Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Kwan Mook Kim' _publ_contact_author_address ; Department of Chemistry/Nano-Sciences Ewha Womans University Daehyun-Dong 11-1 Seodaemoon-Gu Seoul 120-750 SOUTH KOREA ; _publ_contact_author_email KKMOOK@EWHA.AC.KR _publ_section_title ; Tuning the intermolecular dative interactions by altering the ligand planarity and counter cations in vanadyl(IV) complexes ; loop_ _publ_author_name 'Kwan Mook Kim.' 'Moo-Jin Jun.' 'Dongwon Lee.' 'Wonwoo Nam.' ; Hyunjung Park ; 'Mi Sook Seo.' 'Rita Song.' data_v _database_code_depnum_ccdc_archive 'CCDC 262586' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H52 N2 O11 S4 V' _chemical_formula_weight 771.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 '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' 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' N N 0.0061 0.0033 '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_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.134(2) _cell_length_b 13.179(3) _cell_length_c 14.581(2) _cell_angle_alpha 85.200(16) _cell_angle_beta 88.630(15) _cell_angle_gamma 72.880(18) _cell_volume 1854.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 818 _exptl_absorpt_coefficient_mu 0.548 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8314 _exptl_absorpt_correction_T_max 0.9223 _exptl_absorpt_process_details 'Psi scan' _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 CAD4 _diffrn_measurement_method omega/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <3% _diffrn_reflns_number 3093 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 25.65 _reflns_number_total 2957 _reflns_number_gt 2641 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of 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^)+(0.1397P)^2^+5.8798P] 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 2957 _refine_ls_number_parameters 487 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.1020 _refine_ls_R_factor_gt 0.0920 _refine_ls_wR_factor_ref 0.2475 _refine_ls_wR_factor_gt 0.2370 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.138 _refine_ls_shift/su_max 0.003 _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 V V -0.15460(18) 0.33371(14) 0.20267(16) 0.0658(7) Uani 1 1 d . . . S1 S -0.2165(5) 0.7471(3) 0.3253(3) 0.1179(17) Uani 1 1 d . . . S2 S -0.4687(3) 0.7674(2) 0.2261(2) 0.0768(10) Uani 1 1 d . . . S3 S -0.0642(4) -0.0939(3) 0.0913(3) 0.0976(13) Uani 1 1 d . . . S4 S 0.1983(3) -0.0948(3) 0.1715(3) 0.0944(13) Uani 1 1 d . . . O1 O -0.0986(8) 0.4119(6) 0.2942(6) 0.086(3) Uani 1 1 d . . . O2 O -0.3419(7) 0.4236(6) 0.2249(6) 0.072(2) Uani 1 1 d . . . O3 O -0.0991(15) 0.5423(8) 0.3777(10) 0.170(6) Uani 1 1 d . . . O4 O -0.4989(9) 0.5767(7) 0.2186(9) 0.125(4) Uani 1 1 d . . . O5 O 0.0028(7) 0.2199(6) 0.2538(7) 0.085(3) Uani 1 1 d . . . O6 O -0.2398(7) 0.2218(6) 0.1893(7) 0.095(3) Uani 1 1 d . . . O7 O 0.1544(10) 0.0632(7) 0.2763(8) 0.116(4) Uani 1 1 d . . . O8 O -0.2578(9) 0.0732(7) 0.1374(9) 0.116(4) Uani 1 1 d . . . O9 O -0.1141(9) 0.3723(7) 0.1049(7) 0.091(3) Uani 1 1 d . . . C1 C -0.1561(15) 0.5070(11) 0.3207(11) 0.091(4) Uani 1 1 d . . . C2 C -0.3819(12) 0.5230(9) 0.2378(9) 0.068(3) Uani 1 1 d . . . C3 C -0.2890(11) 0.5740(8) 0.2785(8) 0.060(3) Uani 1 1 d . . . C4 C -0.3198(12) 0.6815(8) 0.2771(8) 0.062(3) Uani 1 1 d . . . C5 C -0.3175(17) 0.8786(10) 0.2948(12) 0.107(5) Uani 1 1 d . . . H5A H -0.3558 0.9112 0.3505 0.128 Uiso 1 1 calc R . . H5B H -0.2576 0.9182 0.2673 0.128 Uiso 1 1 calc R . . C6 C -0.425(2) 0.8887(11) 0.2345(15) 0.153(9) Uani 1 1 d . . . H6A H -0.3992 0.9131 0.1739 0.184 Uiso 1 1 calc R . . H6B H -0.5054 0.9427 0.2542 0.184 Uiso 1 1 calc R . . C7 C 0.0446(13) 0.1212(10) 0.2413(11) 0.086(4) Uani 1 1 d . . . C8 C -0.1865(13) 0.1244(9) 0.1687(11) 0.086(4) Uani 1 1 d . . . C9 C -0.0379(11) 0.0698(9) 0.1857(10) 0.076(4) Uani 1 1 d . . . C10 C 0.0227(11) -0.0262(9) 0.1535(9) 0.073(4) Uani 1 1 d . . . C11 C 0.0779(18) -0.2135(13) 0.0830(15) 0.142(7) Uani 1 1 d . . . H11A H 0.0707 -0.2665 0.1317 0.170 Uiso 1 1 calc R . . H11B H 0.0736 -0.2423 0.0245 0.170 Uiso 1 1 calc R . . C12 C 0.2073(16) -0.1909(14) 0.0907(14) 0.136(7) Uani 1 1 d . . . H12A H 0.2330 -0.1644 0.0309 0.163 Uiso 1 1 calc R . . H12B H 0.2784 -0.2562 0.1098 0.163 Uiso 1 1 calc R . . N1 N 0.3204(12) 0.3157(13) 0.1019(10) 0.099(4) Uani 1 1 d D . . N2 N 0.2636(11) 0.7574(8) 0.4797(7) 0.071(3) Uani 1 1 d D . . C13 C 0.444(4) 0.232(2) 0.054(2) 0.113(11) Uani 0.50 1 d P A 1 H13A H 0.4585 0.2613 -0.0078 0.136 Uiso 0.50 1 calc PR A 1 H13B H 0.5284 0.2203 0.0886 0.136 Uiso 0.50 1 calc PR A 1 C14 C 0.412(4) 0.1217(19) 0.048(2) 