# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014


data_Sm2
_database_code_depnum_ccdc_archive 'CCDC 972393'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H48 N6 O16 S2 Sm2'
_chemical_formula_weight         1209.64

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.447(3)
_cell_length_b                   10.886(3)
_cell_length_c                   11.875(3)
_cell_angle_alpha                69.437(5)
_cell_angle_beta                 84.878(5)
_cell_angle_gamma                79.669(5)
_cell_volume                     1243.4(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2530
_cell_measurement_theta_min      2.74
_cell_measurement_theta_max      23.61

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             602
_exptl_absorpt_coefficient_mu    2.491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6914
_exptl_absorpt_correction_T_max  0.8069
_exptl_absorpt_process_details   '(Sadabs; Bruker,2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6294
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0767
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         25.04
_reflns_number_total             4328
_reflns_number_gt                3354
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0732P)²+0.4773P] 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         4328
_refine_ls_number_parameters     295
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0520
_refine_ls_wR_factor_ref         0.1432
_refine_ls_wR_factor_gt          0.1288
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_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
Sm1 Sm 0.48213(4) 0.14861(4) 0.33068(4) 0.03613(18) Uani 1 1 d . . .
N3 N 0.3871(6) 0.3891(7) 0.3290(6) 0.0378(16) Uani 1 1 d . . .
N2 N 0.2596(6) 0.4345(7) 0.2904(6) 0.0424(17) Uani 1 1 d . . .
H2A H 0.2205 0.5125 0.2860 0.051 Uiso 1 1 calc R . .
N1 N -0.1220(7) 0.5527(8) 0.1362(7) 0.052(2) Uani 1 1 d . . .
O2 O 0.6067(6) 0.2187(5) 0.4426(5) 0.0456(15) Uani 1 1 d . . .
O1 O 0.2539(6) 0.2347(6) 0.2732(6) 0.0503(15) Uani 1 1 d . . .
O7 O 0.3971(7) -0.0489(6) 0.3319(5) 0.0549(17) Uani 1 1 d . . .
H7A H 0.4315 -0.1277 0.3905 0.066 Uiso 1 1 calc R . .
O3 O 0.4734(6) 0.1759(6) 0.1133(5) 0.0526(16) Uani 1 1 d U . .
O4 O 0.5728(6) 0.3173(6) 0.1534(5) 0.0528(16) Uani 1 1 d . . .
O6 O 0.6248(5) -0.0640(5) 0.4724(5) 0.0394(13) Uani 1 1 d . . .
O5 O 0.7028(6) 0.0380(6) 0.2932(5) 0.0542(16) Uani 1 1 d . . .
O8 O 0.2816(9) 0.2042(8) 0.9566(7) 0.083(2) Uani 1 1 d . . .
H8 H 0.2778 0.2796 0.9074 0.125 Uiso 1 1 calc R . .
S1 S 0.0492(3) 0.6638(3) 0.1982(3) 0.0657(7) Uani 1 1 d . . .
H1 H 0.0246 0.7593 0.1095 0.099 Uiso 1 1 calc R . .
C13 C 0.6511(8) 0.3289(8) 0.4277(7) 0.038(2) Uani 1 1 d . . .
C12 C 0.7787(9) 0.3214(10) 0.4641(8) 0.053(2) Uani 1 1 d . . .
H12 H 0.8307 0.2390 0.4955 0.064 Uiso 1 1 calc R . .
C11 C 0.8278(10) 0.4391(12) 0.4530(9) 0.062(3) Uani 1 1 d . . .
H11 H 0.9117 0.4325 0.4772 0.074 Uiso 1 1 calc R . .
C10 C 0.7552(11) 0.5595(11) 0.4081(9) 0.059(3) Uani 1 1 d . . .
H10 H 0.7887 0.6356 0.4007 0.071 Uiso 1 1 calc R . .
C9 C 0.6313(10) 0.5689(9) 0.3733(8) 0.050(2) Uani 1 1 d . . .
H9 H 0.5809 0.6525 0.3436 0.060 Uiso 1 1 calc R . .
C8 C 0.5778(9) 0.4568(8) 0.3810(6) 0.039(2) Uani 1 1 d . . .
C7 C 0.4436(8) 0.4777(8) 0.3444(7) 0.039(2) Uani 1 1 d . . .
H7 H 0.3950 0.5617 0.3312 0.047 Uiso 1 1 calc R . .
C6 C 0.2009(8) 0.3517(9) 0.2607(7) 0.040(2) Uani 1 1 d . . .
C1 C 0.0660(8) 0.4001(9) 0.2117(7) 0.042(2) Uani 1 1 d . . .
C5 C -0.0009(9) 0.5326(9) 0.1827(8) 0.048(2) Uani 1 1 d . . .
C4 C -0.1829(9) 0.4594(11) 0.1253(9) 0.060(3) Uani 1 1 d . . .
H4 H -0.2674 0.4815 0.0979 0.072 Uiso 1 1 calc R . .
C3 C -0.1216(10) 0.3352(12) 0.1540(10) 0.068(3) Uani 1 1 d . . .
H3 H -0.1624 0.2702 0.1450 0.081 Uiso 1 1 calc R . .
C2 C 0.0068(8) 0.3017(10) 0.1987(9) 0.053(2) Uani 1 1 d . . .
H2 H 0.0505 0.2148 0.2189 0.064 Uiso 1 1 calc R . .
C16 C 0.3046(17) -0.0632(14) 0.2586(13) 0.118(6) Uani 1 1 d . . .
H16A H 0.2230 -0.0093 0.2660 0.177 Uiso 1 1 calc R . .
H16B H 0.2931 -0.1546 0.2841 0.177 Uiso 1 1 calc R . .
H16C H 0.3351 -0.0353 0.1763 0.177 Uiso 1 1 calc R . .
C14 C 0.5397(9) 0.2709(9) 0.0802(8) 0.047(2) Uani 1 1 d U . .
C17 C 0.5783(12) 0.3317(12) -0.0515(8) 0.076(3) Uani 1 1 d . . .
H17A H 0.5140 0.4066 -0.0900 0.114 Uiso 1 1 calc R . .
H17B H 0.5842 0.2667 -0.0900 0.114 Uiso 1 1 calc R . .
H17C H 0.6612 0.3603 -0.0577 0.114 Uiso 1 1 calc R . .
C15 C 0.7211(8) -0.0423(8) 0.3971(8) 0.044(2) Uani 1 1 d . . .
C18 C 0.8551(9) -0.1114(11) 0.4382(10) 0.071(3) Uani 1 1 d . . .
H18A H 0.8919 -0.1625 0.3883 0.107 Uiso 1 1 calc R . .
H18B H 0.8501 -0.1693 0.5202 0.107 Uiso 1 1 calc R . .
H18C H 0.9090 -0.0465 0.4322 0.107 Uiso 1 1 calc R . .
C19 C 0.3189(15) 0.1119(14) 0.8980(12) 0.108(5) Uani 1 1 d . . .
H19A H 0.4118 0.0862 0.9002 0.162 Uiso 1 1 calc R . .
H19B H 0.2928 0.1511 0.8158 0.162 Uiso 1 1 calc R . .
H19C H 0.2779 0.0350 0.9376 0.162 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 O2 2.328(5) . ?
Sm1 O6 2.440(5) 2_656 ?
Sm1 O1 2.463(6) . ?
Sm1 O7 2.465(6) . ?
Sm1 O5 2.482(6) . ?
Sm1 O4 2.501(6) . ?
Sm1 O3 2.501(6) . ?
Sm1 N3 2.622(7) . ?
Sm1 O6 2.624(5) . ?
N3 C7 1.288(10) . ?
N3 N2 1.394(9) . ?
N2 C6 1.331(11) . ?
N2 H2A 0.8600 . ?
N1 C4 1.338(12) . ?
N1 C5 1.376(11) . ?
O2 C13 1.312(9) . ?
O1 C6 1.257(10) . ?
O7 C16 1.419(15) . ?
O7 H7A 0.9300 . ?
O3 C14 1.275(10) . ?
O4 C14 1.246(11) . ?
O6 C15 1.283(10) . ?
O6 Sm1 2.440(5) 2_656 ?
O5 C15 1.244(10) . ?
O8 C19 1.396(13) . ?
O8 H8 0.8200 . ?
S1 C5 1.679(10) . ?
S1 H1 1.2000 . ?
C13 C8 1.408(12) . ?
C13 C12 1.418(12) . ?
C12 C11 1.424(14) . ?
C12 H12 0.9300 . ?
C11 C10 1.342(14) . ?
C11 H11 0.9300 . ?
C10 C9 1.369(13) . ?
C10 H10 0.9300 . ?
C9 C8 1.403(11) . ?
C9 H9 0.9300 . ?
C8 C7 1.461(12) . ?
C7 H7 0.9300 . ?
C6 C1 1.506(11) . ?
C1 C2 1.388(13) . ?
C1 C5 1.421(12) . ?
C4 C3 1.326(14) . ?
C4 H4 0.9300 . ?
C3 C2 1.425(13) . ?
C3 H3 0.9300 . ?
C2 H2 0.9300 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C14 C17 1.518(12) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C15 C18 1.500(12) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Sm1 O6 80.68(19) . 2_656 ?
O2 Sm1 O1 127.7(2) . . ?
O6 Sm1 O1 80.70(19) 2_656 . ?
O2 Sm1 O7 141.73(19) . . ?
O6 Sm1 O7 74.31(19) 2_656 . ?
O1 Sm1 O7 76.3(2) . . ?
O2 Sm1 O5 79.4(2) . . ?
O6 Sm1 O5 119.34(18) 2_656 . ?
O1 Sm1 O5 150.5(2) . . ?
O7 Sm1 O5 88.1(2) . . ?
O2 Sm1 O4 84.5(2) . . ?
O6 Sm1 O4 156.6(2) 2_656 . ?
O1 Sm1 O4 94.4(2) . . ?
O7 Sm1 O4 127.0(2) . . ?
O5 Sm1 O4 75.1(2) . . ?
O2 Sm1 O3 135.2(2) . . ?
O6 Sm1 O3 143.99(19) 2_656 . ?
O1 Sm1 O3 73.5(2) . . ?
O7 Sm1 O3 75.45(19) . . ?
O5 Sm1 O3 78.5(2) . . ?
O4 Sm1 O3 52.2(2) . . ?
O2 Sm1 N3 68.4(2) . . ?
O6 Sm1 N3 87.82(19) 2_656 . ?
