# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 182 _publ_requested_journal Chem.Commun. _publ_contact_author_name ;Pierre Braunstein ; _publ_contact_author_address ;Laboratoire de Chimie de Coordination, UMR CNRS 7513, Universite Louis Pasteur, Institut Le Bel, 4 rue Blaise Pascal, 67000, STRASBOURG, FRANCE ; _publ_contact_author_email braunst@chimie.u-strasbg.fr _publ_contact_author_phone '+33 390241308' _publ_contact_author_fax '+33 390241322' loop_ _publ_author_name _publ_author_address 'Pierre Braunstein' ;Laboratoire de Chimie de Coordination, UMR CNRS 7513, Universite Louis Pasteur, Institut Le Bel, 4 rue Blaise Pascal, 67000, STRASBOURG, FRANCE ; 'Margraf, Gunter' ;Laboratoire de Chimie de Coordination, UMR CNRS 7513, Universite Louis Pasteur, Institut Le Bel, 4 rue Blaise Pascal, 67000, STRASBOURG, FRANCE ; 'Pattacini, Roberto' ;Laboratoire de Chimie de Coordination, UMR CNRS 7513, Universite Louis Pasteur, Institut Le Bel, 4 rue Blaise Pascal, 67000, STRASBOURG, FRANCE ; ' Messaoudi, Abdelatif' ;Laboratoire de Chimie de Coordination, UMR CNRS 7513, Universite Louis Pasteur, Institut Le Bel, 4 rue Blaise Pascal, 67000, STRASBOURG, FRANCE ; _publ_contact_letter ; ; _publ_requested_category SC _publ_section_title ; Intra- and inter-molecular phosphoryl migration in phosphinothiazolines, precursors to polynuclear complexes and bimetallic coordination polymers. ; data_compound1 _database_code_depnum_ccdc_archive 'CCDC 601675' _audit_creation_date 27-02-05 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H15 N2 P S' _chemical_formula_sum 'C15 H15 N2 P S' _chemical_formula_weight 286.32 _chemical_absolute_configuration . 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.5330(3) _cell_length_b 11.8340(2) _cell_length_c 16.1740(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.3850(10) _cell_angle_gamma 90.00 _cell_volume 2866.52(9) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7019 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.327 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 0.325 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14463 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0577 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 30.05 _reflns_number_total 8350 _reflns_number_gt 5517 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0521P)^2^+0.3845P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8350 _refine_ls_number_parameters 359 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0834 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1245 _refine_ls_wR_factor_gt 0.1078 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.01532(3) 1.07435(4) 0.39175(3) 0.03727(12) Uani 1 1 d . . . S2 S 0.50506(3) 0.57275(4) 0.11778(3) 0.03401(12) Uani 1 1 d . . . P1 P 0.10720(3) 0.87107(3) 0.32651(2) 0.02746(11) Uani 1 1 d . . . P2 P 0.40429(3) 0.36962(3) 0.18133(3) 0.02823(11) Uani 1 1 d . . . N1 N 0.16700(9) 0.94885(11) 0.41168(8) 0.0284(3) Uani 1 1 d D . . N2 N 0.16438(9) 1.09015(12) 0.51059(9) 0.0334(3) Uani 1 1 d D . . N3 N 0.34955(9) 0.45558(11) 0.09900(8) 0.0302(3) Uani 1 1 d D . . N4 N 0.35183(9) 0.60598(11) 0.00758(9) 0.0297(3) Uani 1 1 d D . . C1 C 0.12653(10) 1.03147(13) 0.44164(9) 0.0254(3) Uani 1 1 d . . . C2 C 0.10858(12) 1.17386(15) 0.53696(12) 0.0420(4) Uani 1 1 d . . . H2A H 0.1396 1.2478 0.5454 0.050 Uiso 1 1 calc . . . H2B H 0.0975 1.1509 0.5921 0.050 Uiso 1 1 calc . . . C3 C 0.02121(13) 1.18473(16) 0.46966(12) 0.0463(5) Uani 1 1 d . . . H3A H 0.0173 1.2596 0.4416 0.056 Uiso 1 1 calc . . . H3B H -0.0291 1.1776 0.4963 0.056 Uiso 1 1 calc . . . C4 C 0.19365(11) 0.84203(13) 0.27151(9) 0.0263(3) Uani 1 1 d . . . C5 C 0.26612(12) 0.91286(14) 0.27652(10) 0.0357(4) Uani 1 1 d . . . H5 H 0.2753 0.9759 0.3142 0.043 Uiso 1 1 calc . . . C6 C 0.32532(13) 0.89287(17) 0.22728(12) 0.0427(4) Uani 1 1 d . . . H6 H 0.3747 0.9420 0.2315 0.051 Uiso 1 1 calc . . . C7 C 0.31274(13) 0.80209(17) 0.17238(11) 0.0423(4) Uani 1 1 d . . . H7 H 0.3533 0.7887 0.1386 0.051 Uiso 1 1 calc . . . C8 C 0.24117(14) 0.73035(15) 0.16629(11) 0.0445(5) Uani 1 1 d . . . H8 H 0.2325 0.6677 0.1282 0.053 Uiso 1 1 calc . . . C9 C 0.18232(13) 0.74951(14) 0.21535(10) 0.0368(4) Uani 1 1 d . . . H9 H 0.1335 0.6995 0.2111 0.044 Uiso 1 1 calc . . . C10 C 0.09969(11) 0.73265(13) 0.37526(10) 0.0286(3) Uani 1 1 d . . . C11 C 0.16357(12) 0.69227(14) 0.44671(11) 0.0354(4) Uani 1 1 d . . . H11 H 0.2152 0.7364 0.4711 0.042 Uiso 1 1 calc . . . C12 C 0.15289(14) 0.58858(16) 0.48268(13) 0.0437(5) Uani 1 1 d . . . H12 H 0.1965 0.5624 0.5319 0.052 Uiso 1 1 calc . . . C13 C 0.07869(16) 0.52354(15) 0.44677(13) 0.0484(5) Uani 1 1 d . . . H13 H 0.0718 0.4521 0.4710 0.058 Uiso 1 1 calc . . . C14 C 0.01487(15) 0.56128(17) 0.37642(13) 0.0517(6) Uani 1 1 d . . . H14 H -0.0359 0.5159 0.3519 0.062 Uiso 1 1 calc . . . C15 C 0.02453(12) 0.66667(16) 0.34076(11) 0.0398(4) Uani 1 1 d . . . H15 H -0.0204 0.6934 0.2928 0.048 Uiso 1 1 calc . . . C16 C 0.39090(10) 0.53886(13) 0.07179(9) 0.0254(3) Uani 1 1 d . . . C17 C 0.41081(12) 0.68471(14) -0.01972(10) 0.0337(4) Uani 1 1 d . . . H17A H 0.3810 0.7589 -0.0333 0.040 Uiso 1 1 calc . . . H17B H 0.4252 0.6559 -0.0720 0.040 Uiso 1 1 calc . . . C18 C 0.49581(12) 0.69776(16) 0.05201(12) 0.0441(5) Uani 1 1 d . . . H18A H 0.4927 0.7662 0.0863 0.053 Uiso 1 1 calc . . . H18B H 0.5481 0.7044 0.0283 0.053 Uiso 1 1 calc . . . C19 C 0.40602(11) 0.23413(13) 0.12715(10) 0.0276(3) Uani 1 1 d . . . C20 C 0.47804(12) 0.16262(15) 0.15917(10) 0.0367(4) Uani 1 1 d . . . H20 H 0.5240 0.1846 0.2080 0.044 Uiso 1 1 calc . . . C21 C 0.48327(15) 0.05907(16) 0.12028(12) 0.0484(5) Uani 1 1 d . . . H21 H 0.5326 0.0104 0.1427 0.058 Uiso 1 1 calc . . . C22 C 0.41703(15) 0.02687(15) 0.04917(13) 0.0460(5) Uani 1 1 d . . . H22 H 0.4204 -0.0444 0.0232 0.055 Uiso 1 1 calc . . . C23 C 0.34587(13) 0.09787(16) 0.01551(12) 0.0434(5) Uani 1 1 d . . . H23 H 0.3008 0.0760 -0.0341 0.052 Uiso 1 1 calc . . . C24 C 0.34014(12) 0.20107(15) 0.05413(11) 0.0360(4) Uani 1 1 d . . . H24 H 0.2911 0.2497 0.0308 0.043 Uiso 1 1 calc . . . C25 C 0.31225(11) 0.34662(13) 0.23083(9) 0.0282(3) Uani 1 1 d . . . C26 C 0.29014(13) 0.24143(14) 0.25743(12) 0.0407(4) Uani 1 1 d . . . H26 H 0.3220 0.1762 0.2481 0.049 Uiso 1 1 calc . . . C27 C 0.22190(16) 0.23092(16) 0.29754(14) 0.0544(6) Uani 1 1 d . . . H27 H 0.2076 0.1584 0.3154 0.065 Uiso 1 1 calc . . . C28 C 0.17479(14) 0.32357(18) 0.31175(12) 0.0485(5) Uani 1 1 d . . . H28 H 0.1277 0.3154 0.3387 0.058 Uiso 1 1 calc . . . C29 C 0.19637(15) 0.42872(17) 0.28659(12) 0.0499(5) Uani 1 1 d . . . H29 H 0.1641 0.4935 0.2961 0.060 Uiso 1 1 calc . . . C30 C 0.26513(14) 0.43996(15) 0.24738(11) 0.0439(5) Uani 1 1 d . . . H30 H 0.2804 0.5130 0.2315 0.053 Uiso 1 1 calc . . . H2N H 0.2217(4) 1.084(3) 0.5360(17) 0.021(8) Uiso 0.50 1 d PD . . H4N H 0.2959(6) 0.597(3) -0.0218(17) 0.025(9) Uiso 0.50 1 d PD . . H1N H 0.2240(7) 0.942(4) 0.438(2) 0.059(13) Uiso 0.50 1 d PD . . H3N H 0.2925(6) 0.451(3) 0.0719(19) 0.037(10) Uiso 0.50 1 d PD . . 