# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2017

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

data_1
_database_code_depnum_ccdc_archive 'CCDC 1526560'
_audit_update_record             
;
2017-01-10 deposited with the CCDC.
2017-04-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C38 H36 Eu O20, C6 N H15, 2(H2 O)'
_chemical_formula_sum            'C44 H55 Eu N O22'
_chemical_formula_weight         1101.85

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

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'

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

_cell_length_a                   20.072(4)
_cell_length_b                   16.329(4)
_cell_length_c                   16.631(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5451(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    39894
_cell_measurement_theta_min      3.04
_cell_measurement_theta_max      27.58

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLORLESS
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2260
_exptl_absorpt_coefficient_mu    1.224
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7594
_exptl_absorpt_correction_T_max  0.7990
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      291(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  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            41969
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.18
_diffrn_reflns_theta_max         25.00
_reflns_number_total             9533
_reflns_number_gt                7692
_reflns_threshold_expression     >2sigma(I)

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

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

_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)+(0.0884P)²+3.4106P] 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_abs_structure_details 
'Flack H D (1983), Acta Cryst. A39, 876-881, pairs measured  4222'
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_number_reflns         9533
_refine_ls_number_parameters     617
_refine_ls_number_restraints     64
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0471
_refine_ls_wR_factor_ref         0.1424
_refine_ls_wR_factor_gt          0.1341
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.6981(7) 0.8945(9) 0.1595(10) 0.160(5) Uani 1 1 d D . .
C1 C 0.4020(4) 0.8417(6) -0.1303(6) 0.081(3) Uani 1 1 d . . .
C2 C 0.4342(6) 0.8869(7) -0.0711(7) 0.104(3) Uani 1 1 d . . .
H2 H 0.4718 0.8660 -0.0456 0.125 Uiso 1 1 calc R . .
C4 C 0.3552(7) 0.9922(9) -0.0953(9) 0.133(4) Uani 1 1 d U . .
H4 H 0.3364 1.0424 -0.0815 0.159 Uiso 1 1 calc R . .
C3 C 0.4095(6) 0.9644(7) -0.0501(11) 0.137(5) Uani 1 1 d . . .
H3 H 0.4281 0.9953 -0.0088 0.165 Uiso 1 1 calc R . .
C5 C 0.3293(7) 0.9524(9) -0.1553(10) 0.128(5) Uani 1 1 d U . .
H5 H 0.2960 0.9761 -0.1864 0.153 Uiso 1 1 calc R . .
C6 C 0.3505(4) 0.8793(7) -0.1713(6) 0.080(3) Uani 1 1 d . . .
H6 H 0.3300 0.8505 -0.2127 0.097 Uiso 1 1 calc R . .
C7 C 0.4230(3) 0.7606(5) -0.1522(4) 0.0569(18) Uani 1 1 d . . .
C8 C 0.5024(4) 0.6573(4) -0.1304(3) 0.0439(12) Uani 1 1 d . . .
H8 H 0.4652 0.6191 -0.1230 0.053 Uiso 1 1 calc R . .
C9 C 0.5290(3) 0.6501(4) -0.2169(3) 0.0404(14) Uani 1 1 d . . .
C10 C 0.7286(3) 0.7213(5) -0.0790(4) 0.0544(17) Uani 1 1 d . . .
C11 C 0.7892(4) 0.7043(6) -0.0458(6) 0.083(3) Uani 1 1 d . . .
H11 H 0.7943 0.6624 -0.0084 0.100 Uiso 1 1 calc R . .
C12 C 0.8446(4) 0.7533(7) -0.0708(8) 0.099(3) Uani 1 1 d . . .
H12 H 0.8867 0.7421 -0.0502 0.119 Uiso 1 1 calc R . .
C13 C 0.8371(5) 0.8141(7) -0.1226(8) 0.105(4) Uani 1 1 d . . .
H13 H 0.8740 0.8440 -0.1394 0.126 Uiso 1 1 calc R . .
C14 C 0.7758(5) 0.8330(6) -0.1513(7) 0.093(3) Uani 1 1 d . . .
H14 H 0.7700 0.8783 -0.1845 0.111 Uiso 1 1 calc R . .
C15 C 0.7206(4) 0.7837(5) -0.1304(5) 0.069(2) Uani 1 1 d . . .
H15 H 0.6789 0.7946 -0.1523 0.082 Uiso 1 1 calc R . .
C16 C 0.6716(3) 0.6666(4) -0.0545(4) 0.0482(15) Uani 1 1 d . . .
C17 C 0.5577(3) 0.6374(4) -0.0700(4) 0.0432(14) Uani 1 1 d . . .
H17 H 0.5716 0.5804 -0.0778 0.052 Uiso 1 1 calc R . .
C18 C 0.5328(3) 0.6478(5) 0.0172(4) 0.0460(15) Uani 1 1 d . . .
C19 C 0.3028(3) 0.7754(5) 0.3858(4) 0.0555(17) Uani 1 1 d . . .
C20 C 0.3097(5) 0.8541(5) 0.4069(6) 0.074(2) Uani 1 1 d . . .
H20 H 0.3479 0.8705 0.4341 0.088 Uiso 1 1 calc R . .
C21 C 0.2618(6) 0.9110(6) 0.3895(6) 0.087(3) Uani 1 1 d . . .
H21 H 0.2691 0.9656 0.4028 0.104 Uiso 1 1 calc R . .
C22 C 0.2039(6) 0.8893(8) 0.3533(8) 0.103(4) Uani 1 1 d . . .
H22 H 0.1713 0.9281 0.3418 0.124 Uiso 1 1 calc R . .
C23 C 0.1947(5) 0.8082(8) 0.3339(8) 0.097(3) Uani 1 1 d . . .
H23 H 0.1549 0.7918 0.3103 0.117 Uiso 1 1 calc R . .
C24 C 0.2426(4) 0.7515(6) 0.3484(6) 0.074(2) Uani 1 1 d . . .
H24 H 0.2359 0.6971 0.3339 0.089 Uiso 1 1 calc R . .
C25 C 0.3555(3) 0.7147(4) 0.4045(4) 0.0504(15) Uani 1 1 d . . .
C26 C 0.3808(3) 0.5741(4) 0.4231(3) 0.0387(13) Uani 1 1 d . . .
H26 H 0.4257 0.5893 0.4054 0.046 Uiso 1 1 calc R . .
C27 C 0.3823(3) 0.5657(4) 0.5144(4) 0.0425(14) Uani 1 1 d . . .
C28 C 0.2007(4) 0.3924(5) 0.3902(4) 0.0561(17) Uani 1 1 d . . .
C29 C 0.1607(4) 0.4597(6) 0.3924(8) 0.093(3) Uani 1 1 d . . .
H29 H 0.1793 0.5117 0.3956 0.111 Uiso 1 1 calc R . .
C30 C 0.0911(6) 0.4503(8) 0.3899(9) 0.125(4) Uani 1 1 d U . .
H30 H 0.0634 0.4959 0.3904 0.150 Uiso 1 1 calc R . .
C31 C 0.0640(6) 0.3710(9) 0.3865(10) 0.127(4) Uani 1 1 d U . .
H31 H 0.0181 0.3644 0.3843 0.153 Uiso 1 1 calc R . .
C32 C 0.1037(5) 0.3041(7) 0.3866(7) 0.092(3) Uani 1 1 d . . .
H32 H 0.0856 0.2517 0.3852 0.111 Uiso 1 1 calc R . .
C33 C 0.1720(4) 0.3158(6) 0.3888(5) 0.072(2) Uani 1 1 d . . .
H33 H 0.1996 0.2701 0.3894 0.087 Uiso 1 1 calc R . .
C34 C 0.2740(3) 0.4001(5) 0.3908(4) 0.0520(16) Uani 1 1 d . . .
C35 C 0.3622(2) 0.4971(5) 0.3811(3) 0.0395(11) Uani 1 1 d . . .
H35 H 0.3907 0.4532 0.4016 0.047 Uiso 1 1 calc R . .
C36 C 0.3704(2) 0.5002(5) 0.2882(3) 0.0414(12) Uani 1 1 d . . .
C37 C 0.5229(6) 0.6777(7) 0.2738(5) 0.091(3) Uani 1 1 d . . .
H37A H 0.4869 0.6600 0.3076 0.137 Uiso 1 1 calc R . .
H37B H 0.5213 0.7362 0.2680 0.137 Uiso 1 1 calc R . .
H37C H 0.5646 0.6622 0.2976 0.137 Uiso 1 1 calc R . .
C38 C 0.5477(4) 0.6737(5) 0.5263(4) 0.063(2) Uani 1 1 d . . .
H38A H 0.5954 0.6762 0.5248 0.094 Uiso 1 1 calc R . .
H38B H 0.5298 0.7280 0.5221 0.094 Uiso 1 1 calc R . .
H38C H 0.5318 0.6410 0.4823 0.094 Uiso 1 1 calc R . .
C39 C 0.7395(13) 0.909(2) 0.0861(14) 0.283(14) Uani 1 1 d DU . .
C40 C 0.8103(13) 0.9316(16) 0.1004(17) 0.236(11) Uani 1 1 d DU . .
C41 C 0.7166(18) 0.966(2) 0.206(3) 0.320(18) Uani 1 1 d DU . .
C42 C 0.6761(15) 1.0429(19) 0.193(2) 0.250(12) Uani 1 1 d DU . .
C43 C 0.7173(15) 0.8166(16) 0.1981(19) 0.254(12) Uani 1 1 d DU . .
C44 C 0.6984(10) 0.7369(13) 0.1616(13) 0.170(7) Uani 1 1 d D . .
Eu1 Eu 0.5000 0.5000 0.153596(19) 0.03644(12) Uani 1 2 d S . .
Eu2 Eu 0.5000 0.5000 0.648816(19) 0.03667(12) Uani 1 2 d S . .
O1 O 0.48070(19) 0.7387(3) -0.1132(3) 0.0502(11) Uani 1 1 d . . .
O2 O 0.3920(2) 0.7150(3) -0.1918(3) 0.0645(14) Uani 1 1 d . . .
O3 O 0.5355(2) 0.7129(3) -0.2574(3) 0.0574(12) Uani 1 1 d . . .
O4 O 0.5402(2) 0.5775(3) -0.2402(2) 0.0515(11) Uani 1 1 d . . .
O5 O 0.6776(2) 0.6066(3) -0.0126(3) 0.0661(14) Uani 1 1 d . . .
O6 O 0.6138(2) 0.6907(3) -0.0873(2) 0.0472(10) Uani 1 1 d . . .
O7 O 0.5507(3) 0.7089(3) 0.0576(3) 0.0604(12) Uani 1 1 d . . .
O8 O 0.4932(2) 0.5914(3) 0.0403(2) 0.0484(10) Uani 1 1 d . . .
O9 O 0.4114(2) 0.7326(3) 0.4239(3) 0.0663(14) Uani 1 1 d . . .
O10 O 0.3355(2) 0.6369(3) 0.3960(3) 0.0458(10) Uani 1 1 d . . .
O11 O 0.3423(2) 0.6060(3) 0.5566(3) 0.0565(12) Uani 1 1 d . . .
O12 O 0.42517(19) 0.5170(3) 0.5400(2) 0.0491(11) Uani 1 1 d . . .
O13 O 0.3119(3) 0.3436(3) 0.3809(4) 0.0774(17) Uani 1 1 d . . .
O14 O 0.29400(19) 0.4779(3) 0.4022(2) 0.0442(10) Uani 1 1 d . . .
O15 O 0.32201(19) 0.4848(4) 0.2462(3) 0.0607(14) Uani 1 1 d . . .
O16 O 0.42783(19) 0.5204(3) 0.2661(2) 0.0481(12) Uani 1 1 d . . .
O17 O 0.38582(19) 0.4846(3) 0.1086(2) 0.0497(11) Uani 1 1 d . . .
H103 H 0.3655 0.5067 0.1478 0.075 Uiso 1 1 d R . .
H104 H 0.3579 0.4671 0.0742 0.075 Uiso 1 1 d R . .
O18 O 0.5169(2) 0.6410(3) 0.1980(3) 0.0598(14) Uani 1 1 d . . .
H101 H 0.5086 0.6764 0.1619 0.090 Uiso 1 1 d R . .
O19 O 0.4015(2) 0.5779(3) 0.6971(2) 0.0499(10) Uani 1 1 d . . .
H105 H 0.3844 0.5912 0.6522 0.075 Uiso 1 1 d R . .
H106 H 0.4072 0.6206 0.7253 0.075 Uiso 1 1 d R . .
O20 O 0.5264(2) 0.6371(3) 0.6019(3) 0.0532(11) Uani 1 1 d . . .
H102 H 0.5336 0.6670 0.6429 0.080 Uiso 1 1 d R . .
O22 O 0.6938(9) 0.8484(10) 0.4394(12) 0.261(9) Uani 1 1 d . . .
O21 O 0.5669(8) 0.8706(11) 0.1080(12) 0.250(7) Uani 1 1 d U . .