O1 Sm1 N3 62.5(2) . . ?
O7 Sm1 N3 137.3(2) . . ?
O5 Sm1 N3 133.7(2) . . ?
O4 Sm1 N3 69.8(2) . . ?
O3 Sm1 N3 101.6(2) . . ?
O2 Sm1 O6 72.69(18) . . ?
O6 Sm1 O6 68.8(2) 2_656 . ?
O1 Sm1 O6 140.26(18) . . ?
O7 Sm1 O6 71.46(19) . . ?
O5 Sm1 O6 50.63(18) . . ?
O4 Sm1 O6 123.5(2) . . ?
O3 Sm1 O6 118.52(19) . . ?
N3 Sm1 O6 137.21(19) . . ?
C7 N3 N2 114.4(7) . . ?
C7 N3 Sm1 130.3(6) . . ?
N2 N3 Sm1 114.7(5) . . ?
C6 N2 N3 117.1(7) . . ?
C6 N2 H2A 121.4 . . ?
N3 N2 H2A 121.4 . . ?
C4 N1 C5 126.4(8) . . ?
C13 O2 Sm1 135.4(5) . . ?
C6 O1 Sm1 123.1(5) . . ?
C16 O7 Sm1 131.2(7) . . ?
C16 O7 H7A 114.4 . . ?
Sm1 O7 H7A 114.4 . . ?
C14 O3 Sm1 92.6(5) . . ?
C14 O4 Sm1 93.3(5) . . ?
C15 O6 Sm1 156.3(5) . 2_656 ?
C15 O6 Sm1 89.8(5) . . ?
Sm1 O6 Sm1 111.2(2) 2_656 . ?
C15 O5 Sm1 97.5(5) . . ?
C19 O8 H8 109.5 . . ?
C5 S1 H1 109.5 . . ?
O2 C13 C8 124.0(8) . . ?
O2 C13 C12 119.2(8) . . ?
C8 C13 C12 116.8(8) . . ?
C13 C12 C11 120.4(9) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C10 C11 C12 121.2(9) . . ?
C10 C11 H11 119.4 . . ?
C12 C11 H11 119.4 . . ?
C11 C10 C9 119.3(9) . . ?
C11 C10 H10 120.4 . . ?
C9 C10 H10 120.4 . . ?
C10 C9 C8 122.2(9) . . ?
C10 C9 H9 118.9 . . ?
C8 C9 H9 118.9 . . ?
C9 C8 C13 120.1(8) . . ?
C9 C8 C7 117.7(8) . . ?
C13 C8 C7 122.1(7) . . ?
N3 C7 C8 125.2(8) . . ?
N3 C7 H7 117.4 . . ?
C8 C7 H7 117.4 . . ?
O1 C6 N2 122.2(7) . . ?
O1 C6 C1 119.2(8) . . ?
N2 C6 C1 118.6(8) . . ?
C2 C1 C5 120.7(8) . . ?
C2 C1 C6 114.0(8) . . ?
C5 C1 C6 125.3(8) . . ?
N1 C5 C1 114.2(8) . . ?
N1 C5 S1 117.4(7) . . ?
C1 C5 S1 128.3(7) . . ?
C3 C4 N1 119.4(9) . . ?
C3 C4 H4 120.3 . . ?
N1 C4 H4 120.3 . . ?
C4 C3 C2 119.9(10) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C1 C2 C3 119.2(9) . . ?
C1 C2 H2 120.4 . . ?
C3 C2 H2 120.4 . . ?
O7 C16 H16A 109.5 . . ?
O7 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O7 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O4 C14 O3 121.7(8) . . ?
O4 C14 C17 118.4(8) . . ?
O3 C14 C17 119.9(9) . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O5 C15 O6 119.9(8) . . ?
O5 C15 C18 121.3(8) . . ?
O6 C15 C18 118.8(8) . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O8 C19 H19A 109.5 . . ?
O8 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O8 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Sm1 N3 C7 24.9(6) . . . . ?
O6 Sm1 N3 C7 105.7(7) 2_656 . . . ?
O1 Sm1 N3 C7 -173.6(7) . . . . ?
O7 Sm1 N3 C7 169.6(6) . . . . ?
O5 Sm1 N3 C7 -24.3(8) . . . . ?
O4 Sm1 N3 C7 -67.2(7) . . . . ?
O3 Sm1 N3 C7 -109.3(7) . . . . ?
O6 Sm1 N3 C7 50.8(8) . . . . ?
O2 Sm1 N3 N2 -164.3(5) . . . . ?
O6 Sm1 N3 N2 -83.5(5) 2_656 . . . ?
O1 Sm1 N3 N2 -2.8(5) . . . . ?
O7 Sm1 N3 N2 -19.6(6) . . . . ?
O5 Sm1 N3 N2 146.5(4) . . . . ?
O4 Sm1 N3 N2 103.6(5) . . . . ?
O3 Sm1 N3 N2 61.5(5) . . . . ?
O6 Sm1 N3 N2 -138.4(4) . . . . ?
C7 N3 N2 C6 173.1(7) . . . . ?
Sm1 N3 N2 C6 0.8(8) . . . . ?
O6 Sm1 O2 C13 -134.9(8) 2_656 . . . ?
O1 Sm1 O2 C13 -64.4(8) . . . . ?
O7 Sm1 O2 C13 175.7(7) . . . . ?
O5 Sm1 O2 C13 102.7(8) . . . . ?
O4 Sm1 O2 C13 26.9(8) . . . . ?
O3 Sm1 O2 C13 41.3(9) . . . . ?
N3 Sm1 O2 C13 -43.5(7) . . . . ?
O6 Sm1 O2 C13 154.6(8) . . . . ?
O2 Sm1 O1 C6 27.3(7) . . . . ?
O6 Sm1 O1 C6 97.8(6) 2_656 . . . ?
O7 Sm1 O1 C6 173.8(7) . . . . ?
O5 Sm1 O1 C6 -126.3(6) . . . . ?
O4 Sm1 O1 C6 -59.2(6) . . . . ?
O3 Sm1 O1 C6 -107.6(6) . . . . ?
N3 Sm1 O1 C6 5.4(6) . . . . ?
O6 Sm1 O1 C6 137.3(6) . . . . ?
O2 Sm1 O7 C16 169.6(10) . . . . ?
O6 Sm1 O7 C16 118.5(11) 2_656 . . . ?
O1 Sm1 O7 C16 34.5(11) . . . . ?
O5 Sm1 O7 C16 -120.2(11) . . . . ?
O4 Sm1 O7 C16 -50.6(11) . . . . ?
O3 Sm1 O7 C16 -41.7(11) . . . . ?
N3 Sm1 O7 C16 49.8(12) . . . . ?
O6 Sm1 O7 C16 -169.1(11) . . . . ?
O2 Sm1 O3 C14 -15.7(6) . . . . ?
O6 Sm1 O3 C14 157.8(5) 2_656 . . . ?
O1 Sm1 O3 C14 111.7(5) . . . . ?
O7 Sm1 O3 C14 -168.5(6) . . . . ?
O5 Sm1 O3 C14 -77.5(5) . . . . ?
O4 Sm1 O3 C14 2.5(5) . . . . ?
N3 Sm1 O3 C14 55.2(5) . . . . ?
O6 Sm1 O3 C14 -109.5(5) . . . . ?
O2 Sm1 O4 C14 164.7(5) . . . . ?
O6 Sm1 O4 C14 -144.4(6) 2_656 . . . ?
O1 Sm1 O4 C14 -67.8(5) . . . . ?
O7 Sm1 O4 C14 8.4(6) . . . . ?
O5 Sm1 O4 C14 84.3(5) . . . . ?
O3 Sm1 O4 C14 -2.5(5) . . . . ?
N3 Sm1 O4 C14 -126.4(6) . . . . ?
O6 Sm1 O4 C14 99.6(6) . . . . ?
O2 Sm1 O6 C15 -82.3(5) . . . . ?
O6 Sm1 O6 C15 -168.8(6) 2_656 . . . ?
O1 Sm1 O6 C15 148.8(5) . . . . ?
O7 Sm1 O6 C15 111.3(5) . . . . ?
O5 Sm1 O6 C15 8.1(5) . . . . ?
O4 Sm1 O6 C15 -11.3(5) . . . . ?
O3 Sm1 O6 C15 50.3(5) . . . . ?
N3 Sm1 O6 C15 -107.4(5) . . . . ?
O2 Sm1 O6 Sm1 86.5(2) . . . 2_656 ?
O6 Sm1 O6 Sm1 0.0 2_656 . . 2_656 ?
O1 Sm1 O6 Sm1 -42.4(4) . . . 2_656 ?
O7 Sm1 O6 Sm1 -79.9(2) . . . 2_656 ?
O5 Sm1 O6 Sm1 176.8(3) . . . 2_656 ?
O4 Sm1 O6 Sm1 157.5(2) . . . 2_656 ?
O3 Sm1 O6 Sm1 -140.9(2) . . . 2_656 ?
N3 Sm1 O6 Sm1 61.3(3) . . . 2_656 ?
O2 Sm1 O5 C15 67.9(5) . . . . ?
O6 Sm1 O5 C15 -5.0(6) 2_656 . . . ?
O1 Sm1 O5 C15 -133.1(6) . . . . ?
O7 Sm1 O5 C15 -75.8(6) . . . . ?
O4 Sm1 O5 C15 155.0(6) . . . . ?
O3 Sm1 O5 C15 -151.3(6) . . . . ?
N3 Sm1 O5 C15 113.5(6) . . . . ?
O6 Sm1 O5 C15 -8.4(5) . . . . ?
Sm1 O2 C13 C8 42.4(12) . . . . ?
Sm1 O2 C13 C12 -140.0(6) . . . . ?
O2 C13 C12 C11 -177.8(8) . . . . ?
C8 C13 C12 C11 0.0(12) . . . . ?
C13 C12 C11 C10 0.0(14) . . . . ?
C12 C11 C10 C9 0.5(15) . . . . ?
C11 C10 C9 C8 -1.1(14) . . . . ?
C10 C9 C8 C13 1.1(13) . . . . ?
C10 C9 C8 C7 178.5(8) . . . . ?
O2 C13 C8 C9 177.1(7) . . . . ?
C12 C13 C8 C9 -0.6(11) . . . . ?
O2 C13 C8 C7 -0.1(12) . . . . ?
C12 C13 C8 C7 -177.8(7) . . . . ?
N2 N3 C7 C8 -178.2(7) . . . . ?
Sm1 N3 C7 C8 -7.4(11) . . . . ?
C9 C8 C7 N3 169.0(7) . . . . ?
C13 C8 C7 N3 -13.7(12) . . . . ?
Sm1 O1 C6 N2 -7.6(11) . . . . ?
Sm1 O1 C6 C1 173.0(5) . . . . ?
N3 N2 C6 O1 4.2(12) . . . . ?
N3 N2 C6 C1 -176.5(6) . . . . ?
O1 C6 C1 C2 7.5(11) . . . . ?
N2 C6 C1 C2 -171.8(8) . . . . ?
O1 C6 C1 C5 -174.0(8) . . . . ?
N2 C6 C1 C5 6.6(12) . . . . ?
C4 N1 C5 C1 5.2(13) . . . . ?
C4 N1 C5 S1 -174.7(8) . . . . ?
C2 C1 C5 N1 -3.3(12) . . . . ?
C6 C1 C5 N1 178.3(8) . . . . ?
C2 C1 C5 S1 176.6(7) . . . . ?
C6 C1 C5 S1 -1.7(13) . . . . ?
C5 N1 C4 C3 -4.5(16) . . . . ?
N1 C4 C3 C2 1.5(16) . . . . ?
C5 C1 C2 C3 0.9(14) . . . . ?
C6 C1 C2 C3 179.5(8) . . . . ?
C4 C3 C2 C1 0.1(15) . . . . ?
Sm1 O4 C14 O3 4.6(9) . . . . ?
Sm1 O4 C14 C17 -176.3(8) . . . . ?
Sm1 O3 C14 O4 -4.6(9) . . . . ?
Sm1 O3 C14 C17 176.3(8) . . . . ?
Sm1 O5 C15 O6 15.4(9) . . . . ?
Sm1 O5 C15 C18 -162.4(8) . . . . ?
Sm1 O6 C15 O5 -167.7(8) 2_656 . . . ?
Sm1 O6 C15 O5 -14.4(8) . . . . ?
Sm1 O6 C15 C18 10.2(19) 2_656 . . . ?
Sm1 O6 C15 C18 163.4(8) . . . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        25.04
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         1.731
_refine_diff_density_min         -0.991
_refine_diff_density_rms         0.161

