Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_year 2006 _journal_page_first 3257 _publ_contact_author_name 'Alexander Rothenberger' _publ_contact_author_address ; Department of Inorganic Chemistry University of Karlsruhe Engesserstr. 15 Karlsruhe 76131 GERMANY ; _publ_contact_author_email ROTHENBERGER@CHEMIE.UNI-KARLSRUHE.DE _publ_section_title ; Metal thiophosphonates and related compounds: An emerging area of supramolecular coordination chemistry ; loop_ _publ_author_name 'Alexander Rothenberger' 'Christopher E. Anson' 'Maryam Shafaei-Fallah' 'Weifeng Shi.' data_1 _database_code_depnum_ccdc_archive 'CCDC 601692' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H78 Cu4 O2 P6 S6' _chemical_formula_weight 1703.76 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' P P 0.1023 0.0942 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.420(2) _cell_length_b 16.052(3) _cell_length_c 19.785(4) _cell_angle_alpha 78.256(16) _cell_angle_beta 86.306(15) _cell_angle_gamma 65.845(14) _cell_volume 3806.7(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3069 _cell_measurement_theta_min 3.41 _cell_measurement_theta_max 56.77 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1752 _exptl_absorpt_coefficient_mu 1.440 _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 100(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 'stoe ipds 2' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34222 _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_sigmaI/netI 0.0565 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 28.27 _reflns_number_total 17354 _reflns_number_gt 11922 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'stoe x-area' _computing_cell_refinement 'stoe x-area' _computing_data_reduction 'stoe x-area' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0816P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17354 _refine_ls_number_parameters 883 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0718 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1445 _refine_ls_wR_factor_gt 0.1304 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 Cu1 Cu 0.10707(3) 0.34803(3) 0.490188(19) 0.02804(10) Uani 1 1 d . . . Cu2 Cu -0.11091(4) 0.43792(3) 0.45906(2) 0.03308(11) Uani 1 1 d . . . Cu3 Cu 0.37979(3) 0.15155(3) 0.012820(19) 0.02919(10) Uani 1 1 d . . . Cu4 Cu 0.59297(4) 0.06946(3) 0.04638(2) 0.03285(11) Uani 1 1 d . . . P1 P 0.24823(7) 0.20914(5) 0.49507(4) 0.02464(16) Uani 1 1 d . . . P2 P -0.21423(7) 0.38620(6) 0.41083(4) 0.02707(17) Uani 1 1 d . . . P3 P 0.09855(7) 0.52227(6) 0.39811(4) 0.02604(16) Uani 1 1 d . . . P4 P 0.24463(7) 0.29313(5) 0.00643(4) 0.02478(16) Uani 1 1 d . . . P5 P 0.70026(7) 0.12210(6) 0.08968(4) 0.02691(17) Uani 1 1 d . . . P6 P 0.39690(7) -0.02994(6) 0.09672(4) 0.02788(17) Uani 1 1 d . . . S1 S 0.00562(7) 0.65168(5) 0.41615(4) 0.03066(17) Uani 1 1 d . . . S2 S 0.20730(6) 0.44904(5) 0.47757(4) 0.02628(15) Uani 1 1 d . . . S3 S 0.01852(7) 0.44424(6) 0.38059(4) 0.02817(16) Uani 1 1 d . . . S4 S 0.29361(6) 0.04485(5) 0.01465(4) 0.02736(16) Uani 1 1 d . . . S5 S 0.50194(7) -0.15484(5) 0.07676(4) 0.03068(17) Uani 1 1 d . . . S6 S 0.46356(7) 0.05282(6) 0.12323(4) 0.03080(17) Uani 1 1 d . . . O1 O 0.1550(2) 0.52921(17) 0.32460(11) 0.0328(5) Uani 1 1 d . . . O2 O 0.3371(2) -0.06605(18) 0.16113(12) 0.0412(6) Uani 1 1 d . . . C1 C -0.2801(3) 0.3130(3) 0.53377(17) 0.0364(7) Uani 1 1 d . . . H1A H -0.2115 0.3061 0.5499 0.044 Uiso 1 1 calc R . . C2 C -0.3468(3) 0.2804(3) 0.57813(19) 0.0433(9) Uani 1 1 d . . . H2A H -0.3229 0.2508 0.6244 0.052 Uiso 1 1 calc R . . C3 C -0.4465(3) 0.2908(3) 0.5558(2) 0.0403(8) Uani 1 1 d . . . H3A H -0.4913 0.2682 0.5864 0.048 Uiso 1 1 calc R . . C4 C -0.4818(3) 0.3344(3) 0.4884(2) 0.0383(8) Uani 1 1 d . . . H4A H -0.5515 0.3430 0.4729 0.046 Uiso 1 1 calc R . . C5 C -0.4143(3) 0.3654(2) 0.44357(18) 0.0341(7) Uani 1 1 d . . . H5A H -0.4378 0.3938 0.3971 0.041 Uiso 1 1 calc R . . C6 C -0.3145(3) 0.3558(2) 0.46539(16) 0.0294(6) Uani 1 1 d . . . C7 C -0.2920(3) 0.4746(2) 0.33796(16) 0.0296(7) Uani 1 1 d . . . C8 C -0.2451(3) 0.4785(3) 0.27259(17) 0.0342(7) Uani 1 1 d . . . H8A H -0.1753 0.4321 0.2660 0.041 Uiso 1 1 calc R . . C9 C -0.2990(3) 0.5489(3) 0.21752(17) 0.0380(8) Uani 1 1 d . . . H9A H -0.2661 0.5503 0.1736 0.046 Uiso 1 1 calc R . . C10 C -0.4007(3) 0.6173(3) 0.22637(18) 0.0393(8) Uani 1 1 d . . . H10A H -0.4385 0.6647 0.1883 0.047 Uiso 1 1 calc R . . C11 C -0.4467(3) 0.6161(3) 0.29100(19) 0.0401(8) Uani 1 1 d . . . H11A H -0.5157 0.6637 0.2974 0.048 Uiso 1 1 calc R . . C12 C -0.3926(3) 0.5454(2) 0.34709(18) 0.0379(8) Uani 1 1 d . . . H12A H -0.4244 0.5458 0.3914 0.046 Uiso 1 1 calc R . . C13 C -0.1444(3) 0.2810(2) 0.37400(15) 0.0287(6) Uani 1 1 d . . . C14 C -0.0337(3) 0.2330(2) 0.38355(16) 0.0306(7) Uani 1 1 d . . . H14A H 0.0062 0.2562 0.4068 0.037 Uiso 1 1 calc R . . C15 C 0.0212(3) 0.1496(2) 0.35916(17) 0.0349(7) Uani 1 1 d . . . H15A H 0.0979 0.1164 0.3660 0.042 Uiso 1 1 calc R . . C16 C -0.0370(3) 0.1163(2) 0.32524(16) 0.0356(7) Uani 1 1 d . . . H16A H -0.0002 0.0602 0.3084 0.043 Uiso 1 1 calc R . . C17 C -0.1489(3) 0.1644(3) 0.31567(18) 0.0372(8) Uani 1 1 d . . . H17A H -0.1885 0.1410 0.2923 0.045 Uiso 1 1 calc R . . C18 C -0.2038(3) 0.2465(3) 0.33994(18) 0.0359(7) Uani 1 1 d . . . H18A H -0.2807 0.2790 0.3336 0.043 Uiso 1 1 calc R . . C19 C 0.2246(3) 0.1052(2) 0.49213(15) 0.0284(6) Uani 1 1 d . . . C20 C 0.2918(3) 0.0355(2) 0.45679(19) 0.0368(7) Uani 1 1 d . . . H20A H 0.3511 0.0421 0.4308 0.044 Uiso 1 1 calc R . . C21 C 0.2714(4) -0.0435(3) 0.4599(2) 0.0467(9) Uani 1 1 d . . . H21A H 0.3172 -0.0910 0.4362 0.056 Uiso 1 1 calc R . . C22 C 0.1850(4) -0.0536(3) 0.4971(2) 0.0513(11) Uani 1 1 d . . . H22A H 0.1723 -0.1081 0.4995 0.062 Uiso 1 1 calc R . . C23 C 0.1166(4) 0.0162(3) 0.5310(2) 0.0498(10) Uani 1 1 d . . . H23A H 0.0564 0.0098 0.5558 0.060 Uiso 1 1 calc R . . C24 C 0.1364(3) 0.0955(3) 0.52855(16) 0.0365(8) Uani 1 1 d . . . H24A H 0.0896 0.1431 0.5518 0.044 Uiso 1 1 calc R . . C25 C 0.3240(3) 0.1733(2) 0.57711(15) 0.0276(6) Uani 1 1 d . . . C26 C 0.4009(3) 0.0824(2) 0.60020(17) 0.0322(7) Uani 1 1 d . . . H26A H 0.4183 0.0375 0.5716 0.039 Uiso 1 1 calc R . . C27 C 0.4522(3) 0.0571(3) 0.66450(18) 0.0400(8) Uani 1 1 d . . . H27A H 0.5046 -0.0045 0.6798 0.048 Uiso 1 1 calc R . . C28 C 0.4258(3) 0.1233(3) 0.70643(17) 0.0411(8) Uani 1 1 d . . . H28A H 0.4605 0.1063 0.7505 0.049 Uiso 1 1 calc R . . C29 C 0.3503(3) 0.2127(3) 0.68448(17) 0.0360(7) Uani 1 1 d . . . H29A H 0.3332 0.2570 0.7135 0.043 Uiso 1 1 calc R . . C30 C 0.2987(3) 0.2388(2) 0.61995(16) 0.0301(7) Uani 1 1 d . . . H30A H 0.2466 0.3007 0.6050 0.036 Uiso 1 1 calc R . . C31 C 0.3484(3) 0.2078(2) 0.42752(15) 0.0289(6) Uani 1 1 d . . . C32 C 0.4608(3) 0.1688(2) 0.43850(17) 0.0331(7) Uani 1 1 d . . . H32A H 0.4899 0.1401 0.4839 0.040 Uiso 1 1 calc R . . C33 C 0.5316(3) 0.1710(3) 0.38414(18) 0.0370(8) Uani 1 1 d . . . H33A H 0.6083 0.1438 0.3925 0.044 Uiso 1 1 calc R . . C34 C 0.4897(3) 0.2131(3) 0.31775(18) 0.0402(8) Uani 1 1 d . . . H34A H 0.5377 0.2143 0.2804 0.048 Uiso 1 1 calc R . . C35 C 0.3778(4) 0.2534(3) 0.30599(19) 0.0465(9) Uani 1 1 d . . . H35A H 0.3493 0.2822 0.2604 0.056 Uiso 1 1 calc R . . C36 C 0.3063(3) 0.2522(3) 0.36061(17) 0.0389(8) Uani 1 1 d . . . H36A H 0.2296 0.2813 0.3523 0.047 Uiso 1 1 calc R . . C37 C 0.2370(3) 0.5629(3) 0.29422(17) 0.0339(7) Uani 1 1 d . . . C38 C 0.2469(3) 0.5429(3) 0.22216(18) 0.0415(8) Uani 1 1 d . . . H38A H 0.2761 0.4755 0.2247 0.062 Uiso 1 1 calc R . . H38B H 0.2962 0.5679 0.1957 0.062 Uiso 1 1 calc R . . H38C H 0.1747 0.5724 0.1994 0.062 Uiso 1 1 calc R . . C39 C 0.3432(3) 0.5104(3) 0.33436(19) 0.0440(9) Uani 1 1 d . . . H39A H 0.3684 0.4438 0.3347 0.066 Uiso 1 1 calc R . . H39B H 0.3324 0.5209 0.3819 0.066 Uiso 1 1 calc R . . H39C H 0.3980 0.5324 0.3127 0.066 Uiso 1 1 calc R . . C40 C 0.1924(4) 0.6679(3) 0.2903(2) 0.0449(9) Uani 1 1 d . . . H40A H 0.1236 0.6984 0.2636 0.067 Uiso 1 1 calc R . . H40B H 0.2455 0.6914 0.2678 0.067 Uiso 1 1 calc R . . H40C H 0.1795 0.6811 0.3371 0.067 Uiso 1 1 calc R . . C41 C 0.2756(3) 0.3942(2) 0.00584(15) 0.0281(6) Uani 1 1 d . . . C42 C 0.3678(3) 0.3969(2) -0.02949(16) 0.0328(7) Uani 1 1 d . . . H42A H 0.4136 0.3460 -0.0500 0.039 Uiso 1 1 calc R . . C43 C 0.3934(4) 0.4740(3) -0.03502(18) 0.0431(9) Uani 1 1 d . . . H43A H 0.4563 0.4754 -0.0592 0.052 Uiso 1 1 calc R . . C44 C 0.3268(4) 0.5485(3) -0.0051(2) 0.0449(9) Uani 1 1 d . . . H44A H 0.3434 0.6015 -0.0098 0.054 Uiso 1 1 calc R . . C45 C 0.2361(3) 0.5459(2) 0.0315(2) 0.0407(8) Uani 1 1 d . . . H45A H 0.1917 0.5964 0.0529 0.049 Uiso 1 1 calc R . . C46 C 0.2100(3) 0.4685(2) 0.03683(17) 0.0343(7) Uani 1 1 d . . . H46A H 0.1476 0.4669 0.0616 0.041 Uiso 1 1 calc R . . C47 C 0.1451(3) 0.3007(2) 0.07542(15) 0.0302(7) Uani 1 1 d . . . C48 C 0.0346(3) 0.3259(2) 0.06465(17) 0.0325(7) Uani 1 1 d . . . H48A H 0.0059 0.3436 0.0188 0.039 Uiso 1 1 calc R . . C49 C -0.0349(3) 0.3256(2) 0.12006(19) 0.0374(8) Uani 1 1 d . . . H49A H -0.1104 0.3430 0.1119 0.045 Uiso 1 1 calc R . . C50 C 0.0062(3) 0.2999(3) 0.18676(19) 0.0423(9) Uani 1 1 d . . . H50A H -0.0409 0.2992 0.2246 0.051 Uiso 1 1 calc R . . C51 C 0.1157(3) 0.2753(3) 0.19827(18) 0.0448(9) Uani 1 1 d . . . H51A H 0.1437 0.2583 0.2442 0.054 Uiso 1 1 calc R . . C52 C 0.1854(3) 0.2752(3) 0.14335(17) 0.0393(8) Uani 1 1 d . . . H52A H 0.2609 0.2576 0.1519 0.047 Uiso 1 1 calc R . . C53 C 0.1666(3) 0.3285(2) -0.07495(15) 0.0282(6) Uani 1 1 d . . . C54 C 0.0880(3) 0.4197(2) -0.09691(17) 0.0329(7) Uani 1 1 d . . . H54A H 0.0706 0.4639 -0.0679 0.039 Uiso 1 1 calc R . . C55 C 0.0362(3) 0.4450(3) -0.16049(18) 0.0396(8) Uani 1 1 d . . . H55A H -0.0171 0.5065 -0.1751 0.048 Uiso 1 1 calc R . . C56 C 0.0623(3) 0.3800(3) -0.20331(17) 0.0399(8) Uani 1 1 d . . . H56A H 0.0271 0.3978 -0.2473 0.048 Uiso 1 1 calc R . . C57 C 0.1385(3) 0.2905(3) -0.18230(17) 0.0356(7) Uani 1 1 d . . . H57A H 0.1553 0.2466 -0.2116 0.043 Uiso 1 1 calc R . . C58 C 0.1915(3) 0.2641(2) -0.11783(16) 0.0294(6) Uani 1 1 d . . . H58A H 0.2443 0.2024 -0.1034 0.035 Uiso 1 1 calc R . . C59 C 0.7964(3) 0.1516(2) 0.03021(15) 0.0287(6) Uani 1 1 d . . . C60 C 0.8985(3) 0.1434(2) 0.04956(18) 0.0354(7) Uani 1 1 d . . . H60A H 0.9241 0.1173 0.0960 0.042 Uiso 1 1 calc R . . C61 C 0.9633(3) 0.1730(3) 0.00137(19) 0.0379(8) Uani 1 1 d . . . H61A H 1.0336 0.1657 0.0147 0.046 Uiso 1 1 calc R . . C62 C 0.9257(3) 0.2129(3) -0.06588(19) 0.0397(8) Uani 1 1 d . . . H62A H 0.9693 0.2344 -0.0984 0.048 Uiso 1 1 calc R . . C63 C 0.8248(4) 0.2215(3) -0.08554(18) 0.0420(9) Uani 1 1 d . . . H63A H 0.7989 0.2489 -0.1318 0.050 Uiso 1 1 calc R . . C64 C 0.7605(3) 0.1902(2) -0.03802(16) 0.0350(7) Uani 1 1 d . . . H64A H 0.6917 0.1952 -0.0522 0.042 Uiso 1 1 calc R . . C65 C 0.7835(3) 0.0344(2) 0.16092(16) 0.0288(6) Uani 1 1 d . . . C66 C 0.7412(3) 0.0305(2) 0.22726(16) 0.0325(7) Uani 1 1 d . . . H66A H 0.6717 0.0763 0.2352 0.039 Uiso 1 1 calc R . . C67 C 0.7990(3) -0.0392(2) 0.28191(17) 0.0361(7) Uani 1 1 d . . . H67A H 0.7690 -0.0407 0.3267 0.043 Uiso 1 1 calc R . . C68 C 0.9004(3) -0.1065(3) 0.27105(18) 0.0403(8) Uani 1 1 d . . . H68A H 0.9411 -0.1535 0.3085 0.048 Uiso 1 1 calc R . . C69 C 0.9419(3) -0.1046(3) 0.20507(18) 0.0410(8) Uani 1 1 d . . . H69A H 1.0107 -0.1514 0.1973 0.049 Uiso 1 1 calc R . . C70 C 0.8844(3) -0.0353(2) 0.15001(18) 0.0382(8) Uani 1 1 d . . . H70A H 0.9137 -0.0354 0.1050 0.046 Uiso 1 1 calc R . . C71 C 0.6358(3) 0.2269(2) 0.12706(15) 0.0277(6) Uani 1 1 d . . . C72 C 0.5244(3) 0.2752(2) 0.12036(16) 0.0308(7) Uani 1 1 d . . . H72A H 0.4825 0.2522 0.0987 0.037 Uiso 1 1 calc R . . C73 C 0.4719(3) 0.3584(2) 0.14531(16) 0.0342(7) Uani 1 1 d . . . H73A H 0.3950 0.3919 0.1401 0.041 Uiso 1 1 calc R . . C74 C 0.5332(3) 0.3911(2) 0.17751(16) 0.0352(7) Uani 1 1 d . . . H74A H 0.4982 0.4468 0.1950 0.042 Uiso 1 1 calc R . . C75 C 0.6450(3) 0.3428(3) 0.18421(17) 0.0364(8) Uani 1 1 d . . . H75A H 0.6868 0.3657 0.2062 0.044 Uiso 1 1 calc R . . C76 C 0.6969(3) 0.2614(2) 0.15924(17) 0.0336(7) Uani 1 1 d . . . H76A H 0.7740 0.2287 0.1639 0.040 Uiso 1 1 calc R . . C77 C 0.2438(3) -0.0237(3) 0.20277(17) 0.0410(9) Uani 1 1 d . . . C78 C 0.2768(4) 0.0217(4) 0.2520(2) 0.0649(13) Uani 1 1 d . . . H78A H 0.3402 -0.0248 0.2799 0.097 Uiso 1 1 calc R . . H78B H 0.2159 0.0476 0.2823 0.097 Uiso 1 1 calc R . . H78C H 0.2956 0.0718 0.2256 0.097 Uiso 1 1 calc R . . C79 C 0.1459(4) 0.0437(4) 0.1583(2) 0.0597(12) Uani 1 1 d . . . H79A H 0.1270 0.0110 0.1279 0.090 Uiso 1 1 calc R . . H79B H 0.1631 0.0938 0.1303 0.090 Uiso 1 1 calc R . . H79C H 0.0840 0.0702 0.1878 0.090 Uiso 1 1 calc R . . C80 C 0.2208(5) -0.1034(4) 0.2414(3) 0.0746(17) Uani 1 1 d . . . H80A H 0.1987 -0.1316 0.2088 0.112 Uiso 1 1 calc R . . H80B H 0.1618 -0.0813 0.2738 0.112 Uiso 1 1 calc R . . H80C H 0.2867 -0.1499 0.2671 0.112 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 Cu1 0.0279(2) 0.02600(19) 0.02699(18) -0.00088(14) -0.00023(15) -0.00963(17) Cu2 0.0314(2) 0.0388(2) 0.0363(2) -0.01344(18) 0.00572(17) -0.0193(2) Cu3 0.0305(2) 0.02527(19) 0.02805(18) -0.00126(15) -0.00249(16) -0.00891(17) Cu4 0.0354(2) 0.0344(2) 0.0332(2) -0.00782(16) 0.00012(17) -0.0180(2) P1 0.0245(4) 0.0250(4) 0.0233(3) -0.0012(3) -0.0005(3) -0.0104(3) P2 0.0274(4) 0.0298(4) 0.0262(3) -0.0053(3) 0.0035(3) -0.0142(4) P3 0.0252(4) 0.0280(4) 0.0232(3) -0.0003(3) 0.0012(3) -0.0112(3) P4 0.0253(4) 0.0248(4) 0.0231(3) -0.0010(3) -0.0010(3) -0.0105(3) P5 0.0295(4) 0.0280(4) 0.0240(3) -0.0035(3) 0.0007(3) -0.0132(4) P6 0.0258(4) 0.0292(4) 0.0238(3) 0.0012(3) 0.0020(3) -0.0095(4) S1 0.0293(4) 0.0260(4) 0.0320(4) -0.0005(3) 0.0043(3) -0.0093(3) S2 0.0241(4) 0.0270(4) 0.0257(3) -0.0007(3) -0.0009(3) -0.0102(3) S3 0.0298(4) 0.0318(4) 0.0240(3) -0.0034(3) 0.0007(3) -0.0146(3) S4 0.0246(4) 0.0268(4) 0.0277(3) 0.0010(3) -0.0009(3) -0.0101(3) S5 0.0287(4) 0.0259(4) 0.0329(4) 0.0008(3) 0.0005(3) -0.0095(3) S6 0.0351(5) 0.0305(4) 0.0248(3) -0.0049(3) -0.0021(3) -0.0111(4) O1 0.0286(13) 0.0388(12) 0.0268(10) 0.0011(9) 0.0002(9) -0.0128(11) O2 0.0376(15) 0.0438(14) 0.0331(12) 0.0059(11) 0.0049(11) -0.0143(12) C1 0.038(2) 0.0435(19) 0.0305(15) -0.0073(14) 0.0033(14) -0.0197(17) C2 0.051(2) 0.048(2) 0.0335(17) -0.0049(15) 0.0081(16) -0.025(2) C3 0.042(2) 0.0374(18) 0.0462(19) -0.0107(15) 0.0161(17) -0.0215(17) C4 0.0293(19) 0.0380(18) 0.0486(19) -0.0091(16) 0.0067(16) -0.0151(16) C5 0.0297(18) 0.0358(17) 0.0376(16) -0.0043(14) 0.0025(14) -0.0156(16) C6 0.0314(18) 0.0310(15) 0.0281(14) -0.0070(12) 0.0044(13) -0.0150(14) C7 0.0354(19) 0.0307(15) 0.0272(14) -0.0047(12) 0.0052(13) -0.0188(15) C8 0.0315(19) 0.0384(17) 0.0310(15) -0.0025(13) 0.0029(14) -0.0148(16) C9 0.045(2) 0.0417(19) 0.0288(15) -0.0027(14) 0.0037(15) -0.0209(18) C10 0.049(2) 0.0347(17) 0.0345(16) 0.0019(14) -0.0026(15) -0.0213(18) C11 0.037(2) 0.0318(17) 0.0418(18) 0.0008(14) -0.0004(16) -0.0080(16) C12 0.041(2) 0.0348(17) 0.0356(16) -0.0061(14) 0.0062(15) -0.0144(17) C13 0.0306(18) 0.0293(15) 0.0249(13) -0.0034(12) 0.0020(12) -0.0120(14) C14 0.0288(18) 0.0323(16) 0.0294(14) -0.0048(12) -0.0007(13) -0.0116(15) C15 0.034(2) 0.0326(17) 