# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_paper _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author ; Prof Mir Wais Hosseini Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universit\'e Louis Pasteur, F-67000 Strasbourg, France ; _publ_contact_author_email hosseini@chimie.u-strasbg.fr _publ_contact_author_fax '33 3 90 24 13 23' _publ_contact_author_phone '33 3 90 24 13 25' _publ_requested_category FM loop_ _publ_author_name _publ_author_address S.A.Baudron ; Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universit\'e Louis Pasteur, F-67000 Strasbourg, France ; M.W.Hosseini ; Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universit\'e Louis Pasteur, F-67000 Strasbourg, France ; _publ_section_title ; Modular construction of a series of heteronuclear metallamacrocycles ; _publ_contact_author_name 'Prof Mir Wais Hosseini' ###Material relevant to compound 7 at 173K ######## data_compound7 _database_code_depnum_ccdc_archive 'CCDC 690632' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C78 H64 Br2 Cu2 N4 P4 Pd2 S4, 2(C H2 Cl2)' _chemical_formula_sum 'C80 H68 Br2 Cl4 Cu2 N4 P4 Pd2 S4' _chemical_formula_weight 1979.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' _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 16.2955(4) _cell_length_b 9.4183(2) _cell_length_c 26.7138(7) _cell_angle_alpha 90.00 _cell_angle_beta 103.598(2) _cell_angle_gamma 90.00 _cell_volume 3985.00(17) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6902 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 23.63 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.649 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 2.339 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4864 _exptl_absorpt_correction_T_max 0.7354 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57135 _diffrn_reflns_av_R_equivalents 0.0682 _diffrn_reflns_av_sigmaI/netI 0.0539 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 27.59 _reflns_number_total 9202 _reflns_number_gt 6462 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0867P)^2^+5.5288P] 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 9202 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0844 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1612 _refine_ls_wR_factor_gt 0.1361 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4329(3) 0.0017(5) 0.38194(18) 0.0273(10) Uani 1 1 d . . . C2 C 0.4999(3) 0.0432(5) 0.5806(2) 0.0293(10) Uani 1 1 d . . . C3 C 0.4156(3) -0.0210(6) 0.56688(19) 0.0302(11) Uani 1 1 d . . . C4 C 0.3739(3) -0.1281(6) 0.5872(2) 0.0378(12) Uani 1 1 d . . . H4 H 0.3991 -0.1725 0.6181 0.045 Uiso 1 1 calc R . . C5 C 0.2946(4) -0.1657(7) 0.5601(2) 0.0429(14) Uani 1 1 d . . . H5 H 0.2657 -0.2371 0.5729 0.052 Uiso 1 1 calc R . . C6 C 0.2559(4) -0.0996(7) 0.5136(2) 0.0433(14) Uani 1 1 d . . . H6 H 0.2027 -0.1301 0.4960 0.052 Uiso 1 1 calc R . . C7 C 0.3706(3) 0.0411(6) 0.52088(19) 0.0317(11) Uani 1 1 d . . . C8 C 0.4220(3) 0.1487(5) 0.50536(19) 0.0299(11) Uani 1 1 d . . . C9 C 0.5004(3) 0.1526(5) 0.54085(19) 0.0294(11) Uani 1 1 d . . . C10 C 0.5588(3) 0.2518(5) 0.5308(2) 0.0328(11) Uani 1 1 d . . . H10 H 0.6122 0.2615 0.5524 0.039 Uiso 1 1 calc R . . C11 C 0.5326(4) 0.3349(6) 0.4870(2) 0.0380(12) Uani 1 1 d . . . H11 H 0.5694 0.4030 0.4795 0.046 Uiso 1 1 calc R . . C12 C 0.4538(4) 0.3196(6) 0.4540(2) 0.0387(13) Uani 1 1 d . . . H12 H 0.4397 0.3768 0.4249 0.046 Uiso 1 1 calc R . . C13 C 0.1622(4) 0.3353(6) 0.2282(3) 0.0446(14) Uani 1 1 d . . . H13A H 0.1538 0.3830 0.2588 0.054 Uiso 1 1 calc R . . H13B H 0.1582 0.4065 0.2015 0.054 Uiso 1 1 calc R . . C14 C 0.0911(3) 0.2285(7) 0.2107(2) 0.0432(14) Uani 1 1 d . . . H14A H 0.1045 0.1686 0.1841 0.052 Uiso 1 1 calc R . . H14B H 0.0395 0.2795 0.1956 0.052 Uiso 1 1 calc R . . C15 C 0.0756(3) 0.1338(6) 0.2543(2) 0.0405(13) Uani 1 1 d . . . H15A H 0.0214 0.0871 0.2428 0.049 Uiso 1 1 calc R . . H15B H 0.0728 0.1932 0.2835 0.049 Uiso 1 1 calc R . . C16 C 0.3337(3) 0.4145(6) 0.2640(2) 0.0359(12) Uani 1 1 d . . . C17 C 0.3869(4) 0.4766(7) 0.2363(2) 0.0445(14) Uani 1 1 d . . . H17 H 0.3923 0.4372 0.2053 0.053 Uiso 1 1 calc R . . C18 C 0.4317(4) 0.5976(8) 0.2554(3) 0.0572(18) Uani 1 1 d . . . H18 H 0.4672 0.6391 0.2370 0.069 Uiso 1 1 calc R . . C19 C 0.4249(4) 0.6576(7) 0.3011(3) 0.0517(16) Uani 1 1 d . . . H19 H 0.4544 0.7403 0.3129 0.062 Uiso 1 1 calc R . . C20 C 0.3749(4) 0.5954(7) 0.3288(2) 0.0471(15) Uani 1 1 d . . . H20 H 0.3708 0.6346 0.3601 0.057 Uiso 1 1 calc R . . C21 C 0.3296(4) 0.4732(6) 0.3107(2) 0.0429(13) Uani 1 1 d . . . H21 H 0.2962 0.4306 0.3303 0.051 Uiso 1 1 calc R . . C22 C 0.2899(4) 0.2080(6) 0.1813(2) 0.0408(13) Uani 1 1 d . . . C23 C 0.2568(4) 0.2829(7) 0.1359(2) 0.0498(16) Uani 1 1 d . . . H23 H 0.2199 0.3582 0.1358 0.060 Uiso 1 1 calc R . . C24 C 0.2794(5) 0.2442(8) 0.0914(3) 0.062(2) Uani 1 1 d . . . H24 H 0.2583 0.2946 0.0611 0.074 Uiso 1 1 calc R . . C25 C 0.3320(6) 0.1338(9) 0.0911(3) 0.073(2) Uani 1 1 d . . . H25 H 0.3462 0.1086 0.0606 0.087 Uiso 1 1 calc R . . C26 C 0.3650(5) 0.0579(8) 0.1351(3) 0.063(2) Uani 1 1 d . . . H26 H 0.4014 -0.0177 0.1344 0.076 Uiso 1 1 calc R . . C27 C 0.3437(4) 0.0945(7) 0.1806(3) 0.0504(15) Uani 1 1 d . . . H27 H 0.3654 0.0431 0.2105 0.060 Uiso 1 1 calc R . . C28 C 0.1224(3) -0.1058(6) 0.3237(2) 0.0337(12) Uani 1 1 d . . . C29 C 0.0805(4) -0.0413(6) 0.3574(2) 0.0419(13) Uani 1 1 d . . . H29 H 0.0664 0.0544 0.3535 0.050 Uiso 1 1 calc R . . C30 C 0.0596(4) -0.1191(7) 0.3969(2) 0.0488(16) Uani 1 1 d . . . H30 H 0.0313 -0.0757 0.4192 0.059 Uiso 1 1 calc R . . C31 C 0.0810(4) -0.2599(7) 0.4028(2) 0.0473(15) Uani 1 1 d . . . H31 H 0.0667 -0.3128 0.4289 0.057 Uiso 1 1 calc R . . C32 C 0.1236(4) -0.3222(7) 0.3701(3) 0.0533(17) Uani 1 1 d . . . H32 H 0.1388 -0.4173 0.3747 0.064 Uiso 1 1 calc R . . C33 C 0.1443(4) -0.2476(6) 0.3305(3) 0.0433(14) Uani 1 1 d . . . H33 H 0.1729 -0.2922 0.3085 0.052 Uiso 1 1 calc R . . C34 C 0.1469(3) -0.1197(6) 0.2206(2) 0.0351(12) Uani 1 1 d . . . C35 C 0.2185(4) -0.1928(6) 0.2145(2) 0.0388(13) Uani 1 1 d . . . H35 H 0.2702 -0.1793 0.2377 0.047 Uiso 1 1 calc R . . C36 C 0.2116(4) -0.2858(7) 0.1734(2) 0.0484(15) Uani 1 1 d . . . H36 H 0.2589 -0.3368 0.1701 0.058 Uiso 1 1 calc R . . C37 C 0.1370(4) -0.3042(7) 0.1378(2) 0.0481(15) Uani 1 1 d . . . H37 H 0.1340 -0.3653 0.1101 0.058 Uiso 1 1 calc R . . C38 C 0.0657(4) -0.2309(7) 0.1434(2) 0.0488(16) Uani 1 1 d . . . H38 H 0.0144 -0.2434 0.1196 0.059 Uiso 1 1 calc R . . C39 C 0.0714(4) -0.1404(7) 0.1840(2) 0.0408(13) Uani 1 1 d . . . H39 H 0.0236 -0.0912 0.1874 0.049 Uiso 1 1 calc R . . N1 N 0.2932(3) 0.0065(5) 0.49377(17) 0.0368(10) Uani 1 1 d . . . N2 N 0.3969(3) 0.2254(4) 0.46254(17) 0.0339(10) Uani 1 1 d . . . P1 P 0.26875(9) 0.25987(16) 0.24247(5) 0.0339(3) Uani 1 1 d . . . P2 P 0.15657(8) -0.00040(15) 0.27515(5) 0.0316(3) Uani 1 1 d . . . S1 S 0.43276(8) 0.13377(16) 0.33700(5) 0.0355(3) Uani 1 1 d . . . S2 S 0.32847(8) -0.06195(13) 0.37412(5) 0.0288(3) Uani 1 1 d . . . Cu1 Cu 0.28391(4) 0.12629(8) 0.41859(3) 0.04135(19) Uani 1 1 d . . . Br1 Br 0.17809(4) 0.29457(6) 0.38509(2) 0.04241(17) Uani 1 1 d . . . Pd1 Pd 0.28958(2) 0.08767(4) 0.303407(15) 0.02866(12) Uani 1 1 d . . . C40 C 0.1029(6) 0.1313(10) -0.0045(3) 0.085(3) Uani 1 1 d . . . H40A H 0.1596 0.1420 -0.0094 0.102 Uiso 1 1 calc R . . H40B H 0.0685 0.0883 -0.0354 0.102 Uiso 1 1 calc R . . Cl1 Cl 0.10554(18) 0.0180(3) 0.04787(11) 0.1103(9) Uani 1 1 d . . . Cl2 Cl 0.0622(2) 0.2989(3) 0.00391(11) 0.1076(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.030(2) 0.028(2) 0.026(2) -0.002(2) 0.011(2) 0.0019(19) C2 0.026(2) 0.031(2) 0.032(3) -0.002(2) 0.009(2) 0.003(2) C3 0.028(3) 0.038(3) 0.026(2) -0.004(2) 0.010(2) 0.006(2) C4 0.036(3) 0.049(3) 0.031(3) 0.001(2) 0.014(2) 0.003(2) C5 0.037(3) 0.058(4) 0.036(3) 0.002(3) 0.012(3) -0.011(3) C6 0.033(3) 0.065(4) 0.032(3) -0.005(3) 0.008(2) -0.007(3) C7 0.034(3) 0.036(3) 0.025(2) -0.007(2) 0.007(2) 0.008(2) C8 0.033(3) 0.031(2) 0.025(2) -0.005(2) 0.007(2) 0.007(2) C9 0.031(3) 0.031(2) 0.027(3) -0.003(2) 0.010(2) 0.004(2) C10 0.036(3) 0.031(3) 0.032(3) -0.007(2) 0.008(2) 0.004(2) C11 0.051(3) 0.028(2) 0.035(3) -0.002(2) 0.011(3) -0.002(2) C12 0.049(3) 0.029(3) 0.036(3) 0.003(2) 0.007(3) 0.007(2) C13 0.038(3) 0.038(3) 0.057(4) 0.017(3) 0.009(3) 0.003(2) C14 0.028(3) 0.054(3) 0.044(3) 0.015(3) 0.003(2) 0.007(2) C15 0.026(3) 0.043(3) 0.054(4) 0.009(3) 0.012(3) 0.002(2) C16 0.031(3) 0.043(3) 0.035(3) 0.006(2) 0.011(2) 0.004(2) C17 0.039(3) 0.058(4) 0.039(3) -0.003(3) 0.015(3) -0.011(3) C18 0.042(4) 0.079(5) 0.056(4) -0.012(4) 0.025(3) -0.022(3) C19 0.043(4) 0.056(4) 0.056(4) -0.011(3) 0.011(3) -0.008(3) C20 0.060(4) 0.044(3) 0.040(3) -0.005(3) 0.016(3) 0.004(3) C21 0.052(4) 0.041(3) 0.040(3) 0.003(3) 0.019(3) 0.005(3) C22 0.039(3) 0.046(3) 0.037(3) 0.004(3) 0.007(3) -0.013(3) C23 0.057(4) 0.056(4) 0.034(3) 0.010(3) 0.007(3) -0.014(3) C24 