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

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

data_3-Dy
_database_code_depnum_ccdc_archive 'CCDC 958686'
_audit_update_record             
;
2013-09-02 deposited with the CCDC.
2015-01-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H50 Dy2 N5 O22'
_chemical_formula_weight         1337.90

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'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   13.405(3)
_cell_length_b                   14.705(4)
_cell_length_c                   13.388(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.357(4)
_cell_angle_gamma                90.00
_cell_volume                     2603.9(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1326
_exptl_absorpt_coefficient_mu    2.931
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19652
_diffrn_reflns_av_R_equivalents  0.0202
_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.08
_diffrn_reflns_theta_max         27.49
_reflns_number_total             5951
_reflns_number_gt                5523
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0200P)²+14.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5951
_refine_ls_number_parameters     421
_refine_ls_number_restraints     325
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0316
_refine_ls_wR_factor_ref         0.0748
_refine_ls_wR_factor_gt          0.0730
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.026
_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
Dy1 Dy 0.138930(12) 0.436755(11) 0.509019(13) 0.01730(6) Uani 1 1 d . . .
O1 O -0.0593(3) 0.4391(2) 0.5735(2) 0.0381(7) Uani 1 1 d . . .
O2 O 0.0629(2) 0.3420(2) 0.6181(3) 0.0461(9) Uani 1 1 d . A .
O3 O 0.0102(2) 0.1303(2) 0.8951(2) 0.0331(7) Uani 1 1 d . . .
O4 O -0.1357(2) 0.0524(2) 0.8716(3) 0.0398(8) Uani 1 1 d . . .
O9 O 0.2125(2) 0.2916(2) 0.4892(3) 0.0486(9) Uani 1 1 d . A .
N1 N -0.5850(3) 0.2635(3) 0.5554(4) 0.0566(13) Uani 1 1 d . A .
C1 C -0.0270(3) 0.3662(3) 0.6135(3) 0.0295(9) Uani 1 1 d . . .
C2 C -0.0977(3) 0.3043(3) 0.6572(3) 0.0312(9) Uani 1 1 d . A .
C3 C -0.0584(3) 0.2416(3) 0.7317(3) 0.0323(9) Uani 1 1 d . . .
H3A H 0.0124 0.2391 0.7550 0.039 Uiso 1 1 calc R A .
C4 C -0.1229(3) 0.1828(3) 0.7716(3) 0.0312(9) Uani 1 1 d . A .
C5 C -0.2262(3) 0.1860(3) 0.7363(4) 0.0374(11) Uani 1 1 d . . .
H5A H -0.2699 0.1450 0.7628 0.045 Uiso 1 1 calc R A .
C6 C -0.2664(3) 0.2487(3) 0.6624(4) 0.0372(11) Uani 1 1 d . A .
C7 C -0.2011(3) 0.3084(3) 0.6238(4) 0.0362(10) Uani 1 1 d . . .
H7A H -0.2277 0.3521 0.5743 0.043 Uiso 1 1 calc R A .
C8 C -0.3771(3) 0.2532(4) 0.6249(4) 0.0407(11) Uani 1 1 d . . .
C9 C -0.4463(4) 0.2397(4) 0.6897(5) 0.0538(15) Uani 1 1 d . A .
H9A H -0.4240 0.2263 0.7591 0.065 Uiso 1 1 calc R . .
C10 C -0.5491(4) 0.2461(5) 0.6517(5) 0.0599(16) Uani 1 1 d . . .
H10A H -0.5959 0.2375 0.6971 0.072 Uiso 1 1 calc R A .
C11 C -0.5179(4) 0.2756(4) 0.4938(5) 0.0575(15) Uani 1 1 d . . .
H11A H -0.5423 0.2877 0.4244 0.069 Uiso 1 1 calc R A .
C12 C -0.4149(4) 0.2717(5) 0.5250(5) 0.0557(15) Uani 1 1 d . A .
H12A H -0.3701 0.2816 0.4779 0.067 Uiso 1 1 calc R . .
C13 C -0.0793(3) 0.1156(3) 0.8525(3) 0.0300(9) Uani 1 1 d . . .
O5 O 0.2788(10) 0.4206(9) 0.6533(12) 0.029(2) Uani 0.50 1 d PDU A 1
O6 O 0.3087(10) 0.5010(9) 0.5230(5) 0.035(2) Uani 0.50 1 d PDU . 1
O7 O 0.6972(9) 0.5071(8) 0.5136(5) 0.0240(18) Uani 0.50 1 d PDU . 1
O8 O 0.7886(10) 0.5531(13) 0.6563(13) 0.030(2) Uani 0.50 1 d PDU . 1
C14 C 0.3365(5) 0.4681(5) 0.6096(5) 0.0254(16) Uani 0.50 1 d PDU . 1
C15 C 0.4418(3) 0.4855(4) 0.6635(3) 0.0234(15) Uani 0.50 1 d PGU B 1
C16 C 0.5214(4) 0.4988(4) 0.6103(3) 0.0235(14) Uani 0.50 1 d PGU B 1
C17 C 0.6182(3) 0.5153(5) 0.6622(4) 0.0251(18) Uani 0.50 1 d PGU B 1
C18 C 0.6354(3) 0.5184(5) 0.7674(4) 0.0280(16) Uani 0.50 1 d PGU B 1
H18A H 0.7022 0.5298 0.8032 0.034 Uiso 0.50 1 d PR B 1
C19 C 0.5558(4) 0.5050(4) 0.8206(3) 0.0280(15) Uani 0.50 1 d PGU . 1
C20 C 0.4590(3) 0.4886(4) 0.7687(3) 0.0296(16) Uani 0.50 1 d PGU . 1
H20A H 0.4040 0.4794 0.8055 0.036 Uiso 0.50 1 d PR B 1
C21 C 0.5733(7) 0.5118(6) 0.9346(7) 0.0390(18) Uani 0.50 1 d PDU . 1
C22 C 0.6612(9) 0.5462(7) 0.9892(8) 0.054(2) Uani 0.50 1 d PDU C 1
H22A H 0.7132 0.5678 0.9536 0.065 Uiso 0.50 1 d PR C 1
N2 N 0.6092(9) 0.5222(7) 1.1499(7) 0.068(3) Uani 0.50 1 d PDU . 1
C23 C 0.6775(11) 0.5508(7) 1.0957(9) 0.068(3) Uani 0.50 1 d PDU C 1
H23A H 0.7408 0.5747 1.1294 0.082 Uiso 0.50 1 d PR C 1
C24 C 0.5236(11) 0.4887(8) 1.0976(9) 0.069(3) Uani 0.50 1 d PDU . 1
H24A H 0.4737 0.4678 1.1362 0.083 Uiso 0.50 1 d PR . 1
C25 C 0.5002(14) 0.4812(7) 0.9919(13) 0.052(3) Uani 0.50 1 d PDU . 1
H25A H 0.4368 0.4564 0.9598 0.062 Uiso 0.50 1 d PR . 1
C26 C 0.7064(5) 0.5270(5) 0.6067(5) 0.0228(15) Uani 0.50 1 d PDU . 1
O10 O 0.2572(11) 0.3966(9) 0.6620(12) 0.038(3) Uani 0.50 1 d P A 2
O11 O 0.4331(7) 0.5528(8) 0.6581(6) 0.071(3) Uani 0.50 1 d P D 2
O12 O 0.2210(5) 0.2279(6) 0.7411(8) 0.187(5) Uani 1 1 d . E 2
O13 O 0.1932(15) 0.0706(17) 0.8488(18) 0.059(5) Uani 0.50 1 d P . 2
O14 O 0.3710(10) -0.0094(14) 0.8236(13) 0.135(7) Uani 0.50 1 d P F 2
O15 O 0.1092(7) 0.1367(5) 0.4448(8) 0.162(4) Uani 1 1 d . . .
