# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Chen-Wei Liu' _publ_contact_author_email CHENWEI@MAIL.NDHU.EDU.TW _publ_section_title ; Anion-templated syntheses of octanuclear silver clusters from a silver dithiophosphate chain ; loop_ _publ_author_name 'Chen-Wei Liu.' 'How-Wei Chang.' 'Ching-Shiang Fang.' 'Bijay Sarkar' data_1 _database_code_depnum_ccdc_archive 'CCDC 753439' #TrackingRef 'Ag-dtp-final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H46 Ag5 F6 O9 P5 S8' _chemical_formula_weight 1483.24 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' F F 0.0171 0.0103 '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 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 16.5922(19) _cell_length_b 16.7334(19) _cell_length_c 17.580(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.929(2) _cell_angle_gamma 90.00 _cell_volume 4792.4(9) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9969 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 28.00 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.056 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2896 _exptl_absorpt_coefficient_mu 2.584 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3468 _exptl_absorpt_correction_T_max 0.4401 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57668 _diffrn_reflns_av_R_equivalents 0.0543 _diffrn_reflns_av_sigmaI/netI 0.0397 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 28.40 _reflns_number_total 11939 _reflns_number_gt 8678 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. Disordered atoms were refined isotropically. Bond constrains were applied to those disordered atoms using DFIX command in SHELX program. O7, O8, C6, C13, C14, C18, C19 were split and refined isotropically. Bond constrains are: dfix 1.580 0.005 p4 o71 p4 o72 p4 o73 dfix 1.54 0.01 c5 c6 c3 c4 c15 c16 ; _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^)+(0.0400P)^2^+10.6318P] 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 SHELXL _refine_ls_extinction_coef 0.00103(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11939 _refine_ls_number_parameters 479 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0662 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1156 _refine_ls_wR_factor_gt 0.1015 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.046 _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 Ag1 Ag 0.30269(2) 0.61684(3) 0.24311(2) 0.05508(11) Uani 1 1 d . B . Ag2 Ag 0.23773(3) 0.78158(3) 0.17701(3) 0.06103(12) Uani 1 1 d . . . Ag4 Ag 0.11429(2) 0.64716(2) 0.20930(2) 0.05591(11) Uani 1 1 d . B . Ag3 Ag 0.22924(3) 0.74480(3) 0.36096(3) 0.06526(13) Uani 1 1 d . . . Ag5 Ag 0.22148(3) 0.43267(3) 0.20271(3) 0.07454(15) Uani 1 1 d . . . S1 S 0.38306(8) 0.74211(8) 0.21138(7) 0.0510(3) Uani 1 1 d . . . S2 S 0.35722(9) 0.82713(8) 0.38612(8) 0.0573(3) Uani 1 1 d . . . S3 S 0.08069(8) 0.75463(7) 0.29987(8) 0.0544(3) Uani 1 1 d . B . S4 S 0.15110(8) 0.90144(7) 0.18843(8) 0.0507(3) Uani 1 1 d . . . S5 S 0.11058(8) 0.50773(7) 0.25994(8) 0.0548(3) Uani 1 1 d . B . S6 S 0.27763(8) 0.59719(7) 0.37606(7) 0.0482(3) Uani 1 1 d . B . S7 S 0.28844(9) 0.53558(8) 0.12078(8) 0.0572(3) Uani 1 1 d . . . S8 S 0.14310(8) 0.68648(8) 0.08171(7) 0.0545(3) Uani 1 1 d . . . P1 P 0.42793(8) 0.77313(7) 0.32190(8) 0.0485(3) Uani 1 1 d . B . P2 P 0.06085(7) 0.85295(7) 0.23356(8) 0.0458(3) Uani 1 1 d . B . P3 P 0.17206(8) 0.53596(7) 0.36551(7) 0.0462(3) Uani 1 1 d . . . P4 P 0.21071(9) 0.60055(8) 0.04515(7) 0.0522(3) Uani 1 1 d D A . P5 P 0.2193(2) 0.4559(4) 0.7289(2) 0.201(3) Uani 1 1 d . . . F1 F 0.1755(7) 0.4856(12) 0.6553(5) 0.298(7) Uani 1 1 d . . . F2 F 0.2571(13) 0.4147(17) 0.8046(9) 0.447(17) Uani 1 1 d . . . F3 F 0.1419(7) 0.4656(10) 0.7574(5) 0.308(8) Uani 1 1 d . . . F4 F 0.2937(5) 0.4470(11) 0.6937(7) 0.351(10) Uani 1 1 d . . . F5 F 0.2538(13) 0.5257(16) 0.7717(12) 0.464(17) Uani 1 1 d . . . F6 F 0.1941(11) 0.3742(10) 0.6954(12) 0.331(8) Uani 1 1 d . . . O1 O 0.4599(2) 0.6909(2) 0.3602(2) 0.0633(10) Uani 1 1 d . . . O2 O 0.5022(3) 0.8313(3) 0.3266(3) 0.0794(13) Uani 1 1 d . . . O3 O -0.0085(2) 0.8376(3) 0.1613(2) 0.0696(11) Uani 1 1 d . . . O4 O 0.0275(2) 0.9147(2) 0.2870(2) 0.0644(10) Uani 1 1 d . . . O5 O 0.1177(2) 0.5881(2) 0.4102(2) 0.0628(10) Uani 1 1 d . B . O6 O 0.1885(2) 0.4533(2) 0.4080(2) 0.0609(9) Uani 1 1 d . B . O71 O 0.1653(8) 0.5574(7) -0.0304(5) 0.044(3) Uiso 0.25 1 d PD A 1 O72 O 0.1355(5) 0.5496(6) -0.0004(6) 0.076(3) Uiso 0.50 1 d PD A 2 O73 O 0.1650(8) 0.5221(6) 0.0096(8) 0.046(3) Uiso 0.25 1 d PD A 3 O8 O 0.2585(4) 0.6456(3) -0.0098(3) 0.1004(18) Uani 1 1 d . . . O9 O 0.1907(7) 0.7485(7) 0.4967(7) 0.086(3) Uiso 0.50 1 d P B 1 O9' O 0.2154(11) 0.7857(11) 0.4994(10) 0.141(6) Uiso 0.50 1 d P B 2 C1 C 0.4985(5) 0.6834(5) 0.4409(4) 0.101(3) Uani 1 1 d . B . H1A H 0.4618 0.7031 0.4736 0.121 Uiso 1 1 calc R . . H1B H 0.5484 0.7150 0.4513 0.121 Uiso 1 1 calc R . . C2 C 0.5176(7) 0.5998(5) 0.4582(5) 0.130(4) Uani 1 1 d . . . H2A H 0.5435 0.5945 0.5116 0.195 Uiso 1 1 calc R B . H2B H 0.5541 0.5808 0.4259 0.195 Uiso 1 1 calc R . . H2C H 0.4680 0.5690 0.4485 0.195 Uiso 1 1 calc R . . C3 C 0.5615(5) 0.8316(7) 0.2743(7) 0.133(4) Uani 1 1 d D B . H3A H 0.5810 0.8855 0.2683 0.160 Uiso 1 1 calc R . . H3B H 0.5362 0.8115 0.2236 0.160 Uiso 1 1 calc R . . C4 C 0.6305(8) 0.7792(8) 0.3101(8) 0.192(7) Uani 1 1 d D . . H4A H 0.6706 0.7771 0.2773 0.287 Uiso 1 1 calc R B . H4B H 0.6101 0.7264 0.3163 0.287 Uiso 1 1 calc R . . H4C H 0.6553 0.8003 0.3598 0.287 Uiso 1 1 calc R . . C5 C -0.0884(5) 0.8022(7) 0.1717(6) 0.130(4) Uani 1 1 d D B . H5A H -0.1265 0.8448 0.1772 0.156 Uiso 0.25 1 calc PR C 1 H5B H -0.0798 0.7706 0.2188 0.156 Uiso 0.25 1 calc PR C 1 H5C H -0.0970 0.8124 0.2233 0.156 Uiso 0.75 1 d PR C 2 H5D H -0.0891 0.7455 0.1634 0.156 Uiso 0.75 1 d PR C 2 C6 C -0.125(3) 0.749(3) 0.103(2) 0.18(2) Uiso 0.25 1 d PD B 1 H6A H -0.1759 0.7266 0.1119 0.268 Uiso 0.25 1 calc PR B 1 H6B H -0.0876 0.7074 0.0974 0.268 Uiso 0.25 1 calc PR B 1 H6C H -0.1359 0.7811 0.0567 0.268 Uiso 0.25 1 calc PR B 1 C6' C -0.1514(14) 0.8345(14) 0.1152(13) 0.210(9) Uiso 0.75 1 d P B 2 H6'A H -0.2033 0.8129 0.1217 0.315 Uiso 0.75 1 calc PR B 2 H6'B H -0.1418 0.8212 0.0645 0.315 Uiso 0.75 1 calc PR B 2 H6'C H -0.1522 0.8916 0.1208 0.315 Uiso 0.75 1 calc PR B 2 C7 C 0.0005(4) 0.9942(4) 0.2595(5) 0.0825(19) Uani 1 1 d . B . H7A H -0.0463 0.9901 0.2172 0.099 Uiso 1 1 calc R . . H7B H 0.0443 1.0216 0.2406 0.099 Uiso 1 1 calc R . . C8 C -0.0225(5) 1.0397(5) 0.3243(6) 0.114(3) Uani 1 1 d . . . H8A H -0.0405 1.0922 0.3068 0.172 Uiso 1 1 calc R B . H8B H 0.0242 1.0439 0.3658 0.172 Uiso 1 1 calc R . . H8C H -0.0662 1.0125 0.3425 0.172 Uiso 1 1 calc R . . C9 C 0.0319(5) 0.5690(5) 0.4091(6) 0.109(3) Uani 1 1 d . . . H9A H 0.0007 0.5736 0.3568 0.131 Uiso 1 1 calc R B . H9B H 0.0272 0.5145 0.4265 0.131 Uiso 1 1 calc R . . C10 C 0.0000(7) 0.6225(6) 0.4586(8) 0.158(5) Uani 1 1 d . B . H10A H -0.0568 0.6104 0.4575 0.237 Uiso 1 1 calc R . . H10B H 0.0049 0.6764 0.4413 0.237 Uiso 1 1 calc R . . H10C H 0.0302 0.6169 0.5106 0.237 Uiso 1 1 calc R . . C11 C 0.2298(5) 0.4486(4) 0.4892(4) 0.086(2) Uani 1 1 d . . . H11A H 0.1966 0.4743 0.5219 0.103 Uiso 1 1 calc R B . H11B H 0.2823 0.4760 0.4961 0.103 Uiso 1 1 calc R . . C12 C 0.2427(6) 0.3642(4) 0.5114(4) 0.101(3) Uani 1 1 d . B . H12A H 0.2702 0.3608 0.5645 0.152 Uiso 1 1 calc R . . H12B H 0.2756 0.3391 0.4789 0.152 Uiso 1 1 calc R . . H12C H 0.1906 0.3376 0.5053 0.152 Uiso 1 1 calc R . . C131 C 0.102(2) 0.5051(19) -0.012(2) 0.087(8) Uiso 0.25 1 d P A 1 H13A H 0.0575 0.5384 -0.0026 0.104 Uiso 0.25 1 calc PR A 1 H13B H 0.1249 0.4788 0.0367 0.104 Uiso 0.25 1 calc PR A 1 C141 C 0.0651(18) 0.4381(16) -0.0720(16) 0.053(6) Uiso 0.25 1 d P A 1 H14A H 0.0243 0.4084 -0.0517 0.080 Uiso 0.25 1 calc PR A 1 H14B H 0.1079 0.4026 -0.0805 0.080 Uiso 0.25 1 calc PR A 1 H14C H 0.0403 0.4626 -0.1201 0.080 Uiso 0.25 1 calc PR A 1 C132 C 0.1420(10) 0.4798(9) -0.0450(9) 0.087(4) Uiso 0.50 1 d P A 2 H13C H 0.1609 0.4341 -0.0124 0.104 Uiso 0.50 1 calc PR A 2 H13D H 0.1781 0.4880 -0.0817 0.104 Uiso 0.50 1 calc PR A 2 C142 C 0.0525(9) 0.4705(10) -0.0854(9) 0.077(4) Uiso 0.50 1 d P A 2 H14D H 0.0473 0.4246 -0.1188 0.116 Uiso 0.50 1 calc PR A 2 H14E H 0.0354 0.5174 -0.1156 0.116 Uiso 0.50 1 calc PR A 2 H14F H 0.0186 0.4636 -0.0473 0.116 Uiso 0.50 1 calc PR A 2 C133 C 0.0988(14) 0.5364(14) -0.0622(14) 0.060(5) Uiso 0.25 1 d P A 3 H13E H 0.1183 0.5691 -0.1005 0.072 Uiso 0.25 1 calc PR A 3 H13F H 0.0494 0.5597 -0.0496 0.072 Uiso 0.25 1 calc PR A 3 C143 C 0.0858(18) 0.4425(17) -0.0894(17) 0.061(7) Uiso 0.25 1 d P A 3 H14G H 0.0442 0.4392 -0.1354 0.092 Uiso 0.25 1 calc