# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Alexander Rothenberger' _publ_contact_author_email ROTHENBERGER@CHEMIE.UNI-KARLSRUHE.DE loop_ _publ_author_name A.Rothenberger O.Hampe M.Shafaei-Fallah 'Weifang Shi' data_1 _database_code_depnum_ccdc_archive 'CCDC 623841' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C255 H263 Ag24 P17 S33' _chemical_formula_weight 7501.00 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M F23 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x+1/2, y+1/2' 'z, -x+1/2, -y+1/2' '-z, -x+1/2, y+1/2' '-z, x+1/2, -y+1/2' 'y, z+1/2, x+1/2' '-y, z+1/2, -x+1/2' 'y, -z+1/2, -x+1/2' '-y, -z+1/2, x+1/2' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+1/2, y, -z+1/2' 'x+1/2, -y, -z+1/2' 'z+1/2, x, y+1/2' 'z+1/2, -x, -y+1/2' '-z+1/2, -x, y+1/2' '-z+1/2, x, -y+1/2' 'y+1/2, z, x+1/2' '-y+1/2, z, -x+1/2' 'y+1/2, -z, -x+1/2' '-y+1/2, -z, x+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'z+1/2, x+1/2, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x+1/2, y' '-z+1/2, x+1/2, -y' 'y+1/2, z+1/2, x' '-y+1/2, z+1/2, -x' 'y+1/2, -z+1/2, -x' '-y+1/2, -z+1/2, x' _cell_length_a 31.215(4) _cell_length_b 31.215(4) _cell_length_c 31.215(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 30417(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2658 _cell_measurement_theta_min 4.35 _cell_measurement_theta_max 54.35 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 14816 _exptl_absorpt_coefficient_mu 1.866 _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 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26709 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_sigmaI/netI 0.0260 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 27.19 _reflns_number_total 5565 _reflns_number_gt 4976 _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. ; # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.000 166.8 10.0 2 0.500 0.000 0.000 86.0 -13.3 3 0.000 0.000 0.500 85.9 -13.3 4 0.500 0.000 0.500 166.8 10.1 5 0.250 0.250 0.250 800.4 29.8 6 0.750 0.250 0.750 800.4 29.8 7 0.500 0.500 0.000 166.8 10.1 8 0.000 0.500 0.500 166.8 10.0 9 0.000 0.500 0.000 86.0 -13.3 10 0.500 0.500 0.500 86.0 -13.3 11 0.750 0.750 0.250 800.4 29.8 12 0.250 0.750 0.750 800.4 29.8 _platon_squeeze_details ; Electron Count of 160 per Cell corresponds to four disordered isopropylthiolate anions with 41 electrons each ; _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^)+(0.0647P)^2^+49.4027P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(4) _refine_ls_number_reflns 5565 _refine_ls_number_parameters 189 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.1068 _refine_ls_wR_factor_gt 0.1053 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.122 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag2 Ag 0.577619(14) 0.709812(16) 0.793481(14) 0.04711(13) Uani 1 1 d . . . Ag1 Ag 0.662028(15) 0.741592(18) 0.667294(15) 0.05243(14) Uani 1 1 d . . . P1 P 0.7500 0.7500 0.7500 0.0197(6) Uani 1 12 d S . . P3 P 0.63783(4) 0.63783(4) 0.86217(4) 0.0489(6) Uani 1 3 d S A . P2 P 0.50251(5) 0.72233(6) 0.81016(5) 0.0537(4) Uani 1 1 d . . . S3 S 0.61234(7) 0.63369(7) 0.80298(6) 0.0678(5) Uani 1 1 d . . . S4 S 0.59927(7) 0.59927(7) 0.90073(7) 0.121(2) Uani 1 3 d S . . S1 S 0.71215(3) 0.78785(3) 0.71215(3) 0.0244(3) Uani 1 3 d S . . S2 S 0.60538(4) 0.70717(4) 0.71144(4) 0.0353(2) Uani 1 1 d . . . C1 C 0.57170(9) 0.67245(10) 0.68081(9) 0.0347(10) Uani 1 1 d G A . C2 C 0.57360(9) 0.67177(10) 0.63633(9) 0.0351(10) Uani 1 1 d G . . H2 H 0.5931 0.6900 0.6217 0.042 Uiso 1 1 calc R A . C3 C 0.54700(10) 0.64446(11) 0.61332(7) 0.0435(12) Uani 1 1 d G A . H3 H 0.5483 0.6440 0.5829 0.052 Uiso 1 1 calc R . . C4 C 0.51850(9) 0.61783(10) 0.63480(9) 0.0493(14) Uani 1 1 d G . . C5 C 0.51659(10) 0.61851(11) 0.67928(9) 0.0496(14) Uani 1 1 d G A . H5 H 0.4971 0.6003 