_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
N1 C41 1.44(4) . ?
N1 C43 1.48(3) . ?
N1 C39 1.497(10) . ?
C1 C6 1.382(12) . ?
C1 C2 1.391(13) . ?
C1 C7 1.437(12) . ?
C2 C3 1.402(15) . ?
C2 H2 0.9300 . ?
C4 C5 1.299(18) . ?
C4 C3 1.401(18) . ?
C4 H4 0.9300 . ?
C3 H3 0.9300 . ?
C5 C6 1.295(16) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 O2 1.172(9) . ?
C7 O1 1.374(8) . ?
C8 O1 1.428(7) . ?
C8 C17 1.532(9) . ?
C8 C9 1.539(8) . ?
C8 H8 0.9800 . ?
C9 O3 1.234(8) . ?
C9 O4 1.266(8) . ?
C10 C15 1.341(11) . ?
C10 C11 1.364(11) . ?
C10 C16 1.508(9) . ?
C11 C12 1.432(13) . ?
C11 H11 0.9300 . ?
C12 C13 1.323(15) . ?
C12 H12 0.9300 . ?
C13 C14 1.356(15) . ?
C13 H13 0.9300 . ?
C14 C15 1.411(11) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 O5 1.209(8) . ?
C16 O6 1.340(8) . ?
C17 O6 1.452(7) . ?
C17 C18 1.544(9) . ?
C17 H17 0.9800 . ?
C18 O7 1.256(8) . ?
C18 O8 1.277(8) . ?
C19 C20 1.339(11) . ?
C19 C24 1.413(11) . ?
C19 C25 1.483(10) . ?
C20 C21 1.367(12) . ?
C20 H20 0.9300 . ?
C21 C22 1.357(15) . ?
C21 H21 0.9300 . ?
C22 C23 1.375(16) . ?
C22 H22 0.9300 . ?
C23 C24 1.356(13) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 O9 1.203(8) . ?
C25 O10 1.340(8) . ?
C26 O10 1.443(7) . ?
C26 C35 1.485(9) . ?
C26 C27 1.524(8) . ?
C26 H26 0.9800 . ?
C27 O12 1.247(7) . ?
C27 O11 1.252(7) . ?
C28 C29 1.362(12) . ?
C28 C33 1.377(11) . ?
C28 C34 1.476(10) . ?
C29 C30 1.404(13) . ?
C29 H29 0.9300 . ?
C30 C31 1.406(16) . ?
C30 H30 0.9300 . ?
C31 C32 1.351(16) . ?
C31 H31 0.9300 . ?
C32 C33 1.385(12) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
C34 O13 1.207(9) . ?
C34 O14 1.345(8) . ?
C35 O14 1.448(6) . ?
C35 C36 1.554(7) . ?
C35 H35 0.9800 . ?
C36 O15 1.223(7) . ?
C36 O16 1.254(7) . ?
C37 O18 1.400(10) . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 O20 1.455(8) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 C40 1.485(10) . ?
C41 C42 1.514(10) . ?
C43 C44 1.485(10) . ?
Eu1 O16 2.390(4) 2_665 ?
Eu1 O16 2.390(4) . ?
Eu1 O8 2.407(4) 2_665 ?
Eu1 O8 2.407(4) . ?
Eu1 O17 2.424(4) . ?
Eu1 O17 2.424(4) 2_665 ?
Eu1 O18 2.442(5) . ?
Eu1 O18 2.442(5) 2_665 ?
Eu1 H103 2.7040 . ?
Eu2 O12 2.368(4) 2_665 ?
Eu2 O12 2.368(4) . ?
Eu2 O4 2.379(4) 1_556 ?
Eu2 O4 2.379(4) 2_666 ?
Eu2 O20 2.430(5) 2_665 ?
Eu2 O20 2.430(5) . ?
Eu2 O19 2.484(4) 2_665 ?
Eu2 O19 2.484(4) . ?
Eu2 H105 2.7581 . ?
Eu2 H102 2.8105 . ?
O4 Eu2 2.379(4) 1_554 ?
O17 H103 0.8500 . ?
O17 H104 0.8501 . ?
O18 H101 0.8499 . ?
O19 H105 0.8500 . ?
O19 H106 0.8499 . ?
O20 H102 0.8501 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C41 N1 C43 113(2) . . ?
C41 N1 C39 99(2) . . ?
C43 N1 C39 110(2) . . ?
C6 C1 C2 117.5(10) . . ?
C6 C1 C7 120.2(8) . . ?
C2 C1 C7 122.2(8) . . ?
C1 C2 C3 119.4(11) . . ?
C1 C2 H2 120.3 . . ?
C3 C2 H2 120.3 . . ?
C5 C4 C3 124.1(14) . . ?
C5 C4 H4 117.9 . . ?
C3 C4 H4 117.9 . . ?
C4 C3 C2 115.8(13) . . ?
C4 C3 H3 122.1 . . ?
C2 C3 H3 122.1 . . ?
C6 C5 C4 119.2(14) . . ?
C6 C5 H5 120.4 . . ?
C4 C5 H5 120.4 . . ?
C5 C6 C1 123.7(11) . . ?
C5 C6 H6 118.2 . . ?
C1 C6 H6 118.2 . . ?
O2 C7 O1 123.2(7) . . ?
O2 C7 C1 124.9(7) . . ?
O1 C7 C1 111.5(7) . . ?
O1 C8 C17 106.7(5) . . ?
O1 C8 C9 111.4(5) . . ?
C17 C8 C9 110.2(5) . . ?
O1 C8 H8 109.5 . . ?
C17 C8 H8 109.5 . . ?
C9 C8 H8 109.5 . . ?
O3 C9 O4 126.3(6) . . ?
O3 C9 C8 118.9(6) . . ?
O4 C9 C8 114.7(5) . . ?
C15 C10 C11 121.3(7) . . ?
C15 C10 C16 122.2(6) . . ?
C11 C10 C16 116.6(7) . . ?
C10 C11 C12 117.5(9) . . ?
C10 C11 H11 121.3 . . ?
C12 C11 H11 121.3 . . ?
C13 C12 C11 121.3(8) . . ?
C13 C12 H12 119.3 . . ?
C11 C12 H12 119.3 . . ?
C12 C13 C14 120.2(8) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C13 C14 C15 119.7(10) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
C10 C15 C14 119.8(8) . . ?
C10 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
O5 C16 O6 124.0(6) . . ?
O5 C16 C10 124.0(6) . . ?
O6 C16 C10 111.9(6) . . ?
O6 C17 C8 107.8(5) . . ?
O6 C17 C18 111.8(5) . . ?
C8 C17 C18 111.0(5) . . ?
O6 C17 H17 108.8 . . ?
C8 C17 H17 108.8 . . ?
C18 C17 H17 108.8 . . ?
O7 C18 O8 126.2(6) . . ?
O7 C18 C17 119.9(6) . . ?
O8 C18 C17 113.9(6) . . ?
C20 C19 C24 118.0(8) . . ?
C20 C19 C25 120.9(7) . . ?
C24 C19 C25 121.1(7) . . ?
C19 C20 C21 121.6(9) . . ?
C19 C20 H20 119.2 . . ?
C21 C20 H20 119.2 . . ?
C22 C21 C20 121.2(10) . . ?
C22 C21 H21 119.4 . . ?
C20 C21 H21 119.4 . . ?
C21 C22 C23 118.0(10) . . ?
C21 C22 H22 121.0 . . ?
C23 C22 H22 121.0 . . ?
C24 C23 C22 121.4(10) . . ?
C24 C23 H23 119.3 . . ?
C22 C23 H23 119.3 . . ?
C23 C24 C19 119.7(10) . . ?
C23 C24 H24 120.1 . . ?
C19 C24 H24 120.1 . . ?
O9 C25 O10 122.5(6) . . ?
O9 C25 C19 124.0(7) . . ?
O10 C25 C19 113.5(6) . . ?
O10 C26 C35 107.2(4) . . ?
O10 C26 C27 112.7(5) . . ?
C35 C26 C27 113.4(5) . . ?
O10 C26 H26 107.7 . . ?
C35 C26 H26 107.7 . . ?
C27 C26 H26 107.7 . . ?
O12 C27 O11 125.8(5) . . ?