0.086(6) 0.061(4) 0.037(4) 0.005(3) 0.012(4) -0.028(4) C25 0.103(7) 0.077(5) 0.044(4) -0.014(4) 0.031(4) -0.040(5) C26 0.077(5) 0.062(4) 0.063(5) -0.013(4) 0.039(4) -0.008(4) C27 0.052(4) 0.060(4) 0.041(3) -0.005(3) 0.015(3) -0.003(3) C28 0.025(2) 0.038(3) 0.035(3) 0.005(2) 0.000(2) -0.005(2) C29 0.046(3) 0.041(3) 0.041(3) -0.005(3) 0.015(3) -0.011(3) C30 0.062(4) 0.050(4) 0.040(3) -0.008(3) 0.022(3) -0.017(3) C31 0.050(4) 0.052(4) 0.040(3) 0.011(3) 0.012(3) -0.012(3) C32 0.052(4) 0.039(3) 0.067(4) 0.020(3) 0.011(3) 0.000(3) C33 0.037(3) 0.035(3) 0.058(4) 0.008(3) 0.012(3) 0.007(2) C34 0.029(3) 0.045(3) 0.032(3) 0.003(2) 0.009(2) -0.002(2) C35 0.032(3) 0.046(3) 0.038(3) -0.002(3) 0.008(2) -0.001(2) C36 0.045(4) 0.057(4) 0.048(4) -0.007(3) 0.020(3) 0.001(3) C37 0.053(4) 0.056(4) 0.038(3) -0.001(3) 0.016(3) -0.011(3) C38 0.037(3) 0.072(4) 0.036(3) 0.005(3) 0.006(3) -0.021(3) C39 0.030(3) 0.056(3) 0.036(3) 0.004(3) 0.008(2) -0.003(3) N1 0.031(2) 0.048(3) 0.031(2) -0.002(2) 0.0059(19) 0.003(2) N2 0.041(3) 0.030(2) 0.029(2) -0.0008(19) 0.005(2) 0.0082(19) P1 0.0300(7) 0.0418(7) 0.0307(7) 0.0079(6) 0.0084(6) 0.0010(6) P2 0.0234(6) 0.0398(7) 0.0313(7) 0.0059(6) 0.0061(5) 0.0019(5) S1 0.0275(6) 0.0492(8) 0.0302(7) 0.0100(6) 0.0073(5) -0.0027(6) S2 0.0268(6) 0.0315(6) 0.0286(6) 0.0025(5) 0.0072(5) 0.0004(5) Cu1 0.0342(4) 0.0491(4) 0.0376(4) -0.0050(3) 0.0023(3) 0.0096(3) Br1 0.0371(3) 0.0391(3) 0.0518(4) 0.0036(3) 0.0119(3) 0.0084(2) Pd1 0.0240(2) 0.0359(2) 0.0267(2) 0.00477(16) 0.00703(15) 0.00169(15) C40 0.097(7) 0.094(7) 0.071(6) 0.008(5) 0.031(5) -0.005(5) Cl1 0.1005(19) 0.128(2) 0.0975(19) 0.0239(17) 0.0140(15) -0.0377(17) Cl2 0.125(2) 0.115(2) 0.0959(18) 0.0002(16) 0.0533(17) 0.0002(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.365(7) 3_656 ? C1 S1 1.728(5) . ? C1 S2 1.770(5) . ? C2 C1 1.365(7) 3_656 ? C2 C3 1.467(7) . ? C2 C9 1.482(7) . ? C3 C4 1.395(8) . ? C3 C7 1.402(7) . ? C4 C5 1.373(8) . ? C4 H4 0.9300 . ? C5 C6 1.398(8) . ? C5 H5 0.9300 . ? C6 N1 1.342(8) . ? C6 H6 0.9300 . ? C7 N1 1.340(7) . ? C7 C8 1.436(8) . ? C8 N2 1.333(7) . ? C8 C9 1.401(7) . ? C9 C10 1.403(7) . ? C10 C11 1.389(8) . ? C10 H10 0.9300 . ? C11 C12 1.384(8) . ? C11 H11 0.9300 . ? C12 N2 1.341(7) . ? C12 H12 0.9300 . ? C13 C14 1.522(8) . ? C13 P1 1.832(6) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.534(8) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 P2 1.818(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C21 1.380(8) . ? C16 C17 1.395(8) . ? C16 P1 1.813(6) . ? C17 C18 1.385(9) . ? C17 H17 0.9300 . ? C18 C19 1.371(9) . ? C18 H18 0.9300 . ? C19 C20 1.357(9) . ? C19 H19 0.9300 . ? C20 C21 1.391(9) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C27 1.386(9) . ? C22 C23 1.398(8) . ? C22 P1 1.814(6) . ? C23 C24 1.374(10) . ? C23 H23 0.9300 . ? C24 C25 1.348(12) . ? C24 H24 0.9300 . ? C25 C26 1.373(11) . ? C25 H25 0.9300 . ? C26 C27 1.382(9) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C33 1.384(8) . ? C28 C29 1.391(8) . ? C28 P2 1.821(6) . ? C29 C30 1.390(8) . ? C29 H29 0.9300 . ? C30 C31 1.371(9) . ? C30 H30 0.9300 . ? C31 C32 1.369(10) . ? C31 H31 0.9300 . ? C32 C33 1.376(9) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C39 1.393(7) . ? C34 C35 1.395(8) . ? C34 P2 1.818(6) . ? C35 C36 1.387(8) . ? C35 H35 0.9300 . ? C36 C37 1.368(9) . ? C36 H36 0.9300 . ? C37 C38 1.389(9) . ? C37 H37 0.9300 . ? C38 C39 1.366(9) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? N1 Cu1 2.278(5) . ? N2 Cu1 2.150(5) . ? P1 Pd1 2.2661(14) . ? P2 Pd1 2.2774(14) . ? S1 Pd1 2.3352(14) . ? S2 Pd1 2.3223(13) . ? S2 Cu1 2.3425(14) . ? Cu1 Br1 2.3581(9) . ? Cu1 Pd1 3.1211(8) . ? C40 Cl2 1.747(10) . ? C40 Cl1 1.752(9) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? 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 C2 C1 S1 127.0(4) 3_656 . ? C2 C1 S2 124.4(4) 3_656 . ? S1 C1 S2 108.5(3) . . ? C1 C2 C3 126.8(5) 3_656 . ? C1 C2 C9 127.0(5) 3_656 . ? C3 C2 C9 105.7(4) . . ? C4 C3 C7 116.2(5) . . ? C4 C3 C2 135.5(5) . . ? C7 C3 C2 108.2(5) . . ? C5 C4 C3 117.7(5) . . ? C5 C4 H4 121.1 . . ? C3 C4 H4 121.1 . . ? C4 C5 C6 121.7(6) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? N1 C6 C5 122.1(5) . . ? N1 C6 H6 119.0 . . ? C5 C6 H6 119.0 . . ? N1 C7 C3 127.1(5) . . ? N1 C7 C8 123.7(5) . . ? C3 C7 C8 109.1(4) . . ? N2 C8 C9 127.9(5) . . ? N2 C8 C7 123.2(5) . . ? C9 C8 C7 108.9(4) . . ? C8 C9 C10 116.0(5) . . ? C8 C9 C2 108.0(4) . . ? C10 C9 C2 136.0(5) . . ? C11 C10 C9 116.7(5) . . ? C11 C10 H10 121.6 . . ? C9 C10 H10 121.6 . . ? C12 C11 C10 122.2(5) . . ? C12 C11 H11 118.9 . . ? C10 C11 H11 118.9 . . ? N2 C12 C11 122.4(5) . . ? N2 C12 H12 118.8 . . ? C11 C12 H12 118.8 . . ? C14 C13 P1 115.1(4) . . ? C14 C13 H13A 108.5 . . ? P1 C13 H13A 108.5 . . ? C14 C13 H13B 108.5 . . ? P1 C13 H13B 108.5 . . ? H13A C13 H13B 107.5 . . ? C13 C14 C15 113.6(5) . . ? C13 C14 H14A 108.8 . . ? C15 C14 H14A 108.8 . . ? C13 C14 H14B 108.8 . . ? C15 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? C14 C15 P2 113.6(4) . . ? C14 C15 H15A 108.9 . . ? P2 C15 H15A 108.9 . . ? C14 C15 H15B 108.9 . . ? P2 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? C21 C16 C17 118.7(5) . . ? C21 C16 P1 117.4(4) . . ? C17 C16 P1 123.9(4) . . ? C18 C17 C16 119.2(6) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? C19 C18 C17 121.5(6) . . ? C19 C18 H18 119.2 . . ? C17 C18 H18 119.2 . . ? C20 C19 C18 119.4(6) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C19 C20 C21 120.4(6) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C16 C21 C20 120.7(6) . . ? C16 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C27 C22 C23 119.5(6) . . ? C27 C22 P1 118.4(5) . . ? C23 C22 P1 122.0(5) . . ? C24 C23 C22 119.4(7) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C25 C24 C23 120.6(7) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 121.3(7) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C25 C26 C27 119.6(8) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? C26 C27 C22 119.7(7) . . ? C26 C27 H27 120.1 . . ? C22 C27 H27 120.1 . . ? C33 C28 C29 119.1(5) . . ? C33 C28 P2 120.5(5) . . ? C29 C28 P2 120.1(4) . . ? C30 C29 C28 120.4(6) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C31 C30 C29 119.7(6) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C32 C31 C30 119.6(6) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C31 C32 C33 121.7(6) . . ? C31 C32 H32 119.2 . . ? C33 C32 H32 119.2 . . ? C32 C33 C28 119.4(6) . . ? C32 C33 H33 120.3 . . ? C28 C33 H33 120.3 . . ? C39 C34 C35 118.3(5) . . ? C39 C34 P2 123.0(4) . . ? C35 C34 P2 118.8(4) . . ? C36 C35 C34 119.3(5) . . ? C36 C35 H35 120.4 . . ? C34 C35 H35 120.4 . . ? C37 C36 C35 121.5(6) . . ? C37 C36 H36 119.2 . . ? C35 C36 H36 119.2 . . ? C36 C37 C38 119.5(6) . . ? C36 C37 H37 120.3 . . ? C38 C37 H37 120.3 . . ? C39 C38 C37 119.5(6) . . ? C39 C38 H38 120.3 . . ? C37 C38 H38 120.3 . . ? C38 C39 C34 121.9(6) . . ? C38 C39 H39 119.0 . . ? C34 C39 H39 119.0 . . ? C7 N1 C6 115.1(5) . . ? C7 N1 Cu1 102.4(3) . . ? C6 N1 Cu1 140.8(4) . . ? C8 N2 C12 114.8(5) . . ? C8 N2 Cu1 106.5(3) . . ? C12 N2 Cu1 137.0(4) . . ? C16 P1 C22 106.4(3) . . ? C16 P1 C13 102.0(3) . . ? C22 P1 C13 106.7(3) . . ? C16 P1 Pd1 111.69(18) . . ? C22 P1 Pd1 115.2(2) . . ? C13 P1 Pd1 113.7(2) . . ? C15 P2 C34 105.3(3) . . ? C15 P2 C28 106.0(3) . . ? C34 P2 C28 104.5(3) . . ? C15 P2 Pd1 114.45(19) . . ? C34 P2 Pd1 112.76(18) . . ? C28 P2 Pd1 112.87(17) . . ? C1 S1 Pd1 88.36(17) . . ? C1 S2 Pd1 87.79(16) . . ? C1 S2 Cu1 95.05(16) . . ? Pd1 S2 Cu1 83.99(5) . . ? N2 Cu1 N1 82.11(17) . . ? N2 Cu1 S2 106.14(12) . . ? N1 Cu1 S2 96.20(12) . . ? N2 Cu1 Br1 111.79(11) . . ? N1 Cu1 Br1 123.95(12) . . ? S2 Cu1 Br1 127.05(5) . . ? N2 Cu1 Pd1 111.66(12) . . ? N1 Cu1 Pd1 143.17(12) . . ? S2 Cu1 Pd1 47.73(3) . . ? Br1 Cu1 Pd1 83.84(3) . . ? P1 Pd1 P2 93.00(5) . . ? P1 Pd1 S2 169.97(5) . . ? P2 Pd1 S2 96.03(5) . . ? P1 Pd1 S1 96.34(5) . . ? P2 Pd1 S1 169.17(5) . . ? S2 Pd1 S1 75.13(5) . . ? P1 Pd1 Cu1 126.20(4) . . ? P2 Pd1 Cu1 97.05(4) . . ? S2 Pd1 Cu1 48.28(3) . . ? S1 Pd1 Cu1 81.84(4) . . ? Cl2 C40 Cl1 112.7(5) . . ? Cl2 C40 H40A 109.0 . . ? Cl1 C40 H40A 109.0 . . ? Cl2 C40 H40B 109.0 . . ? Cl1 C40 H40B 109.0 . . ? H40A C40 H40B 107.8 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.271 _refine_diff_density_min -1.202 _refine_diff_density_rms 0.192 #===END ###Material relevant to compound 8 at 173K ## data_compound8 _database_code_depnum_ccdc_archive 'CCDC 690633' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C82 H64 Br2 Cu2 N4 P4 Pd2 S8, 6(C H Cl3)' _chemical_formula_sum 'C88 H70 Br2 Cl18 Cu2 N4 P4 Pd2 S8' _chemical_formula_weight 2701.64 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.5736(5) _cell_length_b 13.6129(6) _cell_length_c 14.8510(6) _cell_angle_alpha 69.876(2) _cell_angle_beta 87.186(2) _cell_angle_gamma 82.441(2) _cell_volume 2554.17(18) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5838 