# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2016

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

data_Eu
_database_code_depnum_ccdc_archive 'CCDC 1441102'
_audit_update_record             
;
2015-12-08 deposited with the CCDC.
2016-02-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C118 H108 N4 O28 Eu4, 15(H2O)'
_chemical_formula_sum            'C118 H138 Eu4 N4 O43'
_chemical_formula_weight         2908.16

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'
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'
N N 0.0061 0.0033 '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                   11.4422(4)
_cell_length_b                   13.6499(5)
_cell_length_c                   23.9769(8)
_cell_angle_alpha                92.915(3)
_cell_angle_beta                 103.671(3)
_cell_angle_gamma                112.821(3)
_cell_volume                     3311.2(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1920
_cell_measurement_theta_min      1.9
_cell_measurement_theta_max      20.4

_exptl_crystal_description       block
_exptl_crystal_colour            whiteless
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1470
_exptl_absorpt_coefficient_mu    1.949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8920
_exptl_absorpt_correction_T_max  0.9261
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_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 Smart Aepex CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26254
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_sigmaI/netI    0.0617
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.21
_diffrn_reflns_theta_max         25.00
_reflns_number_total             11675
_reflns_number_gt                9590
_reflns_threshold_expression     >2sigma(I)

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


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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0039P)²+219.4850P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11675
_refine_ls_number_parameters     772
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.1221
_refine_ls_R_factor_gt           0.1089
_refine_ls_wR_factor_ref         0.3022
_refine_ls_wR_factor_gt          0.2970
_refine_ls_goodness_of_fit_ref   1.224
_refine_ls_restrained_S_all      1.223
_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 0.37634(9) 0.29865(7) 0.51752(4) 0.0237(2) Uani 1 1 d . . .
Eu2 Eu 0.64560(9) -0.40266(7) 0.96192(4) 0.0308(3) Uani 1 1 d . . .
C1 C -0.292(2) 0.5010(18) 0.0763(9) 0.040(5) Uani 1 1 d . . .
C2 C -0.2172(19) 0.4736(17) 0.1287(8) 0.037(5) Uani 1 1 d . . .
C3 C -0.279(2) 0.3817(18) 0.1514(8) 0.042(5) Uani 1 1 d . . .
H3 H -0.3683 0.3393 0.1355 0.050 Uiso 1 1 calc R . .
C4 C -0.208(2) 0.3532(18) 0.1969(9) 0.043(5) Uani 1 1 d . . .
H4 H -0.2494 0.2897 0.2106 0.052 Uiso 1 1 calc R . .
C5 C -0.0757(18) 0.4185(17) 0.2229(8) 0.034(4) Uani 1 1 d . . .
C6 C 0.0195(18) 0.4132(16) 0.2728(8) 0.032(4) Uani 1 1 d . . .
C7 C 0.009(2) 0.3384(17) 0.3111(9) 0.042(5) Uani 1 1 d . . .
H7 H -0.0680 0.2763 0.3044 0.050 Uiso 1 1 calc R . .
C8 C 0.1140(19) 0.3567(15) 0.3585(8) 0.035(5) Uani 1 1 d . . .
H8 H 0.1070 0.3066 0.3838 0.042 Uiso 1 1 calc R . .
C9 C 0.2304(19) 0.4493(14) 0.3692(7) 0.030(4) Uani 1 1 d . . .
C10 C 0.3426(18) 0.4722(14) 0.4212(8) 0.032(4) Uani 1 1 d . . .
C11 C 0.2428(19) 0.5222(16) 0.3309(8) 0.036(5) Uani 1 1 d . . .
H11 H 0.3214 0.5830 0.3372 0.043 Uiso 1 1 calc R . .
C12 C 0.1381(18) 0.5044(16) 0.2834(8) 0.033(4) Uani 1 1 d . . .
C13 C 0.1262(19) 0.5761(17) 0.2370(8) 0.039(5) Uani 1 1 d . . .
C14 C 0.227(2) 0.584(3) 0.2014(11) 0.069(9) Uani 1 1 d . . .
H14A H 0.2195 0.5140 0.1863 0.083 Uiso 1 1 d R . .
H14B H 0.3144 0.6237 0.2267 0.083 Uiso 1 1 d R . .
H14C H 0.2116 0.6215 0.1695 0.083 Uiso 1 1 d R . .
C15 C 0.147(3) 0.6860(19) 0.2634(12) 0.068(8) Uani 1 1 d . . .
H15A H 0.1307 0.7256 0.2326 0.081 Uiso 1 1 d R . .
H15B H 0.2359 0.7237 0.2876 0.081 Uiso 1 1 d R . .
H15C H 0.0873 0.6787 0.2867 0.081 Uiso 1 1 d R . .
C16 C -0.0161(19) 0.5121(16) 0.2007(8) 0.036(5) Uani 1 1 d . . .
C17 C -0.0855(19) 0.5396(18) 0.1536(9) 0.042(5) Uani 1 1 d . . .
H17 H -0.0444 0.6016 0.1388 0.051 Uiso 1 1 calc R . .
C18 C -0.452(2) -0.3362(15) 0.0750(8) 0.036(5) Uani 1 1 d . . .
C19 C -0.3831(15) -0.2800(13) 0.1356(7) 0.020(3) Uani 1 1 d . . .
C20 C -0.432(2) -0.3056(17) 0.1807(9) 0.041(5) Uani 1 1 d . . .
H20 H -0.5148 -0.3624 0.1739 0.050 Uiso 1 1 calc R . .
C21 C -0.368(2) -0.2528(16) 0.2359(9) 0.040(5) Uani 1 1 d . . .
H21 H -0.4060 -0.2733 0.2661 0.047 Uiso 1 1 calc R . .
C22 C -0.2440(19) -0.1669(15) 0.2467(8) 0.032(4) Uani 1 1 d . . .
C23 C -0.1520(19) -0.0962(16) 0.3000(8) 0.034(4) Uani 1 1 d . . .
C24 C -0.157(2) -0.0971(16) 0.3576(8) 0.035(4) Uani 1 1 d . . .
H24 H -0.2278 -0.1488 0.3669 0.042 Uiso 1 1 calc R . .
C25 C -0.0535(19) -0.0196(15) 0.4010(8) 0.034(4) Uani 1 1 d . . .
H25 H -0.0573 -0.0177 0.4393 0.040 Uiso 1 1 calc R . .
C26 C 0.0530(18) 0.0535(16) 0.3879(8) 0.031(4) Uani 1 1 d . . .
C27 C 0.1689(18) 0.1382(15) 0.4353(8) 0.030(4) Uani 1 1 d . . .
C28 C 0.0607(18) 0.0546(15) 0.3300(8) 0.031(4) Uani 1 1 d . . .
H28 H 0.1327 0.1053 0.3208 0.038 Uiso 1 1 calc R . .
C29 C -0.0414(19) -0.0214(16) 0.2884(8) 0.034(4) Uani 1 1 d . . .
C30 C -0.0567(19) -0.0369(16) 0.2224(8) 0.036(5) Uani 1 1 d . . .
C31 C 0.052(2) -0.068(2) 0.2107(11) 0.064(8) Uani 1 1 d . . .
H31A H 0.0563 -0.1260 0.2307 0.077 Uiso 1 1 d R . .
H31B H 0.1340 -0.0062 0.2244 0.077 Uiso 1 1 d R . .
H31C H 0.0336 -0.0887 0.1694 0.077 Uiso 1 1 d R . .
C32 C -0.052(3) 0.061(2) 0.1958(12) 0.067(8) Uani 1 1 d . . .
H32A H -0.0737 0.0446 0.1540 0.081 Uiso 1 1 d R . .
H32B H 0.0328 0.1195 0.2101 0.081 Uiso 1 1 d R . .
H32C H -0.1168 0.0823 0.2060 0.081 Uiso 1 1 d R . .
C33 C -0.1916(19) -0.1330(16) 0.2006(9) 0.036(4) Uani 1 1 d . . .
C34 C -0.2533(17) -0.1876(13) 0.1467(7) 0.024(4) Uani 1 1 d . . .
H34 H -0.2151 -0.1678 0.1166 0.028 Uiso 1 1 calc R . .
C35 C 0.4620(18) 0.1605(16) 0.5814(8) 0.033(4) Uani 1 1 d . . .
C36 C 0.4966(18) 0.0812(15) 0.6144(8) 0.031(4) Uani 1 1 d . . .
C37 C 0.531(2) 0.0066(15) 0.5884(8) 0.035(4) Uani 1 1 d . . .
H37 H 0.5322 0.0070 0.5497 0.042 Uiso 1 1 calc R . .
C38 C 0.563(2) -0.0676(17) 0.6177(9) 0.038(5) Uani 1 1 d . . .
H38 H 0.5874 -0.1158 0.5997 0.046 Uiso 1 1 calc R . .
C39 C 0.5577(19) -0.0680(15) 0.6761(8) 0.030(4) Uani 1 1 d . . .
C40 C 0.579(2) -0.1390(16) 0.7163(9) 0.036(4) Uani 1 1 d . . .
C41 C 0.618(2) -0.2255(17) 0.7132(10) 0.044(5) Uani 1 1 d . . .
H41 H 0.6348 -0.2473 0.6797 0.053 Uiso 1 1 calc R . .
C42 C 0.631(2) -0.2752(16) 0.7599(10) 0.042(5) Uani 1 1 d . . .
H42 H 0.6547 -0.3327 0.7571 0.050 Uiso 1 1 calc R . .
C43 C 0.611(2) -0.2468(16) 0.8108(8) 0.034(4) Uani 1 1 d . . .
C44 C 0.627(2) -0.2983(16) 0.8621(11) 0.046(6) Uani 1 1 d . . .
C45 C 0.575(2) -0.1569(16) 0.8153(9) 0.036(5) Uani 1 1 d . . .
H45 H 0.5645 -0.1334 0.8502 0.044 Uiso 1 1 calc R . .
C46 C 0.5564(17) -0.1062(15) 0.7685(7) 0.028(4) Uani 1 1 d . . .
C47 C 0.5173(19) -0.0139(15) 0.7633(8) 0.030(4) Uani 1 1 d . . .
C48 C 0.611(3) 0.0819(18) 0.8094(9) 0.050(6) Uani 1 1 d . . .
H48A H 0.6165 0.0630 0.8479 0.060 Uiso 1 1 d R . .
H48B H 0.5799 0.1382 0.8061 0.060 Uiso 1 1 d R . .
H48C H 0.6959 0.1063 0.8025 0.060 Uiso 1 1 d R . .
C49 C 0.373(2) -0.0488(18) 0.7681(10) 0.043(5) Uani 1 1 d . . .
H49A H 0.3151 -0.1133 0.7411 0.052 Uiso 1 1 d R . .
H49B H 0.3444 0.0077 0.7594 0.052 Uiso 1 1 d R . .
H49C H 0.3717 -0.0616 0.8073 0.052 Uiso 1 1 d R . .
C50 C 0.5210(17) 0.0045(16) 0.7018(8) 0.030(4) Uani 1 1 d . . .
C51 C 0.4913(19) 0.0791(15) 0.6722(8) 0.032(4) Uani 1 1 d . . .
H51 H 0.4678 0.1278 0.6902 0.038 Uiso 1 1 calc R . .
C52 C 0.113(3) 0.434(3) 0.5376(18) 0.104(11) Uani 1 1 d U . .
H52A H 0.0285 0.3806 0.5374 0.125 Uiso 1 1 d R . .
H52B H 0.1281 0.4241 0.5001 0.125 Uiso 1 1 d R . .
H52C H 0.1152 0.5041 0.5455 0.125 Uiso 1 1 d R . .
C53 C 0.217(3) 0.419(2) 0.5848(14) 0.068(6) Uani 1 1 d U . .
C54 C 0.211(7) 0.555(4) 0.654(2) 0.19(3) Uani 1 1 d U . .
H54A H 0.2503 0.6206 0.6394 0.226 Uiso 1 1 d R . .
H54B H 0.2343 0.5678 0.6957 0.226 Uiso 1 1 d R . .
H54C H 0.1173 0.5263 0.6385 0.226 Uiso 1 1 d R . .
C55 C 0.353(5) 0.450(4) 0.6798(18) 0.15(2) Uani 1 1 d U . .
H55A H 0.3165 0.3864 0.6966 0.181 Uiso 1 1 d R . .
H55B H 0.3942 0.5116 0.7100 0.181 Uiso 1 1 d R . .
H55C H 0.4175 0.4439 0.6619 0.181 Uiso 1 1 d R . .
C56 C 0.807(4) 0.170(4) 0.4214(18) 0.115(15) Uani 1 1 d . . .
H56A H 0.8992 0.1910 0.4267 0.138 Uiso 1 1 d R . .
H56B H 0.7692 0.1869 0.3846 0.138 Uiso 1 1 d R . .
H56C H 0.7652 0.0942 0.4215 0.138 Uiso 1 1 d R . .
C57 C 0.780(4) 0.237(3) 0.479(3) 0.16(3) Uani 1 1 d . . .
C58 C 0.794(4) 0.280(4) 0.5672(19) 0.119(15) Uani 1 1 d . . .
H58A H 0.7604 0.3308 0.5517 0.143 Uiso 1 1 d R . .
H58B H 0.8776 0.3179 0.5952 0.143 Uiso 1 1 d R . .
H58C H 0.7336 0.2327 0.5859 0.143 Uiso 1 1 d R . .
C59 C 0.857(5) 0.129(4) 0.532(3) 0.18(3) Uani 1 1 d . . .
H59A H 0.7867 0.0580 0.5242 0.219 Uiso 1 1 d R . .
H59B H 0.8941 0.1505 0.5734 0.219 Uiso 1 1 d R . .
H59C H 0.9243 0.1275 0.5149 0.219 Uiso 1 1 d R . .
N1 N 0.808(4) 0.201(4) 0.509(3) 0.19(3) Uani 1 1 d . . .
N2 N 0.255(4) 0.476(2) 0.6303(12) 0.096(9) Uani 1 1 d U . .
O1 O -0.2304(15) 0.5607(15) 0.0465(7) 0.059(5) Uani 1 1 d . . .
O2 O -0.4168(14) 0.4630(13) 0.0648(7) 0.056(5) Uani 1 1 d . . .
O3 O 0.4536(13) 0.5438(12) 0.4235(6) 0.048(4) Uani 1 1 d . . .
O4 O 0.3180(13) 0.4203(10) 0.4631(5) 0.033(3) Uani 1 1 d . . .
O5 O -0.3936(16) -0.3087(13) 0.0354(7) 0.051(4) Uani 1 1 d . . .
O6 O -0.5645(14) -0.4124(11) 0.0665(7) 0.046(4) Uani 1 1 d . . .
O7 O 0.2684(13) 0.1961(10) 0.4213(5) 0.032(3) Uani 1 1 d . . .
O8 O 0.1596(14) 0.1463(12) 0.4858(6) 0.044(4) Uani 1 1 d . . .
O9 O 0.4570(15) 0.1563(12) 0.5284(6) 0.043(4) Uani 1 1 d . . .
O10 O 0.4353(15) 0.2304(11) 0.6069(6) 0.038(3) Uani 1 1 d . . .
O11 O 0.6367(18) -0.3892(13) 0.8579(7) 0.056(4) Uani 1 1 d . . .
O12 O 0.6278(18) -0.2584(13) 0.9120(6) 0.051(4) Uani 1 1 d . . .
O13 O 0.5433(15) 0.3584(12) 0.4645(7) 0.049(4) Uani 1 1 d . . .
O14 O 0.2616(17) 0.3528(14) 0.5725(8) 0.057(4) Uani 1 1 d . . .
O15 O 0.739(2) 0.3039(19) 0.4591(12) 0.099(8) Uani 1 1 d . . .
O16 O 0.0000 0.5000 0.0000 0.45(7) Uani 1 2 d SU . .
O17 O 0.887(11) 0.955(9) 0.975(5) 0.25(5) Uani 0.50 1 d PU . .
O18 O 0.436(14) 0.039(14) 0.985(10) 0.48(14) Uani 0.50 1 d P . .
O19 O 0.843(6) -0.424(4) 0.941(2) 0.26(2) Uani 1 1 d DU . .
O20 O 0.871(4) -0.279(3) 0.9779(17) 0.178(15) Uani 1 1 d DU . .
O21 O 0.004(6) 0.707(5) 0.918(5) 0.40(6) Uani 1 1 d . . .
O22 O 0.046(8) 0.816(11) 0.055(3) 0.77(15) Uani 1 1 d . . .
O23 O 0.134(16) 0.711(10) 0.986(4) 0.56(9) 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 O14 2.340(16) . ?
Eu1 O3 2.357(14) 2_666 ?
Eu1 O4 2.361(12) . ?
Eu1 O7 2.406(13) . ?
Eu1 O10 2.435(12) . ?
Eu1 O13 2.444(14) . ?
Eu1 O8 2.449(14) . ?
Eu1 O9 2.455(13) . ?
Eu1 C27 2.763(18) . ?
Eu1 C35 2.807(19) . ?
Eu2 O6 2.326(14) 2_546 ?
Eu2 O2 2.329(14) 2_556 ?
Eu2 O5 2.355(17) 1_656 ?
Eu2 O1 2.380(13) 1_646 ?
Eu2 O20 2.40(4) . ?
Eu2 O12 2.406(14) . ?
Eu2 O11 2.490(15) . ?
Eu2 O19 2.55(5) . ?
Eu2 C44 2.85(2) . ?
Eu2 C1 3.152(19) 1_646 ?
Eu2 Eu2 4.2425(19) 2_647 ?
C1 O1 1.23(3) . ?
C1 O2 1.27(3) . ?
C1 C2 1.49(2) . ?
C1 Eu2 3.152(19) 1_464 ?
C2 C17 1.38(3) . ?
C2 C3 1.39(3) . ?
C3 C4 1.36(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.39(3) . ?
C4 H4 0.9300 . ?
C5 C16 1.40(3) . ?
C5 C6 1.44(2) . ?
C6 C7 1.40(3) . ?
C6 C12 1.40(3) . ?
C7 C8 1.37(3) . ?
C7 H7 0.9300 . ?
C8 C9 1.39(3) . ?
C8 H8 0.9300 . ?
C9 C11 1.38(2) . ?
C9 C10 1.48(2) . ?
C10 O3 1.25(2) . ?
C10 O4 1.28(2) . ?
C11 C12 1.38(2) . ?
C11 H11 0.9300 . ?
C12 C13 1.53(2) . ?
C13 C15 1.50(3) . ?
C13 C16 1.52(3) . ?
C13 C14 1.57(3) . ?
C14 H14A 0.9618 . ?
C14 H14B 0.9562 . ?
C14 H14C 0.9650 . ?
C15 H15A 0.9648 . ?
C15 H15B 0.9560 . ?
C15 H15C 0.9625 . ?
C16 C17 1.38(3) . ?
C17 H17 0.9300 . ?
C18 O6 1.26(2) . ?
C18 O5 1.28(3) . ?
C18 C19 1.48(2) . ?
C19 C20 1.34(3) . ?
C19 C34 1.48(2) . ?