O12 C27 C26 114.3(5) . . ?
O11 C27 C26 119.9(5) . . ?
C29 C28 C33 119.0(7) . . ?
C29 C28 C34 121.3(7) . . ?
C33 C28 C34 119.7(8) . . ?
C28 C29 C30 119.9(9) . . ?
C28 C29 H29 120.1 . . ?
C30 C29 H29 120.1 . . ?
C29 C30 C31 119.1(12) . . ?
C29 C30 H30 120.5 . . ?
C31 C30 H30 120.5 . . ?
C32 C31 C30 121.1(10) . . ?
C32 C31 H31 119.4 . . ?
C30 C31 H31 119.4 . . ?
C31 C32 C33 118.1(9) . . ?
C31 C32 H32 120.9 . . ?
C33 C32 H32 120.9 . . ?
C28 C33 C32 122.7(10) . . ?
C28 C33 H33 118.6 . . ?
C32 C33 H33 118.6 . . ?
O13 C34 O14 123.6(6) . . ?
O13 C34 C28 124.2(7) . . ?
O14 C34 C28 112.2(6) . . ?
O14 C35 C26 107.9(5) . . ?
O14 C35 C36 110.4(4) . . ?
C26 C35 C36 114.4(6) . . ?
O14 C35 H35 108.0 . . ?
C26 C35 H35 108.0 . . ?
C36 C35 H35 108.0 . . ?
O15 C36 O16 128.1(5) . . ?
O15 C36 C35 118.5(5) . . ?
O16 C36 C35 113.4(4) . . ?
O18 C37 H37A 109.5 . . ?
O18 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
O18 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O20 C38 H38A 109.5 . . ?
O20 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
O20 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C40 C39 N1 116(2) . . ?
N1 C41 C42 118(3) . . ?
N1 C43 C44 121(2) . . ?
O16 Eu1 O16 76.91(19) 2_665 . ?
O16 Eu1 O8 119.47(16) 2_665 2_665 ?
O16 Eu1 O8 137.19(14) . 2_665 ?
O16 Eu1 O8 137.19(14) 2_665 . ?
O16 Eu1 O8 119.47(16) . . ?
O8 Eu1 O8 77.0(2) 2_665 . ?
O16 Eu1 O17 143.18(13) 2_665 . ?
O16 Eu1 O17 71.54(13) . . ?
O8 Eu1 O17 75.39(14) 2_665 . ?
O8 Eu1 O17 76.63(14) . . ?
O16 Eu1 O17 71.54(13) 2_665 2_665 ?
O16 Eu1 O17 143.18(13) . 2_665 ?
O8 Eu1 O17 76.63(14) 2_665 2_665 ?
O8 Eu1 O17 75.39(14) . 2_665 ?
O17 Eu1 O17 144.01(19) . 2_665 ?
O16 Eu1 O18 79.06(16) 2_665 . ?
O16 Eu1 O18 73.50(15) . . ?
O8 Eu1 O18 144.43(14) 2_665 . ?
O8 Eu1 O18 70.12(14) . . ?
O17 Eu1 O18 108.81(16) . . ?
O17 Eu1 O18 82.21(16) 2_665 . ?
O16 Eu1 O18 73.50(15) 2_665 2_665 ?
O16 Eu1 O18 79.06(16) . 2_665 ?
O8 Eu1 O18 70.12(14) 2_665 2_665 ?
O8 Eu1 O18 144.43(14) . 2_665 ?
O17 Eu1 O18 82.21(16) . 2_665 ?
O17 Eu1 O18 108.81(16) 2_665 2_665 ?
O18 Eu1 O18 144.8(2) . 2_665 ?
O16 Eu1 H103 129.7 2_665 . ?
O16 Eu1 H103 54.3 . . ?
O8 Eu1 H103 93.1 2_665 . ?
O8 Eu1 H103 83.7 . . ?
O17 Eu1 H103 18.0 . . ?
O17 Eu1 H103 158.2 2_665 . ?
O18 Eu1 H103 96.4 . . ?
O18 Eu1 H103 84.9 2_665 . ?
O12 Eu2 O12 80.3(2) 2_665 . ?
O12 Eu2 O4 116.14(15) 2_665 1_556 ?
O12 Eu2 O4 138.21(15) . 1_556 ?
O12 Eu2 O4 138.21(15) 2_665 2_666 ?
O12 Eu2 O4 116.14(15) . 2_666 ?
O4 Eu2 O4 78.2(2) 1_556 2_666 ?
O12 Eu2 O20 77.60(16) 2_665 2_665 ?
O12 Eu2 O20 73.99(15) . 2_665 ?
O4 Eu2 O20 144.42(15) 1_556 2_665 ?
O4 Eu2 O20 71.63(16) 2_666 2_665 ?
O12 Eu2 O20 73.99(15) 2_665 . ?
O12 Eu2 O20 77.60(16) . . ?
O4 Eu2 O20 71.63(16) 1_556 . ?
O4 Eu2 O20 144.42(15) 2_666 . ?
O20 Eu2 O20 142.6(2) 2_665 . ?
O12 Eu2 O19 71.45(14) 2_665 2_665 ?
O12 Eu2 O19 144.27(14) . 2_665 ?
O4 Eu2 O19 75.63(15) 1_556 2_665 ?
O4 Eu2 O19 75.34(15) 2_666 2_665 ?
O20 Eu2 O19 78.81(15) 2_665 2_665 ?
O20 Eu2 O19 113.67(16) . 2_665 ?
O12 Eu2 O19 144.27(14) 2_665 . ?
O12 Eu2 O19 71.45(14) . . ?
O4 Eu2 O19 75.34(15) 1_556 . ?
O4 Eu2 O19 75.63(15) 2_666 . ?
O20 Eu2 O19 113.67(16) 2_665 . ?
O20 Eu2 O19 78.81(15) . . ?
O19 Eu2 O19 142.31(19) 2_665 . ?
O12 Eu2 H105 127.8 2_665 . ?
O12 Eu2 H105 54.4 . . ?
O4 Eu2 H105 89.0 1_556 . ?
O4 Eu2 H105 89.2 2_666 . ?
O20 Eu2 H105 108.7 2_665 . ?
O20 Eu2 H105 72.1 . . ?
O19 Eu2 H105 160.0 2_665 . ?
O19 Eu2 H105 17.7 . . ?
O12 Eu2 H102 86.3 2_665 . ?
O12 Eu2 H102 90.7 . . ?
O4 Eu2 H102 55.2 1_556 . ?
O4 Eu2 H102 128.6 2_666 . ?
O20 Eu2 H102 159.3 2_665 . ?
O20 Eu2 H102 16.7 . . ?
O19 Eu2 H102 108.5 2_665 . ?
O19 Eu2 H102 72.9 . . ?
H105 Eu2 H102 71.2 . . ?
C7 O1 C8 113.9(5) . . ?
C9 O4 Eu2 132.5(4) . 1_554 ?
C16 O6 C17 114.5(5) . . ?
C18 O8 Eu1 130.4(4) . . ?
C25 O10 C26 116.9(5) . . ?
C27 O12 Eu2 140.7(4) . . ?
C34 O14 C35 116.9(5) . . ?
C36 O16 Eu1 138.6(4) . . ?
Eu1 O17 H103 99.9 . . ?
Eu1 O17 H104 150.0 . . ?
H103 O17 H104 110.0 . . ?
C37 O18 Eu1 133.4(5) . . ?
C37 O18 H101 111.2 . . ?
Eu1 O18 H101 113.6 . . ?
Eu2 O19 H105 99.7 . . ?
Eu2 O19 H106 119.4 . . ?
H105 O19 H106 109.3 . . ?
C38 O20 Eu2 136.0(4) . . ?
C38 O20 H102 114.1 . . ?
Eu2 O20 H102 107.9 . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.253
_refine_diff_density_min         -1.158
_refine_diff_density_rms         0.099
####################################################################### 
# 
# 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 1526606'
_audit_update_record             
;
2017-01-10 deposited with the CCDC.
2017-04-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_absolute_configuration rm
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H36 O20 Sm, C6 H16 N, 2(H2 O)'
_chemical_formula_sum            'C44 H56 N O22 Sm'
_chemical_formula_weight         1101.25

