Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2008

data_global

_journal_coden_Cambridge         222

loop_
_publ_author_name
'Leonard Lindoy'

_publ_contact_author_name        'Leonard Lindoy'
_publ_contact_author_address     
;
School of Chemistry F11
University of Sydney
Sydney
NSW
2006.
AUSTRALIA
;

_publ_contact_author_email       LINDOY@GMAIL.COM

_publ_requested_journal          'Dalton Transactions'

_publ_section_title              
;
Assembly of a trinuclear metallo-capsule from a
tripodal tris(?-diketone) derivative and copper(II)
;

data_ld01sad
_database_code_depnum_ccdc_archive 'CCDC 667849'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H21 N3 O6 S3'
_chemical_formula_sum            'C18 H21 N3 O6 S3'
_chemical_formula_weight         471.56

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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Intl_tables_number     2

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

_cell_length_a                   7.0789(4)
_cell_length_b                   9.7470(7)
_cell_length_c                   16.2360(11)
_cell_angle_alpha                101.357(3)
_cell_angle_beta                 99.921(3)
_cell_angle_gamma                94.398(3)
_cell_volume                     1074.77(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6782
_cell_measurement_theta_min      2.68
_cell_measurement_theta_max      28.25

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             492
_exptl_absorpt_coefficient_mu    0.385
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.853
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'

