27 C28 C29 113.3(4) . . ?
C30 C29 C36 106.4(5) . . ?
C30 C29 C28 125.2(5) . . ?
C36 C29 C28 128.3(4) . . ?
C29 C30 N4 110.0(5) . . ?
N4 C31 C32 131.3(5) . . ?
N4 C31 C36 107.0(5) . . ?
C32 C31 C36 121.6(5) . . ?
C33 C32 C31 117.3(6) . . ?
C32 C33 C34 122.0(7) . . ?
C35 C34 C33 121.1(7) . . ?
C34 C35 C36 119.0(6) . . ?
C35 C36 C31 118.9(5) . . ?
C35 C36 C29 133.9(5) . . ?
C31 C36 C29 107.2(4) . . ?
O5 C37 O6 126.9(3) . . ?
O5 C37 C38 114.4(3) . . ?
O6 C37 C38 118.7(3) . . ?
C39 C38 C37 117.2(3) . . ?
C38 C39 C40 110.8(3) . . ?
C41 C40 C39 113.8(3) . . ?
C42 C41 C48 106.0(3) . . ?
C42 C41 C40 126.9(4) . . ?
C48 C41 C40 127.1(4) . . ?
C41 C42 N5 110.9(4) . . ?
N5 C43 C44 129.3(4) . . ?
N5 C43 C48 107.9(4) . . ?
C44 C43 C48 122.8(4) . . ?
C45 C44 C43 116.6(5) . . ?
C44 C45 C46 122.6(5) . . ?
C45 C46 C47 120.5(5) . . ?
C48 C47 C46 118.4(5) . . ?
C47 C48 C43 119.1(4) . . ?
C47 C48 C41 134.0(4) . . ?
C43 C48 C41 106.9(4) . . ?
N6 C49 C50 122.6(5) . . ?
C51 C50 C49 119.5(5) . . ?
C50 C51 C52 119.7(5) . . ?
C51 C52 C60 116.6(5) . . ?
C51 C52 C53 123.2(5) . . ?
C60 C52 C53 120.2(5) . . ?
C54 C53 C52 121.1(4) . . ?
C53 C54 C55 121.4(4) . . ?
C56 C55 C59 117.7(4) . . ?
C56 C55 C54 123.9(4) . . ?
C59 C55 C54 118.4(4) . . ?
C57 C56 C55 120.6(4) . . ?
C56 C57 C58 120.3(4) . . ?
N7 C58 C57 119.9(4) . . ?
N7 C59 C55 119.3(4) . . ?
N7 C59 C60 119.0(3) . . ?
C55 C59 C60 121.7(4) . . ?
N6 C60 C52 124.5(4) . . ?
N6 C60 C59 118.3(3) . . ?
C52 C60 C59 117.2(4) . . ?

_diffrn_measured_fraction_theta_max 0.972
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.972
_refine_diff_density_max         1.091
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.134
####################################################################### 
# 
# 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_x
_database_code_depnum_ccdc_archive 'CCDC 1044889'
_audit_update_record             
;
2015-11-09 deposited with the CCDC.
2015-11-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C96 H80 N14 O14 Sm2'
_chemical_formula_weight         1954.44

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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

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

_cell_length_a                   11.7356(10)
_cell_length_b                   13.5161(11)
_cell_length_c                   13.8113(11)
_cell_angle_alpha                101.229(2)
_cell_angle_beta                 98.590(2)
_cell_angle_gamma                100.386(2)
_cell_volume                     2074.6(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1874
_cell_measurement_theta_min      1.53
_cell_measurement_theta_max      28.22

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             990
_exptl_absorpt_coefficient_mu    1.479
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5558
_exptl_absorpt_correction_T_max  0.8310
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker AXS SMART APEX II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            11109
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_sigmaI/netI    0.0887
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.53
_diffrn_reflns_theta_max         25.00
_reflns_number_total             7226
_reflns_number_gt                6059
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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)+(0.0460P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7226
_refine_ls_number_parameters     587
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0498
_refine_ls_wR_factor_ref         0.1247
_refine_ls_wR_factor_gt          0.1060
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.036
_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
O7 O 0.1297(14) 0.1865(12) 0.2310(10) 0.133(6) Uani 0.584(19) 1 d PDU A 1
O5 O 0.2286(17) 0.0782(13) 0.2166(13) 0.159(7) Uani 0.584(19) 1 d PDU A 1
O7B O 0.203(3) 0.2126(11) 0.1850(18) 0.138(9) Uani 0.416(19) 1 d PDU A 2
O5B O 0.2660(11) 0.143(3) 0.1716(17) 0.188(15) Uani 0.416(19) 1 d PD A 2
Sm1 Sm 0.58332(3) 0.14278(2) 0.52068(2) 0.03988(12) Uani 1 1 d . . .
O1 O 0.5354(4) 0.1096(3) 0.6753(3) 0.0459(10) Uani 1 1 d . . .
O2 O 0.4511(4) -0.0575(3) 0.6499(3) 0.0482(10) Uani 1 1 d . . .
O3 O 0.3871(4) 0.1882(3) 0.5174(3) 0.0543(11) Uani 1 1 d . . .
O4 O 0.3757(3) 0.0218(3) 0.4740(3) 0.0433(9) Uani 1 1 d . . .
N1 N 0.7797(4) 0.2085(4) 0.4555(4) 0.0489(13) Uani 1 1 d . . .
N2 N 0.7901(4) 0.1813(4) 0.6451(3) 0.0465(12) Uani 1 1 d . . .
N3 N 0.6342(4) 0.3340(3) 0.6257(3) 0.0432(12) Uani 1 1 d . . .
N4 N 0.5633(5) 0.2911(4) 0.4212(3) 0.0477(12) Uani 1 1 d . . .
N5 N 0.8653(6) 0.1482(5) 1.0691(4) 0.0687(16) Uani 1 1 d . . .
H5A H 0.9236 0.1191 1.0813 0.082 Uiso 1 1 calc R . .
N6 N 0.1371(6) 0.1277(6) 0.9056(5) 0.084(2) Uani 1 1 d . . .
H6A H 0.1066 0.1137 0.9556 0.101 Uiso 1 1 calc R . .
C1 C 0.7805(6) 0.2141(5) 0.3602(5) 0.0604(18) Uani 1 1 d . . .
H1A H 0.7183 0.1734 0.3104 0.072 Uiso 1 1 calc R . .
C2 C 0.8702(8) 0.2780(7) 0.3322(6) 0.081(2) Uani 1 1 d . . .
H2A H 0.8689 0.2788 0.2648 0.097 Uiso 1 1 calc R . .
C3 C 0.9594(7) 0.3391(7) 0.4044(7) 0.083(2) Uani 1 1 d . . .
H3A H 1.0179 0.3846 0.3867 0.100 Uiso 1 1 calc R . .
C4 C 0.9647(6) 0.3349(5) 0.5045(5) 0.0579(17) Uani 1 1 d . . .
C5 C 1.0571(7) 0.3950(6) 0.5853(7) 0.079(2) Uani 1 1 d . . .
H5B H 1.1146 0.4450 0.5721 0.095 Uiso 1 1 calc R . .
C6 C 1.0632(6) 0.3814(6) 0.6791(7) 0.074(2) Uani 1 1 d . . .
H6B H 1.1259 0.4204 0.7293 0.089 Uiso 1 1 calc R . .
C7 C 0.9751(5) 0.3084(5) 0.7032(5) 0.0515(16) Uani 1 1 d . . .
C8 C 0.9796(6) 0.2845(6) 0.7985(5) 0.067(2) Uani 1 1 d . . .
H8A H 1.0410 0.3205 0.8512 0.081 Uiso 1 1 calc R . .
C9 C 0.8963(6) 0.2105(6) 0.8138(5) 0.065(2) Uani 1 1 d . . .
H9A H 0.9007 0.1933 0.8760 0.078 Uiso 1 1 calc R . .
C10 C 0.8030(6) 0.1596(5) 0.7350(5) 0.0552(17) Uani 1 1 d . . .
H10A H 0.7465 0.1075 0.7462 0.066 Uiso 1 1 calc R . .
C11 C 0.8784(5) 0.2527(5) 0.6285(4) 0.0446(14) Uani 1 1 d . . .
C12 C 0.8727(5) 0.2659(5) 0.5273(5) 0.0478(15) Uani 1 1 d . . .
C13 C 0.5204(6) 0.2705(5) 0.3229(5) 0.0604(18) Uani 1 1 d . . .
H13A H 0.4853 0.2027 0.2896 0.072 Uiso 1 1 calc R . .
C14 C 0.5263(8) 0.3478(6) 0.2677(5) 0.073(2) Uani 1 1 d . . .
H14A H 0.4966 0.3309 0.1988 0.088 Uiso 1 1 calc R . .
C15 C 0.5749(7) 0.4463(6) 0.3151(6) 0.070(2) Uani 1 1 d . . .
H15A H 0.5816 0.4972 0.2784 0.084 Uiso 1 1 calc R . .
C16 C 0.6164(6) 0.4732(5) 0.4208(5) 0.0544(17) Uani 1 1 d . . .
C17 C 0.6606(6) 0.5773(5) 0.4772(6) 0.065(2) Uani 1 1 d . . .
H17A H 0.6635 0.6312 0.4442 0.078 Uiso 1 1 calc R . .
C18 C 0.6977(6) 0.5981(5) 0.5767(6) 0.066(2) Uani 1 1 d . . .
H18A H 0.7279 0.6662 0.6118 0.079 Uiso 1 1 calc R . .
C19 C 0.6916(6) 0.5172(5) 0.6305(5) 0.0543(17) Uani 1 1 d . . .
C20 C 0.7237(6) 0.5361(5) 0.7352(6) 0.066(2) Uani 1 1 d . . .
H20A H 0.7557 0.6031 0.7725 0.079 Uiso 1 1 calc R . .
C21 C 0.7085(7) 0.4573(6) 0.7824(5) 0.069(2) Uani 1 1 d . . .
H21A H 0.7277 0.4693 0.8521 0.082 Uiso 1 1 calc R . .
C22 C 0.6633(6) 0.3579(5) 0.7239(5) 0.0566(17) Uani 1 1 d . . .
H22A H 0.6529 0.3043 0.7571 0.068 Uiso 1 1 calc R . .
C23 C 0.6476(5) 0.4137(4) 0.5771(5) 0.0453(14) Uani 1 1 d . . .
C24 C 0.6088(5) 0.3915(4) 0.4702(5) 0.0439(14) Uani 1 1 d . . .
C25 C 0.5014(5) 0.0296(4) 0.7064(4) 0.0414(14) Uani 1 1 d . . .
C26 C 0.5228(6) 0.0364(5) 0.8183(4) 0.0518(17) Uani 1 1 d . . .
H26A H 0.6019 0.0264 0.8390 0.062 Uiso 1 1 calc R . .
H26B H 0.4679 -0.0199 0.8316 0.062 Uiso 1 1 calc R . .
C27 C 0.5103(6) 0.1372(5) 0.8831(4) 0.0558(17) Uani 1 1 d . . .
H27A H 0.4285 0.1428 0.8696 0.067 Uiso 1 1 calc R . .
H27B H 0.5572 0.1943 0.8637 0.067 Uiso 1 1 calc R . .
C28 C 0.5487(6) 0.1472(5) 0.9957(4) 0.0532(16) Uani 1 1 d . . .
H28A H 0.5191 0.2030 1.0321 0.064 Uiso 1 1 calc R . .
H28B H 0.5133 0.0839 1.0129 0.064 Uiso 1 1 calc R . .
C29 C 0.6794(6) 0.1677(5) 1.0292(4) 0.0512(16) Uani 1 1 d . . .
C30 C 0.7471(7) 0.0992(6) 1.0441(5) 0.067(2) Uani 1 1 d . . .
H30A H 0.7185 0.0291 1.0384 0.080 Uiso 1 1 calc R . .
C31 C 0.8734(6) 0.2514(6) 1.0711(4) 0.0564(17) Uani 1 1 d . . .
C32 C 0.9722(7) 0.3304(6) 1.0917(5) 0.069(2) Uani 1 1 d . . .
H32A H 1.0479 0.3193 1.1078 0.083 Uiso 1 1 calc R . .
C33 C 0.9524(8) 0.4254(7) 1.0870(6) 0.085(3) Uani 1 1 d . . .
H33A H 1.0171 0.4806 1.1009 0.102 Uiso 1 1 calc R . .
C34 C 0.8396(8) 0.4444(6) 1.0622(6) 0.081(2) Uani 1 1 d . . .
H34A H 0.8303 0.5108 1.0600 0.097 Uiso 1 1 calc R . .
C35 C 0.7427(7) 0.3642(5) 1.0413(5) 0.0624(19) Uani 1 1 d . . .
H35A H 0.6673 0.3759 1.0243 0.075 Uiso 1 1 calc R . .
C36 C 0.7581(6) 0.2656(5) 1.0457(4) 0.0517(16) Uani 1 1 d . . .
C37 C 0.3260(5) 0.0991(5) 0.4873(4) 0.0434(14) Uani 1 1 d . . .
C38 C 0.1928(6) 0.0810(5) 0.4671(5) 0.0557(17) Uani 1 1 d . . .