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'

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

_cell_length_a                   20.118(4)
_cell_length_b                   16.652(3)
_cell_length_c                   16.747(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5610.1(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    37934
_cell_measurement_theta_min      3.04
_cell_measurement_theta_max      27.58

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2260
_exptl_absorpt_coefficient_mu    1.118
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7289
_exptl_absorpt_correction_T_max  0.7667
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            50255
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_av_sigmaI/netI    0.0617
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.17
_diffrn_reflns_theta_max         27.48
_reflns_number_total             12840
_reflns_number_gt                8695
_reflns_threshold_expression     >2sigma(I)

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

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

_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)+(0.1161P)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_abs_structure_details 
'Flack H D (1983), Acta Cryst. A39, 876-881, Friedel pairs 5782'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_number_reflns         12840
_refine_ls_number_parameters     616
_refine_ls_number_restraints     73
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0585
_refine_ls_wR_factor_ref         0.1944
_refine_ls_wR_factor_gt          0.1770
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.6956(10) 0.8986(10) 0.1600(10) 0.166(7) Uani 1 1 d D . .
C1 C 0.3991(4) 0.8318(6) -0.1352(5) 0.053(2) Uani 1 1 d . . .
C2 C 0.4288(5) 0.8786(5) -0.0748(6) 0.065(2) Uani 1 1 d . . .
H2 H 0.4657 0.8594 -0.0473 0.078 Uiso 1 1 calc R . .
C4 C 0.3497(6) 0.9847(7) -0.0967(7) 0.087(3) Uani 1 1 d U . .
H4 H 0.3339 1.0358 -0.0850 0.104 Uiso 1 1 calc R . .
C3 C 0.4023(5) 0.9543(6) -0.0565(7) 0.078(3) Uani 1 1 d . . .
H3 H 0.4214 0.9844 -0.0157 0.094 Uiso 1 1 calc R . .
C5 C 0.3200(6) 0.9391(8) -0.1551(7) 0.085(3) Uani 1 1 d U . .
H5 H 0.2833 0.9591 -0.1824 0.102 Uiso 1 1 calc R . .
C6 C 0.3440(4) 0.8647(6) -0.1731(5) 0.064(2) Uani 1 1 d . . .
H6 H 0.3227 0.8348 -0.2123 0.077 Uiso 1 1 calc R . .
C7 C 0.4209(4) 0.7537(5) -0.1543(4) 0.0454(17) Uani 1 1 d . . .
C8 C 0.5037(4) 0.6518(4) -0.1346(3) 0.0363(13) Uani 1 1 d . . .
H8 H 0.4673 0.6132 -0.1278 0.044 Uiso 1 1 calc R . .
C9 C 0.5286(3) 0.6477(5) -0.2209(4) 0.0361(15) Uani 1 1 d . . .
C10 C 0.7274(4) 0.7200(5) -0.0794(5) 0.0513(19) Uani 1 1 d . . .
C11 C 0.7887(4) 0.7038(6) -0.0494(7) 0.074(3) Uani 1 1 d . . .
H11 H 0.7940 0.6605 -0.0149 0.089 Uiso 1 1 calc R . .
C12 C 0.8443(5) 0.7507(8) -0.0693(8) 0.091(4) Uani 1 1 d . . .
H12 H 0.8863 0.7374 -0.0503 0.109 Uiso 1 1 calc R . .
C13 C 0.8358(5) 0.8143(9) -0.1155(10) 0.107(5) Uani 1 1 d . . .
H13 H 0.8715 0.8488 -0.1238 0.129 Uiso 1 1 calc R . .
C14 C 0.7715(6) 0.8323(8) -0.1544(9) 0.101(4) Uani 1 1 d . . .
H14 H 0.7672 0.8735 -0.1916 0.121 Uiso 1 1 calc R . .
C15 C 0.7184(5) 0.7853(6) -0.1328(6) 0.069(3) Uani 1 1 d . . .
H15 H 0.6764 0.7962 -0.1533 0.083 Uiso 1 1 calc R . .
C16 C 0.6709(4) 0.6660(5) -0.0606(5) 0.0488(18) Uani 1 1 d . . .
C17 C 0.5574(3) 0.6334(4) -0.0747(4) 0.0366(14) Uani 1 1 d . . .
H17 H 0.5716 0.5776 -0.0820 0.044 Uiso 1 1 calc R . .
C18 C 0.5334(3) 0.6444(5) 0.0125(4) 0.0394(16) Uani 1 1 d . . .
C19 C 0.3012(4) 0.7688(5) 0.3842(4) 0.0511(19) Uani 1 1 d . . .
C20 C 0.3107(5) 0.8466(6) 0.4085(6) 0.071(3) Uani 1 1 d . . .
H20 H 0.3499 0.8620 0.4337 0.085 Uiso 1 1 calc R . .
C21 C 0.2600(7) 0.9023(7) 0.3943(8) 0.098(4) Uani 1 1 d . . .
H21 H 0.2658 0.9550 0.4113 0.118 Uiso 1 1 calc R . .
C22 C 0.2047(7) 0.8828(9) 0.3581(8) 0.096(4) Uani 1 1 d . . .
H22 H 0.1722 0.9214 0.3488 0.115 Uiso 1 1 calc R . .
C23 C 0.1952(6) 0.8066(9) 0.3346(9) 0.103(4) Uani 1 1 d . . .
H23 H 0.1556 0.7922 0.3099 0.124 Uiso 1 1 calc R . .
C24 C 0.2443(5) 0.7486(7) 0.3470(7) 0.077(3) Uani 1 1 d . . .
H24 H 0.2378 0.6962 0.3295 0.093 Uiso 1 1 calc R . .
C25 C 0.3563(4) 0.7101(5) 0.4013(4) 0.0480(17) Uani 1 1 d . . .
C26 C 0.3816(3) 0.5717(4) 0.4184(4) 0.0370(15) Uani 1 1 d . . .
H26 H 0.4265 0.5877 0.4020 0.044 Uiso 1 1 calc R . .
C27 C 0.3809(4) 0.5633(5) 0.5092(4) 0.0422(16) Uani 1 1 d . . .
C28 C 0.2046(5) 0.3881(5) 0.3917(5) 0.061(2) Uani 1 1 d D . .
C29 C 0.1642(5) 0.4534(7) 0.4002(7) 0.084(3) Uani 1 1 d . . .
H29 H 0.1822 0.5048 0.4027 0.100 Uiso 1 1 calc R . .
C30 C 0.0938(7) 0.4420(8) 0.4050(8) 0.108(4) Uani 1 1 d DU . .
H30 H 0.0648 0.4850 0.4116 0.130 Uiso 1 1 calc R . .
C31 C 0.0701(7) 0.3616(8) 0.3994(9) 0.109(4) Uani 1 1 d DU . .
H31 H 0.0244 0.3528 0.4009 0.131 Uiso 1 1 calc R . .
C32 C 0.1114(7) 0.2965(8) 0.3920(7) 0.095(4) Uani 1 1 d . . .
H32 H 0.0948 0.2444 0.3896 0.114 Uiso 1 1 calc R . .
C33 C 0.1775(5) 0.3115(6) 0.3882(6) 0.071(3) Uani 1 1 d D . .
H33 H 0.2064 0.2681 0.3830 0.085 Uiso 1 1 calc R . .
C34 C 0.2777(4) 0.3977(5) 0.3867(5) 0.0533(19) Uani 1 1 d . . .
C35 C 0.3644(3) 0.4938(5) 0.3765(3) 0.0381(14) Uani 1 1 d . . .
H35 H 0.3936 0.4509 0.3959 0.046 Uiso 1 1 calc R . .
C36 C 0.3711(3) 0.5009(5) 0.2849(3) 0.0370(12) Uani 1 1 d . . .
C37 C 0.5213(8) 0.6756(9) 0.2685(7) 0.111(5) Uani 1 1 d . . .
H37A H 0.5016 0.6413 0.3080 0.167 Uiso 1 1 calc R . .
H37B H 0.4981 0.7260 0.2673 0.167 Uiso 1 1 calc R . .
H37C H 0.5672 0.6848 0.2818 0.167 Uiso 1 1 calc R . .
C38 C 0.5471(6) 0.6691(6) 0.5239(5) 0.069(3) Uani 1 1 d . . .
H38A H 0.5947 0.6721 0.5231 0.103 Uiso 1 1 calc R . .
H38B H 0.5288 0.7220 0.5174 0.103 Uiso 1 1 calc R . .
H38C H 0.5320 0.6353 0.4812 0.103 Uiso 1 1 calc R . .
C39 C 0.7294(10) 0.9086(17) 0.0812(12) 0.206(10) Uani 1 1 d DU . .
H39A H 0.7196 0.8615 0.0493 0.247 Uiso 1 1 calc R . .
H39B H 0.7092 0.9542 0.0545 0.247 Uiso 1 1 calc R . .
C40 C 0.8024(10) 0.9207(15) 0.0798(14) 0.196(9) Uani 1 1 d DU . .
H40A H 0.8151 0.9650 0.1132 0.295 Uiso 1 1 d R . .
H40B H 0.8166 0.9308 0.0260 0.295 Uiso 1 1 d R . .
H40C H 0.8229 0.8724 0.0990 0.295 Uiso 1 1 d R . .
C41 C 0.7083(18) 0.9653(15) 0.2182(18) 0.288(17) Uani 1 1 d DU . .
H41A H 0.7556 0.9714 0.2279 0.346 Uiso 1 1 calc R . .
H41B H 0.6862 0.9548 0.2686 0.346 Uiso 1 1 calc R . .
C42 C 0.6803(16) 1.0400(18) 0.179(2) 0.273(16) Uani 1 1 d DU . .
H42A H 0.6328 1.0437 0.1843 0.410 Uiso 1 1 d R . .
H42B H 0.6922 1.0393 0.1238 0.410 Uiso 1 1 d R . .
H42C H 0.7005 1.0855 0.2048 0.410 Uiso 1 1 d R . .
C43 C 0.7123(13) 0.8309(14) 0.1980(16) 0.192(9) Uani 1 1 d DU . .
H43A H 0.6922 0.8330 0.2506 0.231 Uiso 1 1 calc R . .
H43B H 0.7601 0.8321 0.2058 0.231 Uiso 1 1 calc R . .
C44 C 0.6957(11) 0.7520(15) 0.1631(15) 0.196(11) Uani 1 1 d D . .
H44A H 0.6484 0.7509 0.1551 0.294 Uiso 1 1 d R . .
H44B H 0.7083 0.7096 0.1988 0.294 Uiso 1 1 d R . .
H44C H 0.7177 0.7449 0.1127 0.294 Uiso 1 1 d R . .
Sm1 Sm 0.5000 0.5000 0.14861(2) 0.03271(13) Uani 1 2 d S . .
Sm2 Sm 0.5000 0.5000 0.64360(2) 0.03330(13) Uani 1 2 d S . .
O1 O 0.4791(2) 0.7318(3) -0.1171(3) 0.0412(11) Uani 1 1 d . . .
O2 O 0.3926(3) 0.7078(4) -0.1980(3) 0.0625(16) Uani 1 1 d . . .
O3 O 0.5358(3) 0.7097(3) -0.2605(3) 0.0519(13) Uani 1 1 d . . .
O4 O 0.5404(3) 0.5763(3) -0.2452(3) 0.0463(12) Uani 1 1 d . . .
O5 O 0.6769(3) 0.6060(4) -0.0164(4) 0.0632(16) Uani 1 1 d . . .
O6 O 0.6134(2) 0.6863(3) -0.0927(3) 0.0424(11) Uani 1 1 d . . .
O7 O 0.5497(3) 0.7046(3) 0.0505(3) 0.0525(14) Uani 1 1 d . . .
O8 O 0.4945(3) 0.5896(3) 0.0352(2) 0.0450(11) Uani 1 1 d . . .
O9 O 0.4112(3) 0.7285(4) 0.4201(4) 0.0659(17) Uani 1 1 d . . .
O10 O 0.3354(2) 0.6336(3) 0.3928(3) 0.0449(11) Uani 1 1 d . . .
O11 O 0.3418(3) 0.6023(4) 0.5504(3) 0.0601(15) Uani 1 1 d . . .
O12 O 0.4256(2) 0.5149(3) 0.5348(2) 0.0454(13) Uani 1 1 d . . .
O13 O 0.3167(4) 0.3453(4) 0.3742(5) 0.080(2) Uani 1 1 d . . .
O14 O 0.2965(2) 0.4756(3) 0.3976(3) 0.0447(11) Uani 1 1 d . . .
O15 O 0.3229(2) 0.4847(4) 0.2423(3) 0.0597(16) Uani 1 1 d . . .
O16 O 0.4288(2) 0.5201(3) 0.2616(3) 0.0495(14) Uani 1 1 d . . .
O17 O 0.3850(2) 0.4850(3) 0.1050(3) 0.0498(13) Uani 1 1 d . . .
H103 H 0.3647 0.5071 0.1442 0.075 Uiso 1 1 d R . .
H104 H 0.3571 0.4675 0.0706 0.075 Uiso 1 1 d R . .
O18 O 0.5173(3) 0.6391(3) 0.1937(3) 0.0595(17) Uani 1 1 d . . .
H101 H 0.5090 0.6745 0.1577 0.089 Uiso 1 1 d R . .
O19 O 0.4003(2) 0.5735(3) 0.6913(3) 0.0493(13) Uani 1 1 d . . .
H105 H 0.3832 0.5868 0.6464 0.074 Uiso 1 1 d R . .
H106 H 0.4061 0.6163 0.7195 0.074 Uiso 1 1 d R . .
O20 O 0.5257(3) 0.6364(3) 0.5986(3) 0.0542(14) Uani 1 1 d . . .
H102 H 0.5328 0.6662 0.6396 0.081 Uiso 1 1 d R . .
O22 O 0.5891(5) 0.8538(7) -0.0122(8) 0.148(4) Uani 1 1 d U . .
O21 O 0.5714(6) 0.8629(8) 0.8046(9) 0.170(5) Uani 1 1 d U . .