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 27.53 _exptl_crystal_description rod _exptl_crystal_colour orange-brown _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.756 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1340 _exptl_absorpt_coefficient_mu 2.283 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6456 _exptl_absorpt_correction_T_max 0.9347 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29900 _diffrn_reflns_av_R_equivalents 0.0593 _diffrn_reflns_av_sigmaI/netI 0.0914 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 27.44 _reflns_number_total 11264 _reflns_number_gt 8365 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1194P)^2^+24.7745P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0218(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11264 _refine_ls_number_parameters 578 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1289 _refine_ls_R_factor_gt 0.0961 _refine_ls_wR_factor_ref 0.2714 _refine_ls_wR_factor_gt 0.2409 _refine_ls_goodness_of_fit_ref 1.130 _refine_ls_restrained_S_all 1.131 _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 C1 C 0.0448(7) 0.0866(7) 0.2222(6) 0.0208(18) Uani 1 1 d . . . C2 C 0.0446(6) 0.1890(7) 0.1660(6) 0.0204(18) Uani 1 1 d . . . C3 C 0.0684(7) -0.1092(8) -0.0789(6) 0.0239(19) Uani 1 1 d . . . C4 C 0.1207(7) -0.0905(7) -0.0105(6) 0.0208(18) Uani 1 1 d . . . C5 C 0.1560(6) 0.0093(7) -0.0178(6) 0.0198(17) Uani 1 1 d . . . C6 C 0.1521(7) 0.1098(7) -0.0876(7) 0.0241(19) Uani 1 1 d . . . H6 H 0.1224 0.1251 -0.1468 0.029 Uiso 1 1 calc R . . C7 C 0.1941(8) 0.1854(8) -0.0650(7) 0.029(2) Uani 1 1 d . . . H7 H 0.1939 0.2524 -0.1105 0.035 Uiso 1 1 calc R . . C8 C 0.2365(8) 0.1641(9) 0.0241(7) 0.032(2) Uani 1 1 d . . . H8 H 0.2618 0.2178 0.0375 0.039 Uiso 1 1 calc R . . C9 C 0.2046(7) -0.0059(7) 0.0675(6) 0.0214(18) Uani 1 1 d . . . C10 C 0.2009(7) -0.1125(7) 0.1306(6) 0.0199(17) Uani 1 1 d . . . C11 C 0.1519(6) -0.1665(7) 0.0839(6) 0.0180(17) Uani 1 1 d . . . C12 C 0.1406(8) -0.2699(7) 0.1360(7) 0.028(2) Uani 1 1 d . . . H12 H 0.1086 -0.3101 0.1098 0.033 Uiso 1 1 calc R . . C13 C 0.1779(8) -0.3125(8) 0.2283(7) 0.031(2) Uani 1 1 d . . . H13 H 0.1723 -0.3827 0.2639 0.037 Uiso 1 1 calc R . . C14 C 0.2235(8) -0.2521(7) 0.2685(7) 0.028(2) Uani 1 1 d . . . H14 H 0.2456 -0.2824 0.3315 0.033 Uiso 1 1 calc R . . C15 C 0.4241(7) 0.2307(8) 0.3688(7) 0.028(2) Uani 1 1 d . . . H15A H 0.4541 0.1816 0.3382 0.033 Uiso 1 1 calc R . . H15B H 0.4658 0.2868 0.3550 0.033 Uiso 1 1 calc R . . C16 C 0.4227(7) 0.1734(7) 0.4773(7) 0.026(2) Uani 1 1 d . . . H16A H 0.3860 0.2204 0.5070 0.031 Uiso 1 1 calc R . . H16B H 0.4905 0.1594 0.5004 0.031 Uiso 1 1 calc R . . C17 C 0.3771(7) 0.0684(8) 0.5115(7) 0.027(2) Uani 1 1 d . . . H17A H 0.3840 0.0378 0.5806 0.032 Uiso 1 1 calc R . . H17B H 0.4159 0.0203 0.4841 0.032 Uiso 1 1 calc R . . C18 C 0.2243(7) -0.0627(7) 0.5318(7) 0.0220(18) Uani 1 1 d . . . C19 C 0.2822(7) -0.1351(7) 0.4996(7) 0.028(2) Uani 1 1 d . . . H19 H 0.3320 -0.1133 0.4545 0.034 Uiso 1 1 calc R . . C20 C 0.2664(9) -0.2403(8) 0.5341(7) 0.033(2) Uani 1 1 d . . . H20 H 0.3055 -0.2892 0.5126 0.040 Uiso 1 1 calc R . . C21 C 0.1910(9) -0.2719(8) 0.6015(8) 0.034(2) Uani 1 1 d . . . H21 H 0.1793 -0.3421 0.6245 0.041 Uiso 1 1 calc R . . C22 C 0.1343(9) -0.1998(8) 0.6337(8) 0.034(2) Uani 1 1 d . . . H22 H 0.0849 -0.2219 0.6792 0.041 Uiso 1 1 calc R . . C23 C 0.1492(8) -0.0949(8) 0.6000(7) 0.031(2) Uani 1 1 d . . . H23 H 0.1102 -0.0464 0.6221 0.038 Uiso 1 1 calc R . . C24 C 0.1730(7) 0.1435(7) 0.5520(7) 0.0244(19) Uani 1 1 d . . . C25 C 0.2143(8) 0.1830(7) 0.6149(7) 0.028(2) Uani 1 1 d . . . H25 H 0.2822 0.1694 0.6270 0.033 Uiso 1 1 calc R . . C26 C 0.1514(9) 0.2442(8) 0.6601(7) 0.034(2) Uani 1 1 d . . . H26 H 0.1790 0.2741 0.6991 0.040 Uiso 1 1 calc R . . C27 C 0.0519(9) 0.2596(8) 0.6470(8) 0.036(2) Uani 1 1 d . . . H27 H 0.0116 0.2982 0.6786 0.043 Uiso 1 1 calc R . . C28 C 0.0094(8) 0.2188(8) 0.5874(8) 0.034(2) Uani 1 1 d . . . H28 H -0.0593 0.2290 0.5799 0.040 Uiso 1 1 calc R . . C29 C 0.0692(8) 0.1620(8) 0.5382(7) 0.029(2) Uani 1 1 d . . . H29 H 0.0406 0.1365 0.4964 0.035 Uiso 1 1 calc R . . C30 C 0.3335(7) 0.3622(7) 0.1949(7) 0.025(2) Uani 1 1 d . . . C31 C 0.3797(9) 0.3124(8) 0.1339(8) 0.034(2) Uani 1 1 d . . . H31 H 0.3951 0.2394 0.1569 0.041 Uiso 1 1 calc R . . C32 C 0.4029(8) 0.3668(10) 0.0419(8) 0.039(3) Uani 1 1 d . . . H32 H 0.4352 0.3310 0.0035 0.047 Uiso 1 1 calc R . . C33 C 0.3797(10) 0.4721(10) 0.0056(8) 0.044(3) Uani 1 1 d . . . H33 H 0.3953 0.5084 -0.0578 0.053 Uiso 1 1 calc R . . C34 C 0.3336(12) 0.5256(11) 0.0613(9) 0.058(4) Uani 1 1 d . . . H34 H 0.3183 0.5984 0.0358 0.070 Uiso 1 1 calc R . . C35 C 0.3093(10) 0.4718(9) 0.1564(9) 0.044(3) Uani 1 1 d . . . H35 H 0.2772 0.5085 0.1941 0.053 Uiso 1 1 calc R . . C36 C 0.2529(7) 0.3805(7) 0.3754(7) 0.0238(19) Uani 1 1 d . . . C37 C 0.3128(9) 0.4286(8) 0.4160(8) 0.035(2) Uani 1 1 d . . . H37 H 0.3815 0.4176 0.4096 0.042 Uiso 1 1 calc R . . C38 C 0.2714(10) 0.4928(9) 0.4660(8) 0.042(3) Uani 1 1 d . . . H38 H 0.3121 0.5237 0.4943 0.050 Uiso 1 1 calc R . . C39 C 0.1705(10) 0.5108(8) 0.4736(8) 0.041(3) Uani 1 1 d . . . H39 H 0.1428 0.5543 0.5071 0.050 Uiso 1 1 calc R . . C40 C 0.1095(9) 0.4655(8) 0.4323(8) 0.034(2) Uani 1 1 d . . . H40 H 0.0408 0.4796 0.4363 0.041 Uiso 1 1 calc R . . C41 C 0.1514(8) 0.3985(7) 0.3843(7) 0.026(2) Uani 1 1 d . . . H41 H 0.1106 0.3656 0.3582 0.031 Uiso 1 1 calc R . . N1 N 0.2420(6) 0.0658(6) 0.0926(6) 0.0267(17) Uani 1 1 d . . . N2 N 0.2367(6) -0.1515(6) 0.2198(5) 0.0232(16) Uani 1 1 d . . . P1 P 0.24623(17) 0.07596(18) 0.48176(16) 0.0197(5) Uani 1 1 d . . . P2 P 0.30232(18) 0.28703(18) 0.31633(17) 0.0213(5) Uani 1 1 d . . . S1 S 0.12176(17) 0.02415(17) 0.32317(15) 0.0208(5) Uani 1 1 d . . . S2 S 0.11707(19) 0.27520(17) 0.18659(17) 0.0254(5) Uani 1 1 d . . . S3 S -0.02683(17) 0.01033(18) 0.18495(16) 0.0228(5) Uani 1 1 d . . . S4 S -0.03013(18) 0.23074(18) 0.06484(16) 0.0246(5) Uani 1 1 d . . . Cu1 Cu 0.27220(9) 0.00063(10) 0.24372(9) 0.0285(3) Uani 1 1 d . . . Br1 Br 0.44090(9) -0.01116(10) 0.28225(9) 0.0425(3) Uani 1 1 d . . . Pd1 Pd 0.20031(5) 0.16419(5) 0.32614(5) 0.0179(2) Uani 1 1 d . . . C42 C 0.4980(13) 0.7220(19) 0.2600(13) 0.085(6) Uani 1 1 d . . . H42 H 0.4500 0.7856 0.2462 0.101 Uiso 1 1 calc R . . Cl1 Cl 0.4544(4) 0.6440(6) 0.2042(4) 0.108(2) Uani 1 1 d . . . Cl2 Cl 0.4975(5) 0.6593(5) 0.3851(4) 0.112(2) Uani 1 1 d . . . Cl3 Cl 0.6082(4) 0.7625(7) 0.2156(7) 0.150(3) Uani 1 1 d . . . C43 C 0.3665(18) 0.8532(14) 0.8292(12) 0.089(6) Uani 1 1 d . . . H43 H 0.4322 0.8713 0.8037 0.106 Uiso 1 1 calc R . . Cl4 Cl 0.3755(5) 0.8166(5) 0.9584(4) 0.115(2) Uani 1 1 d . . . Cl5 Cl 0.2890(4) 0.9592(5) 0.7809(4) 0.0976(17) Uani 1 1 d . . . Cl6 Cl 0.3488(5) 0.7434(5) 0.8010(5) 0.117(2) Uani 1 1 d . . . C44 C 0.8655(12) 0.4912(17) 0.1700(10) 0.21(2) Uani 1 1 d D . . H44 H 0.8781 0.4141 0.1901 0.253 Uiso 1 1 calc R . . Cl7 Cl 0.9449(9) 0.5294(8) 0.2317(8) 0.187(4) Uani 1 1 d D . . Cl8 Cl 0.7456(12) 0.5216(15) 0.2021(11) 0.304(9) Uani 1 1 d D . . Cl9 Cl 0.8808(9) 0.5375(10) 0.0504(9) 0.200(4) Uani 1 1 d 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 C1 0.021(4) 0.020(4) 0.024(4) -0.012(4) -0.002(3) -0.002(3) C2 0.020(4) 0.020(4) 0.021(4) -0.007(3) -0.006(3) 0.001(3) C3 0.024(4) 0.031(5) 0.020(4) -0.010(4) 0.003(4) -0.011(4) C4 0.025(4) 0.022(4) 0.015(4) -0.008(3) -0.002(3) -0.001(4) C5 0.018(4) 0.019(4) 0.023(4) -0.009(3) 0.000(3) -0.001(3) C6 0.030(5) 0.020(4) 0.022(4) -0.006(4) -0.008(4) -0.002(4) C7 0.039(5) 0.019(4) 0.025(5) -0.003(4) -0.004(4) -0.004(4) C8 0.044(6) 0.035(6) 0.022(5) -0.012(4) 0.000(4) -0.017(5) C9 0.023(4) 0.024(4) 0.021(4) -0.012(4) -0.001(3) -0.006(4) C10 0.024(4) 0.019(4) 0.020(4) -0.011(3) -0.001(3) -0.004(3) C11 0.023(4) 0.014(4) 0.018(4) -0.007(3) -0.004(3) -0.002(3) C12 0.038(5) 0.015(4) 0.027(5) -0.004(4) -0.002(4) -0.003(4) C13 0.041(6) 0.019(4) 0.028(5) -0.003(4) -0.006(4) 0.003(4) C14 0.036(5) 0.023(5) 0.021(4) -0.004(4) -0.010(4) 0.004(4) C15 0.029(5) 0.026(5) 0.031(5) -0.012(4) -0.004(4) -0.008(4) C16 0.021(4) 0.025(5) 0.036(5) -0.013(4) -0.014(4) -0.003(4) C17 0.033(5) 0.025(5) 0.023(4) -0.010(4) -0.005(4) -0.002(4) C18 0.023(4) 0.016(4) 0.028(4) -0.009(4) -0.001(4) -0.003(3) C19 0.027(5) 0.021(5) 0.036(5) -0.008(4) -0.008(4) -0.001(4) C20 0.044(6) 0.030(5) 0.031(5) -0.018(4) 0.002(5) -0.003(5) C21 0.048(6) 0.020(5) 0.036(5) -0.010(4) -0.001(5) -0.011(4) C22 0.045(6) 0.028(5) 0.031(5) -0.013(4) 0.007(5) -0.011(5) C23 0.041(6) 0.021(5) 0.027(5) -0.003(4) 0.001(4) -0.004(4) C24 0.029(5) 0.018(4) 0.023(4) -0.005(4) 0.000(4) 0.001(4) C25 0.037(5) 0.023(5) 0.024(5) -0.008(4) -0.007(4) -0.004(4) C26 0.064(7) 0.021(5) 0.020(4) -0.011(4) 0.004(5) -0.009(5) C27 0.046(6) 0.021(5) 0.037(6) -0.007(4) 0.011(5) -0.004(5) C28 0.032(5) 0.028(5) 0.038(6) -0.008(4) 0.007(5) -0.006(4) C29 