0.6940 0.060 Uiso 1 1 calc R . . C6 C 0.54320(11) 0.64582(12) 0.70229(7) 0.0428(12) Uani 1 1 d G . . H6 H 0.5419 0.6463 0.7327 0.051 Uiso 1 1 calc R A . C7 C 0.48902(15) 0.58733(16) 0.61005(14) 0.072(2) Uani 1 1 d G A . H7A H 0.4642 0.6033 0.5992 0.108 Uiso 1 1 calc R . . H7B H 0.4792 0.5645 0.6292 0.108 Uiso 1 1 calc R . . H7C H 0.5048 0.5748 0.5860 0.108 Uiso 1 1 calc R . . C8 C 0.4718(3) 0.6692(3) 0.8123(3) 0.035(2) Uiso 0.50 1 d PG A 1 C9 C 0.4917(2) 0.6304(3) 0.8213(4) 0.069(4) Uiso 0.50 1 d PG A 1 H9 H 0.5217 0.6294 0.8263 0.083 Uiso 0.50 1 calc PR A 1 C10 C 0.4677(4) 0.5929(3) 0.8229(5) 0.109(7) Uiso 0.50 1 d PG A 1 H10 H 0.4813 0.5664 0.8290 0.131 Uiso 0.50 1 calc PR A 1 C11 C 0.4238(4) 0.5942(3) 0.8155(4) 0.073(4) Uiso 0.50 1 d PG A 1 H11 H 0.4074 0.5686 0.8166 0.088 Uiso 0.50 1 calc PR A 1 C12 C 0.4039(2) 0.6330(3) 0.8066(4) 0.068(4) Uiso 0.50 1 d PG A 1 H12 H 0.3739 0.6339 0.8015 0.082 Uiso 0.50 1 calc PR A 1 C13 C 0.4279(3) 0.6705(3) 0.8049(3) 0.054(3) Uiso 0.50 1 d PG A 1 H13 H 0.4143 0.6970 0.7988 0.064 Uiso 0.50 1 calc PR A 1 C8' C 0.4642(3) 0.6822(3) 0.8044(3) 0.042(3) Uiso 0.50 1 d PG A 2 C9' C 0.4824(2) 0.6418(3) 0.8082(3) 0.063(4) Uiso 0.50 1 d PG A 2 H9' H 0.5124 0.6389 0.8124 0.075 Uiso 0.50 1 calc PR A 2 C10' C 0.4567(3) 0.6055(3) 0.8059(4) 0.074(4) Uiso 0.50 1 d PG A 2 H10' H 0.4691 0.5778 0.8085 0.089 Uiso 0.50 1 calc PR A 2 C11' C 0.4128(3) 0.6097(3) 0.7998(4) 0.069(4) Uiso 0.50 1 d PG A 2 H11' H 0.3952 0.5849 0.7982 0.083 Uiso 0.50 1 calc PR A 2 C12' C 0.3946(2) 0.6501(4) 0.7960(4) 0.089(5) Uiso 0.50 1 d PG A 2 H12' H 0.3646 0.6530 0.7918 0.107 Uiso 0.50 1 calc PR A 2 C13' C 0.4203(3) 0.6864(3) 0.7983(4) 0.063(3) Uiso 0.50 1 d PG A 2 H13' H 0.4079 0.7141 0.7957 0.076 Uiso 0.50 1 calc PR A 2 C14 C 0.49264(10) 0.74621(12) 0.86299(9) 0.0507(15) Uani 1 1 d G A . C15 C 0.51720(13) 0.73113(15) 0.89694(11) 0.067(2) Uani 1 1 d G . . H15 H 0.5385 0.7099 0.8921 0.080 Uiso 1 1 calc R A . C16 C 0.51067(14) 0.74713(16) 0.93797(9) 0.073(2) Uani 1 1 d G A . H16 H 0.5275 0.7368 0.9612 0.088 Uiso 1 1 calc R . . C17 C 0.47957(15) 0.77820(15) 0.94507(8) 0.0626(19) Uani 1 1 d G . . H17 H 0.4751 0.7891 0.9731 0.075 Uiso 1 1 calc R A . C18 C 0.45501(15) 0.79327(15) 0.91112(10) 0.071(2) Uani 1 1 d G A . H18 H 0.4338 0.8145 0.9160 0.085 Uiso 1 1 calc R . . C19 C 0.46154(11) 0.77728(13) 0.87008(9) 0.066(2) Uani 1 1 d G . . H19 H 0.4448 0.7876 0.8469 0.080 Uiso 1 1 calc R A . C20 C 0.4777(2) 0.7600(2) 0.77270(8) 0.073(2) Uani 1 1 d G . . H20A H 0.4479 0.7662 0.7818 0.088 Uiso 1 1 calc R . . H20B H 0.4939 0.7872 0.7725 0.088 Uiso 1 1 calc R . . C21 C 0.6020(10) 0.6024(11) 0.9472(10) 0.087(8) Uiso 0.33 1 d P A . H21 H 0.6219 0.6268 0.9528 0.105 Uiso 0.33 1 calc PR . . C22 C 0.5558(18) 0.6161(19) 0.9714(19) 0.17(2) Uiso 0.33 1 d P . . H22A H 0.5443 0.6421 0.9580 0.248 Uiso 0.33 1 calc PR A . H22B H 0.5612 0.6216 1.0018 0.248 Uiso 0.33 1 calc PR . . H22C H 0.5351 0.5927 0.9684 0.248 Uiso 0.33 1 calc PR . . C23 C 0.6260(18) 0.5603(18) 0.9666(17) 0.157(18) Uiso 0.33 1 d P . . H23A H 0.6524 0.5550 0.9505 0.235 Uiso 0.33 1 calc PR A . H23B H 0.6071 0.5354 0.9642 0.235 Uiso 0.33 1 calc PR . . H23C H 0.6330 0.5653 0.9968 0.235 Uiso 0.33 1 calc PR . . 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 Ag2 0.0413(2) 0.0571(3) 0.0429(2) -0.01332(19) 0.01257(18) -0.01440(19) Ag1 0.0411(2) 0.0745(3) 0.0417(2) -0.0151(2) 0.00056(18) -0.0226(2) P1 0.0197(6) 0.0197(6) 0.0197(6) 0.000 0.000 0.000 P3 0.0489(6) 0.0489(6) 0.0489(6) 0.0135(6) 0.0135(6) -0.0135(6) P2 0.0410(8) 0.0789(11) 0.0411(8) -0.0272(8) 0.0150(6) -0.0214(8) S3 0.0757(12) 0.0813(13) 0.0464(9) 0.0028(8) 0.0102(8) -0.0102(10) S4 0.121(2) 0.121(2) 0.121(2) 0.0483(15) 0.0483(15) -0.0483(15) S1 0.0244(3) 0.0244(3) 0.0244(3) 0.0016(4) -0.0016(4) 0.0016(4) S2 0.0309(6) 0.0374(6) 0.0377(6) -0.0082(5) 0.0021(5) -0.0033(5) C1 