H38A H 0.1593 0.0076 0.4428 0.067 Uiso 1 1 calc R . .
H38B H 0.1670 0.1158 0.4154 0.067 Uiso 1 1 calc R . .
C39 C 0.1486(6) 0.1213(5) 0.5623(5) 0.0589(17) Uani 1 1 d . . .
H39A H 0.0635 0.1130 0.5467 0.071 Uiso 1 1 calc R . .
H39B H 0.1832 0.1944 0.5874 0.071 Uiso 1 1 calc R . .
C40 C 0.1809(7) 0.0632(6) 0.6434(5) 0.069(2) Uani 1 1 d . . .
H40A H 0.1294 -0.0050 0.6244 0.083 Uiso 1 1 calc R . .
H40B H 0.2609 0.0539 0.6428 0.083 Uiso 1 1 calc R . .
C41 C 0.1740(7) 0.1108(6) 0.7488(5) 0.0646(19) Uani 1 1 d . . .
C42 C 0.1106(7) 0.0669(6) 0.8105(7) 0.076(2) Uani 1 1 d . . .
H42A H 0.0565 0.0040 0.7904 0.091 Uiso 1 1 calc R . .
C43 C 0.2198(8) 0.2144(7) 0.9089(6) 0.073(2) Uani 1 1 d . . .
C44 C 0.2775(10) 0.2949(9) 0.9893(7) 0.098(3) Uani 1 1 d . . .
H44A H 0.2622 0.2971 1.0537 0.118 Uiso 1 1 calc R . .
C45 C 0.3586(10) 0.3715(8) 0.9693(8) 0.102(3) Uani 1 1 d . . .
H45A H 0.3974 0.4280 1.0209 0.123 Uiso 1 1 calc R . .
C46 C 0.3838(9) 0.3661(7) 0.8730(8) 0.095(3) Uani 1 1 d . . .
H46A H 0.4404 0.4184 0.8621 0.114 Uiso 1 1 calc R . .
C47 C 0.3269(7) 0.2854(7) 0.7939(6) 0.076(2) Uani 1 1 d . . .
H47A H 0.3445 0.2835 0.7302 0.091 Uiso 1 1 calc R . .
C48 C 0.2428(7) 0.2066(6) 0.8096(5) 0.0645(19) Uani 1 1 d . . .
O6 O 0.0899(5) 0.0762(5) 0.0953(4) 0.0855(17) Uani 1 1 d D A .
N7 N 0.1668(7) 0.1257(6) 0.1695(6) 0.093(2) Uani 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O7 N7 1.246(6) . ?
O5 N7 1.246(6) . ?
O7B N7 1.139(12) . ?
O7B O5B 1.31(4) . ?
O5B N7 1.140(12) . ?
Sm1 O2 2.352(4) 2_656 ?
Sm1 O4 2.372(4) 2_656 ?
Sm1 O1 2.392(4) . ?
Sm1 O3 2.484(4) . ?
Sm1 O4 2.590(4) . ?
Sm1 N3 2.619(4) . ?
Sm1 N2 2.657(5) . ?
Sm1 N1 2.666(5) . ?
Sm1 N4 2.666(5) . ?
Sm1 Sm1 3.8903(6) 2_656 ?
O1 C25 1.261(6) . ?
O2 C25 1.264(6) . ?
O2 Sm1 2.352(4) 2_656 ?
O3 C37 1.242(6) . ?
O4 C37 1.281(7) . ?
O4 Sm1 2.372(4) 2_656 ?
N1 C1 1.334(7) . ?
N1 C12 1.359(7) . ?
N2 C10 1.324(7) . ?
N2 C11 1.361(7) . ?
N3 C22 1.309(7) . ?
N3 C23 1.374(7) . ?
N4 C13 1.331(7) . ?
N4 C24 1.363(7) . ?
N5 C31 1.374(9) . ?
N5 C30 1.385(9) . ?
N6 C42 1.365(10) . ?
N6 C43 1.368(10) . ?
C1 C2 1.389(9) . ?
C2 C3 1.353(11) . ?
C3 C4 1.388(10) . ?
C4 C12 1.411(8) . ?
C4 C5 1.431(10) . ?
C5 C6 1.337(11) . ?
C6 C7 1.420(9) . ?
C7 C11 1.400(8) . ?
C7 C8 1.410(9) . ?
C8 C9 1.339(10) . ?
C9 C10 1.391(9) . ?
C11 C12 1.436(8) . ?
C13 C14 1.407(9) . ?
C14 C15 1.341(10) . ?
C15 C16 1.420(9) . ?
C16 C24 1.404(8) . ?
C16 C17 1.430(9) . ?
C17 C18 1.336(10) . ?
C18 C19 1.434(9) . ?
C19 C20 1.399(9) . ?
C19 C23 1.411(8) . ?
C20 C21 1.352(10) . ?
C21 C22 1.390(9) . ?
C23 C24 1.433(8) . ?
C25 C26 1.510(7) . ?
C26 C27 1.521(8) . ?
C27 C28 1.526(8) . ?
C28 C29 1.492(9) . ?
C29 C30 1.349(9) . ?
C29 C36 1.427(9) . ?
C31 C32 1.379(9) . ?
C31 C36 1.404(9) . ?
C32 C33 1.357(11) . ?
C33 C34 1.399(12) . ?
C34 C35 1.374(10) . ?
C35 C36 1.388(9) . ?
C37 C38 1.513(9) . ?
C38 C39 1.523(8) . ?
C39 C40 1.529(9) . ?
C40 C41 1.494(9) . ?
C41 C42 1.362(9) . ?
C41 C48 1.425(10) . ?
C43 C44 1.384(12) . ?
C43 C48 1.425(10) . ?
C44 C45 1.374(13) . ?
C45 C46 1.396(13) . ?
C46 C47 1.372(11) . ?
C47 C48 1.390(10) . ?
O6 N7 1.246(6) . ?

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
N7 O7B O5B 55.0(11) . . ?
N7 O5B O7B 55.0(11) . . ?
O2 Sm1 O4 76.48(13) 2_656 2_656 ?
O2 Sm1 O1 138.77(13) 2_656 . ?
O4 Sm1 O1 74.82(13) 2_656 . ?
O2 Sm1 O3 96.34(15) 2_656 . ?
O4 Sm1 O3 125.87(13) 2_656 . ?
O1 Sm1 O3 77.65(14) . . ?
O2 Sm1 O4 71.09(12) 2_656 . ?
O4 Sm1 O4 76.82(15) 2_656 . ?
O1 Sm1 O4 73.98(12) . . ?
O3 Sm1 O4 50.98(13) . . ?
O2 Sm1 N3 137.14(14) 2_656 . ?
O4 Sm1 N3 141.45(14) 2_656 . ?
O1 Sm1 N3 81.78(13) . . ?
O3 Sm1 N3 76.63(14) . . ?
O4 Sm1 N3 125.42(14) . . ?
O2 Sm1 N2 124.10(15) 2_656 . ?
O4 Sm1 N2 74.84(14) 2_656 . ?
O1 Sm1 N2 75.21(14) . . ?
O3 Sm1 N2 139.13(15) . . ?
O4 Sm1 N2 142.46(13) . . ?
N3 Sm1 N2 69.75(15) . . ?
O2 Sm1 N1 74.55(14) 2_656 . ?
O4 Sm1 N1 94.11(15) 2_656 . ?
O1 Sm1 N1 136.19(14) . . ?
O3 Sm1 N1 136.29(15) . . ?
O4 Sm1 N1 145.61(14) . . ?
N3 Sm1 N1 81.94(15) . . ?
N2 Sm1 N1 61.01(15) . . ?
O2 Sm1 N4 75.57(14) 2_656 . ?
O4 Sm1 N4 149.81(14) 2_656 . ?
O1 Sm1 N4 135.05(14) . . ?
O3 Sm1 N4 68.77(14) . . ?
O4 Sm1 N4 104.39(14) . . ?
N3 Sm1 N4 62.37(14) . . ?
N2 Sm1 N4 112.51(15) . . ?
N1 Sm1 N4 67.56(16) . . ?
O2 Sm1 Sm1 69.01(9) 2_656 2_656 ?
O4 Sm1 Sm1 40.40(9) 2_656 2_656 ?
O1 Sm1 Sm1 69.92(9) . 2_656 ?
O3 Sm1 Sm1 86.45(9) . 2_656 ?
O4 Sm1 Sm1 36.41(9) . 2_656 ?
N3 Sm1 Sm1 149.61(10) . 2_656 ?
N2 Sm1 Sm1 111.61(10) . 2_656 ?
N1 Sm1 Sm1 126.37(11) . 2_656 ?
N4 Sm1 Sm1 133.82(11) . 2_656 ?
C25 O1 Sm1 135.1(4) . . ?
C25 O2 Sm1 139.4(3) . 2_656 ?
C37 O3 Sm1 97.4(4) . . ?
C37 O4 Sm1 160.0(4) . 2_656 ?
C37 O4 Sm1 91.4(3) . . ?
Sm1 O4 Sm1 103.18(15) 2_656 . ?
C1 N1 C12 118.2(5) . . ?
C1 N1 Sm1 123.0(4) . . ?
C12 N1 Sm1 115.9(4) . . ?
C10 N2 C11 116.9(5) . . ?
C10 N2 Sm1 123.5(4) . . ?
C11 N2 Sm1 116.7(4) . . ?
C22 N3 C23 117.3(5) . . ?
C22 N3 Sm1 122.5(4) . . ?
C23 N3 Sm1 119.6(4) . . ?
C13 N4 C24 118.3(5) . . ?
C13 N4 Sm1 122.4(4) . . ?
C24 N4 Sm1 119.0(4) . . ?
C31 N5 C30 108.3(6) . . ?
C42 N6 C43 109.2(7) . . ?
N1 C1 C2 122.8(7) . . ?
C3 C2 C1 118.9(7) . . ?
C2 C3 C4 120.8(7) . . ?
C3 C4 C12 117.2(7) . . ?
C3 C4 C5 124.5(7) . . ?
C12 C4 C5 118.3(7) . . ?
C6 C5 C4 122.0(7) . . ?
C5 C6 C7 120.9(7) . . ?
C11 C7 C8 116.3(6) . . ?
C11 C7 C6 119.4(6) . . ?
C8 C7 C6 124.2(6) . . ?
C9 C8 C7 120.6(6) . . ?
C8 C9 C10 119.0(7) . . ?
N2 C10 C9 123.7(6) . . ?
N2 C11 C7 123.3(6) . . ?
N2 C11 C12 116.9(5) . . ?
C7 C11 C12 119.7(6) . . ?
N1 C12 C4 121.9(6) . . ?
N1 C12 C11 118.6(5) . . ?
C4 C12 C11 119.5(6) . . ?
N4 C13 C14 122.3(7) . . ?
C15 C14 C13 119.5(7) . . ?
C14 C15 C16 120.5(6) . . ?
C24 C16 C15 116.5(6) . . ?
C24 C16 C17 120.0(6) . . ?
C15 C16 C17 123.5(6) . . ?
C18 C17 C16 120.8(6) . . ?
C17 C18 C19 121.1(7) . . ?
C20 C19 C23 117.7(6) . . ?
C20 C19 C18 122.9(6) . . ?
C23 C19 C18 119.4(7) . . ?
C21 C20 C19 120.3(6) . . ?
C20 C21 C22 118.2(7) . . ?
N3 C22 C21 125.0(7) . . ?
N3 C23 C19 121.6(6) . . ?
N3 C23 C24 118.9(5) . . ?
C19 C23 C24 119.3(6) . . ?
N4 C24 C16 122.8(6) . . ?
N4 C24 C23 117.9(5) . . ?
C16 C24 C23 119.3(6) . . ?
O1 C25 O2 124.3(5) . . ?
O1 C25 C26 118.7(5) . . ?
O2 C25 C26 117.1(5) . . ?
C25 C26 C27 115.4(5) . . ?
C26 C27 C28 113.9(5) . . ?
C29 C28 C27 113.4(5) . . ?
C30 C29 C36 106.5(6) . . ?
C30 C29 C28 128.2(7) . . ?
C36 C29 C28 125.2(6) . . ?
C29 C30 N5 110.3(7) . . ?
N5 C31 C32 129.5(7) . . ?
N5 C31 C36 107.2(6) . . ?
C32 C31 C36 123.2(7) . . ?
C33 C32 C31 116.1(8) . . ?
C32 C33 C34 123.2(8) . . ?
C35 C34 C33 119.6(8) . . ?
C34 C35 C36 119.5(7) . . ?
C35 C36 C31 118.4(6) . . ?
C35 C36 C29 134.0(7) . . ?
C31 C36 C29 107.7(6) . . ?
O3 C37 O4 120.1(5) . . ?
O3 C37 C38 120.3(5) . . ?
O4 C37 C38 119.7(5) . . ?
C37 C38 C39 110.9(5) . . ?
C38 C39 C40 110.9(6) . . ?
C41 C40 C39 117.5(6) . . ?
C42 C41 C48 105.6(7) . . ?
C42 C41 C40 127.2(8) . . ?
C48 C41 C40 126.9(6) . . ?