C20 C21 1.36(3) . ?
C20 H20 0.9300 . ?
C21 C22 1.40(3) . ?
C21 H21 0.9300 . ?
C22 C33 1.39(3) . ?
C22 C23 1.46(3) . ?
C23 C29 1.38(3) . ?
C23 C24 1.40(3) . ?
C24 C25 1.39(3) . ?
C24 H24 0.9300 . ?
C25 C26 1.36(3) . ?
C25 H25 0.9300 . ?
C26 C28 1.41(3) . ?
C26 C27 1.53(2) . ?
C27 O7 1.24(2) . ?
C27 O8 1.24(2) . ?
C28 C29 1.36(3) . ?
C28 H28 0.9300 . ?
C29 C30 1.55(3) . ?
C30 C32 1.50(3) . ?
C30 C31 1.53(3) . ?
C30 C33 1.53(3) . ?
C31 H31A 0.9630 . ?
C31 H31B 0.9548 . ?
C31 H31C 0.9665 . ?
C32 H32A 0.9665 . ?
C32 H32B 0.9546 . ?
C32 H32C 0.9612 . ?
C33 C34 1.34(2) . ?
C34 H34 0.9300 . ?
C35 O9 1.25(2) . ?
C35 O10 1.28(2) . ?
C35 C36 1.49(3) . ?
C36 C37 1.39(3) . ?
C36 C51 1.40(3) . ?
C37 C38 1.38(3) . ?
C37 H37 0.9300 . ?
C38 C39 1.42(3) . ?
C38 H38 0.9300 . ?
C39 C50 1.39(3) . ?
C39 C40 1.45(3) . ?
C40 C41 1.42(3) . ?
C40 C46 1.42(3) . ?
C41 C42 1.34(3) . ?
C41 H41 0.9300 . ?
C42 C43 1.36(3) . ?
C42 H42 0.9300 . ?
C43 C45 1.44(3) . ?
C43 C44 1.46(3) . ?
C44 O12 1.28(3) . ?
C44 O11 1.29(3) . ?
C45 C46 1.37(2) . ?
C45 H45 0.9300 . ?
C46 C47 1.49(3) . ?
C47 C48 1.51(3) . ?
C47 C50 1.51(2) . ?
C47 C49 1.57(3) . ?
C48 H48A 0.9666 . ?
C48 H48B 0.9621 . ?
C48 H48C 0.9573 . ?
C49 H49A 0.9588 . ?
C49 H49B 0.9622 . ?
C49 H49C 0.9669 . ?
C50 C51 1.37(3) . ?
C51 H51 0.9300 . ?
C52 C53 1.51(4) . ?
C52 H52A 0.9552 . ?
C52 H52B 0.9669 . ?
C52 H52C 0.9616 . ?
C53 N2 1.18(4) . ?
C53 O14 1.26(3) . ?
C54 N2 1.49(4) . ?
C54 H54A 0.9603 . ?
C54 H54B 0.9665 . ?
C54 H54C 0.9553 . ?
C55 N2 1.59(5) . ?
C55 H55A 0.9609 . ?
C55 H55B 0.9614 . ?
C55 H55C 0.9617 . ?
C56 C57 1.77(8) . ?
C56 H56A 0.9559 . ?
C56 H56B 0.9650 . ?
C56 H56C 0.9587 . ?
C57 N1 0.95(6) . ?
C57 O15 1.24(5) . ?
C58 N1 1.80(8) . ?
C58 H58A 0.9625 . ?
C58 H58B 0.9570 . ?
C58 H58C 0.9601 . ?
C59 N1 1.40(5) . ?
C59 H59A 0.9600 . ?
C59 H59B 0.9600 . ?
C59 H59C 0.9600 . ?
O1 Eu2 2.380(13) 1_464 ?
O2 Eu2 2.329(14) 2_556 ?
O3 Eu1 2.357(14) 2_666 ?
O5 Eu2 2.355(17) 1_454 ?
O6 Eu2 2.326(14) 2_546 ?

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
O14 Eu1 O3 78.8(6) . 2_666 ?
O14 Eu1 O4 77.9(5) . . ?
O3 Eu1 O4 84.0(5) 2_666 . ?
O14 Eu1 O7 121.7(6) . . ?
O3 Eu1 O7 147.1(5) 2_666 . ?
O4 Eu1 O7 76.8(4) . . ?
O14 Eu1 O10 79.7(5) . . ?
O3 Eu1 O10 79.0(5) 2_666 . ?
O4 Eu1 O10 154.0(5) . . ?
O7 Eu1 O10 126.9(5) . . ?
O14 Eu1 O13 145.4(6) . . ?
O3 Eu1 O13 75.0(6) 2_666 . ?
O4 Eu1 O13 77.3(5) . . ?
O7 Eu1 O13 74.9(5) . . ?
O10 Eu1 O13 116.3(5) . . ?
O14 Eu1 O8 79.2(6) . . ?
O3 Eu1 O8 157.3(5) 2_666 . ?
O4 Eu1 O8 97.0(5) . . ?
O7 Eu1 O8 53.4(4) . . ?
O10 Eu1 O8 91.4(5) . . ?
O13 Eu1 O8 127.5(5) . . ?
O14 Eu1 O9 129.4(5) . . ?
O3 Eu1 O9 106.4(5) 2_666 . ?
O4 Eu1 O9 151.8(5) . . ?
O7 Eu1 O9 81.1(5) . . ?
O10 Eu1 O9 53.5(5) . . ?
O13 Eu1 O9 80.3(5) . . ?
O8 Eu1 O9 83.3(5) . . ?
O14 Eu1 C27 100.6(6) . . ?
O3 Eu1 C27 169.9(5) 2_666 . ?
O4 Eu1 C27 86.0(5) . . ?
O7 Eu1 C27 26.7(5) . . ?
O10 Eu1 C27 111.0(5) . . ?
O13 Eu1 C27 101.3(6) . . ?
O8 Eu1 C27 26.7(5) . . ?
O9 Eu1 C27 81.9(5) . . ?
O14 Eu1 C35 104.7(6) . . ?
O3 Eu1 C35 93.9(5) 2_666 . ?
O4 Eu1 C35 176.3(5) . . ?
O7 Eu1 C35 103.7(5) . . ?
O10 Eu1 C35 27.1(5) . . ?
O13 Eu1 C35 99.3(5) . . ?
O8 Eu1 C35 86.1(5) . . ?
O9 Eu1 C35 26.5(5) . . ?
C27 Eu1 C35 96.1(6) . . ?
O6 Eu2 O2 74.9(6) 2_546 2_556 ?
O6 Eu2 O5 128.6(6) 2_546 1_656 ?
O2 Eu2 O5 76.5(6) 2_556 1_656 ?
O6 Eu2 O1 82.9(6) 2_546 1_646 ?
O2 Eu2 O1 124.2(6) 2_556 1_646 ?
O5 Eu2 O1 79.3(6) 1_656 1_646 ?
O6 Eu2 O20 124.8(10) 2_546 . ?
O2 Eu2 O20 157.4(10) 2_556 . ?
O5 Eu2 O20 95.2(11) 1_656 . ?
O1 Eu2 O20 73.4(10) 1_646 . ?
O6 Eu2 O12 133.3(5) 2_546 . ?
O2 Eu2 O12 81.2(6) 2_556 . ?
O5 Eu2 O12 81.8(5) 1_656 . ?
O1 Eu2 O12 142.7(6) 1_646 . ?
O20 Eu2 O12 76.8(10) . . ?
O6 Eu2 O11 85.8(5) 2_546 . ?
O2 Eu2 O11 87.9(6) 2_556 . ?
O5 Eu2 O11 134.4(5) 1_656 . ?
O1 Eu2 O11 141.0(6) 1_646 . ?
O20 Eu2 O11 83.1(10) . . ?
O12 Eu2 O11 53.4(5) . . ?
O6 Eu2 O19 77.7(11) 2_546 . ?
O2 Eu2 O19 146.3(12) 2_556 . ?
O5 Eu2 O19 136.9(12) 1_656 . ?
O1 Eu2 O19 70.4(14) 1_646 . ?
O20 Eu2 O19 47.6(7) . . ?
O12 Eu2 O19 104.4(13) . . ?
O11 Eu2 O19 70.8(13) . . ?
O6 Eu2 C44 110.1(6) 2_546 . ?
O2 Eu2 C44 83.6(6) 2_556 . ?
O5 Eu2 C44 108.0(6) 1_656 . ?
O1 Eu2 C44 152.0(6) 1_646 . ?
O20 Eu2 C44 79.0(10) . . ?
O12 Eu2 C44 26.6(6) . . ?
O11 Eu2 C44 26.8(6) . . ?
O19 Eu2 C44 87.8(14) . . ?
O6 Eu2 C1 73.9(5) 2_546 1_646 ?
O2 Eu2 C1 104.0(6) 2_556 1_646 ?
O5 Eu2 C1 73.0(6) 1_656 1_646 ?
O1 Eu2 C1 20.3(6) 1_646 1_646 ?
O20 Eu2 C1 93.2(10) . 1_646 ?
O12 Eu2 C1 151.9(6) . 1_646 ?
O11 Eu2 C1 152.5(6) . 1_646 ?
O19 Eu2 C1 86.6(13) . 1_646 ?
C44 Eu2 C1 172.2(6) . 1_646 ?
O6 Eu2 Eu2 63.9(4) 2_546 2_647 ?
O2 Eu2 Eu2 48.2(4) 2_556 2_647 ?
O5 Eu2 Eu2 65.1(4) 1_656 2_647 ?
O1 Eu2 Eu2 76.1(4) 1_646 2_647 ?
O20 Eu2 Eu2 146.3(9) . 2_647 ?
O12 Eu2 Eu2 123.3(4) . 2_647 ?
O11 Eu2 Eu2 130.4(4) . 2_647 ?
O19 Eu2 Eu2 131.4(12) . 2_647 ?
C44 Eu2 Eu2 131.8(4) . 2_647 ?
C1 Eu2 Eu2 55.9(4) 1_646 2_647 ?
O1 C1 O2 122.4(18) . . ?
O1 C1 C2 119.2(19) . . ?
O2 C1 C2 118.3(19) . . ?
O1 C1 Eu2 41.9(9) . 1_464 ?
O2 C1 Eu2 80.6(11) . 1_464 ?
C2 C1 Eu2 161.0(15) . 1_464 ?
C17 C2 C3 120.2(17) . . ?
C17 C2 C1 119.2(19) . . ?
C3 C2 C1 120.5(18) . . ?
C4 C3 C2 120.5(18) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 120.4(19) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C4 C5 C16 118.5(17) . . ?
C4 C5 C6 132.7(18) . . ?
C16 C5 C6 108.7(16) . . ?
C7 C6 C12 118.6(16) . . ?
C7 C6 C5 131.6(17) . . ?
C12 C6 C5 109.7(16) . . ?
C8 C7 C6 119.9(17) . . ?
C8 C7 H7 120.1 . . ?
C6 C7 H7 120.1 . . ?
C7 C8 C9 120.8(16) . . ?
C7 C8 H8 119.6 . . ?
C9 C8 H8 119.6 . . ?
C11 C9 C8 119.9(16) . . ?
C11 C9 C10 118.6(17) . . ?
C8 C9 C10 121.5(16) . . ?
O3 C10 O4 123.4(16) . . ?
O3 C10 C9 119.3(17) . . ?
O4 C10 C9 117.1(17) . . ?
C9 C11 C12 119.5(18) . . ?
C9 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
C11 C12 C6 121.2(17) . . ?
C11 C12 C13 128.9(17) . . ?
C6 C12 C13 109.8(15) . . ?
C15 C13 C16 111.5(19) . . ?
C15 C13 C12 111.8(18) . . ?
C16 C13 C12 101.0(15) . . ?
C15 C13 C14 111(2) . . ?
C16 C13 C14 112.0(18) . . ?
C12 C13 C14 109.0(18) . . ?
C13 C14 H14A 112.5 . . ?
C13 C14 H14B 107.9 . . ?
H14A C14 H14B 109.4 . . ?
C13 C14 H14C 108.1 . . ?
H14A C14 H14C 109.2 . . ?
H14B C14 H14C 109.7 . . ?
C13 C15 H15A 108.7 . . ?
C13 C15 H15B 110.4 . . ?
H15A C15 H15B 109.7 . . ?
C13 C15 H15C 109.3 . . ?
H15A C15 H15C 109.7 . . ?
H15B C15 H15C 108.9 . . ?
C17 C16 C5 121.4(18) . . ?
C17 C16 C13 127.8(17) . . ?
C5 C16 C13 110.8(15) . . ?
C16 C17 C2 119.0(18) . . ?
C16 C17 H17 120.5 . . ?
C2 C17 H17 120.5 . . ?
O6 C18 O5 124.1(19) . . ?
O6 C18 C19 116.7(18) . . ?
O5 C18 C19 119.1(18) . . ?
C20 C19 C34 117.7(15) . . ?
C20 C19 C18 124.1(16) . . ?
C34 C19 C18 118.2(15) . . ?
C19 C20 C21 123.3(18) . . ?
C19 C20 H20 118.3 . . ?
C21 C20 H20 118.3 . . ?
C20 C21 C22 119.0(19) . . ?
C20 C21 H21 120.5 . . ?
C22 C21 H21 120.5 . . ?
C33 C22 C21 120.0(18) . . ?
C33 C22 C23 108.0(17) . . ?
C21 C22 C23 131.9(19) . . ?
C29 C23 C24 118.6(18) . . ?
C29 C23 C22 110.6(17) . . ?
C24 C23 C22 130.7(18) . . ?
C25 C24 C23 119.0(18) . . ?
C25 C24 H24 120.5 . . ?
C23 C24 H24 120.5 . . ?
C26 C25 C24 120.6(18) . . ?
C26 C25 H25 119.7 . . ?
C24 C25 H25 119.7 . . ?
C25 C26 C28 121.2(17) . . ?
C25 C26 C27 121.3(17) . . ?
C28 C26 C27 117.5(17) . . ?
O7 C27 O8 122.8(17) . . ?
O7 C27 C26 118.2(17) . . ?
O8 C27 C26 119.1(17) . . ?
O7 C27 Eu1 60.4(9) . . ?
O8 C27 Eu1 62.4(10) . . ?
C26 C27 Eu1 177.1(13) . . ?
C29 C28 C26 117.1(17) . . ?
C29 C28 H28 121.5 . . ?
C26 C28 H28 121.5 . . ?
C28 C29 C23 123.4(18) . . ?
C28 C29 C30 127.1(18) . . ?
C23 C29 C30 109.5(16) . . ?
C32 C30 C31 109(2) . . ?
C32 C30 C33 113.2(18) . . ?
C31 C30 C33 110.4(18) . . ?
C32 C30 C29 112.9(18) . . ?
C31 C30 C29 109.9(18) . . ?
C33 C30 C29 100.9(15) . . ?
C30 C31 H31A 110.5 . . ?
C30 C31 H31B 108.2 . . ?
H31A C31 H31B 109.4 . . ?
C30 C31 H31C 109.6 . . ?
H31A C31 H31C 109.7 . . ?
H31B C31 H31C 109.4 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 111.1 . . ?
H32A C32 H32B 109.4 . . ?
C30 C32 H32C 108.0 . . ?
H32A C32 H32C 109.8 . . ?
H32B C32 H32C 109.1 . . ?
C34 C33 C22 120.5(18) . . ?
C34 C33 C30 128.3(18) . . ?
C22 C33 C30 111.0(17) . . ?
C33 C34 C19 119.3(15) . . ?
C33 C34 H34 120.3 . . ?
C19 C34 H34 120.3 . . ?
O9 C35 O10 120.8(17) . . ?
O9 C35 C36 119.4(18) . . ?
O10 C35 C36 119.7(16) . . ?
O9 C35 Eu1 60.9(10) . . ?
O10 C35 Eu1 60.0(9) . . ?
C36 C35 Eu1 175.6(13) . . ?
C37 C36 C51 119.0(17) . . ?
C37 C36 C35 121.1(17) . . ?
C51 C36 C35 119.9(17) . . ?
C38 C37 C36 122.4(18) . . ?
C38 C37 H37 118.8 . . ?
C36 C37 H37 118.8 . . ?
C37 C38 C39 117.6(18) . . ?
C37 C38 H38 121.2 . . ?
C39 C38 H38 121.2 . . ?
C50 C39 C38 120.1(17) . . ?
C50 C39 C40 109.8(16) . . ?
C38 C39 C40 130.0(18) . . ?
C41 C40 C46 119.5(18) . . ?
C41 C40 C39 133.8(19) . . ?
C46 C40 C39 106.7(17) . . ?
C42 C41 C40 119(2) . . ?
C42 C41 H41 120.7 . . ?
C40 C41 H41 120.7 . . ?
C41 C42 C43 124(2) . . ?
C41 C42 H42 117.9 . . ?
C43 C42 H42 117.9 . . ?
C42 C43 C45 117.9(17) . . ?
C42 C43 C44 124.8(19) . . ?
C45 C43 C44 117.3(18) . . ?
O12 C44 O11 117.5(19) . . ?
O12 C44 C43 122.6(18) . . ?
O11 C44 C43 120(2) . . ?
O12 C44 Eu2 56.9(10) . . ?
O11 C44 Eu2 60.6(11) . . ?
C43 C44 Eu2 177.4(15) . . ?
C46 C45 C43 120.1(19) . . ?
C46 C45 H45 120.0 . . ?
C43 C45 H45 120.0 . . ?
C45 C46 C40 119.6(18) . . ?
C45 C46 C47 128.9(18) . . ?
C40 C46 C47 111.4(15) . . ?
C46 C47 C48 111.4(16) . . ?
C46 C47 C50 101.4(15) . . ?
C48 C47 C50 114.1(16) . . ?
C46 C47 C49 110.0(15) . . ?
C48 C47 C49 109.9(18) . . ?
C50 C47 C49 109.8(16) . . ?
C47 C48 H48A 111.3 . . ?
C47 C48 H48B 109.1 . . ?
H48A C48 H48B 109.4 . . ?
C47 C48 H48C 107.8 . . ?
H48A C48 H48C 109.7 . . ?
H48B C48 H48C 109.5 . . ?
C47 C49 H49A 109.7 . . ?
C47 C49 H49B 109.4 . . ?
H49A C49 H49B 109.5 . . ?
C47 C49 H49C 109.0 . . ?
H49A C49 H49C 109.8 . . ?
H49B C49 H49C 109.5 . . ?
C51 C50 C39 121.4(17) . . ?
C51 C50 C47 128.0(18) . . ?
C39 C50 C47 110.6(16) . . ?
C50 C51 C36 119.4(18) . . ?
C50 C51 H51 120.3 . . ?
C36 C51 H51 120.3 . . ?
C53 C52 H52A 108.1 . . ?
C53 C52 H52B 110.5 . . ?
H52A C52 H52B 109.6 . . ?
C53 C52 H52C 109.8 . . ?
H52A C52 H52C 109.3 . . ?
H52B C52 H52C 109.5 . . ?
N2 C53 O14 124(3) . . ?
