#------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_global _publ_requested_journal 'Organometallics (2013)' #------------------ AUTHOR DETAILS -------------------------------------------# # Name and address of author for correspondence _publ_contact_author_name 'Gomez-Sal,P' _publ_contact_author_address ; Department of Chemistry University of Alcala Alcala de Henares. Spain ; _publ_contact_author_email pilar.gomez@uah.es _publ_contact_author_fax '00(000)0000000' _publ_contact_author_phone '00(000)0000000' # Insert blank lines between references _publ_section_references ; Blessing, R. H. (1995) Acta Cryst., A51, 33-38. Blessing, R. H. (1987) Cryst. Rev. 1, 3-58. Blessing, R. H. (1989) J. Appl. Cryst. 22, 396-397. C Flack H. D. & Bernardinelli, G. (71999). Acta Cryst. A55, 908-915. Flack H. D. & Bernardinelli, G. (2000). J. Appl. Cryst. 33, 1143-1148. Lehman, M. S. and Larsen, F. K. (1974) Acta. Cryst. A30, 580 LePage, Y. (1987). J. Appl. Cryst. 20, 264-269. North, A. C. T., Phillips, D. C. & Mathews, F. S. (1968) Acta Cryst, A24, 351-359 Streltsov, V. A. & Zavodnik, V. E. (1989) Sov. Phys. Crystallogr. 34, 824-828 Streltsov, V. A. & Zavodnik, V. E. (1990) Sov. Phys. Crystallogr. 35, 281. ABSCOR: Higashi, T. (1995). ABSCOR. Rigaku Corporation, Tokyo, Japan. Cambridge Structural Database: Allen, F. R. (2002). Acta Cryst. B58, 380-388. CAMERON: Watkin, D. J., Prout, C. K. & Pearce, L. J. (1996). CAMERON. Chemical Crystallography Laboratory, Oxford, England. CrysAlis CCD, CrysAlis RED and associated programs: Oxford Diffraction (2006). Program name(s). Oxford Diffraction Ltd, Abingdon, England. CRYSTALS: Betteridge, P. W., Carruthers, J. R., Cooper, R. I., Prout, K. & Watkin, D. J. (2003). J. Appl. Cryst. 36, 1487. COLLECT: Nonius [or Hooft, R. W. W.] (1998). COLLECT. Nonius BV, Delft, The Netherlands. DENZO/SCALEPACK: Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, Macromolecular Crystallography, Part A, edited by C. W. Carter Jr & R. M. Sweet, pp. 307-326. New York: Academic Press. DIAMOND: Brandenburg, K. [or Brandenburg, K. & Putz, H., or Brandenburg, K. & Berndt, M.] (1999). DIAMOND. Crystal Impact GbR, Bonn, Germany. DIF4 and REDU4: Stoe & Cie (1991). Program name(s). Stoe & Cie, Darmstadt, Germany. DIFABS: Walker, N. & Stuart, D. (1983). Acta Cryst., A39, 158 - 166. DIRAX: Duisenberg, A. J. M. (1992). J. Appl. Cryst. 25, 92-96. DIRDIF99: Beurskens, P.T., Beurskens, G., de Gelder, R., Garci\'ia-Granda, S., Gould, R.O., Israel, R. & Smits, J.M.M. (1999) The DIRDIF-99 program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. enCIFer: Allen, F. H., Johnson, O., Shields, G. P., Smith, B. R. & Towler, M. (2004). J. Appl. Cryst. 37, 335-338. EVALCCD: Duisenberg, A. J. M., Kroon-Batenburg, L. M. J. & Schreurs, A. M. M. (2003). J. Appl. Cryst. 36, 220-229. JANA2000: Petricek, V. & Dusek, M. (2000). JANA2000. Institute of Physics, Czech Academy of Sciences, Prague, Czech Republic. Mercury: Macrae, C. F., Edgington, P. R., McCabe, P., Pidcock, E., Shields, G. P., Taylor, R., Towler, M. & van de Streek, J. (2006). J. Appl. Cryst. 39, 453-457. Mogul: Bruno, I. J., Cole, J. C., Kessler, M., Luo, J., Motherwell, W. D. S., Purkis, L. H., Smith, B. R., Taylor, R., Cooper, R. I., Harris, S. E. & Orpen, A. G. (2004). J. Chem. Inf. Comput. Sci. 44, 2133-2144. ORTEPII: Johnson, C. K. (1976). ORTEPII. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. ORTEPIII: Burnett, M. N. & Johnson, C. K. (1996). ORTEPIII. Report ORNL-6895. Oak Ridge National Laboratory, Tennessee, USA. ORTEP-3: Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. PARST: Nardelli, M. (1995). J. Appl. Cryst. 28, 659. PLATON: Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. PROCESS: Rigaku (1996). PROCESS. Rigaku Corporation, Tokyo, Japan. PROCESS-AUTO: Rigaku (1998). PROCESS-AUTO. Rigaku Corporation, Tokyo, Japan. publCIF: Westrip, S. P. (2008). publCIF. In preparation. SADABS, TWINABS: Bruker (2001). Program name. Bruker AXS Inc., Madison, Wisconsin, USA. or Sheldrick, G. M. (1996). Program name. University of Gottingen, Germany. SHELX Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122. SIR92: Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. SIR97: Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115-119. SIR2002: Burla, M. C., Camalli, M., Carrozzini, B., Cascarano, G. L., Giacovazzo, C., Polidori, G. & Spagna, R. (2003). J. Appl. Cryst. 36, 1103. SUPERFLIP Palatinus, L. & Chapuis, G. (2007) J. Appl. Cryst. 40, 786-790. TEXSAN: Molecular Structure Corporation & Rigaku (2000). TEXSAN. MSC, The Woodlands, Texas, USA, and Rigaku Corporation, Tokyo, Japan. WinGX: Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838. X-AREA, X-RED, X-RED32, X-SHAPE: Stoe & Cie (2002). Program name(s). Stoe & Cie GmbH, Darmstadt, Germany. XCAD4: Harms, K. & Wocadlo, S. (1995). XCAD4. University of Marburg, Germany. XSCANS: Siemens (1994). XSCANS. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. ; #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# #----------------------------------------------------------------------------# #----------------------------------------------------------------------------# # COMPOUND 1 OF 5 # #----------------------------------------------------------------------------# #----------------------------------------------------------------------------# data_2e.6MeOH #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_date 2013-03-21T11:05:10-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'Na[Ag(NHC)2].6MeOH' _chemical_formula_moiety 'C60 H92 Ag1 N4 Na3 O18 S4' _chemical_formula_sum 'C60 H92 Ag N4 Na3 O18 S4' _chemical_formula_weight 1462.46 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _space_group_crystal_system triclinic _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _space_group_IT_number 2 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0810(11) _cell_length_b 17.746(2) _cell_length_c 19.4760(12) _cell_angle_alpha 83.536(5) _cell_angle_beta 73.590(7) _cell_angle_gamma 72.324(10) _cell_volume 3498.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 234 _cell_measurement_theta_min 3.54 _cell_measurement_theta_max 16.35 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour white _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.64 _exptl_crystal_size_min 0.24 _exptl_crystal_density_diffrn 1.388 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 2 8 -9 0.22 2 1 3 0.26 -3 -4 0 0.216 3 -1 13 0.254 -1 -1 -7 0.15 1 10 17 0.225 1 -6 -2 0.446 -2 6 -5 0.333 4 0 1 0.37 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.494 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.727 _exptl_absorpt_correction_T_max 0.906 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_ub_11 0.01 _diffrn_orient_matrix_ub_12 0 _diffrn_orient_matrix_ub_13 0 _diffrn_orient_matrix_ub_21 0 _diffrn_orient_matrix_ub_22 0.01 _diffrn_orient_matrix_ub_23 0 _diffrn_orient_matrix_ub_31 0 _diffrn_orient_matrix_ub_32 0 _diffrn_orient_matrix_ub_33 0.01 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0665 _diffrn_reflns_av_unetI/netI 0.1292 _diffrn_reflns_number 30781 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 16021 _reflns_number_gt 9107 _reflns_threshold_expression >2\s(I) _diffrn_reflns_reduction_process ; Scaled and merged with Sortav R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SIR2002 (Giacovazzo et al, 2003)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0794P)^2^+11.7405P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 16021 _refine_ls_number_parameters 821 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1425 _refine_ls_R_factor_gt 0.074 _refine_ls_wR_factor_ref 0.208 _refine_ls_wR_factor_gt 0.1858 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.51 _refine_diff_density_min -0.932 _refine_diff_density_rms 0.119 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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' 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 0.91744(4) 0.25032(2) 0.25191(2) 0.02443(13) Uani 1 1 d . . . N1 N 0.9841(5) 0.2173(3) 0.0874(2) 0.0240(10) Uani 1 1 d . . . N2 N 0.9928(5) 0.3326(3) 0.1015(2) 0.0251(10) Uani 1 1 d . . . N3 N 0.9269(5) 0.1681(3) 0.4016(2) 0.0249(10) Uani 1 1 d . . . N4 N 0.7878(5) 0.2826(3) 0.4162(2) 0.0233(10) Uani 1 1 d . . . S1 S 0.97115(14) -0.11823(8) 0.13001(7) 0.0250(3) Uani 1 1 d . . . S2 S 0.91049(17) 0.65548(9) 0.19680(9) 0.0366(4) Uani 1 1 d . . . S3 S 1.25536(16) -0.15128(9) 0.29640(9) 0.0349(4) Uani 1 1 d . A . S4 S 0.48480(15) 0.61663(8) 0.37121(8) 0.0282(3) Uani 1 1 d . . . O11 O 1.0979(4) -0.1641(2) 0.0890(2) 0.0381(10) Uani 1 1 d . . . O12 O 0.9496(4) -0.1378(2) 0.2074(2) 0.0324(10) Uani 1 1 d . . . O13 O 0.8625(4) -0.1210(2) 0.1032(2) 0.0309(9) Uani 1 1 d . . . O21 O 0.8001(10) 0.6743(5) 0.2591(5) 0.044(3) Uiso 0.539(14) 1 d P . 1 O22 O 0.8671(11) 0.6997(6) 0.1328(6) 0.053(3) Uiso 0.539(14) 1 d P . 1 O23 O 1.0261(9) 0.6606(6) 0.2095(7) 0.046(3) Uiso 0.539(14) 1 d P . 1 O21A O 0.877(2) 0.6537(12) 0.2764(11) 0.119(7) Uiso 0.461(14) 1 d P . 2 O22A O 0.8062(14) 0.7040(7) 0.1746(8) 0.064(4) Uiso 0.461(14) 1 d P . 2 O23A O 1.0361(10) 0.6697(6) 0.1748(7) 0.034(3) Uiso 0.461(14) 1 d P . 2 O31 O 1.1818(6) -0.2002(3) 0.3423(5) 0.103(3) Uani 1 1 d . A . O32 O 1.3821(4) -0.1636(3) 0.3052(3) 0.0466(12) Uani 1 1 d . . . O33 O 1.2533(7) -0.1551(4) 0.2232(4) 0.086(2) Uani 1 1 d . A . O41 O 0.5229(5) 0.6316(3) 0.2945(2) 0.0521(13) Uani 1 1 d . . . O42 O 0.5239(4) 0.6646(2) 0.4116(2) 0.0400(11) Uani 1 1 d . . . O43 O 0.3471(4) 0.6195(2) 0.3972(2) 0.0358(10) Uani 1 1 d . . . Na1 Na 1.5759(3) -0.25407(17) 0.24324(17) 0.0552(8) Uani 1 1 d . . . Na2 Na 1.1458(4) -0.25809(18) 0.2189(2) 0.0705(10) Uani 1 1 d . . . Na3 Na 0.8049(3) 0.80053(17) 0.29352(15) 0.0490(7) Uani 1 1 d . . . C1 C 0.9674(5) 0.2676(3) 0.1393(3) 0.0229(12) Uani 1 1 d . . . C2 C 1.0176(6) 0.2509(3) 0.0194(3) 0.0275(13) Uani 1 1 d . . . H2 H 1.0327 0.2281 -0.024 0.033 Uiso 1 1 calc R . . C3 C 1.0236(6) 0.3223(3) 0.0293(3) 0.0304(13) Uani 1 1 d . . . H3 H 1.045 0.359 -0.0066 0.036 Uiso 1 1 calc R . . C4 C 0.8732(5) 0.2325(3) 0.3640(3) 0.0215(11) Uani 1 1 d . . . C5 C 0.8752(6) 0.1780(3) 0.4751(3) 0.0299(13) Uani 1 1 d . . . H5 H 0.8969 0.1414 0.5109 0.036 Uiso 1 1 calc R . . C6 C 0.7889(6) 0.2497(3) 0.4847(3) 0.0270(13) Uani 1 1 d . . . H6 H 0.7397 0.273 0.5281 0.032 Uiso 1 1 calc R . . C11 C 0.9784(6) 0.1363(3) 0.0995(3) 0.0231(12) Uani 1 1 d . A . C12 C 1.0918(6) 0.0785(3) 0.1082(3) 0.0264(12) Uani 1 1 d . . . C13 C 1.0853(6) 0.0001(3) 0.1196(3) 0.0291(13) Uani 1 1 d . A . H13 H 1.1565 -0.0398 0.1286 0.035 Uiso 1 1 calc R . . C14 C 0.9740(6) -0.0178(3) 0.1177(3) 0.0250(12) Uani 1 1 d . . . C15 C 0.8661(6) 0.0394(3) 0.1057(3) 0.0245(12) Uani 1 1 d . A . H15 H 0.7936 0.025 0.103 0.029 Uiso 1 1 calc R . . C16 C 0.8635(6) 0.1194(3) 0.0976(3) 0.0235(12) Uani 1 1 d . . . C17 C 1.2192(6) 0.0972(3) 0.1021(3) 0.0323(14) Uani 1 1 d . . . H17 H 1.2035 0.1545 0.0936 0.039 Uiso 1 1 calc R . . C17A C 1.2600(8) 0.0764(5) 0.1714(4) 0.057(2) Uani 1 1 d . . . H17A H 1.1908 0.104 0.2099 0.085 Uiso 1 1 calc R . . H17B H 1.338 0.0915 0.1672 0.085 Uiso 1 1 calc R . . H17C H 1.2772 0.0204 0.1809 0.085 Uiso 1 1 calc R . . C17B C 1.3240(7) 0.0568(5) 0.0378(4) 0.057(2) Uani 1 1 d . . . H17D H 1.4042 0.069 0.0341 0.086 Uiso 1 1 calc R . . H17E H 1.2956 0.0751 -0.0049 0.086 Uiso 1 1 calc R . . H17F H 1.3383 0.0005 0.0435 0.086 Uiso 1 1 calc R . . C18 C 0.7435(6) 0.1839(3) 0.0862(3) 0.0268(12) Uani 1 1 d . A . H18 H 0.7746 0.2242 0.0535 0.032 Uiso 1 1 calc R . . C18A C 0.6577(7) 0.1540(4) 0.0524(4) 0.0386(15) Uani 1 1 d . . . H18A H 0.5839 0.1971 0.0465 0.058 Uiso 1 1 calc R A . H18B H 0.6271 0.1136 0.083 0.058 Uiso 1 1 calc R . . H18C H 0.7085 0.1326 0.0065 0.058 Uiso 1 1 calc R . . C18B C 0.6604(7) 0.2239(4) 0.1573(4) 0.0448(17) Uani 1 1 d . . . H18D H 0.5855 0.2647 0.1491 0.067 Uiso 1 1 calc R A . H18E H 0.7124 0.2468 0.1759 0.067 Uiso 1 1 calc R . . H18F H 0.6314 0.1853 0.1912 0.067 Uiso 1 1 calc R . . C21 C 0.9747(6) 0.4074(3) 0.1311(3) 0.0242(12) Uani 1 1 d . . . C22 C 0.8457(6) 0.4581(3) 0.1507(3) 0.0263(12) Uani 1 1 d . . . C23 C 0.8294(6) 0.5328(3) 0.1744(3) 0.0295(13) Uani 1 1 d . . . H23 H 0.7454 0.5672 0.1894 0.035 Uiso 1 1 calc R . . C24 C 0.9361(6) 0.5562(3) 0.1759(3) 0.0242(12) Uani 1 1 d . . . C25 C 1.0607(6) 0.5050(3) 0.1568(3) 0.0261(12) Uani 1 1 d . . . H25 H 1.1313 0.5217 0.1589 0.031 Uiso 1 1 calc R . . C26 C 1.0839(6) 0.4293(3) 0.1347(3) 0.0271(13) Uani 1 1 d . . . C27 C 0.7286(6) 0.4370(3) 0.1414(3) 0.0312(13) Uani 1 1 d . . . H27 H 0.7591 0.3821 0.1261 0.037 Uiso 1 1 calc R . . C27A C 0.6238(7) 0.4414(5) 0.2114(4) 0.058(2) Uani 1 1 d . . . H27A H 0.5512 0.4276 0.2039 0.088 Uiso 1 1 calc R . . H27B H 0.5943 0.4943 0.2286 0.088 Uiso 1 1 calc R . . H27C H 0.6595 0.4052 0.246 0.088 Uiso 1 1 calc R . . C27B C 0.6761(9) 0.4886(5) 0.0828(5) 0.067(2) Uani 1 1 d . . . H27D H 0.6025 0.4743 0.0773 0.1 Uiso 1 1 calc R . . H27E H 0.7437 0.4811 0.0386 0.1 Uiso 1 1 calc R . . H27F H 0.6488 0.5431 0.0955 0.1 Uiso 1 1 calc R . . C28 C 1.2222(6) 0.3714(3) 0.1141(3) 0.0331(14) Uani 1 1 d . . . H28 H 1.2295 0.345 0.0709 0.04 Uiso 1 1 calc R . . C28A C 1.2462(7) 0.3075(4) 0.1712(5) 0.055(2) Uani 1 1 d . . . H28A H 1.3334 0.2727 0.1559 0.083 Uiso 1 1 calc R . . H28B H 1.1837 0.2779 0.179 0.083 Uiso 1 1 calc R . . H28C H 1.2366 0.3314 0.215 0.083 Uiso 1 1 calc R . . C28B C 1.3320(7) 0.4114(4) 0.0962(4) 0.0447(17) Uani 1 1 d . . . H28D H 1.4154 0.372 0.0837 0.067 Uiso 1 1 calc R . . H28E H 1.3264 0.4391 0.1372 0.067 Uiso 1 1 calc R . . H28F H 1.3231 0.4482 0.0566 0.067 Uiso 1 1 calc R . . C31 C 1.0118(6) 0.0943(3) 0.3711(3) 0.0231(12) Uani 1 1 d . A . C32 C 1.1449(6) 0.0719(3) 0.3694(3) 0.0257(12) Uani 1 1 d . . . C33 C 1.2197(6) -0.0041(3) 0.3458(3) 0.0262(12) Uani 1 1 d . A . H33 H 1.3078 -0.0219 0.3456 0.031 Uiso 1 1 calc R . . C34 C 1.1631(6) -0.0531(3) 0.3227(3) 0.0252(12) Uani 1 1 d . . . C35 C 1.0309(6) -0.0292(3) 0.3241(3) 0.0274(13) Uani 1 1 d . A . H35 H 0.9958 -0.0627 0.3074 0.033 Uiso 1 1 calc R . . C36 C 0.9508(6) 