_exptl_special_details           
;
The crystal was coated in Exxon Paratone N hydrocarbon
oil and mounted on a thin mohair fibre attached to a copper pin.
Upon mounting on the diffractometer,
the crystal was quenched to 150(K) under a cold nitrogen gas stream
supplied by an Oxford Cryosystems Cryostream and data were
collected at this temperature.
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  APEXII-FR591
_diffrn_measurement_method       \w+\f
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            20872
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_sigmaI/netI    0.0516
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.61
_diffrn_reflns_theta_max         28.34
_reflns_number_total             5224
_reflns_number_gt                3847
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX (Bruker-Nonius, 2003)'
_computing_cell_refinement       'SAINT (Bruker-Nonius, 2003)'
_computing_data_reduction        
'SAINT (Bruker-Nonius, 2003), XPREP (Bruker-Nonius, 2003)'
_computing_structure_solution    'SIR97 (Altomare, et. al. 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    
;ORTEP-3 (Farrugia, 1997)
WINGX-32 (Farrugia, 1999)
;
_computing_publication_material  'enCIFer 1.1 (CCDC, 2005)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0390P)^2^+0.5838P] where P=(Fo^2^+2Fc^2^)/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         5224
_refine_ls_number_parameters     292
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0382
_refine_ls_wR_factor_ref         0.0970
_refine_ls_wR_factor_gt          0.0864
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.018
_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 0.5107(3) -0.0402(2) 0.71021(15) 0.0322(5) Uani 1 1 d . A .
H1A H 0.5011 -0.1418 0.7077 0.048 Uiso 1 1 calc R . .
H1B H 0.5749 0.0104 0.7677 0.048 Uiso 1 1 calc R . .
H1C H 0.5858 -0.0176 0.6683 0.048 Uiso 1 1 calc R . .
C2 C 0.3134(3) 0.0031(2) 0.69032(13) 0.0230(4) Uani 1 1 d . . .
C3 C 0.2411(3) 0.11146(19) 0.74450(12) 0.0199(4) Uani 1 1 d . A .
C4 C 0.0539(3) 0.1474(2) 0.71865(13) 0.0249(4) Uani 1 1 d . . .
C5 C -0.0307(3) 0.2638(2) 0.77000(16) 0.0343(5) Uani 1 1 d . A .
H5A H 0.0246 0.3548 0.7625 0.052 Uiso 1 1 calc R . .
H5B H -0.0010 0.2599 0.8307 0.052 Uiso 1 1 calc R . .
H5C H -0.1710 0.2529 0.7505 0.052 Uiso 1 1 calc R . .
C6 C 0.5007(3) 0.34635(19) 0.82412(11) 0.0152(4) Uani 1 1 d . A .
C7 C 0.5238(4) 0.2309(3) 0.53293(15) 0.0370(6) Uani 1 1 d . C .
H7A H 0.5745 0.2046 0.5870 0.055 Uiso 1 1 calc R . .
H7B H 0.6143 0.3045 0.5231 0.055 Uiso 1 1 calc R . .
H7C H 0.5077 0.1482 0.4859 0.055 Uiso 1 1 calc R . .
C8 C 0.3339(3) 0.2846(2) 0.53709(13) 0.0273(5) Uani 1 1 d . . .
C9 C 0.3124(3) 0.4195(2) 0.58219(12) 0.0221(4) Uani 1 1 d . C .
C10 C 0.1255(3) 0.4566(2) 0.59076(13) 0.0273(5) Uani 1 1 d . . .
C11 C 0.0921(4) 0.5928(3) 0.64416(15) 0.0367(6) Uani 1 1 d . C .
H11A H -0.0470 0.5986 0.6386 0.055 Uiso 1 1 calc R . .
H11B H 0.1522 0.6714 0.6247 0.055 Uiso 1 1 calc R . .
H11C H 0.1492 0.5976 0.7042 0.055 Uiso 1 1 calc R . .
C12 C 0.5587(3) 0.48853(19) 0.73651(11) 0.0161(4) Uani 1 1 d . C .
C13 C 1.2571(3) 0.6389(2) 0.89474(14) 0.0288(5) Uani 1 1 d . F .
H13A H 1.3615 0.6403 0.8623 0.043 Uiso 1 1 calc R . .
H13B H 1.1712 0.5508 0.8726 0.043 Uiso 1 1 calc R . .
H13C H 1.3119 0.6459 0.9553 0.043 Uiso 1 1 calc R . .
C14 C 1.1456(3) 0.7603(2) 0.88564(12) 0.0205(4) Uani 1 1 d . . .
C15 C 0.9719(3) 0.7776(2) 0.91591(12) 0.0184(4) Uani 1 1 d . F .
