Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2003

data_global
_journal_name_full               'Dalton Trans.'

_refine_special_details          # For THNPOK
; 
3.5 molecules of Et2O included in asymmetric unit. 3 coordinated to K, one
ordered, 2 show disorder. O3 modelled with C33 anc C34 common to both
components and C31, C32 and O3 over 2 sites with occupancies 0.6:0.4. Minor 
component refined with common Uiso. O4 modelled with 3 components O4' and
C atoms with occupancy 0.4. C41 and C42 common to 2 remaining components
(occupancy 0.6) and remaining atoms split over 2 sites with occupancies 
0.45:0.15,
all modelled with common Uiso. O6, 0.5 Et2O non-coordated, O6 and C63 modelled
over 2 sites with cocupancies 0.3:0.2, again with common Uiso. Hydrogens omitted
from disordered Et2O.
OH not located, assumed to be O1 as longer (>10 sigma difference) K-O1 than
K-O(2).
;

_journal_coden_Cambridge         0222

loop_
_publ_author_name
'Polly Arnold'
'Alexander J. Blake'
'Jonathan J. Hall'
'Louise S. Natrajan'
'Claire Wilson'

_publ_contact_author_name        'Dr P.L. Arnold'
_publ_contact_author_address     
;
School of Chemistry
The University of Nottingham
University Park
Nottingham  NG7 2RD
England UK
;

_publ_contact_author_email       Polly.Arnold@nottingham.ac.uk
_publ_contact_author_fax         '0115 951 3563'
_publ_contact_author_phone       '0115 951 3437'
_publ_section_title              
;
Synthesis of mono- and di-potassium salts and methoxy adducts of
sulfur-bridged biphenols by selective deprotonation
;
#=============================================================== 
data_Compound_3
_database_code_CSD               202297
# Code METHOK

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
[1,1-S(2-KO)(2-HO)(C6H2But-3-Me-5)2(ether)] 
;
_chemical_name_common            KHLs.Et2O
_chemical_melting_point          '231-235 C'
_chemical_formula_moiety         'C52 H78 K2 O6 S2'
_chemical_formula_sum            'C52 H78 K2 O6 S2'
_chemical_formula_weight         941.46

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'
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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   12.065(2)
_cell_length_b                   17.968(3)
_cell_length_c                   12.609(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.857(4)
_cell_angle_gamma                90.00
_cell_volume                     2693.0(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4343
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      27.2

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1016
_exptl_absorpt_coefficient_mu    0.297
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       omega
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            16742
_diffrn_reflns_av_R_equivalents  0.049
_diffrn_reflns_av_sigmaI/netI    0.052
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.99
_diffrn_reflns_theta_max         28.31
_reflns_number_total             6310
_reflns_number_gt                4477
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART version 5.624 (Bruker,2001)'
_computing_cell_refinement       'Bruker SAINT version 6.02a (Bruker,2000)'
_computing_data_reduction        'Bruker SAINT Bruker SHELXTL (Bruker,1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  'SHELXL-97 PLATON (Spek, 2001)'

_refine_special_details          
; 
?
;