0.0437(3) 0.3501(3) 0.0263(12) Uani 1 1 d . . . C37 C 1.2052(6) 0.1285(3) 0.3905(3) 0.0328(14) Uani 1 1 d . . . H37 H 1.146 0.1526 0.4352 0.039 Uiso 1 1 calc R . . C37A C 1.3421(7) 0.0882(4) 0.4048(4) 0.0469(17) Uani 1 1 d . . . H37A H 1.3743 0.1274 0.4181 0.07 Uiso 1 1 calc R . . H37B H 1.4022 0.0631 0.3622 0.07 Uiso 1 1 calc R . . H37C H 1.3341 0.0492 0.4429 0.07 Uiso 1 1 calc R . . C37B C 1.2183(8) 0.1957(4) 0.3347(4) 0.0495(18) Uani 1 1 d . . . H37D H 1.2564 0.2303 0.3504 0.074 Uiso 1 1 calc R . . H37E H 1.1331 0.2249 0.329 0.074 Uiso 1 1 calc R . . H37F H 1.2736 0.1739 0.2897 0.074 Uiso 1 1 calc R . . C38 C 0.8047(6) 0.0655(4) 0.3602(3) 0.0315(13) Uani 1 1 d . A . H38 H 0.768 0.1212 0.3732 0.038 Uiso 1 1 calc R . . C38A C 0.7444(8) 0.0163(5) 0.4221(4) 0.060(2) Uani 1 1 d . . . H38A H 0.6512 0.0307 0.4285 0.09 Uiso 1 1 calc R A . H38B H 0.7625 0.026 0.4651 0.09 Uiso 1 1 calc R . . H38C H 0.7816 -0.0388 0.4115 0.09 Uiso 1 1 calc R . . C38B C 0.7708(7) 0.0570(5) 0.2917(4) 0.054(2) Uani 1 1 d . . . H38D H 0.6772 0.0714 0.3 0.082 Uiso 1 1 calc R A . H38E H 0.808 0.0032 0.277 0.082 Uiso 1 1 calc R . . H38F H 0.8059 0.0911 0.2548 0.082 Uiso 1 1 calc R . . C41 C 0.7136(6) 0.3630(3) 0.4039(3) 0.0241(12) Uani 1 1 d . . . C42 C 0.5803(6) 0.3794(3) 0.4061(3) 0.0238(12) Uani 1 1 d . . . C43 C 0.5134(6) 0.4581(3) 0.3970(3) 0.0253(12) Uani 1 1 d . . . H43 H 0.4248 0.4714 0.3985 0.03 Uiso 1 1 calc R . . C44 C 0.5744(6) 0.5169(3) 0.3858(3) 0.0235(12) Uani 1 1 d . . . C45 C 0.7042(6) 0.4996(3) 0.3839(3) 0.0270(13) Uani 1 1 d . . . H45 H 0.7452 0.5397 0.3743 0.032 Uiso 1 1 calc R . . C46 C 0.7756(6) 0.4220(3) 0.3962(3) 0.0245(12) Uani 1 1 d . . . C47 C 0.5151(6) 0.3138(3) 0.4158(3) 0.0314(13) Uani 1 1 d . . . H47 H 0.5532 0.2735 0.4484 0.038 Uiso 1 1 calc R . . C47A C 0.5431(7) 0.2745(4) 0.3446(4) 0.0464(18) Uani 1 1 d . . . H47A H 0.5014 0.233 0.3523 0.07 Uiso 1 1 calc R . . H47B H 0.6361 0.2527 0.3261 0.07 Uiso 1 1 calc R . . H47C H 0.5094 0.3132 0.311 0.07 Uiso 1 1 calc R . . C47B C 0.3655(6) 0.3420(4) 0.4490(4) 0.0383(15) Uani 1 1 d . . . H47D H 0.3297 0.2981 0.4541 0.057 Uiso 1 1 calc R . . H47E H 0.3256 0.3822 0.4185 0.057 Uiso 1 1 calc R . . H47F H 0.3481 0.3631 0.4952 0.057 Uiso 1 1 calc R . . C48 C 0.9171(6) 0.4045(3) 0.4018(3) 0.0310(13) Uani 1 1 d . . . H48 H 0.9504 0.3473 0.4099 0.037 Uiso 1 1 calc R . . C48A C 0.9204(8) 0.4449(5) 0.4647(5) 0.062(2) Uani 1 1 d . . . H48A H 0.8644 0.4289 0.5075 0.092 Uiso 1 1 calc R . . H48B H 0.8902 0.5012 0.4576 0.092 Uiso 1 1 calc R . . H48C H 1.0087 0.4304 0.4692 0.092 Uiso 1 1 calc R . . C48B C 1.0045(8) 0.4272(6) 0.3313(4) 0.063(2) Uani 1 1 d . . . H48D H 0.9998 0.3998 0.2928 0.094 Uiso 1 1 calc R . . H48E H 1.0936 0.4128 0.3345 0.094 Uiso 1 1 calc R . . H48F H 0.9748 0.4832 0.3224 0.094 Uiso 1 1 calc R . . O51 O 1.3077(6) -0.2853(3) 0.1055(3) 0.0673(16) Uani 1 1 d . A . H51 H 1.3619 -0.2529 0.0865 0.081 Uiso 1 1 calc R . . O52 O 0.9351(7) 0.7849(4) 0.3671(3) 0.0801(19) Uani 1 1 d . . . H52 H 0.9866 0.8189 0.3629 0.096 Uiso 1 1 calc R . . O53 O 0.6256(6) 0.7899(3) 0.3842(3) 0.0597(16) Uani 1 1 d . . . O54 O 1.6582(5) -0.1407(3) 0.2150(3) 0.0500(13) Uani 1 1 d . . . O55 O 1.5502(7) -0.2766(4) 0.1338(3) 0.0835(19) Uani 1 1 d . . . H55 H 1.5089 -0.3141 0.1309 0.1 Uiso 1 1 calc R . . O56 O 1.261(3) -0.3707(12) 0.2671(17) 0.124(8) Uani 0.82(5) 1 d P A 3 H56 H 1.3367 -0.3663 0.276 0.186 Uiso 0.82(5) 1 calc PR A 3 O56A O 1.221(4) -0.365(2) 0.2941(19) 0.027(12) Uiso 0.18(5) 1 d P A 4 H56D H 1.2391 -0.3526 0.3344 0.041 Uiso 0.18(5) 1 calc PR A 4 C51 C 1.3177(9) -0.3527(5) 0.0684(5) 0.064(2) Uani 1 1 d . . . H51A H 1.3855 -0.3569 0.0244 0.096 Uiso 1 1 calc R A . H51B H 1.2355 -0.3471 0.0582 0.096 Uiso 1 1 calc R . . H51C H 1.3388 -0.3996 0.0977 0.096 Uiso 1 1 calc R . . C52 C 0.9383(10) 0.7232(7) 0.4200(5) 0.086(3) Uani 1 1 d . . . H52A H 0.9979 0.7246 0.447 0.128 Uiso 1 1 calc R . . H52B H 0.9673 0.6732 0.3973 0.128 Uiso 1 1 calc R . . H52C H 0.852 0.7299 0.4515 0.128 Uiso 1 1 calc R . . C53 C 0.5311(9) 0.8508(5) 0.4257(5) 0.065(2) Uani 1 1 d . . . H53A H 0.4671 0.8297 0.4596 0.098 Uiso 1 1 calc R . . H53B H 0.4888 0.8899 0.3952 0.098 Uiso 1 1 calc R . . H53C H 0.5726 0.8747 0.4508 0.098 Uiso 1 1 calc R . . C54 C 1.5794(9) -0.0620(5) 0.2115(6) 0.076(3) Uani 1 1 d . . . H54A H 1.6341 -0.0271 0.199 0.113 Uiso 1 1 calc R . . H54B H 1.518 -0.0483 0.2573 0.113 Uiso 1 1 calc R . . H54C H 1.5326 -0.0571 0.1759 0.113 Uiso 1 1 calc R . . C55 C 1.5943(11) -0.2360(9) 0.0754(5) 0.110(5) Uani 1 1 d . . . H55A H 1.5755 -0.2523 0.0352 0.165 Uiso 1 1 calc R . . H55B H 1.6874 -0.2459 0.0667 0.165 Uiso 1 1 calc R . . H55C H 1.5518 -0.1805 0.0822 0.165 Uiso 1 1 calc R . . C56 C 1.2408(11) -0.4441(5) 0.2856(6) 0.078(3) Uani 1 1 d . . . H56A H 1.3016 -0.4743 0.312 0.118 Uiso 1 1 calc R A 3 H56B H 1.2538 -0.4712 0.243 0.118 Uiso 1 1 calc R A 3 H56C H 1.1527 -0.4377 0.3147 0.118 Uiso 1 1 calc R A 3 H54 H 1.721(10) -0.150(5) 0.181(5) 0.08(3) Uiso 1 1 d . . . H53 H 0.607(11) 0.756(6) 0.384(6) 0.084 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0300(3) 0.0204(2) 0.0210(2) -0.00284(15) -0.00381(17) -0.00638(17) N1 0.033(3) 0.016(2) 0.024(2) -0.0022(18) -0.006(2) -0.010(2) N2 0.031(3) 0.017(2) 0.027(2) -0.0038(18) -0.005(2) -0.008(2) N3 0.029(3) 0.020(2) 0.024(2) -0.0069(18) -0.003(2) -0.006(2) N4 0.028(3) 0.019(2) 0.020(2) -0.0038(18) -0.0028(19) -0.005(2) S1 0.0306(8) 0.0176(7) 0.0253(7) -0.0034(5) -0.0016(6) -0.0090(6) S2 0.0392(9) 0.0210(8) 0.0472(9) -0.0132(7) -0.0061(8) -0.0058(7) S3 0.0295(9) 0.0199(7) 0.0531(10) -0.0121(7) -0.0069(7) -0.0036(6) S4 0.0352(9) 0.0176(7) 0.0280(7) -0.0040(5) -0.0071(6) -0.0020(6) O11 0.036(3) 0.025(2) 0.047(3) -0.0087(19) 0.001(2) -0.0071(19) O12 0.053(3) 0.026(2) 0.025(2) 0.0015(16) -0.0130(19) -0.019(2) O13 0.038(2) 0.025(2) 0.032(2) -0.0070(17) -0.0073(19) -0.0119(18) O31 0.041(3) 0.019(3) 0.218(9) 0.007(4) 0.009(4) -0.004(2) O32 0.034(3) 0.032(2) 0.073(3) -0.013(2) -0.015(2) -0.003(2) O33 0.091(5) 0.062(4) 0.098(5) -0.056(4) -0.052(4) 0.032(3) O41 0.069(4) 0.031(2) 0.035(3) 0.003(2) -0.001(2) 0.001(2) O42 0.047(3) 0.019(2) 0.056(3) -0.0100(19) -0.019(2) -0.0057(19) O43 0.034(2) 0.025(2) 0.044(2) -0.0056(18) -0.009(2) -0.0005(18) Na1 0.0399(16) 0.0408(15) 0.073(2) -0.0041(14) -0.0023(14) -0.0056(13) Na2 0.080(2) 0.0448(18) 0.105(3) -0.0128(17) -0.048(2) -0.0186(17) Na3 0.0518(18) 0.0484(16) 0.0478(16) -0.0057(13) -0.0090(13) -0.0180(14) C1 0.026(3) 0.019(3) 0.023(3) -0.003(2) -0.004(2) -0.007(2) C2 0.038(4) 0.024(3) 0.020(3) -0.003(2) -0.003(2) -0.012(3) C3 0.043(4) 0.025(3) 0.019(3) -0.001(2) -0.003(3) -0.010(3) C4 0.023(3) 0.016(3) 0.024(3) -0.005(2) -0.005(2) -0.002(2) C5 0.040(4) 0.023(3) 0.021(3) -0.003(2) -0.006(3) -0.003(3) C6 0.035(3) 0.026(3) 0.016(3) -0.003(2) -0.002(2) -0.007(3) C11 0.030(3) 0.016(3) 0.021(3) -0.004(2) -0.002(2) -0.006(2) C12 0.032(3) 0.023(3) 0.025(3) 0.000(2) -0.006(2) -0.011(3) C13 0.033(3) 0.018(3) 0.035(3) -0.003(2) -0.010(3) -0.003(2) C14 0.035(3) 0.017(3) 0.021(3) -0.003(2) -0.002(2) -0.007(2) C15 0.025(3) 0.025(3) 0.024(3) -0.003(2) -0.002(2) -0.011(2) C16 0.029(3) 0.022(3) 0.020(3) -0.005(2) -0.005(2) -0.007(2) C17 0.034(4) 0.021(3) 0.043(4) -0.001(3) -0.010(3) -0.010(3) C17A 0.064(5) 0.073(6) 0.054(5) 0.011(4) -0.031(4) -0.039(5) C17B 0.041(4) 0.065(5) 0.062(5) -0.020(4) 0.009(4) -0.025(4) C18 0.028(3) 0.021(3) 0.031(3) 0.001(2) -0.008(2) -0.006(2) C18A 0.036(4) 0.041(4) 0.040(4) 0.002(3) -0.015(3) -0.010(3) C18B 0.036(4) 0.038(4) 0.054(4) -0.016(3) -0.010(3) 0.002(3) C21 0.039(3) 0.017(3) 0.017(3) -0.003(2) -0.004(2) -0.010(2) C22 0.037(3) 0.022(3) 0.020(3) 0.001(2) -0.005(2) -0.011(3) C23 0.030(3) 0.027(3) 0.029(3) -0.008(2) -0.005(3) -0.006(3) C24 0.031(3) 0.018(3) 0.020(3) -0.004(2) 0.000(2) -0.006(2) C25 0.028(3) 0.026(3) 0.023(3) -0.008(2) -0.002(2) -0.007(2) C26 0.040(4) 0.021(3) 0.021(3) -0.004(2) -0.008(3) -0.008(3) C27 0.032(3) 0.025(3) 0.035(3) -0.009(2) -0.005(3) -0.007(3) C27A 0.041(4) 0.080(6) 0.060(5) -0.021(4) 0.007(4) -0.037(4) C27B 0.075(6) 0.080(6) 0.069(6) 0.016(5) -0.042(5) -0.041(5) C28 0.030(3) 0.023(3) 0.042(4) -0.008(3) -0.007(3) -0.001(3) C28A 0.036(4) 0.042(4) 0.081(6) 0.017(4) -0.011(4) -0.011(3) C28B 0.036(4) 0.041(4) 0.049(4) 0.002(3) -0.004(3) -0.008(3) C31 0.029(3) 0.016(3) 0.021(3) -0.004(2) -0.003(2) -0.003(2) C32 0.031(3) 0.022(3) 0.026(3) 0.000(2) -0.010(2) -0.008(2) C33 0.020(3) 0.022(3) 0.032(3) -0.002(2) -0.005(2) -0.001(2) C34 0.028(3) 0.020(3) 0.024(3) -0.002(2) -0.003(2) -0.005(2) C35 0.031(3) 0.021(3) 0.032(3) -0.004(2) -0.006(3) -0.012(2) C36 0.025(3) 0.022(3) 0.027(3) -0.005(2) 0.000(2) -0.006(2) C37 0.034(4) 0.025(3) 0.038(3) -0.007(3) -0.006(3) -0.008(3) C37A 0.052(5) 0.045(4) 0.050(4) 0.005(3) -0.025(4) -0.013(3) C37B 0.055(5) 0.031(4) 0.069(5) 0.007(3) -0.026(4) -0.015(3) C38 0.029(3) 0.027(3) 0.038(3) -0.007(3) -0.006(3) -0.006(3) C38A 0.043(5) 0.066(5) 0.064(5) 0.014(4) -0.007(4) -0.018(4) C38B 0.033(4) 0.068(5) 0.057(5) -0.020(4) -0.015(4) 0.003(4) C41 0.028(3) 0.018(3) 0.023(3) -0.005(2) -0.006(2) -0.001(2) C42 0.030(3) 0.019(3) 0.022(3) -0.005(2) -0.005(2) -0.006(2) C43 0.024(3) 0.027(3) 0.023(3) -0.004(2) -0.004(2) -0.006(2) C44 0.029(3) 0.018(3) 0.019(3) -0.004(2) -0.005(2) 0.000(2) C45 0.036(4) 0.017(3) 0.028(3) -0.005(2) -0.005(3) -0.009(2) C46 0.029(3) 0.019(3) 0.024(3) -0.006(2) -0.005(2) -0.004(2) C47 0.032(3) 0.028(3) 0.032(3) -0.002(2) -0.005(3) -0.008(3) C47A 0.048(4) 0.047(4) 0.047(4) -0.016(3) -0.003(3) -0.022(3) C47B 0.034(4) 0.037(4) 0.043(4) -0.003(3) -0.005(3) -0.012(3) C48 0.031(3) 0.024(3) 0.039(3) 0.001(2) -0.012(3) -0.008(3) C48A 0.052(5) 0.064(5) 0.072(6) -0.024(4) -0.031(4) -0.001(4) C48B 0.035(4) 0.087(6) 0.060(5) 0.012(4) -0.008(4) -0.017(4) O51 0.064(4) 0.065(4) 0.077(4) -0.009(3) -0.012(3) -0.027(3) O52 0.095(5) 0.085(5) 0.075(4) 0.033(3) -0.039(4) -0.046(4) O53 0.044(3) 0.047(3) 0.078(4) -0.006(3) 0.006(3) -0.017(3) O54 0.033(3) 0.044(3) 0.058(3) 0.009(2) 0.003(3) -0.006(2) O55 0.095(5) 0.108(5) 0.060(4) 0.005(4) -0.020(4) -0.050(4) O56 0.179(18) 0.112(9) 0.161(17) 0.074(11) -0.139(15) -0.099(11) C51 0.071(6) 0.047(5) 0.064(5) -0.003(4) -0.017(5) -0.004(4) C52 0.082(7) 0.115(8) 0.075(6) 0.051(6) -0.034(5) -0.056(7) C53 0.068(6) 0.046(5) 0.084(6) -0.008(4) -0.019(5) -0.019(4) C54 0.052(5) 0.045(5) 0.102(7) -0.001(5) 0.013(5) -0.005(4) C55 0.088(8) 0.209(15) 0.056(6) 0.034(8) -0.028(6) -0.082(9) C56 0.110(8) 0.046(5) 0.102(8) -0.001(5) -0.059(7) -0.027(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C4 2.108(5) . ? Ag1 C1 2.115(5) . ? N1 C1 1.361(7) . ? N1 C2 1.387(7) . ? N1 C11 1.447(7) . ? N2 C1 1.357(7) . ? N2 C3 1.371(7) . ? N2 C21 1.442(7) . ? N3 C4 1.355(7) . ? N3 C5 1.392(7) . ? N3 C31 1.437(7) . ? N4 C4 1.366(7) . ? N4 C6 1.397(7) . ? N4 C41 1.446(7) . ? S1 O11 1.447(4) . ? S1 O13 1.456(4) . ? S1 O12 1.476(4) . ? S1 C14 1.779(5) . ? S1 Na2 3.304(4) . ? S2 O22A 1.363(13) . ? S2 O23 1.401(10) . ? S2 O23A 1.426(10) . ? S2 O21 1.443(9) . ? S2 O21A 1.49(2) . ? S2 O22 1.514(10) . ? S2 C24 1.772(5) . ? S2 Na3 3.092(3) . ? S3 O32 1.411(5) . ? S3 O31 1.436(6) . ? S3 O33 1.442(6) . ? S3 C34 1.780(5) . ? S3 Na2 3.228(3) . ? S3 Na1 3.380(3) . ? S4 O42 1.449(4) . ? S4 O41 1.450(5) . ? S4 O43 1.452(5) . ? S4 C44 1.783(5) . ? S4 Na1 3.346(3) 1_465 ? O11 Na2 2.956(6) . ? O12 Na3 2.390(5) 1_545 ? O12 Na2 2.585(5) . ? O21 Na3 2.429(9) . ? O21 Na1 2.513(11) 1_465 ? O23 Na2 2.289(10) 1_565 ? O21A Na3 2.51(2) . ? O22A Na1 2.449(15) 1_465 ? O23A Na2 2.377(10) 1_565 ? O31 Na2 2.887(10) . ? O32 Na1 2.350(5) . ? O33 Na2 2.485(8) . ? O41 Na1 2.323(6) 1_465 ? Na1 O55 2.320(7) . ? Na1 O41 2.323(6) 1_645 ? Na1 O54 2.401(6) . ? Na1 O22A 2.449(15) 1_645 ? Na1 O21 2.513(11) 1_645 ? Na1 S4 3.346(3) 1_645 ? Na1 Na3 3.384(4) 1_645 ? Na2 O56 2.283(16) . ? Na2 O23 2.289(10) 1_545 ? Na2 O56A 2.36(4) . ? Na2 O23A 2.377(10) 1_545 ? Na2 O51 2.410(7) . ? Na2 Na3 3.509(5) 1_545 ? Na3 O52 2.247(7) . ? Na3 O53 2.296(6) . ? Na3 O12 2.390(5) 1_565 ? Na3 O54 2.466(6) 1_465 ? Na3 Na1 3.384(4) 1_465 ? Na3 Na2 3.509(5) 1_565 ? C2 C3 1.328(8) . ? C5 C6 1.335(8) . ? C11 C12 1.400(8) . ? C11 C16 1.406(8) . ? C12 C13 1.404(8) . ? C12 C17 1.517(8) . ? C13 C14 1.375(8) . ? C14 C15 1.373(8) . ? C15 C16 1.402(7) . ? C16 C18 1.520(8) . ? C17 C17A 1.514(9) . ? C17 C17B 1.519(9) . ? C18 C18A 1.537(8) . ? C18 C18B 1.540(8) . ? C21 C26 1.400(8) . ? C21 C22 1.409(8) . ? C22 C23 1.397(8) . ? C22 C27 1.517(8) . ? C23 C24 1.375(8) . ? C24 C25 1.377(8) . ? C25 C26 1.383(8) . ? C26 C28 1.535(8) . ? C27 C27A 1.512(9) . ? C27 C27B 1.514(10) . ? C28 C28A 1.515(9) . ? C28 C28B 1.527(9) . ? C31 C32 1.397(8) . ? C31 C36 1.427(8) . ? C32 C33 1.401(8) . ? C32 C37 1.511(8) . ? C33 C34 1.389(8) . ? C34 C35 1.388(8) . ? C35 C36 1.384(8) . ? C36 C38 1.506(8) . ? C37 C37B 1.532(9) . ? C37 C37A 1.557(9) . ? C38 C38B 1.519(9) . ? C38 C38A 1.524(9) . ? C41 C46 1.392(8) . ? C41 C42 1.405(8) . ? C42 C43 1.385(8) . ? C42 C47 1.516(8) . ? C43 C44 1.374(8) . ? C44 C45 1.367(8) . ? C45 C46 1.396(8) . ? C46 C48 1.536(8) . ? C47 C47A 1.532(9) . ? C47 C47B 1.542(9) . ? C48 C48A 1.502(9) . ? C48 C48B 1.532(10) . ? O51 C51 1.426(10) . ? O52 C52 1.416(10) . ? O53 C53 1.396(10) . ? O54 C54 1.410(9) . ? O54 Na3 2.466(6) 1_645 ? O55 C55 1.329(11) . ? O56 C56 1.378(14) . ? O56A C56 1.37(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 Ag1 C1 178.4(2) . . ? C1 N1 C2 111.7(4) . . ? C1 N1 C11 125.3(4) . . ? C2 N1 C11 122.8(4) . . ? C1 N2 C3 111.3(4) . . ? C1 N2 C21 125.9(4) . . ? C3 N2 C21 122.4(4) . . ? C4 N3 C5 111.4(4) . . ? C4 N3 C31 125.1(4) . . ? C5 N3 C31 122.9(5) . . ? C4 N4 C6 111.8(4) . . ? C4 N4 C41 125.2(4) . . ? C6 N4 C41 122.7(4) . . ? O11 S1 O13 113.5(2) . . ? O11 S1 O12 112.0(3) . . ? O13 S1 O12 112.4(2) . . ? O11 S1 C14 105.9(3) . . ? O13 S1 C14 105.2(3) . . ? O12 S1 C14 107.3(2) . . ? O11 S1 Na2 63.5(2) . . ? O13 S1 Na2 128.14(18) . . ? O12 S1 Na2 48.90(19) . . ? C14 S1 Na2 126.0(2) . . ? O22A S2 O23 138.2(7) . . ? O22A S2 O23A 121.4(7) . . ? O23 S2 O23A 27.1(4) . . ? O22A S2 O21 72.4(7) . . ? O23 S2 O21 112.2(6) . . ? O23A S2 O21 134.6(6) . . ? O22A S2 O21A 108.9(10) . . ? O23 S2 O21A 78.2(9) . . ? O23A S2 O21A 104.7(9) . . ? O21 S2 O21A 38.0(8) . . ? O22A S2 O22 35.7(6) . . ? O23 S2 O22 119.2(6) . . ? O23A S2 O22 93.9(6) . . ? O21 S2 O22 108.0(6) . . ? O21A S2 O22 143.0(9) . . ? O22A S2 C24 110.2(6) . . ? O23 S2 C24 107.7(4) . . ? O23A S2 C24 106.5(4) . . ? O21 S2 C24 107.4(4) . . ? O21A S2 C24 103.7(8) . . ? O22 S2 C24 101.2(4) . . ? O22A S2 Na3 74.4(6) . . ? O23 S2 Na3 78.6(4) . . ? O23A S2 Na3 89.7(4) . . ? O21 S2 Na3 50.0(4) . . ? O21A S2 Na3 53.6(8) . . ? O22 S2 Na3 95.6(4) . . ? C24 S2 Na3 155.6(2) . . ? O32 S3 O31 114.5(4) . . ? O32 S3 O33 113.8(4) . . ? O31 S3 O33 110.3(5) . . ? O32 S3 C34 107.2(3) . . ? O31 S3 C34 104.4(3) . . ? O33 S3 C34 105.7(3) . . ? O32 S3 Na2 130.1(2) . . ? O31 S3 Na2 63.4(4) . . ? O33 S3 Na2 47.2(3) . . ? C34 S3 Na2 121.9(2) . . ? O32 S3 Na1 34.2(2) . . ? O31 S3 Na1 110.1(2) . . ? O33 S3 Na1 86.0(3) . . ? C34 S3 Na1 136.9(2) . . ? Na2 S3 Na1 96.80(9) . . ? O42 S4 O41 113.3(3) . . ? O42 S4 O43 113.3(3) . . ? O41 S4 O43 112.1(3) . . ? O42 S4 C44 105.8(3) . . ? O41 S4 C44 105.7(3) . . ? O43 S4 C44 105.8(3) . . ? O42 S4 Na1 79.6(2) . 