N3 N -0.0539(9) 0.0894(6) 0.4063(7) 0.132(4) Uani 1 1 d . . .
C27 C 0.0137(10) 0.1463(7) 0.4516(9) 0.116(4) Uani 1 1 d . . .
H27A H -0.0069 0.1952 0.4898 0.139 Uiso 1 1 calc R . .
C28 C -0.1609(11) 0.1058(13) 0.4257(18) 0.263(12) Uani 1 1 d . . .
H28A H -0.1619 0.1595 0.4688 0.394 Uiso 1 1 calc R . .
H28B H -0.1841 0.0526 0.4595 0.394 Uiso 1 1 calc R . .
H28C H -0.2056 0.1158 0.3611 0.394 Uiso 1 1 calc R . .
C29 C -0.0241(13) 0.0090(8) 0.3432(8) 0.190(8) Uani 1 1 d . . .
H29A H 0.0491 0.0100 0.3435 0.285 Uiso 1 1 calc R . .
H29B H -0.0596 0.0142 0.2734 0.285 Uiso 1 1 calc R . .
H29C H -0.0429 -0.0484 0.3725 0.285 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O1 2.304(3) 3_566 ?
Dy1 O3 2.328(3) 4_565 ?
Dy1 O4 2.339(3) 2_556 ?
Dy1 O2 2.366(3) . ?
Dy1 O13 2.38(2) 4_565 ?
Dy1 O9 2.384(3) . ?
Dy1 O7 2.411(12) 3_666 ?
Dy1 O6 2.442(13) . ?
Dy1 O10 2.450(16) . ?
Dy1 O5 2.475(16) . ?
Dy1 O8 2.56(2) 3_666 ?
Dy1 C14 2.807(7) . ?
O1 C1 1.244(5) . ?
O1 Dy1 2.304(3) 3_566 ?
O2 C1 1.249(5) . ?
O3 C13 1.260(5) . ?
O3 Dy1 2.328(3) 4_566 ?
O4 C13 1.250(5) . ?
O4 Dy1 2.339(3) 2_546 ?
N1 C10 1.326(8) . ?
N1 C11 1.327(8) . ?
C1 C2 1.500(5) . ?
C2 C7 1.386(6) . ?
C2 C3 1.397(6) . ?
C3 C4 1.389(6) . ?
C3 H3A 0.9500 . ?
C4 C5 1.389(6) . ?
C4 C13 1.511(5) . ?
C5 C6 1.395(6) . ?
C5 H5A 0.9500 . ?
C6 C7 1.397(6) . ?
C6 C8 1.489(6) . ?
C7 H7A 0.9500 . ?
C8 C12 1.377(7) . ?
C8 C9 1.384(7) . ?
C9 C10 1.392(7) . ?
C9 H9A 0.9500 . ?
C10 H10A 0.9500 . ?
C11 C12 1.378(7) . ?
C11 H11A 0.9500 . ?
C12 H12A 0.9500 . ?
O5 C14 1.255(8) . ?
O6 O7 0.498(9) 3_666 ?
O6 C14 1.256(8) . ?
O6 C26 1.763(10) 3_666 ?
O7 O6 0.498(9) 3_666 ?
O7 C26 1.266(7) . ?
O7 C14 1.678(11) 3_666 ?
O7 Dy1 2.411(12) 3_666 ?
O8 C26 1.251(9) . ?
O8 Dy1 2.562(19) 3_666 ?
C14 C15 1.499(8) . ?
C14 O7 1.678(11) 3_666 ?
C15 C16 1.3900 . ?
C15 C20 1.3900 . ?
C16 C17 1.3900 . ?
C17 C18 1.3900 . ?
C17 C26 1.506(8) . ?
C18 C19 1.3900 . ?
C18 H18A 0.9599 . ?
C19 C20 1.3900 . ?
C19 C21 1.510(10) . ?
C19 C24 1.649(13) 3_667 ?
C20 N2 1.540(12) 3_667 ?
C20 C24 1.798(13) 3_667 ?
C20 H20A 0.9600 . ?
C21 C24 1.300(16) 3_667 ?
C21 C22 1.378(14) . ?
C21 C25 1.41(2) . ?
C21 C25 1.50(2) 3_667 ?
C22 C23 1.409(15) . ?
C22 H22A 0.9600 . ?
N2 C23 1.326(17) . ?
N2 C24 1.337(17) . ?
N2 C20 1.540(16) 3_667 ?
C23 H23A 0.9600 . ?
C24 C25 1.27(2) 3_667 ?
C24 C21 1.300(16) 3_667 ?
C24 C25 1.40(2) . ?
C24 C19 1.649(15) 3_667 ?
C24 C20 1.798(13) 3_667 ?
C24 H24A 0.9600 . ?
C25 C25 0.59(2) 3_667 ?
C25 C24 1.27(2) 3_667 ?
C25 C21 1.50(2) 3_667 ?
C25 H25A 0.9600 . ?
C26 O6 1.763(10) 3_666 ?
C26 Dy1 2.833(7) 3_666 ?
O13 Dy1 2.38(2) 4_566 ?
O15 C27 1.306(13) . ?
N3 C27 1.308(12) . ?
N3 C28 1.518(16) . ?
N3 C29 1.543(15) . ?
C27 H27A 0.9500 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Dy1 O3 77.59(12) 3_566 4_565 ?
O1 Dy1 O4 72.12(12) 3_566 2_556 ?
O3 Dy1 O4 131.39(10) 4_565 2_556 ?
O1 Dy1 O2 123.39(12) 3_566 . ?
O3 Dy1 O2 78.87(13) 4_565 . ?