_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
N1 C43 1.34(3) . ?
N1 C39 1.495(10) . ?
N1 C41 1.499(10) . ?
C1 C6 1.390(11) . ?
C1 C7 1.408(11) . ?
C1 C2 1.409(12) . ?
C2 C3 1.404(12) . ?
C2 H2 0.9300 . ?
C4 C3 1.352(15) . ?
C4 C5 1.375(16) . ?
C4 H4 0.9300 . ?
C3 H3 0.9300 . ?
C5 C6 1.364(14) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 O2 1.202(9) . ?
C7 O1 1.375(8) . ?
C8 O1 1.450(8) . ?
C8 C17 1.506(9) . ?
C8 C9 1.531(8) . ?
C8 H8 0.9800 . ?
C9 O3 1.235(9) . ?
C9 O4 1.279(9) . ?
C10 C11 1.360(11) . ?
C10 C15 1.419(12) . ?
C10 C16 1.482(10) . ?
C11 C12 1.405(13) . ?
C11 H11 0.9300 . ?
C12 C13 1.322(18) . ?
C12 H12 0.9300 . ?
C13 C14 1.479(17) . ?
C13 H13 0.9300 . ?
C14 C15 1.374(13) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 O5 1.251(9) . ?
C16 O6 1.319(8) . ?
C17 O6 1.462(8) . ?
C17 C18 1.549(10) . ?
C17 H17 0.9800 . ?
C18 O7 1.231(9) . ?
C18 O8 1.261(8) . ?
C19 C24 1.345(13) . ?
C19 C20 1.371(13) . ?
C19 C25 1.506(11) . ?
C20 C21 1.398(15) . ?
C20 H20 0.9300 . ?
C21 C22 1.308(17) . ?
C21 H21 0.9300 . ?
C22 C23 1.342(18) . ?
C22 H22 0.9300 . ?
C23 C24 1.397(16) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 O9 1.189(9) . ?
C25 O10 1.350(9) . ?
C26 O10 1.454(8) . ?
C26 C35 1.515(10) . ?
C26 C27 1.526(9) . ?
C26 H26 0.9800 . ?
C27 O11 1.232(8) . ?
C27 O12 1.281(8) . ?
C28 C29 1.365(14) . ?
C28 C33 1.388(8) . ?
C28 C34 1.481(12) . ?
C29 C30 1.432(16) . ?
C29 H29 0.9300 . ?
C30 C31 1.425(9) . ?
C30 H30 0.9300 . ?
C31 C32 1.372(18) . ?
C31 H31 0.9300 . ?
C32 C33 1.356(15) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
C34 O13 1.192(10) . ?
C34 O14 1.364(9) . ?
C35 O14 1.442(8) . ?
C35 C36 1.544(8) . ?
C35 H35 0.9800 . ?
C36 O15 1.234(7) . ?
C36 O16 1.264(7) . ?
C37 O18 1.395(12) . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 O20 1.431(10) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 C40 1.481(10) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 C42 1.512(10) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 C44 1.476(10) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
Sm1 O16 2.397(5) 2_665 ?
Sm1 O16 2.397(5) . ?
Sm1 O8 2.419(4) . ?
Sm1 O8 2.419(4) 2_665 ?
Sm1 O17 2.439(5) . ?
Sm1 O17 2.439(5) 2_665 ?
Sm1 O18 2.460(5) . ?
Sm1 O18 2.460(5) 2_665 ?
Sm2 O12 2.371(4) . ?
Sm2 O12 2.371(4) 2_665 ?
Sm2 O4 2.396(5) 1_556 ?
Sm2 O4 2.396(5) 2_666 ?
Sm2 O20 2.448(5) . ?
Sm2 O20 2.448(5) 2_665 ?
Sm2 O19 2.481(5) . ?
Sm2 O19 2.481(5) 2_665 ?
O4 Sm2 2.396(5) 1_554 ?
O17 H103 0.8570 . ?
O17 H104 0.8556 . ?
O18 H101 0.8607 . ?
O19 H105 0.8560 . ?
O19 H106 0.8632 . ?
O20 H102 0.8596 . ?

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
C43 N1 C39 114(2) . . ?
C43 N1 C41 105.9(19) . . ?
C39 N1 C41 114(2) . . ?
C6 C1 C7 120.6(8) . . ?
C6 C1 C2 116.6(9) . . ?
C7 C1 C2 122.8(8) . . ?
C3 C2 C1 119.5(9) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
C3 C4 C5 119.3(10) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
C4 C3 C2 121.6(10) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C6 C5 C4 120.2(10) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C1 122.7(10) . . ?
C5 C6 H6 118.6 . . ?
C1 C6 H6 118.6 . . ?
O2 C7 O1 120.7(7) . . ?
O2 C7 C1 125.3(7) . . ?
O1 C7 C1 114.0(7) . . ?
O1 C8 C17 107.3(5) . . ?
O1 C8 C9 110.1(5) . . ?
C17 C8 C9 112.6(6) . . ?
O1 C8 H8 108.9 . . ?
C17 C8 H8 108.9 . . ?
C9 C8 H8 108.9 . . ?
O3 C9 O4 125.7(6) . . ?
O3 C9 C8 120.5(6) . . ?
O4 C9 C8 113.8(6) . . ?
C11 C10 C15 120.0(7) . . ?
C11 C10 C16 119.9(8) . . ?
C15 C10 C16 120.0(7) . . ?
C10 C11 C12 121.6(9) . . ?
C10 C11 H11 119.2 . . ?
C12 C11 H11 119.2 . . ?
C13 C12 C11 118.8(10) . . ?
C13 C12 H12 120.6 . . ?
C11 C12 H12 120.6 . . ?
C12 C13 C14 122.3(10) . . ?
C12 C13 H13 118.9 . . ?
C14 C13 H13 118.9 . . ?
C15 C14 C13 116.6(10) . . ?
C15 C14 H14 121.7 . . ?
C13 C14 H14 121.7 . . ?
C14 C15 C10 120.2(9) . . ?
C14 C15 H15 119.9 . . ?
C10 C15 H15 119.9 . . ?
O5 C16 O6 122.1(7) . . ?
O5 C16 C10 122.3(7) . . ?
O6 C16 C10 115.5(7) . . ?
O6 C17 C8 107.1(5) . . ?
O6 C17 C18 111.3(5) . . ?
C8 C17 C18 112.3(5) . . ?
O6 C17 H17 108.7 . . ?
C8 C17 H17 108.7 . . ?
C18 C17 H17 108.7 . . ?
O7 C18 O8 126.7(7) . . ?
O7 C18 C17 120.1(6) . . ?
O8 C18 C17 113.1(6) . . ?
C24 C19 C20 119.5(9) . . ?
C24 C19 C25 123.5(9) . . ?
C20 C19 C25 117.0(8) . . ?
C19 C20 C21 118.3(10) . . ?
C19 C20 H20 120.9 . . ?
C21 C20 H20 120.9 . . ?
C22 C21 C20 122.3(12) . . ?
C22 C21 H21 118.8 . . ?
C20 C21 H21 118.8 . . ?
C21 C22 C23 119.4(12) . . ?
C21 C22 H22 120.3 . . ?
C23 C22 H22 120.3 . . ?
C22 C23 C24 120.7(12) . . ?
C22 C23 H23 119.7 . . ?
C24 C23 H23 119.7 . . ?
C19 C24 C23 119.8(11) . . ?
C19 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
O9 C25 O10 124.2(7) . . ?
O9 C25 C19 124.6(8) . . ?
O10 C25 C19 111.2(7) . . ?
O10 C26 C35 108.9(5) . . ?
O10 C26 C27 110.7(6) . . ?
C35 C26 C27 112.4(6) . . ?
O10 C26 H26 108.3 . . ?
C35 C26 H26 108.3 . . ?
C27 C26 H26 108.3 . . ?
O11 C27 O12 126.3(6) . . ?
O11 C27 C26 121.0(6) . . ?
O12 C27 C26 112.6(6) . . ?
C29 C28 C33 120.2(9) . . ?
C29 C28 C34 120.7(8) . . ?
C33 C28 C34 119.1(9) . . ?
C28 C29 C30 119.3(10) . . ?
C28 C29 H29 120.4 . . ?
C30 C29 H29 120.4 . . ?
C31 C30 C29 116.9(12) . . ?
C31 C30 H30 121.5 . . ?
C29 C30 H30 121.5 . . ?
C32 C31 C30 123.1(12) . . ?
C32 C31 H31 118.5 . . ?
C30 C31 H31 118.5 . . ?
C33 C32 C31 117.0(11) . . ?
C33 C32 H32 121.5 . . ?
C31 C32 H32 121.5 . . ?
C32 C33 C28 123.6(11) . . ?
C32 C33 H33 118.2 . . ?
C28 C33 H33 118.2 . . ?
O13 C34 O14 122.4(8) . . ?
O13 C34 C28 125.7(8) . . ?
O14 C34 C28 111.8(8) . . ?
O14 C35 C26 106.4(5) . . ?
O14 C35 C36 110.1(5) . . ?
C26 C35 C36 112.0(6) . . ?
O14 C35 H35 109.4 . . ?
C26 C35 H35 109.4 . . ?
C36 C35 H35 109.4 . . ?
O15 C36 O16 126.7(5) . . ?
O15 C36 C35 119.2(5) . . ?
O16 C36 C35 114.0(5) . . ?
O18 C37 H37A 109.5 . . ?
O18 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
O18 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O20 C38 H38A 109.5 . . ?
O20 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
O20 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C40 C39 N1 119(2) . . ?
C40 C39 H39A 107.6 . . ?
N1 C39 H39A 107.6 . . ?
C40 C39 H39B 107.6 . . ?
N1 C39 H39B 107.6 . . ?
H39A C39 H39B 107.1 . . ?
C39 C40 H40A 111.1 . . ?
C39 C40 H40B 109.4 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 107.9 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
N1 C41 C42 105(2) . . ?
N1 C41 H41A 110.7 . . ?
C42 C41 H41A 110.7 . . ?
N1 C41 H41B 110.7 . . ?
C42 C41 H41B 110.7 . . ?
H41A C41 H41B 108.8 . . ?
C41 C42 H42A 112.7 . . ?
C41 C42 H42B 108.2 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 107.4 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N1 C43 C44 120(2) . . ?
N1 C43 H43A 107.2 . . ?
C44 C43 H43A 107.2 . . ?
N1 C43 H43B 107.2 . . ?
C44 C43 H43B 107.2 . . ?
H43A C43 H43B 106.9 . . ?
C43 C44 H44A 107.3 . . ?
C43 C44 H44B 110.4 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 110.7 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O16 Sm1 O16 75.7(2) 2_665 . ?
O16 Sm1 O8 137.20(17) 2_665 . ?
O16 Sm1 O8 120.45(18) . . ?
O16 Sm1 O8 120.45(18) 2_665 2_665 ?
O16 Sm1 O8 137.20(17) . 2_665 ?
O8 Sm1 O8 76.5(2) . 2_665 ?
O16 Sm1 O17 142.10(16) 2_665 . ?
O16 Sm1 O17 71.59(15) . . ?
O8 Sm1 O17 77.54(17) . . ?
O8 Sm1 O17 75.23(17) 2_665 . ?
O16 Sm1 O17 71.59(15) 2_665 2_665 ?
O16 Sm1 O17 142.10(16) . 2_665 ?
O8 Sm1 O17 75.23(17) . 2_665 ?
O8 Sm1 O17 77.54(17) 2_665 2_665 ?
O17 Sm1 O17 145.1(2) . 2_665 ?
O16 Sm1 O18 78.70(19) 2_665 . ?
O16 Sm1 O18 73.19(17) . . ?
O8 Sm1 O18 70.55(16) . . ?
O8 Sm1 O18 144.65(16) 2_665 . ?
O17 Sm1 O18 108.82(19) . . ?
O17 Sm1 O18 82.04(19) 2_665 . ?
O16 Sm1 O18 73.19(17) 2_665 2_665 ?
O16 Sm1 O18 78.70(19) . 2_665 ?
O8 Sm1 O18 144.65(16) . 2_665 ?
O8 Sm1 O18 70.55(16) 2_665 2_665 ?
O17 Sm1 O18 82.04(19) . 2_665 ?
O17 Sm1 O18 108.82(19) 2_665 2_665 ?
O18 Sm1 O18 144.2(2) . 2_665 ?
O12 Sm2 O12 79.5(2) . 2_665 ?
O12 Sm2 O4 139.11(17) . 1_556 ?
O12 Sm2 O4 116.03(18) 2_665 1_556 ?
O12 Sm2 O4 116.03(18) . 2_666 ?
O12 Sm2 O4 139.11(17) 2_665 2_666 ?
O4 Sm2 O4 78.0(3) 1_556 2_666 ?
O12 Sm2 O20 78.44(18) . . ?
O12 Sm2 O20 74.16(18) 2_665 . ?
O4 Sm2 O20 71.09(17) 1_556 . ?
O4 Sm2 O20 143.38(17) 2_666 . ?
O12 Sm2 O20 74.16(18) . 2_665 ?
O12 Sm2 O20 78.44(18) 2_665 2_665 ?
O4 Sm2 O20 143.38(17) 1_556 2_665 ?
O4 Sm2 O20 71.09(17) 2_666 2_665 ?
O20 Sm2 O20 144.1(2) . 2_665 ?
O12 Sm2 O19 71.69(16) . . ?
O12 Sm2 O19 143.97(16) 2_665 . ?
O4 Sm2 O19 76.25(17) 1_556 . ?
O4 Sm2 O19 74.79(17) 2_666 . ?
O20 Sm2 O19 79.15(19) . . ?
O20 Sm2 O19 112.72(18) 2_665 . ?
O12 Sm2 O19 143.97(16) . 2_665 ?
O12 Sm2 O19 71.69(16) 2_665 2_665 ?
O4 Sm2 O19 74.79(17) 1_556 2_665 ?
O4 Sm2 O19 76.25(17) 2_666 2_665 ?
O20 Sm2 O19 112.72(18) . 2_665 ?
O20 Sm2 O19 79.15(19) 2_665 2_665 ?
O19 Sm2 O19 142.5(2) . 2_665 ?
C7 O1 C8 116.3(5) . . ?
C9 O4 Sm2 132.7(4) . 1_554 ?
C16 O6 C17 116.0(5) . . ?
C18 O8 Sm1 130.9(4) . . ?
C25 O10 C26 116.0(5) . . ?
C27 O12 Sm2 140.0(4) . . ?
C34 O14 C35 115.5(6) . . ?
C36 O16 Sm1 139.1(4) . . ?
Sm1 O17 H103 100.3 . . ?
Sm1 O17 H104 149.3 . . ?
H103 O17 H104 110.4 . . ?
C37 O18 Sm1 134.0(7) . . ?
C37 O18 H101 110.0 . . ?
Sm1 O18 H101 113.7 . . ?
Sm2 O19 H105 99.8 . . ?
Sm2 O19 H106 118.4 . . ?
H105 O19 H106 108.7 . . ?
C38 O20 Sm2 133.3(5) . . ?
C38 O20 H102 115.3 . . ?
Sm2 O20 H102 109.0 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.453
_refine_diff_density_min         -1.166
_refine_diff_density_rms         0.133
####################################################################### 
# 
# 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_21212
_database_code_depnum_ccdc_archive 'CCDC 1526605'
_audit_update_record             
;
2017-01-10 deposited with the CCDC.
2017-04-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_absolute_configuration rm
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H36 O20 Tb, C6 H16 N, 2(H2 O)'
_chemical_formula_sum            'C44 H56 N O22 Tb'
_chemical_formula_weight         1109.82