0.0308(15) -0.0037(13) -0.0008(14) -0.0068(15) C16 0.044(2) 0.0322(16) 0.0282(14) -0.0056(13) 0.0056(14) -0.0142(16) C17 0.043(2) 0.0382(18) 0.0355(16) -0.0088(14) -0.0012(15) -0.0208(18) C18 0.034(2) 0.0414(19) 0.0366(16) -0.0088(15) 0.0023(14) -0.0188(17) C19 0.0277(18) 0.0254(14) 0.0285(14) 0.0030(11) -0.0084(12) -0.0098(14) C20 0.035(2) 0.0313(17) 0.0444(18) -0.0078(14) -0.0056(15) -0.0125(16) C21 0.048(3) 0.0278(17) 0.059(2) -0.0060(16) -0.0216(19) -0.0082(18) C22 0.074(3) 0.039(2) 0.050(2) 0.0089(17) -0.022(2) -0.036(2) C23 0.071(3) 0.056(2) 0.0377(18) 0.0065(17) -0.0060(18) -0.048(2) C24 0.047(2) 0.0439(19) 0.0246(14) 0.0008(13) 0.0005(14) -0.0280(18) C25 0.0251(16) 0.0319(15) 0.0257(13) 0.0001(12) -0.0012(12) -0.0139(14) C26 0.0314(19) 0.0287(15) 0.0331(15) -0.0013(13) -0.0013(14) -0.0107(15) C27 0.037(2) 0.0386(19) 0.0373(17) 0.0067(15) -0.0091(15) -0.0136(18) C28 0.041(2) 0.055(2) 0.0272(15) 0.0015(15) -0.0060(14) -0.023(2) C29 0.037(2) 0.047(2) 0.0280(15) -0.0046(14) 0.0002(14) -0.0227(18) C30 0.0309(18) 0.0334(16) 0.0263(14) -0.0034(12) 0.0011(12) -0.0145(15) C31 0.0326(18) 0.0296(15) 0.0261(14) -0.0038(12) 0.0008(13) -0.0150(15) C32 0.0324(19) 0.0359(17) 0.0308(15) -0.0039(13) 0.0045(14) -0.0154(16) C33 0.0305(19) 0.0376(18) 0.0401(17) -0.0064(15) 0.0078(15) -0.0126(16) C34 0.043(2) 0.0400(19) 0.0349(16) -0.0027(15) 0.0108(16) -0.0175(18) C35 0.047(2) 0.053(2) 0.0303(16) 0.0000(16) 0.0057(16) -0.015(2) C36 0.035(2) 0.048(2) 0.0246(14) 0.0018(14) 0.0024(14) -0.0123(17) C37 0.0298(18) 0.0400(18) 0.0301(15) -0.0016(13) 0.0047(13) -0.0156(16) C38 0.041(2) 0.052(2) 0.0322(16) -0.0076(16) 0.0079(15) -0.0218(19) C39 0.040(2) 0.059(2) 0.0353(17) 0.0015(16) 0.0029(16) -0.027(2) C40 0.055(3) 0.042(2) 0.0393(18) 0.0002(16) 0.0054(17) -0.026(2) C41 0.0286(18) 0.0298(15) 0.0240(13) 0.0015(11) -0.0052(12) -0.0120(14) C42 0.040(2) 0.0346(17) 0.0257(14) 0.0000(12) 0.0006(13) -0.0200(16) C43 0.055(3) 0.050(2) 0.0326(16) 0.0038(15) -0.0050(16) -0.034(2) C44 0.061(3) 0.0348(19) 0.0439(19) 0.0064(15) -0.0175(18) -0.028(2) C45 0.047(2) 0.0250(16) 0.0447(19) -0.0037(14) -0.0143(17) -0.0091(17) C46 0.035(2) 0.0296(16) 0.0367(16) -0.0032(13) -0.0087(14) -0.0118(16) C47 0.0351(19) 0.0308(15) 0.0253(14) -0.0025(12) 0.0011(13) -0.0155(15) C48 0.0307(18) 0.0346(16) 0.0319(15) -0.0046(13) 0.0030(13) -0.0141(15) C49 0.031(2) 0.0368(18) 0.0415(18) -0.0047(15) 0.0073(15) -0.0137(16) C50 0.045(2) 0.043(2) 0.0355(17) -0.0027(15) 0.0108(16) -0.0184(19) C51 0.046(2) 0.057(2) 0.0276(15) -0.0013(16) 0.0048(16) -0.022(2) C52 0.034(2) 0.051(2) 0.0291(15) -0.0021(15) 0.0020(14) -0.0166(18) C53 0.0272(17) 0.0302(15) 0.0260(13) 0.0003(12) -0.0013(12) -0.0130(14) C54 0.0296(19) 0.0309(16) 0.0335(15) 0.0000(13) -0.0032(13) -0.0100(15) C55 0.036(2) 0.0383(19) 0.0375(17) 0.0077(15) -0.0100(15) -0.0135(17) C56 0.036(2) 0.055(2) 0.0284(15) 0.0055(15) -0.0062(14) -0.0223(19) C57 0.039(2) 0.0456(19) 0.0277(15) -0.0051(14) 0.0002(14) -0.0231(18) C58 0.0275(17) 0.0324(16) 0.0269(14) -0.0022(12) 0.0010(12) -0.0124(14) C59 0.0330(18) 0.0271(14) 0.0251(13) -0.0050(11) 0.0047(13) -0.0120(14) C60 0.033(2) 0.0376(18) 0.0352(16) -0.0057(14) 0.0009(14) -0.0148(16) C61 0.033(2) 0.0370(18) 0.0440(18) -0.0099(15) 0.0090(16) -0.0149(16) C62 0.046(2) 0.0373(18) 0.0401(18) -0.0097(15) 0.0164(16) -0.0224(18) C63 0.056(3) 0.043(2) 0.0291(16) -0.0022(14) 0.0071(16) -0.0247(19) C64 0.040(2) 0.0411(18) 0.0267(14) -0.0047(13) 0.0027(14) -0.0201(17) C65 0.0328(18) 0.0273(15) 0.0274(14) -0.0035(12) 0.0026(13) -0.0144(14) C66 0.0305(19) 0.0375(17) 0.0272(14) -0.0029(13) 0.0027(13) -0.0132(15) C67 0.038(2) 0.0376(18) 0.0291(15) 0.0014(13) -0.0004(14) -0.0147(17) C68 0.046(2) 0.0386(19) 0.0345(17) -0.0004(14) -0.0032(16) -0.0186(18) C69 0.041(2) 0.0350(18) 0.0360(17) 0.0000(14) 0.0012(16) -0.0073(17) C70 0.042(2) 0.0342(17) 0.0320(16) -0.0048(13) 0.0032(15) -0.0104(17) C71 0.0296(17) 0.0290(15) 0.0234(13) -0.0039(11) 0.0017(12) -0.0115(14) C72 0.0312(19) 0.0307(16) 0.0277(14) -0.0014(12) -0.0041(13) -0.0111(15) C73 0.0325(19) 0.0321(16) 0.0299(15) -0.0013(13) 0.0001(14) -0.0071(15) C74 0.044(2) 0.0307(16) 0.0287(15) -0.0038(13) 0.0029(14) -0.0137(16) C75 0.045(2) 0.0383(18) 0.0329(16) -0.0073(14) 0.0016(15) -0.0236(18) C76 0.0322(19) 0.0356(17) 0.0356(16) -0.0071(14) 0.0008(14) -0.0163(16) C77 0.036(2) 0.060(2) 0.0273(15) -0.0057(16) 0.0086(14) -0.0221(19) C78 0.058(3) 0.089(4) 0.053(2) -0.029(3) 0.011(2) -0.029(3) C79 0.034(2) 0.088(3) 0.041(2) -0.010(2) 0.0023(18) -0.009(2) C80 0.079(4) 0.059(3) 0.075(3) 0.000(3) 0.035(3) -0.028(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 Cu1 P1 2.2467(10) . ? Cu1 S1 2.3147(9) 2_566 ? Cu1 S3 2.4426(11) . ? Cu1 S2 2.4651(9) . ? Cu1 Cu2 2.7268(9) . ? Cu2 P2 2.2264(9) . ? Cu2 S3 2.2739(9) . ? Cu2 S2 2.3095(10) 2_566 ? Cu2 S1 2.7390(12) 2_566 ? Cu3 P4 2.2383(10) . ? Cu3 S5 2.3089(9) 2_655 ? Cu3 S4 2.4213(9) . ? Cu3 S6 2.4487(11) . ? Cu3 Cu4 2.6769(9) . ? Cu4 P5 2.2295(9) . ? Cu4 S6 2.2964(10) . ? Cu4 S4 2.3498(10) 2_655 ? Cu4 S5 2.6549(11) 2_655 ? P1 C31 1.830(3) . ? P1 C25 1.831(3) . ? P1 C19 1.833(3) . ? P2 C7 1.825(4) . ? P2 C6 1.830(3) . ? P2 C13 1.837(3) . ? P3 O1 1.601(2) . ? P3 S1 2.0302(12) . ? P3 S2 2.0304(13) . ? P3 S3 2.0416(11) . ? P4 C41 1.831(3) . ? P4 C47 1.834(3) . ? P4 C53 1.836(3) . ? P5 C65 1.823(3) . ? P5 C59 1.831(3) . ? P5 C71 1.833(3) . ? P6 O2 1.597(2) . ? P6 S5 2.0250(12) . ? P6 S4 2.0333(13) . ? P6 S6 2.0388(12) . ? S1 Cu1 2.3147(9) 2_566 ? S1 Cu2 2.7389(12) 2_566 ? S2 Cu2 2.3096(10) 2_566 ? S4 Cu4 2.3498(10) 2_655 ? S5 Cu3 2.3090(9) 2_655 ? S5 Cu4 2.6550(11) 2_655 ? O1 C37 1.462(4) . ? O2 C77 1.452(4) . ? C1 C2 1.392(5) . ? C1 C6 1.399(5) . ? C2 C3 1.371(6) . ? C3 C4 1.387(6) . ? C4 C5 1.393(4) . ? C5 C6 1.372(5) . ? C7 C12 1.394(5) . ? C7 C8 1.403(4) . ? C8 C9 1.385(5) . ? C9 C10 1.385(6) . ? C10 C11 1.384(5) . ? C11 C12 1.401(5) . ? C13 C14 1.370(5) . ? C13 C18 1.407(5) . ? C14 C15 1.406(5) . ? C15 C16 1.379(5) . ? C16 C17 1.385(6) . ? C17 C18 1.388(5) . ? C19 C24 1.393(4) . ? C19 C20 1.402(5) . ? C20 C21 1.393(5) . ? C21 C22 1.380(6) . ? C22 C23 1.389(7) . ? C23 C24 1.395(5) . ? C25 C26 1.401(5) . ? C25 C30 1.405(4) . ? C26 C27 1.389(5) . ? C27 C28 1.398(5) . ? C28 C29 1.374(6) . ? C29 C30 1.394(5) . ? C31 C32 1.389(5) . ? C31 C36 1.400(5) . ? C32 C33 1.393(4) . ? C33 C34 1.386(5) . ? C34 C35 1.384(6) . ? C35 C36 1.401(5) . ? C37 C39 1.504(6) . ? C37 C38 1.510(5) . ? C37 C40 1.526(5) . ? C41 C42 1.393(4) . ? C41 C46 1.394(5) . ? C42 C43 1.395(5) . ? C43 C44 1.388(6) . ? C44 C45 1.386(6) . ? C45 C46 1.406(5) . ? C47 C48 1.387(5) . ? C47 C52 1.398(5) . ? C48 C49 1.393(4) . ? C49 C50 1.379(6) . ? C50 C51 1.379(6) . ? C51 C52 1.387(5) . ? C53 C58 1.392(4) . ? C53 C54 1.407(5) . ? C54 C55 1.380(5) . ? C55 C56 1.396(5) . ? C56 C57 1.376(6) . ? C57 C58 1.401(5) . ? C59 C60 1.392(5) . ? C59 C64 1.392(5) . ? C60 C61 1.393(5) . ? C61 C62 1.382(6) . ? C62 C63 1.378(6) . ? C63 C64 1.392(4) . ? C65 C66 1.396(4) . ? C65 C70 1.398(5) . ? C66 C67 1.388(5) . ? C67 C68 1.386(5) . ? C68 C69 1.385(5) . ? C69 C70 1.389(5) . ? C71 C72 1.374(5) . ? C71 C76 1.402(4) . ? C72 C73 1.405(5) . ? C73 C74 1.383(5) . ? C74 C75 1.380(5) . ? C75 C76 1.382(5) . ? C77 C80 1.487(6) . ? C77 C79 1.506(6) . ? C77 C78 1.511(6) . ? 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 P1 Cu1 S1 111.87(4) . 2_566 ? P1 Cu1 S3 121.66(3) . . ? S1 Cu1 S3 116.49(4) 2_566 . ? P1 Cu1 S2 99.75(4) . . ? S1 Cu1 S2 118.17(3) 2_566 . ? S3 Cu1 S2 84.80(3) . . ? P1 Cu1 Cu2 141.83(3) . . ? S1 Cu1 Cu2 65.22(3) 2_566 . ? S3 Cu1 Cu2 51.84(3) . . ? S2 Cu1 Cu2 115.29(3) . . ? P2 Cu2 S3 105.87(3) . . ? P2 Cu2 S2 114.05(4) . 2_566 ? S3 Cu2 S2 125.52(3) . 2_566 ? P2 Cu2 Cu1 127.31(3) . . ? S3 Cu2 Cu1 57.63(3) . . ? S2 Cu2 Cu1 114.88(3) 2_566 . ? P2 Cu2 S1 121.99(3) . 2_566 ? S3 Cu2 S1 107.26(3) . 2_566 ? S2 Cu2 S1 81.62(3) 2_566 2_566 ? Cu1 Cu2 S1 50.11(2) . 2_566 ? P4 Cu3 S5 109.50(4) . 2_655 ? P4 Cu3 S4 106.48(4) . . ? S5 Cu3 S4 115.13(3) 2_655 . ? P4 Cu3 S6 122.05(3) . . ? S5 Cu3 S6 116.08(4) 2_655 . ? S4 Cu3 S6 84.95(3) . . ? P4 Cu3 Cu4 137.10(3) . . ? S5 Cu3 Cu4 63.85(3) 2_655 . ? S4 Cu3 Cu4 114.56(3) . . ? S6 Cu3 Cu4 53.01(3) . . ? P5 Cu4 S6 112.05(3) . . ? P5 Cu4 S4 106.68(4) . 2_655 ? S6 Cu4 S4 124.67(3) . 2_655 ? P5 Cu4 S5 119.03(3) . 2_655 ? S6 Cu4 S5 109.03(4) . 2_655 ? S4 Cu4 S5 83.27(3) 2_655 2_655 ? P5 Cu4 Cu3 130.70(3) . . ? S6 Cu4 Cu3 58.39(3) . . ? S4 Cu4 Cu3 117.66(3) 2_655 . ? S5 Cu4 Cu3 51.32(3) 2_655 . ? C31 P1 C25 105.83(15) . . ? C31 P1 C19 102.93(14) . . ? C25 P1 C19 101.29(14) . . ? C31 P1 Cu1 114.00(11) . . ? C25 P1 Cu1 110.60(11) . . ? C19 P1 Cu1 120.56(11) . . ? C7 P2 C6 105.80(15) . . ? C7 P2 C13 103.98(14) . . ? C6 P2 C13 101.16(14) . . ? C7 P2 Cu2 109.49(10) . . ? C6 P2 Cu2 117.37(11) . . ? C13 P2 Cu2 117.61(12) . . ? O1 P3 S1 110.12(10) . . ? O1 P3 S2 113.32(10) . . ? S1 P3 S2 109.47(5) . . ? O1 P3 S3 97.72(10) . . ? S1 P3 S3 117.19(5) . . ? S2 P3 S3 108.73(5) . . ? C41 P4 C47 102.96(14) . . ? C41 P4 C53 101.48(14) . . ? C47 P4 C53 106.01(15) . . ? C41 P4 Cu3 120.31(11) . . ? C47 P4 Cu3 114.06(11) . . ? C53 P4 Cu3 110.46(11) . . ? C65 P5 C59 105.75(15) . . ? C65 P5 C71 103.51(14) . . ? C59 P5 C71 101.58(14) . . ? C65 P5 Cu4 109.71(10) . . ? C59 P5 Cu4 116.46(11) . . ? C71 P5 Cu4 118.38(11) . . ? O2 P6 S5 98.63(11) . . ? O2 P6 S4 112.56(11) . . ? S5 P6 S4 110.41(5) . . ? O2 P6 S6 110.46(11) . . ? S5 P6 S6 116.98(6) . . ? S4 P6 S6 107.73(5) . . ? P3 S1 Cu1 113.44(4) . 2_566 ? P3 S1 Cu2 77.96(4) . 2_566 ? Cu1 S1 Cu2 64.67(3) 2_566 2_566 ? P3 S2 Cu2 89.07(4) . 2_566 ? P3 S2 Cu1 82.22(4) . . ? Cu2 S2 Cu1 105.07(3) 2_566 . ? P3 S3 Cu2 114.60(4) . . ? P3 S3 Cu1 82.57(4) . . ? Cu2 S3 Cu1 70.54(3) . . ? P6 S4 Cu4 86.36(4) . 2_655 ? P6 S4 Cu3 83.18(4) . . ? Cu4 S4 Cu3 106.76(3) 2_655 . ? P6 S5 Cu3 116.38(4) . 2_655 ? P6 S5 Cu4 78.74(4) . 2_655 ? Cu3 S5 Cu4 64.83(3) 2_655 2_655 ? P6 S6 Cu4 111.84(4) . . ? P6 S6 Cu3 82.38(4) . . ? Cu4 S6 Cu3 68.60(3) . . ? C37 O1 P3 135.9(2) . . ? C77 O2 P6 136.0(2) . . ? C2 C1 C6 119.8(4) . . ? C3 C2 C1 120.7(4) . . ? C2 C3 C4 119.8(3) . . ? C3 C4 C5 119.5(4) . . ? C6 C5 C4 121.2(3) . . ? C5 C6 C1 118.9(3) . . ? C5 C6 P2 125.7(3) . . ? C1 C6 P2 115.2(3) . . ? C12 C7 C8 118.4(3) . . ? C12 C7 P2 121.4(2) . . ? C8 C7 P2 119.8(3) . . ? C9 C8 C7 121.0(3) . . ? C10 C9 C8 120.2(3) . . ? C11 C10 C9 119.5(3) . . ? C10 C11 C12 120.7(4) . . ? C7 C12 C11 120.0(3) . . ? C14 C13 C18 119.8(3) . . ? C14 C13 P2 119.1(2) . . ? C18 C13 P2 121.0(3) . . ? C13 C14 C15 120.4(3) . . ? C16 C15 C14 119.7(4) . . ? C15 C16 C17 120.1(3) . . ? C16 C17 C18 120.5(3) . . ? C17 C18 C13 119.4(4) . . ? C24 C19 C20 119.4(3) . . ? C24 C19 P1 117.2(3) . . ? C20 C19 P1 123.4(2) . . ? C21 C20 C19 119.8(4) . . ? C22 C21 C20 120.6(4) . . ? C21 C22 C23 120.0(3) . . ? C22 C23 C24 120.1(4) . . ? C19 C24 C23 120.2(4) . . ? C26 C25 C30 119.2(3) . . ? C26 C25 P1 122.6(2) . . ? C30 C25 P1 118.1(3) . . ? C27 C26 C25 120.6(3) . . ? C26 C27 C28 119.4(3) . . ? C29 C28 C27 120.6(3) . . ? C28 C29 C30 120.4(3) . . ? C29 C30 C25 119.8(3) . . ? C32 C31 C36 118.8(3) . . ? C32 C31 P1 124.8(2) . . ? C36 C31 P1 116.4(3) . . ? C31 C32 C33 121.2(3) . . ? C34 C33 C32 119.8(4) . . ? C35 C34 C33 119.8(3) . . ? C34 C35 C36 120.6(4) . . ? C31 C36 C35 119.8(4) . . ? O1 C37 C39 110.3(3) . . ? O1 C37 C38 102.8(3) . . ? C39 C37 C38 111.6(3) . . ? O1 C37 C40 109.1(3) . . ? C39 C37 C40 113.0(3) . . ? C38 C37 C40 109.5(3) . . ? C42 C41 C46 119.4(3) . . ? C42 C41 P4 117.3(2) . . ? C46 C41 P4 123.2(2) . . ? C41 C42 C43 120.5(3) . . ? C44 C43 C42 119.9(4) . . ? C45 C44 C43 120.3(3) . . ? C44 C45 C46 119.9(3) . . ? C41 C46 C45 120.0(3) . . ? C48 C47 C52 118.5(3) . . ? C48 C47 P4 124.5(2) . . ? C52 C47 P4 117.0(3) . . ? C47 C48 C49 121.0(3) . . ? C50 C49 C48 119.9(4) . . ? C49 C50 C51 119.8(3) . . ? C50 C51 C52 120.6(4) . . ? C51 C52 C47 120.3(4) . . ? C58 C53 C54 119.4(3) . . ? C58 C53 P4 118.3(3) . . ? C54 C53 P4 122.1(2) . . ? C55 C54 C53 120.2(3) . . ? C54 C55 C56 119.9(4) . . ? C57 C56 C55 120.5(3) . . ? C56 C57 C58 120.1(3) . . ? C53 C58 C57 119.9(3) . . ? C60 C59 C64 118.8(3) . . ? C60 C59 P5 124.6(2) . . ? C64 C59 P5 116.5(3) . . ? C59 C60 C61 120.5(3) . . ? C62 C61 C60 120.2(4) . . ? C63 C62 C61 119.8(3) . . ? C62 C63 C64 120.3(3) . . ? C59 C64 C63 120.4(3) . . ? C66 C65 C70 118.5(3) . . ? C66 C65 P5 119.5(3) . . ? C70 C65 P5 121.7(2) . . ? C67 C66 C65 121.2(3) . . ? C68 C67 C66 120.0(3) . . ? C69 C68 C67 119.3(4) . . ? C68 C69 C70 121.1(4) . . ? C69 C70 C65 119.9(3) . . ? C72 C71 C76 119.3(3) . . ? C72 C71 P5 118.6(2) . . ? C76 C71 P5 122.1(3) . . ? C71 C72 C73 120.6(3) . . ? C74 C73 C72 119.5(3) . . ? C75 C74 C73 120.1(3) . . ? C74 C75 C76 120.5(3) . . ? C75 C76 C71 120.0(3) . . ? O2 C77 C80 104.2(3) . . ? O2 C77 C79 111.4(3) . . ? C80 C77 C79 109.6(4) . . ? O2 C77 C78 108.4(3) . . ? C80 C77 C78 110.5(4) . . ? C79 C77 C78 112.4(4) . . ? _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 1.387 _refine_diff_density_min -0.949 _refine_diff_density_rms 0.090 data_1a _database_code_depnum_ccdc_archive 'CCDC 601693' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H78 Cu4 O2 P6 S6' _chemical_formula_weight 1703.76 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' P P 0.1023 0.0942 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8442(10) _cell_length_b 13.4796(12) _cell_length_c 13.6857(12) _cell_angle_alpha 101.538(7) _cell_angle_beta 101.470(7) _cell_angle_gamma 109.779(6) _cell_volume 1928.5(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 14268 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 28 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 876 _exptl_absorpt_coefficient_mu 1.421 _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 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'stoe ipds 2' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16967 _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_sigmaI/netI 0.0708 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 28.16 _reflns_number_total 8709 _reflns_number_gt 6235 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'stoe winexpose' _computing_cell_refinement 'stoe winexpose' _computing_data_reduction 'stoe winexpose' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0596P)^2^+1.1404P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8709 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0806 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1323 _refine_ls_wR_factor_gt 0.1197 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 O1 O -0.1968(3) 0.3203(3) 0.1508(3) 0.0438(8) Uani 1 1 d . . . Cu1 Cu 0.02607(6) 0.67255(4) 0.10596(4) 0.03549(14) Uani 1 1 d . . . Cu2 Cu 0.14442(5) 0.54135(4) 0.15966(4) 0.02954(12) Uani 1 1 d . . . P1 P -0.12062(10) 0.38067(9) 0.08132(8) 0.0264(2) Uani 1 1 d . . . P2 P 0.03201(10) 0.82810(8) 0.20540(7) 0.0262(2) Uani 1 1 d . . . P3 P 0.28862(9) 0.54175(8) 0.29437(7) 0.02393(19) Uani 1 1 d . . . S1 S -0.05958(10) 0.53667(9) 0.17747(7) 0.0299(2) Uani 1 1 d . . . S2 S 0.03075(9) 0.34355(8) 0.07091(7) 0.02493(19) Uani 1 1 d . . . S3 S 0.23393(10) 0.65312(9) 0.06381(8) 0.0326(2) Uani 1 1 d . . . C1 C -0.2558(5) 0.2081(4) 