0.27(2) Uani 1 1 d D . . H14A H 0.4910 0.0709 0.0240 0.330 Uiso 0.50 1 calc PR A 1 H14B H 0.3345 0.1320 0.0075 0.330 Uiso 0.50 1 calc PR A 1 H14C H 0.3903 0.0957 0.1080 0.330 Uiso 0.50 1 calc PR A 1 H14D H 0.3915 0.0548 0.0504 0.330 Uiso 0.50 1 calc PR A 2 H14E H 0.4955 0.1132 0.0809 0.330 Uiso 0.50 1 calc PR A 2 H14F H 0.4227 0.1454 -0.0153 0.330 Uiso 0.50 1 calc PR A 2 C15 C 0.198(3) 0.320(4) 0.052(3) 0.157(18) Uani 0.50 1 d P A 1 H15A H 0.1194 0.3649 0.0831 0.188 Uiso 0.50 1 calc PR A 1 H15B H 0.1875 0.2486 0.0570 0.188 Uiso 0.50 1 calc PR A 1 C16 C 0.187(2) 0.3587(16) -0.0491(14) 0.153(8) Uani 1 1 d . . . H16A H 0.1023 0.3539 -0.0737 0.183 Uiso 0.50 1 calc PR A 1 H16B H 0.2637 0.3155 -0.0817 0.183 Uiso 0.50 1 calc PR A 1 H16C H 0.1884 0.4315 -0.0558 0.183 Uiso 0.50 1 calc PR A 1 H16D H 0.1929 0.3956 -0.1079 0.183 Uiso 0.50 1 calc PR A 2 H16E H 0.1047 0.3962 -0.0181 0.183 Uiso 0.50 1 calc PR A 2 H16F H 0.1844 0.2879 -0.0575 0.183 Uiso 0.50 1 calc PR A 2 C17 C 0.318(4) 0.258(5) 0.189(3) 0.17(2) Uani 0.50 1 d P A 1 H17A H 0.2421 0.3002 0.2245 0.201 Uiso 0.50 1 calc PR A 1 H17B H 0.2966 0.1930 0.1784 0.201 Uiso 0.50 1 calc PR A 1 C18 C 0.437(2) 0.230(2) 0.2440(17) 0.235(15) Uani 1 1 d D . . H18A H 0.4214 0.1917 0.2999 0.283 Uiso 0.50 1 calc PR A 1 H18B H 0.4573 0.2940 0.2583 0.283 Uiso 0.50 1 calc PR A 1 H18C H 0.5129 0.1869 0.2112 0.283 Uiso 0.50 1 calc PR A 1 H18D H 0.5206 0.2172 0.2782 0.283 Uiso 0.50 1 calc PR A 2 H18E H 0.4213 0.1640 0.2334 0.283 Uiso 0.50 1 calc PR A 2 H18F H 0.3608 0.2721 0.2782 0.283 Uiso 0.50 1 calc PR A 2 C19 C 0.347(4) 0.412(5) 0.117(4) 0.21(2) Uani 0.50 1 d PDU A 1 H19A H 0.3598 0.4500 0.0589 0.258 Uiso 0.50 1 calc PR A 1 H19B H 0.4282 0.3995 0.1548 0.258 Uiso 0.50 1 calc PR A 1 C20 C 0.214(3) 0.474(2) 0.167(2) 0.256(17) Uani 1 1 d D . . H20A H 0.1767 0.4244 0.2027 0.307 Uiso 0.50 1 calc PR A 1 H20B H 0.1472 0.5149 0.1224 0.307 Uiso 0.50 1 calc PR A 1 H20C H 0.2367 0.5208 0.2069 0.307 Uiso 0.50 1 calc PR A 1 H20D H 0.1463 0.5101 0.2096 0.307 Uiso 0.50 1 calc PR A 2 H20E H 0.2001 0.5137 0.1080 0.307 Uiso 0.50 1 calc PR A 2 H20F H 0.3048 0.4677 0.1892 0.307 Uiso 0.50 1 calc PR A 2 C21 C 0.198(3) 0.843(2) 0.4064(19) 0.085(8) Uani 0.50 1 d P B 1 H21A H 0.2211 0.8169 0.3460 0.102 Uiso 0.50 1 calc PR B 1 H21B H 0.2313 0.9042 0.4105 0.102 Uiso 0.50 1 calc PR B 1 C22 C 0.035(2) 0.8754(15) 0.4215(19) 0.184(11) Uani 1 1 d D . . H22A H -0.0093 0.9319 0.3765 0.221 Uiso 0.50 1 calc PR B 1 H22B H 0.0134 0.8989 0.4821 0.221 Uiso 0.50 1 calc PR B 1 H22C H 0.0025 0.8148 0.4149 0.221 Uiso 0.50 1 calc PR B 1 H22D H -0.0613 0.9049 0.4350 0.221 Uiso 0.50 1 calc PR B 2 H22E H 0.0448 0.8340 0.3692 0.221 Uiso 0.50 1 calc PR B 2 H22F H 0.0758 0.9320 0.4080 0.221 Uiso 0.50 1 calc PR B 2 C23 C 0.214(3) 0.660(2) 0.465(2) 0.095(9) Uani 0.50 1 d P B 1 H23A H 0.2640 0.6032 0.5097 0.114 Uiso 0.50 1 calc PR B 1 H23B H 0.1179 0.6782 0.4841 0.114 Uiso 0.50 1 calc PR B 1 C24 C 0.221(2) 0.6155(13) 0.3852(17) 0.147(8) Uani 1 1 d . . . H24A H 0.1850 0.5554 0.3932 0.177 Uiso 0.50 1 calc PR B 1 H24B H 0.3148 0.5925 0.3651 0.177 Uiso 0.50 1 calc PR B 1 H24C H 0.1664 0.6670 0.3399 0.177 Uiso 0.50 1 calc PR B 1 H24D H 0.2388 0.5910 0.3247 0.177 Uiso 0.50 1 calc PR B 2 H24E H 0.1227 0.6370 0.3960 0.177 Uiso 0.50 1 calc PR B 2 H24F H 0.2649 0.5590 0.4302 0.177 Uiso 0.50 1 calc PR B 2 C25 C 0.416(3) 0.723(2) 0.469(2) 0.094(9) Uani 0.50 1 d P B 1 H25A H 0.4355 0.7003 0.4072 0.112 Uiso 0.50 1 calc PR B 1 H25B H 0.4468 0.7858 0.4717 0.112 Uiso 0.50 1 calc PR B 1 C26 C 0.5029(18) 0.6397(13) 0.5315(15) 0.142(7) Uani 1 1 d . . . H26A H 0.5978 0.6268 0.5136 0.170 Uiso 0.50 1 calc PR B 1 H26B H 0.4769 0.5755 0.5293 0.170 Uiso 0.50 1 calc PR B 1 H26C H 0.4912 0.6617 0.5931 0.170 Uiso 0.50 1 calc PR B 1 H26D H 0.5485 0.5913 0.5818 0.170 Uiso 0.50 1 calc PR B 2 H26E H 0.5458 0.6955 0.5205 0.170 Uiso 0.50 1 calc PR B 2 H26F H 0.5097 0.6020 0.4772 0.170 Uiso 0.50 1 calc PR B 2 C27 C 0.240(4) 0.805(3) 0.5750(17) 0.25(4) Uani 0.50 1 d PD B 1 H27A H 0.2876 0.7530 0.6234 0.297 Uiso 0.50 1 calc PR B 1 H27B H 0.1425 0.8292 0.5896 0.297 Uiso 0.50 1 calc PR B 1 C28 C 0.302(4) 0.901(2) 0.563(2) 0.45(5) Uani 1 1 d D . . H28A H 0.3980 0.8755 0.5463 0.537 Uiso 0.50 1 calc PR B 1 H28B H 0.2940 0.9343 0.6197 0.537 Uiso 0.50 1 calc PR B 1 H28C H 0.2531 0.9517 0.5153 0.537 Uiso 0.50 1 calc PR B 1 H28D H 0.3534 0.8480 0.6084 0.537 Uiso 0.50 1 calc PR B 2 H28E H 0.2066 0.9230 0.5800 0.537 Uiso 0.50 1 calc PR B 2 H28F H 0.3375 0.9612 0.5589 0.537 Uiso 0.50 1 calc PR B 2 C13A C 0.293(3) 0.204(3) 0.091(4) 0.22(3) Uani 0.50 1 d PD A 2 H13C H 0.2744 0.1746 0.1513 0.269 Uiso 0.50 1 calc PR A 2 H13D H 