1_465 ? O41 S4 Na1 35.5(2) . 1_465 ? O43 S4 Na1 119.58(19) . 1_465 ? C44 S4 Na1 127.93(19) . 1_465 ? S1 O11 Na2 90.6(2) . . ? S1 O12 Na3 135.0(2) . 1_545 ? S1 O12 Na2 105.6(2) . . ? Na3 O12 Na2 89.62(17) 1_545 . ? S2 O21 Na3 103.0(5) . . ? S2 O21 Na1 119.4(5) . 1_465 ? Na3 O21 Na1 86.4(3) . 1_465 ? S2 O23 Na2 146.5(6) . 1_565 ? S2 O21A Na3 97.9(10) . . ? S2 O22A Na1 127.9(9) . 1_465 ? S2 O23A Na2 135.9(7) . 1_565 ? S3 O31 Na2 90.2(4) . . ? S3 O32 Na1 126.1(3) . . ? S3 O33 Na2 107.6(4) . . ? S4 O41 Na1 123.3(3) . 1_465 ? O55 Na1 O41 92.0(2) . 1_645 ? O55 Na1 O32 108.4(3) . . ? O41 Na1 O32 96.9(2) 1_645 . ? O55 Na1 O54 101.8(3) . . ? O41 Na1 O54 165.0(2) 1_645 . ? O32 Na1 O54 84.31(19) . . ? O55 Na1 O22A 80.0(4) . 1_645 ? O41 Na1 O22A 106.3(3) 1_645 1_645 ? O32 Na1 O22A 155.1(3) . 1_645 ? O54 Na1 O22A 70.9(3) . 1_645 ? O55 Na1 O21 113.0(3) . 1_645 ? O41 Na1 O21 84.5(3) 1_645 1_645 ? O32 Na1 O21 138.5(3) . 1_645 ? O54 Na1 O21 84.8(3) . 1_645 ? O22A Na1 O21 39.0(4) 1_645 1_645 ? O55 Na1 S4 112.3(2) . 1_645 ? O41 Na1 S4 21.25(12) 1_645 1_645 ? O32 Na1 S4 84.31(15) . 1_645 ? O54 Na1 S4 145.91(19) . 1_645 ? O22A Na1 S4 114.8(3) 1_645 1_645 ? O21 Na1 S4 82.7(2) 1_645 1_645 ? O55 Na1 S3 90.6(2) . . ? O41 Na1 S3 89.44(15) 1_645 . ? O32 Na1 S3 19.70(12) . . ? O54 Na1 S3 96.11(15) . . ? O22A Na1 S3 161.8(3) 1_645 . ? O21 Na1 S3 155.8(2) 1_645 . ? S4 Na1 S3 83.18(8) 1_645 . ? O55 Na1 Na3 134.2(2) . 1_645 ? O41 Na1 Na3 118.72(18) 1_645 1_645 ? O32 Na1 Na3 101.07(16) . 1_645 ? O54 Na1 Na3 46.75(15) . 1_645 ? O22A Na1 Na3 60.0(3) 1_645 1_645 ? O21 Na1 Na3 45.8(2) 1_645 1_645 ? S4 Na1 Na3 104.75(10) 1_645 1_645 ? S3 Na1 Na3 120.46(10) . 1_645 ? O56 Na2 O23 81.9(4) . 1_545 ? O56 Na2 O56A 14.3(12) . . ? O23 Na2 O56A 79.5(11) 1_545 . ? O56 Na2 O23A 91.4(4) . 1_545 ? O23 Na2 O23A 16.2(3) 1_545 1_545 ? O56A Na2 O23A 91.9(11) . 1_545 ? O56 Na2 O51 89.7(10) . . ? O23 Na2 O51 98.0(3) 1_545 . ? O56A Na2 O51 103.9(7) . . ? O23A Na2 O51 84.9(3) 1_545 . ? O56 Na2 O33 105.8(4) . . ? O23 Na2 O33 172.2(3) 1_545 . ? O56A Na2 O33 107.9(11) . . ? O23A Na2 O33 158.8(4) 1_545 . ? O51 Na2 O33 83.0(2) . . ? O56 Na2 O12 158.4(10) . . ? O23 Na2 O12 88.8(3) 1_545 . ? O56A Na2 O12 144.4(8) . . ? O23A Na2 O12 84.5(3) 1_545 . ? O51 Na2 O12 111.0(2) . . ? O33 Na2 O12 83.72(18) . . ? O56 Na2 O31 77.7(6) . . ? O23 Na2 O31 131.5(4) 1_545 . ? O56A Na2 O31 70.2(10) . . ? O23A Na2 O31 147.3(4) 1_545 . ? O51 Na2 O31 125.2(2) . . ? O33 Na2 O31 51.5(2) . . ? O12 Na2 O31 94.50(17) . . ? O56 Na2 O11 148.0(10) . . ? O23 Na2 O11 92.7(3) 1_545 . ? O56A Na2 O11 161.0(8) . . ? O23A Na2 O11 77.9(3) 1_545 . ? O51 Na2 O11 59.73(19) . . ? O33 Na2 O11 81.1(2) . . ? O12 Na2 O11 51.33(13) . . ? O31 Na2 O11 126.13(17) . . ? O56 Na2 S3 90.8(4) . . ? O23 Na2 S3 157.7(4) 1_545 . ? O56A Na2 S3 88.2(10) . . ? O23A Na2 S3 171.7(3) 1_545 . ? O51 Na2 S3 103.10(18) . . ? O33 Na2 S3 25.20(16) . . ? O12 Na2 S3 90.60(12) . . ? O31 Na2 S3 26.41(12) . . ? O11 Na2 S3 104.22(13) . . ? O56 Na2 S1 169.1(5) . . ? O23 Na2 S1 89.0(3) 1_545 . ? O56A Na2 S1 165.8(10) . . ? O23A Na2 S1 78.4(3) 1_545 . ? O51 Na2 S1 85.69(18) . . ? O33 Na2 S1 83.38(17) . . ? O12 Na2 S1 25.48(10) . . ? O31 Na2 S1 113.00(15) . . ? O11 Na2 S1 25.97(9) . . ? S3 Na2 S1 99.85(9) . . ? O56 Na2 Na3 116.2(9) . 1_545 ? O23 Na2 Na3 61.2(3) 1_545 1_545 ? O56A Na2 Na3 103.4(8) . 1_545 ? O23A Na2 Na3 67.4(3) 1_545 1_545 ? O51 Na2 Na3 141.4(2) . 1_545 ? O33 Na2 Na3 113.59(18) . 1_545 ? O12 Na2 Na3 42.93(12) . 1_545 ? O31 Na2 Na3 89.73(16) . 1_545 ? O11 Na2 Na3 87.56(13) . 1_545 ? S3 Na2 Na3 104.51(11) . 1_545 ? S1 Na2 Na3 63.49(8) . 1_545 ? O52 Na3 O53 94.1(3) . . ? O52 Na3 O12 88.5(2) . 1_565 ? O53 Na3 O12 158.7(2) . 1_565 ? O52 Na3 O21 111.8(3) . . ? O53 Na3 O21 83.6(3) . . ? O12 Na3 O21 115.0(3) 1_565 . ? O52 Na3 O54 162.9(2) . 1_465 ? O53 Na3 O54 89.1(2) . 1_465 ? O12 Na3 O54 82.60(18) 1_565 1_465 ? O21 Na3 O54 85.2(3) . 1_465 ? O52 Na3 O21A 90.5(6) . . ? O53 Na3 O21A 90.8(5) . . ? O12 Na3 O21A 110.4(5) 1_565 . ? O21 Na3 O21A 22.2(5) . . ? O54 Na3 O21A 106.3(6) 1_465 . ? O52 Na3 S2 108.3(2) . . ? O53 Na3 S2 110.70(17) . . ? O12 Na3 S2 88.44(13) 1_565 . ? O21 Na3 S2 27.1(2) . . ? O54 Na3 S2 86.12(15) 1_465 . ? O21A Na3 S2 28.4(5) . . ? O52 Na3 Na1 149.6(2) . 1_465 ? O53 Na3 Na1 64.56(19) . 1_465 ? O12 Na3 Na1 119.47(15) 1_565 1_465 ? O21 Na3 Na1 47.8(3) . 1_465 ? O54 Na3 Na1 45.16(14) 1_465 1_465 ? O21A Na3 Na1 69.7(6) . 1_465 ? S2 Na3 Na1 64.37(8) . 1_465 ? O52 Na3 Na2 62.0(2) . 1_565 ? O53 Na3 Na2 149.4(2) . 1_565 ? O12 Na3 Na2 47.45(13) 1_565 1_565 ? O21 Na3 Na2 88.0(2) . 1_565 ? O54 Na3 Na2 119.42(17) 1_465 1_565 ? O21A Na3 Na2 71.9(5) . 1_565 ? S2 Na3 Na2 64.55(8) . 1_565 ? Na1 Na3 Na2 127.30(11) 1_465 1_565 ? N2 C1 N1 103.2(4) . . ? N2 C1 Ag1 127.4(4) . . ? N1 C1 Ag1 129.4(4) . . ? C3 C2 N1 105.8(5) . . ? C2 C3 N2 108.0(5) . . ? N3 C4 N4 103.4(4) . . ? N3 C4 Ag1 127.5(4) . . ? N4 C4 Ag1 129.1(4) . . ? C6 C5 N3 107.5(5) . . ? C5 C6 N4 105.9(5) . . ? C12 C11 C16 123.7(5) . . ? C12 C11 N1 117.4(5) . . ? C16 C11 N1 118.7(5) . . ? C11 C12 C13 116.9(5) . . ? C11 C12 C17 122.6(5) . . ? C13 C12 C17 120.4(5) . . ? C14 C13 C12 120.2(5) . . ? C15 C14 C13 121.7(5) . . ? C15 C14 S1 119.3(4) . . ? C13 C14 S1 118.9(4) . . ? C14 C15 C16 120.9(5) . . ? C15 C16 C11 116.3(5) . . ? C15 C16 C18 121.8(5) . . ? C11 C16 C18 121.9(5) . . ? C17A C17 C12 111.0(5) . . ? C17A C17 C17B 113.1(6) . . ? C12 C17 C17B 109.8(5) . . ? C16 C18 C18A 113.2(5) . . ? C16 C18 C18B 110.6(5) . . ? C18A C18 C18B 109.9(5) . . ? C26 C21 C22 122.7(5) . . ? C26 C21 N2 119.9(5) . . ? C22 C21 N2 117.3(5) . . ? C23 C22 C21 117.2(5) . . ? C23 C22 C27 119.8(5) . . ? C21 C22 C27 122.8(5) . . ? C24 C23 C22 120.7(5) . . ? C23 C24 C25 120.4(5) . . ? C23 C24 S2 118.5(4) . . ? C25 C24 S2 120.9(4) . . ? C24 C25 C26 121.9(6) . . ? C25 C26 C21 116.9(5) . . ? C25 C26 C28 122.4(5) . . ? C21 C26 C28 120.7(5) . . ? C27A C27 C27B 112.1(7) . . ? C27A C27 C22 111.3(5) . . ? C27B C27 C22 110.5(5) . . ? C28A C28 C28B 108.7(6) . . ? C28A C28 C26 112.5(5) . . ? C28B C28 C26 113.8(5) . . ? C32 C31 C36 123.1(5) . . ? C32 C31 N3 119.9(5) . . ? C36 C31 N3 116.7(5) . . ? C31 C32 C33 117.2(5) . . ? C31 C32 C37 121.0(5) . . ? C33 C32 C37 121.8(5) . . ? C34 C33 C32 120.5(5) . . ? C35 C34 C33 121.3(5) . . ? C35 C34 S3 117.8(4) . . ? C33 C34 S3 120.8(4) . . ? C36 C35 C34 120.7(5) . . ? C35 C36 C31 117.1(5) . . ? C35 C36 C38 120.7(5) . . ? C31 C36 C38 122.1(5) . . ? C32 C37 C37B 112.3(5) . . ? C32 C37 C37A 113.9(5) . . ? C37B C37 C37A 108.3(6) . . ? C36 C38 C38B 111.7(5) . . ? C36 C38 C38A 109.8(5) . . ? C38B C38 C38A 111.8(6) . . ? C46 C41 C42 122.6(5) . . ? C46 C41 N4 117.8(5) . . ? C42 C41 N4 119.4(5) . . ? C43 C42 C41 116.5(5) . . ? C43 C42 C47 122.1(5) . . ? C41 C42 C47 121.3(5) . . ? C44 C43 C42 121.8(5) . . ? C45 C44 C43 120.7(5) . . ? C45 C44 S4 119.4(4) . . ? C43 C44 S4 119.8(4) . . ? C44 C45 C46 120.3(5) . . ? C41 C46 C45 117.8(5) . . ? C41 C46 C48 122.3(5) . . ? C45 C46 C48 119.9(5) . . ? C42 C47 C47A 111.1(5) . . ? C42 C47 C47B 113.2(5) . . ? C47A C47 C47B 109.4(5) . . ? C48A C48 C48B 112.4(6) . . ? C48A C48 C46 110.7(5) . . ? C48B C48 C46 110.3(5) . . ? C51 O51 Na2 117.9(5) . . ? C52 O52 Na3 119.6(6) . . ? C53 O53 Na3 127.0(5) . . ? C54 O54 Na1 124.5(5) . . ? C54 O54 Na3 128.7(6) . 1_645 ? Na1 O54 Na3 88.09(19) . 1_645 ? C55 O55 Na1 120.2(7) . . ? C56 O56 Na2 132.7(12) . . ? C56 O56A Na2 128(3) . . ? O56A C56 O56 24.4(18) . . ? #===END #----------------------------------------------------------------------------# #----------------------------------------------------------------------------# # COMPOUND 2 OF 5 # #----------------------------------------------------------------------------# #----------------------------------------------------------------------------# data_2eAg+ #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_date 2013-03-20T18:35:10-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'Ag[Ag(NHC)2].2H2O' _chemical_formula_moiety 'C54 H68 Ag2 N4 Na2 O12 S4' _chemical_formula_sum 'C54 H68 Ag2 N4 Na2 O15 S4' _chemical_formula_weight 1403.08 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 1 2/c 1' _space_group_name_Hall '-P 2yc' _space_group_IT_number 13 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 11.119(2) _cell_length_b 17.365(4) _cell_length_c 18.3179(19) _cell_angle_alpha 90 _cell_angle_beta 81.104(14) _cell_angle_gamma 90 _cell_volume 3494.4(11) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 275 _cell_measurement_theta_min 3.45 _cell_measurement_theta_max 16.32 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 7 -1 0.168 -12 11 19 0.18 1 -19 6 0.11 1 -1 -3 0.204 -1 -1 4 0.214 0 2 -1 0.236 10 -13 11 0.119 -4 5 -4 0.214 1 5 0 0.202 -1 -4 0 0.195 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.75 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.505 _exptl_absorpt_correction_T_max 0.746 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_ub_11 0.01 _diffrn_orient_matrix_ub_12 0 _diffrn_orient_matrix_ub_13 0 _diffrn_orient_matrix_ub_21 0 _diffrn_orient_matrix_ub_22 0.01 _diffrn_orient_matrix_ub_23 0 _diffrn_orient_matrix_ub_31 0 _diffrn_orient_matrix_ub_32 0 _diffrn_orient_matrix_ub_33 0.01 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.1053 _diffrn_reflns_av_unetI/netI 0.1 _diffrn_reflns_number 7973 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.58 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.984 _reflns_number_total 7973 _reflns_number_gt 4981 _reflns_threshold_expression >2\s(I) _diffrn_reflns_reduction_process ; Scaled and merged with Sortav R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7973 _refine_ls_number_parameters 380 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1421 _refine_ls_R_factor_gt 0.11 _refine_ls_wR_factor_ref 0.3227 _refine_ls_wR_factor_gt 0.2993 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.137 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 2.751 _refine_diff_density_min -4.978 _refine_diff_density_rms 0.244 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' N N 0.0061 0.0033 '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' O O 0.0106 0.006 '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' 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 0.24305(4) 0.25 0.0278(3) Uani 1 2 d S . . Ag2 Ag 0 0.74260(11) 0.25 0.1049(6) Uani 1 2 d S . . N1 N -0.0593(6) 0.1870(3) 0.4155(3) 0.0330(13) Uani 1 1 d . . . N2 N 0.0126(6) 0.3019(3) 0.4099(3) 0.0321(13) Uani 1 1 d . . . Na1 Na -0.4993(2) 0.79290(15) 0.34891(12) 0.0268(6) Uani 1 1 d . . . O1 O 0.3208(10) 0.6090(7) 0.2941(10) 0.121(6) Uani 0.849(16) 1 d P A 1 O2 O 0.1538(17) 0.6243(6) 0.2328(7) 0.126(6) Uani 0.849(16) 1 d P A 1 O3 O 0.1163(17) 0.6695(5) 0.3460(9) 0.152(10) Uani 0.849(16) 1 d P A 1 O1A O 0.238(3) 0.6513(15) 0.3800(15) 0.022(8) Uiso 0.151(16) 1 d P A 2 O2A O 0.271(3) 0.6207(16) 0.2566(15) 0.021(8) Uiso 0.151(16) 1 d P A 2 O3A O 0.086(5) 0.661(3) 0.297(3) 0.062(14) Uiso 0.151(16) 1 d P A 2 O4 O -0.1089(7) 0.8148(4) 0.3553(5) 0.073(2) Uani 1 1 d . A . O5 O -0.3219(7) 0.8546(4) 0.3697(5) 0.075(2) Uani 1 1 d . A . O6 O -0.1874(9) 0.8718(4) 0.2565(4) 0.081(3) Uani 1 1 d . A . O7 O -0.5 0.7062(7) 0.25 0.072(3) Uani 1 2 d S . . O8 O -0.7213(6) 0.8075(4) 0.3649(4) 0.0609(17) Uani 1 1 d . . . S1 S 0.1896(2) 0.61554(14) 0.30775(16) 0.0584(7) Uani 1 1 d . . . S2 S -0.19826(17) 0.86806(10) 0.33437(11) 0.0383(5) Uani 1 1 d . . . C1 C -0.0181(6) 0.2432(4) 0.3664(4) 0.0308(14) Uani 1 1 d . . . C2 C -0.0061(8) 0.2808(4) 0.4850(4) 0.0399(17) Uani 1 1 d . . . H2 H 0.0096 0.3111 0.5244 0.048 Uiso 1 1 calc R . . C3 C -0.0501(8) 0.2102(5) 0.4893(4) 0.0422(18) Uani 1 1 d . . . H3 H -0.071 0.1811 0.532 0.051 Uiso 1 1 calc R . . C4 C 0.0555(7) 0.3770(4) 0.3838(4) 0.0318(14) Uani 1 1 d . . . C5 C -0.0302(7) 0.4369(4) 0.3824(4) 0.0343(15) Uani 1 1 d . A . C6 C 0.0134(7) 0.5097(4) 0.3569(4) 0.0370(16) Uani 1 1 d . . . H6 H -0.0408 0.5498 0.3537 0.044 Uiso 1 1 calc R A . C7 C 0.1352(7) 0.5212(4) 0.3370(4) 0.0403(17) Uani 1 1 d . A . C8 C 0.2212(8) 0.4637(5) 0.3411(5) 0.0445(18) Uani 1 1 d . . . H8 H 0.3038 0.4747 0.3295 0.053 Uiso 1 1 calc R A . C9 C 0.1821(8) 0.3884(5) 0.3631(5) 0.0457(19) Uani 1 1 d . A . C10 C -0.1657(7) 0.4235(5) 0.4089(5) 0.0432(18) Uani 1 1 d . . . H10 H -0.1769 0.3719 0.4304 0.052 Uiso 1 1 calc R A . C11 C -0.2382(10) 0.4300(11) 0.3455(8) 0.098(5) Uani 1 1 d . A . H11A H -0.3228 0.4212 0.3636 0.147 Uiso 1 1 calc R . . H11B H -0.2097 0.3923 0.3085 0.147 Uiso 1 1 calc R . . H11C H -0.228 0.4806 0.3244 0.147 Uiso 1 1 calc R . . C12 C -0.2129(11) 0.4833(8) 0.4683(7) 0.084(4) Uani 1 1 d . A . H12A H -0.1684 0.4787 0.509 0.126 Uiso 1 1 calc R . . H12B H -0.2978 0.4745 0.4853 0.126 Uiso 1 1 calc R . . H12C H -0.2018 0.5341 0.4476 0.126 Uiso 1 1 calc R . . C13 C 0.2727(9) 0.3240(7) 0.3713(6) 0.071(3) Uani 1 1 d . . . H13 H 0.235 0.2815 0.4018 0.085 Uiso 1 1 calc R A . C14 C 0.3910(17) 0.3647(12) 0.4072(11) 0.135(8) Uani 1 1 d . A . H14A H 0.3619 0.3842 0.4558 0.203 Uiso 1 1 calc R . . H14B H 0.4248 