N2 C53 C52 118(3) . . ?
O14 C53 C52 118(3) . . ?
N2 C54 H54A 107.8 . . ?
N2 C54 H54B 113.5 . . ?
H54A C54 H54B 109.9 . . ?
N2 C54 H54C 107.1 . . ?
H54A C54 H54C 109.0 . . ?
H54B C54 H54C 109.4 . . ?
N2 C55 H55A 117.3 . . ?
N2 C55 H55B 106.1 . . ?
H55A C55 H55B 108.9 . . ?
N2 C55 H55C 104.8 . . ?
H55A C55 H55C 109.4 . . ?
H55B C55 H55C 110.1 . . ?
C57 C56 H56A 110.5 . . ?
C57 C56 H56B 110.3 . . ?
H56A C56 H56B 109.3 . . ?
C57 C56 H56C 108.0 . . ?
H56A C56 H56C 109.1 . . ?
H56B C56 H56C 109.7 . . ?
N1 C57 O15 155(10) . . ?
N1 C57 C56 97(7) . . ?
O15 C57 C56 108(6) . . ?
N1 C58 H58A 109.3 . . ?
N1 C58 H58B 110.6 . . ?
H58A C58 H58B 109.6 . . ?
N1 C58 H58C 108.8 . . ?
H58A C58 H58C 109.7 . . ?
H58B C58 H58C 108.8 . . ?
N1 C59 H59A 109.5 . . ?
N1 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
N1 C59 H59C 109.4 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C57 N1 C59 156(10) . . ?
C57 N1 C58 96(7) . . ?
C59 N1 C58 108(5) . . ?
C53 N2 C54 132(4) . . ?
C53 N2 C55 115(3) . . ?
C54 N2 C55 112(3) . . ?
C1 O1 Eu2 117.9(13) . 1_464 ?
C1 O2 Eu2 175.3(15) . 2_556 ?
C10 O3 Eu1 142.1(15) . 2_666 ?
C10 O4 Eu1 141.3(13) . . ?
C18 O5 Eu2 134.6(13) . 1_454 ?
C18 O6 Eu2 133.1(14) . 2_546 ?
C27 O7 Eu1 92.9(11) . . ?
C27 O8 Eu1 90.9(11) . . ?
C35 O9 Eu1 92.6(12) . . ?
C35 O10 Eu1 92.9(10) . . ?
C44 O11 Eu2 92.5(14) . . ?
C44 O12 Eu2 96.6(12) . . ?
C53 O14 Eu1 149.1(17) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         5.792
_refine_diff_density_min         -2.282
_refine_diff_density_rms         0.265
####################################################################### 
# 
# 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_gd
_database_code_depnum_ccdc_archive 'CCDC 1441103'
_audit_update_record             
;
2015-12-08 deposited with the CCDC.
2016-02-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C118 H108 N4 O28 Gd4, 15(H2O)'
_chemical_formula_sum            'C118 H138 Gd4 N4 O43'
_chemical_formula_weight         2929.32

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
H H 0.0000 0.0000 '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'

_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                   11.4957(4)
_cell_length_b                   13.6804(4)
_cell_length_c                   23.9693(8)
_cell_angle_alpha                76.328(3)
_cell_angle_beta                 76.214(3)
_cell_angle_gamma                66.917(3)
_cell_volume                     3324.48(19)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1873
_cell_measurement_theta_min      2.0
_cell_measurement_theta_max      20.1

_exptl_crystal_description       block
_exptl_crystal_colour            whiteless
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1474
_exptl_absorpt_coefficient_mu    2.049
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7624
_exptl_absorpt_correction_T_max  0.7911
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_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 Smart Aepex CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25537
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_sigmaI/netI    0.0843
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.21
_diffrn_reflns_theta_max         25.00
_reflns_number_total             11710
_reflns_number_gt                8215
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0543P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11710
_refine_ls_number_parameters     777
_refine_ls_number_restraints     27
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0455
_refine_ls_wR_factor_ref         0.1189
_refine_ls_wR_factor_gt          0.1085
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.039
_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
Gd1 Gd 0.64066(3) 0.29881(2) 0.482698(13) 0.02253(10) Uani 1 1 d . . .
Gd2 Gd 0.81596(3) -0.40190(3) 0.038273(14) 0.03074(12) Uani 1 1 d DU . .
C1 C 0.8744(8) 0.5006(6) 0.9230(3) 0.043(2) Uani 1 1 d . . .
C2 C 0.8487(7) 0.4730(6) 0.8713(3) 0.0381(18) Uani 1 1 d . . .
C3 C 0.9299(7) 0.3816(6) 0.8495(3) 0.042(2) Uani 1 1 d . . .
H3 H 1.0017 0.3377 0.8665 0.051 Uiso 1 1 calc R . .
C4 C 0.9067(7) 0.3535(6) 0.8024(3) 0.042(2) Uani 1 1 d . . .
H4 H 0.9622 0.2908 0.7881 0.050 Uiso 1 1 calc R . .
C5 C 0.8003(6) 0.4193(6) 0.7770(3) 0.0325(17) Uani 1 1 d . . .
C6 C 0.7542(6) 0.4132(5) 0.7263(3) 0.0311(16) Uani 1 1 d . . .
C7 C 0.8032(7) 0.3383(6) 0.6886(3) 0.0377(19) Uani 1 1 d . . .
H7 H 0.8746 0.2767 0.6951 0.045 Uiso 1 1 calc R . .
C8 C 0.7437(7) 0.3571(6) 0.6412(3) 0.0394(19) Uani 1 1 d . . .
H8 H 0.7757 0.3073 0.6157 0.047 Uiso 1 1 calc R . .
C9 C 0.6382(6) 0.4479(5) 0.6309(3) 0.0280(16) Uani 1 1 d . . .
C10 C 0.5797(7) 0.4709(5) 0.5780(3) 0.0311(16) Uani 1 1 d . . .
C11 C 0.5867(6) 0.5219(6) 0.6701(3) 0.0326(17) Uani 1 1 d . . .
H11 H 0.5135 0.5821 0.6644 0.039 Uiso 1 1 calc R . .
C12 C 0.6450(6) 0.5047(6) 0.7170(3) 0.0324(17) Uani 1 1 d . . .
C13 C 0.6111(6) 0.5757(6) 0.7626(3) 0.0374(19) Uani 1 1 d . . .
C14 C 0.4781(7) 0.5882(8) 0.7975(4) 0.073(3) Uani 1 1 d . . .
H14A H 0.4157 0.6254 0.7721 0.087 Uiso 1 1 d R . .
H14B H 0.4614 0.6290 0.8279 0.087 Uiso 1 1 d R . .
H14C H 0.4732 0.5186 0.8143 0.087 Uiso 1 1 d R . .
C15 C 0.6181(9) 0.6881(7) 0.7347(4) 0.066(3) Uani 1 1 d . . .
H15A H 0.6992 0.6798 0.7098 0.079 Uiso 1 1 d R . .
H15B H 0.6093 0.7272 0.7648 0.079 Uiso 1 1 d R . .
H15C H 0.5501 0.7270 0.7123 0.079 Uiso 1 1 d R . .
C16 C 0.7168(6) 0.5128(6) 0.7995(3) 0.0337(17) Uani 1 1 d . . .
C17 C 0.7412(7) 0.5390(6) 0.8461(3) 0.042(2) Uani 1 1 d . . .
H17 H 0.6858 0.6011 0.8610 0.050 Uiso 1 1 calc R . .
C18 C 1.0262(7) -0.3382(6) 0.9258(3) 0.0378(18) Uani 1 1 d . . .
C19 C 1.0155(6) -0.2753(6) 0.8657(3) 0.0348(18) Uani 1 1 d . . .
C20 C 1.1153(7) -0.3059(6) 0.8201(3) 0.0388(19) Uani 1 1 d . . .
H20 H 1.1900 -0.3637 0.8273 0.047 Uiso 1 1 calc R . .
C21 C 1.1048(7) -0.2511(6) 0.7635(3) 0.0392(19) Uani 1 1 d . . .
H21 H 1.1721 -0.2717 0.7331 0.047 Uiso 1 1 calc R . .
C22 C 0.9937(6) -0.1661(5) 0.7530(3) 0.0302(16) Uani 1 1 d . . .
C23 C 0.9538(6) -0.0962(5) 0.6990(3) 0.0289(16) Uani 1 1 d . . .
C24 C 1.0164(6) -0.0967(6) 0.6425(3) 0.0362(18) Uani 1 1 d . . .
H24 H 1.0971 -0.1480 0.6335 0.043 Uiso 1 1 calc R . .
C25 C 0.9578(6) -0.0205(5) 0.5996(3) 0.0336(17) Uani 1 1 d . . .
H25 H 1.0008 -0.0187 0.5614 0.040 Uiso 1 1 calc R . .
C26 C 0.8331(6) 0.0558(5) 0.6121(3) 0.0321(17) Uani 1 1 d . . .
C27 C 0.7679(6) 0.1369(5) 0.5659(3) 0.0306(16) Uani 1 1 d . . .
C28 C 0.7709(6) 0.0548(6) 0.6690(3) 0.0330(17) Uani 1 1 d . . .
H28 H 0.6891 0.1044 0.6781 0.040 Uiso 1 1 calc R . .
C29 C 0.8314(6) -0.0204(6) 0.7119(3) 0.0324(17) Uani 1 1 d . . .
C30 C 0.7794(6) -0.0375(6) 0.7779(3) 0.0361(18) Uani 1 1 d . . .
C31 C 0.6595(7) -0.0670(8) 0.7885(4) 0.062(3) Uani 1 1 d . . .
H31A H 0.6748 -0.1221 0.7663 0.074 Uiso 1 1 d R . .
H31B H 0.5889 -0.0044 0.7768 0.074 Uiso 1 1 d R . .
H31C H 0.6395 -0.0929 0.8291 0.074 Uiso 1 1 d R . .
C32 C 0.7512(8) 0.0629(7) 0.8042(3) 0.060(3) Uani 1 1 d . . .
H32A H 0.7355 0.0460 0.8459 0.072 Uiso 1 1 d R . .
H32B H 0.6771 0.1197 0.7911 0.072 Uiso 1 1 d R . .
H32C H 0.8236 0.0858 0.7922 0.072 Uiso 1 1 d R . .
C33 C 0.8941(7) -0.1333(5) 0.7990(3) 0.0340(17) Uani 1 1 d . . .
C34 C 0.9045(7) -0.1888(6) 0.8553(3) 0.0396(19) Uani 1 1 d . . .
H34 H 0.8375 -0.1680 0.8857 0.047 Uiso 1 1 calc R . .
C35 C 0.6190(6) 0.1615(5) 0.4185(3) 0.0303(16) Uani 1 1 d . . .
C36 C 0.6167(6) 0.0826(5) 0.3850(3) 0.0286(16) Uani 1 1 d . . .
C37 C 0.5538(7) 0.0101(6) 0.4112(3) 0.0363(18) Uani 1 1 d . . .
H37 H 0.5104 0.0134 0.4491 0.044 Uiso 1 1 calc R . .
C38 C 0.5542(7) -0.0662(6) 0.3822(3) 0.0367(18) Uani 1 1 d . . .
H38 H 0.5130 -0.1146 0.4004 0.044 Uiso 1 1 calc R . .
C39 C 0.6178(6) -0.0684(5) 0.3252(3) 0.0291(16) Uani 1 1 d . . .
C40 C 0.6366(6) -0.1388(5) 0.2834(3) 0.0307(16) Uani 1 1 d . . .
C41 C 0.5955(7) -0.2231(6) 0.2880(3) 0.0385(18) Uani 1 1 d . . .
H41 H 0.5471 -0.2445 0.3223 0.046 Uiso 1 1 calc R . .
C42 C 0.6281(7) -0.2754(6) 0.2402(3) 0.0411(19) Uani 1 1 d . . .
H42 H 0.6009 -0.3322 0.2427 0.049 Uiso 1 1 calc R . .
C43 C 0.7004(7) -0.2448(6) 0.1888(3) 0.0352(17) Uani 1 1 d . . .
C44 C 0.7362(7) -0.3018(6) 0.1370(3) 0.0393(19) Uani 1 1 d . . .
C45 C 0.7392(6) -0.1602(6) 0.1851(3) 0.0347(17) Uani 1 1 d . . .
H45 H 0.7861 -0.1381 0.1505 0.042 Uiso 1 1 calc R . .
C46 C 0.7090(6) -0.1071(5) 0.2323(3) 0.0307(16) Uani 1 1 d . . .
C47 C 0.7461(6) -0.0149(5) 0.2373(3) 0.0299(16) Uani 1 1 d . . .
C48 C 0.6963(8) 0.0849(6) 0.1922(3) 0.048(2) Uani 1 1 d . . .
H48A H 0.7285 0.0664 0.1538 0.058 Uiso 1 1 d R . .
H48B H 0.7248 0.1399 0.1959 0.058 Uiso 1 1 d R . .
H48C H 0.6043 0.1110 0.1986 0.058 Uiso 1 1 d R . .
C49 C 0.8915(7) -0.0496(7) 0.2332(4) 0.051(2) Uani 1 1 d . . .
H49A H 0.9233 -0.1156 0.2592 0.061 Uiso 1 1 d R . .
H49B H 0.9104 0.0057 0.2434 0.061 Uiso 1 1 d R . .
H49C H 0.9320 -0.0600 0.1940 0.061 Uiso 1 1 d R . .
C50 C 0.6807(6) 0.0050(5) 0.2989(3) 0.0288(16) Uani 1 1 d . . .
C51 C 0.6789(6) 0.0796(5) 0.3284(3) 0.0291(16) Uani 1 1 d . . .
H51 H 0.7197 0.1283 0.3103 0.035 Uiso 1 1 calc R . .
C52 C 0.9233(9) 0.4342(9) 0.4619(6) 0.099(4) Uani 1 1 d U . .
H52A H 1.0043 0.4421 0.4448 0.119 Uiso 1 1 d R . .
H52B H 0.9359 0.3727 0.4922 0.119 Uiso 1 1 d R . .
H52C H 0.8667 0.4976 0.4780 0.119 Uiso 1 1 d R . .
C53 C 0.8643(9) 0.4171(8) 0.4140(5) 0.068(2) Uani 1 1 d U . .
C54 C 0.9428(17) 0.5520(12) 0.3506(7) 0.191(9) Uani 1 1 d U . .
H54A H 0.8908 0.6145 0.3278 0.230 Uiso 1 1 d R . .
H54B H 1.0248 0.5212 0.3276 0.230 Uiso 1 1 d R . .
H54C H 0.9544 0.5722 0.3841 0.230 Uiso 1 1 d R . .
C55 C 0.8159(18) 0.4565(12) 0.3247(6) 0.158(6) Uani 1 1 d U . .
H55A H 0.7275 0.4695 0.3413 0.190 Uiso 1 1 d R . .
H55B H 0.8560 0.3841 0.3164 0.190 Uiso 1 1 d R . .
H55C H 0.8213 0.5062 0.2893 0.190 Uiso 1 1 d R . .
C56 C 0.1171(10) 0.1714(9) 0.5803(6) 0.108(5) Uani 1 1 d D . .
H56A H 0.0626 0.2209 0.6064 0.129 Uiso 1 1 calc R . .
H56B H 0.1778 0.1118 0.6009 0.129 Uiso 1 1 calc R . .
H56C H 0.0660 0.1455 0.5654 0.129 Uiso 1 1 calc R . .
C57 C 0.1877(14) 0.2279(16) 0.5306(8) 0.190(14) Uani 1 1 d D . .
C58 C 0.2782(10) 0.2748(11) 0.4313(5) 0.106(5) Uani 1 1 d . . .
H58A H 0.3382 0.2939 0.4443 0.128 Uiso 1 1 d R . .
H58B H 0.2142 0.3390 0.4157 0.128 Uiso 1 1 d R . .
H58C H 0.3226 0.2305 0.4016 0.128 Uiso 1 1 d R . .
C59 C 0.1763(14) 0.1264(13) 0.4664(9) 0.194(10) Uani 1 1 d . . .
H59A H 0.1801 0.0694 0.4990 0.233 Uiso 1 1 calc R . .
H59B H 0.2346 0.0977 0.4332 0.233 Uiso 1 1 calc R . .
H59C H 0.0907 0.1584 0.4576 0.233 Uiso 1 1 calc R . .
N1 N 0.2171(13) 0.2193(13) 0.4826(9) 0.165(7) Uani 1 1 d D . .
N2 N 0.8828(11) 0.4719(8) 0.3697(5) 0.114(4) Uani 1 1 d U . .
O1 O 0.7794(5) 0.5619(5) 0.9528(2) 0.0566(16) Uani 1 1 d . . .
O2 O 0.9849(5) 0.4634(4) 0.9346(2) 0.0500(14) Uani 1 1 d . . .
O3 O 0.4689(5) 0.5427(4) 0.57593(19) 0.0446(14) Uani 1 1 d . . .
O4 O 0.6432(4) 0.4190(4) 0.53689(18) 0.0317(11) Uani 1 1 d . . .
O5 O 0.9289(5) -0.3122(4) 0.9645(2) 0.0519(15) Uani 1 1 d . . .
O6 O 1.1309(5) -0.4136(4) 0.9334(2) 0.0412(13) Uani 1 1 d . . .
O7 O 0.6533(4) 0.1954(4) 0.57847(19) 0.0312(11) Uani 1 1 d . . .
O8 O 0.8264(4) 0.1476(4) 0.5139(2) 0.0435(14) Uani 1 1 d . . .
O9 O 0.5698(5) 0.1592(4) 0.47175(19) 0.0432(13) Uani 1 1 d . . .
O10 O 0.6697(4) 0.2307(4) 0.3933(2) 0.0371(12) Uani 1 1 d . . .
O11 O 0.7216(6) -0.3891(5) 0.1420(2) 0.0564(16) Uani 1 1 d . . .
O12 O 0.7841(6) -0.2583(4) 0.0888(2) 0.0519(15) Uani 1 1 d . . .
O13 O 0.4216(4) 0.3587(4) 0.5347(2) 0.0444(13) Uani 1 1 d . . .
O14 O 0.8081(5) 0.3523(4) 0.4283(2) 0.0463(13) Uani 1 1 d U . .
O15 O 0.2239(7) 0.3041(7) 0.5396(5) 0.101(3) Uani 1 1 d . . .
O16 O 0.468(4) 0.554(3) 0.0023(18) 0.260(16) Uani 0.50 1 d PU . .
O17 O 0.581(3) 0.9624(19) 0.0359(14) 0.244(15) Uani 0.50 1 d P . .
O18 O 0.4182(13) 0.6978(15) 0.0641(14) 0.46(2) Uani 1 1 d . . .
O19 O 0.5956(9) -0.4214(12) 0.0582(6) 0.189(5) Uani 1 1 d DU . .
O20 O 0.6235(11) -0.2643(12) 0.0154(5) 0.261(10) Uani 1 1 d . . .
O21 O 0.965(3) 0.946(2) 0.005(2) 0.51(2) Uani 1 1 d . . .