0.2113 0.2166 0.0536 0.269 Uiso 0.50 1 calc PR A 2 C15A C 0.318(4) 0.353(4) 0.011(4) 0.166(18) Uani 0.50 1 d P A 2 H15C H 0.3990 0.3081 -0.0182 0.199 Uiso 0.50 1 calc PR A 2 H15D H 0.3287 0.4238 0.0087 0.199 Uiso 0.50 1 calc PR A 2 C17A C 0.449(4) 0.293(3) 0.150(2) 0.136(13) Uani 0.50 1 d PDU A 2 H17C H 0.4692 0.3584 0.1597 0.163 Uiso 0.50 1 calc PR A 2 H17D H 0.5230 0.2500 0.1135 0.163 Uiso 0.50 1 calc PR A 2 C19A C 0.201(4) 0.365(3) 0.158(3) 0.30(5) Uani 0.50 1 d PD A 2 H19C H 0.2039 0.3263 0.2177 0.357 Uiso 0.50 1 calc PR A 2 H19D H 0.1150 0.3694 0.1274 0.357 Uiso 0.50 1 calc PR A 2 C21A C 0.109(3) 0.803(2) 0.506(2) 0.22(3) Uani 0.50 1 d PD B 2 H21C H 0.0682 0.7451 0.5205 0.259 Uiso 0.50 1 calc PR B 2 H21D H 0.0996 0.8435 0.5594 0.259 Uiso 0.50 1 calc PR B 2 C23A C 0.275(3) 0.707(3) 0.393(2) 0.103(10) Uani 0.50 1 d P B 2 H23C H 0.3718 0.6846 0.3764 0.123 Uiso 0.50 1 calc PR B 2 H23D H 0.2289 0.7623 0.3458 0.123 Uiso 0.50 1 calc PR B 2 C25A C 0.356(4) 0.686(3) 0.555(2) 0.113(11) Uani 0.50 1 d P B 2 H25C H 0.3519 0.7273 0.6074 0.136 Uiso 0.50 1 calc PR B 2 H25D H 0.3183 0.6282 0.5737 0.136 Uiso 0.50 1 calc PR B 2 C27A C 0.318(3) 0.8525(19) 0.466(2) 0.120(12) Uani 0.50 1 d PD B 2 H27C H 0.2642 0.9043 0.4199 0.144 Uiso 0.50 1 calc PR B 2 H27D H 0.4135 0.8311 0.4474 0.144 Uiso 0.50 1 calc PR B 2 OW1 O 0.1345(13) 0.3601(11) 0.4455(9) 0.164(5) Uani 1 1 d . . . OW2 O 0.254(2) 0.1421(15) 0.4265(10) 0.219(8) 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 V 0.0444(11) 0.0456(11) 0.1047(18) 0.0090(10) -0.0082(10) -0.0125(8) S1 0.144(4) 0.066(2) 0.153(4) 0.007(2) -0.074(3) -0.043(2) S2 0.071(2) 0.0593(18) 0.092(3) -0.0140(17) -0.0048(17) -0.0043(15) S3 0.072(2) 0.065(2) 0.155(4) -0.007(2) -0.011(2) -0.0180(17) S4 0.060(2) 0.074(2) 0.132(3) 0.002(2) -0.013(2) 0.0065(16) O1 0.070(5) 0.061(5) 0.123(8) 0.007(5) -0.045(5) -0.013(4) O2 0.043(4) 0.063(5) 0.115(7) -0.016(5) 0.000(4) -0.021(4) O3 0.234(14) 0.085(7) 0.190(13) 0.004(8) -0.158(12) -0.036(8) O4 0.049(5) 0.072(6) 0.253(14) -0.056(7) -0.023(7) -0.004(4) O5 0.046(5) 0.054(5) 0.149(8) 0.012(5) -0.027(5) -0.009(4) O6 0.039(4) 0.052(5) 0.192(10) -0.004(5) -0.013(5) -0.011(3) O7 0.079(6) 0.065(6) 0.190(11) 0.003(6) -0.050(7) -0.002(5) O8 0.059(6) 0.063(5) 0.226(13) -0.017(7) -0.022(6) -0.013(4) O9 0.074(6) 0.085(6) 0.110(8) 0.003(5) 0.009(5) -0.021(5) C1 0.112(12) 0.065(9) 0.098(11) 0.015(8) -0.041(9) -0.031(8) C2 0.053(7) 0.050(7) 0.101(10) -0.020(6) -0.001(7) -0.009(6) C3 0.065(7) 0.053(7) 0.061(8) 0.010(6) -0.008(6) -0.017(5) C4 0.076(8) 0.054(7) 0.055(8) 0.003(5) -0.007(6) -0.019(6) C5 0.120(13) 0.061(8) 0.142(15) -0.014(9) -0.018(11) -0.027(8) C6 0.186(19) 0.062(9) 0.21(2) 0.048(11) -0.100(17) -0.048(11) C7 0.059(8) 0.049(7) 0.135(13) 0.013(8) -0.013(8) 0.001(6) C8 0.063(8) 0.032(6) 0.157(13) 0.004(7) -0.006(8) -0.010(6) C9 0.049(7) 0.046(7) 0.129(12) 0.010(7) -0.005(7) -0.010(5) C10 0.047(7) 0.062(7) 0.103(10) 0.014(7) 0.002(6) -0.011(5) C11 0.114(14) 0.096(12) 0.21(2) -0.075(13) -0.011(13) 0.000(10) C12 0.068(10) 0.124(14) 0.20(2) -0.066(14) -0.016(11) 0.010(9) N1 0.058(8) 0.171(14) 0.058(9) -0.007(9) 0.005(6) -0.021(8) N2 0.102(9) 0.064(6) 0.047(7) -0.010(6) 0.012(6) -0.022(6) C13 0.16(3) 0.10(2) 0.07(2) 0.009(17) -0.02(2) -0.02(2) C14 0.42(5) 0.101(18) 0.28(4) -0.04(2) -0.16(4) -0.02(2) C15 0.045(18) 0.28(6) 0.13(3) -0.01(3) -0.03(2) -0.02(2) C16 0.138(18) 0.162(19) 0.133(18) 0.013(15) -0.014(14) -0.011(14) C17 0.08(3) 0.34(7) 0.11(3) 0.03(4) -0.04(2) -0.12(4) C18 0.14(2) 0.38(4) 0.16(2) 0.04(2) -0.038(17) -0.03(2) C19 0.23(3) 0.20(3) 0.22(3) -0.02(2) -0.04(2) -0.07(2) C20 0.20(3) 0.27(3) 0.34(4) -0.20(3) 0.06(3) -0.08(2) C21 0.09(2) 0.061(15) 0.081(19) 0.005(14) 0.005(15) 0.010(13) C22 0.137(18) 0.085(12) 0.30(3) 0.018(16) -0.089(19) 0.016(11) C23 0.12(3) 0.071(18) 0.10(2) -0.018(17) 0.019(19) -0.035(17) C24 0.136(16) 0.084(12) 0.22(2) -0.032(14) -0.039(15) -0.025(11) C25 0.071(19) 0.11(2) 0.11(3) -0.06(2) 0.027(17) -0.026(16) C26 0.102(14) 0.090(12) 0.21(2) -0.015(13) -0.049(13) 0.015(10) C27 0.19(5) 0.29(7) 0.11(4) 0.11(4) 0.08(4) 0.13(5) C28 0.48(6) 0.18(3) 0.57(7) -0.28(4) -0.39(6) 0.17(3) C13A 0.07(2) 0.11(3) 0.50(11) 0.03(5) -0.05(4) -0.04(2) C15A 0.10(3) 0.17(4) 0.20(6) -0.02(4) 0.04(3) -0.01(3) C17A 0.13(2) 0.15(2) 0.14(2) -0.038(17) -0.030(16) -0.042(16) C19A 0.16(5) 0.53(13) 0.26(7) -0.32(9) 0.04(5) -0.11(6) C21A 0.21(5) 0.07(2) 0.38(8) -0.07(3) 0.25(6) -0.06(3) C23A 0.08(2) 0.11(2) 0.11(3) 0.04(2) -0.001(18) -0.024(17) C25A 0.14(3) 0.12(3) 0.08(2) 0.03(2) -0.04(2) -0.04(2) C27A 0.12(3) 0.068(18) 0.18(4) 0.01(2) -0.04(2) -0.035(17) OW1 0.116(9) 0.177(12) 0.176(12) 