0.032(5) 0.026(5) 0.029(5) -0.010(4) 0.000(4) -0.001(4) C30 0.034(5) 0.020(4) 0.025(4) -0.010(4) -0.007(4) -0.005(4) C31 0.050(7) 0.022(5) 0.034(5) -0.015(4) -0.001(5) 0.000(5) C32 0.036(6) 0.051(7) 0.028(5) -0.011(5) 0.003(4) -0.007(5) C33 0.055(7) 0.046(7) 0.030(5) -0.008(5) 0.005(5) -0.021(6) C34 0.087(11) 0.037(7) 0.038(7) 0.005(6) 0.004(7) -0.012(7) C35 0.063(8) 0.024(5) 0.043(6) -0.006(5) 0.015(6) -0.012(5) C36 0.036(5) 0.011(4) 0.025(4) -0.007(3) -0.003(4) -0.003(4) C37 0.045(6) 0.025(5) 0.040(6) -0.014(4) -0.019(5) -0.002(4) C38 0.061(8) 0.028(5) 0.045(6) -0.018(5) -0.023(6) -0.006(5) C39 0.071(9) 0.021(5) 0.035(6) -0.015(4) 0.007(6) -0.003(5) C40 0.047(6) 0.023(5) 0.035(5) -0.013(4) 0.010(5) -0.007(4) C41 0.035(5) 0.019(4) 0.024(4) -0.010(4) 0.007(4) -0.005(4) N1 0.030(4) 0.027(4) 0.026(4) -0.010(3) -0.005(3) -0.009(3) N2 0.024(4) 0.026(4) 0.022(4) -0.013(3) -0.001(3) 0.002(3) P1 0.0221(11) 0.0185(11) 0.0202(11) -0.0079(9) -0.0054(9) -0.0027(9) P2 0.0240(11) 0.0172(11) 0.0250(11) -0.0090(9) -0.0036(9) -0.0048(9) S1 0.0258(11) 0.0164(10) 0.0214(10) -0.0059(8) -0.0057(8) -0.0051(8) S2 0.0348(12) 0.0162(10) 0.0255(11) -0.0054(9) -0.0110(9) -0.0052(9) S3 0.0278(11) 0.0204(10) 0.0210(10) -0.0056(8) -0.0069(9) -0.0071(9) S4 0.0322(12) 0.0180(10) 0.0241(11) -0.0056(9) -0.0118(9) -0.0044(9) Cu1 0.0305(7) 0.0331(7) 0.0264(6) -0.0160(5) -0.0081(5) 0.0001(5) Br1 0.0394(6) 0.0454(7) 0.0439(7) -0.0145(5) -0.0072(5) -0.0088(5) Pd1 0.0224(4) 0.0152(3) 0.0185(3) -0.0077(2) -0.0043(2) -0.0036(2) C42 0.052(9) 0.136(18) 0.083(12) -0.055(13) 0.007(9) -0.026(10) Cl1 0.092(4) 0.173(6) 0.106(4) -0.096(4) 0.022(3) -0.053(4) Cl2 0.137(5) 0.121(5) 0.085(3) -0.043(3) -0.051(4) 0.000(4) Cl3 0.066(3) 0.194(7) 0.252(9) -0.146(7) 0.056(4) -0.061(4) C43 0.139(18) 0.058(10) 0.063(10) -0.011(8) 0.034(11) -0.028(11) Cl4 0.110(4) 0.125(5) 0.079(3) -0.010(3) -0.002(3) 0.020(4) Cl5 0.075(3) 0.114(4) 0.078(3) -0.008(3) 0.010(2) 0.004(3) Cl6 0.123(5) 0.116(5) 0.108(4) -0.028(4) -0.015(4) -0.023(4) C44 0.10(2) 0.20(3) 0.17(3) 0.11(3) 0.04(2) 0.07(2) Cl7 0.181(9) 0.163(9) 0.206(10) -0.048(7) -0.064(8) -0.001(7) Cl8 0.267(17) 0.38(2) 0.213(13) 0.004(14) -0.039(12) -0.117(16) Cl9 0.191(10) 0.208(11) 0.239(12) -0.121(10) 0.027(9) -0.050(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.356(12) . ? C1 S3 1.745(9) . ? C1 S1 1.761(9) . ? C2 S2 1.737(9) . ? C2 S4 1.738(9) . ? C3 C4 1.378(12) . ? C3 S4 1.740(9) 2 ? C3 S3 1.743(9) 2 ? C4 C5 1.467(12) . ? C4 C11 1.469(11) . ? C5 C9 1.396(12) . ? C5 C6 1.400(12) . ? C6 C7 1.381(13) . ? C6 H6 0.9300 . ? C7 C8 1.390(13) . ? C7 H7 0.9300 . ? C8 N1 1.369(13) . ? C8 H8 0.9300 . ? C9 N1 1.322(12) . ? C9 C10 1.437(12) . ? C10 N2 1.336(11) . ? C10 C11 1.411(11) . ? C11 C12 1.378(12) . ? C12 C13 1.384(13) . ? C12 H12 0.9300 . ? C13 C14 1.387(14) . ? C13 H13 0.9300 . ? C14 N2 1.342(12) . ? C14 H14 0.9300 . ? C15 C16 1.530(13) . ? C15 P2 1.819(10) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.545(13) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 P1 1.833(10) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.379(14) . ? C18 C23 1.402(13) . ? C18 P1 1.834(9) . ? C19 C20 1.387(14) . ? C19 H19 0.9300 . ? C20 C21 1.398(15) . ? C20 H20 0.9300 . ? C21 C22 1.368(16) . ? C21 H21 0.9300 . ? C22 C23 1.381(14) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.397(13) . ? C24 C29 1.410(14) . ? C24 P1 1.801(10) . ? C25 C26 1.419(15) . ? C25 H25 0.9300 . ? C26 C27 1.353(17) . ? C26 H26 0.9300 . ? C27 C28 1.377(16) . ? C27 H27 0.9300 . ? C28 C29 1.399(15) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.389(15) . ? C30 C35 1.402(14) . ? C30 P2 1.802(10) . ? C31 C32 1.356(15) . ? C31 H31 0.9300 . ? C32 C33 1.345(17) . ? C32 H32 0.9300 . ? C33 C34 1.36(2) . ? C33 H33 0.9300 . ? C34 C35 1.396(16) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C41 1.375(14) . ? C36 C37 1.384(13) . ? C36 P2 1.823(10) . ? C37 C38 1.380(17) . ? C37 H37 0.9300 . ? C38 C39 1.365(18) . ? C38 H38 0.9300 . ? C39 C40 1.374(16) . ? C39 H39 0.9300 . ? C40 C41 1.391(14) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? N1 Cu1 2.149(8) . ? N2 Cu1 2.331(8) . ? P1 Pd1 2.282(2) . ? P2 Pd1 2.271(2) . ? S1 Pd1 2.317(2) . ? S1 Cu1 2.349(3) . ? S2 Pd1 2.341(2) . ? S3 C3 1.743(9) 2 ? S4 C3 1.740(9) 2 ? Cu1 Br1 2.3591(17) . ? Cu1 Pd1 2.9315(14) . ? C42 Cl3 1.686(17) . ? C42 Cl1 1.727(19) . ? C42 Cl2 1.76(2) . ? C42 H42 0.9800 . ? C43 Cl5 1.63(2) . ? C43 Cl6 1.73(2) . ? C43 Cl4 1.815(18) . ? C43 H43 0.9800 . ? C44 Cl9 1.679(9) . ? C44 Cl7 1.686(10) . ? C44 Cl8 1.712(10) . ? C44 H44 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 S3 117.3(7) . . ? C2 C1 S1 123.8(7) . . ? S3 C1 S1 118.6(5) . . ? C1 C2 S2 124.2(7) . . ? C1 C2 S4 115.7(7) . . ? S2 C2 S4 120.0(5) . . ? C4 C3 S4 123.6(7) . 2 ? C4 C3 S3 122.8(7) . 2 ? S4 C3 S3 113.4(5) 2 2 ? C3 C4 C5 126.5(8) . . ? C3 C4 C11 126.7(8) . . ? C5 C4 C11 106.7(7) . . ? C9 C5 C6 116.7(8) . . ? C9 C5 C4 107.9(7) . . ? C6 C5 C4 135.5(8) . . ? C7 C6 C5 117.3(8) . . ? C7 C6 H6 121.4 . . ? C5 C6 H6 121.4 . . ? C6 C7 C8 121.8(9) . . ? C6 C7 H7 119.1 . . ? C8 C7 H7 119.1 . . ? N1 C8 C7 121.5(9) . . ? N1 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? N1 C9 C5 127.3(9) . . ? N1 C9 C10 123.3(8) . . ? C5 C9 C10 109.1(8) . . ? N2 C10 C11 126.5(8) . . ? N2 C10 C9 124.4(8) . . ? C11 C10 C9 109.1(7) . . ? C12 C11 C10 116.2(8) . . ? C12 C11 C4 136.6(8) . . ? C10 C11 C4 107.1(7) . . ? C11 C12 C13 118.5(9) . . ? C11 C12 H12 120.8 . . ? C13 C12 H12 120.8 . . ? C12 C13 C14 121.0(9) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? N2 C14 C13 122.3(8) . . ? N2 C14 H14 118.8 . . ? C13 C14 H14 118.8 . . ? C16 C15 P2 114.5(7) . . ? C16 C15 H15A 108.6 . . ? P2 C15 H15A 108.6 . . ? C16 C15 H15B 108.6 . . ? P2 C15 H15B 108.6 . . ? H15A C15 H15B 107.6 . . ? C15 C16 C17 115.9(8) . . ? C15 C16 H16A 108.3 . . ? C17 C16 H16A 108.3 . . ? C15 C16 H16B 108.3 . . ? C17 C16 H16B 108.3 . . ? H16A C16 H16B 107.4 . . ? C16 C17 P1 116.4(7) . . ? C16 C17 H17A 108.2 . . ? P1 C17 H17A 108.2 . . ? C16 C17 H17B 108.2 . . ? P1 C17 H17B 108.2 . . ? H17A C17 H17B 107.3 . . ? C19 C18 C23 120.3(9) . . ? C19 C18 P1 118.5(7) . . ? C23 C18 P1 121.2(7) . . ? C18 C19 C20 120.3(10) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C19 C20 C21 119.3(10) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.4 . . ? C22 C21 C20 120.2(9) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 121.2(10) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C22 C23 C18 118.8(10) . . ? C22 C23 H23 120.6 . . ? C18 C23 H23 120.6 . . ? C25 C24 C29 119.0(9) . . ? C25 C24 P1 123.3(8) . . ? C29 C24 P1 117.6(8) . . ? C24 C25 C26 119.2(10) . . ? C24 C25 H25 120.4 . . ? C26 C25 H25 120.4 . . ? C27 C26 C25 120.8(10) . . ? C27 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C26 C27 C28 120.8(10) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? C27 C28 C29 120.1(10) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C28 C29 C24 119.9(10) . . ? C28 C29 H29 120.0 . . ? C24 C29 H29 120.0 . . ? C31 C30 C35 117.0(10) . . ? C31 C30 P2 120.8(7) . . ? C35 C30 P2 122.2(8) . . ? C32 C31 C30 122.0(10) . . ? C32 C31 H31 119.0 . . ? C30 C31 H31 119.0 . . ? C33 C32 C31 120.6(12) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C32 C33 C34 120.3(11) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? C33 C34 C35 120.4(12) . . ? C33 C34 H34 119.8 . . ? C35 C34 H34 119.8 . . ? C34 C35 C30 119.7(12) . . ? C34 C35 H35 120.2 . . ? C30 C35 H35 120.2 . . ? C41 C36 C37 119.2(10) . . ? C41 C36 P2 117.8(7) . . ? C37 C36 P2 123.0(8) . . ? C38 C37 C36 120.5(11) . . ? C38 C37 H37 119.7 . . ? C36 C37 H37 119.7 . . ? C39 C38 C37 119.7(10) . . ? C39 C38 H38 120.1 . . ? C37 C38 H38 120.1 . . ? C38 C39 C40 120.8(11) . . ? C38 C39 H39 119.6 . . ? C40 C39 H39 119.6 . . ? C39 C40 C41 119.4(11) . . ? C39 C40 H40 120.3 . . ? C41 C40 H40 120.3 . . ? C36 C41 C40 120.4(10) . . ? C36 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C9 N1 C8 115.2(8) . . ? C9 N1 Cu1 108.0(6) . . ? C8 N1 Cu1 135.6(7) . . ? C10 N2 C14 115.5(8) . . ? C10 N2 Cu1 101.5(6) . . ? C14 N2 Cu1 141.2(6) . . ? C24 P1 C17 107.6(5) . . ? C24 P1 C18 106.7(4) . . ? C17 P1 C18 102.0(4) . . ? C24 P1 Pd1 106.1(3) . . ? C17 P1 Pd1 117.2(3) . . ? C18 P1 Pd1 116.6(3) . . ? C30 P2 C15 102.2(5) . . ? C30 P2 C36 107.5(4) . . ? C15 P2 C36 105.8(5) . . ? C30 P2 Pd1 113.4(3) . . ? C15 P2 Pd1 113.5(3) . . ? C36 P2 Pd1 113.7(3) . . ? C1 S1 Pd1 100.6(3) . . ? C1 S1 Cu1 98.8(3) . . ? Pd1 S1 Cu1 77.84(7) . . ? C2 S2 Pd1 100.6(3) . . ? C3 S3 C1 96.1(4) 2 . ? C2 S4 C3 97.2(4) . 