0.026(2) 0.040(3) 0.039(3) -0.007(2) 0.0029(19) -0.0024(19) C2 0.028(2) 0.038(3) 0.040(3) 0.000(2) -0.0011(19) -0.002(2) C3 0.039(3) 0.056(3) 0.035(3) -0.004(2) -0.003(2) -0.001(3) C4 0.037(3) 0.056(4) 0.055(4) -0.012(3) -0.009(2) -0.006(3) C5 0.033(3) 0.062(4) 0.054(3) -0.006(3) 0.002(2) -0.019(3) C6 0.037(3) 0.052(3) 0.040(3) -0.006(2) 0.010(2) -0.013(2) C7 0.065(5) 0.087(6) 0.064(5) -0.016(4) -0.009(4) -0.036(4) C14 0.034(3) 0.076(4) 0.042(3) -0.016(3) 0.011(2) -0.019(3) C15 0.059(4) 0.099(6) 0.043(3) -0.023(4) 0.012(3) -0.001(4) C16 0.069(5) 0.105(6) 0.045(3) -0.022(4) 0.005(3) 0.004(5) C17 0.070(4) 0.083(5) 0.035(3) -0.015(3) 0.013(3) -0.016(4) C18 0.078(5) 0.085(5) 0.050(4) -0.023(4) 0.005(3) -0.002(4) C19 0.071(5) 0.088(5) 0.040(3) -0.021(3) 0.007(3) -0.005(4) C20 0.070(5) 0.114(7) 0.036(3) -0.033(4) 0.004(3) 0.013(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag2 P2 2.4334(17) . ? Ag2 S3 2.628(2) . ? Ag2 S2 2.7048(14) . ? Ag2 S2 2.7369(14) 16_566 ? Ag2 Ag1 3.2776(8) 16_566 ? Ag1 S2 2.4861(14) . ? Ag1 S1 2.5482(8) . ? Ag1 S2 2.5703(14) 9 ? Ag1 S3 2.720(2) 9 ? Ag1 Ag2 3.2777(8) 16_566 ? P1 S1 2.0464(17) 38_665 ? P1 S1 2.0465(17) . ? P1 S1 2.0465(17) 27_656 ? P1 S1 2.0465(17) 16_566 ? P3 S3 2.016(2) . ? P3 S3 2.016(2) 32_656 ? P3 S3 2.016(2) 23_566 ? P3 S4 2.085(4) . ? P2 C8' 1.740(7) . ? P2 C20 1.830(6) . ? P2 C14 1.836(3) . ? P2 C8 1.917(7) . ? S3 Ag1 2.720(2) 5 ? S4 C21 1.46(3) 23_566 ? S4 C21 1.46(3) . ? S4 C21 1.46(3) 32_656 ? S1 Ag1 2.5483(8) 18_566 ? S1 Ag1 2.5483(8) 48_665 ? S2 C1 1.787(2) . ? S2 Ag1 2.5704(14) 5 ? S2 Ag2 2.7369(14) 16_566 ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? C4 C7 1.5330 . ? C5 C6 1.3900 . ? C8 C9 1.3900 . ? C8 C13 1.3900 . ? C9 C10 1.3900 . ? C10 C11 1.3900 . ? C11 C12 1.3900 . ? C12 C13 1.3900 . ? C8' C9' 1.3900 . ? C8' C13' 1.3900 . ? C9' C10' 1.3900 . ? C10' C11' 1.3900 . ? C11' C12' 1.3900 . ? C12' C13' 1.3900 . ? C14 C15 1.3900 . ? C14 C19 1.3900 . ? C15 C16 1.3900 . ? C16 C17 1.3900 . ? C17 C18 1.3900 . ? C18 C19 1.3900 . ? C20 C20 1.548(7) 16_566 ? C21 C23 1.63(6) . ? C21 C22 1.68(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 P2 Ag2 S3 121.22(7) . . ? P2 Ag2 S2 121.07(5) . . ? S3 Ag2 S2 86.97(5) . . ? P2 Ag2 S2 99.50(5) . 16_566 ? S3 Ag2 S2 137.04(6) . 16_566 ? S2 Ag2 S2 82.78(4) . 16_566 ? P2 Ag2 Ag1 128.34(4) . 16_566 ? S3 Ag2 Ag1 92.57(5) . 16_566 ? S2 Ag2 Ag1 96.33(3) . 16_566 ? S2 Ag2 Ag1 47.79(3) 16_566 16_566 ? S2 Ag1 S1 112.15(4) . . ? S2 Ag1 S2 130.43(6) . 9 ? S1 Ag1 S2 106.50(3) . 9 ? S2 Ag1 S3 115.01(6) . 9 ? S1 Ag1 S3 98.46(6) . 9 ? S2 Ag1 S3 87.82(6) 9 9 ? S2 Ag1 Ag2 54.63(3) . 16_566 ? S1 Ag1 Ag2 91.49(3) . 16_566 ? S2 Ag1 Ag2 153.00(4) 9 16_566 ? S3 Ag1 Ag2 69.39(5) 9 16_566 ? S1 P1 S1 109.467(1) 38_665 . ? S1 P1 S1 109.477(1) 38_665 27_656 ? S1 P1 S1 109.470(1) . 27_656 ? S1 P1 S1 109.5 38_665 16_566 ? S1 P1 S1 109.5 . 16_566 ? S1 P1 S1 109.466(1) 27_656 16_566 ? S3 P3 S3 113.27(7) . 32_656 ? S3 P3 S3 113.27(7) . 23_566 ? S3 P3 S3 113.28(7) 32_656 23_566 ? S3 P3 S4 105.33(9) . . ? S3 P3 S4 105.33(9) 32_656 . ? S3 P3 S4 105.33(9) 23_566 . ? C8' P2 C20 96.0(4) . . ? C8' P2 C14 105.6(3) . . ? C20 P2 C14 104.0(2) . . ? C8' P2 C8 15.8(4) . . ? C20 P2 C8 111.5(4) . . ? C14 P2 C8 103.7(3) . . ? C8' P2 Ag2 121.6(3) . . ? C20 P2 Ag2 112.0(2) . . ? C14 P2 Ag2 114.78(13) . . ? C8 P2 Ag2 110.5(3) . . ? P3 S3 Ag2 102.02(9) . . ? P3 S3 Ag1 112.09(11) . 5 ? Ag2 S3 Ag1 83.49(6) . 5 ? C21 S4 C21 96.9(18) 23_566 . ? C21 S4 C21 96.9(18) 23_566 32_656 ? C21 S4 C21 96.9(18) . 32_656 ? C21 S4 P3 120.2(14) 23_566 . ? C21 S4 P3 120.2(14) . . ? C21 S4 P3 120.2(14) 32_656 . ? P1 S1 Ag1 110.15(4) . . ? P1 S1 Ag1 110.15(4) . 18_566 ? Ag1 S1 Ag1 108.78(4) . 18_566 ? P1 S1 Ag1 110.15(4) . 48_665 ? Ag1 S1 Ag1 108.78(4) . 48_665 ? Ag1 S1 Ag1 108.78(4) 18_566 48_665 ? C1 S2 Ag1 112.58(11) . . ? C1 S2 Ag1 107.80(13) . 