0.049(10) -0.052(9) -0.022(8) OW2 0.265(19) 0.231(18) 0.129(12) 0.023(12) -0.057(12) -0.028(14) _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 V O9 1.560(9) . ? V O6 1.941(8) . ? V O1 1.943(9) . ? V O5 1.952(7) . ? V O2 1.955(7) . ? S1 C4 1.734(12) . ? S1 C5 1.759(14) . ? S2 C4 1.738(11) . ? S2 C6 1.796(15) . ? S3 C10 1.740(13) . ? S3 C11 1.806(15) . ? S4 C10 1.757(11) . ? S4 C12 1.783(16) . ? O1 C1 1.304(16) . ? O2 C2 1.281(12) . ? O3 C1 1.219(15) . ? O4 C2 1.214(13) . ? O5 C7 1.271(14) . ? O6 C8 1.295(13) . ? O7 C7 1.243(13) . ? O8 C8 1.240(14) . ? C1 C3 1.490(17) . ? C2 C3 1.468(15) . ? C3 C4 1.357(14) . ? C5 C6 1.38(2) . ? C7 C9 1.508(18) . ? C8 C9 1.483(16) . ? C9 C10 1.351(16) . ? C11 C12 1.44(2) . ? N1 C15A 1.37(5) . ? N1 C19 1.40(6) . ? N1 C17 1.43(4) . ? N1 C17A 1.43(4) . ? N1 C15 1.44(3) . ? N1 C19A 1.47(2) . ? N1 C13A 1.59(4) . ? N1 C13 1.60(3) . ? N2 C23A 1.47(4) . ? N2 C25 1.48(3) . ? N2 C21 1.50(3) . ? N2 C27A 1.504(18) . ? N2 C25A 1.52(3) . ? N2 C23 1.55(3) . ? N2 C27 1.56(2) . ? N2 C21A 1.56(3) . ? C13 C14 1.59(4) . ? C14 C13A 1.53(2) . ? C15 C16 1.51(4) . ? C16 C15A 1.59(5) . ? C17 C18 1.40(3) . ? C18 C17A 1.56(2) . ? C19 C20 1.56(2) . ? C20 C19A 1.49(2) . ? C21 C22 1.60(3) . ? C22 C21A 1.56(2) . ? C23 C24 1.34(3) . ? C24 C23A 1.48(3) . ? C25 C26 1.46(3) . ? C26 C25A 1.47(4) . ? C27 C28 1.57(2) . ? C28 C27A 1.58(2) . ? 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 O9 V O6 108.1(5) . . ? O9 V O1 109.4(4) . . ? O6 V O1 142.5(4) . . ? O9 V O5 108.2(4) . . ? O6 V O5 85.6(3) . . ? O1 V O5 81.7(3) . . ? O9 V O2 106.0(4) . . ? O6 V O2 85.6(3) . . ? O1 V O2 85.4(3) . . ? O5 V O2 145.8(4) . . ? C4 S1 C5 98.1(7) . . ? C4 S2 C6 97.0(7) . . ? C10 S3 C11 96.9(7) . . ? C10 S4 C12 95.9(7) . . ? C1 O1 V 131.2(8) . . ? C2 O2 V 128.3(7) . . ? C7 O5 V 131.2(9) . . ? C8 O6 V 130.7(8) . . ? O3 C1 O1 120.1(13) . . ? O3 C1 C3 120.1(14) . . ? O1 C1 C3 119.7(12) . . ? O4 C2 O2 120.6(11) . . ? O4 C2 C3 118.5(10) . . ? O2 C2 C3 120.9(10) . . ? C4 C3 C2 121.5(10) . . ? C4 C3 C1 118.7(11) . . ? C2 C3 C1 119.8(10) . . ? C3 C4 S1 124.1(9) . . ? C3 C4 S2 122.7(9) . . ? S1 C4 S2 113.2(6) . . ? C6 C5 S1 115.3(11) . . ? C5 C6 S2 113.8(11) . . ? O7 C7 O5 120.8(13) . . ? O7 C7 C9 117.6(11) . . ? O5 C7 C9 121.6(10) . . ? O8 C8 O6 121.6(11) . . ? O8 C8 C9 118.2(11) . . ? O6 C8 C9 120.1(12) . . ? C10 C9 C8 120.5(12) . . ? C10 C9 C7 120.2(10) . . ? C8 C9 C7 119.3(11) . . ? C9 C10 S3 123.8(9) . . ? C9 C10 S4 122.6(10) . . ? S3 C10 S4 113.7(7) . . ? C12 C11 S3 110.4(12) . . ? C11 C12 S4 111.7(12) . . ? C15A N1 C19 83(3) . . ? C15A N1 C17 168(3) . . ? C19 N1 C17 108(4) . . ? C15A N1 C17A 117(2) . . ? C19 N1 C17A 71(2) . . ? C17 N1 C17A 68.3(18) . . ? C15A N1 C15 65(2) . . ? C19 N1 C15 119(3) . . ? C17 N1 C15 108(2) . . ? C17A N1 C15 170(3) . . ? C15A N1 C19A 117(3) . . ? C19 N1 C19A 80(2) . . ? C17 N1 C19A 67(3) . . ? C17A N1 C19A 113(3) . . ? C15 N1 C19A 72(2) . . ? C15A N1 C13A 100(3) . . ? C19 N1 C13A 177(4) . . ? C17 N1 C13A 68(3) . . ? C17A N1 C13A 107(2) . . ? C15 N1 C13A 64(3) . . ? C19A N1 C13A 100(2) . . ? C15A N1 C13 74(2) . . ? C19 N1 C13 114(2) . . ? C17 N1 C13 100(3) . . ? C17A N1 C13 66.9(19) . . ? C15 N1 C13 106(2) . . ? C19A N1 C13 164(2) . . ? C13A N1 C13 66.1(19) . . ? C23A N2 C25 80.3(16) . . ? C23A N2 C21 72.5(15) . . ? C25 N2 C21 110.5(18) . . ? C23A N2 C27A 109.1(17) . . ? C25 N2 C27A 69.4(17) . . ? C21 N2 C27A 62.2(16) . . ? C23A N2 C25A 113(2) . . ? C25 N2 C25A 59.1(19) . . ? C21 N2 C25A 165.7(19) . . ? C27A N2 C25A 103.6(19) . . ? C23A N2 C23 55.7(15) . . ? C25 N2 C23 106.7(17) . . ? C21 N2 C23 107.5(18) . . ? C27A N2 C23 164.7(18) . . ? C25A N2 C23 85.8(18) . . ? C23A N2 C27 174(2) . . ? C25 N2 C27 104(2) . . ? C21 N2 C27 109.1(19) . . ? C27A N2 C27 76.3(16) . . ? C25A N2 C27 67(2) . . ? C23 N2 C27 118.8(19) . . ? C23A N2 C21A 109.7(19) . . ? C25 N2 C21A 170.0(19) . . ? C21 N2 C21A 72.9(15) . . ? C27A N2 C21A 105.5(17) . . ? C25A N2 C21A 115.6(19) . . ? C23 N2 C21A 80.5(17) . . ? C27 N2 C21A 66.0(19) . . ? C14 C13 N1 111(3) . . ? C13A C14 C13 68(2) . . ? N1 C15 C16 119(3) . . ? C15 C16 C15A 58(2) . . ? C18 C17 N1 118(3) . . ? C17 C18 C17A 65(2) . . ? N1 C19 C20 103(3) . . ? C19A C20 C19 74(3) . . ? N2 C21 C22 107.9(18) . . ? C21A C22 C21 70.4(15) . . ? C24 C23 N2 124(2) . . ? C23 C24 C23A 59.7(18) . . ? C26 C25 N2 121(2) . . ? C25 C26 C25A 60.9(16) . . ? N2 C27 C28 103.9(16) . . ? C27 C28 C27A 74.0(15) . . ? C14 C13A N1 115(2) . . ? N1 C15A C16 118(3) . . ? N1 C17A C18 108(2) . . ? N1 C19A C20 103(2) . . ? C22 C21A N2 106.9(18) . . ? N2 C23A C24 120(2) . . ? C26 C25A N2 117(3) . . ? N2 C27A C28 105.7(18) . . ? _diffrn_measured_fraction_theta_max 