O4 Dy1 O2 87.06(14) 2_556 . ?
O1 Dy1 O13 77.8(7) 3_566 4_565 ?
O3 Dy1 O13 72.1(4) 4_565 4_565 ?
O4 Dy1 O13 133.8(6) 2_556 4_565 ?
O2 Dy1 O13 139.1(5) . 4_565 ?
O1 Dy1 O9 145.48(13) 3_566 . ?
O3 Dy1 O9 79.88(11) 4_565 . ?
O4 Dy1 O9 141.33(12) 2_556 . ?
O2 Dy1 O9 76.62(14) . . ?
O13 Dy1 O9 70.5(7) 4_565 . ?
O1 Dy1 O7 91.7(3) 3_566 3_666 ?
O3 Dy1 O7 131.01(17) 4_565 3_666 ?
O4 Dy1 O7 87.4(2) 2_556 3_666 ?
O2 Dy1 O7 140.5(3) . 3_666 ?
O13 Dy1 O7 58.9(4) 4_565 3_666 ?
O9 Dy1 O7 83.7(3) . 3_666 ?
O1 Dy1 O6 94.8(3) 3_566 . ?
O3 Dy1 O6 142.8(2) 4_565 . ?
O4 Dy1 O6 77.7(3) 2_556 . ?
O2 Dy1 O6 132.0(2) . . ?
O13 Dy1 O6 70.7(4) 4_565 . ?
O9 Dy1 O6 87.6(3) . . ?
O7 Dy1 O6 11.7(2) 3_666 . ?
O1 Dy1 O10 141.1(3) 3_566 . ?
O3 Dy1 O10 139.1(3) 4_565 . ?
O4 Dy1 O10 71.7(4) 2_556 . ?
O2 Dy1 O10 68.1(3) . . ?
O13 Dy1 O10 119.5(7) 4_565 . ?
O9 Dy1 O10 69.7(4) . . ?
O7 Dy1 O10 73.1(3) 3_666 . ?
O6 Dy1 O10 64.0(3) . . ?
O1 Dy1 O5 133.1(3) 3_566 . ?
O3 Dy1 O5 149.0(3) 4_565 . ?
O4 Dy1 O5 68.4(4) 2_556 . ?
O2 Dy1 O5 79.0(2) . . ?
O13 Dy1 O5 113.3(6) 4_565 . ?
O9 Dy1 O5 74.1(4) . . ?
O7 Dy1 O5 62.7(3) 3_666 . ?
O6 Dy1 O5 53.1(3) . . ?
O10 Dy1 O5 11.3(3) . . ?
O1 Dy1 O8 75.6(5) 3_566 3_666 ?
O3 Dy1 O8 78.7(2) 4_565 3_666 ?
O4 Dy1 O8 126.9(4) 2_556 3_666 ?
O2 Dy1 O8 146.0(4) . 3_666 ?
O13 Dy1 O8 7.4(7) 4_565 3_666 ?
O9 Dy1 O8 74.6(5) . 3_666 ?
O7 Dy1 O8 52.5(3) 3_666 3_666 ?
O6 Dy1 O8 64.2(3) . 3_666 ?
O10 Dy1 O8 116.9(5) . 3_666 ?
O5 Dy1 O8 109.5(4) . 3_666 ?
O1 Dy1 C14 115.29(18) 3_566 . ?
O3 Dy1 C14 157.66(17) 4_565 . ?
O4 Dy1 C14 70.95(18) 2_556 . ?
O2 Dy1 C14 105.54(17) . . ?
O13 Dy1 C14 92.1(4) 4_565 . ?
O9 Dy1 C14 79.93(18) . . ?
O7 Dy1 C14 36.5(2) 3_666 . ?
O6 Dy1 C14 26.53(19) . . ?
O10 Dy1 C14 37.5(3) . . ?
O5 Dy1 C14 26.54(18) . . ?
O8 Dy1 C14 86.8(3) 3_666 . ?
C1 O1 Dy1 172.1(3) . 3_566 ?
C1 O2 Dy1 108.1(3) . . ?
C13 O3 Dy1 140.7(3) . 4_566 ?
C13 O4 Dy1 139.4(3) . 2_546 ?
C10 N1 C11 117.0(5) . . ?
O1 C1 O2 122.2(4) . . ?
O1 C1 C2 119.6(4) . . ?
O2 C1 C2 118.2(4) . . ?
O1 C1 Dy1 74.6(2) . . ?
O2 C1 Dy1 48.6(2) . . ?
C2 C1 Dy1 162.9(3) . . ?
C7 C2 C3 120.0(4) . . ?
C7 C2 C1 120.6(4) . . ?
C3 C2 C1 119.4(4) . . ?
C4 C3 C2 120.0(4) . . ?
C4 C3 H3A 120.0 . . ?
C2 C3 H3A 120.0 . . ?
C3 C4 C5 119.7(4) . . ?
C3 C4 C13 119.4(4) . . ?
C5 C4 C13 120.9(4) . . ?
C4 C5 C6 120.9(4) . . ?
C4 C5 H5A 119.6 . . ?
C6 C5 H5A 119.6 . . ?
C5 C6 C7 118.9(4) . . ?
C5 C6 C8 121.2(4) . . ?
C7 C6 C8 119.8(4) . . ?
C2 C7 C6 120.5(4) . . ?
C2 C7 H7A 119.8 . . ?
C6 C7 H7A 119.8 . . ?
C12 C8 C9 117.3(5) . . ?
C12 C8 C6 121.7(5) . . ?
C9 C8 C6 121.0(5) . . ?
C8 C9 C10 119.1(5) . . ?
C8 C9 H9A 120.5 . . ?
C10 C9 H9A 120.5 . . ?
N1 C10 C9 123.3(6) . . ?
N1 C10 H10A 118.3 . . ?
C9 C10 H10A 118.3 . . ?
N1 C11 C12 123.6(6) . . ?
N1 C11 H11A 118.2 . . ?
C12 C11 H11A 118.2 . . ?
C8 C12 C11 119.7(6) . . ?
C8 C12 H12A 120.2 . . ?
C11 C12 H12A 120.2 . . ?
O4 C13 O3 126.7(4) . . ?
O4 C13 C4 117.2(4) . . ?
O3 C13 C4 116.2(4) . . ?
C14 O5 Dy1 91.7(9) . . ?
O7 O6 C14 142(3) 3_666 . ?
O7 O6 C26 3(2) 3_666 3_666 ?
C14 O6 C26 142.1(11) . 3_666 ?
O7 O6 Dy1 81(3) 3_666 . ?
C14 O6 Dy1 93.2(7) . . ?
C26 O6 Dy1 83.0(5) 3_666 . ?
O6 O7 C26 176(3) 3_666 . ?