#===END

data_Gd2
_database_code_depnum_ccdc_archive 'CCDC 972394'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H48 Gd2 N6 O16 S2'
_chemical_formula_weight         1223.44

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.198(11)
_cell_length_b                   10.642(11)
_cell_length_c                   11.568(12)
_cell_angle_alpha                69.60(2)
_cell_angle_beta                 85.69(2)
_cell_angle_gamma                81.48(2)
_cell_volume                     1163(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1872
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      23.20

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             606
_exptl_absorpt_coefficient_mu    2.989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5340
_exptl_absorpt_correction_T_max  0.6463
_exptl_absorpt_process_details   '(Sadabs; Bruker,2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6677
_diffrn_reflns_av_R_equivalents  0.0938
_diffrn_reflns_av_unetI/netI     0.1838
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.88
_diffrn_reflns_theta_max         25.58
_reflns_number_total             4223
_reflns_number_gt                2330
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1481P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4223
_refine_ls_number_parameters     297
_refine_ls_number_restraints     35
_refine_ls_R_factor_all          0.1575
_refine_ls_R_factor_gt           0.0931
_refine_ls_wR_factor_ref         0.2698
_refine_ls_wR_factor_gt          0.2218
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_restrained_S_all      0.956
_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
O4 O 0.5686(12) 0.3178(13) 0.1552(11) 0.058(3) Uani 1 1 d . . .
Gd1 Gd 0.47949(8) 0.14877(9) 0.33030(8) 0.0472(4) Uani 1 1 d . . .
N3 N 0.3923(12) 0.3872(15) 0.3280(12) 0.047(4) Uani 1 1 d . . .
N2 N 0.2636(14) 0.4341(17) 0.2917(13) 0.059(4) Uani 1 1 d . . .
H2 H 0.2259 0.5126 0.2897 0.071 Uiso 1 1 calc R . .
N1 N -0.1183(15) 0.5577(19) 0.1334(15) 0.071(5) Uani 1 1 d . . .
O2 O 0.6078(11) 0.2191(11) 0.4389(10) 0.048(3) Uani 1 1 d . . .
O1 O 0.2546(11) 0.2345(14) 0.2699(12) 0.063(4) Uani 1 1 d . . .
O7 O 0.3920(13) -0.0473(14) 0.3312(11) 0.068(4) Uani 1 1 d U . .
H7A H 0.4198 -0.1245 0.3972 0.081 Uiso 1 1 calc R . .
O3 O 0.4676(12) 0.1705(14) 0.1159(11) 0.066(4) Uani 1 1 d . . .
O6 O 0.6212(10) -0.0646(11) 0.4743(9) 0.047(3) Uani 1 1 d . . .
O5 O 0.6978(12) 0.0421(14) 0.2872(11) 0.061(3) Uani 1 1 d . . .
O8 O 0.2703(19) 0.205(2) 0.959(2) 0.117(6) Uani 1 1 d DU . .
H8 H 0.1915 0.2298 0.9681 0.175 Uiso 1 1 calc R . .
S1 S 0.0584(5) 0.6668(6) 0.1945(6) 0.0794(17) Uani 1 1 d D . .
H1 H 0.001(15) 0.7680(19) 0.136(16) 0.119 Uiso 1 1 d D . .
C13 C 0.6570(15) 0.3283(19) 0.4281(14) 0.047(4) Uani 1 1 d . . .
C12 C 0.7853(17) 0.322(2) 0.4629(18) 0.067(6) Uani 1 1 d . . .
H12 H 0.8375 0.2386 0.4931 0.081 Uiso 1 1 calc R . .
C11 C 0.835(2) 0.436(2) 0.4532(19) 0.070(6) Uani 1 1 d . . .
H11 H 0.9214 0.4282 0.4789 0.084 Uiso 1 1 calc R . .
C10 C 0.7642(19) 0.565(2) 0.406(2) 0.070(6) Uani 1 1 d . . .
H10 H 0.8006 0.6425 0.3989 0.084 Uiso 1 1 calc R . .
C9 C 0.6439(18) 0.5694(18) 0.3740(16) 0.056(5) Uani 1 1 d . . .
H9 H 0.5955 0.6547 0.3422 0.067 Uiso 1 1 calc R . .
C8 C 0.5809(15) 0.4609(19) 0.3820(14) 0.047(4) Uani 1 1 d . . .
C7 C 0.4480(18) 0.4780(19) 0.3475(14) 0.052(4) Uani 1 1 d . . .
H7 H 0.3973 0.5609 0.3382 0.063 Uiso 1 1 calc R . .
C6 C 0.2015(15) 0.3513(19) 0.2601(14) 0.047(4) Uani 1 1 d . . .
C1 C 0.0660(17) 0.401(2) 0.2112(16) 0.054(5) Uani 1 1 d . . .
C4 C -0.1810(18) 0.462(3) 0.122(2) 0.078(6) Uani 1 1 d U . .
H4 H -0.2674 0.4837 0.0937 0.094 Uiso 1 1 calc R . .
C3 C -0.1231(18) 0.336(3) 0.150(2) 0.083(6) Uani 1 1 d U . .
H3 H -0.1666 0.2693 0.1403 0.099 Uiso 1 1 calc R . .
C2 C 0.0054(17) 0.306(2) 0.1937(16) 0.060(5) Uani 1 1 d . . .
H2A H 0.0497 0.2186 0.2112 0.072 Uiso 1 1 calc R . .
C16 C 0.309(3) -0.070(3) 0.255(2) 0.106(8) Uani 1 1 d U . .
H16A H 0.3060 0.0034 0.1770 0.159 Uiso 1 1 calc R . .
H16B H 0.2221 -0.0751 0.2917 0.159 Uiso 1 1 calc R . .
H16C H 0.3423 -0.1531 0.2414 0.159 Uiso 1 1 calc R . .
C14 C 0.5357(18) 0.2666(18) 0.0804(16) 0.050(4) Uani 1 1 d . . .
C17 C 0.569(2) 0.330(2) -0.0509(17) 0.077(6) Uani 1 1 d . . .
H17A H 0.5417 0.4258 -0.0756 0.116 Uiso 1 1 calc R . .
H17B H 0.5237 0.2929 -0.0988 0.116 Uiso 1 1 calc R . .
H17C H 0.6629 0.3132 -0.0642 0.116 Uiso 1 1 calc R . .
C15 C 0.7143(16) -0.0419(17) 0.3987(17) 0.050(4) Uani 1 1 d . . .
C18 C 0.8521(17) -0.104(2) 0.4365(19) 0.074(6) Uani 1 1 d . . .
H18A H 0.8889 -0.0518 0.4758 0.110 Uiso 1 1 calc R . .
H18B H 0.9054 -0.1059 0.3650 0.110 Uiso 1 1 calc R . .
H18C H 0.8507 -0.1947 0.4931 0.110 Uiso 1 1 calc R . .
C19 C 0.283(3) 0.098(3) 0.909(3) 0.142(8) Uani 1 1 d DU . .
H19A H 0.3606 0.0352 0.9408 0.213 Uiso 1 1 calc R . .
H19B H 0.2911 0.1350 0.8206 0.213 Uiso 1 1 calc R . .
H19C H 0.2060 0.0516 0.9317 0.213 Uiso 1 1 calc R . .
C5 C 0.0026(17) 0.535(2) 0.1785(15) 0.054(5) Uani 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O4 C14 1.26(2) . ?
O4 Gd1 2.415(11) . ?
Gd1 O2 2.246(10) . ?
Gd1 O6 2.340(10) 2_656 ?
Gd1 O7 2.385(13) . ?
Gd1 O1 2.399(11) . ?
Gd1 O3 2.420(12) . ?
Gd1 O5 2.444(12) . ?
Gd1 N3 2.553(16) . ?
Gd1 O6 2.602(11) . ?
N3 C7 1.28(2) . ?
N3 N2 1.375(18) . ?
N2 C6 1.32(2) . ?
N2 H2 0.8600 . ?
N1 C5 1.33(2) . ?
N1 C4 1.33(3) . ?
O2 C13 1.30(2) . ?
O1 C6 1.25(2) . ?
O7 C16 1.37(2) . ?
O7 H7A 0.9300 . ?
O3 C14 1.25(2) . ?
O6 C15 1.233(19) . ?
O6 Gd1 2.340(10) 2_656 ?
O5 C15 1.29(2) . ?
O8 C19 1.430(10) . ?
O8 H8 0.8200 . ?
S1 C5 1.66(2) . ?
S1 H1 1.1500(14) . ?
C13 C12 1.38(2) . ?
C13 C8 1.45(3) . ?
C12 C11 1.35(3) . ?
C12 H12 0.9300 . ?
C11 C10 1.40(3) . ?
C11 H11 0.9300 . ?
C10 C9 1.30(3) . ?
C10 H10 0.9300 . ?
C9 C8 1.38(2) . ?
C9 H9 0.9300 . ?
C8 C7 1.41(2) . ?
C7 H7 0.9300 . ?
C6 C1 1.48(2) . ?
C1 C2 1.34(3) . ?
C1 C5 1.41(3) . ?
C4 C3 1.32(3) . ?
C4 H4 0.9300 . ?
C3 C2 1.39(2) . ?
C3 H3 0.9300 . ?
C2 H2A 0.9300 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C14 C17 1.47(2) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C15 C18 1.49(2) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?

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
C14 O4 Gd1 92.6(10) . . ?
O2 Gd1 O6 80.6(4) . 2_656 ?
O2 Gd1 O7 141.9(4) . . ?
O6 Gd1 O7 75.0(4) 2_656 . ?
O2 Gd1 O1 128.3(5) . . ?
O6 Gd1 O1 82.6(4) 2_656 . ?
O7 Gd1 O1 77.1(5) . . ?
O2 Gd1 O4 83.8(4) . . ?
O6 Gd1 O4 155.8(5) 2_656 . ?
O7 Gd1 O4 127.3(4) . . ?
O1 Gd1 O4 92.9(4) . . ?
O2 Gd1 O3 135.4(4) . . ?
O6 Gd1 O3 144.0(4) 2_656 . ?
O7 Gd1 O3 74.1(4) . . ?
O1 Gd1 O3 72.8(4) . . ?
O4 Gd1 O3 53.7(4) . . ?
O2 Gd1 O5 79.5(4) . . ?
O6 Gd1 O5 119.8(4) 2_656 . ?
O7 Gd1 O5 87.7(5) . . ?
O1 Gd1 O5 148.9(5) . . ?
O4 Gd1 O5 74.8(4) . . ?
O3 Gd1 O5 77.0(4) . . ?
O2 Gd1 N3 68.4(4) . . ?
O6 Gd1 N3 88.4(4) 2_656 . ?
O7 Gd1 N3 138.1(4) . . ?
O1 Gd1 N3 62.6(4) . . ?
O4 Gd1 N3 68.7(4) . . ?
O3 Gd1 N3 102.6(4) . . ?
O5 Gd1 N3 133.1(4) . . ?
O2 Gd1 O6 72.6(4) . . ?
O6 Gd1 O6 68.0(4) 2_656 . ?
O7 Gd1 O6 71.3(4) . . ?
O1 Gd1 O6 141.2(4) . . ?
O4 Gd1 O6 124.1(4) . . ?
O3 Gd1 O6 117.7(4) . . ?
O5 Gd1 O6 51.8(4) . . ?
N3 Gd1 O6 137.1(4) . . ?
C7 N3 N2 111.5(16) . . ?
C7 N3 Gd1 132.3(11) . . ?
N2 N3 Gd1 116.0(11) . . ?
C6 N2 N3 115.9(16) . . ?
C6 N2 H2 122.0 . . ?
N3 N2 H2 122.0 . . ?
C5 N1 C4 124.0(19) . . ?
C13 O2 Gd1 137.9(9) . . ?
C6 O1 Gd1 123.8(11) . . ?
C16 O7 Gd1 133.2(14) . . ?
C16 O7 H7A 113.4 . . ?
Gd1 O7 H7A 113.4 . . ?
C14 O3 Gd1 92.5(10) . . ?
C15 O6 Gd1 156.1(11) . 2_656 ?
C15 O6 Gd1 89.2(9) . . ?
Gd1 O6 Gd1 112.0(4) 2_656 . ?
C15 O5 Gd1 95.0(10) . . ?
C19 O8 H8 109.5 . . ?
C5 S1 H1 112.2(16) . . ?
O2 C13 C12 120.7(18) . . ?
O2 C13 C8 122.2(13) . . ?
C12 C13 C8 117.1(17) . . ?
C11 C12 C13 121(2) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
C12 C11 C10 123.0(17) . . ?
C12 C11 H11 118.5 . . ?
C10 C11 H11 118.5 . . ?
C9 C10 C11 115.8(18) . . ?
C9 C10 H10 122.1 . . ?
C11 C10 H10 122.1 . . ?
C10 C9 C8 126.6(19) . . ?
C10 C9 H9 116.7 . . ?
C8 C9 H9 116.7 . . ?
C9 C8 C7 121.6(18) . . ?
C9 C8 C13 116.9(14) . . ?
C7 C8 C13 121.5(15) . . ?
N3 C7 C8 124.5(18) . . ?
N3 C7 H7 117.7 . . ?
C8 C7 H7 117.7 . . ?
O1 C6 N2 121.5(15) . . ?
O1 C6 C1 120.5(17) . . ?
N2 C6 C1 118.0(17) . . ?
C2 C1 C5 120.0(16) . . ?
C2 C1 C6 113.7(18) . . ?
C5 C1 C6 126.2(17) . . ?
C3 C4 N1 121.2(18) . . ?
C3 C4 H4 119.4 . . ?
N1 C4 H4 119.4 . . ?
C4 C3 C2 118(2) . . ?
C4 C3 H3 121.1 . . ?
C2 C3 H3 121.1 . . ?
C1 C2 C3 121(2) . . ?
C1 C2 H2A 119.6 . . ?
C3 C2 H2A 119.6 . . ?
O7 C16 H16A 109.5 . . ?
O7 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O7 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O3 C14 O4 120.7(16) . . ?
O3 C14 C17 120.8(17) . . ?
O4 C14 C17 118.2(17) . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O6 C15 O5 121.9(14) . . ?
O6 C15 C18 120.3(16) . . ?
O5 C15 C18 117.7(16) . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O8 C19 H19A 109.5 . . ?
O8 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O8 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N1 C5 C1 116.0(17) . . ?
N1 C5 S1 116.3(16) . . ?
C1 C5 S1 127.7(13) . . ?