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 S1 0.0312(2) 0.0411(3) 0.0368(2) -0.00365(19) 0.00425(18) 0.01301(19) S2 0.0281(2) 0.0372(2) 0.0347(2) 0.00175(18) 0.00478(17) -0.00600(18) P1 0.0252(2) 0.0288(2) 0.0273(2) -0.00306(16) 0.00494(16) 0.00202(17) P2 0.0276(2) 0.0273(2) 0.0283(2) 0.00259(16) 0.00487(17) -0.00146(17) N1 0.0253(7) 0.0281(7) 0.0315(7) -0.0064(6) 0.0068(6) 0.0019(6) N2 0.0264(7) 0.0335(8) 0.0407(8) -0.0122(6) 0.0097(6) 0.0011(6) N3 0.0269(7) 0.0296(7) 0.0326(7) 0.0066(6) 0.0053(6) -0.0022(6) N4 0.0270(8) 0.0301(7) 0.0337(7) 0.0068(6) 0.0110(6) -0.0010(6) C1 0.0235(8) 0.0253(8) 0.0300(8) 0.0016(6) 0.0117(6) -0.0001(6) C2 0.0366(10) 0.0406(10) 0.0499(10) -0.0172(9) 0.0135(9) 0.0065(8) C3 0.0410(11) 0.0442(11) 0.0555(12) -0.0119(9) 0.0162(9) 0.0117(9) C4 0.0301(8) 0.0254(8) 0.0236(7) 0.0007(6) 0.0072(6) 0.0020(6) C5 0.0393(10) 0.0362(9) 0.0333(8) -0.0061(7) 0.0128(8) -0.0058(8) C6 0.0366(10) 0.0557(12) 0.0386(10) -0.0047(9) 0.0145(8) -0.0088(9) C7 0.0467(12) 0.0526(11) 0.0337(9) 0.0027(8) 0.0211(8) 0.0064(9) C8 0.0679(14) 0.0371(10) 0.0349(9) -0.0076(8) 0.0245(10) -0.0015(10) C9 0.0489(11) 0.0331(9) 0.0313(8) -0.0064(7) 0.0155(8) -0.0104(8) C10 0.0293(8) 0.0306(8) 0.0299(8) -0.0073(7) 0.0148(7) -0.0015(7) C11 0.0324(9) 0.0340(9) 0.0421(9) 0.0024(8) 0.0139(8) 0.0000(7) C12 0.0477(12) 0.0371(10) 0.0529(11) 0.0088(9) 0.0249(10) 0.0078(9) C13 0.0705(15) 0.0327(10) 0.0557(12) -0.0053(9) 0.0409(12) -0.0074(10) C14 0.0616(14) 0.0506(12) 0.0520(12) -0.0210(10) 0.0313(11) -0.0307(11) C15 0.0379(10) 0.0500(11) 0.0341(9) -0.0122(8) 0.0141(8) -0.0141(9) C16 0.0250(8) 0.0275(8) 0.0258(7) -0.0038(6) 0.0102(6) 0.0000(6) C17 0.0346(9) 0.0322(9) 0.0363(9) 0.0053(7) 0.0128(7) -0.0048(7) C18 0.0347(10) 0.0477(11) 0.0507(11) 0.0105(9) 0.0128(9) -0.0112(8) C19 0.0280(8) 0.0270(8) 0.0311(8) 0.0047(6) 0.0136(7) -0.0012(6) C20 0.0402(10) 0.0401(10) 0.0315(8) 0.0098(7) 0.0126(8) 0.0088(8) C21 0.0624(14) 0.0408(11) 0.0479(11) 0.0143(9) 0.0252(10) 0.0206(10) C22 0.0667(14) 0.0278(9) 0.0539(12) -0.0015(8) 0.0344(11) 0.0010(9) C23 0.0430(11) 0.0415(10) 0.0496(11) -0.0116(9) 0.0190(9) -0.0119(9) C24 0.0285(9) 0.0360(9) 0.0440(9) -0.0059(8) 0.0106(8) -0.0029(7) C25 0.0310(9) 0.0290(8) 0.0246(7) 0.0024(6) 0.0072(6) 0.0029(7) C26 0.0435(11) 0.0310(9) 0.0547(11) 0.0065(8) 0.0256(9) 0.0057(8) C27 0.0651(15) 0.0389(11) 0.0739(14) 0.0070(10) 0.0439(12) 0.0002(10) C28 0.0483(12) 0.0576(13) 0.0485(11) 0.0001(10) 0.0285(10) 0.0029(10) C29 0.0624(14) 0.0497(12) 0.0467(11) 0.0022(9) 0.0305(10) 0.0186(10) C30 0.0625(14) 0.0338(10) 0.0422(10) 0.0045(8) 0.0261(10) 0.0085(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C1 1.7757(16) . ? S1 C3 1.8004(18) . ? S2 C16 1.7773(16) . ? S2 C18 1.8054(18) . ? P1 N1 1.7113(13) . ? P1 C4 1.8293(16) . ? P1 C10 1.8350(17) . ? P2 N3 1.7118(14) . ? P2 C19 1.8308(16) . ? P2 C25 1.8348(16) . ? N1 C1 1.3220(19) . ? N1 H1N 0.8799(11) . ? N2 C1 1.313(2) . ? N2 C2 1.453(2) . ? N2 H2N 0.8799(11) . ? N3 C16 1.3143(19) . ? N3 H3N 0.8799(10) . ? N4 C16 1.320(2) . ? N4 C17 1.455(2) . ? N4 H4N 0.8799(10) . ? C2 C3 1.503(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.388(2) . ? C4 C9 1.404(2) . ? C5 C6 1.387(2) . ? C5 H5 0.9500 . ? C6 C7 1.374(3) . ? C6 H6 0.9500 . ? C7 C8 1.381(3) . ? C7 H7 0.9500 . ? C8 C9 1.379(2) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C15 1.392(2) . ? C10 C11 1.393(2) . ? C11 C12 1.387(2) . ? C11 H11 0.9500 . ? C12 C13 1.380(3) . ? C12 H12 0.9500 . ? C13 C14 1.371(3) . ? C13 H13 0.9500 . ? C14 C15 1.399(3) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C17 C18 1.517(2) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.389(2) . ? C19 C24 1.398(2) . ? C20 C21 1.390(3) . ? C20 H20 0.9500 . ? C21 C22 1.378(3) . ? C21 H21 0.9500 . ? C22 C23 1.380(3) . ? C22 H22 0.9500 . ? C23 C24 1.385(2) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.390(2) . ? C25 C30 1.390(2) . ? C26 C27 1.387(2) . ? C26 H26 0.9500 . ? C27 C28 1.371(3) . ? C27 H27 0.9500 . ? C28 C29 1.378(3) . ? C28 H28 0.9500 . ? C29 C30 1.386(3) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? 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 S1 C3 91.52(8) . . ? C16 S2 C18 91.36(8) . . ? N1 P1 C4 100.42(7) . . ? N1 P1 C10 102.54(7) . . ? C4 P1 C10 100.36(7) . . ? N3 P2 C19 102.44(7) . . ? N3 P2 C25 98.27(7) . . ? C19 P2 C25 101.01(7) . . ? C1 N1 P1 118.92(11) . . ? C1 N1 H1N 114(3) . . ? P1 N1 H1N 127(3) . . ? C1 N2 C2 116.26(14) . . ? C1 N2 H2N 121(2) . . ? C2 N2 H2N 122(2) . . ? C16 N3 P2 121.34(12) . . ? C16 N3 H3N 113(2) . . ? P2 N3 H3N 126(2) . . ? C16 N4 C17 115.40(14) . . ? C16 N4 H4N 122(2) . . ? C17 N4 H4N 122(2) . . ? N2 C1 N1 123.59(15) . . ? N2 C1 S1 113.41(11) . . ? N1 C1 S1 123.00(12) . . ? N2 C2 C3 109.89(14) . . ? N2 C2 H2A 109.7 . . ? C3 C2 H2A 109.7 . . ? N2 C2 H2B 109.7 . . ? C3 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C2 C3 S1 108.25(12) . . ? C2 C3 H3A 110.0 . . ? S1 C3 H3A 110.0 . . ? C2 C3 H3B 110.0 . . ? S1 C3 H3B 110.0 . . ? H3A C3 H3B 108.4 . . ? C5 C4 C9 117.98(15) . . ? C5 C4 P1 123.14(12) . . ? C9 C4 P1 118.62(13) . . ? C6 C5 C4 120.95(15) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C7 C6 C5 120.13(17) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C8 120.02(16) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C9 C8 C7 120.11(16) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C4 120.81(16) . . ? C8 C9 H9 119.6 . . ? C4 C9 H9 119.6 . . ? C15 C10 C11 118.50(15) . . ? C15 C10 P1 118.07(13) . . ? C11 C10 P1 123.38(13) . . ? C12 C11 C10 120.90(17) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C13 C12 C11 119.78(19) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C14 C13 C12 120.48(17) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C15 119.99(18) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C10 C15 C14 120.34(18) . . ? C10 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? N3 C16 N4 123.44(15) . . ? N3 C16 S2 123.43(12) . . ? N4 C16 S2 113.13(11) . . ? N4 C17 C18 108.87(13) . . ? N4 C17 H17A 109.9 . . ? C18 C17 H17A 109.9 . . ? N4 C17 H17B 109.9 . . ? C18 C17 H17B 109.9 . . ? H17A C17 H17B 108.3 . . ? C17 C18 S2 106.52(12) . . ? C17 C18 H18A 110.4 . . ? S2 C18 H18A 110.4 . . ? C17 C18 H18B 110.4 . . ? S2 C18 H18B 110.4 . . ? H18A C18 H18B 108.6 . . ? C20 C19 C24 118.77(15) . . ? C20 C19 P2 117.90(13) . . ? C24 C19 P2 123.30(12) . . ? C19 C20 C21 120.44(17) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C22 C21 C20 120.09(18) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 120.22(17) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C22 C23 C24 119.96(18) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C19 120.50(17) . . ? C23 C24 H24 119.8 . . ? C19 C24 H24 119.8 . . ? C26 C25 C30 117.79(15) . . ? C26 C25 P2 123.59(12) . . ? C30 C25 P2 118.51(13) . . ? C27 C26 C25 120.49(16) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C28 C27 C26 120.98(17) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C29 119.35(17) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? C28 C29 C30 119.95(17) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C29 C30 C25 121.41(17) . . ? C29 C30 H30 119.3 . . ? C25 C30 H30 119.