PR A 3 H14H H 0.0691 0.4119 -0.0488 0.092 Uiso 0.25 1 calc PR A 3 H14I H 0.1364 0.4215 -0.0998 0.092 Uiso 0.25 1 calc PR A 3 C15 C 0.3239(7) 0.6173(7) -0.0391(7) 0.153(5) Uani 1 1 d D B . H15A H 0.3055 0.5714 -0.0715 0.184 Uiso 1 1 calc R . . H15B H 0.3652 0.5986 0.0038 0.184 Uiso 1 1 calc R . . C16 C 0.3625(8) 0.6736(7) -0.0844(7) 0.159(5) Uani 1 1 d D . . H16A H 0.4064 0.6474 -0.1031 0.238 Uiso 1 1 calc R B . H16B H 0.3841 0.7180 -0.0523 0.238 Uiso 1 1 calc R . . H16C H 0.3226 0.6924 -0.1275 0.238 Uiso 1 1 calc R . . C17 C 0.1556(6) 0.8021(7) 0.5292(5) 0.111(3) Uani 1 1 d . . . C19 C 0.1504(16) 0.7684(15) 0.6100(15) 0.129(8) Uiso 0.50 1 d P B 1 H19A H 0.1488 0.7111 0.6078 0.194 Uiso 0.50 1 calc PR B 1 H19B H 0.1015 0.7880 0.6254 0.194 Uiso 0.50 1 calc PR B 1 H19C H 0.1976 0.7853 0.6469 0.194 Uiso 0.50 1 calc PR B 1 C18 C 0.1424(15) 0.8756(14) 0.5055(15) 0.115(7) Uiso 0.50 1 d P B 1 H18A H 0.1482 0.8796 0.4524 0.173 Uiso 0.50 1 calc PR B 1 H18B H 0.1814 0.9103 0.5368 0.173 Uiso 0.50 1 calc PR B 1 H18C H 0.0878 0.8912 0.5101 0.173 Uiso 0.50 1 calc PR B 1 C18' C 0.1026(16) 0.8751(15) 0.4975(15) 0.125(8) Uiso 0.50 1 d P B 2 H18D H 0.1138 0.8896 0.4477 0.188 Uiso 0.50 1 calc PR B 2 H18E H 0.1155 0.9192 0.5326 0.188 Uiso 0.50 1 calc PR B 2 H18F H 0.0455 0.8618 0.4925 0.188 Uiso 0.50 1 calc PR B 2 C19' C 0.1120(15) 0.7720(14) 0.5880(15) 0.124(7) Uiso 0.50 1 d P B 2 H19D H 0.0550 0.7857 0.5740 0.187 Uiso 0.50 1 calc PR B 2 H19E H 0.1348 0.7956 0.6372 0.187 Uiso 0.50 1 calc PR B 2 H19F H 0.1177 0.7150 0.5916 0.187 Uiso 0.50 1 calc PR B 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 Ag1 0.0550(2) 0.0640(2) 0.0466(2) -0.00310(17) 0.01055(16) 0.00038(17) Ag2 0.0597(2) 0.0673(3) 0.0572(2) 0.00686(19) 0.01401(19) 0.01113(19) Ag4 0.0573(2) 0.0561(2) 0.0543(2) 0.00690(17) 0.01058(17) 0.00334(17) Ag3 0.0689(3) 0.0664(3) 0.0639(3) 0.0005(2) 0.0213(2) 0.0046(2) Ag5 0.0882(3) 0.0629(3) 0.0717(3) -0.0018(2) 0.0132(2) -0.0032(2) S1 0.0500(6) 0.0621(7) 0.0425(6) -0.0021(5) 0.0126(5) -0.0007(5) S2 0.0766(9) 0.0494(7) 0.0444(7) -0.0068(5) 0.0078(6) 0.0011(6) S3 0.0632(7) 0.0469(6) 0.0587(8) 0.0088(5) 0.0255(6) 0.0040(5) S4 0.0547(7) 0.0438(6) 0.0547(7) 0.0063(5) 0.0130(6) -0.0022(5) S5 0.0551(7) 0.0463(6) 0.0603(8) -0.0005(5) 0.0045(6) -0.0053(5) S6 0.0519(6) 0.0481(6) 0.0450(6) -0.0015(5) 0.0099(5) -0.0017(5) S7 0.0770(9) 0.0472(6) 0.0501(7) -0.0006(5) 0.0193(6) 0.0065(6) S8 0.0612(7) 0.0599(7) 0.0396(6) 0.0052(5) 0.0024(5) 0.0066(6) P1 0.0464(6) 0.0443(6) 0.0515(7) -0.0038(5) 0.0006(5) -0.0044(5) P2 0.0447(6) 0.0437(6) 0.0496(7) 0.0009(5) 0.0107(5) 0.0044(5) P3 0.0555(7) 0.0393(6) 0.0472(7) 0.0049(5) 0.0183(5) 0.0011(5) P4 0.0665(8) 0.0552(7) 0.0344(6) -0.0078(5) 0.0081(6) -0.0072(6) P5 0.130(3) 0.382(8) 0.087(2) -0.088(3) 0.0111(18) 0.059(4) F1 0.242(12) 0.53(3) 0.120(7) 0.001(11) 0.020(7) 0.029(13) F2 0.39(2) 0.76(5) 0.167(11) 0.05(2) -0.015(13) 0.28(3) F3 0.205(9) 0.59(2) 0.149(7) -0.023(11) 0.074(7) 0.127(13) F4 0.120(6) 0.67(3) 0.276(13) -0.273(16) 0.074(7) -0.061(11) F5 0.35(2) 0.68(4) 0.34(2) -0.38(3) 0.018(18) -0.05(3) F6 0.36(2) 0.34(2) 0.34(2) -0.069(17) 0.179(17) 0.008(16) O1 0.071(2) 0.055(2) 0.053(2) -0.0049(17) -0.0146(18) 0.0095(17) O2 0.060(2) 0.073(3) 0.105(4) -0.017(2) 0.014(2) -0.025(2) O3 0.053(2) 0.084(3) 0.066(3) 0.005(2) -0.0020(18) -0.0074(19) O4 0.071(2) 0.053(2) 0.074(3) -0.0007(18) 0.027(2) 0.0157(17) O5 0.067(2) 0.059(2) 0.072(3) -0.0006(18) 0.038(2) 0.0007(17) O6 0.086(3) 0.0437(18) 0.054(2) 0.0112(15) 0.0150(19) -0.0004(17) O8 0.128(4) 0.110(4) 0.082(3) 0.045(3) 0.067(3) 0.041(3) C1 0.129(6) 0.090(5) 0.063(4) -0.009(4) -0.036(4) 0.020(5) C2 0.158(9) 0.104(6) 0.100(7) 0.025(5) -0.045(6) 0.028(6) C3 0.072(5) 0.166(10) 0.163(10) -0.033(8) 0.030(6) -0.043(6) C4 0.141(10) 0.255(18) 0.173(13) -0.081(12) 0.017(10) 0.034(11) C5 0.066(5) 0.178(10) 0.134(8) 0.017(7) -0.015(5) -0.038(5) C7 0.079(4) 0.059(3) 0.111(6) 0.003(3) 0.021(4) 0.023(3) C8 0.099(6) 0.076(5) 0.178(10) -0.036(5) 0.050(6) 0.017(4) C9 0.089(5) 0.103(6) 0.161(8) -0.021(5) 0.090(6) -0.016(4) C10 0.137(8) 0.134(8) 0.245(15) -0.015(9) 0.141(10) -0.005(7) C11 0.147(7) 0.064(4) 0.045(3) 0.009(3) 0.013(4) 0.004(4) C12 0.161(8) 0.076(4) 0.072(5) 0.023(4) 0.035(5) 0.040(5) C15 0.147(9) 0.183(11) 0.157(10) 0.080(9) 0.099(8) 0.049(8) C16 0.177(11) 0.153(10) 0.181(12) 0.015(9) 0.125(10) 0.002(8) C17 0.127(7) 0.142(8) 0.076(5) -0.015(5) 0.048(5) 0.007(6) _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 Ag1 S6 2.4723(13) . ? Ag1 S7 2.5174(14) . ? Ag1 S1 2.6011(14) . ? Ag1 Ag2 3.1042(7) . ? Ag1 Ag4 3.1109(7) . ? Ag1 Ag3 3.3644(7) . ? Ag2 S1 2.4624(13) . ? Ag2 S4 2.4978(13) . ? Ag2 S8 2.6090(14) . ? Ag2 Ag4 3.1651(7) . ? Ag2 Ag5 3.2831(7) 2 ? Ag2 Ag3 3.3211(7) . ? Ag4 S8 2.4696(14) . ? Ag4 S5 2.5021(13) . ? Ag4 S3 2.5331(14) . ? Ag3 S2 2.4992(15) . ? Ag3 S3 2.5004(15) . ? Ag3 O9' 2.579(18) . ? Ag3 O9 2.585(12) . ? Ag3 S6 2.5952(13) . ? Ag5 S2 2.5475(15) 2_545 ? Ag5 S5 2.5842(15) . ? Ag5 S4 2.6212(14) 2_545 ? Ag5 S7 2.6232(15) . ? Ag5 Ag2 3.2831(7) 2_545 ? S1 P1 2.0126(18) . ? S2 P1 1.992(2) . ? S2 Ag5 2.5475(15) 2 ? S3 P2 2.0072(18) . ? S4 P2 1.9950(18) . ? S4 Ag5 2.6212(14) 2 ? S5 P3 1.9975(19) . ? S6 P3 2.0074(17) . ? S7 P4 1.991(2) . ? S8 P4 2.003(2) . ? P1 O2 1.560(4) . ? P1 O1 1.579(4) . ? P2 O3 1.564(4) . ? P2 O4 1.565(4) . ? P3 O5 1.568(4) . ? P3 O6 1.571(3) . ? P4 O8 1.556(5) . ? P4 O71 1.572(5) . ? P4 O73 1.584(5) . ? P4 O72 1.596(5) . ? P5 F1 1.445(12) . ? P5 F5 1.447(17) . ? P5 F3 1.473(10) . ? P5 F4 1.490(9) . ? P5 F6 1.516(17) . ? P5 F2 1.525(15) . ? O1 C1 1.447(7) . ? O2 C3 1.469(11) . ? O3 C5 1.495(9) . ? O4 C7 1.458(7) . ? O5 C9 1.457(8) . ? O6 C11 1.465(7) . ? O71 C131 1.45(3) . ? O72 C132 1.423(18) . ? O73 C133 1.53(3) . ? O8 C15 1.370(10) . ? O9 C17 1.264(14) . ? O9' C17 1.238(18) . ? C1 C2 1.454(10) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C4 1.484(9) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6' 1.41(2) . ? C5 C6 1.527(10) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9602 . ? C5 H5D 0.9598 . ? C6 H5D 1.1169 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C6' H6'A 0.9600 . ? C6' H6'B 0.9600 . ? C6' H6'C 0.9600 . ? C7 C8 1.480(10) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.418(12) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.469(9) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C131 C141 1.59(4) . ? C131 H13A 0.9700 . ? C131 H13B 0.9700 . ? C141 H14A 0.9600 . ? C141 H14B 0.9600 . ? C141 H14C 0.9600 . ? C132 C142 1.53(2) . ? C132 H13C 0.9700 . ? C132 H13D 0.9700 . ? C142 H14D 0.9600 . ? C142 H14E 0.9600 . ? C142 H14F 0.9600 . ? C133 C143 1.65(4) . ? C133 H13E 0.9700 . ? C133 H13F 0.9700 . ? C143 H14G 0.9600 . ? C143 H14H 0.9600 . ? C143 H14I 0.9600 . ? C15 C16 1.458(8) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.30(2) . ? C17 C19' 1.46(3) . ? C17 C19 1.54(3) . ? C17 C18' 1.55(3) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C18' H18D 0.9600 . ? C18' H18E 0.9600 . ? C18' H18F 0.9600 . ? C19' H19D 0.9600 . ? C19' H19E 0.9600 . ? C19' H19F 0.9600 . ? 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 S6 Ag1 S7 136.92(5) . . ? S6 Ag1 S1 119.67(4) . . ? S7 Ag1 S1 102.77(5) . . ? S6 Ag1 Ag2 111.31(3) . . ? S7 Ag1 Ag2 100.96(3) . . ? S1 Ag1 Ag2 50.19(3) . . ? S6 Ag1 Ag4 81.91(3) . . ? S7 Ag1 Ag4 89.81(4) . . ? S1 Ag1 Ag4 111.41(3) . . ? Ag2 Ag1 Ag4 61.228(13) . . ? S6 Ag1 Ag3 49.99(3) . . ? S7 Ag1 Ag3 152.07(4) . . ? S1 Ag1 Ag3 83.08(3) . . ? Ag2 Ag1 Ag3 61.628(15) . . ? Ag4 Ag1 Ag3 62.981(14) . . ? S1 Ag2 S4 138.36(5) . . ? S1 Ag2 S8 115.86(5) . . ? S4 Ag2 S8 104.83(4) . . ? S1 Ag2 Ag1 54.24(3) . . ? S4 Ag2 Ag1 147.91(4) . . ? S8 Ag2 Ag1 79.79(3) . . ? S1 Ag2 Ag4 113.72(4) . . ? S4 Ag2 Ag4 98.88(3) . . ? S8 Ag2 Ag4 49.50(3) . . ? Ag1 Ag2 Ag4 59.490(15) . . ? S1 Ag2 Ag5 88.61(3) . 2 ? S4 Ag2 Ag5 51.78(3) . 2 ? S8 Ag2 Ag5 155.33(4) . 2 ? Ag1 Ag2 Ag5 115.353(19) . 2 ? Ag4 Ag2 Ag5 119.547(19) . 2 ? S1 Ag2 Ag3 86.08(3) . . ? S4 Ag2 Ag3 86.51(3) . . ? S8 Ag2 Ag3 112.38(3) . . ? Ag1 Ag2 Ag3 63.044(14) . . ? Ag4 Ag2 Ag3 62.952(14) . . ? Ag5 Ag2 Ag3 63.716(16) 2 . ? S8 Ag4 S5 126.42(5) . . ? S8 Ag4 S3 119.03(5) . . ? S5 Ag4 S3 114.52(5) . . ? S8 Ag4 Ag1 81.75(3) . . ? S5 Ag4 Ag1 82.63(3) . . ? S3 Ag4 Ag1 109.18(4) . . ? S8 Ag4 Ag2 53.45(3) . . ? S5 Ag4 Ag2 141.90(3) . . ? S3 Ag4 Ag2 80.52(3) . . ? Ag1 Ag4 Ag2 59.282(14) . . ? S2 Ag3 S3 140.81(5) . . ? S2 Ag3 O9' 84.9(4) . . ? S3 Ag3 O9' 97.5(4) . . ? S2 Ag3 O9 100.0(3) . . ? S3 Ag3 O9 89.9(2) . . ? O9' Ag3 O9 16.5(4) . . ? S2 Ag3 S6 105.70(4) . . ? S3 Ag3 S6 111.54(4) . . ? O9' Ag3 S6 103.7(4) . . ? O9 Ag3 S6 93.1(3) . . ? S2 Ag3 Ag2 83.03(3) . . ? S3 Ag3 Ag2 77.87(3) . . ? O9' Ag3 Ag2 153.8(4) . . ? O9 Ag3 Ag2 163.3(2) . . ? S6 Ag3 Ag2 101.92(3) . . ? S2 Ag3 Ag1 93.73(3) . . ? S3 Ag3 Ag1 102.71(4) . . ? O9' Ag3 Ag1 149.0(4) . . ? O9 Ag3 Ag1 139.9(3) . . ? S6 Ag3 Ag1 46.85(3) . . ? Ag2 Ag3 Ag1 55.328(14) . . ? S2 Ag5 S5 104.81(5) 2_545 . ? S2 Ag5 S4 123.92(4) 2_545 2_545 ? S5 Ag5 S4 110.37(5) . 