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

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'

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

_cell_length_a                   20.056(4)
_cell_length_b                   16.412(3)
_cell_length_c                   16.648(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5479.7(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    39155
_cell_measurement_theta_min      3.05
_cell_measurement_theta_max      28.02

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2272
_exptl_absorpt_coefficient_mu    1.363
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7400
_exptl_absorpt_correction_T_max  0.7914
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            51678
_diffrn_reflns_av_R_equivalents  0.0763
_diffrn_reflns_av_sigmaI/netI    0.0689
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.18
_diffrn_reflns_theta_max         27.48
_reflns_number_total             12432
_reflns_number_gt                8854
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1039P)²+8.6426P] 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_abs_structure_details 
'Flack H D (1983), Acta Cryst. A39, 876-881, Friedel pairs  5539'
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_number_reflns         12432
_refine_ls_number_parameters     616
_refine_ls_number_restraints     74
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0679
_refine_ls_wR_factor_ref         0.2020
_refine_ls_wR_factor_gt          0.1853
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.072
_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
N1 N 0.3047(11) 0.1081(13) 0.8474(13) 0.170(8) Uani 1 1 d D . .
C1 C 0.5997(6) 0.1674(8) 1.1344(7) 0.071(3) Uani 1 1 d . . .
C2 C 0.5700(7) 0.1188(8) 1.0721(7) 0.082(4) Uani 1 1 d . . .
H2 H 0.5332 0.1396 1.0449 0.099 Uiso 1 1 calc R . .
C4 C 0.6482(8) 0.0112(11) 1.0956(9) 0.106(5) Uani 1 1 d U . .
H4 H 0.6659 -0.0392 1.0815 0.128 Uiso 1 1 calc R . .
C3 C 0.5932(8) 0.0434(8) 1.0511(10) 0.098(4) Uani 1 1 d . . .
H3 H 0.5738 0.0141 1.0093 0.117 Uiso 1 1 calc R . .
C5 C 0.6764(9) 0.0552(12) 1.1613(12) 0.119(6) Uani 1 1 d U . .
H5 H 0.7099 0.0325 1.1929 0.143 Uiso 1 1 calc R . .
C6 C 0.6533(6) 0.1297(8) 1.1756(6) 0.074(3) Uani 1 1 d . . .
H6 H 0.6739 0.1595 1.2161 0.089 Uiso 1 1 calc R . .
C7 C 0.5788(5) 0.2449(7) 1.1532(5) 0.053(2) Uani 1 1 d . . .
C8 C 0.4973(5) 0.3470(5) 1.1323(4) 0.0396(16) Uani 1 1 d . . .
H8 H 0.5341 0.3856 1.1251 0.048 Uiso 1 1 calc R . .
C9 C 0.4716(4) 0.3531(5) 1.2191(4) 0.0317(16) Uani 1 1 d . . .
C10 C 0.2713(5) 0.2810(6) 1.0777(5) 0.054(2) Uani 1 1 d . . .
C11 C 0.2113(5) 0.2964(8) 1.0470(8) 0.075(3) Uani 1 1 d . . .
H11 H 0.2063 0.3394 1.0112 0.090 Uiso 1 1 calc R . .
C12 C 0.1547(7) 0.2489(10) 1.0675(9) 0.093(4) Uani 1 1 d . . .
H12 H 0.1129 0.2619 1.0470 0.112 Uiso 1 1 calc R . .
C13 C 0.1622(7) 0.1860(10) 1.1161(12) 0.111(6) Uani 1 1 d . . .
H13 H 0.1255 0.1535 1.1277 0.133 Uiso 1 1 calc R . .
C14 C 0.2273(8) 0.1657(9) 1.1526(11) 0.103(5) Uani 1 1 d . . .
H14 H 0.2326 0.1220 1.1877 0.124 Uiso 1 1 calc R . .
C15 C 0.2807(6) 0.2164(8) 1.1309(7) 0.071(3) Uani 1 1 d . . .
H15 H 0.3228 0.2068 1.1523 0.085 Uiso 1 1 calc R . .
C16 C 0.3287(4) 0.3357(6) 1.0575(5) 0.049(2) Uani 1 1 d . . .
C17 C 0.4429(4) 0.3671(5) 1.0731(4) 0.0367(17) Uani 1 1 d . . .
H17 H 0.4291 0.4238 1.0808 0.044 Uiso 1 1 calc R . .
C18 C 0.4678(4) 0.3559(6) 0.9856(5) 0.0412(19) Uani 1 1 d . . .
C19 C 0.6977(5) 0.2286(6) 0.6150(5) 0.054(2) Uani 1 1 d . . .
C20 C 0.6899(6) 0.1489(7) 0.5918(7) 0.073(3) Uani 1 1 d . . .
H20 H 0.6512 0.1326 0.5654 0.087 Uiso 1 1 calc R . .
C21 C 0.7398(8) 0.0930(9) 0.6078(8) 0.090(4) Uani 1 1 d . . .
H21 H 0.7347 0.0393 0.5911 0.108 Uiso 1 1 calc R . .
C22 C 0.7939(8) 0.1147(11) 0.6459(10) 0.104(5) Uani 1 1 d . . .
H22 H 0.8250 0.0753 0.6602 0.125 Uiso 1 1 calc R . .
C23 C 0.8053(7) 0.1940(10) 0.6651(9) 0.087(4) Uani 1 1 d . . .
H23 H 0.8460 0.2102 0.6865 0.104 Uiso 1 1 calc R . .
C24 C 0.7554(5) 0.2498(8) 0.6522(8) 0.072(3) Uani 1 1 d . . .
H24 H 0.7612 0.3033 0.6693 0.087 Uiso 1 1 calc R . .
C25 C 0.6429(5) 0.2884(6) 0.5973(5) 0.049(2) Uani 1 1 d . . .
C26 C 0.6172(4) 0.4281(5) 0.5795(4) 0.0335(16) Uani 1 1 d . . .
H26 H 0.5724 0.4126 0.5973 0.040 Uiso 1 1 calc R . .
C27 C 0.6159(4) 0.4349(5) 0.4885(4) 0.0399(18) Uani 1 1 d . . .
C28 C 0.7966(5) 0.6098(6) 0.6100(5) 0.054(2) Uani 1 1 d D . .
C29 C 0.8364(6) 0.5428(8) 0.6045(9) 0.085(4) Uani 1 1 d . . .
H29 H 0.8179 0.4908 0.6040 0.102 Uiso 1 1 calc R . .
C30 C 0.9075(8) 0.5534(10) 0.5995(11) 0.112(5) Uani 1 1 d DU . .
H30 H 0.9357 0.5094 0.5902 0.134 Uiso 1 1 calc R . .
C31 C 0.9328(10) 0.6322(11) 0.6091(13) 0.128(6) Uani 1 1 d DU . .
H31 H 0.9787 0.6395 0.6128 0.154 Uiso 1 1 calc R . .
C32 C 0.8926(7) 0.6984(10) 0.6131(8) 0.092(4) Uani 1 1 d . . .
H32 H 0.9107 0.7504 0.6169 0.111 Uiso 1 1 calc R . .
C33 C 0.8245(6) 0.6875(7) 0.6115(6) 0.072(3) Uani 1 1 d D . .
H33 H 0.7967 0.7328 0.6114 0.086 Uiso 1 1 calc R . .
C34 C 0.7239(5) 0.6002(7) 0.6127(5) 0.051(2) Uani 1 1 d . . .
C35 C 0.6358(3) 0.5051(6) 0.6221(4) 0.0390(16) Uani 1 1 d . . .
H35 H 0.6074 0.5493 0.6022 0.047 Uiso 1 1 calc R . .
C36 C 0.6287(3) 0.5003(7) 0.7135(4) 0.0399(16) Uani 1 1 d . . .
C37 C 0.4777(8) 0.3249(10) 0.7297(7) 0.097(5) Uani 1 1 d . . .
H37A H 0.4332 0.3046 0.7226 0.146 Uiso 1 1 calc R . .
H37B H 0.5088 0.2805 0.7259 0.146 Uiso 1 1 calc R . .
H37C H 0.4874 0.3643 0.6887 0.146 Uiso 1 1 calc R . .
C38 C 0.4517(6) 0.3298(7) 0.4739(6) 0.068(3) Uani 1 1 d . . .
H38A H 0.4694 0.3608 0.5179 0.101 Uiso 1 1 calc R . .
H38B H 0.4676 0.2747 0.4772 0.101 Uiso 1 1 calc R . .
H38C H 0.4039 0.3301 0.4764 0.101 Uiso 1 1 calc R . .
C39 C 0.287(2) 0.114(3) 0.9345(16) 0.35(3) Uani 1 1 d DU . .
H39A H 0.2849 0.1691 0.9542 0.422 Uiso 1 1 calc R . .
H39B H 0.3155 0.0806 0.9686 0.422 Uiso 1 1 calc R . .
C40 C 0.2199(19) 0.076(2) 0.920(2) 0.257(16) Uani 1 1 d DU . .
H40A H 0.1864 0.1081 0.9466 0.385 Uiso 1 1 d R . .
H40B H 0.2182 0.0212 0.9387 0.385 Uiso 1 1 d R . .
H40C H 0.2121 0.0775 0.8629 0.385 Uiso 1 1 d R . .
C41 C 0.294(3) 0.044(2) 0.784(3) 0.38(3) Uani 1 1 d DU . .
H41A H 0.3161 0.0599 0.7346 0.460 Uiso 1 1 calc R . .
H41B H 0.2466 0.0382 0.7730 0.460 Uiso 1 1 calc R . .
C42 C 0.326(2) -0.044(3) 0.820(2) 0.29(2) Uani 1 1 d DU . .
H42A H 0.3489 -0.0353 0.8697 0.435 Uiso 1 1 d R . .
H42B H 0.3567 -0.0643 0.7804 0.435 Uiso 1 1 d R . .
H42C H 0.2908 -0.0829 0.8278 0.435 Uiso 1 1 d R . .
C43 C 0.288(2) 0.1760(16) 0.7921(17) 0.239(15) Uani 1 1 d DU . .
H43A H 0.2409 0.1736 0.7768 0.287 Uiso 1 1 calc R . .
H43B H 0.3147 0.1739 0.7440 0.287 Uiso 1 1 calc R . .
C44 C 0.3018(14) 0.251(2) 0.8391(18) 0.219(16) Uani 1 1 d D . .
H44A H 0.2787 0.2484 0.8896 0.328 Uiso 1 1 d R . .
H44B H 0.2867 0.2978 0.8095 0.328 Uiso 1 1 d R . .
H44C H 0.3489 0.2553 0.8485 0.328 Uiso 1 1 d R . .
Tb1 Tb 0.5000 0.5000 0.84903(2) 0.03349(14) Uani 1 2 d S . .
Tb2 Tb 0.5000 0.5000 0.35444(2) 0.03407(14) Uani 1 2 d S . .
O1 O 0.5207(3) 0.2665(4) 1.1149(3) 0.0445(14) Uani 1 1 d . . .
O2 O 0.6079(3) 0.2900(5) 1.1960(4) 0.0632(19) Uani 1 1 d . . .
O3 O 0.4647(3) 0.2894(4) 1.2592(4) 0.0540(16) Uani 1 1 d . . .
O4 O 0.4600(3) 0.4248(4) 1.2432(3) 0.0464(14) Uani 1 1 d . . .
O5 O 0.3227(3) 0.3948(5) 1.0144(4) 0.0608(18) Uani 1 1 d . . .
O6 O 0.3867(3) 0.3139(4) 1.0905(3) 0.0453(14) Uani 1 1 d . . .
O7 O 0.4502(3) 0.2953(4) 0.9454(4) 0.0543(16) Uani 1 1 d . . .
O8 O 0.5064(3) 0.4100(4) 0.9621(3) 0.0460(13) Uani 1 1 d . . .
O9 O 0.5872(4) 0.2688(4) 0.5806(5) 0.067(2) Uani 1 1 d . . .
O10 O 0.6634(3) 0.3653(4) 0.6069(3) 0.0449(13) Uani 1 1 d . . .
O11 O 0.6567(3) 0.3946(4) 0.4466(3) 0.0577(17) Uani 1 1 d . . .
O12 O 0.5733(3) 0.4849(4) 0.4631(3) 0.0465(15) Uani 1 1 d . . .
O13 O 0.6844(4) 0.6568(5) 0.6244(6) 0.079(2) Uani 1 1 d . . .
O14 O 0.7041(3) 0.5233(3) 0.6014(3) 0.0405(13) Uani 1 1 d . . .
O15 O 0.6769(3) 0.5151(5) 0.7569(3) 0.0579(19) Uani 1 1 d . . .
O16 O 0.5699(3) 0.4809(4) 0.7376(3) 0.0449(16) Uani 1 1 d . . .
O17 O 0.6125(3) 0.5156(4) 0.8930(3) 0.0477(15) Uani 1 1 d . . .
H103 H 0.6328 0.4935 0.8537 0.072 Uiso 1 1 d R . .
H104 H 0.6405 0.5331 0.9273 0.072 Uiso 1 1 d R . .
O18 O 0.4834(3) 0.3620(4) 0.8061(3) 0.0527(18) Uani 1 1 d . . .
H101 H 0.4917 0.3266 0.8422 0.079 Uiso 1 1 d R . .
O19 O 0.5985(3) 0.4267(4) 0.3068(3) 0.0518(16) Uani 1 1 d . . .
H105 H 0.6156 0.4134 0.3517 0.078 Uiso 1 1 d R . .
H106 H 0.5928 0.3839 0.2786 0.078 Uiso 1 1 d R . .
O20 O 0.4727(3) 0.3650(4) 0.4003(3) 0.0527(15) Uani 1 1 d . . .
H102 H 0.4656 0.3351 0.3593 0.079 Uiso 1 1 d R . .
O22 O 0.4083(13) 0.1434(16) 0.9965(17) 0.279(11) Uani 1 1 d U . .
O21 O 0.426(2) 0.115(3) 0.239(2) 0.41(2) Uani 1 1 d U . .