_diffrn_measured_fraction_theta_max 0.967
_diffrn_reflns_theta_full        25.58
_diffrn_measured_fraction_theta_full 0.967
_refine_diff_density_max         2.324
_refine_diff_density_min         -3.417
_refine_diff_density_rms         0.266

#===END

data_Dy2
_database_code_depnum_ccdc_archive 'CCDC 972395'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H48 Dy2 N6 O16 S2'
_chemical_formula_weight         1233.96

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'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.310(5)
_cell_length_b                   10.622(5)
_cell_length_c                   11.674(6)
_cell_angle_alpha                69.650(9)
_cell_angle_beta                 85.710(8)
_cell_angle_gamma                81.099(8)
_cell_volume                     1183.9(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2096
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      24.07

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             610
_exptl_absorpt_coefficient_mu    3.291
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5589
_exptl_absorpt_correction_T_max  0.6935
_exptl_absorpt_process_details   '(Sadabs; Bruker,2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6506
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.86
_diffrn_reflns_theta_max         26.06
_reflns_number_total             4584
_reflns_number_gt                3769
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0445P)²+0.4314P] 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         4584
_refine_ls_number_parameters     299
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0405
_refine_ls_wR_factor_ref         0.0982
_refine_ls_wR_factor_gt          0.0896
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.034
_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
C1 C 0.0695(6) 0.8949(7) 0.7107(5) 0.0436(16) Uani 1 1 d . . .
C2 C 0.0058(6) 0.7976(8) 0.6966(7) 0.0564(19) Uani 1 1 d . . .
H2 H 0.0488 0.7093 0.7165 0.068 Uiso 1 1 calc R . .
C3 C -0.1201(7) 0.8265(9) 0.6537(7) 0.064(2) Uani 1 1 d . . .
H3 H -0.1635 0.7591 0.6466 0.077 Uiso 1 1 calc R . .
C4 C -0.1781(7) 0.9569(9) 0.6223(7) 0.062(2) Uani 1 1 d . . .
H4 H -0.2631 0.9795 0.5929 0.075 Uiso 1 1 calc R . .
C5 C 0.0058(6) 1.0301(7) 0.6801(6) 0.0473(16) Uani 1 1 d . . .
C6 C 0.2040(6) 0.8460(7) 0.7591(5) 0.0393(15) Uani 1 1 d . . .
C7 C 0.4500(6) 0.9759(7) 0.8463(5) 0.0406(15) Uani 1 1 d . . .
H7 H 0.4019 1.0609 0.8343 0.049 Uiso 1 1 calc R . .
C8 C 0.5846(6) 0.9563(7) 0.8808(5) 0.0385(14) Uani 1 1 d . . .
C9 C 0.6407(7) 1.0702(7) 0.8736(6) 0.0507(17) Uani 1 1 d . . .
H9 H 0.5904 1.1551 0.8458 0.061 Uiso 1 1 calc R . .
C10 C 0.7674(7) 1.0610(9) 0.9063(7) 0.061(2) Uani 1 1 d U . .
H10 H 0.8043 1.1384 0.8978 0.073 Uiso 1 1 calc R . .
C11 C 0.8387(7) 0.9345(9) 0.9519(7) 0.057(2) Uani 1 1 d . . .
H11 H 0.9243 0.9264 0.9764 0.068 Uiso 1 1 calc R . .
C12 C 0.7862(6) 0.8190(8) 0.9623(6) 0.0544(19) Uani 1 1 d . . .
H12 H 0.8374 0.7349 0.9928 0.065 Uiso 1 1 calc R . .
C13 C 0.6584(6) 0.8260(7) 0.9280(5) 0.0405(15) Uani 1 1 d . . .
C14 C 0.5335(6) 0.7682(7) 0.5826(6) 0.0445(16) Uani 1 1 d . . .
C15 C 0.7140(6) 0.4590(6) 0.8974(6) 0.0409(15) Uani 1 1 d . . .
C16 C 0.3158(10) 0.4251(10) 0.7571(8) 0.088(3) Uani 1 1 d U . .
H16A H 0.3434 0.4663 0.6737 0.132 Uiso 1 1 calc R . .
H16B H 0.2263 0.4611 0.7682 0.132 Uiso 1 1 calc R . .
H16C H 0.3227 0.3288 0.7765 0.132 Uiso 1 1 calc R . .
C17 C 0.5700(8) 0.8280(9) 0.4499(6) 0.068(2) Uani 1 1 d . . .
H17A H 0.6634 0.8100 0.4391 0.102 Uiso 1 1 calc R . .
H17B H 0.5429 0.9242 0.4220 0.102 Uiso 1 1 calc R . .
H17C H 0.5270 0.7881 0.4035 0.102 Uiso 1 1 calc R . .
C18 C 0.8506(7) 0.3955(8) 0.9332(8) 0.070(2) Uani 1 1 d . . .
H18A H 0.9004 0.3872 0.8628 0.104 Uiso 1 1 calc R . .
H18B H 0.8491 0.3073 0.9939 0.104 Uiso 1 1 calc R . .
H18C H 0.8904 0.4511 0.9661 0.104 Uiso 1 1 calc R . .
Dy1 Dy 0.47906(3) 0.64912(3) 0.83039(2) 0.03612(12) Uani 1 1 d . . .
N1 N -0.1167(5) 1.0527(7) 0.6323(5) 0.0567(16) Uani 1 1 d . . .
N2 N 0.2643(5) 0.9307(6) 0.7917(5) 0.0451(13) Uani 1 1 d . . .
H2A H 0.2256 1.0096 0.7883 0.054 Uiso 1 1 calc R . .
N3 N 0.3912(5) 0.8857(5) 0.8309(4) 0.0373(12) Uani 1 1 d . . .
O1 O 0.2567(4) 0.7307(5) 0.7730(4) 0.0493(11) Uani 1 1 d . . .
O2 O 0.6081(4) 0.7164(4) 0.9394(4) 0.0437(10) Uani 1 1 d . . .
O3 O 0.4670(4) 0.6713(5) 0.6167(4) 0.0521(12) Uani 1 1 d . . .
O4 O 0.5685(4) 0.8162(5) 0.6562(4) 0.0488(11) Uani 1 1 d . . .
O5 O 0.6926(4) 0.5394(5) 0.7929(4) 0.0541(12) Uani 1 1 d . . .
O6 O 0.6207(4) 0.4328(4) 0.9754(4) 0.0409(10) Uani 1 1 d . . .
O7 O 0.3942(5) 0.4525(5) 0.8326(4) 0.0532(12) Uani 1 1 d D . .
S S 0.05968(19) 1.1651(2) 0.6939(2) 0.0682(6) Uani 1 1 d . . .
H1 H -0.0142 1.2655 0.6439 0.102 Uiso 1 1 calc R . .
O8 O 0.2668(7) 0.7043(6) 0.4605(6) 0.091(2) Uani 1 1 d U . .
H8 H 0.3170 0.6841 0.5174 0.136 Uiso 1 1 calc R . .
C19 C 0.2810(13) 0.5961(13) 0.4115(11) 0.138(5) Uani 1 1 d U . .
H19A H 0.2104 0.5431 0.4418 0.207 Uiso 1 1 calc R . .
H19B H 0.3633 0.5394 0.4359 0.207 Uiso 1 1 calc R . .
H19C H 0.2789 0.6333 0.3239 0.207 Uiso 1 1 calc R . .
H5 H 0.390(6) 0.402(5) 0.9068(19) 0.040(18) Uiso 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.368(10) . ?
C1 C5 1.417(9) . ?
C1 C6 1.484(8) . ?
C2 C3 1.377(9) . ?
C2 H2 0.9300 . ?
C3 C4 1.355(11) . ?
C3 H3 0.9300 . ?
C4 N1 1.321(10) . ?
C4 H4 0.9300 . ?
C5 N1 1.372(8) . ?
C5 S 1.676(8) . ?
C6 O1 1.221(7) . ?
C6 N2 1.336(8) . ?
C7 N3 1.278(8) . ?
C7 C8 1.438(8) . ?
C7 H7 0.9300 . ?
C8 C9 1.395(9) . ?
C8 C13 1.416(9) . ?
C9 C10 1.368(10) . ?
C9 H9 0.9300 . ?
C10 C11 1.373(11) . ?
C10 H10 0.9300 . ?
C11 C12 1.380(10) . ?
C11 H11 0.9300 . ?
C12 C13 1.390(9) . ?
C12 H12 0.9300 . ?
C13 O2 1.308(7) . ?
C14 O4 1.239(8) . ?
C14 O3 1.258(8) . ?
C14 C17 1.499(9) . ?
C15 O5 1.234(7) . ?
C15 O6 1.268(7) . ?
C15 C18 1.486(9) . ?
C16 O7 1.367(9) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
Dy1 O2 2.254(4) . ?
Dy1 O6 2.348(4) 2_667 ?
Dy1 O7 2.378(5) . ?
Dy1 O1 2.380(4) . ?
Dy1 O5 2.411(5) . ?
Dy1 O4 2.419(4) . ?
Dy1 O3 2.434(4) . ?
Dy1 N3 2.538(5) . ?
Dy1 O6 2.628(4) . ?
N2 N3 1.376(6) . ?
N2 H2A 0.8600 . ?
O6 Dy1 2.348(4) 2_667 ?
O7 H5 0.848(10) . ?
S H1 1.2000 . ?
O8 C19 1.437(13) . ?
O8 H8 0.8200 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?