2_545 ? S2 Ag5 S7 109.86(5) 2_545 . ? S5 Ag5 S7 107.56(4) . . ? S4 Ag5 S7 99.49(5) 2_545 . ? S2 Ag5 Ag2 83.11(3) 2_545 2_545 ? S5 Ag5 Ag2 101.45(4) . 2_545 ? S4 Ag5 Ag2 48.47(3) 2_545 2_545 ? S7 Ag5 Ag2 143.34(4) . 2_545 ? P1 S1 Ag2 109.48(7) . . ? P1 S1 Ag1 96.41(6) . . ? Ag2 S1 Ag1 75.57(4) . . ? P1 S2 Ag3 102.80(6) . . ? P1 S2 Ag5 104.80(7) . 2 ? Ag3 S2 Ag5 87.37(5) . 2 ? P2 S3 Ag3 110.07(7) . . ? P2 S3 Ag4 104.37(7) . . ? Ag3 S3 Ag4 84.65(4) . . ? P2 S4 Ag2 101.08(6) . . ? P2 S4 Ag5 110.68(7) . 2 ? Ag2 S4 Ag5 79.74(4) . 2 ? P3 S5 Ag4 93.86(6) . . ? P3 S5 Ag5 101.58(6) . . ? Ag4 S5 Ag5 104.32(5) . . ? P3 S6 Ag1 106.31(6) . . ? P3 S6 Ag3 103.22(6) . . ? Ag1 S6 Ag3 83.16(4) . . ? P4 S7 Ag1 102.69(6) . . ? P4 S7 Ag5 115.92(8) . . ? Ag1 S7 Ag5 82.33(4) . . ? P4 S8 Ag4 108.47(7) . . ? P4 S8 Ag2 109.78(7) . . ? Ag4 S8 Ag2 77.05(4) . . ? O2 P1 O1 108.9(2) . . ? O2 P1 S2 103.39(19) . . ? O1 P1 S2 109.84(18) . . ? O2 P1 S1 110.8(2) . . ? O1 P1 S1 102.71(15) . . ? S2 P1 S1 120.95(8) . . ? O3 P2 O4 107.8(2) . . ? O3 P2 S4 103.63(18) . . ? O4 P2 S4 110.35(17) . . ? O3 P2 S3 110.57(17) . . ? O4 P2 S3 103.30(17) . . ? S4 P2 S3 120.76(8) . . ? O5 P3 O6 108.5(2) . . ? O5 P3 S5 110.86(18) . . ? O6 P3 S5 104.20(16) . . ? O5 P3 S6 104.11(16) . . ? O6 P3 S6 109.62(17) . . ? S5 P3 S6 119.31(8) . . ? O8 P4 O71 85.3(6) . . ? O8 P4 O73 114.8(6) . . ? O71 P4 O73 33.8(6) . . ? O8 P4 O72 113.0(5) . . ? O71 P4 O72 29.3(5) . . ? O73 P4 O72 24.3(5) . . ? O8 P4 S7 109.7(2) . . ? O71 P4 S7 117.3(5) . . ? O73 P4 S7 90.7(5) . . ? O72 P4 S7 112.9(4) . . ? O8 P4 S8 103.5(2) . . ? O71 P4 S8 113.1(5) . . ? O73 P4 S8 117.8(5) . . ? O72 P4 S8 96.4(4) . . ? S7 P4 S8 120.60(8) . . ? F1 P5 F5 105.7(15) . . ? F1 P5 F3 86.8(7) . . ? F5 P5 F3 91.1(9) . . ? F1 P5 F4 88.8(8) . . ? F5 P5 F4 91.1(10) . . ? F3 P5 F4 175.5(7) . . ? F1 P5 F6 84.7(9) . . ? F5 P5 F6 169.3(15) . . ? F3 P5 F6 92.2(10) . . ? F4 P5 F6 86.4(8) . . ? F1 P5 F2 171.9(15) . . ? F5 P5 F2 81.6(12) . . ? F3 P5 F2 89.6(9) . . ? F4 P5 F2 94.6(10) . . ? F6 P5 F2 88.2(14) . . ? C1 O1 P1 123.0(4) . . ? C3 O2 P1 125.9(5) . . ? C5 O3 P2 119.9(5) . . ? C7 O4 P2 121.7(4) . . ? C9 O5 P3 121.7(4) . . ? C11 O6 P3 121.2(4) . . ? C131 O71 P4 109.7(16) . . ? C132 O72 P4 125.5(9) . . ? C133 O73 P4 114.4(12) . . ? C15 O8 P4 126.7(5) . . ? C17 O9 Ag3 130.6(9) . . ? C17 O9' Ag3 132.9(12) . . ? O1 C1 C2 109.1(6) . . ? O1 C1 H1A 109.9 . . ? C2 C1 H1A 109.9 . . ? O1 C1 H1B 109.9 . . ? C2 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? 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 . . ? O2 C3 C4 106.6(10) . . ? O2 C3 H3A 110.4 . . ? C4 C3 H3A 110.4 . . ? O2 C3 H3B 110.4 . . ? C4 C3 H3B 110.4 . . ? H3A C3 H3B 108.6 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6' C5 O3 108.6(12) . . ? C6' C5 C6 62(2) . . ? O3 C5 C6 111(2) . . ? C6' C5 H5A 51.4 . . ? O3 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? C6' C5 H5B 141.4 . . ? O3 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? C6' C5 H5C 112.0 . . ? O3 C5 H5C 109.8 . . ? C6 C5 H5C 137.8 . . ? H5A C5 H5C 63.8 . . ? H5B C5 H5C 46.7 . . ? C6' C5 H5D 106.6 . . ? O3 C5 H5D 111.1 . . ? C6 C5 H5D 46.8 . . ? H5A C5 H5D 138.7 . . ? H5B C5 H5D 65.6 . . ? H5C C5 H5D 108.7 . . ? C5 C6 H5D 38.8 . . ? C5 C6 H6A 109.5 . . ? H5D C6 H6A 98.7 . . ? C5 C6 H6B 109.5 . . ? H5D C6 H6B 79.1 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H5D C6 H6C 144.8 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C6' H6'A 109.5 . . ? C5 C6' H6'B 109.5 . . ? H6'A C6' H6'B 109.5 . . ? C5 C6' H6'C 109.5 . . ? H6'A C6' H6'C 109.5 . . ? H6'B C6' H6'C 109.5 . . ? O4 C7 C8 108.8(6) . . ? O4 C7 H7A 109.9 . . ? C8 C7 H7A 109.9 . . ? O4 C7 H7B 109.9 . . ? C8 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 O5 109.4(7) . . ? C10 C9 H9A 109.8 . . ? O5 C9 H9A 109.8 . . ? C10 C9 H9B 109.8 . . ? O5 C9 H9B 109.8 . . ? H9A C9 H9B 108.2 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O6 C11 C12 109.2(6) . . ? O6 C11 H11A 109.8 . . ? C12 C11 H11A 109.8 . . ? O6 C11 H11B 109.8 . . ? C12 C11 H11B 109.8 . . ? H11A C11 H11B 108.3 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O71 C131 C141 119(3) . . ? O71 C131 H13A 107.5 . . ? C141 C131 H13A 107.5 . . ? O71 C131 H13B 107.5 . . ? C141 C131 H13B 107.5 . . ? H13A C131 H13B 107.0 . . ? C131 C141 H14A 109.5 . . ? C131 C141 H14B 109.5 . . ? H14A C141 H14B 109.5 . . ? C131 C141 H14C 109.5 . . ? H14A C141 H14C 109.5 . . ? H14B C141 H14C 109.5 . . ? O72 C132 C142 99.8(12) . . ? O72 C132 H13C 111.8 . . ? C142 C132 H13C 111.8 . . ? O72 C132 H13D 111.8 . . ? C142 C132 H13D 111.8 . . ? H13C C132 H13D 109.5 . . ? C132 C142 H14D 109.5 . . ? C132 C142 H14E 109.5 . . ? H14D C142 H14E 109.5 . . ? C132 C142 H14F 109.5 . . ? H14D C142 H14F 109.5 . . ? H14E C142 H14F 109.5 . . ? O73 C133 C143 97.1(16) . . ? O73 C133 H13E 112.3 . . ? C143 C133 H13E 112.3 . . ? O73 C133 H13F 112.3 . . ? C143 C133 H13F 112.3 . . ? H13E C133 H13F 109.9 . . ? C133 C143 H14G 109.5 . . ? C133 C143 H14H 109.5 . . ? H14G C143 H14H 109.5 . . ? C133 C143 H14I 109.5 . . ? H14G C143 H14I 109.5 . . ? H14H C143 H14I 109.5 . . ? O8 C15 C16 116.3(9) . . ? O8 C15 H15A 108.2 . . ? C16 C15 H15A 108.2 . . ? O8 C15 H15B 108.2 . . ? C16 C15 H15B 108.2 . . ? H15A C15 H15B 107.4 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O9' C17 O9 34.5(8) . . ? O9' C17 C18 100.0(16) . . ? O9 C17 C18 126.1(14) . . ? O9' C17 C19' 140.2(16) . . ? O9 C17 C19' 114.1(14) . . ? C18 C17 C19' 118.4(16) . . ? O9' C17 C19 119.8(15) . . ? O9 C17 C19 105.6(13) . . ? C18 C17 C19 127.0(16) . . ? C19' C17 C19 26.0(13) . . ? O9' C17 C18' 118.0(15) . . ? O9 C17 C18' 132.6(13) . . ? C18 C17 C18' 24.4(14) . . ? C19' C17 C18' 101.7(15) . . ? C19 C17 C18' 119.5(15) . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? C17 C18' H18D 109.5 . . ? C17 C18' H18E 109.5 . . ? H18D C18' H18E 109.5 . . ? C17 C18' H18F 109.5 . . ? H18D C18' H18F 109.5 . . ? H18E C18' H18F 109.5 . . ? C17 C19' H19D 109.5 . . ? C17 C19' H19E 109.5 . . ? H19D C19' H19E 109.5 . . ? C17 C19' H19F 109.5 . . ? H19D C19' H19F 109.5 . . ? H19E C19' H19F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.40 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.278 _refine_diff_density_min -1.033 _refine_diff_density_rms 0.113 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 753440' #TrackingRef 'Ag-dtp-final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H61 Ag8 F7 O12.50 P7 S12' _chemical_formula_weight 2147.20 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' F F 0.0171 0.0103 '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 Trigonal _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 17.6341(9) _cell_length_b 17.6341(9) _cell_length_c 73.951(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 19915.1(18) _cell_formula_units_Z 12 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9809 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 26.64 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.148 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 12492 _exptl_absorpt_coefficient_mu 2.917 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3738 _exptl_absorpt_correction_T_max 0.6369 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 69781 _diffrn_reflns_av_R_equivalents 0.0493 _diffrn_reflns_av_sigmaI/netI 0.0191 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -87 _diffrn_reflns_limit_l_max 87 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3919 _reflns_number_gt 2993 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. Disordered atoms were refined isotropically. Bond constrains were applied to those disordered atoms using DFIX command in SHELX program. O3, O4, C5, C7, C8 were split and refined isotropically. Bond constrains are: dfix 1.54 0.01 c7 c8 c7' c8' c5 c6 c5' c6 dfix 1.575 0.005 P2 O3 P2 O3' P2 O4 P2 O4' dfix 1.500 0.005 O3 C5 O3' C5' O4 C7 O4 C7' dfix 2.670 0.005 P2 C7 Co-crystallized water molecule was added in this structure resulting in significant lowering the R-values. Ratio between cluster and water is 1/2. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1010P)^2^+127.6166P] 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 3919 _refine_ls_number_parameters 224 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0714 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1804 _refine_ls_wR_factor_gt 0.1661 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.088 _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 Ag1 Ag 0.3333 0.6667 0.053122(14) 0.0682(3) Uani 1 3 d S . . Ag2 Ag 0.45425(5) 0.81253(5) 0.099002(10) 0.0940(3) Uani 1 1 d . . . Ag3 Ag 0.3021(6) 0.8045(8) 0.07680(15) 0.0847(10) Uani 0.50 1 d P . . Ag3' Ag 0.2839(6) 0.8064(8) 0.07452(15) 0.106(2) Uani 0.50 1 d P . . Ag4 Ag 0.3333 0.6667 0.126585(18) 0.1027(4) Uani 1 3 d S . . S1 S 0.45536(15) 0.91195(12) 0.07472(3) 0.0810(6) Uani 1 1 d . . . S2 S 0.49285(11) 0.77215(11) 0.04741(2) 0.0634(4) Uani 1 1 d . . . S3 S 0.58475(15) 0.79118(17) 0.10353(3) 0.0929(7) Uani 1 1 d . . . S4 S 0.43799(19) 0.61044(18) 0.12855(3) 0.0990(7) Uani 1 1 d . . . P1 P 0.49429(12) 0.88453(11) 0.05124(3) 0.0656(5) Uani 1 1 d . . . P2 P 0.55842(17) 0.70629(17) 0.12371(3) 0.0925(7) Uani 1 1 d D . . P3 P 0.3333 0.6667 0.35763(8) 0.160(3) Uani 1 3 d S . . F1 F 0.3333 0.6667 0.08811(8) 0.0656(16) Uani 1 3 d S . . F2 F 0.4064(9) 0.7263(10) 0.3696(3) 0.285(7) Uani 1 1 d . . . F3 F 0.3489(16) 0.7412(13) 0.3463(3) 0.402(14) Uani 1 1 d . . . O1 O 0.4351(4) 0.8946(4) 0.03680(7) 0.0843(15) Uani 1 1 d . . . O2 O 0.5922(4) 0.9561(4) 0.04738(10) 0.1005(19) Uani 1 1 d . . . O3 O 0.6189(7) 0.7603(6) 0.13987(12) 0.081(3) Uiso 0.50 1 d PD A 1 O4 O 0.6265(10) 0.6893(10) 0.1131(2) 0.151(6) Uiso 0.50 1 d PD A 1 O3' O 0.5748(12) 0.7489(9) 0.14314(11) 0.120(5) Uiso 0.50 1 d PD A 2 O4' O 0.6229(8) 0.6703(9) 0.12690(19) 0.112(4) Uiso 0.50 1 d PD A 2 O5 O 0.380(3) 0.747(3) 0.4171(6) 0.117(18) Uani 0.17 1 d P . . C1 C 0.4313(8) 0.8679(8) 0.01794(11) 0.108(3) Uani 1 1 d . . . H1A H 0.4899 0.8936 0.0130 0.129 Uiso 1 1 calc R . . H1B H 0.4040 0.8047 0.0172 0.129 Uiso 1 1 calc R . . C2 C 0.3804(10) 0.8976(11) 0.00788(15) 0.156(6) Uani 1 1 d . . . H2A H 0.3762 0.8799 -0.0045 0.235 Uiso 1 1 calc R . . H2B H 0.4086 0.9603 0.0085 0.235 Uiso 1 1 calc R . . H2C H 0.3227 0.8724 0.0130 0.235 Uiso 1 1 calc R . . C3 C 0.6282(8) 1.0463(7) 0.0494(2) 0.157(6) Uani 1 1 d . . . H3A H 0.5931 1.0639 0.0424 0.188 Uiso 1 1 calc R . . H3B H 0.6221 1.0577 0.0620 0.188 Uiso 1 1 calc R . . C4 C 0.7121(8) 1.0982(9) 0.0447(3) 0.179(7) Uani 1 1 d . . . H4A H 0.7288 1.1582 0.0469 0.269 Uiso 1 1 calc R . . H4B H 0.7193 1.0902 0.0321 0.269 Uiso 1 1 calc R . . H4C H 0.7485 1.0833 0.0518 0.269 Uiso 1 1 calc R . . C5 C 0.5834(11) 0.8109(13) 0.1494(3) 0.112(6) Uiso 0.50 1 d PD A 1 H5A H 0.5312 0.7718 0.1563 0.135 Uiso 0.50 1 calc PR A 1 H5B H 0.5687 0.8431 0.1408 0.135 Uiso 0.50 1 calc PR A 1 C5' C 0.6237(19) 0.8471(10) 0.1430(2) 0.146(10) Uiso 0.50 1 d PD A 2 H5'A H 0.5853 0.8692 0.1396 0.175 Uiso 0.50 1 calc PR A 2 H5'B H 0.6723 0.8693 0.1346 0.175 Uiso 0.50 1 calc PR A 2 C6 C 0.6565(9) 0.8739(11) 0.16215(15) 0.166(7) Uani 1 1 d D . . H6A H 0.6385 0.9097 0.1685 0.249 Uiso 0.50 1 d PR A 1 H6B H 0.6641 0.8368 0.1706 0.249 Uiso 0.50 1 d PR A 1 H6C H 0.7108 0.9107 0.1560 0.249 Uiso 0.50 1 d PR A 1 H6D H 0.6955 0.9358 0.1633 0.249 Uiso 0.50 1 d PR A 2 H6E H 0.6047 0.8570 0.1692 0.249 Uiso 0.50 1 d PR A 2 H6F H 0.6850 0.8431 0.1664 0.249 Uiso 0.50 1 d PR A 2 C7 C 0.6452(15) 0.6198(14) 0.1192(3) 0.114(7) Uiso 0.50 1 d PD A 1 H7A H 0.5998 0.5851 0.1279 0.137 Uiso 0.50 1 calc PR A 1 H7B H 0.6993 0.6501 0.1261 0.137 Uiso 0.50 1 calc PR A 1 C8 C 0.6544(16) 0.5545(14) 0.1077(3) 0.117(7) Uiso 0.50 1 d PD A 1 H8A H 0.6486 0.5072 0.1151 0.175 Uiso 0.50 1 calc PR A 1 H8B H 0.7110 0.5826 0.1020 0.175 Uiso 0.50 1 calc PR A 1 H8C H 0.6096 0.5319 0.0986 0.175 Uiso 0.50 1 calc PR A 1 C7' C 0.612(2) 0.5983(12) 0.1138(6) 0.198(18) Uiso 0.50 1 d PD A 2 H7'A H 0.5515 0.5510 0.1133 0.237 Uiso 0.50 1 calc PR A 2 H7'B H 0.6316 0.6211 0.1017 0.237 Uiso 0.50 1 calc PR A 2 C8' C 0.6713(17) 0.5693(18) 0.1227(3) 0.132(8) Uiso 0.50 1 d PD A 2 H8'A H 0.6841 0.5361 0.1142 0.199 Uiso 0.50 1 calc PR A 2 H8'B H 0.6424 0.5337 0.1330 0.199 Uiso 0.50 1 calc PR A 2 H8'C H 0.7249 0.6200 0.1264 0.199 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 Ag1 0.0582(3) 0.0582(3) 0.0883(6) 0.000 0.000 0.02909(17) Ag2 0.1071(5) 0.0839(5) 0.0895(5) 0.0016(3) 0.0116(4) 0.0465(4) Ag3A 0.0784(17) 0.0841(15) 0.076(2) -0.0067(14) 0.0086(13) 0.0291(13) Ag3B 0.118(5) 0.0879(19) 0.077(3) -0.0078(17) 0.022(3) 0.024(3) Ag4 0.1093(6) 0.1093(6) 0.0896(8) 0.000 0.000 0.0546(3) S1 0.1035(15) 0.0547(9) 0.0766(11) -0.0051(8) 0.0135(10) 0.0333(10) S2 0.0555(9) 0.0590(9) 0.0703(10) -0.0037(7) 0.0061(7) 0.0247(7) S3 0.0727(12) 0.1084(16) 0.0768(11) -0.0109(11) -0.0129(10) 0.0298(12) S4 0.1164(18) 0.1022(16) 0.0803(13) 0.0050(12) -0.0254(12) 0.0562(14) P1 0.0634(10) 0.0502(9) 0.0697(10) 0.0010(7) 0.0091(8) 0.0184(8) P2 0.1055(17) 0.0994(16) 0.0944(15) -0.0309(13) -0.0410(13) 0.0675(14) P3 0.198(5) 0.198(5) 0.082(3) 0.000 0.000 0.099(2) F1 0.063(2) 0.063(2) 0.070(4) 0.000 0.000 0.0317(12) F2 0.256(16) 0.232(15) 0.349(18) -0.064(13) -0.123(13) 0.109(11) F3 0.34(2) 0.41(3) 0.42(2) 0.253(19) -0.03(2) 0.16(3) O1 0.103(4) 0.077(3) 0.083(3) 0.006(3) 0.007(3) 0.053(3) O2 0.071(3) 0.065(3) 0.135(5) 0.004(3) 0.022(3) 0.011(3) O5 0.17(4) 0.13(3) 0.051(13) 0.01(3) -0.01(4) 0.08(3) C1 0.144(9) 0.129(8) 0.071(5) 0.014(5) 0.015(6) 0.083(8) C2 0.177(13) 0.248(18) 0.086(7) 0.025(9) -0.012(8) 0.137(13) C3 0.119(9) 0.072(6) 0.220(14) -0.003(8) 0.056(9) 0.004(6) C4 0.092(8) 0.093(8) 0.32(2) -0.008(11) -0.040(11) 0.019(7) C6 0.151(12) 0.165(13) 0.106(8) -0.029(8) 0.006(8) 0.022(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 Ag1 S2 2.5136(16) 2_665 ? Ag1 S2 2.5136(16) . ? Ag1 S2 2.5136(16) 3_565 ? Ag1 Ag3 3.259(12) . ? Ag1 Ag3 3.259(12) 2_665 ? Ag1 Ag3 3.259(12) 3_565 ? Ag2 S1 2.503(2) . ? Ag2 F1 2.515(2) . ? Ag2 S3 2.533(3) . ? Ag2 S4 2.539(2) 2_665 ? Ag2 Ag3 3.036(12) 3_565 ? Ag2 Ag3 3.089(7) . ? Ag2 Ag3' 3.108(12) 3_565 ? Ag2 Ag4 3.1367(11) . ? Ag3 S1 2.408(10) . ? Ag3 S3 2.516(12) 2_665 ? Ag3 S2 2.586(11) 2_665 ? Ag3 Ag2 3.036(12) 2_665 ? Ag3' S2 2.405(12) 2_665 ? Ag3' S3 2.471(12) 2_665 ? Ag3' S1 2.642(10) . ? Ag3' Ag2 3.108(12) 2_665 ? Ag4 S4 2.498(3) 2_665 ? Ag4 S4 2.498(3) 3_565 ? Ag4 S4 2.498(3) . ? Ag4 Ag2 3.1367(11) 2_665 ? Ag4 Ag2 3.1367(11) 3_565 ? S1 P1 2.012(3) . ? S2 P1 1.989(2) . ? S2 Ag3' 2.405(12) 3_565 ? S2 Ag3 2.586(11) 3_565 ? S3 P2 1.997(4) . ? S3 Ag3' 2.471(12) 3_565 ? S3 Ag3 2.516(12) 3_565 ? S4 P2 1.976(4) . ? S4 Ag2 2.539(2) 3_565 ? P1 O1 1.565(6) . ? P1 O2 1.573(6) . ? P2 O3 1.568(5) . ? P2 O4' 1.573(5) . ? P2 O3' 1.580(5) . ? P2 O4 1.582(5) . ? P3 F3 1.466(13) . ? P3 F3 1.466(14) 2_665 ? P3 F3 1.466(13) 3_565 ? P3 F2 1.480(12) 2_665 ? P3 F2 1.480(12) . ? P3 F2 1.480(12) 3_565 ? F1 Ag2 2.515(2) 2_665 ? F1 Ag2 2.515(2) 3_565 ? O1 C1 1.463(10) . ? O2 C3 1.395(13) . ? O3 C5 1.500(5) . ? O4 C7 1.490(5) . ? O3' C5' 1.499(5) . ? O4' C7' 1.53(3) . ? O5 O5 1.03(8) 10_455 ? O5 O5 1.42(8) 12 ? C1 C2 1.451(15) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C4 1.340(17) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.532(10) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5' C6 1.511(10) . ? C5' H5'A 0.9700 . ? C5' H5'B 0.9700 . ? C6 H6A 0.9597 . ? C6 H6B 0.9599 . ? C6 H6C 0.9600 . ? C6 H6D 0.9600 . ? C6 H6E 0.9599 . ? C6 H6F 0.9603 . ? C7 C8 1.505(10) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C7' C8' 1.528(10) . ? C7' H7'A 0.9700 . ? C7' H7'B 0.9700 . ? C8' H8'A 0.9600 . ? C8' H8'B 0.9600 . ? C8' H8'C 0.9600 . ? 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 S2 Ag1 S2 117.24(3) 2_665 . ? S2 Ag1 S2 117.24(3) 2_665 3_565 ? S2 Ag1 S2 117.24(3) . 3_565 ? S2 Ag1 Ag3 51.26(14) 2_665 . ? S2 Ag1 Ag3 94.73(18) . . ? S2 Ag1 Ag3 144.5(2) 3_565 . ? S2 Ag1 Ag3 94.73(18) 2_665 2_665 ? S2 Ag1 Ag3 144.5(2) . 2_665 ? S2 Ag1 Ag3 51.26(14) 3_565 2_665 ? Ag3 Ag1 Ag3 93.8(3) . 2_665 ? S2 Ag1 Ag3 144.5(2) 2_665 3_565 ? S2 Ag1 Ag3 51.26(14) . 3_565 ? S2 Ag1 Ag3 94.73(18) 3_565 3_565 ? Ag3 Ag1 Ag3 93.8(3) . 3_565 ? Ag3 Ag1 Ag3 93.8(3) 2_665 3_565 ? S1 Ag2 F1 101.09(12) . . ? S1 Ag2 S3 120.62(8) . . ? F1 Ag2 S3 105.00(6) . . ? S1 Ag2 S4 113.02(9) . 2_665 ? F1 Ag2 S4 100.77(13) . 2_665 ? S3 Ag2 S4 113.00(9) . 2_665 ? S1 Ag2 Ag3 99.9(2) . 3_565 ? F1 Ag2 Ag3 61.49(17) . 3_565 ? S3 Ag2 Ag3 52.8(2) . 3_565 ? S4 Ag2 Ag3 145.54(18) 2_665 3_565 ? S1 Ag2 Ag3 49.7(2) . . ? F1 Ag2 Ag3 60.7(2) . . ? S3 Ag2 Ag3 153.7(2) . . ? S4 Ag2 Ag3 92.1(2) 2_665 . ? Ag3 Ag2 Ag3 102.0(4) 3_565 . ? S1 Ag2 Ag3' 95.5(2) . 3_565 ? F1 Ag2 Ag3' 67.43(18) . 3_565 ? S3 Ag2 Ag3' 50.7(2) . 3_565 ? S4 Ag2 Ag3' 151.06(19) 2_665 3_565 ? Ag3 Ag2 Ag3' 6.9(2) 3_565 3_565 ? Ag3 Ag2 Ag3' 103.33(4) . 