5 ? Ag1 S2 Ag1 84.55(5) . 5 ? C1 S2 Ag2 109.67(11) . . ? Ag1 S2 Ag2 137.69(5) . . ? Ag1 S2 Ag2 84.89(4) 5 . ? C1 S2 Ag2 110.98(13) . 16_566 ? Ag1 S2 Ag2 77.57(4) . 16_566 ? Ag1 S2 Ag2 141.05(5) 5 16_566 ? Ag2 S2 Ag2 85.58(4) . 16_566 ? C2 C1 C6 120.0 . . ? C2 C1 S2 121.23(17) . . ? C6 C1 S2 118.77(17) . . ? C1 C2 C3 120.0 . . ? C4 C3 C2 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 C7 119.2 . . ? C3 C4 C7 120.8 . . ? C4 C5 C6 120.0 . . ? C5 C6 C1 120.0 . . ? C9 C8 C13 120.0 . . ? C9 C8 P2 122.6(5) . . ? C13 C8 P2 117.4(5) . . ? C8 C9 C10 120.0 . . ? C11 C10 C9 120.0 . . ? C12 C11 C10 120.0 . . ? C13 C12 C11 120.0 . . ? C12 C13 C8 120.0 . . ? C9' C8' C13' 120.0 . . ? C9' C8' P2 111.4(6) . . ? C13' C8' P2 128.6(6) . . ? C8' C9' C10' 120.0 . . ? C11' C10' C9' 120.0 . . ? C10' C11' C12' 120.0 . . ? C13' C12' C11' 120.0 . . ? C12' C13' C8' 120.0 . . ? C15 C14 C19 120.0 . . ? C15 C14 P2 117.06(18) . . ? C19 C14 P2 122.92(17) . . ? C16 C15 C14 120.0 . . ? C17 C16 C15 120.0 . . ? C16 C17 C18 120.0 . . ? C19 C18 C17 120.0 . . ? C18 C19 C14 120.0 . . ? C20 C20 P2 109.0(7) 16_566 . ? S4 C21 C23 110(3) . . ? S4 C21 C22 114(3) . . ? C23 C21 C22 116(3) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.280 _refine_diff_density_min -1.353 _refine_diff_density_rms 0.095 data_2 _database_code_depnum_ccdc_archive 'CCDC 623842' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H38 Na4 O4 P2 S8' _chemical_formula_weight 704.84 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' 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' 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 10.8600(6) _cell_length_b 11.8116(7) _cell_length_c 13.6914(7) _cell_angle_alpha 89.670(4) _cell_angle_beta 82.780(4) _cell_angle_gamma 83.450(5) _cell_volume 1730.89(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 20653 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 54.22 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 736 _exptl_absorpt_coefficient_mu 0.679 _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 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13736 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0376 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 27.00 _reflns_number_total 7000 _reflns_number_gt 5635 _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^)+(0.0292P)^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 7000 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0343 _refine_ls_R_factor_gt 0.0235 _refine_ls_wR_factor_ref 0.0549 _refine_ls_wR_factor_gt 0.0527 _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_restrained_S_all 0.950 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Na1 Na 0.63806(6) 0.90220(5) 0.52014(5) 0.01882(14) Uani 1 1 d . . . Na2 Na 0.51507(6) 0.77321(5) 0.21411(5) 0.02325(15) Uani 1 1 d . . . Na3 Na 0.48993(6) 1.27668(5) 0.28400(5) 0.02299(15) Uani 1 1 d . . . Na4 Na 0.35782(6) 0.43372(5) -0.02206(5) 0.01820(13) Uani 1 1 d . . . S1 S 0.69873(4) 0.85689(3) 0.31281(3) 0.01950(9) Uani 1 1 d . . . S2 S 0.62550(4) 1.11470(3) 0.41594(3) 0.01756(8) Uani 1 1 d . . . S3 S 0.43046(4) 1.01415(3) 0.27453(3) 0.01923(9) Uani 1 1 d . . . S4 S 0.67295(4) 1.09536(3) 0.16721(3) 0.01715(8) Uani 1 1 d . . . S5 S 0.57098(4) 0.50030(3) 0.22662(3) 0.01824(8) Uani 1 1 d . . . S6 S 0.38071(4) 0.64086(3) 0.07988(3) 0.01667(8) Uani 1 1 d . . . S7 S 0.30485(4) 0.39840(3) 0.18464(3) 0.01849(8) Uani 1 1 d . . . S8 S 0.32554(4) 0.63207(3) 0.32799(3) 0.01646(8) Uani 1 1 d . . . P1 P 0.60974(4) 1.01365(3) 0.30067(3) 0.01496(8) Uani 1 1 d . . . P2 P 0.39302(4) 0.53700(3) 0.19671(3) 0.01429(8) Uani 1 1 d . . . O1 O 0.65025(11) 0.69823(9) 0.55595(9) 0.0191(2) Uani 1 1 d . . . O2 O 0.84057(11) 0.84305(9) 0.55682(9) 0.0197(2) Uani 1 1 d . . . O3 O 0.34469(10) 0.23029(9) -0.05300(9) 0.0183(2) Uani 