0.4062 0.3759 0.203 Uiso 1 1 calc R . . H14C H 0.4526 0.3266 0.4101 0.203 Uiso 1 1 calc R . . C15 C 0.3393(17) 0.2980(10) 0.3039(8) 0.126(7) Uani 1 1 d . A . H15A H 0.3922 0.2567 0.3134 0.189 Uiso 1 1 calc R . . H15B H 0.3871 0.3397 0.2802 0.189 Uiso 1 1 calc R . . H15C H 0.284 0.28 0.2722 0.189 Uiso 1 1 calc R . . C16 C -0.0939(7) 1.1095(4) 0.3976(3) 0.0315(14) Uani 1 1 d . . . C17 C -0.0019(6) 1.0555(4) 0.3760(3) 0.0313(14) Uani 1 1 d . A . C18 C -0.0335(6) 0.9814(4) 0.3568(4) 0.0311(14) Uani 1 1 d . . . H18 H 0.0266 0.9453 0.341 0.037 Uiso 1 1 calc R A . C19 C -0.1564(7) 0.9618(4) 0.3616(4) 0.0326(14) Uani 1 1 d . A . C20 C -0.2470(7) 1.0148(4) 0.3880(4) 0.0348(15) Uani 1 1 d . . . H20 H -0.3282 0.9999 0.3934 0.042 Uiso 1 1 calc R A . C21 C -0.2182(6) 1.0896(4) 0.4062(4) 0.0330(15) Uani 1 1 d . A . C22 C 0.1341(7) 1.0758(4) 0.3755(4) 0.0353(15) Uani 1 1 d . . . H22 H 0.1372 1.1274 0.3967 0.042 Uiso 1 1 calc R A . C23 C 0.1922(9) 1.0196(6) 0.4256(6) 0.059(2) Uani 1 1 d . A . H23A H 0.1462 1.0204 0.4744 0.088 Uiso 1 1 calc R . . H23B H 0.2744 1.0352 0.4276 0.088 Uiso 1 1 calc R . . H23C H 0.192 0.9685 0.4057 0.088 Uiso 1 1 calc R . . C24 C 0.2017(8) 1.0789(6) 0.2973(5) 0.052(2) Uani 1 1 d . A . H24A H 0.1624 1.1149 0.2691 0.078 Uiso 1 1 calc R . . H24B H 0.2015 1.0287 0.2753 0.078 Uiso 1 1 calc R . . H24C H 0.2842 1.0949 0.298 0.078 Uiso 1 1 calc R . . C25 C -0.3187(8) 1.1489(5) 0.4343(5) 0.0453(18) Uani 1 1 d . . . H25 H -0.2834 1.1848 0.4664 0.054 Uiso 1 1 calc R A . C26 C -0.4279(10) 1.1126(7) 0.4809(6) 0.070(3) Uani 1 1 d . A . H26A H -0.4017 1.0832 0.5199 0.105 Uiso 1 1 calc R . . H26B H -0.4684 1.0793 0.4506 0.105 Uiso 1 1 calc R . . H26C H -0.4829 1.1523 0.5017 0.105 Uiso 1 1 calc R . . C27 C -0.3479(12) 1.1956(8) 0.3687(7) 0.085(4) Uani 1 1 d . A . H27A H -0.274 1.2163 0.3418 0.128 Uiso 1 1 calc R . . H27B H -0.4019 1.2371 0.3862 0.128 Uiso 1 1 calc R . . H27C H -0.3862 1.163 0.3368 0.128 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 Ag1 0.0313(4) 0.0323(4) 0.0198(4) 0 -0.0039(2) 0 Ag2 0.0985(13) 0.1182(14) 0.0966(12) 0 -0.0102(9) 0 N1 0.040(3) 0.032(3) 0.026(3) -0.001(2) -0.004(2) 0.000(2) N2 0.044(4) 0.031(3) 0.019(3) -0.001(2) -0.001(2) 0.003(2) Na1 0.0202(12) 0.0407(14) 0.0190(11) -0.0089(9) -0.0012(9) -0.0180(10) O1 0.055(6) 0.077(7) 0.222(17) 0.049(9) 0.004(8) -0.020(5) O2 0.230(17) 0.069(6) 0.093(8) 0.039(6) -0.075(9) -0.057(8) O3 0.212(18) 0.040(5) 0.153(14) -0.019(6) 0.129(14) -0.042(7) O4 0.074(5) 0.039(3) 0.113(6) -0.006(3) -0.034(4) 0.002(3) O5 0.049(4) 0.059(4) 0.110(6) -0.029(4) 0.012(4) -0.016(3) O6 0.131(7) 0.062(4) 0.050(4) -0.015(3) -0.011(4) -0.047(5) O7 0.041(5) 0.103(8) 0.068(6) 0 0.005(4) 0 O8 0.062(4) 0.069(4) 0.053(4) -0.004(3) -0.012(3) 0.000(3) S1 0.0421(12) 0.0465(12) 0.0860(17) 0.0263(11) -0.0080(11) -0.0133(10) S2 0.0344(10) 0.0333(9) 0.0476(11) -0.0046(7) -0.0074(8) -0.0044(7) C1 0.031(3) 0.032(3) 0.028(3) 0.003(2) -0.002(3) 0.003(3) C2 0.063(5) 0.036(4) 0.021(3) -0.003(3) -0.008(3) 0.000(3) C3 0.060(5) 0.044(4) 0.020(3) 0.001(3) 0.002(3) 0.001(4) C4 0.034(4) 0.034(3) 0.027(3) -0.003(2) -0.006(3) 0.003(3) C5 0.037(4) 0.037(3) 0.029(3) 0.003(3) -0.004(3) 0.003(3) C6 0.037(4) 0.032(3) 0.041(4) 0.006(3) -0.002(3) 0.000(3) C7 0.035(4) 0.042(4) 0.044(4) 0.007(3) -0.007(3) -0.005(3) C8 0.033(4) 0.050(4) 0.050(4) 0.014(3) -0.004(3) -0.001(3) C9 0.040(4) 0.048(4) 0.045(4) 0.014(3) 0.006(3) 0.010(3) C10 0.031(4) 0.046(4) 0.051(4) 0.012(3) 0.000(3) 0.000(3) C11 0.036(6) 0.168(15) 0.094(9) 0.006(9) -0.021(6) -0.032(7) C12 0.048(6) 0.119(10) 0.072(8) -0.018(6) 0.030(5) -0.006(6) C13 0.041(5) 0.077(7) 0.087(7) 0.042(6) 0.017(5) 0.028(5) C14 0.124(14) 0.151(16) 0.152(16) -0.071(13) -0.086(12) 0.083(12) C15 0.150(15) 0.146(14) 0.087(9) -0.041(9) -0.033(9) 0.121(13) C16 0.041(4) 0.032(3) 0.021(3) 0.002(2) -0.004(3) -0.002(3) C17 0.034(4) 0.035(3) 0.025(3) 0.000(2) -0.004(3) -0.004(3) C18 0.028(4) 0.035(3) 0.030(3) 0.000(2) -0.002(3) 0.004(3) C19 0.033(4) 0.035(3) 0.031(3) -0.001(3) -0.010(3) 0.001(3) C20 0.030(4) 0.037(4) 0.036(4) 0.003(3) -0.002(3) 0.001(3) C21 0.031(4) 0.041(4) 0.026(3) 0.007(3) -0.002(3) 0.001(3) C22 0.030(4) 0.035(3) 0.042(4) -0.006(3) -0.008(3) -0.003(3) C23 0.050(6) 0.074(6) 0.060(6) 0.013(4) -0.029(4) -0.004(5) C24 0.033(4) 0.077(6) 0.044(4) 0.007(4) -0.003(3) -0.004(4) C25 0.044(5) 0.042(4) 0.049(4) -0.003(3) -0.003(3) 0.007(3) C26 0.053(6) 0.074(7) 0.073(7) -0.002(5) 0.023(5) 0.011(5) C27 0.079(8) 0.095(9) 0.075(7) 0.026(6) 0.008(6) 0.051(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 2.111(7) . ? Ag1 C1 2.111(7) 2 ? Ag2 O3A 1.99(5) 2 ? Ag2 O3A 1.99(5) . ? Ag2 O4 2.457(8) . ? Ag2 O4 2.457(8) 2 ? N1 C1 1.358(9) . ? N1 C3 1.429(9) . ? N1 C16 1.452(9) 1_545 ? N2 C1 1.369(9) . ? N2 C2 1.408(9) . ? N2 C4 1.444(9) . ? Na1 O5 2.327(7) . ? Na1 O7 2.357(8) . ? Na1 O8 2.454(8) . ? Na1 Na1 3.626(4) 2_455 ? O1 S1 1.446(12) . ? O2 S1 1.495(12) . ? O3 S1 1.362(11) . ? O1A S1 1.63(3) . ? O2A S1 1.20(3) . ? O3A S1 1.43(5) . ? O4 S2 1.452(8) . ? O5 S2 1.445(7) . ? O6 S2 1.413(8) . ? O7 Na1 2.357(8) 2_455 ? S1 C7 1.800(8) . ? S2 C19 1.786(7) . ? C2 C3 1.319(12) . ? C4 C9 1.413(11) . ? C4 C5 1.415(10) . ? C5 C6 1.407(10) . ? C5 C10 1.527(11) . ? C6 C7 1.361(11) . ? C7 C8 1.392(12) . ? C8 C9 1.418(12) . ? C9 C13 1.528(12) . ? C10 C11 1.517(15) . ? C10 C12 1.536(14) . ? C13 C15 1.412(17) . ? C13 C14 1.71(2) . ? C16 C17 1.400(10) . ? C16 C21 1.409(10) . ? C16 N1 1.452(9) 1_565 ? C17 C18 1.392(10) . ? C17 C22 1.552(10) . ? C18 C19 1.397(10) . ? C19 C20 1.395(10) . ? C20 C21 1.390(10) . ? C21 C25 1.548(10) . ? C22 C24 1.512(11) . ? C22 C23 1.546(12) . ? C25 C26 1.510(13) . ? C25 C27 1.526(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ag1 C1 179.8(4) . 2 ? O3A Ag2 O3A 89(3) 2 . ? O3A Ag2 O4 119.7(16) 2 . ? O3A Ag2 O4 103.6(18) . . ? O3A Ag2 O4 103.6(18) 2 2 ? O3A Ag2 O4 119.7(16) . 2 ? O4 Ag2 O4 118.6(4) . 2 ? C1 N1 C3 111.0(6) . . ? C1 N1 C16 126.2(5) . 1_545 ? C3 N1 C16 122.3(6) . 1_545 ? C1 N2 C2 111.3(6) . . ? C1 N2 C4 125.4(5) . . ? C2 N2 C4 123.3(6) . . ? O5 Na1 O7 121.6(2) . . ? O5 Na1 O8 142.7(3) . . ? O7 Na1 O8 92.00(18) . . ? O5 Na1 Na1 107.4(2) . 2_455 ? O7 Na1 Na1 39.7(2) . 2_455 ? O8 Na1 Na1 87.68(18) . 2_455 ? S1 O3A Ag2 155(4) . . ? S2 O4 Ag2 113.1(5) . . ? S2 O5 Na1 140.6(5) . . ? Na1 O7 Na1 100.6(5) . 2_455 ? O2A S1 O3 132.0(14) . . ? O2A S1 O3A 112(3) . . ? O3 S1 O3A 42(2) . . ? O2A S1 O1 41.7(14) . . ? O3 S1 O1 130.6(11) . . ? O3A S1 O1 146(2) . . ? O2A S1 O2 63.3(17) . . ? O3 S1 O2 100.3(12) . . ? O3A S1 O2 59(2) . . ? O1 S1 O2 104.7(10) . . ? O2A S1 O1A 107.6(17) . . ? O3 S1 O1A 64.3(13) . . ? O3A S1 O1A 106(3) . . ? O1 S1 O1A 73.7(13) . . ? O2 S1 O1A 151.3(10) . . ? O2A S1 C7 118.5(14) . . ? O3 S1 C7 109.0(5) . . ? O3A S1 C7 107(2) . . ? O1 S1 C7 105.3(5) . . ? O2 S1 C7 104.0(5) . . ? O1A S1 C7 104.1(10) . . ? O6 S2 O5 112.7(6) . . ? O6 S2 O4 109.9(6) . . ? O5 S2 O4 114.9(5) . . ? O6 S2 C19 104.8(4) . . ? O5 S2 C19 107.1(4) . . ? O4 S2 C19 106.7(4) . . ? N1 C1 N2 103.8(6) . . ? N1 C1 Ag1 129.6(5) . . ? N2 C1 Ag1 126.5(5) . . ? C3 C2 N2 107.3(6) . . ? C2 C3 N1 106.6(6) . . ? C9 C4 C5 122.5(7) . . ? C9 C4 N2 118.7(6) . . ? C5 C4 N2 118.7(6) . . ? C6 C5 C4 117.9(7) . . ? C6 C5 C10 121.0(7) . . ? C4 C5 C10 121.1(6) . . ? C7 C6 C5 119.9(7) . . ? C6 C7 C8 123.0(7) . . ? C6 C7 S1 119.2(6) . . ? C8 C7 S1 117.8(6) . . ? C7 C8 C9 119.5(7) . . ? C4 C9 C8 117.1(7) . . ? C4 C9 C13 121.0(7) . . ? C8 C9 C13 121.7(8) . . ? C11 C10 C5 111.1(7) . . ? C11 C10 C12 109.1(10) . . ? C5 C10 C12 109.6(8) . . ? C15 C13 C9 114.4(9) . . ? C15 C13 C14 97.9(12) . . ? C9 C13 C14 107.1(10) . . ? C17 C16 C21 121.9(6) . . ? C17 C16 N1 118.5(6) . 1_565 ? C21 C16 N1 119.5(6) . 1_565 ? C18 C17 C16 119.2(7) . . ? C18 C17 C22 119.5(6) . . ? C16 C17 C22 121.2(6) . . ? C17 C18 C19 119.5(6) . . ? C20 C19 C18 120.5(6) . . ? C20 C19 S2 119.5(6) . . ? C18 C19 S2 119.9(5) . . ? C21 C20 C19 121.2(7) . . ? C20 C21 C16 117.4(7) . . ? C20 C21 C25 121.3(7) . . ? C16 C21 C25 121.3(7) . . ? C24 C22 C23 113.1(7) . . ? C24 C22 C17 110.8(6) . . ? C23 C22 C17 110.5(6) . . ? C26 C25 C27 114.6(9) . . ? C26 C25 C21 112.7(7) . . ? C27 C25 C21 108.8(7) . . ? 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 _platon_squeeze_void_content 1 0.500 0.338 0.750 237 49 ' ' 2 0.500 0.663 0.250 236 46 ' ' 3 0.500 0.006 0.750 74 16 ' ' 4 0.500 0.993 0.250 74 15 ' ' _platon_squeeze_details ; ; #===END #----------------------------------------------------------------------------# #----------------------------------------------------------------------------# # COMPOUND 3 OF 5 # #----------------------------------------------------------------------------# #----------------------------------------------------------------------------# data_2e.5dmso.H2O #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_method 'APEX2 v2010.9-1' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ? _chemical_name_common 'Na[Ag(NHC)2].5dmso.2H2O' _chemical_formula_moiety ? _chemical_formula_sum 'C64 H98 Ag N4 Na3 O17.50 S9' _chemical_formula_iupac ? _chemical_formula_weight 1668.84 _chemical_compound_source 'synthesis as described' _chemical_melting_point ? #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_operation_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 21.864(2) _cell_length_b 14.9797(19) _cell_length_c 24.108(2) _cell_angle_alpha 90 _cell_angle_beta 93.662(4) _cell_angle_gamma 90 _cell_volume 7879.6(15) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9940 _cell_measurement_theta_min 2.7613 _cell_measurement_theta_max 20.9133 _cell_measurement_temperature 100.(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prismatic _exptl_crystal_colour 'translucent colourless' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.050 _exptl_crystal_density_diffrn 1.407 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3496 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.576 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 0.97 _exptl_special_details ; ; _diffrn_ambient_temperature 100.(2) #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source ? _diffrn_source_type ? _diffrn_radiation_type ? _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 8.3333 _diffrn_reflns_number 34390 _diffrn_reflns_av_R_equivalents 0.0510 _diffrn_reflns_av_sigmaI/netI 0.0539 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 20.91 _diffrn_reflns_theta_full 20.91 _diffrn_measured_fraction_theta_max 0.961 _diffrn_measured_fraction_theta_full 0.961 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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. ; _reflns_number_total 8022 _reflns_number_gt 6369 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.1164 _refine_ls_R_factor_gt 0.0868 _refine_ls_wR_factor_gt 0.2540 _refine_ls_wR_factor_ref 0.3027 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _refine_ls_number_reflns 8022 _refine_ls_number_parameters 874 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment refxyz _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1885P)^2^+105.8561P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.952 _refine_diff_density_min -2.167 _refine_ls_extinction_method none _refine_ls_extinction_coef ? #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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' _computing_data_collection 'Bruker Instrument Service v2010.9.0.0' _computing_cell_refinement 'SAINT V7.68A (Bruker AXS, 2009)' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag1 0.58820(4) 0.76286(6) 0.83435(3) 0.0152(4) Uani d . 1.0 . . C C1 0.5623(5) 0.6649(8) 0.8901(4) 0.018(3) Uani d . 1.0 . . C C2 0.5093(6) 0.5579(9) 0.9333(5) 0.025(3) Uani d . 1.0 . . H H2 0.477 0.5183 0.9411 0.03 Uiso calc R 1.0 . . C C3 0.5638(5) 0.5658(9) 0.9625(5) 0.023(3) Uani d . 1.0 . . H H3 0.5773 0.5344 0.9953 0.028 Uiso calc R 1.0 . . C C4 0.6572(5) 0.6568(8) 0.9536(4) 0.0139(19) Uani d . 1.0 . . C C5 0.6645(5) 0.7315(8) 0.9873(5) 0.016(3) Uani d . 1.0 . . C C6 0.7239(6) 0.7556(8) 1.0048(5) 0.018(3) Uani d . 1.0 . . H H6 0.7313 0.8091 1.0254 0.022 Uiso calc R 1.0 . . C C7 0.7720(5) 0.7021(9) 0.9923(4) 0.019(2) Uani d . 1.0 . . C C8 0.7629(5) 0.6263(8) 0.9599(4) 0.017(3) Uani d . 1.0 . . H H8 0.7971 0.5903 0.952 0.02 Uiso calc R 1.0 . . C C9 0.7055(5) 0.6024(8) 0.9393(4) 0.015(2) Uani d . 1.0 . . C C10 0.6954(5) 0.5170(8) 0.9044(5) 0.021(3) Uani d . 1.0 . . H H10 0.6529 0.5201 0.8865 0.025 Uiso calc R 1.0 . . C C11 0.6983(7) 0.4342(10) 0.9422(6) 0.040(4) Uani d . 1.0 . . H H11A 0.7411 0.4211 0.9538 0.06 Uiso calc R 1.0 . . H H11B 0.6803 0.383 0.9217 0.06 Uiso calc R 1.0 . . H H11C 0.6753 0.4457 0.975 0.06 Uiso calc R 1.0 . . C C12 0.7387(6) 0.5113(9) 0.8582(5) 0.027(3) Uani d . 1.0 . . H H12A 0.7315 0.5619 0.8329 0.04 Uiso calc R 1.0 . . H H12B 0.7316 0.4554 0.8377 0.04 Uiso calc R 1.0 . . H H12C 0.7811 0.5129 0.8741 0.04 Uiso calc R 1.0 . . C C13 0.6097(6) 0.7871(9) 1.0056(5) 0.027(3) Uani d . 1.0 . . H H13 0.5717 0.7625 0.9859 0.033 Uiso calc R 1.0 . . C C14 0.6048(9) 0.7714(13) 1.0680(7) 0.064(6) Uani d . 1.0 . . H H14A 0.6405 0.7976 1.0887 0.096 Uiso calc R 1.0 . . H H14B 0.6035 0.7071 1.0754 0.096 Uiso calc R 1.0 . . H H14C 0.5673 0.7994 1.0799 0.096 Uiso calc R 1.0 . . C C15 0.6128(7) 0.8833(10) 0.9918(7) 0.045(4) Uani d . 1.0 . . H H15A 0.5742 0.9122 1.0 0.068 Uiso calc R 1.0 . . H H15B 0.6195 0.8902 0.9523 0.068 Uiso calc R 1.0 . . H H15C 0.6467 0.911 1.0141 0.068 Uiso calc R 1.0 . . C C16 0.4563(5) 0.6292(8) 0.8513(4) 0.017(2) Uani d . 1.0 . . C C17 0.4512(5) 0.5757(9) 0.8042(5) 0.022(3) Uani d . 1.0 . . C C18 0.3995(5) 0.5822(8) 0.7701(5) 0.020(3) Uani d . 1.0 . . H H18 0.3948 0.5463 0.7376 0.024 Uiso calc R 1.0 . . C C19 0.8592(5) 0.8049(9) 1.3298(5) 0.023(3) Uani d . 1.0 . . H H19 0.8274 0.7643 1.3373 0.027 Uiso calc R 1.0 . . C C20 0.8529(5) 0.8578(8) 1.2830(5) 0.021(3) Uani d . 1.0 . . C C21 0.4106(5) 0.6904(8) 0.8658(5) 0.021(3) Uani d . 1.0 . . C C22 0.4178(6) 0.7480(9) 0.9180(5) 0.026(3) Uani d . 1.0 . . H H22 0.4568 0.7309 0.9393 0.031 Uiso calc R 1.0 . . C C23 0.3655(7) 0.7336(11) 0.9547(6) 0.042(4) Uani d . 