0.1540(4) 0.0419(11) Uani 1 1 d . . . C2 C -0.3685(7) 0.1468(6) 0.0521(5) 0.0683(17) Uani 1 1 d . . . H2A H -0.4250 0.1858 0.0489 0.102 Uiso 1 1 calc R . . H2B H -0.4142 0.0713 0.0525 0.102 Uiso 1 1 calc R . . H2C H -0.3367 0.1452 -0.0088 0.102 Uiso 1 1 calc R . . C3 C -0.1638(7) 0.1539(6) 0.1644(6) 0.072(2) Uani 1 1 d . . . H3A H -0.0960 0.1950 0.2294 0.108 Uiso 1 1 calc R . . H3B H -0.1289 0.1534 0.1052 0.108 Uiso 1 1 calc R . . H3C H -0.2066 0.0781 0.1655 0.108 Uiso 1 1 calc R . . C4 C -0.3088(6) 0.2174(5) 0.2437(5) 0.0575(15) Uani 1 1 d . . . H4A H -0.2403 0.2553 0.3087 0.086 Uiso 1 1 calc R . . H4B H -0.3593 0.1436 0.2453 0.086 Uiso 1 1 calc R . . H4C H -0.3616 0.2594 0.2361 0.086 Uiso 1 1 calc R . . C5 C 0.1185(4) 0.9573(3) 0.1796(3) 0.0293(8) Uani 1 1 d . . . C6 C 0.2302(5) 0.9642(4) 0.1572(4) 0.0390(10) Uani 1 1 d . . . H6A H 0.2526 0.9024 0.1498 0.047 Uiso 1 1 calc R . . C7 C 0.3096(5) 1.0630(5) 0.1456(4) 0.0499(12) Uani 1 1 d . . . H7A H 0.3865 1.0685 0.1315 0.060 Uiso 1 1 calc R . . C8 C 0.2757(5) 1.1515(4) 0.1547(4) 0.0463(12) Uani 1 1 d . . . H8A H 0.3297 1.2183 0.1474 0.056 Uiso 1 1 calc R . . C9 C 0.1631(5) 1.1439(4) 0.1746(4) 0.0446(11) Uani 1 1 d . . . H9A H 0.1387 1.2045 0.1785 0.053 Uiso 1 1 calc R . . C10 C 0.0861(5) 1.0472(4) 0.1888(3) 0.0371(9) Uani 1 1 d . . . H10A H 0.0106 1.0430 0.2049 0.044 Uiso 1 1 calc R . . C11 C -0.1286(4) 0.8203(3) 0.1900(3) 0.0284(8) Uani 1 1 d . . . C12 C -0.1897(4) 0.8487(4) 0.1090(4) 0.0414(10) Uani 1 1 d . . . H12A H -0.1464 0.8775 0.0629 0.050 Uiso 1 1 calc R . . C13 C -0.3141(5) 0.8351(5) 0.0955(4) 0.0466(11) Uani 1 1 d . . . H13A H -0.3543 0.8570 0.0415 0.056 Uiso 1 1 calc R . . C14 C -0.3806(5) 0.7900(4) 0.1597(4) 0.0431(11) Uani 1 1 d . . . H14A H -0.4656 0.7809 0.1499 0.052 Uiso 1 1 calc R . . C15 C -0.3214(5) 0.7585(4) 0.2379(4) 0.0439(11) Uani 1 1 d . . . H15A H -0.3663 0.7265 0.2817 0.053 Uiso 1 1 calc R . . C16 C -0.1958(5) 0.7734(4) 0.2534(3) 0.0368(10) Uani 1 1 d . . . H16A H -0.1560 0.7513 0.3075 0.044 Uiso 1 1 calc R . . C17 C 0.0974(4) 0.8642(3) 0.3472(3) 0.0266(7) Uani 1 1 d . . . C18 C 0.0988(5) 0.9578(4) 0.4143(3) 0.0352(9) Uani 1 1 d . . . H18A H 0.0621 1.0029 0.3871 0.042 Uiso 1 1 calc R . . C19 C 0.1535(5) 0.9848(4) 0.5204(3) 0.0414(10) Uani 1 1 d . . . H19A H 0.1535 1.0481 0.5658 0.050 Uiso 1 1 calc R . . C20 C 0.2082(4) 0.9203(4) 0.5608(3) 0.0393(10) Uani 1 1 d . . . H20A H 0.2459 0.9393 0.6337 0.047 Uiso 1 1 calc R . . C21 C 0.2077(4) 0.8282(4) 0.4950(3) 0.0372(10) Uani 1 1 d . . . H21A H 0.2454 0.7839 0.5226 0.045 Uiso 1 1 calc R . . C22 C 0.1525(4) 0.7999(4) 0.3885(3) 0.0325(9) Uani 1 1 d . . . H22A H 0.1523 0.7362 0.3436 0.039 Uiso 1 1 calc R . . C23 C 0.3876(4) 0.6703(4) 0.3969(3) 0.0300(8) Uani 1 1 d . . . C24 C 0.4278(5) 0.7664(4) 0.3665(4) 0.0392(10) Uani 1 1 d . . . H24A H 0.3994 0.7640 0.2957 0.047 Uiso 1 1 calc R . . C25 C 0.5100(5) 0.8658(4) 0.4402(5) 0.0532(14) Uani 1 1 d . . . H25A H 0.5381 0.9308 0.4192 0.064 Uiso 1 1 calc R . . C26 C 0.5506(5) 0.8704(5) 0.5431(5) 0.0578(15) Uani 1 1 d . . . H26A H 0.6071 0.9385 0.5925 0.069 Uiso 1 1 calc R . . C27 C 0.5100(5) 0.7774(5) 0.5751(4) 0.0539(15) Uani 1 1 d . . . H27A H 0.5377 0.7815 0.6464 0.065 Uiso 1 1 calc R . . C28 C 0.4279(4) 0.6763(4) 0.5025(3) 0.0391(10) Uani 1 1 d . . . H28A H 0.3996 0.6121 0.5246 0.047 Uiso 1 1 calc R . . C29 C 0.2241(4) 0.4475(3) 0.3671(3) 0.0297(8) Uani 1 1 d . . . C30 C 0.2677(4) 0.3687(4) 0.3898(3) 0.0348(9) Uani 1 1 d . . . H30A H 0.3374 0.3631 0.3684 0.042 Uiso 1 1 calc R . . C31 C 0.2109(5) 0.2973(4) 0.4435(4) 0.0435(11) Uani 1 1 d . . . H31A H 0.2413 0.2433 0.4579 0.052 Uiso 1 1 calc R . . C32 C 0.1104(5) 0.3059(5) 0.4755(4) 0.0494(12) Uani 1 1 d . . . H32A H 0.0729 0.2593 0.5138 0.059 Uiso 1 1 calc R . . C33 C 0.0640(5) 0.3825(5) 0.4519(5) 0.0573(15) Uani 1 1 d . . . H33A H -0.0060 0.3873 0.4732 0.069 Uiso 1 1 calc R . . C34 C 0.1193(5) 0.4523(5) 0.3972(5) 0.0517(14) Uani 1 1 d . . . H34A H 0.0857 0.5035 0.3801 0.062 Uiso 1 1 calc R . . C35 C 0.4064(4) 0.4997(3) 0.2500(3) 0.0275(8) Uani 1 1 d . . . C36 C 0.5185(4) 0.5132(4) 0.3181(4) 0.0369(9) Uani 1 1 d . . . H36A H 0.5339 0.5410 0.3911 0.044 Uiso 1 1 calc R . . C37 C 0.6085(5) 0.4861(5) 0.2799(5) 0.0481(12) Uani 1 1 d . . . H37A H 0.6843 0.4946 0.3268 0.058 Uiso 1 1 calc R . . C38 C 0.5867(5) 0.4465(4) 0.1729(4) 0.0457(12) Uani 1 1 d . . . H38A H 0.6482 0.4289 0.1467 0.055 Uiso 1 1 calc R . . C39 C 0.4762(5) 0.4328(4) 0.1051(4) 0.0418(11) Uani 1 1 d . . . H39A H 0.4617 0.4053 0.0322 0.050 Uiso 1 1 calc R . . C40 C 0.3851(4) 0.4590(3) 0.1424(3) 0.0320(9) Uani 1 1 d . . . H40A H 0.3090 0.4492 0.0951 0.038 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 O1 0.039(2) 0.0460(19) 0.066(2) 0.0338(18) 0.0301(17) 0.0219(18) Cu1 0.0496(4) 0.0303(3) 0.0262(2) 0.0046(2) 0.0106(2) 0.0176(3) Cu2 0.0248(3) 0.0350(3) 0.0274(2) 0.0075(2) 0.00462(19) 0.0127(2) P1 0.0232(5) 0.0306(5) 0.0317(5) 0.0156(4) 0.0111(4) 0.0126(5) P2 0.0306(6) 0.0259(5) 0.0228(4) 0.0068(4) 0.0089(4) 0.0114(5) P3 0.0214(5) 0.0272(5) 0.0229(4) 0.0066(4) 0.0058(4) 0.0100(4) S1 0.0314(5) 0.0372(5) 0.0268(4) 0.0096(4) 0.0129(4) 0.0177(5) S2 0.0233(5) 0.0277(5) 0.0271(4) 0.0105(4) 0.0074(4) 0.0126(4) S3 0.0250(5) 0.0345(5) 0.0346(5) 0.0127(4) 0.0029(4) 0.0090(5) C1 0.050(3) 0.038(2) 0.053(3) 0.025(2) 0.033(2) 0.018(2) C2 0.062(4) 0.057(4) 0.066(4) 0.011(3) 0.020(3) 0.003(4) C3 0.087(5) 0.068(4) 0.117(6) 0.064(4) 0.070(5) 0.055(4) C4 0.068(4) 0.063(4) 0.059(3) 0.034(3) 0.035(3) 0.029(3) C5 0.033(2) 0.029(2) 0.0229(17) 0.0084(15) 0.0062(16) 0.0094(19) C6 0.040(3) 0.041(2) 0.041(2) 0.016(2) 0.021(2) 0.016(2) C7 0.047(3) 0.055(3) 0.048(3) 0.020(2) 0.023(2) 0.012(3) C8 0.055(3) 0.036(2) 0.035(2) 0.0165(19) 0.008(2) 0.002(3) C9 0.059(3) 0.032(2) 0.041(2) 0.017(2) 0.008(2) 0.015(3) C10 0.042(3) 0.034(2) 0.038(2) 0.0152(18) 0.011(2) 0.017(2) C11 0.032(2) 0.0254(19) 0.0233(17) 0.0028(14) 0.0063(16) 0.0090(19) C12 0.028(2) 0.056(3) 0.035(2) 0.018(2) 0.0060(19) 0.010(2) C13 0.035(3) 0.058(3) 0.041(2) 0.017(2) 0.002(2) 0.015(3) C14 0.033(3) 0.052(3) 0.042(2) 0.011(2) 0.012(2) 0.016(3) C15 0.037(3) 0.049(3) 0.049(3) 0.019(2) 0.020(2) 0.013(3) C16 0.043(3) 0.040(2) 0.033(2) 0.0149(18) 0.0150(19) 0.018(2) C17 0.024(2) 0.0264(18) 0.0253(17) 0.0079(15) 0.0065(15) 0.0056(18) C18 0.044(3) 0.033(2) 0.0287(19) 0.0067(16) 0.0087(18) 0.018(2) C19 0.043(3) 0.040(2) 0.032(2) -0.0024(18) 0.0118(19) 0.012(2) C20 0.035(3) 0.049(3) 0.0247(19) 0.0076(18) 0.0076(18) 0.009(2) C21 0.033(2) 0.050(3) 0.032(2) 0.0165(19) 0.0089(18) 0.019(2) C22 0.032(2) 0.041(2) 0.0273(19) 0.0095(17) 0.0092(17) 0.018(2) C23 0.019(2) 0.035(2) 0.0321(19) 0.0042(16) 0.0051(15) 0.0108(19) C24 0.037(3) 0.039(2) 0.041(2) 0.0081(19) 0.018(2) 0.012(2) C25 0.041(3) 0.035(3) 0.072(4) 0.001(2) 0.026(3) 0.004(3) C26 0.028(3) 0.050(3) 0.065(3) -0.018(3) 0.005(2) 0.003(3) C27 0.039(3) 0.067(4) 0.041(3) -0.013(2) -0.004(2) 0.027(3) C28 0.039(3) 0.043(3) 0.033(2) 0.0028(18) 0.0015(18) 0.022(2) C29 0.028(2) 0.031(2) 0.0278(18) 0.0097(16) 0.0073(16) 0.0094(19) C30 0.037(2) 0.034(2) 0.037(2) 0.0148(18) 0.0123(19) 0.015(2) C31 0.044(3) 0.040(3) 0.045(3) 0.020(2) 0.009(2) 0.012(3) C32 0.044(3) 0.057(3) 0.046(3) 0.027(2) 0.015(2) 0.011(3) C33 0.045(3) 0.076(4) 0.072(4) 0.043(3) 0.032(3) 0.029(3) C34 0.046(3) 0.065(4) 0.069(3) 0.037(3) 0.033(3) 0.033(3) C35 0.027(2) 0.0244(18) 0.0301(19) 0.0077(15) 0.0091(16) 0.0085(18) C36 0.029(2) 0.041(2) 0.040(2) 0.0112(19) 0.0079(18) 0.016(2) C37 0.030(3) 0.049(3) 0.071(3) 0.020(3) 0.015(2) 0.021(3) C38 0.044(3) 0.043(3) 0.070(3) 0.023(2) 0.037(3) 0.025(3) C39 0.051(3) 0.039(2) 0.048(3) 0.017(2) 0.031(2) 0.021(2) C40 0.034(2) 0.031(2) 0.035(2) 0.0101(17) 0.0148(18) 0.014(2) _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 O1 C1 1.449(5) . ? O1 P1 1.592(3) . ? Cu1 P2 2.2303(11) . ? Cu1 S1 2.2794(12) . ? Cu1 S2 2.3243(10) 2_565 ? Cu1 S3 2.7210(12) . ? Cu1 Cu2 2.7241(7) . ? Cu2 P3 2.2479(11) . ? Cu2 S3 2.3190(12) . ? Cu2 S2 2.4538(12) . ? Cu2 S1 2.4574(11) . ? P1 S3 2.0292(15) 2_565 ? P1 S1 2.0400(15) . ? P1 S2 2.0410(13) . ? P2 C11 1.836(4) . ? P2 C17 1.836(4) . ? P2 C5 1.841(4) . ? P3 C29 1.828(4) . ? P3 C23 1.829(4) . ? P3 C35 1.836(4) . ? S2 Cu1 2.3243(10) 2_565 ? S3 P1 2.0292(15) 2_565 ? C1 C4 1.487(6) . ? C1 C3 1.504(7) . ? C1 C2 1.569(9) . ? C5 C10 1.379(6) . ? C5 C6 1.394(6) . ? C6 C7 1.407(7) . ? C7 C8 1.372(7) . ? C8 C9 1.388(8) . ? C9 C10 1.391(6) . ? C11 C16 1.392(6) . ? C11 C12 1.393(6) . ? C12 C13 1.391(7) . ? C13 C14 1.387(7) . ? C14 C15 1.379(7) . ? C15 C16 1.398(7) . ? C17 C22 1.389(5) . ? C17 C18 1.397(5) . ? C18 C19 1.384(6) . ? C19 C20 1.383(7) . ? C20 C21 1.377(6) . ? C21 C22 1.388(6) . ? C23 C24 1.398(6) . ? C23 C28 1.405(6) . ? C24 C25 1.395(7) . ? C25 C26 1.376(9) . ? C26 C27 1.375(9) . ? C27 C28 1.402(7) . ? C29 C30 1.390(5) . ? C29 C34 1.400(6) . ? C30 C31 1.401(6) . ? C31 C32 1.380(7) . ? C32 C33 1.384(7) . ? C33 C34 1.391(7) . ? C35 C36 1.393(6) . ? C35 C40 1.403(5) . ? C36 C37 1.397(6) . ? C37 C38 1.393(8) . ? C38 C39 1.376(7) . ? C39 C40 1.399(5) . ? 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 C1 O1 P1 136.9(3) . . ? P2 Cu1 S1 106.78(4) . . ? P2 Cu1 S2 112.97(4) . 2_565 ? S1 Cu1 S2 124.25(4) . 2_565 ? P2 Cu1 S3 122.34(5) . . ? S1 Cu1 S3 107.86(4) . . ? S2 Cu1 S3 82.06(3) 2_565 . ? P2 Cu1 Cu2 128.46(4) . . ? S1 Cu1 Cu2 58.02(3) . . ? S2 Cu1 Cu2 115.14(3) 2_565 . ? S3 Cu1 Cu2 50.41(3) . . ? P3 Cu2 S3 112.20(4) . . ? P3 Cu2 S2 101.71(4) . . ? S3 Cu2 S2 117.60(4) . . ? P3 Cu2 S1 120.59(4) . . ? S3 Cu2 S1 115.95(4) . . ? S2 Cu2 S1 85.12(4) . . ? P3 Cu2 Cu1 139.36(4) . . ? S3 Cu2 Cu1 64.72(3) . . ? S2 Cu2 Cu1 115.64(3) . . ? S1 Cu2 Cu1 51.89(3) . . ? O1 P1 S3 110.95(15) . 2_565 ? O1 P1 S1 96.34(14) . . ? S3 P1 S1 117.06(6) 2_565 . ? O1 P1 S2 113.52(12) . . ? S3 P1 S2 109.58(6) 2_565 . ? S1 P1 S2 108.98(6) . . ? C11 P2 C17 103.09(17) . . ? C11 P2 C5 105.87(18) . . ? C17 P2 C5 101.10(18) . . ? C11 P2 Cu1 109.20(13) . . ? C17 P2 Cu1 118.79(13) . . ? C5 P2 Cu1 117.22(12) . . ? C29 P3 C23 103.05(19) . . ? C29 P3 C35 105.67(17) . . ? C23 P3 C35 101.52(18) . . ? C29 P3 Cu2 113.96(14) . . ? C23 P3 Cu2 119.88(13) . . ? C35 P3 Cu2 111.18(13) . . ? P1 S1 Cu1 114.55(5) . . ? P1 S1 Cu2 82.12(4) . . ? Cu1 S1 Cu2 70.10(3) . . ? P1 S2 Cu1 88.31(5) . 2_565 ? P1 S2 Cu2 82.19(5) . . ? Cu1 S2 Cu2 105.92(4) 2_565 . ? P1 S3 Cu2 113.70(6) 2_565 . ? P1 S3 Cu1 78.33(4) 2_565 . ? Cu2 S3 Cu1 64.86(3) . . ? O1 C1 C4 105.1(4) . . ? O1 C1 C3 111.3(4) . . ? C4 C1 C3 113.0(5) . . ? O1 C1 C2 106.5(4) . . ? C4 C1 C2 107.6(5) . . ? C3 C1 C2 112.8(5) . . ? C10 C5 C6 119.5(4) . . ? C10 C5 P2 125.3(3) . . ? C6 C5 P2 114.9(3) . . ? C5 C6 C7 119.8(4) . . ? C8 C7 C6 119.9(5) . . ? C7 C8 C9 120.4(5) . . ? C8 C9 C10 119.8(4) . . ? C5 C10 C9 120.6(4) . . ? C16 C11 C12 118.9(4) . . ? C16 C11 P2 119.2(3) . . ? C12 C11 P2 121.5(3) . . ? C13 C12 C11 120.0(4) . . ? C14 C13 C12 121.1(5) . . ? C15 C14 C13 119.0(4) . . ? C14 C15 C16 120.6(4) . . ? C11 C16 C15 120.4(4) . . ? C22 C17 C18 119.0(4) . . ? C22 C17 P2 119.2(3) . . ? C18 C17 P2 121.7(3) . . ? C19 C18 C17 120.0(4) . . ? C20 C19 C18 120.5(4) . . ? C21 C20 C19 119.7(4) . . ? C20 C21 C22 120.3(4) . . ? C21 C22 C17 120.4(4) . . ? C24 C23 C28 119.1(4) . . ? C24 C23 P3 117.2(3) . . ? C28 C23 P3 123.6(3) . . ? C25 C24 C23 119.8(5) . . ? C26 C25 C24 120.5(5) . . ? C27 C26 C25 120.5(5) . . ? C26 C27 C28 120.1(5) . . ? C27 C28 C23 119.9(5) . . ? C30 C29 C34 118.3(4) . . ? C30 C29 P3 124.7(3) . . ? C34 C29 P3 116.9(3) . . ? C29 C30 C31 121.3(4) . . ? C32 C31 C30 119.4(4) . . ? C31 C32 C33 120.2(4) . . ? C32 C33 C34 120.4(5) . . ? C33 C34 C29 120.4(5) . . ? C36 C35 C40 119.2(4) . . ? C36 C35 P3 122.7(3) . . ? C40 C35 P3 117.9(3) . . ? C35 C36 C37 120.5(4) . . ? C38 C37 C36 119.8(5) . . ? C39 C38 C37 120.1(4) . . ? C38 C39 C40 120.6(4) . . ? C39 C40 C35 119.8(4) . . ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 1.491 _refine_diff_density_min -0.655 _refine_diff_density_rms 0.093 data_2 _database_code_depnum_ccdc_archive 'CCDC 601694' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H46 Cu O P3 S3' _chemical_formula_weight 879.47 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' P P 0.1023 0.0942 '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' Cu Cu 0.3201 1.2651 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4902(4) _cell_length_b 13.0272(5) _cell_length_c 15.6664(5) _cell_angle_alpha 74.107(3) _cell_angle_beta 71.686(3) _cell_angle_gamma 83.651(3) _cell_volume 2140.38(13) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 5 _cell_measurement_theta_max 50 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.365 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 916 _exptl_absorpt_coefficient_mu 0.804 _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 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'stoe stadi 4' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17126 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0251 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 31.79 _reflns_number_total 9353 _reflns_number_gt 8249 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'kuma ccd' _computing_cell_refinement 'kuma ccd' _computing_data_reduction 'kuma ccd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1053P)^2^+0.1311P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9353 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1452 _refine_ls_wR_factor_gt 0.1265 _refine_ls_goodness_of_fit_ref 1.146 _refine_ls_restrained_S_all 1.146 _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 O1 O 0.90275(16) 0.71523(14) 0.28796(11) 0.0346(4) Uani 1 1 d . . . Cu1 Cu 0.41934(2) 0.745667(18) 0.783574(15) 0.02004(10) Uani 1 1 d . . . P1 P 0.64060(4) 0.84018(4) 0.63897(3) 0.01920(12) Uani 1 1 d . . . P2 P 0.31401(4) 0.83233(4) 0.89339(3) 0.01911(13) Uani 1 1 d . . . P3 P 0.34909(5) 0.59784(4) 0.76831(3) 0.01965(13) Uani 1 1 d . . . S1 S 0.47023(4) 0.89256(4) 0.64221(3) 0.02316(13) Uani 1 1 d . . . S2 S 0.64369(5) 0.71749(4) 0.74768(3) 0.02425(13) Uani 1 1 d . . . S3 S 0.75711(5) 0.94595(4) 0.65063(3) 0.02465(13) Uani 1 1 d . . . C1 C 0.71737(18) 0.80634(16) 0.52977(13) 0.0210(4) Uani 1 1 d . . . C2 C 0.66409(19) 0.82853(17) 0.45870(14) 0.0252(4) Uani 1 1 d . . . H2A H 0.5859 0.8637 0.4667 0.030 Uiso 1 1 calc R . . C3 C 0.7227(2) 0.80043(18) 0.37586(14) 0.0278(4) Uani 1 1 d . . . H3A H 0.6854 0.8167 0.3274 0.033 Uiso 1 1 calc R . . C4 C 0.8361(2) 0.74839(17) 0.36472(14) 0.0257(4) Uani 1 1 d . . . C5 C 0.8911(2) 0.72664(18) 0.43554(15) 0.0284(4) Uani 1 1 d . . . H5A H 0.9693 0.6914 0.4276 0.034 Uiso 1 1 calc R . . C6 C 0.83302(19) 0.75575(18) 0.51684(15) 0.0259(4) Uani 1 1 d . . . H6A H 0.8716 0.7414 0.5645 0.031 Uiso 1 1 calc R . . C8 C 0.7669(2) 1.07372(18) 0.55911(16) 0.0290(5) Uani 1 1 d . . . C9 C 0.6431(3) 1.1240(2) 0.5625(3) 0.0573(9) Uani 1 1 d . . . H9A H 0.6512 1.1910 0.5138 0.086 Uiso 1 1 calc R . . H9B H 0.6044 1.1387 0.6234 0.086 Uiso 1 1 calc R . . H9C H 0.5924 1.0754 0.5524 0.086 Uiso 1 1 calc R . . C10 C 0.8414(3) 1.1431(2) 0.5855(2) 0.0466(7) Uani 1 1 d . . . H10A H 0.8517 1.2134 0.5411 0.070 Uiso 1 1 calc R . . H10B H 0.9221 