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 P1 N1 C1 145.74(12) . . . . ? C10 P1 N1 C1 -111.06(13) . . . . ? C19 P2 N3 C16 -112.10(13) . . . . ? C25 P2 N3 C16 144.62(13) . . . . ? C2 N2 C1 N1 -176.83(15) . . . . ? C2 N2 C1 S1 3.50(19) . . . . ? P1 N1 C1 N2 174.52(12) . . . . ? P1 N1 C1 S1 -5.85(18) . . . . ? C3 S1 C1 N2 1.61(13) . . . . ? C3 S1 C1 N1 -178.06(14) . . . . ? C1 N2 C2 C3 -8.0(2) . . . . ? N2 C2 C3 S1 8.5(2) . . . . ? C1 S1 C3 C2 -5.81(14) . . . . ? N1 P1 C4 C5 -27.74(15) . . . . ? C10 P1 C4 C5 -132.69(14) . . . . ? N1 P1 C4 C9 158.27(13) . . . . ? C10 P1 C4 C9 53.32(14) . . . . ? C9 C4 C5 C6 0.2(3) . . . . ? P1 C4 C5 C6 -173.84(14) . . . . ? C4 C5 C6 C7 0.1(3) . . . . ? C5 C6 C7 C8 -0.2(3) . . . . ? C6 C7 C8 C9 -0.1(3) . . . . ? C7 C8 C9 C4 0.4(3) . . . . ? C5 C4 C9 C8 -0.5(3) . . . . ? P1 C4 C9 C8 173.83(14) . . . . ? N1 P1 C10 C15 149.28(13) . . . . ? C4 P1 C10 C15 -107.48(13) . . . . ? N1 P1 C10 C11 -28.28(15) . . . . ? C4 P1 C10 C11 74.96(15) . . . . ? C15 C10 C11 C12 0.2(2) . . . . ? P1 C10 C11 C12 177.74(13) . . . . ? C10 C11 C12 C13 0.9(3) . . . . ? C11 C12 C13 C14 -0.8(3) . . . . ? C12 C13 C14 C15 -0.3(3) . . . . ? C11 C10 C15 C14 -1.3(2) . . . . ? P1 C10 C15 C14 -178.97(14) . . . . ? C13 C14 C15 C10 1.4(3) . . . . ? P2 N3 C16 N4 178.76(12) . . . . ? P2 N3 C16 S2 -1.34(19) . . . . ? C17 N4 C16 N3 -173.12(14) . . . . ? C17 N4 C16 S2 6.98(17) . . . . ? C18 S2 C16 N3 -173.60(14) . . . . ? C18 S2 C16 N4 6.31(13) . . . . ? C16 N4 C17 C18 -19.8(2) . . . . ? N4 C17 C18 S2 22.62(17) . . . . ? C16 S2 C18 C17 -16.43(13) . . . . ? N3 P2 C19 C20 148.55(12) . . . . ? C25 P2 C19 C20 -110.32(13) . . . . ? N3 P2 C19 C24 -29.48(15) . . . . ? C25 P2 C19 C24 71.65(15) . . . . ? C24 C19 C20 C21 -1.4(2) . . . . ? P2 C19 C20 C21 -179.52(14) . . . . ? C19 C20 C21 C22 0.4(3) . . . . ? C20 C21 C22 C23 0.9(3) . . . . ? C21 C22 C23 C24 -1.1(3) . . . . ? C22 C23 C24 C19 0.0(3) . . . . ? C20 C19 C24 C23 1.2(2) . . . . ? P2 C19 C24 C23 179.23(13) . . . . ? N3 P2 C25 C26 134.82(15) . . . . ? C19 P2 C25 C26 30.33(16) . . . . ? N3 P2 C25 C30 -49.09(15) . . . . ? C19 P2 C25 C30 -153.58(14) . . . . ? C30 C25 C26 C27 1.3(3) . . . . ? P2 C25 C26 C27 177.40(16) . . . . ? C25 C26 C27 C28 0.1(3) . . . . ? C26 C27 C28 C29 -0.7(3) . . . . ? C27 C28 C29 C30 0.0(3) . . . . ? C28 C29 C30 C25 1.4(3) . . . . ? C26 C25 C30 C29 -2.0(3) . . . . ? P2 C25 C30 C29 -178.36(16) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.343 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.055 # Attachment 'compound2.cif' data_compound2 _database_code_depnum_ccdc_archive 'CCDC 601676' _audit_creation_date 27-02-05 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H24 N2 P2 S' _chemical_formula_sum 'C27 H24 N2 P2 S' _chemical_formula_weight 470.48 _chemical_absolute_configuration . 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1420(2) _cell_length_b 10.0760(2) _cell_length_c 14.4330(4) _cell_angle_alpha 92.1400(9) _cell_angle_beta 105.8700(9) _cell_angle_gamma 107.9900(12) _cell_volume 1205.47(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 11070 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.296 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 492 _exptl_absorpt_coefficient_mu 0.285 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71070 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10874 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0609 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 30.06 _reflns_number_total 7015 _reflns_number_gt 4950 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0712P)^2^+0.2278P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7015 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0792 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.1401 _refine_ls_wR_factor_gt 0.1229 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S S 0.74874(5) 0.81672(5) 0.33097(4) 0.03485(14) Uani 1 1 d . . . P1 P 0.42166(5) 0.42873(5) 0.16618(3) 0.02512(12) Uani 1 1 d . . . P2 P 0.39043(5) 0.83395(5) 0.28885(4) 0.02671(13) Uani 1 1 d . . . N1 N 0.59311(17) 0.56438(15) 0.23704(11) 0.0250(3) Uani 1 1 d . . . N2 N 0.42135(17) 0.68391(15) 0.25254(12) 0.0280(3) Uani 1 1 d . . . C1 C 0.5650(2) 0.68121(17) 0.26796(13) 0.0235(4) Uani 1 1 d . . . C2 C 0.8665(2) 0.7174(2) 0.30093(17) 0.0396(5) Uani 1 1 d . . . H2A H 0.9095 0.7556 0.2480 0.048 Uiso 1 1 calc . . . H2B H 0.9585 0.7234 0.3583 0.048 Uiso 1 1 calc . . . C3 C 0.7604(2) 0.5689(2) 0.26956(18) 0.0419(5) Uani 1 1 d . . . H3A H 0.7875 0.5275 0.2159 0.050 Uiso 1 1 calc . . . H3B H 0.7764 0.5134 0.3244 0.050 Uiso 1 1 calc . . . C4 C 0.5203(2) 0.30655(18) 0.13648(13) 0.0267(4) Uani 1 1 d . . . C5 C 0.5629(3) 0.3217(2) 0.05117(16) 0.0396(5) Uani 1 1 d . . . H5 H 0.5409 0.3924 0.0134 0.048 Uiso 1 1 calc . . . C6 C 0.6369(3) 0.2352(3) 0.02042(18) 0.0484(6) Uani 1 1 d . . . H6 H 0.6668 0.2478 -0.0376 0.058 Uiso 1 1 calc . . . C7 C 0.6674(3) 0.1313(2) 0.07348(18) 0.0438(5) Uani 1 1 d . . . H7 H 0.7179 0.0717 0.0522 0.053 Uiso 1 1 calc . . . C8 C 0.6244(2) 0.1137(2) 0.15790(17) 0.0394(5) Uani 1 1 d . . . H8 H 0.6452 0.0415 0.1945 0.047 Uiso 1 1 calc . . . C9 C 0.5512(2) 0.20030(19) 0.18959(14) 0.0305(4) Uani 1 1 d . . . H9 H 0.5220 0.1873 0.2478 0.037 Uiso 1 1 calc . . . C10 C 0.3304(2) 0.34980(18) 0.25783(13) 0.0253(4) Uani 1 1 d . . . C11 C 0.4154(2) 0.3489(2) 0.35349(15) 0.0326(4) Uani 1 1 d . . . H11 H 0.5295 0.3896 0.3745 0.039 Uiso 1 1 calc . . . C12 C 0.3356(2) 0.2891(2) 0.41873(15) 0.0377(5) Uani 1 1 d . . . H12 H 0.3950 0.2893 0.4840 0.045 Uiso 1 1 calc . . . C13 C 0.1691(3) 0.2293(2) 0.38847(17) 0.0393(5) Uani 1 1 d . . . H13 H 0.1145 0.1871 0.4328 0.047 Uiso 1 1 calc . . . C14 C 0.0828(2) 0.2308(2) 0.29409(16) 0.0391(5) Uani 1 1 d . . . H14 H -0.0313 0.1904 0.2735 0.047 Uiso 1 1 calc . . . C15 C 0.1625(2) 0.2914(2) 0.22908(14) 0.0313(4) Uani 1 1 d . . . H15 H 0.1023 0.2931 0.1643 0.038 Uiso 1 1 calc . . . C16 C 0.2011(2) 0.81376(18) 0.19428(14) 0.0264(4) Uani 1 1 d . . . C17 C 0.1543(2) 0.9322(2) 0.17995(15) 0.0346(4) Uani 1 1 d . . . H17 H 0.2212 1.0201 0.2178 0.042 Uiso 1 1 calc . . . C18 C 0.0112(3) 0.9234(2) 0.11114(17) 0.0428(5) Uani 1 1 d . . . H18 H -0.0207 1.0045 0.1029 0.051 Uiso 1 1 calc . . . C19 C -0.0856(3) 0.7964(2) 0.05432(16) 0.0418(5) Uani 1 1 d . . . H19 H -0.1833 0.7905 0.0067 0.050 Uiso 1 1 calc . . . C20 C -0.0396(2) 0.6783(2) 0.06714(15) 0.0392(5) Uani 1 1 d . . . H20 H -0.1058 0.5913 0.0279 0.047 Uiso 1 1 calc . . . C21 C 0.1025(2) 0.6861(2) 0.13690(14) 0.0320(4) Uani 1 1 d . . . H21 H 0.1328 0.6042 0.1457 0.038 Uiso 1 1 calc . . . C22 C 0.30568(19) 0.77813(18) 0.38829(13) 0.0254(4) Uani 1 1 d . . . C23 C 0.2475(2) 0.63714(19) 0.40182(14) 0.0290(4) Uani 1 1 d . . . H23 H 0.2506 0.5656 0.3584 0.035 Uiso 1 1 calc . . . C24 C 0.1852(2) 0.6010(2) 0.47822(15) 0.0336(4) Uani 1 1 d . . . H24 H 0.1459 0.5048 0.4869 0.040 Uiso 1 1 calc . . . C25 C 0.1799(2) 0.7048(2) 0.54221(15) 0.0367(5) Uani 1 1 d . . . H25 H 0.1372 0.6797 0.5946 0.044 Uiso 1 1 calc . . . C26 C 0.2372(3) 0.8445(2) 0.52925(16) 0.0401(5) Uani 1 1 d . . . H26 H 0.2333 0.9157 0.5727 0.048 Uiso 1 1 calc . . . C27 C 0.3003(2) 0.8813(2) 0.45296(15) 0.0333(4) Uani 1 1 d . . . H27 H 0.3401 0.9777 0.4448 0.040 Uiso 1 1 calc . . . 