C41 C42 N6 111.0(8) . . ?
N6 C43 C44 130.2(9) . . ?
N6 C43 C48 106.4(8) . . ?
C44 C43 C48 123.4(9) . . ?
C45 C44 C43 116.8(9) . . ?
C44 C45 C46 121.3(10) . . ?
C47 C46 C45 121.5(10) . . ?
C46 C47 C48 119.6(8) . . ?
C47 C48 C43 117.3(8) . . ?
C47 C48 C41 134.7(7) . . ?
C43 C48 C41 107.9(7) . . ?
O7B N7 O5B 70(2) . . ?
O7B N7 O5 115.0(17) . . ?
O5B N7 O5 61.4(18) . . ?
O7B N7 O6 123.7(15) . . ?
O5B N7 O6 125.4(14) . . ?
O5 N7 O6 119.0(11) . . ?
O7B N7 O7 59.3(14) . . ?
O5B N7 O7 116.7(19) . . ?
O5 N7 O7 108.7(13) . . ?
O6 N7 O7 113.7(10) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.197
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.149
####################################################################### 
# 
# 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_bai-480
_database_code_depnum_ccdc_archive 'CCDC 1044890'
_audit_update_record             
;
2015-11-09 deposited with the CCDC.
2015-11-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C96 H88 Eu2 N10 O12'
_chemical_formula_weight         1877.68

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   13.811(3)
_cell_length_b                   18.430(4)
_cell_length_c                   17.214(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.47(3)
_cell_angle_gamma                90.00
_cell_volume                     4201.7(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3850
_cell_measurement_theta_min      3.14
_cell_measurement_theta_max      27.47

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1912
_exptl_absorpt_coefficient_mu    1.549
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5555
_exptl_absorpt_correction_T_max  0.6536
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            39507
_diffrn_reflns_av_R_equivalents  0.1116
_diffrn_reflns_av_sigmaI/netI    0.0958
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.14
_diffrn_reflns_theta_max         27.47
_reflns_number_total             9560
_reflns_number_gt                6495
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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)+(0.0206P)²+1.3888P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9560
_refine_ls_number_parameters     541
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0485
_refine_ls_wR_factor_ref         0.0833
_refine_ls_wR_factor_gt          0.0745
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.013
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu1 Eu 0.129145(16) -0.010805(11) 0.471896(12) 0.02226(6) Uani 1 1 d . . .
O1 O 0.1562(3) -0.12830(17) 0.41604(18) 0.0389(8) Uani 1 1 d . . .
O2 O 0.2478(2) -0.11173(17) 0.54221(18) 0.0363(8) Uani 1 1 d . . .
O3 O 0.1170(2) 0.12195(16) 0.44467(17) 0.0337(8) Uani 1 1 d . . .
O4 O -0.0129(2) 0.08040(15) 0.48032(15) 0.0272(7) Uani 1 1 d . . .
O5 O 0.1613(2) 0.02971(16) 0.60944(16) 0.0311(7) Uani 1 1 d . . .
N1 N 0.1981(3) 0.0122(2) 0.3470(2) 0.0326(8) Uani 1 1 d . . .
N2 N 0.3125(3) 0.0411(2) 0.5013(2) 0.0319(9) Uani 1 1 d . . .
N3 N 0.2755(4) -0.2876(2) 0.1378(3) 0.0590(14) Uani 1 1 d . . .
H3A H 0.2961 -0.3098 0.1015 0.071 Uiso 1 1 calc R . .
N4 N 0.1899(4) 0.3312(2) 0.7887(2) 0.0517(12) Uani 1 1 d . . .
H4A H 0.1905 0.3493 0.8349 0.062 Uiso 1 1 calc R . .
N5 N 0.5857(4) 0.1348(3) 0.8507(3) 0.0590(13) Uani 1 1 d . . .
H5A H 0.6242 0.1711 0.8488 0.071 Uiso 1 1 calc R . .
C1 C 0.3690(4) 0.0561(3) 0.5757(3) 0.0403(12) Uani 1 1 d . . .
H1A H 0.3420 0.0471 0.6185 0.048 Uiso 1 1 calc R . .
C2 C 0.4655(4) 0.0844(3) 0.5935(3) 0.0422(13) Uani 1 1 d . . .
H2A H 0.5022 0.0933 0.6469 0.051 Uiso 1 1 calc R . .
C3 C 0.5066(4) 0.0992(3) 0.5312(3) 0.0450(13) Uani 1 1 d . . .
H3B H 0.5712 0.1184 0.5418 0.054 Uiso 1 1 calc R . .
C4 C 0.4496(3) 0.0848(3) 0.4518(3) 0.0344(11) Uani 1 1 d . . .
C5 C 0.4883(4) 0.0991(3) 0.3830(3) 0.0461(14) Uani 1 1 d . . .
H5B H 0.5526 0.1184 0.3915 0.055 Uiso 1 1 calc R . .
C6 C 0.4316(4) 0.0846(3) 0.3074(3) 0.0484(14) Uani 1 1 d . . .
H6B H 0.4572 0.0943 0.2640 0.058 Uiso 1 1 calc R . .
C7 C 0.3329(4) 0.0546(3) 0.2924(3) 0.0363(11) Uani 1 1 d . . .
C8 C 0.2711(4) 0.0387(3) 0.2141(3) 0.0473(14) Uani 1 1 d . . .
H8A H 0.2943 0.0480 0.1693 0.057 Uiso 1 1 calc R . .
C9 C 0.1781(4) 0.0098(3) 0.2037(3) 0.0536(14) Uani 1 1 d . . .
H9A H 0.1375 -0.0014 0.1520 0.064 Uiso 1 1 calc R . .
C10 C 0.1437(4) -0.0030(3) 0.2721(3) 0.0427(12) Uani 1 1 d . . .
H10A H 0.0799 -0.0230 0.2643 0.051 Uiso 1 1 calc R . .
C11 C 0.2921(3) 0.0400(2) 0.3580(3) 0.0292(10) Uani 1 1 d . . .
C12 C 0.3538(3) 0.0558(2) 0.4386(3) 0.0295(10) Uani 1 1 d . . .
C13 C 0.2194(3) -0.1517(3) 0.4798(3) 0.0322(11) Uani 1 1 d . . .
C14 C 0.2607(4) -0.2280(3) 0.4811(3) 0.0425(13) Uani 1 1 d . . .
H14A H 0.3328 -0.2269 0.5075 0.051 Uiso 1 1 calc R . .
H14B H 0.2298 -0.2584 0.5134 0.051 Uiso 1 1 calc R . .
C15 C 0.2431(4) -0.2621(3) 0.3981(3) 0.0458(13) Uani 1 1 d . . .
H15A H 0.1717 -0.2595 0.3695 0.055 Uiso 1 1 calc R . .
H15B H 0.2618 -0.3130 0.4046 0.055 Uiso 1 1 calc R . .
C16 C 0.3038(4) -0.2249(3) 0.3469(3) 0.0455(13) Uani 1 1 d . . .
H16A H 0.2971 -0.1728 0.3514 0.055 Uiso 1 1 calc R . .
H16B H 0.3746 -0.2369 0.3697 0.055 Uiso 1 1 calc R . .
C17 C 0.2734(4) -0.2447(3) 0.2595(3) 0.0445(14) Uani 1 1 d . . .
C18 C 0.3258(5) -0.2850(3) 0.2180(4) 0.0548(15) Uani 1 1 d . . .
H18A H 0.3874 -0.3075 0.2416 0.066 Uiso 1 1 calc R . .
C19 C 0.1872(5) -0.2496(3) 0.1236(3) 0.0470(14) Uani 1 1 d . . .
C20 C 0.1121(5) -0.2360(3) 0.0533(4) 0.0610(17) Uani 1 1 d . . .
H20A H 0.1161 -0.2546 0.0040 0.073 Uiso 1 1 calc R . .
C21 C 0.0313(5) -0.1945(4) 0.0573(4) 0.0678(18) Uani 1 1 d . . .
H21A H -0.0195 -0.1843 0.0101 0.081 Uiso 1 1 calc R . .
C22 C 0.0243(5) -0.1671(3) 0.1319(4) 0.0658(17) Uani 1 1 d . . .
H22A H -0.0314 -0.1395 0.1335 0.079 Uiso 1 1 calc R . .
C23 C 0.0991(4) -0.1809(3) 0.2025(3) 0.0502(14) Uani 1 1 d . . .
H23A H 0.0937 -0.1631 0.2516 0.060 Uiso 1 1 calc R . .
C24 C 0.1830(4) -0.2215(3) 0.1996(3) 0.0419(13) Uani 1 1 d . . .
C25 C 0.0335(3) 0.1333(2) 0.4597(2) 0.0272(10) Uani 1 1 d . . .
C26 C -0.0106(3) 0.2081(2) 0.4533(3) 0.0329(11) Uani 1 1 d . . .
H26A H -0.0791 0.2054 0.4575 0.039 Uiso 1 1 calc R . .
H26B H -0.0134 0.2284 0.4007 0.039 Uiso 1 1 calc R . .
C27 C 0.0522(4) 0.2582(3) 0.5202(3) 0.0444(13) Uani 1 1 d . . .
H27A H 0.1155 0.2695 0.5088 0.053 Uiso 1 1 calc R . .
H27B H 0.0160 0.3033 0.5197 0.053 Uiso 1 1 calc R . .
C28 C 0.0743(4) 0.2240(3) 0.6034(3) 0.0456(13) Uani 1 1 d . . .
H28A H 0.0108 0.2129 0.6144 0.055 Uiso 1 1 calc R . .
H28B H 0.1096 0.1786 0.6032 0.055 Uiso 1 1 calc R . .
C29 C 0.1367(4) 0.2710(3) 0.6710(3) 0.0430(13) Uani 1 1 d . . .
C30 C 0.1134(5) 0.2906(3) 0.7403(3) 0.0523(15) Uani 1 1 d . . .
H30A H 0.0541 0.2783 0.7526 0.063 Uiso 1 1 calc R . .
C31 C 0.2657(4) 0.3385(3) 0.7521(3) 0.0402(12) Uani 1 1 d . . .
C32 C 0.3559(4) 0.3740(3) 0.7774(3) 0.0512(15) Uani 1 1 d . . .
H32A H 0.3746 0.3985 0.8266 0.061 Uiso 1 1 calc R . .
C33 C 0.4179(5) 0.3722(3) 0.7281(4) 0.0642(17) Uani 1 1 d . . .
H33A H 0.4796 0.3963 0.7439 0.077 Uiso 1 1 calc R . .
C34 C 0.3903(5) 0.3353(4) 0.6551(4) 0.084(2) Uani 1 1 d . . .
H34A H 0.4337 0.3353 0.6225 0.101 Uiso 1 1 calc R . .
C35 C 0.3009(5) 0.2989(4) 0.6299(3) 0.0681(19) Uani 1 1 d . . .
H35A H 0.2842 0.2734 0.5812 0.082 Uiso 1 1 calc R . .
C36 C 0.2346(4) 0.3003(3) 0.6781(3) 0.0398(12) Uani 1 1 d . . .
C37 C 0.1068(3) 0.0399(2) 0.6564(2) 0.0266(10) Uani 1 1 d . . .
C38 C 0.1528(4) 0.0732(3) 0.7398(3) 0.0382(12) Uani 1 1 d . . .
H38A H 0.1467 0.0379 0.7800 0.046 Uiso 1 1 calc R . .
H38B H 0.1120 0.1148 0.7449 0.046 Uiso 1 1 calc R . .
C39 C 0.2628(4) 0.0977(3) 0.7614(3) 0.0424(13) Uani 1 1 d . . .
H39A H 0.2752 0.1193 0.7137 0.051 Uiso 1 1 calc R . .
H39B H 0.2731 0.1352 0.8025 0.051 Uiso 1 1 calc R . .
C40 C 0.3399(4) 0.0380(3) 0.7923(3) 0.0452(13) Uani 1 1 d . . .
H40A H 0.3225 0.0122 0.8356 0.054 Uiso 1 1 calc R . .
H40B H 0.3360 0.0037 0.7487 0.054 Uiso 1 1 calc R . .
C41 C 0.4466(4) 0.0649(3) 0.8231(3) 0.0391(12) Uani 1 1 d . . .
C42 C 0.4855(4) 0.1288(3) 0.8074(3) 0.0492(14) Uani 1 1 d . . .
H42A H 0.4494 0.1640 0.7722 0.059 Uiso 1 1 calc R . .
C43 C 0.6140(4) 0.0743(3) 0.8968(3) 0.0474(14) Uani 1 1 d . . .
C44 C 0.7069(4) 0.0566(4) 0.9528(4) 0.0635(17) Uani 1 1 d . . .
H44A H 0.7624 0.0874 0.9632 0.076 Uiso 1 1 calc R . .
C45 C 0.7104(5) -0.0088(4) 0.9910(4) 0.075(2) Uani 1 1 d . . .
H45A H 0.7701 -0.0221 1.0292 0.090 Uiso 1 1 calc R . .
C46 C 0.6289(6) -0.0563(4) 0.9753(4) 0.0714(18) Uani 1 1 d . . .
H46A H 0.6357 -0.1006 1.0023 0.086 Uiso 1 1 calc R . .