1.1090 0.5844 0.070 Uiso 1 1 calc R . . H10C H 0.7984 1.1515 0.6481 0.070 Uiso 1 1 calc R . . C11 C 0.8345(4) 1.0578(3) 0.4630(2) 0.0629(10) Uani 1 1 d . . . H11A H 0.8381 1.1262 0.4164 0.094 Uiso 1 1 calc R . . H11B H 0.7910 1.0065 0.4494 0.094 Uiso 1 1 calc R . . H11C H 0.9180 1.0305 0.4611 0.094 Uiso 1 1 calc R . . C12 C 0.16703(18) 0.88134(16) 0.87312(14) 0.0220(4) Uani 1 1 d . . . C13 C 0.05534(19) 0.83987(18) 0.93329(15) 0.0277(4) Uani 1 1 d . . . H13A H 0.0527 0.7895 0.9906 0.033 Uiso 1 1 calc R . . C14 C -0.0520(2) 0.8721(2) 0.90963(17) 0.0325(5) Uani 1 1 d . . . H14A H -0.1278 0.8436 0.9510 0.039 Uiso 1 1 calc R . . C15 C -0.0498(2) 0.94517(19) 0.82663(17) 0.0326(5) Uani 1 1 d . . . H15A H -0.1237 0.9665 0.8108 0.039 Uiso 1 1 calc R . . C16 C 0.0610(2) 0.98743(18) 0.76630(16) 0.0308(5) Uani 1 1 d . . . H16A H 0.0631 1.0382 0.7093 0.037 Uiso 1 1 calc R . . C17 C 0.1684(2) 0.95506(17) 0.78986(15) 0.0266(4) Uani 1 1 d . . . H17A H 0.2441 0.9838 0.7484 0.032 Uiso 1 1 calc R . . C18 C 0.38272(19) 0.95410(16) 0.88921(13) 0.0215(4) Uani 1 1 d . . . C19 C 0.3143(2) 1.04390(18) 0.90988(16) 0.0273(4) Uani 1 1 d . . . H19A H 0.2274 1.0443 0.9255 0.033 Uiso 1 1 calc R . . C20 C 0.3724(2) 1.13282(18) 0.90776(16) 0.0310(5) Uani 1 1 d . . . H20A H 0.3250 1.1938 0.9219 0.037 Uiso 1 1 calc R . . C21 C 0.4985(2) 1.13336(19) 0.88524(16) 0.0319(5) Uani 1 1 d . . . H21A H 0.5381 1.1943 0.8840 0.038 Uiso 1 1 calc R . . C22 C 0.5668(2) 1.0441(2) 0.86447(17) 0.0335(5) Uani 1 1 d . . . H22A H 0.6537 1.0439 0.8490 0.040 Uiso 1 1 calc R . . C23 C 0.50931(19) 0.95508(17) 0.86609(15) 0.0266(4) Uani 1 1 d . . . H23A H 0.5570 0.8945 0.8513 0.032 Uiso 1 1 calc R . . C24 C 0.26997(18) 0.76392(17) 1.01663(14) 0.0224(4) Uani 1 1 d . . . C25 C 0.2147(2) 0.81737(19) 1.08592(15) 0.0285(5) Uani 1 1 d . . . H25A H 0.1987 0.8922 1.0694 0.034 Uiso 1 1 calc R . . C26 C 0.1831(2) 0.7619(2) 1.17850(15) 0.0332(5) Uani 1 1 d . . . H26A H 0.1450 0.7989 1.2252 0.040 Uiso 1 1 calc R . . C27 C 0.2064(2) 0.6531(2) 1.20375(16) 0.0368(5) Uani 1 1 d . . . H27A H 0.1858 0.6155 1.2675 0.044 Uiso 1 1 calc R . . C28 C 0.2595(2) 0.5999(2) 1.13590(17) 0.0383(5) Uani 1 1 d . . . H28A H 0.2744 0.5250 1.1528 0.046 Uiso 1 1 calc R . . C29 C 0.2917(2) 0.65477(19) 1.04290(15) 0.0317(5) Uani 1 1 d . . . H29A H 0.3290 0.6171 0.9966 0.038 Uiso 1 1 calc R . . C30 C 0.45936(19) 0.52694(17) 0.69089(14) 0.0238(4) Uani 1 1 d . . . C31 C 0.4810(2) 0.4170(2) 0.71407(17) 0.0365(5) Uani 1 1 d . . . H31A H 0.4358 0.3744 0.7725 0.044 Uiso 1 1 calc R . . C32 C 0.5683(3) 0.3700(2) 0.65178(19) 0.0479(7) Uani 1 1 d . . . H32A H 0.5831 0.2950 0.6678 0.057 Uiso 1 1 calc R . . C33 C 0.6345(3) 0.4312(2) 0.5664(2) 0.0450(6) Uani 1 1 d . . . H33A H 0.6956 0.3985 0.5245 0.054 Uiso 1 1 calc R . . C34 C 0.6114(2) 0.5401(2) 0.54232(18) 0.0412(6) Uani 1 1 d . . . H34A H 0.6550 0.5822 0.4831 0.049 Uiso 1 1 calc R . . C35 C 0.5247(2) 0.58793(19) 0.60459(16) 0.0321(5) Uani 1 1 d . . . H35A H 0.5099 0.6629 0.5882 0.039 Uiso 1 1 calc R . . C36 C 0.21201(19) 0.61053(16) 0.73074(13) 0.0223(4) Uani 1 1 d . . . C37 C 0.1280(2) 0.69252(17) 0.74779(15) 0.0271(4) Uani 1 1 d . . . H37A H 0.1472 0.7462 0.7715 0.032 Uiso 1 1 calc R . . C38 C 0.0160(2) 0.69719(19) 0.73061(16) 0.0322(5) Uani 1 1 d . . . H38A H -0.0410 0.7540 0.7425 0.039 Uiso 1 1 calc R . . C39 C -0.0128(2) 0.6198(2) 0.69636(17) 0.0359(5) Uani 1 1 d . . . H39A H -0.0909 0.6213 0.6871 0.043 Uiso 1 1 calc R . . C40 C 0.0728(3) 0.5398(2) 0.6756(2) 0.0423(6) Uani 1 1 d . . . H40A H 0.0544 0.4878 0.6498 0.051 Uiso 1 1 calc R . . C41 C 0.1846(2) 0.53518(19) 0.69215(18) 0.0341(5) Uani 1 1 d . . . H41A H 0.2431 0.4804 0.6772 0.041 Uiso 1 1 calc R . . C42 C 0.30582(19) 0.49639(16) 0.87852(14) 0.0218(4) Uani 1 1 d . . . C43 C 0.1859(2) 0.46630(18) 0.92549(15) 0.0278(4) Uani 1 1 d . . . H43A H 0.1227 0.4951 0.8979 0.033 Uiso 1 1 calc R . . C44 C 0.1572(2) 0.3947(2) 1.01215(16) 0.0343(5) Uani 1 1 d . . . H44A H 0.0743 0.3758 1.0440 0.041 Uiso 1 1 calc R . . C45 C 0.2481(2) 0.35042(19) 1.05266(16) 0.0335(5) Uani 1 1 d . . . H45A H 0.2281 0.3005 1.1118 0.040 Uiso 1 1 calc R . . C46 C 0.3682(2) 0.37932(19) 1.00658(16) 0.0310(5) Uani 1 1 d . . . H46A H 0.4312 0.3493 1.0340 0.037 Uiso 1 1 calc R . . C47 C 0.3970(2) 0.45214(18) 0.92036(15) 0.0269(4) Uani 1 1 d . . . H47A H 0.4797 0.4722 0.8893 0.032 Uiso 1 1 calc R . . C7 C 0.8577(3) 0.7426(2) 0.20984(17) 0.0435(6) Uani 1 1 d . . . H7A H 0.9142 0.7141 0.1598 0.065 Uiso 1 1 calc R . . H7B H 0.8510 0.8205 0.1884 0.065 Uiso 1 1 calc R . . H7C H 0.7766 0.7122 0.2274 0.065 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 O1 0.0367(9) 0.0392(9) 0.0249(8) -0.0128(7) -0.0013(7) -0.0005(7) Cu1 0.01870(15) 0.01978(15) 0.01820(16) -0.00420(11) -0.00081(11) -0.00187(10) P1 0.0149(2) 0.0241(3) 0.0155(2) -0.00101(19) -0.00373(19) -0.00019(19) P2 0.0174(3) 0.0196(3) 0.0179(2) -0.00503(19) -0.00097(19) -0.00237(18) P3 0.0196(3) 0.0178(2) 0.0189(3) -0.00326(19) -0.00303(19) -0.00103(18) S1 0.0157(2) 0.0268(3) 0.0211(3) 0.0014(2) -0.00431(19) 0.00108(18) S2 0.0202(3) 0.0290(3) 0.0176(2) 0.0022(2) -0.00553(19) 0.00260(19) S3 0.0216(3) 0.0317(3) 0.0215(3) -0.0049(2) -0.0085(2) -0.0026(2) C1 0.0187(9) 0.0232(10) 0.0176(9) -0.0011(7) -0.0033(7) -0.0029(7) C2 0.0210(10) 0.0300(11) 0.0216(10) -0.0012(8) -0.0070(8) 0.0000(8) C3 0.0280(11) 0.0339(12) 0.0194(10) -0.0026(8) -0.0073(8) -0.0021(9) C4 0.0265(11) 0.0252(10) 0.0203(10) -0.0050(8) 0.0014(8) -0.0069(8) C5 0.0209(10) 0.0308(11) 0.0310(11) -0.0085(9) -0.0045(8) 0.0019(8) C6 0.0209(10) 0.0322(11) 0.0234(10) -0.0034(8) -0.0082(8) 0.0005(8) C8 0.0325(12) 0.0251(11) 0.0307(11) -0.0043(9) -0.0125(9) -0.0048(9) C9 0.0461(16) 0.0248(13) 0.105(3) -0.0015(14) -0.0401(18) -0.0011(11) C10 0.0473(16) 0.0349(13) 0.0650(18) -0.0045(12) -0.0299(14) -0.0128(12) C11 0.103(3) 0.0400(16) 0.0309(14) 0.0012(12) -0.0045(16) -0.0148(17) C12 0.0188(9) 0.0225(10) 0.0246(10) -0.0107(8) -0.0018(8) -0.0017(7) C13 0.0228(10) 0.0331(12) 0.0244(10) -0.0080(9) -0.0010(8) -0.0047(8) C14 0.0189(10) 0.0392(13) 0.0391(13) -0.0173(10) -0.0012(9) -0.0034(9) C15 0.0241(11) 0.0345(12) 0.0458(14) -0.0202(11) -0.0133(10) 0.0064(9) C16 0.0331(12) 0.0277(11) 0.0334(12) -0.0098(9) -0.0131(10) 0.0070(9) C17 0.0229(10) 0.0258(10) 0.0278(11) -0.0064(8) -0.0036(8) -0.0001(8) C18 0.0223(10) 0.0226(10) 0.0181(9) -0.0044(8) -0.0036(7) -0.0033(7) C19 0.0211(10) 0.0261(11) 0.0345(11) -0.0113(9) -0.0043(8) -0.0017(8) C20 0.0291(11) 0.0287(11) 0.0366(12) -0.0137(9) -0.0065(9) -0.0022(9) C21 0.0316(12) 0.0301(11) 0.0340(12) -0.0112(9) -0.0039(9) -0.0099(9) C22 0.0216(11) 0.0387(13) 0.0407(13) -0.0161(11) -0.0023(9) -0.0085(9) C23 0.0235(10) 0.0268(11) 0.0293(11) -0.0117(9) -0.0028(8) -0.0033(8) C24 0.0200(10) 0.0262(10) 0.0194(9) -0.0053(8) -0.0026(7) -0.0042(8) C25 0.0310(11) 0.0291(11) 0.0243(10) -0.0095(9) -0.0017(9) -0.0079(9) C26 0.0321(12) 0.0441(14) 0.0218(10) -0.0123(10) 0.0011(9) -0.0109(10) C27 0.0353(13) 0.0491(15) 0.0188(10) -0.0009(10) -0.0020(9) -0.0097(11) C28 0.0430(14) 0.0308(12) 0.0306(12) 0.0018(10) -0.0049(10) -0.0004(10) C29 0.0360(13) 0.0293(12) 0.0238(11) -0.0061(9) -0.0015(9) -0.0001(9) C30 0.0226(10) 0.0234(10) 0.0251(10) -0.0075(8) -0.0057(8) 0.0002(8) C31 0.0442(14) 0.0277(12) 0.0309(12) -0.0068(10) -0.0048(10) 0.0055(10) C32 0.0621(19) 0.0371(15) 0.0410(15) -0.0149(12) -0.0134(13) 0.0198(13) C33 0.0373(14) 0.0502(16) 0.0449(15) -0.0264(13) 0.0006(11) 0.0087(12) C34 0.0371(14) 0.0422(14) 0.0364(13) -0.0171(11) 0.0095(11) -0.0104(11) C35 0.0336(12) 0.0282(11) 0.0298(11) -0.0104(9) 0.0019(9) -0.0071(9) C36 0.0240(10) 0.0207(9) 0.0186(9) -0.0002(7) -0.0050(8) -0.0019(7) C37 0.0304(11) 0.0235(10) 0.0248(10) -0.0047(8) -0.0067(8) 0.0020(8) C38 0.0302(12) 0.0303(12) 0.0299(11) -0.0016(9) -0.0084(9) 0.0073(9) C39 0.0301(12) 0.0351(13) 0.0394(13) 0.0028(10) -0.0167(10) -0.0011(10) C40 0.0444(15) 0.0345(13) 0.0607(17) -0.0166(12) -0.0301(13) 0.0015(11) C41 0.0347(12) 0.0269(11) 0.0479(14) -0.0144(10) -0.0201(11) 0.0055(9) C42 0.0234(10) 0.0209(9) 0.0202(9) -0.0046(8) -0.0056(8) -0.0014(7) C43 0.0258(11) 0.0308(11) 0.0239(10) -0.0015(9) -0.0075(8) -0.0031(8) C44 0.0300(12) 0.0355(13) 0.0287(11) 0.0035(10) -0.0035(9) -0.0105(9) C45 0.0420(13) 0.0293(12) 0.0245(11) 0.0021(9) -0.0093(10) -0.0053(10) C46 0.0365(12) 0.0286(11) 0.0297(11) -0.0045(9) -0.0159(10) 0.0025(9) C47 0.0264(11) 0.0282(11) 0.0259(10) -0.0069(9) -0.0083(8) 0.0012(8) C7 0.0565(17) 0.0466(15) 0.0269(12) -0.0140(11) -0.0072(11) -0.0024(12) _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 O1 C4 1.361(2) . ? O1 C7 1.419(3) . ? Cu1 P3 2.2659(5) . ? Cu1 P2 2.2698(5) . ? Cu1 S1 2.4538(5) . ? Cu1 S2 2.4675(6) . ? P1 C1 1.810(2) . ? P1 S1 1.9903(7) . ? P1 S2 1.9978(7) . ? P1 S3 2.1033(7) . ? P2 C24 1.822(2) . ? P2 C18 1.825(2) . ? P2 C12 1.830(2) . ? P3 C30 1.822(2) . ? P3 C36 1.824(2) . ? P3 C42 1.825(2) . ? S3 C8 1.863(2) . ? C1 C2 1.382(3) . ? C1 C6 1.397(3) . ? C2 C3 1.389(3) . ? C3 C4 1.384(3) . ? C4 C5 1.392(3) . ? C5 C6 1.373(3) . ? C8 C9 1.490(4) . ? C8 C11 1.522(4) . ? C8 C10 1.523(3) . ? C12 C17 1.389(3) . ? C12 C13 1.393(3) . ? C13 C14 1.386(3) . ? C14 C15 1.380(4) . ? C15 C16 1.389(3) . ? C16 C17 1.387(3) . ? C18 C23 1.385(3) . ? C18 C19 1.391(3) . ? C19 C20 1.388(3) . ? C20 C21 1.379(3) . ? C21 C22 1.385(3) . ? C22 C23 1.388(3) . ? C24 C29 1.385(3) . ? C24 C25 1.396(3) . ? C25 C26 1.382(3) . ? C26 C27 1.383(4) . ? C27 C28 1.373(4) . ? C28 C29 1.386(3) . ? C30 C35 1.389(3) . ? C30 C31 1.392(3) . ? C31 C32 1.382(4) . ? C32 C33 1.383(4) . ? C33 C34 1.384(4) . ? C34 C35 1.384(3) . ? C36 C37 1.382(3) . ? C36 C41 1.393(3) . ? C37 C38 1.387(3) . ? C38 C39 1.377(4) . ? C39 C40 1.384(4) . ? C40 C41 1.381(3) . ? C42 C43 1.385(3) . ? C42 C47 1.396(3) . ? C43 C44 1.384(3) . ? C44 C45 1.382(3) . ? C45 C46 1.381(3) . ? C46 C47 1.386(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 C4 O1 C7 117.94(19) . . ? P3 Cu1 P2 122.69(2) . . ? P3 Cu1 S1 115.14(2) . . ? P2 Cu1 S1 102.08(2) . . ? P3 Cu1 S2 105.41(2) . . ? P2 Cu1 S2 120.83(2) . . ? S1 Cu1 S2 84.288(18) . . ? C1 P1 S1 109.65(7) . . ? C1 P1 S2 111.73(7) . . ? S1 P1 S2 111.79(3) . . ? C1 P1 S3 105.32(7) . . ? S1 P1 S3 117.09(3) . . ? S2 P1 S3 100.89(3) . . ? C24 P2 C18 103.24(9) . . ? C24 P2 C12 103.10(9) . . ? C18 P2 C12 102.69(9) . . ? C24 P2 Cu1 121.37(7) . . ? C18 P2 Cu1 115.57(7) . . ? C12 P2 Cu1 108.72(6) . . ? C30 P3 C36 103.76(9) . . ? C30 P3 C42 103.19(10) . . ? C36 P3 C42 102.17(9) . . ? C30 P3 Cu1 115.41(7) . . ? C36 P3 Cu1 118.65(7) . . ? C42 P3 Cu1 111.76(6) . . ? P1 S1 Cu1 82.20(2) . . ? P1 S2 Cu1 81.70(2) . . ? C8 S3 P1 110.78(7) . . ? C2 C1 C6 118.87(18) . . ? C2 C1 P1 121.69(16) . . ? C6 C1 P1 119.44(15) . . ? C1 C2 C3 121.3(2) . . ? C4 C3 C2 119.26(19) . . ? O1 C4 C3 125.4(2) . . ? O1 C4 C5 114.7(2) . . ? C3 C4 C5 119.91(19) . . ? C6 C5 C4 120.4(2) . . ? C5 C6 C1 120.26(19) . . ? C9 C8 C11 111.2(3) . . ? C9 C8 C10 109.8(2) . . ? C11 C8 C10 109.9(2) . . ? C9 C8 S3 111.36(18) . . ? C11 C8 S3 111.40(18) . . ? C10 C8 S3 102.98(16) . . ? C17 C12 C13 118.86(19) . . ? C17 C12 P2 118.23(15) . . ? C13 C12 P2 122.58(17) . . ? C14 C13 C12 120.1(2) . . ? C15 C14 C13 120.7(2) . . ? C14 C15 C16 119.7(2) . . ? C17 C16 C15 119.6(2) . . ? C16 C17 C12 121.1(2) . . ? C23 C18 C19 119.08(19) . . ? C23 C18 P2 117.60(16) . . ? C19 C18 P2 123.30(16) . . ? C20 C19 C18 120.3(2) . . ? C21 C20 C19 120.5(2) . . ? C20 C21 C22 119.3(2) . . ? C21 C22 C23 120.5(2) . . ? C18 C23 C22 120.3(2) . . ? C29 C24 C25 118.54(19) . . ? C29 C24 P2 119.00(16) . . ? C25 C24 P2 122.46(17) . . ? C26 C25 C24 120.3(2) . . ? C25 C26 C27 120.6(2) . . ? C28 C27 C26 119.4(2) . . ? C27 C28 C29 120.5(2) . . ? C24 C29 C28 120.7(2) . . ? C35 C30 C31 119.4(2) . . ? C35 C30 P3 116.93(16) . . ? C31 C30 P3 123.63(17) . . ? C32 C31 C30 119.8(2) . . ? C31 C32 C33 120.7(3) . . ? C32 C33 C34 119.7(2) . . ? C33 C34 C35 120.0(2) . . ? C34 C35 C30 120.4(2) . . ? C37 C36 C41 118.9(2) . . ? C37 C36 P3 118.99(16) . . ? C41 C36 P3 121.90(16) . . ? C36 C37 C38 120.6(2) . . ? C39 C38 C37 120.2(2) . . ? C38 C39 C40 119.5(2) . . ? C41 C40 C39 120.4(2) . . ? C40 C41 C36 120.3(2) . . ? C43 C42 C47 118.4(2) . . ? C43 C42 P3 123.16(16) . . ? C47 C42 P3 118.28(16) . . ? C44 C43 C42 120.7(2) . . ? C45 C44 C43 120.5(2) . . ? C46 C45 C44 119.5(2) . . ? C45 C46 C47 120.1(2) . . ? C46 C47 C42 120.8(2) . . ? _diffrn_measured_fraction_theta_max 0.641 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.079 _refine_diff_density_min -1.021 _refine_diff_density_rms 0.200 data_3 _database_code_depnum_ccdc_archive 'CCDC 601695' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H24 Na O3 P S2' _chemical_formula_weight 370.42 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' P P 0.1023 0.0942 '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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.0592(11) _cell_length_b 8.7781(9) _cell_length_c 16.8189(15) _cell_angle_alpha 90.00 _cell_angle_beta 102.117(7) _cell_angle_gamma 90.00 _cell_volume 1885.