0.422 _diffrn_reflns_theta_full 25.65 _diffrn_measured_fraction_theta_full 0.422 _refine_diff_density_max 0.789 _refine_diff_density_min -0.450 _refine_diff_density_rms 0.085 data_v_b _database_code_depnum_ccdc_archive 'CCDC 262587' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H16 K2 O13 S4 V' _chemical_formula_weight 625.63 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' V V 0.3005 0.5294 '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 'C-centered monoclinic' _symmetry_space_group_name_H-M C2/c _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.781(6) _cell_length_b 4.1320(8) _cell_length_c 22.063(4) _cell_angle_alpha 90.00 _cell_angle_beta 116.68(2) _cell_angle_gamma 90.00 _cell_volume 2263.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour 'brownish yellow' _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.836 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1268 _exptl_absorpt_coefficient_mu 1.237 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5494 _exptl_absorpt_correction_T_max 0.9407 _exptl_absorpt_process_details 'Psi scan' _exptl_special_details ; Hydrogens of water molecules are not assigned. Other C-H hydrogens are included by riding model ; _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 CAD4 _diffrn_measurement_method omega/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <3% _diffrn_reflns_number 1781 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0547 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 3 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.49 _reflns_number_total 1040 _reflns_number_gt 966 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of 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^)+(0.0521P)^2^+4.0818P] 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 1040 _refine_ls_number_parameters 146 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1067 _refine_ls_wR_factor_gt 0.1029 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.135 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.0000 0.1198(8) 0.2500 0.0305(9) Uani 1 2 d S . . S1 S 0.22206(7) 0.4273(6) 0.29795(8) 0.0353(7) Uani 1 1 d . . . S2 S 0.22231(7) 0.5285(6) 0.42897(8) 0.0374(7) Uani 1 1 d . . . K1 K 0.01345(7) -0.2858(5) 0.39357(8) 0.0414(7) Uani 1 1 d . . . O1 O 0.0000 -0.282(3) 0.2500 0.032(3) Uani 1 2 d S . . O2 O 0.05626(16) 0.2213(13) 0.33984(19) 0.0288(15) Uani 1 1 d . . . O3 O 0.05133(16) 0.2099(14) 0.21453(19) 0.0287(16) Uani 1 1 d . . . O4 O 0.12610(18) 0.4634(17) 0.4183(2) 0.0491(19) Uani 1 1 d . . . O5 O 0.12895(16) 0.2197(14) 0.2115(2) 0.0355(16) Uani 1 1 d . . . C1 C 0.1042(2) 0.341(2) 0.3606(3) 0.029(2) Uani 1 1 d . . . C2 C 0.1027(2) 0.2505(19) 0.2446(3) 0.022(2) Uani 1 1 d . . . C3 C 0.1315(2) 0.342(2) 0.3170(3) 0.021(2) Uani 1 1 d . . . C4 C 0.1855(2) 0.420(2) 0.3447(3) 0.025(2) Uani 1 1 d . . . C5 C 0.2823(3) 0.609(2) 0.3631(3) 0.041(2) Uani 1 1 d . . . H5A H 0.3136 0.5393 0.3579 0.049 Uiso 1 1 calc R . . H5B H 0.2799 0.8427 0.3593 0.049 Uiso 1 1 calc R . . C6 C 0.2878(2) 0.505(2) 0.4318(3) 0.041(3) Uani 1 1 d . . . H6A H 0.3128 0.6460 0.4670 0.049 Uiso 1 1 calc R . . H6B H 0.3014 0.2851 0.4416 0.049 Uiso 1 1 calc R . . OW1 O -0.0915(2) -0.2709(16) 0.3811(2) 0.0485(18) Uani 1 1 d . . . OW2 O 0.0655(2) 0.2047(16) 0.4829(2) 0.0484(19) 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 V1 0.0205(8) 0.058(3) 0.0117(8) 0.000 0.0056(6) 0.000 S1 0.0267(8) 0.053(2) 0.0296(8) -0.0032(11) 0.0153(7) -0.0020(11) S2 0.0265(8) 0.058(2) 0.0226(8) -0.0079(10) 0.0066(7) -0.0066(11) K1 0.0522(10) 0.0439(19) 0.0318(8) 0.0019(10) 0.0222(8) 0.0042(11) O1 0.055(5) 0.001(10) 0.038(4) 0.000 0.020(4) 0.000 O2 0.024(2) 0.046(5) 0.015(2) -0.001(2) 0.0078(18) -0.001(2) O3 0.023(2) 0.050(5) 0.0138(19) -0.001(2) 0.0080(17) -0.002(3) O4 0.036(3) 0.089(6) 0.024(2) -0.019(3) 0.015(2) -0.017(3) O5 0.029(3) 0.058(5) 0.026(2) -0.012(3) 0.018(2) -0.008(3) C1 0.021(3) 0.048(8) 0.018(3) 0.000(4) 0.008(3) 0.001(4) C2 0.027(3) 0.018(7) 0.022(3) 0.003(3) 0.013(3) 0.000(4) C3 0.023(3) 0.023(7) 0.015(3) -0.002(3) 0.005(2) 0.007(4) C4 0.026(3) 0.026(7) 0.021(3) 0.002(4) 0.009(3) 0.004(4) C5 0.027(4) 0.051(8) 0.042(4) -0.007(5) 0.014(3) -0.005(5) C6 0.022(3) 0.055(8) 0.036(4) -0.010(4) 0.005(3) -0.006(4) OW1 0.056(3) 0.063(6) 0.032(3) 0.003(3) 0.025(3) 0.006(3) OW2 0.054(3) 0.058(6) 0.030(2) 0.001(3) 0.016(2) -0.005(3) _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 V1 O1 1.662(10) . ? V1 O2 1.941(4) . ? V1 O2 1.941(4) 2 ? V1 O3 1.946(4) 2 ? V1 O3 1.946(4) . ? V1 O1 2.470(10) 1_565 ? V1 K1 3.452(2) . ? V1 K1 3.452(2) 2 ? V1 K1 3.891(3) 1_565 ? V1 K1 3.891(3) 2_565 ? S1 C4 1.744(6) . ? S1 C5 1.809(7) . ? S2 C4 1.730(6) . ? S2 C6 1.797(7) . ? K1 OW2 2.743(6) . ? K1 OW2 2.802(6) 1_545 ? K1 OW1 2.804(5) . ? K1 O2 2.869(5) 1_545 ? K1 O2 2.911(5) . ? K1 O1 3.0184(16) . ? K1 O3 3.044(5) 2 ? K1 O3 3.068(5) 2_545 ? K1 O4 3.104(5) 1_545 ? K1 C1 3.304(7) 1_545 ? K1 V1 3.891(3) 1_545 ? O1 V1 2.470(10) 1_545 ? O1 K1 3.0184(16) 2 ? O2 C1 1.298(8) . ? O2 K1 2.869(5) 1_565 ? O3 C2 1.287(7) . ? O3 K1 3.044(5) 2 ? O3 K1 3.068(5) 2_565 ? O4 C1 1.244(8) . ? O4 K1 3.104(5) 1_565 ? O5 C2 1.248(7) . ? C1 C3 1.467(8) . ? C1 K1 3.304(7) 1_565 ? C2 C3 1.479(8) . ? C3 C4 1.380(8) . ? C5 C6 1.514(10) . ? OW2 K1 2.802(6) 1_565 ? 