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
C2 C1 C5 119.8(6) . . ?
C2 C1 C6 114.9(6) . . ?
C5 C1 C6 125.3(6) . . ?
C1 C2 C3 121.9(7) . . ?
C1 C2 H2 119.0 . . ?
C3 C2 H2 119.0 . . ?
C4 C3 C2 117.4(8) . . ?
C4 C3 H3 121.3 . . ?
C2 C3 H3 121.3 . . ?
N1 C4 C3 121.4(6) . . ?
N1 C4 H4 119.3 . . ?
C3 C4 H4 119.3 . . ?
N1 C5 C1 115.0(6) . . ?
N1 C5 S 116.1(5) . . ?
C1 C5 S 129.0(5) . . ?
O1 C6 N2 120.7(6) . . ?
O1 C6 C1 121.4(6) . . ?
N2 C6 C1 117.8(6) . . ?
N3 C7 C8 125.2(6) . . ?
N3 C7 H7 117.4 . . ?
C8 C7 H7 117.4 . . ?
C9 C8 C13 119.5(6) . . ?
C9 C8 C7 118.0(6) . . ?
C13 C8 C7 122.4(6) . . ?
C10 C9 C8 122.0(7) . . ?
C10 C9 H9 119.0 . . ?
C8 C9 H9 119.0 . . ?
C9 C10 C11 118.3(7) . . ?
C9 C10 H10 120.9 . . ?
C11 C10 H10 120.9 . . ?
C10 C11 C12 121.5(7) . . ?
C10 C11 H11 119.3 . . ?
C12 C11 H11 119.3 . . ?
C11 C12 C13 121.3(7) . . ?
C11 C12 H12 119.4 . . ?
C13 C12 H12 119.4 . . ?
O2 C13 C12 121.2(6) . . ?
O2 C13 C8 121.4(5) . . ?
C12 C13 C8 117.4(6) . . ?
O4 C14 O3 121.4(6) . . ?
O4 C14 C17 119.3(7) . . ?
O3 C14 C17 119.2(7) . . ?
O5 C15 O6 120.4(6) . . ?
O5 C15 C18 119.8(6) . . ?
O6 C15 C18 119.7(6) . . ?
O7 C16 H16A 109.5 . . ?
O7 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O7 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O2 Dy1 O6 80.13(15) . 2_667 ?
O2 Dy1 O7 140.75(15) . . ?
O6 Dy1 O7 75.25(16) 2_667 . ?
O2 Dy1 O1 129.68(16) . . ?
O6 Dy1 O1 81.71(15) 2_667 . ?
O7 Dy1 O1 76.34(17) . . ?
O2 Dy1 O5 78.49(17) . . ?
O6 Dy1 O5 118.87(15) 2_667 . ?
O7 Dy1 O5 87.16(18) . . ?
O1 Dy1 O5 149.61(17) . . ?
O2 Dy1 O4 84.31(16) . . ?
O6 Dy1 O4 155.87(16) 2_667 . ?
O7 Dy1 O4 127.18(16) . . ?
O1 Dy1 O4 94.41(16) . . ?
O5 Dy1 O4 75.32(16) . . ?
O2 Dy1 O3 135.51(16) . . ?
O6 Dy1 O3 144.33(15) 2_667 . ?
O7 Dy1 O3 74.57(16) . . ?
O1 Dy1 O3 73.07(16) . . ?
O5 Dy1 O3 78.05(16) . . ?
O4 Dy1 O3 53.33(15) . . ?
O2 Dy1 N3 69.07(15) . . ?
O6 Dy1 N3 87.07(15) 2_667 . ?
O7 Dy1 N3 138.04(17) . . ?
O1 Dy1 N3 63.47(16) . . ?
O5 Dy1 N3 134.13(17) . . ?
O4 Dy1 N3 70.11(16) . . ?
O3 Dy1 N3 103.12(16) . . ?
O2 Dy1 O6 71.74(14) . . ?
O6 Dy1 O6 68.14(16) 2_667 . ?
O7 Dy1 O6 70.90(15) . . ?
O1 Dy1 O6 139.85(14) . . ?
O5 Dy1 O6 50.83(14) . . ?
O4 Dy1 O6 123.80(15) . . ?
O3 Dy1 O6 118.02(15) . . ?
N3 Dy1 O6 136.50(14) . . ?
C4 N1 C5 124.4(6) . . ?
C6 N2 N3 116.9(5) . . ?
C6 N2 H2A 121.5 . . ?
N3 N2 H2A 121.5 . . ?
C7 N3 N2 114.5(5) . . ?
C7 N3 Dy1 130.6(4) . . ?
N2 N3 Dy1 114.3(4) . . ?
C6 O1 Dy1 124.1(4) . . ?
C13 O2 Dy1 137.3(4) . . ?
C14 O3 Dy1 91.9(4) . . ?
C14 O4 Dy1 93.1(4) . . ?
C15 O5 Dy1 98.6(4) . . ?
C15 O6 Dy1 157.1(4) . 2_667 ?
C15 O6 Dy1 87.6(4) . . ?
Dy1 O6 Dy1 111.86(16) 2_667 . ?
C16 O7 Dy1 134.7(5) . . ?
C16 O7 H5 114(4) . . ?
Dy1 O7 H5 107(4) . . ?
C5 S H1 109.5 . . ?
C19 O8 H8 109.5 . . ?
O8 C19 H19A 109.5 . . ?
O8 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O8 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 C1 C2 C3 -0.4(11) . . . . ?
C6 C1 C2 C3 179.4(6) . . . . ?
C1 C2 C3 C4 1.9(12) . . . . ?
C2 C3 C4 N1 -0.1(12) . . . . ?
C2 C1 C5 N1 -2.8(9) . . . . ?
C6 C1 C5 N1 177.5(6) . . . . ?
C2 C1 C5 S 177.5(6) . . . . ?
C6 C1 C5 S -2.3(10) . . . . ?
C2 C1 C6 O1 6.9(9) . . . . ?
C5 C1 C6 O1 -173.3(6) . . . . ?
C2 C1 C6 N2 -170.6(6) . . . . ?
C5 C1 C6 N2 9.2(9) . . . . ?
N3 C7 C8 C9 169.2(6) . . . . ?
N3 C7 C8 C13 -14.6(9) . . . . ?
C13 C8 C9 C10 2.7(10) . . . . ?
C7 C8 C9 C10 179.0(6) . . . . ?
C8 C9 C10 C11 -2.6(11) . . . . ?
C9 C10 C11 C12 1.6(11) . . . . ?
C10 C11 C12 C13 -0.7(11) . . . . ?
C11 C12 C13 O2 -179.1(6) . . . . ?
C11 C12 C13 C8 0.7(10) . . . . ?
C9 C8 C13 O2 178.1(6) . . . . ?
C7 C8 C13 O2 1.9(9) . . . . ?
C9 C8 C13 C12 -1.6(9) . . . . ?
C7 C8 C13 C12 -177.8(6) . . . . ?
C3 C4 N1 C5 -3.5(12) . . . . ?
C1 C5 N1 C4 4.8(10) . . . . ?
S C5 N1 C4 -175.4(6) . . . . ?
O1 C6 N2 N3 5.5(9) . . . . ?
C1 C6 N2 N3 -177.0(5) . . . . ?
C8 C7 N3 N2 -176.7(5) . . . . ?
C8 C7 N3 Dy1 -6.9(9) . . . . ?
C6 N2 N3 C7 171.7(5) . . . . ?
C6 N2 N3 Dy1 0.1(6) . . . . ?
O2 Dy1 N3 C7 24.5(5) . . . . ?
O6 Dy1 N3 C7 105.1(5) 2_667 . . . ?
O7 Dy1 N3 C7 169.1(5) . . . . ?
O1 Dy1 N3 C7 -172.7(6) . . . . ?
O5 Dy1 N3 C7 -23.5(6) . . . . ?
O4 Dy1 N3 C7 -66.9(5) . . . . ?
O3 Dy1 N3 C7 -109.5(5) . . . . ?
O6 Dy1 N3 C7 51.6(6) . . . . ?
O2 Dy1 N3 N2 -165.6(4) . . . . ?
O6 Dy1 N3 N2 -85.1(4) 2_667 . . . ?
O7 Dy1 N3 N2 -21.0(5) . . . . ?
O1 Dy1 N3 N2 -2.9(3) . . . . ?
O5 Dy1 N3 N2 146.3(3) . . . . ?
O4 Dy1 N3 N2 102.9(4) . . . . ?
O3 Dy1 N3 N2 60.4(4) . . . . ?
O6 Dy1 N3 N2 -138.5(3) . . . . ?
N2 C6 O1 Dy1 -9.1(8) . . . . ?
C1 C6 O1 Dy1 173.5(4) . . . . ?
O2 Dy1 O1 C6 27.4(6) . . . . ?
O6 Dy1 O1 C6 97.2(5) 2_667 . . . ?
O7 Dy1 O1 C6 173.9(5) . . . . ?
O5 Dy1 O1 C6 -127.1(5) . . . . ?
O4 Dy1 O1 C6 -58.8(5) . . . . ?
O3 Dy1 O1 C6 -108.3(5) . . . . ?
N3 Dy1 O1 C6 6.3(5) . . . . ?
O6 Dy1 O1 C6 138.0(5) . . . . ?
C12 C13 O2 Dy1 -139.4(5) . . . . ?
C8 C13 O2 Dy1 40.9(9) . . . . ?
O6 Dy1 O2 C13 -134.4(6) 2_667 . . . ?
O7 Dy1 O2 C13 174.0(5) . . . . ?
O1 Dy1 O2 C13 -63.9(6) . . . . ?
O5 Dy1 O2 C13 103.2(6) . . . . ?
O4 Dy1 O2 C13 27.1(6) . . . . ?
O3 Dy1 O2 C13 43.8(7) . . . . ?
N3 Dy1 O2 C13 -43.7(6) . . . . ?
O6 Dy1 O2 C13 155.5(6) . . . . ?
O4 C14 O3 Dy1 -4.2(6) . . . . ?
C17 C14 O3 Dy1 176.5(5) . . . . ?
O2 Dy1 O3 C14 -18.6(5) . . . . ?
O6 Dy1 O3 C14 158.3(3) 2_667 . . . ?
O7 Dy1 O3 C14 -168.6(4) . . . . ?
O1 Dy1 O3 C14 111.3(4) . . . . ?
O5 Dy1 O3 C14 -78.2(4) . . . . ?
O4 Dy1 O3 C14 2.3(3) . . . . ?
N3 Dy1 O3 C14 54.7(4) . . . . ?
O6 Dy1 O3 C14 -110.7(4) . . . . ?
O3 C14 O4 Dy1 4.2(6) . . . . ?
C17 C14 O4 Dy1 -176.5(5) . . . . ?
O2 Dy1 O4 C14 163.1(4) . . . . ?
O6 Dy1 O4 C14 -146.9(4) 2_667 . . . ?
O7 Dy1 O4 C14 8.8(5) . . . . ?
O1 Dy1 O4 C14 -67.4(4) . . . . ?
O5 Dy1 O4 C14 83.6(4) . . . . ?
O3 Dy1 O4 C14 -2.3(4) . . . . ?
N3 Dy1 O4 C14 -127.1(4) . . . . ?
O6 Dy1 O4 C14 99.6(4) . . . . ?
O6 C15 O5 Dy1 17.2(7) . . . . ?
C18 C15 O5 Dy1 -161.1(6) . . . . ?
O2 Dy1 O5 C15 66.6(4) . . . . ?
O6 Dy1 O5 C15 -5.2(5) 2_667 . . . ?
O7 Dy1 O5 C15 -76.6(4) . . . . ?
O1 Dy1 O5 C15 -133.2(4) . . . . ?
O4 Dy1 O5 C15 153.7(4) . . . . ?
O3 Dy1 O5 C15 -151.5(4) . . . . ?
N3 Dy1 O5 C15 111.8(4) . . . . ?
O6 Dy1 O5 C15 -9.1(4) . . . . ?
O5 C15 O6 Dy1 -164.6(7) . . . 2_667 ?
C18 C15 O6 Dy1 13.7(15) . . . 2_667 ?
O5 C15 O6 Dy1 -15.5(6) . . . . ?
C18 C15 O6 Dy1 162.7(6) . . . . ?
O2 Dy1 O6 C15 -81.1(4) . . . . ?
O6 Dy1 O6 C15 -167.5(5) 2_667 . . . ?
O7 Dy1 O6 C15 111.2(4) . . . . ?
O1 Dy1 O6 C15 148.2(4) . . . . ?
O5 Dy1 O6 C15 8.8(4) . . . . ?
O4 Dy1 O6 C15 -11.4(4) . . . . ?
O3 Dy1 O6 C15 51.4(4) . . . . ?
N3 Dy1 O6 C15 -107.7(4) . . . . ?
O2 Dy1 O6 Dy1 86.44(19) . . . 2_667 ?
O6 Dy1 O6 Dy1 0.0 2_667 . . 2_667 ?
O7 Dy1 O6 Dy1 -81.3(2) . . . 2_667 ?
O1 Dy1 O6 Dy1 -44.2(3) . . . 2_667 ?
O5 Dy1 O6 Dy1 176.3(3) . . . 2_667 ?
O4 Dy1 O6 Dy1 156.16(17) . . . 2_667 ?
O3 Dy1 O6 Dy1 -141.08(17) . . . 2_667 ?
N3 Dy1 O6 Dy1 59.8(3) . . . 2_667 ?
O2 Dy1 O7 C16 -178.9(7) . . . . ?
O6 Dy1 O7 C16 128.1(8) 2_667 . . . ?
O1 Dy1 O7 C16 43.3(8) . . . . ?
O5 Dy1 O7 C16 -111.0(8) . . . . ?
O4 Dy1 O7 C16 -41.9(9) . . . . ?
O3 Dy1 O7 C16 -32.6(8) . . . . ?
N3 Dy1 O7 C16 60.0(9) . . . . ?
O6 Dy1 O7 C16 -160.3(8) . . . . ?

_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full        26.06
_diffrn_measured_fraction_theta_full 0.977
_refine_diff_density_max         0.903
_refine_diff_density_min         -1.064
_refine_diff_density_rms         0.128

#===END

data_Tm2
_database_code_depnum_ccdc_archive 'CCDC 972396'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H56 N6 O20 S2 Tm2'
_chemical_formula_weight         1318.87

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   9.3882(12)
_cell_length_b                   10.9654(14)
_cell_length_c                   13.1679(16)
_cell_angle_alpha                111.464(2)
_cell_angle_beta                 92.422(2)
_cell_angle_gamma                91.767(2)
_cell_volume                     1258.9(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5020
_cell_measurement_theta_min      2.66
_cell_measurement_theta_max      26.20