3_565 ? S1 Ag2 Ag4 143.61(6) . . ? F1 Ag2 Ag4 59.24(13) . . ? S3 Ag2 Ag4 95.04(6) . . ? S4 Ag2 Ag4 50.90(7) 2_665 . ? Ag3 Ag2 Ag4 96.18(14) 3_565 . ? Ag3 Ag2 Ag4 95.1(2) . . ? Ag3' Ag2 Ag4 102.74(15) 3_565 . ? S1 Ag3 S3 123.0(5) . 2_665 ? S1 Ag3 S2 116.4(5) . 2_665 ? S3 Ag3 S2 119.5(3) 2_665 2_665 ? S1 Ag3 Ag2 137.1(3) . 2_665 ? S3 Ag3 Ag2 53.3(2) 2_665 2_665 ? S2 Ag3 Ag2 90.4(3) 2_665 2_665 ? S1 Ag3 Ag2 52.41(14) . . ? S3 Ag3 Ag2 96.1(3) 2_665 . ? S2 Ag3 Ag2 130.7(4) 2_665 . ? Ag2 Ag3 Ag2 84.7(3) 2_665 . ? S1 Ag3 Ag1 90.6(3) . . ? S3 Ag3 Ag1 135.5(5) 2_665 . ? S2 Ag3 Ag1 49.3(2) 2_665 . ? Ag2 Ag3 Ag1 82.3(3) 2_665 . ? Ag2 Ag3 Ag1 81.5(2) . . ? S2 Ag3' S3 129.3(4) 2_665 2_665 ? S2 Ag3' S1 114.4(4) 2_665 . ? S3 Ag3' S1 115.6(4) 2_665 . ? S2 Ag3' Ag2 92.2(4) 2_665 2_665 ? S3 Ag3' Ag2 52.5(2) 2_665 2_665 ? S1 Ag3' Ag2 123.6(3) . 2_665 ? S4 Ag4 S4 119.666(12) 2_665 3_565 ? S4 Ag4 S4 119.666(13) 2_665 . ? S4 Ag4 S4 119.666(13) 3_565 . ? S4 Ag4 Ag2 91.66(7) 2_665 2_665 ? S4 Ag4 Ag2 52.08(6) 3_565 2_665 ? S4 Ag4 Ag2 134.34(7) . 2_665 ? S4 Ag4 Ag2 52.08(6) 2_665 . ? S4 Ag4 Ag2 134.34(7) 3_565 . ? S4 Ag4 Ag2 91.66(7) . . ? Ag2 Ag4 Ag2 82.28(3) 2_665 . ? S4 Ag4 Ag2 134.34(7) 2_665 3_565 ? S4 Ag4 Ag2 91.66(7) 3_565 3_565 ? S4 Ag4 Ag2 52.08(6) . 3_565 ? Ag2 Ag4 Ag2 82.28(3) 2_665 3_565 ? Ag2 Ag4 Ag2 82.28(3) . 3_565 ? P1 S1 Ag3 104.5(3) . . ? P1 S1 Ag2 109.56(10) . . ? Ag3 S1 Ag2 77.9(2) . . ? P1 S1 Ag3' 103.5(3) . . ? Ag3 S1 Ag3' 6.7(5) . . ? Ag2 S1 Ag3' 84.5(2) . . ? P1 S2 Ag3' 113.2(3) . 3_565 ? P1 S2 Ag1 99.52(9) . . ? Ag3' S2 Ag1 87.0(2) 3_565 . ? P1 S2 Ag3 114.4(3) . 3_565 ? Ag3' S2 Ag3 7.6(4) 3_565 3_565 ? Ag1 S2 Ag3 79.4(2) . 3_565 ? P2 S3 Ag3' 111.9(2) . 3_565 ? P2 S3 Ag3 104.8(2) . 3_565 ? Ag3' S3 Ag3 8.6(3) 3_565 3_565 ? P2 S3 Ag2 108.79(12) . . ? Ag3' S3 Ag2 76.8(3) 3_565 . ? Ag3 S3 Ag2 73.9(3) 3_565 . ? P2 S4 Ag4 109.96(13) . . ? P2 S4 Ag2 110.20(13) . 3_565 ? Ag4 S4 Ag2 77.03(7) . 3_565 ? O1 P1 O2 108.1(4) . . ? O1 P1 S2 109.8(2) . . ? O2 P1 S2 103.7(3) . . ? O1 P1 S1 103.5(2) . . ? O2 P1 S1 109.4(3) . . ? S2 P1 S1 121.75(12) . . ? O3 P2 O4' 73.8(7) . . ? O3 P2 O3' 27.2(6) . . ? O4' P2 O3' 93.3(9) . . ? O3 P2 O4 98.2(9) . . ? O4' P2 O4 39.4(7) . . ? O3' P2 O4 124.3(10) . . ? O3 P2 S4 119.7(5) . . ? O4' P2 S4 108.2(6) . . ? O3' P2 S4 96.0(6) . . ? O4 P2 S4 121.4(7) . . ? O3 P2 S3 106.4(5) . . ? O4' P2 S3 118.1(6) . . ? O3' P2 S3 113.9(6) . . ? O4 P2 S3 81.8(5) . . ? S4 P2 S3 121.60(14) . . ? F3 P3 F3 90.4(14) . 2_665 ? F3 P3 F3 90.4(14) . 3_565 ? F3 P3 F3 90.4(14) 2_665 3_565 ? F3 P3 F2 91.6(12) . 2_665 ? F3 P3 F2 90.0(11) 2_665 2_665 ? F3 P3 F2 178.0(12) 3_565 2_665 ? F3 P3 F2 90.0(11) . . ? F3 P3 F2 178.0(12) 2_665 . ? F3 P3 F2 91.6(12) 3_565 . ? F2 P3 F2 88.0(11) 2_665 . ? F3 P3 F2 178.0(13) . 3_565 ? F3 P3 F2 91.6(12) 2_665 3_565 ? F3 P3 F2 90.0(11) 3_565 3_565 ? F2 P3 F2 88.0(11) 2_665 3_565 ? F2 P3 F2 88.0(11) . 3_565 ? Ag2 F1 Ag2 110.26(13) 2_665 . ? Ag2 F1 Ag2 110.26(13) 2_665 3_565 ? Ag2 F1 Ag2 110.26(13) . 3_565 ? C1 O1 P1 122.7(6) . . ? C3 O2 P1 125.9(7) . . ? C5 O3 P2 111.2(8) . . ? C7 O4 P2 120.5(6) . . ? C5' O3' P2 114.0(10) . . ? C7' O4' P2 114.9(13) . . ? O5 O5 O5 119.7(9) 10_455 12 ? C2 C1 O1 108.0(9) . . ? C2 C1 H1A 110.1 . . ? O1 C1 H1A 110.1 . . ? C2 C1 H1B 110.1 . . ? O1 C1 H1B 110.1 . . ? H1A C1 H1B 108.4 . . ? 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 . . ? C4 C3 O2 117.9(13) . . ? C4 C3 H3A 107.8 . . ? O2 C3 H3A 107.8 . . ? C4 C3 H3B 107.8 . . ? O2 C3 H3B 107.8 . . ? H3A C3 H3B 107.2 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O3 C5 C6 105.7(10) . . ? O3 C5 H5A 110.6 . . ? C6 C5 H5A 110.6 . . ? O3 C5 H5B 110.6 . . ? C6 C5 H5B 110.6 . . ? H5A C5 H5B 108.7 . . ? O3' C5' C6 105.4(11) . . ? O3' C5' H5'A 110.7 . . ? C6 C5' H5'A 110.7 . . ? O3' C5' H5'B 110.7 . . ? C6 C5' H5'B 110.7 . . ? H5'A C5' H5'B 108.8 . . ? C5' C6 C5 31.5(11) . . ? C5' C6 H6A 117.8 . . ? C5 C6 H6A 110.1 . . ? C5' C6 H6B 123.7 . . ? C5 C6 H6B 104.9 . . ? H6A C6 H6B 109.5 . . ? C5' C6 H6C 82.4 . . ? C5 C6 H6C 113.3 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.4 . . ? C5' C6 H6D 112.7 . . ? C5 C6 H6D 138.2 . . ? H6A C6 H6D 59.5 . . ? H6B C6 H6D 116.8 . . ? H6C C6 H6D 50.9 . . ? C5' C6 H6E 104.7 . . ? C5 C6 H6E 77.4 . . ? H6A C6 H6E 50.4 . . ? H6B C6 H6E 82.7 . . ? H6C C6 H6E 159.7 . . ? H6D C6 H6E 109.5 . . ? C5' C6 H6F 110.9 . . ? C5 C6 H6F 106.3 . . ? H6A C6 H6F 130.5 . . ? H6B C6 H6F 27.1 . . ? H6C C6 H6F 84.7 . . ? H6D C6 H6F 109.5 . . ? H6E C6 H6F 109.5 . . ? O4 C7 C8 127.7(17) . . ? O4 C7 H7A 105.4 . . ? C8 C7 H7A 105.4 . . ? O4 C7 H7B 105.4 . . ? C8 C7 H7B 105.4 . . ? H7A C7 H7B 106.0 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C8' C7' O4' 100(2) . . ? C8' C7' H7'A 111.7 . . ? O4' C7' H7'A 111.7 . . ? C8' C7' H7'B 111.7 . . ? O4' C7' H7'B 111.7 . . ? H7'A C7' H7'B 109.5 . . ? C7' C8' H8'A 109.5 . . ? C7' C8' H8'B 109.5 . . ? H8'A C8' H8'B 109.5 . . ? C7' C8' H8'C 109.5 . . ? H8'A C8' H8'C 109.5 . . ? H8'B C8' H8'C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.421 _refine_diff_density_min -0.877 _refine_diff_density_rms 0.162 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 753441' #TrackingRef 'Ag-dtp-final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H61 Ag8 Cl F6 O12.50 P7 S12' _chemical_formula_weight 2163.65 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' F F 0.0171 0.0103 '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' Cl Cl 0.1484 0.1585 '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 Trigonal _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 17.6921(8) _cell_length_b 17.6921(8) _cell_length_c 73.951(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 20046.1(16) _cell_formula_units_Z 12 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3820 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 21.47 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.160 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 12648 _exptl_absorpt_coefficient_mu 2.936 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4883 _exptl_absorpt_correction_T_max 0.5393 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25198 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -81 _diffrn_reflns_limit_l_max 87 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.03 _reflns_number_total 3941 _reflns_number_gt 2546 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. Disordered atoms were refined isotropically. Bond constrains were applied to those disordered atoms using DFIX command in SHELX program. O3, C1, C2, C5, C6 were split and refined isotropically. Bond constrains are: dfix 1.54 0.01 c1 c2 c1' c2' c5 c6 c5' c6' c7 c8 dfix 1.50 0.01 o3 c5 o3' c5' o4 c7 dfix 1.580 0.005 p2 o3 p2 o4 p2 o3' Additional constrain for C5 and C5' is applied. It sets the same displacement parameters for them using SHELX command: eadp c5 c5'. New position of O-atom of water was located and refined with sof = 0.16667. So the ratio of cluster and solvent is 1/2. H-atoms on this water are not observed. ; _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^)+(0.0601P)^2^+231.2577P] 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 3941 _refine_ls_number_parameters 207 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0877 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1620 _refine_ls_wR_factor_gt 0.1413 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.078 _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 Ag1 Ag 0.3333 0.6667 0.12693(2) 0.1018(5) Uani 1 3 d S . . Ag2 Ag 0.17357(5) 0.53335(6) 0.100289(12) 0.0878(3) Uani 1 1 d . . . Ag3 Ag 0.29334(6) 0.48765(6) 0.075484(12) 0.0932(3) Uani 1 1 d . . . Ag4 Ag 0.3333 0.6667 0.049401(17) 0.0655(3) Uani 1 3 d S . . Cl1 Cl 0.3333 0.6667 0.08774(5) 0.0600(9) Uani 1 3 d S . . S1 S 0.27978(15) 0.77403(14) 0.04702(3) 0.0644(6) Uani 1 1 d . . . S2 S 0.08738(15) 0.54476(18) 0.07445(3) 0.0785(7) Uani 1 1 d . . . S3 S 0.2099(2) 0.41288(17) 0.10362(4) 0.0903(8) Uani 1 1 d . A . S4 S 0.1725(2) 0.6110(2) 0.12919(4) 0.0975(9) Uani 1 1 d . . . P1 P 0.39023(16) 0.88568(15) 0.05123(3) 0.0666(6) Uani 1 1 d . . . P2 P 0.2948(2) 0.4413(2) 0.12385(4) 0.0918(9) Uani 1 1 d D . . P3 P 0.3333 0.6667 0.35711(11) 0.157(3) Uani 1 3 d S . . F1 F 0.3878(14) 0.7433(14) 0.3455(3) 0.393(14) Uani 1 1 d . . . F2 F 0.3154(13) 0.7253(11) 0.3668(3) 0.310(9) Uani 1 1 d . . . O1 O 0.3634(5) 0.9565(4) 0.04757(11) 0.097(2) Uani 1 1 d D . . O2 O 0.4594(4) 0.8960(4) 0.03671(9) 0.0842(19) Uani 1 1 d . . . O3 O 0.3146(13) 0.3719(12) 0.1149(3) 0.166(8) Uiso 0.50 1 d PD A 1 O3' O 0.3331(12) 0.3797(11) 0.1282(2) 0.129(6) Uiso 0.50 1 d PD A 2 O4 O 0.2445(6) 0.3954(8) 0.14157(10) 0.158(4) Uani 1 1 d D A . C1 C 0.4286(12) 1.0493(12) 0.0469(3) 0.112(4) Uiso 0.67 1 d