1 1 d . . . O4 O 0.15571(11) 0.41641(9) -0.05899(9) 0.0202(2) Uani 1 1 d . . . C1 C 0.83682(15) 1.12965(14) 0.16305(13) 0.0212(3) Uani 1 1 d . . . C2 C 0.92394(16) 1.02787(14) 0.19139(15) 0.0254(4) Uani 1 1 d . . . H2A H 1.0102 1.0468 0.1823 0.038 Uiso 1 1 calc R . . H2B H 0.9173 0.9623 0.1496 0.038 Uiso 1 1 calc R . . H2C H 0.9004 1.0090 0.2605 0.038 Uiso 1 1 calc R . . C3 C 0.84182(17) 1.23203(14) 0.22982(15) 0.0266(4) Uani 1 1 d . . . H3A H 0.9273 1.2528 0.2232 0.040 Uiso 1 1 calc R . . H3B H 0.8161 1.2122 0.2984 0.040 Uiso 1 1 calc R . . H3C H 0.7852 1.2967 0.2107 0.040 Uiso 1 1 calc R . . C4 C 0.87048(17) 1.15942(18) 0.05505(15) 0.0322(4) Uani 1 1 d . . . H4A H 0.9553 1.1819 0.0451 0.048 Uiso 1 1 calc R . . H4B H 0.8113 1.2227 0.0370 0.048 Uiso 1 1 calc R . . H4C H 0.8665 1.0928 0.0137 0.048 Uiso 1 1 calc R . . C5 C 0.16261(15) 0.70103(13) 0.32740(13) 0.0213(3) Uani 1 1 d . . . C6 C 0.07529(17) 0.61787(16) 0.30126(18) 0.0359(5) Uani 1 1 d . . . H6A H -0.0105 0.6559 0.3080 0.054 Uiso 1 1 calc R . . H6B H 0.0797 0.5526 0.3457 0.054 Uiso 1 1 calc R . . H6C H 0.1001 0.5913 0.2332 0.054 Uiso 1 1 calc R . . C7 C 0.15972(19) 0.80211(16) 0.25817(17) 0.0345(4) Uani 1 1 d . . . H7A H 0.0746 0.8413 0.2632 0.052 Uiso 1 1 calc R . . H7B H 0.1863 0.7752 0.1904 0.052 Uiso 1 1 calc R . . H7C H 0.2165 0.8550 0.2763 0.052 Uiso 1 1 calc R . . C8 C 0.12746(18) 0.74168(18) 0.43350(15) 0.0342(4) Uani 1 1 d . . . H8A H 0.0437 0.7840 0.4409 0.051 Uiso 1 1 calc R . . H8B H 0.1879 0.7915 0.4506 0.051 Uiso 1 1 calc R . . H8C H 0.1281 0.6758 0.4773 0.051 Uiso 1 1 calc R . . C9 C 0.58887(18) 0.62926(14) 0.49484(14) 0.0275(4) Uani 1 1 d . . . H9A H 0.5963 0.5504 0.5180 0.041 Uiso 1 1 calc R . . H9B H 0.6283 0.6315 0.4265 0.041 Uiso 1 1 calc R . . H9C H 0.5004 0.6589 0.4985 0.041 Uiso 1 1 calc R . . C10 C 0.78027(16) 0.65675(13) 0.55115(14) 0.0231(4) Uani 1 1 d . . . H10A H 0.8190 0.6515 0.4817 0.028 Uiso 1 1 calc R . . H10B H 0.7899 0.5797 0.5801 0.028 Uiso 1 1 calc R . . C11 C 0.84372(16) 0.73712(14) 0.60719(14) 0.0228(4) Uani 1 1 d . . . H11A H 0.8001 0.7483 0.6750 0.027 Uiso 1 1 calc R . . H11B H 0.9313 0.7053 0.6112 0.027 Uiso 1 1 calc R . . C12 C 0.90174(17) 0.92316(15) 0.60540(15) 0.0294(4) Uani 1 1 d . . . H12A H 0.9899 0.8940 0.6054 0.044 Uiso 1 1 calc R . . H12B H 0.8617 0.9344 0.6734 0.044 Uiso 1 1 calc R . . H12C H 0.8955 0.9960 0.5707 0.044 Uiso 1 1 calc R . . C13 C 0.40855(17) 0.14901(14) 0.00707(14) 0.0247(4) Uani 1 1 d . . . H13A H 0.3966 0.0717 -0.0125 0.037 Uiso 1 1 calc R . . H13B H 0.3747 0.1622 0.0764 0.037 Uiso 1 1 calc R . . H13C H 0.4979 0.1577 -0.0017 0.037 Uiso 1 1 calc R . . C14 C 0.21399(15) 0.21791(13) -0.04154(14) 0.0224(4) Uani 1 1 d . . . H14A H 0.1795 0.2258 0.0289 0.027 Uiso 1 1 calc R . . H14B H 0.2013 0.1413 -0.0646 0.027 Uiso 1 1 calc R . . C15 C 0.14748(16) 0.30765(13) -0.10031(14) 0.0213(3) Uani 1 1 d . . . H15A H 0.1864 0.3041 -0.1698 0.026 Uiso 1 1 calc R . . H15B H 0.0588 0.2947 -0.0986 0.026 Uiso 1 1 calc R . . C16 C 0.09322(17) 0.50590(14) -0.11042(15) 0.0269(4) Uani 1 1 d . . . H16A H 0.0040 0.4970 -0.1048 0.040 Uiso 1 1 calc R . . H16B H 0.1284 0.5029 -0.1800 0.040 Uiso 1 1 calc R . . H16C H 0.1042 0.5794 -0.0819 0.040 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 Na1 0.0209(3) 0.0183(3) 0.0168(4) 0.0018(2) -0.0014(3) -0.0014(2) Na2 0.0267(3) 0.0217(3) 0.0222(4) -0.0042(3) -0.0006(3) -0.0091(3) Na3 0.0263(3) 0.0182(3) 0.0231(4) 0.0039(2) -0.0008(3) 0.0006(2) Na4 0.0196(3) 0.0194(3) 0.0164(3) -0.0021(2) -0.0015(3) -0.0060(2) S1 0.0266(2) 0.01463(17) 0.0168(2) -0.00041(14) -0.00307(18) -0.00020(14) S2 0.02231(19) 0.01515(17) 0.0158(2) -0.00145(13) -0.00358(17) -0.00330(14) S3 0.01794(18) 0.02191(19) 0.0185(2) -0.00138(15) -0.00213(17) -0.00518(14) S4 0.01684(17) 0.01941(18) 0.0154(2) 0.00309(14) -0.00236(17) -0.00288(13) S5 