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 V1 O2 102.48(18) . . ? O1 V1 O2 102.48(18) . 2 ? O2 V1 O2 155.0(4) . 2 ? O1 V1 O3 101.03(19) . 2 ? O2 V1 O3 86.99(17) . 2 ? O2 V1 O3 88.27(17) 2 2 ? O1 V1 O3 101.03(19) . . ? O2 V1 O3 88.27(17) . . ? O2 V1 O3 86.99(17) 2 . ? O3 V1 O3 157.9(4) 2 . ? O1 V1 O1 180.000(4) . 1_565 ? O2 V1 O1 77.52(18) . 1_565 ? O2 V1 O1 77.52(18) 2 1_565 ? O3 V1 O1 78.97(19) 2 1_565 ? O3 V1 O1 78.97(19) . 1_565 ? O1 V1 K1 60.96(6) . . ? O2 V1 K1 57.45(15) . . ? O2 V1 K1 138.40(15) 2 . ? O3 V1 K1 61.37(15) 2 . ? O3 V1 K1 131.67(14) . . ? O1 V1 K1 119.04(6) 1_565 . ? O1 V1 K1 60.96(6) . 2 ? O2 V1 K1 138.40(15) . 2 ? O2 V1 K1 57.45(15) 2 2 ? O3 V1 K1 131.67(14) 2 2 ? O3 V1 K1 61.37(15) . 2 ? O1 V1 K1 119.04(6) 1_565 2 ? K1 V1 K1 121.92(12) . 2 ? O1 V1 K1 129.14(5) . 1_565 ? O2 V1 K1 45.03(15) . 1_565 ? O2 V1 K1 115.73(18) 2 1_565 ? O3 V1 K1 51.08(15) 2 1_565 ? O3 V1 K1 112.75(18) . 1_565 ? O1 V1 K1 50.86(5) 1_565 1_565 ? K1 V1 K1 68.18(3) . 1_565 ? K1 V1 K1 169.91(10) 2 1_565 ? O1 V1 K1 129.14(5) . 2_565 ? O2 V1 K1 115.73(18) . 2_565 ? O2 V1 K1 45.03(15) 2 2_565 ? O3 V1 K1 112.75(18) 2 2_565 ? O3 V1 K1 51.08(15) . 2_565 ? O1 V1 K1 50.86(5) 1_565 2_565 ? K1 V1 K1 169.91(10) . 2_565 ? K1 V1 K1 68.18(3) 2 2_565 ? K1 V1 K1 101.73(10) 1_565 2_565 ? C4 S1 C5 96.5(3) . . ? C4 S2 C6 97.1(3) . . ? OW2 K1 OW2 96.35(15) . 1_545 ? OW2 K1 OW1 104.09(17) . . ? OW2 K1 OW1 105.71(17) 1_545 . ? OW2 K1 O2 129.72(16) . 1_545 ? OW2 K1 O2 65.09(14) 1_545 1_545 ? OW1 K1 O2 125.49(17) . 1_545 ? OW2 K1 O2 65.24(14) . . ? OW2 K1 O2 130.65(16) 1_545 . ? OW1 K1 O2 122.77(17) . . ? O2 K1 O2 91.25(12) 1_545 . ? OW2 K1 O1 121.9(2) . . ? OW2 K1 O1 121.6(2) 1_545 . ? OW1 K1 O1 105.28(11) . . ? O2 K1 O1 56.54(19) 1_545 . ? O2 K1 O1 56.64(19) . . ? OW2 K1 O3 90.08(16) . 2 ? OW2 K1 O3 173.51(16) 1_545 2 ? OW1 K1 O3 71.67(14) . 2 ? O2 K1 O3 111.27(12) 1_545 2 ? O2 K1 O3 53.32(12) . 2 ? O1 K1 O3 54.81(19) . 2 ? OW2 K1 O3 175.06(16) . 2_545 ? OW2 K1 O3 88.51(16) 1_545 2_545 ? OW1 K1 O3 73.59(14) . 2_545 ? O2 K1 O3 53.42(12) 1_545 2_545 ? O2 K1 O3 112.12(12) . 2_545 ? O1 K1 O3 55.55(19) . 2_545 ? O3 K1 O3 85.05(10) 2 2_545 ? OW2 K1 O4 87.49(17) . 1_545 ? OW2 K1 O4 57.63(16) 1_545 1_545 ? OW1 K1 O4 161.21(19) . 1_545 ? O2 K1 O4 42.55(13) 1_545 1_545 ? O2 K1 O4 75.39(16) . 1_545 ? O1 K1 O4 79.96(12) . 1_545 ? O3 K1 O4 123.85(14) 2 1_545 ? O3 K1 O4 95.91(15) 2_545 1_545 ? OW2 K1 C1 107.16(19) . 1_545 ? OW2 K1 C1 66.47(17) 1_545 1_545 ? OW1 K1 C1 148.4(2) . 1_545 ? O2 K1 C1 22.91(16) 1_545 1_545 ? O2 K1 C1 75.78(18) . 1_545 ? O1 K1 C1 61.19(16) . 1_545 ? O3 K1 C1 112.50(15) 2 1_545 ? O3 K1 C1 75.60(15) 2_545 1_545 ? O4 K1 C1 22.11(13) 1_545 1_545 ? OW2 K1 V1 96.07(13) . . ? OW2 K1 V1 145.04(13) 1_545 . ? OW1 K1 V1 102.70(11) . . ? O2 K1 V1 81.94(10) 1_545 . ? O2 K1 V1 34.18(8) . . ? O1 K1 V1 28.78(19) . . ? O3 K1 V1 34.13(8) 2 . ? O3 K1 V1 80.35(10) 2_545 . ? O4 K1 V1 90.48(11) 1_545 . ? C1 K1 V1 78.66(13) 1_545 . ? OW2 K1 V1 151.45(12) . 1_545 ? OW2 K1 V1 85.94(13) 1_545 1_545 ? OW1 K1 V1 102.61(12) . 1_545 ? O2 K1 V1 28.58(8) 1_545 1_545 ? O2 K1 V1 91.73(10) . 1_545 ? O1 K1 V1 39.4(2) . 1_545 ? O3 K1 V1 88.85(10) 2 1_545 ? O3 K1 V1 29.56(8) 2_545 1_545 ? O4 K1 V1 69.69(10) 1_545 1_545 ? C1 K1 V1 47.94(12) 1_545 1_545 ? V1 K1 V1 68.18(3) . 1_545 ? V1 O1 V1 180.000(1) . 1_545 ? V1 O1 K1 90.3(2) . . ? V1 O1 K1 89.7(2) 1_545 . ? V1 O1 K1 90.3(2) . 2 ? V1 O1 K1 89.7(2) 1_545 2 ? K1 O1 K1 179.5(4) . 2 ? C1 O2 V1 132.2(4) . . ? C1 O2 K1 97.7(4) . 1_565 ? V1 O2 K1 106.39(19) . 1_565 ? C1 O2 K1 132.4(4) . . ? V1 O2 K1 88.37(19) . . ? K1 O2 K1 91.25(12) 1_565 . ? C2 O3 V1 131.4(4) . . ? C2 O3 K1 128.3(4) . 2 ? V1 O3 K1 84.50(17) . 2 ? C2 O3 K1 116.1(4) . 2_565 ? V1 O3 K1 99.35(18) . 2_565 ? K1 O3 K1 85.05(10) 2 2_565 ? C1 O4 K1 88.0(4) . 1_565 ? O4 C1 O2 117.9(6) . . ? O4 C1 C3 120.7(6) . . ? O2 C1 C3 121.3(6) . . ? O4 C1 K1 69.9(4) . 1_565 ? O2 C1 K1 59.4(4) . 1_565 ? C3 C1 K1 144.4(5) . 