_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
N1 C43 1.486(10) . ?
N1 C39 1.494(10) . ?
N1 C41 1.502(10) . ?
C1 C7 1.375(16) . ?
C1 C6 1.417(15) . ?
C1 C2 1.437(16) . ?
C2 C3 1.366(17) . ?
C2 H2 0.9300 . ?
C4 C5 1.43(2) . ?
C4 C3 1.43(2) . ?
C4 H4 0.9300 . ?
C3 H3 0.9300 . ?
C5 C6 1.33(2) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 O2 1.182(12) . ?
C7 O1 1.375(11) . ?
C8 O1 1.432(10) . ?
C8 C17 1.506(11) . ?
C8 C9 1.537(9) . ?
C8 H8 0.9800 . ?
C9 O3 1.249(10) . ?
C9 O4 1.265(10) . ?
C10 C11 1.332(14) . ?
C10 C15 1.396(14) . ?
C10 C16 1.496(12) . ?
C11 C12 1.418(17) . ?
C11 H11 0.9300 . ?
C12 C13 1.32(2) . ?
C12 H12 0.9300 . ?
C13 C14 1.48(2) . ?
C13 H13 0.9300 . ?
C14 C15 1.403(16) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 O5 1.214(11) . ?
C16 O6 1.336(10) . ?
C17 O6 1.455(9) . ?
C17 C18 1.551(11) . ?
C17 H17 0.9800 . ?
C18 O8 1.241(10) . ?
C18 O7 1.250(11) . ?
C19 C24 1.358(15) . ?
C19 C20 1.372(15) . ?
C19 C25 1.503(12) . ?
C20 C21 1.384(17) . ?
C20 H20 0.9300 . ?
C21 C22 1.31(2) . ?
C21 H21 0.9300 . ?
C22 C23 1.36(2) . ?
C22 H22 0.9300 . ?
C23 C24 1.373(17) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 O9 1.195(11) . ?
C25 O10 1.338(11) . ?
C26 O10 1.459(9) . ?
C26 C35 1.497(12) . ?
C26 C27 1.519(10) . ?
C26 H26 0.9800 . ?
C27 O12 1.258(9) . ?
C27 O11 1.263(10) . ?
C28 C29 1.363(15) . ?
C28 C33 1.393(8) . ?
C28 C34 1.467(13) . ?
C29 C30 1.439(19) . ?
C29 H29 0.9300 . ?
C30 C31 1.399(9) . ?
C30 H30 0.9300 . ?
C31 C32 1.35(2) . ?
C31 H31 0.9300 . ?
C32 C33 1.378(18) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
C34 O13 1.237(12) . ?
C34 O14 1.336(11) . ?
C35 O14 1.443(9) . ?
C35 C36 1.531(8) . ?
C35 H35 0.9800 . ?
C36 O15 1.232(9) . ?
C36 O16 1.286(9) . ?
C37 O18 1.415(12) . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 O20 1.418(11) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 C40 1.498(10) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 C42 1.70(4) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 C44 1.487(10) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
Tb1 O16 2.346(5) 2_665 ?
Tb1 O16 2.346(5) . ?
Tb1 O17 2.386(5) . ?
Tb1 O17 2.386(5) 2_665 ?
Tb1 O8 2.395(5) 2_665 ?
Tb1 O8 2.395(5) . ?
Tb1 O18 2.398(6) . ?
Tb1 O18 2.398(6) 2_665 ?
Tb2 O12 2.344(5) . ?
Tb2 O12 2.344(5) 2_665 ?
Tb2 O4 2.366(6) 1_554 ?
Tb2 O4 2.366(6) 2_664 ?
Tb2 O20 2.407(6) 2_665 ?
Tb2 O20 2.407(6) . ?
Tb2 O19 2.445(6) . ?
Tb2 O19 2.445(6) 2_665 ?
O4 Tb2 2.366(6) 1_556 ?
O17 H103 0.8511 . ?
O17 H104 0.8507 . ?
O18 H101 0.8523 . ?
O19 H105 0.8509 . ?
O19 H106 0.8531 . ?
O20 H102 0.8521 . ?