0.01689(18) 0.01955(18) 0.0180(2) 0.00113(14) -0.00244(17) -0.00046(13) S6 0.02006(18) 0.01541(17) 0.0150(2) 0.00178(13) -0.00278(17) -0.00345(13) S7 0.0252(2) 0.01537(17) 0.0158(2) -0.00011(13) -0.00166(18) -0.00698(14) S8 0.01724(18) 0.01742(17) 0.0146(2) -0.00286(13) -0.00147(16) -0.00186(13) P1 0.01797(19) 0.01359(17) 0.0134(2) 0.00009(14) -0.00197(17) -0.00235(14) P2 0.01653(18) 0.01323(17) 0.0132(2) -0.00002(14) -0.00163(17) -0.00257(13) O1 0.0215(6) 0.0176(5) 0.0192(6) -0.0012(4) -0.0050(5) -0.0038(4) O2 0.0214(6) 0.0185(5) 0.0200(7) 0.0001(4) -0.0031(5) -0.0045(4) O3 0.0184(5) 0.0187(5) 0.0187(6) 0.0019(4) -0.0036(5) -0.0045(4) O4 0.0207(6) 0.0178(5) 0.0227(7) -0.0024(4) -0.0045(5) -0.0029(4) C1 0.0162(7) 0.0236(8) 0.0238(10) 0.0039(6) -0.0016(7) -0.0044(6) C2 0.0191(8) 0.0251(8) 0.0328(11) -0.0009(7) -0.0069(8) -0.0020(6) C3 0.0229(8) 0.0210(8) 0.0369(12) 0.0017(7) -0.0033(8) -0.0077(6) C4 0.0229(9) 0.0457(11) 0.0284(12) 0.0098(8) 0.0009(9) -0.0103(8) C5 0.0175(7) 0.0211(8) 0.0245(10) -0.0029(6) -0.0026(7) 0.0013(6) C6 0.0212(9) 0.0295(9) 0.0591(15) -0.0080(9) -0.0147(10) -0.0004(7) C7 0.0300(10) 0.0297(10) 0.0378(13) 0.0052(8) 0.0046(9) 0.0118(7) C8 0.0255(9) 0.0464(11) 0.0270(12) -0.0084(8) 0.0023(9) 0.0069(8) C9 0.0369(10) 0.0209(8) 0.0278(10) -0.0030(7) -0.0118(9) -0.0078(7) C10 0.0218(8) 0.0168(7) 0.0290(10) 0.0016(6) 0.0018(8) -0.0001(6) C11 0.0203(8) 0.0257(8) 0.0226(10) 0.0068(7) -0.0027(8) -0.0040(6) C12 0.0258(9) 0.0297(9) 0.0337(11) -0.0090(8) -0.0026(9) -0.0087(7) C13 0.0292(9) 0.0190(8) 0.0275(10) 0.0039(6) -0.0096(8) -0.0032(6) C14 0.0203(8) 0.0200(8) 0.0279(10) 0.0011(6) -0.0026(8) -0.0071(6) C15 0.0203(8) 0.0203(8) 0.0241(10) -0.0045(6) -0.0038(7) -0.0040(6) C16 0.0279(9) 0.0230(8) 0.0299(11) 0.0030(7) -0.0056(9) -0.0014(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Na1 O2 2.3453(12) . ? Na1 O1 2.4479(12) . ? Na1 S1 2.8714(8) . ? Na1 S2 2.8781(7) . ? Na1 S2 2.9150(8) 2_676 ? Na1 S3 2.9617(8) 2_676 ? Na1 P1 3.3091(8) . ? Na1 Na3 3.6408(10) 2_676 ? Na1 Na1 3.6679(12) 2_676 ? Na2 O3 2.5156(14) 2_665 ? Na2 S1 2.8150(7) . ? Na2 S3 2.9778(8) . ? Na2 S6 3.0295(7) . ? Na2 S8 3.0649(8) . ? Na2 S5 3.2191(8) . ? Na2 P2 3.2449(7) . ? Na2 P1 3.3968(7) . ? Na2 Na4 3.6311(9) 2_665 ? Na3 O1 2.5047(15) 2_676 ? Na3 S7 2.8219(8) 1_565 ? Na3 S5 2.9498(8) 1_565 ? Na3 S2 3.0128(7) . ? Na3 S4 3.0599(8) . ? Na3 S3 3.2452(7) . ? Na3 P1 3.2468(7) . ? Na3 P2 3.3949(7) 1_565 ? Na3 Na1 3.6407(10) 2_676 ? Na4 O4 2.3447(12) . ? Na4 O3 2.4655(12) . ? Na4 S7 2.8541(8) . ? Na4 S6 2.8742(7) . ? Na4 S6 2.8876(8) 2_665 ? Na4 S5 2.9355(8) 2_665 ? Na4 P2 3.3229(7) . ? Na4 P2 3.4259(8) 2_665 ? Na4 Na2 3.6311(9) 2_665 ? Na4 Na4 3.7331(12) 2_665 ? S1 P1 2.0046(5) . ? S2 P1 2.0201(5) . ? S2 Na1 2.9149(8) 2_676 ? S3 P1 2.0228(6) . ? S3 Na1 2.9617(8) 2_676 ? S4 C1 1.8636(16) . ? S4 P1 2.1347(6) . ? S5 P2 2.0240(5) . ? S5 Na4 2.9355(8) 2_665 ? S5 Na3 2.9498(8) 1_545 ? S6 P2 2.0187(6) . ? S6 Na4 2.8876(8) 2_665 ? S7 P2 2.0061(5) . ? S7 Na3 2.8218(8) 1_545 ? S8 C5 1.8626(16) . ? S8 P2 2.1291(6) . ? P2 Na3 3.3950(7) 1_545 ? P2 Na4 3.4259(8) 2_665 ? O1 C10 1.434(2) . ? O1 C9 1.4422(18) . ? O1 Na3 2.5047(15) 2_676 ? O2 C11 1.4242(19) . ? O2 C12 1.4286(19) . ? O3 C14 1.4324(19) . ? O3 C13 1.4358(19) . ? O3 Na2 2.5157(14) 2_665 ? O4 C16 1.4218(19) . ? O4 C15 1.4234(18) . ? C1 C2 1.523(2) . ? C1 C4 1.527(3) . ? C1 C3 1.530(2) . ? C5 C6 1.515(2) . ? C5 C7 1.520(3) . ? C5 C8 1.521(3) . ? C10 C11 1.502(2) . ? C14 C15 1.501(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 O2 Na1 O1 72.35(4) . . ? O2 Na1 S1 94.45(4) . . ? O1 Na1 S1 91.41(4) . . ? O2 Na1 S2 111.92(4) . . ? O1 Na1 S2 161.84(4) . . ? S1 Na1 S2 70.878(19) . . ? O2 Na1 S2 143.29(4) . 2_676 ? O1 Na1 S2 80.81(3) . 2_676 ? S1 Na1 S2 111.07(2) . 2_676 ? S2 Na1 S2 101.44(2) . 2_676 ? O2 Na1 S3 89.06(4) . 2_676 ? O1 Na1 S3 97.26(4) . 