O22 O 0.520(2) 0.827(3) 0.9532(10) 0.68(4) Uani 1 1 d . . .
O23 O 0.281(2) 0.718(3) 0.0156(12) 0.215(13) Uani 0.50 1 d P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O14 2.324(5) . ?
Gd1 O4 2.336(4) . ?
Gd1 O3 2.350(5) 2_666 ?
Gd1 O7 2.399(4) . ?
Gd1 O10 2.435(5) . ?
Gd1 O13 2.436(4) . ?
Gd1 O9 2.437(5) . ?
Gd1 O8 2.442(5) . ?
Gd1 C27 2.791(7) . ?
Gd1 C35 2.806(7) . ?
Gd2 O2 2.304(5) 2_756 ?
Gd2 O6 2.320(5) 2_746 ?
Gd2 O5 2.334(5) 1_554 ?
Gd2 O20 2.359(9) . ?
Gd2 O1 2.381(5) 1_544 ?
Gd2 O12 2.410(5) . ?
Gd2 O11 2.483(5) . ?
Gd2 O19 2.570(7) . ?
Gd2 C44 2.799(7) . ?
C1 O2 1.244(9) . ?
C1 O1 1.266(8) . ?
C1 C2 1.499(10) . ?
C2 C3 1.367(10) . ?
C2 C17 1.388(10) . ?
C3 C4 1.386(10) . ?
C3 H3 0.9300 . ?
C4 C5 1.383(9) . ?
C4 H4 0.9300 . ?
C5 C16 1.403(9) . ?
C5 C6 1.468(9) . ?
C6 C7 1.386(9) . ?
C6 C12 1.401(9) . ?
C7 C8 1.387(10) . ?
C7 H7 0.9300 . ?
C8 C9 1.375(9) . ?
C8 H8 0.9300 . ?
C9 C11 1.404(9) . ?
C9 C10 1.488(9) . ?
C10 O4 1.261(7) . ?
C10 O3 1.271(8) . ?
C11 C12 1.369(9) . ?
C11 H11 0.9300 . ?
C12 C13 1.513(9) . ?
C13 C14 1.523(11) . ?
C13 C16 1.527(9) . ?
C13 C15 1.551(11) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.369(9) . ?
C17 H17 0.9300 . ?
C18 O6 1.260(8) . ?
C18 O5 1.260(8) . ?
C18 C19 1.499(10) . ?
C19 C34 1.385(9) . ?
C19 C20 1.390(9) . ?
C20 C21 1.394(10) . ?
C20 H20 0.9300 . ?
C21 C22 1.378(9) . ?
C21 H21 0.9300 . ?
C22 C33 1.398(9) . ?
C22 C23 1.468(9) . ?
C23 C24 1.375(9) . ?
C23 C29 1.397(8) . ?
C24 C25 1.368(9) . ?
C24 H24 0.9300 . ?
C25 C26 1.416(9) . ?
C25 H25 0.9300 . ?
C26 C28 1.381(9) . ?
C26 C27 1.476(9) . ?
C27 O7 1.251(7) . ?
C27 O8 1.273(7) . ?
C28 C29 1.371(9) . ?
C28 H28 0.9300 . ?
C29 C30 1.548(9) . ?
C30 C31 1.533(11) . ?
C30 C32 1.534(11) . ?
C30 C33 1.536(9) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 C34 1.391(9) . ?
C34 H34 0.9300 . ?
C35 O10 1.262(8) . ?
C35 O9 1.265(8) . ?
C35 C36 1.502(9) . ?
C36 C51 1.376(8) . ?
C36 C37 1.397(9) . ?
C37 C38 1.381(10) . ?
C37 H37 0.9300 . ?
C38 C39 1.389(9) . ?
C38 H38 0.9300 . ?
C39 C50 1.408(9) . ?
C39 C40 1.471(9) . ?
C40 C41 1.382(10) . ?
C40 C46 1.388(9) . ?
C41 C42 1.393(9) . ?
C41 H41 0.9300 . ?
C42 C43 1.386(10) . ?
C42 H42 0.9300 . ?
C43 C45 1.373(10) . ?
C43 C44 1.510(10) . ?
C44 O11 1.245(9) . ?
C44 O12 1.273(9) . ?
C45 C46 1.391(9) . ?
C45 H45 0.9300 . ?
C46 C47 1.517(10) . ?
C47 C50 1.524(8) . ?
C47 C48 1.532(10) . ?
C47 C49 1.534(9) . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C50 C51 1.363(9) . ?
C51 H51 0.9300 . ?
C52 C53 1.568(15) . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C53 N2 1.174(12) . ?
C53 O14 1.232(11) . ?
C54 N2 1.446(15) . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C55 N2 1.558(18) . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?
C56 C57 1.508(10) . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
C57 N1 1.138(10) . ?
C57 O15 1.34(3) . ?
C58 N1 1.47(2) . ?
C58 H58A 0.9600 . ?
C58 H58B 0.9600 . ?
C58 H58C 0.9600 . ?
C59 N1 1.67(2) . ?
C59 H59A 0.9600 . ?
C59 H59B 0.9600 . ?
C59 H59C 0.9600 . ?
O1 Gd2 2.381(5) 1_566 ?
O2 Gd2 2.304(5) 2_756 ?
O3 Gd1 2.350(5) 2_666 ?
O5 Gd2 2.334(5) 1_556 ?
O6 Gd2 2.320(5) 2_746 ?
O16 O16 1.39(6) 2_665 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O14 Gd1 O4 78.10(17) . . ?
O14 Gd1 O3 78.32(19) . 2_666 ?
O4 Gd1 O3 83.35(17) . 2_666 ?
O14 Gd1 O7 121.78(17) . . ?
O4 Gd1 O7 77.05(16) . . ?
O3 Gd1 O7 147.31(15) 2_666 . ?
O14 Gd1 O10 80.05(17) . . ?
O4 Gd1 O10 154.43(16) . . ?
O3 Gd1 O10 79.36(16) 2_666 . ?
O7 Gd1 O10 126.45(16) . . ?
O14 Gd1 O13 145.42(18) . . ?
O4 Gd1 O13 77.41(17) . . ?
O3 Gd1 O13 74.93(17) 2_666 . ?
O7 Gd1 O13 75.42(16) . . ?
O10 Gd1 O13 115.44(17) . . ?
O14 Gd1 O9 129.76(16) . . ?
O4 Gd1 O9 151.33(15) . . ?
O3 Gd1 O9 106.69(19) 2_666 . ?
O7 Gd1 O9 80.93(16) . . ?
O10 Gd1 O9 53.40(15) . . ?
O13 Gd1 O9 79.45(17) . . ?
O14 Gd1 O8 78.63(18) . . ?
O4 Gd1 O8 96.96(17) . . ?
O3 Gd1 O8 156.35(17) 2_666 . ?
O7 Gd1 O8 53.65(14) . . ?
O10 Gd1 O8 91.56(17) . . ?
O13 Gd1 O8 128.36(16) . . ?
O9 Gd1 O8 84.32(19) . . ?
O14 Gd1 C27 100.42(19) . . ?
O4 Gd1 C27 85.86(17) . . ?
O3 Gd1 C27 169.17(18) 2_666 . ?
O7 Gd1 C27 26.55(15) . . ?
O10 Gd1 C27 111.14(18) . . ?
O13 Gd1 C27 101.76(18) . . ?
O9 Gd1 C27 82.50(19) . . ?
O8 Gd1 C27 27.12(16) . . ?
O14 Gd1 C35 104.66(19) . . ?
O4 Gd1 C35 176.02(16) . . ?
O3 Gd1 C35 94.35(19) 2_666 . ?
O7 Gd1 C35 103.53(18) . . ?
O10 Gd1 C35 26.69(17) . . ?
O13 Gd1 C35 98.87(18) . . ?
O9 Gd1 C35 26.77(17) . . ?
O8 Gd1 C35 86.45(18) . . ?
C27 Gd1 C35 96.37(19) . . ?
O2 Gd2 O6 74.39(19) 2_756 2_746 ?
O2 Gd2 O5 76.66(19) 2_756 1_554 ?
O6 Gd2 O5 127.41(17) 2_746 1_554 ?
O2 Gd2 O20 152.7(4) 2_756 . ?
O6 Gd2 O20 131.8(5) 2_746 . ?
O5 Gd2 O20 88.8(5) 1_554 . ?
O2 Gd2 O1 123.55(18) 2_756 1_544 ?
O6 Gd2 O1 82.96(19) 2_746 1_544 ?
O5 Gd2 O1 77.9(2) 1_554 1_544 ?
O20 Gd2 O1 74.2(2) . 1_544 ?
O2 Gd2 O12 81.3(2) 2_756 . ?
O6 Gd2 O12 133.06(17) 2_746 . ?
O5 Gd2 O12 83.09(18) 1_554 . ?
O20 Gd2 O12 74.0(3) . . ?
O1 Gd2 O12 143.06(19) 1_544 . ?
O2 Gd2 O11 87.80(19) 2_756 . ?
O6 Gd2 O11 85.72(17) 2_746 . ?
O5 Gd2 O11 135.7(2) 1_554 . ?
O20 Gd2 O11 86.8(3) . . ?
O1 Gd2 O11 141.7(2) 1_544 . ?
O12 Gd2 O11 53.41(18) . . ?
O2 Gd2 O19 146.4(4) 2_756 . ?
O6 Gd2 O19 78.2(4) 2_746 . ?
O5 Gd2 O19 136.5(4) 1_554 . ?
O20 Gd2 O19 54.4(5) . . ?
O1 Gd2 O19 70.8(3) 1_544 . ?
O12 Gd2 O19 104.5(3) . . ?
O11 Gd2 O19 71.1(3) . . ?
O2 Gd2 C44 83.7(2) 2_756 . ?
O6 Gd2 C44 109.5(2) 2_746 . ?
O5 Gd2 C44 109.7(2) 1_554 . ?
O20 Gd2 C44 79.6(3) . . ?
O1 Gd2 C44 152.6(2) 1_544 . ?
O12 Gd2 C44 27.0(2) . . ?
O11 Gd2 C44 26.4(2) . . ?
O19 Gd2 C44 87.6(3) . . ?
O2 C1 O1 123.3(7) . . ?
O2 C1 C2 119.9(7) . . ?
O1 C1 C2 116.8(7) . . ?
C3 C2 C17 119.9(7) . . ?
C3 C2 C1 120.0(7) . . ?
C17 C2 C1 120.2(6) . . ?
C2 C3 C4 120.9(6) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C5 C4 C3 119.5(6) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C16 119.5(6) . . ?
C4 C5 C6 131.8(6) . . ?
C16 C5 C6 108.6(6) . . ?
C7 C6 C12 120.4(6) . . ?
C7 C6 C5 131.2(6) . . ?
C12 C6 C5 108.4(5) . . ?
C6 C7 C8 118.7(6) . . ?
C6 C7 H7 120.7 . . ?
C8 C7 H7 120.7 . . ?
C9 C8 C7 121.4(6) . . ?
C9 C8 H8 119.3 . . ?
C7 C8 H8 119.3 . . ?
C8 C9 C11 119.7(6) . . ?
C8 C9 C10 121.0(6) . . ?
C11 C9 C10 119.3(6) . . ?
O4 C10 O3 123.0(6) . . ?
O4 C10 C9 118.3(6) . . ?
O3 C10 C9 118.7(6) . . ?
C12 C11 C9 119.6(6) . . ?
C12 C11 H11 120.2 . . ?
C9 C11 H11 120.2 . . ?
C11 C12 C6 120.2(6) . . ?
C11 C12 C13 128.7(6) . . ?
C6 C12 C13 111.0(6) . . ?
C12 C13 C14 111.1(7) . . ?
C12 C13 C16 101.7(5) . . ?
C14 C13 C16 112.2(6) . . ?
C12 C13 C15 111.3(6) . . ?
C14 C13 C15 109.7(7) . . ?
C16 C13 C15 110.6(7) . . ?
C13 C14 H14A 109.0 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.9 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.4 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C5 120.1(6) . . ?
C17 C16 C13 129.5(6) . . ?
C5 C16 C13 110.3(6) . . ?
C16 C17 C2 120.1(6) . . ?
C16 C17 H17 119.9 . . ?
C2 C17 H17 119.9 . . ?
O6 C18 O5 125.3(7) . . ?
O6 C18 C19 117.6(7) . . ?
O5 C18 C19 117.2(6) . . ?
C34 C19 C20 120.0(7) . . ?
C34 C19 C18 120.1(6) . . ?
C20 C19 C18 119.9(6) . . ?
C19 C20 C21 120.7(6) . . ?
C19 C20 H20 119.6 . . ?
C21 C20 H20 119.6 . . ?
C22 C21 C20 119.3(6) . . ?
C22 C21 H21 120.4 . . ?
C20 C21 H21 120.4 . . ?
C21 C22 C33 120.3(6) . . ?
C21 C22 C23 131.6(6) . . ?
C33 C22 C23 108.1(6) . . ?
C24 C23 C29 120.3(6) . . ?
C24 C23 C22 130.5(6) . . ?
C29 C23 C22 109.2(5) . . ?
C25 C24 C23 118.8(6) . . ?
C25 C24 H24 120.6 . . ?
C23 C24 H24 120.6 . . ?
C24 C25 C26 121.4(6) . . ?
C24 C25 H25 119.3 . . ?
C26 C25 H25 119.3 . . ?
C28 C26 C25 119.1(6) . . ?
C28 C26 C27 119.1(6) . . ?
C25 C26 C27 121.8(6) . . ?
O7 C27 O8 119.9(6) . . ?
O7 C27 C26 119.1(6) . . ?
O8 C27 C26 121.0(6) . . ?
O7 C27 Gd1 59.0(3) . . ?
O8 C27 Gd1 61.0(3) . . ?
C26 C27 Gd1 176.8(5) . . ?
C29 C28 C26 119.2(6) . . ?
C29 C28 H28 120.4 . . ?
C26 C28 H28 120.4 . . ?
C28 C29 C23 121.2(6) . . ?
C28 C29 C30 127.9(6) . . ?
C23 C29 C30 110.8(5) . . ?
C31 C30 C32 111.0(6) . . ?
C31 C30 C33 111.8(6) . . ?
C32 C30 C33 112.6(7) . . ?
C31 C30 C29 110.2(6) . . ?
C32 C30 C29 110.8(6) . . ?
C33 C30 C29 99.9(5) . . ?
C30 C31 H31A 109.7 . . ?
C30 C31 H31B 109.4 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.3 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.4 . . ?
C30 C32 H32B 109.7 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.4 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 C22 120.3(6) . . ?
C34 C33 C30 127.8(6) . . ?
C22 C33 C30 111.9(6) . . ?
C19 C34 C33 119.5(6) . . ?
C19 C34 H34 120.2 . . ?
C33 C34 H34 120.2 . . ?
O10 C35 O9 120.0(6) . . ?
O10 C35 C36 119.8(6) . . ?
O9 C35 C36 120.2(6) . . ?
O10 C35 Gd1 60.1(3) . . ?
O9 C35 Gd1 60.1(4) . . ?
C36 C35 Gd1 175.9(5) . . ?
C51 C36 C37 119.3(6) . . ?
C51 C36 C35 120.2(6) . . ?
C37 C36 C35 120.5(6) . . ?
C38 C37 C36 121.9(6) . . ?
C38 C37 H37 119.1 . . ?
C36 C37 H37 119.1 . . ?
C37 C38 C39 118.1(6) . . ?
C37 C38 H38 120.9 . . ?
C39 C38 H38 120.9 . . ?
C38 C39 C50 119.8(6) . . ?
C38 C39 C40 131.4(6) . . ?
C50 C39 C40 108.8(6) . . ?
C41 C40 C46 120.7(6) . . ?
C41 C40 C39 131.4(6) . . ?
C46 C40 C39 107.8(6) . . ?
C40 C41 C42 118.4(7) . . ?
C40 C41 H41 120.8 . . ?
C42 C41 H41 120.8 . . ?
C43 C42 C41 121.6(7) . . ?
C43 C42 H42 119.2 . . ?
C41 C42 H42 119.2 . . ?
C45 C43 C42 119.0(6) . . ?
C45 C43 C44 119.5(6) . . ?
C42 C43 C44 121.5(7) . . ?
O11 C44 O12 121.7(7) . . ?
O11 C44 C43 120.8(7) . . ?
O12 C44 C43 117.5(7) . . ?
O11 C44 Gd2 62.5(4) . . ?
O12 C44 Gd2 59.2(4) . . ?
C43 C44 Gd2 176.1(6) . . ?
C43 C45 C46 120.7(7) . . ?
C43 C45 H45 119.6 . . ?
C46 C45 H45 119.6 . . ?
C40 C46 C45 119.5(7) . . ?
C40 C46 C47 111.9(6) . . ?
C45 C46 C47 128.6(6) . . ?
C46 C47 C50 101.2(5) . . ?
C46 C47 C48 112.4(6) . . ?
C50 C47 C48 111.6(5) . . ?
C46 C47 C49 111.3(5) . . ?
C50 C47 C49 109.5(6) . . ?
C48 C47 C49 110.6(6) . . ?
C47 C48 H48A 109.4 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C49 H49A 110.2 . . ?
C47 C49 H49B 109.1 . . ?
H49A C49 H49B 109.5 . . ?
C47 C49 H49C 109.1 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C51 C50 C39 120.9(6) . . ?
C51 C50 C47 128.9(6) . . ?
C39 C50 C47 110.2(6) . . ?
C50 C51 C36 120.0(6) . . ?
C50 C51 H51 120.0 . . ?
C36 C51 H51 120.0 . . ?
C53 C52 H52A 109.2 . . ?
C53 C52 H52B 109.1 . . ?
H52A C52 H52B 109.5 . . ?
C53 C52 H52C 110.1 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
N2 C53 O14 131.8(13) . . ?
N2 C53 C52 110.7(11) . . ?
O14 C53 C52 117.5(10) . . ?
N2 C54 H54A 110.7 . . ?
N2 C54 H54B 108.6 . . ?
H54A C54 H54B 109.5 . . ?
N2 C54 H54C 109.2 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
N2 C55 H55A 108.2 . . ?
N2 C55 H55B 109.8 . . ?
H55A C55 H55B 109.5 . . ?
N2 C55 H55C 110.4 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C57 C56 H56A 109.5 . . ?
C57 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C57 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
N1 C57 O15 109.0(17) . . ?
N1 C57 C56 131(3) . . ?
O15 C57 C56 120.1(18) . . ?
N1 C58 H58A 106.7 . . ?
N1 C58 H58B 109.2 . . ?
H58A C58 H58B 109.5 . . ?
N1 C58 H58C 112.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
N1 C59 H59A 109.5 . . ?
N1 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
N1 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C57 N1 C58 134(2) . . ?
C57 N1 C59 113(2) . . ?
C58 N1 C59 112.4(15) . . ?
C53 N2 C54 134.7(15) . . ?
C53 N2 C55 108.5(11) . . ?
C54 N2 C55 116.6(13) . . ?
C1 O1 Gd2 117.2(5) . 1_566 ?