2 ? N1 Cu1 N2 81.2(3) . . ? N1 Cu1 S1 106.9(2) . . ? N2 Cu1 S1 94.5(2) . . ? N1 Cu1 Br1 113.9(2) . . ? N2 Cu1 Br1 111.7(2) . . ? S1 Cu1 Br1 133.87(8) . . ? N1 Cu1 Pd1 107.3(2) . . ? N2 Cu1 Pd1 145.1(2) . . ? S1 Cu1 Pd1 50.60(6) . . ? Br1 Cu1 Pd1 95.97(5) . . ? P2 Pd1 P1 90.23(8) . . ? P2 Pd1 S1 168.95(9) . . ? P1 Pd1 S1 90.92(8) . . ? P2 Pd1 S2 91.18(8) . . ? P1 Pd1 S2 164.19(10) . . ? S1 Pd1 S2 90.70(8) . . ? P2 Pd1 Cu1 117.44(7) . . ? P1 Pd1 Cu1 99.24(7) . . ? S1 Pd1 Cu1 51.55(7) . . ? S2 Pd1 Cu1 94.06(7) . . ? Cl3 C42 Cl1 112.9(11) . . ? Cl3 C42 Cl2 113.7(11) . . ? Cl1 C42 Cl2 110.2(12) . . ? Cl3 C42 H42 106.5 . . ? Cl1 C42 H42 106.5 . . ? Cl2 C42 H42 106.5 . . ? Cl5 C43 Cl6 116.3(14) . . ? Cl5 C43 Cl4 113.0(11) . . ? Cl6 C43 Cl4 109.3(9) . . ? Cl5 C43 H43 105.8 . . ? Cl6 C43 H43 105.8 . . ? Cl4 C43 H43 105.8 . . ? Cl9 C44 Cl7 114.6(11) . . ? Cl9 C44 Cl8 111.4(11) . . ? Cl7 C44 Cl8 109.9(11) . . ? Cl9 C44 H44 106.8 . . ? Cl7 C44 H44 106.8 . . ? Cl8 C44 H44 106.8 . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 2.328 _refine_diff_density_min -1.599 _refine_diff_density_rms 0.316 #===END ###Material relevant to compound 9 at 173K ## data_compound9 _database_code_depnum_ccdc_archive 'CCDC 690634' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C82 H64 Br2 Cu2 N4 P4 Pt2 S8, 6(C H Cl3)' _chemical_formula_sum 'C88 H70 Br2 Cl18 Cu2 N4 P4 Pt2 S8' _chemical_formula_weight 2879.02 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.5454(13) _cell_length_b 13.6020(13) _cell_length_c 14.9359(15) _cell_angle_alpha 70.051(6) _cell_angle_beta 87.390(6) _cell_angle_gamma 82.447(6) _cell_volume 2564.3(4) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 958 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.864 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1404 _exptl_absorpt_coefficient_mu 4.648 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6288 _exptl_absorpt_correction_T_max 0.8731 _exptl_absorpt_process_details sadabs _exptl_special_details ; The crystal showed very limited diffracting power and therefore only a limited number of peaks could be collected ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16484 _diffrn_reflns_av_R_equivalents 0.0834 _diffrn_reflns_av_sigmaI/netI 0.1889 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 26.68 _reflns_number_total 10180 _reflns_number_gt 5169 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1619P)^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 SHELXL _refine_ls_extinction_coef 0.0131(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10180 _refine_ls_number_parameters 566 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1807 _refine_ls_R_factor_gt 0.0934 _refine_ls_wR_factor_ref 0.2944 _refine_ls_wR_factor_gt 0.2233 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _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 C1 C 0.0445(13) 0.0836(14) 0.2221(11) 0.034(3) Uani 1 1 d . . . C2 C 0.0444(13) 0.1888(14) 0.1660(11) 0.034(3) Uani 1 1 d . . . C3 C 0.0708(14) -0.1085(14) -0.0782(11) 0.037(4) Uani 1 1 d . . . C4 C 0.1221(13) -0.0894(12) -0.0094(10) 0.030(4) Uani 1 1 d . . . C5 C 0.1569(13) 0.0067(15) -0.0164(10) 0.036(4) Uani 1 1 d . . . C6 C 0.1525(13) 0.1074(12) -0.0849(10) 0.035(4) Uani 1 1 d . . . H6 H 0.1222 0.1230 -0.1436 0.042 Uiso 1 1 calc R . . C7 C 0.1941(15) 0.1814(15) -0.0625(12) 0.046(5) Uani 1 1 d . . . H7 H 0.1928 0.2484 -0.1078 0.056 Uiso 1 1 calc R . . C8 C 0.2373(15) 0.1627(14) 0.0222(13) 0.045(5) Uani 1 1 d . . . H8 H 0.2655 0.2166 0.0326 0.054 Uiso 1 1 calc R . . C9 C 0.2024(12) -0.0055(13) 0.0689(10) 0.030(4) Uani 1 1 d . . . C10 C 0.2020(12) -0.1145(14) 0.1312(10) 0.032(4) Uani 1 1 d . . . C11 C 0.1517(12) -0.1648(12) 0.0825(10) 0.027(4) Uani 1 1 d . . . C12 C 0.1389(14) -0.2704(15) 0.1361(11) 0.042(5) Uani 1 1 d . . . H12 H 0.1074 -0.3118 0.1108 0.051 Uiso 1 1 calc R . . C13 C 0.1764(14) -0.3095(14) 0.2297(11) 0.041(5) Uani 1 1 d . . . H13 H 0.1699 -0.3787 0.2673 0.049 Uiso 1 1 calc R . . C14 C 0.2211(13) -0.2491(14) 0.2656(11) 0.037(4) Uani 1 1 d . . . H14 H 0.2456 -0.2797 0.3274 0.044 Uiso 1 1 calc R . . C15 C 0.4224(14) 0.2288(13) 0.3656(11) 0.037(4) Uani 1 1 d . . . H15A H 0.4506 0.1799 0.3340 0.044 Uiso 1 1 calc R . . H15B H 0.4653 0.2839 0.3521 0.044 Uiso 1 1 calc R . . C16 C 0.4221(15) 0.1694(14) 0.4747(11) 0.044(5) Uani 1 1 d . . . H16A H 0.4906 0.1523 0.4964 0.053 Uiso 1 1 calc R . . H16B H 0.3889 0.2174 0.5050 0.053 Uiso 1 1 calc R . . C17 C 0.3745(12) 0.0714(14) 0.5088(11) 0.037(4) Uani 1 1 d . . . H17A H 0.3805 0.0436 0.5777 0.044 Uiso 1 1 calc R . . H17B H 0.4130 0.0206 0.4845 0.044 Uiso 1 1 calc R . . C18 C 0.2236(12) -0.0609(12) 0.5278(11) 0.030(4) Uani 1 1 d . . . C19 C 0.2798(14) -0.1318(14) 0.4953(13) 0.042(4) Uani 1 1 d . . . H19 H 0.3273 -0.1095 0.4483 0.051 Uiso 1 1 calc R . . C20 C 0.2665(16) -0.2386(14) 0.5324(13) 0.049(4) Uani 1 1 d . . . H20 H 0.3068 -0.2876 0.5118 0.059 Uiso 1 1 calc R . . C21 C 0.1935(16) -0.2709(14) 0.5992(13) 0.049(4) Uani 1 1 d . . . H21 H 0.1839 -0.3416 0.6232 0.059 Uiso 1 1 calc R . . C22 C 0.1344(16) -0.1981(15) 0.6309(13) 0.050(5) Uani 1 1 d . . . H22 H 0.0844 -0.2201 0.6753 0.061 Uiso 1 1 calc R . . C23 C 0.1487(16) -0.0953(14) 0.5976(11) 0.044(5) Uani 1 1 d . . . H23 H 0.1098 -0.0472 0.6203 0.053 Uiso 1 1 calc R . . C24 C 0.1746(15) 0.1451(14) 0.5517(12) 0.044(5) Uani 1 1 d . . . C25 C 0.2188(15) 0.1808(14) 0.6157(11) 0.040(4) Uani 1 1 d . . . H25 H 0.2868 0.1656 0.6277 0.048 Uiso 1 1 calc R . . C26 C 0.1553(18) 0.2419(16) 0.6624(12) 0.052(6) Uani 1 1 d . . . H26 H 0.1834 0.2697 0.7028 0.062 Uiso 1 1 calc R . . C27 C 0.0571(18) 0.2595(15) 0.6488(13) 0.048(5) Uani 1 1 d . . . H27 H 0.0178 0.2987 0.6804 0.057 Uiso 1 1 calc R . . C28 C 0.0127(15) 0.2207(15) 0.5887(15) 0.050(5) Uani 1 1 d . . . H28 H -0.0560 0.2328 0.5804 0.060 Uiso 1 1 calc R . . C29 C 0.0713(14) 0.1635(13) 0.5410(11) 0.038(4) Uani 1 1 d . . . H29 H 0.0413 0.1369 0.5008 0.046 Uiso 1 1 calc R . . C30 C 0.3329(12) 0.3654(14) 0.1933(11) 0.034(4) Uani 1 1 d . . . C31 C 0.3819(14) 0.3153(17) 0.1366(14) 0.048(5) Uani 1 1 d . . . H31 H 0.4028 0.2433 0.1613 0.057 Uiso 1 1 calc R . . C32 C 0.4003(17) 0.3695(19) 0.0443(14) 0.060(6) Uani 1 1 d . . . H32 H 0.4276 0.3330 0.0048 0.072 Uiso 1 1 calc R . . C33 C 0.3792(18) 0.4803(19) 0.0067(15) 0.075(8) Uani 1 1 d . . . H33 H 0.3992 0.5194 -0.0540 0.090 Uiso 1 1 calc R . . C34 C 0.3265(19) 0.5264(18) 0.0667(13) 0.066(7) Uani 1 1 d . . . H34 H 0.3036 0.5979 0.0430 0.080 Uiso 1 1 calc R . . C35 C 0.3077(17) 0.4726(14) 0.1561(14) 0.055(6) Uani 1 1 d . . . H35 H 0.2765 0.5082 0.1950 0.066 Uiso 1 1 calc R . . C36 C 0.2517(14) 0.3831(13) 0.3732(11) 0.035(4) Uani 1 1 d . . . C37 C 0.3135(18) 0.4286(14) 0.4116(13) 0.053(6) Uani 1 1 d . . . H37 H 0.3822 0.4155 0.4060 0.064 Uiso 1 1 calc R . . C38 C 0.271(2) 0.4966(16) 0.4604(13) 0.072(8) Uani 1 1 d . . . H38 H 0.3121 0.5309 0.4846 0.086 Uiso 1 1 calc R . . C39 C 0.172(2) 0.5130(15) 0.4726(13) 0.060(7) Uani 1 1 d . . . H39 H 0.1454 0.5550 0.5076 0.072 Uiso 1 1 calc R . . C40 C 0.1130(18) 0.4664(15) 0.4325(13) 0.054(6) Uani 1 1 d . . . H40 H 0.0443 0.4814 0.4362 0.065 Uiso 1 1 calc R . . C41 C 0.1513(15) 0.3973(15) 0.3862(13) 0.046(5) Uani 1 1 d . . . H41 H 0.1095 0.3614 0.3643 0.056 Uiso 1 1 calc R . . N1 N 0.2411(10) 0.0660(12) 0.0942(9) 0.036(3) Uani 1 1 d . . . N2 N 0.2333(11) -0.1485(11) 0.2197(9) 0.037(3) Uani 1 1 d . . . P1 P 0.2464(4) 0.0772(4) 0.4798(3) 0.0335(10) Uani 1 1 d . . . P2 P 0.3002(4) 0.2875(4) 0.3158(3) 0.0349(11) Uani 1 1 d . . . S1 S 0.1185(3) 0.0254(3) 0.3220(3) 0.0346(10) Uani 1 1 d . . . S2 S 0.1187(4) 0.2728(4) 0.1854(3) 0.0409(11) Uani 1 1 d . . . S3 S -0.0287(3) 0.0100(3) 0.1846(3) 0.0360(10) Uani 1 1 d . . . S4 S -0.0296(4) 0.2293(4) 0.0640(3) 0.0391(11) Uani 1 1 d . . . Cu1 Cu 0.27345(18) 0.00406(18) 0.24287(15) 0.0431(6) Uani 1 1 d . . . Br1 Br 0.44409(16) -0.01414(16) 0.28227(13) 0.0499(5) Uani 1 1 d . . . Pt1 Pt 0.19936(5) 0.16435(5) 0.32601(4) 0.0335(3) Uani 1 1 d . . . C42 C 0.495(2) 0.723(2) 0.257(2) 0.088(9) Uani 1 1 d . . . H42 H 0.4453 0.7852 0.2458 0.106 Uiso 1 1 calc R . . Cl1 Cl 0.4516(7) 0.6421(8) 0.2048(6) 0.120(3) Uani 1 1 d . . . Cl2 Cl 0.5047(9) 0.6600(8) 0.3804(7) 0.147(4) Uani 1 1 d . . . Cl3 Cl 0.6060(7) 0.7649(10) 0.2072(10) 0.169(5) Uani 1 1 d . . . C43 C 0.362(4) 0.848(2) 0.8300(19) 0.16(2) Uani 1 1 d . . . H43 H 0.4273 0.8661 0.8038 0.191 Uiso 1 1 calc R . . Cl4 Cl 0.3751(9) 0.8198(9) 0.9588(7) 0.154(5) Uani 1 1 d . . . Cl5 Cl 0.2876(7) 0.9546(9) 0.7816(6) 0.132(4) Uani 1 1 d . . . Cl6 Cl 0.3473(9) 0.7386(9) 0.8044(8) 0.148(4) Uani 1 1 d . . . C44 C 0.884(3) 0.489(5) 0.162(3) 0.22(3) Uani 1 1 d . . . H44 H 0.8988 0.4120 0.1789 0.260 Uiso 1 1 calc R . . Cl7 Cl 0.9446(11) 0.5248(11) 0.2329(11) 0.186(5) Uani 1 1 d . . . Cl8 Cl 0.7441(18) 0.521(2) 0.2011(12) 0.342(15) Uani 1 1 d . . . Cl9 Cl 0.8823(12) 0.5380(12) 0.0504(10) 0.196(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.048(8) 0.040(7) 0.029(6) -0.022(5) -0.005(5) -0.022(7) C2 0.048(8) 0.040(7) 0.029(6) -0.022(5) -0.005(5) -0.022(7) C3 0.045(11) 0.037(10) 0.023(7) -0.003(7) -0.008(7) 0.001(9) C4 0.052(11) 0.021(8) 0.022(7) -0.004(6) -0.007(7) -0.025(9) C5 0.037(10) 0.048(11) 