_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^)+(0.045P)^2] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   'geometrically placed'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6100
_refine_ls_number_parameters     282
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0405
_refine_ls_wR_factor_ref         0.0952
_refine_ls_wR_factor_gt          0.0900
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_restrained_S_all      0.954
_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
K1 K 0.49353(3) 0.08227(2) 0.10211(3) 0.03130(11) Uani 1 1 d . . .
S1 S 0.26063(4) 0.13606(2) -0.05858(3) 0.02451(11) Uani 1 1 d . . .
O1 O 0.64991(9) 0.01863(6) 0.00466(9) 0.0245(3) Uani 1 1 d . . .
C11 C 0.79360(14) -0.06752(9) -0.02175(13) 0.0232(4) Uani 1 1 d . . .
C12 C 0.73994(14) 0.00247(9) -0.04034(13) 0.0220(4) Uani 1 1 d . . .
C13 C 0.78429(14) 0.05410(9) -0.10818(13) 0.0238(4) Uani 1 1 d . . .
C131 C 0.73623(15) 0.13343(9) -0.12393(14) 0.0281(4) Uani 1 1 d . . .
C132 C 0.79835(18) 0.18069(10) -0.19720(16) 0.0424(5) Uani 1 1 d . . .
H13A H 0.8785 0.1832 -0.1662 0.064 Uiso 1 1 calc R . .
H13B H 0.7668 0.2311 -0.2033 0.064 Uiso 1 1 calc R . .
H13C H 0.7893 0.1579 -0.2688 0.064 Uiso 1 1 calc R . .
C133 C 0.75061(16) 0.17303(9) -0.01476(15) 0.0345(4) Uani 1 1 d . . .
H13D H 0.8305 0.1740 0.0175 0.052 Uiso 1 1 calc R . .
H13E H 0.7082 0.1463 0.0330 0.052 Uiso 1 1 calc R . .
H13F H 0.7223 0.2241 -0.0250 0.052 Uiso 1 1 calc R . .
C134 C 0.61098(16) 0.13123(10) -0.17708(15) 0.0364(5) Uani 1 1 d . . .
H13G H 0.5685 0.1019 -0.1322 0.055 Uiso 1 1 calc R . .
H13H H 0.6040 0.1084 -0.2485 0.055 Uiso 1 1 calc R . .
H13I H 0.5811 0.1820 -0.1842 0.055 Uiso 1 1 calc R . .
C14 C 0.87456(15) 0.03119(9) -0.15607(13) 0.0268(4) Uani 1 1 d . . .
H14A H 0.9036 0.0653 -0.2020 0.032 Uiso 1 1 calc R . .
C15 C 0.92483(14) -0.03897(9) -0.14056(14) 0.0273(4) Uani 1 1 d . . .
C151 C 1.02159(16) -0.06019(11) -0.19710(16) 0.0388(5) Uani 1 1 d . . .
H15A H 1.0929 -0.0543 -0.1473 0.058 Uiso 1 1 calc R . .
H15B H 1.0214 -0.0278 -0.2597 0.058 Uiso 1 1 calc R . .
H15C H 1.0130 -0.1121 -0.2208 0.058 Uiso 1 1 calc R . .
C16 C 0.88496(14) -0.08692(9) -0.07110(13) 0.0265(4) Uani 1 1 d . . .
H16A H 0.9200 -0.1340 -0.0563 0.032 Uiso 1 1 calc R . .
O2 O 0.66076(10) -0.01216(6) 0.19550(9) 0.0275(3) Uani 1 1 d . . .
H2A H 0.6692 -0.0068 0.1312 0.041 Uiso 1 1 calc R . .
C31 C 0.20664(13) 0.11180(9) -0.19542(13) 0.0218(4) Uani 1 1 d . . .
C32 C 0.25440(13) 0.05459(9) -0.24842(13) 0.0229(4) Uani 1 1 d . . .
C33 C 0.21404(14) 0.04154(9) -0.35910(14) 0.0247(4) Uani 1 1 d . . .
C331 C 0.26298(15) -0.02127(9) -0.41945(14) 0.0292(4) Uani 1 1 d . . .
C332 C 0.38861(16) -0.00572(11) -0.42038(16) 0.0388(5) Uani 1 1 d . . .
H33A H 0.3965 0.0425 -0.4547 0.058 Uiso 1 1 calc R . .
H33B H 0.4194 -0.0450 -0.4608 0.058 Uiso 1 1 calc R . .
H33C H 0.4297 -0.0047 -0.3463 0.058 Uiso 1 1 calc R . .
C333 C 0.24895(17) -0.09727(9) -0.36590(15) 0.0362(5) Uani 1 1 d . . .
H33D H 0.2860 -0.0957 -0.2904 0.054 Uiso 1 1 calc R . .
H33E H 0.2833 -0.1364 -0.4038 0.054 Uiso 1 1 calc R . .
H33F H 0.1687 -0.1079 -0.3695 0.054 Uiso 1 1 calc R . .
C334 C 0.20365(18) -0.02723(11) -0.53777(15) 0.0412(5) Uani 1 1 d . . .
H33G H 0.2105 0.0202 -0.5745 0.062 Uiso 1 1 calc R . .
H33H H 0.1239 -0.0389 -0.5400 0.062 Uiso 1 1 calc R . .
H33I H 0.2389 -0.0668 -0.5739 0.062 Uiso 1 1 calc R . .
C34 C 0.12965(15) 0.08872(9) -0.41148(14) 0.0285(4) Uani 1 1 d . . .
H34A H 0.1027 0.0808 -0.4859 0.034 Uiso 1 1 calc R . .
C35 C 0.08296(14) 0.14681(9) -0.36008(14) 0.0282(4) Uani 1 1 d . . .
C351 C -0.00557(16) 0.19804(10) -0.42198(16) 0.0414(5) Uani 1 1 d . . .
H35A H -0.0195 0.2396 -0.3757 0.062 Uiso 1 1 calc R . .
H35B H -0.0755 0.1702 -0.4444 0.062 Uiso 1 1 calc R . .
H35C H 0.0213 0.2173 -0.4857 0.062 Uiso 1 1 calc R . .
C36 C 0.12155(14) 0.15656(9) -0.25161(14) 0.0260(4) Uani 1 1 d . . .
H36A H 0.0895 0.1946 -0.2141 0.031 Uiso 1 1 calc R . .
C61 C 0.33538(19) 0.13065(11) 0.30113(16) 0.0474(5) Uani 1 1 d . . .
H61A H 0.2798 0.1281 0.3493 0.071 Uiso 1 1 calc R . .
H61B H 0.4110 0.1240 0.3430 0.071 Uiso 1 1 calc R . .
H61C H 0.3202 0.0912 0.2469 0.071 Uiso 1 1 calc R . .
C62 C 0.32800(17) 0.20514(11) 0.24628(16) 0.0407(5) Uani 1 1 d . . .
H62A H 0.2514 0.2125 0.2047 0.049 Uiso 1 1 calc R . .
H62B H 0.3432 0.2452 0.3007 0.049 Uiso 1 1 calc R . .
O6 O 0.40907(10) 0.20802(6) 0.17557(10) 0.0327(3) Uani 1 1 d . . .
C63 C 0.40314(17) 0.27708(10) 0.11860(16) 0.0378(5) Uani 1 1 d . . .
H63A H 0.4099 0.3192 0.1699 0.045 Uiso 1 1 calc R . .
H63B H 0.3301 0.2813 0.0693 0.045 Uiso 1 1 calc R . .
C64 C 0.49853(18) 0.27888(11) 0.05541(17) 0.0456(5) Uani 1 1 d . . .
H64A H 0.4962 0.3258 0.0154 0.068 Uiso 1 1 calc R . .
H64B H 0.4910 0.2371 0.0048 0.068 Uiso 1 1 calc R . .
H64C H 0.5703 0.2750 0.1049 0.068 Uiso 1 1 calc R . .

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
K1 0.0251(2) 0.0279(2) 0.0397(2) -0.00931(18) 0.00207(17) 0.00621(17)
S1 0.0264(2) 0.0194(2) 0.0278(2) -0.00050(18) 0.00488(18) -0.00068(17)
O1 0.0230(6) 0.0236(6) 0.0280(7) 0.0010(5) 0.0074(5) 0.0033(5)
C11 0.0249(9) 0.0211(8) 0.0233(9) -0.0010(7) 0.0034(7) -0.0009(7)
C12 0.0206(9) 0.0241(8) 0.0202(9) -0.0041(7) 0.0005(7) -0.0010(7)
C13 0.0235(9) 0.0218(8) 0.0250(9) -0.0015(7) 0.0009(7) -0.0026(7)
C131 0.0311(10) 0.0232(9) 0.0302(10) 0.0022(8) 0.0054(8) 0.0003(8)
C132 0.0545(14) 0.0265(10) 0.0499(13) 0.0078(9) 0.0193(11) 0.0002(9)
C133 0.0382(11) 0.0249(9) 0.0406(11) -0.0038(8) 0.0072(9) -0.0012(8)
C134 0.0388(12) 0.0315(10) 0.0367(11) 0.0049(9) 0.0004(9) 0.0057(9)
C14 0.0273(10) 0.0274(9) 0.0258(9) 0.0007(7) 0.0053(8) -0.0047(8)
C15 0.0212(9) 0.0319(10) 0.0290(10) -0.0034(8) 0.0049(8) -0.0007(8)
C151 0.0307(11) 0.0438(11) 0.0455(12) -0.0001(10) 0.0166(9) 0.0026(9)
C16 0.0230(9) 0.0256(9) 0.0299(10) -0.0032(8) 0.0019(8) 0.0033(7)
O2 0.0272(7) 0.0318(7) 0.0241(6) 0.0023(5) 0.0058(5) 0.0089(5)
C31 0.0196(9) 0.0210(8) 0.0253(9) 0.0012(7) 0.0051(7) -0.0034(7)
C32 0.0196(9) 0.0219(8) 0.0280(9) 0.0045(7) 0.0058(7) -0.0013(7)
C33 0.0238(9) 0.0218(8) 0.0294(10) 0.0026(7) 0.0070(7) -0.0060(7)
C331 0.0322(10) 0.0291(9) 0.0282(10) -0.0014(8) 0.0103(8) -0.0038(8)
C332 0.0358(11) 0.0404(11) 0.0443(12) -0.0045(9) 0.0186(10) 0.0004(9)
C333 0.0470(12) 0.0254(10) 0.0381(12) -0.0045(8) 0.0125(10) -0.0017(9)
C334 0.0536(14) 0.0420(11) 0.0298(11) -0.0067(9) 0.0116(10) -0.0070(10)
C34 0.0297(10) 0.0280(9) 0.0264(10) 0.0043(8) 0.0012(8) -0.0079(8)
C35 0.0233(9) 0.0229(9) 0.0366(11) 0.0061(8) 0.0002(8) -0.0026(7)
C351 0.0403(12) 0.0301(10) 0.0488(13) 0.0093(9) -0.0064(10) 0.0029(9)
C36 0.0237(9) 0.0185(8) 0.0362(10) 0.0019(7) 0.0065(8) -0.0010(7)
C61 0.0526(14) 0.0518(13) 0.0395(12) -0.0007(10) 0.0125(10) -0.0004(11)
C62 0.0398(12) 0.0407(11) 0.0427(12) -0.0111(10) 0.0103(10) 0.0091(9)
O6 0.0369(8) 0.0262(6) 0.0348(7) -0.0037(5) 0.0055(6) 0.0091(6)
C63 0.0397(12) 0.0248(9) 0.0446(12) -0.0038(9) -0.0055(10) 0.0044(8)
C64 0.0561(14) 0.0384(11) 0.0417(12) 0.0008(10) 0.0063(11) -0.0038(10)