O6 O7 C14 27(2) 3_666 3_666 ?
C26 O7 C14 152.2(10) . 3_666 ?
O6 O7 Dy1 88(3) 3_666 3_666 ?
C26 O7 Dy1 95.7(6) . 3_666 ?
C14 O7 Dy1 84.7(5) 3_666 3_666 ?
C26 O8 Dy1 89.1(10) . 3_666 ?
O5 C14 O6 122.1(11) . . ?
O5 C14 C15 118.3(9) . . ?
O6 C14 C15 119.6(8) . . ?
O5 C14 O7 119.4(10) . 3_666 ?
O6 C14 O7 10.4(9) . 3_666 ?
C15 C14 O7 121.2(6) . 3_666 ?
O5 C14 Dy1 61.8(8) . . ?
O6 C14 Dy1 60.3(7) . . ?
C15 C14 Dy1 179.6(6) . . ?
O7 C14 Dy1 58.8(4) 3_666 . ?
C16 C15 C20 120.0 . . ?
C16 C15 C14 121.2(4) . . ?
C20 C15 C14 118.8(4) . . ?
C15 C16 C17 120.0 . . ?
C18 C17 C16 120.0 . . ?
C18 C17 C26 118.8(4) . . ?
C16 C17 C26 121.2(4) . . ?
C17 C18 C19 120.0 . . ?
C17 C18 H18A 120.0 . . ?
C19 C18 H18A 120.0 . . ?
C18 C19 C20 120.0 . . ?
C18 C19 C21 120.2(5) . . ?
C20 C19 C21 119.7(5) . . ?
C18 C19 C24 164.7(6) . 3_667 ?
C20 C19 C24 72.0(6) . 3_667 ?
C21 C19 C24 48.4(6) . 3_667 ?
C19 C20 C15 120.0 . . ?
C19 C20 N2 106.1(5) . 3_667 ?
C15 C20 N2 133.9(5) . 3_667 ?
C19 C20 C24 60.7(5) . 3_667 ?
C15 C20 C24 171.0(5) . 3_667 ?
N2 C20 C24 46.4(6) 3_667 3_667 ?
C19 C20 H20A 120.0 . . ?
C15 C20 H20A 120.0 . . ?
N2 C20 H20A 13.9 3_667 . ?
C24 C20 H20A 60.1 3_667 . ?
C24 C21 C22 154.1(9) 3_667 . ?
C24 C21 C25 55.6(9) 3_667 . ?
C22 C21 C25 116.0(10) . . ?
C24 C21 C25 59.5(10) 3_667 3_667 ?
C22 C21 C25 102.9(9) . 3_667 ?
C25 C21 C25 23.2(8) . 3_667 ?
C24 C21 C19 71.4(7) 3_667 . ?
C22 C21 C19 122.6(8) . . ?
C25 C21 C19 121.4(9) . . ?
C25 C21 C19 130.9(9) 3_667 . ?
C21 C22 C23 122.2(11) . . ?
C21 C22 H22A 119.1 . . ?
C23 C22 H22A 118.8 . . ?
C23 N2 C24 116.1(11) . . ?
C23 N2 C20 164.2(12) . 3_667 ?
C24 N2 C20 77.0(10) . 3_667 ?
N2 C23 C22 122.1(13) . . ?
N2 C23 H23A 119.7 . . ?
C22 C23 H23A 118.2 . . ?
C25 C24 C21 66.7(12) 3_667 3_667 ?
C25 C24 N2 115.4(13) 3_667 . ?
C21 C24 N2 154.3(10) 3_667 . ?
C25 C24 C25 25.0(9) 3_667 . ?
C21 C24 C25 67.5(11) 3_667 . ?
N2 C24 C25 126.1(13) . . ?
C25 C24 C19 121.2(15) 3_667 3_667 ?
C21 C24 C19 60.2(8) 3_667 3_667 ?
N2 C24 C19 102.9(10) . 3_667 ?
C25 C24 C19 127.7(13) . 3_667 ?
C25 C24 C20 147.9(14) 3_667 3_667 ?
C21 C24 C20 107.0(10) 3_667 3_667 ?
N2 C24 C20 56.5(9) . 3_667 ?
C25 C24 C20 171.8(10) . 3_667 ?
C19 C24 C20 47.3(3) 3_667 3_667 ?
C25 C24 H24A 122.0 3_667 . ?
C21 C24 H24A 55.3 3_667 . ?
N2 C24 H24A 116.7 . . ?
C25 C24 H24A 117.1 . . ?
C19 C24 H24A 22.9 3_667 . ?
C20 C24 H24A 60.8 3_667 . ?
C25 C25 C24 90(3) 3_667 3_667 ?
C25 C25 C24 65(3) 3_667 . ?
C24 C25 C24 155.0(9) 3_667 . ?
C25 C25 C21 87(4) 3_667 . ?
C24 C25 C21 57.7(10) 3_667 . ?
C24 C25 C21 117.5(14) . . ?
C25 C25 C21 70(4) 3_667 3_667 ?
C24 C25 C21 120.2(15) 3_667 3_667 ?
C24 C25 C21 53.0(9) . 3_667 ?
C21 C25 C21 156.8(8) . 3_667 ?
C25 C25 H25A 117.3 3_667 . ?
C24 C25 H25A 69.0 3_667 . ?
C24 C25 H25A 121.3 . . ?
C21 C25 H25A 121.3 . . ?
C21 C25 H25A 72.2 3_667 . ?
O8 C26 O7 122.0(12) . . ?
O8 C26 C17 117.9(10) . . ?
O7 C26 C17 120.1(7) . . ?
O8 C26 O6 123.0(11) . 3_666 ?
O7 C26 O6 1.0(9) . 3_666 ?
C17 C26 O6 119.1(6) . 3_666 ?
O8 C26 Dy1 64.7(9) . 3_666 ?
O7 C26 Dy1 57.9(6) . 3_666 ?
C17 C26 Dy1 174.2(5) . 3_666 ?
O6 C26 Dy1 58.8(5) 3_666 3_666 ?
C27 N3 C28 114.9(13) . . ?
C27 N3 C29 121.5(13) . . ?
C28 N3 C29 123.4(12) . . ?
O15 C27 N3 120.8(12) . . ?
O15 C27 H27A 119.6 . . ?
N3 C27 H27A 119.6 . . ?
N3 C28 H28A 109.5 . . ?
N3 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
N3 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N3 C29 H29A 109.5 . . ?
N3 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
N3 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.467
_refine_diff_density_min         -0.680
_refine_diff_density_rms         0.113
####################################################################### 
# 
# 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_Compound_1
_database_code_depnum_ccdc_archive 'CCDC 1010482'
_audit_update_record             
;
2014-06-26 deposited with the CCDC.