C1 O2 Gd2 175.8(5) . 2_756 ?
C10 O3 Gd1 141.1(4) . 2_666 ?
C10 O4 Gd1 142.8(5) . . ?
C18 O5 Gd2 136.5(5) . 1_556 ?
C18 O6 Gd2 132.4(5) . 2_746 ?
C27 O7 Gd1 94.5(4) . . ?
C27 O8 Gd1 91.9(4) . . ?
C35 O9 Gd1 93.1(4) . . ?
C35 O10 Gd1 93.2(4) . . ?
C44 O11 Gd2 91.1(4) . . ?
C44 O12 Gd2 93.7(4) . . ?
C53 O14 Gd1 150.9(5) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.497
_refine_diff_density_min         -1.155
_refine_diff_density_rms         0.123
####################################################################### 
# 
# 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_Sm
_database_code_depnum_ccdc_archive 'CCDC 1441104'
_audit_update_record             
;
2015-12-08 deposited with the CCDC.
2016-02-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C118 H108 N4 O28 Sm4, 15(H2O)'
_chemical_formula_sum            'C118 H138 N4 O43 Sm4'
_chemical_formula_weight         2901.72

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'
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'
N N 0.0061 0.0033 '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                   11.4087(8)
_cell_length_b                   13.6584(8)
_cell_length_c                   24.0230(12)
_cell_angle_alpha                93.171(4)
_cell_angle_beta                 103.627(5)
_cell_angle_gamma                112.671(6)
_cell_volume                     3312.0(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1923
_cell_measurement_theta_min      1.9
_cell_measurement_theta_max      20.3

_exptl_crystal_description       block
_exptl_crystal_colour            whiteless
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1466
_exptl_absorpt_coefficient_mu    1.827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8676
_exptl_absorpt_correction_T_max  0.8983
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_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 Smart Aepex CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26109
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_av_sigmaI/netI    0.0806
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.21
_diffrn_reflns_theta_max         25.00
_reflns_number_total             11677
_reflns_number_gt                8923
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0827P)²+50.0286P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11677
_refine_ls_number_parameters     772
_refine_ls_number_restraints     27
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_gt           0.0899
_refine_ls_wR_factor_ref         0.2595
_refine_ls_wR_factor_gt          0.2464
_refine_ls_goodness_of_fit_ref   1.225
_refine_ls_restrained_S_all      1.225
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.37573(6) 0.29807(5) 0.51771(3) 0.0325(2) Uani 1 1 d . . .
Sm2 Sm 0.64698(7) -0.40226(5) 0.96206(3) 0.0394(2) Uani 1 1 d . . .
C1 C -0.2930(15) 0.5044(12) 0.0771(6) 0.049(4) Uani 1 1 d . . .
C2 C -0.2165(14) 0.4749(12) 0.1295(6) 0.046(3) Uani 1 1 d . . .
C3 C -0.2785(14) 0.3822(12) 0.1505(6) 0.049(4) Uani 1 1 d . . .
H3 H -0.3674 0.3391 0.1328 0.059 Uiso 1 1 calc R . .
C4 C -0.2110(14) 0.3526(12) 0.1971(6) 0.050(4) Uani 1 1 d . . .
H4 H -0.2525 0.2902 0.2113 0.060 Uiso 1 1 calc R . .
C5 C -0.0762(13) 0.4208(11) 0.2226(6) 0.037(3) Uani 1 1 d . . .
C6 C 0.0207(13) 0.4142(11) 0.2734(5) 0.037(3) Uani 1 1 d . . .
C7 C 0.0081(13) 0.3377(11) 0.3105(6) 0.046(3) Uani 1 1 d . . .
H7 H -0.0697 0.2758 0.3033 0.055 Uiso 1 1 calc R . .
C8 C 0.1133(16) 0.3558(11) 0.3580(6) 0.049(4) Uani 1 1 d . . .
H8 H 0.1061 0.3056 0.3831 0.059 Uiso 1 1 calc R . .
C9 C 0.2297(13) 0.4477(10) 0.3690(5) 0.037(3) Uani 1 1 d . . .
C10 C 0.3414(14) 0.4707(10) 0.4216(6) 0.039(3) Uani 1 1 d . . .
C11 C 0.2426(13) 0.5213(11) 0.3301(6) 0.041(3) Uani 1 1 d . . .
H11 H 0.3222 0.5811 0.3362 0.049 Uiso 1 1 calc R . .
C12 C 0.1400(14) 0.5058(11) 0.2839(6) 0.043(3) Uani 1 1 d . . .
C13 C 0.1261(14) 0.5762(12) 0.2383(6) 0.047(4) Uani 1 1 d . . .
C14 C 0.2277(15) 0.5883(17) 0.2030(8) 0.074(6) Uani 1 1 d . . .
H14A H 0.2198 0.5187 0.1879 0.088 Uiso 1 1 d R . .
H14B H 0.3147 0.6283 0.2283 0.088 Uiso 1 1 d R . .
H14C H 0.2119 0.6261 0.1711 0.088 Uiso 1 1 d R . .
C15 C 0.1462(18) 0.6873(13) 0.2656(8) 0.076(6) Uani 1 1 d . . .
H15A H 0.1296 0.7269 0.2347 0.091 Uiso 1 1 d R . .
H15B H 0.2347 0.7250 0.2898 0.091 Uiso 1 1 d R . .
H15C H 0.0862 0.6800 0.2888 0.091 Uiso 1 1 d R . .
C16 C -0.0143(14) 0.5141(12) 0.2016(6) 0.045(3) Uani 1 1 d . . .
C17 C -0.0854(14) 0.5409(12) 0.1541(6) 0.049(4) Uani 1 1 d . . .
H17 H -0.0447 0.6027 0.1392 0.059 Uiso 1 1 calc R . .
C18 C -0.4519(17) -0.3352(11) 0.0735(7) 0.051(4) Uani 1 1 d . . .
C19 C -0.3821(14) -0.2745(11) 0.1338(6) 0.040(3) Uani 1 1 d . . .
C20 C -0.4354(16) -0.3052(12) 0.1792(6) 0.049(4) Uani 1 1 d . . .
H20 H -0.5175 -0.3626 0.1718 0.059 Uiso 1 1 calc R . .
C21 C -0.3683(15) -0.2516(12) 0.2360(6) 0.046(3) Uani 1 1 d . . .
H21 H -0.4055 -0.2719 0.2664 0.056 Uiso 1 1 calc R . .
C22 C -0.2442(15) -0.1667(11) 0.2462(6) 0.042(3) Uani 1 1 d . . .
C23 C -0.1522(14) -0.0975(11) 0.3003(6) 0.044(3) Uani 1 1 d . . .
C24 C -0.1586(13) -0.0972(11) 0.3566(5) 0.040(3) Uani 1 1 d . . .
H24 H -0.2314 -0.1477 0.3653 0.048 Uiso 1 1 calc R . .
C25 C -0.0550(15) -0.0207(12) 0.4008(6) 0.046(3) Uani 1 1 d . . .
H25 H -0.0587 -0.0194 0.4391 0.056 Uiso 1 1 calc R . .
C26 C 0.0522(15) 0.0524(11) 0.3874(6) 0.043(3) Uani 1 1 d . . .
C27 C 0.1641(13) 0.1365(10) 0.4341(6) 0.033(3) Uani 1 1 d . . .
C28 C 0.0619(13) 0.0537(11) 0.3301(6) 0.040(3) Uani 1 1 d . . .
H28 H 0.1353 0.1031 0.3213 0.048 Uiso 1 1 calc R . .
C29 C -0.0439(14) -0.0228(11) 0.2872(6) 0.041(3) Uani 1 1 d . . .
C30 C -0.0573(15) -0.0394(12) 0.2218(6) 0.046(3) Uani 1 1 d . . .
C31 C 0.0516(18) -0.0686(17) 0.2096(8) 0.076(6) Uani 1 1 d . . .
H31A H 0.0562 -0.1269 0.2297 0.091 Uiso 1 1 d R . .
H31B H 0.1339 -0.0071 0.2233 0.091 Uiso 1 1 d R . .
H31C H 0.0335 -0.0897 0.1683 0.091 Uiso 1 1 d R . .
C32 C -0.0540(18) 0.0615(14) 0.1953(8) 0.067(5) Uani 1 1 d . . .
H32A H -0.0752 0.0447 0.1535 0.080 Uiso 1 1 d R . .
H32B H 0.0312 0.1196 0.2096 0.080 Uiso 1 1 d R . .
H32C H -0.1183 0.0824 0.2056 0.080 Uiso 1 1 d R . .
C33 C -0.1925(14) -0.1337(11) 0.1999(6) 0.042(3) Uani 1 1 d . . .
C34 C -0.2582(14) -0.1873(11) 0.1442(6) 0.040(3) Uani 1 1 d . . .
H34 H -0.2214 -0.1663 0.1139 0.049 Uiso 1 1 calc R . .
C35 C 0.4636(13) 0.1621(11) 0.5819(6) 0.038(3) Uani 1 1 d . . .
C36 C 0.4968(13) 0.0795(11) 0.6155(6) 0.037(3) Uani 1 1 d . . .
C37 C 0.5325(14) 0.0061(11) 0.5887(6) 0.040(3) Uani 1 1 d . . .
H37 H 0.5353 0.0069 0.5504 0.048 Uiso 1 1 calc R . .
C38 C 0.5636(14) -0.0672(12) 0.6190(6) 0.042(3) Uani 1 1 d . . .
H38 H 0.5875 -0.1159 0.6012 0.051 Uiso 1 1 calc R . .
C39 C 0.5592(13) -0.0685(10) 0.6756(6) 0.036(3) Uani 1 1 d . . .
C40 C 0.5799(14) -0.1392(10) 0.7175(6) 0.039(3) Uani 1 1 d . . .
C41 C 0.6165(15) -0.2247(11) 0.7126(6) 0.045(3) Uani 1 1 d . . .
H41 H 0.6309 -0.2468 0.6785 0.054 Uiso 1 1 calc R . .
C42 C 0.6309(15) -0.2761(11) 0.7607(7) 0.048(4) Uani 1 1 d . . .
H42 H 0.6533 -0.3345 0.7578 0.058 Uiso 1 1 calc R . .
C43 C 0.6134(15) -0.2444(11) 0.8115(6) 0.043(3) Uani 1 1 d . . .
C44 C 0.6256(14) -0.3003(11) 0.8631(7) 0.046(3) Uani 1 1 d . . .
C45 C 0.5767(13) -0.1574(11) 0.8155(6) 0.039(3) Uani 1 1 d . . .
H45 H 0.5650 -0.1344 0.8501 0.047 Uiso 1 1 calc R . .
C46 C 0.5583(13) -0.1069(10) 0.7691(6) 0.037(3) Uani 1 1 d . . .
C47 C 0.5160(13) -0.0137(10) 0.7631(6) 0.037(3) Uani 1 1 d . . .
C48 C 0.6110(19) 0.0843(12) 0.8088(6) 0.060(4) Uani 1 1 d . . .
H48A H 0.6168 0.0654 0.8473 0.072 Uiso 1 1 d R . .
H48B H 0.5801 0.1406 0.8055 0.072 Uiso 1 1 d R . .
H48C H 0.6961 0.1087 0.8019 0.072 Uiso 1 1 d R . .
C49 C 0.3765(16) -0.0487(14) 0.7686(7) 0.057(4) Uani 1 1 d . . .
H49A H 0.3186 -0.1132 0.7415 0.068 Uiso 1 1 d R . .
H49B H 0.3480 0.0078 0.7599 0.068 Uiso 1 1 d R . .
H49C H 0.3752 -0.0615 0.8078 0.068 Uiso 1 1 d R . .
C50 C 0.5199(13) 0.0031(10) 0.7022(6) 0.035(3) Uani 1 1 d . . .
C51 C 0.4922(13) 0.0796(10) 0.6721(6) 0.037(3) Uani 1 1 d . . .
H51 H 0.4709 0.1299 0.6901 0.044 Uiso 1 1 calc R . .
C52 C 0.115(2) 0.439(2) 0.5384(13) 0.117(8) Uani 1 1 d U . .
H52A H 0.0304 0.3861 0.5382 0.140 Uiso 1 1 d R . .
H52B H 0.1301 0.4297 0.5009 0.140 Uiso 1 1 d R . .
H52C H 0.1172 0.5097 0.5463 0.140 Uiso 1 1 d R . .
C53 C 0.213(2) 0.4157(15) 0.5851(10) 0.079(5) Uani 1 1 d U . .
C54 C 0.206(5) 0.555(3) 0.6509(15) 0.202(18) Uani 1 1 d U . .
H54A H 0.2451 0.6211 0.6366 0.243 Uiso 1 1 d R . .
H54B H 0.2291 0.5683 0.6928 0.243 Uiso 1 1 d R . .
H54C H 0.1121 0.5268 0.6356 0.243 Uiso 1 1 d R . .
C55 C 0.361(4) 0.452(3) 0.6773(12) 0.194(18) Uani 1 1 d U . .
H55A H 0.3242 0.3883 0.6941 0.233 Uiso 1 1 d R . .
H55B H 0.4019 0.5136 0.7074 0.233 Uiso 1 1 d R . .
H55C H 0.4251 0.4458 0.6593 0.233 Uiso 1 1 d R . .
C56 C 0.804(3) 0.168(2) 0.4190(14) 0.130(11) Uani 1 1 d . . .
H56A H 0.8961 0.1888 0.4243 0.156 Uiso 1 1 d R . .
H56B H 0.7662 0.1847 0.3822 0.156 Uiso 1 1 d R . .
H56C H 0.7622 0.0920 0.4192 0.156 Uiso 1 1 d R . .
C57 C 0.778(2) 0.239(2) 0.475(2) 0.156(18) Uani 1 1 d . . .
C58 C 0.791(3) 0.277(3) 0.5672(13) 0.135(11) Uani 1 1 d . . .
H58A H 0.7577 0.3278 0.5517 0.162 Uiso 1 1 d R . .
H58B H 0.8749 0.3150 0.5953 0.162 Uiso 1 1 d R . .
H58C H 0.7309 0.2297 0.5859 0.162 Uiso 1 1 d R . .
C59 C 0.860(3) 0.128(3) 0.533(2) 0.22(2) Uani 1 1 d . . .
H59A H 0.8012 0.0621 0.5076 0.265 Uiso 1 1 d R . .
H59B H 0.8621 0.1180 0.5730 0.265 Uiso 1 1 d R . .
H59C H 0.9464 0.1485 0.5283 0.265 Uiso 1 1 d R . .
N1 N 0.808(2) 0.205(2) 0.511(2) 0.181(18) Uani 1 1 d . . .
N2 N 0.249(3) 0.4739(18) 0.6328(10) 0.131(8) Uani 1 1 d U . .
O1 O -0.2274(11) 0.5647(10) 0.0481(5) 0.070(4) Uani 1 1 d . . .
O2 O -0.4157(11) 0.4683(9) 0.0654(5) 0.059(3) Uani 1 1 d . . .
O3 O 0.4528(10) 0.5419(8) 0.4236(4) 0.055(3) Uani 1 1 d . . .
O4 O 0.3173(9) 0.4180(7) 0.4627(4) 0.039(2) Uani 1 1 d . . .
O5 O -0.3959(12) -0.3104(8) 0.0350(4) 0.057(3) Uani 1 1 d . . .
O6 O -0.5665(11) -0.4100(8) 0.0659(5) 0.057(3) Uani 1 1 d . . .
O7 O 0.2682(9) 0.1951(7) 0.4212(4) 0.041(2) Uani 1 1 d . . .
O8 O 0.1579(10) 0.1480(9) 0.4851(4) 0.053(3) Uani 1 1 d . . .
O9 O 0.4561(11) 0.1550(8) 0.5289(4) 0.050(3) Uani 1 1 d . . .
O10 O 0.4396(10) 0.2305(7) 0.6078(4) 0.045(2) Uani 1 1 d . . .
O11 O 0.6370(12) -0.3893(9) 0.8576(5) 0.060(3) Uani 1 1 d . . .
O12 O 0.6268(11) -0.2582(8) 0.9118(4) 0.053(3) Uani 1 1 d . . .
O13 O 0.5423(10) 0.3567(8) 0.4651(5) 0.056(3) Uani 1 1 d . . .
O14 O 0.2587(11) 0.3505(9) 0.5733(5) 0.059(3) Uani 1 1 d . . .
O15 O 0.7350(16) 0.3033(13) 0.4574(9) 0.110(6) Uani 1 1 d . . .
O16 O 0.0000 0.5000 0.0000 0.56(9) Uani 1 2 d S . .
O17 O 0.888(9) 0.967(8) 0.979(4) 0.32(4) Uani 0.50 1 d PU . .
O18 O 0.438(11) 0.046(13) 0.997(7) 0.52(10) Uani 0.50 1 d P . .
O19 O 0.857(4) -0.411(3) 0.9407(16) 0.278(17) Uani 1 1 d DU . .
O20 O 0.867(3) -0.275(2) 0.9807(12) 0.202(11) Uani 1 1 d DU . .
O21 O 0.004(4) 0.707(3) 0.905(2) 0.31(2) Uani 1 1 d . . .
O22 O 0.050(6) 0.814(7) 0.054(2) 0.66(8) Uani 1 1 d . . .
O23 O 0.112(10) 0.718(5) 0.982(2) 0.60(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
Sm1 O4 2.354(8) . ?
Sm1 O14 2.356(10) . ?
Sm1 O3 2.378(10) 2_666 ?
Sm1 O7 2.415(9) . ?
Sm1 O13 2.433(11) . ?
Sm1 O8 2.444(11) . ?
Sm1 O9 2.461(9) . ?
Sm1 O10 2.463(9) . ?
Sm1 C27 2.802(13) . ?
Sm1 C35 2.803(12) . ?
Sm2 O2 2.343(11) 2_556 ?
Sm2 O5 2.348(10) 1_656 ?
Sm2 O20 2.35(3) . ?
Sm2 O6 2.361(10) 2_546 ?
Sm2 O1 2.395(10) 1_646 ?
Sm2 O12 2.422(9) . ?
Sm2 O11 2.504(10) . ?
Sm2 O19 2.61(4) . ?
Sm2 C44 2.830(13) . ?
C1 O2 1.244(18) . ?
C1 O1 1.249(18) . ?
C1 C2 1.522(18) . ?
C2 C17 1.37(2) . ?
C2 C3 1.38(2) . ?
C3 C4 1.376(19) . ?
C3 H3 0.9300 . ?
C4 C5 1.413(19) . ?
C4 H4 0.9300 . ?
C5 C16 1.386(18) . ?
C5 C6 1.473(17) . ?
C6 C7 1.399(17) . ?
C6 C12 1.404(19) . ?
C7 C8 1.378(19) . ?
C7 H7 0.9300 . ?
C8 C9 1.386(19) . ?
C8 H8 0.9300 . ?
C9 C11 1.400(17) . ?
C9 C10 1.487(18) . ?
C10 O3 1.256(16) . ?
C10 O4 1.272(15) . ?
C11 C12 1.349(18) . ?
C11 H11 0.9300 . ?