C47 C 0.5384(4) -0.0385(3) 0.9204(3) 0.0520(14) Uani 1 1 d . . .
H47A H 0.4844 -0.0707 0.9102 0.062 Uiso 1 1 calc R . .
C48 C 0.5279(4) 0.0282(3) 0.8800(3) 0.0413(13) Uani 1 1 d . . .
O6 O 0.0143(2) 0.02488(16) 0.64016(15) 0.0301(7) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 O6 2.355(3) 3_556 ?
Eu1 O4 2.377(3) 3_556 ?
Eu1 O5 2.401(3) . ?
Eu1 O1 2.441(3) . ?
Eu1 O3 2.488(3) . ?
Eu1 O2 2.547(3) . ?
Eu1 N2 2.618(4) . ?
Eu1 O4 2.618(3) . ?
Eu1 N1 2.621(3) . ?
Eu1 C13 2.866(5) . ?
Eu1 C25 2.946(4) . ?
Eu1 Eu1 3.9720(9) 3_556 ?
O1 C13 1.268(5) . ?
O2 C13 1.269(5) . ?
O3 C25 1.268(5) . ?
O4 C25 1.271(5) . ?
O4 Eu1 2.377(3) 3_556 ?
O5 C37 1.266(5) . ?
N1 C10 1.324(5) . ?
N1 C11 1.358(5) . ?
N2 C1 1.326(5) . ?
N2 C12 1.384(5) . ?
N3 C18 1.359(7) . ?
N3 C19 1.366(7) . ?
N3 H3A 0.8600 . ?
N4 C30 1.368(7) . ?
N4 C31 1.372(6) . ?
N4 H4A 0.8600 . ?
N5 C43 1.361(7) . ?
N5 C42 1.377(6) . ?
N5 H5A 0.8600 . ?
C1 C2 1.383(6) . ?
C1 H1A 0.9300 . ?
C2 C3 1.375(6) . ?
C2 H2A 0.9300 . ?
C3 C4 1.395(6) . ?
C3 H3B 0.9300 . ?
C4 C12 1.385(6) . ?
C4 C5 1.454(6) . ?
C5 C6 1.342(7) . ?
C5 H5B 0.9300 . ?
C6 C7 1.425(7) . ?
C6 H6B 0.9300 . ?
C7 C8 1.408(6) . ?
C7 C11 1.422(5) . ?
C8 C9 1.354(7) . ?
C8 H8A 0.9300 . ?
C9 C10 1.409(6) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
C11 C12 1.439(6) . ?
C13 C14 1.516(6) . ?
C14 C15 1.515(6) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.540(6) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.489(7) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.370(6) . ?
C17 C24 1.440(7) . ?
C18 H18A 0.9300 . ?
C19 C20 1.375(8) . ?
C19 C24 1.423(6) . ?
C20 C21 1.370(8) . ?
C20 H20A 0.9300 . ?
C21 C22 1.409(8) . ?
C21 H21A 0.9300 . ?
C22 C23 1.377(8) . ?
C22 H22A 0.9300 . ?
C23 C24 1.393(7) . ?
C23 H23A 0.9300 . ?
C25 C26 1.499(6) . ?
C26 C27 1.537(6) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.516(6) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C29 1.509(7) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.369(6) . ?
C29 C36 1.429(7) . ?
C30 H30A 0.9300 . ?
C31 C32 1.364(7) . ?
C31 C36 1.411(6) . ?
C32 C33 1.366(7) . ?
C32 H32A 0.9300 . ?
C33 C34 1.385(8) . ?
C33 H33A 0.9300 . ?
C34 C35 1.364(8) . ?
C34 H34A 0.9300 . ?
C35 C36 1.400(7) . ?
C35 H35A 0.9300 . ?
C37 O6 1.259(5) . ?
C37 C38 1.524(6) . ?
C38 C39 1.527(6) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 C40 1.520(7) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 C41 1.502(7) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 C42 1.353(7) . ?
C41 C48 1.434(7) . ?
C42 H42A 0.9300 . ?
C43 C44 1.409(7) . ?
C43 C48 1.422(7) . ?
C44 C45 1.366(9) . ?
C44 H44A 0.9300 . ?
C45 C46 1.392(9) . ?
C45 H45A 0.9300 . ?
C46 C47 1.376(8) . ?
C46 H46A 0.9300 . ?
C47 C48 1.400(7) . ?
C47 H47A 0.9300 . ?
O6 Eu1 2.355(3) 3_556 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Eu1 O4 74.34(9) 3_556 3_556 ?
O6 Eu1 O5 136.02(9) 3_556 . ?
O4 Eu1 O5 77.34(9) 3_556 . ?
O6 Eu1 O1 76.51(10) 3_556 . ?
O4 Eu1 O1 81.46(10) 3_556 . ?
O5 Eu1 O1 131.16(10) . . ?
O6 Eu1 O3 87.58(10) 3_556 . ?
O4 Eu1 O3 125.43(9) 3_556 . ?
O5 Eu1 O3 82.16(10) . . ?
O1 Eu1 O3 143.90(10) . . ?
O6 Eu1 O2 125.97(10) 3_556 . ?
O4 Eu1 O2 81.27(10) 3_556 . ?
O5 Eu1 O2 81.03(10) . . ?
O1 Eu1 O2 52.37(10) . . ?
O3 Eu1 O2 143.88(10) . . ?
O6 Eu1 N2 137.87(10) 3_556 . ?
O4 Eu1 N2 147.27(11) 3_556 . ?
O5 Eu1 N2 78.28(10) . . ?
O1 Eu1 N2 98.77(11) . . ?
O3 Eu1 N2 71.78(11) . . ?
O2 Eu1 N2 73.62(11) . . ?
O6 Eu1 O4 69.31(9) 3_556 . ?
O4 Eu1 O4 74.76(10) 3_556 . ?
O5 Eu1 O4 71.21(9) . . ?
O1 Eu1 O4 142.39(10) . . ?
O3 Eu1 O4 50.75(9) . . ?
O2 Eu1 O4 146.49(9) . . ?
N2 Eu1 O4 116.97(10) . . ?
O6 Eu1 N1 76.27(10) 3_556 . ?
O4 Eu1 N1 144.03(10) 3_556 . ?
O5 Eu1 N1 138.58(11) . . ?
O1 Eu1 N1 71.86(11) . . ?
O3 Eu1 N1 72.97(10) . . ?
O2 Eu1 N1 100.01(11) . . ?
N2 Eu1 N1 62.84(11) . . ?
O4 Eu1 N1 113.16(10) . . ?
O6 Eu1 C13 101.11(12) 3_556 . ?
O4 Eu1 C13 79.76(11) 3_556 . ?
O5 Eu1 C13 106.16(12) . . ?
O1 Eu1 C13 26.11(11) . . ?
O3 Eu1 C13 154.81(11) . . ?
O2 Eu1 C13 26.27(11) . . ?
N2 Eu1 C13 86.43(12) . . ?
O4 Eu1 C13 154.35(10) . . ?
N1 Eu1 C13 86.07(12) . . ?
O6 Eu1 C25 77.57(11) 3_556 . ?
O4 Eu1 C25 100.25(11) 3_556 . ?
O5 Eu1 C25 75.18(10) . . ?
O1 Eu1 C25 152.50(11) . . ?
O3 Eu1 C25 25.22(10) . . ?
O2 Eu1 C25 155.12(11) . . ?
N2 Eu1 C25 94.25(12) . . ?
O4 Eu1 C25 25.54(10) . . ?
N1 Eu1 C25 93.16(11) . . ?
C13 Eu1 C25 178.61(13) . . ?
O6 Eu1 Eu1 66.77(6) 3_556 3_556 ?
O4 Eu1 Eu1 39.49(7) 3_556 3_556 ?
O5 Eu1 Eu1 69.92(7) . 3_556 ?
O1 Eu1 Eu1 115.68(8) . 3_556 ?
O3 Eu1 Eu1 85.98(6) . 3_556 ?
O2 Eu1 Eu1 117.31(7) . 3_556 ?
N2 Eu1 Eu1 143.35(8) . 3_556 ?
O4 Eu1 Eu1 35.27(6) . 3_556 ?
N1 Eu1 Eu1 138.04(8) . 3_556 ?
C13 Eu1 Eu1 119.19(8) . 3_556 ?
C25 Eu1 Eu1 60.78(8) . 3_556 ?
C13 O1 Eu1 96.0(3) . . ?
C13 O2 Eu1 91.1(3) . . ?
C25 O3 Eu1 98.1(3) . . ?
C25 O4 Eu1 162.6(3) . 3_556 ?
C25 O4 Eu1 91.8(2) . . ?
Eu1 O4 Eu1 105.24(10) 3_556 . ?
C37 O5 Eu1 134.4(3) . . ?
C10 N1 C11 118.1(3) . . ?
C10 N1 Eu1 121.8(3) . . ?
C11 N1 Eu1 120.1(3) . . ?
C1 N2 C12 116.9(4) . . ?
C1 N2 Eu1 122.4(3) . . ?
C12 N2 Eu1 120.7(3) . . ?
C18 N3 C19 109.7(4) . . ?
C18 N3 H3A 125.2 . . ?
C19 N3 H3A 125.2 . . ?
C30 N4 C31 109.4(4) . . ?
C30 N4 H4A 125.3 . . ?
C31 N4 H4A 125.3 . . ?
C43 N5 C42 109.1(5) . . ?
C43 N5 H5A 125.4 . . ?
C42 N5 H5A 125.4 . . ?
N2 C1 C2 124.0(4) . . ?
N2 C1 H1A 118.0 . . ?
C2 C1 H1A 118.0 . . ?
C3 C2 C1 119.2(5) . . ?
C3 C2 H2A 120.4 . . ?
C1 C2 H2A 120.4 . . ?
C2 C3 C4 118.9(5) . . ?
C2 C3 H3B 120.5 . . ?
C4 C3 H3B 120.5 . . ?
C12 C4 C3 118.7(4) . . ?
C12 C4 C5 119.4(4) . . ?
C3 C4 C5 121.9(4) . . ?
C6 C5 C4 120.4(5) . . ?
C6 C5 H5B 119.8 . . ?
C4 C5 H5B 119.8 . . ?
C5 C6 C7 121.1(4) . . ?
C5 C6 H6B 119.4 . . ?
C7 C6 H6B 119.4 . . ?
C8 C7 C11 116.8(4) . . ?
C8 C7 C6 122.9(4) . . ?
C11 C7 C6 120.3(4) . . ?
C9 C8 C7 120.2(4) . . ?
C9 C8 H8A 119.9 . . ?
C7 C8 H8A 119.9 . . ?
C8 C9 C10 119.1(5) . . ?
C8 C9 H9A 120.4 . . ?
C10 C9 H9A 120.4 . . ?
N1 C10 C9 123.1(4) . . ?
N1 C10 H10A 118.5 . . ?
C9 C10 H10A 118.5 . . ?
N1 C11 C7 122.6(4) . . ?
N1 C11 C12 119.5(4) . . ?
C7 C11 C12 117.8(4) . . ?
N2 C12 C4 122.3(4) . . ?
N2 C12 C11 116.7(4) . . ?
C4 C12 C11 120.9(4) . . ?
O1 C13 O2 120.5(4) . . ?
O1 C13 C14 119.4(4) . . ?
O2 C13 C14 120.1(4) . . ?
O1 C13 Eu1 57.9(2) . . ?
O2 C13 Eu1 62.7(2) . . ?
C14 C13 Eu1 176.4(3) . . ?
C15 C14 C13 114.4(4) . . ?
C15 C14 H14A 108.7 . . ?
C13 C14 H14A 108.7 . . ?
C15 C14 H14B 108.7 . . ?
C13 C14 H14B 108.7 . . ?
H14A C14 H14B 107.6 . . ?
C14 C15 C16 112.7(4) . . ?
C14 C15 H15A 109.0 . . ?
C16 C15 H15A 109.0 . . ?
C14 C15 H15B 109.0 . . ?
C16 C15 H15B 109.0 . . ?
H15A C15 H15B 107.8 . . ?
C17 C16 C15 115.3(4) . . ?
C17 C16 H16A 108.5 . . ?
C15 C16 H16A 108.5 . . ?
C17 C16 H16B 108.5 . . ?
C15 C16 H16B 108.5 . . ?
H16A C16 H16B 107.5 . . ?
C18 C17 C24 105.5(5) . . ?
C18 C17 C16 128.3(5) . . ?
C24 C17 C16 126.2(4) . . ?
N3 C18 C17 110.8(5) . . ?
N3 C18 H18A 124.6 . . ?
C17 C18 H18A 124.6 . . ?
N3 C19 C20 131.5(5) . . ?
N3 C19 C24 106.8(5) . . ?
C20 C19 C24 121.7(6) . . ?
C21 C20 C19 118.6(5) . . ?
C21 C20 H20A 120.7 . . ?
C19 C20 H20A 120.7 . . ?
C20 C21 C22 120.9(6) . . ?
C20 C21 H21A 119.6 . . ?
C22 C21 H21A 119.6 . . ?
C23 C22 C21 120.7(6) . . ?
C23 C22 H22A 119.7 . . ?