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             656
_exptl_absorpt_coefficient_mu    3.662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5279
_exptl_absorpt_correction_T_max  0.5919
_exptl_absorpt_process_details   '(Sadabs; Bruker,2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7023
_diffrn_reflns_av_R_equivalents  0.0209
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.66
_diffrn_reflns_theta_max         26.20
_reflns_number_total             4934
_reflns_number_gt                4341
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0387P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4934
_refine_ls_number_parameters     316
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0310
_refine_ls_wR_factor_ref         0.0765
_refine_ls_wR_factor_gt          0.0729
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.054
_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
Tm1 Tm 0.87093(2) 0.974045(18) 0.361152(14) 0.03185(8) Uani 1 1 d . . .
N1 N 0.2982(4) 0.6120(4) 0.0192(3) 0.0447(10) Uani 1 1 d . . .
N3 N 0.8557(4) 0.8592(4) 0.1589(3) 0.0356(9) Uani 1 1 d . . .
O1 O 0.6521(3) 0.8652(4) 0.2878(2) 0.0497(9) Uani 1 1 d . . .
O2 O 1.0917(3) 0.9704(3) 0.3063(2) 0.0384(7) Uani 1 1 d . . .
O3 O 0.8791(4) 1.1514(3) 0.2812(3) 0.0542(9) Uani 1 1 d . . .
O4 O 0.7037(4) 1.1427(4) 0.3808(4) 0.0650(11) Uani 1 1 d . . .
O5 O 0.8967(4) 0.7441(3) 0.3360(2) 0.0436(8) Uani 1 1 d . . .
O6 O 1.0194(3) 0.8712(3) 0.4830(2) 0.0399(8) Uani 1 1 d . . .
O7 O 0.7385(3) 0.9729(3) 0.5067(2) 0.0410(8) Uani 1 1 d . . .
O8 O 0.5252(5) 0.7950(4) 0.4950(4) 0.0796(14) Uani 1 1 d . . .
H8 H 0.4613 0.8102 0.5379 0.119 Uiso 1 1 calc R . .
O9 O 0.0352(6) 0.3318(5) 0.2230(5) 0.0899(15) Uani 1 1 d . . .
H9 H -0.0006 0.2663 0.2299 0.135 Uiso 1 1 calc R . .
O10 O 0.8929(4) 0.5075(4) 0.1552(3) 0.0581(10) Uani 1 1 d . . .
S1 S 0.52829(15) 0.64584(14) -0.07565(10) 0.0491(3) Uani 1 1 d D . .
H1 H 0.4503(14) 0.638(5) -0.1478(13) 0.074 Uiso 1 1 d D . .
C5 C 0.4375(5) 0.6664(4) 0.0375(3) 0.0362(10) Uani 1 1 d D . .
C4 C 0.2121(5) 0.6169(5) 0.0990(4) 0.0513(13) Uani 1 1 d . . .
H4 H 0.1208 0.5772 0.0809 0.062 Uiso 1 1 calc R . .
C3 C 0.2560(6) 0.6793(5) 0.2063(5) 0.0504(13) Uani 1 1 d . . .
H3 H 0.1962 0.6823 0.2616 0.060 Uiso 1 1 calc R . .
C2 C 0.3929(5) 0.7384(5) 0.2306(4) 0.0442(12) Uani 1 1 d . . .
H2 H 0.4240 0.7829 0.3032 0.053 Uiso 1 1 calc R . .
C1 C 0.4834(5) 0.7325(4) 0.1495(4) 0.0365(10) Uani 1 1 d . . .
C6 C 0.6258(5) 0.8010(4) 0.1891(4) 0.0379(11) Uani 1 1 d . . .
N2 N 0.7248(4) 0.7932(4) 0.1185(3) 0.0425(10) Uani 1 1 d . . .
H3A H 0.7085 0.7486 0.0499 0.051 Uiso 1 1 calc R . .
C7 C 0.9456(5) 0.8572(4) 0.0879(4) 0.0389(11) Uani 1 1 d . . .
H7 H 0.9170 0.8123 0.0148 0.047 Uiso 1 1 calc R . .
C8 C 1.0869(5) 0.9185(4) 0.1117(3) 0.0368(11) Uani 1 1 d . . .
C9 C 1.1630(6) 0.9213(5) 0.0224(4) 0.0474(12) Uani 1 1 d . . .
H9A H 1.1206 0.8828 -0.0478 0.057 Uiso 1 1 calc R . .
C10 C 1.2985(6) 0.9793(5) 0.0361(4) 0.0528(14) Uani 1 1 d . . .
H10 H 1.3461 0.9827 -0.0234 0.063 Uiso 1 1 calc R . .
C11 C 1.3615(6) 1.0323(5) 0.1406(4) 0.0528(14) Uani 1 1 d . . .
H11 H 1.4531 1.0712 0.1508 0.063 Uiso 1 1 calc R . .
C12 C 1.2939(5) 1.0295(5) 0.2295(4) 0.0463(12) Uani 1 1 d . . .
H12 H 1.3408 1.0654 0.2984 0.056 Uiso 1 1 calc R . .
C13 C 1.1535(5) 0.9729(4) 0.2190(4) 0.0359(10) Uani 1 1 d . . .
C14 C 0.7627(6) 1.1940(5) 0.3210(4) 0.0470(12) Uani 1 1 d . . .
C16 C 0.6970(7) 1.3063(6) 0.2999(6) 0.0717(18) Uani 1 1 d . . .
H16A H 0.5958 1.3023 0.3074 0.108 Uiso 1 1 calc R . .
H16B H 0.7150 1.3007 0.2271 0.108 Uiso 1 1 calc R . .
H16C H 0.7381 1.3878 0.3516 0.108 Uiso 1 1 calc R . .
C15 C 0.9690(5) 0.7584(4) 0.4211(4) 0.0370(11) Uani 1 1 d . . .
C17 C 0.9991(8) 0.6441(5) 0.4523(5) 0.075(2) Uani 1 1 d . . .
H17A H 0.9516 0.5664 0.3999 0.113 Uiso 1 1 calc R . .
H17B H 0.9649 0.6590 0.5234 0.113 Uiso 1 1 calc R . .
H17C H 1.1001 0.6332 0.4539 0.113 Uiso 1 1 calc R . .
C18 C 0.5468(10) 0.6612(8) 0.4543(7) 0.104(3) Uani 1 1 d . . .
H18A H 0.6150 0.6423 0.3989 0.156 Uiso 1 1 calc R . .
H18B H 0.4581 0.6136 0.4233 0.156 Uiso 1 1 calc R . .
H18C H 0.5823 0.6355 0.5125 0.156 Uiso 1 1 calc R . .
C19 C 0.1795(9) 0.3453(7) 0.2560(7) 0.100(3) Uani 1 1 d . . .
H19A H 0.2172 0.4299 0.2614 0.149 Uiso 1 1 calc R . .
H19B H 0.2299 0.2781 0.2035 0.149 Uiso 1 1 calc R . .
H19C H 0.1909 0.3372 0.3261 0.149 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
Tm1 O2 2.220(3) . ?
Tm1 O6 2.306(3) 2_776 ?
Tm1 O1 2.328(3) . ?
Tm1 O7 2.332(3) . ?
Tm1 O4 2.411(4) . ?
Tm1 O5 2.441(3) . ?
Tm1 N3 2.490(3) . ?
Tm1 O3 2.528(3) . ?
Tm1 O6 2.649(3) . ?
N1 C4 1.339(6) . ?
N1 C5 1.394(6) . ?
N3 C7 1.280(5) . ?
N3 N2 1.388(5) . ?
O1 C6 1.240(5) . ?
O2 C13 1.318(5) . ?
O3 C14 1.260(6) . ?
O4 C14 1.258(6) . ?
O5 C15 1.241(6) . ?
O6 C15 1.270(5) . ?
O6 Tm1 2.306(3) 2_776 ?
O8 C18 1.390(8) . ?
O8 H8 0.8200 . ?
O9 C19 1.391(9) . ?
O9 H9 0.8200 . ?
S1 C5 1.694(4) . ?
S1 H1 1.1500(10) . ?
C5 C1 1.426(6) . ?
C4 C3 1.364(7) . ?
C4 H4 0.9300 . ?
C3 C2 1.392(7) . ?
C3 H3 0.9300 . ?
C2 C1 1.376(6) . ?
C2 H2 0.9300 . ?
C1 C6 1.488(6) . ?
C6 N2 1.324(6) . ?
N2 H3A 0.8600 . ?
C7 C8 1.437(6) . ?
C7 H7 0.9300 . ?
C8 C9 1.411(6) . ?
C8 C13 1.424(6) . ?
C9 C10 1.379(7) . ?
C9 H9A 0.9300 . ?
C10 C11 1.381(7) . ?
C10 H10 0.9300 . ?
C11 C12 1.364(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.419(6) . ?
C12 H12 0.9300 . ?
C14 C16 1.503(7) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C15 C17 1.486(7) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Tm1 O6 80.95(11) . 2_776 ?
O2 Tm1 O1 136.46(11) . . ?
O6 Tm1 O1 142.58(11) 2_776 . ?
O2 Tm1 O7 143.17(11) . . ?
O6 Tm1 O7 73.35(10) 2_776 . ?
O1 Tm1 O7 72.63(11) . . ?
O2 Tm1 O4 126.87(12) . . ?
O6 Tm1 O4 83.28(13) 2_776 . ?
O1 Tm1 O4 73.95(14) . . ?
O7 Tm1 O4 76.22(12) . . ?
O2 Tm1 O5 86.09(11) . . ?
O6 Tm1 O5 116.93(11) 2_776 . ?
O1 Tm1 O5 73.36(12) . . ?
O7 Tm1 O5 82.66(11) . . ?
O4 Tm1 O5 145.08(13) . . ?
O2 Tm1 N3 72.99(11) . . ?
O6 Tm1 N3 150.03(11) 2_776 . ?
O1 Tm1 N3 65.12(11) . . ?
O7 Tm1 N3 136.57(11) . . ?
O4 Tm1 N3 100.55(14) . . ?
O5 Tm1 N3 76.33(11) . . ?
O2 Tm1 O3 76.50(12) . . ?
O6 Tm1 O3 86.22(11) 2_776 . ?
O1 Tm1 O3 101.73(13) . . ?
O7 Tm1 O3 126.33(12) . . ?
O4 Tm1 O3 52.02(12) . . ?
O5 Tm1 O3 148.60(11) . . ?
N3 Tm1 O3 73.69(12) . . ?
O2 Tm1 O6 75.47(10) . . ?
O6 Tm1 O6 66.48(12) 2_776 . ?
O1 Tm1 O6 114.83(11) . . ?
O7 Tm1 O6 70.31(11) . . ?
O4 Tm1 O6 139.81(12) . . ?
O5 Tm1 O6 50.53(10) . . ?
N3 Tm1 O6 118.97(11) . . ?
O3 Tm1 O6 143.36(11) . . ?
C4 N1 C5 124.0(4) . . ?
C7 N3 N2 116.3(4) . . ?
C7 N3 Tm1 130.4(3) . . ?
N2 N3 Tm1 113.2(2) . . ?
C6 O1 Tm1 123.9(3) . . ?
C13 O2 Tm1 137.0(3) . . ?
C14 O3 Tm1 91.7(3) . . ?
C14 O4 Tm1 97.3(3) . . ?
C15 O5 Tm1 99.5(3) . . ?
C15 O6 Tm1 156.4(3) . 2_776 ?
C15 O6 Tm1 88.9(3) . . ?
Tm1 O6 Tm1 113.52(12) 2_776 . ?
C18 O8 H8 109.5 . . ?
C19 O9 H9 109.5 . . ?
C5 S1 H1 110.1(8) . . ?
N1 C5 C1 115.1(4) . . ?
N1 C5 S1 115.9(3) . . ?
C1 C5 S1 129.0(3) . . ?
N1 C4 C3 121.1(5) . . ?
N1 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C4 C3 C2 118.1(5) . . ?
C4 C3 H3 121.0 . . ?
C2 C3 H3 121.0 . . ?
C1 C2 C3 121.5(5) . . ?
C1 C2 H2 119.2 . . ?
C3 C2 H2 119.2 . . ?
C2 C1 C5 120.2(4) . . ?
C2 C1 C6 114.9(4) . . ?
C5 C1 C6 124.9(4) . . ?
O1 C6 N2 119.9(4) . . ?
O1 C6 C1 120.3(4) . . ?
N2 C6 C1 119.8(4) . . ?
C6 N2 N3 117.9(4) . . ?
C6 N2 H3A 121.1 . . ?
N3 N2 H3A 121.1 . . ?
N3 C7 C8 125.5(4) . . ?
N3 C7 H7 117.2 . . ?
C8 C7 H7 117.2 . . ?
C9 C8 C13 119.2(4) . . ?
C9 C8 C7 117.2(4) . . ?
C13 C8 C7 123.6(4) . . ?
C10 C9 C8 122.0(5) . . ?
C10 C9 H9A 119.0 . . ?
C8 C9 H9A 119.0 . . ?
C9 C10 C11 118.2(4) . . ?
C9 C10 H10 120.9 . . ?
C11 C10 H10 120.9 . . ?
C12 C11 C10 122.2(5) . . ?
C12 C11 H11 118.9 . . ?
C10 C11 H11 118.9 . . ?
C11 C12 C13 121.3(5) . . ?
C11 C12 H12 119.4 . . ?
C13 C12 H12 119.4 . . ?
O2 C13 C12 119.9(4) . . ?
O2 C13 C8 123.0(4) . . ?
C12 C13 C8 117.1(4) . . ?
O4 C14 O3 118.9(5) . . ?
O4 C14 C16 120.4(5) . . ?
O3 C14 C16 120.7(5) . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O5 C15 O6 120.5(4) . . ?
O5 C15 C17 120.9(4) . . ?
O6 C15 C17 118.6(5) . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O8 C18 H18A 109.5 . . ?
O8 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O8 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O9 C19 H19A 109.5 . . ?
O9 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O9 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full        26.20
_diffrn_measured_fraction_theta_full 0.976
_refine_diff_density_max         0.665
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.107

#===END

data_Yb2
_database_code_depnum_ccdc_archive 'CCDC 972397'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C70 H84 N12 O32 S4 Yb4'
_chemical_formula_weight         2425.89

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.885(4)
_cell_length_b                   12.424(4)
_cell_length_c                   17.847(7)
_cell_angle_alpha                70.887(6)
_cell_angle_beta                 73.303(6)
_cell_angle_gamma                89.712(6)
_cell_volume                     2173.8(14)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7339
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      24.99