_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
K1 O1 2.6778(11) . ?
K1 O1 2.7012(12) 3_655 ?
K1 O6 2.7064(12) . ?
K1 O2 2.7428(12) . ?
K1 C12 3.1793(17) 3_655 ?
K1 S1 3.3145(7) . ?
K1 C11 3.4490(18) 3_655 ?
K1 C61 3.512(2) . ?
K1 K1 3.9412(9) 3_655 ?
S1 C11 1.7882(16) 3_655 ?
S1 C31 1.7907(17) . ?
O1 C12 1.3406(19) . ?
O1 K1 2.7012(12) 3_655 ?
C11 C16 1.399(2) . ?
C11 C12 1.415(2) . ?
C11 S1 1.7882(16) 3_655 ?
C11 K1 3.4490(18) 3_655 ?
C12 C13 1.427(2) . ?
C12 K1 3.1793(17) 3_655 ?
C13 C14 1.395(2) . ?
C13 C131 1.539(2) . ?
C131 C133 1.533(2) . ?
C131 C132 1.540(2) . ?
C131 C134 1.545(2) . ?
C14 C15 1.398(2) . ?
C15 C16 1.373(2) . ?
C15 C151 1.517(2) . ?
O2 C32 1.3566(19) 3_655 ?
C31 C36 1.398(2) . ?
C31 C32 1.403(2) . ?
C32 O2 1.3566(19) 3_655 ?
C32 C33 1.417(2) . ?
C33 C34 1.400(2) . ?
C33 C331 1.535(2) . ?
C331 C332 1.543(2) . ?
C331 C334 1.544(3) . ?
C331 C333 1.546(2) . ?
C34 C35 1.397(2) . ?
C35 C36 1.378(2) . ?
C35 C351 1.520(2) . ?
C61 C62 1.502(3) . ?
C62 O6 1.433(2) . ?
O6 C63 1.429(2) . ?
C63 C64 1.508(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 K1 O1 85.78(4) . 3_655 ?
O1 K1 O6 148.17(4) . . ?
O1 K1 O6 118.97(4) 3_655 . ?
O1 K1 O2 53.74(3) . . ?
O1 K1 O2 99.22(4) 3_655 . ?
O6 K1 O2 131.44(4) . . ?
O1 K1 C12 110.33(4) . 3_655 ?
O1 K1 C12 24.68(3) 3_655 3_655 ?
O6 K1 C12 96.54(4) . 3_655 ?
O2 K1 C12 111.39(4) . 3_655 ?
O1 K1 S1 115.73(3) . . ?
O1 K1 S1 59.16(3) 3_655 . ?
O6 K1 S1 68.67(3) . . ?
O2 K1 S1 158.00(3) . . ?
C12 K1 S1 50.73(3) 3_655 . ?
O1 K1 C11 125.70(4) . 3_655 ?
O1 K1 C11 43.65(3) 3_655 3_655 ?
O6 K1 C11 75.32(4) . 3_655 ?
O2 K1 C11 134.96(4) . 3_655 ?
C12 K1 C11 24.22(4) 3_655 3_655 ?
S1 K1 C11 30.58(3) . 3_655 ?
O1 K1 C61 160.95(4) . . ?
O1 K1 C61 98.17(4) 3_655 . ?
O6 K1 C61 42.81(4) . . ?
O2 K1 C61 107.22(5) . . ?
C12 K1 C61 74.14(5) 3_655 . ?
S1 K1 C61 81.79(4) . . ?
C11 K1 C61 65.65(5) 3_655 . ?
O1 K1 K1 43.12(3) . 3_655 ?
O1 K1 K1 42.66(2) 3_655 3_655 ?
O6 K1 K1 155.40(3) . 3_655 ?
O2 K1 K1 73.02(3) . 3_655 ?
C12 K1 K1 67.25(3) 3_655 3_655 ?
S1 K1 K1 86.769(18) . 3_655 ?
C11 K1 K1 84.30(3) 3_655 3_655 ?
C61 K1 K1 137.71(4) . 3_655 ?
C11 S1 C31 105.67(7) 3_655 . ?
C11 S1 K1 78.87(6) 3_655 . ?
C31 S1 K1 130.43(6) . . ?
C12 O1 K1 166.49(10) . . ?
C12 O1 K1 98.05(9) . 3_655 ?
K1 O1 K1 94.22(4) . 3_655 ?
C16 C11 C12 121.36(15) . . ?
C16 C11 S1 118.21(12) . 3_655 ?
C12 C11 S1 120.29(12) . 3_655 ?
C16 C11 K1 132.70(11) . 3_655 ?
C12 C11 K1 67.15(9) . 3_655 ?
S1 C11 K1 70.55(5) 3_655 3_655 ?
O1 C12 C11 120.21(14) . . ?
O1 C12 C13 121.81(14) . . ?
C11 C12 C13 117.98(15) . . ?
O1 C12 K1 57.27(8) . 3_655 ?
C11 C12 K1 88.63(10) . 3_655 ?
C13 C12 K1 124.89(11) . 3_655 ?
C14 C13 C12 117.93(15) . . ?
C14 C13 C131 121.49(15) . . ?
C12 C13 C131 120.54(14) . . ?
C133 C131 C13 109.38(14) . . ?
C133 C131 C132 106.90(14) . . ?
C13 C131 C132 112.14(14) . . ?
C133 C131 C134 110.69(15) . . ?
C13 C131 C134 110.56(14) . . ?
C132 C131 C134 107.11(15) . . ?
C13 C14 C15 123.90(16) . . ?
C16 C15 C14 117.65(15) . . ?
C16 C15 C151 121.59(16) . . ?
C14 C15 C151 120.75(16) . . ?
C15 C16 C11 121.06(16) . . ?
C32 O2 K1 175.18(10) 3_655 . ?
C36 C31 C32 120.41(16) . . ?
C36 C31 S1 117.57(12) . . ?
C32 C31 S1 121.75(13) . . ?
O2 C32 C31 120.96(15) 3_655 . ?
O2 C32 C33 119.65(14) 3_655 . ?
C31 C32 C33 119.39(15) . . ?
C34 C33 C32 117.65(15) . . ?
C34 C33 C331 121.44(16) . . ?
C32 C33 C331 120.90(15) . . ?
C33 C331 C332 109.42(14) . . ?
C33 C331 C334 112.09(15) . . ?
C332 C331 C334 107.38(14) . . ?
C33 C331 C333 110.66(14) . . ?
C332 C331 C333 110.15(16) . . ?
C334 C331 C333 107.07(14) . . ?
C35 C34 C33 123.48(17) . . ?
C36 C35 C34 117.44(16) . . ?
C36 C35 C351 121.38(16) . . ?
C34 C35 C351 121.18(17) . . ?
C35 C36 C31 121.59(16) . . ?
C62 C61 K1 83.58(10) . . ?
O6 C62 C61 109.01(15) . . ?
C63 O6 C62 111.30(13) . . ?
C63 O6 K1 122.83(10) . . ?
C62 O6 K1 121.33(10) . . ?
O6 C63 C64 107.88(15) . . ?