1_565 ? O5 C2 O3 119.3(6) . . ? O5 C2 C3 118.9(6) . . ? O3 C2 C3 121.8(5) . . ? C4 C3 C1 119.2(5) . . ? C4 C3 C2 119.5(5) . . ? C1 C3 C2 121.3(5) . . ? C3 C4 S2 122.5(5) . . ? C3 C4 S1 123.2(5) . . ? S2 C4 S1 114.3(4) . . ? C6 C5 S1 108.7(5) . . ? C5 C6 S2 107.7(5) . . ? K1 OW2 K1 96.35(15) . 1_565 ? _diffrn_measured_fraction_theta_max 0.499 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.499 _refine_diff_density_max 0.430 _refine_diff_density_min -0.311 _refine_diff_density_rms 0.083 data_co _database_code_depnum_ccdc_archive 'CCDC 266145' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H36 Co K2 O12 S4' _chemical_formula_weight 733.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Co Co 0.3494 0.9721 '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' 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' K K 0.2009 0.2494 '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_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.2415(19) _cell_length_b 8.8575(16) _cell_length_c 13.519(2) _cell_angle_alpha 104.580(14) _cell_angle_beta 90.401(17) _cell_angle_gamma 95.754(18) _cell_volume 834.5(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour 'red purple' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 381 _exptl_absorpt_coefficient_mu 1.064 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6755 _exptl_absorpt_correction_T_max 0.9010 _exptl_absorpt_process_details 'psi scan' _exptl_special_details ; Hydrogens of methanol oxygens O5, O6 are not assigned. ; _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 CAD4 _diffrn_measurement_method omega/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3217 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.1152 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.08 _reflns_number_total 2961 _reflns_number_gt 1608 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of 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^)+(0.0624P)^2^+0.0000P] 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 2961 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1437 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.1367 _refine_ls_wR_factor_gt 0.1131 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.5000 0.0000 0.0000 0.0336(3) Uani 1 2 d S . . K1 K 0.78466(17) -0.41481(14) -0.05234(12) 0.0576(4) Uani 1 1 d . . . S1 S 0.8493(3) -0.1280(2) -0.35373(13) 0.0733(5) Uani 1 1 d . . . S2 S 0.7436(2) 0.2066(2) -0.30000(14) 0.0644(5) Uani 1 1 d . . . O1 O 0.6904(4) -0.1391(4) -0.0745(3) 0.0436(9) Uani 1 1 d . . . O2 O 0.9704(4) -0.1657(4) -0.1355(3) 0.0456(9) Uani 1 1 d . . . O3 O 0.9164(4) 0.3085(4) -0.0705(3) 0.0455(9) Uani 1 1 d . . . O4 O 0.6573(4) 0.1971(3) -0.0223(3) 0.0398(9) Uani 1 1 d . . . O5 O 0.3276(5) -0.0336(4) -0.1369(3) 0.0500(10) Uani 1 1 d . . . O6 O 0.4059(5) -0.4704(4) -0.1059(3) 0.0596(11) Uani 1 1 d . . . C1 C 0.8288(6) -0.0962(5) -0.1212(4) 0.0331(11) Uani 1 1 d . . . C2 C 0.7962(6) 0.1962(5) -0.0795(4) 0.0327(11) Uani 1 1 d . . . C3 C 0.8128(6) 0.0479(5) -0.1602(4) 0.0320(11) Uani 1 1 d . . . C4 C 0.8049(7) 0.0415(6) -0.2592(4) 0.0476(14) Uani 1 1 d . . . C5 C 0.6598(15) -0.1545(12) -0.4445(7) 0.116(3) Uani 1 1 d . . . H5A H 0.6358 -0.0528 -0.4532 0.139 Uiso 1 1 calc R . . H5B H 0.6957 -0.2167 -0.5100 0.139 Uiso 1 1 calc R . . C6 C 0.4912(19) -0.2303(18) -0.4153(12) 0.236(8) Uani 1 1 d . . . H6A H 0.3958 -0.2409 -0.4670 0.353 Uiso 1 1 calc R . . H6B H 0.4527 -0.1682 -0.3514 0.353 Uiso 1 1 calc R . . H6C H 0.5128 -0.3322 -0.4080 0.353 Uiso 1 1 calc R . . C7 C 0.9465(11) 0.2571(10) -0.3630(7) 0.108(3) Uani 1 1 d . . . H7A H 1.0555 0.2611 -0.3199 0.130 Uiso 1 1 calc R . . H7B H 0.9569 0.1776 -0.4263 0.130 Uiso 1 1 calc R . . C8 C 0.9375(13) 0.4146(11) -0.3860(8) 0.127(4) Uani 1 1 d . . . H8A H 1.0477 0.4407 -0.4199 0.191 Uiso 1 1 calc R . . H8B H 0.9286 0.4933 -0.3232 0.191 Uiso 1 1 calc R . . H8C H 0.8305 0.4099 -0.4294 0.191 Uiso 1 1 calc R . . C9 C 0.3077(8) 0.0863(8) -0.1868(5) 0.0699(19) Uani 1 1 d . . . H9A H 0.2258 0.0461 -0.2457 0.105 Uiso 1 1 calc R . . H9B H 0.4270 0.1222 -0.2078 0.105 Uiso 1 1 calc R . . H9C H 0.2569 0.1721 -0.1408 0.105 Uiso 1 1 calc R . . C10 C 0.3684(16) -0.4733(11) -0.2056(7) 0.137(4) Uani 1 1 d . . . H10A H 0.2368 -0.4929 -0.2193 0.205 Uiso 1 1 calc R . . H10B H 0.4291 -0.5549 -0.2496 0.205 Uiso 1 1 calc R . . H10C H 0.4130 -0.3740 -0.2178 0.205 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 Co1 0.0231(5) 0.0288(5) 0.0533(7) 0.0181(5) 0.0067(5) 0.0039(4) K1 0.0438(7) 0.0389(7) 0.0968(11) 0.0311(7) -0.0133(7) 0.0011(5) S1 0.0861(13) 0.0758(12) 0.0534(11) 0.0027(9) 0.0033(9) 0.0222(10) S2 0.0652(10) 0.0743(11) 0.0723(12) 0.0495(9) 0.0046(9) 0.0158(9) O1 