C21 C22 H22A 119.7 . . ?
C22 C23 C24 119.4(5) . . ?
C22 C23 H23A 120.3 . . ?
C24 C23 H23A 120.3 . . ?
C23 C24 C19 118.7(5) . . ?
C23 C24 C17 134.0(5) . . ?
C19 C24 C17 107.3(5) . . ?
O3 C25 O4 119.4(4) . . ?
O3 C25 C26 120.7(4) . . ?
O4 C25 C26 119.9(4) . . ?
O3 C25 Eu1 56.7(2) . . ?
O4 C25 Eu1 62.6(2) . . ?
C26 C25 Eu1 177.4(3) . . ?
C25 C26 C27 111.5(4) . . ?
C25 C26 H26A 109.3 . . ?
C27 C26 H26A 109.3 . . ?
C25 C26 H26B 109.3 . . ?
C27 C26 H26B 109.3 . . ?
H26A C26 H26B 108.0 . . ?
C28 C27 C26 112.2(4) . . ?
C28 C27 H27A 109.2 . . ?
C26 C27 H27A 109.2 . . ?
C28 C27 H27B 109.2 . . ?
C26 C27 H27B 109.2 . . ?
H27A C27 H27B 107.9 . . ?
C29 C28 C27 114.1(4) . . ?
C29 C28 H28A 108.7 . . ?
C27 C28 H28A 108.7 . . ?
C29 C28 H28B 108.7 . . ?
C27 C28 H28B 108.7 . . ?
H28A C28 H28B 107.6 . . ?
C30 C29 C36 106.0(5) . . ?
C30 C29 C28 126.9(5) . . ?
C36 C29 C28 127.0(4) . . ?
N4 C30 C29 110.1(5) . . ?
N4 C30 H30A 125.0 . . ?
C29 C30 H30A 125.0 . . ?
C32 C31 N4 130.3(5) . . ?
C32 C31 C36 123.0(5) . . ?
N4 C31 C36 106.8(5) . . ?
C31 C32 C33 117.8(5) . . ?
C31 C32 H32A 121.1 . . ?
C33 C32 H32A 121.1 . . ?
C32 C33 C34 121.1(6) . . ?
C32 C33 H33A 119.5 . . ?
C34 C33 H33A 119.5 . . ?
C35 C34 C33 121.5(6) . . ?
C35 C34 H34A 119.3 . . ?
C33 C34 H34A 119.3 . . ?
C34 C35 C36 119.1(5) . . ?
C34 C35 H35A 120.4 . . ?
C36 C35 H35A 120.4 . . ?
C35 C36 C31 117.5(5) . . ?
C35 C36 C29 134.8(5) . . ?
C31 C36 C29 107.7(4) . . ?
O6 C37 O5 125.1(4) . . ?
O6 C37 C38 115.0(3) . . ?
O5 C37 C38 119.8(4) . . ?
C37 C38 C39 117.9(4) . . ?
C37 C38 H38A 107.8 . . ?
C39 C38 H38A 107.8 . . ?
C37 C38 H38B 107.8 . . ?
C39 C38 H38B 107.8 . . ?
H38A C38 H38B 107.2 . . ?
C40 C39 C38 114.9(4) . . ?
C40 C39 H39A 108.6 . . ?
C38 C39 H39A 108.6 . . ?
C40 C39 H39B 108.6 . . ?
C38 C39 H39B 108.6 . . ?
H39A C39 H39B 107.5 . . ?
C41 C40 C39 113.8(4) . . ?
C41 C40 H40A 108.8 . . ?
C39 C40 H40A 108.8 . . ?
C41 C40 H40B 108.8 . . ?
C39 C40 H40B 108.8 . . ?
H40A C40 H40B 107.7 . . ?
C42 C41 C48 105.6(5) . . ?
C42 C41 C40 128.5(5) . . ?
C48 C41 C40 125.8(5) . . ?
C41 C42 N5 110.9(5) . . ?
C41 C42 H42A 124.5 . . ?
N5 C42 H42A 124.5 . . ?
N5 C43 C44 130.2(6) . . ?
N5 C43 C48 106.6(5) . . ?
C44 C43 C48 123.2(6) . . ?
C45 C44 C43 115.8(6) . . ?
C45 C44 H44A 122.1 . . ?
C43 C44 H44A 122.1 . . ?
C44 C45 C46 123.1(6) . . ?
C44 C45 H45A 118.5 . . ?
C46 C45 H45A 118.5 . . ?
C47 C46 C45 120.7(6) . . ?
C47 C46 H46A 119.6 . . ?
C45 C46 H46A 119.6 . . ?
C46 C47 C48 119.7(6) . . ?
C46 C47 H47A 120.1 . . ?
C48 C47 H47A 120.1 . . ?
C47 C48 C43 117.5(5) . . ?
C47 C48 C41 134.8(5) . . ?
C43 C48 C41 107.7(5) . . ?
C37 O6 Eu1 140.5(2) . 3_556 ?

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
N3 H3A O3 0.86 2.05 2.863(5) 157.7 2_545
N4 H4A O2 0.86 2.17 2.983(5) 158.3 2_556

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.664
_refine_diff_density_min         -1.157
_refine_diff_density_rms         0.118
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_bai-716
_database_code_depnum_ccdc_archive 'CCDC 1044891'
_audit_update_record             
;
2015-11-09 deposited with the CCDC.
2015-11-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C96 H88 N10 O12 Tb2'
_chemical_formula_weight         1891.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   13.766(3)
_cell_length_b                   18.430(4)
_cell_length_c                   17.190(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.34(3)
_cell_angle_gamma                90.00
_cell_volume                     4185.2(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6445
_cell_measurement_theta_min      3.08
_cell_measurement_theta_max      29.43

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1920
_exptl_absorpt_coefficient_mu    1.746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.693
_exptl_absorpt_correction_T_max  0.840
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            37765
_diffrn_reflns_av_R_equivalents  0.1199
_diffrn_reflns_av_sigmaI/netI    0.1054
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.08
_diffrn_reflns_theta_max         27.43
_reflns_number_total             9467
_reflns_number_gt                6445
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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)+(0.0000P)²+13.3612P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9467
_refine_ls_number_parameters     541
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1035
_refine_ls_R_factor_gt           0.0613
_refine_ls_wR_factor_ref         0.1056
_refine_ls_wR_factor_gt          0.0912
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_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
Tb1 Tb 0.628774(19) 0.510107(14) 0.471799(17) 0.02325(8) Uani 1 1 d . . .
O1 O 0.7466(3) 0.6094(2) 0.5429(3) 0.0378(11) Uani 1 1 d . . .
O2 O 0.6577(3) 0.6265(2) 0.4167(3) 0.0396(11) Uani 1 1 d . . .
O3 O 0.6156(3) 0.3791(2) 0.4438(2) 0.0348(10) Uani 1 1 d . . .
O4 O 0.4856(3) 0.4198(2) 0.4805(2) 0.0278(9) Uani 1 1 d . . .
O5 O 0.6603(3) 0.4701(2) 0.6078(2) 0.0291(9) Uani 1 1 d . . .
O6 O 0.5129(3) 0.4754(2) 0.6390(2) 0.0307(10) Uani 1 1 d . . .
N1 N 0.8104(3) 0.4592(3) 0.5018(3) 0.0305(12) Uani 1 1 d . . .
N2 N 0.6970(3) 0.4883(3) 0.3472(3) 0.0314(11) Uani 1 1 d . . .
N3 N 0.7769(5) 0.7870(3) 0.1371(4) 0.0612(19) Uani 1 1 d . . .
H3A H 0.7989 0.8085 0.1010 0.073 Uiso 1 1 calc R . .
N4 N 0.6895(5) 0.1680(3) 0.7889(4) 0.0565(17) Uani 1 1 d . . .
H4A H 0.6895 0.1492 0.8347 0.068 Uiso 1 1 calc R . .
N5 N 1.0853(4) 0.3652(3) 0.8520(4) 0.0595(18) Uani 1 1 d . . .
H5A H 1.1238 0.3289 0.8503 0.071 Uiso 1 1 calc R . .
C1 C 0.8671(5) 0.4441(4) 0.5752(4) 0.0438(17) Uani 1 1 d . . .
H1A H 0.8396 0.4529 0.6179 0.053 Uiso 1 1 calc R . .
C2 C 0.9653(5) 0.4160(4) 0.5947(4) 0.0473(18) Uani 1 1 d . . .
H2A H 1.0021 0.4077 0.6483 0.057 Uiso 1 1 calc R . .
C3 C 1.0052(5) 0.4012(4) 0.5320(4) 0.0470(19) Uani 1 1 d . . .
H3B H 1.0699 0.3815 0.5427 0.056 Uiso 1 1 calc R . .
C4 C 0.9493(5) 0.4155(4) 0.4517(4) 0.0393(16) Uani 1 1 d . . .
C5 C 0.9872(5) 0.4005(4) 0.3833(5) 0.0476(19) Uani 1 1 d . . .
H5B H 1.0515 0.3807 0.3919 0.057 Uiso 1 1 calc R . .
C6 C 0.9316(5) 0.4147(4) 0.3078(5) 0.0486(19) Uani 1 1 d . . .
H6A H 0.9578 0.4050 0.2646 0.058 Uiso 1 1 calc R . .
C7 C 0.8324(5) 0.4446(3) 0.2926(4) 0.0347(15) Uani 1 1 d . . .
C8 C 0.7722(5) 0.4608(4) 0.2149(5) 0.052(2) Uani 1 1 d . . .
H8A H 0.7962 0.4515 0.1704 0.062 Uiso 1 1 calc R . .
C9 C 0.6778(5) 0.4905(4) 0.2034(4) 0.0522(19) Uani 1 1 d . . .
H9A H 0.6374 0.5017 0.1517 0.063 Uiso 1 1 calc R . .
C10 C 0.6437(5) 0.5035(4) 0.2719(4) 0.0451(17) Uani 1 1 d . . .
H10A H 0.5799 0.5239 0.2639 0.054 Uiso 1 1 calc R . .
C11 C 0.7924(4) 0.4603(3) 0.3583(4) 0.0300(14) Uani 1 1 d . . .
C12 C 0.8514(4) 0.4439(3) 0.4389(4) 0.0275(13) Uani 1 1 d . . .
C13 C 0.7201(5) 0.6494(3) 0.4809(4) 0.0321(15) Uani 1 1 d . . .
C14 C 0.7630(5) 0.7243(4) 0.4833(4) 0.0474(19) Uani 1 1 d . . .
H14A H 0.8354 0.7221 0.5085 0.057 Uiso 1 1 calc R . .
H14B H 0.7338 0.7546 0.5171 0.057 Uiso 1 1 calc R . .
C15 C 0.7433(6) 0.7605(4) 0.3984(5) 0.057(2) Uani 1 1 d . . .
H15A H 0.6716 0.7580 0.3705 0.068 Uiso 1 1 calc R . .
H15B H 0.7622 0.8114 0.4054 0.068 Uiso 1 1 calc R . .
C16 C 0.8031(6) 0.7240(4) 0.3463(5) 0.056(2) Uani 1 1 d . . .
H16A H 0.8742 0.7354 0.3692 0.067 Uiso 1 1 calc R . .
H16B H 0.7958 0.6719 0.3500 0.067 Uiso 1 1 calc R . .
C17 C 0.7738(5) 0.7443(4) 0.2595(5) 0.051(2) Uani 1 1 d . . .
C18 C 0.8250(6) 0.7838(4) 0.2177(6) 0.062(2) Uani 1 1 d . . .
H18A H 0.8866 0.8064 0.2416 0.075 Uiso 1 1 calc R . .
C19 C 0.6872(7) 0.7498(4) 0.1231(5) 0.058(2) Uani 1 1 d . . .
C20 C 0.6101(7) 0.7356(5) 0.0526(5) 0.069(3) Uani 1 1 d . . .
H20A H 0.6132 0.7540 0.0030 0.083 Uiso 1 1 calc R . .
C21 C 0.5298(7) 0.6942(6) 0.0577(6) 0.081(3) Uani 1 1 d . . .
H21A H 0.4789 0.6840 0.0105 0.097 Uiso 1 1 calc R . .
C22 C 0.5217(7) 0.6670(5) 0.1303(6) 0.078(3) Uani 1 1 d . . .
H22A H 0.4652 0.6399 0.1316 0.094 Uiso 1 1 calc R . .
C23 C 0.5984(6) 0.6801(4) 0.2021(5) 0.061(2) Uani 1 1 d . . .
H23A H 0.5936 0.6614 0.2511 0.074 Uiso 1 1 calc R . .
C24 C 0.6819(5) 0.7217(4) 0.1991(5) 0.050(2) Uani 1 1 d . . .
C25 C 0.5323(4) 0.3671(3) 0.4599(3) 0.0268(13) Uani 1 1 d . . .
C26 C 0.4895(4) 0.2922(3) 0.4529(4) 0.0351(15) Uani 1 1 d . . .
H26A H 0.4885 0.2720 0.4005 0.042 Uiso 1 1 calc R . .
H26B H 0.4203 0.2942 0.4560 0.042 Uiso 1 1 calc R . .