2_676 ? S1 Na1 S3 171.28(3) . 2_676 ? S2 Na1 S3 100.41(2) . 2_676 ? S2 Na1 S3 69.693(19) 2_676 2_676 ? O2 Na1 P1 117.51(4) . . ? O1 Na1 P1 124.64(4) . . ? S1 Na1 P1 37.001(13) . . ? S2 Na1 P1 37.296(13) . . ? S2 Na1 P1 98.22(2) 2_676 . ? S3 Na1 P1 134.65(2) 2_676 . ? O2 Na1 Na3 90.11(4) . 2_676 ? O1 Na1 Na3 43.29(3) . 2_676 ? S1 Na1 Na3 130.05(2) . 2_676 ? S2 Na1 Na3 149.68(3) . 2_676 ? S2 Na1 Na3 53.333(17) 2_676 2_676 ? S3 Na1 Na3 57.788(18) 2_676 2_676 ? P1 Na1 Na3 146.69(2) . 2_676 ? O2 Na1 Na1 158.43(4) . 2_676 ? O1 Na1 Na1 128.22(4) . 2_676 ? S1 Na1 Na1 91.65(3) . 2_676 ? S2 Na1 Na1 51.164(17) . 2_676 ? S2 Na1 Na1 50.273(18) 2_676 2_676 ? S3 Na1 Na1 82.30(2) 2_676 2_676 ? P1 Na1 Na1 59.292(19) . 2_676 ? Na3 Na1 Na1 101.70(3) 2_676 2_676 ? O3 Na2 S1 91.04(3) 2_665 . ? O3 Na2 S3 109.22(3) 2_665 . ? S1 Na2 S3 71.066(18) . . ? O3 Na2 S6 77.08(3) 2_665 . ? S1 Na2 S6 163.82(3) . . ? S3 Na2 S6 123.01(3) . . ? O3 Na2 S8 139.87(3) 2_665 . ? S1 Na2 S8 119.29(3) . . ? S3 Na2 S8 105.46(3) . . ? S6 Na2 S8 67.307(17) . . ? O3 Na2 S5 89.84(3) 2_665 . ? S1 Na2 S5 104.61(2) . . ? S3 Na2 S5 160.29(3) . . ? S6 Na2 S5 64.959(16) . . ? S8 Na2 S5 59.031(16) . . ? O3 Na2 P2 100.58(3) 2_665 . ? S1 Na2 P2 138.26(3) . . ? S3 Na2 P2 138.04(3) . . ? S6 Na2 P2 37.336(12) . . ? S8 Na2 P2 39.311(13) . . ? S5 Na2 P2 36.493(12) . . ? O3 Na2 P1 95.18(3) 2_665 . ? S1 Na2 P1 36.141(13) . . ? S3 Na2 P1 36.252(12) . . ? S6 Na2 P1 154.26(3) . . ? S8 Na2 P1 124.90(3) . . ? S5 Na2 P1 140.32(2) . . ? P2 Na2 P1 163.65(3) . . ? O3 Na2 Na4 42.66(3) 2_665 2_665 ? S1 Na2 Na4 113.50(3) . 2_665 ? S3 Na2 Na4 149.36(3) . 2_665 ? S6 Na2 Na4 50.396(16) . 2_665 ? S8 Na2 Na4 98.27(2) . 2_665 ? S5 Na2 Na4 50.308(16) . 2_665 ? P2 Na2 Na4 59.451(16) . 2_665 ? P1 Na2 Na4 134.67(2) . 2_665 ? O1 Na3 S7 90.73(3) 2_676 1_565 ? O1 Na3 S5 108.00(3) 2_676 1_565 ? S7 Na3 S5 71.389(19) 1_565 1_565 ? O1 Na3 S2 77.99(3) 2_676 . ? S7 Na3 S2 163.82(3) 1_565 . ? S5 Na3 S2 122.95(2) 1_565 . ? O1 Na3 S4 140.36(4) 2_676 . ? S7 Na3 S4 117.70(3) 1_565 . ? S5 Na3 S4 107.11(3) 1_565 . ? S2 Na3 S4 67.738(17) . . ? O1 Na3 S3 89.27(3) 2_676 . ? S7 Na3 S3 103.98(2) 1_565 . ? S5 Na3 S3 161.94(3) 1_565 . ? S2 Na3 S3 64.781(16) . . ? S4 Na3 S3 58.783(16) . . ? O1 Na3 P1 100.93(3) 2_676 . ? S7 Na3 P1 137.18(3) 1_565 . ? S5 Na3 P1 139.16(3) 1_565 . ? S2 Na3 P1 37.419(12) . . ? S4 Na3 P1 39.429(13) . . ? S3 Na3 P1 36.308(12) . . ? O1 Na3 P2 94.72(3) 2_676 1_565 ? S7 Na3 P2 36.186(12) 1_565 1_565 ? S5 Na3 P2 36.356(12) 1_565 1_565 ? S2 Na3 P2 154.86(2) . 1_565 ? S4 Na3 P2 124.69(3) . 1_565 ? S3 Na3 P2 139.84(2) . 1_565 ? P1 Na3 P2 163.44(3) . 1_565 ? O1 Na3 Na1 42.08(3) 2_676 2_676 ? S7 Na3 Na1 113.14(2) 1_565 2_676 ? S5 Na3 Na1 147.50(3) 1_565 2_676 ? S2 Na3 Na1 50.901(17) . 2_676 ? S4 Na3 Na1 98.93(2) . 2_676 ? S3 Na3 Na1 50.550(16) . 2_676 ? P1 Na3 Na1 60.088(17) . 2_676 ? P2 Na3 Na1 133.81(2) 1_565 2_676 ? O4 Na4 O3 72.31(4) . . ? O4 Na4 S7 96.10(4) . . ? O3 Na4 S7 90.07(3) . . ? O4 Na4 S6 114.35(4) . . ? O3 Na4 S6 160.43(4) . . ? S7 Na4 S6 71.242(19) . . ? O4 Na4 S6 143.70(4) . 2_665 ? O3 Na4 S6 80.63(3) . 2_665 ? S7 Na4 S6 107.87(2) . 2_665 ? S6 Na4 S6 99.23(2) . 2_665 ? O4 Na4 S5 89.41(4) . 2_665 ? O3 Na4 S5 97.74(4) . 2_665 ? S7 Na4 S5 171.53(2) . 2_665 ? S6 Na4 S5 100.63(2) . 2_665 ? S6 Na4 S5 70.460(19) 2_665 2_665 ? O4 Na4 P2 118.98(4) . . ? O3 Na4 P2 123.30(4) . . ? S7 Na4 P2 36.925(13) . . ? S6 Na4 P2 37.136(13) . . ? S6 Na4 P2 95.943(19) 2_665 . ? S5 Na4 P2 134.61(2) 2_665 . ? O4 Na4 P2 123.74(4) . 2_665 ? O3 Na4 P2 96.94(3) . 2_665 ? S7 Na4 P2 139.84(2) . 2_665 ? S6 Na4 P2 93.98(2) . 2_665 ? S6 Na4 P2 36.033(13) 2_665 2_665 ? S5 Na4 P2 36.073(13) 2_665 2_665 ? P2 Na4 P2 112.852(19) . 2_665 ? O4 Na4 Na2 89.82(3) . 2_665 ? O3 Na4 Na2 43.75(3) . 2_665 ? S7 Na4 Na2 128.66(2) . 2_665 ? S6 Na4 Na2 148.38(3) . 