0.0354(19) 0.0311(18) 0.074(3) 0.0265(18) 0.0191(18) 0.0125(14) O2 0.0277(18) 0.044(2) 0.074(3) 0.0267(19) 0.0117(18) 0.0151(16) O3 0.0347(19) 0.0332(18) 0.072(3) 0.0224(18) 0.0006(18) -0.0058(16) O4 0.0316(18) 0.0297(18) 0.061(2) 0.0164(17) 0.0139(17) 0.0012(14) O5 0.036(2) 0.057(2) 0.065(3) 0.030(2) -0.0002(18) 0.0035(17) O6 0.056(3) 0.049(2) 0.072(3) 0.013(2) 0.000(2) 0.0033(19) C1 0.029(3) 0.030(2) 0.043(3) 0.014(2) -0.002(2) 0.002(2) C2 0.027(3) 0.026(2) 0.050(3) 0.019(2) -0.003(2) 0.002(2) C3 0.018(2) 0.034(3) 0.047(3) 0.016(2) 0.001(2) 0.0027(19) C4 0.042(3) 0.053(3) 0.053(4) 0.022(3) 0.004(3) 0.009(3) C5 0.136(9) 0.121(7) 0.077(6) 0.003(6) -0.045(6) 0.002(7) C6 0.157(13) 0.28(2) 0.260(18) 0.091(16) -0.105(13) -0.057(14) C7 0.098(6) 0.104(6) 0.151(9) 0.083(6) 0.037(6) 0.009(5) C8 0.121(7) 0.136(8) 0.157(9) 0.109(7) -0.020(7) -0.018(6) C9 0.046(4) 0.091(5) 0.089(5) 0.052(4) -0.002(3) 0.005(3) C10 0.183(11) 0.113(7) 0.100(8) -0.016(6) -0.054(7) 0.061(7) _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 Co1 O1 2.042(3) . ? Co1 O1 2.042(3) 2_655 ? Co1 O4 2.076(3) 2_655 ? Co1 O4 2.076(3) . ? Co1 O5 2.165(4) 2_655 ? Co1 O5 2.165(4) . ? K1 O3 2.662(4) 2_755 ? K1 O3 2.673(3) 1_545 ? K1 O1 2.687(3) . ? K1 O6 2.795(4) . ? K1 O6 2.893(4) 2_645 ? K1 O2 2.935(3) . ? K1 C1 3.175(4) . ? K1 C2 3.381(4) 1_545 ? K1 K1 3.995(2) 2_745 ? K1 K1 4.603(3) 2_645 ? S1 C4 1.768(6) . ? S1 C5 1.791(8) . ? S2 C7 1.778(7) . ? S2 C4 1.780(5) . ? O1 C1 1.265(5) . ? O2 C1 1.240(5) . ? O3 C2 1.235(5) . ? O3 K1 2.662(4) 2_755 ? O3 K1 2.673(3) 1_565 ? O4 C2 1.272(6) . ? O5 C9 1.412(6) . ? O6 C10 1.366(9) . ? O6 K1 2.893(4) 2_645 ? C1 C3 1.513(6) . ? C2 C3 1.498(7) . ? C2 K1 3.381(4) 1_565 ? C3 C4 1.326(7) . ? C5 C6 1.440(14) . ? C7 C8 1.512(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 O1 Co1 O1 180.0(2) . 2_655 ? O1 Co1 O4 89.77(12) . 2_655 ? O1 Co1 O4 90.23(12) 2_655 2_655 ? O1 Co1 O4 90.23(12) . . ? O1 Co1 O4 89.77(12) 2_655 . ? O4 Co1 O4 180.00(18) 2_655 . ? O1 Co1 O5 86.86(14) . 2_655 ? O1 Co1 O5 93.14(14) 2_655 2_655 ? O4 Co1 O5 94.18(13) 2_655 2_655 ? O4 Co1 O5 85.82(13) . 2_655 ? O1 Co1 O5 93.14(14) . . ? O1 Co1 O5 86.86(14) 2_655 . ? O4 Co1 O5 85.82(13) 2_655 . ? O4 Co1 O5 94.18(13) . . ? O5 Co1 O5 180.00(12) 2_655 . ? O3 K1 O3 83.00(11) 2_755 1_545 ? O3 K1 O1 98.69(11) 2_755 . ? O3 K1 O1 166.93(12) 1_545 . ? O3 K1 O6 156.41(13) 2_755 . ? O3 K1 O6 108.22(11) 1_545 . ? O1 K1 O6 75.16(11) . . ? O3 K1 O6 91.01(12) 2_755 2_645 ? O3 K1 O6 77.71(11) 1_545 2_645 ? O1 K1 O6 115.11(12) . 2_645 ? O6 K1 O6 71.98(15) . 2_645 ? O3 K1 O2 76.23(10) 2_755 . ? O3 K1 O2 123.01(10) 1_545 . ? O1 K1 O2 45.95(9) . . ? O6 K1 O2 111.75(11) . . ? O6 K1 O2 153.03(12) 2_645 . ? O3 K1 C1 88.58(11) 2_755 . ? O3 K1 C1 145.17(12) 1_545 . ? O1 K1 C1 23.06(10) . . ? O6 K1 C1 92.70(12) . . ? O6 K1 C1 136.39(12) 2_645 . ? O2 K1 C1 22.98(10) . . ? O3 K1 C2 98.95(11) 2_755 1_545 ? O3 K1 C2 19.38(10) 1_545 1_545 ? O1 K1 C2 162.24(13) . 1_545 ? O6 K1 C2 89.33(11) . 1_545 ? O6 K1 C2 66.57(12) 2_645 1_545 ? O2 K1 C2 138.18(12) . 1_545 ? C1 K1 C2 156.08(14) . 1_545 ? O3 K1 K1 41.61(7) 2_755 2_745 ? O3 K1 K1 41.39(8) 1_545 2_745 ? O1 K1 K1 138.79(9) . 2_745 ? O6 K1 K1 145.05(9) . 2_745 ? O6 K1 K1 82.49(9) 2_645 2_745 ? O2 K1 K1 101.89(8) . 2_745 ? C1 K1 K1 122.18(10) . 2_745 ? C2 K1 K1 58.17(8) 1_545 2_745 ? O3 K1 K1 124.59(10) 2_755 2_645 ? O3 K1 K1 93.21(8) 1_545 2_645 ? O1 K1 K1 96.38(8) . 2_645 ? O6 K1 K1 36.71(9) . 2_645 ? O6 K1 K1 35.28(9) 2_645 2_645 ? O2 K1 K1 141.74(8) . 2_645 ? C1 K1 K1 118.93(9) . 2_645 ? C2 K1 K1 75.11(9) 1_545 2_645 ? K1 K1 K1 114.56(6) 2_745 2_645 ? C4 S1 C5 103.3(4) . . ? C7 S2 C4 101.9(3) . . ? C1 O1 Co1 126.5(3) . . ? C1 O1 K1 100.7(3) . . ? Co1 O1 K1 130.25(14) . . ? C1 O2 K1 89.4(3) . . ? C2 O3 K1 133.6(3) . 2_755 ? C2 O3 K1 114.7(3) . 1_565 ? K1 O3 K1 97.00(11) 2_755 1_565 ? C2 O4 Co1 125.6(3) . . ? C9 O5 Co1 123.3(4) . . ? C10 O6 K1 113.4(5) . . ? C10 O6 K1 136.2(6) . 2_645 ? K1 O6 K1 108.02(15) . 2_645 ? O2 C1 O1 123.5(4) . . ? O2 C1 C3 120.7(4) . . ? O1 C1 C3 115.8(4) . . ? O2 C1 K1 67.6(2) . . ? O1 C1 K1 56.3(2) . . ? C3 C1 K1 169.5(3) . . ? O3 C2 O4 123.7(4) . . ? O3 C2 C3 119.5(4) . . ? O4 C2 C3 116.8(4) . . ? O3 C2 K1 45.9(2) . 1_565 ? O4 C2 K1 89.0(3) . 1_565 ? C3 C2 K1 140.8(3) . 1_565 ? C4 C3 C2 122.4(4) . . ? C4 C3 C1 122.2(5) . . ? C2 C3 C1 115.3(4) . . ? C3 C4 S1 122.2(4) . . ? C3 C4 S2 119.6(4) . . ? S1 C4 S2 118.2(3) . . ? C6 C5 S1 113.7(8) . . ? C8 C7 S2 110.2(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.08 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.449 _refine_diff_density_min -0.495 _refine_diff_density_rms 0.082