C27 C 0.5522(5) 0.2426(3) 0.5205(4) 0.0434(17) Uani 1 1 d . . .
H27A H 0.5158 0.1975 0.5202 0.052 Uiso 1 1 calc R . .
H27B H 0.6158 0.2312 0.5093 0.052 Uiso 1 1 calc R . .
C28 C 0.5742(5) 0.2765(4) 0.6035(4) 0.0474(18) Uani 1 1 d . . .
H28A H 0.5105 0.2873 0.6147 0.057 Uiso 1 1 calc R . .
H28B H 0.6092 0.3221 0.6032 0.057 Uiso 1 1 calc R . .
C29 C 0.6373(5) 0.2296(4) 0.6711(4) 0.0463(18) Uani 1 1 d . . .
C30 C 0.6146(6) 0.2093(4) 0.7406(5) 0.053(2) Uani 1 1 d . . .
H30A H 0.5554 0.2221 0.7532 0.064 Uiso 1 1 calc R . .
C31 C 0.7653(6) 0.1617(4) 0.7515(4) 0.0463(18) Uani 1 1 d . . .
C32 C 0.8557(6) 0.1263(4) 0.7770(5) 0.057(2) Uani 1 1 d . . .
H32A H 0.8742 0.1020 0.8264 0.068 Uiso 1 1 calc R . .
C33 C 0.9190(6) 0.1276(5) 0.7272(6) 0.073(3) Uani 1 1 d . . .
H33A H 0.9803 0.1028 0.7427 0.087 Uiso 1 1 calc R . .
C34 C 0.8920(6) 0.1655(6) 0.6541(6) 0.089(3) Uani 1 1 d . . .
H34A H 0.9361 0.1661 0.6219 0.107 Uiso 1 1 calc R . .
C35 C 0.8006(6) 0.2025(5) 0.6285(5) 0.072(3) Uani 1 1 d . . .
H35A H 0.7829 0.2277 0.5796 0.086 Uiso 1 1 calc R . .
C36 C 0.7360(5) 0.2005(4) 0.6786(4) 0.0448(18) Uani 1 1 d . . .
C37 C 0.6063(4) 0.4602(3) 0.6554(4) 0.0295(14) Uani 1 1 d . . .
C38 C 0.6514(4) 0.4278(4) 0.7389(4) 0.0391(16) Uani 1 1 d . . .
H38A H 0.6101 0.3865 0.7443 0.047 Uiso 1 1 calc R . .
H38B H 0.6451 0.4635 0.7786 0.047 Uiso 1 1 calc R . .
C39 C 0.7624(4) 0.4026(3) 0.7616(4) 0.0410(17) Uani 1 1 d . . .
H39A H 0.7721 0.3655 0.8031 0.049 Uiso 1 1 calc R . .
H39B H 0.7758 0.3807 0.7144 0.049 Uiso 1 1 calc R . .
C40 C 0.8387(5) 0.4631(4) 0.7925(4) 0.0414(17) Uani 1 1 d . . .
H40A H 0.8350 0.4972 0.7488 0.050 Uiso 1 1 calc R . .
H40B H 0.8203 0.4890 0.8355 0.050 Uiso 1 1 calc R . .
C41 C 0.9467(5) 0.4364(4) 0.8244(4) 0.0397(16) Uani 1 1 d . . .
C42 C 0.9837(5) 0.3718(4) 0.8080(4) 0.0480(18) Uani 1 1 d . . .
H42A H 0.9468 0.3370 0.7727 0.058 Uiso 1 1 calc R . .
C43 C 1.1132(5) 0.4262(4) 0.8981(4) 0.0477(19) Uani 1 1 d . . .
C44 C 1.2052(6) 0.4439(5) 0.9539(5) 0.070(3) Uani 1 1 d . . .
H44A H 1.2602 0.4124 0.9655 0.084 Uiso 1 1 calc R . .
C45 C 1.2102(6) 0.5106(6) 0.9909(5) 0.076(3) Uani 1 1 d . . .
H45A H 1.2705 0.5245 1.0281 0.091 Uiso 1 1 calc R . .
C46 C 1.1274(7) 0.5583(5) 0.9744(5) 0.070(2) Uani 1 1 d . . .
H46A H 1.1339 0.6030 1.0004 0.084 Uiso 1 1 calc R . .
C47 C 1.0373(5) 0.5395(4) 0.9203(4) 0.054(2) Uani 1 1 d . . .
H47A H 0.9823 0.5709 0.9104 0.064 Uiso 1 1 calc R . .
C48 C 1.0286(5) 0.4731(4) 0.8803(4) 0.0409(17) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O6 2.326(4) 3_666 ?
Tb1 O4 2.355(4) 3_666 ?
Tb1 O5 2.372(4) . ?
Tb1 O2 2.423(4) . ?
Tb1 O3 2.459(4) . ?
Tb1 O1 2.522(4) . ?
Tb1 N1 2.582(4) . ?
Tb1 N2 2.601(4) . ?
Tb1 O4 2.616(4) . ?
Tb1 C13 2.843(6) . ?
Tb1 C25 2.933(6) . ?
Tb1 Tb1 3.9475(10) 3_666 ?
O1 C13 1.263(7) . ?
O2 C13 1.265(7) . ?
O3 C25 1.272(6) . ?
O4 C25 1.269(6) . ?
O4 Tb1 2.355(4) 3_666 ?
O5 C37 1.264(6) . ?
O6 C37 1.269(6) . ?
O6 Tb1 2.326(4) 3_666 ?
N1 C1 1.314(8) . ?
N1 C12 1.382(7) . ?
N2 C10 1.325(7) . ?
N2 C11 1.374(7) . ?
N3 C18 1.359(10) . ?
N3 C19 1.373(10) . ?
N4 C30 1.361(9) . ?
N4 C31 1.375(8) . ?
N5 C43 1.368(9) . ?
N5 C42 1.395(8) . ?
C1 C2 1.397(8) . ?
C2 C3 1.368(9) . ?
C3 C4 1.404(9) . ?
C4 C12 1.404(8) . ?
C4 C5 1.441(8) . ?
C5 C6 1.333(9) . ?
C6 C7 1.427(8) . ?
C7 C8 1.392(9) . ?
C7 C11 1.417(8) . ?
C8 C9 1.373(9) . ?
C9 C10 1.405(8) . ?
C11 C12 1.428(8) . ?
C13 C14 1.498(8) . ?
C14 C15 1.558(9) . ?
C15 C16 1.533(9) . ?
C16 C17 1.479(10) . ?
C17 C18 1.353(9) . ?
C17 C24 1.453(10) . ?
C19 C20 1.393(11) . ?
C19 C24 1.427(10) . ?
C20 C21 1.365(11) . ?
C21 C22 1.378(11) . ?
C22 C23 1.401(11) . ?
C23 C24 1.395(9) . ?
C25 C26 1.492(8) . ?
C26 C27 1.538(8) . ?
C27 C28 1.509(9) . ?
C28 C29 1.512(9) . ?
C29 C30 1.369(9) . ?
C29 C36 1.432(9) . ?
C31 C32 1.363(9) . ?
C31 C36 1.400(9) . ?
C32 C33 1.383(10) . ?
C33 C34 1.395(11) . ?
C34 C35 1.389(10) . ?
C35 C36 1.403(9) . ?
C37 C38 1.516(8) . ?
C38 C39 1.539(8) . ?
C39 C40 1.522(9) . ?
C40 C41 1.515(8) . ?
C41 C42 1.355(9) . ?
C41 C48 1.430(9) . ?
C43 C44 1.395(10) . ?
C43 C48 1.412(9) . ?
C44 C45 1.376(12) . ?
C45 C46 1.404(11) . ?
C46 C47 1.369(10) . ?
C47 C48 1.393(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Tb1 O4 74.57(13) 3_666 3_666 ?
O6 Tb1 O5 136.19(12) 3_666 . ?
O4 Tb1 O5 77.44(12) 3_666 . ?
O6 Tb1 O2 76.72(14) 3_666 . ?
O4 Tb1 O2 81.35(13) 3_666 . ?
O5 Tb1 O2 131.00(14) . . ?
O6 Tb1 O3 87.33(14) 3_666 . ?
O4 Tb1 O3 125.94(12) 3_666 . ?
O5 Tb1 O3 82.55(13) . . ?
O2 Tb1 O3 143.54(14) . . ?
O6 Tb1 O1 126.20(14) 3_666 . ?
O4 Tb1 O1 80.47(13) 3_666 . ?
O5 Tb1 O1 80.38(14) . . ?
O2 Tb1 O1 52.65(14) . . ?
O3 Tb1 O1 144.07(14) . . ?
O6 Tb1 N1 138.27(14) 3_666 . ?
O4 Tb1 N1 146.51(14) 3_666 . ?
O5 Tb1 N1 77.98(14) . . ?
O2 Tb1 N1 98.24(15) . . ?
O3 Tb1 N1 72.35(14) . . ?
O1 Tb1 N1 73.28(15) . . ?
O6 Tb1 N2 75.93(13) 3_666 . ?
O4 Tb1 N2 143.43(14) 3_666 . ?
O5 Tb1 N2 139.05(14) . . ?
O2 Tb1 N2 71.19(15) . . ?
O3 Tb1 N2 73.22(14) . . ?
O1 Tb1 N2 100.35(14) . . ?
N1 Tb1 N2 63.56(15) . . ?
O6 Tb1 O4 69.40(12) 3_666 . ?
O4 Tb1 O4 74.99(14) 3_666 . ?
O5 Tb1 O4 71.21(12) . . ?
O2 Tb1 O4 142.64(13) . . ?
O3 Tb1 O4 51.02(12) . . ?
O1 Tb1 O4 145.69(12) . . ?
N1 Tb1 O4 117.41(14) . . ?
N2 Tb1 O4 113.66(13) . . ?
O6 Tb1 C13 101.39(17) 3_666 . ?
O4 Tb1 C13 79.28(14) 3_666 . ?
O5 Tb1 C13 105.72(16) . . ?
O2 Tb1 C13 26.29(15) . . ?
O3 Tb1 C13 154.77(14) . . ?
O1 Tb1 C13 26.37(15) . . ?
N1 Tb1 C13 85.90(16) . . ?
N2 Tb1 C13 85.88(16) . . ?
O4 Tb1 C13 154.14(14) . . ?
O6 Tb1 C25 77.70(15) 3_666 . ?
O4 Tb1 C25 100.57(14) 3_666 . ?
O5 Tb1 C25 75.11(14) . . ?
O2 Tb1 C25 152.81(15) . . ?
O3 Tb1 C25 25.39(13) . . ?
O1 Tb1 C25 154.54(15) . . ?
N1 Tb1 C25 94.68(16) . . ?
N2 Tb1 C25 93.74(15) . . ?
O4 Tb1 C25 25.64(13) . . ?
C13 Tb1 C25 179.08(18) . . ?
O6 Tb1 Tb1 66.93(9) 3_666 3_666 ?
O4 Tb1 Tb1 39.81(9) 3_666 3_666 ?
O5 Tb1 Tb1 69.93(9) . 3_666 ?
O2 Tb1 Tb1 115.92(10) . 3_666 ?
O3 Tb1 Tb1 86.17(8) . 3_666 ?
O1 Tb1 Tb1 116.66(9) . 3_666 ?
N1 Tb1 Tb1 143.38(11) . 3_666 ?
N2 Tb1 Tb1 138.17(10) . 3_666 ?
O4 Tb1 Tb1 35.18(8) . 3_666 ?
C13 Tb1 Tb1 119.05(11) . 3_666 ?
C25 Tb1 Tb1 60.78(11) . 3_666 ?
C13 O1 Tb1 91.1(4) . . ?
C13 O2 Tb1 95.7(4) . . ?
C25 O3 Tb1 98.6(3) . . ?
C25 O4 Tb1 163.3(4) . 3_666 ?
C25 O4 Tb1 91.3(3) . . ?
Tb1 O4 Tb1 105.02(14) 3_666 . ?
C37 O5 Tb1 134.8(4) . . ?
C37 O6 Tb1 140.5(4) . 3_666 ?
C1 N1 C12 116.3(5) . . ?
C1 N1 Tb1 123.4(4) . . ?
C12 N1 Tb1 120.3(4) . . ?
C10 N2 C11 117.4(5) . . ?
C10 N2 Tb1 122.9(4) . . ?
C11 N2 Tb1 119.8(4) . . ?
C18 N3 C19 108.2(6) . . ?
C30 N4 C31 107.8(6) . . ?
C43 N5 C42 108.6(6) . . ?
N1 C1 C2 125.7(6) . . ?
C3 C2 C1 117.4(7) . . ?
C2 C3 C4 120.5(6) . . ?
C3 C4 C12 117.4(6) . . ?
C3 C4 C5 122.9(6) . . ?
C12 C4 C5 119.7(6) . . ?
C6 C5 C4 121.1(6) . . ?
C5 C6 C7 120.8(6) . . ?
C8 C7 C11 117.4(6) . . ?
C8 C7 C6 122.6(6) . . ?
C11 C7 C6 119.9(6) . . ?
C9 C8 C7 120.5(6) . . ?
C8 C9 C10 118.2(7) . . ?
N2 C10 C9 124.0(6) . . ?