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 S 0.0224(2) 0.0297(2) 0.0489(3) -0.0049(2) 0.0085(2) 0.00678(18) P1 0.0240(2) 0.0258(2) 0.0268(3) 0.00250(18) 0.00777(18) 0.00985(18) P2 0.0196(2) 0.0232(2) 0.0375(3) 0.00085(19) 0.00926(19) 0.00713(17) N1 0.0194(7) 0.0249(7) 0.0317(9) 0.0011(6) 0.0080(6) 0.0089(6) N2 0.0221(7) 0.0259(7) 0.0387(9) 0.0024(7) 0.0113(6) 0.0103(6) C1 0.0224(8) 0.0253(8) 0.0256(9) 0.0046(7) 0.0110(7) 0.0081(6) C2 0.0220(9) 0.0392(11) 0.0548(14) -0.0067(10) 0.0080(9) 0.0108(8) C3 0.0229(9) 0.0340(10) 0.0693(16) 0.0016(10) 0.0118(9) 0.0128(8) C4 0.0259(8) 0.0268(8) 0.0279(10) 0.0005(7) 0.0093(7) 0.0088(7) C5 0.0543(13) 0.0392(11) 0.0374(12) 0.0114(9) 0.0248(10) 0.0219(10) C6 0.0575(14) 0.0559(14) 0.0460(14) 0.0037(11) 0.0323(12) 0.0241(12) C7 0.0396(11) 0.0432(12) 0.0563(15) -0.0032(10) 0.0210(10) 0.0198(9) C8 0.0354(11) 0.0319(10) 0.0529(14) 0.0041(9) 0.0129(10) 0.0145(8) C9 0.0291(9) 0.0293(9) 0.0354(11) 0.0056(8) 0.0123(8) 0.0103(7) C10 0.0242(8) 0.0240(8) 0.0294(10) 0.0001(7) 0.0092(7) 0.0096(7) C11 0.0256(9) 0.0407(10) 0.0333(11) 0.0075(8) 0.0100(8) 0.0124(8) C12 0.0380(11) 0.0475(12) 0.0349(12) 0.0132(9) 0.0151(9) 0.0196(9) C13 0.0411(11) 0.0396(11) 0.0469(13) 0.0109(10) 0.0270(10) 0.0143(9) C14 0.0274(10) 0.0415(11) 0.0464(13) -0.0010(10) 0.0163(9) 0.0049(8) C15 0.0260(9) 0.0337(10) 0.0328(11) -0.0018(8) 0.0085(8) 0.0091(7) C16 0.0229(8) 0.0278(9) 0.0313(10) 0.0031(7) 0.0122(7) 0.0089(7) C17 0.0309(10) 0.0295(9) 0.0414(12) 0.0058(8) 0.0070(8) 0.0105(8) C18 0.0412(12) 0.0390(11) 0.0481(14) 0.0109(10) 0.0055(10) 0.0197(9) C19 0.0365(11) 0.0516(13) 0.0339(12) 0.0059(10) 0.0021(9) 0.0173(10) C20 0.0349(10) 0.0452(12) 0.0303(11) -0.0054(9) 0.0046(8) 0.0093(9) C21 0.0327(10) 0.0324(9) 0.0318(11) -0.0001(8) 0.0103(8) 0.0118(8) C22 0.0169(7) 0.0279(8) 0.0296(10) -0.0022(7) 0.0023(6) 0.0100(6) C23 0.0278(9) 0.0277(9) 0.0322(11) -0.0022(8) 0.0090(7) 0.0112(7) C24 0.0336(10) 0.0333(10) 0.0363(11) 0.0048(8) 0.0113(8) 0.0137(8) C25 0.0366(10) 0.0483(12) 0.0283(11) 0.0020(9) 0.0113(8) 0.0175(9) C26 0.0408(11) 0.0417(11) 0.0366(12) -0.0115(9) 0.0102(9) 0.0153(9) C27 0.0264(9) 0.0280(9) 0.0418(12) -0.0073(8) 0.0053(8) 0.0096(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S C1 1.7796(17) . ? S C2 1.800(2) . ? P1 N1 1.7511(15) . ? P1 C10 1.8305(19) . ? P1 C4 1.8358(18) . ? P2 N2 1.7105(15) . ? P2 C16 1.8354(19) . ? P2 C22 1.8373(19) . ? N1 C1 1.364(2) . ? N1 C3 1.458(2) . ? N2 C1 1.280(2) . ? C2 C3 1.482(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.390(3) . ? C4 C9 1.394(3) . ? C5 C6 1.383(3) . ? C5 H5 0.9500 . ? C6 C7 1.373(3) . ? C6 H6 0.9500 . ? C7 C8 1.380(3) . ? C7 H7 0.9500 . ? C8 C9 1.385(3) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.389(3) . ? C10 C15 1.396(2) . ? C11 C12 1.388(3) . ? C11 H11 0.9500 . ? C12 C13 1.386(3) . ? C12 H12 0.9500 . ? C13 C14 1.378(3) . ? C13 H13 0.9500 . ? C14 C15 1.388(3) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.392(3) . ? C16 C21 1.396(2) . ? C17 C18 1.385(3) . ? C17 H17 0.9500 . ? C18 C19 1.385(3) . ? C18 H18 0.9500 . ? C19 C20 1.382(3) . ? C19 H19 0.9500 . ? C20 C21 1.387(3) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C27 1.392(2) . ? C22 C23 1.396(3) . ? C23 C24 1.385(3) . ? C23 H23 0.9500 . ? C24 C25 1.390(3) . ? C24 H24 0.9500 . ? C25 C26 1.382(3) . ? C25 H25 0.9500 . ? C26 C27 1.389(3) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? 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 S C2 91.78(8) . . ? N1 P1 C10 102.16(7) . . ? N1 P1 C4 98.80(7) . . ? C10 P1 C4 103.98(8) . . ? N2 P2 C16 98.80(8) . . ? N2 P2 C22 100.74(8) . . ? C16 P2 C22 98.20(8) . . ? C1 N1 C3 115.53(14) . . ? C1 N1 P1 115.13(12) . . ? C3 N1 P1 129.32(12) . . ? C1 N2 P2 119.99(12) . . ? N2 C1 N1 121.16(15) . . ? N2 C1 S 127.67(13) . . ? N1 C1 S 111.16(12) . . ? C3 C2 S 108.00(13) . . ? C3 C2 H2A 110.1 . . ? S C2 H2A 110.1 . . ? C3 C2 H2B 110.1 . . ? S C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? N1 C3 C2 109.00(16) . . ? N1 C3 H3A 109.9 . . ? C2 C3 H3A 109.9 . . ? N1 C3 H3B 109.9 . . ? C2 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? C5 C4 C9 118.39(17) . . ? C5 C4 P1 115.35(15) . . ? C9 C4 P1 126.24(14) . . ? C6 C5 C4 120.9(2) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C7 C6 C5 120.2(2) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C8 119.74(18) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? C7 C8 C9 120.5(2) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C8 C9 C4 120.26(18) . . ? C8 C9 H9 119.9 . . ? C4 C9 H9 119.9 . . ? C11 C10 C15 118.49(17) . . ? C11 C10 P1 124.76(13) . . ? C15 C10 P1 116.70(15) . . ? C12 C11 C10 120.83(17) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C13 C12 C11 119.90(19) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C14 C13 C12 120.01(18) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 120.07(18) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C10 120.68(19) . . ? C14 C15 H15 119.7 . . ? C10 C15 H15 119.7 . . ? C17 C16 C21 118.83(18) . . ? C17 C16 P2 117.85(13) . . ? C21 C16 P2 123.32(14) . . ? C18 C17 C16 120.69(18) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C18 C19 120.1(2) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C20 C19 C18 119.8(2) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C21 120.37(19) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C20 C21 C16 120.23(19) . . ? C20 C21 H21 119.9 . . ? C16 C21 H21 119.9 . . ? C27 C22 C23 118.87(17) . . ? C27 C22 P2 118.34(14) . . ? C23 C22 P2 122.79(13) . . ? C24 C23 C22 120.37(16) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 120.31(18) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C26 C25 C24 119.66(19) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C25 C26 C27 120.23(17) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C26 C27 C22 120.55(18) . . ? C26 C27 H27 119.7 . . ? C22 C27 H27 119.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 P1 N1 C1 -77.41(14) . . . . ? C4 P1 N1 C1 176.12(13) . . . . ? C10 P1 N1 C3 100.92(18) . . . . ? C4 P1 N1 C3 -5.54(19) . . . . ? C16 P2 N2 C1 149.24(16) . . . . ? C22 P2 N2 C1 -110.62(16) . . . . ? P2 N2 C1 N1 -177.92(13) . . . . ? P2 N2 C1 S 3.6(2) . . . . ? C3 N1 C1 N2 -172.74(18) . . . . ? P1 N1 C1 N2 5.8(2) . . . . ? C3 N1 C1 S 6.0(2) . . . . ? P1 N1 C1 S -175.45(8) . . . . ? C2 S C1 N2 -174.71(19) . . . . ? C2 S C1 N1 6.67(15) . . . . ? C1 S C2 C3 -16.77(18) . . . . ? C1 N1 C3 C2 -18.9(3) . . . . ? P1 N1 C3 C2 162.80(15) . . . . ? S C2 C3 N1 22.4(2) . . . . ? N1 P1 C4 C5 -91.14(16) . . . . ? C10 P1 C4 C5 163.89(15) . . . . ? N1 P1 C4 C9 90.64(17) . . . . ? C10 P1 C4 C9 -14.32(18) . . . . ? C9 C4 C5 C6 -1.1(3) . . . . ? P1 C4 C5 C6 -179.51(18) . . . . ? C4 C5 C6 C7 0.9(4) . . . . ? C5 C6 C7 C8 -0.2(4) . . . . ? C6 C7 C8 C9 -0.2(3) . . . . ? C7 C8 C9 C4 -0.1(3) . . . . ? C5 C4 C9 C8 0.7(3) . . . . ? P1 C4 C9 C8 178.88(15) . . . . ? N1 P1 C10 C11 -29.10(17) . . . . ? C4 P1 C10 C11 73.31(17) . . . . ? N1 P1 C10 C15 148.46(14) . . . . ? C4 P1 C10 C15 -109.13(15) . . . . ? C15 C10 C11 C12 1.0(3) . . . . ? P1 C10 C11 C12 178.57(15) . . . . ? C10 C11 C12 C13 0.1(3) . . . . ? C11 C12 C13 C14 -0.9(3) . . . . ? C12 C13 C14 C15 0.5(3) . . . . ? C13 C14 C15 C10 0.7(3) . . . . ? C11 C10 C15 C14 -1.5(3) . . . . ? P1 C10 C15 C14 -179.19(15) . . . . ? N2 P2 C16 C17 -162.62(15) . . . . ? C22 P2 C16 C17 95.10(16) . . . . ? N2 P2 C16 C21 17.70(17) . . . . ? C22 P2 C16 C21 -84.59(16) . . . . ? C21 C16 C17 C18 1.0(3) . . . . ? P2 C16 C17 C18 -178.67(17) . . . . ? C16 C17 C18 C19 -1.3(3) . . . . ? C17 C18 C19 C20 0.6(4) . . . . ? C18 C19 C20 C21 0.3(3) . . . . ? C19 C20 C21 C16 -0.5(3) . . . . ? C17 C16 C21 C20 -0.1(3) . . . . ? P2 C16 C21 C20 179.56(15) . . . . ? N2 P2 C22 C27 164.43(14) . . . . ? C16 P2 C22 C27 -94.93(15) . . . . ? N2 P2 C22 C23 -15.24(17) . . . . ? C16 P2 C22 C23 85.40(16) . . . . ? C27 C22 C23 C24 0.2(3) . . . . ? P2 C22 C23 C24 179.83(14) . . . . ? C22 C23 C24 C25 0.0(3) . . . . ? C23 C24 C25 C26 0.0(3) . . . . ? C24 C25 C26 C27 -0.3(3) . . . . ? C25 C26 C27 C22 0.5(3) . . . . ? C23 C22 C27 C26 -0.4(3) . . . . ? P2 C22 C27 C26 179.91(15) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.06 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.454 _refine_diff_density_min -0.449 _refine_diff_density_rms 0.081 # Attachment 'compound4.cif' data_compound4 _database_code_depnum_ccdc_archive 'CCDC 601677' _audit_creation_date 27-02-05 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H25 Au2 Cl5 N2 P2 S' _chemical_formula_sum 'C28 H25 Au2 Cl5 N2 P2 S' _chemical_formula_weight 1054.68 _chemical_absolute_configuration . 