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 5 _cell_measurement_theta_max 50 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.305 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 0.398 _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 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'stoe stadi 4' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10946 _diffrn_reflns_av_R_equivalents 0.0570 _diffrn_reflns_av_sigmaI/netI 0.0516 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -3 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.95 _diffrn_reflns_theta_max 31.75 _reflns_number_total 4416 _reflns_number_gt 2888 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'kuma ccd' _computing_cell_refinement 'kuma ccd' _computing_data_reduction 'kuma ccd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.2000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4416 _refine_ls_number_parameters 195 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1252 _refine_ls_R_factor_gt 0.0957 _refine_ls_wR_factor_ref 0.3278 _refine_ls_wR_factor_gt 0.2834 _refine_ls_goodness_of_fit_ref 1.228 _refine_ls_restrained_S_all 1.250 _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 Na1 Na 0.28012(14) 0.5146(2) 0.29810(11) 0.0572(6) Uani 1 1 d . . . P1 P 0.32725(8) 0.70836(14) 0.14169(6) 0.0444(4) Uani 1 1 d . . . S1 S 0.18682(8) 0.70632(14) 0.17111(6) 0.0474(4) Uani 1 1 d . . . S2 S 0.42696(10) 0.55185(18) 0.19400(8) 0.0662(5) Uani 1 1 d . A . O1 O 0.3660(2) 0.8803(4) 0.16326(17) 0.0460(7) Uani 1 1 d . . . O2 O 0.2653(2) 0.7400(4) -0.21832(18) 0.0526(8) Uani 1 1 d . . . C1 C 0.3081(3) 0.7021(5) 0.0327(3) 0.0396(9) Uani 1 1 d . . . C2 C 0.3595(3) 0.6016(5) -0.0094(3) 0.0481(10) Uani 1 1 d . A . H2A H 0.4040 0.5259 0.0198 0.058 Uiso 1 1 calc R . . C3 C 0.3472(3) 0.6096(6) -0.0931(3) 0.0502(11) Uani 1 1 d . . . H3A H 0.3835 0.5408 -0.1210 0.060 Uiso 1 1 calc R A . C4 C 0.2818(3) 0.7185(5) -0.1353(2) 0.0438(10) Uani 1 1 d . A . C5 C 0.2260(3) 0.8154(6) -0.0946(3) 0.0479(10) Uani 1 1 d . . . H5A H 0.1780 0.8866 -0.1243 0.057 Uiso 1 1 calc R A . C6 C 0.2402(3) 0.8084(5) -0.0119(2) 0.0423(9) Uani 1 1 d . A . H6A H 0.2032 0.8769 0.0157 0.051 Uiso 1 1 calc R . . C7 C 0.3159(4) 0.6384(7) -0.2643(3) 0.0606(13) Uani 1 1 d . . . H7A H 0.2981 0.6671 -0.3218 0.091 Uiso 1 1 calc R . . H7B H 0.2924 0.5340 -0.2579 0.091 Uiso 1 1 calc R . . H7C H 0.3919 0.6446 -0.2446 0.091 Uiso 1 1 calc R . . C8 C 0.4702(3) 0.9524(6) 0.1651(3) 0.0524(11) Uani 1 1 d . A . C9 C 0.5301(3) 0.8742(7) 0.1067(3) 0.0606(13) Uani 1 1 d . . . H9A H 0.5483 0.7700 0.1254 0.091 Uiso 1 1 calc R A . H9B H 0.5942 0.9314 0.1057 0.091 Uiso 1 1 calc R . . H9C H 0.4858 0.8714 0.0519 0.091 Uiso 1 1 calc R . . C10 C 0.4426(4) 1.1145(7) 0.1358(3) 0.0640(13) Uani 1 1 d . . . H10A H 0.4050 1.1652 0.1731 0.096 Uiso 1 1 calc R A . H10B H 0.3980 1.1117 0.0811 0.096 Uiso 1 1 calc R . . H10C H 0.5069 1.1709 0.1343 0.096 Uiso 1 1 calc R . . C11 C 0.5305(4) 0.9482(10) 0.2513(3) 0.0787(19) Uani 1 1 d . . . H11A H 0.4903 0.9999 0.2864 0.118 Uiso 1 1 calc R A . H11B H 0.5979 0.9998 0.2551 0.118 Uiso 1 1 calc R . . H11C H 0.5427 0.8420 0.2688 0.118 Uiso 1 1 calc R . . O3 O 0.3467(3) 0.6614(6) 0.4139(3) 0.0794(12) Uani 0.50 1 d PD A 1 C12 C 0.2991(9) 0.7350(13) 0.4735(7) 0.069(3) Uiso 0.50 1 d PD A 1 H12A H 0.2729 0.6593 0.5081 0.083 Uiso 0.50 1 calc PR A 1 H12B H 0.2405 0.8016 0.4473 0.083 Uiso 0.50 1 calc PR A 1 C13 C 0.3865(13) 0.8252(17) 0.5213(7) 0.085(4) Uiso 0.50 1 d PD A 1 H13A H 0.4206 0.7694 0.5710 0.102 Uiso 0.50 1 calc PR A 1 H13B H 0.3609 0.9244 0.5374 0.102 Uiso 0.50 1 calc PR A 1 C14 C 0.4621(9) 0.8481(14) 0.4652(9) 0.082(3) Uiso 0.50 1 d PD A 1 H14A H 0.5346 0.8616 0.4966 0.099 Uiso 0.50 1 calc PR A 1 H14B H 0.4423 0.9379 0.4297 0.099 Uiso 0.50 1 calc PR A 1 C15 C 0.4517(11) 0.702(2) 0.4156(12) 0.136(7) Uiso 0.50 1 d PD A 1 H15A H 0.4636 0.7199 0.3602 0.163 Uiso 0.50 1 calc PR A 1 H15B H 0.5008 0.6224 0.4426 0.163 Uiso 0.50 1 calc PR A 1 O3A O 0.3467(3) 0.6614(6) 0.4139(3) 0.0794(12) Uani 0.50 1 d PD A 2 C12A C 0.3163(15) 0.8068(14) 0.4332(8) 0.110(5) Uiso 0.50 1 d PD A 2 H12C H 0.2404 0.8247 0.4132 0.132 Uiso 0.50 1 calc PR A 2 H12D H 0.3569 0.8879 0.4129 0.132 Uiso 0.50 1 calc PR A 2 C14A C 0.4259(12) 0.6744(18) 0.5446(6) 0.093(4) Uiso 0.50 1 d PD A 2 H14C H 0.4018 0.5874 0.5733 0.112 Uiso 0.50 1 calc PR A 2 H14D H 0.4909 0.7159 0.5789 0.112 Uiso 0.50 1 calc PR A 2 C13A C 0.3463(18) 0.790(2) 0.5275(9) 0.118(7) Uiso 0.50 1 d PD A 2 H13C H 0.3733 0.8880 0.5529 0.141 Uiso 0.50 1 calc PR A 2 H13D H 0.2843 0.7599 0.5491 0.141 Uiso 0.50 1 calc PR A 2 C15A C 0.4459(11) 0.623(2) 0.4595(10) 0.113(5) Uiso 0.50 1 d PD A 2 H15C H 0.5027 0.6814 0.4430 0.136 Uiso 0.50 1 calc PR A 2 H15D H 0.4604 0.5121 0.4576 0.136 Uiso 0.50 1 calc PR A 2 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 Na1 0.0438(10) 0.0823(14) 0.0491(10) 0.0221(9) 0.0182(8) 0.0060(9) P1 0.0330(6) 0.0684(8) 0.0358(6) 0.0146(4) 0.0163(4) 0.0133(4) S1 0.0348(6) 0.0699(8) 0.0423(6) 0.0137(5) 0.0189(4) 0.0100(4) S2 0.0489(7) 0.1003(11) 0.0567(8) 0.0379(7) 0.0275(6) 0.0331(7) O1 0.0302(13) 0.074(2) 0.0372(14) -0.0018(13) 0.0139(11) 0.0012(13) O2 0.0432(16) 0.084(2) 0.0323(14) -0.0015(14) 0.0115(12) 0.0101(16) C1 0.0350(18) 0.049(2) 0.039(2) 0.0068(16) 0.0169(15) 0.0074(15) C2 0.043(2) 0.058(2) 0.048(2) 0.0116(19) 0.0217(18) 0.0149(19) C3 0.043(2) 0.068(3) 0.046(2) 0.001(2) 0.0231(18) 0.012(2) C4 0.0338(19) 0.066(3) 0.0329(19) 0.0017(17) 0.0108(16) 0.0005(18) C5 0.039(2) 0.069(3) 0.037(2) 0.0087(18) 0.0112(17) 0.0108(19) C6 0.044(2) 0.048(2) 0.038(2) 0.0079(16) 0.0175(17) 0.0154(16) C7 0.050(2) 0.090(4) 0.046(2) -0.011(2) 0.019(2) 0.006(3) C8 0.0287(18) 0.091(3) 0.041(2) -0.004(2) 0.0149(16) -0.002(2) C9 0.039(2) 0.096(4) 0.054(3) 0.002(3) 0.0254(19) -0.002(2) C10 0.053(3) 0.082(4) 0.065(3) -0.002(3) 0.028(2) -0.007(3) C11 0.038(2) 0.149(6) 0.047(3) -0.005(3) 0.004(2) -0.003(3) O3 0.050(2) 0.117(3) 0.069(2) 0.021(2) 0.0068(18) -0.004(2) O3A 0.050(2) 0.117(3) 0.069(2) 0.021(2) 0.0068(18) -0.004(2) _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 Na1 O3 2.345(5) . ? Na1 O1 2.445(3) 2_545 ? Na1 S1 2.772(2) 2_545 ? Na1 S1 2.790(2) . ? Na1 S2 2.874(2) . ? Na1 C15 3.124(14) . ? Na1 P1 3.288(2) 2_545 ? Na1 P1 3.297(2) . ? P1 O1 1.609(3) . ? P1 C1 1.799(4) . ? P1 S2 1.9688(16) . ? P1 S1 1.9973(14) . ? P1 Na1 3.288(2) 2 ? S1 Na1 2.772(2) 2 ? O1 C8 1.495(5) . ? O1 Na1 2.445(3) 2 ? O2 C4 1.380(5) . ? O2 C7 1.429(6) . ? C1 C2 1.388(6) . ? C1 C6 1.393(6) . ? C2 C3 1.385(6) . ? C3 C4 1.375(6) . ? C4 C5 1.390(6) . ? C5 C6 1.366(6) . ? C8 C11 1.497(7) . ? C8 C10 1.525(8) . ? C8 C9 1.539(6) . ? O3 C15 1.411(11) . ? O3 C12 1.438(9) . ? C12 C13 1.480(16) . ? C13 C14 1.516(19) . ? C14 C15 1.523(19) . ? C12A C13A 1.560(19) . ? C14A C13A 1.44(2) . ? C14A C15A 1.57(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 O3 Na1 O1 102.59(13) . 2_545 ? O3 Na1 S1 111.43(13) . 2_545 ? O1 Na1 S1 65.12(9) 2_545 2_545 ? O3 Na1 S1 109.29(14) . . ? O1 Na1 S1 104.74(10) 2_545 . ? S1 Na1 S1 139.26(9) 2_545 . ? O3 Na1 S2 105.38(12) . . ? O1 Na1 S2 151.04(12) 2_545 . ? S1 Na1 S2 97.31(7) 2_545 . ? S1 Na1 S2 72.85(5) . . ? O3 Na1 C15 25.1(2) . . ? O1 Na1 C15 125.6(3) 2_545 . ? S1 Na1 C15 109.4(5) 2_545 . ? S1 Na1 C15 107.9(5) . . ? S2 Na1 C15 81.0(3) . . ? O3 Na1 P1 107.52(12) . 2_545 ? O1 Na1 P1 27.96(8) 2_545 2_545 ? S1 Na1 P1 37.27(4) 2_545 2_545 ? S1 Na1 P1 125.65(7) . 2_545 ? S2 Na1 P1 131.52(8) . 2_545 ? C15 Na1 P1 122.0(4) . 2_545 ? O3 Na1 P1 106.29(13) . . ? O1 Na1 P1 138.40(10) 2_545 . ? S1 Na1 P1 127.22(7) 2_545 . ? S1 Na1 P1 37.14(3) . . ? S2 Na1 P1 36.40(4) . . ? C15 Na1 P1 90.2(4) . . ? P1 Na1 P1 146.15(8) 2_545 . ? O1 P1 C1 103.21(17) . . ? O1 P1 S2 113.98(13) . . ? C1 P1 S2 111.81(14) . . ? O1 P1 S1 102.39(11) . . ? C1 P1 S1 108.30(14) . . ? S2 P1 S1 116.01(7) . . ? O1 P1 Na1 45.43(10) . 2 ? C1 P1 Na1 111.23(13) . 2 ? S2 P1 Na1 135.85(8) . 2 ? S1 P1 Na1 57.18(5) . 2 ? O1 P1 Na1 114.00(11) . . ? C1 P1 Na1 142.02(15) . . ? S2 P1 Na1 60.01(5) . . ? S1 P1 Na1 57.51(5) . . ? Na1 P1 Na1 90.74(3) 2 . ? P1 S1 Na1 85.55(6) . 2 ? P1 S1 Na1 85.35(6) . . ? Na1 S1 Na1 114.83(5) 2 . ? P1 S2 Na1 83.59(6) . . ? C8 O1 P1 130.1(3) . . ? C8 O1 Na1 123.3(3) . 2 ? P1 O1 Na1 106.61(13) . 2 ? C4 O2 C7 118.1(4) . . ? C2 C1 C6 118.2(4) . . ? C2 C1 P1 124.1(3) . . ? C6 C1 P1 117.6(3) . . ? C3 C2 C1 121.4(4) . . ? C4 C3 C2 119.1(4) . . ? C3 C4 O2 124.4(4) . . ? C3 C4 C5 120.3(4) . . ? O2 C4 C5 115.3(4) . . ? C6 C5 C4 120.0(4) . . ? C5 C6 C1 120.9(4) . . ? O1 C8 C11 107.5(4) . . ? O1 C8 C10 103.6(3) . . ? C11 C8 C10 112.1(5) . . ? O1 C8 C9 112.3(4) . . ? C11 C8 C9 111.9(4) . . ? C10 C8 C9 109.1(4) . . ? C15 O3 C12 115.7(9) . . ? C15 O3 Na1 110.1(7) . . ? C12 O3 Na1 133.4(5) . . ? O3 C12 C13 102.9(8) . . ? C12 C13 C14 105.1(7) . . ? C13 C14 C15 103.6(8) . . ? O3 C15 C14 101.4(9) . . ? O3 C15 Na1 44.8(5) . . ? C14 C15 Na1 139.5(10) . . ? C13A C14A C15A 105.9(8) . . ? C14A C13A C12A 106.6(8) . . ? _diffrn_measured_fraction_theta_max 0.690 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.538 _refine_diff_density_min -1.040 _refine_diff_density_rms 0.175 data_4 _database_code_depnum_ccdc_archive 'CCDC 601696' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H52 Na2 O8 P2 S4' _chemical_formula_weight 776.88 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.2730(17) _cell_length_b 11.841(2) _cell_length_c 20.614(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.61(3) _cell_angle_gamma 90.00 _cell_volume 1996.6(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2 _cell_measurement_theta_max 50 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.292 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 0.382 _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 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'stoe stadi IV' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15549 _diffrn_reflns_av_R_equivalents 0.0588 _diffrn_reflns_av_sigmaI/netI 0.0485 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 31.81 _reflns_number_total 4733 _reflns_number_gt 3563 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'kuma ccd' _computing_cell_refinement 'kuma ccd' _computing_data_reduction 'kuma ccd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1318P)^2^+0.3750P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4733 _refine_ls_number_parameters 202 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0857 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.2077 _refine_ls_wR_factor_gt 0.1808 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.125 _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 Na1 Na 0.04108(14) 0.61847(9) 0.44172(5) 0.0315(3) Uani 1 1 d . . . P1 P 0.07943(8) 0.34449(6) 0.41308(3) 0.0268(2) Uani 1 1 d . . . S1 S -0.01541(8) 0.44584(6) 0.34141(3) 0.0318(2) Uani 1 1 d . A . S2 S 0.22320(8) 0.41626(6) 0.48743(3) 0.0328(2) Uani 1 1 d . . . O1 O 0.4426(3) -0.03951(17) 0.31664(11) 0.0412(5) Uani 1 1 d . . . O2 O -0.0560(2) 0.28125(14) 0.44932(8) 0.0267(4) Uani 1 1 d . . . C1 C 0.1889(3) 0.2297(2) 0.38106(13) 0.0299(5) Uani 1 1 d . . . C2 C 0.2111(3) 0.2254(3) 0.31575(13) 0.0342(6) Uani 1 1 d . A . H2A H 0.1681 0.2842 0.2869 0.041 Uiso 1 1 calc R . . C3 C 0.2951(4) 0.1366(3) 0.29170(14) 0.0367(6) Uani 1 1 d . . . H3A H 0.3090 0.1345 0.2468 0.044 Uiso 1 1 calc R A . C4 C 0.3579(3) 0.0517(2) 0.33390(14) 0.0318(6) Uani 1 1 d . A . C5 C 0.3360(3) 0.0543(2) 0.39946(14) 0.0325(6) Uani 1 1 d . . . H5A H 0.3787 -0.0046 0.4283 0.039 Uiso 1 1 calc R A . C6 C 0.2525(3) 0.1425(2) 0.42246(14) 0.0318(6) Uani 1 1 d . A . H6A H 0.2380 0.1440 0.4673 0.038 Uiso 1 1 calc R . . C7 C 0.4658(4) -0.0473(3) 0.24947(16) 0.0495(8) Uani 1 1 d . . . H7A H 0.5287 -0.1155 0.2431 0.074 Uiso 1 1 calc R . . H7B H 0.5254 0.0193 0.2377 0.074 Uiso 1 1 calc R . . H7C H 0.3591 -0.0511 0.2215 0.074 Uiso 1 1 calc R . . C8 C -0.2082(3) 0.2229(2) 0.42045(12) 0.0280(5) Uani 1 1 d . A . C9 C -0.2270(4) 0.1315(3) 0.46945(14) 0.0407(7) Uani 1 1 d . . . H9A H -0.2350 0.1657 0.5121 0.061 Uiso 1 1 calc R A . H9B H -0.1320 0.0812 0.4736 0.061 Uiso 1 1 calc R . . H9C H -0.3265 0.0881 0.4545 0.061 Uiso 1 1 calc R . . C10 C -0.1963(4) 0.1720(3) 0.35346(14) 0.0378(6) Uani 1 1 d . . . H10A H -0.1060 0.1176 0.3576 0.057 Uiso 1 1 calc R A . H10B H -0.1762 0.2322 0.3230 0.057 Uiso 1 1 calc R . . H10C H -0.2989 0.1335 0.3367 0.057 Uiso 1 1 calc R . . C11 C -0.3452(3) 0.3072(2) 0.41664(14) 0.0342(6) Uani 1 1 d . . . H11A H -0.3499 0.3381 0.4604 0.051 Uiso 1 1 calc R A . H11B H -0.4490 0.2699 0.4002 0.051 Uiso 1 1 calc R . . H11C H -0.3259 0.3686 0.3868 0.051 Uiso 1 1 calc R . . O3 O 0.2789(6) 0.6826(4) 0.3914(2) 0.0377(10) Uiso 0.50 1 d P A 1 O4 O -0.0447(6) 0.7590(4) 0.3646(2) 0.0403(12) Uiso 0.50 1 d P A 1 C12 C 0.4065(10) 0.6033(7) 0.3891(4) 0.0499(17) Uiso 0.50 1 d P A 1 H12A H 0.4932 0.6380 0.3683 0.075 Uiso 0.50 1 calc PR A 1 H12B H 0.3633 0.5371 0.3637 0.075 Uiso 0.50 1 calc PR A 1 H12C H 0.4511 0.5799 0.4338 0.075 Uiso 0.50 1 calc PR A 1 C13 C 0.2102(9) 0.7219(6) 0.3290(3) 0.0418(14) Uiso 0.50 1 d P A 1 H13A H 0.1585 0.6586 0.3021 0.050 Uiso 0.50 1 calc PR A 1 H13B H 0.2965 0.7547 0.3062 0.050 Uiso 0.50 1 calc PR A 1 C14 C 0.0879(9) 0.8078(6) 0.3370(3) 0.0379(13) Uiso 0.50 1 d P A 1 H14A H 0.1389 0.8686 0.3661 0.045 Uiso 0.50 1 calc PR A 1 H14B H 0.0460 0.8417 0.2938 0.045 Uiso 0.50 1 calc PR A 1 C15 C -0.1671(12) 0.8379(8) 0.3775(4) 0.061(2) Uiso 0.50 1 d P A 1 H15A H -0.1898 0.8909 0.3407 0.091 Uiso 0.50 1 calc PR A 1 H15B H -0.1279 0.8797 0.4178 0.091 Uiso 0.50 1 calc PR A 1 H15C H -0.2674 0.7971 0.3827 0.091 Uiso 0.50 1 calc PR A 1 O3A O 0.2338(5) 0.7174(4) 0.3888(2) 0.0325(9) Uiso 0.50 1 d P A 2 O4A O -0.0969(6) 0.7673(4) 0.3753(2) 0.0332(10) Uiso 0.50 1 d P A 2 C12A C 0.3713(9) 0.6503(7) 0.3774(3) 0.0449(15) Uiso 0.50 1 d P A 2 H12D H 0.4455 0.6963 0.3555 0.067 Uiso 0.50 1 calc PR A 2 H12E H 0.3330 0.5857 0.3495 0.067 Uiso 0.50 1 calc PR A 2 H12F H 0.4293 0.6229 0.4194 0.067 Uiso 0.50 1 calc PR A 2 C13A C 0.1481(8) 0.7605(5) 0.3291(3) 0.0289(11) Uiso 0.50 1 d P A 2 H13C H 0.1012 0.6978 0.3005 0.035 Uiso 0.50 1 calc PR A 2 H13D H 0.2233 0.8040 0.3054 0.035 Uiso 0.50 1 calc PR A 2 C14A C 0.0170(7) 0.8341(5) 0.3455(3) 0.0288(11) Uiso 0.50 1 d P A 2 H14C H 0.0639 0.8939 0.3763 0.035 Uiso 0.50 1 calc PR A 2 H14D H -0.0398 0.8707 0.3053 0.035 Uiso 0.50 1 calc PR A 2 C15A C -0.2304(10) 0.8285(6) 0.3895(4) 0.0442(15) Uiso 0.50 1 d P A 2 H15D H -0.2624 0.8841 0.3548 0.066 Uiso 0.50 1 calc PR A 2 H15E H -0.2011 0.8675 0.4316 0.066 Uiso 0.50 1 calc PR A 2 H15F H -0.3219 0.7770 0.3922 0.066 Uiso 0.50 1 calc PR A 2 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 Na1 0.0395(6) 0.0270(5) 0.0282(6) 0.0008(4) 0.0060(4) -0.0052(4) P1 0.0216(4) 0.0296(4) 0.0293(4) -0.0063(2) 0.0043(3) -0.0020(2) S1 0.0325(4) 0.0323(4) 0.0305(4) -0.0031(2) 0.0041(3) -0.0016(3) S2 0.0242(4) 0.0365(4) 0.0366(4) -0.0105(3) 0.0006(3) -0.0038(2) O1 0.0425(12) 0.0351(11) 0.0491(12) -0.0103(9) 0.0168(10) 0.0037(9) O2 0.0220(9) 0.0309(9) 0.0267(9) -0.0054(7) 0.0018(7) -0.0045(7) C1 0.0229(12) 0.0325(13) 0.0344(14) -0.0085(10) 0.0045(10) -0.0041(10) C2 0.0294(14) 0.0424(15) 0.0311(14) -0.0044(11) 0.0053(11) 0.0018(11) C3 0.0336(15) 0.0438(16) 0.0339(15) -0.0090(11) 0.0086(11) 0.0000(12) C4 0.0249(13) 0.0305(13) 0.0417(16) -0.0094(10) 0.0098(11) -0.0034(10) C5 0.0281(14) 0.0301(13) 0.0407(15) -0.0038(10) 0.0092(11) -0.0033(10) C6 0.0266(13) 0.0356(14) 0.0350(14) -0.0054(11) 0.0106(11) -0.0029(10) C7 0.0452(19) 0.058(2) 0.0469(18) -0.0198(15) 0.0127(15) 0.0117(15) C8 0.0250(12) 0.0309(13) 0.0275(13) -0.0042(10) 0.0018(10) -0.0073(10) C9 0.0469(18) 0.0332(15) 0.0393(16) 0.0006(11) -0.0021(13) -0.0137(13) C10 0.0336(15) 0.0460(16) 0.0338(15) -0.0124(12) 0.0048(12) -0.0100(12) C11 0.0236(13) 0.0391(14) 0.0392(15) -0.0010(11) 0.0025(11) -0.0029(11) _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 Na1 O4 2.337(5) . ? Na1 O3A 2.371(4) . ? Na1 O4A 2.412(5) . ? Na1 O3 2.477(5) . ? Na1 O2 2.527(2) 3_566 ? Na1 S2 2.8352(14) 3_566 ? Na1 S1 2.8954(13) . ? Na1 S2 2.9096(14) . ? Na1 C13A 3.102(5) . ? Na1 P1 3.3211(14) . ? Na1 P1 3.3224(14) 3_566 ? Na1 Na1 3.820(2) 3_566 ? P1 O2 1.6201(19) . ? P1 C1 1.812(3) . ? P1 S1 1.9725(10) . ? P1 S2 1.9849(10) . ? P1 Na1 3.3224(14) 3_566 ? S2 Na1 2.8352(14) 3_566 ? O1 C4 1.363(3) . ? O1 C7 1.429(4) . ? O2 C8 1.480(3) . ? O2 Na1 2.527(2) 3_566 ? C1 C2 1.387(4) . ? C1 C6 1.391(4) . ? C2 C3 1.392(4) . ? C3 C4 1.379(4) . ? C4 C5 1.390(4) . ? C5 C6 1.375(4) . ? C8 C11 1.504(4) . ? C8 C9 1.504(4) . ? C8 C10 1.523(4) . ? O3 C13 1.406(8) . ? O3 C12 1.419(9) . ? O4 C14 1.431(8) . ? O4 C15 1.432(10) . ? C13 C14 1.462(9) . ? O3A C13A 1.422(7) . ? O3A C12A 1.436(9) . ? O4A C15A 1.388(9) . ? O4A C14A 1.436(7) . ? C13A C14A 1.470(8) . ? 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 O4 Na1 O3A 59.48(18) . . ? O4 Na1 O4A 12.52(14) . . ? O3A Na1 O4A 70.83(17) . . ? O4 Na1 O3 71.09(19) . . ? O3A Na1 O3 12.86(12) . . ? O4A Na1 O3 82.88(17) . . ? O4 Na1 O2 103.86(14) . 3_566 ? O3A Na1 O2 103.28(11) . 3_566 ? O4A Na1 O2 96.72(12) . 3_566 ? O3 Na1 O2 106.99(12) . 3_566 ? O4 Na1 S2 105.95(14) . 3_566 ? O3A Na1 S2 158.73(12) . 3_566 ? O4A Na1 S2 93.58(13) . 3_566 ? O3 Na1 S2 169.24(12) . 