_diffrn_measured_fraction_theta_max 0.911
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.967
_refine_diff_density_max         0.37
_refine_diff_density_min         -0.19
_refine_diff_density_rms         0.05
#================================================================   

data_Compound_5
_database_code_CSD               202298

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C50 H80 K O5.50 S'
_chemical_formula_weight         840.30

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'
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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   12.9794(15)
_cell_length_b                   23.913(3)
_cell_length_c                   17.896(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.092(2)
_cell_angle_gamma                90.00
_cell_volume                     5216.5(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7714
_cell_measurement_theta_min      2.4
_cell_measurement_theta_max      28.1

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.070
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1836
_exptl_absorpt_coefficient_mu    0.183
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.716
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'Bruker SADABS v2.03 (2001)'

_exptl_special_details           
; 
? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART1000 CCD area detector'
_diffrn_measurement_method       omega
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            32548
_diffrn_reflns_av_R_equivalents  0.047
_diffrn_reflns_av_sigmaI/netI    0.052
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.70
_diffrn_reflns_theta_max         25.00
_reflns_number_total             9168
_reflns_number_gt                5471
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART version 5.624 (Bruker, 2001)'
_computing_cell_refinement       'Bruker SAINT version 6.02a (Bruker, 2000)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXL-97; PLATON (Spek, 2003)'

_refine_special_details          
; 
3.5 molecules of Et2O included in asymmetric unit. 3 coordinated to K, one
ordered, 2 show disorder. O3 modelled with C33 anc C34 common to both
components and C31, C32 and O3 over 2 sites with occupancies 0.6:0.4. Minor 
component refined with common Uiso. O4 modelled with 3 components O4' and
C atoms with occupancy 0.4. C41 and C42 common to 2 remaining components
(occupancy 0.6) and remaining atoms split over 2 sites with occupancies 
0.45:0.15,
all modelled with common Uiso. O6, 0.5 Et2O non-coordated, O6 and C63 modelled
over 2 sites with cocupancies 0.3:0.2, again with common Uiso. Hydrogens omitted
from disordered Et2O.
OH not located, assumed to be O1 as longer (>10 sigma difference) K-O1 than
K-O(2).
;