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' Cl Cl 0.1484 0.1585 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6100(10) _cell_length_b 13.281(2) _cell_length_c 13.769(2) _cell_angle_alpha 98.04(5) _cell_angle_beta 101.87(5) _cell_angle_gamma 104.52(5) _cell_volume 1630.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 11705 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.148 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 9.582 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71070 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean . _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 9537 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0892 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 30.03 _reflns_number_total 9536 _reflns_number_gt 7031 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9536 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1244 _refine_ls_wR_factor_gt 0.1074 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.38027(3) 0.69537(2) 0.021616(19) 0.01985(8) Uani 1 1 d . . . Au2 Au -0.03645(3) 0.70933(2) -0.41832(2) 0.02156(8) Uani 1 1 d . . . Cl1 Cl 0.5629(2) 0.66314(15) 0.13914(14) 0.0277(4) Uani 1 1 d . . . Cl2 Cl -0.2773(2) 0.7038(2) -0.42321(17) 0.0429(5) Uani 1 1 d . . . Cl3 Cl -0.1111(3) 0.8352(2) 0.3867(2) 0.0600(7) Uani 1 1 d . . . Cl4 Cl 0.0129(4) 1.0126(2) 0.3021(3) 0.0780(10) Uani 1 1 d . . . Cl5 Cl 0.0319(4) 0.8055(3) 0.2264(3) 0.0840(11) Uani 1 1 d . . . S S 0.3362(2) 0.54882(15) -0.19563(14) 0.0249(4) Uani 1 1 d . . . P1 P 0.21456(19) 0.74158(14) -0.08853(13) 0.0181(3) Uani 1 1 d . . . P2 P 0.19544(19) 0.71420(14) -0.42101(13) 0.0176(3) Uani 1 1 d . . . N1 N 0.2180(6) 0.7175(4) -0.2106(4) 0.0202(12) Uani 1 1 d . . . N2 N 0.2625(6) 0.6299(4) -0.3536(4) 0.0182(11) Uani 1 1 d . . . C1 C 0.2649(7) 0.6433(5) -0.2520(5) 0.0172(13) Uani 1 1 d . . . C2 C 0.3429(9) 0.5560(6) -0.3882(6) 0.0280(16) Uani 1 1 d . . . H2A H 0.4460 0.5956 -0.3859 0.034 Uiso 1 1 calc . . . H2B H 0.2927 0.5177 -0.4587 0.034 Uiso 1 1 calc . . . C3 C 0.3434(10) 0.4787(7) -0.3182(6) 0.0344(18) Uani 1 1 d . . . H3A H 0.4348 0.4557 -0.3111 0.041 Uiso 1 1 calc . . . H3B H 0.2563 0.4152 -0.3449 0.041 Uiso 1 1 calc . . . C4 C 0.0250(7) 0.6881(5) -0.0833(5) 0.0193(13) Uani 1 1 d . . . C5 C -0.0053(8) 0.6340(6) -0.0063(6) 0.0271(16) Uani 1 1 d . . . H5 H 0.0732 0.6217 0.0405 0.033 Uiso 1 1 calc . . . C6 C -0.1495(9) 0.5986(6) 0.0016(6) 0.0315(17) Uani 1 1 d . . . H6 H -0.1695 0.5629 0.0546 0.038 Uiso 1 1 calc . . . C7 C -0.2657(8) 0.6148(6) -0.0671(6) 0.0313(18) Uani 1 1 d . . . H7 H -0.3649 0.5892 -0.0620 0.038 Uiso 1 1 calc . . . C8 C -0.2354(8) 0.6689(7) -0.1436(6) 0.0336(18) Uani 1 1 d . . . H8 H -0.3146 0.6801 -0.1908 0.040 Uiso 1 1 calc . . . C9 C -0.0913(8) 0.7065(6) -0.1515(6) 0.0266(16) Uani 1 1 d . . . H9 H -0.0712 0.7446 -0.2029 0.032 Uiso 1 1 calc . . . C10 C 0.2437(7) 0.8845(5) -0.0634(5) 0.0188(13) Uani 1 1 d . . . C11 C 0.1805(10) 0.9299(6) 0.0074(7) 0.0359(19) Uani 1 1 d . . . H11 H 0.1205 0.8867 0.0414 0.043 Uiso 1 1 calc . . . C12 C 0.2067(10) 1.0388(6) 0.0273(7) 0.040(2) Uani 1 1 d . . . H12 H 0.1663 1.0707 0.0767 0.048 Uiso 1 1 calc . . . C13 C 0.2899(9) 1.1015(6) -0.0233(6) 0.0316(17) Uani 1 1 d . . . H13 H 0.3044 1.1760 -0.0102 0.038 Uiso 1 1 calc . . . C14 C 0.3529(9) 1.0568(6) -0.0936(6) 0.0310(17) Uani 1 1 d . . . H14 H 0.4121 1.1006 -0.1276 0.037 Uiso 1 1 calc . . . C15 C 0.3295(9) 0.9485(6) -0.1140(6) 0.0280(16) Uani 1 1 d . . . H15 H 0.3718 0.9174 -0.1626 0.034 Uiso 1 1 calc . . . C16 C 0.3337(8) 0.8427(5) -0.3783(5) 0.0212(14) Uani 1 1 d . . . C17 C 0.2974(9) 0.9318(7) -0.4046(7) 0.0350(19) Uani 1 1 d . . . H17 H 0.1988 0.9252 -0.4405 0.042 Uiso 1 1 calc . . . C18 C 0.4024(11) 1.0298(7) -0.3794(9) 0.049(3) Uani 1 1 d . . . H18 H 0.3762 1.0903 -0.3976 0.059 Uiso 1 1 calc . . . C19 C 0.5445(10) 1.0393(7) -0.3281(9) 0.051(3) Uani 1 1 d . . . H19 H 0.6173 1.1066 -0.3112 0.062 Uiso 1 1 calc . . . C20 C 0.5830(8) 0.9521(7) -0.3006(7) 0.039(2) Uani 1 1 d . . . H20 H 0.6817 0.9599 -0.2642 0.047 Uiso 1 1 calc . . . C21 C 0.4790(8) 0.8530(6) -0.3255(6) 0.0271(16) Uani 1 1 d . . . H21 H 0.5060 0.7930 -0.3069 0.033 Uiso 1 1 calc . . . C22 C 0.2146(8) 0.6666(5) -0.5461(5) 0.0208(14) Uani 1 1 d . . . C23 C 0.3428(9) 0.7065(6) -0.5760(6) 0.0276(16) Uani 1 1 d . . . H23 H 0.4241 0.7597 -0.5302 0.033 Uiso 1 1 calc . . . C24 C 0.3528(9) 0.6692(6) -0.6718(6) 0.0317(17) Uani 1 1 d . . . H24 H 0.4415 0.6959 -0.6920 0.038 Uiso 1 1 calc . . . C25 C 0.2360(11) 0.5941(7) -0.7375(6) 0.037(2) Uani 1 1 d . . . H25 H 0.2430 0.5694 -0.8040 0.045 Uiso 1 1 calc . . . C26 C 0.1066(10) 0.5532(7) -0.7089(7) 0.040(2) Uani 1 1 d . . . H26 H 0.0263 0.4995 -0.7549 0.048 Uiso 1 1 calc . . . C27 C 0.0952(8) 0.5906(6) -0.6136(6) 0.0310(17) Uani 1 1 d . . . H27 H 0.0058 0.5646 -0.5941 0.037 Uiso 1 1 calc . . . C28 C -0.0765(10) 0.8774(8) 0.2779(7) 0.042(2) Uani 1 1 d . . . H28 H -0.1735 0.8627 0.2271 0.050 Uiso 1 1 calc . . . 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 Au1 0.01894(13) 0.02185(14) 0.02036(14) 0.00709(10) 0.00527(10) 0.00688(10) Au2 0.01618(13) 0.02703(15) 0.02346(15) 0.00657(11) 0.00633(10) 0.00785(10) Cl1 0.0263(9) 0.0362(10) 0.0263(9) 0.0142(8) 0.0062(7) 0.0150(8) Cl2 0.0209(9) 0.0650(15) 0.0486(13) 0.0132(11) 0.0134(9) 0.0180(9) Cl3 0.0698(18) 0.0752(19) 0.0474(15) 0.0290(13) 0.0190(13) 0.0306(15) Cl4 0.075(2) 0.0471(16) 0.129(3) 0.0248(17) 0.056(2) 0.0183(15) Cl5 0.103(3) 0.0598(19) 0.095(2) -0.0049(17) 0.057(2) 0.0188(18) S 0.0293(9) 0.0273(9) 0.0254(9) 0.0116(7) 0.0093(7) 0.0158(8) P1 0.0177(8) 0.0191(8) 0.0187(8) 0.0048(7) 0.0056(7) 0.0061(6) P2 0.0165(8) 0.0197(8) 0.0186(8) 0.0051(7) 0.0059(6) 0.0069(6) N1 0.020(3) 0.018(3) 0.025(3) 0.006(2) 0.009(2) 0.007(2) N2 0.018(3) 0.020(3) 0.019(3) 0.006(2) 0.006(2) 0.007(2) C1 0.013(3) 0.016(3) 0.020(3) 0.005(2) 0.003(2) 0.001(2) C2 0.034(4) 0.032(4) 0.030(4) 0.012(3) 0.017(3) 0.022(3) C3 0.048(5) 0.035(4) 0.031(4) 0.008(3) 0.015(4) 0.025(4) C4 0.013(3) 0.019(3) 0.023(3) -0.001(3) 0.006(3) 0.002(2) C5 0.023(4) 0.032(4) 0.028(4) 0.010(3) 0.010(3) 0.005(3) C6 0.029(4) 0.032(4) 0.036(4) 0.012(3) 0.019(3) 0.002(3) C7 0.022(4) 0.031(4) 0.037(5) -0.004(3) 0.014(3) 0.002(3) C8 0.021(4) 0.038(5) 0.041(5) 0.003(4) 0.009(3) 