3_566 ? O2 Na1 S2 63.20(5) 3_566 3_566 ? O4 Na1 S1 90.95(13) . . ? O3A Na1 S1 93.91(11) . . ? O4A Na1 S1 95.65(11) . . ? O3 Na1 S1 88.31(11) . . ? O2 Na1 S1 161.37(6) 3_566 . ? S2 Na1 S1 102.18(4) 3_566 . ? O4 Na1 S2 153.62(14) . . ? O3A Na1 S2 101.78(12) . . ? O4A Na1 S2 164.45(12) . . ? O3 Na1 S2 89.01(13) . . ? O2 Na1 S2 98.33(6) 3_566 . ? S2 Na1 S2 96.65(4) 3_566 . ? S1 Na1 S2 70.77(4) . . ? O4 Na1 C13A 36.50(18) . . ? O3A Na1 C13A 25.98(15) . . ? O4A Na1 C13A 48.89(17) . . ? O3 Na1 C13A 35.55(17) . . ? O2 Na1 C13A 115.41(12) 3_566 . ? S2 Na1 C13A 142.45(14) 3_566 . ? S1 Na1 C13A 83.21(11) . . ? S2 Na1 C13A 119.78(14) . . ? O4 Na1 P1 127.00(13) . . ? O3A Na1 P1 108.19(12) . . ? O4A Na1 P1 131.51(11) . . ? O3 Na1 P1 97.00(13) . . ? O2 Na1 P1 128.59(6) 3_566 . ? S2 Na1 P1 92.95(3) 3_566 . ? S1 Na1 P1 36.19(2) . . ? S2 Na1 P1 36.40(2) . . ? C13A Na1 P1 110.55(12) . . ? O4 Na1 P1 114.68(14) . 3_566 ? O3A Na1 P1 131.45(11) . 3_566 ? O4A Na1 P1 103.57(12) . 3_566 ? O3 Na1 P1 134.54(11) . 3_566 ? O2 Na1 P1 28.20(4) 3_566 3_566 ? S2 Na1 P1 36.54(3) 3_566 3_566 ? S1 Na1 P1 134.30(4) . 3_566 ? S2 Na1 P1 91.58(4) . 3_566 ? C13A Na1 P1 139.52(12) . 3_566 ? P1 Na1 P1 109.79(3) . 3_566 ? O4 Na1 Na1 152.40(14) . 3_566 ? O3A Na1 Na1 147.89(13) . 3_566 ? O4A Na1 Na1 141.27(13) . 3_566 ? O3 Na1 Na1 135.72(13) . 3_566 ? O2 Na1 Na1 77.04(5) 3_566 3_566 ? S2 Na1 Na1 49.16(3) 3_566 3_566 ? S1 Na1 Na1 84.59(4) . 3_566 ? S2 Na1 Na1 47.49(3) . 3_566 ? C13A Na1 Na1 165.17(13) . 3_566 ? P1 Na1 Na1 54.91(3) . 3_566 ? P1 Na1 Na1 54.88(3) 3_566 3_566 ? O2 P1 C1 103.83(11) . . ? O2 P1 S1 113.68(8) . . ? C1 P1 S1 110.37(10) . . ? O2 P1 S2 102.57(7) . . ? C1 P1 S2 109.15(9) . . ? S1 P1 S2 116.30(5) . . ? O2 P1 Na1 106.17(7) . . ? C1 P1 Na1 149.76(9) . . ? S1 P1 Na1 60.07(3) . . ? S2 P1 Na1 60.44(3) . . ? O2 P1 Na1 47.47(6) . 3_566 ? C1 P1 Na1 131.37(10) . 3_566 ? S1 P1 Na1 117.07(4) . 3_566 ? S2 P1 Na1 58.25(3) . 3_566 ? Na1 P1 Na1 70.20(3) . 3_566 ? P1 S1 Na1 83.75(4) . . ? P1 S2 Na1 85.21(4) . 3_566 ? P1 S2 Na1 83.16(4) . . ? Na1 S2 Na1 83.35(4) 3_566 . ? C4 O1 C7 116.9(2) . . ? C8 O2 P1 129.45(15) . . ? C8 O2 Na1 120.13(14) . 3_566 ? P1 O2 Na1 104.33(8) . 3_566 ? C2 C1 C6 118.4(2) . . ? C2 C1 P1 121.8(2) . . ? C6 C1 P1 119.8(2) . . ? C1 C2 C3 121.3(3) . . ? C4 C3 C2 119.2(3) . . ? O1 C4 C3 124.9(3) . . ? O1 C4 C5 114.7(3) . . ? C3 C4 C5 120.3(2) . . ? C6 C5 C4 119.9(3) . . ? C5 C6 C1 121.0(3) . . ? O2 C8 C11 107.5(2) . . ? O2 C8 C9 103.5(2) . . ? C11 C8 C9 111.1(2) . . ? O2 C8 C10 112.5(2) . . ? C11 C8 C10 111.5(2) . . ? C9 C8 C10 110.6(2) . . ? C13 O3 C12 113.0(6) . . ? C13 O3 Na1 104.3(4) . . ? C12 O3 Na1 116.9(4) . . ? C14 O4 C15 114.5(6) . . ? C14 O4 Na1 112.7(4) . . ? C15 O4 Na1 119.3(5) . . ? O3 C13 C14 108.6(6) . . ? O4 C14 C13 110.4(5) . . ? C13A O3A C12A 111.2(5) . . ? C13A O3A Na1 107.1(3) . . ? C12A O3A Na1 113.9(4) . . ? C15A O4A C14A 113.4(5) . . ? C15A O4A Na1 125.8(4) . . ? C14A O4A Na1 111.1(3) . . ? O3A C13A C14A 107.6(5) . . ? O3A C13A Na1 47.0(2) . . ? C14A C13A Na1 81.1(3) . . ? O4A C14A C13A 109.1(4) . . ? _diffrn_measured_fraction_theta_max 0.693 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.103 _refine_diff_density_min -0.651 _refine_diff_density_rms 0.157 data_5 _database_code_depnum_ccdc_archive 'CCDC 601697' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H24 K O3 P S2' _chemical_formula_weight 386.53 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' P P 0.1023 0.0942 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.264(6) _cell_length_b 11.2990(9) _cell_length_c 11.3100(8) _cell_angle_alpha 96.849(6) _cell_angle_beta 102.612(6) _cell_angle_gamma 111.286(7) _cell_volume 937.1(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2000 _cell_measurement_theta_min 5 _cell_measurement_theta_max 50 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 408 _exptl_absorpt_coefficient_mu 0.600 _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 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'stoe stadi IV' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7578 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.86 _diffrn_reflns_theta_max 31.83 _reflns_number_total 4099 _reflns_number_gt 3473 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'kuma ccd' _computing_cell_refinement 'kuma ccd' _computing_data_reduction 'kuma ccd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1100P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4099 _refine_ls_number_parameters 203 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.1430 _refine_ls_wR_factor_gt 0.1029 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 P1 P 0.42961(7) 0.31269(5) 0.26777(5) 0.01669(16) Uani 1 1 d . . . K1 K 0.55732(6) 0.36255(5) 0.60413(4) 0.02319(16) Uani 1 1 d . . . S1 S 0.34180(8) 0.15995(5) 0.34146(5) 0.02442(17) Uani 1 1 d . . . S2 S 0.65845(7) 0.46024(5) 0.36516(5) 0.02139(16) Uani 1 1 d . . . C1 C 0.4519(3) 0.2640(2) 0.11531(18) 0.0170(4) Uani 1 1 d . . . C2 C 0.5254(3) 0.3614(2) 0.0526(2) 0.0211(4) Uani 1 1 d . . . H2A H 0.5741 0.4503 0.0941 0.025 Uiso 1 1 calc R . . C3 C 0.5277(3) 0.3298(2) -0.06776(19) 0.0215(4) Uani 1 1 d . . . H3A H 0.5773 0.3967 -0.1092 0.026 Uiso 1 1 calc R . . C4 C 0.4574(3) 0.1999(2) -0.12924(19) 0.0186(4) Uani 1 1 d . . . C5 C 0.3922(3) 0.1020(2) -0.0671(2) 0.0232(5) Uani 1 1 d . . . H5A H 0.3501 0.0132 -0.1073 0.028 Uiso 1 1 calc R . . C6 C 0.3892(3) 0.1353(2) 0.0548(2) 0.0229(4) Uani 1 1 d . . . H6A H 0.3432 0.0683 0.0971 0.027 Uiso 1 1 calc R . . C7 C 0.3790(4) 0.0478(2) -0.3202(2) 0.0299(5) Uani 1 1 d . . . H7A H 0.3830 0.0468 -0.4062 0.045 Uiso 1 1 calc R . . H7B H 0.2529 0.0059 -0.3188 0.045 Uiso 1 1 calc R . . H7C H 0.4480 0.0004 -0.2829 0.045 Uiso 1 1 calc R . . C8 C 0.0875(3) 0.3194(2) 0.1873(2) 0.0221(4) Uani 1 1 d . . . C9 C 0.0443(3) 0.4239(3) 0.1326(3) 0.0347(6) Uani 1 1 d . . . H9A H 0.0805 0.5006 0.1988 0.052 Uiso 1 1 calc R . . H9B H -0.0861 0.3909 0.0924 0.052 Uiso 1 1 calc R . . H9C H 0.1105 0.4479 0.0711 0.052 Uiso 1 1 calc R . . C10 C 0.0029(3) 0.2903(3) 0.2926(2) 0.0343(6) Uani 1 1 d . . . H10A H 0.0498 0.3697 0.3575 0.051 Uiso 1 1 calc R . . H10B H 0.0332 0.2230 0.3272 0.051 Uiso 1 1 calc R . . H10C H -0.1289 0.2595 0.2609 0.051 Uiso 1 1 calc R . . C11 C 0.0252(3) 0.1973(2) 0.0869(2) 0.0294(5) Uani 1 1 d . . . H11A H 0.0525 0.1301 0.1239 0.044 Uiso 1 1 calc R . . H11B H 0.0885 0.2176 0.0233 0.044 Uiso 1 1 calc R . . H11C H -0.1056 0.1655 0.0489 0.044 Uiso 1 1 calc R . . C12 C 0.8890(3) 0.2528(3) 0.5628(2) 0.0309(5) Uani 1 1 d . . . H12A H 0.9688 0.3415 0.5595 0.037 Uiso 1 1 calc R . . H12B H 0.8016 0.2093 0.4798 0.037 Uiso 1 1 calc R . . C13 C 0.9996(4) 0.1755(3) 0.6017(3) 0.0376(6) Uani 1 1 d . . . H13A H 0.9286 0.0810 0.5682 0.045 Uiso 1 1 calc R . . H13B H 1.1112 0.2033 0.5745 0.045 Uiso 1 1 calc R . . C14 C 1.0426(3) 0.2094(3) 0.7415(3) 0.0385(6) Uani 1 1 d . . . H14A H 1.1474 0.2939 0.7774 0.046 Uiso 1 1 calc R . . H14B H 1.0682 0.1410 0.7791 0.046 Uiso 1 1 calc R . . C15 C 0.8702(3) 0.2168(3) 0.7602(2) 0.0296(5) Uani 1 1 d . . . H15A H 0.7846 0.1305 0.7647 0.036 Uiso 1 1 calc R . . H15B H 0.8971 0.2798 0.8379 0.036 Uiso 1 1 calc R . . O1 O 0.28732(18) 0.38101(13) 0.23995(13) 0.0181(3) Uani 1 1 d . . . O2 O 0.4566(2) 0.17980(15) -0.25084(14) 0.0242(4) Uani 1 1 d . . . O3 O 0.7955(2) 0.25837(19) 0.65533(15) 0.0323(4) 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 P1 0.0214(3) 0.0161(3) 0.0132(3) 0.00398(19) 0.0037(2) 0.0088(2) K1 0.0330(3) 0.0245(3) 0.0163(3) 0.00602(18) 0.0049(2) 0.0169(2) S1 0.0378(3) 0.0188(3) 0.0177(3) 0.0080(2) 0.0076(2) 0.0115(2) S2 0.0205(3) 0.0222(3) 0.0185(3) 0.00213(19) 0.0017(2) 0.0082(2) C1 0.0208(10) 0.0189(9) 0.0134(9) 0.0044(7) 0.0042(8) 0.0103(8) C2 0.0205(10) 0.0182(9) 0.0207(11) 0.0018(7) 0.0038(8) 0.0054(8) C3 0.0227(10) 0.0222(10) 0.0193(10) 0.0073(8) 0.0078(8) 0.0066(8) C4 0.0194(10) 0.0242(10) 0.0143(10) 0.0031(7) 0.0054(8) 0.0111(8) C5 0.0339(12) 0.0178(10) 0.0198(11) 0.0040(8) 0.0074(9) 0.0126(9) C6 0.0339(12) 0.0181(10) 0.0210(11) 0.0068(8) 0.0109(9) 0.0128(9) C7 0.0413(13) 0.0278(12) 0.0181(11) 0.0010(9) 0.0094(10) 0.0119(10) C8 0.0157(10) 0.0259(11) 0.0220(11) 0.0059(8) 0.0033(8) 0.0064(8) C9 0.0234(12) 0.0331(13) 0.0445(15) 0.0122(11) -0.0014(10) 0.0132(10) C10 0.0275(12) 0.0488(16) 0.0301(13) 0.0111(11) 0.0146(10) 0.0146(11) C11 0.0251(11) 0.0269(11) 0.0262(12) 0.0007(9) 0.0028(9) 0.0035(9) C12 0.0310(12) 0.0391(14) 0.0260(12) 0.0095(10) 0.0100(10) 0.0161(10) C13 0.0341(13) 0.0509(17) 0.0372(15) 0.0093(12) 0.0155(11) 0.0248(12) C14 0.0296(13) 0.0500(16) 0.0373(15) 0.0134(12) 0.0018(11) 0.0206(12) C15 0.0359(13) 0.0344(13) 0.0247(12) 0.0112(10) 0.0070(10) 0.0205(10) O1 0.0181(7) 0.0169(7) 0.0186(7) 0.0038(5) 0.0031(6) 0.0074(6) O2 0.0327(9) 0.0247(8) 0.0163(8) 0.0043(6) 0.0106(6) 0.0107(7) O3 0.0367(9) 0.0519(11) 0.0250(9) 0.0181(8) 0.0129(7) 0.0310(8) _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 P1 O1 1.6226(17) . ? P1 C1 1.816(2) . ? P1 S1 1.9742(8) . ? P1 S2 1.9830(10) . ? P1 K1 3.6342(7) . ? P1 K1 3.7352(8) 2_666 ? K1 O3 2.635(2) . ? K1 O2 2.7935(16) 1_556 ? K1 O1 2.8715(15) 2_666 ? K1 S2 3.1632(13) 2_666 ? K1 S2 3.2015(8) . ? K1 S1 3.2164(8) . ? K1 C12 3.487(3) . ? K1 P1 3.7352(8) 2_666 ? K1 K1 4.3588(10) 2_666 ? S2 K1 3.1632(13) 2_666 ? C1 C6 1.383(3) . ? C1 C2 1.404(3) . ? C2 C3 1.372(3) . ? C3 C4 1.392(3) . ? C4 O2 1.365(2) . ? C4 C5 1.388(3) . ? C5 C6 1.393(3) . ? C7 O2 1.435(3) . ? C8 O1 1.484(3) . ? C8 C9 1.513(3) . ? C8 C10 1.517(3) . ? C8 C11 1.521(3) . ? C12 O3 1.439(3) . ? C12 C13 1.512(4) . ? C13 C14 1.512(4) . ? C14 C15 1.514(4) . ? C15 O3 1.426(3) . ? O1 K1 2.8715(15) 2_666 ? O2 K1 2.7934(16) 1_554 ? 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 P1 C1 103.30(8) . . ? O1 P1 S1 113.00(7) . . ? C1 P1 S1 110.55(7) . . ? O1 P1 S2 103.07(7) . . ? C1 P1 S2 108.10(7) . . ? S1 P1 S2 117.64(3) . . ? O1 P1 K1 103.11(6) . . ? C1 P1 K1 153.25(7) . . ? S1 P1 K1 61.90(2) . . ? S2 P1 K1 61.44(2) . . ? O1 P1 K1 46.53(5) . 2_666 ? C1 P1 K1 125.00(7) . 2_666 ? S1 P1 K1 123.09(3) . 2_666 ? S2 P1 K1 57.87(4) . 2_666 ? K1 P1 K1 72.510(17) . 2_666 ? O3 K1 O2 69.03(6) . 1_556 ? O3 K1 O1 107.36(6) . 2_666 ? O2 K1 O1 108.86(4) 1_556 2_666 ? O3 K1 S2 160.81(5) . 2_666 ? O2 K1 S2 105.87(4) 1_556 2_666 ? O1 K1 S2 55.72(4) 2_666 2_666 ? O3 K1 S2 97.16(5) . . ? O2 K1 S2 155.23(4) 1_556 . ? O1 K1 S2 94.68(3) 2_666 . ? S2 K1 S2 93.56(2) 2_666 . ? O3 K1 S1 92.80(5) . . ? O2 K1 S1 95.60(4) 1_556 . ? O1 K1 S1 152.49(3) 2_666 . ? S2 K1 S1 106.24(3) 2_666 . ? S2 K1 S1 63.67(2) . . ? O3 K1 C12 22.05(5) . . ? O2 K1 C12 88.52(6) 1_556 . ? O1 K1 C12 111.72(6) 2_666 . ? S2 K1 C12 163.12(5) 2_666 . ? S2 K1 C12 75.32(5) . . ? S1 K1 C12 80.50(5) . . ? O3 K1 P1 104.47(4) . . ? O2 K1 P1 128.35(4) 1_556 . ? O1 K1 P1 121.27(3) 2_666 . ? S2 K1 P1 93.17(2) 2_666 . ? S2 K1 P1 32.959(18) . . ? S1 K1 P1 32.781(14) . . ? C12 K1 P1 84.36(5) . . ? O3 K1 P1 131.57(5) . 2_666 ? O2 K1 P1 113.96(4) 1_556 2_666 ? O1 K1 P1 24.21(3) 2_666 2_666 ? S2 K1 P1 32.066(19) 2_666 2_666 ? S2 K1 P1 90.673(18) . 2_666 ? S1 K1 P1 132.43(2) . 2_666 ? C12 K1 P1 133.53(5) . 2_666 ? P1 K1 P1 107.490(17) . 2_666 ? O3 K1 K1 140.98(4) . 2_666 ? O2 K1 K1 149.92(4) 1_556 2_666 ? O1 K1 K1 69.59(3) 2_666 2_666 ? S2 K1 K1 47.145(14) 2_666 2_666 ? S2 K1 K1 46.41(2) . 2_666 ? S1 K1 K1 82.945(19) . 2_666 ? C12 K1 K1 120.55(5) . 2_666 ? P1 K1 K1 54.816(14) . 2_666 ? P1 K1 K1 52.674(14) 2_666 2_666 ? P1 S1 K1 85.32(3) . . ? P1 S2 K1 90.06(5) . 2_666 ? P1 S2 K1 85.60(3) . . ? K1 S2 K1 86.44(2) 2_666 . ? C6 C1 C2 118.46(19) . . ? C6 C1 P1 122.98(16) . . ? C2 C1 P1 118.42(16) . . ? C3 C2 C1 120.82(19) . . ? C2 C3 C4 120.07(19) . . ? O2 C4 C5 124.80(19) . . ? O2 C4 C3 115.15(18) . . ? C5 C4 C3 120.05(19) . . ? C4 C5 C6 119.3(2) . . ? C1 C6 C5 121.2(2) . . ? O1 C8 C9 103.29(17) . . ? O1 C8 C10 108.50(18) . . ? C9 C8 C10 110.7(2) . . ? O1 C8 C11 112.43(18) . . ? C9 C8 C11 110.3(2) . . ? C10 C8 C11 111.3(2) . . ? O3 C12 C13 105.9(2) . . ? O3 C12 K1 43.42(10) . . ? C13 C12 K1 148.75(17) . . ? C14 C13 C12 101.8(2) . . ? C13 C14 C15 102.55(19) . . ? O3 C15 C14 105.8(2) . . ? C8 O1 P1 129.11(13) . . ? C8 O1 K1 117.55(12) . 2_666 ? P1 O1 K1 109.25(7) . 2_666 ? C4 O2 C7 117.55(17) . . ? C4 O2 K1 128.94(12) . 1_554 ? C7 O2 K1 113.25(12) . 1_554 ? C15 O3 C12 109.86(18) . . ? C15 O3 K1 135.23(14) . . ? C12 O3 K1 114.54(14) . . ? _diffrn_measured_fraction_theta_max 0.638 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.777 _refine_diff_density_min -0.734 _refine_diff_density_rms 0.243 data_6 _database_code_depnum_ccdc_archive 'CCDC 601698' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H26 K O4 P S2' _chemical_formula_weight 404.55 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' P P 0.1023 0.0942 '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.6833(9) _cell_length_b 10.9392(8) _cell_length_c 17.6407(14) _cell_angle_alpha 90.00 _cell_angle_beta 106.174(7) _cell_angle_gamma 90.00 _cell_volume 1980.