C16 C 0.8776(3) 0.8983(2) 0.90776(12) 0.0206(4) Uani 1 1 d . . .
C17 C 0.6954(3) 0.9258(2) 0.93888(14) 0.0274(5) Uani 1 1 d . F .
H17A H 0.6802 1.0263 0.9456 0.041 Uiso 1 1 calc R . .
H17B H 0.7003 0.8988 0.9942 0.041 Uiso 1 1 calc R . .
H17C H 0.5857 0.8705 0.8974 0.041 Uiso 1 1 calc R . .
C18 C 0.7160(3) 0.53834(19) 0.87301(11) 0.0155(4) Uani 1 1 d . F .
N1 N 0.4578(2) 0.37318(16) 0.74547(10) 0.0170(3) Uani 1 1 d . . .
N2 N 0.6928(2) 0.57537(16) 0.79690(9) 0.0170(3) Uani 1 1 d . . .
N3 N 0.6258(2) 0.42461(16) 0.89093(9) 0.0171(3) Uani 1 1 d . . .
O1 O 0.2076(2) -0.06382(16) 0.61944(10) 0.0318(4) Uani 1 1 d D A 1
H1O H 0.097(2) -0.023(3) 0.6159(17) 0.048 Uiso 1 1 d D B 1
O2 O -0.0539(2) 0.08184(17) 0.64779(10) 0.0345(4) Uani 1 1 d . A .
O3 O 0.1835(2) 0.19736(17) 0.49859(11) 0.0391(4) Uani 1 1 d D C 1
H2O H 0.080(6) 0.242(6) 0.504(4) 0.059 Uiso 0.50 1 d PD D 1
O4 O -0.0240(2) 0.37083(18) 0.55311(11) 0.0379(4) Uani 1 1 d D C 2
H2OA H 0.007(9) 0.289(3) 0.527(4) 0.057 Uiso 0.50 1 d PD E 2
O5 O 1.2168(2) 0.85252(16) 0.84915(10) 0.0278(3) Uani 1 1 d D F 1
H3O H 1.133(6) 0.915(5) 0.847(4) 0.042 Uiso 0.50 1 d PD G 1
O6 O 0.9495(2) 0.99191(15) 0.87191(10) 0.0278(3) Uani 1 1 d D F 3
H3OA H 1.058(5) 0.962(6) 0.859(4) 0.042 Uiso 0.50 1 d PD H 3
S1 S 0.38157(8) 0.19529(5) 0.84484(3) 0.02114(12) Uani 1 1 d . . .
S2 S 0.51677(8) 0.53723(5) 0.63671(3) 0.02240(13) Uani 1 1 d . . .
S3 S 0.87249(7) 0.64713(5) 0.96201(3) 0.01935(12) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0316(13) 0.0320(12) 0.0314(12) 0.0015(10) 0.0063(10) 0.0065(10)
C2 0.0272(12) 0.0195(10) 0.0225(10) 0.0064(8) 0.0055(9) -0.0028(8)
C3 0.0249(11) 0.0141(9) 0.0201(9) 0.0045(7) 0.0043(8) -0.0037(8)
C4 0.0257(12) 0.0205(10) 0.0283(11) 0.0061(8) 0.0064(9) -0.0025(9)
C5 0.0308(13) 0.0288(12) 0.0419(13) 0.0033(10) 0.0063(10) 0.0069(10)
C6 0.0165(10) 0.0150(9) 0.0155(9) 0.0046(7) 0.0049(7) 0.0021(7)
C7 0.0418(15) 0.0361(13) 0.0302(12) -0.0003(10) 0.0068(11) 0.0065(11)
C8 0.0348(13) 0.0285(11) 0.0157(9) 0.0056(8) -0.0021(9) -0.0018(10)
C9 0.0241(11) 0.0255(11) 0.0150(9) 0.0076(8) -0.0016(8) -0.0029(9)
C10 0.0302(12) 0.0295(12) 0.0207(10) 0.0098(9) -0.0016(9) -0.0030(9)
C11 0.0376(14) 0.0376(14) 0.0353(13) 0.0073(10) 0.0071(11) 0.0079(11)
C12 0.0172(10) 0.0175(9) 0.0146(8) 0.0043(7) 0.0043(7) 0.0026(7)
C13 0.0280(12) 0.0300(12) 0.0307(11) 0.0072(9) 0.0101(9) 0.0069(9)
C14 0.0206(11) 0.0228(10) 0.0148(9) 0.0014(7) -0.0002(8) -0.0023(8)
C15 0.0194(10) 0.0196(10) 0.0144(9) 0.0029(7) 0.0019(7) -0.0034(8)
C16 0.0209(10) 0.0209(10) 0.0172(9) 0.0036(7) -0.0016(8) -0.0019(8)
C17 0.0230(12) 0.0302(12) 0.0291(11) 0.0071(9) 0.0039(9) 0.0044(9)
C18 0.0153(10) 0.0168(9) 0.0149(8) 0.0033(7) 0.0036(7) 0.0036(7)
N1 0.0194(9) 0.0165(8) 0.0147(7) 0.0044(6) 0.0020(6) -0.0004(6)
N2 0.0183(8) 0.0182(8) 0.0143(7) 0.0043(6) 0.0029(6) -0.0005(6)
N3 0.0202(9) 0.0177(8) 0.0140(7) 0.0052(6) 0.0029(6) 0.0013(6)
O1 0.0327(9) 0.0289(9) 0.0280(8) -0.0036(6) 0.0014(7) 0.0024(7)
O2 0.0292(9) 0.0341(9) 0.0334(9) 0.0003(7) -0.0031(7) 0.0003(7)
O3 0.0400(11) 0.0311(9) 0.0353(9) -0.0024(7) -0.0074(8) -0.0053(8)
O4 0.0259(9) 0.0380(10) 0.0449(10) 0.0088(8) -0.0028(7) -0.0046(7)
O5 0.0243(8) 0.0301(9) 0.0324(8) 0.0116(7) 0.0106(7) 0.0001(6)
O6 0.0262(9) 0.0242(8) 0.0363(8) 0.0139(7) 0.0069(7) 0.0012(6)
S1 0.0286(3) 0.0181(2) 0.0169(2) 0.00676(18) 0.0042(2) -0.0042(2)
S2 0.0270(3) 0.0248(3) 0.0144(2) 0.00892(19) -0.00023(19) -0.0062(2)
S3 0.0233(3) 0.0207(2) 0.0125(2) 0.00471(17) 0.00046(18) -0.00378(19)