0.009(3) C9 0.026(4) 0.031(4) 0.025(4) 0.008(3) 0.009(3) 0.009(3) C10 0.021(3) 0.016(3) 0.019(3) 0.004(2) 0.003(3) 0.006(3) C11 0.040(5) 0.030(4) 0.040(5) 0.004(4) 0.026(4) 0.003(4) C12 0.047(5) 0.024(4) 0.052(6) 0.003(4) 0.023(4) 0.010(4) C13 0.033(4) 0.021(4) 0.039(5) 0.004(3) 0.008(3) 0.006(3) C14 0.034(4) 0.023(4) 0.032(4) 0.004(3) 0.008(3) 0.001(3) C15 0.036(4) 0.020(3) 0.026(4) 0.002(3) 0.011(3) 0.005(3) C16 0.022(3) 0.021(3) 0.023(3) 0.004(3) 0.011(3) 0.007(3) C17 0.026(4) 0.029(4) 0.050(5) 0.011(4) 0.007(4) 0.008(3) C18 0.037(5) 0.025(4) 0.088(8) 0.022(5) 0.014(5) 0.008(4) C19 0.033(5) 0.029(5) 0.082(8) 0.003(5) 0.014(5) -0.004(4) C20 0.014(3) 0.039(5) 0.056(6) 0.007(4) 0.004(4) -0.004(3) C21 0.019(3) 0.027(4) 0.035(4) 0.007(3) 0.006(3) 0.007(3) C22 0.024(3) 0.022(3) 0.019(3) 0.004(3) 0.006(3) 0.010(3) C23 0.028(4) 0.028(4) 0.027(4) 0.005(3) 0.010(3) 0.006(3) C24 0.034(4) 0.036(4) 0.033(4) 0.009(4) 0.019(4) 0.013(3) C25 0.055(6) 0.036(5) 0.026(4) 0.002(3) 0.016(4) 0.019(4) C26 0.035(5) 0.039(5) 0.037(5) -0.010(4) 0.008(4) 0.002(4) C27 0.026(4) 0.034(4) 0.030(4) -0.003(3) 0.010(3) 0.005(3) C28 0.031(5) 0.053(6) 0.040(5) 0.014(4) 0.004(4) 0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.229(2) . ? Au1 Cl1 2.299(2) . ? Au2 P2 2.2212(17) . ? Au2 Cl2 2.2834(19) . ? Cl3 C28 1.736(9) . ? Cl4 C28 1.736(10) . ? Cl5 C28 1.765(10) . ? S C1 1.769(7) . ? S C3 1.834(8) . ? P1 N1 1.675(6) . ? P1 C4 1.802(6) . ? P1 C10 1.819(7) . ? P2 N2 1.713(6) . ? P2 C16 1.812(7) . ? P2 C22 1.813(7) . ? N1 C1 1.294(8) . ? N2 C1 1.379(8) . ? N2 C2 1.480(8) . ? C2 C3 1.503(11) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.400(10) . ? C4 C9 1.401(10) . ? C5 C6 1.379(10) . ? C5 H5 0.9500 . ? C6 C7 1.390(12) . ? C6 H6 0.9500 . ? C7 C8 1.394(12) . ? C7 H7 0.9500 . ? C8 C9 1.382(10) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C15 1.393(10) . ? C10 C11 1.395(10) . ? C11 C12 1.382(11) . ? C11 H11 0.9500 . ? C12 C13 1.370(11) . ? C12 H12 0.9500 . ? C13 C14 1.384(11) . ? C13 H13 0.9500 . ? C14 C15 1.377(10) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.389(10) . ? C16 C21 1.398(10) . ? C17 C18 1.380(11) . ? C17 H17 0.9500 . ? C18 C19 1.368(13) . ? C18 H18 0.9500 . ? C19 C20 1.380(13) . ? C19 H19 0.9500 . ? C20 C21 1.386(10) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.382(10) . ? C22 C27 1.384(10) . ? C23 C24 1.374(10) . ? C23 H23 0.9500 . ? C24 C25 1.357(12) . ? C24 H24 0.9500 . ? C25 C26 1.386(12) . ? C25 H25 0.9500 . ? C26 C27 1.373(11) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 H28 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 Cl1 174.99(7) . . ? P2 Au2 Cl2 177.44(7) . . ? C1 S C3 92.1(3) . . ? N1 P1 C4 107.1(3) . . ? N1 P1 C10 101.7(3) . . ? C4 P1 C10 103.7(3) . . ? N1 P1 Au1 117.2(2) . . ? C4 P1 Au1 114.2(2) . . ? C10 P1 Au1 111.4(2) . . ? N2 P2 C16 106.3(3) . . ? N2 P2 C22 101.4(3) . . ? C16 P2 C22 104.1(3) . . ? N2 P2 Au2 113.4(2) . . ? C16 P2 Au2 116.9(2) . . ? C22 P2 Au2 113.2(2) . . ? C1 N1 P1 124.8(5) . . ? C1 N2 C2 115.1(5) . . ? C1 N2 P2 117.7(4) . . ? C2 N2 P2 126.3(5) . . ? N1 C1 N2 120.1(6) . . ? N1 C1 S 128.7(5) . . ? N2 C1 S 111.2(5) . . ? N2 C2 C3 107.4(6) . . ? N2 C2 H2A 110.2 . . ? C3 C2 H2A 110.2 . . ? N2 C2 H2B 110.2 . . ? C3 C2 H2B 110.2 . . ? H2A C2 H2B 108.5 . . ? C2 C3 S 106.4(5) . . ? C2 C3 H3A 110.4 . . ? S C3 H3A 110.4 . . ? C2 C3 H3B 110.4 . . ? S C3 H3B 110.4 . . ? H3A C3 H3B 108.6 . . ? C5 C4 C9 119.7(6) . . ? C5 C4 P1 119.8(5) . . ? C9 C4 P1 120.4(5) . . ? C6 C5 C4 119.9(7) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C7 120.6(7) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C6 C7 C8 119.5(7) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C9 C8 C7 120.6(7) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C4 119.7(7) . . ? C8 C9 H9 120.2 . . ? C4 C9 H9 120.2 . . ? C15 C10 C11 120.0(6) . . ? C15 C10 P1 120.2(5) . . ? C11 C10 P1 119.7(5) . . ? C12 C11 C10 119.0(7) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C13 C12 C11 120.9(8) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C12 C13 C14 120.3(7) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C15 C14 C13 119.8(7) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C10 120.0(7) . . ? C14 C15 H15 120.0 . . ? C10 C15 H15 120.0 . . ? C17 C16 C21 119.2(7) . . ? C17 C16 P2 119.2(6) . . ? C21 C16 P2 121.4(5) . . ? C18 C17 C16 121.0(8) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C19 C18 C17 119.5(8) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C18 C19 C20 120.5(8) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C19 C20 C21 120.6(8) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C20 C21 C16 119.1(7) . . ? C20 C21 H21 120.4 . . ? C16 C21 H21 120.4 . . ? C23 C22 C27 119.9(7) . . ? C23 C22 P2 121.6(6) . . ? C27 C22 P2 118.5(5) . . ? C24 C23 C22 120.0(7) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C25 C24 C23 119.9(7) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 120.8(7) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C27 C26 C25 119.6(8) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C26 C27 C22 119.7(7) . . ? C26 C27 H27 120.1 . . ? C22 C27 H27 120.1 . . ? Cl3 C28 Cl4 111.7(5) . . ? Cl3 C28 Cl5 109.7(5) . . ? Cl4 C28 Cl5 109.9(5) . . ? Cl3 C28 H28 108.5 . . ? Cl4 C28 H28 108.5 . . ? Cl5 C28 H28 108.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.606 _refine_diff_density_min -3.783 _refine_diff_density_rms 0.315 # Attachment 'compound6.cif' data_compond6 _database_code_depnum_ccdc_archive 'CCDC 601678' _audit_creation_date 27-02-05 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H28 Ag N4 P2 Pt S2, C F3 O3 S, 3(C H2 Cl2)' _chemical_formula_sum 'C34 H34 Ag Cl6 F3 N4 O3 P2 Pt S3' _chemical_formula_weight 1277.43 _chemical_absolute_configuration . 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_int_tables_number 14 _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.185(3) _cell_length_b 19.488(6) _cell_length_c 25.892(9) _cell_angle_alpha 90.00 _cell_angle_beta 99.74(2) _cell_angle_gamma 90.00 _cell_volume 4568(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 12176 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.858 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2488 _exptl_absorpt_coefficient_mu 4.097 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22964 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.0538 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 30.03 _reflns_number_total 13265 _reflns_number_gt 10225 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0536P)^2^+18.1277P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13265 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0720 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1295 _refine_ls_wR_factor_gt 0.1198 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt 0.70001(2) 0.214335(10) 0.297622(7) 0.02646(6) Uani 1 1 d . . . Ag Ag 0.83662(5) -0.03655(2) 0.267267(18) 0.03585(11) Uani 1 1 d . . . Cl1 Cl 0.2181(5) 0.0010(4) 0.0117(2) 0.208(3) Uani 1 1 d . . . Cl2 Cl 0.1335(4) 0.0564(2) 0.10197(14) 0.1313(14) Uani 1 1 d . . . Cl3 Cl 0.9605(4) 0.22676(19) 0.42765(14) 0.1167(12) Uani 1 1 d . . . Cl4 Cl 0.9502(6) 0.3742(2) 0.4331(2) 0.174(2) Uani 1 1 d . . . Cl5 Cl 0.2216(14) -0.0070(5) 0.3703(4) 0.331(6) Uani 1 1 d . . . Cl6 Cl 0.1186(12) 0.0249(4) 0.4565(3) 0.302(5) Uani 1 1 d . . . S1 S 0.6897(3) 0.00494(9) 0.37619(8) 0.0610(5) Uani 1 1 d . . . S2 S 0.5282(2) 0.42135(8) 0.34421(6) 0.0439(4) Uani 1 1 d . . . S3 S 0.9812(3) 0.23989(15) 0.02623(8) 0.0710(6) Uani 1 1 d . . . P1 P 0.80679(15) 0.13085(7) 0.25836(5) 0.0282(3) Uani 1 1 d . . . P2 P 0.71552(16) 0.29822(7) 0.24017(5) 0.0276(3) Uani 1 1 d . . . F1 F 1.0064(17) 0.3686(5) 0.0350(5) 0.200(5) Uani 1 1 d . . . F2 F 0.7939(13) 0.3342(7) 0.0374(4) 0.218(6) Uani 1 1 d . . . F3 F 0.8707(9) 0.3352(7) -0.0358(4) 0.196(6) Uani 1 1 d . . . O1 O 0.8686(9) 0.1979(5) -0.0016(3) 0.121(3) Uani 1 1 d . . . O2 O 1.1112(7) 0.2425(4) 0.0035(2) 0.086(2) Uani 1 1 d . . . O3 O 1.0029(8) 0.2317(4) 0.0820(2) 0.084(2) Uani 1 1 d . . . N1 N 0.7851(5) 0.0605(2) 0.29415(19) 0.0329(10) Uani 1 1 d . . . N2 N 0.6841(5) 0.1339(2) 0.35015(18) 0.0334(10) Uani 1 1 d . . . N3 N 0.6416(5) 0.3673(2) 0.26532(18) 0.0330(10) Uani 1 1 d . . . N4 N 0.5980(5) 0.2926(2) 0.33318(17) 0.0319(10) Uani 1 1 d . . . C1 C 0.7232(6) 0.0733(3) 0.3357(2) 0.0337(11) Uani 1 1 d . . . C2 C 0.6086(8) 0.1314(3) 0.3963(3) 0.0466(15) Uani 1 1 d . . . H2A H 0.5002 0.1328 0.3848 0.056 Uiso 1 1 calc . . . H2B H 0.6380 0.1713 0.4193 0.056 Uiso 1 1 calc . . . C3 C 0.6525(12) 0.0648(4) 0.4260(3) 0.072(3) Uani 1 1 d . . . H3A H 0.5713 0.0479 0.4433 0.087 Uiso 1 1 calc . . . H3B H 0.7416 0.0717 0.4529 0.087 Uiso 1 1 calc . . . C4 C 0.5954(6) 0.3533(3) 0.3105(2) 0.0311(11) Uani 1 1 d . . . C5 C 0.5514(8) 0.2960(3) 0.3850(2) 0.0399(13) Uani 1 1 d . . . H5A H 0.6393 0.2956 0.4130 0.048 Uiso 1 1 calc . . . H5B H 0.4898 0.2556 0.3898 0.048 Uiso 1 1 calc . . . C6 C 0.4635(11) 0.3614(4) 0.3885(3) 0.068(2) Uani 1 1 d . . . H6A H 0.4812 0.3795 0.4248 0.082 Uiso 1 1 calc . . . H6B H 0.3564 0.3527 0.3779 0.082 Uiso 1 1 calc . . . C7 C 1.0032(6) 0.1385(3) 0.2598(2) 0.0324(11) Uani 1 1 d . . . C8 C 1.0846(7) 0.1862(3) 0.2922(3) 0.0453(15) Uani 1 1 d . . . H8 H 1.0359 0.2180 0.3112 0.054 Uiso 1 1 calc . . . C9 C 1.2380(8) 0.1878(4) 0.2969(3) 0.0577(19) Uani 1 1 d . . . H9 H 1.2933 0.2213 0.3185 0.069 Uiso 1 1 calc . . . C10 C 1.3092(8) 0.1412(5) 0.2704(3) 0.061(2) Uani 1 1 d . . . H10 H 1.4139 0.1421 0.2744 0.073 Uiso 1 1 calc . . . C11 C 1.2302(8) 0.0929(5) 0.2380(3) 0.058(2) Uani 1 1 d . . . H11 H 1.2805 0.0607 0.2197 0.070 Uiso 1 1 calc . . . C12 C 1.0771(7) 0.0915(3) 0.2323(3) 0.0431(14) Uani 1 1 d . . . H12 H 1.0224 0.0587 0.2098 0.052 Uiso 1 1 calc . . . C13 C 0.7280(6) 0.1068(3) 0.1923(2) 0.0315(11) Uani 1 1 d . . . C14 C 0.7830(7) 0.1319(3) 0.1492(2) 0.0367(12) Uani 1 1 d . . . H14 H 0.8661 0.1617 0.1541 0.044 Uiso 1 1 calc . . . C15 C 0.7160(8) 0.1135(4) 0.0988(3) 0.0487(15) Uani 1 1 d . . . H15 H 0.7530 0.1310 0.0694 0.058 Uiso 1 1 calc . . . C16 C 0.5977(9) 0.0703(4) 0.0916(3) 0.0566(18) Uani 1 1 d . . . H16 H 0.5529 0.0581 0.0571 0.068 Uiso 1 1 calc . . . C17 C 0.5417(8) 0.0440(4) 0.1341(3) 0.0508(17) Uani 1 1 d . . . H17 H 0.4600 0.0134 0.1287 0.061 Uiso 1 1 calc . . . C18 C 0.6059(6) 0.0627(3) 0.1843(2) 0.0380(13) Uani 1 1 d . . . H18 H 0.5669 0.0456 0.2135 0.046 Uiso 1 1 calc . . . C19 C 0.8997(6) 0.3265(3) 0.2338(2) 0.0315(11) Uani 1 1 d . . . C20 C 0.9772(7) 0.3663(3) 0.2741(3) 0.0436(14) Uani 1 1 d . . . H20 H 0.9306 0.3803 0.3025 0.052 Uiso 1 1 calc . . . C21 C 1.1204(8) 0.3852(4) 0.2730(3) 0.0562(18) Uani 1 1 d . . . H21 H 1.1726 0.4120 0.3008 0.067 Uiso 1 1 calc . . . C22 C 1.1896(8) 0.3655(4) 0.2318(4) 0.067(2) Uani 1 1 d . . . H22 H 1.2887 0.3792 0.2312 0.081 Uiso 1 1 calc . . . C23 C 1.1145(8) 0.3261(4) 0.1915(3) 0.0601(19) Uani 1 1 d . . . H23 H 1.1620 0.3121 0.1633 0.072 Uiso 1 1 calc . . . C24 C 0.9690(7) 0.3070(3) 0.1924(3) 0.0442(14) Uani 1 1 d . . . H24 H 0.9167 0.2804 0.1645 0.053 Uiso 1 1 calc . . . C25 C 0.6072(6) 0.2888(3) 0.1755(2) 0.0315(11) Uani 1 1 d . . . C26 C 0.6255(8) 0.3336(4) 0.1350(3) 0.0505(16) Uani 1 1 d . . . H26 H 0.7051 0.3653 0.1391 0.061 Uiso 1 1 calc . . . C27 C 0.5244(10) 0.3308(5) 0.0885(3) 0.070(2) Uani 1 1 d . . . H27 H 0.5357 0.3611 0.0608 0.083 Uiso 1 1 calc . . . C28 C 0.4107(9) 0.2859(5) 0.0818(3) 0.065(2) Uani 1 1 d . . . H28 H 0.3436 0.2848 0.0496 0.078 Uiso 1 1 calc . . . C29 C 0.3921(7) 0.2419(4) 0.1216(3) 0.0517(17) Uani 1 1 d . . . H29 H 0.3116 0.2107 0.1168 0.062 Uiso 1 1 calc . . . C30 C 0.4888(7) 0.2427(3) 0.1682(2) 0.0384(13) Uani 1 1 d . . . H30 H 0.4753 0.2120 0.1955 0.046 Uiso 1 1 calc . . . C31 C 0.9141(17) 0.3152(15) 0.0138(7) 0.195(11) Uani 1 1 d . . . C32 C 0.1639(15) 0.0742(7) 0.0398(5) 0.108(4) Uani 1 1 d . . . H32A H 0.0723 0.0922 0.0185 0.129 Uiso 1 1 calc . . . H32B H 0.2416 0.1097 0.0412 0.129 Uiso 1 1 calc . . . C33 C 1.0141(14) 0.2993(6) 0.4643(4) 0.095(4) Uani 1 1 d . . . H33A H 0.9769 0.2961 0.4980 0.114 Uiso 1 1 calc . . . H33B H 1.1233 0.3008 0.4723 0.114 Uiso 1 1 calc . . . C34 C 0.1193(17) 0.0504(9) 0.3958(6) 0.134(5) Uani 1 1 d . . . H34A H 0.1630 0.0968 0.3954 0.161 Uiso 1 1 calc . . . H34B H 0.0176 0.0516 0.3757 0.161 Uiso 1 1 calc . . . 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 Pt 0.03358(11) 0.01777(9) 0.02932(10) -0.00092(7) 0.00907(7) -0.00064(7) Ag 0.0473(2) 0.01722(18) 0.0464(2) 0.00079(16) 0.01756(19) 0.00002(16) Cl1 0.113(3) 0.297(7) 0.214(5) -0.168(5) 0.025(3) 0.005(4) Cl2 0.102(2) 0.191(4) 0.106(2) 0.040(2) 0.0294(18) -0.026(2) Cl3 0.099(2) 0.131(3) 0.112(2) -0.054(2) -0.0060(18) 0.0094(19) Cl4 0.207(5) 0.113(3) 0.176(4) 0.050(3) -0.043(4) -0.024(3) Cl5 0.426(15) 0.263(10) 0.363(12) -0.017(9) 0.236(12) 0.028(10) Cl6 0.436(13) 0.281(9) 0.161(5) 0.044(6) -0.029(7) -0.144(9) S1 0.0938(14) 0.0281(8) 0.0733(12) 0.0172(8) 0.0490(11) 0.0085(8) S2 0.0672(10) 0.0276(7) 0.0392(8) -0.0071(6) 0.0158(7) 0.0096(7) S3 0.0648(13) 0.0984(18) 0.0511(11) -0.0155(11) 0.0136(10) -0.0162(12) P1 0.0320(7) 0.0180(6) 0.0364(7) -0.0010(5) 0.0107(6) -0.0012(5) P2 0.0342(7) 0.0195(6) 0.0307(6) -0.0015(5) 0.0101(5) -0.0011(5) F1 0.252(14) 0.094(7) 0.258(14) -0.011(8) 0.058(11) 0.014(8) F2 0.245(11) 0.272(13) 0.185(9) 0.119(9) 0.171(9) 0.162(10) F3 0.125(6) 0.332(14) 0.151(7) 0.158(9) 0.083(6) 0.091(8) O1 0.089(6) 0.165(9) 0.101(6) -0.010(6) -0.007(5) -0.044(6) O2 0.061(4) 0.153(7) 0.046(3) -0.023(4) 0.013(3) -0.005(4) O3 0.107(5) 0.100(5) 0.047(3) -0.001(3) 0.021(3) -0.012(4) N1 0.038(2) 0.022(2) 0.042(3) 0.0011(18) 0.015(2) 0.0015(18) N2 0.047(3) 0.021(2) 0.036(2) 0.0044(18) 0.016(2) 0.0022(18) N3 0.043(3) 0.024(2) 0.034(2) 0.0030(18) 0.012(2) 0.0035(18) N4 0.044(3) 0.024(2) 0.030(2) -0.0039(17) 0.0142(19) 0.0013(18) C1 0.044(3) 0.017(2) 0.042(3) 0.004(2) 0.012(2) -0.003(2) C2 0.071(4) 0.034(3) 0.043(3) 0.004(3) 0.030(3) 0.006(3) C3 0.120(8) 0.046(4) 0.063(5) 0.018(4) 0.049(5) 0.022(5) C4 0.039(3) 0.023(2) 0.032(3) -0.004(2) 0.005(2) 0.002(2) C5 0.055(4) 0.034(3) 0.033(3) 0.000(2) 0.014(3) 0.005(3) C6 0.117(7) 0.045(4) 0.054(4) 0.007(3) 0.045(5) 0.030(4) C7 0.032(3) 0.025(2) 0.041(3) 0.005(2) 0.009(2) -0.001(2) C8 0.037(3) 0.038(3) 0.057(4) 0.002(3) -0.002(3) -0.004(3) C9 0.041(4) 0.052(4) 0.073(5) 0.006(4) -0.009(3) -0.013(3) C10 0.033(3) 0.070(5) 0.078(5) 0.014(4) 0.005(3) -0.003(3) C11 0.037(4) 0.076(6) 0.066(5) 0.007(4) 0.018(3) 0.010(3) C12 0.036(3) 0.040(3) 0.056(4) -0.005(3) 0.015(3) 0.001(2) C13 0.034(3) 0.021(2) 0.041(3) -0.006(2) 0.011(2) 0.004(2) C14 