PD B 1 H1A H 0.4762 1.0588 0.0389 0.134 Uiso 0.67 1 calc PR B 1 H1B H 0.4521 1.0703 0.0589 0.134 Uiso 0.67 1 calc PR B 1 C2 C 0.3832(16) 1.0973(16) 0.0397(3) 0.137(8) Uiso 0.67 1 d PD B 1 H2A H 0.4177 1.1583 0.0426 0.205 Uiso 0.67 1 calc PR B 1 H2B H 0.3267 1.0737 0.0453 0.205 Uiso 0.67 1 calc PR B 1 H2C H 0.3767 1.0903 0.0269 0.205 Uiso 0.67 1 calc PR B 1 C1' C 0.401(3) 1.0367(14) 0.0590(4) 0.112(4) Uiso 0.33 1 d PD B 2 H1'A H 0.4628 1.0590 0.0608 0.134 Uiso 0.33 1 calc PR B 2 H1'B H 0.3729 1.0224 0.0708 0.134 Uiso 0.33 1 calc PR B 2 C2' C 0.387(2) 1.106(2) 0.0501(5) 0.091(10) Uiso 0.33 1 d PD B 2 H2'A H 0.4381 1.1624 0.0517 0.137 Uiso 0.33 1 calc PR B 2 H2'B H 0.3375 1.1060 0.0554 0.137 Uiso 0.33 1 calc PR B 2 H2'C H 0.3769 1.0939 0.0374 0.137 Uiso 0.33 1 calc PR B 2 C3 C 0.4392(9) 0.8724(9) 0.01828(14) 0.110(4) Uani 1 1 d . B . H3A H 0.4093 0.9010 0.0133 0.131 Uiso 1 1 calc R . . H3B H 0.4006 0.8098 0.0173 0.131 Uiso 1 1 calc R . . C4 C 0.5194(11) 0.8980(13) 0.0080(2) 0.165(7) Uani 1 1 d . . . H4A H 0.5050 0.8823 -0.0045 0.248 Uiso 1 1 calc R B . H4B H 0.5481 0.8685 0.0128 0.248 Uiso 1 1 calc R . . H4C H 0.5575 0.9599 0.0090 0.248 Uiso 1 1 calc R . . C5 C 0.4027(14) 0.3892(16) 0.1188(4) 0.112(4) Uiso 0.50 1 d PD A 1 H5A H 0.4251 0.4343 0.1280 0.134 Uiso 0.50 1 calc PR A 1 H5B H 0.4363 0.4161 0.1080 0.134 Uiso 0.50 1 calc PR A 1 C6 C 0.4296(19) 0.3245(17) 0.1247(4) 0.131(10) Uiso 0.50 1 d PD A 1 H6A H 0.4877 0.3553 0.1296 0.197 Uiso 0.50 1 calc PR A 1 H6B H 0.4280 0.2901 0.1146 0.197 Uiso 0.50 1 calc PR A 1 H6C H 0.3901 0.2870 0.1339 0.197 Uiso 0.50 1 calc PR A 1 C5' C 0.3590(15) 0.3460(18) 0.1126(3) 0.112(4) Uiso 0.50 1 d PD A 2 H5'A H 0.3542 0.3768 0.1022 0.134 Uiso 0.50 1 calc PR A 2 H5'B H 0.3128 0.2858 0.1113 0.134 Uiso 0.50 1 calc PR A 2 C6' C 0.4434(14) 0.3447(17) 0.1098(4) 0.108(7) Uiso 0.50 1 d PD A 2 H6'A H 0.4415 0.3179 0.0984 0.163 Uiso 0.50 1 calc PR A 2 H6'B H 0.4504 0.3119 0.1194 0.163 Uiso 0.50 1 calc PR A 2 H6'C H 0.4918 0.4034 0.1100 0.163 Uiso 0.50 1 calc PR A 2 C7 C 0.1737(12) 0.4064(13) 0.1483(2) 0.186(8) Uani 1 1 d D . . H7A H 0.1329 0.3968 0.1386 0.223 Uiso 1 1 calc R A . H7B H 0.1965 0.4654 0.1528 0.223 Uiso 1 1 calc R . . C8 C 0.1278(12) 0.3422(9) 0.16327(19) 0.174(8) Uani 1 1 d D A . H8A H 0.0796 0.3478 0.1675 0.261 Uiso 1 1 calc R . . H8B H 0.1678 0.3536 0.1731 0.261 Uiso 1 1 calc R . . H8C H 0.1067 0.2840 0.1588 0.261 Uiso 1 1 calc R . . O5 O 0.582(3) 0.284(2) 0.0838(6) 0.092(12) Uiso 0.17 1 d P . . 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 Ag1 0.1114(8) 0.1114(8) 0.0826(10) 0.000 0.000 0.0557(4) Ag2 0.0763(5) 0.0923(6) 0.0866(6) 0.0011(4) 0.0094(4) 0.0359(5) Ag3 0.1030(7) 0.1145(7) 0.0827(6) 0.0232(5) 0.0199(5) 0.0699(6) Ag4 0.0599(4) 0.0599(4) 0.0767(8) 0.000 0.000 0.0300(2) Cl1 0.0605(13) 0.0605(13) 0.059(2) 0.000 0.000 0.0302(6) S1 0.0661(13) 0.0607(13) 0.0707(14) -0.0037(11) -0.0102(11) 0.0349(11) S2 0.0568(13) 0.0956(18) 0.0785(16) -0.0121(14) 0.0044(12) 0.0347(13) S3 0.104(2) 0.0685(16) 0.0813(17) 0.0124(13) 0.0153(15) 0.0302(15) S4 0.106(2) 0.096(2) 0.0819(19) 0.0012(15) 0.0260(16) 0.0445(18) P1 0.0742(15) 0.0553(13) 0.0707(15) 0.0038(11) -0.0059(12) 0.0327(12) P2 0.102(2) 0.103(2) 0.093(2) 0.0373(17) 0.0300(17) 0.0680(19) P3 0.193(5) 0.193(5) 0.087(5) 0.000 0.000 0.096(3) F1 0.35(3) 0.49(3) 0.42(2) 0.30(2) 0.23(2) 0.26(2) F2 0.297(19) 0.238(17) 0.39(2) -0.081(16) 0.09(2) 0.134(14) O1 0.109(5) 0.060(4) 0.127(6) -0.002(4) -0.028(5) 0.047(4) O2 0.078(4) 0.083(5) 0.075(4) 0.001(4) 0.000(4) 0.027(4) O4 0.130(8) 0.210(11) 0.121(8) 0.071(8) 0.023(6) 0.075(8) C3 0.120(10) 0.126(10) 0.069(7) 0.015(7) 0.008(7) 0.052(8) C4 0.144(14) 0.25(2) 0.115(12) 0.024(13) 0.039(11) 0.111(15) C7 0.24(2) 0.28(3) 0.120(13) 0.040(15) 0.032(15) 0.19(2) C8 0.176(16) 0.133(13) 0.114(12) -0.023(10) 0.032(11) 0.004(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 Ag1 S4 2.509(3) . ? Ag1 S4 2.509(3) 3_565 ? Ag1 S4 2.509(3) 2_665 ? Ag1 Cl1 2.898(4) . ? Ag1 Ag2 3.2813(13) 3_565 ? Ag1 Ag2 3.2813(13) . ? Ag1 Ag2 3.2813(13) 2_665 ? Ag2 S2 2.515(3) . ? Ag2 S3 2.527(3) . ? Ag2 S4 2.546(3) . ? Ag2 Cl1 2.7834(14) . ? Ag2 Ag3 3.1972(12) . ? Ag3 S3 2.511(3) . ? Ag3 S1 2.517(3) 2_665 ? Ag3 S2 2.524(3) 2_665 ? Ag4 S1 2.517(2) . ? Ag4 S1 2.517(2) 2_665 ? Ag4 S1 2.517(2) 3_565 ? Ag4 Cl1 2.835(4) . ? Cl1 Ag2 2.7834(14) 3_565 ? Cl1 Ag2 2.7834(14) 2_665 ? S1 P1 1.989(3) . ? S1 Ag3 2.517(3) 3_565 ? S2 P1 2.006(3) 2_665 ? S2 Ag3 2.524(3) 3_565 ? S3 P2 1.999(5) . ? S4 P2 1.977(5) 3_565 ? P1 O1 1.569(7) . ? P1 O2 1.569(7) . ? P1 S2 2.006(3) 3_565 ? P2 O4 1.564(5) . ? P2 O3' 1.577(5) . ? P2 O3 1.582(5) . ? P2 S4 1.977(5) 2_665 ? P3 F2 1.423(12) . ? P3 F2 1.423(12) 2_665 ? P3 F2 1.423(12) 3_565 ? P3 F1 1.482(14) 2_665 ? P3 F1 1.482(14) . ? P3 F1 1.482(14) 3_565 ? O1 C1 1.46(2) . ? O1 C1' 1.494(10) . ? O2 C3 1.418(12) . ? O3 C5 1.459(10) . ? O3' C5' 1.471(10) . ? O4 C7 1.450(9) . ? C1 C2 1.527(10) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C1' C2' 1.519(10) . ? C1' H1'A 0.9700 . ? C1' H1'B 0.9700 . ? C2' H2'A 0.9600 . ? C2' H2'B 0.9600 . ? C2' H2'C 0.9600 . ? C3 C4 1.466(18) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.507(10) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C5' C6' 1.521(10) . ? C5' H5'A 0.9700 . ? C5' H5'B 0.9700 . ? C6' H6'A 0.9600 . ? C6' H6'B 0.9600 . ? C6' H6'C 0.9600 . ? C7 C8 1.499(9) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? O5 O5 1.08(7) 16_544 ? O5 O5 1.51(8) 17_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 S4 Ag1 S4 119.560(18) . 3_565 ? S4 Ag1 S4 119.560(18) . 2_665 ? S4 Ag1 S4 119.560(19) 3_565 2_665 ? S4 Ag1 Cl1 93.82(8) . . ? S4 Ag1 Cl1 93.82(8) 3_565 . ? S4 Ag1 Cl1 93.82(8) 2_665 . ? S4 Ag1 Ag2 91.33(8) . 3_565 ? S4 Ag1 Ag2 50.03(7) 3_565 3_565 ? S4 Ag1 Ag2 137.67(8) 2_665 3_565 ? Cl1 Ag1 Ag2 53.10(3) . 3_565 ? S4 Ag1 Ag2 50.03(7) . . ? S4 Ag1 Ag2 137.67(8) 3_565 . ? S4 Ag1 Ag2 91.33(8) 2_665 . ? Cl1 Ag1 Ag2 53.10(3) . . ? Ag2 Ag1 Ag2 87.67(4) 3_565 . ? S4 Ag1 Ag2 137.67(8) . 2_665 ? S4 Ag1 Ag2 91.33(8) 3_565 2_665 ? S4 Ag1 Ag2 50.03(7) 2_665 2_665 ? Cl1 Ag1 Ag2 53.10(3) . 2_665 ? Ag2 Ag1 Ag2 87.67(4) 3_565 2_665 ? Ag2 Ag1 Ag2 87.67(4) . 2_665 ? S2 Ag2 S3 124.18(10) . . ? S2 Ag2 S4 115.20(11) . . ? S3 Ag2 S4 116.56(11) . . ? S2 Ag2 Cl1 94.49(9) . . ? S3 Ag2 Cl1 99.70(7) . . ? S4 Ag2 Cl1 95.81(9) . . ? S2 Ag2 Ag3 95.14(6) . . ? S3 Ag2 Ag3 50.39(6) . . ? S4 Ag2 Ag3 143.42(9) . . ? Cl1 Ag2 Ag3 60.16(4) . . ? S2 Ag2 Ag1 137.51(7) . . ? S3 Ag2 Ag1 93.25(7) . . ? S4 Ag2 Ag1 49.04(8) . . ? Cl1 Ag2 Ag1 56.38(7) . . ? Ag3 Ag2 Ag1 94.85(3) . . ? S3 Ag3 S1 124.67(10) . 2_665 ? S3 Ag3 S2 118.88(10) . 2_665 ? S1 Ag3 S2 116.36(8) 2_665 2_665 ? S3 Ag3 Ag2 50.83(7) . . ? S1 Ag3 Ag2 91.82(6) 2_665 . ? S2 Ag3 Ag2 133.46(7) 2_665 . ? S1 Ag4 S1 119.515(15) . 2_665 ? S1 Ag4 S1 119.515(15) . 3_565 ? S1 Ag4 S1 119.515(15) 2_665 3_565 ? S1 Ag4 Cl1 94.01(6) . . ? S1 Ag4 Cl1 94.01(6) 2_665 . ? S1 Ag4 Cl1 94.01(6) 3_565 . ? Ag2 Cl1 Ag2 109.46(7) 3_565 . ? Ag2 Cl1 Ag2 109.46(7) 3_565 2_665 ? Ag2 Cl1 Ag2 109.46(7) . 2_665 ? Ag2 Cl1 Ag4 109.48(7) 3_565 . ? Ag2 Cl1 Ag4 109.48(7) . . ? Ag2 Cl1 Ag4 109.48(7) 2_665 . ? Ag2 Cl1 Ag1 70.52(7) 3_565 . ? Ag2 Cl1 Ag1 70.52(7) . . ? Ag2 Cl1 Ag1 70.52(7) 2_665 . ? Ag4 Cl1 Ag1 180.0 . . ? P1 S1 Ag3 113.49(13) . 3_565 ? P1 S1 Ag4 100.65(11) . . ? Ag3 S1 Ag4 87.01(8) 3_565 . ? P1 S2 Ag2 111.16(13) 2_665 . ? P1 S2 Ag3 104.61(13) 2_665 3_565 ? Ag2 S2 Ag3 85.85(8) . 3_565 ? P2 S3 Ag3 108.53(15) . . ? P2 S3 Ag2 109.70(15) . . ? Ag3 S3 Ag2 78.78(8) . . ? P2 S4 Ag1 110.63(16) 3_565 . ? P2 S4 Ag2 110.79(16) 3_565 . ? Ag1 S4 Ag2 80.93(9) . . ? O1 P1 O2 108.6(4) . . ? O1 P1 S1 103.1(3) . . ? O2 P1 S1 109.3(3) . . ? O1 P1 S2 109.7(3) . 3_565 ? O2 P1 S2 102.9(3) . 3_565 ? S1 P1 S2 122.75(15) . 3_565 ? O4 P2 O3' 78.4(8) . . ? O4 P2 O3 103.8(10) . . ? O3' P2 O3 37.9(9) . . ? O4 P2 S4 110.2(5) . 2_665 ? O3' P2 S4 106.3(8) . 2_665 ? O3 P2 S4 121.6(8) . 2_665 ? O4 P2 S3 109.6(4) . . ? O3' P2 S3 120.5(7) . . ? O3 P2 S3 85.4(8) . . ? S4 P2 S3 122.91(18) 2_665 . ? F2 P3 F2 96.7(12) . 2_665 ? F2 P3 F2 96.7(12) . 3_565 ? F2 P3 F2 96.7(12) 2_665 3_565 ? F2 P3 F1 88.8(12) . 2_665 ? F2 P3 F1 84.7(12) 2_665 2_665 ? F2 P3 F1 174.2(14) 3_565 2_665 ? F2 P3 F1 84.7(12) . . ? F2 P3 F1 174.2(14) 2_665 . ? F2 P3 F1 88.8(12) 3_565 . ? F1 P3 F1 89.8(14) 2_665 . ? F2 P3 F1 174.2(14) . 3_565 ? F2 P3 F1 88.8(12) 2_665 3_565 ? F2 P3 F1 84.7(12) 3_565 3_565 ? F1 P3 F1 89.8(14) 2_665 3_565 ? F1 P3 F1 89.8(14) . 3_565 ? C1 O1 C1' 39.3(15) . . ? C1 O1 P1 121.3(8) . . ? C1' O1 P1 119.6(12) . . ? C3 O2 P1 123.8(7) . . ? C5 O3 P2 112.4(15) . . ? C5' O3' P2 116.6(14) . . ? C7 O4 P2 121.6(9) . . ? O1 C1 C2 107.4(16) . . ? O1 C1 H1A 110.2 . . ? C2 C1 H1A 110.2 . . ? O1 C1 H1B 110.2 . . ? C2 C1 H1B 110.2 . . ? H1A C1 H1B 108.5 . . ? 