_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^)+(0.192P)^2^+10.83P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   
'geometrically placed, OH and disordered Et2O omitted'
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9168
_refine_ls_number_parameters     473
_refine_ls_number_restraints     52
_refine_ls_R_factor_all          0.181
_refine_ls_R_factor_gt           0.124
_refine_ls_wR_factor_ref         0.410
_refine_ls_wR_factor_gt          0.328
_refine_ls_goodness_of_fit_ref   1.20
_refine_ls_restrained_S_all      1.40
_refine_ls_shift/su_max          0.005
_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
S1 S 0.04665(14) 0.82763(8) 0.02769(12) 0.0531(6) Uani 1 1 d . A .
K1 K 0.24273(17) 0.84281(9) -0.05991(13) 0.0794(7) Uani 1 1 d . . .
O1 O 0.2823(4) 0.8570(2) 0.1016(3) 0.0606(14) Uani 1 1 d . A .
O2 O 0.2520(4) 0.7634(2) 0.0493(4) 0.0645(15) Uani 1 1 d . A .
C11 C 0.1102(5) 0.8632(3) 0.1199(4) 0.0460(16) Uani 1 1 d . . .
C12 C 0.2219(5) 0.8756(3) 0.1429(4) 0.0480(16) Uani 1 1 d . A .
C13 C 0.2730(5) 0.9092(3) 0.2126(4) 0.0448(15) Uani 1 1 d . . .
C14 C 0.2111(5) 0.9244(3) 0.2569(4) 0.0429(15) Uani 1 1 d . A .
H14A H 0.2453 0.9453 0.3041 0.052 Uiso 1 1 calc R . .
C15 C 0.0404(5) 0.9262(3) 0.2871(4) 0.0438(15) Uani 1 1 d . A .
H15A H 0.0776 0.9457 0.3351 0.053 Uiso 1 1 calc R . .
C16 C -0.0691(5) 0.9139(3) 0.2686(4) 0.0471(16) Uani 1 1 d . . .
C17 C -0.1207(5) 0.8856(3) 0.1963(5) 0.0517(17) Uani 1 1 d . A .
H17A H -0.1966 0.8772 0.1814 0.062 Uiso 1 1 calc R . .
C18 C -0.0661(5) 0.8698(3) 0.1469(4) 0.0487(16) Uani 1 1 d . . .
H18A H -0.1050 0.8511 0.0985 0.058 Uiso 1 1 calc R A .
C19 C 0.0463(5) 0.8805(3) 0.1659(4) 0.0414(14) Uani 1 1 d . A .
C20 C 0.0990(5) 0.9109(3) 0.2370(4) 0.0417(14) Uani 1 1 d . . .
C21 C 0.0681(5) 0.7549(3) 0.0466(4) 0.0511(17) Uani 1 1 d . . .
C22 C 0.1701(5) 0.7317(3) 0.0534(5) 0.0553(19) Uani 1 1 d . A .
C23 C 0.1862(5) 0.6723(3) 0.0602(4) 0.0530(18) Uani 1 1 d . . .
C24 C 0.1033(5) 0.6404(3) 0.0675(4) 0.0530(18) Uani 1 1 d . A .
H24A H 0.1153 0.6013 0.0760 0.064 Uiso 1 1 calc R . .
C25 C -0.0832(5) 0.6268(3) 0.0694(4) 0.0479(16) Uani 1 1 d . A .
H25A H -0.0675 0.5883 0.0803 0.058 Uiso 1 1 calc R . .
C26 C -0.1855(5) 0.6461(3) 0.0602(4) 0.0471(16) Uani 1 1 d . . .
C27 C -0.2057(5) 0.7034(3) 0.0443(5) 0.0538(18) Uani 1 1 d . A .
H27A H -0.2767 0.7177 0.0370 0.065 Uiso 1 1 calc R . .
C28 C -0.1263(5) 0.7393(3) 0.0389(5) 0.0546(19) Uani 1 1 d . . .
H28A H -0.1436 0.7777 0.0275 0.066 Uiso 1 1 calc R A .
C29 C -0.0186(5) 0.7201(3) 0.0501(4) 0.0500(17) Uani 1 1 d . A .
C30 C 0.0000(5) 0.6625(3) 0.0632(4) 0.0484(16) Uani 1 1 d . . .
C130 C 0.3962(5) 0.9237(3) 0.2388(4) 0.0524(17) Uani 1 1 d . A .
C131 C 0.4217(7) 0.9535(4) 0.1713(5) 0.069(2) Uani 1 1 d . . .
H13A H 0.5002 0.9622 0.1885 0.104 Uiso 1 1 calc R A .
H13B H 0.3792 0.9882 0.1577 0.104 Uiso 1 1 calc R . .
H13C H 0.4020 0.9291 0.1244 0.104 Uiso 1 1 calc R . .
C132 C 0.4635(6) 0.8705(4) 0.2620(5) 0.067(2) Uani 1 1 d . . .
H13D H 0.5417 0.8797 0.2783 0.100 Uiso 1 1 calc R A .
H13E H 0.4439 0.8450 0.2164 0.100 Uiso 1 1 calc R . .
H13F H 0.4483 0.8524 0.3063 0.100 Uiso 1 1 calc R . .
C133 C 0.4297(6) 0.9627(4) 0.3098(5) 0.065(2) Uani 1 1 d . . .
H13G H 0.5081 0.9712 0.3252 0.098 Uiso 1 1 calc R A .
H13H H 0.4152 0.9448 0.3545 0.098 Uiso 1 1 calc R . .
H13I H 0.3874 0.9975 0.2958 0.098 Uiso 1 1 calc R . .
C160 C -0.1342(6) 0.9268(3) 0.3228(5) 0.0564(18) Uani 1 1 d . . .
C161 C -0.1704(8) 0.8718(4) 0.3507(6) 0.080(3) Uani 1 1 d . . .
H16A H -0.2147 0.8501 0.3043 0.120 Uiso 1 1 calc R . .
H16B H -0.2141 0.8801 0.3844 0.120 Uiso 1 1 calc R . .
H16C H -0.1055 0.8501 0.3812 0.120 Uiso 1 1 calc R . .
C162 C -0.2357(6) 0.9614(4) 0.2768(6) 0.073(2) Uani 1 1 d . . .
H16D H -0.2799 0.9407 0.2293 0.110 Uiso 1 1 calc R . .
H16E H -0.2126 0.9971 0.2609 0.110 Uiso 1 1 calc R . .
H16F H -0.2795 0.9684 0.3109 0.110 Uiso 1 1 calc R . .
C163 C -0.0657(7) 0.9598(4) 0.3966(5) 0.067(2) Uani 1 1 d . . .
H16G H -0.0005 0.9381 0.4264 0.100 Uiso 1 1 calc R . .
H16H H -0.1098 0.9669 0.4304 0.100 Uiso 1 1 calc R . .
H16I H -0.0432 0.9955 0.3800 0.100 Uiso 1 1 calc R . .
C230 C 0.2926(6) 0.6461(4) 0.0583(5) 0.064(2) Uani 1 1 d . A .
C231 C 0.3914(6) 0.6685(5) 0.1273(7) 0.089(3) Uani 1 1 d . . .
H23A H 0.3948 0.7092 0.1233 0.134 Uiso 1 1 calc R A .
H23B H 0.4591 0.6520 0.1244 0.134 Uiso 1 1 calc R . .
H23C H 0.3834 0.6584 0.1780 0.134 Uiso 1 1 calc R . .
C232 C 0.2912(7) 0.5831(4) 0.0660(7) 0.083(3) Uani 1 1 d . . .
H23D H 0.2293 0.5677 0.0223 0.125 Uiso 1 1 calc R A .
H23E H 0.2835 0.5732 0.1169 0.125 Uiso 1 1 calc R . .
H23F H 0.3599 0.5676 0.0636 0.125 Uiso 1 1 calc R . .
C233 C 0.3067(7) 0.6596(4) -0.0216(7) 0.080(3) Uani 1 1 d . . .
H23G H 0.2440 0.6448 -0.0652 0.120 Uiso 1 1 calc R A .
H23H H 0.3745 0.6425 -0.0232 0.120 Uiso 1 1 calc R . .
H23I H 0.3106 0.7002 -0.0273 0.120 Uiso 1 1 calc R . .
C260 C -0.2776(5) 0.6088(3) 0.0672(4) 0.0519(17) Uani 1 1 d . . .
C261 C -0.3787(7) 0.6145(4) -0.0053(6) 0.080(3) Uani 1 1 d . . .
H26A H -0.4365 0.5902 0.0001 0.120 Uiso 1 1 calc R . .
H26B H -0.3617 0.6035 -0.0526 0.120 Uiso 1 1 calc R . .
H26C H -0.4037 0.6534 -0.0108 0.120 Uiso 1 1 calc R . .
C262 C -0.3058(7) 0.6270(4) 0.1398(6) 0.078(3) Uani 1 1 d . . .
H26D H -0.3644 0.6031 0.1449 0.116 Uiso 1 1 calc R . .
H26E H -0.3304 0.6660 0.1333 0.116 Uiso 1 1 calc R . .
H26F H -0.2406 0.6235 0.1877 0.116 Uiso 1 1 calc R . .
C263 C -0.2442(7) 0.5482(4) 0.0784(7) 0.078(3) Uani 1 1 d . . .
H26G H -0.3051 0.5258 0.0827 0.117 Uiso 1 1 calc R . .
H26H H -0.1804 0.5441 0.1272 0.117 Uiso 1 1 calc R . .
H26I H -0.2253 0.5354 0.0328 0.117 Uiso 1 1 calc R . .
O3 O 0.1730(10) 0.9522(6) -0.1048(8) 0.120(5) Uiso 0.60 1 d PD A 1
C31 C 0.3408(15) 1.0041(13) -0.0303(19) 0.177(12) Uiso 0.60 1 d PD A 1
C32 C 0.2151(14) 0.9964(9) -0.0516(12) 0.133(8) Uiso 0.60 1 d PD A 1
C33 C 0.0629(11) 0.9563(7) -0.1546(9) 0.172(7) Uiso 1 1 d D . .
C34 C 0.0319(14) 0.9200(8) -0.2296(8) 0.177(7) Uiso 1 1 d D A .
O3' O 0.130(2) 0.9283(11) -0.0868(9) 0.136(6) Uiso 0.40 1 d PD A 2
C31' C 0.073(3) 0.9858(15) 0.006(2) 0.136(6) Uiso 0.40 1 d PD . 2
C32' C 0.1663(19) 0.9679(17) -0.0249(9) 0.136(6) Uiso 0.40 1 d PD A 2
O4 O 0.446(5) 0.8419(11) -0.0704(18) 0.116(3) Uiso 0.15 1 d PD A 1
C41 C 0.3920(16) 0.9384(8) -0.1189(12) 0.116(3) Uiso 0.60 1 d PD A 1
C42 C 0.410(4) 0.8951(17) -0.053(2) 0.116(3) Uiso 0.15 1 d PD A 1
C43 C 0.542(3) 0.8261(12) -0.007(3) 0.116(3) Uiso 0.15 1 d PD A 1
C44 C 0.521(2) 0.7884(8) 0.0558(13) 0.116(3) Uiso 0.60 1 d PD A 1
O4" O 0.4675(14) 0.8704(8) -0.0090(11) 0.116(3) Uiso 0.45 1 d PD A 3
C42" C 0.4909(18) 0.9170(8) -0.0512(13) 0.116(3) Uiso 0.45 1 d PD A 3
C43" C 0.558(2) 0.8481(8) 0.0567(14) 0.116(3) Uiso 0.45 1 d PD A 3
O4' O 0.4584(19) 0.8585(9) -0.0497(11) 0.116(3) Uiso 0.40 1 d PD A 2
C41' C 0.400(2) 0.9092(13) -0.1787(14) 0.116(3) Uiso 0.40 1 d PD A 2
C42' C 0.489(2) 0.8759(13) -0.1159(15) 0.116(3) Uiso 0.40 1 d PD A 2
C43' C 0.5678(18) 0.8553(13) 0.0072(16) 0.116(3) Uiso 0.40 1 d PD A 2
C44' C 0.530(3) 0.8067(13) 0.0790(14) 0.116(3) Uiso 0.40 1 d PD A 2
O5 O 0.1378(5) 0.7706(3) -0.1742(4) 0.092(2) Uiso 1 1 d D A .
C52 C 0.0413(7) 0.7434(5) -0.1725(7) 0.106(4) Uiso 1 1 d D . .
H52A H 0.0372 0.7473 -0.1185 0.127 Uiso 1 1 calc R A .
H52B H 0.0468 0.7030 -0.1827 0.127 Uiso 1 1 calc R . .
C51 C -0.0634(7) 0.7661(6) -0.2323(8) 0.121(4) Uiso 1 1 d D A .
H51A H -0.1264 0.7458 -0.2273 0.181 Uiso 1 1 calc R . .
H51B H -0.0615 0.7610 -0.2862 0.181 Uiso 1 1 calc R . .
H51C H -0.0701 0.8059 -0.2223 0.181 Uiso 1 1 calc R . .
C53 C 0.1761(10) 0.7440(6) -0.2303(8) 0.133(5) Uiso 1 1 d D . .
H53A H 0.1277 0.7543 -0.2846 0.159 Uiso 1 1 calc R A .
H53B H 0.1715 0.7030 -0.2247 0.159 Uiso 1 1 calc R . .
C54 C 0.2930(9) 0.7596(7) -0.2206(9) 0.140(5) Uiso 1 1 d D A .
H54A H 0.3150 0.7402 -0.2610 0.210 Uiso 1 1 calc R . .
H54B H 0.3417 0.7485 -0.1675 0.210 Uiso 1 1 calc R . .
H54C H 0.2979 0.8001 -0.2269 0.210 Uiso 1 1 calc R . .
O6 O 0.699(3) 0.8367(10) -0.1030(16) 0.154(6) Uiso 0.30 1 d PD B 1
C63 C 0.769(3) 0.8655(14) -0.136(3) 0.154(6) Uiso 0.30 1 d PD B 1
O6' O 0.695(4) 0.8428(12) -0.180(2) 0.154(6) Uiso 0.20 1 d PD B 3
C63' C 0.746(6) 0.880(3) -0.116(4) 0.154(6) Uiso 0.20 1 d PD B 3
C61 C 0.634(3) 0.7463(10) -0.1751(19) 0.154(6) Uiso 0.50 1 d PD B .
C62 C 0.6175(19) 0.8077(11) -0.1618(18) 0.154(6) Uiso 0.50 1 d PD . .
C64 C 0.797(3) 0.9252(11) -0.1069(19) 0.154(6) Uiso 0.50 1 d PD . .