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 4 _cell_measurement_theta_max 50 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 0.574 _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 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'stoe stadi 4' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15474 _diffrn_reflns_av_R_equivalents 0.0885 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 32.05 _reflns_number_total 4755 _reflns_number_gt 3914 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'kuma ccd' _computing_cell_refinement 'kuma ccd' _computing_data_reduction 'kuma ccd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1030P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4755 _refine_ls_number_parameters 214 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1637 _refine_ls_wR_factor_gt 0.1402 _refine_ls_goodness_of_fit_ref 1.146 _refine_ls_restrained_S_all 1.146 _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 P1 P 0.57943(5) 0.31741(5) 0.40624(3) 0.01908(16) Uani 1 1 d . . . S1 S 0.62745(5) 0.33368(5) 0.52257(3) 0.02300(16) Uani 1 1 d . . . K1 K 0.32678(5) 0.37310(4) 0.51781(3) 0.02560(16) Uani 1 1 d . . . O1 O 0.42707(15) 0.35320(14) 0.37836(9) 0.0230(3) Uani 1 1 d . . . O2 O 0.59833(17) -0.21516(14) 0.34402(9) 0.0286(4) Uani 1 1 d . . . C1 C 0.5839(2) 0.15741(19) 0.38168(12) 0.0208(4) Uani 1 1 d . . . C3 C 0.5093(2) -0.0473(2) 0.39287(12) 0.0234(4) Uani 1 1 d . . . H3A H 0.4535 -0.1021 0.4098 0.028 Uiso 1 1 calc R . . C5 C 0.6752(2) -0.0115(2) 0.32631(13) 0.0253(5) Uani 1 1 d . . . H5A H 0.7325 -0.0408 0.2978 0.030 Uiso 1 1 calc R . . O4 O 0.0733(2) 0.34557(19) 0.53938(13) 0.0462(5) Uani 1 1 d . . . O3 O 0.1672(2) 0.16229(19) 0.45086(13) 0.0473(5) Uani 1 1 d . . . C6 C 0.6683(2) 0.1119(2) 0.34143(13) 0.0248(5) Uani 1 1 d . . . H6A H 0.7228 0.1671 0.3237 0.030 Uiso 1 1 calc R . . C15 C 0.0179(3) 0.4060(3) 0.5940(2) 0.0524(8) Uani 1 1 d . . . H15A H -0.0711 0.4320 0.5669 0.079 Uiso 1 1 calc R . . H15B H 0.0707 0.4777 0.6157 0.079 Uiso 1 1 calc R . . H15C H 0.0160 0.3498 0.6369 0.079 Uiso 1 1 calc R . . C13 C 0.0366(3) 0.2058(3) 0.4342(2) 0.0545(8) Uani 1 1 d . . . H13A H -0.0232 0.1406 0.4066 0.065 Uiso 1 1 calc R . . H13B H 0.0262 0.2765 0.3979 0.065 Uiso 1 1 calc R . . C2 C 0.5041(2) 0.0751(2) 0.40687(13) 0.0237(4) Uani 1 1 d . . . H2A H 0.4452 0.1048 0.4342 0.028 Uiso 1 1 calc R . . C11 C 0.3605(3) 0.5076(2) 0.27585(15) 0.0394(6) Uani 1 1 d . . . H11A H 0.3496 0.5620 0.3177 0.059 Uiso 1 1 calc R . . H11B H 0.2955 0.5279 0.2262 0.059 Uiso 1 1 calc R . . H11C H 0.4481 0.5180 0.2695 0.059 Uiso 1 1 calc R . . C10 C 0.2080(3) 0.3544(4) 0.30594(18) 0.0519(8) Uani 1 1 d . . . H10A H 0.1878 0.4166 0.3407 0.078 Uiso 1 1 calc R . . H10B H 0.2043 0.2731 0.3286 0.078 Uiso 1 1 calc R . . H10C H 0.1444 0.3591 0.2539 0.078 Uiso 1 1 calc R . . C14 C -0.0019(3) 0.2432(3) 0.5050(2) 0.0490(7) Uani 1 1 d . . . H14A H -0.0957 0.2644 0.4902 0.059 Uiso 1 1 calc R . . H14B H 0.0129 0.1751 0.5434 0.059 Uiso 1 1 calc R . . C4 C 0.5972(2) -0.09172(19) 0.35344(12) 0.0222(4) Uani 1 1 d . . . C7 C 0.6682(3) -0.2599(2) 0.29155(15) 0.0342(6) Uani 1 1 d . . . H7A H 0.6512 -0.3475 0.2826 0.051 Uiso 1 1 calc R . . H7B H 0.7617 -0.2466 0.3149 0.051 Uiso 1 1 calc R . . H7C H 0.6395 -0.2162 0.2412 0.051 Uiso 1 1 calc R . . C12 C 0.1776(3) 0.0351(3) 0.46057(18) 0.0456(7) Uani 1 1 d . . . H12A H 0.1299 -0.0051 0.4114 0.068 Uiso 1 1 calc R . . H12B H 0.1407 0.0103 0.5032 0.068 Uiso 1 1 calc R . . H12C H 0.2696 0.0113 0.4739 0.068 Uiso 1 1 calc R . . C9 C 0.3698(3) 0.2881(2) 0.23798(14) 0.0352(6) Uani 1 1 d . . . H9A H 0.3585 0.2040 0.2540 0.053 Uiso 1 1 calc R . . H9B H 0.4596 0.2994 0.2354 0.053 Uiso 1 1 calc R . . H9C H 0.3093 0.3038 0.1859 0.053 Uiso 1 1 calc R . . C8 C 0.3422(2) 0.3763(2) 0.29767(13) 0.0297(5) Uani 1 1 d . . . S2 S 0.68646(6) 0.41126(5) 0.35205(3) 0.02874(18) 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 P1 0.0223(3) 0.0142(3) 0.0213(3) -0.00041(18) 0.0069(2) -0.00074(17) S1 0.0241(3) 0.0227(3) 0.0209(3) -0.00153(19) 0.0040(2) -0.00177(18) K1 0.0265(3) 0.0220(3) 0.0296(3) -0.00075(17) 0.0099(2) -0.00201(16) O1 0.0224(8) 0.0242(8) 0.0208(7) 0.0017(6) 0.0036(6) 0.0039(6) O2 0.0418(10) 0.0161(8) 0.0319(8) -0.0007(6) 0.0168(7) 0.0005(6) C1 0.0246(10) 0.0172(9) 0.0203(10) 0.0007(8) 0.0060(8) -0.0025(7) C3 0.0283(11) 0.0200(10) 0.0235(10) -0.0002(8) 0.0098(8) -0.0055(8) C5 0.0306(12) 0.0206(11) 0.0277(10) -0.0010(8) 0.0129(9) 0.0013(8) O4 0.0320(10) 0.0429(11) 0.0648(14) 0.0014(10) 0.0156(10) -0.0073(8) O3 0.0325(11) 0.0435(12) 0.0616(13) 0.0060(9) 0.0059(9) -0.0088(8) C6 0.0269(11) 0.0206(10) 0.0301(11) 0.0017(8) 0.0134(9) -0.0002(8) C15 0.0393(17) 0.0520(19) 0.071(2) 0.0006(16) 0.0248(15) -0.0026(13) C13 0.0341(16) 0.0553(19) 0.065(2) 0.0029(16) -0.0016(14) -0.0046(13) C2 0.0258(11) 0.0222(11) 0.0259(11) -0.0029(8) 0.0116(9) -0.0021(8) C11 0.0533(17) 0.0303(13) 0.0293(12) 0.0035(10) 0.0026(11) 0.0105(11) C10 0.0271(15) 0.087(2) 0.0375(15) 0.0136(15) 0.0027(12) 0.0079(14) C14 0.0300(14) 0.0539(19) 0.0608(18) 0.0045(14) 0.0091(13) -0.0129(12) C4 0.0280(11) 0.0161(10) 0.0214(10) -0.0003(7) 0.0053(8) 0.0012(8) C7 0.0545(16) 0.0182(11) 0.0359(12) -0.0004(9) 0.0226(11) 0.0054(10) C12 0.0442(16) 0.0392(16) 0.0488(16) 0.0010(12) 0.0052(13) -0.0106(12) C9 0.0451(15) 0.0301(12) 0.0241(11) -0.0024(10) -0.0009(10) -0.0034(10) C8 0.0310(13) 0.0333(13) 0.0207(11) 0.0021(9) 0.0007(9) 0.0057(9) S2 0.0369(3) 0.0198(3) 0.0349(3) -0.0006(2) 0.0188(3) -0.0045(2) _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 P1 O1 1.6121(16) . ? P1 C1 1.807(2) . ? P1 S2 1.9708(8) . ? P1 S1 1.9799(7) . ? P1 K1 3.6762(7) 3_666 ? P1 K1 3.8066(8) . ? S1 K1 3.2188(8) . ? S1 K1 3.3510(7) 3_666 ? K1 O4 2.854(2) . ? K1 O2 2.9121(17) 3_656 ? K1 O3 2.915(2) . ? K1 O1 2.9521(16) . ? K1 S2 3.3221(7) 3_666 ? K1 S1 3.3510(7) 3_666 ? K1 P1 3.6761(7) 3_666 ? K1 K1 4.8060(10) 3_666 ? O1 C8 1.481(3) . ? O2 C4 1.361(2) . ? O2 C7 1.427(3) . ? O2 K1 2.9121(17) 3_656 ? C1 C6 1.386(3) . ? C1 C2 1.395(3) . ? C3 C2 1.366(3) . ? C3 C4 1.403(3) . ? C5 C6 1.383(3) . ? C5 C4 1.384(3) . ? O4 C14 1.412(4) . ? O4 C15 1.426(4) . ? O3 C12 1.402(4) . ? O3 C13 1.425(4) . ? C13 C14 1.478(5) . ? C11 C8 1.514(4) . ? C10 C8 1.500(4) . ? C9 C8 1.517(3) . ? S2 K1 3.3221(8) 3_666 ? 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 P1 C1 104.72(9) . . ? O1 P1 S2 113.48(6) . . ? C1 P1 S2 109.30(7) . . ? O1 P1 S1 104.03(6) . . ? C1 P1 S1 108.61(7) . . ? S2 P1 S1 115.98(3) . . ? O1 P1 K1 92.12(6) . 3_666 ? C1 P1 K1 163.09(7) . 3_666 ? S2 P1 K1 63.96(2) . 3_666 ? S1 P1 K1 64.77(2) . 3_666 ? O1 P1 K1 46.98(5) . . ? C1 P1 K1 110.42(7) . . ? S2 P1 K1 139.30(3) . . ? S1 P1 K1 57.72(2) . . ? K1 P1 K1 79.903(15) 3_666 . ? P1 S1 K1 90.94(3) . . ? P1 S1 K1 82.92(2) . 3_666 ? K1 S1 K1 94.007(18) . 3_666 ? O4 K1 O2 82.84(6) . 3_656 ? O4 K1 O3 60.06(6) . . ? O2 K1 O3 82.13(5) 3_656 . ? O4 K1 O1 132.96(6) . . ? O2 K1 O1 125.09(4) 3_656 . ? O3 K1 O1 84.90(6) . . ? O4 K1 S1 163.66(5) . . ? O2 K1 S1 81.91(4) 3_656 . ? O3 K1 S1 111.80(5) . . ? O1 K1 S1 54.60(3) . . ? O4 K1 S2 76.00(5) . 3_666 ? O2 K1 S2 84.12(3) 3_656 3_666 ? O3 K1 S2 135.15(5) . 3_666 ? O1 K1 S2 136.34(4) . 3_666 ? S1 K1 S2 108.14(2) . 3_666 ? O4 K1 S1 109.23(5) . 3_666 ? O2 K1 S1 136.34(4) 3_656 3_666 ? O3 K1 S1 140.77(5) . 3_666 ? O1 K1 S1 77.59(3) . 3_666 ? S1 K1 S1 85.993(18) . 3_666 ? S2 K1 S1 60.264(16) 3_666 3_666 ? O4 K1 P1 102.77(5) . 3_666 ? O2 K1 P1 104.95(4) 3_656 3_666 ? O3 K1 P1 160.99(5) . 3_666 ? O1 K1 P1 104.26(3) . 3_666 ? S1 K1 P1 86.856(17) . 3_666 ? S2 K1 P1 32.207(14) 3_666 3_666 ? S1 K1 P1 32.308(13) 3_666 3_666 ? O4 K1 P1 152.62(5) . . ? O2 K1 P1 105.59(4) 3_656 . ? O3 K1 P1 94.75(5) . . ? O1 K1 P1 23.53(3) . . ? S1 K1 P1 31.335(13) . . ? S2 K1 P1 130.073(19) 3_666 . ? S1 K1 P1 82.925(16) 3_666 . ? P1 K1 P1 100.098(15) 3_666 . ? O4 K1 K1 150.74(5) . 3_666 ? O2 K1 K1 114.22(4) 3_656 3_666 ? O3 K1 K1 142.08(5) . 3_666 ? O1 K1 K1 57.46(3) . 3_666 ? S1 K1 K1 44.072(13) . 3_666 ? S2 K1 K1 82.108(17) 3_666 3_666 ? S1 K1 K1 41.922(12) 3_666 3_666 ? P1 K1 K1 51.241(12) 3_666 3_666 ? P1 K1 K1 48.857(12) . 3_666 ? C8 O1 P1 129.08(15) . . ? C8 O1 K1 121.42(13) . . ? P1 O1 K1 109.50(7) . . ? C4 O2 C7 116.30(17) . . ? C4 O2 K1 119.74(12) . 3_656 ? C7 O2 K1 105.55(13) . 3_656 ? C6 C1 C2 118.3(2) . . ? C6 C1 P1 122.35(16) . . ? C2 C1 P1 119.29(16) . . ? C2 C3 C4 119.73(19) . . ? C6 C5 C4 118.9(2) . . ? C14 O4 C15 111.3(2) . . ? C14 O4 K1 118.28(18) . . ? C15 O4 K1 128.99(18) . . ? C12 O3 C13 113.4(2) . . ? C12 O3 K1 135.86(17) . . ? C13 O3 K1 104.36(18) . . ? C5 C6 C1 121.8(2) . . ? O3 C13 C14 113.9(3) . . ? C3 C2 C1 121.1(2) . . ? O4 C14 C13 108.9(3) . . ? O2 C4 C5 124.1(2) . . ? O2 C4 C3 115.73(19) . . ? C5 C4 C3 120.19(19) . . ? O1 C8 C10 103.0(2) . . ? O1 C8 C11 108.59(19) . . ? C10 C8 C11 111.8(2) . . ? O1 C8 C9 111.92(19) . . ? C10 C8 C9 110.0(2) . . ? C11 C8 C9 111.3(2) . . ? P1 S2 K1 83.83(3) . 3_666 ? _diffrn_measured_fraction_theta_max 0.689 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.289 _refine_diff_density_min -0.737 _refine_diff_density_rms 0.165 data_7 _database_code_depnum_ccdc_archive 'CCDC 601699' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H64 Cd2 O8 P4 S8' _chemical_formula_weight 1326.11 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' P P 0.1023 0.0942 '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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3883(9) _cell_length_b 11.8699(9) _cell_length_c 12.2242(9) _cell_angle_alpha 74.356(6) _cell_angle_beta 65.181(5) _cell_angle_gamma 77.253(6) _cell_volume 1433.30(19) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 10398 _cell_measurement_theta_min 3.47 _cell_measurement_theta_max 56.37 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 676 _exptl_absorpt_coefficient_mu 1.190 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7967 _exptl_absorpt_correction_T_max 0.8902 _exptl_absorpt_process_details 'stoe x-shape' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'stoe ipds 2' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12818 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 28.23 _reflns_number_total 6527 _reflns_number_gt 5479 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'stoe winexpose' _computing_cell_refinement 'stoe winexpose' _computing_data_reduction 'stoe winexpose' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0462P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6527 _refine_ls_number_parameters 291 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0405 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0763 _refine_ls_wR_factor_gt 0.0732 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.014 _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 Cd1 Cd 0.645117(15) 0.401939(15) 0.396260(18) 0.02355(6) Uani 1 1 d . . . P1 P 0.60771(5) 0.72021(5) 0.37097(6) 0.02078(12) Uani 1 1 d . . . P2 P 0.92598(5) 0.27556(5) 0.29142(6) 0.02048(12) Uani 1 1 d . . . S1 S 0.52649(5) 0.60116(5) 0.33943(6) 0.02175(12) Uani 1 1 d . . . S2 S 0.52577(6) 0.73645(6) 0.54724(6) 0.02648(13) Uani 1 1 d . . . S3 S 0.82352(6) 0.34288(6) 0.18513(6) 0.02697(13) Uani 1 1 d . . . S4 S 0.84322(6) 0.33568(6) 0.45024(6) 0.02816(14) Uani 1 1 d . . . O1 O 0.60316(16) 0.84043(15) 0.27671(18) 0.0268(4) Uani 1 1 d . A . O2 O 1.18354(17) 0.6093(2) 0.18342(19) 0.0350(5) Uani 1 1 d . . . O3 O 0.93386(18) 0.13682(16) 0.33780(19) 0.0299(4) Uani 1 1 d . . . O4 O 1.48103(17) 0.36484(19) 0.02965(19) 0.0336(4) Uani 1 1 d . . . C1 C 0.4964(3) 0.9220(2) 0.2471(3) 0.0350(6) Uani 1 1 d D . . C2 C 0.5562(7) 1.0352(6) 0.1833(7) 0.0464(7) Uiso 0.50 1 d PD A 1 H2A H 0.6221 1.0269 0.1017 0.070 Uiso 0.50 1 calc PR A 1 H2B H 0.5972 1.0527 0.2321 0.070 Uiso 0.50 1 calc PR A 1 H2C H 0.4881 1.0996 0.1747 0.070 Uiso 0.50 1 calc PR A 1 C2A C 0.5653(7) 1.0156(7) 0.1455(7) 0.0464(7) Uiso 0.50 1 d PD A 2 H2AA H 0.6221 0.9815 0.0732 0.070 Uiso 0.50 1 calc PR A 2 H2AB H 0.6180 1.0492 0.1718 0.070 Uiso 0.50 1 calc PR A 2 H2AC H 0.5012 1.0778 0.1245 0.070 Uiso 0.50 1 calc PR A 2 C3 C 0.3749(7) 0.9340(6) 0.3560(7) 0.0464(7) Uiso 0.50 1 d PD A 1 H3A H 0.3159 0.8810 0.3634 0.070 Uiso 0.50 1 calc PR A 1 H3B H 0.3329 1.0156 0.3470 0.070 Uiso 0.50 1 calc PR A 1 H3C H 0.3951 0.9134 0.4300 0.070 Uiso 0.50 1 calc PR A 1 C3A C 0.4034(7) 0.9739(6) 0.3653(6) 0.0464(7) Uiso 0.50 1 d PD A 2 H3AA H 0.4559 0.9986 0.3989 0.070 Uiso 0.50 1 calc PR A 2 H3AC H 0.3513 0.9133 0.4273 0.070 Uiso 0.50 1 calc PR A 2 H3AD H 0.3453 1.0419 0.3431 0.070 Uiso 0.50 1 calc PR A 2 C4 C 0.4757(7) 0.8698(6) 0.1528(7) 0.0464(7) Uiso 0.50 1 d PD A 1 H4A H 0.5606 0.8470 0.0910 0.070 Uiso 0.50 1 calc PR A 1 H4B H 0.4243 0.9293 0.1122 0.070 Uiso 0.50 1 calc PR A 1 H4C H 0.4293 0.8004 0.1961 0.070 Uiso 0.50 1 calc PR A 1 C4A C 0.4164(7) 0.8645(6) 0.2139(7) 0.0464(7) Uiso 0.50 1 d PD A 2 H4AA H 0.4718 0.8313 0.1407 0.070 Uiso 0.50 1 calc PR A 2 H4AB H 0.3475 0.9229 0.1966 0.070 Uiso 0.50 1 calc PR A 2 H4AC H 0.3769 0.8013 0.2825 0.070 Uiso 0.50 1 calc PR A 2 C5 C 0.7807(2) 0.6827(2) 0.3223(2) 0.0216(5) Uani 1 1 d . . . C6 C 0.8446(2) 0.6565(2) 0.4027(2) 0.0236(5) Uani 1 1 d . . . H6A H 0.7954 0.6565 0.4876 0.028 Uiso 1 1 calc R . . C7 C 0.9799(2) 0.6303(2) 0.3607(2) 0.0251(5) Uani 1 1 d . . . H7A H 1.0227 0.6121 0.4165 0.030 Uiso 1 1 calc R . . C8 C 1.0515(2) 0.6309(2) 0.2365(3) 0.0259(5) Uani 1 1 d . . . C9 C 0.9877(3) 0.6551(3) 0.1553(3) 0.0391(7) Uani 1 1 d . . . H9A H 1.0366 0.6536 0.0707 0.047 Uiso 1 1 calc R . . C10 C 0.8534(2) 0.6814(3) 0.1981(3) 0.0344(6) Uani 1 1 d . . . H10A H 0.8105 0.6985 0.1425 0.041 Uiso 1 1 calc R . . C11 C 1.2561(2) 0.5942(3) 0.2580(3) 0.0320(6) Uani 1 1 d . . . H11A H 1.3494 0.5795 0.2083 0.048 Uiso 1 1 calc R . . H11B H 1.2299 0.5270 0.3264 0.048 Uiso 1 1 calc R . . H11C H 1.2391 0.6657 0.2905 0.048 Uiso 1 1 calc R . . C12 C 0.9657(3) 0.0398(3) 0.2713(3) 0.0391(7) Uani 1 1 d . . . C13 C 1.0169(5) -0.0633(3) 0.3518(5) 0.0664(12) Uani 1 1 d . . . H13A H 0.9481 -0.0800 0.4338 0.100 Uiso 1 1 calc R . . H13B H 1.0921 -0.0431 0.3586 0.100 Uiso 1 1 calc R . . H13C H 1.0432 -0.1331 0.3147 0.100 Uiso 1 1 calc R . . C14 C 0.8411(4) 0.0187(4) 0.2692(5) 0.0615(11) Uani 1 1 d . . . H14A H 0.8112 0.0864 0.2165 0.092 Uiso 1 1 calc R . . H14B H 0.7743 0.0088 0.3529 0.092 Uiso 1 1 calc R . . H14C H 0.8566 -0.0526 0.2369 0.092 Uiso 1 1 calc R . . C15 C 1.0701(4) 0.0676(3) 0.1429(4) 0.0550(10) Uani 1 1 d . . . H15A H 1.0352 0.1340 0.0927 0.082 Uiso 1 1 calc R . . H15B H 1.0965 -0.0016 0.1049 0.082 Uiso 1 1 calc R . . H15C H 1.1458 0.0885 0.1483 0.082 Uiso 1 1 calc R . . C16 C 1.0923(2) 0.3085(2) 0.2131(2) 0.0213(5) Uani 1 1 d . . . C17 C 1.1734(2) 0.2776(2) 0.2788(2) 0.0255(5) Uani 1 1 d . . . H17A H 1.1393 0.2430 0.3639 0.031 Uiso 1 1 calc R . . C18 C 1.3038(2) 0.2968(2) 0.2211(3) 0.0256(5) Uani 1 1 d . . . H18A H 1.3579 0.2771 0.2670 0.031 Uiso 1 1 calc R . . C19 C 1.3544(2) 0.3450(2) 0.0959(2) 0.0244(5) Uani 1 1 d . . . C20 C 1.2736(2) 0.3766(2) 0.0301(3) 0.0276(5) Uani 1 1 d . . . H20A H 1.3082 0.4095 -0.0554 0.033 Uiso 1 1 calc R . . C21 C 1.1426(2) 0.3605(2) 0.0888(2) 0.0255(5) Uani 1 1 d . . . H21A H 1.0873 0.3849 0.0440 0.031 Uiso 1 1 calc R . . C22 C 1.5631(2) 0.3526(3) 0.0960(3) 0.0325(6) Uani 1 1 d . . . H22A H 1.6510 0.3692 0.0377 0.049 Uiso 1 1 calc R . . H22B H 1.5673 0.2720 0.1437 0.049 Uiso 1 1 calc R . . H22C H 1.5271 0.4083 0.1519 0.049 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 Cd1 0.01428(8) 0.02777(9) 0.02591(11) -0.00520(7) -0.00599(6) -0.00105(6) P1 0.0155(3) 0.0252(3) 0.0214(3) -0.0038(2) -0.0070(2) -0.0033(2) P2 0.0144(2) 0.0259(3) 0.0212(3) -0.0051(2) -0.0069(2) -0.0022(2) S1 0.0166(2) 0.0261(3) 0.0233(3) -0.0042(2) -0.0084(2) -0.0035(2) S2 0.0205(3) 0.0364(3) 0.0232(3) -0.0095(3) -0.0053(2) -0.0069(2) S3 0.0166(2) 0.0429(3) 0.0217(3) -0.0084(3) -0.0085(2) 0.0002(2) S4 0.0181(3) 0.0445(4) 0.0226(3) -0.0111(3) -0.0074(2) -0.0007(2) O1 0.0218(8) 0.0265(8) 0.0295(11) 0.0005(7) -0.0107(7) -0.0038(7) O2 0.0160(8) 0.0623(13) 0.0303(11) -0.0209(10) -0.0081(7) 0.0009(8) O3 0.0272(9) 0.0275(9) 0.0349(12) -0.0042(8) -0.0121(8) -0.0056(7) O4 0.0176(8) 0.0550(12) 0.0279(11) -0.0068(9) -0.0059(7) -0.0116(8) C1 0.0298(13) 0.0298(13) 0.0440(19) 0.0004(12) -0.0204(12) 0.0020(10) C5 0.0166(10) 0.0252(11) 0.0237(13) -0.0072(9) -0.0068(8) -0.0029(8) C6 0.0194(11) 0.0296(12) 0.0205(13) -0.0030(9) -0.0060(9) -0.0060(9) C7 0.0201(11) 0.0317(12) 0.0263(14) -0.0053(10) -0.0115(9) -0.0040(9) C8 0.0160(10) 0.0346(13) 0.0293(14) -0.0118(11) -0.0077(9) -0.0027(9) C9 0.0232(13) 0.072(2) 0.0247(16) -0.0181(14) -0.0083(10) -0.0021(12) C10 0.0209(12) 0.0611(18) 0.0252(15) -0.0153(13) -0.0100(10) -0.0021(11) C11 0.0192(11) 0.0493(16) 0.0323(16) -0.0137(12) -0.0119(10) -0.0026(10) C12 0.0369(15) 0.0303(13) 0.052(2) -0.0146(13) -0.0148(13) -0.0047(11) C13 0.083(3) 0.0293(16) 0.092(4) -0.0078(18) -0.044(3) -0.0008(17) C14 0.055(2) 0.062(2) 0.085(3) -0.028(2) -0.028(2) -0.0218(18) C15 0.054(2) 0.0453(18) 0.057(2) -0.0299(17) -0.0027(17) -0.0045(15) C16 0.0156(10) 0.0249(11) 0.0226(13) -0.0061(9) -0.0063(8) -0.0016(8) C17 0.0193(11) 0.0334(12) 0.0220(13) -0.0002(10) -0.0089(9) -0.0043(9) C18 0.0164(10) 0.0308(12) 0.0303(15) -0.0046(10) -0.0110(9) -0.0022(8) C19 0.0158(10) 0.0306(12) 0.0262(14) -0.0083(10) -0.0060(9) -0.0030(8) C20 0.0207(11) 0.0412(14) 0.0204(13) -0.0034(10) -0.0066(9) -0.0090(10) C21 0.0214(11) 0.0338(12) 0.0231(14) -0.0070(10) -0.0091(9) -0.0042(9) C22 0.0190(11) 0.0436(15) 0.0358(17) -0.0051(12) -0.0112(10) -0.0077(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 Cd1 S4 2.5160(7) . ? Cd1 S1 2.5282(6) . ? Cd1 S2 2.5756(6) 2_666 ? Cd1 S3 2.6881(7) . ? Cd1 S1 2.9877(7) 2_666 ? P1 O1 1.5804(19) . ? P1 C5 1.790(2) . ? P1 S2 2.0018(9) . ? P1 S1 2.0424(8) . ? P2 O3 1.5860(19) . ? P2 C16 1.805(2) . ? P2 S3 1.9973(9) . ? P2 S4 2.0202(9) . ? S1 Cd1 2.9877(7) 2_666 ? S2 Cd1 2.5756(6) 2_666 ? O1 C1 1.486(3) . ? O2 C8 1.360(3) . ? O2 C11 1.423(3) . ? O3 C12 1.481(3) . ? O4 C19 1.363(3) . ? O4 C22 1.437(3) . ? C1 C4A 1.482(7) . ? C1 C3 1.476(7) . ? C1 C2A 1.488(7) . ? C1 C2 1.506(7) . ? C1 C4 1.564(7) . ? C1 C3A 1.580(7) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C2A H2AA 0.9800 . ? C2A H2AB 0.9800 . ? C2A H2AC 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C3A H3AA 0.9800 . ? C3A H3AC 0.9800 . ? C3A H3AD 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C4A H4AA 0.9800 . ? C4A H4AB 0.9800 . ? C4A H4AC 0.9800 . ? C5 C6 1.388(4) . ? C5 C10 1.394(4) . ? C6 C7 1.395(3) . ? C6 H6A 0.9500 . ? C7 C8 1.388(4) . ? C7 H7A 0.9500 . ? C8 C9 1.397(4) . ? C9 C10 1.385(4) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C14 1.506(4) . ? C12 C15 1.521(5) . ? C12 C13 1.524(5) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.396(3) . ? C16 C21 1.392(4) . ? C17 C18 1.392(3) . ? C17 H17A 0.9500 . ? C18 C19 1.391(4) . ? C18 H18A 0.9500 . ? C19 C20 1.393(4) . ? C20 C21 1.390(3) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S4 Cd1 S1 134.00(2) . . ? S4 Cd1 S2 122.13(2) . 