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 . . ? O1 C1' C2' 110(2) . . ? O1 C1' H1'A 109.6 . . ? C2' C1' H1'A 109.6 . . ? O1 C1' H1'B 109.6 . . ? C2' C1' H1'B 109.6 . . ? H1'A C1' H1'B 108.1 . . ? C1' C2' H2'A 109.5 . . ? C1' C2' H2'B 109.5 . . ? H2'A C2' H2'B 109.5 . . ? C1' C2' H2'C 109.5 . . ? H2'A C2' H2'C 109.5 . . ? H2'B C2' H2'C 109.5 . . ? O2 C3 C4 110.2(12) . . ? O2 C3 H3A 109.6 . . ? C4 C3 H3A 109.6 . . ? O2 C3 H3B 109.6 . . ? C4 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O3 C5 C6 127(2) . . ? O3 C5 H5A 105.4 . . ? C6 C5 H5A 105.4 . . ? O3 C5 H5B 105.4 . . ? C6 C5 H5B 105.4 . . ? H5A C5 H5B 106.0 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O3' C5' C6' 128(2) . . ? O3' C5' H5'A 105.2 . . ? C6' C5' H5'A 105.2 . . ? O3' C5' H5'B 105.2 . . ? C6' C5' H5'B 105.2 . . ? H5'A C5' H5'B 105.9 . . ? C5' C6' H6'A 109.5 . . ? C5' C6' H6'B 109.5 . . ? H6'A C6' H6'B 109.5 . . ? C5' C6' H6'C 109.5 . . ? H6'A C6' H6'C 109.5 . . ? H6'B C6' H6'C 109.5 . . ? O4 C7 C8 109.2(12) . . ? O4 C7 H7A 109.8 . . ? C8 C7 H7A 109.8 . . ? O4 C7 H7B 109.8 . . ? C8 C7 H7B 109.8 . . ? H7A C7 H7B 108.3 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O5 O5 O5 119.7(8) 16_544 17_554 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.439 _refine_diff_density_min -0.978 _refine_diff_density_rms 0.118 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 753442' #TrackingRef 'Ag-dtp-final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H62 Ag8 F6 O12.50 P7 S12' _chemical_formula_weight 2129.21 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' F F 0.0171 0.0103 '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 Trigonal _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 17.4115(10) _cell_length_b 17.4115(10) _cell_length_c 74.436(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 19543(2) _cell_formula_units_Z 12 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4277 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 23.98 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.171 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 12396 _exptl_absorpt_coefficient_mu 2.970 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2725 _exptl_absorpt_correction_T_max 0.8556 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36231 _diffrn_reflns_av_R_equivalents 0.0495 _diffrn_reflns_av_sigmaI/netI 0.0251 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -73 _diffrn_reflns_limit_l_max 88 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3831 _reflns_number_gt 3006 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. Disordered atoms were refined isotropically. Bond constrains were applied to those disordered atoms using DFIX command in SHELX program. O4, C1, C2, C7, C8 were split and refined isotropically. Bond constrains are: dfix 1.50 0.01 o3 c5 dfix 1.54 0.01 c1 c2 c1' c2' c5 c6 Additional constrain for C2 and C2' is applied. It sets the same displacement parameters for them using SHELX command: eadp c2 c2'. New and more reasonable H-atom on water (with sof = 1/6) was located from difference map and was not refined during least-square refinements (riding on the O5-atom). Small void (less than 2%) was observed in the unit cell. ; _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^)+(0.0767P)^2^+408.2965P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3831 _refine_ls_number_parameters 208 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0773 _refine_ls_R_factor_gt 0.0616 _refine_ls_wR_factor_ref 0.1732 _refine_ls_wR_factor_gt 0.1652 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.076 _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 Ag1 Ag 0.3333 0.6667 0.05926(2) 0.0643(4) Uani 1 3 d S . . Ag2 Ag 0.22035(5) 0.57837(6) 0.094260(11) 0.0688(3) Uani 1 1 d . . . Ag3 Ag 0.3333 0.6667 0.12706(2) 0.0771(4) Uani 1 3 d S . . Ag4 Ag 0.18420(7) 0.71834(8) 0.073295(13) 0.1001(4) Uani 1 1 d . . . S1 S 0.22750(15) 0.51030(15) 0.04615(3) 0.0561(5) Uani 1 1 d . . . S2 S 0.08906(16) 0.5493(2) 0.07376(3) 0.0750(8) Uani 1 1 d . . . S3 S 0.1976(2) 0.41871(17) 0.10242(4) 0.0787(8) Uani 1 1 d . . . S4 S 0.16877(18) 0.60998(19) 0.12562(4) 0.0701(7) Uani 1 1 d . A . P1 P 0.11425(15) 0.51049(17) 0.05015(3) 0.0584(6) Uani 1 1 d . B . P2 P 0.15249(19) 0.7141(2) 0.12139(4) 0.0767(8) Uani 1 1 d . . . P3 P 0.3333 0.6667 0.35827(12) 0.155(4) Uani 1 3 d S . . F1 F 0.3161(13) 0.7292(11) 0.3686(3) 0.270(9) Uani 1 1 d . . . F2 F 0.3911(19) 0.7416(18) 0.3466(3) 0.400(19) Uani 1 1 d . . . O1 O 0.0405(5) 0.4121(5) 0.04615(11) 0.088(2) Uani 1 1 d . . . O2 O 0.1054(5) 0.5709(5) 0.03604(9) 0.0714(18) Uani 1 1 d . . . O3 O 0.1571(8) 0.7619(6) 0.13880(14) 0.138(5) Uani 1 1 d D A . O4 O 0.0547(9) 0.6853(9) 0.11194(18) 0.059(3) Uiso 0.50 1 d P A 1 O4' O 0.0555(13) 0.6791(13) 0.1257(3) 0.101(5) Uiso 0.50 1 d P A 2 O5 O 0.3333 0.725(3) 0.4167 0.17(3) Uani 0.33 2 d SP . . H5O H 0.2754 0.7279 0.4153 0.207 Uiso 0.33 1 d PR . . C1 C -0.0503(11) 0.3837(10) 0.0477(2) 0.085(4) Uiso 0.75 1 d PD B 1 H1A H -0.0691 0.4055 0.0376 0.102 Uiso 0.75 1 calc PR B 1 H1B H -0.0610 0.4070 0.0586 0.102 Uiso 0.75 1 calc PR B 1 C2 C -0.103(2) 0.2828(11) 0.0480(4) 0.157(10) Uiso 0.75 1 d PD B 1 H2A H -0.1648 0.2631 0.0492 0.236 Uiso 0.75 1 calc PR B 1 H2B H -0.0839 0.2616 0.0580 0.236 Uiso 0.75 1 calc PR B 1 H2C H -0.0926 0.2602 0.0371 0.236 Uiso 0.75 1 calc PR B 1 C1' C -0.039(4) 0.349(4) 0.0570(7) 0.099(16) Uiso 0.25 1 d PD B 2 H1'A H -0.0675 0.3768 0.0633 0.119 Uiso 0.25 1 calc PR B 2 H1'B H -0.0283 0.3113 0.0650 0.119 Uiso 0.25 1 calc PR B 2 C2' C -0.087(6) 0.302(6) 0.0394(9) 0.157(10) Uiso 0.25 1 d PD B 2 H2'A H -0.1445 0.2530 0.0421 0.236 Uiso 0.25 1 calc PR B 2 H2'B H -0.0526 0.2807 0.0332 0.236 Uiso 0.25 1 calc PR B 2 H2'C H -0.0929 0.3433 0.0318 0.236 Uiso 0.25 1 calc PR B 2 C3 C 0.1312(9) 0.5739(10) 0.01730(15) 0.090(3) Uani 1 1 d . B . H3A H 0.1950 0.5993 0.0165 0.108 Uiso 1 1 calc R . . H3B H 0.1031 0.5143 0.0124 0.108 Uiso 1 1 calc R . . C4 C 0.1045(14) 0.6265(14) 0.0074(2) 0.150(7) Uani 1 1 d . . . H4A H 0.1226 0.6301 -0.0049 0.224 Uiso 1 1 calc R B . H4B H 0.1316 0.6851 0.0124 0.224 Uiso 1 1 calc R . . H4C H 0.0411 0.5999 0.0079 0.224 Uiso 1 1 calc R . . C5 C 0.2399(10) 0.8308(15) 0.1462(2) 0.180(11) Uani 1 1 d D . . H5A H 0.2700 0.8777 0.1374 0.216 Uiso 1 1 calc R A . H5B H 0.2780 0.8067 0.1491 0.216 Uiso 1 1 calc R . . C6 C 0.2223(15) 0.8681(12) 0.16295(18) 0.152(8) Uani 1 1 d D A . H6A H 0.2766 0.9179 0.1671 0.228 Uiso 1 1 calc R . . H6B H 0.1988 0.8233 0.1721 0.228 Uiso 1 1 calc R . . H6C H 0.1801 0.8868 0.1603 0.228 Uiso 1 1 calc R . . C7 C -0.0251(16) 0.6122(16) 0.1204(3) 0.069(6) Uiso 0.50 1 d P A 1 H7A H -0.0083 0.5753 0.1272 0.083 Uiso 0.50 1 calc PR A 1 H7B H -0.0498 0.6368 0.1288 0.083 Uiso 0.50 1 calc PR A 1 C8 C -0.0898(16) 0.5598(16) 0.1079(3) 0.083(6) Uiso 0.50 1 d P A 1 H8A H -0.1403 0.5136 0.1140 0.124 Uiso 0.50 1 calc PR A 1 H8B H -0.0663 0.5339 0.0998 0.124 Uiso 0.50 1 calc PR A 1 H8C H -0.1074 0.5959 0.1013 0.124 Uiso 0.50 1 calc PR A 1 C7' C -0.007(3) 0.624(3) 0.1120(5) 0.126(12) Uiso 0.50 1 d P A 2 H7'A H 0.0117 0.5860 0.1062 0.151 Uiso 0.50 1 calc PR A 2 H7'B H -0.0162 0.6589 0.1031 0.151 Uiso 0.50 1 calc PR A 2 C8' C -0.091(2) 0.570(2) 0.1245(5) 0.123(10) Uiso 0.50 1 d P A 2 H8'A H -0.1395 0.5279 0.1174 0.184 Uiso 0.50 1 calc PR A 2 H8'B H -0.1059 0.6103 0.1301 0.184 Uiso 0.50 1 calc PR A 2 H8'C H -0.0770 0.5395 0.1336 0.184 Uiso 0.50 1 calc PR A 2 H0 H 0.3333 0.6667 0.0840(18) 0.050 Uiso 1 3 d S . . 