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
S1 0.0364(9) 0.0574(11) 0.0626(11) -0.0164(9) 0.0132(8) -0.0030(7)
K1 0.0757(13) 0.0789(14) 0.0850(14) -0.0225(10) 0.0297(11) -0.0177(10)
O1 0.035(2) 0.071(3) 0.078(4) -0.028(3) 0.023(2) -0.009(2)
O2 0.036(3) 0.070(3) 0.092(4) -0.026(3) 0.027(3) -0.009(2)
C11 0.036(3) 0.043(4) 0.055(4) -0.012(3) 0.011(3) -0.001(3)
C12 0.034(3) 0.051(4) 0.060(4) -0.009(3) 0.017(3) -0.005(3)
C13 0.033(3) 0.045(4) 0.055(4) -0.003(3) 0.012(3) -0.003(3)
C14 0.033(3) 0.043(3) 0.049(4) -0.001(3) 0.008(3) -0.001(3)
C15 0.040(3) 0.043(3) 0.047(4) 0.000(3) 0.013(3) -0.001(3)
C16 0.038(3) 0.053(4) 0.053(4) -0.001(3) 0.018(3) 0.000(3)
C17 0.032(3) 0.058(4) 0.066(5) -0.005(3) 0.017(3) -0.003(3)
C18 0.033(3) 0.052(4) 0.058(4) -0.007(3) 0.012(3) 0.000(3)
C19 0.034(3) 0.038(3) 0.050(4) -0.002(3) 0.011(3) -0.001(3)
C20 0.035(3) 0.039(3) 0.050(4) 0.001(3) 0.013(3) 0.001(3)
C21 0.032(3) 0.056(4) 0.063(4) -0.022(3) 0.014(3) -0.005(3)
C22 0.033(3) 0.066(5) 0.066(5) -0.029(4) 0.016(3) -0.002(3)
C23 0.033(3) 0.066(5) 0.060(4) -0.018(4) 0.015(3) 0.003(3)
C24 0.035(3) 0.058(4) 0.063(4) -0.008(3) 0.013(3) 0.006(3)
C25 0.039(3) 0.053(4) 0.051(4) -0.004(3) 0.013(3) 0.004(3)
C26 0.035(3) 0.058(4) 0.046(4) -0.009(3) 0.011(3) 0.001(3)
C27 0.030(3) 0.062(5) 0.067(5) -0.015(4) 0.013(3) 0.001(3)
C28 0.033(3) 0.050(4) 0.076(5) -0.019(4) 0.012(3) 0.001(3)
C29 0.031(3) 0.060(4) 0.056(4) -0.016(3) 0.010(3) 0.001(3)
C30 0.033(3) 0.060(4) 0.049(4) -0.009(3) 0.011(3) 0.006(3)
C130 0.034(3) 0.065(5) 0.057(4) -0.008(3) 0.014(3) -0.008(3)
C131 0.058(5) 0.077(6) 0.076(6) -0.007(4) 0.027(4) -0.025(4)
C132 0.042(4) 0.078(5) 0.076(5) -0.012(4) 0.016(4) 0.003(4)
C133 0.037(4) 0.079(5) 0.075(5) -0.019(4) 0.014(4) -0.010(4)
C160 0.045(4) 0.068(5) 0.061(5) -0.006(4) 0.025(3) -0.006(3)
C161 0.074(6) 0.099(7) 0.077(6) -0.001(5) 0.040(5) -0.024(5)
C162 0.048(4) 0.095(7) 0.079(6) -0.013(5) 0.027(4) 0.007(4)
C163 0.060(5) 0.084(6) 0.066(5) -0.010(4) 0.034(4) -0.008(4)
C230 0.035(4) 0.073(5) 0.087(6) -0.020(4) 0.025(4) 0.004(3)
C231 0.031(4) 0.118(8) 0.112(8) -0.025(6) 0.015(4) 0.008(4)
C232 0.048(4) 0.077(6) 0.133(9) -0.008(6) 0.041(5) 0.017(4)
C233 0.058(5) 0.082(6) 0.113(8) -0.023(5) 0.047(5) 0.007(4)
C260 0.038(3) 0.061(4) 0.057(4) -0.002(3) 0.018(3) 0.002(3)
C261 0.050(5) 0.102(7) 0.081(6) 0.007(5) 0.014(4) -0.021(5)
C262 0.065(5) 0.098(7) 0.083(6) -0.008(5) 0.043(5) -0.002(5)
C263 0.064(5) 0.063(5) 0.120(8) 0.002(5) 0.050(5) 0.002(4)