2_666 ? S1 Cd1 S2 101.85(2) . 2_666 ? S4 Cd1 S3 79.16(2) . . ? S1 Cd1 S3 106.97(2) . . ? S2 Cd1 S3 100.91(2) 2_666 . ? S4 Cd1 S1 90.77(2) . 2_666 ? S1 Cd1 S1 89.21(2) . 2_666 ? S2 Cd1 S1 73.578(19) 2_666 2_666 ? S3 Cd1 S1 163.75(2) . 2_666 ? O1 P1 C5 99.30(10) . . ? O1 P1 S2 113.90(8) . . ? C5 P1 S2 111.36(9) . . ? O1 P1 S1 109.04(8) . . ? C5 P1 S1 110.85(8) . . ? S2 P1 S1 111.75(4) . . ? O3 P2 C16 106.18(10) . . ? O3 P2 S3 115.12(8) . . ? C16 P2 S3 111.60(9) . . ? O3 P2 S4 102.74(8) . . ? C16 P2 S4 109.30(8) . . ? S3 P2 S4 111.38(4) . . ? P1 S1 Cd1 105.48(3) . . ? P1 S1 Cd1 81.19(3) . 2_666 ? Cd1 S1 Cd1 90.79(2) . 2_666 ? P1 S2 Cd1 93.27(3) . 2_666 ? P2 S3 Cd1 81.36(3) . . ? P2 S4 Cd1 85.43(3) . . ? C1 O1 P1 133.77(16) . . ? C8 O2 C11 118.1(2) . . ? C12 O3 P2 131.4(2) . . ? C19 O4 C22 117.9(2) . . ? O1 C1 C4A 113.8(3) . . ? O1 C1 C3 113.4(4) . . ? C4A C1 C3 82.9(4) . . ? O1 C1 C2A 103.7(4) . . ? C4A C1 C2A 113.0(5) . . ? C3 C1 C2A 129.1(5) . . ? O1 C1 C2 102.9(4) . . ? C4A C1 C2 129.3(5) . . ? C3 C1 C2 113.7(4) . . ? C2A C1 C2 20.6(4) . . ? O1 C1 C4 105.0(3) . . ? C4A C1 C4 29.0(3) . . ? C3 C1 C4 111.4(4) . . ? C2A C1 C4 90.0(4) . . ? C2 C1 C4 109.8(4) . . ? O1 C1 C3A 107.6(4) . . ? C4A C1 C3A 107.7(4) . . ? C3 C1 C3A 25.7(3) . . ? C2A C1 C3A 110.9(4) . . ? C2 C1 C3A 92.1(4) . . ? C4 C1 C3A 135.0(4) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C2A H2AA 109.5 . . ? C1 C2A H2AB 109.5 . . ? H2AA C2A H2AB 109.5 . . ? C1 C2A H2AC 109.5 . . ? H2AA C2A H2AC 109.5 . . ? H2AB C2A H2AC 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C3A H3AA 109.5 . . ? C1 C3A H3AC 109.5 . . ? H3AA C3A H3AC 109.5 . . ? C1 C3A H3AD 109.5 . . ? H3AA C3A H3AD 109.5 . . ? H3AC C3A H3AD 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C1 C4A H4AA 109.5 . . ? C1 C4A H4AB 109.5 . . ? H4AA C4A H4AB 109.5 . . ? C1 C4A H4AC 109.5 . . ? H4AA C4A H4AC 109.5 . . ? H4AB C4A H4AC 109.5 . . ? C6 C5 C10 119.2(2) . . ? C6 C5 P1 122.72(19) . . ? C10 C5 P1 118.10(19) . . ? C5 C6 C7 121.0(2) . . ? C5 C6 H6A 119.5 . . ? C7 C6 H6A 119.5 . . ? C8 C7 C6 119.3(2) . . ? C8 C7 H7A 120.3 . . ? C6 C7 H7A 120.3 . . ? O2 C8 C7 125.2(2) . . ? O2 C8 C9 114.8(2) . . ? C7 C8 C9 120.0(2) . . ? C10 C9 C8 120.1(3) . . ? C10 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? C9 C10 C5 120.4(3) . . ? C9 C10 H10A 119.8 . . ? C5 C10 H10A 119.8 . . ? O2 C11 H11A 109.5 . . ? O2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O3 C12 C14 107.7(3) . . ? O3 C12 C15 111.4(2) . . ? C14 C12 C15 112.4(3) . . ? O3 C12 C13 102.5(3) . . ? C14 C12 C13 111.6(3) . . ? C15 C12 C13 110.8(3) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 119.3(2) . . ? C17 C16 P2 118.73(19) . . ? C21 C16 P2 121.96(19) . . ? C18 C17 C16 120.8(2) . . ? C18 C17 H17A 119.6 . . ? C16 C17 H17A 119.6 . . ? C17 C18 C19 119.5(2) . . ? C17 C18 H18A 120.3 . . ? C19 C18 H18A 120.3 . . ? O4 C19 C20 115.7(2) . . ? O4 C19 C18 124.5(2) . . ? C20 C19 C18 119.9(2) . . ? C19 C20 C21 120.5(2) . . ? C19 C20 H20A 119.8 . . ? C21 C20 H20A 119.8 . . ? C20 C21 C16 120.0(2) . . ? C20 C21 H21A 120.0 . . ? C16 C21 H21A 120.0 . . ? O4 C22 H22A 109.5 . . ? O4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 1.038 _refine_diff_density_min -0.543 _refine_diff_density_rms 0.109 data_8 _database_code_depnum_ccdc_archive 'CCDC 601700' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H96 K4 O8 P4 S12' _chemical_formula_weight 1610.37 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' P P 0.1023 0.0942 '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 tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 26.4622(16) _cell_length_b 26.4622(16) _cell_length_c 11.2432(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7873.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 12555 _cell_measurement_theta_min 3.83 _cell_measurement_theta_max 54.02 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.359 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3392 _exptl_absorpt_coefficient_mu 0.672 _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 110(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 'stoe ipds2' _diffrn_measurement_method rotation _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11638 _diffrn_reflns_av_R_equivalents 0.0827 _diffrn_reflns_av_sigmaI/netI 0.0681 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 27.02 _reflns_number_total 4276 _reflns_number_gt 2963 _reflns_threshold_expression >2sigma(I) _computing_data_collection x-area _computing_cell_refinement x-area _computing_data_reduction x-area _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1772P)^2^+14.1495P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4276 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1233 _refine_ls_R_factor_gt 0.0917 _refine_ls_wR_factor_ref 0.2778 _refine_ls_wR_factor_gt 0.2527 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 P1 P 0.96224(6) 0.12318(5) 0.32362(12) 0.0344(4) Uani 1 1 d . . . K1 K 0.93896(5) 0.16344(5) 0.01964(11) 0.0411(4) Uani 1 1 d . . . S1 S 0.95962(6) 0.19686(5) 0.29242(13) 0.0405(4) Uani 1 1 d . . . S2 S 1.01256(6) 0.08531(6) 0.22764(13) 0.0421(4) Uani 1 1 d . . . S3 S 0.89620(6) 0.08207(6) 0.27753(14) 0.0437(4) Uani 1 1 d . . . O1 O 0.97886(19) 0.09223(15) 0.8481(3) 0.0438(11) Uani 1 1 d . . . O2 O 0.8640(2) 0.1089(2) -0.0925(5) 0.0675(15) Uani 1 1 d . . . C1 C 0.9714(2) 0.1127(2) 0.4816(4) 0.0327(11) Uani 1 1 d . . . C2 C 0.9782(2) 0.1532(2) 0.5610(5) 0.0378(12) Uani 1 1 d . . . H2A H 0.9802 0.1867 0.5311 0.045 Uiso 1 1 calc R . . C3 C 0.9819(2) 0.1447(2) 0.6819(5) 0.0383(12) Uani 1 1 d . . . H3A H 0.9872 0.1724 0.7344 0.046 Uiso 1 1 calc R . . C4 C 0.9778(2) 0.0961(2) 0.7268(5) 0.0353(12) Uani 1 1 d . . . C5 C 0.9741(2) 0.0554(2) 0.6498(5) 0.0336(11) Uani 1 1 d . . . H5A H 0.9741 0.0218 0.6798 0.040 Uiso 1 1 calc R . . C6 C 0.9705(2) 0.0641(2) 0.5293(5) 0.0354(12) Uani 1 1 d . . . H6A H 0.9673 0.0361 0.4771 0.042 Uiso 1 1 calc R . . C7 C 0.9696(4) 0.0434(2) 0.8975(5) 0.0561(19) Uani 1 1 d . . . H7A H 0.9710 0.0454 0.9845 0.084 Uiso 1 1 calc R . . H7B H 0.9954 0.0197 0.8691 0.084 Uiso 1 1 calc R . . H7C H 0.9361 0.0316 0.8729 0.084 Uiso 1 1 calc R . . C8 C 0.8384(3) 0.1114(3) 0.3451(6) 0.0504(16) Uani 1 1 d . . . C9 C 0.8000(3) 0.0670(3) 0.3436(9) 0.066(2) Uani 1 1 d . . . H9A H 0.7678 0.0782 0.3779 0.100 Uiso 1 1 calc R . . H9B H 0.8134 0.0388 0.3905 0.100 Uiso 1 1 calc R . . H9C H 0.7945 0.0559 0.2614 0.100 Uiso 1 1 calc R . . C10 C 0.8478(3) 0.1291(3) 0.4688(7) 0.0595(19) Uani 1 1 d . . . H10A H 0.8168 0.1441 0.5010 0.089 Uiso 1 1 calc R . . H10B H 0.8748 0.1544 0.4684 0.089 Uiso 1 1 calc R . . H10C H 0.8579 0.1003 0.5183 0.089 Uiso 1 1 calc R . . C11 C 0.8202(3) 0.1533(3) 0.2680(9) 0.066(2) Uani 1 1 d . . . H11A H 0.7901 0.1686 0.3036 0.099 Uiso 1 1 calc R . . H11B H 0.8118 0.1399 0.1891 0.099 Uiso 1 1 calc R . . H11C H 0.8469 0.1788 0.2604 0.099 Uiso 1 1 calc R . . C12 C 0.8261(5) 0.0759(6) -0.0536(12) 0.114(5) Uani 1 1 d . . . H12A H 0.8232 0.0771 0.0341 0.137 Uiso 1 1 calc R . . H12B H 0.8342 0.0408 -0.0776 0.137 Uiso 1 1 calc R . . C13 C 0.7791(4) 0.0919(6) -0.1078(13) 0.114(5) Uani 1 1 d . . . H13A H 0.7588 0.1123 -0.0516 0.137 Uiso 1 1 calc R . . H13B H 0.7589 0.0624 -0.1336 0.137 Uiso 1 1 calc R . . C14 C 0.7957(4) 0.1234(6) -0.2142(11) 0.107(4) Uani 1 1 d . . . H14A H 0.7863 0.1065 -0.2895 0.128 Uiso 1 1 calc R . . H14B H 0.7795 0.1571 -0.2121 0.128 Uiso 1 1 calc R . . C15 C 0.8491(4) 0.1283(4) -0.2059(8) 0.074(2) Uani 1 1 d . . . H15A H 0.8591 0.1642 -0.2132 0.089 Uiso 1 1 calc R . . H15B H 0.8657 0.1090 -0.2703 0.089 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 P1 0.0417(8) 0.0345(7) 0.0270(7) 0.0041(5) 0.0013(6) 0.0010(6) K1 0.0457(7) 0.0442(7) 0.0335(6) -0.0013(5) -0.0008(5) -0.0013(5) S1 0.0551(9) 0.0333(7) 0.0330(7) 0.0065(5) 0.0046(6) 0.0060(6) S2 0.0538(9) 0.0381(8) 0.0343(7) -0.0014(6) 0.0092(6) 0.0034(6) S3 0.0469(9) 0.0483(9) 0.0360(7) 0.0031(6) -0.0054(6) -0.0037(6) O1 0.078(3) 0.031(2) 0.0228(18) 0.0026(15) -0.0072(18) -0.0024(19) O2 0.077(4) 0.062(3) 0.063(3) -0.005(3) -0.010(3) -0.015(3) C1 0.043(3) 0.033(3) 0.022(2) 0.002(2) -0.001(2) 0.001(2) C2 0.053(3) 0.032(3) 0.029(3) 0.003(2) -0.003(2) -0.004(2) C3 0.053(3) 0.032(3) 0.029(3) 0.002(2) -0.008(2) -0.004(2) C4 0.050(3) 0.033(3) 0.022(2) 0.000(2) -0.004(2) -0.005(2) C5 0.047(3) 0.028(2) 0.026(2) 0.003(2) -0.004(2) 0.002(2) C6 0.048(3) 0.030(3) 0.028(2) -0.002(2) -0.001(2) 0.001(2) C7 0.107(6) 0.034(3) 0.028(3) 0.003(2) -0.005(3) -0.001(3) C8 0.042(3) 0.062(4) 0.047(3) 0.005(3) -0.004(3) -0.004(3) C9 0.046(4) 0.071(5) 0.083(6) 0.003(4) -0.005(4) -0.010(4) C10 0.046(4) 0.079(5) 0.053(4) -0.009(4) -0.001(3) 0.009(3) C11 0.049(4) 0.067(5) 0.082(6) 0.016(4) -0.005(4) 0.005(3) C12 0.127(11) 0.125(10) 0.091(8) 0.024(7) -0.023(7) -0.072(9) C13 0.056(6) 0.174(14) 0.111(9) 0.034(9) 0.011(6) -0.016(7) C14 0.066(6) 0.178(14) 0.076(7) 0.033(8) -0.002(5) 0.025(7) C15 0.095(7) 0.072(6) 0.056(5) -0.004(4) -0.008(4) -0.025(5) _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 P1 C1 1.814(5) . ? P1 S1 1.982(2) . ? P1 S2 1.985(2) . ? P1 S3 2.123(2) . ? P1 K1 3.6325(19) . ? P1 K1 3.867(2) 12_756 ? K1 O2 2.758(6) . ? K1 O1 2.896(4) 1_554 ? K1 S1 3.238(2) . ? K1 S1 3.333(2) 12_756 ? K1 S2 3.370(2) 15_665 ? K1 S1 3.437(2) 15_665 ? K1 S2 3.679(2) . ? K1 S3 3.785(2) . ? K1 P1 3.867(2) 15_665 ? K1 K1 4.618(2) 15_665 ? K1 K1 4.618(2) 12_756 ? S1 K1 3.333(2) 15_665 ? S1 K1 3.437(2) 12_756 ? S2 K1 3.370(2) 12_756 ? S3 C8 1.877(8) . ? O1 C4 1.368(6) . ? O1 C7 1.428(7) . ? O1 K1 2.896(4) 1_556 ? O2 C12 1.401(12) . ? O2 C15 1.429(11) . ? C1 C6 1.395(8) . ? C1 C2 1.404(8) . ? C2 C3 1.381(8) . ? C3 C4 1.386(8) . ? C4 C5 1.387(8) . ? C5 C6 1.377(7) . ? C8 C11 1.486(10) . ? C8 C10 1.488(10) . ? C8 C9 1.554(10) . ? C12 C13 1.446(18) . ? C13 C14 1.525(17) . ? C14 C15 1.422(15) . ? 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 C1 P1 S1 109.13(19) . . ? C1 P1 S2 111.4(2) . . ? S1 P1 S2 115.07(9) . . ? C1 P1 S3 105.7(2) . . ? S1 P1 S3 115.60(10) . . ? S2 P1 S3 99.26(9) . . ? C1 P1 K1 171.38(19) . . ? S1 P1 K1 62.55(6) . . ? S2 P1 K1 75.55(6) . . ? S3 P1 K1 77.35(6) . . ? C1 P1 K1 102.71(19) . 12_756 ? S1 P1 K1 62.55(6) . 12_756 ? S2 P1 K1 60.60(6) . 12_756 ? S3 P1 K1 149.87(7) . 12_756 ? K1 P1 K1 75.94(4) . 12_756 ? O2 K1 O1 67.51(17) . 1_554 ? O2 K1 S1 134.20(14) . . ? O1 K1 S1 138.32(10) 1_554 . ? O2 K1 S1 138.43(14) . 12_756 ? O1 K1 S1 76.62(10) 1_554 12_756 ? S1 K1 S1 86.85(6) . 12_756 ? O2 K1 S2 73.90(14) . 15_665 ? O1 K1 S2 132.92(10) 1_554 15_665 ? S1 K1 S2 88.29(5) . 15_665 ? S1 K1 S2 121.78(6) 12_756 15_665 ? O2 K1 S1 117.53(14) . 15_665 ? O1 K1 S1 118.60(9) 1_554 15_665 ? S1 K1 S1 85.13(5) . 15_665 ? S1 K1 S1 62.88(5) 12_756 15_665 ? S2 K1 S1 58.90(4) 15_665 15_665 ? O2 K1 P1 113.49(14) . . ? O1 K1 P1 111.95(9) 1_554 . ? S1 K1 P1 32.90(4) . . ? S1 K1 P1 98.67(5) 12_756 . ? S2 K1 P1 107.45(5) 15_665 . ? S1 K1 P1 117.86(5) 15_665 . ? O2 K1 S2 112.17(14) . . ? O1 K1 S2 82.22(9) 1_554 . ? S1 K1 S2 57.46(4) . . ? S1 K1 S2 81.90(5) 12_756 . ? S2 K1 S2 138.72(4) 15_665 . ? S1 K1 S2 130.24(5) 15_665 . ? P1 K1 S2 31.50(3) . . ? O2 K1 S3 80.65(13) . . ? O1 K1 S3 104.42(9) 1_554 . ? S1 K1 S3 58.69(4) . . ? S1 K1 S3 129.79(5) 12_756 . ? S2 K1 S3 94.61(5) 15_665 . ? S1 K1 S3 136.86(5) 15_665 . ? P1 K1 S3 33.18(4) . . ? S2 K1 S3 49.58(4) . . ? O2 K1 P1 89.85(14) . 15_665 ? O1 K1 P1 122.50(9) 1_554 15_665 ? S1 K1 P1 95.77(5) . 15_665 ? S1 K1 P1 92.26(5) 12_756 15_665 ? S2 K1 P1 30.88(4) 15_665 15_665 ? S1 K1 P1 30.78(3) 15_665 15_665 ? P1 K1 P1 125.52(4) . 15_665 ? S2 K1 P1 152.71(5) . 15_665 ? S3 K1 P1 123.86(5) . 15_665 ? O2 K1 K1 124.87(15) . 15_665 ? O1 K1 K1 160.99(10) 1_554 15_665 ? S1 K1 K1 46.20(4) . 15_665 ? S1 K1 K1 85.98(3) 12_756 15_665 ? S2 K1 K1 52.04(4) 15_665 15_665 ? S1 K1 K1 44.48(3) 15_665 15_665 ? P1 K1 K1 77.89(4) . 15_665 ? S2 K1 K1 103.10(4) . 15_665 ? S3 K1 K1 92.55(5) . 15_665 ? P1 K1 K1 49.74(3) 15_665 15_665 ? O2 K1 K1 156.84(14) . 12_756 ? O1 K1 K1 97.38(10) 1_554 12_756 ? S1 K1 K1 48.04(4) . 12_756 ? S1 K1 K1 44.53(3) 12_756 12_756 ? S2 K1 K1 126.78(5) 15_665 12_756 ? S1 K1 K1 84.83(3) 15_665 12_756 ? P1 K1 K1 54.32(4) . 12_756 ? S2 K1 K1 46.24(4) . 12_756 ? S3 K1 K1 86.73(5) . 12_756 ? P1 K1 K1 113.29(3) 15_665 12_756 ? K1 K1 K1 74.74(3) 15_665 12_756 ? P1 S1 K1 84.54(7) . . ? P1 S1 K1 160.30(9) . 15_665 ? K1 S1 K1 89.28(4) . 15_665 ? P1 S1 K1 86.67(7) . 12_756 ? K1 S1 K1 87.49(4) . 12_756 ? K1 S1 K1 111.77(5) 15_665 12_756 ? P1 S2 K1 88.51(7) . 12_756 ? P1 S2 K1 72.95(6) . . ? K1 S2 K1 81.72(5) 12_756 . ? C8 S3 P1 111.2(2) . . ? C8 S3 K1 108.6(2) . . ? P1 S3 K1 69.47(6) . . ? C4 O1 C7 116.9(4) . . ? C4 O1 K1 127.4(3) . 1_556 ? C7 O1 K1 105.5(4) . 1_556 ? C12 O2 C15 107.7(7) . . ? C12 O2 K1 134.4(6) . . ? C15 O2 K1 114.7(5) . . ? C6 C1 C2 117.4(5) . . ? C6 C1 P1 121.0(4) . . ? C2 C1 P1 121.6(4) . . ? C3 C2 C1 120.8(5) . . ? C2 C3 C4 120.2(5) . . ? O1 C4 C3 115.6(5) . . ? O1 C4 C5 124.4(5) . . ? C3 C4 C5 120.0(5) . . ? C6 C5 C4 119.3(5) . . ? C5 C6 C1 122.1(5) . . ? C11 C8 C10 111.4(7) . . ? C11 C8 C9 110.3(6) . . ? C10 C8 C9 110.9(7) . . ? C11 C8 S3 109.6(5) . . ? C10 C8 S3 111.8(5) . . ? C9 C8 S3 102.5(5) . . ? O2 C12 C13 107.6(11) . . ? C12 C13 C14 104.1(9) . . ? C15 C14 C13 106.5(9) . . ? C14 C15 O2 107.5(8) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.100 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.132