1.0 . . H H23A 0.3272 0.7531 0.9351 0.063 Uiso calc R 1.0 . . H H23B 0.3727 0.7683 0.9889 0.063 Uiso calc R 1.0 . . H H23C 0.3627 0.6701 0.9639 0.063 Uiso calc R 1.0 . . C C24 0.4214(8) 0.8488(12) 0.9024(6) 0.054(5) Uani d . 1.0 . . H H24A 0.4591 0.86 0.8836 0.082 Uiso calc R 1.0 . . H H24B 0.4215 0.8851 0.9362 0.082 Uiso calc R 1.0 . . H H24C 0.3859 0.8648 0.8775 0.082 Uiso calc R 1.0 . . C C25 0.5007(6) 0.5068(9) 0.7930(5) 0.029(3) Uani d . 1.0 . . H H25 0.5357 0.5166 0.8211 0.035 Uiso calc R 1.0 . . C C26 0.4765(7) 0.4123(10) 0.8016(6) 0.044(4) Uani d . 1.0 . . H H26A 0.443 0.3998 0.7737 0.066 Uiso calc R 1.0 . . H H26B 0.4614 0.4074 0.8389 0.066 Uiso calc R 1.0 . . H H26C 0.5097 0.3692 0.7977 0.066 Uiso calc R 1.0 . . C C27 0.5248(7) 0.5186(12) 0.7361(6) 0.049(4) Uani d . 1.0 . . H H27A 0.5587 0.4769 0.7318 0.073 Uiso calc R 1.0 . . H H27B 0.5394 0.5799 0.7321 0.073 Uiso calc R 1.0 . . H H27C 0.4919 0.5065 0.7076 0.073 Uiso calc R 1.0 . . C C28 0.6116(5) 0.8628(8) 0.7785(4) 0.019(3) Uani d . 1.0 . . C C29 0.6471(5) 0.9894(8) 0.7396(4) 0.0174(19) Uani d . 1.0 . . H H29 0.6659 1.0462 0.7367 0.021 Uiso calc R 1.0 . . C C30 0.6213(5) 0.9423(8) 0.6983(5) 0.0174(19) Uani d . 1.0 . . H H30 0.6187 0.9579 0.66 0.021 Uiso calc R 1.0 . . C C31 0.6735(5) 0.9647(8) 0.8405(4) 0.0139(19) Uani d . 1.0 . . C C32 0.6483(5) 1.0316(8) 0.8729(4) 0.015(3) Uani d . 1.0 . . C C33 0.6819(5) 1.0583(9) 0.9217(5) 0.021(3) Uani d . 1.0 . . H H33 0.6685 1.1068 0.9431 0.026 Uiso calc R 1.0 . . C C34 0.7359(5) 1.0117(8) 0.9380(4) 0.016(3) Uani d . 1.0 . . C C35 0.7594(5) 0.9470(8) 0.9055(5) 0.019(3) Uani d . 1.0 . . H H35 0.7969 0.9185 0.9172 0.023 Uiso calc R 1.0 . . C C36 0.7290(5) 0.9224(8) 0.8553(4) 0.015(2) Uani d . 1.0 . . C C37 0.7586(5) 0.8569(8) 0.8176(4) 0.020(3) Uani d . 1.0 . . H H37 0.729 0.8454 0.785 0.024 Uiso calc R 1.0 . . C C38 0.7716(6) 0.7672(9) 0.8469(5) 0.028(3) Uani d . 1.0 . . H H38A 0.8004 0.7764 0.8792 0.043 Uiso calc R 1.0 . . H H38B 0.7894 0.7255 0.8211 0.043 Uiso calc R 1.0 . . H H38C 0.7332 0.7425 0.8592 0.043 Uiso calc R 1.0 . . C C39 0.8167(6) 0.8971(9) 0.7954(5) 0.033(3) Uani d . 1.0 . . H H39A 0.8066 0.9539 0.7769 0.05 Uiso calc R 1.0 . . H H39B 0.8335 0.8557 0.7688 0.05 Uiso calc R 1.0 . . H H39C 0.8472 0.9073 0.8263 0.05 Uiso calc R 1.0 . . C C40 0.5887(5) 1.0806(9) 0.8562(5) 0.025(3) Uani d . 1.0 . . H H40 0.5711 1.0521 0.8212 0.03 Uiso calc R 1.0 . . C C41 0.5428(6) 1.0662(11) 0.9003(6) 0.041(3) Uani d . 1.0 . . H H41A 0.5579 1.0948 0.9351 0.062 Uiso calc R 1.0 . . H H41B 0.5377 1.002 0.9065 0.062 Uiso calc R 1.0 . . H H41C 0.5033 1.0924 0.8876 0.062 Uiso calc R 1.0 . . C C42 0.5986(6) 1.1763(10) 0.8437(6) 0.041(3) Uani d . 1.0 . . H H42A 0.6173 1.2061 0.8768 0.062 Uiso calc R 1.0 . . H H42B 0.5592 1.2045 0.8329 0.062 Uiso calc R 1.0 . . H H42C 0.6259 1.1815 0.8132 0.062 Uiso calc R 1.0 . . C C43 0.5740(5) 0.7901(8) 0.6886(4) 0.017(2) Uani d . 1.0 . . C C44 0.5110(5) 0.7857(8) 0.6758(4) 0.015(3) Uani d . 1.0 . . C C45 0.4906(6) 0.7151(9) 0.6411(5) 0.024(3) Uani d . 1.0 . . H H45 0.4481 0.7088 0.6311 0.028 Uiso calc R 1.0 . . C C46 1.0317(5) 0.8451(8) 1.1214(4) 0.019(2) Uani d . 1.0 . . C C47 0.5932(5) 0.6609(8) 0.6348(4) 0.016(3) Uani d . 1.0 . . H H47 0.6202 0.6181 0.6205 0.02 Uiso calc R 1.0 . . C C48 0.6170(5) 0.7294(8) 0.6692(4) 0.016(3) Uani d . 1.0 . . C C49 0.6855(5) 0.7376(8) 0.6818(5) 0.018(3) Uani d . 1.0 . . H H49 0.6934 0.79 0.707 0.022 Uiso calc R 1.0 . . C C50 0.7107(6) 0.6537(11) 0.7115(6) 0.044(4) Uani d . 1.0 . . H H50A 0.6858 0.6399 0.7428 0.067 Uiso calc R 1.0 . . H H50B 0.7532 0.6642 0.7253 0.067 Uiso calc R 1.0 . . H H50C 0.7091 0.6035 0.6854 0.067 Uiso calc R 1.0 . . C C51 0.7181(6) 0.7527(10) 0.6295(6) 0.036(4) Uani d . 1.0 . . H H51A 0.7068 0.7055 0.6026 0.054 Uiso calc R 1.0 . . H H51B 0.7625 0.7515 0.6382 0.054 Uiso calc R 1.0 . . H H51C 0.7062 0.8108 0.6136 0.054 Uiso calc R 1.0 . . C C52 0.4666(5) 0.8570(9) 0.6938(5) 0.022(3) Uani d . 1.0 . . H H52 0.4867 0.8881 0.7268 0.027 Uiso calc R 1.0 . . C C53 0.4084(7) 0.8159(12) 0.7120(8) 0.060(5) Uani d . 1.0 . . H H53A 0.3869 0.7857 0.6804 0.091 Uiso calc R 1.0 . . H H53B 0.382 0.8627 0.7259 0.091 Uiso calc R 1.0 . . H H53C 0.4182 0.7725 0.7417 0.091 Uiso calc R 1.0 . . C C54 0.4547(7) 0.9260(10) 0.6490(6) 0.046(4) Uani d . 1.0 . . H H54A 0.4353 0.8975 0.6158 0.068 Uiso calc R 1.0 . . H H54B 0.4936 0.9532 0.6399 0.068 Uiso calc R 1.0 . . H H54C 0.4274 0.9723 0.6622 0.068 Uiso calc R 1.0 . . C C55 0.7525(6) 1.0967(10) 1.1731(6) 0.037(4) Uani d . 1.0 . . H H55A 0.7335 1.1012 1.1353 0.056 Uiso calc R 1.0 . . H H55B 0.7304 1.1351 1.198 0.056 Uiso calc R 1.0 . . H H55C 0.7508 1.0347 1.1859 0.056 Uiso calc R 1.0 . . C C56 0.8190(7) 1.2376(9) 1.1413(6) 0.034(3) Uani d . 1.0 . . H H56A 0.8585 1.2678 1.139 0.05 Uiso calc R 1.0 . . H H56B 0.7922 1.274 1.1632 0.05 Uiso calc R 1.0 . . H H56C 0.7998 1.2294 1.1037 0.05 Uiso calc R 1.0 . . C C57 1.0331(10) 1.227(2) 1.1857(10) 0.135(13) Uani d . 1.0 A . H H57A 1.0185 1.2836 1.2005 0.202 Uiso calc R 1.0 A . H H57B 1.0745 1.2147 1.2017 0.202 Uiso calc R 1.0 A . H H57C 1.0056 1.1786 1.1955 0.202 Uiso calc R 1.0 A . C C58 1.0583(10) 1.3438(13) 1.1126(9) 0.082(6) Uani d . 1.0 A . H H58A 1.0524 1.3646 1.0741 0.123 Uiso calc R 1.0 A . H H58B 1.1018 1.3477 1.1249 0.123 Uiso calc R 1.0 A . H H58C 1.0343 1.3813 1.1365 0.123 Uiso calc R 1.0 A . C C59 0.9575(11) 0.3405(13) 0.9706(7) 0.082(7) Uani d . 1.0 B . H H59A 0.9279 0.2934 0.9778 0.123 Uiso calc R 1.0 B . H H59B 0.9922 0.3371 0.9983 0.123 Uiso calc R 1.0 B . H H59C 0.9721 0.3325 0.9333 0.123 Uiso calc R 1.0 B . C C60 0.8958(13) 0.4388(14) 1.0382(7) 0.102(9) Uani d . 1.0 B . H H60A 0.8594 0.4768 1.0386 0.153 Uiso calc R 1.0 B . H H60B 0.9272 0.4609 1.0657 0.153 Uiso calc R 1.0 B . H H60C 0.8849 0.3774 1.0474 0.153 Uiso calc R 1.0 B . C C61 0.8991(7) 0.3022(10) 0.2760(6) 0.042(4) Uani d . 1.0 C . H H61A 0.9167 0.2566 0.2526 0.064 Uiso calc R 1.0 C . H H61B 0.8544 0.2962 0.2741 0.064 Uiso calc R 1.0 C . H H61C 0.9153 0.2944 0.3146 0.064 Uiso calc R 1.0 C . C C62 0.8931(8) 0.4700(12) 0.3024(7) 0.058(5) Uani d . 1.0 C . H H62A 0.9023 0.4433 0.3391 0.086 Uiso calc R 1.0 C . H H62B 0.8487 0.4784 0.2962 0.086 Uiso calc R 1.0 C . H H62C 0.9136 0.528 0.3006 0.086 Uiso calc R 1.0 C . C C63 0.7548(7) -0.0175(13) 0.4012(6) 0.056(5) Uani d . 1.0 D . H H63A 0.7354 0.0316 0.4204 0.083 Uiso calc R 1.0 D . H H63B 0.7623 -0.0675 0.427 0.083 Uiso calc R 1.0 D . H H63C 0.7278 -0.037 0.3695 0.083 Uiso calc R 1.0 D . C C64 0.8008(8) 0.1084(12) 0.3422(7) 0.059(5) Uani d . 1.0 D . H H64A 0.7821 0.1509 0.367 0.089 Uiso calc R 1.0 D . H H64B 0.7707 0.0912 0.3123 0.089 Uiso calc R 1.0 D . H H64C 0.8362 0.1364 0.3262 0.089 Uiso calc R 1.0 D . N N1 0.5961(4) 0.6298(7) 0.9345(4) 0.019(2) Uani d . 1.0 . . N N2 0.5094(4) 0.6184(7) 0.8900(4) 0.021(2) Uani d . 1.0 . . N N3 0.6418(4) 0.9403(6) 0.7887(3) 0.012(2) Uani d . 1.0 . . N N4 0.5984(4) 0.8645(6) 0.7221(3) 0.013(2) Uani d . 1.0 . . Na Na1 0.9140(2) 1.1149(4) 1.0535(2) 0.0479(17) Uani d . 1.0 . . Na Na2 0.9141(2) 0.9202(4) 0.97984(18) 0.0281(12) Uani d . 1.0 . . Na Na3 0.83679(19) 0.9245(3) 1.10498(16) 0.0200(11) Uani d . 1.0 . . O O1 0.8826(4) 0.6528(6) 1.0224(4) 0.039(2) Uani d . 1.0 . . O O2 0.8441(4) 0.7848(7) 1.0649(4) 0.052(3) Uani d . 1.0 . . O O3 0.8693(4) 0.7860(8) 0.9698(5) 0.052(3) Uani d . 1.0 . . O O4 0.7619(4) 0.7635(6) 1.2416(3) 0.030(2) Uani d . 1.0 . . O O5 0.7995(4) 0.8822(6) 1.1852(3) 0.031(2) Uani d . 1.0 . . O O6 0.7418(4) 0.9171(6) 1.2653(3) 0.033(2) Uani d . 1.0 . . O O7 0.7547(4) 0.9774(6) 1.0432(3) 0.031(2) Uani d . 1.0 . . O O8 0.8406(4) 1.0312(7) 0.9945(3) 0.033(2) Uani d . 1.0 . . O O9 0.7577(4) 1.1328(6) 1.0149(3) 0.039(2) Uani d . 1.0 . . O O10 0.9413(3) 0.9441(6) 1.0789(3) 0.022(2) Uani d . 1.0 . . O O11 1.0208(4) 0.9019(6) 1.0195(3) 0.023(2) Uani d . 1.0 . . O O12 1.0423(4) 1.0114(5) 1.0931(3) 0.025(2) Uani d . 1.0 . . O O13 0.8604(4) 1.0746(6) 1.1316(3) 0.026(2) Uani d . 1.0 . . O O14 0.9669(4) 1.2340(8) 1.0934(4) 0.050(3) Uani d . 1.0 A . O O16 0.8760(5) 0.4502(10) 0.9335(4) 0.070(2) Uani d . 1.0 B . O O17 0.9795(5) 0.4122(10) 0.2524(4) 0.070(2) Uani d . 1.0 C . O O18 0.8657(5) 0.0320(10) 0.4222(4) 0.070(2) Uani d . 1.0 D . O O19 0.8454(9) 1.2479(13) 1.0068(8) 0.044(5) Uani d P 0.5 E . S S1 0.84843(14) 0.7340(2) 1.01491(14) 0.0271(9) Uani d . 1.0 . . S S2 0.78277(14) 0.8543(2) 1.23997(12) 0.0234(8) Uani d . 1.0 . . S S3 0.77560(14) 1.0415(2) 1.00319(11) 0.0209(8) Uani d . 1.0 . . S S4 1.00725(13) 0.9325(2) 1.07532(11) 0.0161(8) Uani d . 1.0 . . S S5 0.83065(14) 1.1319(2) 1.17357(12) 0.0220(8) Uani d . 1.0 . . S S7 0.92329(16) 0.4412(3) 0.97457(15) 0.0379(9) Uani d . 1.0 B . S S8 0.9178(5) 0.4029(7) 0.2537(6) 0.174(4) Uani d . 1.0 C . S S6A 1.0340(3) 1.2339(4) 1.1167(2) 0.0856(17) Uani d . 1.0 A . S S9A 0.8235(3) 0.0185(5) 0.3779(3) 0.0564(18) Uani d P 0.662(8) D . S S9B 0.8080(6) 0.0628(11) 0.4080(5) 0.0564(18) Uani d P 0.338(8) D . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ag1 0.0179(6) 0.0138(6) 0.0135(6) -0.0004(4) -0.0031(4) 0.0031(4) C1 0.018(7) 0.021(8) 0.016(6) 0.004(6) 0.006(5) 0.001(6) C2 0.024(8) 0.032(9) 0.018(6) -0.004(6) 0.001(6) 0.008(6) C3 0.022(7) 0.022(8) 0.026(7) -0.009(6) 0.001(6) 0.008(6) C4 0.020(5) 0.010(5) 0.011(4) -0.007(4) -0.002(3) 0.004(4) C5 0.013(7) 0.015(7) 0.021(6) 0.002(5) -0.002(5) 0.006(5) C6 0.032(8) 0.009(7) 0.014(6) 0.008(6) -0.002(5) 0.004(5) C7 0.019(5) 0.024(6) 0.012(4) 0.001(4) -0.010(4) 0.001(4) C8 0.024(7) 0.017(7) 0.008(6) 0.005(5) -0.007(5) 0.003(5) C9 0.023(5) 0.011(5) 0.011(4) -0.001(4) -0.006(4) 0.003(4) C10 0.020(7) 0.015(7) 0.026(7) 0.000(5) -0.005(5) 0.000(6) C11 0.049(9) 0.034(10) 0.039(8) -0.009(7) 0.016(7) -0.008(7) C12 0.042(8) 0.015(8) 0.021(7) 0.001(6) -0.011(6) -0.002(6) C13 0.024(7) 0.029(9) 0.029(7) 0.003(6) 0.005(6) -0.009(6) C14 0.078(13) 0.071(13) 0.047(10) 0.050(10) 0.032(9) 0.015(9) C15 0.033(8) 0.025(10) 0.079(11) 0.016(7) 0.016(8) 0.015(8) C16 0.022(5) 0.014(5) 0.015(4) -0.001(4) -0.006(4) 0.009(4) C17 0.017(7) 0.025(8) 0.023(7) 0.004(6) -0.004(5) 0.008(6) C18 0.021(7) 0.016(8) 0.022(6) 0.003(6) -0.001(6) 0.005(5) C19 0.019(7) 0.027(8) 0.023(7) -0.005(6) -0.001(6) -0.003(6) C20 0.018(7) 0.023(8) 0.023(7) 0.004(6) -0.004(5) 0.000(6) C21 0.025(7) 0.013(7) 0.023(7) -0.006(6) -0.002(6) 0.005(5) C22 0.018(7) 0.038(9) 0.021(7) 0.005(6) -0.003(5) -0.009(6) C23 0.055(10) 0.047(11) 0.024(8) -0.005(8) 0.000(7) -0.006(7) C24 0.067(11) 0.056(12) 0.039(9) -0.024(9) -0.008(8) -0.005(8) C25 0.029(8) 0.025(9) 0.032(7) 0.001(6) 0.003(6) 0.006(6) C26 0.057(10) 0.028(10) 0.047(9) 0.012(8) 0.009(7) 0.001(7) C27 0.039(9) 0.070(12) 0.040(8) 0.027(8) 0.018(7) 0.018(8) C28 0.015(6) 0.024(9) 0.016(7) 0.011(6) -0.002(5) -0.007(5) C29 0.023(5) 0.014(5) 0.015(4) -0.002(4) -0.004(3) 0.004(4) C30 0.023(5) 0.014(5) 0.015(4) -0.002(4) -0.004(3) 0.004(4) C31 0.020(5) 0.010(5) 0.011(4) -0.007(4) -0.002(3) 0.004(4) C32 0.016(6) 0.012(7) 0.017(6) -0.002(5) -0.002(5) 0.003(5) C33 0.024(7) 0.026(8) 0.015(6) 0.004(6) -0.002(5) 0.005(6) C34 0.023(7) 0.011(7) 0.013(6) -0.001(6) -0.010(5) -0.005(5) C35 0.014(6) 0.021(8) 0.022(7) 0.003(6) 0.001(5) 0.009(6) C36 0.023(5) 0.011(5) 0.011(4) -0.001(4) -0.006(4) 0.003(4) C37 0.023(7) 0.024(8) 0.012(6) 0.001(6) -0.008(5) -0.003(5) C38 0.035(8) 0.018(8) 0.032(7) 0.002(6) -0.001(6) -0.005(6) C39 0.054(9) 0.013(8) 0.034(7) 0.010(7) 0.017(7) -0.007(6) C40 0.020(7) 0.030(9) 0.024(7) 0.015(6) -0.006(5) -0.006(6) C41 0.029(6) 0.042(7) 0.050(6) 0.019(5) -0.022(5) -0.005(5) C42 0.029(6) 0.042(7) 0.050(6) 0.019(5) -0.022(5) -0.005(5) C43 0.022(5) 0.014(5) 0.015(4) -0.001(4) -0.006(4) 0.009(4) C44 0.022(7) 0.016(7) 0.009(6) -0.002(6) 0.000(5) 0.003(5) C45 0.022(7) 0.031(9) 0.018(6) 0.005(6) 0.001(5) -0.001(6) C46 0.019(5) 0.024(6) 0.012(4) 0.001(4) -0.010(4) 0.001(4) C47 0.020(7) 0.014(7) 0.013(6) 0.000(5) -0.005(5) -0.008(5) C48 0.019(7) 0.015(7) 0.015(6) 0.007(6) 0.000(5) 0.009(5) C49 0.017(7) 0.014(7) 0.024(7) -0.002(5) -0.003(5) 0.000(5) C50 0.026(8) 0.066(12) 0.040(8) 0.005(8) -0.015(6) 0.019(8) C51 0.016(7) 0.049(10) 0.043(9) -0.008(6) -0.002(6) -0.004(7) C52 0.023(7) 0.023(8) 0.021(6) 0.000(6) 0.003(5) -0.010(6) C53 0.051(10) 0.043(11) 0.091(13) -0.009(8) 0.028(9) -0.028(10) C54 0.058(10) 0.032(10) 0.045(9) 0.021(8) -0.014(7) -0.005(7) C55 0.026(8) 0.049(10) 0.039(8) 0.006(7) 0.015(6) -0.005(7) C56 0.040(9) 0.030(9) 0.031(8) 0.009(7) 0.010(6) 0.006(6) C57 0.054(14) 0.24(4) 0.113(19) 0.037(17) -0.013(13) 0.10(2) C58 0.104(16) 0.040(12) 0.097(15) -0.016(11) -0.028(12) -0.005(11) C59 0.16(2) 0.047(12) 0.044(10) 0.045(13) 0.015(11) -0.004(9) C60 0.21(3) 0.055(14) 0.048(11) 0.078(16) 0.045(14) 0.012(10) C61 0.046(9) 0.032(10) 0.049(9) -0.005(7) -0.005(7) 0.003(7) C62 0.066(11) 0.048(12) 0.056(10) 0.014(9) -0.016(8) -0.014(9) C63 0.055(10) 0.080(14) 0.030(8) -0.003(9) -0.009(7) 0.005(8) C64 0.069(12) 0.057(12) 0.048(9) -0.028(9) -0.029(8) 0.024(9) N1 0.018(6) 0.022(6) 0.016(5) 0.001(5) 0.001(4) 0.006(5) N2 0.018(6) 0.020(6) 0.025(6) -0.007(5) 0.004(4) 0.012(5) N3 0.018(5) 0.003(6) 0.013(5) -0.005(4) -0.006(4) 0.000(4) N4 0.022(5) 0.005(6) 0.013(5) 0.005(4) -0.005(4) -0.002(4) Na1 0.045(3) 0.066(4) 0.034(3) -0.040(3) 0.018(3) -0.032(3) Na2 0.020(3) 0.040(3) 0.023(2) -0.007(2) -0.0081(19) -0.001(2) Na3 0.022(2) 0.022(3) 0.015(2) -0.001(2) -0.0021(18) -0.003(2) O1 0.035(5) 0.024(6) 0.056(6) 0.010(5) -0.026(4) -0.010(5) O2 0.033(6) 0.051(7) 0.068(7) 0.013(5) -0.031(5) -0.037(6) O3 0.025(5) 0.053(7) 0.074(7) -0.013(5) -0.021(5) 0.008(6) O4 0.032(5) 0.022(6) 0.034(5) -0.009(4) -0.009(4) 0.004(4) O5 0.028(5) 0.043(6) 0.021(5) -0.011(4) -0.007(4) 0.009(4) O6 0.021(5) 0.045(6) 0.031(5) 0.004(4) -0.005(4) -0.004(4) O7 0.042(5) 0.031(6) 0.020(4) -0.002(4) -0.004(4) 0.000(4) O8 0.025(5) 0.049(7) 0.025(5) 0.008(4) -0.005(4) -0.016(4) O9 0.060(6) 0.023(6) 0.031(5) 0.015(5) -0.019(4) -0.014(4) O10 0.017(5) 0.028(5) 0.022(4) 0.005(4) 0.006(3) 0.004(4) O11 0.027(5) 0.022(5) 0.019(4) 0.010(4) 0.003(3) 0.003(4) O12 0.039(5) 0.012(5) 0.021(4) -0.008(4) -0.018(4) 0.003(4) O13 0.032(5) 0.017(5) 0.029(5) 0.000(4) 0.009(4) -0.007(4) O14 0.030(6) 0.061(8) 0.059(7) -0.015(5) -0.010(5) -0.013(5) O16 0.044(4) 0.124(7) 0.040(4) 0.016(4) -0.022(3) -0.011(4) O17 0.044(4) 0.124(7) 0.040(4) 0.016(4) -0.022(3) -0.011(4) O18 0.044(4) 0.124(7) 0.040(4) 0.016(4) -0.022(3) -0.011(4) O19 0.044(13) 0.032(13) 0.056(13) -0.006(9) 0.003(10) -0.006(10) S1 0.0213(19) 0.018(2) 0.040(2) 0.0012(15) -0.0138(15) -0.0080(16) S2 0.0236(18) 0.029(2) 0.0170(16) -0.0049(15) -0.0066(13) 0.0048(14) S3 0.0262(19) 0.021(2) 0.0143(15) 0.0078(14) -0.0070(13) -0.0034(14) S4 0.0192(17) 0.0161(19) 0.0126(15) 0.0025(13) -0.0030(12) 0.0022(13) S5 0.0285(18) 0.020(2) 0.0177(16) 0.0012(14) 0.0005(13) -0.0040(13) S7 0.039(2) 0.030(2) 0.045(2) -0.0003(17) -0.0007(17) 0.0010(17) S8 0.126(7) 0.120(8) 0.280(13) -0.033(6) 0.049(8) -0.013(8) S6A 0.100(5) 0.072(4) 0.085(4) -0.006(3) 0.007(3) 0.007(3) S9A 0.055(4) 0.070(5) 0.044(4) -0.003(3) -0.003(3) 0.000(3) S9B 0.055(4) 0.070(5) 0.044(4) -0.003(3) -0.003(3) 0.000(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ag1 C1 . 