0.019(7) -0.006(7) -0.005(6) -0.004(9) C6 0.056(12) 0.024(8) 0.024(7) -0.003(7) -0.011(7) -0.013(9) C7 0.066(14) 0.035(10) 0.034(9) -0.008(8) 0.001(9) -0.003(10) C8 0.062(14) 0.034(10) 0.045(10) -0.014(9) -0.001(9) -0.023(10) C9 0.028(9) 0.036(10) 0.027(7) -0.011(7) -0.006(6) -0.003(8) C10 0.031(9) 0.045(11) 0.023(7) -0.014(7) 0.001(6) -0.005(8) C11 0.039(10) 0.022(8) 0.023(7) -0.004(6) -0.007(6) -0.017(8) C12 0.051(12) 0.048(12) 0.032(9) -0.017(8) -0.008(8) -0.007(10) C13 0.057(12) 0.033(10) 0.020(7) 0.010(7) -0.007(7) -0.013(9) C14 0.045(11) 0.039(10) 0.027(8) -0.010(8) -0.014(7) -0.008(9) C15 0.053(12) 0.022(8) 0.034(8) -0.006(7) 0.000(8) -0.011(9) C16 0.057(13) 0.042(11) 0.028(8) -0.003(8) -0.019(8) -0.010(10) C17 0.034(10) 0.044(11) 0.029(8) -0.007(8) -0.007(7) -0.002(9) C18 0.034(10) 0.023(8) 0.031(8) -0.008(7) -0.007(7) 0.002(8) C19 0.040(11) 0.043(11) 0.044(10) -0.016(9) -0.009(8) 0.001(9) C20 0.077(11) 0.022(7) 0.044(7) -0.007(6) -0.002(7) -0.007(7) C21 0.077(11) 0.022(7) 0.044(7) -0.007(6) -0.002(7) -0.007(7) C22 0.072(15) 0.038(11) 0.040(10) -0.007(9) 0.014(9) -0.024(11) C23 0.079(15) 0.029(9) 0.025(8) -0.010(7) -0.002(8) -0.008(10) C24 0.061(13) 0.040(11) 0.031(9) -0.013(8) -0.006(8) -0.004(10) C25 0.051(12) 0.041(11) 0.025(8) -0.003(8) -0.001(7) -0.020(10) C26 0.080(17) 0.050(13) 0.030(9) -0.016(9) 0.019(9) -0.024(12) C27 0.072(16) 0.032(10) 0.042(10) -0.015(8) 0.006(10) -0.012(11) C28 0.040(12) 0.038(11) 0.067(13) -0.010(10) 0.001(10) -0.010(10) C29 0.049(12) 0.028(9) 0.034(9) -0.003(7) -0.002(8) -0.008(9) C30 0.030(10) 0.046(11) 0.032(8) -0.015(8) 0.002(7) -0.017(9) C31 0.045(12) 0.052(12) 0.056(12) -0.026(10) -0.005(9) -0.013(10) C32 0.067(15) 0.076(17) 0.039(10) -0.014(11) -0.003(10) -0.030(13) C33 0.082(18) 0.071(17) 0.042(12) 0.019(11) 0.022(11) -0.013(14) C34 0.11(2) 0.055(13) 0.026(9) -0.008(9) 0.004(11) -0.009(14) C35 0.093(18) 0.022(9) 0.046(11) -0.004(8) -0.002(10) -0.010(11) C36 0.052(12) 0.034(10) 0.026(8) -0.013(7) -0.011(7) -0.014(9) C37 0.087(17) 0.023(9) 0.043(10) 0.005(8) -0.018(10) -0.020(11) C38 0.14(3) 0.037(12) 0.031(10) -0.001(9) -0.030(13) 0.004(15) C39 0.12(2) 0.027(10) 0.036(10) -0.017(9) -0.013(12) 0.013(13) C40 0.079(16) 0.039(11) 0.040(10) -0.018(9) 0.017(10) 0.013(11) C41 0.043(12) 0.042(11) 0.049(11) -0.012(9) -0.001(9) 0.003(10) N1 0.034(8) 0.046(9) 0.030(7) -0.012(7) 0.001(6) -0.011(7) N2 0.046(9) 0.029(8) 0.034(7) -0.005(6) -0.014(6) -0.007(7) P1 0.043(3) 0.029(2) 0.029(2) -0.0082(18) -0.0045(18) -0.010(2) P2 0.045(3) 0.030(2) 0.029(2) -0.0076(18) -0.0039(18) -0.006(2) S1 0.047(3) 0.031(2) 0.0242(18) -0.0061(17) -0.0060(17) -0.007(2) S2 0.057(3) 0.030(2) 0.034(2) -0.0047(19) -0.013(2) -0.012(2) S3 0.046(3) 0.033(2) 0.0273(19) -0.0063(18) -0.0098(17) -0.008(2) S4 0.048(3) 0.034(2) 0.033(2) -0.0073(19) -0.0121(19) -0.007(2) Cu1 0.0503(15) 0.0469(14) 0.0348(11) -0.0171(10) -0.0092(10) -0.0039(12) Br1 0.0533(13) 0.0524(12) 0.0448(10) -0.0154(9) -0.0070(9) -0.0097(10) Pt1 0.0438(5) 0.0304(4) 0.0271(3) -0.0091(3) -0.0054(3) -0.0073(3) C42 0.08(2) 0.073(19) 0.11(2) -0.034(17) 0.011(17) -0.028(16) Cl1 0.116(7) 0.177(9) 0.116(6) -0.103(7) 0.023(5) -0.055(6) Cl2 0.210(11) 0.124(8) 0.116(7) -0.053(6) -0.087(7) 0.014(7) Cl3 0.087(7) 0.202(11) 0.286(15) -0.157(11) 0.062(8) -0.073(7) C43 0.33(6) 0.08(2) 0.048(16) -0.008(15) 0.03(2) 0.03(3) Cl4 0.162(10) 0.166(10) 0.091(6) -0.011(6) 0.004(6) 0.041(8) Cl5 0.116(7) 0.155(9) 0.093(6) -0.010(6) 0.008(5) 0.006(6) Cl6 0.172(10) 0.143(9) 0.130(8) -0.040(7) -0.034(7) -0.029(8) C44 0.09(3) 0.34(8) 0.10(3) 0.06(4) 0.00(2) -0.01(4) Cl7 0.195(14) 0.169(12) 0.195(13) -0.054(10) -0.051(11) -0.026(10) Cl8 0.35(3) 0.41(3) 0.177(15) 0.074(18) -0.092(17) -0.16(2) Cl9 0.260(18) 0.198(13) 0.157(11) -0.087(10) 0.011(11) -0.056(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.39(2) . ? C1 S1 1.726(16) . ? C1 S3 1.730(16) . ? C2 S2 1.720(17) . ? C2 S4 1.745(16) . ? C3 C4 1.38(2) . ? C3 S4 1.747(19) 2 ? C3 S3 1.754(15) 2 ? C4 C5 1.42(2) . ? C4 C11 1.441(19) . ? C5 C9 1.39(2) . ? C5 C6 1.40(2) . ? C6 C7 1.36(2) . ? C6 H6 0.9300 . ? C7 C8 1.35(3) . ? C7 H7 0.9300 . ? C8 N1 1.38(2) . ? C8 H8 0.9300 . ? C9 N1 1.33(2) . ? C9 C10 1.46(2) . ? C10 N2 1.312(19) . ? C10 C11 1.40(2) . ? C11 C12 1.42(2) . ? C12 C13 1.41(2) . ? C12 H12 0.9300 . ? C13 C14 1.34(2) . ? C13 H13 0.9300 . ? C14 N2 1.33(2) . ? C14 H14 0.9300 . ? C15 C16 1.55(2) . ? C15 P2 1.814(18) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.48(2) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 P1 1.794(17) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.36(2) . ? C18 C23 1.42(2) . ? C18 P1 1.830(17) . ? C19 C20 1.40(3) . ? C19 H19 0.9300 . ? C20 C21 1.38(3) . ? C20 H20 0.9300 . ? C21 C22 1.39(3) . ? C21 H21 0.9300 . ? C22 C23 1.35(2) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C29 1.40(3) . ? C24 C25 1.40(2) . ? C24 P1 1.816(18) . ? C25 C26 1.44(3) . ? C25 H25 0.9300 . ? C26 C27 1.33(3) . ? C26 H26 0.9300 . ? C27 C28 1.38(3) . ? C27 H27 0.9300 . ? C28 C29 1.38(3) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.36(2) . ? C30 C35 1.37(2) . ? C30 P2 1.842(16) . ? C31 C32 1.35(3) . ? C31 H31 0.9300 . ? C32 C33 1.41(3) . ? C32 H32 0.9300 . ? C33 C34 1.38(3) . ? C33 H33 0.9300 . ? C34 C35 1.32(2) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C37 1.35(2) . ? C36 C41 1.36(2) . ? C36 P2 1.829(17) . ? C37 C38 1.42(3) . ? C37 H37 0.9300 . ? C38 C39 1.33(3) . ? C38 H38 0.9300 . ? C39 C40 1.36(3) . ? C39 H39 0.9300 . ? C40 C41 1.38(2) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? N1 Cu1 2.132(13) . ? N2 Cu1 2.351(15) . ? P1 Pt1 2.272(4) . ? P2 Pt1 2.259(5) . ? S1 Pt1 2.325(5) . ? S1 Cu1 2.395(5) . ? S2 Pt1 2.334(4) . ? S3 C3 1.754(15) 2 ? S4 C3 1.747(19) 2 ? Cu1 Br1 2.372(3) . ? Cu1 Pt1 2.909(2) . ? C42 Cl1 1.72(3) . ? C42 Cl3 1.73(3) . ? C42 Cl2 1.75(3) . ? C42 H42 0.9800 . ? C43 Cl5 1.61(3) . ? C43 Cl6 1.70(4) . ? C43 Cl4 1.84(3) . ? C43 H43 0.9800 . ? C44 Cl9 1.57(4) . ? C44 Cl7 1.61(6) . ? C44 Cl8 2.00(4) . ? C44 H44 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 S1 122.3(12) . . ? C2 C1 S3 117.2(12) . . ? S1 C1 S3 120.5(10) . . ? C1 C2 S2 124.5(13) . . ? C1 C2 S4 114.8(12) . . ? S2 C2 S4 120.4(10) . . ? C4 C3 S4 123.9(12) . 2 ? C4 C3 S3 123.3(13) . 2 ? S4 C3 S3 112.5(10) 2 2 ? C3 C4 C5 126.6(14) . . ? C3 C4 C11 125.9(14) . . ? C5 C4 C11 107.5(13) . . ? C9 C5 C6 115.5(17) . . ? C9 C5 C4 108.8(14) . . ? C6 C5 C4 135.6(15) . . ? C7 C6 C5 117.4(15) . . ? C7 C6 H6 121.3 . . ? C5 C6 H6 121.3 . . ? C8 C7 C6 123.3(18) . . ? C8 C7 H7 118.4 . . ? C6 C7 H7 118.4 . . ? C7 C8 N1 122.2(18) . . ? C7 C8 H8 118.9 . . ? N1 C8 H8 118.9 . . ? N1 C9 C5 128.7(16) . . ? N1 C9 C10 123.0(14) . . ? C5 C9 C10 108.3(15) . . ? N2 C10 C11 129.8(16) . . ? N2 C10 C9 122.7(16) . . ? C11 C10 C9 107.0(13) . . ? C10 C11 C12 114.2(14) . . ? C10 C11 C4 108.3(13) . . ? C12 C11 C4 137.4(14) . . ? C13 C12 C11 116.5(16) . . ? C13 C12 H12 121.7 . . ? C11 C12 H12 121.7 . . ? C14 C13 C12 121.2(17) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? N2 C14 C13 125.1(15) . . ? N2 C14 H14 117.4 . . ? C13 C14 H14 117.4 . . ? C16 C15 P2 114.0(12) . . ? C16 C15 H15A 108.7 . . ? P2 C15 H15A 108.7 . . ? C16 C15 H15B 108.7 . . ? P2 C15 H15B 108.7 . . ? H15A C15 H15B 107.6 . . ? C17 C16 C15 117.3(14) . . ? C17 C16 H16A 108.0 . . ? C15 C16 H16A 108.0 . . ? C17 C16 H16B 108.0 . . ? C15 C16 H16B 108.0 . . ? H16A C16 H16B 107.2 . . ? C16 C17 P1 118.7(12) . . ? C16 C17 H17A 107.6 . . ? P1 C17 H17A 107.6 . . ? C16 C17 H17B 107.6 . . ? P1 C17 H17B 107.6 . . ? H17A C17 H17B 107.1 . . ? C19 C18 C23 119.5(16) . . ? C19 C18 P1 118.5(14) . . ? C23 C18 P1 122.0(12) . . ? C18 C19 C20 120.2(18) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C21 C20 C19 119.8(18) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C20 C21 C22 120.1(18) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23 C22 C21 120.5(18) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C18 119.9(17) . . ? C22 C23 H23 120.1 . . ? C18 C23 H23 120.1 . . ? C29 C24 C25 119.1(17) . . ? C29 C24 P1 118.2(14) . . ? C25 C24 P1 122.7(16) . . ? C24 C25 C26 117.7(18) . . ? C24 C25 H25 121.1 . . ? C26 C25 H25 121.1 . . ? C27 C26 C25 121(2) . . ? C27 C26 H26 119.4 . . ? C25 C26 H26 119.4 . . ? C26 C27 C28 121.2(19) . . ? C26 C27 H27 119.4 . . ? C28 C27 H27 119.4 . . ? C27 C28 C29 119.3(19) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? C28 C29 C24 121.3(18) . . ? C28 C29 H29 119.4 . . ? C24 C29 H29 119.4 . . ? C31 C30 C35 118.4(16) . . ? C31 C30 P2 119.1(14) . . ? C35 C30 P2 122.4(14) . . ? C32 C31 C30 120(2) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C31 C32 C33 122(2) . . ? C31 C32 H32 119.2 . . ? C33 C32 H32 119.2 . . ? C34 C33 C32 115.1(17) . . ? C34 C33 H33 122.4 . . ? C32 C33 H33 122.4 . . ? C35 C34 C33 122(2) . . ? C35 C34 H34 118.8 . . ? C33 C34 H34 118.8 . . ? C34 C35 C30 122(2) . . ? C34 C35 H35 119.2 . . ? C30 C35 H35 119.2 . . ? C37 C36 C41 120.9(19) . . ? C37 C36 P2 121.3(16) . . ? C41 C36 P2 117.4(14) . . ? C36 C37 C38 118(2) . . ? C36 C37 H37 120.9 . . ? C38 C37 H37 120.9 . . ? C39 C38 C37 122(2) . . ? C39 C38 H38 119.1 . . ? C37 C38 H38 119.1 . . ? C38 C39 C40 118.0(19) . . ? C38 C39 H39 121.0 . . ? C40 C39 H39 121.0 . . ? C39 C40 C41 122(2) . . ? C39 C40 H40 118.9 . . ? C41 C40 H40 118.9 . . ? C36 C41 C40 119(2) . . ? C36 C41 H41 120.7 . . ? C40 C41 H41 120.7 . . ? C9 N1 C8 112.9(14) . . ? C9 N1 Cu1 109.3(11) . . ? C8 N1 Cu1 137.1(12) . . ? C10 N2 C14 112.9(15) . . ? C10 N2 Cu1 103.7(11) . . ? C14 N2 Cu1 142.8(11) . . ? C17 P1 C24 106.0(9) . . ? C17 P1 C18 103.2(8) . . ? C24 P1 C18 106.9(8) . . ? C17 P1 Pt1 117.4(5) . . ? C24 P1 Pt1 106.9(6) . . ? C18 P1 Pt1 115.6(5) . . ? C15 P2 C36 107.5(8) . . ? C15 P2 C30 101.1(8) . . ? C36 P2 C30 106.0(8) . . ? C15 P2 Pt1 112.0(6) . . ? C36 P2 Pt1 114.6(6) . . ? C30 P2 Pt1 114.6(6) . . ? C1 S1 Pt1 102.2(6) . . ? C1 S1 Cu1 97.9(6) . . ? Pt1 S1 Cu1 76.07(15) . . ? C2 S2 Pt1 101.2(6) . . ? C1 S3 C3 97.3(8) . 