C12 C13 1.517(17) . ?
C13 C16 1.51(2) . ?
C13 C15 1.53(2) . ?
C13 C14 1.56(2) . ?
C14 H14A 0.9613 . ?
C14 H14B 0.9550 . ?
C14 H14C 0.9679 . ?
C15 H15A 0.9676 . ?
C15 H15B 0.9547 . ?
C15 H15C 0.9618 . ?
C16 C17 1.391(18) . ?
C17 H17 0.9300 . ?
C18 O5 1.235(18) . ?
C18 O6 1.275(19) . ?
C18 C19 1.49(2) . ?
C19 C20 1.38(2) . ?
C19 C34 1.407(19) . ?
C20 C21 1.40(2) . ?
C20 H20 0.9300 . ?
C21 C22 1.40(2) . ?
C21 H21 0.9300 . ?
C22 C33 1.395(19) . ?
C22 C23 1.46(2) . ?
C23 C24 1.371(19) . ?
C23 C29 1.383(19) . ?
C24 C25 1.40(2) . ?
C24 H24 0.9300 . ?
C25 C26 1.37(2) . ?
C25 H25 0.9300 . ?
C26 C28 1.408(19) . ?
C26 C27 1.503(19) . ?
C27 O8 1.249(15) . ?
C27 O7 1.272(15) . ?
C28 C29 1.390(19) . ?
C28 H28 0.9300 . ?
C29 C30 1.539(19) . ?
C30 C33 1.52(2) . ?
C30 C31 1.53(2) . ?
C30 C32 1.54(2) . ?
C31 H31A 0.9656 . ?
C31 H31B 0.9545 . ?
C31 H31C 0.9674 . ?
C32 H32A 0.9677 . ?
C32 H32B 0.9541 . ?
C32 H32C 0.9585 . ?
C33 C34 1.372(19) . ?
C34 H34 0.9300 . ?
C35 O10 1.245(16) . ?
C35 O9 1.253(16) . ?
C35 C36 1.534(16) . ?
C36 C51 1.371(18) . ?
C36 C37 1.398(18) . ?
C37 C38 1.375(17) . ?
C37 H37 0.9300 . ?
C38 C39 1.374(18) . ?
C38 H38 0.9300 . ?
C39 C50 1.401(17) . ?
C39 C40 1.473(17) . ?
C40 C41 1.392(18) . ?
C40 C46 1.400(18) . ?
C41 C42 1.394(18) . ?
C41 H41 0.9300 . ?
C42 C43 1.36(2) . ?
C42 H42 0.9300 . ?
C43 C45 1.409(18) . ?
C43 C44 1.498(18) . ?
C44 O12 1.269(18) . ?
C44 O11 1.274(17) . ?
C45 C46 1.360(17) . ?
C45 H45 0.9300 . ?
C46 C47 1.527(17) . ?
C47 C50 1.504(18) . ?
C47 C49 1.515(19) . ?
C47 C48 1.53(2) . ?
C48 H48A 0.9695 . ?
C48 H48B 0.9615 . ?
C48 H48C 0.9557 . ?
C49 H49A 0.9586 . ?
C49 H49B 0.9623 . ?
C49 H49C 0.9695 . ?
C50 C51 1.395(17) . ?
C51 H51 0.9300 . ?
C52 C53 1.53(3) . ?
C52 H52A 0.9551 . ?
C52 H52B 0.9676 . ?
C52 H52C 0.9615 . ?
C53 O14 1.24(2) . ?
C53 N2 1.24(3) . ?
C54 N2 1.46(3) . ?
C54 H54A 0.9631 . ?
C54 H54B 0.9679 . ?
C54 H54C 0.9533 . ?
C55 N2 1.59(4) . ?
C55 H55A 0.9639 . ?
C55 H55B 0.9610 . ?
C55 H55C 0.9598 . ?
C56 C57 1.76(5) . ?
C56 H56A 0.9535 . ?
C56 H56B 0.9670 . ?
C56 H56C 0.9604 . ?
C57 N1 1.07(4) . ?
C57 O15 1.21(3) . ?
C58 N1 1.72(5) . ?
C58 H58A 0.9631 . ?
C58 H58B 0.9560 . ?
C58 H58C 0.9619 . ?
C59 N1 1.45(3) . ?
C59 H59A 0.9583 . ?
C59 H59B 0.9695 . ?
C59 H59C 0.9553 . ?
O1 Sm2 2.395(9) 1_464 ?
O2 Sm2 2.343(11) 2_556 ?
O3 Sm1 2.378(10) 2_666 ?
O5 Sm2 2.348(10) 1_454 ?
O6 Sm2 2.361(10) 2_546 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Sm1 O14 79.1(3) . . ?
O4 Sm1 O3 83.8(3) . 2_666 ?
O14 Sm1 O3 79.4(4) . 2_666 ?
O4 Sm1 O7 76.2(3) . . ?
O14 Sm1 O7 121.8(4) . . ?
O3 Sm1 O7 146.4(3) 2_666 . ?
O4 Sm1 O13 77.0(3) . . ?
O14 Sm1 O13 146.3(4) . . ?
O3 Sm1 O13 74.7(4) 2_666 . ?
O7 Sm1 O13 74.6(3) . . ?
O4 Sm1 O8 96.0(3) . . ?
O14 Sm1 O8 78.4(4) . . ?
O3 Sm1 O8 157.4(4) 2_666 . ?
O7 Sm1 O8 53.4(3) . . ?
O13 Sm1 O8 127.3(3) . . ?
O4 Sm1 O9 151.4(3) . . ?
O14 Sm1 O9 128.3(3) . . ?
O3 Sm1 O9 107.0(4) 2_666 . ?
O7 Sm1 O9 81.0(3) . . ?
O13 Sm1 O9 80.5(3) . . ?
O8 Sm1 O9 83.9(4) . . ?
O4 Sm1 O10 155.0(3) . . ?
O14 Sm1 O10 79.9(3) . . ?
O3 Sm1 O10 79.0(3) 2_666 . ?
O7 Sm1 O10 127.1(3) . . ?
O13 Sm1 O10 115.2(3) . . ?
O8 Sm1 O10 93.0(3) . . ?
O9 Sm1 O10 52.8(3) . . ?
O4 Sm1 C27 85.1(3) . . ?
O14 Sm1 C27 99.9(4) . . ?
O3 Sm1 C27 168.8(3) 2_666 . ?
O7 Sm1 C27 26.9(3) . . ?
O13 Sm1 C27 101.3(4) . . ?
O8 Sm1 C27 26.4(3) . . ?
O9 Sm1 C27 82.3(3) . . ?
O10 Sm1 C27 111.9(3) . . ?
O4 Sm1 C35 175.8(3) . . ?
O14 Sm1 C35 104.0(4) . . ?
O3 Sm1 C35 93.9(4) 2_666 . ?
O7 Sm1 C35 104.1(4) . . ?
O13 Sm1 C35 99.0(4) . . ?
O8 Sm1 C35 87.5(4) . . ?
O9 Sm1 C35 26.5(3) . . ?
O10 Sm1 C35 26.3(3) . . ?
C27 Sm1 C35 97.0(4) . . ?
O2 Sm2 O5 76.8(4) 2_556 1_656 ?
O2 Sm2 O20 157.4(7) 2_556 . ?
O5 Sm2 O20 93.4(8) 1_656 . ?
O2 Sm2 O6 73.6(4) 2_556 2_546 ?
O5 Sm2 O6 127.7(4) 1_656 2_546 ?
O20 Sm2 O6 126.9(8) . 2_546 ?
O2 Sm2 O1 123.6(4) 2_556 1_646 ?
O5 Sm2 O1 78.5(4) 1_656 1_646 ?
O20 Sm2 O1 72.9(7) . 1_646 ?
O6 Sm2 O1 83.3(4) 2_546 1_646 ?
O2 Sm2 O12 82.2(4) 2_556 . ?
O5 Sm2 O12 82.0(4) 1_656 . ?
O20 Sm2 O12 76.3(7) . . ?
O6 Sm2 O12 133.7(4) 2_546 . ?
O1 Sm2 O12 142.1(4) 1_646 . ?
O2 Sm2 O11 87.7(4) 2_556 . ?
O5 Sm2 O11 134.4(3) 1_656 . ?
O20 Sm2 O11 84.8(7) . . ?
O6 Sm2 O11 86.3(4) 2_546 . ?
O1 Sm2 O11 142.0(4) 1_646 . ?
O12 Sm2 O11 53.3(3) . . ?
O2 Sm2 O19 147.2(9) 2_556 . ?
O5 Sm2 O19 136.0(9) 1_656 . ?
O20 Sm2 O19 47.1(6) . . ?
O6 Sm2 O19 80.8(8) 2_546 . ?
O1 Sm2 O19 72.1(9) 1_646 . ?
O12 Sm2 O19 101.9(9) . . ?
O11 Sm2 O19 70.2(9) . . ?
O2 Sm2 C44 83.9(4) 2_556 . ?
O5 Sm2 C44 108.1(4) 1_656 . ?
O20 Sm2 C44 79.8(7) . . ?
O6 Sm2 C44 110.5(4) 2_546 . ?
O1 Sm2 C44 152.3(4) 1_646 . ?
O12 Sm2 C44 26.5(4) . . ?
O11 Sm2 C44 26.8(4) . . ?
O19 Sm2 C44 86.1(9) . . ?
O2 C1 O1 123.4(13) . . ?
O2 C1 C2 119.4(13) . . ?
O1 C1 C2 117.2(14) . . ?
C17 C2 C3 121.5(12) . . ?
C17 C2 C1 118.6(13) . . ?
C3 C2 C1 119.9(13) . . ?
C4 C3 C2 121.1(13) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C3 C4 C5 117.4(13) . . ?
C3 C4 H4 121.3 . . ?
C5 C4 H4 121.3 . . ?
C16 C5 C4 121.4(12) . . ?
C16 C5 C6 107.9(11) . . ?
C4 C5 C6 130.7(12) . . ?
C7 C6 C12 120.1(11) . . ?
C7 C6 C5 130.9(12) . . ?
C12 C6 C5 109.0(10) . . ?
C8 C7 C6 118.7(13) . . ?
C8 C7 H7 120.6 . . ?
C6 C7 H7 120.6 . . ?
C7 C8 C9 120.9(12) . . ?
C7 C8 H8 119.5 . . ?
C9 C8 H8 119.5 . . ?
C8 C9 C11 119.6(12) . . ?
C8 C9 C10 121.4(11) . . ?
C11 C9 C10 118.9(12) . . ?
O3 C10 O4 123.8(12) . . ?
O3 C10 C9 118.5(11) . . ?
O4 C10 C9 117.6(12) . . ?
C12 C11 C9 120.2(13) . . ?
C12 C11 H11 119.9 . . ?
C9 C11 H11 119.9 . . ?
C11 C12 C6 120.4(12) . . ?
C11 C12 C13 130.3(13) . . ?
C6 C12 C13 109.3(11) . . ?
C16 C13 C12 102.5(11) . . ?
C16 C13 C15 110.9(13) . . ?
C12 C13 C15 111.6(13) . . ?
C16 C13 C14 112.0(13) . . ?
C12 C13 C14 110.0(12) . . ?
C15 C13 C14 109.6(14) . . ?
C13 C14 H14A 110.1 . . ?
C13 C14 H14B 108.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.8 . . ?
H14A C14 H14C 109.3 . . ?
H14B C14 H14C 109.7 . . ?
C13 C15 H15A 108.4 . . ?
C13 C15 H15B 110.2 . . ?
H15A C15 H15B 109.6 . . ?
C13 C15 H15C 109.9 . . ?
H15A C15 H15C 110.0 . . ?
H15B C15 H15C 108.8 . . ?
C5 C16 C17 119.6(13) . . ?
C5 C16 C13 111.2(11) . . ?
C17 C16 C13 129.1(13) . . ?
C2 C17 C16 119.0(13) . . ?
C2 C17 H17 120.5 . . ?
C16 C17 H17 120.5 . . ?
O5 C18 O6 124.8(15) . . ?
O5 C18 C19 118.8(15) . . ?
O6 C18 C19 116.5(13) . . ?
C20 C19 C34 120.0(13) . . ?
C20 C19 C18 120.9(13) . . ?
C34 C19 C18 119.1(12) . . ?
C19 C20 C21 121.3(14) . . ?
C19 C20 H20 119.4 . . ?
C21 C20 H20 119.4 . . ?
C22 C21 C20 118.3(13) . . ?
C22 C21 H21 120.8 . . ?
C20 C21 H21 120.8 . . ?
C33 C22 C21 120.2(13) . . ?
C33 C22 C23 109.4(13) . . ?
C21 C22 C23 130.4(13) . . ?
C24 C23 C29 120.4(13) . . ?
C24 C23 C22 131.4(14) . . ?
C29 C23 C22 108.2(12) . . ?
C23 C24 C25 119.5(13) . . ?
C23 C24 H24 120.2 . . ?
C25 C24 H24 120.2 . . ?
C26 C25 C24 119.6(13) . . ?
C26 C25 H25 120.2 . . ?
C24 C25 H25 120.2 . . ?
C25 C26 C28 122.1(13) . . ?
C25 C26 C27 120.5(12) . . ?
C28 C26 C27 117.3(13) . . ?
O8 C27 O7 119.8(12) . . ?
O8 C27 C26 121.5(12) . . ?
O7 C27 C26 118.6(12) . . ?
O8 C27 Sm1 60.6(7) . . ?
O7 C27 Sm1 59.3(6) . . ?
C26 C27 Sm1 177.7(9) . . ?
C29 C28 C26 116.6(13) . . ?
C29 C28 H28 121.7 . . ?
C26 C28 H28 121.7 . . ?
C23 C29 C28 121.7(13) . . ?
C23 C29 C30 111.3(12) . . ?
C28 C29 C30 127.0(13) . . ?
C33 C30 C31 111.5(13) . . ?
C33 C30 C29 100.7(11) . . ?
C31 C30 C29 111.4(12) . . ?
C33 C30 C32 112.4(12) . . ?
C31 C30 C32 109.2(14) . . ?
C29 C30 C32 111.5(12) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 108.7 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.9 . . ?
H31A C31 H31C 109.9 . . ?
H31B C31 H31C 109.3 . . ?
C30 C32 H32A 109.0 . . ?
C30 C32 H32B 111.0 . . ?
H32A C32 H32B 109.3 . . ?
C30 C32 H32C 108.7 . . ?
H32A C32 H32C 109.8 . . ?
H32B C32 H32C 109.0 . . ?
C34 C33 C22 121.1(13) . . ?
C34 C33 C30 128.4(13) . . ?
C22 C33 C30 110.4(12) . . ?
C33 C34 C19 119.0(12) . . ?
C33 C34 H34 120.5 . . ?
C19 C34 H34 120.5 . . ?
O10 C35 O9 122.6(11) . . ?
O10 C35 C36 118.7(12) . . ?
O9 C35 C36 118.6(12) . . ?
O10 C35 Sm1 61.4(6) . . ?
O9 C35 Sm1 61.3(6) . . ?
C36 C35 Sm1 174.1(9) . . ?
C51 C36 C37 120.7(11) . . ?
C51 C36 C35 119.2(12) . . ?
C37 C36 C35 120.0(11) . . ?
C38 C37 C36 120.1(12) . . ?
C38 C37 H37 120.0 . . ?
C36 C37 H37 120.0 . . ?
C39 C38 C37 119.9(12) . . ?
C39 C38 H38 120.0 . . ?
C37 C38 H38 120.0 . . ?
C38 C39 C50 120.1(11) . . ?
C38 C39 C40 132.4(12) . . ?
C50 C39 C40 107.3(11) . . ?
C41 C40 C46 120.6(12) . . ?
C41 C40 C39 130.8(12) . . ?
C46 C40 C39 108.7(11) . . ?
C40 C41 C42 117.7(13) . . ?
C40 C41 H41 121.2 . . ?
C42 C41 H41 121.2 . . ?
C43 C42 C41 122.6(12) . . ?
C43 C42 H42 118.7 . . ?
C41 C42 H42 118.7 . . ?
C42 C43 C45 118.7(12) . . ?
C42 C43 C44 123.2(12) . . ?
C45 C43 C44 118.1(13) . . ?
O12 C44 O11 120.7(12) . . ?
O12 C44 C43 120.1(12) . . ?
O11 C44 C43 119.2(14) . . ?
O12 C44 Sm2 58.5(7) . . ?
O11 C44 Sm2 62.2(7) . . ?
C43 C44 Sm2 178.5(11) . . ?
C46 C45 C43 120.5(13) . . ?
C46 C45 H45 119.7 . . ?
C43 C45 H45 119.7 . . ?
C45 C46 C40 119.9(12) . . ?
C45 C46 C47 129.4(12) . . ?
C40 C46 C47 110.7(10) . . ?
C50 C47 C49 110.9(11) . . ?
C50 C47 C48 113.4(11) . . ?
C49 C47 C48 110.3(13) . . ?
C50 C47 C46 101.0(10) . . ?
C49 C47 C46 109.7(11) . . ?
C48 C47 C46 111.0(11) . . ?
C47 C48 H48A 110.1 . . ?
C47 C48 H48B 109.6 . . ?
H48A C48 H48B 109.6 . . ?
C47 C48 H48C 108.4 . . ?
H48A C48 H48C 109.8 . . ?
H48B C48 H48C 109.2 . . ?
C47 C49 H49A 109.8 . . ?
C47 C49 H49B 108.2 . . ?
H49A C49 H49B 109.5 . . ?
C47 C49 H49C 109.9 . . ?
H49A C49 H49C 109.7 . . ?
H49B C49 H49C 109.7 . . ?
C51 C50 C39 119.9(12) . . ?
C51 C50 C47 127.8(12) . . ?
C39 C50 C47 112.2(10) . . ?
C36 C51 C50 119.1(12) . . ?
C36 C51 H51 120.4 . . ?
C50 C51 H51 120.4 . . ?
C53 C52 H52A 104.3 . . ?
C53 C52 H52B 110.3 . . ?
H52A C52 H52B 109.6 . . ?
C53 C52 H52C 113.7 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.3 . . ?
O14 C53 N2 125(2) . . ?
O14 C53 C52 121(2) . . ?
N2 C53 C52 114(2) . . ?
N2 C54 H54A 111.9 . . ?
N2 C54 H54B 108.7 . . ?
H54A C54 H54B 110.1 . . ?
N2 C54 H54C 107.7 . . ?
H54A C54 H54C 109.0 . . ?
H54B C54 H54C 109.4 . . ?
N2 C55 H55A 112.1 . . ?
N2 C55 H55B 104.5 . . ?
H55A C55 H55B 108.9 . . ?
N2 C55 H55C 111.6 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 110.1 . . ?
C57 C56 H56A 110.2 . . ?
C57 C56 H56B 108.6 . . ?
H56A C56 H56B 109.1 . . ?
C57 C56 H56C 109.9 . . ?
H56A C56 H56C 109.2 . . ?
H56B C56 H56C 109.9 . . ?
N1 C57 O15 146(6) . . ?
N1 C57 C56 102(4) . . ?