2015-01-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H50 N5 O22 Sm2'
_chemical_formula_weight         1313.60

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

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   13.4721(6)
_cell_length_b                   14.8138(7)
_cell_length_c                   13.4131(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.142(3)
_cell_angle_gamma                90.00
_cell_volume                     2642.9(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    7595
_cell_measurement_theta_min      2.0576
_cell_measurement_theta_max      27.4779

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.2000
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1310
_exptl_absorpt_coefficient_mu    2.282
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8056
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21479
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_sigmaI/netI    0.0667
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.71
_diffrn_reflns_theta_max         27.45
_reflns_number_total             5978
_reflns_number_gt                4651
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0300P)²+6.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5978
_refine_ls_number_parameters     423
_refine_ls_number_restraints     382
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0411
_refine_ls_wR_factor_ref         0.0989
_refine_ls_wR_factor_gt          0.0959
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.077
_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
Sm1 Sm 0.137983(17) 0.438329(17) 0.508184(19) 0.01797(8) Uani 1 1 d . . .
O1 O -0.0473(3) 0.4386(3) 0.5759(3) 0.0364(10) Uani 1 1 d . . .
O2 O 0.0671(3) 0.3354(4) 0.6184(4) 0.0675(17) Uani 1 1 d . A .
O3 O 0.0091(3) 0.1311(3) 0.8927(3) 0.0445(12) Uani 1 1 d . . .
O4 O -0.1400(3) 0.0606(3) 0.8754(3) 0.0457(12) Uani 1 1 d . . .
O9 O 0.2184(3) 0.2936(3) 0.4830(4) 0.0484(12) Uani 1 1 d . A .
N1 N -0.5802(4) 0.2679(4) 0.5536(5) 0.0576(17) Uani 1 1 d . A .
C1 C -0.0208(4) 0.3640(4) 0.6154(5) 0.0383(15) Uani 1 1 d . . .
C2 C -0.0936(4) 0.3058(4) 0.6579(5) 0.0392(15) Uani 1 1 d . A .
C3 C -0.0575(4) 0.2437(4) 0.7326(5) 0.0409(16) Uani 1 1 d . . .
H3A H 0.0127 0.2396 0.7559 0.049 Uiso 1 1 calc R A .
C4 C -0.1232(4) 0.1877(4) 0.7733(4) 0.0379(15) Uani 1 1 d . A .
C5 C -0.2262(4) 0.1916(5) 0.7368(5) 0.0420(16) Uani 1 1 d . . .
H5A H -0.2707 0.1513 0.7627 0.050 Uiso 1 1 calc R A .
C6 C -0.2641(4) 0.2539(5) 0.6628(5) 0.0414(16) Uani 1 1 d . A .
C7 C -0.1967(4) 0.3112(5) 0.6232(5) 0.0415(15) Uani 1 1 d . . .
H7A H -0.2215 0.3538 0.5724 0.050 Uiso 1 1 calc R A .
C8 C -0.3741(4) 0.2587(5) 0.6235(5) 0.0429(16) Uani 1 1 d . . .
C9 C -0.4429(5) 0.2444(6) 0.6868(6) 0.060(2) Uani 1 1 d . A .
H9A H -0.4208 0.2307 0.7559 0.071 Uiso 1 1 calc R . .
C10 C -0.5449(5) 0.2500(6) 0.6499(7) 0.064(2) Uani 1 1 d . . .
H10A H -0.5915 0.2406 0.6952 0.077 Uiso 1 1 calc R A .
C11 C -0.5141(5) 0.2804(5) 0.4944(6) 0.060(2) Uani 1 1 d . . .
H11A H -0.5381 0.2928 0.4252 0.072 Uiso 1 1 calc R A .
C12 C -0.4115(5) 0.2771(5) 0.5247(6) 0.060(2) Uani 1 1 d . A .
H12A H -0.3671 0.2874 0.4775 0.072 Uiso 1 1 calc R . .
C13 C -0.0818(4) 0.1205(4) 0.8531(5) 0.0395(15) Uani 1 1 d . . .
O5 O 0.2798(13) 0.4228(13) 0.6575(16) 0.032(3) Uani 0.50 1 d PDU A 1
O6 O 0.3134(10) 0.4942(11) 0.5229(6) 0.033(3) Uani 0.50 1 d PDU . 1
O7 O 0.6948(10) 0.5040(11) 0.5161(6) 0.028(2) Uani 0.50 1 d PDU . 1
O8 O 0.7913(8) 0.5450(9) 0.6581(9) 0.022(2) Uani 0.50 1 d PDU . 1
C14 C 0.3377(7) 0.4680(7) 0.6126(6) 0.029(2) Uani 0.50 1 d PDU . 1
C15 C 0.4422(4) 0.4849(5) 0.6668(5) 0.024(2) Uani 0.50 1 d PGU B 1
C16 C 0.5222(5) 0.4963(6) 0.6141(3) 0.024(2) Uani 0.50 1 d PGU B 1
C17 C 0.6183(4) 0.5118(6) 0.6662(4) 0.019(2) Uani 0.50 1 d PGU B 1
C18 C 0.6345(4) 0.5159(6) 0.7711(4) 0.029(2) Uani 0.50 1 d PGU B 1
H18A H 0.7019 0.5267 0.8077 0.035 Uiso 0.50 1 d PR B 1
C19 C 0.5545(5) 0.5045(5) 0.8238(3) 0.031(2) Uani 0.50 1 d PGU . 1
C20 C 0.4583(4) 0.4890(6) 0.7716(5) 0.028(2) Uani 0.50 1 d PGU . 1
H20A H 0.4025 0.4811 0.8079 0.034 Uiso 0.50 1 d PR B 1
C21 C 0.5731(7) 0.5120(7) 0.9366(8) 0.038(2) Uani 0.50 1 d PDU . 1
C22 C 0.6590(10) 0.5534(8) 0.9871(10) 0.053(3) Uani 0.50 1 d PDU C 1
H22A H 0.7109 0.5750 0.9515 0.064 Uiso 0.50 1 d PR C 1
N2 N 0.6079(10) 0.5221(8) 1.1501(9) 0.071(3) Uani 0.50 1 d PDU . 1
C23 C 0.6746(13) 0.5575(9) 1.0947(12) 0.071(4) Uani 0.50 1 d PDU C 1
H23A H 0.7379 0.5814 1.1283 0.085 Uiso 0.50 1 d PR C 1
C24 C 0.5257(12) 0.4825(9) 1.0998(11) 0.067(3) Uani 0.50 1 d PDU . 1
H24A H 0.4757 0.4616 1.1384 0.080 Uiso 0.50 1 d PR . 1
C25 C 0.5063(15) 0.4764(9) 0.9955(15) 0.054(3) Uani 0.50 1 d PDU . 1
H25A H 0.4430 0.4515 0.9633 0.065 Uiso 0.50 1 d PR . 1
C26 C 0.7069(6) 0.5241(7) 0.6092(6) 0.024(2) Uani 0.50 1 d PDU . 1
O10 O 0.2561(14) 0.3985(14) 0.6639(17) 0.044(4) Uani 0.50 1 d P A 2
O11 O 0.4301(9) 0.5555(10) 0.6569(9) 0.088(4) Uani 0.50 1 d P D 2
O12 O 0.2251(6) 0.2263(8) 0.7395(10) 0.253(8) Uani 1 1 d . E 2
O13 O 0.1842(14) 0.0682(13) 0.8468(16) 0.072(6) Uani 0.50 1 d P . 2
O14 O 0.3779(18) 0.000(3) 0.827(2) 0.245(14) Uani 0.50 1 d P F 2
O15 O 0.1134(9) 0.1374(8) 0.4479(11) 0.207(5) Uani 1 1 d DU . .