2.092(12) ? Ag1 C28 . 2.099(12) ? C1 N2 . 1.351(15) ? C1 N1 . 1.365(15) ? C2 C3 . 1.351(17) ? C2 N2 . 1.382(15) ? C3 N1 . 1.391(15) ? C4 C5 . 1.386(17) ? C4 C9 . 1.395(17) ? C4 N1 . 1.443(15) ? C5 C6 . 1.388(17) ? C5 C13 . 1.547(17) ? C6 C7 . 1.371(17) ? C7 C8 . 1.385(17) ? C7 S1 . 1.789(12) ? C8 C9 . 1.368(16) ? C9 C10 . 1.539(17) ? C10 C12 . 1.509(17) ? C10 C11 . 1.538(19) ? C13 C15 . 1.48(2) ? C13 C14 . 1.53(2) ? C16 C17 . 1.388(17) ? C16 C21 . 1.416(17) ? C16 N2 . 1.453(15) ? C17 C18 . 1.359(17) ? C17 C25 . 1.530(18) ? C18 C20 4_575 1.407(17) ? C19 C21 4_676 1.379(17) ? C19 C20 . 1.378(17) ? C20 C18 4_676 1.407(17) ? C20 S2 . 1.796(12) ? C21 C19 4_575 1.379(17) ? C21 C22 . 1.525(17) ? C22 C23 . 1.504(19) ? C22 C24 . 1.56(2) ? C25 C27 . 1.511(18) ? C25 C26 . 1.53(2) ? C28 N3 . 1.351(15) ? C28 N4 . 1.372(14) ? C29 C30 . 1.316(17) ? C29 N3 . 1.405(14) ? C30 N4 . 1.406(15) ? C31 C36 . 1.394(16) ? C31 C32 . 1.404(16) ? C31 N3 . 1.437(14) ? C32 C33 . 1.405(17) ? C32 C40 . 1.525(17) ? C33 C34 . 1.406(17) ? C34 C35 . 1.368(17) ? C34 S3 . 1.801(11) ? C35 C36 . 1.392(16) ? C36 C37 . 1.513(17) ? C37 C39 . 1.532(18) ? C37 C38 . 1.537(18) ? C40 C42 . 1.48(2) ? C40 C41 . 1.523(19) ? C43 C44 . 1.393(17) ? C43 C48 . 1.409(17) ? C43 N4 . 1.458(15) ? C44 C45 . 1.403(18) ? C44 C52 . 1.525(17) ? C45 C46 4_575 1.378(17) ? C46 C47 4_676 1.366(16) ? C46 C45 4_676 1.378(18) ? C46 S4 . 1.778(12) ? C47 C46 4_575 1.366(16) ? C47 C48 . 1.399(17) ? C48 C49 . 1.515(17) ? C49 C51 . 1.505(18) ? C49 C50 . 1.532(19) ? C52 C53 . 1.504(19) ? C52 C54 . 1.506(19) ? C55 S5 . 1.788(13) ? C56 S5 . 1.777(13) ? C57 S6A . 1.67(2) ? C58 S6A . 1.74(2) ? C59 S7 . 1.689(18) ? C60 S7 . 1.683(17) ? C61 S8 . 1.662(18) ? C62 S8 . 1.662(19) ? C63 S9A . 1.723(17) ? C64 S9A . 1.657(18) ? Na1 O14 . 2.304(11) ? Na1 O11 3_777 2.349(9) ? Na1 O13 . 2.358(9) ? Na1 O8 . 2.425(10) ? Na1 O10 . 2.688(11) ? Na1 O19 . 2.70(2) ? Na1 S3 . 3.372(6) ? Na1 Na2 . 3.415(7) ? Na1 Na3 . 3.575(7) ? Na1 Na2 3_777 3.929(7) ? Na2 O3 . 2.244(12) ? Na2 O12 3_777 2.294(9) ? Na2 O8 . 2.354(10) ? Na2 O10 . 2.451(9) ? Na2 O11 . 2.480(9) ? Na2 S4 . 2.980(5) ? Na2 S4 3_777 3.144(6) ? Na2 S1 . 3.274(6) ? Na2 Na3 . 3.552(6) ? Na2 Na1 3_777 3.929(7) ? Na3 O5 . 2.237(9) ? Na3 O2 . 2.315(11) ? Na3 O13 . 2.385(10) ? Na3 O7 . 2.392(10) ? Na3 O10 . 2.425(9) ? Na3 S3 . 3.234(5) ? O1 S1 . 1.433(10) ? O2 S1 . 1.434(10) ? O3 S1 . 1.435(11) ? O4 S2 . 1.436(9) ? O5 S2 . 1.454(9) ? O6 S2 . 1.460(9) ? O7 S3 . 1.455(9) ? O8 S3 . 1.459(9) ? O9 S3 . 1.455(9) ? O10 S4 . 1.461(8) ? O11 S4 . 1.470(8) ? O11 Na1 3_777 2.349(9) ? O12 S4 . 1.458(8) ? O12 Na2 3_777 2.294(9) ? O13 S5 . 1.506(8) ? O14 S6A . 1.537(12) ? O16 S7 . 1.392(11) ? O17 S8 . 1.357(14) ? O18 S9A . 1.381(12) ? S4 Na2 3_777 3.143(6) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 Ag1 C28 . . 178.3(4) ? N2 C1 N1 . . 102.8(9) ? N2 C1 Ag1 . . 128.9(8) ? N1 C1 Ag1 . . 128.3(8) ? C3 C2 N2 . . 107.0(10) ? C2 C3 N1 . . 105.4(10) ? C5 C4 C9 . . 123.7(10) ? C5 C4 N1 . . 118.9(10) ? C9 C4 N1 . . 117.2(10) ? C4 C5 C6 . . 117.4(10) ? C4 C5 C13 . . 122.6(10) ? C6 C5 C13 . . 120.0(11) ? C7 C6 C5 . . 119.7(11) ? C6 C7 C8 . . 121.3(11) ? C6 C7 S1 . . 119.4(10) ? C8 C7 S1 . . 119.2(9) ? C9 C8 C7 . . 121.0(11) ? C8 C9 C4 . . 116.7(10) ? C8 C9 C10 . . 120.8(10) ? C4 C9 C10 . . 122.4(10) ? C12 C10 C11 . . 112.8(10) ? C12 C10 C9 . . 112.0(10) ? C11 C10 C9 . . 110.3(9) ? C15 C13 C14 . . 112.1(13) ? C15 C13 C5 . . 114.4(11) ? C14 C13 C5 . . 107.5(11) ? C17 C16 C21 . . 123.8(10) ? C17 C16 N2 . . 118.7(10) ? C21 C16 N2 . . 117.4(10) ? C18 C17 C16 . . 118.2(11) ? C18 C17 C25 . . 120.8(11) ? C16 C17 C25 . . 120.9(10) ? C17 C18 C20 . 4_575 119.9(11) ? C21 C19 C20 4_676 . 121.4(12) ? C19 C20 C18 . 4_676 120.8(11) ? C19 C20 S2 . . 119.5(9) ? C18 C20 S2 4_676 . 119.7(9) ? C19 C21 C16 4_575 . 115.8(11) ? C19 C21 C22 4_575 . 121.9(11) ? C16 C21 C22 . . 122.3(10) ? C23 C22 C21 . . 111.2(11) ? C23 C22 C24 . . 109.4(12) ? C21 C22 C24 . . 110.6(10) ? C27 C25 C26 . . 112.0(12) ? C27 C25 C17 . . 111.9(11) ? C26 C25 C17 . . 110.3(11) ? N3 C28 N4 . . 103.5(10) ? N3 C28 Ag1 . . 129.2(8) ? N4 C28 Ag1 . . 127.2(9) ? C30 C29 N3 . . 107.7(10) ? C29 C30 N4 . . 106.4(9) ? C36 C31 C32 . . 123.3(10) ? C36 C31 N3 . . 118.0(10) ? C32 C31 N3 . . 118.6(10) ? C33 C32 C31 . . 117.6(10) ? C33 C32 C40 . . 118.5(10) ? C31 C32 C40 . . 123.8(10) ? C32 C33 C34 . . 118.7(11) ? C35 C34 C33 . . 122.0(10) ? C35 C34 S3 . . 119.9(9) ? C33 C34 S3 . . 118.1(9) ? C34 C35 C36 . . 120.6(11) ? C35 C36 C31 . . 117.5(10) ? C35 C36 C37 . . 119.6(10) ? C31 C36 C37 . . 122.7(9) ? C36 C37 C39 . . 110.6(10) ? C36 C37 C38 . . 111.3(9) ? C39 C37 C38 . . 111.8(10) ? C42 C40 C41 . . 113.0(11) ? C42 C40 C32 . . 112.6(10) ? C41 C40 C32 . . 109.7(10) ? C44 C43 C48 . . 124.5(11) ? C44 C43 N4 . . 118.8(10) ? C48 C43 N4 . . 116.6(10) ? C43 C44 C45 . . 116.1(11) ? C43 C44 C52 . . 122.9(11) ? C45 C44 C52 . . 120.9(10) ? C46 C45 C44 4_575 . 120.6(11) ? C47 C46 C45 4_676 4_676 122.0(11) ? C47 C46 S4 4_676 . 116.6(9) ? C45 C46 S4 4_676 . 121.4(9) ? C46 C47 C48 4_575 . 120.7(11) ? C47 C48 C43 . . 116.1(11) ? C47 C48 C49 . . 120.3(10) ? C43 C48 C49 . . 123.6(11) ? C51 C49 C48 . . 111.1(10) ? C51 C49 C50 . . 109.8(11) ? C48 C49 C50 . . 110.4(10) ? C53 C52 C54 . . 112.3(13) ? C53 C52 C44 . . 111.3(11) ? C54 C52 C44 . . 111.1(10) ? C1 N1 C3 . . 112.4(10) ? C1 N1 C4 . . 125.8(10) ? C3 N1 C4 . . 121.7(9) ? C1 N2 C2 . . 112.3(10) ? C1 N2 C16 . . 126.4(9) ? C2 N2 C16 . . 121.3(9) ? C28 N3 C29 . . 111.2(9) ? C28 N3 C31 . . 125.5(9) ? C29 N3 C31 . . 122.6(9) ? C28 N4 C30 . . 111.2(9) ? C28 N4 C43 . . 125.5(10) ? C30 N4 C43 . . 122.4(8) ? O14 Na1 O11 . 3_777 94.8(4) ? O14 Na1 O13 . . 97.3(4) ? O11 Na1 O13 3_777 . 158.0(4) ? O14 Na1 O8 . . 160.3(5) ? O11 Na1 O8 3_777 . 85.1(3) ? O13 Na1 O8 . . 89.6(3) ? O14 Na1 O10 . . 122.9(4) ? O11 Na1 O10 3_777 . 86.1(3) ? O13 Na1 O10 . . 71.9(3) ? O8 Na1 O10 . . 76.7(3) ? O14 Na1 O19 . . 81.6(5) ? O11 Na1 O19 3_777 . 96.5(5) ? O13 Na1 O19 . . 103.4(5) ? O8 Na1 O19 . . 78.9(5) ? O10 Na1 O19 . . 155.1(5) ? O14 Na1 S3 . . 144.9(4) ? O11 Na1 S3 3_777 . 105.6(3) ? O13 Na1 S3 . . 74.0(2) ? O8 Na1 S3 . . 22.4(2) ? O10 Na1 S3 . . 87.3(2) ? O19 Na1 S3 . . 68.2(4) ? O14 Na1 Na2 . . 149.5(3) ? O11 Na1 Na2 3_777 . 59.9(2) ? O13 Na1 Na2 . . 102.3(3) ? O8 Na1 Na2 . . 43.6(2) ? O10 Na1 Na2 . . 45.5(2) ? O19 Na1 Na2 . . 115.6(5) ? S3 Na1 Na2 . . 64.19(13) ? O14 Na1 Na3 . . 135.1(3) ? O11 Na1 Na3 3_777 . 119.8(3) ? O13 Na1 Na3 . . 41.4(2) ? O8 Na1 Na3 . . 58.8(3) ? O10 Na1 Na3 . . 42.69(19) ? O19 Na1 Na3 . . 118.1(5) ? S3 Na1 Na3 . . 55.40(11) ? Na2 Na1 Na3 . . 61.03(14) ? O14 Na1 Na2 . 3_777 74.2(3) ? O11 Na1 Na2 3_777 3_777 36.7(2) ? O13 Na1 Na2 . 3_777 131.3(3) ? O8 Na1 Na2 . 3_777 114.6(3) ? O10 Na1 Na2 . 3_777 73.6(2) ? O19 Na1 Na2 . 3_777 121.8(5) ? S3 Na1 Na2 . 3_777 136.95(17) ? Na2 Na1 Na2 . 3_777 75.31(16) ? Na3 Na1 Na2 . 3_777 116.3(2) ? O3 Na2 O12 . 3_777 121.2(4) ? O3 Na2 O8 . . 110.6(4) ? O12 Na2 O8 3_777 . 96.9(4) ? O3 Na2 O10 . . 108.2(4) ? O12 Na2 O10 3_777 . 126.5(3) ? O8 Na2 O10 . . 82.9(3) ? O3 Na2 O11 . . 109.6(4) ? O12 Na2 O11 3_777 . 85.3(3) ? O8 Na2 O11 . . 130.9(3) ? O10 Na2 O11 . . 58.5(3) ? O3 Na2 S4 . . 114.3(3) ? O12 Na2 S4 3_777 . 105.5(3) ? O8 Na2 S4 . . 106.3(3) ? O10 Na2 S4 . . 29.20(19) ? O11 Na2 S4 . . 29.45(19) ? O3 Na2 S4 . 3_777 146.1(3) ? O12 Na2 S4 3_777 3_777 25.5(2) ? O8 Na2 S4 . 3_777 88.0(3) ? O10 Na2 S4 . 3_777 101.8(2) ? O11 Na2 S4 . 3_777 73.4(2) ? S4 Na2 S4 . 3_777 85.30(14) ? O3 Na2 S1 . . 21.3(3) ? O12 Na2 S1 3_777 . 142.1(3) ? O8 Na2 S1 . . 104.4(3) ? O10 Na2 S1 . . 87.5(2) ? O11 Na2 S1 . . 102.9(3) ? S4 Na2 S1 . . 98.20(15) ? S4 Na2 S1 3_777 . 165.49(19) ? O3 Na2 Na1 . . 143.8(3) ? O12 Na2 Na1 3_777 . 91.8(3) ? O8 Na2 Na1 . . 45.2(2) ? O10 Na2 Na1 . . 51.4(2) ? O11 Na2 Na1 . . 85.8(2) ? S4 Na2 Na1 . . 64.44(15) ? S4 Na2 Na1 3_777 . 68.87(14) ? S1 Na2 Na1 . . 125.34(17) ? O3 Na2 Na3 . . 83.1(3) ? O12 Na2 Na3 3_777 . 152.4(3) ? O8 Na2 Na3 . . 59.6(2) ? O10 Na2 Na3 . . 43.0(2) ? O11 Na2 Na3 . . 99.3(2) ? S4 Na2 Na3 . . 71.43(12) ? S4 Na2 Na3 3_777 . 130.50(18) ? S1 Na2 Na3 . . 63.62(12) ? Na1 Na2 Na3 . . 61.72(14) ? O3 Na2 Na1 . 3_777 106.0(3) ? O12 Na2 Na1 3_777 3_777 56.8(2) ? O8 Na2 Na1 . 3_777 142.8(3) ? O10 Na2 Na1 . 3_777 92.5(2) ? O11 Na2 Na1 . 3_777 34.44(19) ? S4 Na2 Na1 . 3_777 63.33(12) ? S4 Na2 Na1 3_777 3_777 56.71(13) ? S1 Na2 Na1 . 3_777 112.34(18) ? Na1 Na2 Na1 . 3_777 104.68(16) ? Na3 Na2 Na1 . 3_777 133.62(16) ? O5 Na3 O2 . . 98.2(4) ? O5 Na3 O13 . . 96.8(3) ? O2 Na3 O13 . . 160.9(4) ? O5 Na3 O7 . . 109.4(3) ? O2 Na3 O7 . . 96.2(3) ? O13 Na3 O7 . . 89.8(3) ? O5 Na3 O10 . . 131.2(3) ? O2 Na3 O10 . . 84.8(4) ? O13 Na3 O10 . . 76.4(3) ? O7 Na3 O10 . . 118.7(3) ? O5 Na3 S3 . . 130.8(3) ? O2 Na3 S3 . . 102.1(3) ? O13 Na3 S3 . . 76.5(2) ? O7 Na3 S3 . . 24.6(2) ? O10 Na3 S3 . . 95.1(2) ? O5 Na3 Na2 . . 161.5(3) ? O2 Na3 Na2 . . 65.2(3) ? O13 Na3 Na2 . . 98.0(2) ? O7 Na3 Na2 . . 81.7(2) ? O10 Na3 Na2 . . 43.5(2) ? S3 Na3 Na2 . . 64.00(12) ? O5 Na3 Na1 . . 137.0(3) ? O2 Na3 Na1 . . 122.0(4) ? O13 Na3 Na1 . . 40.8(2) ? O7 Na3 Na1 . . 82.7(3) ? O10 Na3 Na1 . . 48.7(2) ? S3 Na3 Na1 . . 59.10(14) ? Na2 Na3 Na1 . . 57.25(13) ? S1 O2 Na3 . . 147.2(8) ? S1 O3 Na2 . . 124.2(7) ? S2 O5 Na3 . . 173.3(5) ? S3 O7 Na3 . . 112.1(5) ? S3 O8 Na2 . . 141.0(6) ? S3 O8 Na1 . . 118.3(5) ? Na2 O8 Na1 . . 91.2(3) ? S4 O10 Na3 . . 162.0(5) ? S4 O10 Na2 . . 95.9(4) ? Na3 O10 Na2 . . 93.5(3) ? S4 O10 Na1 . . 107.8(4) ? Na3 O10 Na1 . . 88.6(3) ? Na2 O10 Na1 . . 83.1(3) ? S4 O11 Na1 . 3_777 152.6(5) ? S4 O11 Na2 . . 94.5(4) ? Na1 O11 Na2 3_777 . 108.9(3) ? S4 O12 Na2 . 3_777 111.9(4) ? S5 O13 Na1 . . 130.4(5) ? S5 O13 Na3 . . 128.5(5) ? Na1 O13 Na3 . . 97.8(3) ? S6A O14 Na1 . . 126.4(7) ? O1 S1 O2 . . 114.0(6) ? O1 S1 O3 . . 111.6(6) ? O2 S1 O3 . . 113.0(7) ? O1 S1 C7 . . 106.3(6) ? O2 S1 C7 . . 106.7(6) ? O3 S1 C7 . . 104.5(5) ? O1 S1 Na2 . . 121.5(4) ? O2 S1 Na2 . . 79.5(5) ? O3 S1 Na2 . . 34.5(5) ? C7 S1 Na2 . . 124.5(4) ? O4 S2 O5 . . 113.4(5) ? O4 S2 O6 . . 113.2(6) ? O5 S2 O6 . . 113.0(6) ? O4 S2 C20 . . 105.9(6) ? O5 S2 C20 . . 105.1(5) ? O6 S2 C20 . . 105.3(5) ? O9 S3 O8 . . 113.8(6) ? O9 S3 O7 . . 113.1(5) ? O8 S3 O7 . . 112.1(5) ? O9 S3 C34 . . 106.4(5) ? O8 S3 C34 . . 105.5(5) ? O7 S3 C34 . . 105.1(5) ? O9 S3 Na3 . . 117.7(4) ? O8 S3 Na3 . . 72.1(4) ? O7 S3 Na3 . . 43.3(4) ? C34 S3 Na3 . . 132.9(4) ? O9 S3 Na1 . . 82.5(4) ? O8 S3 Na1 . . 39.3(3) ? O7 S3 Na1 . . 106.8(4) ? C34 S3 Na1 . . 140.0(4) ? Na3 S3 Na1 . . 65.50(15) ? O12 S4 O10 . . 112.8(5) ? O12 S4 O11 . . 112.9(5) ? O10 S4 O11 . . 110.5(5) ? O12 S4 C46 . . 106.4(5) ? O10 S4 C46 . . 108.0(5) ? O11 S4 C46 . . 105.8(5) ? O12 S4 Na2 . . 126.7(3) ? O10 S4 Na2 . . 54.9(3) ? O11 S4 Na2 . . 56.1(3) ? C46 S4 Na2 . . 126.9(4) ? O12 S4 Na2 . 3_777 42.6(3) ? O10 S4 Na2 . 3_777 120.7(4) ? O11 S4 Na2 . 3_777 71.6(4) ? C46 S4 Na2 . 3_777 129.1(4) ? Na2 S4 Na2 . 3_777 94.69(14) ? O13 S5 C56 . . 105.7(6) ? O13 S5 C55 . . 106.4(6) ? C56 S5 C55 . . 98.6(7) ? O16 S7 C59 . . 110.9(10) ? O16 S7 C60 . . 111.1(11) ? C59 S7 C60 . . 102.6(9) ? O17 S8 C61 . . 111.5(11) ? O17 S8 C62 . . 108.9(11) ? C61 S8 C62 . . 102.9(11) ? O14 S6A C57 . . 107.0(9) ? O14 S6A C58 . . 105.4(9) ? C57 S6A C58 . . 98.0(15) ? O18 S9A C64 . . 116.5(10) ? O18 S9A C63 . . 110.2(8) ? C64 S9A C63 . . 100.7(9) ? # start Validation Reply Form _vrf_PLAT222_ALERT_3_A ; PROBLEM: Large Non-Solvent H Uiso(max)/Uiso(min) .. 10.0 Ratio RESPONSE: This alert is due to the disorder found in the methyl groups present in the DMSO molecules, as well as some of the CH3 substituents in the ligand. ; # end Validation Reply Form #===END #----------------------------------------------------------------------------# #----------------------------------------------------------------------------# # COMPOUND 4 OF 5 # #----------------------------------------------------------------------------# #----------------------------------------------------------------------------# data_3e #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_method 'APEX2 v2010.9-1' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ? _chemical_name_common 'Na[Ag(NHC)Cl].2SOMe2' _chemical_formula_moiety ? _chemical_formula_sum 'C31 H49 Ag Cl N2 Na2 O8 S4' _chemical_formula_weight 895.26 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.2882(3) _cell_length_b 14.4724(4) _cell_length_c 31.0300(9) _cell_angle_alpha 90 _cell_angle_beta 91.9910(10) _cell_angle_gamma 90 _cell_volume 4617.4(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 296.(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prismatic _exptl_crystal_colour 'clear pale yellow' _exptl_crystal_size_max 0.370 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.288 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1852 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.735 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_absorpt_correction_T_min 0.77 _exptl_absorpt_correction_T_max 0.93 _exptl_special_details ; ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 296.