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.853
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1188
_exptl_absorpt_coefficient_mu    4.447
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4700
_exptl_absorpt_correction_T_max  0.5364
_exptl_absorpt_process_details   '(Sadabs; Bruker,2000)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12326
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.27
_diffrn_reflns_theta_max         25.02
_reflns_number_total             7599
_reflns_number_gt                6296
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0283P)²+6.1818P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7599
_refine_ls_number_parameters     557
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0302
_refine_ls_wR_factor_ref         0.0751
_refine_ls_wR_factor_gt          0.0700
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_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
Yb1 Yb 0.65250(2) 0.101580(19) 0.487661(14) 0.02603(7) Uani 1 1 d . . .
Yb2 Yb 0.55934(2) 0.83491(2) 1.032947(15) 0.03244(8) Uani 1 1 d . . .
N1 N 1.0167(5) 0.4030(5) 0.6302(3) 0.0477(14) Uani 1 1 d . . .
N2 N 0.9295(4) 0.2040(4) 0.4898(3) 0.0344(11) Uani 1 1 d . . .
H2A H 1.0094 0.2274 0.4776 0.041 Uiso 1 1 calc R . .
N3 N 0.8898(4) 0.1360(4) 0.4500(3) 0.0285(10) Uani 1 1 d . . .
N4 N 1.0844(5) 0.6942(4) 0.7574(3) 0.0437(13) Uani 1 1 d . . .
N5 N 0.6883(5) 0.7113(4) 0.8918(3) 0.0469(14) Uani 1 1 d . . .
H5 H 0.7000 0.6720 0.8590 0.056 Uiso 1 1 calc RD . .
N6 N 0.5665(5) 0.7203(4) 0.9402(3) 0.0399(12) Uani 1 1 d . . .
O1 O 0.7222(3) 0.1949(4) 0.5639(2) 0.0385(10) Uani 1 1 d . . .
O2 O 0.7356(3) 0.0188(3) 0.3945(2) 0.0354(9) Uani 1 1 d . . .
O3 O 0.7002(4) -0.0590(3) 0.5893(3) 0.0435(10) Uani 1 1 d . . .
O4 O 0.4727(4) 0.1261(4) 0.5864(3) 0.0482(11) Uani 1 1 d . . .
O5 O 0.6813(4) 0.2825(3) 0.3990(2) 0.0386(10) Uani 1 1 d . . .
O6 O 0.4762(3) 0.0871(3) 0.4399(2) 0.0308(9) Uani 1 1 d . . .
O7 O 0.8095(4) 0.4442(3) 0.3412(3) 0.0483(11) Uani 1 1 d . . .
O8 O 0.7663(4) 0.8265(4) 0.9453(3) 0.0478(11) Uani 1 1 d . . .
O9 O 0.3623(4) 0.8153(3) 1.0229(3) 0.0450(11) Uani 1 1 d . . .
O10 O 0.4842(6) 0.6408(4) 1.1198(3) 0.0675(15) Uani 1 1 d . . .
O11 O 0.6703(5) 0.7026(4) 1.1207(3) 0.0605(13) Uani 1 1 d . . .
O12 O 0.4751(4) 0.8484(4) 1.1696(3) 0.0461(11) Uani 1 1 d . . .
O13 O 0.7054(4) 0.9729(4) 1.0361(3) 0.0442(10) Uani 1 1 d . . .
H13 H 0.6813 1.0471 1.0216 0.053 Uiso 1 1 calc R . .
O14 O 0.5631(4) 0.9976(4) 0.9214(2) 0.0425(10) Uani 1 1 d . . .
O15 O 0.8106(6) 0.6794(5) 0.2318(4) 0.0905(19) Uani 1 1 d . . .
O16 O 0.4301(5) 0.2458(4) 0.6932(3) 0.0637(14) Uani 1 1 d . . .
S1 S 1.13901(17) 0.35081(19) 0.49912(13) 0.0635(6) Uani 1 1 d . . .
H1 H 1.1999 0.2740 0.5246 0.095 Uiso 1 1 calc R . .
S2 S 0.85412(18) 0.65038(17) 0.74916(12) 0.0558(5) Uani 1 1 d . . .
H2 H 0.8150 0.5528 0.7913 0.084 Uiso 1 1 calc RD . .
C1 C 0.8756(6) 0.2995(5) 0.5932(4) 0.0351(13) Uani 1 1 d . . .
C2 C 0.7771(6) 0.3104(5) 0.6586(4) 0.0450(16) Uani 1 1 d . . .
H2B H 0.6940 0.2804 0.6674 0.054 Uiso 1 1 calc R . .
C3 C 0.7971(7) 0.3642(6) 0.7121(5) 0.0568(19) Uani 1 1 d . . .
H3 H 0.7303 0.3693 0.7566 0.068 Uiso 1 1 calc R . .
C4 C 0.9202(7) 0.4092(6) 0.6955(5) 0.0544(18) Uani 1 1 d . . .
H4 H 0.9379 0.4449 0.7301 0.065 Uiso 1 1 calc R . .
C5 C 1.0040(6) 0.3483(5) 0.5762(4) 0.0371(14) Uani 1 1 d . . .
C6 C 0.8384(5) 0.2306(5) 0.5473(3) 0.0322(13) Uani 1 1 d . . .
C7 C 0.9832(5) 0.0973(5) 0.4056(3) 0.0318(13) Uani 1 1 d . . .
H7 H 1.0663 0.1144 0.4055 0.038 Uiso 1 1 calc R . .
C8 C 0.9681(5) 0.0293(5) 0.3558(3) 0.0308(12) Uani 1 1 d . . .
C9 C 1.0827(6) 0.0013(5) 0.3075(4) 0.0424(15) Uani 1 1 d . . .
H9 H 1.1614 0.0244 0.3110 0.051 Uiso 1 1 calc R . .
C10 C 1.0813(6) -0.0589(6) 0.2556(4) 0.0490(17) Uani 1 1 d . . .
H10 H 1.1578 -0.0765 0.2243 0.059 Uiso 1 1 calc R . .
C11 C 0.9633(6) -0.0934(6) 0.2506(4) 0.0492(17) Uani 1 1 d . . .
H11 H 0.9611 -0.1345 0.2158 0.059 Uiso 1 1 calc R . .
C12 C 0.8498(6) -0.0671(5) 0.2967(4) 0.0449(16) Uani 1 1 d . . .
H12 H 0.7722 -0.0907 0.2921 0.054 Uiso 1 1 calc R . .
C13 C 0.8480(5) -0.0049(5) 0.3510(3) 0.0315(12) Uani 1 1 d . . .
C14 C 0.7094(5) 0.3846(5) 0.3938(4) 0.0351(13) Uani 1 1 d . . .
C15 C 0.3943(5) 0.1247(5) 0.4010(4) 0.0367(14) Uani 1 1 d . . .
C16 C 0.6182(7) 0.4358(6) 0.4510(5) 0.061(2) Uani 1 1 d . . .
H16A H 0.6463 0.5153 0.4357 0.091 Uiso 1 1 calc R . .
H16B H 0.6170 0.3962 0.5073 0.091 Uiso 1 1 calc R . .
H16C H 0.5331 0.4285 0.4464 0.091 Uiso 1 1 calc R . .
C17 C 0.4125(8) 0.2475(6) 0.3450(6) 0.083(3) Uani 1 1 d . . .
H17A H 0.3485 0.2608 0.3164 0.124 Uiso 1 1 calc R . .
H17B H 0.4968 0.2636 0.3052 0.124 Uiso 1 1 calc R . .
H17C H 0.4038 0.2966 0.3777 0.124 Uiso 1 1 calc R . .
C18 C 0.9207(6) 0.7547(5) 0.8531(4) 0.0372(14) Uani 1 1 d . . .
C19 C 1.0203(6) 0.7969(6) 0.8751(4) 0.0485(16) Uani 1 1 d . . .
H19 H 0.9995 0.8322 0.9151 0.058 Uiso 1 1 calc R . .
C20 C 1.1471(6) 0.7871(6) 0.8387(4) 0.0529(17) Uani 1 1 d . . .
H20 H 1.2119 0.8154 0.8537 0.063 Uiso 1 1 calc R . .
C21 C 1.1770(7) 0.7350(6) 0.7800(4) 0.0518(17) Uani 1 1 d . . .
H21 H 1.2629 0.7276 0.7552 0.062 Uiso 1 1 calc R . .
C22 C 0.9540(6) 0.7019(5) 0.7905(4) 0.0391(14) Uani 1 1 d . . .
C23 C 0.7868(6) 0.7673(5) 0.8988(4) 0.0399(14) Uani 1 1 d . . .
C24 C 0.4750(6) 0.6520(5) 0.9410(4) 0.0462(16) Uani 1 1 d . . .
H24 H 0.4978 0.6036 0.9100 0.055 Uiso 1 1 calc R . .
C25 C 0.3414(6) 0.6465(5) 0.9866(4) 0.0460(16) Uani 1 1 d . . .
C26 C 0.2581(7) 0.5572(6) 0.9906(5) 0.0551(18) Uani 1 1 d . . .
H26 H 0.2913 0.5054 0.9641 0.066 Uiso 1 1 calc R . .
C27 C 0.1273(8) 0.5447(6) 1.0331(5) 0.064(2) Uani 1 1 d . . .
H27 H 0.0740 0.4835 1.0371 0.077 Uiso 1 1 calc R . .
C28 C 0.0774(7) 0.6248(7) 1.0696(5) 0.066(2) Uani 1 1 d . . .
H28 H -0.0105 0.6181 1.0967 0.079 Uiso 1 1 calc R . .
C29 C 0.1558(6) 0.7145(6) 1.0666(5) 0.0556(18) Uani 1 1 d . . .
H29 H 0.1194 0.7663 1.0921 0.067 Uiso 1 1 calc R . .
C30 C 0.2905(6) 0.7292(5) 1.0253(4) 0.0407(14) Uani 1 1 d . . .
C31 C 0.5525(5) 1.0490(5) 0.8494(4) 0.0385(14) Uani 1 1 d . . .
C32 C 0.8206(9) 0.9633(8) 1.0558(8) 0.113(4) Uani 1 1 d . . .
H32A H 0.8460 0.8876 1.0617 0.170 Uiso 1 1 calc R . .
H32B H 0.8090 0.9772 1.1071 0.170 Uiso 1 1 calc R . .
H32C H 0.8863 1.0184 1.0122 0.170 Uiso 1 1 calc R . .
C33 C 0.5666(7) 0.9872(6) 0.7882(4) 0.0563(18) Uani 1 1 d . . .
H33A H 0.4835 0.9543 0.7937 0.084 Uiso 1 1 calc R . .
H33B H 0.6222 0.9276 0.7991 0.084 Uiso 1 1 calc R . .
H33C H 0.6031 1.0403 0.7327 0.084 Uiso 1 1 calc R . .
C39 C 0.5766(8) 0.6265(6) 1.1486(5) 0.0545(18) Uani 1 1 d . . .
C41 C 0.5764(11) 0.5179(7) 1.2187(6) 0.106(4) Uani 1 1 d . . .
H41A H 0.5098 0.4625 1.2250 0.158 Uiso 1 1 calc R . .
H41B H 0.5609 0.5343 1.2695 0.158 Uiso 1 1 calc R . .
H41C H 0.6584 0.4880 1.2064 0.158 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
Yb1 O2 2.211(4) . ?
Yb1 O5 2.246(4) . ?
Yb1 O4 2.322(4) . ?
Yb1 O1 2.324(4) . ?
Yb1 O6 2.342(3) . ?
Yb1 O3 2.388(4) . ?
Yb1 N3 2.476(4) . ?
Yb1 O6 2.477(4) 2_656 ?
Yb1 C15 2.808(6) 2_656 ?
Yb1 Yb1 4.0129(12) 2_656 ?
Yb2 O9 2.224(4) . ?
Yb2 O14 2.317(4) . ?
Yb2 O8 2.369(4) . ?
Yb2 O13 2.370(4) . ?
Yb2 O10 2.394(5) . ?
Yb2 O12 2.407(4) . ?
Yb2 O11 2.448(5) . ?
Yb2 N6 2.498(5) . ?
Yb2 O14 2.688(4) 2_677 ?
Yb2 C39 2.778(7) . ?
Yb2 C31 2.911(6) 2_677 ?
Yb2 Yb2 4.1881(14) 2_677 ?
N1 C4 1.349(8) . ?
N1 C5 1.386(7) . ?
N2 C6 1.334(7) . ?
N2 N3 1.406(6) . ?
N2 H2A 0.8600 . ?
N3 C7 1.294(7) . ?
N4 C21 1.345(8) . ?
N4 C22 1.388(8) . ?
N5 C23 1.338(8) . ?
N5 N6 1.386(7) . ?
N5 H5 0.8600 . ?
N6 C24 1.306(8) . ?
O1 C6 1.261(6) . ?
O2 C13 1.336(6) . ?
O3 C15 1.252(6) 2_656 ?
O5 C14 1.274(7) . ?
O6 C15 1.278(6) . ?
O6 Yb1 2.477(4) 2_656 ?
O7 C14 1.258(7) . ?
O8 C23 1.254(7) . ?
O9 C30 1.309(7) . ?
O10 C39 1.241(9) . ?
O11 C39 1.262(8) . ?
O12 C31 1.267(7) 2_677 ?
O13 C32 1.390(9) . ?
O13 H13 0.9300 . ?
O14 C31 1.273(7) . ?
O14 Yb2 2.688(4) 2_677 ?
S1 C5 1.692(6) . ?
S1 H1 1.2000 . ?
S2 C22 1.706(7) . ?
S2 H2 1.2000 . ?
C1 C2 1.384(8) . ?
C1 C5 1.434(8) . ?
C1 C6 1.491(7) . ?
C2 C3 1.394(9) . ?
C2 H2B 0.9300 . ?