N3 N -0.0428(10) 0.0801(9) 0.3958(11) 0.172(5) Uani 1 1 d DU . .
C27 C 0.0202(10) 0.1457(12) 0.4526(14) 0.181(6) Uani 1 1 d DU . .
H27A H -0.0054 0.1918 0.4908 0.217 Uiso 1 1 calc R . .
C28 C -0.1393(12) 0.1022(13) 0.4288(16) 0.233(7) Uani 1 1 d DU . .
H28A H -0.1472 0.1680 0.4307 0.349 Uiso 1 1 calc R . .
H28B H -0.1402 0.0773 0.4963 0.349 Uiso 1 1 calc R . .
H28C H -0.1947 0.0762 0.3812 0.349 Uiso 1 1 calc R . .
C29 C -0.0086(14) -0.0020(12) 0.3461(13) 0.204(7) Uani 1 1 d DU . .
H29A H 0.0647 -0.0073 0.3628 0.306 Uiso 1 1 calc R . .
H29B H -0.0279 0.0031 0.2727 0.306 Uiso 1 1 calc R . .
H29C H -0.0402 -0.0557 0.3701 0.306 Uiso 1 1 calc R . .


_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 O13 2.35(2) 4_565 ?
Sm1 O3 2.370(4) 4_565 ?
Sm1 O1 2.377(4) 3_566 ?
Sm1 O4 2.389(4) 2_556 ?
Sm1 O2 2.423(4) . ?
Sm1 O9 2.450(4) . ?
Sm1 O7 2.479(14) 3_666 ?
Sm1 O6 2.483(14) . ?
Sm1 O10 2.49(2) . ?
Sm1 O5 2.55(2) . ?
Sm1 O8 2.572(12) 3_666 ?
Sm1 O1 2.788(4) . ?
O1 C1 1.252(7) . ?
O1 Sm1 2.377(4) 3_566 ?
O2 C1 1.253(7) . ?
O3 C13 1.264(6) . ?
O3 Sm1 2.370(4) 4_566 ?
O4 C13 1.252(7) . ?
O4 Sm1 2.389(4) 2_546 ?
N1 C11 1.298(9) . ?
N1 C10 1.331(9) . ?
C1 C2 1.486(8) . ?
C2 C3 1.389(7) . ?
C2 C7 1.395(7) . ?
C3 C4 1.387(7) . ?
C3 H3A 0.9500 . ?
C4 C5 1.397(7) . ?
C4 C13 1.502(8) . ?
C5 C6 1.392(8) . ?
C5 H5A 0.9500 . ?
C6 C7 1.408(8) . ?
C6 C8 1.494(7) . ?
C7 H7A 0.9500 . ?
C8 C9 1.369(9) . ?
C8 C12 1.368(9) . ?
C9 C10 1.387(8) . ?
C9 H9A 0.9500 . ?
C10 H10A 0.9500 . ?
C11 C12 1.379(9) . ?
C11 H11A 0.9500 . ?
C12 H12A 0.9500 . ?
O5 C14 1.254(9) . ?
O6 O7 0.518(9) 3_666 ?
O6 C14 1.257(8) . ?
O6 C26 1.770(12) 3_666 ?
O7 O6 0.518(9) 3_666 ?
O7 C26 1.268(8) . ?
O7 C14 1.762(12) 3_666 ?
O7 Sm1 2.479(14) 3_666 ?
O8 C26 1.258(9) . ?
O8 Sm1 2.572(12) 3_666 ?
C14 C15 1.499(10) . ?
C14 O7 1.762(12) 3_666 ?
C15 C16 1.3900 . ?
C15 C20 1.3900 . ?
C16 C17 1.3900 . ?
C17 C18 1.3900 . ?
C17 C26 1.527(10) . ?
C18 C19 1.3900 . ?
C18 H18A 0.9746 . ?
C19 C20 1.3900 . ?
C19 C21 1.499(12) . ?
C19 C24 1.614(16) 3_667 ?
C20 N2 1.491(14) 3_667 ?
C20 C24 1.756(16) 3_667 ?
C20 H20A 0.9661 . ?
C21 C24 1.345(18) 3_667 ?
C21 C22 1.386(16) . ?
C21 C25 1.39(2) . ?
C21 C25 1.52(2) 3_667 ?
C22 C23 1.426(19) . ?
C22 H22A 0.9629 . ?
N2 C24 1.34(2) . ?
N2 C23 1.36(2) . ?
N2 C20 1.49(2) 3_667 ?
C23 H23A 0.9661 . ?
C24 C21 1.345(18) 3_667 ?
C24 C25 1.38(2) . ?
C24 C25 1.42(2) 3_667 ?
C24 C19 1.614(19) 3_667 ?
C24 C20 1.756(17) 3_667 ?
C24 H24A 0.9626 . ?
C25 C25 0.74(2) 3_667 ?
C25 C24 1.42(2) 3_667 ?
C25 C21 1.52(2) 3_667 ?
C25 H25A 0.9662 . ?
C26 O6 1.770(12) 3_666 ?
C26 Sm1 2.864(9) 3_666 ?
O13 Sm1 2.35(2) 4_566 ?
O15 C27 1.274(9) . ?
N3 C27 1.428(19) . ?
N3 C28 1.476(9) . ?
N3 C29 1.494(9) . ?
C27 H27A 0.9500 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?

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
O13 Sm1 O3 69.7(4) 4_565 4_565 ?
O13 Sm1 O1 77.6(5) 4_565 3_566 ?
O3 Sm1 O1 75.80(15) 4_565 3_566 ?
O13 Sm1 O4 131.1(4) 4_565 2_556 ?