N2 C11 C7 122.4(6) . . ?
N2 C11 C12 118.3(5) . . ?
C7 C11 C12 119.2(5) . . ?
N1 C12 C4 122.7(6) . . ?
N1 C12 C11 118.0(5) . . ?
C4 C12 C11 119.3(5) . . ?
O1 C13 O2 120.5(6) . . ?
O1 C13 C14 119.7(6) . . ?
O2 C13 C14 119.8(6) . . ?
O1 C13 Tb1 62.5(3) . . ?
O2 C13 Tb1 58.0(3) . . ?
C14 C13 Tb1 177.0(5) . . ?
C13 C14 C15 113.9(6) . . ?
C16 C15 C14 112.3(6) . . ?
C17 C16 C15 116.1(6) . . ?
C18 C17 C24 104.7(7) . . ?
C18 C17 C16 129.5(8) . . ?
C24 C17 C16 125.7(6) . . ?
C17 C18 N3 112.8(8) . . ?
N3 C19 C20 132.4(8) . . ?
N3 C19 C24 107.2(8) . . ?
C20 C19 C24 120.4(8) . . ?
C21 C20 C19 118.8(8) . . ?
C20 C21 C22 122.3(9) . . ?
C21 C22 C23 120.1(9) . . ?
C24 C23 C22 119.2(8) . . ?
C23 C24 C19 119.2(8) . . ?
C23 C24 C17 133.8(7) . . ?
C19 C24 C17 107.0(7) . . ?
O4 C25 O3 119.0(5) . . ?
O4 C25 C26 120.8(5) . . ?
O3 C25 C26 120.2(5) . . ?
O4 C25 Tb1 63.1(3) . . ?
O3 C25 Tb1 56.0(3) . . ?
C26 C25 Tb1 176.1(4) . . ?
C25 C26 C27 111.3(5) . . ?
C28 C27 C26 112.9(5) . . ?
C27 C28 C29 114.2(6) . . ?
C30 C29 C36 105.2(6) . . ?
C30 C29 C28 127.2(7) . . ?
C36 C29 C28 127.5(6) . . ?
N4 C30 C29 111.4(6) . . ?
C32 C31 N4 129.3(7) . . ?
C32 C31 C36 122.6(7) . . ?
N4 C31 C36 108.0(6) . . ?
C31 C32 C33 118.1(7) . . ?
C32 C33 C34 120.7(7) . . ?
C35 C34 C33 121.4(8) . . ?
C34 C35 C36 117.8(8) . . ?
C31 C36 C35 119.4(7) . . ?
C31 C36 C29 107.4(6) . . ?
C35 C36 C29 133.2(7) . . ?
O5 C37 O6 124.6(5) . . ?
O5 C37 C38 120.7(5) . . ?
O6 C37 C38 114.6(5) . . ?
C37 C38 C39 118.2(5) . . ?
C40 C39 C38 113.9(5) . . ?
C41 C40 C39 113.4(5) . . ?
C42 C41 C48 106.5(6) . . ?
C42 C41 C40 126.8(6) . . ?
C48 C41 C40 126.7(6) . . ?
C41 C42 N5 110.0(7) . . ?
N5 C43 C44 130.1(8) . . ?
N5 C43 C48 107.2(6) . . ?
C44 C43 C48 122.7(8) . . ?
C45 C44 C43 116.3(8) . . ?
C44 C45 C46 122.3(8) . . ?
C47 C46 C45 120.5(8) . . ?
C46 C47 C48 119.6(7) . . ?
C47 C48 C43 118.6(7) . . ?
C47 C48 C41 133.6(6) . . ?
C43 C48 C41 107.6(6) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        27.43
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.978
_refine_diff_density_min         -1.479
_refine_diff_density_rms         0.148
####################################################################### 
# 
# 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_bai-703
_database_code_depnum_ccdc_archive 'CCDC 1044892'
_audit_update_record             
;
2015-11-09 deposited with the CCDC.
2015-11-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C96 H88 N10 O12 Yb2'
_chemical_formula_weight         1919.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.887(2)
_cell_length_b                   12.286(3)
_cell_length_c                   16.566(3)
_cell_angle_alpha                78.38(3)
_cell_angle_beta                 86.60(3)
_cell_angle_gamma                71.74(3)
_cell_volume                     2061.1(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    275(2)
_cell_measurement_reflns_used    9253
_cell_measurement_theta_min      3.03
_cell_measurement_theta_max      27.43

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             970
_exptl_absorpt_coefficient_mu    2.326
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.646
_exptl_absorpt_correction_T_max  0.870
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      275(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            20088
_diffrn_reflns_av_R_equivalents  0.1583
_diffrn_reflns_av_sigmaI/netI    0.2257
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         27.43
_reflns_number_total             9253
_reflns_number_gt                5673
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker 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)+(0.1127P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9253
_refine_ls_number_parameters     541
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.1734
_refine_ls_R_factor_gt           0.1089
_refine_ls_wR_factor_ref         0.2703
_refine_ls_wR_factor_gt          0.2245
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Yb1 Yb 0.54655(3) 0.45118(3) 0.12760(2) 0.03310(10) Uani 1 1 d . . .
O1 O 0.5165(5) 0.3294(5) 0.2566(4) 0.0432(17) Uani 1 1 d . . .
O2 O 0.3952(5) 0.5125(5) 0.2389(4) 0.0508(19) Uani 1 1 d . . .
O3 O 0.3561(5) 0.4254(5) 0.0983(4) 0.0476(17) Uani 1 1 d . . .
O4 O 0.3160(5) 0.4858(5) -0.0366(4) 0.0530(19) Uani 1 1 d . . .
O5 O 0.5974(5) 0.3076(5) 0.0547(4) 0.0472(18) Uani 1 1 d . . .
O6 O 0.5624(6) 0.3560(5) -0.0815(4) 0.0513(19) Uani 1 1 d . . .
N1 N 0.7717(6) 0.3193(6) 0.1748(4) 0.042(2) Uani 1 1 d . . .
N2 N 0.6596(6) 0.5317(6) 0.2169(4) 0.0358(18) Uani 1 1 d . . .
N3 N 0.2698(8) 0.7066(8) 0.6041(7) 0.079(3) Uani 1 1 d U . .
H3A H 0.3061 0.7379 0.6338 0.095 Uiso 1 1 calc R . .
N4 N -0.1420(7) 0.2962(8) -0.1988(6) 0.066(3) Uani 1 1 d . . .
H4A H -0.2124 0.3198 -0.2271 0.079 Uiso 1 1 calc R . .
N5 N 0.5426(7) -0.1214(7) -0.2552(7) 0.070(3) Uani 1 1 d . . .
H5A H 0.5099 -0.1701 -0.2695 0.084 Uiso 1 1 calc R . .
C1 C 0.8257(8) 0.2121(7) 0.1614(6) 0.042(2) Uani 1 1 d . . .
H1A H 0.7753 0.1767 0.1392 0.051 Uiso 1 1 calc R . .
C2 C 0.9554(9) 0.1499(9) 0.1794(6) 0.057(3) Uani 1 1 d . . .
H2A H 0.9877 0.0734 0.1711 0.068 Uiso 1 1 calc R . .
C3 C 1.0325(9) 0.1970(8) 0.2075(6) 0.057(3) Uani 1 1 d . . .
H3B H 1.1197 0.1562 0.2170 0.069 Uiso 1 1 calc R . .
C4 C 0.9780(7) 0.3144(9) 0.2235(6) 0.052(3) Uani 1 1 d . . .
C5 C 1.0543(9) 0.3655(9) 0.2581(7) 0.066(4) Uani 1 1 d . . .
H5B H 1.1422 0.3271 0.2667 0.079 Uiso 1 1 calc R . .
C6 C 0.9994(8) 0.4731(10) 0.2794(7) 0.064(3) Uani 1 1 d . . .
H6A H 1.0509 0.5085 0.3005 0.077 Uiso 1 1 calc R . .
C7 C 0.8634(8) 0.5306(8) 0.2692(6) 0.051(3) Uani 1 1 d . . .
C8 C 0.7976(8) 0.6389(9) 0.2928(6) 0.055(3) Uani 1 1 d . . .
H8A H 0.8435 0.6768 0.3165 0.066 Uiso 1 1 calc R . .
C9 C 0.6675(9) 0.6875(8) 0.2810(6) 0.053(3) Uani 1 1 d . . .
H9A H 0.6228 0.7566 0.2985 0.063 Uiso 1 1 calc R . .
C10 C 0.6025(9) 0.6296(8) 0.2414(6) 0.052(3) Uani 1 1 d . . .
H10A H 0.5140 0.6632 0.2323 0.062 Uiso 1 1 calc R . .
C11 C 0.7865(7) 0.4805(7) 0.2314(5) 0.034(2) Uani 1 1 d . . .
C12 C 0.8490(7) 0.3700(8) 0.2091(5) 0.042(2) Uani 1 1 d . . .
C13 C 0.4263(7) 0.4132(7) 0.2808(5) 0.039(2) Uani 1 1 d . . .
C14 C 0.3652(8) 0.3895(8) 0.3638(6) 0.053(3) Uani 1 1 d . . .
H14A H 0.2963 0.3573 0.3577 0.064 Uiso 1 1 calc R . .
H14B H 0.4296 0.3307 0.4006 0.064 Uiso 1 1 calc R . .
C15 C 0.3106(10) 0.4948(10) 0.4031(7) 0.069(4) Uani 1 1 d . . .
H15A H 0.3719 0.5387 0.3953 0.083 Uiso 1 1 calc R . .
H15B H 0.2320 0.5441 0.3739 0.083 Uiso 1 1 calc R . .
C16 C 0.2801(11) 0.4716(9) 0.4929(7) 0.072(4) Uani 1 1 d . . .
H16A H 0.2096 0.4381 0.4992 0.086 Uiso 1 1 calc R . .
H16B H 0.3549 0.4123 0.5205 0.086 Uiso 1 1 calc R . .
C17 C 0.2455(9) 0.5672(9) 0.5360(6) 0.059(3) Uani 1 1 d . . .
C18 C 0.3278(12) 0.6036(11) 0.5753(7) 0.080(4) Uani 1 1 d U . .
H18A H 0.4154 0.5629 0.5824 0.096 Uiso 1 1 calc R . .
C19 C 0.1493(11) 0.7477(10) 0.5775(7) 0.074(3) Uani 1 1 d U . .
C20 C 0.0485(13) 0.8486(12) 0.5871(8) 0.101(5) Uani 1 1 d . . .
H20A H 0.0623 0.9030 0.6143 0.122 Uiso 1 1 calc R . .
C21 C -0.0740(2) 0.86547(13) 0.5542(2) 0.130(5) Uani 1 1 d DU . .
H21A H -0.1422 0.9333 0.5557 0.156 Uiso 1 1 calc R . .
C22 C -0.0888(6) 0.7735(3) 0.5185(4) 0.137(4) Uani 1 1 d DU . .
H22A H -0.1733 0.7771 0.5089 0.164 Uiso 1 1 calc R . .
C23 C 0.0027(12) 0.6842(12) 0.4975(8) 0.095(5) Uani 1 1 d . . .
H23A H -0.0125 0.6384 0.4632 0.115 Uiso 1 1 calc R . .
C24 C 0.1264(11) 0.6641(11) 0.5316(7) 0.076(3) Uani 1 1 d U . .
C25 C 0.2977(8) 0.4331(8) 0.0338(6) 0.042(2) Uani 1 1 d . . .
C26 C 0.1896(8) 0.3747(8) 0.0412(6) 0.049(3) Uani 1 1 d . . .
H26A H 0.2191 0.3006 0.0794 0.059 Uiso 1 1 calc R . .
H26B H 0.1148 0.4235 0.0657 0.059 Uiso 1 1 calc R . .
C27 C 0.1459(8) 0.3520(8) -0.0360(6) 0.051(3) Uani 1 1 d . . .
H27A H 0.1068 0.4260 -0.0726 0.061 Uiso 1 1 calc R . .
H27B H 0.2205 0.3083 -0.0638 0.061 Uiso 1 1 calc R . .
C28 C 0.0505(8) 0.2852(8) -0.0194(6) 0.055(3) Uani 1 1 d . . .
H28A H -0.0189 0.3246 0.0141 0.066 Uiso 1 1 calc R . .
H28B H 0.0929 0.2081 0.0123 0.066 Uiso 1 1 calc R . .
C29 C -0.0074(7) 0.2721(7) -0.0967(6) 0.041(2) Uani 1 1 d . . .
C30 C -0.1267(8) 0.3318(9) -0.1286(7) 0.061(3) Uani 1 1 d . . .
H30A H -0.1888 0.3886 -0.1059 0.073 Uiso 1 1 calc R . .
C31 C -0.0325(8) 0.2193(7) -0.2175(6) 0.050(3) Uani 1 1 d . . .
C32 C 0.0017(9) 0.1663(9) -0.2870(7) 0.060(3) Uani 1 1 d . . .
H32A H -0.0565 0.1823 -0.3299 0.072 Uiso 1 1 calc R . .
C33 C 0.1265(10) 0.0888(9) -0.2887(8) 0.076(4) Uani 1 1 d . . .