2_665 ? S6 Na4 Na2 53.936(17) 2_665 2_665 ? S5 Na4 Na2 57.547(18) 2_665 2_665 ? P2 Na4 Na2 145.23(2) . 2_665 ? P2 Na4 Na2 54.656(16) 2_665 2_665 ? O4 Na4 Na4 160.20(4) . 2_665 ? O3 Na4 Na4 126.84(4) . 2_665 ? S7 Na4 Na4 89.41(2) . 2_665 ? S6 Na4 Na4 49.772(16) . 2_665 ? S6 Na4 Na4 49.460(17) 2_665 2_665 ? S5 Na4 Na4 83.30(2) 2_665 2_665 ? P2 Na4 Na4 57.744(18) . 2_665 ? P2 Na4 Na4 55.108(18) 2_665 2_665 ? Na2 Na4 Na4 101.55(3) 2_665 2_665 ? P1 S1 Na2 87.95(2) . . ? P1 S1 Na1 83.45(2) . . ? Na2 S1 Na1 117.39(2) . . ? P1 S2 Na1 83.02(2) . . ? P1 S2 Na1 87.22(2) . 2_676 ? Na1 S2 Na1 78.56(2) . 2_676 ? P1 S2 Na3 77.59(2) . . ? Na1 S2 Na3 148.35(2) . . ? Na1 S2 Na3 75.76(2) 2_676 . ? P1 S3 Na1 85.90(2) . 2_676 ? P1 S3 Na2 83.23(2) . . ? Na1 S3 Na2 125.53(2) 2_676 . ? P1 S3 Na3 71.888(19) . . ? Na1 S3 Na3 71.66(2) 2_676 . ? Na2 S3 Na3 149.10(2) . . ? C1 S4 P1 112.56(6) . . ? C1 S4 Na3 111.00(6) . . ? P1 S4 Na3 75.01(2) . . ? P2 S5 Na4 85.28(2) . 2_665 ? P2 S5 Na3 83.88(2) . 1_545 ? Na4 S5 Na3 123.81(2) 2_665 1_545 ? P2 S5 Na2 72.447(19) . . ? Na4 S5 Na2 72.15(2) 2_665 . ? Na3 S5 Na2 150.68(2) 1_545 . ? P2 S6 Na4 83.60(2) . . ? P2 S6 Na4 86.68(2) . 2_665 ? Na4 S6 Na4 80.77(2) . 2_665 ? P2 S6 Na2 77.13(2) . . ? Na4 S6 Na2 150.20(2) . . ? Na4 S6 Na2 75.67(2) 2_665 . ? P2 S7 Na3 87.66(2) . 1_545 ? P2 S7 Na4 84.35(2) . . ? Na3 S7 Na4 118.82(2) 1_545 . ? C5 S8 P2 112.40(6) . . ? C5 S8 Na2 111.36(6) . . ? P2 S8 Na2 74.91(2) . . ? S1 P1 S2 111.85(2) . . ? S1 P1 S3 113.56(2) . . ? S2 P1 S3 112.33(3) . . ? S1 P1 S4 112.73(3) . . ? S2 P1 S4 109.07(2) . . ? S3 P1 S4 96.33(2) . . ? S1 P1 Na3 174.64(2) . . ? S2 P1 Na3 64.993(19) . . ? S3 P1 Na3 71.80(2) . . ? S4 P1 Na3 65.559(19) . . ? S1 P1 Na1 59.550(19) . . ? S2 P1 Na1 59.688(18) . . ? S3 P1 Na1 108.61(2) . . ? S4 P1 Na1 154.96(2) . . ? Na3 P1 Na1 119.66(2) . . ? S1 P1 Na2 55.912(18) . . ? S2 P1 Na2 149.22(3) . . ? S3 P1 Na2 60.521(19) . . ? S4 P1 Na2 101.61(2) . . ? Na3 P1 Na2 129.07(2) . . ? Na1 P1 Na2 92.849(19) . . ? S7 P2 S6 111.98(2) . . ? S7 P2 S5 113.44(2) . . ? S6 P2 S5 112.39(3) . . ? S7 P2 S8 112.56(3) . . ? S6 P2 S8 109.00(2) . . ? S5 P2 S8 96.48(2) . . ? S7 P2 Na2 175.49(2) . . ? S6 P2 Na2 65.531(19) . . ? S5 P2 Na2 71.060(19) . . ? S8 P2 Na2 65.777(19) . . ? S7 P2 Na4 58.730(19) . . ? S6 P2 Na4 59.269(18) . . ? S5 P2 Na4 111.17(2) . . ? S8 P2 Na4 152.28(2) . . ? Na2 P2 Na4 120.61(2) . . ? S7 P2 Na3 56.150(18) . 1_545 ? S6 P2 Na3 148.21(2) . 1_545 ? S5 P2 Na3 59.761(18) . 1_545 ? S8 P2 Na3 102.63(2) . 1_545 ? Na2 P2 Na3 128.01(2) . 1_545 ? Na4 P2 Na3 93.315(19) . 1_545 ? S7 P2 Na4 116.36(2) . 2_665 ? S6 P2 Na4 57.292(19) . 2_665 ? S5 P2 Na4 58.644(19) . 2_665 ? S8 P2 Na4 130.68(2) . 2_665 ? Na2 P2 Na4 65.893(18) . 2_665 ? Na4 P2 Na4 67.146(19) . 2_665 ? Na3 P2 Na4 99.133(19) 1_545 2_665 ? C10 O1 C9 110.41(13) . . ? C10 O1 Na1 106.97(9) . . ? C9 O1 Na1 116.76(9) . . ? C10 O1 Na3 122.13(10) . 2_676 ? C9 O1 Na3 105.68(10) . 2_676 ? Na1 O1 Na3 94.63(4) . 2_676 ? C11 O2 C12 111.15(13) . . ? C11 O2 Na1 110.42(9) . . ? C12 O2 Na1 117.45(10) . . ? C14 O3 C13 110.07(13) . . ? C14 O3 Na4 105.60(9) . . ? C13 O3 Na4 117.31(9) . . ? C14 O3 Na2 125.55(10) . 2_665 ? C13 O3 Na2 104.61(10) . 2_665 ? Na4 O3 Na2 93.59(4) . 2_665 ? C16 O4 C15 111.82(12) . . ? C16 O4 Na4 119.00(10) . . ? C15 O4 Na4 111.71(9) . . ? C2 C1 C4 110.39(16) . . ? C2 C1 C3 110.53(14) . . ? C4 C1 C3 110.83(15) . . ? C2 C1 S4 111.84(11) . . ? C4 C1 S4 102.76(11) . . ? C3 C1 S4 110.27(12) . . ? C6 C5 C7 110.66(16) . . ? C6 C5 C8 110.42(17) . . ? C7 C5 C8 110.20(15) . . ? C6 C5 S8 112.29(12) . . ? C7 C5 S8 110.64(13) . . ? C8 C5 S8 102.36(11) . . ? O1 C10 C11 108.96(13) . . ? O2 C11 C10 108.21(13) . . ? O3 C14 C15 109.43(14) . . ? O4 C15 C14 108.66(13) . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 0.540 _refine_diff_density_min -0.318 _refine_diff_density_rms 0.051