O3 Sm1 O4 133.41(13) 4_565 2_556 ?
O1 Sm1 O4 71.33(15) 3_566 2_556 ?
O13 Sm1 O2 136.4(4) 4_565 . ?
O3 Sm1 O2 78.88(19) 4_565 . ?
O1 Sm1 O2 123.32(14) 3_566 . ?
O4 Sm1 O2 92.5(2) 2_556 . ?
O13 Sm1 O9 69.4(5) 4_565 . ?
O3 Sm1 O9 79.88(13) 4_565 . ?
O1 Sm1 O9 144.21(15) 3_566 . ?
O4 Sm1 O9 142.61(14) 2_556 . ?
O2 Sm1 O9 76.06(17) . . ?
O13 Sm1 O7 60.9(4) 4_565 3_666 ?
O3 Sm1 O7 130.5(2) 4_565 3_666 ?
O1 Sm1 O7 94.8(4) 3_566 3_666 ?
O4 Sm1 O7 84.8(3) 2_556 3_666 ?
O2 Sm1 O7 138.7(3) . 3_666 ?
O9 Sm1 O7 81.5(4) . 3_666 ?
O13 Sm1 O6 72.4(4) 4_565 . ?
O3 Sm1 O6 141.8(3) 4_565 . ?
O1 Sm1 O6 101.1(3) 3_566 . ?
O4 Sm1 O6 77.5(4) 2_556 . ?
O2 Sm1 O6 128.6(3) . . ?
O9 Sm1 O6 82.3(4) . . ?
O7 Sm1 O6 12.0(2) 3_666 . ?
O13 Sm1 O10 122.4(7) 4_565 . ?
O3 Sm1 O10 138.6(4) 4_565 . ?
O1 Sm1 O10 142.4(5) 3_566 . ?
O4 Sm1 O10 72.0(6) 2_556 . ?
O2 Sm1 O10 66.4(3) . . ?
O9 Sm1 O10 70.7(6) . . ?
O7 Sm1 O10 73.7(4) 3_666 . ?
O6 Sm1 O10 62.5(4) . . ?
O13 Sm1 O5 116.4(6) 4_565 . ?
O3 Sm1 O5 148.7(4) 4_565 . ?
O1 Sm1 O5 135.0(5) 3_566 . ?
O4 Sm1 O5 68.0(5) 2_556 . ?
O2 Sm1 O5 77.4(3) . . ?
O9 Sm1 O5 74.7(5) . . ?
O7 Sm1 O5 63.3(3) 3_666 . ?
O6 Sm1 O5 51.9(3) . . ?
O10 Sm1 O5 11.2(4) . . ?
O13 Sm1 O8 10.1(5) 4_565 3_666 ?
O3 Sm1 O8 79.0(2) 4_565 3_666 ?
O1 Sm1 O8 75.4(3) 3_566 3_666 ?
O4 Sm1 O8 121.8(3) 2_556 3_666 ?
O2 Sm1 O8 145.6(3) . 3_666 ?
O9 Sm1 O8 74.4(4) . 3_666 ?
O7 Sm1 O8 51.9(2) 3_666 3_666 ?
O6 Sm1 O8 63.8(3) . 3_666 ?
O10 Sm1 O8 118.4(5) . 3_666 ?
O5 Sm1 O8 110.8(4) . 3_666 ?
O13 Sm1 O1 133.1(5) 4_565 . ?
O3 Sm1 O1 67.22(14) 4_565 . ?
O1 Sm1 O1 74.57(13) 3_566 . ?
O4 Sm1 O1 72.78(14) 2_556 . ?
O2 Sm1 O1 48.87(13) . . ?
O9 Sm1 O1 118.98(14) . . ?
O7 Sm1 O1 157.2(3) 3_666 . ?
O6 Sm1 O1 149.8(3) . . ?
O10 Sm1 O1 102.3(5) . . ?
O5 Sm1 O1 110.0(4) . . ?
O8 Sm1 O1 139.1(3) 3_666 . ?
C1 O1 Sm1 165.4(4) . 3_566 ?
C1 O1 Sm1 85.9(3) . . ?
Sm1 O1 Sm1 105.43(13) 3_566 . ?
C1 O2 Sm1 103.3(4) . . ?
C13 O3 Sm1 141.3(4) . 4_566 ?
C13 O4 Sm1 138.7(4) . 2_546 ?
C11 N1 C10 116.7(6) . . ?
O1 C1 O2 121.0(5) . . ?
O1 C1 C2 120.9(5) . . ?
O2 C1 C2 118.0(5) . . ?
O1 C1 Sm1 69.3(3) . . ?
O2 C1 Sm1 52.5(3) . . ?
C2 C1 Sm1 165.9(5) . . ?
C3 C2 C7 119.6(5) . . ?
C3 C2 C1 119.0(5) . . ?
C7 C2 C1 121.4(5) . . ?
C4 C3 C2 120.6(5) . . ?
C4 C3 H3A 119.7 . . ?
C2 C3 H3A 119.7 . . ?
C3 C4 C5 119.8(5) . . ?
C3 C4 C13 119.3(5) . . ?
C5 C4 C13 120.8(5) . . ?
C6 C5 C4 120.6(5) . . ?
C6 C5 H5A 119.7 . . ?
C4 C5 H5A 119.7 . . ?
C5 C6 C7 118.9(5) . . ?
C5 C6 C8 121.0(5) . . ?
C7 C6 C8 120.1(5) . . ?
C2 C7 C6 120.4(5) . . ?
C2 C7 H7A 119.8 . . ?
C6 C7 H7A 119.8 . . ?
C9 C8 C12 116.7(6) . . ?
C9 C8 C6 120.4(6) . . ?
C12 C8 C6 122.9(6) . . ?
C8 C9 C10 120.0(7) . . ?
C8 C9 H9A 120.0 . . ?
C10 C9 H9A 120.0 . . ?
N1 C10 C9 122.6(7) . . ?
N1 C10 H10A 118.7 . . ?
C9 C10 H10A 118.7 . . ?
N1 C11 C12 124.6(7) . . ?
N1 C11 H11A 117.7 . . ?
C12 C11 H11A 117.7 . . ?
C8 C12 C11 119.4(7) . . ?
C8 C12 H12A 120.3 . . ?
C11 C12 H12A 120.3 . . ?
O4 C13 O3 126.1(5) . . ?
O4 C13 C4 117.6(5) . . ?
O3 C13 C4 116.2(5) . . ?
C14 O5 Sm1 91.1(12) . . ?
O7 O6 C14 165(4) 3_666 . ?
O7 O6 C26 12(3) 3_666 3_666 ?
C14 O6 C26 152.4(14) . 3_666 ?
O7 O6 Sm1 84(3) 3_666 . ?