H33A H 0.1515 0.0529 -0.3339 0.091 Uiso 1 1 calc R . .
C34 C 0.2165(10) 0.0631(9) -0.2238(9) 0.077(4) Uani 1 1 d . . .
H34A H 0.2991 0.0114 -0.2269 0.092 Uiso 1 1 calc R . .
C35 C 0.1804(9) 0.1157(9) -0.1550(8) 0.067(4) Uani 1 1 d . . .
H35A H 0.2369 0.0971 -0.1108 0.080 Uiso 1 1 calc R . .
C36 C 0.0566(8) 0.1978(8) -0.1542(6) 0.049(3) Uani 1 1 d . . .
C37 C 0.6029(7) 0.2853(7) -0.0164(6) 0.042(3) Uani 1 1 d . . .
C38 C 0.6588(10) 0.1587(8) -0.0254(6) 0.055(3) Uani 1 1 d . . .
H38A H 0.7508 0.1428 -0.0357 0.066 Uiso 1 1 calc R . .
H38B H 0.6492 0.1097 0.0269 0.066 Uiso 1 1 calc R . .
C39 C 0.6018(10) 0.1225(9) -0.0913(7) 0.061(3) Uani 1 1 d . . .
H39A H 0.5965 0.1792 -0.1421 0.074 Uiso 1 1 calc R . .
H39B H 0.5145 0.1222 -0.0757 0.074 Uiso 1 1 calc R . .
C40 C 0.6788(10) 0.0043(8) -0.1062(6) 0.058(3) Uani 1 1 d . . .
H40A H 0.6777 -0.0535 -0.0569 0.070 Uiso 1 1 calc R . .
H40B H 0.7680 0.0024 -0.1170 0.070 Uiso 1 1 calc R . .
C41 C 0.6273(8) -0.0275(9) -0.1780(7) 0.053(3) Uani 1 1 d . . .
C42 C 0.5735(8) -0.1187(8) -0.1752(7) 0.056(3) Uani 1 1 d . . .
H42A H 0.5607 -0.1690 -0.1277 0.067 Uiso 1 1 calc R . .
C43 C 0.5742(9) -0.0315(9) -0.3070(7) 0.058(3) Uani 1 1 d . . .
C44 C 0.5572(12) 0.0059(13) -0.3930(8) 0.088(4) Uani 1 1 d U . .
H44A H 0.5177 -0.0311 -0.4224 0.105 Uiso 1 1 calc R . .
C45 C 0.5975(15) 0.0935(13) -0.4319(10) 0.107(5) Uani 1 1 d U . .
H45A H 0.5895 0.1150 -0.4890 0.129 Uiso 1 1 calc R . .
C46 C 0.6517(13) 0.1543(13) -0.3893(8) 0.097(5) Uani 1 1 d . . .
H46A H 0.6764 0.2177 -0.4174 0.116 Uiso 1 1 calc R . .
C47 C 0.6689(9) 0.1189(9) -0.3026(7) 0.065(3) Uani 1 1 d . . .
H47A H 0.7074 0.1575 -0.2739 0.078 Uiso 1 1 calc R . .
C48 C 0.6290(7) 0.0282(8) -0.2617(6) 0.044(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Yb1 O5 2.246(6) . ?
Yb1 O4 2.258(6) 2_665 ?
Yb1 O6 2.285(5) 2_665 ?
Yb1 O3 2.286(6) . ?
Yb1 O1 2.419(6) . ?
Yb1 O2 2.470(6) . ?
Yb1 N2 2.500(8) . ?
Yb1 N1 2.544(6) . ?
Yb1 Yb1 4.2477(13) 2_665 ?
O1 C13 1.293(9) . ?
O2 C13 1.231(10) . ?
O3 C25 1.248(11) . ?
O4 C25 1.252(10) . ?
O4 Yb1 2.258(6) 2_665 ?
O5 C37 1.255(12) . ?
O6 C37 1.246(10) . ?
O6 Yb1 2.285(5) 2_665 ?
N1 C1 1.321(11) . ?
N1 C12 1.396(12) . ?
N2 C10 1.302(12) . ?
N2 C11 1.340(9) . ?
N3 C19 1.317(14) . ?
N3 C18 1.390(15) . ?
N4 C31 1.334(11) . ?
N4 C30 1.358(15) . ?
N5 C43 1.377(13) . ?
N5 C42 1.396(15) . ?
C1 C2 1.395(11) . ?
C2 C3 1.311(16) . ?
C3 C4 1.449(14) . ?
C4 C12 1.368(10) . ?
C4 C5 1.394(15) . ?
C5 C6 1.377(15) . ?
C6 C7 1.430(11) . ?
C7 C11 1.419(13) . ?
C7 C8 1.420(14) . ?
C8 C9 1.363(12) . ?
C9 C10 1.413(15) . ?
C11 C12 1.426(12) . ?
C13 C14 1.506(12) . ?
C14 C15 1.504(15) . ?
C15 C16 1.494(14) . ?
C16 C17 1.435(16) . ?
C17 C18 1.367(17) . ?
C17 C24 1.453(14) . ?
C19 C20 1.404(16) . ?
C19 C24 1.482(19) . ?
C20 C21 1.409(15) . ?
C21 C22 1.4302(11) . ?
C22 C23 1.321(14) . ?
C23 C24 1.421(17) . ?
C25 C26 1.547(13) . ?
C26 C27 1.496(14) . ?
C27 C28 1.496(13) . ?
C28 C29 1.519(14) . ?
C29 C30 1.353(11) . ?
C29 C36 1.449(14) . ?
C31 C36 1.399(14) . ?
C31 C32 1.408(15) . ?
C32 C33 1.397(13) . ?
C33 C34 1.418(18) . ?
C34 C35 1.398(18) . ?
C35 C36 1.409(12) . ?
C37 C38 1.517(12) . ?
C38 C39 1.492(15) . ?
C39 C40 1.493(13) . ?
C40 C41 1.512(16) . ?
C41 C42 1.409(14) . ?
C41 C48 1.420(14) . ?
C43 C44 1.411(16) . ?
C43 C48 1.416(15) . ?
C44 C45 1.322(19) . ?
C45 C46 1.39(2) . ?
C46 C47 1.419(17) . ?
C47 C48 1.362(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Yb1 O4 81.1(2) . 2_665 ?
O5 Yb1 O6 127.1(2) . 2_665 ?
O4 Yb1 O6 76.2(2) 2_665 2_665 ?
O5 Yb1 O3 73.4(2) . . ?
O4 Yb1 O3 127.0(2) 2_665 . ?
O6 Yb1 O3 83.3(2) 2_665 . ?
O5 Yb1 O1 95.3(2) . . ?
O4 Yb1 O1 148.2(2) 2_665 . ?
O6 Yb1 O1 127.5(2) 2_665 . ?
O3 Yb1 O1 80.9(2) . . ?
O5 Yb1 O2 137.4(2) . . ?
O4 Yb1 O2 141.1(2) 2_665 . ?
O6 Yb1 O2 74.2(2) 2_665 . ?
O3 Yb1 O2 73.7(2) . . ?
O1 Yb1 O2 53.30(19) . . ?
O5 Yb1 N2 137.9(2) . . ?
O4 Yb1 N2 78.9(2) 2_665 . ?
O6 Yb1 N2 83.0(2) 2_665 . ?
O3 Yb1 N2 146.3(2) . . ?
O1 Yb1 N2 83.3(2) . . ?
O2 Yb1 N2 73.0(2) . . ?
O5 Yb1 N1 73.7(2) . . ?
O4 Yb1 N1 74.5(2) 2_665 . ?
O6 Yb1 N1 140.2(2) 2_665 . ?
O3 Yb1 N1 136.2(2) . . ?
O1 Yb1 N1 74.2(2) . . ?
O2 Yb1 N1 115.4(2) . . ?
N2 Yb1 N1 65.4(2) . . ?
O5 Yb1 Yb1 62.93(15) . 2_665 ?
O4 Yb1 Yb1 60.01(17) 2_665 2_665 ?
O6 Yb1 Yb1 64.25(18) 2_665 2_665 ?
O3 Yb1 Yb1 67.00(16) . 2_665 ?
O1 Yb1 Yb1 144.89(15) . 2_665 ?
O2 Yb1 Yb1 124.69(13) . 2_665 ?
N2 Yb1 Yb1 131.59(14) . 2_665 ?
N1 Yb1 Yb1 119.94(17) . 2_665 ?
C13 O1 Yb1 93.3(5) . . ?
C13 O2 Yb1 92.5(5) . . ?
C25 O3 Yb1 134.9(6) . . ?
C25 O4 Yb1 148.5(6) . 2_665 ?
C37 O5 Yb1 144.7(5) . . ?
C37 O6 Yb1 140.7(6) . 2_665 ?
C1 N1 C12 117.6(7) . . ?
C1 N1 Yb1 125.5(6) . . ?
C12 N1 Yb1 116.5(5) . . ?
C10 N2 C11 118.9(8) . . ?
C10 N2 Yb1 121.7(6) . . ?
C11 N2 Yb1 118.9(6) . . ?
C19 N3 C18 107.6(11) . . ?
C31 N4 C30 110.4(8) . . ?
C43 N5 C42 107.1(9) . . ?
N1 C1 C2 122.7(9) . . ?
C3 C2 C1 121.4(10) . . ?
C2 C3 C4 118.1(8) . . ?
C12 C4 C5 121.1(10) . . ?
C12 C4 C3 118.6(10) . . ?
C5 C4 C3 120.2(8) . . ?
C6 C5 C4 119.9(9) . . ?
C5 C6 C7 120.4(10) . . ?
C11 C7 C8 116.0(8) . . ?
C11 C7 C6 119.7(9) . . ?
C8 C7 C6 124.3(10) . . ?
C9 C8 C7 120.4(10) . . ?
C8 C9 C10 117.9(9) . . ?
N2 C10 C9 123.7(8) . . ?
N2 C11 C7 123.0(8) . . ?
N2 C11 C12 119.6(8) . . ?
C7 C11 C12 117.4(7) . . ?
C4 C12 N1 121.5(9) . . ?
C4 C12 C11 121.4(9) . . ?
N1 C12 C11 117.0(7) . . ?
O2 C13 O1 120.8(8) . . ?
O2 C13 C14 120.1(8) . . ?
O1 C13 C14 119.0(7) . . ?
C15 C14 C13 114.7(8) . . ?
C16 C15 C14 116.5(9) . . ?
C17 C16 C15 118.6(10) . . ?
C18 C17 C16 126.7(10) . . ?
C18 C17 C24 102.4(11) . . ?
C16 C17 C24 129.2(11) . . ?
C17 C18 N3 114.5(10) . . ?
N3 C19 C20 131.9(14) . . ?
N3 C19 C24 108.1(10) . . ?
C20 C19 C24 120.0(12) . . ?
C19 C20 C21 118.3(13) . . ?
C20 C21 C22 117.0(6) . . ?
C23 C22 C21 128.1(8) . . ?
C22 C23 C24 114.3(13) . . ?
C23 C24 C17 132.3(13) . . ?
C23 C24 C19 120.7(11) . . ?
C17 C24 C19 107.0(11) . . ?
O3 C25 O4 126.4(9) . . ?
O3 C25 C26 117.2(8) . . ?
O4 C25 C26 116.3(8) . . ?
C27 C26 C25 117.7(7) . . ?
C28 C27 C26 112.3(8) . . ?
C27 C28 C29 113.9(8) . . ?
C30 C29 C36 105.7(9) . . ?
C30 C29 C28 127.2(9) . . ?
C36 C29 C28 127.0(7) . . ?
C29 C30 N4 109.7(9) . . ?
N4 C31 C36 107.7(10) . . ?
N4 C31 C32 131.0(10) . . ?
C36 C31 C32 121.2(8) . . ?
C33 C32 C31 117.2(10) . . ?
C32 C33 C34 122.2(12) . . ?
C35 C34 C33 119.7(10) . . ?
C34 C35 C36 118.5(11) . . ?
C31 C36 C35 120.9(10) . . ?
C31 C36 C29 106.3(7) . . ?
C35 C36 C29 132.7(10) . . ?
O6 C37 O5 127.0(8) . . ?
O6 C37 C38 115.1(9) . . ?
O5 C37 C38 117.9(7) . . ?
C39 C38 C37 116.6(8) . . ?
C38 C39 C40 112.6(8) . . ?
C39 C40 C41 112.4(8) . . ?
C42 C41 C48 107.7(10) . . ?
C42 C41 C40 127.1(9) . . ?
C48 C41 C40 125.2(9) . . ?
N5 C42 C41 109.0(9) . . ?
N5 C43 C44 129.5(12) . . ?
N5 C43 C48 110.5(10) . . ?
C44 C43 C48 120.0(10) . . ?
C45 C44 C43 120.0(14) . . ?
C44 C45 C46 121.4(15) . . ?
C45 C46 C47 119.6(13) . . ?
C48 C47 C46 119.7(12) . . ?
C47 C48 C43 119.2(10) . . ?
C47 C48 C41 135.1(11) . . ?
C43 C48 C41 105.7(8) . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        27.43
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         3.590
_refine_diff_density_min         -3.142
_refine_diff_density_rms         0.269