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
C43 N1 C39 120(3) . . ?
C43 N1 C41 93(2) . . ?
C39 N1 C41 134(3) . . ?
C7 C1 C6 121.6(10) . . ?
C7 C1 C2 123.5(11) . . ?
C6 C1 C2 114.9(12) . . ?
C3 C2 C1 123.1(13) . . ?
C3 C2 H2 118.4 . . ?
C1 C2 H2 118.4 . . ?
C5 C4 C3 121.1(15) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C2 C3 C4 117.6(14) . . ?
C2 C3 H3 121.2 . . ?
C4 C3 H3 121.2 . . ?
C6 C5 C4 117.6(15) . . ?
C6 C5 H5 121.2 . . ?
C4 C5 H5 121.2 . . ?
C5 C6 C1 125.4(13) . . ?
C5 C6 H6 117.3 . . ?
C1 C6 H6 117.3 . . ?
O2 C7 O1 122.4(9) . . ?
O2 C7 C1 124.5(10) . . ?
O1 C7 C1 113.0(9) . . ?
O1 C8 C17 107.9(6) . . ?
O1 C8 C9 111.1(6) . . ?
C17 C8 C9 111.0(7) . . ?
O1 C8 H8 108.9 . . ?
C17 C8 H8 108.9 . . ?
C9 C8 H8 108.9 . . ?
O3 C9 O4 126.1(6) . . ?
O3 C9 C8 119.0(7) . . ?
O4 C9 C8 114.9(7) . . ?
C11 C10 C15 120.5(9) . . ?
C11 C10 C16 119.7(9) . . ?
C15 C10 C16 119.7(9) . . ?
C10 C11 C12 121.9(11) . . ?
C10 C11 H11 119.1 . . ?
C12 C11 H11 119.1 . . ?
C13 C12 C11 119.0(13) . . ?
C13 C12 H12 120.5 . . ?
C11 C12 H12 120.5 . . ?
C12 C13 C14 122.0(12) . . ?
C12 C13 H13 119.0 . . ?
C14 C13 H13 119.0 . . ?
C15 C14 C13 115.7(13) . . ?
C15 C14 H14 122.1 . . ?
C13 C14 H14 122.1 . . ?
C10 C15 C14 120.8(11) . . ?
C10 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
O5 C16 O6 122.9(8) . . ?
O5 C16 C10 122.4(8) . . ?
O6 C16 C10 114.6(8) . . ?
O6 C17 C8 107.4(6) . . ?
O6 C17 C18 111.4(7) . . ?
C8 C17 C18 110.8(6) . . ?
O6 C17 H17 109.0 . . ?
C8 C17 H17 109.0 . . ?
C18 C17 H17 109.0 . . ?
O8 C18 O7 125.2(8) . . ?
O8 C18 C17 114.4(8) . . ?
O7 C18 C17 120.4(7) . . ?
C24 C19 C20 118.0(10) . . ?
C24 C19 C25 123.1(10) . . ?
C20 C19 C25 118.9(10) . . ?
C19 C20 C21 119.6(12) . . ?
C19 C20 H20 120.2 . . ?
C21 C20 H20 120.2 . . ?
C22 C21 C20 120.9(15) . . ?
C22 C21 H21 119.5 . . ?
C20 C21 H21 119.5 . . ?
C21 C22 C23 120.9(14) . . ?
C21 C22 H22 119.5 . . ?
C23 C22 H22 119.5 . . ?
C22 C23 C24 118.6(14) . . ?
C22 C23 H23 120.7 . . ?
C24 C23 H23 120.7 . . ?
C19 C24 C23 121.5(13) . . ?
C19 C24 H24 119.3 . . ?
C23 C24 H24 119.3 . . ?
O9 C25 O10 124.7(9) . . ?
O9 C25 C19 123.7(10) . . ?
O10 C25 C19 111.6(8) . . ?
O10 C26 C35 106.8(6) . . ?
O10 C26 C27 112.0(6) . . ?
C35 C26 C27 114.5(7) . . ?
O10 C26 H26 107.8 . . ?
C35 C26 H26 107.8 . . ?
C27 C26 H26 107.8 . . ?
O12 C27 O11 126.6(7) . . ?
O12 C27 C26 113.3(7) . . ?
O11 C27 C26 120.1(7) . . ?
C29 C28 C33 120.3(10) . . ?
C29 C28 C34 119.9(9) . . ?
C33 C28 C34 119.8(10) . . ?
C28 C29 C30 119.2(12) . . ?
C28 C29 H29 120.4 . . ?
C30 C29 H29 120.4 . . ?
C31 C30 C29 117.7(16) . . ?
C31 C30 H30 121.2 . . ?
C29 C30 H30 121.2 . . ?
C32 C31 C30 122.1(17) . . ?
C32 C31 H31 118.9 . . ?
C30 C31 H31 118.9 . . ?
C31 C32 C33 119.0(13) . . ?
C31 C32 H32 120.5 . . ?
C33 C32 H32 120.5 . . ?
C32 C33 C28 121.2(13) . . ?
C32 C33 H33 119.4 . . ?
C28 C33 H33 119.4 . . ?
O13 C34 O14 122.7(8) . . ?
O13 C34 C28 124.2(10) . . ?
O14 C34 C28 113.2(9) . . ?
O14 C35 C26 107.4(6) . . ?
O14 C35 C36 109.6(6) . . ?
C26 C35 C36 113.9(8) . . ?
O14 C35 H35 108.6 . . ?
C26 C35 H35 108.6 . . ?
C36 C35 H35 108.6 . . ?
O15 C36 O16 125.9(6) . . ?
O15 C36 C35 120.0(6) . . ?
O16 C36 C35 114.1(6) . . ?
O18 C37 H37A 109.5 . . ?
O18 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
O18 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O20 C38 H38A 109.5 . . ?
O20 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
O20 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N1 C39 C40 92(2) . . ?
N1 C39 H39A 113.3 . . ?
C40 C39 H39A 113.3 . . ?
N1 C39 H39B 113.3 . . ?
C40 C39 H39B 113.3 . . ?
H39A C39 H39B 110.7 . . ?
C39 C40 H40A 109.6 . . ?
C39 C40 H40B 111.4 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 107.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
N1 C41 C42 107(3) . . ?
N1 C41 H41A 110.3 . . ?
C42 C41 H41A 110.3 . . ?
N1 C41 H41B 110.3 . . ?
C42 C41 H41B 110.3 . . ?
H41A C41 H41B 108.6 . . ?
C41 C42 H42A 111.1 . . ?
C41 C42 H42B 107.4 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.9 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N1 C43 C44 105(2) . . ?
N1 C43 H43A 110.9 . . ?
C44 C43 H43A 110.9 . . ?
N1 C43 H43B 110.9 . . ?
C44 C43 H43B 110.9 . . ?
H43A C43 H43B 108.9 . . ?
C43 C44 H44A 109.4 . . ?
C43 C44 H44B 109.4 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.6 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O16 Tb1 O16 75.5(2) 2_665 . ?
O16 Tb1 O17 142.48(18) 2_665 . ?
O16 Tb1 O17 72.05(17) . . ?
O16 Tb1 O17 72.05(17) 2_665 2_665 ?
O16 Tb1 O17 142.48(18) . 2_665 ?
O17 Tb1 O17 144.3(3) . 2_665 ?
O16 Tb1 O8 120.5(2) 2_665 2_665 ?
O16 Tb1 O8 137.3(2) . 2_665 ?
O17 Tb1 O8 75.1(2) . 2_665 ?
O17 Tb1 O8 77.0(2) 2_665 2_665 ?
O16 Tb1 O8 137.3(2) 2_665 . ?
O16 Tb1 O8 120.5(2) . . ?
O17 Tb1 O8 77.0(2) . . ?
O17 Tb1 O8 75.1(2) 2_665 . ?
O8 Tb1 O8 76.5(3) 2_665 . ?
O16 Tb1 O18 78.9(2) 2_665 . ?
O16 Tb1 O18 73.8(2) . . ?
O17 Tb1 O18 108.9(2) . . ?
O17 Tb1 O18 81.9(2) 2_665 . ?
O8 Tb1 O18 143.98(18) 2_665 . ?
O8 Tb1 O18 70.08(19) . . ?
O16 Tb1 O18 73.8(2) 2_665 2_665 ?
O16 Tb1 O18 78.9(2) . 2_665 ?
O17 Tb1 O18 81.9(2) . 2_665 ?
O17 Tb1 O18 108.9(2) 2_665 2_665 ?
O8 Tb1 O18 70.08(19) 2_665 2_665 ?
O8 Tb1 O18 143.98(18) . 2_665 ?
O18 Tb1 O18 145.3(2) . 2_665 ?
O12 Tb2 O12 78.9(3) . 2_665 ?
O12 Tb2 O4 139.7(2) . 1_554 ?
O12 Tb2 O4 116.5(2) 2_665 1_554 ?
O12 Tb2 O4 116.5(2) . 2_664 ?
O12 Tb2 O4 139.7(2) 2_665 2_664 ?
O4 Tb2 O4 77.0(3) 1_554 2_664 ?
O12 Tb2 O20 73.1(2) . 2_665 ?
O12 Tb2 O20 78.5(2) 2_665 2_665 ?
O4 Tb2 O20 143.7(2) 1_554 2_665 ?
O4 Tb2 O20 72.0(2) 2_664 2_665 ?
O12 Tb2 O20 78.5(2) . . ?
O12 Tb2 O20 73.1(2) 2_665 . ?
O4 Tb2 O20 72.0(2) 1_554 . ?
O4 Tb2 O20 143.7(2) 2_664 . ?
O20 Tb2 O20 143.0(3) 2_665 . ?
O12 Tb2 O19 72.05(19) . . ?
O12 Tb2 O19 143.96(19) 2_665 . ?
O4 Tb2 O19 76.3(2) 1_554 . ?
O4 Tb2 O19 74.2(2) 2_664 . ?
O20 Tb2 O19 111.9(2) 2_665 . ?
O20 Tb2 O19 80.4(2) . . ?
O12 Tb2 O19 143.96(19) . 2_665 ?
O12 Tb2 O19 72.05(19) 2_665 2_665 ?
O4 Tb2 O19 74.2(2) 1_554 2_665 ?
O4 Tb2 O19 76.3(2) 2_664 2_665 ?
O20 Tb2 O19 80.4(2) 2_665 2_665 ?
O20 Tb2 O19 111.9(2) . 2_665 ?
O19 Tb2 O19 142.2(3) . 2_665 ?
C7 O1 C8 115.0(7) . . ?
C9 O4 Tb2 132.1(5) . 1_556 ?
C16 O6 C17 115.6(6) . . ?
C18 O8 Tb1 131.0(5) . . ?
C25 O10 C26 115.7(7) . . ?
C27 O12 Tb2 138.9(5) . . ?
C34 O14 C35 116.4(7) . . ?
C36 O16 Tb1 139.6(5) . . ?
Tb1 O17 H103 99.9 . . ?
Tb1 O17 H104 149.9 . . ?
H103 O17 H104 110.1 . . ?
C37 O18 Tb1 133.3(7) . . ?
C37 O18 H101 110.8 . . ?
Tb1 O18 H101 114.0 . . ?
Tb2 O19 H105 99.6 . . ?
Tb2 O19 H106 118.4 . . ?
H105 O19 H106 109.1 . . ?
C38 O20 Tb2 135.7(6) . . ?
C38 O20 H102 114.1 . . ?
Tb2 O20 H102 108.3 . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.585
_refine_diff_density_min         -2.553
_refine_diff_density_rms         0.140