(2) _diffrn_source ? _diffrn_source_type ? _diffrn_radiation_type ? _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 67891 _diffrn_reflns_av_R_equivalents 0.0801 _diffrn_reflns_av_sigmaI/netI 0.0579 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 25.39 _diffrn_reflns_theta_full 25.39 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measured_fraction_theta_full 0.985 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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. ; _reflns_number_total 8389 _reflns_number_gt 4984 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.1390 _refine_ls_R_factor_gt 0.0822 _refine_ls_wR_factor_gt 0.2467 _refine_ls_wR_factor_ref 0.2975 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.131 _refine_ls_number_reflns 8389 _refine_ls_number_parameters 487 _refine_ls_number_restraints 28 _refine_ls_hydrogen_treatment refxyz _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1646P)^2^+5.8423P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.353 _refine_diff_density_min -0.969 _refine_ls_extinction_method none _refine_ls_extinction_coef ? #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag1 0.33509(7) 0.14813(4) 0.758533(19) 0.0668(3) Uani d . 1.0 . . C C1 0.2429(7) 0.0412(5) 0.7260(2) 0.0442(16) Uani d . 1.0 . . C C2 0.1282(9) -0.0886(6) 0.7147(2) 0.065(2) Uani d . 1.0 . . H H2 0.0798 -0.1415 0.7201 0.078 Uiso calc R 1.0 . . C C3 0.1630(9) -0.0568(6) 0.6757(3) 0.064(2) Uani d . 1.0 . . H H3 0.1429 -0.0832 0.649 0.077 Uiso calc R 1.0 . . C C4 0.2807(8) 0.0834(5) 0.6509(2) 0.0467(18) Uani d . 1.0 . . C C5 0.1965(8) 0.1543(5) 0.6364(2) 0.0501(18) Uani d . 1.0 . . C C6 0.2413(8) 0.2140(5) 0.6045(2) 0.0545(19) Uani d . 1.0 . . H H6 0.1885 0.2614 0.5937 0.065 Uiso calc R 1.0 . . C C7 0.3640(8) 0.2016(5) 0.5893(2) 0.0507(18) Uani d . 1.0 . . C C8 0.4469(8) 0.1318(5) 0.6044(3) 0.0551(19) Uani d . 1.0 . . H H8 0.5303 0.1267 0.5939 0.066 Uiso calc R 1.0 . . C C9 0.4049(8) 0.0699(5) 0.6351(2) 0.0489(18) Uani d . 1.0 . . C C10 0.4908(8) -0.0091(6) 0.6511(3) 0.061(2) Uani d . 1.0 . . H H10 0.4351 -0.0516 0.6667 0.073 Uiso calc R 1.0 . . C C11 0.5508(16) -0.0630(11) 0.6164(5) 0.140(3) Uani d . 1.0 . . H H11A 0.5351 -0.1277 0.6209 0.211 Uiso calc R 1.0 . . H H11B 0.6428 -0.0518 0.617 0.211 Uiso calc R 1.0 . . H H11C 0.5134 -0.0446 0.589 0.211 Uiso calc R 1.0 . . C C12 0.5929(16) 0.0249(11) 0.6828(5) 0.140(3) Uani d . 1.0 . . H H12A 0.6499 -0.0251 0.691 0.211 Uiso calc R 1.0 . . H H12B 0.5521 0.0484 0.708 0.211 Uiso calc R 1.0 . . H H12C 0.6422 0.0733 0.6699 0.211 Uiso calc R 1.0 . . C C13 0.0612(10) 0.1682(7) 0.6537(3) 0.077(3) Uani d . 1.0 . . H H13 0.0469 0.1206 0.6755 0.092 Uiso calc R 1.0 . . C C14 0.0530(17) 0.2638(11) 0.6757(5) 0.140(3) Uani d . 1.0 . . H H14A 0.1277 0.2724 0.6947 0.211 Uiso calc R 1.0 . . H H14B -0.0246 0.2668 0.692 0.211 Uiso calc R 1.0 . . H H14C 0.0507 0.3114 0.6542 0.211 Uiso calc R 1.0 . . C C15 -0.0470(17) 0.1587(10) 0.6178(5) 0.140(3) Uani d . 1.0 . . H H15A -0.0398 0.2085 0.5976 0.211 Uiso calc R 1.0 . . H H15B -0.1306 0.161 0.6305 0.211 Uiso calc R 1.0 . . H H15C -0.0373 0.1009 0.6032 0.211 Uiso calc R 1.0 . . C C16 0.1576(7) -0.0353(5) 0.7907(2) 0.0450(17) Uani d . 1.0 . . C C17 0.0461(8) 0.0069(5) 0.8062(2) 0.0512(18) Uani d . 1.0 . . C C18 0.9710(7) 0.5021(5) 0.6498(2) 0.0510(18) Uani d . 1.0 . . H H18 1.0439 0.5292 0.6382 0.061 Uiso calc R 1.0 . . C C19 0.8812(7) 0.4574(5) 0.6227(2) 0.0421(16) Uani d . 1.0 . . C C20 0.7713(7) 0.4180(5) 0.6386(2) 0.0497(18) Uani d . 1.0 . . H H20 0.7114 0.3892 0.62 0.06 Uiso calc R 1.0 . . C C21 0.2510(7) -0.0790(5) 0.8168(2) 0.0447(17) Uani d . 1.0 . . C C22 -0.0540(10) 0.0571(7) 0.7783(3) 0.078(3) Uani d . 1.0 . . H H22 -0.0269 0.0496 0.7485 0.093 Uiso calc R 1.0 . . C C23 -0.1880(13) 0.0093(12) 0.7806(6) 0.153(7) Uani d . 1.0 . . H H23A -0.2076 -0.0013 0.8102 0.23 Uiso calc R 1.0 . . H H23B -0.1859 -0.0487 0.7656 0.23 Uiso calc R 1.0 . . H H23C -0.2537 0.0482 0.7674 0.23 Uiso calc R 1.0 . . C C24 -0.0510(16) 0.1596(8) 0.7873(5) 0.127(5) Uani d . 1.0 . . H H24A 0.0351 0.1829 0.7831 0.19 Uiso calc R 1.0 . . H H24B -0.0747 0.1706 0.8165 0.19 Uiso calc R 1.0 . . H H24C -0.1115 0.1905 0.7679 0.19 Uiso calc R 1.0 . . C C25 0.3716(8) -0.1266(6) 0.7991(3) 0.058(2) Uani d . 1.0 . . H H25 0.3676 -0.1199 0.7677 0.07 Uiso calc R 1.0 . . C C26 0.3714(12) -0.2303(8) 0.8095(4) 0.100(4) Uani d . 1.0 . . H H26A 0.3915 -0.2391 0.8397 0.15 Uiso calc R 1.0 . . H H26B 0.4356 -0.2609 0.7929 0.15 Uiso calc R 1.0 . . H H26C 0.2872 -0.2556 0.8025 0.15 Uiso calc R 1.0 . . C C27 0.4931(10) -0.0799(10) 0.8158(4) 0.116(5) Uani d . 1.0 . . H H27A 0.4992 -0.0852 0.8467 0.174 Uiso calc R 1.0 . . H H27B 0.4907 -0.0158 0.8079 0.174 Uiso calc R 1.0 . . H H27C 0.5673 -0.1088 0.8036 0.174 Uiso calc R 1.0 . . Cl Cl1 0.4383(5) 0.2619(3) 0.79843(11) 0.1489(18) Uani d . 1.0 . . N N1 0.2335(6) 0.0219(4) 0.68349(17) 0.0477(15) Uani d . 1.0 . . N N2 0.1776(6) -0.0286(4) 0.74444(16) 0.0465(15) Uani d . 1.0 . . Na Na1 0.7844(3) 0.5318(3) 0.47591(10) 0.0687(9) Uani d . 1.0 . . Na Na2 0.7114(5) 0.2941(3) 0.51771(13) 0.0910(12) Uani d . 1.0 A . O O1 0.3308(9) 0.3471(7) 0.5423(4) 0.155(5) Uani d . 1.0 . . O O2 0.4452(13) 0.2249(7) 0.5115(2) 0.144(4) Uani d . 1.0 . . O O3 0.5452(8) 0.3140(7) 0.5657(3) 0.125(3) Uani d . 1.0 . . O O4 1.0404(8) 0.4739(10) 0.5623(2) 0.170(6) Uani d . 1.0 . . O O5 0.8190(8) 0.5073(6) 0.5460(2) 0.1083(19) Uani d . 1.0 A . O O6 0.8882(11) 0.3567(5) 0.5551(2) 0.120(3) Uani d . 1.0 . . O O9 1.018(3) 0.833(2) 0.5965(6) 0.224(17) Uani d P 0.5 . . S S1 0.4233(2) 0.27908(16) 0.54903(7) 0.0632(6) Uani d . 1.0 A . S S2 0.91138(19) 0.44836(15) 0.56688(6) 0.0533(5) Uani d . 1.0 A . O O7 0.6820(8) 0.3926(7) 0.4585(2) 0.1083(19) Uani d . 1.0 A . S S3A 0.6301(5) 0.3957(5) 0.41179(16) 0.094(3) Uani d P 0.637(14) A 1 C C29A 0.631(5) 0.283(2) 0.3982(12) 0.214(19) Uani d PU 0.637(14) A 1 C C28 0.4625(12) 0.4128(11) 0.4176(5) 0.124(4) Uani d . 1.0 A 1 S S3B 0.5954(8) 0.3360(7) 0.4256(3) 0.078(4) Uani d P 0.363(14) A 2 C C29B 0.683(4) 0.369(5) 0.3787(9) 0.16(2) Uani d PU 0.363(14) A 2 S S4A 0.7251(8) 0.0711(5) 0.4761(4) 0.077(4) Uani d PD 0.319(11) A 3 C C30 0.8387(19) -0.0043(13) 0.4629(7) 0.107(9) Uani d PDU 0.5 A 3 C C31 0.632(3) 0.008(2) 0.5080(11) 0.166(15) Uani d PDU 0.5 A 3 S S4B 0.781(3) 0.0604(13) 0.5043(6) 0.141(13) Uani d PD 0.181(11) A 4 O O8 0.7795(13) 0.1498(8) 0.5013(6) 0.102(6) Uani d P 0.5 . . S S5 0.9499(9) 0.7909(8) 0.5821(3) 0.158(4) Uani d P 0.5 . . C C32 0.947(3) 0.743(2) 0.5305(9) 0.124(4) Uani d P 0.5 . . H H32A 1.0082 0.7741 0.5132 0.185 Uiso calc PR 0.5 . . H H32B 0.861 0.7489 0.5176 0.185 Uiso calc PR 0.5 . . H H32C 0.9691 0.6783 0.5325 0.185 Uiso calc PR 0.5 . . C C33 0.822(2) 0.7351(17) 0.6053(7) 0.098(7) Uani d P 0.5 . . H H33A 0.8334 0.7369 0.6362 0.148 Uiso calc PR 0.5 . . H H33B 0.8189 0.672 0.5959 0.148 Uiso calc PR 0.5 . . H H33C 0.7418 0.7654 0.597 0.148 Uiso calc PR 0.5 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ag1 0.1066(6) 0.0504(4) 0.0436(4) -0.0277(3) 0.0045(3) -0.0077(3) C1 0.064(5) 0.038(4) 0.031(3) -0.008(3) 0.000(3) 0.003(3) C2 0.111(7) 0.047(5) 0.036(4) -0.036(5) -0.008(4) 0.002(3) C3 0.097(6) 0.049(5) 0.045(5) -0.022(5) -0.005(4) -0.007(4) C4 0.076(5) 0.034(4) 0.030(4) -0.009(3) -0.005(3) -0.001(3) C5 0.064(5) 0.044(4) 0.044(4) 0.003(4) 0.010(3) 0.003(3) C6 0.066(5) 0.047(5) 0.051(4) 0.008(4) 0.006(4) 0.012(4) C7 0.062(5) 0.045(4) 0.045(4) -0.005(4) -0.003(3) 0.013(3) C8 0.064(5) 0.048(5) 0.053(5) 0.000(4) 0.000(4) 0.006(4) C9 0.069(5) 0.038(4) 0.040(4) 0.000(3) -0.005(3) 0.004(3) C10 0.070(5) 0.054(5) 0.059(5) 0.011(4) 0.001(4) 0.014(4) C11 0.168(7) 0.127(6) 0.126(6) 0.070(6) 0.000(5) 0.012(5) C12 0.168(7) 0.127(6) 0.126(6) 0.070(6) 0.000(5) 0.012(5) C13 0.086(7) 0.072(6) 0.073(6) 0.012(5) 0.025(5) 0.031(5) C14 0.168(7) 0.127(6) 0.126(6) 0.070(6) 0.000(5) 0.012(5) C15 0.168(7) 0.127(6) 0.126(6) 0.070(6) 0.000(5) 0.012(5) C16 0.059(5) 0.042(4) 0.034(4) -0.008(3) 0.000(3) 0.005(3) C17 0.060(5) 0.050(5) 0.043(4) -0.001(4) -0.004(3) 0.006(3) C18 0.049(4) 0.047(4) 0.057(5) 0.004(3) 0.005(3) 0.005(4) C19 0.047(4) 0.044(4) 0.035(4) 0.002(3) 0.005(3) -0.004(3) C20 0.058(5) 0.055(5) 0.036(4) 0.001(4) 0.007(3) -0.004(3) C21 0.055(4) 0.042(4) 0.037(4) -0.006(3) 0.009(3) 0.000(3) C22 0.085(7) 0.083(7) 0.065(6) 0.013(5) -0.005(5) 0.018(5) C23 0.105(10) 0.159(15) 0.192(16) -0.027(9) -0.068(10) 0.080(13) C24 0.167(13) 0.086(9) 0.125(11) 0.050(9) -0.033(10) 0.022(8) C25 0.066(5) 0.066(5) 0.045(4) 0.008(4) 0.017(4) 0.009(4) C26 0.109(9) 0.071(7) 0.123(10) 0.021(6) 0.048(7) -0.002(6) C27 0.059(7) 0.154(13) 0.137(11) -0.017(7) 0.036(6) -0.025(9) Cl1 0.249(5) 0.112(3) 0.085(2) -0.099(3) -0.005(2) -0.0338(19) N1 0.079(4) 0.036(3) 0.028(3) -0.009(3) -0.001(3) 0.001(2) N2 0.077(4) 0.033(3) 0.029(3) -0.009(3) 0.002(3) 0.003(2) Na1 0.079(2) 0.078(2) 0.0503(18) 0.0007(18) 0.0143(15) 0.0107(16) Na2 0.122(3) 0.072(3) 0.079(3) 0.005(2) 0.011(2) -0.010(2) O1 0.112(7) 0.136(8) 0.221(11) 0.046(6) 0.069(7) 0.134(8) O2 0.259(12) 0.115(7) 0.059(5) -0.024(7) 0.040(6) 0.012(5) O3 0.110(6) 0.165(8) 0.099(6) -0.080(6) -0.018(5) 0.057(6) O4 0.094(6) 0.354(17) 0.064(5) -0.091(8) 0.039(4) -0.040(7) O5 0.131(5) 0.139(5) 0.055(3) 0.038(4) -0.001(3) 0.011(3) O6 0.213(10) 0.092(6) 0.057(4) -0.024(6) 0.041(5) -0.024(4) O9 0.27(3) 0.31(4) 0.090(13) -0.20(3) 0.081(17) -0.120(19) S1 0.0679(14) 0.0602(13) 0.0613(13) -0.0062(11) 0.0010(10) 0.0260(11) S2 0.0555(12) 0.0691(14) 0.0356(10) 0.0016(10) 0.0070(8) -0.0003(9) O7 0.131(5) 0.139(5) 0.055(3) 0.038(4) -0.001(3) 0.011(3) S3A 0.089(3) 0.118(5) 0.072(3) -0.027(3) -0.015(2) 0.020(3) C29A 0.36(5) 0.13(2) 0.14(3) 0.00(3) -0.11(3) -0.06(2) C28 0.084(7) 0.135(11) 0.151(11) -0.009(7) -0.015(7) 0.009(9) S3B 0.091(5) 0.083(7) 0.059(5) -0.036(4) -0.006(4) 0.007(4) C29B 0.11(3) 0.36(7) 0.020(14) -0.06(3) 0.013(15) 0.01(2) S4A 0.076(6) 0.048(4) 0.105(9) 0.000(3) -0.028(5) -0.008(4) C30 0.136(19) 0.096(16) 0.091(15) -0.060(15) 0.038(13) -0.062(13) C31 0.22(4) 0.13(3) 0.15(3) 0.00(3) 0.10(3) -0.03(2) S4B 0.27(3) 0.081(13) 0.071(12) 0.064(16) -0.063(16) -0.050(9) O8 0.069(8) 0.042(7) 0.196(18) -0.001(6) 0.016(9) -0.059(9) S5 0.140(6) 0.222(10) 0.112(6) -0.112(7) 0.034(5) -0.098(7) C32 0.084(7) 0.135(11) 0.151(11) -0.009(7) -0.015(7) 0.009(9) C33 0.122(18) 0.093(16) 0.083(15) 0.010(14) 0.037(13) 0.014(12) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ag1 C1 . 2.061(7) ? Ag1 Cl1 . 2.298(3) ? C1 N1 . 1.347(8) ? C1 N2 . 1.352(9) ? C2 C3 . 1.355(11) ? C2 N2 . 1.353(9) ? C3 N1 . 1.367(10) ? C4 C9 . 1.398(11) ? C4 C5 . 1.407(10) ? C4 N1 . 1.445(9) ? C5 C6 . 1.403(10) ? C5 C13 . 1.523(12) ? C6 C7 . 1.374(11) ? C7 C8 . 1.393(11) ? C7 S1 . 1.802(7) ? C8 C9 . 1.387(11) ? C9 C10 . 1.517(11) ? C10 C11 . 1.481(16) ? C10 C12 . 1.498(18) ? C13 C14 . 1.547(18) ? C13 C15 . 1.552(19) ? C16 C17 . 1.400(11) ? C16 C21 . 1.388(10) ? C16 N2 . 1.459(8) ? C17 C18 2_646 1.383(10) ? C17 C22 . 1.510(12) ? C18 C17 2_656 1.383(10) ? C18 C19 . 1.387(10) ? C19 C20 . 1.373(10) ? C19 S2 . 1.775(7) ? C20 C21 2_656 1.409(9) ? C21 C20 2_646 1.409(9) ? C21 C25 . 1.537(11) ? C22 C24 . 1.510(15) ? C22 C23 . 1.546(17) ? C25 C27 . 1.497(14) ? C25 C26 . 1.535(13) ? Na1 O1 3_666 2.179(8) ? Na1 O4 3_766 2.193(8) ? Na1 O5 . 2.221(7) ? Na1 O7 . 2.327(11) ? Na1 S3A . 3.184(7) ? Na1 S2 . 3.298(4) ? Na1 Na2 . 3.761(6) ? Na2 O8 . 2.266(11) ? Na2 O6 . 2.308(11) ? Na2 O3 . 2.324(11) ? Na2 O7 . 2.337(8) ? Na2 O2 . 2.916(13) ? Na2 S3B . 3.119(9) ? Na2 S1 . 3.158(5) ? Na2 S2 . 3.366(5) ? O1 S1 . 1.381(8) ? O1 Na1 3_666 2.179(8) ? O2 S1 . 1.428(9) ? O3 S1 . 1.431(8) ? O4 S2 . 1.390(8) ? O4 Na1 3_766 2.193(8) ? O5 S2 . 1.416(8) ? O6 S2 . 1.394(8) ? O9 S5 . 1.02(2) ? O7 S3A . 1.528(8) ? O7 S3B . 1.565(11) ? S3A C29A . 1.69(3) ? S3A C28 . 1.758(14) ? S3B C29B . 1.80(3) ? S4A O8 . 1.480(15) ? S4A C31 . 1.667(17) ? S4A C30 . 1.661(16) ? S4B O8 . 1.30(2) ? S5 C32 . 1.75(3) ? S5 C33 . 1.72(2) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 Ag1 Cl1 . . 176.6(2) ? N1 C1 N2 . . 103.9(6) ? N1 C1 Ag1 . . 130.7(5) ? N2 C1 Ag1 . . 125.4(5) ? C3 C2 N2 . . 106.6(7) ? C2 C3 N1 . . 106.3(7) ? C9 C4 C5 . . 123.3(6) ? C9 C4 N1 . . 119.6(6) ? C5 C4 N1 . . 117.1(7) ? C6 C5 C4 . . 117.5(7) ? C6 C5 C13 . . 119.6(7) ? C4 C5 C13 . . 123.0(7) ? C7 C6 C5 . . 119.3(7) ? C6 C7 C8 . . 122.6(7) ? C6 C7 S1 . . 119.6(6) ? C8 C7 S1 . . 117.8(6) ? C7 C8 C9 . . 119.8(8) ? C8 C9 C4 . . 117.5(7) ? C8 C9 C10 . . 121.3(7) ? C4 C9 C10 . . 121.3(7) ? C11 C10 C12 . . 110.5(11) ? C11 C10 C9 . . 114.3(8) ? C12 C10 C9 . . 110.8(8) ? C5 C13 C14 . . 109.8(10) ? C5 C13 C15 . . 112.2(9) ? C14 C13 C15 . . 110.3(9) ? C17 C16 C21 . . 123.7(6) ? C17 C16 N2 . . 117.1(6) ? C21 C16 N2 . . 119.1(6) ? C18 C17 C16 2_646 . 116.9(7) ? C18 C17 C22 2_646 . 118.9(7) ? C16 C17 C22 . . 124.2(7) ? C17 C18 C19 2_656 . 121.1(7) ? C20 C19 C18 . . 121.0(6) ? C20 C19 S2 . . 119.7(5) ? C18 C19 S2 . . 119.3(5) ? C19 C20 C21 . 2_656 120.3(7) ? C16 C21 C20 . 2_646 117.1(7) ? C16 C21 C25 . . 123.1(6) ? C20 C21 C25 2_646 . 119.8(7) ? C24 C22 C17 . . 110.9(9) ? C24 C22 C23 . . 116.3(12) ? C17 C22 C23 . . 110.5(9) ? C27 C25 C21 . . 110.5(8) ? C27 C25 C26 . . 112.0(10) ? C21 C25 C26 . . 110.8(7) ? C1 N1 C3 . . 111.4(6) ? C1 N1 C4 . . 122.8(6) ? C3 N1 C4 . . 125.4(6) ? C1 N2 C2 . . 111.8(6) ? C1 N2 C16 . . 123.8(6) ? C2 N2 C16 . . 124.3(6) ? O1 Na1 O4 3_666 3_766 109.9(5) ? O1 Na1 O5 3_666 . 116.7(4) ? O4 Na1 O5 3_766 . 114.6(4) ? O1 Na1 O7 3_666 . 113.5(4) ? O4 Na1 O7 3_766 . 102.5(4) ? O5 Na1 O7 . . 98.4(3) ? O1 Na1 S3A 3_666 . 94.6(4) ? O4 Na1 S3A 3_766 . 92.3(3) ? O5 Na1 S3A . . 125.0(3) ? O7 Na1 S3A . . 26.9(2) ? O1 Na1 S2 3_666 . 135.4(4) ? O4 Na1 S2 3_766 . 98.1(3) ? O5 Na1 S2 . . 19.6(2) ? O7 Na1 S2 . . 92.6(2) ? S3A Na1 S2 . . 118.85(17) ? O1 Na1 Na2 3_666 . 135.4(3) ? O4 Na1 Na2 3_766 . 109.3(4) ? O5 Na1 Na2 . . 62.8(3) ? O7 Na1 Na2 . . 36.35(18) ? S3A Na1 Na2 . . 63.16(15) ? S2 Na1 Na2 . . 56.49(9) ? O8 Na2 O6 . . 103.3(5) ? O8 Na2 O3 . . 119.9(5) ? O6 Na2 O3 . . 102.4(3) ? O8 Na2 O7 . . 114.7(6) ? O6 Na2 O7 . . 103.5(3) ? O3 Na2 O7 . . 110.5(3) ? O8 Na2 O2 . . 88.0(4) ? O6 Na2 O2 . . 152.8(3) ? O3 Na2 O2 . . 51.3(3) ? O7 Na2 O2 . . 