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 Ag1 0.0492(4) 0.0492(4) 0.0945(10) 0.000 0.000 0.0246(2) Ag2 0.0621(5) 0.0731(5) 0.0678(5) -0.0089(4) -0.0023(4) 0.0313(4) Ag3 0.0763(6) 0.0763(6) 0.0787(9) 0.000 0.000 0.0382(3) Ag4 0.0758(6) 0.1328(9) 0.0716(6) -0.0305(6) -0.0008(4) 0.0371(6) S1 0.0521(12) 0.0525(12) 0.0576(12) -0.0063(10) 0.0027(10) 0.0215(10) S2 0.0447(12) 0.112(2) 0.0597(14) -0.0183(14) 0.0005(10) 0.0328(14) S3 0.0905(19) 0.0522(14) 0.0589(14) 0.0037(11) 0.0119(13) 0.0099(13) S4 0.0661(15) 0.0764(17) 0.0673(15) 0.0032(12) 0.0152(12) 0.0353(13) P1 0.0409(12) 0.0636(15) 0.0549(13) -0.0102(11) -0.0022(10) 0.0144(11) P2 0.0591(15) 0.0710(17) 0.096(2) -0.0318(15) 0.0069(14) 0.0294(14) P3 0.191(6) 0.191(6) 0.082(5) 0.000 0.000 0.096(3) F1 0.270(19) 0.187(15) 0.35(2) -0.074(15) 0.074(19) 0.112(14) F2 0.43(4) 0.54(5) 0.35(2) 0.27(3) 0.27(3) 0.33(3) O1 0.050(4) 0.078(5) 0.101(6) -0.024(4) -0.001(4) 0.006(4) O2 0.069(4) 0.088(5) 0.063(4) -0.010(4) -0.006(3) 0.044(4) O3 0.177(11) 0.085(6) 0.098(7) -0.025(5) 0.052(7) 0.027(7) O5 0.28(7) 0.20(4) 0.06(2) -0.011(19) -0.02(4) 0.14(3) C3 0.101(9) 0.111(10) 0.071(7) 0.002(7) -0.009(6) 0.062(8) C4 0.22(2) 0.19(2) 0.091(10) 0.008(12) 0.001(12) 0.147(19) C5 0.128(15) 0.28(3) 0.090(11) -0.022(15) 0.001(11) 0.066(19) C6 0.26(2) 0.150(15) 0.092(10) -0.056(10) -0.052(13) 0.139(18) _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 Ag1 S1 2.597(2) 3_565 ? Ag1 S1 2.597(2) . ? Ag1 S1 2.597(2) 2_665 ? Ag1 Ag2 3.1619(15) 3_565 ? Ag1 Ag2 3.1619(15) . ? Ag1 Ag2 3.1619(15) 2_665 ? Ag1 Ag4 3.3136(12) . ? Ag1 Ag4 3.3136(12) 3_565 ? Ag1 Ag4 3.3136(12) 2_665 ? Ag1 H0 1.85(14) . ? Ag2 S2 2.579(3) . ? Ag2 S4 2.655(3) . ? Ag2 S3 2.674(3) . ? Ag2 Ag3 3.0285(15) . ? Ag2 Ag4 3.0828(13) 2_665 ? Ag2 Ag2 3.1028(14) 3_565 ? Ag2 Ag2 3.1028(14) 2_665 ? Ag2 Ag4 3.2100(16) . ? Ag2 H0 1.95(5) . ? Ag3 S4 2.523(3) . ? Ag3 S4 2.523(3) 3_565 ? Ag3 S4 2.523(3) 2_665 ? Ag3 Ag2 3.0285(15) 3_565 ? Ag3 Ag2 3.0285(15) 2_665 ? Ag4 S1 2.510(3) 3_565 ? Ag4 S3 2.513(3) 3_565 ? Ag4 S2 2.557(4) . ? Ag4 Ag2 3.0828(13) 3_565 ? S1 P1 1.996(3) . ? S1 Ag4 2.510(3) 2_665 ? S2 P1 2.008(3) . ? S3 P2 1.988(5) 2_665 ? S3 Ag4 2.513(3) 2_665 ? S4 P2 1.994(4) . ? P1 O2 1.548(8) . ? P1 O1 1.572(7) . ? P2 O4' 1.52(2) . ? P2 O3 1.521(9) . ? P2 O4 1.670(14) . ? P2 S3 1.988(5) 3_565 ? P3 F2 1.468(18) 2_665 ? P3 F2 1.468(19) . ? P3 F2 1.468(18) 3_565 ? P3 F1 1.480(14) . ? P3 F1 1.480(14) 2_665 ? P3 F1 1.480(14) 3_565 ? O1 C1 1.405(18) . ? O1 C1' 1.51(6) . ? O2 C3 1.458(13) . ? O3 C5 1.446(9) . ? O4 C7 1.48(3) . ? O4' C7' 1.44(4) . ? O5 O5 1.77(9) 2_665 ? O5 O5 1.77(9) 3_565 ? O5 H5O 1.0366 . ? C1 C2 1.521(10) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C1' C2' 1.545(10) . ? C1' H1'A 0.9700 . ? C1' H1'B 0.9700 . ? C2' H2'A 0.9600 . ? C2' H2'B 0.9600 . ? C2' H2'C 0.9600 . ? C3 C4 1.425(19) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.505(9) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.39(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C7' C8' 1.58(5) . ? C7' H7'A 0.9700 . ? C7' H7'B 0.9700 . ? C8' H8'A 0.9600 . ? C8' H8'B 0.9600 . ? C8' H8'C 0.9600 . ? 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 S1 Ag1 S1 106.75(7) 3_565 . ? S1 Ag1 S1 106.75(7) 3_565 2_665 ? S1 Ag1 S1 106.75(7) . 2_665 ? S1 Ag1 Ag2 81.78(6) 3_565 3_565 ? S1 Ag1 Ag2 140.03(7) . 3_565 ? S1 Ag1 Ag2 107.78(6) 2_665 3_565 ? S1 Ag1 Ag2 107.78(6) 3_565 . ? S1 Ag1 Ag2 81.78(6) . . ? S1 Ag1 Ag2 140.03(7) 2_665 . ? Ag2 Ag1 Ag2 58.77(3) 3_565 . ? S1 Ag1 Ag2 140.03(7) 3_565 2_665 ? S1 Ag1 Ag2 107.78(6) . 2_665 ? S1 Ag1 Ag2 81.78(6) 2_665 2_665 ? Ag2 Ag1 Ag2 58.77(3) 3_565 2_665 ? Ag2 Ag1 Ag2 58.77(3) . 2_665 ? S1 Ag1 Ag4 48.41(6) 3_565 . ? S1 Ag1 Ag4 99.30(5) . . ? S1 Ag1 Ag4 149.05(6) 2_665 . ? Ag2 Ag1 Ag4 56.80(3) 3_565 . ? Ag2 Ag1 Ag4 59.38(3) . . ? Ag2 Ag1 Ag4 106.10(5) 2_665 . ? S1 Ag1 Ag4 99.30(5) 3_565 3_565 ? S1 Ag1 Ag4 149.05(6) . 3_565 ? S1 Ag1 Ag4 48.41(6) 2_665 3_565 ? Ag2 Ag1 Ag4 59.38(3) 3_565 3_565 ? Ag2 Ag1 Ag4 106.10(5) . 3_565 ? Ag2 Ag1 Ag4 56.80(3) 2_665 3_565 ? Ag4 Ag1 Ag4 110.54(3) . 3_565 ? S1 Ag1 Ag4 149.05(6) 3_565 2_665 ? S1 Ag1 Ag4 48.41(6) . 2_665 ? S1 Ag1 Ag4 99.30(5) 2_665 2_665 ? Ag2 Ag1 Ag4 106.10(5) 3_565 2_665 ? Ag2 Ag1 Ag4 56.80(3) . 2_665 ? Ag2 Ag1 Ag4 59.38(3) 2_665 2_665 ? Ag4 Ag1 Ag4 110.54(3) . 2_665 ? Ag4 Ag1 Ag4 110.54(3) 3_565 2_665 ? S1 Ag1 H0 112.07(6) 3_565 . ? S1 Ag1 H0 112.07(6) . . ? S1 Ag1 H0 112.07(6) 2_665 . ? Ag2 Ag1 H0 34.51(2) 3_565 . ? Ag2 Ag1 H0 34.51(2) . . ? Ag2 Ag1 H0 34.51(2) 2_665 . ? Ag4 Ag1 H0 71.62(3) . . ? Ag4 Ag1 H0 71.62(3) 3_565 . ? Ag4 Ag1 H0 71.62(3) 2_665 . ? S2 Ag2 S4 101.69(9) . . ? S2 Ag2 S3 105.89(10) . . ? S4 Ag2 S3 97.24(9) . . ? S2 Ag2 Ag3 149.75(7) . . ? S4 Ag2 Ag3 52.21(7) . . ? S3 Ag2 Ag3 93.77(7) . . ? S2 Ag2 Ag4 97.47(7) . 2_665 ? S4 Ag2 Ag4 146.83(7) . 2_665 ? S3 Ag2 Ag4 51.16(6) . 2_665 ? Ag3 Ag2 Ag4 112.79(3) . 2_665 ? S2 Ag2 Ag2 109.29(8) . 3_565 ? S4 Ag2 Ag2 85.20(7) . 3_565 ? S3 Ag2 Ag2 143.46(8) . 3_565 ? Ag3 Ag2 Ag2 59.185(19) . 3_565 ? Ag4 Ag2 Ag2 113.60(3) 2_665 3_565 ? S2 Ag2 Ag2 143.32(6) . 2_665 ? S4 Ag2 Ag2 111.39(6) . 2_665 ? S3 Ag2 Ag2 85.70(8) . 2_665 ? Ag3 Ag2 Ag2 59.185(19) . 2_665 ? Ag4 Ag2 Ag2 62.52(4) 2_665 2_665 ? Ag2 Ag2 Ag2 60.0 3_565 2_665 ? S2 Ag2 Ag1 83.27(6) . . ? S4 Ag2 Ag1 144.71(7) . . ? S3 Ag2 Ag1 115.18(7) . . ? Ag3 Ag2 Ag1 109.23(3) . . ? Ag4 Ag2 Ag1 64.08(3) 2_665 . ? Ag2 Ag2 Ag1 60.617(17) 3_565 . ? Ag2 Ag2 Ag1 60.617(17) 2_665 . ? S2 Ag2 Ag4 51.00(8) . . ? S4 Ag2 Ag4 93.15(7) . . ? S3 Ag2 Ag4 156.36(7) . . ? Ag3 Ag2 Ag4 109.32(3) . . ? Ag4 Ag2 Ag4 119.86(4) 2_665 . ? Ag2 Ag2 Ag4 58.43(3) 3_565 . ? Ag2 Ag2 Ag4 110.14(3) 2_665 . ? Ag1 Ag2 Ag4 62.66(2) . . ? S2 Ag2 H0 112(3) . . ? S4 Ag2 H0 120(3) . . ? S3 Ag2 H0 118.4(2) . . ? Ag3 Ag2 H0 77(4) . . ? Ag4 Ag2 H0 76.7(17) 2_665 . ? Ag2 Ag2 H0 37(2) 3_565 . ? Ag2 Ag2 H0 37(2) 2_665 . ? Ag1 Ag2 H0 32(4) . . ? Ag4 Ag2 H0 73.4(16) . . ? S4 Ag3 S4 119.819(11) . 3_565 ? S4 Ag3 S4 119.819(11) . 2_665 ? S4 Ag3 S4 119.819(11) 3_565 2_665 ? S4 Ag3 Ag2 56.27(7) . . ? S4 Ag3 Ag2 117.89(8) 3_565 . ? S4 Ag3 Ag2 89.10(7) 2_665 . ? S4 Ag3 Ag2 89.10(7) . 3_565 ? S4 Ag3 Ag2 56.27(7) 3_565 3_565 ? S4 Ag3 Ag2 117.89(8) 2_665 3_565 ? Ag2 Ag3 Ag2 61.63(4) . 3_565 ? S4 Ag3 Ag2 117.89(8) . 2_665 ? S4 Ag3 Ag2 89.10(7) 3_565 2_665 ? S4 Ag3 Ag2 56.27(7) 2_665 2_665 ? Ag2 Ag3 Ag2 61.63(4) . 2_665 ? Ag2 Ag3 Ag2 61.63(4) 3_565 2_665 ? S1 Ag4 S3 123.22(11) 3_565 3_565 ? S1 Ag4 S2 111.78(8) 3_565 . ? S3 Ag4 S2 119.28(10) 3_565 . ? S1 Ag4 Ag2 84.77(6) 3_565 3_565 ? S3 Ag4 Ag2 55.99(7) 3_565 3_565 ? S2 Ag4 Ag2 110.53(8) . 3_565 ? S1 Ag4 Ag2 108.65(7) 3_565 . ? S3 Ag4 Ag2 86.15(7) 3_565 . ? S2 Ag4 Ag2 51.63(7) . . ? Ag2 Ag4 Ag2 59.04(4) 3_565 . ? S1 Ag4 Ag1 50.70(6) 3_565 . ? S3 Ag4 Ag1 115.04(8) 3_565 . ? S2 Ag4 Ag1 80.56(6) . . ? Ag2 Ag4 Ag1 59.12(3) 3_565 . ? Ag2 Ag4 Ag1 57.96(3) . . ? P1 S1 Ag4 113.83(13) . 2_665 ? P1 S1 Ag1 97.23(11) . . ? Ag4 S1 Ag1 80.89(8) 2_665 . ? P1 S2 Ag4 104.52(14) . . ? P1 S2 Ag2 105.24(13) . . ? Ag4 S2 Ag2 77.37(8) . . ? P2 S3 Ag4 106.38(16) 2_665 2_665 ? P2 S3 Ag2 106.38(14) 2_665 . ? Ag4 S3 Ag2 72.85(7) 2_665 . ? P2 S4 Ag3 107.51(14) . . ? P2 S4 Ag2 105.43(14) . . ? Ag3 S4 Ag2 71.52(8) . . ? O2 P1 O1 107.9(4) . . ? O2 P1 S1 109.5(3) . . ? O1 P1 S1 103.8(3) . . ? O2 P1 S2 104.6(3) . . ? O1 P1 S2 109.6(3) . . ? S1 P1 S2 120.89(15) . . ? O4' P2 O3 77.4(9) . . ? O3 P2 O4 106.8(7) . . ? O4' P2 S3 125.4(8) . 3_565 ? O3 P2 S3 109.6(4) . 3_565 ? O4 P2 S3 93.5(5) . 3_565 ? O4' P2 S4 103.8(8) . . ? O3 P2 S4 111.7(5) . . ? O4 P2 S4 112.4(5) . . ? S3 P2 S4 120.79(17) 3_565 . ? F2 P3 F2 88.6(17) 2_665 . ? F2 P3 F2 88.6(17) 2_665 3_565 ? F2 P3 F2 88.6(16) . 3_565 ? F2 P3 F1 88.2(14) 2_665 . ? F2 P3 F1 87.3(13) . . ? F2 P3 F1 174.9(17) 3_565 . ? F2 P3 F1 87.3(14) 2_665 2_665 ? F2 P3 F1 174.9(17) . 2_665 ? F2 P3 F1 88.2(14) 3_565 2_665 ? F1 P3 F1 95.6(13) . 2_665 ? F2 P3 F1 174.9(17) 2_665 3_565 ? F2 P3 F1 88.2(14) . 3_565 ? F2 P3 F1 87.3(13) 3_565 3_565 ? F1 P3 F1 95.6(13) . 3_565 ? F1 P3 F1 95.6(13) 2_665 3_565 ? C1 O1 P1 122.0(9) . . ? C1' O1 P1 131(2) . . ? C3 O2 P1 122.6(7) . . ? C5 O3 P2 122.5(9) . . ? C7 O4 P2 117.2(12) . . ? C7' O4' P2 116(2) . . ? O5 O5 O5 60.000(7) 2_665 3_565 ? O5 O5 H5O 92.1 2_665 . ? O5 O5 H5O 151.6 3_565 . ? O1 C1 C2 109.2(17) . . ? O1 C1 H1A 109.8 . . ? C2 C1 H1A 109.8 . . ? O1 C1 H1B 109.8 . . ? C2 C1 H1B 109.8 . . ? H1A C1 H1B 108.3 . . ? 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 . . ? O1 C1' C2' 89(5) . . ? O1 C1' H1'A 113.8 . . ? C2' C1' H1'A 113.8 . . ? O1 C1' H1'B 113.8 . . ? C2' C1' H1'B 113.8 . . ? H1'A C1' H1'B 111.0 . . ? C1' C2' H2'A 109.5 . . ? C1' C2' H2'B 109.5 . . ? H2'A C2' H2'B 109.5 . . ? C1' C2' H2'C 109.5 . . ? H2'A C2' H2'C 109.5 . . ? H2'B C2' H2'C 109.5 . . ? C4 C3 O2 108.9(12) . . ? C4 C3 H3A 109.9 . . ? O2 C3 H3A 109.9 . . ? C4 C3 H3B 109.9 . . ? O2 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O3 C5 C6 109.9(12) . . ? O3 C5 H5A 109.7 . . ? C6 C5 H5A 109.7 . . ? O3 C5 H5B 109.7 . . ? C6 C5 H5B 109.7 . . ? H5A C5 H5B 108.2 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 O4 113(2) . . ? C8 C7 H7A 109.1 . . ? O4 C7 H7A 109.1 . . ? C8 C7 H7B 109.1 . . ? O4 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O4' C7' C8' 98(3) . . ? O4' C7' H7'A 112.1 . . ? C8' C7' H7'A 112.1 . . ? O4' C7' H7'B 112.1 . . ? C8' C7' H7'B 112.1 . . ? H7'A C7' H7'B 109.8 . . ? C7' C8' H8'A 109.5 . . ? C7' C8' H8'B 109.5 . . ? H8'A C8' H8'B 109.5 . . ? C7' C8' H8'C 109.5 . . ? H8'A C8' H8'C 109.5 . . ? H8'B C8' H8'C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.705 _refine_diff_density_min -1.497 _refine_diff_density_rms 0.160