C14 O6 Sm1 94.2(8) . . ?
C26 O6 Sm1 82.8(6) 3_666 . ?
O6 O7 C26 163(4) 3_666 . ?
O6 O7 C14 11(3) 3_666 3_666 ?
C26 O7 C14 152.0(14) . 3_666 ?
O6 O7 Sm1 84(3) 3_666 3_666 ?
C26 O7 Sm1 94.1(8) . 3_666 ?
C14 O7 Sm1 83.1(6) 3_666 3_666 ?
C26 O8 Sm1 90.0(7) . 3_666 ?
O5 C14 O6 122.6(15) . . ?
O5 C14 C15 117.7(11) . . ?
O6 C14 C15 119.6(10) . . ?
O5 C14 O7 121.3(13) . 3_666 ?
O6 C14 O7 4.5(12) . 3_666 ?
C15 C14 O7 120.2(8) . 3_666 ?
O5 C14 Sm1 62.9(11) . . ?
O6 C14 Sm1 59.9(8) . . ?
C15 C14 Sm1 179.2(7) . . ?
O7 C14 Sm1 59.3(5) 3_666 . ?
C16 C15 C20 120.0 . . ?
C16 C15 C14 121.2(5) . . ?
C20 C15 C14 118.8(5) . . ?
C17 C16 C15 120.0 . . ?
C16 C17 C18 120.0 . . ?
C16 C17 C26 120.5(5) . . ?
C18 C17 C26 119.5(5) . . ?
C17 C18 C19 120.0 . . ?
C17 C18 H18A 120.0 . . ?
C19 C18 H18A 120.0 . . ?
C18 C19 C20 120.0 . . ?
C18 C19 C21 119.0(6) . . ?
C20 C19 C21 120.9(5) . . ?
C18 C19 C24 163.6(7) . 3_667 ?
C20 C19 C24 71.1(7) . 3_667 ?
C21 C19 C24 51.1(6) . 3_667 ?
C19 C20 C15 120.0 . . ?
C19 C20 N2 106.1(6) . 3_667 ?
C15 C20 N2 133.9(6) . 3_667 ?
C19 C20 C24 60.4(6) . 3_667 ?
C15 C20 C24 168.4(6) . 3_667 ?
N2 C20 C24 47.8(7) 3_667 3_667 ?
C19 C20 H20A 120.3 . . ?
C15 C20 H20A 119.7 . . ?
N2 C20 H20A 14.2 3_667 . ?
C24 C20 H20A 61.2 3_667 . ?
C24 C21 C22 148.2(10) 3_667 . ?
C24 C21 C25 62.5(11) 3_667 . ?
C22 C21 C25 117.1(13) . . ?
C24 C21 C19 68.9(8) 3_667 . ?
C22 C21 C19 121.2(10) . . ?
C25 C21 C19 121.6(11) . . ?
C24 C21 C25 57.4(11) 3_667 3_667 ?
C22 C21 C25 105.6(11) . 3_667 ?
C25 C21 C25 28.8(9) . 3_667 ?
C19 C21 C25 126.3(10) . 3_667 ?
C21 C22 C23 119.4(14) . . ?
C21 C22 H22A 121.4 . . ?
C23 C22 H22A 119.0 . . ?
C24 N2 C23 117.4(13) . . ?
C24 N2 C20 76.5(13) . 3_667 ?
C23 N2 C20 161.7(15) . 3_667 ?
N2 C23 C22 122.2(15) . . ?
N2 C23 H23A 119.7 . . ?
C22 C23 H23A 117.8 . . ?
N2 C24 C21 148.1(10) . 3_667 ?
N2 C24 C25 123.1(16) . . ?
C21 C24 C25 67.7(12) 3_667 . ?
N2 C24 C25 112.0(14) . 3_667 ?
C21 C24 C25 60.4(12) 3_667 3_667 ?
C25 C24 C25 30.4(9) . 3_667 ?
N2 C24 C19 102.2(13) . 3_667 ?
C21 C24 C19 60.0(10) 3_667 3_667 ?
C25 C24 C19 127.7(14) . 3_667 ?
C25 C24 C19 112.5(15) 3_667 3_667 ?
N2 C24 C20 55.7(11) . 3_667 ?
C21 C24 C20 107.6(13) 3_667 3_667 ?
C25 C24 C20 169.2(13) . 3_667 ?
C25 C24 C20 138.9(16) 3_667 3_667 ?
C19 C24 C20 48.5(5) 3_667 3_667 ?
N2 C24 H24A 117.6 . . ?
C21 C24 H24A 58.6 3_667 . ?
C25 C24 H24A 119.1 . . ?
C25 C24 H24A 118.9 3_667 . ?
C19 C24 H24A 26.1 3_667 . ?
C20 C24 H24A 62.4 3_667 . ?
C25 C25 C24 77(3) 3_667 . ?
C25 C25 C21 85(3) 3_667 . ?
C24 C25 C21 120.9(17) . . ?
C25 C25 C24 72(3) 3_667 3_667 ?
C24 C25 C24 149.6(9) . 3_667 ?
C21 C25 C24 57.2(10) . 3_667 ?
C25 C25 C21 66(3) 3_667 3_667 ?
C24 C25 C21 54.9(10) . 3_667 ?
C21 C25 C21 151.2(9) . 3_667 ?
C24 C25 C21 110.4(14) 3_667 3_667 ?
C25 C25 H25A 103.0 3_667 . ?
C24 C25 H25A 119.1 . . ?
C21 C25 H25A 119.8 . . ?
C24 C25 H25A 69.0 3_667 . ?
C21 C25 H25A 69.8 3_667 . ?
O8 C26 O7 122.3(11) . . ?
O8 C26 C17 118.8(8) . . ?
O7 C26 C17 118.5(9) . . ?
O8 C26 O6 122.9(10) . 3_666 ?
O7 C26 O6 4.9(12) . 3_666 ?
C17 C26 O6 118.3(7) . 3_666 ?
O8 C26 Sm1 63.9(7) . 3_666 ?
O7 C26 Sm1 59.7(7) . 3_666 ?
C17 C26 Sm1 174.3(7) . 3_666 ?
O6 C26 Sm1 59.3(5) 3_666 3_666 ?
C27 N3 C28 99.5(15) . . ?
C27 N3 C29 126.4(14) . . ?
C28 N3 C29 131.6(15) . . ?
O15 C27 N3 114.4(16) . . ?
O15 C27 H27A 122.8 . . ?
N3 C27 H27A 122.8 . . ?
N3 C28 H28A 109.5 . . ?
N3 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
N3 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N3 C29 H29A 109.5 . . ?
N3 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
N3 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        27.45
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         1.580
_refine_diff_density_min         -1.097
_refine_diff_density_rms         0.137