0.040(3) 0.031(3) 0.040(3) -0.003(2) 0.009(2) -0.002(2) C15 0.057(4) 0.050(4) 0.040(3) -0.005(3) 0.013(3) 0.000(3) C16 0.060(4) 0.066(5) 0.042(4) -0.016(3) 0.003(3) -0.001(4) C17 0.044(4) 0.048(4) 0.057(4) -0.017(3) -0.001(3) -0.004(3) C18 0.030(3) 0.037(3) 0.047(3) -0.006(3) 0.007(2) -0.005(2) C19 0.033(3) 0.021(2) 0.041(3) 0.003(2) 0.010(2) -0.004(2) C20 0.050(4) 0.030(3) 0.053(4) 0.001(3) 0.012(3) -0.008(3) C21 0.047(4) 0.048(4) 0.069(5) -0.003(3) -0.001(3) -0.019(3) C22 0.042(4) 0.058(5) 0.104(7) 0.010(5) 0.018(4) -0.010(3) C23 0.049(4) 0.060(5) 0.078(5) -0.002(4) 0.030(4) -0.005(3) C24 0.046(3) 0.036(3) 0.057(4) -0.005(3) 0.025(3) -0.005(3) C25 0.039(3) 0.025(2) 0.033(3) -0.002(2) 0.012(2) 0.000(2) C26 0.055(4) 0.055(4) 0.042(3) 0.005(3) 0.009(3) -0.008(3) C27 0.069(5) 0.098(7) 0.039(4) 0.019(4) 0.003(4) -0.006(5) C28 0.052(4) 0.099(7) 0.040(4) -0.005(4) -0.004(3) 0.010(4) C29 0.034(3) 0.057(4) 0.062(4) -0.015(4) 0.003(3) -0.005(3) C30 0.038(3) 0.034(3) 0.045(3) -0.006(2) 0.011(3) 0.001(2) C31 0.103(11) 0.36(3) 0.123(12) 0.162(17) 0.024(9) -0.022(15) C32 0.130(11) 0.102(9) 0.089(8) -0.008(7) 0.015(7) 0.013(8) C33 0.123(9) 0.081(7) 0.071(6) -0.002(5) -0.014(6) 0.012(6) C34 0.125(11) 0.164(15) 0.109(10) 0.044(10) 0.003(9) 0.034(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt N4 2.084(4) . ? Pt N2 2.096(4) . ? Pt P2 2.2309(14) . ? Pt P1 2.2314(14) . ? Ag N3 2.078(4) 2_645 ? Ag N1 2.096(5) . ? Cl1 C32 1.713(13) . ? Cl2 C32 1.714(13) . ? Cl3 C33 1.727(11) . ? Cl4 C33 1.723(11) . ? Cl5 C34 1.668(18) . ? Cl6 C34 1.648(15) . ? S1 C1 1.754(5) . ? S1 C3 1.813(8) . ? S2 C4 1.756(5) . ? S2 C6 1.807(8) . ? S3 O1 1.417(8) . ? S3 O2 1.419(6) . ? S3 O3 1.432(6) . ? S3 C31 1.60(3) . ? P1 N1 1.686(5) . ? P1 C13 1.802(6) . ? P1 C7 1.804(6) . ? P2 N3 1.687(5) . ? P2 C25 1.806(6) . ? P2 C19 1.814(6) . ? F1 C31 1.39(2) . ? F2 C31 1.40(2) . ? F3 C31 1.337(14) . ? N1 C1 1.324(7) . ? N2 C1 1.307(7) . ? N2 C2 1.479(7) . ? N3 C4 1.339(7) . ? N3 Ag 2.078(4) 2_655 ? N4 C4 1.319(7) . ? N4 C5 1.477(7) . ? C2 C3 1.527(10) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C5 C6 1.520(9) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.385(8) . ? C7 C12 1.404(8) . ? C8 C9 1.393(10) . ? C8 H8 0.9500 . ? C9 C10 1.368(12) . ? C9 H9 0.9500 . ? C10 C11 1.383(12) . ? C10 H10 0.9500 . ? C11 C12 1.389(9) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.389(8) . ? C13 C18 1.400(8) . ? C14 C15 1.393(9) . ? C14 H14 0.9500 . ? C15 C16 1.361(10) . ? C15 H15 0.9500 . ? C16 C17 1.389(11) . ? C16 H16 0.9500 . ? C17 C18 1.383(9) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.389(8) . ? C19 C20 1.395(8) . ? C20 C21 1.370(9) . ? C20 H20 0.9500 . ? C21 C22 1.386(12) . ? C21 H21 0.9500 . ? C22 C23 1.383(12) . ? C22 H22 0.9500 . ? C23 C24 1.391(9) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.398(8) . ? C25 C26 1.397(9) . ? C26 C27 1.391(10) . ? C26 H26 0.9500 . ? C27 C28 1.351(12) . ? C27 H27 0.9500 . ? C28 C29 1.372(12) . ? C28 H28 0.9500 . ? C29 C30 1.373(9) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? 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 N4 Pt N2 100.04(18) . . ? N4 Pt P2 80.95(13) . . ? N2 Pt P2 178.67(13) . . ? N4 Pt P1 179.09(14) . . ? N2 Pt P1 80.49(13) . . ? P2 Pt P1 98.51(5) . . ? N3 Ag N1 172.08(19) 2_645 . ? C1 S1 C3 90.5(3) . . ? C4 S2 C6 90.4(3) . . ? O1 S3 O2 113.8(5) . . ? O1 S3 O3 114.4(5) . . ? O2 S3 O3 116.0(4) . . ? O1 S3 C31 101.8(9) . . ? O2 S3 C31 101.9(6) . . ? O3 S3 C31 106.7(8) . . ? N1 P1 C13 104.1(3) . . ? N1 P1 C7 105.4(2) . . ? C13 P1 C7 106.3(3) . . ? N1 P1 Pt 103.94(17) . . ? C13 P1 Pt 119.02(18) . . ? C7 P1 Pt 116.47(19) . . ? N3 P2 C25 104.2(2) . . ? N3 P2 C19 103.6(2) . . ? C25 P2 C19 108.8(3) . . ? N3 P2 Pt 104.61(17) . . ? C25 P2 Pt 117.13(18) . . ? C19 P2 Pt 116.72(18) . . ? C1 N1 P1 113.6(4) . . ? C1 N1 Ag 126.4(4) . . ? P1 N1 Ag 119.8(3) . . ? C1 N2 C2 112.9(5) . . ? C1 N2 Pt 115.9(4) . . ? C2 N2 Pt 130.0(4) . . ? C4 N3 P2 112.5(4) . . ? C4 N3 Ag 127.3(4) . 2_655 ? P2 N3 Ag 119.4(2) . 2_655 ? C4 N4 C5 112.2(4) . . ? C4 N4 Pt 115.8(4) . . ? C5 N4 Pt 131.0(4) . . ? N2 C1 N1 125.5(5) . . ? N2 C1 S1 115.6(4) . . ? N1 C1 S1 119.0(4) . . ? N2 C2 C3 108.4(5) . . ? N2 C2 H2A 110.0 . . ? C3 C2 H2A 110.0 . . ? N2 C2 H2B 110.0 . . ? C3 C2 H2B 110.0 . . ? H2A C2 H2B 108.4 . . ? C2 C3 S1 104.7(5) . . ? C2 C3 H3A 110.8 . . ? S1 C3 H3A 110.8 . . ? C2 C3 H3B 110.8 . . ? S1 C3 H3B 110.8 . . ? H3A C3 H3B 108.9 . . ? N4 C4 N3 126.0(5) . . ? N4 C4 S2 116.0(4) . . ? N3 C4 S2 118.0(4) . . ? N4 C5 C6 109.3(5) . . ? N4 C5 H5A 109.8 . . ? C6 C5 H5A 109.8 . . ? N4 C5 H5B 109.8 . . ? C6 C5 H5B 109.8 . . ? H5A C5 H5B 108.3 . . ? C5 C6 S2 105.6(5) . . ? C5 C6 H6A 110.6 . . ? S2 C6 H6A 110.6 . . ? C5 C6 H6B 110.6 . . ? S2 C6 H6B 110.6 . . ? H6A C6 H6B 108.8 . . ? C8 C7 C12 119.2(5) . . ? C8 C7 P1 120.2(5) . . ? C12 C7 P1 120.2(4) . . ? C7 C8 C9 120.1(7) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C10 C9 C8 120.3(7) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 120.6(6) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C10 C11 C12 119.7(7) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C11 C12 C7 120.1(6) . . ? C11 C12 H12 120.0 . . ? C7 C12 H12 120.0 . . ? C14 C13 C18 119.2(5) . . ? C14 C13 P1 121.8(4) . . ? C18 C13 P1 118.9(4) . . ? C13 C14 C15 119.9(6) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C16 C15 C14 120.3(6) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C17 120.9(6) . . ? C15 C16 H16 119.5 . . ? C17 C16 H16 119.5 . . ? C18 C17 C16 119.4(6) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C17 C18 C13 120.4(6) . . ? C17 C18 H18 119.8 . . ? C13 C18 H18 119.8 . . ? C24 C19 C20 119.2(5) . . ? C24 C19 P2 122.9(4) . . ? C20 C19 P2 117.8(4) . . ? C21 C20 C19 120.2(6) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C22 120.6(7) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C23 C22 C21 119.9(7) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 119.6(7) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C19 C24 C23 120.4(6) . . ? C19 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C30 C25 C26 119.3(6) . . ? C30 C25 P2 119.0(4) . . ? C26 C25 P2 121.0(5) . . ? C27 C26 C25 118.5(7) . . ? C27 C26 H26 120.7 . . ? C25 C26 H26 120.7 . . ? C28 C27 C26 121.7(7) . . ? C28 C27 H27 119.1 . . ? C26 C27 H27 119.1 . . ? C27 C28 C29 120.0(7) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C28 C29 C30 120.6(7) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C29 C30 C25 120.0(6) . . ? C29 C30 H30 120.0 . . ? C25 C30 H30 120.0 . . ? F3 C31 F1 102.8(15) . . ? F3 C31 F2 102.3(13) . . ? F1 C31 F2 96(2) . . ? F3 C31 S3 120(2) . . ? F1 C31 S3 114.7(12) . . ? F2 C31 S3 117.4(10) . . ? Cl1 C32 Cl2 109.6(8) . . ? Cl1 C32 H32A 109.7 . . ? Cl2 C32 H32A 109.7 . . ? Cl1 C32 H32B 109.7 . . ? Cl2 C32 H32B 109.7 . . ? H32A C32 H32B 108.2 . . ? Cl4 C33 Cl3 113.1(6) . . ? Cl4 C33 H33A 109.0 . . ? Cl3 C33 H33A 109.0 . . ? Cl4 C33 H33B 109.0 . . ? Cl3 C33 H33B 109.0 . . ? H33A C33 H33B 107.8 . . ? Cl6 C34 Cl5 105.5(10) . . ? Cl6 C34 H34A 110.6 . . ? Cl5 C34 H34A 110.6 . . ? Cl6 C34 H34B 110.6 . . ? Cl5 C34 H34B 110.6 . . ? H34A C34 H34B 108.8 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.968 _refine_diff_density_min -2.310 _refine_diff_density_rms 0.159