_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
S1 C21 1.774(8) . ?
S1 C11 1.786(7) . ?
S1 K1 3.436(3) . ?
K1 O3' 2.46(2) . ?
K1 C42 2.47(6) . ?
K1 O5 2.666(7) . ?
K1 O2 2.697(7) . ?
K1 O4 2.71(6) . ?
K1 O4' 2.77(2) . ?
K1 O1 2.776(6) . ?
K1 O3 2.795(14) . ?
K1 O4" 2.819(17) . ?
K1 C32' 3.28(3) . ?
K1 C41 3.39(2) . ?
O1 C12 1.327(8) . ?
O2 C22 1.330(8) . ?
C11 C12 1.396(9) . ?
C11 C19 1.416(9) . ?
C12 C13 1.439(10) . ?
C13 C14 1.358(9) . ?
C13 C130 1.543(9) . ?
C14 C20 1.412(8) . ?
C15 C16 1.376(9) . ?
C15 C20 1.409(9) . ?
C16 C17 1.409(10) . ?
C16 C160 1.521(10) . ?
C17 C18 1.363(10) . ?
C18 C19 1.404(9) . ?
C19 C20 1.420(9) . ?
C21 C22 1.402(9) . ?
C21 C29 1.419(10) . ?
C22 C23 1.433(11) . ?
C23 C24 1.362(10) . ?
C23 C230 1.529(9) . ?
C24 C30 1.418(9) . ?
C25 C26 1.361(9) . ?
C25 C30 1.411(10) . ?
C26 C27 1.405(10) . ?
C26 C260 1.531(10) . ?
C27 C28 1.369(10) . ?
C28 C29 1.419(9) . ?
C29 C30 1.403(10) . ?
C130 C133 1.516(10) . ?
C130 C132 1.517(11) . ?
C130 C131 1.535(11) . ?
C160 C163 1.533(11) . ?
C160 C162 1.533(11) . ?
C160 C161 1.537(12) . ?
C230 C232 1.514(13) . ?
C230 C233 1.536(14) . ?
C230 C231 1.538(12) . ?
C260 C261 1.501(11) . ?
C260 C263 1.506(11) . ?
C260 C262 1.529(11) . ?
O3 C32 1.401(10) . ?
O3 C33 1.404(10) . ?
C31 C32 1.554(11) . ?
C33 O3' 1.40(2) . ?
C33 C34 1.531(10) . ?
O3' C32' 1.41(3) . ?
C31' C32' 1.560(11) . ?
O4 C43 1.424(12) . ?
O4 C42 1.427(12) . ?
C41 C42 1.532(12) . ?
C43 C44 1.532(12) . ?
O4" C42" 1.437(11) . ?
O4" C43" 1.450(11) . ?
O4' C42' 1.436(11) . ?
O4' C43' 1.437(12) . ?
C41' C42' 1.529(11) . ?
O5 C53 1.415(9) . ?
O5 C52 1.422(8) . ?
C52 C51 1.512(9) . ?
C53 C54 1.512(10) . ?
O6 C62 1.391(11) . ?
O6 C63 1.424(12) . ?
C63 C64 1.519(12) . ?
O6' C63' 1.410(12) . ?
O6' C62 1.435(12) . ?
C63' C64 1.26(4) . ?
C61 C62 1.516(11) . ?