2 ? C2 S4 C3 98.1(8) . 2 ? N1 Cu1 N2 80.2(5) . . ? N1 Cu1 Br1 115.1(4) . . ? N2 Cu1 Br1 111.0(4) . . ? N1 Cu1 S1 105.9(4) . . ? N2 Cu1 S1 91.9(4) . . ? Br1 Cu1 S1 135.42(14) . . ? N1 Cu1 Pt1 108.2(4) . . ? N2 Cu1 Pt1 142.7(4) . . ? Br1 Cu1 Pt1 98.31(9) . . ? S1 Cu1 Pt1 50.88(12) . . ? P2 Pt1 P1 90.30(16) . . ? P2 Pt1 S1 169.64(16) . . ? P1 Pt1 S1 91.68(15) . . ? P2 Pt1 S2 90.85(16) . . ? P1 Pt1 S2 165.85(17) . . ? S1 Pt1 S2 89.72(15) . . ? P2 Pt1 Cu1 116.59(13) . . ? P1 Pt1 Cu1 99.61(12) . . ? S1 Pt1 Cu1 53.05(12) . . ? S2 Pt1 Cu1 92.48(12) . . ? Cl1 C42 Cl3 111.5(17) . . ? Cl1 C42 Cl2 110.6(15) . . ? Cl3 C42 Cl2 111.7(18) . . ? Cl1 C42 H42 107.6 . . ? Cl3 C42 H42 107.6 . . ? Cl2 C42 H42 107.6 . . ? Cl5 C43 Cl6 119(3) . . ? Cl5 C43 Cl4 111.8(18) . . ? Cl6 C43 Cl4 111.9(17) . . ? Cl5 C43 H43 104.2 . . ? Cl6 C43 H43 104.2 . . ? Cl4 C43 H43 104.2 . . ? Cl9 C44 Cl7 126(4) . . ? Cl9 C44 Cl8 104(2) . . ? Cl7 C44 Cl8 101(3) . . ? Cl9 C44 H44 108.1 . . ? Cl7 C44 H44 108.1 . . ? Cl8 C44 H44 108.1 . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 26.68 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 2.773 _refine_diff_density_min -3.841 _refine_diff_density_rms 0.378 #===END ###Material relevant to compound 10 at 173K ## data_compound10 _database_code_depnum_ccdc_archive 'CCDC 690635' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C78 H64 Ag2 Cl2 N4 P4 Pt2 S4, C H2 Cl2' _chemical_formula_sum 'C79 H66 Ag2 Cl4 N4 P4 Pt2 S4' _chemical_formula_weight 2071.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9781(2) _cell_length_b 12.6890(3) _cell_length_c 17.2016(4) _cell_angle_alpha 101.3700(10) _cell_angle_beta 96.1060(10) _cell_angle_gamma 109.7470(10) _cell_volume 1974.00(8) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6020 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 23.84 _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.742 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1010 _exptl_absorpt_coefficient_mu 4.388 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4593 _exptl_absorpt_correction_T_max 0.8104 _exptl_absorpt_process_details sadabs _exptl_special_details ; The CH2Cl2 molecule is disordered owing to its proximity with an inversion center. The PART -1 command has been used to account for this. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28772 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0586 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 27.54 _reflns_number_total 8915 _reflns_number_gt 7051 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0658P)^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 8915 _refine_ls_number_parameters 448 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0529 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.1140 _refine_ls_wR_factor_gt 0.0981 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 C1 C 0.0420(6) 0.7467(5) 0.0767(4) 0.0277(13) Uani 1 1 d . . . C2 C -0.0250(6) 0.6574(5) 0.0090(3) 0.0270(13) Uani 1 1 d . . . C3 C 0.0358(6) 0.6317(5) -0.0640(4) 0.0289(13) Uani 1 1 d . . . C4 C 0.1623(7) 0.6838(6) -0.0894(4) 0.0352(15) Uani 1 1 d . . . H4 H 0.2318 0.7534 -0.0587 0.042 Uiso 1 1 calc R . . C5 C 0.1822(8) 0.6283(6) -0.1629(4) 0.0425(17) Uani 1 1 d . . . H5 H 0.2670 0.6614 -0.1815 0.051 Uiso 1 1 calc R . . C6 C 0.0800(9) 0.5262(6) -0.2086(4) 0.0481(19) Uani 1 1 d . . . H6 H 0.0986 0.4915 -0.2569 0.058 Uiso 1 1 calc R . . C7 C -0.0651(7) 0.5268(5) -0.1157(4) 0.0337(15) Uani 1 1 d . . . C8 C -0.1855(6) 0.4851(5) -0.0777(4) 0.0306(14) Uani 1 1 d . . . C9 C -0.1666(6) 0.5622(5) -0.0019(4) 0.0303(14) Uani 1 1 d . . . C10 C -0.2722(7) 0.5345(6) 0.0438(4) 0.0363(15) Uani 1 1 d . . . H10 H -0.2653 0.5834 0.0933 0.044 Uiso 1 1 calc R . . C11 C -0.3892(8) 0.4314(6) 0.0136(5) 0.0509(19) Uani 1 1 d . . . H11 H -0.4618 0.4098 0.0435 0.061 Uiso 1 1 calc R . . C12 C -0.3997(9) 0.3578(6) -0.0632(5) 0.054(2) Uani 1 1 d . . . H12 H -0.4787 0.2885 -0.0823 0.064 Uiso 1 1 calc R . . N1 N -0.0469(7) 0.4736(5) -0.1865(3) 0.0420(14) Uani 1 1 d . . . N2 N -0.2959(6) 0.3873(5) -0.1090(4) 0.0424(14) Uani 1 1 d . . . Ag1 Ag -0.25532(8) 0.28298(5) -0.22766(3) 0.05762(19) Uani 1 1 d . . . Cl1 Cl -0.39940(15) 0.20627(13) -0.36471(9) 0.0316(3) Uani 1 1 d . . . C13 C 0.5404(6) 1.0243(5) 0.2023(4) 0.0277(13) Uani 1 1 d . . . C14 C 0.5989(6) 0.9485(5) 0.2274(4) 0.0335(14) Uani 1 1 d . . . H14 H 0.5794 0.9259 0.2745 0.040 Uiso 1 1 calc R . . C15 C 0.6845(6) 0.9073(6) 0.1835(4) 0.0339(14) Uani 1 1 d . . . H15 H 0.7245 0.8579 0.2014 0.041 Uiso 1 1 calc R . . C16 C 0.7122(7) 0.9384(6) 0.1126(4) 0.0395(16) Uani 1 1 d . . . H16 H 0.7705 0.9098 0.0828 0.047 Uiso 1 1 calc R . . C17 C 0.6539(7) 1.0116(6) 0.0860(4) 0.0421(17) Uani 1 1 d . . . H17 H 0.6722 1.0319 0.0380 0.051 Uiso 1 1 calc R . . C18 C 0.5679(7) 1.0554(6) 0.1302(4) 0.0365(15) Uani 1 1 d . . . H18 H 0.5286 1.1050 0.1121 0.044 Uiso 1 1 calc R . . C19 C 0.4117(6) 1.1997(5) 0.2298(4) 0.0296(13) Uani 1 1 d . . . C20 C 0.3164(7) 1.1912(6) 0.1617(4) 0.0413(16) Uani 1 1 d . . . H20 H 0.2548 1.1187 0.1306 0.050 Uiso 1 1 calc R . . C21 C 0.3121(8) 1.2885(7) 0.1400(5) 0.052(2) Uani 1 1 d . . . H21 H 0.2503 1.2809 0.0931 0.062 Uiso 1 1 calc R . . C22 C 0.3973(8) 1.3969(7) 0.1862(5) 0.052(2) Uani 1 1 d . . . H22 H 0.3908 1.4623 0.1721 0.062 Uiso 1 1 calc R . . C23 C 0.4927(8) 1.4073(6) 0.2540(5) 0.053(2) Uani 1 1 d . . . H23 H 0.5524 1.4804 0.2851 0.064 Uiso 1 1 calc R . . C24 C 0.5004(7) 1.3100(6) 0.2761(4) 0.0395(16) Uani 1 1 d . . . H24 H 0.5650 1.3182 0.3220 0.047 Uiso 1 1 calc R . . C25 C 0.0448(6) 1.0893(5) 0.3389(4) 0.0291(13) Uani 1 1 d . . . C26 C -0.0003(8) 1.1379(6) 0.4052(4) 0.0426(17) Uani 1 1 d . . . H26 H 0.0151 1.1180 0.4536 0.051 Uiso 1 1 calc R . . C27 C -0.0680(8) 1.2161(7) 0.4006(4) 0.0472(19) Uani 1 1 d . . . H27 H -0.1012 1.2460 0.4451 0.057 Uiso 1 1 calc R . . C28 C -0.0861(7) 1.2495(6) 0.3300(4) 0.0427(17) Uani 1 1 d . . . H28 H -0.1294 1.3033 0.3270 0.051 Uiso 1 1 calc R . . C29 C -0.0398(8) 1.2025(6) 0.2641(4) 0.0455(17) Uani 1 1 d . . . H29 H -0.0524 1.2247 0.2163 0.055 Uiso 1 1 calc R . . C30 C 0.0251(7) 1.1231(6) 0.2676(4) 0.0364(15) Uani 1 1 d . . . H30 H 0.0558 1.0920 0.2224 0.044 Uiso 1 1 calc R . . C31 C -0.0097(6) 0.8613(5) 0.3652(3) 0.0278(13) Uani 1 1 d . . . C32 C -0.1534(7) 0.8520(6) 0.3639(4) 0.0344(15) Uani 1 1 d . . . H32 H -0.1822 0.9101 0.3515 0.041 Uiso 1 1 calc R . . C33 C -0.2539(7) 0.7569(6) 0.3809(4) 0.0391(16) Uani 1 1 d . . . H33 H -0.3492 0.7518 0.3803 0.047 Uiso 1 1 calc R . . C34 C -0.2113(7) 0.6698(6) 0.3987(4) 0.0404(16) Uani 1 1 d . . . H34 H -0.2784 0.6063 0.4103 0.049 Uiso 1 1 calc R . . C35 C -0.0697(7) 0.6766(5) 0.3993(4) 0.0355(15) Uani 1 1 d . . . H35 H -0.0423 0.6172 0.4105 0.043 Uiso 1 1 calc R . . C36 C 0.0317(7) 0.7725(5) 0.3832(4) 0.0328(14) Uani 1 1 d . . . H36 H 0.1272 0.7775 0.3845 0.039 Uiso 1 1 calc R . . C37 C 0.2714(6) 1.0423(5) 0.4293(3) 0.0288(13) Uani 1 1 d . . . H37A H 0.2331 1.0688 0.4756 0.035 Uiso 1 1 calc R . . H37B H 0.3042 0.9818 0.4400 0.035 Uiso 1 1 calc R . . C38 C 0.4012(6) 1.1427(5) 0.4206(4) 0.0330(14) Uani 1 1 d . . . H38A H 0.4616 1.1820 0.4734 0.040 Uiso 1 1 calc R . . H38B H 0.3663 1.1974 0.4014 0.040 Uiso 1 1 calc R . . C39 C 0.4944(6) 1.1080(5) 0.3633(3) 0.0294(13) Uani 1 1 d . . . H39A H 0.5147 1.0433 0.3765 0.035 Uiso 1 1 calc R . . H39B H 0.5862 1.1720 0.3724 0.035 Uiso 1 1 calc R . . P1 P 0.41279(15) 1.06747(13) 0.25678(9) 0.0247(3) Uani 1 1 d . . . P2 P 0.12540(16) 0.98078(13) 0.34065(9) 0.0239(3) Uani 1 1 d . . . S1 S 0.21586(16) 0.85081(14) 0.09125(9) 0.0302(3) Uani 1 1 d . . . S2 S -0.02741(15) 0.77047(13) 0.16510(9) 0.0294(3) Uani 1 1 d . . . Pt1 Pt 0.19034(2) 0.925861(18) 0.221795(13) 0.02169(8) Uani 1 1 d . . . Cl2 Cl 0.2087(6) 0.5664(5) 0.4993(4) 0.0901(12) Uani 0.50 1 d P A -1 Cl3 Cl 0.4413(5) 0.5004(5) 0.4651(4) 