_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 1.490(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 O1 1.282(2) . ?
C2 C3 1.423(3) . ?
C3 C4 1.412(3) . ?
C3 S1 1.762(2) . ?
C4 O2 1.283(3) . ?
C4 C5 1.498(3) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 N3 1.335(2) . ?
C6 N1 1.342(2) . ?
C6 S1 1.7591(18) . ?
C7 C8 1.487(3) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 O3 1.292(3) . ?
C8 C9 1.407(3) . ?
C9 C10 1.420(3) . ?
C9 S2 1.760(2) . ?
C10 O4 1.278(3) . ?
C10 C11 1.495(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 N1 1.331(2) . ?
C12 N2 1.345(2) . ?
C12 S2 1.7601(19) . ?
C13 C14 1.488(3) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 O5 1.287(2) . ?
C14 C15 1.410(3) . ?
C15 C16 1.413(3) . ?
C15 S3 1.7585(19) . ?
C16 O6 1.292(2) . ?
C16 C17 1.489(3) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 N2 1.341(2) . ?
C18 N3 1.343(2) . ?
C18 S3 1.7619(19) . ?
O1 H1O 0.902(10) . ?
O3 H2O 0.887(10) . ?
O4 H2OA 0.888(10) . ?
O5 H3O 0.886(10) . ?
O6 H3OA 0.883(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 120.2(2) . . ?
O1 C2 C1 115.86(18) . . ?
C3 C2 C1 123.93(19) . . ?
C4 C3 C2 119.57(18) . . ?
C4 C3 S1 120.44(15) . . ?
C2 C3 S1 119.94(16) . . ?
O2 C4 C3 121.04(19) . . ?
O2 C4 C5 115.8(2) . . ?
C3 C4 C5 123.12(19) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C6 N1 126.55(17) . . ?
N3 C6 S1 114.82(13) . . ?
N1 C6 S1 118.63(14) . . ?
C8 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C8 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O3 C8 C9 120.2(2) . . ?
O3 C8 C7 116.0(2) . . ?
C9 C8 C7 123.8(2) . . ?
C8 C9 C10 119.99(19) . . ?
C8 C9 S2 120.35(17) . . ?
C10 C9 S2 119.39(16) . . ?
O4 C10 C9 120.1(2) . . ?
O4 C10 C11 116.8(2) . . ?
C9 C10 C11 123.1(2) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N1 C12 N2 126.68(17) . . ?
N1 C12 S2 118.59(14) . . ?
N2 C12 S2 114.73(13) . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O5 C14 C15 120.33(19) . . ?
O5 C14 C13 116.61(18) . . ?
C15 C14 C13 123.06(19) . . ?
C14 C15 C16 119.87(18) . . ?
C14 C15 S3 119.56(15) . . ?
C16 C15 S3 120.56(15) . . ?
O6 C16 C15 120.05(18) . . ?
O6 C16 C17 116.54(18) . . ?
C15 C16 C17 123.41(18) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C18 N3 126.41(17) . . ?
N2 C18 S3 119.67(14) . . ?
N3 C18 S3 113.89(13) . . ?
C12 N1 C6 113.57(16) . . ?
C18 N2 C12 113.22(16) . . ?
C6 N3 C18 113.50(15) . . ?
C2 O1 H1O 105.0(18) . . ?
C8 O3 H2O 108(4) . . ?
C10 O4 H2OA 112(4) . . ?
C14 O5 H3O 106(4) . . ?
C16 O6 H3OA 105(4) . . ?
C6 S1 C3 103.65(9) . . ?
C9 S2 C12 101.41(9) . . ?
C15 S3 C18 101.99(9) . . ?