93.6(3) ? O8 Na2 S3B . . 94.9(5) ? O6 Na2 S3B . . 130.8(3) ? O3 Na2 S3B . . 107.2(3) ? O7 Na2 S3B . . 29.1(3) ? O2 Na2 S3B . . 71.2(3) ? O8 Na2 S1 . . 107.9(4) ? O6 Na2 S1 . . 127.2(3) ? O3 Na2 S1 . . 24.8(2) ? O7 Na2 S1 . . 100.8(3) ? O2 Na2 S1 . . 26.81(18) ? S3B Na2 S1 . . 87.8(2) ? O8 Na2 S2 . . 121.6(4) ? O6 Na2 S2 . . 18.8(2) ? O3 Na2 S2 . . 94.5(2) ? O7 Na2 S2 . . 90.7(3) ? O2 Na2 S2 . . 144.6(2) ? S3B Na2 S2 . . 119.7(2) ? S1 Na2 S2 . . 118.13(13) ? O8 Na2 Na1 . . 134.3(5) ? O6 Na2 Na1 . . 69.6(2) ? O3 Na2 Na1 . . 105.5(3) ? O7 Na2 Na1 . . 36.2(2) ? O2 Na2 Na1 . . 119.3(2) ? S3B Na2 Na1 . . 65.2(2) ? S1 Na2 Na1 . . 111.71(14) ? S2 Na2 Na1 . . 54.79(9) ? S1 O1 Na1 . 3_666 168.2(5) ? S1 O2 Na2 . . 86.1(5) ? S1 O3 Na2 . . 112.3(6) ? S2 O4 Na1 . 3_766 148.3(6) ? S2 O5 Na1 . . 128.8(5) ? S2 O6 Na2 . . 129.1(7) ? O1 S1 O2 . . 113.4(8) ? O1 S1 O3 . . 113.2(7) ? O2 S1 O3 . . 109.1(7) ? O1 S1 C7 . . 107.5(4) ? O2 S1 C7 . . 106.9(5) ? O3 S1 C7 . . 106.5(4) ? O1 S1 Na2 . . 123.6(3) ? O2 S1 Na2 . . 67.1(5) ? O3 S1 Na2 . . 42.9(4) ? C7 S1 Na2 . . 126.9(3) ? O4 S2 O6 . . 112.5(7) ? O4 S2 O5 . . 114.9(7) ? O6 S2 O5 . . 110.3(6) ? O4 S2 C19 . . 106.3(4) ? O6 S2 C19 . . 107.0(4) ? O5 S2 C19 . . 105.3(4) ? O4 S2 Na1 . . 99.6(5) ? O6 S2 Na1 . . 93.7(4) ? O5 S2 Na1 . . 31.7(3) ? C19 S2 Na1 . . 137.0(2) ? O4 S2 Na2 . . 134.5(5) ? O6 S2 Na2 . . 32.2(5) ? O5 S2 Na2 . . 78.6(4) ? C19 S2 Na2 . . 111.5(3) ? Na1 S2 Na2 . . 68.71(10) ? S3A O7 S3B . . 39.0(4) ? S3A O7 Na1 . . 109.6(5) ? S3B O7 Na1 . . 148.0(6) ? S3A O7 Na2 . . 142.6(7) ? S3B O7 Na2 . . 104.4(6) ? Na1 O7 Na2 . . 107.5(3) ? O7 S3A C29A . . 101.8(12) ? O7 S3A C28 . . 102.6(7) ? C29A S3A C28 . . 100.1(19) ? O7 S3A Na1 . . 43.5(4) ? C29A S3A Na1 . . 138.5(12) ? C28 S3A Na1 . . 108.5(6) ? O7 S3B C29B . . 95.6(16) ? O7 S3B Na2 . . 46.5(4) ? C29B S3B Na2 . . 127.3(13) ? O8 S4A C31 . . 108.7(15) ? O8 S4A C30 . . 112.3(9) ? C31 S4A C30 . . 102.2(15) ? S4B O8 S4A . . 43.5(9) ? S4B O8 Na2 . . 155.1(15) ? S4A O8 Na2 . . 135.5(9) ? O9 S5 C32 . . 129.3(15) ? O9 S5 C33 . . 128.2(15) ? C32 S5 C33 . . 101.9(13) ? #===END #----------------------------------------------------------------------------# #----------------------------------------------------------------------------# # COMPOUND 5 OF 5 # #----------------------------------------------------------------------------# #----------------------------------------------------------------------------# data_4a #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_method 'APEX2 v2010.9-1' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ? _chemical_name_common 'Na[Pt(NHC)Cl2(dmso)].3H2O' _chemical_formula_moiety ? _chemical_formula_sum 'C22 H40 Cl4 N4 Na4 O20 Pt2 S6' _chemical_formula_iupac ? _chemical_formula_weight 1496.88 _chemical_compound_source 'synthesis as described' _chemical_melting_point ? #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _space_group_crystal_system triclinic _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2265(2) _cell_length_b 10.4402(2) _cell_length_c 16.4703(4) _cell_angle_alpha 96.1470(10) _cell_angle_beta 93.5040(10) _cell_angle_gamma 95.0300(10) _cell_volume 1397.47(5) _cell_formula_units_Z 1 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 293.(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prismatic _exptl_crystal_colour ? _exptl_crystal_size_max 0.270 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.120 _exptl_crystal_density_diffrn 1.779 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.508 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_absorpt_correction_T_min 0.35 _exptl_absorpt_correction_T_max 0.56 _exptl_special_details ; ; _diffrn_ambient_temperature 293.(2) #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source ? _diffrn_source_type ? _diffrn_radiation_type ? _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 35550 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.0217 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 25.35 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measured_fraction_theta_full 0.986 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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. ; _reflns_number_total 5064 _reflns_number_gt 4933 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0906 _refine_ls_R_factor_gt 0.0849 _refine_ls_wR_factor_gt 0.2411 _refine_ls_wR_factor_ref 0.2560 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _refine_ls_number_reflns 5064 _refine_ls_number_parameters 262 _refine_ls_number_restraints 4 _refine_ls_hydrogen_treatment refxyz _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1482P)^2^+65.3091P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.082 _refine_ls_shift/su_mean 0.002 _refine_diff_density_max 7.466 _refine_diff_density_min -6.153 _refine_ls_extinction_method none _refine_ls_extinction_coef ? #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt1 0.50625(6) 0.80879(5) 0.59926(3) 0.0215(3) Uani d . 1.0 . . Cl Cl1 0.2708(5) 0.9225(5) 0.6022(3) 0.0389(10) Uani d . 1.0 A . Cl Cl2 0.3646(6) 0.6413(5) 0.5133(3) 0.0415(11) Uani d . 1.0 A . C C1 0.6976(19) 0.7078(16) 0.5984(9) 0.025(3) Uani d . 1.0 A 1 C C2 0.877(2) 0.5667(17) 0.6255(11) 0.032(4) Uani d . 1.0 A 1 H H2 0.9232 0.4985 0.6473 0.038 Uiso calc R 1.0 A 1 C C3 0.946(2) 0.6432(18) 0.5745(10) 0.031(4) Uani d . 1.0 A 1 H H3 1.049 0.6393 0.5548 0.037 Uiso calc R 1.0 A 1 C C4 0.862(2) 0.8331(16) 0.5051(10) 0.029(3) Uani d . 1.0 A 1 H H4A 0.9439 0.8986 0.5324 0.035 Uiso calc R 1.0 A 1 H H4B 0.7607 0.8732 0.4974 0.035 Uiso calc R 1.0 A 1 C C5 0.918(2) 0.7825(17) 0.4208(11) 0.033(3) Uani d . 1.0 A 1 H H5A 0.9268 0.8531 0.3871 0.039 Uiso calc R 1.0 A 1 H H5B 1.0254 0.7525 0.4283 0.039 Uiso calc R 1.0 A 1 C C6 0.801(2) 0.6730(19) 0.3767(10) 0.036(3) Uani d . 1.0 A 1 H H6A 0.6896 0.6916 0.3847 0.043 Uiso calc R 1.0 A 1 H H6B 0.8191 0.5935 0.4 0.043 Uiso calc R 1.0 A 1 C C7 0.612(2) 0.5462(17) 0.6931(10) 0.033(4) Uani d D 1.0 . . H H7A 0.6396 0.4588 0.6984 0.04 Uiso calc R 1.0 B 1 H H7B 0.5015 0.5412 0.6685 0.04 Uiso calc R 1.0 B 1 C C10 0.650(3) 1.1152(19) 0.6273(15) 0.053(6) Uani d . 1.0 . . H H10A 0.6852 1.1887 0.6665 0.08 Uiso calc R 1.0 A . H H10B 0.5422 1.1238 0.6043 0.08 Uiso calc R 1.0 . . H H10C 0.7243 1.1104 0.5846 0.08 Uiso calc R 1.0 . . C C11 0.548(4) 1.022(3) 0.7658(14) 0.062(7) Uani d . 1.0 . . H H11A 0.581 0.9736 0.8094 0.093 Uiso calc R 1.0 A . H H11B 0.4317 1.0066 0.7542 0.093 Uiso calc R 1.0 . . H H11C 0.5776 1.1124 0.7817 0.093 Uiso calc R 1.0 . . C C8A 0.623(3) 0.624(3) 0.7785(15) 0.033(3) Uani d PD 0.51(2) C 1 H H8A1 0.5644 0.5733 0.8153 0.039 Uiso calc PR 0.51(2) C 1 H H8A2 0.5683 0.7023 0.7746 0.039 Uiso calc PR 0.51(2) C 1 C C9A 0.799(4) 0.662(4) 0.816(2) 0.036(3) Uani d PD 0.51(2) C 1 H H9A1 0.8536 0.7279 0.7867 0.043 Uiso calc PR 0.51(2) C 1 H H9A2 0.8613 0.5879 0.8139 0.043 Uiso calc PR 0.51(2) C 1 C C8B 0.669(4) 0.555(3) 0.7841(13) 0.033(3) Uani d PD 0.49(2) C 2 H H8B1 0.7781 0.5266 0.7903 0.039 Uiso calc PR 0.49(2) C 2 H H8B2 0.5956 0.4988 0.8118 0.039 Uiso calc PR 0.49(2) C 2 C C9B 0.669(5) 0.695(3) 0.821(2) 0.036(3) Uani d PD 0.49(2) C 2 H H9B1 0.5573 0.7162 0.8247 0.043 Uiso calc PR 0.49(2) C 2 H H9B2 0.7222 0.7514 0.7857 0.043 Uiso calc PR 0.49(2) C 2 N N1 0.8357(15) 0.7282(13) 0.5569(8) 0.023(3) Uani d . 1.0 . . N N2 0.7256(16) 0.6076(13) 0.6398(8) 0.023(3) Uani d . 1.0 A . Na Na1 0.782(3) 0.252(2) 0.2354(11) 0.101(6) Uani d P 0.75 . . Na Na2 0.912(3) 0.973(2) 0.1840(14) 0.108(7) Uani d P 0.75 . . Na Na3 0.759(3) 0.278(3) -0.0170(15) 0.085(7) Uani d P 0.5 . . O O1 1.006(3) 0.664(3) 0.2621(11) 0.108(7) Uani d . 1.0 A . O O2 0.757(4) 0.5231(19) 0.2399(11) 0.101(6) Uani d . 1.0 A . O O3 0.750(2) 0.7511(18) 0.2317(13) 0.067(3) Uani d . 1.0 A . O O4 0.929(3) 0.722(3) 0.9317(11) 0.108(7) Uani d . 1.0 . . O O5 0.703(4) 0.630(2) 0.9641(11) 0.101(6) Uani d . 1.0 C . O O6 0.707(2) 0.8440(18) 0.9349(13) 0.067(3) Uani d . 1.0 C . O O7 0.8154(19) 0.9513(15) 0.7020(11) 0.059(4) Uani d . 1.0 . . O O8 0.841(2) 0.1670(17) 0.1041(10) 0.059(4) Uani d . 1.0 . . O O9 0.868(2) 1.0092(19) 0.0528(13) 0.070(5) Uani d . 1.0 . . O O10 0.495(3) 0.293(3) -0.108(2) 0.142(14) Uani d . 1.0 . . S S1 0.8290(9) 0.6509(6) 0.2698(3) 0.0542(11) Uani d . 1.0 . . S S2 0.7718(9) 0.7259(6) 0.9207(3) 0.0542(11) Uani d . 1.0 . . S S3 0.6479(5) 0.9714(4) 0.6767(3) 0.0306(9) Uani d . 1.0 A . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pt1 0.0190(4) 0.0244(4) 0.0219(4) 0.0055(2) 0.0022(2) 0.0026(2) Cl1 0.029(2) 0.042(2) 0.049(3) 0.0169(18) 0.0030(18) 0.0055(19) Cl2 0.030(2) 0.038(2) 0.051(3) 0.0020(17) -0.0059(19) -0.011(2) C1 0.023(8) 0.032(8) 0.020(7) 0.001(6) 0.002(6) 0.003(6) C2 0.029(9) 0.036(9) 0.033(9) 0.016(7) 0.001(7) 0.006(7) C3 0.022(8) 0.041(10) 0.031(8) 0.011(7) 0.006(6) 0.003(7) C4 0.032(8) 0.023(8) 0.033(9) 0.002(6) 0.007(7) 0.004(6) C5 0.034(8) 0.036(8) 0.032(7) 0.006(6) 0.013(6) 0.010(6) C6 0.040(8) 0.045(8) 0.023(7) 0.007(6) 0.005(6) 0.001(6) C7 0.030(9) 0.034(9) 0.036(9) -0.002(7) 0.006(7) 0.011(7) C10 0.069(15) 0.022(9) 0.065(14) -0.009(9) 0.000(11) 0.000(9) C11 0.087(18) 0.060(15) 0.035(11) -0.002(13) 0.018(11) -0.013(10) C8A 0.034(8) 0.036(8) 0.032(7) 0.006(6) 0.013(6) 0.010(6) C9A 0.040(8) 0.045(8) 0.023(7) 0.007(6) 0.005(6) 0.001(6) C8B 0.034(8) 0.036(8) 0.032(7) 0.006(6) 0.013(6) 0.010(6) C9B 0.040(8) 0.045(8) 0.023(7) 0.007(6) 0.005(6) 0.001(6) N1 0.017(6) 0.029(7) 0.023(6) 0.002(5) 0.001(5) 0.003(5) N2 0.025(7) 0.025(7) 0.020(6) -0.001(5) 0.003(5) 0.004(5) Na1 0.141(18) 0.095(13) 0.069(10) 0.008(12) 0.021(11) 0.013(9) Na2 0.115(16) 0.101(14) 0.106(15) -0.007(12) -0.022(12) 0.030(11) Na3 0.079(16) 0.104(19) 0.068(14) -0.010(14) 0.018(12) 0.009(13) O1 0.091(11) 0.21(2) 0.043(7) 0.095(13) 0.030(7) 0.042(10) O2 0.21(2) 0.055(8) 0.037(7) 0.012(10) 0.018(9) -0.006(6) O3 0.059(7) 0.056(7) 0.090(9) 0.019(6) 0.003(7) 0.013(6) O4 0.091(11) 0.21(2) 0.043(7) 0.095(13) 0.030(7) 0.042(10) O5 0.21(2) 0.055(8) 0.037(7) 0.012(10) 0.018(9) -0.006(6) O6 0.059(7) 0.056(7) 0.090(9) 0.019(6) 0.003(7) 0.013(6) O7 0.045(9) 0.046(9) 0.078(11) 0.010(7) -0.027(8) -0.016(8) O8 0.066(11) 0.061(10) 0.048(9) -0.003(8) 0.001(8) 0.001(7) O9 0.057(10) 0.068(12) 0.082(13) 0.016(9) -0.006(9) -0.003(10) O10 0.081(17) 0.17(3) 0.16(3) 0.052(18) -0.061(18) -0.06(2) S1 0.089(3) 0.048(2) 0.0263(17) 0.025(2) -0.0064(17) 0.0001(15) S2 0.089(3) 0.048(2) 0.0263(17) 0.025(2) -0.0064(17) 0.0001(15) S3 0.034(2) 0.028(2) 0.029(2) 0.0072(16) -0.0011(16) -0.0027(16) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pt1 C1 . 1.970(16) ? Pt1 S3 . 2.208(4) ? Pt1 Cl2 . 2.310(4) ? Pt1 Cl1 . 2.359(4) ? C1 N2 . 1.34(2) ? C1 N1 . 1.37(2) ? C2 N2 . 1.38(2) ? C2 C3 . 1.34(3) ? C3 N1 . 1.36(2) ? C4 N1 . 1.47(2) ? C4 C5 . 1.54(2) ? C5 C6 . 1.52(3) ? C6 S1 . 1.781(17) ? C7 N2 . 1.47(2) ? C7 C8B . 1.535(18) ? C7 C8A . 1.543(18) ? C10 S3 . 1.78(2) ? C11 S3 . 1.78(2) ? C8A C9A . 1.536(19) ? C9A S2 . 1.82(3) ? C8B C9B . 1.529(19) ? C9B S2 . 1.78(4) ? Na1 O8 . 2.34(2) ? Na1 O2 . 2.85(3) ? Na1 Na2 1_545 3.24(3) ? Na1 Na3 . 4.19(3) ? Na2 O9 . 2.24(3) ? Na2 O8 1_565 2.62(3) ? Na2 O3 . 2.78(3) ? Na2 O7 2_776 2.83(2) ? Na2 Na1 1_565 3.24(3) ? Na3 O8 . 2.50(3) ? Na3 O10 . 2.59(4) ? Na3 O4 2_766 2.84(4) ? O1 S1 . 1.46(2) ? O2 S1 . 1.44(2) ? O3 S1 . 1.455(18) ? O4 S2 . 1.30(2) ? O4 Na3 2_766 2.84(4) ? O5 S2 . 1.40(2) ? O6 S2 . 1.388(18) ? O7 S3 . 1.455(15) ? O7 Na2 2_776 2.83(3) ? O8 O9 1_545 1.81(3) ? O8 Na2 1_545 2.62(3) ? O9 O8 1_565 1.81(3) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 Pt1 S3 . . 91.0(5) ? C1 Pt1 Cl2 . . 88.3(5) ? S3 Pt1 Cl2 . . 177.38(17) ? C1 Pt1 Cl1 . . 177.6(5) ? S3 Pt1 Cl1 . . 90.40(16) ? Cl2 Pt1 Cl1 . . 90.39(17) ? N2 C1 N1 . . 104.4(13) ? N2 C1 Pt1 . . 128.3(12) ? N1 C1 Pt1 . . 127.3(12) ? N2 C2 C3 . . 107.4(14) ? C2 C3 N1 . . 106.9(14) ? N1 C4 C5 . . 111.4(13) ? C6 C5 C4 . . 112.7(14) ? C5 C6 S1 . . 111.8(13) ? N2 C7 C8B . . 116.7(18) ? N2 C7 C8A . . 110.6(17) ? C8B C7 C8A . . 32.5(16) ? C7 C8A C9A . . 114.(2) ? C8A C9A S2 . . 103.8(19) ? C7 C8B C9B . . 108.(2) ? C8B C9B S2 . . 113.(2) ? C3 N1 C1 . . 110.7(13) ? C3 N1 C4 . . 125.7(14) ? C1 N1 C4 . . 123.5(13) ? C2 N2 C1 . . 110.7(13) ? C2 N2 C7 . . 123.4(14) ? C1 N2 C7 . . 125.9(14) ? O8 Na1 O2 . . 110.0(9) ? O8 Na1 Na2 . 1_545 53.0(7) ? O2 Na1 Na2 . 1_545 158.5(10) ? O8 Na1 Na3 . . 31.2(7) ? O2 Na1 Na3 . . 81.5(7) ? Na2 Na1 Na3 1_545 . 83.9(7) ? O9 Na2 O8 . 1_565 42.8(7) ? O9 Na2 O3 . . 117.0(11) ? O8 Na2 O3 1_565 . 137.9(10) ? O9 Na2 O7 . 2_776 131.1(12) ? O8 Na2 O7 1_565 2_776 110.5(9) ? O3 Na2 O7 . 2_776 107.3(9) ? O9 Na2 Na1 . 1_565 87.7(9) ? O8 Na2 Na1 1_565 1_565 45.7(6) ? O3 Na2 Na1 . 1_565 119.6(10) ? O7 Na2 Na1 2_776 1_565 87.9(8) ? O8 Na3 O10 . . 137.4(15) ? O8 Na3 O4 . 2_766 49.8(8) ? O10 Na3 O4 . 2_766 172.8(15) ? O8 Na3 Na1 . . 29.1(6) ? O10 Na3 Na1 . . 125.4(12) ? O4 Na3 Na1 2_766 . 61.1(7) ? S1 O2 Na1 . . 146.5(18) ? S1 O3 Na2 . . 125.1(11) ? S2 O4 Na3 . 2_766 158.6(12) ? S3 O7 Na2 . 2_776 146.6(11) ? O9 O8 Na1 1_545 . 136.6(12) ? O9 O8 Na3 1_545 . 99.6(11) ? Na1 O8 Na3 . . 119.7(11) ? O9 O8 Na2 1_545 1_545 57.6(10) ? Na1 O8 Na2 . 1_545 81.2(9) ? Na3 O8 Na2 . 1_545 156.9(11) ? O8 O9 Na2 1_565 . 79.6(11) ? O1 S1 O3 . . 111.4(13) ? O1 S1 O2 . . 111.6(18) ? O3 S1 O2 . . 112.5(14) ? O1 S1 C6 . . 106.3(10) ? O3 S1 C6 . . 108.0(11) ? O2 S1 C6 . . 106.7(11) ? O4 S2 O6 . . 118.9(17) ? O4 S2 O5 . . 105.4(18) ? O6 S2 O5 . . 114.1(14) ? O4 S2 C9B . . 121.4(15) ? O6 S2 C9B . . 91.7(14) ? O5 S2 C9B . . 104.7(16) ? O4 S2 C9A . . 84.8(13) ? O6 S2 C9A . . 118.6(15) ? O5 S2 C9A . . 111.2(15) ? C9B S2 C9A . . 37.3(15) ? O7 S3 C10 . . 108.6(12) ? O7 S3 C11 . . 108.1(12) ? C10 S3 C11 . . 99.9(12) ? O7 S3 Pt1 . . 116.1(6) ? C10 S3 Pt1 . . 110.5(8) ? C11 S3 Pt1 . . 112.4(9) ? # start Validation Reply Form _vrf_PLAT780_ALERT_1_A ; PROBLEM: Coordinates do not Form a Properly Connected Set ? RESPONSE: This alert is probably generated due to the ionic nature of the Na+ bonds (the distances between Na and O atoms are not considered as bonding distances). However, it does not affect the validity of the structural data. ; # end Validation Reply Form #===END