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
C21 S1 C11 107.3(3) . . ?
C21 S1 K1 95.6(2) . . ?
C11 S1 K1 101.1(2) . . ?
O3' K1 C42 92.4(9) . . ?
O3' K1 O5 106.0(5) . . ?
C42 K1 O5 125.2(9) . . ?
O3' K1 O2 127.0(6) . . ?
C42 K1 O2 119.9(6) . . ?
O5 K1 O2 89.1(2) . . ?
O3' K1 O4 121.3(8) . . ?
C42 K1 O4 31.6(7) . . ?
O5 K1 O4 101.2(7) . . ?
O2 K1 O4 104.0(4) . . ?
O3' K1 O4' 114.7(8) . . ?
C42 K1 O4' 22.6(7) . . ?
O5 K1 O4' 112.2(5) . . ?
O2 K1 O4' 104.8(4) . . ?
O4 K1 O4' 11.0(9) . . ?
O3' K1 O1 89.3(4) . . ?
C42 K1 O1 92.2(9) . . ?
O5 K1 O1 137.8(2) . . ?
O2 K1 O1 52.08(16) . . ?
O4 K1 O1 103.7(7) . . ?
O4' K1 O1 95.3(4) . . ?
O3' K1 O3 19.0(6) . . ?
C42 K1 O3 74.6(6) . . ?
O5 K1 O3 110.9(3) . . ?
O2 K1 O3 142.8(3) . . ?
O4 K1 O3 102.4(5) . . ?
O4' K1 O3 96.5(5) . . ?
O1 K1 O3 96.3(3) . . ?
O3' K1 O4" 110.3(8) . . ?
C42 K1 O4" 21.8(5) . . ?
O5 K1 O4" 126.8(4) . . ?
O2 K1 O4" 98.4(4) . . ?
O4 K1 O4" 25.8(8) . . ?
O4' K1 O4" 15.4(5) . . ?
O1 K1 O4" 80.5(4) . . ?
O3 K1 O4" 94.1(5) . . ?
O3' K1 C32' 23.3(5) . . ?
C42 K1 C32' 81.2(9) . . ?
O5 K1 C32' 129.0(4) . . ?
O2 K1 C32' 116.4(5) . . ?
O4 K1 C32' 112.7(8) . . ?
O4' K1 C32' 103.2(7) . . ?
O1 K1 C32' 69.5(4) . . ?
O3 K1 C32' 27.3(4) . . ?
O4" K1 C32' 94.2(6) . . ?
O3' K1 C41 75.1(8) . . ?
C42 K1 C41 24.4(6) . . ?
O5 K1 C41 113.2(4) . . ?
O2 K1 C41 144.3(3) . . ?
O4 K1 C41 46.3(4) . . ?
O4' K1 C41 41.9(5) . . ?
O1 K1 C41 108.7(4) . . ?
O3 K1 C41 56.1(4) . . ?
O4" K1 C41 45.9(4) . . ?
C32' K1 C41 71.8(7) . . ?
O3' K1 S1 72.2(7) . . ?
C42 K1 S1 143.6(9) . . ?
O5 K1 S1 91.07(15) . . ?
O2 K1 S1 56.69(11) . . ?
O4 K1 S1 157.3(6) . . ?
O4' K1 S1 151.0(4) . . ?
O1 K1 S1 55.89(11) . . ?
O3 K1 S1 90.7(3) . . ?
O4" K1 S1 136.4(4) . . ?
C32' K1 S1 71.9(6) . . ?
C41 K1 S1 143.6(4) . . ?
C12 O1 K1 133.5(4) . . ?
C22 O2 K1 127.2(5) . . ?
C12 C11 C19 121.4(6) . . ?
C12 C11 S1 118.5(5) . . ?
C19 C11 S1 120.0(5) . . ?
O1 C12 C11 121.1(6) . . ?
O1 C12 C13 119.1(6) . . ?
C11 C12 C13 119.9(6) . . ?
C14 C13 C12 117.8(6) . . ?
C14 C13 C130 121.4(6) . . ?
C12 C13 C130 120.6(6) . . ?
C13 C14 C20 123.8(6) . . ?
C16 C15 C20 122.0(6) . . ?
C15 C16 C17 116.7(6) . . ?
C15 C16 C160 123.8(6) . . ?
C17 C16 C160 119.4(6) . . ?
C18 C17 C16 122.7(6) . . ?
C17 C18 C19 121.4(6) . . ?
C18 C19 C11 124.9(6) . . ?
C18 C19 C20 116.8(6) . . ?
C11 C19 C20 118.2(5) . . ?
C15 C20 C14 120.9(6) . . ?
C15 C20 C19 120.3(6) . . ?
C14 C20 C19 118.8(6) . . ?
C22 C21 C29 120.1(7) . . ?
C22 C21 S1 119.2(6) . . ?
C29 C21 S1 120.6(5) . . ?
O2 C22 C21 121.2(7) . . ?
O2 C22 C23 118.3(6) . . ?
C21 C22 C23 120.4(6) . . ?
C24 C23 C22 117.8(6) . . ?
C24 C23 C230 121.4(7) . . ?
C22 C23 C230 120.7(7) . . ?
C23 C24 C30 123.2(7) . . ?
C26 C25 C30 121.8(7) . . ?
C25 C26 C27 117.5(6) . . ?
C25 C26 C260 123.3(6) . . ?
C27 C26 C260 119.3(6) . . ?
C28 C27 C26 122.2(6) . . ?
C27 C28 C29 121.0(7) . . ?
C30 C29 C28 116.5(6) . . ?
C30 C29 C21 119.3(6) . . ?
C28 C29 C21 124.1(7) . . ?
C29 C30 C25 120.9(6) . . ?
C29 C30 C24 118.7(6) . . ?
C25 C30 C24 120.3(7) . . ?
C133 C130 C132 108.4(6) . . ?
C133 C130 C131 107.3(6) . . ?
C132 C130 C131 110.2(6) . . ?
C133 C130 C13 111.2(6) . . ?
C132 C130 C13 109.5(6) . . ?
C131 C130 C13 110.3(6) . . ?
C16 C160 C163 111.7(6) . . ?
C16 C160 C162 109.3(7) . . ?
C163 C160 C162 108.8(7) . . ?
C16 C160 C161 109.4(7) . . ?
C163 C160 C161 108.2(7) . . ?
C162 C160 C161 109.5(7) . . ?
C232 C230 C23 111.5(6) . . ?
C232 C230 C233 107.6(7) . . ?
C23 C230 C233 109.4(7) . . ?
C232 C230 C231 107.8(8) . . ?
C23 C230 C231 110.5(6) . . ?
C233 C230 C231 109.9(7) . . ?
C261 C260 C263 109.2(7) . . ?
C261 C260 C262 108.4(7) . . ?
C263 C260 C262 107.6(7) . . ?
C261 C260 C26 110.6(6) . . ?
C263 C260 C26 112.0(6) . . ?
C262 C260 C26 109.0(6) . . ?
C32 O3 C33 117.0(11) . . ?
C32 O3 K1 119.9(11) . . ?
C33 O3 K1 113.9(10) . . ?
O3 C32 C31 112.8(11) . . ?
O3' C33 C34 112.8(14) . . ?
O3 C33 C34 114.9(11) . . ?
C33 O3' C32' 107(2) . . ?
C33 O3' K1 136.0(11) . . ?
C32' O3' K1 112.9(15) . . ?
O3' C32' C31' 112.0(18) . . ?
C31' C32' K1 130(2) . . ?
C43 O4 C42 108.7(12) . . ?
C43 O4 K1 124(2) . . ?
C42 O4 K1 65(3) . . ?
O4 C42 C41 113.9(13) . . ?
O4 C42 K1 83(3) . . ?
C41 C42 K1 114(3) . . ?
O4 C43 C44 114.5(13) . . ?
C42" O4" C43" 116.9(11) . . ?
C42" O4" K1 113.2(12) . . ?
C43" O4" K1 129.7(12) . . ?
C42' O4' C43' 97(2) . . ?
C42' O4' K1 123.1(13) . . ?
C43' O4' K1 140.4(14) . . ?
O4' C42' C41' 113.8(12) . . ?
O4' C43' C44' 95.2(8) . . ?
C53 O5 C52 109.7(7) . . ?
C53 O5 K1 128.6(6) . . ?
C52 O5 K1 120.1(6) . . ?
O5 C52 C51 113.9(8) . . ?
O5 C53 C54 113.0(9) . . ?
C62 O6 C63 111.0(12) . . ?
O6 C63 C64 115.3(13) . . ?
C63' O6' C62 110.6(13) . . ?
C64 C63' O6' 137(4) . . ?
O6 C62 O6' 58.0(19) . . ?
O6 C62 C61 119.3(14) . . ?
O6' C62 C61 112.4(12) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.31
_refine_diff_density_min         -0.80
_refine_diff_density_rms         0.11

#===END of CIF