O15 C57 C56 112(4) . . ?
N1 C58 H58A 108.7 . . ?
N1 C58 H58B 109.8 . . ?
H58A C58 H58B 109.5 . . ?
N1 C58 H58C 110.2 . . ?
H58A C58 H58C 110.0 . . ?
H58B C58 H58C 108.6 . . ?
N1 C59 H59A 103.3 . . ?
N1 C59 H59B 116.4 . . ?
H59A C59 H59B 109.6 . . ?
N1 C59 H59C 108.5 . . ?
H59A C59 H59C 108.9 . . ?
H59B C59 H59C 109.8 . . ?
C57 N1 C59 147(6) . . ?
C57 N1 C58 103(4) . . ?
C59 N1 C58 110(4) . . ?
C53 N2 C54 130(3) . . ?
C53 N2 C55 110(2) . . ?
C54 N2 C55 120(3) . . ?
C1 O1 Sm2 115.9(10) . 1_464 ?
C1 O2 Sm2 176.8(11) . 2_556 ?
C10 O3 Sm1 141.9(10) . 2_666 ?
C10 O4 Sm1 142.7(9) . . ?
C18 O5 Sm2 136.1(10) . 1_454 ?
C18 O6 Sm2 131.1(10) . 2_546 ?
C27 O7 Sm1 93.7(7) . . ?
C27 O8 Sm1 93.0(8) . . ?
C35 O9 Sm1 92.2(8) . . ?
C35 O10 Sm1 92.3(8) . . ?
C44 O11 Sm2 91.0(9) . . ?
C44 O12 Sm2 95.0(8) . . ?
C53 O14 Sm1 148.2(12) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         3.015
_refine_diff_density_min         -2.731
_refine_diff_density_rms         0.202
####################################################################### 
# 
# 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_Tb
_database_code_depnum_ccdc_archive 'CCDC 1441105'
_audit_update_record             
;
2015-12-08 deposited with the CCDC.
2016-02-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C118 H108 N4 O28 Tb4, 15(H2O)'
_chemical_formula_sum            'C118 H138 N4 O43 Tb4'
_chemical_formula_weight         2936.00

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'
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'
N N 0.0061 0.0033 '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                   11.4646(4)
_cell_length_b                   13.6288(5)
_cell_length_c                   23.7978(7)
_cell_angle_alpha                92.929(3)
_cell_angle_beta                 103.548(3)
_cell_angle_gamma                112.494(3)
_cell_volume                     3298.61(19)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1987
_cell_measurement_theta_min      2.1
_cell_measurement_theta_max      20.3

_exptl_crystal_description       block
_exptl_crystal_colour            whiteless
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1478
_exptl_absorpt_coefficient_mu    2.198
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8267
_exptl_absorpt_correction_T_max  0.8613
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_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 Smart Aepex CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26114
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.22
_diffrn_reflns_theta_max         25.00
_reflns_number_total             11622
_reflns_number_gt                9770
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0178P)²+31.3194P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11622
_refine_ls_number_parameters     772
_refine_ls_number_restraints     35
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0503
_refine_ls_wR_factor_ref         0.1314
_refine_ls_wR_factor_gt          0.1269
_refine_ls_goodness_of_fit_ref   1.230
_refine_ls_restrained_S_all      1.236
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.37832(4) 0.30086(3) 0.517674(15) 0.02364(11) Uani 1 1 d . . .
Tb2 Tb 0.64148(4) -0.40528(3) 0.961627(16) 0.03054(12) Uani 1 1 d U . .
C1 C -0.2960(10) 0.4941(8) 0.0730(4) 0.047(2) Uani 1 1 d . . .
C2 C -0.2180(8) 0.4652(8) 0.1257(4) 0.040(2) Uani 1 1 d . . .
C3 C -0.2788(9) 0.3747(8) 0.1487(4) 0.047(2) Uani 1 1 d . . .
H3 H -0.3676 0.3316 0.1324 0.057 Uiso 1 1 calc R . .
C4 C -0.2070(8) 0.3480(7) 0.1965(4) 0.043(2) Uani 1 1 d . . .
H4 H -0.2466 0.2861 0.2118 0.052 Uiso 1 1 calc R . .
C5 C -0.0755(8) 0.4148(7) 0.2211(3) 0.0323(19) Uani 1 1 d . . .
C6 C 0.0199(8) 0.4102(7) 0.2728(3) 0.0320(19) Uani 1 1 d . . .
C7 C 0.0102(8) 0.3361(7) 0.3113(4) 0.041(2) Uani 1 1 d . . .
H7 H -0.0660 0.2737 0.3048 0.049 Uiso 1 1 calc R . .
C8 C 0.1153(8) 0.3565(6) 0.3592(4) 0.037(2) Uani 1 1 d . . .
H8 H 0.1091 0.3080 0.3857 0.045 Uiso 1 1 calc R . .
C9 C 0.2310(8) 0.4489(6) 0.3687(3) 0.0308(18) Uani 1 1 d . . .
C10 C 0.3425(8) 0.4719(6) 0.4216(3) 0.0305(18) Uani 1 1 d . . .
C11 C 0.2430(8) 0.5208(7) 0.3290(4) 0.035(2) Uani 1 1 d . . .
H11 H 0.3212 0.5808 0.3342 0.042 Uiso 1 1 calc R . .
C12 C 0.1364(8) 0.5014(7) 0.2816(3) 0.0327(19) Uani 1 1 d . . .
C13 C 0.1242(8) 0.5710(8) 0.2341(4) 0.043(2) Uani 1 1 d . . .
C14 C 0.2243(10) 0.5825(12) 0.1994(5) 0.079(4) Uani 1 1 d . . .
H14A H 0.2163 0.5128 0.1843 0.095 Uiso 1 1 d R . .
H14B H 0.3112 0.6224 0.2246 0.095 Uiso 1 1 d R . .
H14C H 0.2085 0.6203 0.1675 0.095 Uiso 1 1 d R . .
C15 C 0.1423(12) 0.6825(8) 0.2605(5) 0.077(4) Uani 1 1 d . . .
H15A H 0.1256 0.7221 0.2297 0.093 Uiso 1 1 d R . .
H15B H 0.2308 0.7202 0.2847 0.093 Uiso 1 1 d R . .
H15C H 0.0823 0.6752 0.2838 0.093 Uiso 1 1 d R . .
C16 C -0.0165(8) 0.5076(7) 0.1982(4) 0.038(2) Uani 1 1 d . . .
C17 C -0.0878(9) 0.5312(8) 0.1495(4) 0.049(3) Uani 1 1 d . . .
H17 H -0.0479 0.5913 0.1331 0.059 Uiso 1 1 calc R . .
C18 C -0.4441(9) -0.3384(7) 0.0771(4) 0.039(2) Uani 1 1 d . . .
C19 C -0.3752(8) -0.2756(7) 0.1375(4) 0.036(2) Uani 1 1 d . . .
C20 C -0.4264(9) -0.3038(7) 0.1832(4) 0.039(2) Uani 1 1 d . . .
H20 H -0.5080 -0.3608 0.1763 0.047 Uiso 1 1 calc R . .
C21 C -0.3605(9) -0.2501(7) 0.2397(4) 0.039(2) Uani 1 1 d . . .
H21 H -0.3963 -0.2709 0.2706 0.047 Uiso 1 1 calc R . .
C22 C -0.2390(8) -0.1639(6) 0.2490(4) 0.0327(19) Uani 1 1 d . . .
C23 C -0.1478(8) -0.0927(7) 0.3027(3) 0.0319(18) Uani 1 1 d . . .
C24 C -0.1531(8) -0.0935(7) 0.3606(4) 0.037(2) Uani 1 1 d . . .
H24 H -0.2238 -0.1442 0.3704 0.044 Uiso 1 1 calc R . .
C25 C -0.0502(8) -0.0167(7) 0.4026(4) 0.036(2) Uani 1 1 d . . .
H25 H -0.0529 -0.0147 0.4414 0.044 Uiso 1 1 calc R . .
C26 C 0.0577(8) 0.0580(7) 0.3891(3) 0.0330(19) Uani 1 1 d . . .
C27 C 0.1713(8) 0.1403(6) 0.4363(4) 0.0307(18) Uani 1 1 d . . .
C28 C 0.0633(8) 0.0571(7) 0.3317(4) 0.0339(19) Uani 1 1 d . . .
H28 H 0.1354 0.1068 0.3224 0.041 Uiso 1 1 calc R . .
C29 C -0.0391(8) -0.0183(7) 0.2887(3) 0.0321(18) Uani 1 1 d . . .
C30 C -0.0545(8) -0.0354(7) 0.2230(4) 0.038(2) Uani 1 1 d . . .
C31 C 0.0553(10) -0.0638(10) 0.2107(5) 0.065(3) Uani 1 1 d . . .
H31A H 0.0599 -0.1221 0.2307 0.078 Uiso 1 1 d R . .
H31B H 0.1376 -0.0023 0.2244 0.078 Uiso 1 1 d R . .
H31C H 0.0372 -0.0849 0.1694 0.078 Uiso 1 1 d R . .
C32 C -0.0540(11) 0.0633(8) 0.1953(5) 0.061(3) Uani 1 1 d . . .
H32A H -0.0753 0.0464 0.1535 0.073 Uiso 1 1 d R . .
H32B H 0.0312 0.1213 0.2096 0.073 Uiso 1 1 d R . .
H32C H -0.1184 0.0841 0.2055 0.073 Uiso 1 1 d R . .
C33 C -0.1877(8) -0.1312(7) 0.2025(4) 0.0343(19) Uani 1 1 d . . .
C34 C -0.2544(8) -0.1865(6) 0.1462(3) 0.0325(19) Uani 1 1 d . . .
H34 H -0.2202 -0.1652 0.1149 0.039 Uiso 1 1 calc R . .
C35 C 0.4632(8) 0.1640(7) 0.5819(3) 0.0304(18) Uani 1 1 d . . .
C36 C 0.4984(8) 0.0834(6) 0.6152(3) 0.0309(18) Uani 1 1 d . . .
C37 C 0.5345(9) 0.0099(7) 0.5887(4) 0.038(2) Uani 1 1 d . . .
H37 H 0.5382 0.0116 0.5501 0.045 Uiso 1 1 calc R . .
C38 C 0.5647(9) -0.0648(7) 0.6185(4) 0.038(2) Uani 1 1 d . . .
H38 H 0.5893 -0.1131 0.6005 0.045 Uiso 1 1 calc R . .
C39 C 0.5579(8) -0.0672(6) 0.6761(3) 0.0299(18) Uani 1 1 d . . .
C40 C 0.5813(8) -0.1373(7) 0.7178(4) 0.0335(19) Uani 1 1 d . . .
C41 C 0.6166(9) -0.2236(7) 0.7127(4) 0.039(2) Uani 1 1 d . . .
H41 H 0.6290 -0.2465 0.6779 0.047 Uiso 1 1 calc R . .
C42 C 0.6328(9) -0.2743(7) 0.7609(4) 0.042(2) Uani 1 1 d . . .
H42 H 0.6585 -0.3309 0.7580 0.050 Uiso 1 1 calc R . .
C43 C 0.6131(8) -0.2459(7) 0.8122(3) 0.0345(19) Uani 1 1 d . . .
C44 C 0.6274(9) -0.3007(7) 0.8644(4) 0.039(2) Uani 1 1 d . . .
C45 C 0.5771(8) -0.1573(7) 0.8171(4) 0.036(2) Uani 1 1 d . . .
H45 H 0.5653 -0.1348 0.8521 0.044 Uiso 1 1 calc R . .
C46 C 0.5598(8) -0.1051(7) 0.7698(4) 0.0325(19) Uani 1 1 d . . .
C47 C 0.5182(8) -0.0126(6) 0.7645(3) 0.0311(18) Uani 1 1 d . . .
C48 C 0.6143(11) 0.0859(8) 0.8101(4) 0.050(3) Uani 1 1 d . . .
H48A H 0.6201 0.0670 0.8487 0.060 Uiso 1 1 d R . .
H48B H 0.5834 0.1422 0.8068 0.060 Uiso 1 1 d R . .
H48C H 0.6994 0.1103 0.8033 0.060 Uiso 1 1 d R . .
C49 C 0.3776(10) -0.0462(9) 0.7705(5) 0.052(3) Uani 1 1 d . . .
H49A H 0.3198 -0.1107 0.7434 0.062 Uiso 1 1 d R . .
H49B H 0.3491 0.0103 0.7618 0.062 Uiso 1 1 d R . .
H49C H 0.3764 -0.0590 0.8097 0.062 Uiso 1 1 d R . .
C50 C 0.5227(8) 0.0064(7) 0.7029(3) 0.0300(18) Uani 1 1 d . . .
C51 C 0.4932(8) 0.0820(6) 0.6726(3) 0.0305(18) Uani 1 1 d . . .
H51 H 0.4702 0.1312 0.6907 0.037 Uiso 1 1 calc R . .
C52 C 0.1103(13) 0.4314(14) 0.5376(8) 0.114(5) Uani 1 1 d U . .
H52A H 0.0259 0.3784 0.5375 0.137 Uiso 1 1 d R . .
H52B H 0.1255 0.4219 0.5001 0.137 Uiso 1 1 d R . .
H52C H 0.1126 0.5019 0.5456 0.137 Uiso 1 1 d R . .
C53 C 0.2200(13) 0.4190(10) 0.5857(6) 0.073(3) Uani 1 1 d U . .
C54 C 0.201(3) 0.5503(17) 0.6500(10) 0.211(12) Uani 1 1 d U . .
H54A H 0.2398 0.6164 0.6357 0.254 Uiso 1 1 d R . .
H54B H 0.2238 0.5635 0.6920 0.254 Uiso 1 1 d R . .
H54C H 0.1068 0.5221 0.6347 0.254 Uiso 1 1 d R . .
C55 C 0.364(3) 0.4628(15) 0.6783(7) 0.172(10) Uani 1 1 d U . .
H55A H 0.3271 0.3993 0.6951 0.206 Uiso 1 1 d R . .
H55B H 0.4048 0.5245 0.7085 0.206 Uiso 1 1 d R . .
H55C H 0.4281 0.4568 0.6604 0.206 Uiso 1 1 d R . .
C56 C 0.8046(16) 0.1710(14) 0.4240(9) 0.126(7) Uani 1 1 d D . .
H56A H 0.8970 0.1919 0.4294 0.151 Uiso 1 1 d R . .
H56B H 0.7671 0.1878 0.3873 0.151 Uiso 1 1 d R . .
H56C H 0.7631 0.0951 0.4242 0.151 Uiso 1 1 d R . .
C57 C 0.7775(15) 0.2335(14) 0.4729(10) 0.132(9) Uani 1 1 d D . .
C58 C 0.7909(18) 0.2769(17) 0.5698(8) 0.133(8) Uani 1 1 d . . .
H58A H 0.7575 0.3276 0.5543 0.160 Uiso 1 1 d R . .
H58B H 0.8748 0.3147 0.5978 0.160 Uiso 1 1 d R . .
H58C H 0.7308 0.2295 0.5885 0.160 Uiso 1 1 d R . .
C59 C 0.856(2) 0.1300(18) 0.5342(13) 0.215(15) Uani 1 1 d . . .
H59A H 0.7975 0.0640 0.5085 0.258 Uiso 1 1 d R . .
H59B H 0.8584 0.1200 0.5740 0.258 Uiso 1 1 d R . .
H59C H 0.9427 0.1505 0.5293 0.258 Uiso 1 1 d R . .
N1 N 0.8043(16) 0.2097(17) 0.5161(13) 0.171(11) Uani 1 1 d . . .
N2 N 0.2495(17) 0.4749(10) 0.6312(6) 0.112(4) Uani 1 1 d U . .
O1 O -0.2341(7) 0.5514(6) 0.0422(3) 0.063(2) Uani 1 1 d . . .
O2 O -0.4183(6) 0.4575(6) 0.0630(3) 0.0568(19) Uani 1 1 d . . .
O3 O 0.4514(5) 0.5449(5) 0.4234(3) 0.0434(16) Uani 1 1 d . . .
O4 O 0.3207(5) 0.4211(4) 0.4636(2) 0.0323(13) Uani 1 1 d . . .
O5 O -0.3858(7) -0.3131(5) 0.0376(3) 0.0529(18) Uani 1 1 d . . .
O6 O -0.5570(6) -0.4135(5) 0.0700(3) 0.0458(16) Uani 1 1 d . . .
O7 O 0.2717(5) 0.1986(4) 0.4223(2) 0.0333(13) Uani 1 1 d . . .
O8 O 0.1634(6) 0.1509(5) 0.4882(3) 0.0463(16) Uani 1 1 d . . .
O9 O 0.4601(6) 0.1610(5) 0.5284(2) 0.0417(15) Uani 1 1 d . . .
O10 O 0.4343(6) 0.2314(5) 0.6072(2) 0.0366(14) Uani 1 1 d . . .
O11 O 0.6318(8) -0.3911(5) 0.8588(3) 0.0558(19) Uani 1 1 d . . .
O12 O 0.6320(8) -0.2573(5) 0.9138(3) 0.0547(19) Uani 1 1 d . . .
O13 O 0.5421(6) 0.3589(5) 0.4644(3) 0.0440(15) Uani 1 1 d . . .
O14 O 0.2675(7) 0.3562(6) 0.5730(3) 0.0490(16) Uani 1 1 d . . .
O15 O 0.7368(10) 0.3045(8) 0.4594(6) 0.105(4) Uani 1 1 d . . .
O16 O 0.0000 0.5000 0.0000 0.47(3) Uani 1 2 d SU . .
O17 O 0.876(5) 0.960(4) 0.977(2) 0.29(2) Uani 0.50 1 d PU . .
O18 O 0.463(7) 0.050(6) 0.993(4) 0.39(4) Uani 0.50 1 d P . .
O19 O 0.846(4) -0.430(2) 0.9356(15) 0.42(2) Uani 1 1 d DU . .
O20 O 0.8600(13) -0.2911(13) 0.9740(6) 0.156(5) Uani 1 1 d DU . .
O21 O 0.011(3) 0.708(3) 0.922(3) 0.46(3) Uani 1 1 d . . .
O22 O 0.038(3) 0.790(3) 0.0549(14) 0.43(2) Uani 1 1 d . . .
O23 O 0.119(8) 0.736(4) 0.9934(14) 0.65(5) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O14 2.310(6) . ?
Tb1 O4 2.329(5) . ?
Tb1 O3 2.340(6) 2_666 ?
Tb1 O7 2.378(5) . ?
Tb1 O13 2.416(6) . ?
Tb1 O10 2.425(5) . ?
Tb1 O9 2.425(6) . ?
Tb1 O8 2.435(6) . ?
Tb1 C27 2.759(8) . ?
Tb1 C35 2.783(8) . ?
Tb2 O6 2.290(6) 2_546 ?
Tb2 O2 2.293(6) 2_556 ?
Tb2 O5 2.297(7) 1_656 ?
Tb2 O20 2.326(13) . ?
Tb2 O1 2.354(6) 1_646 ?