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
O1 C2 C3 C4 -1.7(3) . . . . ?
C1 C2 C3 C4 178.14(19) . . . . ?
O1 C2 C3 S1 175.99(15) . . . . ?
C1 C2 C3 S1 -4.2(3) . . . . ?
C2 C3 C4 O2 1.5(3) . . . . ?
S1 C3 C4 O2 -176.19(16) . . . . ?
C2 C3 C4 C5 -177.52(19) . . . . ?
S1 C3 C4 C5 4.8(3) . . . . ?
O3 C8 C9 C10 4.6(3) . . . . ?
C7 C8 C9 C10 -173.0(2) . . . . ?
O3 C8 C9 S2 178.59(16) . . . . ?
C7 C8 C9 S2 1.0(3) . . . . ?
C8 C9 C10 O4 -4.3(3) . . . . ?
S2 C9 C10 O4 -178.42(16) . . . . ?
C8 C9 C10 C11 174.3(2) . . . . ?
S2 C9 C10 C11 0.3(3) . . . . ?
O5 C14 C15 C16 -1.3(3) . . . . ?
C13 C14 C15 C16 177.69(18) . . . . ?
O5 C14 C15 S3 177.68(14) . . . . ?
C13 C14 C15 S3 -3.3(3) . . . . ?
C14 C15 C16 O6 0.7(3) . . . . ?
S3 C15 C16 O6 -178.33(14) . . . . ?
C14 C15 C16 C17 -179.22(18) . . . . ?
S3 C15 C16 C17 1.8(3) . . . . ?
N2 C12 N1 C6 0.0(3) . . . . ?
S2 C12 N1 C6 -179.72(13) . . . . ?
N3 C6 N1 C12 2.0(3) . . . . ?
S1 C6 N1 C12 -178.87(14) . . . . ?
N3 C18 N2 C12 2.7(3) . . . . ?
S3 C18 N2 C12 -175.26(13) . . . . ?
N1 C12 N2 C18 -2.1(3) . . . . ?
S2 C12 N2 C18 177.60(13) . . . . ?
N1 C6 N3 C18 -1.5(3) . . . . ?
S1 C6 N3 C18 179.34(13) . . . . ?
N2 C18 N3 C6 -1.1(3) . . . . ?
S3 C18 N3 C6 176.99(13) . . . . ?
N3 C6 S1 C3 -176.62(14) . . . . ?
N1 C6 S1 C3 4.16(17) . . . . ?
C4 C3 S1 C6 -87.46(17) . . . . ?
C2 C3 S1 C6 94.90(16) . . . . ?
C8 C9 S2 C12 -86.93(17) . . . . ?
C10 C9 S2 C12 87.12(17) . . . . ?
N1 C12 S2 C9 8.75(18) . . . . ?
N2 C12 S2 C9 -171.00(15) . . . . ?
C14 C15 S3 C18 -91.92(16) . . . . ?
C16 C15 S3 C18 87.06(17) . . . . ?
N2 C18 S3 C15 -4.34(17) . . . . ?
N3 C18 S3 C15 177.44(14) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1O O2 0.902(10) 1.615(14) 2.468(2) 156(3) .
O3 H2O O4 0.887(10) 1.65(3) 2.457(2) 151(6) .
O4 H2OA O3 0.888(10) 1.67(4) 2.457(2) 147(6) .
O6 H3OA O5 0.883(10) 1.62(3) 2.450(2) 156(6) .
O5 H3O O6 0.886(10) 1.62(3) 2.450(2) 155(6) .

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        28.34
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.066