C3 C4 1.366(9) . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C7 C8 1.451(8) . ?
C7 H7 0.9300 . ?
C8 C13 1.412(7) . ?
C8 C9 1.412(8) . ?
C9 C10 1.371(9) . ?
C9 H9 0.9300 . ?
C10 C11 1.392(9) . ?
C10 H10 0.9300 . ?
C11 C12 1.377(8) . ?
C11 H11 0.9300 . ?
C12 C13 1.420(8) . ?
C12 H12 0.9300 . ?
C14 C16 1.506(8) . ?
C15 O3 1.252(6) 2_656 ?
C15 C17 1.502(9) . ?
C15 Yb1 2.808(6) 2_656 ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C19 1.410(9) . ?
C18 C22 1.434(8) . ?
C18 C23 1.488(8) . ?
C19 C20 1.370(9) . ?
C19 H19 0.9300 . ?
C20 C21 1.367(9) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C24 C25 1.438(9) . ?
C24 H24 0.9300 . ?
C25 C26 1.407(9) . ?
C25 C30 1.443(9) . ?
C26 C27 1.390(10) . ?
C26 H26 0.9300 . ?
C27 C28 1.388(11) . ?
C27 H27 0.9300 . ?
C28 C29 1.384(9) . ?
C28 H28 0.9300 . ?
C29 C30 1.422(9) . ?
C29 H29 0.9300 . ?
C31 O12 1.267(7) 2_677 ?
C31 C33 1.501(8) . ?
C31 Yb2 2.911(6) 2_677 ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C39 C41 1.510(10) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Yb1 O5 97.39(15) . . ?
O2 Yb1 O4 148.32(13) . . ?
O5 Yb1 O4 96.07(16) . . ?
O2 Yb1 O1 138.77(13) . . ?
O5 Yb1 O1 80.31(15) . . ?
O4 Yb1 O1 71.88(13) . . ?
O2 Yb1 O6 79.36(13) . . ?
O5 Yb1 O6 83.63(13) . . ?
O4 Yb1 O6 73.80(14) . . ?
O1 Yb1 O6 140.06(13) . . ?
O2 Yb1 O3 87.91(15) . . ?
O5 Yb1 O3 155.83(14) . . ?
O4 Yb1 O3 91.40(16) . . ?
O1 Yb1 O3 80.25(15) . . ?
O6 Yb1 O3 120.54(13) . . ?
O2 Yb1 N3 73.14(13) . . ?
O5 Yb1 N3 80.56(15) . . ?
O4 Yb1 N3 137.57(14) . . ?
O1 Yb1 N3 65.84(14) . . ?
O6 Yb1 N3 146.03(14) . . ?
O3 Yb1 N3 78.46(14) . . ?
O2 Yb1 O6 81.22(13) . 2_656 ?
O5 Yb1 O6 150.71(13) . 2_656 ?
O4 Yb1 O6 73.16(14) . 2_656 ?
O1 Yb1 O6 119.76(13) . 2_656 ?
O6 Yb1 O6 67.29(14) . 2_656 ?
O3 Yb1 O6 53.36(12) . 2_656 ?
N3 Yb1 O6 125.89(13) . 2_656 ?
O2 Yb1 C15 83.17(17) . 2_656 ?
O5 Yb1 C15 177.65(15) . 2_656 ?
O4 Yb1 C15 82.35(17) . 2_656 ?
O1 Yb1 C15 100.79(16) . 2_656 ?
O6 Yb1 C15 94.24(15) . 2_656 ?
O3 Yb1 C15 26.32(14) . 2_656 ?
N3 Yb1 C15 101.79(15) . 2_656 ?
O6 Yb1 C15 27.07(14) 2_656 2_656 ?
O2 Yb1 Yb1 78.35(9) . 2_656 ?
O5 Yb1 Yb1 118.27(10) . 2_656 ?
O4 Yb1 Yb1 70.02(10) . 2_656 ?
O1 Yb1 Yb1 138.93(9) . 2_656 ?
O6 Yb1 Yb1 34.71(9) . 2_656 ?
O3 Yb1 Yb1 85.88(9) . 2_656 ?
N3 Yb1 Yb1 147.78(10) . 2_656 ?
O6 Yb1 Yb1 32.58(8) 2_656 2_656 ?
C15 Yb1 Yb1 59.57(12) 2_656 2_656 ?
O9 Yb2 O14 78.61(15) . . ?
O9 Yb2 O8 132.34(16) . . ?
O14 Yb2 O8 82.21(15) . . ?
O9 Yb2 O13 140.76(14) . . ?
O14 Yb2 O13 74.72(15) . . ?
O8 Yb2 O13 71.56(14) . . ?
O9 Yb2 O10 77.03(18) . . ?
O14 Yb2 O10 152.50(17) . . ?
O8 Yb2 O10 105.22(18) . . ?
O13 Yb2 O10 132.77(17) . . ?
O9 Yb2 O12 91.84(16) . . ?
O14 Yb2 O12 116.68(15) . . ?
O8 Yb2 O12 135.58(15) . . ?
O13 Yb2 O12 75.47(15) . . ?
O10 Yb2 O12 76.79(16) . . ?
O9 Yb2 O11 130.13(17) . . ?
O14 Yb2 O11 150.60(16) . . ?
O8 Yb2 O11 73.13(16) . . ?
O13 Yb2 O11 82.35(16) . . ?
O10 Yb2 O11 53.38(18) . . ?
O12 Yb2 O11 73.72(16) . . ?
O9 Yb2 N6 71.93(16) . . ?
O14 Yb2 N6 88.14(16) . . ?
O8 Yb2 N6 64.19(15) . . ?
O13 Yb2 N6 134.28(15) . . ?
O10 Yb2 N6 72.32(17) . . ?
O12 Yb2 N6 147.56(16) . . ?
O11 Yb2 N6 95.10(17) . . ?
O9 Yb2 O14 74.84(14) . 2_677 ?
O14 Yb2 O14 66.63(16) . 2_677 ?
O8 Yb2 O14 134.17(13) . 2_677 ?
O13 Yb2 O14 68.40(13) . 2_677 ?
O10 Yb2 O14 118.07(17) . 2_677 ?
O12 Yb2 O14 50.65(13) . 2_677 ?
O11 Yb2 O14 121.29(15) . 2_677 ?
N6 Yb2 O14 141.56(14) . 2_677 ?
O9 Yb2 C39 103.2(2) . . ?
O14 Yb2 C39 171.27(18) . . ?
O8 Yb2 C39 90.5(2) . . ?
O13 Yb2 C39 107.6(2) . . ?
O10 Yb2 C39 26.46(19) . . ?
O12 Yb2 C39 71.94(18) . . ?
O11 Yb2 C39 27.00(19) . . ?
N6 Yb2 C39 84.36(19) . . ?
O14 Yb2 C39 122.09(17) 2_677 . ?
O9 Yb2 C31 86.60(16) . 2_677 ?
O14 Yb2 C31 91.32(17) . 2_677 ?
O8 Yb2 C31 137.27(15) . 2_677 ?
O13 Yb2 C31 66.01(15) . 2_677 ?
O10 Yb2 C31 99.74(18) . 2_677 ?
O12 Yb2 C31 25.36(15) . 2_677 ?
O11 Yb2 C31 95.99(17) . 2_677 ?
N6 Yb2 C31 158.20(16) . 2_677 ?
O14 Yb2 C31 25.89(14) 2_677 2_677 ?
C39 Yb2 C31 97.30(19) . 2_677 ?
O9 Yb2 Yb2 73.91(11) . 2_677 ?
O14 Yb2 Yb2 36.10(11) . 2_677 ?
O8 Yb2 Yb2 111.86(11) . 2_677 ?
O13 Yb2 Yb2 67.53(10) . 2_677 ?
O10 Yb2 Yb2 142.45(15) . 2_677 ?
O12 Yb2 Yb2 80.88(10) . 2_677 ?
O11 Yb2 Yb2 144.64(13) . 2_677 ?
N6 Yb2 Yb2 119.00(12) . 2_677 ?
O14 Yb2 Yb2 30.53(9) 2_677 2_677 ?
C39 Yb2 Yb2 152.62(15) . 2_677 ?
C31 Yb2 Yb2 55.62(13) 2_677 2_677 ?
C4 N1 C5 124.7(5) . . ?
C6 N2 N3 117.3(4) . . ?
C6 N2 H2A 121.3 . . ?
N3 N2 H2A 121.3 . . ?
C7 N3 N2 114.3(4) . . ?
C7 N3 Yb1 132.4(3) . . ?
N2 N3 Yb1 113.2(3) . . ?
C21 N4 C22 123.6(5) . . ?
C23 N5 N6 116.2(5) . . ?
C23 N5 H5 121.9 . . ?
N6 N5 H5 121.9 . . ?
C24 N6 N5 114.5(5) . . ?
C24 N6 Yb2 128.7(4) . . ?
N5 N6 Yb2 115.6(3) . . ?
C6 O1 Yb1 123.0(3) . . ?
C13 O2 Yb1 142.0(3) . . ?
C15 O3 Yb1 95.9(3) 2_656 . ?
C14 O5 Yb1 141.0(4) . . ?
C15 O6 Yb1 155.6(4) . . ?
C15 O6 Yb1 91.1(3) . 2_656 ?
Yb1 O6 Yb1 112.71(14) . 2_656 ?
C23 O8 Yb2 123.4(4) . . ?
C30 O9 Yb2 133.8(4) . . ?
C39 O10 Yb2 94.3(4) . . ?
C39 O11 Yb2 91.2(4) . . ?
C31 O12 Yb2 100.2(4) 2_677 . ?
C32 O13 Yb2 131.7(5) . . ?
C32 O13 H13 114.1 . . ?
Yb2 O13 H13 114.1 . . ?
C31 O14 Yb2 152.9(4) . . ?
C31 O14 Yb2 86.9(4) . 2_677 ?
Yb2 O14 Yb2 113.37(16) . 2_677 ?
C5 S1 H1 109.5 . . ?
C22 S2 H2 109.5 . . ?
C2 C1 C5 120.0(5) . . ?
C2 C1 C6 115.3(5) . . ?
C5 C1 C6 124.6(5) . . ?
C1 C2 C3 122.8(6) . . ?
C1 C2 H2B 118.6 . . ?
C3 C2 H2B 118.6 . . ?
C4 C3 C2 116.4(6) . . ?
C4 C3 H3 121.8 . . ?
C2 C3 H3 121.8 . . ?
N1 C4 C3 121.7(6) . . ?
N1 C4 H4 119.1 . . ?
C3 C4 H4 119.1 . . ?
N1 C5 C1 114.3(5) . . ?
N1 C5 S1 116.3(4) . . ?
C1 C5 S1 129.4(4) . . ?
O1 C6 N2 119.9(5) . . ?
O1 C6 C1 120.5(5) . . ?
N2 C6 C1 119.6(5) . . ?
N3 C7 C8 125.0(5) . . ?
N3 C7 H7 117.5 . . ?
C8 C7 H7 117.5 . . ?
C13 C8 C9 119.6(5) . . ?
C13 C8 C7 123.8(5) . . ?
C9 C8 C7 116.5(5) . . ?
C10 C9 C8 121.9(6) . . ?
C10 C9 H9 119.0 . . ?
C8 C9 H9 119.0 . . ?
C9 C10 C11 118.9(6) . . ?
C9 C10 H10 120.6 . . ?
C11 C10 H10 120.6 . . ?
C12 C11 C10 120.7(6) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C11 C12 C13 121.8(6) . . ?
C11 C12 H12 119.1 . . ?
C13 C12 H12 119.1 . . ?
O2 C13 C8 123.1(5) . . ?
O2 C13 C12 119.8(5) . . ?
C8 C13 C12 117.1(5) . . ?
O7 C14 O5 121.8(5) . . ?
O7 C14 C16 119.4(5) . . ?
O5 C14 C16 118.8(5) . . ?
O3 C15 O6 119.5(5) 2_656 . ?
O3 C15 C17 121.1(5) 2_656 . ?
O6 C15 C17 119.3(5) . . ?
O3 C15 Yb1 57.7(3) 2_656 2_656 ?
O6 C15 Yb1 61.9(3) . 2_656 ?
C17 C15 Yb1 176.6(5) . 2_656 ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 C22 118.9(5) . . ?
C19 C18 C23 116.4(5) . . ?
C22 C18 C23 124.7(6) . . ?
C20 C19 C18 121.4(6) . . ?
C20 C19 H19 119.3 . . ?
C18 C19 H19 119.3 . . ?
C21 C20 C19 119.0(7) . . ?
C21 C20 H20 120.5 . . ?
C19 C20 H20 120.5 . . ?
N4 C21 C20 121.1(6) . . ?
N4 C21 H21 119.5 . . ?
C20 C21 H21 119.5 . . ?
N4 C22 C18 116.1(6) . . ?
N4 C22 S2 115.5(5) . . ?
C18 C22 S2 128.3(5) . . ?
O8 C23 N5 120.4(6) . . ?
O8 C23 C18 120.6(6) . . ?
N5 C23 C18 119.0(5) . . ?
N6 C24 C25 124.3(6) . . ?
N6 C24 H24 117.8 . . ?
C25 C24 H24 117.8 . . ?
C26 C25 C24 117.1(6) . . ?
C26 C25 C30 119.9(6) . . ?
C24 C25 C30 123.0(6) . . ?
C27 C26 C25 121.4(7) . . ?
C27 C26 H26 119.3 . . ?
C25 C26 H26 119.3 . . ?
C28 C27 C26 119.0(7) . . ?
C28 C27 H27 120.5 . . ?
C26 C27 H27 120.5 . . ?
C29 C28 C27 121.4(7) . . ?
C29 C28 H28 119.3 . . ?
C27 C28 H28 119.3 . . ?
C28 C29 C30 121.5(7) . . ?
C28 C29 H29 119.2 . . ?
C30 C29 H29 119.2 . . ?
O9 C30 C29 120.3(6) . . ?
O9 C30 C25 123.0(5) . . ?
C29 C30 C25 116.8(6) . . ?
O12 C31 O14 119.6(6) 2_677 . ?
O12 C31 C33 119.8(6) 2_677 . ?
O14 C31 C33 120.6(6) . . ?
O12 C31 Yb2 54.5(3) 2_677 2_677 ?
O14 C31 Yb2 67.2(3) . 2_677 ?
C33 C31 Yb2 161.7(4) . 2_677 ?
O13 C32 H32A 109.5 . . ?
O13 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
O13 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O10 C39 O11 120.7(7) . . ?
O10 C39 C41 119.9(8) . . ?
O11 C39 C41 119.4(8) . . ?
O10 C39 Yb2 59.2(4) . . ?
O11 C39 Yb2 61.8(4) . . ?
C41 C39 Yb2 173.6(6) . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.012
_refine_diff_density_min         -0.977
_refine_diff_density_rms         0.113