Tb2 O12 2.392(6) . ?
Tb2 O11 2.443(6) . ?
Tb2 O19 2.69(4) . ?
Tb2 C44 2.783(8) . ?
C1 O1 1.236(12) . ?
C1 O2 1.252(11) . ?
C1 C2 1.524(11) . ?
C2 C17 1.373(12) . ?
C2 C3 1.377(13) . ?
C3 C4 1.392(12) . ?
C3 H3 0.9300 . ?
C4 C5 1.387(11) . ?
C4 H4 0.9300 . ?
C5 C16 1.393(11) . ?
C5 C6 1.466(10) . ?
C6 C7 1.388(11) . ?
C6 C12 1.394(11) . ?
C7 C8 1.378(11) . ?
C7 H7 0.9300 . ?
C8 C9 1.396(11) . ?
C8 H8 0.9300 . ?
C9 C11 1.387(11) . ?
C9 C10 1.488(10) . ?
C10 O3 1.253(10) . ?
C10 O4 1.263(9) . ?
C11 C12 1.384(10) . ?
C11 H11 0.9300 . ?
C12 C13 1.527(11) . ?
C13 C16 1.514(11) . ?
C13 C14 1.531(15) . ?
C13 C15 1.533(15) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.381(11) . ?
C17 H17 0.9300 . ?
C18 O5 1.266(11) . ?
C18 O6 1.271(10) . ?
C18 C19 1.499(12) . ?
C19 C20 1.357(12) . ?
C19 C34 1.411(11) . ?
C20 C21 1.384(12) . ?
C20 H20 0.9300 . ?
C21 C22 1.395(11) . ?
C21 H21 0.9300 . ?
C22 C33 1.388(12) . ?
C22 C23 1.461(11) . ?
C23 C24 1.395(12) . ?
C23 C29 1.397(11) . ?
C24 C25 1.372(12) . ?
C24 H24 0.9300 . ?
C25 C26 1.388(12) . ?
C25 H25 0.9300 . ?
C26 C28 1.382(11) . ?
C26 C27 1.511(11) . ?
C27 O7 1.255(10) . ?
C27 O8 1.263(10) . ?
C28 C29 1.375(11) . ?
C28 H28 0.9300 . ?
C29 C30 1.527(11) . ?
C30 C32 1.527(14) . ?
C30 C33 1.528(11) . ?
C30 C31 1.534(14) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 C34 1.385(11) . ?
C34 H34 0.9300 . ?
C35 O10 1.260(10) . ?
C35 O9 1.264(9) . ?
C35 C36 1.509(10) . ?
C36 C51 1.381(11) . ?
C36 C37 1.395(12) . ?
C37 C38 1.375(11) . ?
C37 H37 0.9300 . ?
C38 C39 1.393(11) . ?
C38 H38 0.9300 . ?
C39 C50 1.393(11) . ?
C39 C40 1.462(11) . ?
C40 C41 1.391(12) . ?
C40 C46 1.396(12) . ?
C41 C42 1.380(12) . ?
C41 H41 0.9300 . ?
C42 C43 1.357(12) . ?
C42 H42 0.9300 . ?
C43 C45 1.424(12) . ?
C43 C44 1.490(11) . ?
C44 O11 1.254(11) . ?
C44 O12 1.269(11) . ?
C45 C46 1.379(11) . ?
C45 H45 0.9300 . ?
C46 C47 1.511(11) . ?
C47 C50 1.512(11) . ?
C47 C48 1.533(12) . ?
C47 C49 1.541(12) . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C50 C51 1.388(11) . ?
C51 H51 0.9300 . ?
C52 C53 1.56(2) . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C53 N2 1.190(17) . ?
C53 O14 1.235(14) . ?
C54 N2 1.44(2) . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C55 N2 1.58(2) . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?
C56 C57 1.564(10) . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
C57 N1 1.10(2) . ?
C57 O15 1.25(2) . ?
C58 N1 1.60(3) . ?
C58 H58A 0.9600 . ?
C58 H58B 0.9600 . ?
C58 H58C 0.9600 . ?
C59 N1 1.46(2) . ?
C59 H59A 0.9600 . ?
C59 H59B 0.9600 . ?
C59 H59C 0.9600 . ?
O1 Tb2 2.354(6) 1_464 ?
O2 Tb2 2.293(6) 2_556 ?
O3 Tb1 2.340(6) 2_666 ?
O5 Tb2 2.297(7) 1_454 ?
O6 Tb2 2.290(6) 2_546 ?
O21 O23 1.77(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
O14 Tb1 O4 77.9(2) . . ?
O14 Tb1 O3 79.0(2) . 2_666 ?
O4 Tb1 O3 84.93(19) . 2_666 ?
O14 Tb1 O7 122.2(2) . . ?
O4 Tb1 O7 77.09(19) . . ?
O3 Tb1 O7 147.5(2) 2_666 . ?
O14 Tb1 O13 145.1(2) . . ?
O4 Tb1 O13 77.3(2) . . ?
O3 Tb1 O13 74.7(2) 2_666 . ?
O7 Tb1 O13 75.0(2) . . ?
O14 Tb1 O10 79.2(2) . . ?
O4 Tb1 O10 154.1(2) . . ?
O3 Tb1 O10 78.8(2) 2_666 . ?
O7 Tb1 O10 126.2(2) . . ?
O13 Tb1 O10 116.9(2) . . ?
O14 Tb1 O9 129.8(2) . . ?
O4 Tb1 O9 151.5(2) . . ?
O3 Tb1 O9 105.0(2) 2_666 . ?
O7 Tb1 O9 80.93(19) . . ?
O13 Tb1 O9 79.7(2) . . ?
O10 Tb1 O9 53.85(19) . . ?
O14 Tb1 O8 78.7(2) . . ?
O4 Tb1 O8 97.3(2) . . ?
O3 Tb1 O8 156.6(2) 2_666 . ?
O7 Tb1 O8 54.24(19) . . ?
O13 Tb1 O8 128.5(2) . . ?
O10 Tb1 O8 90.1(2) . . ?
O9 Tb1 O8 84.2(2) . . ?
O14 Tb1 C27 100.7(2) . . ?
O4 Tb1 C27 86.3(2) . . ?
O3 Tb1 C27 171.1(2) 2_666 . ?
O7 Tb1 C27 27.0(2) . . ?
O13 Tb1 C27 101.8(2) . . ?
O10 Tb1 C27 109.9(2) . . ?
O9 Tb1 C27 82.2(2) . . ?
O8 Tb1 C27 27.2(2) . . ?
O14 Tb1 C35 104.4(2) . . ?
O4 Tb1 C35 176.4(2) . . ?
O3 Tb1 C35 92.8(2) 2_666 . ?
O7 Tb1 C35 103.7(2) . . ?
O13 Tb1 C35 99.5(2) . . ?
O10 Tb1 C35 26.9(2) . . ?
O9 Tb1 C35 27.0(2) . . ?
O8 Tb1 C35 85.9(2) . . ?
C27 Tb1 C35 95.9(2) . . ?
O6 Tb2 O2 75.5(2) 2_546 2_556 ?
O6 Tb2 O5 129.7(2) 2_546 1_656 ?
O2 Tb2 O5 77.6(3) 2_556 1_656 ?
O6 Tb2 O20 123.6(5) 2_546 . ?
O2 Tb2 O20 157.0(4) 2_556 . ?
O5 Tb2 O20 95.5(5) 1_656 . ?
O6 Tb2 O1 82.9(2) 2_546 1_646 ?
O2 Tb2 O1 125.6(3) 2_556 1_646 ?
O5 Tb2 O1 79.4(3) 1_656 1_646 ?
O20 Tb2 O1 73.3(4) . 1_646 ?
O6 Tb2 O12 132.8(2) 2_546 . ?
O2 Tb2 O12 81.9(3) 2_556 . ?
O5 Tb2 O12 83.2(2) 1_656 . ?
O20 Tb2 O12 75.4(4) . . ?
O1 Tb2 O12 142.3(3) 1_646 . ?
O6 Tb2 O11 84.2(2) 2_546 . ?
O2 Tb2 O11 88.3(3) 2_556 . ?
O5 Tb2 O11 136.4(2) 1_656 . ?
O20 Tb2 O11 81.7(4) . . ?
O1 Tb2 O11 138.7(3) 1_646 . ?
O12 Tb2 O11 53.8(2) . . ?
O6 Tb2 O19 77.9(6) 2_546 . ?
O2 Tb2 O19 146.8(7) 2_556 . ?
O5 Tb2 O19 135.4(7) 1_656 . ?
O20 Tb2 O19 46.0(5) . . ?
O1 Tb2 O19 69.4(8) 1_646 . ?
O12 Tb2 O19 102.5(8) . . ?
O11 Tb2 O19 69.6(8) . . ?
O6 Tb2 C44 108.7(2) 2_546 . ?
O2 Tb2 C44 84.1(3) 2_556 . ?
O5 Tb2 C44 109.9(3) 1_656 . ?
O20 Tb2 C44 77.6(4) . . ?
O1 Tb2 C44 150.2(3) 1_646 . ?
O12 Tb2 C44 27.1(2) . . ?
O11 Tb2 C44 26.8(2) . . ?
O19 Tb2 C44 85.9(8) . . ?
O1 C1 O2 124.0(8) . . ?
O1 C1 C2 117.6(9) . . ?
O2 C1 C2 118.4(9) . . ?
C17 C2 C3 121.4(8) . . ?
C17 C2 C1 118.7(8) . . ?
C3 C2 C1 119.9(8) . . ?
C2 C3 C4 119.7(8) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C5 C4 C3 119.1(8) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C4 C5 C16 120.3(7) . . ?
C4 C5 C6 130.7(8) . . ?
C16 C5 C6 108.9(7) . . ?
C7 C6 C12 120.2(7) . . ?
C7 C6 C5 131.7(7) . . ?
C12 C6 C5 108.1(7) . . ?
C8 C7 C6 118.9(8) . . ?
C8 C7 H7 120.6 . . ?
C6 C7 H7 120.6 . . ?
C7 C8 C9 121.0(7) . . ?
C7 C8 H8 119.5 . . ?
C9 C8 H8 119.5 . . ?
C11 C9 C8 120.3(7) . . ?
C11 C9 C10 119.2(7) . . ?
C8 C9 C10 120.5(7) . . ?
O3 C10 O4 123.4(7) . . ?
O3 C10 C9 118.1(7) . . ?
O4 C10 C9 118.3(7) . . ?
C12 C11 C9 118.7(7) . . ?
C12 C11 H11 120.7 . . ?
C9 C11 H11 120.7 . . ?
C11 C12 C6 120.9(7) . . ?
C11 C12 C13 128.1(7) . . ?
C6 C12 C13 111.0(6) . . ?
C16 C13 C12 101.1(7) . . ?
C16 C13 C14 113.3(8) . . ?
C12 C13 C14 111.0(8) . . ?
C16 C13 C15 110.4(8) . . ?
C12 C13 C15 111.1(8) . . ?
C14 C13 C15 109.8(9) . . ?
C13 C14 H14A 110.2 . . ?
C13 C14 H14B 109.1 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.1 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.4 . . ?
C13 C15 H15B 109.2 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.7 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C5 119.9(8) . . ?
C17 C16 C13 129.2(8) . . ?
C5 C16 C13 110.9(7) . . ?
C2 C17 C16 119.5(9) . . ?
C2 C17 H17 120.3 . . ?
C16 C17 H17 120.3 . . ?
O5 C18 O6 125.3(8) . . ?
O5 C18 C19 117.9(8) . . ?
O6 C18 C19 116.8(8) . . ?
C20 C19 C34 120.3(8) . . ?
C20 C19 C18 121.3(8) . . ?
C34 C19 C18 118.5(8) . . ?
C19 C20 C21 121.9(8) . . ?
C19 C20 H20 119.1 . . ?
C21 C20 H20 119.1 . . ?
C20 C21 C22 118.3(8) . . ?
C20 C21 H21 120.9 . . ?
C22 C21 H21 120.9 . . ?
C33 C22 C21 120.6(8) . . ?
C33 C22 C23 108.5(7) . . ?
C21 C22 C23 130.9(8) . . ?
C24 C23 C29 120.8(7) . . ?
C24 C23 C22 130.5(8) . . ?
C29 C23 C22 108.6(7) . . ?
C25 C24 C23 117.5(8) . . ?
C25 C24 H24 121.2 . . ?
C23 C24 H24 121.2 . . ?
C24 C25 C26 122.1(8) . . ?
C24 C25 H25 118.9 . . ?
C26 C25 H25 118.9 . . ?
C28 C26 C25 120.0(7) . . ?
C28 C26 C27 118.8(7) . . ?
C25 C26 C27 121.2(7) . . ?
O7 C27 O8 121.3(7) . . ?
O7 C27 C26 118.3(7) . . ?
O8 C27 C26 120.4(7) . . ?
O7 C27 Tb1 59.4(4) . . ?
O8 C27 Tb1 62.0(4) . . ?
C26 C27 Tb1 176.1(6) . . ?
C29 C28 C26 119.1(8) . . ?
C29 C28 H28 120.5 . . ?
C26 C28 H28 120.5 . . ?
C28 C29 C23 120.5(8) . . ?
C28 C29 C30 128.5(8) . . ?
C23 C29 C30 111.0(7) . . ?
C32 C30 C29 112.2(8) . . ?
C32 C30 C33 112.6(8) . . ?
C29 C30 C33 100.4(6) . . ?
C32 C30 C31 109.1(9) . . ?
C29 C30 C31 110.7(8) . . ?
C33 C30 C31 111.6(8) . . ?
C30 C31 H31A 109.2 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.7 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.8 . . ?
C30 C32 H32B 109.7 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 108.9 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 C22 120.4(8) . . ?
C34 C33 C30 128.1(8) . . ?
C22 C33 C30 111.5(7) . . ?
C33 C34 C19 118.6(8) . . ?
C33 C34 H34 120.7 . . ?
C19 C34 H34 120.7 . . ?
O10 C35 O9 120.9(7) . . ?
O10 C35 C36 119.8(7) . . ?
O9 C35 C36 119.2(8) . . ?
O10 C35 Tb1 60.5(4) . . ?
O9 C35 Tb1 60.5(4) . . ?
C36 C35 Tb1 175.6(6) . . ?
C51 C36 C37 119.9(7) . . ?
C51 C36 C35 119.2(7) . . ?
C37 C36 C35 120.9(7) . . ?
C38 C37 C36 121.2(8) . . ?
C38 C37 H37 119.4 . . ?
C36 C37 H37 119.4 . . ?
C37 C38 C39 118.9(8) . . ?
C37 C38 H38 120.5 . . ?
C39 C38 H38 120.5 . . ?
C38 C39 C50 120.0(7) . . ?
C38 C39 C40 131.4(8) . . ?
C50 C39 C40 108.6(7) . . ?
C41 C40 C46 120.7(8) . . ?
C41 C40 C39 131.5(8) . . ?
C46 C40 C39 107.8(7) . . ?
C42 C41 C40 117.9(9) . . ?
C42 C41 H41 121.0 . . ?
C40 C41 H41 121.0 . . ?
C43 C42 C41 123.5(8) . . ?
C43 C42 H42 118.3 . . ?
C41 C42 H42 118.3 . . ?
C42 C43 C45 118.2(8) . . ?
C42 C43 C44 124.4(8) . . ?
C45 C43 C44 117.4(8) . . ?
O11 C44 O12 120.3(8) . . ?
O11 C44 C43 119.5(8) . . ?
O12 C44 C43 120.1(8) . . ?
O11 C44 Tb2 61.3(5) . . ?
O12 C44 Tb2 59.0(4) . . ?
C43 C44 Tb2 177.2(6) . . ?
C46 C45 C43 119.8(8) . . ?
C46 C45 H45 120.1 . . ?
C43 C45 H45 120.1 . . ?
C45 C46 C40 119.9(8) . . ?
C45 C46 C47 128.7(8) . . ?
C40 C46 C47 111.4(7) . . ?
C46 C47 C50 101.1(7) . . ?
C46 C47 C48 111.2(7) . . ?
C50 C47 C48 112.0(7) . . ?
C46 C47 C49 110.8(7) . . ?
C50 C47 C49 110.9(7) . . ?
C48 C47 C49 110.5(8) . . ?
C47 C48 H48A 109.6 . . ?
C47 C48 H48B 109.3 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.2 . . ?
H49A C49 H49B 109.5 . . ?
C47 C49 H49C 109.8 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C51 C50 C39 120.6(7) . . ?
C51 C50 C47 128.3(8) . . ?
C39 C50 C47 111.0(7) . . ?
C36 C51 C50 119.3(8) . . ?
C36 C51 H51 120.4 . . ?
C50 C51 H51 120.4 . . ?
C53 C52 H52A 110.0 . . ?
C53 C52 H52B 109.2 . . ?
H52A C52 H52B 109.5 . . ?
C53 C52 H52C 109.2 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
N2 C53 O14 127.6(16) . . ?
N2 C53 C52 113.8(15) . . ?
O14 C53 C52 118.6(13) . . ?
N2 C54 H54A 108.7 . . ?
N2 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
N2 C54 H54C 110.2 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
N2 C55 H55A 108.7 . . ?
N2 C55 H55B 109.4 . . ?
H55A C55 H55B 109.5 . . ?
N2 C55 H55C 110.3 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C57 C56 H56A 111.6 . . ?
C57 C56 H56B 107.1 . . ?
H56A C56 H56B 109.5 . . ?
C57 C56 H56C 109.7 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
N1 C57 O15 130(2) . . ?
N1 C57 C56 112(2) . . ?
O15 C57 C56 118.2(19) . . ?
N1 C58 H58A 107.7 . . ?
N1 C58 H58B 110.6 . . ?
H58A C58 H58B 109.5 . . ?
N1 C58 H58C 110.1 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
N1 C59 H59A 105.6 . . ?
N1 C59 H59B 112.3 . . ?
H59A C59 H59B 109.5 . . ?
N1 C59 H59C 110.4 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C57 N1 C59 131(3) . . ?
C57 N1 C58 115(2) . . ?
C59 N1 C58 113(2) . . ?
C53 N2 C54 132(2) . . ?
C53 N2 C55 112.4(14) . . ?
C54 N2 C55 116.0(17) . . ?
C1 O1 Tb2 116.4(6) . 1_464 ?
C1 O2 Tb2 173.7(7) . 2_556 ?
C10 O3 Tb1 142.8(6) . 2_666 ?
C10 O4 Tb1 142.2(6) . . ?
C18 O5 Tb2 135.7(6) . 1_454 ?
C18 O6 Tb2 132.8(6) . 2_546 ?
C27 O7 Tb1 93.6(5) . . ?
C27 O8 Tb1 90.8(5) . . ?
C35 O9 Tb1 92.5(5) . . ?
C35 O10 Tb1 92.6(4) . . ?
C44 O11 Tb2 91.9(5) . . ?
C44 O12 Tb2 93.9(5) . . ?
C53 O14 Tb1 151.0(7) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.607
_refine_diff_density_min         -1.079
_refine_diff_density_rms         0.139