0.0901(12) Uani 0.50 1 d P A -1 C40 C 0.272(2) 0.5149(19) 0.4099(15) 0.0901(12) Uani 0.50 1 d P A -1 H40A H 0.2962 0.5709 0.3775 0.108 Uiso 0.50 1 calc PR A -1 H40B H 0.2028 0.4414 0.3768 0.108 Uiso 0.50 1 calc PR A -1 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 C1 0.028(3) 0.035(3) 0.023(3) 0.008(3) 0.004(2) 0.015(3) C2 0.031(3) 0.029(3) 0.023(3) 0.007(2) 0.002(2) 0.014(3) C3 0.034(3) 0.024(3) 0.028(3) 0.005(2) -0.001(3) 0.013(3) C4 0.042(4) 0.040(4) 0.022(3) 0.000(3) 0.004(3) 0.018(3) C5 0.051(4) 0.054(5) 0.028(4) 0.007(3) 0.011(3) 0.028(4) C6 0.074(5) 0.051(5) 0.026(4) 0.003(3) 0.011(4) 0.035(4) C7 0.049(4) 0.029(3) 0.023(3) 0.002(3) -0.003(3) 0.020(3) C8 0.036(3) 0.021(3) 0.031(3) 0.005(2) -0.006(3) 0.011(3) C9 0.031(3) 0.027(3) 0.027(3) 0.004(3) -0.002(3) 0.009(3) C10 0.035(3) 0.034(4) 0.038(4) 0.008(3) 0.001(3) 0.012(3) C11 0.044(4) 0.049(5) 0.050(5) 0.016(4) 0.004(3) 0.005(4) C12 0.059(5) 0.035(4) 0.057(5) 0.008(4) -0.013(4) 0.013(4) N1 0.061(4) 0.036(3) 0.027(3) 0.001(2) -0.003(3) 0.023(3) N2 0.049(3) 0.034(3) 0.036(3) 0.004(3) -0.008(3) 0.013(3) Ag1 0.0921(5) 0.0371(3) 0.0357(3) -0.0054(2) -0.0222(3) 0.0321(3) Cl1 0.0310(7) 0.0433(9) 0.0232(7) 0.0093(6) 0.0026(6) 0.0173(7) C13 0.023(3) 0.030(3) 0.026(3) 0.005(3) 0.002(2) 0.006(2) C14 0.032(3) 0.041(4) 0.030(3) 0.012(3) 0.008(3) 0.015(3) C15 0.034(3) 0.042(4) 0.030(3) 0.008(3) 0.009(3) 0.019(3) C16 0.034(3) 0.047(4) 0.034(4) 0.001(3) 0.011(3) 0.015(3) C17 0.045(4) 0.054(5) 0.031(4) 0.014(3) 0.018(3) 0.017(3) C18 0.041(4) 0.039(4) 0.031(4) 0.015(3) 0.009(3) 0.012(3) C19 0.029(3) 0.030(3) 0.034(3) 0.011(3) 0.012(3) 0.013(3) C20 0.036(3) 0.043(4) 0.045(4) 0.016(3) 0.002(3) 0.013(3) C21 0.045(4) 0.058(5) 0.059(5) 0.031(4) 0.004(4) 0.020(4) C22 0.054(4) 0.045(5) 0.070(6) 0.028(4) 0.018(4) 0.025(4) C23 0.061(5) 0.023(4) 0.068(6) 0.010(4) 0.007(4) 0.008(3) C24 0.044(4) 0.040(4) 0.034(4) 0.009(3) 0.009(3) 0.015(3) C25 0.031(3) 0.028(3) 0.029(3) 0.005(3) 0.002(3) 0.014(3) C26 0.060(4) 0.056(5) 0.023(3) 0.005(3) 0.005(3) 0.039(4) C27 0.062(5) 0.057(5) 0.034(4) 0.000(3) 0.007(3) 0.043(4) C28 0.049(4) 0.042(4) 0.046(4) 0.010(3) 0.008(3) 0.029(3) C29 0.059(4) 0.049(4) 0.041(4) 0.019(3) 0.008(3) 0.032(4) C30 0.045(4) 0.042(4) 0.029(3) 0.007(3) 0.009(3) 0.025(3) C31 0.032(3) 0.037(3) 0.017(3) 0.005(2) 0.010(2) 0.015(3) C32 0.038(3) 0.046(4) 0.024(3) 0.007(3) 0.002(3) 0.024(3) C33 0.029(3) 0.050(4) 0.036(4) 0.010(3) 0.009(3) 0.010(3) C34 0.038(4) 0.042(4) 0.027(3) 0.006(3) 0.008(3) -0.001(3) C35 0.047(4) 0.027(3) 0.031(4) 0.005(3) 0.011(3) 0.012(3) C36 0.032(3) 0.039(4) 0.034(4) 0.013(3) 0.013(3) 0.016(3) C37 0.036(3) 0.036(3) 0.017(3) 0.005(2) 0.003(2) 0.018(3) C38 0.035(3) 0.036(4) 0.021(3) 0.002(3) -0.003(3) 0.009(3) C39 0.028(3) 0.036(3) 0.026(3) 0.008(3) 0.002(2) 0.014(3) P1 0.0248(7) 0.0294(8) 0.0213(7) 0.0078(6) 0.0048(6) 0.0106(6) P2 0.0281(7) 0.0305(8) 0.0170(7) 0.0054(6) 0.0071(6) 0.0148(6) S1 0.0312(7) 0.0353(9) 0.0198(7) 0.0011(6) 0.0085(6) 0.0089(7) S2 0.0284(7) 0.0286(8) 0.0262(8) 0.0014(6) 0.0086(6) 0.0060(6) Pt1 0.02442(12) 0.02574(13) 0.01679(12) 0.00553(8) 0.00564(8) 0.01093(9) Cl2 0.081(2) 0.088(2) 0.148(4) 0.073(3) 0.059(2) 0.054(2) Cl3 0.081(2) 0.088(2) 0.148(4) 0.073(3) 0.059(2) 0.054(2) C40 0.081(2) 0.088(2) 0.148(4) 0.073(3) 0.059(2) 0.054(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.374(8) . ? C1 S1 1.745(6) . ? C1 S2 1.752(6) . ? C2 C3 1.478(8) . ? C2 C9 1.480(8) . ? C3 C4 1.374(9) . ? C3 C7 1.419(8) . ? C4 C5 1.389(9) . ? C4 H4 0.9300 . ? C5 C6 1.368(10) . ? C5 H5 0.9300 . ? C6 N1 1.350(10) . ? C6 H6 0.9300 . ? C7 N1 1.333(8) . ? C7 C8 1.423(9) . ? C8 N2 1.316(8) . ? C8 C9 1.418(8) . ? C9 C10 1.373(9) . ? C10 C11 1.384(9) . ? C10 H10 0.9300 . ? C11 C12 1.431(11) . ? C11 H11 0.9300 . ? C12 N2 1.364(10) . ? C12 H12 0.9300 . ? N1 Ag1 2.508(6) . ? N2 Ag1 2.357(6) . ? Ag1 Cl1 2.4495(15) . ? Ag1 Pt1 2.9506(6) 2_565 ? C13 C14 1.393(8) . ? C13 C18 1.401(9) . ? C13 P1 1.823(6) . ? C14 C15 1.363(8) . ? C14 H14 0.9300 . ? C15 C16 1.381(9) . ? C15 H15 0.9300 . ? C16 C17 1.375(10) . ? C16 H16 0.9300 . ? C17 C18 1.385(9) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.389(9) . ? C19 C24 1.397(9) . ? C19 P1 1.830(6) . ? C20 C21 1.371(10) . ? C20 H20 0.9300 . ? C21 C22 1.371(10) . ? C21 H21 0.9300 . ? C22 C23 1.378(11) . ? C22 H22 0.9300 . ? C23 C24 1.385(10) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.379(9) . ? C25 C30 1.392(9) . ? C25 P2 1.818(6) . ? C26 C27 1.385(9) . ? C26 H26 0.9300 . ? C27 C28 1.376(10) . ? C27 H27 0.9300 . ? C28 C29 1.374(10) . ? C28 H28 0.9300 . ? C29 C30 1.377(9) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.396(8) . ? C31 C36 1.401(8) . ? C31 P2 1.813(6) . ? C32 C33 1.389(9) . ? C32 H32 0.9300 . ? C33 C34 1.385(10) . ? C33 H33 0.9300 . ? C34 C35 1.385(9) . ? C34 H34 0.9300 . ? C35 C36 1.394(9) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C38 1.525(8) . ? C37 P2 1.830(5) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.525(8) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 P1 1.821(6) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? P1 Pt1 2.2610(15) . ? P2 Pt1 2.2606(15) . ? S1 Pt1 2.3360(14) . ? S2 Pt1 2.3358(14) . ? Pt1 Ag1 2.9506(6) 2_565 ? Cl2 C40 1.81(2) . ? Cl3 C40 1.93(2) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? 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 C2 C1 S1 125.5(5) . . ? C2 C1 S2 126.0(5) . . ? S1 C1 S2 108.4(3) . . ? C1 C2 C3 126.7(5) . . ? C1 C2 C9 126.5(6) . . ? C3 C2 C9 106.6(5) . . ? C4 C3 C7 117.3(6) . . ? C4 C3 C2 135.0(5) . . ? C7 C3 C2 107.7(5) . . ? C3 C4 C5 117.4(6) . . ? C3 C4 H4 121.3 . . ? C5 C4 H4 121.3 . . ? C6 C5 C4 121.5(7) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? N1 C6 C5 122.9(6) . . ? N1 C6 H6 118.6 . . ? C5 C6 H6 118.6 . . ? N1 C7 C3 125.5(6) . . ? N1 C7 C8 125.7(6) . . ? C3 C7 C8 108.7(5) . . ? N2 C8 C9 125.9(6) . . ? N2 C8 C7 123.7(6) . . ? C9 C8 C7 110.4(5) . . ? C10 C9 C8 118.3(6) . . ? C10 C9 C2 135.0(6) . . ? C8 C9 C2 106.7(5) . . ? C9 C10 C11 117.7(6) . . ? C9 C10 H10 121.2 . . ? C11 C10 H10 121.2 . . ? C10 C11 C12 120.7(7) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? N2 C12 C11 121.2(7) . . ? N2 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C7 N1 C6 115.4(6) . . ? C7 N1 Ag1 104.9(5) . . ? C6 N1 Ag1 138.9(5) . . ? C8 N2 C12 116.2(6) . . ? C8 N2 Ag1 111.1(5) . . ? C12 N2 Ag1 131.9(5) . . ? N2 Ag1 Cl1 131.04(14) . . ? N2 Ag1 N1 74.0(2) . . ? Cl1 Ag1 N1 122.12(14) . . ? N2 Ag1 Pt1 118.45(14) . 2_565 ? Cl1 Ag1 Pt1 95.55(4) . 2_565 ? N1 Ag1 Pt1 117.41(13) . 2_565 ? C14 C13 C18 119.1(6) . . ? C14 C13 P1 119.6(5) . . ? C18 C13 P1 120.9(5) . . ? C15 C14 C13 120.6(6) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 120.4(6) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C17 C16 C15 120.1(6) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 120.3(7) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C18 C13 119.5(6) . . ? C17 C18 H18 120.2 . . ? C13 C18 H18 120.2 . . ? C20 C19 C24 118.0(6) . . ? C20 C19 P1 119.2(5) . . ? C24 C19 P1 122.7(5) . . ? C21 C20 C19 120.8(7) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C20 C21 C22 121.2(7) . . ? C20 C21 H21 119.4 . . ? C22 C21 H21 119.4 . . ? C21 C22 C23 119.0(7) . . ? C21 C22 H22 120.5 . . ? C23 C22 H22 120.5 . . ? C22 C23 C24 120.6(7) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C23 C24 C19 120.3(7) . . ? C23 C24 H24 119.8 . . ? C19 C24 H24 119.8 . . ? C26 C25 C30 118.7(6) . . ? C26 C25 P2 122.4(5) . . ? C30 C25 P2 118.9(5) . . ? C25 C26 C27 121.0(7) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C28 C27 C26 119.9(7) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C29 C28 C27 119.4(6) . . ? C29 C28 H28 120.3 . . ? C27 C28 H28 120.3 . . ? C28 C29 C30 121.0(7) . . ? C28 C29 H29 119.5 . . ? C30 C29 H29 119.5 . . ? C29 C30 C25 120.0(6) . . ? C29 C30 H30 120.0 . . ? C25 C30 H30 120.0 . . ? C32 C31 C36 118.9(6) . . ? C32 C31 P2 123.0(5) . . ? C36 C31 P2 118.0(4) . . ? C33 C32 C31 120.8(6) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C34 C33 C32 119.6(6) . . ? C34 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? C33 C34 C35 120.5(6) . . ? C33 C34 H34 119.7 . . ? C35 C34 H34 119.7 . . ? C34 C35 C36 119.9(6) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C35 C36 C31 120.2(6) . . ? C35 C36 H36 119.9 . . ? C31 C36 H36 119.9 . . ? C38 C37 P2 114.1(4) . . ? C38 C37 H37A 108.7 . . ? P2 C37 H37A 108.7 . . ? C38 C37 H37B 108.7 . . ? P2 C37 H37B 108.7 . . ? H37A C37 H37B 107.6 . . ? C37 C38 C39 114.6(5) . . ? C37 C38 H38A 108.6 . . ? C39 C38 H38A 108.6 . . ? C37 C38 H38B 108.6 . . ? C39 C38 H38B 108.6 . . ? H38A C38 H38B 107.6 . . ? C38 C39 P1 114.5(4) . . ? C38 C39 H39A 108.6 . . ? P1 C39 H39A 108.6 . . ? C38 C39 H39B 108.6 . . ? P1 C39 H39B 108.6 . . ? H39A C39 H39B 107.6 . . ? C39 P1 C13 105.8(3) . . ? C39 P1 C19 107.0(3) . . ? C13 P1 C19 105.6(3) . . ? C39 P1 Pt1 115.3(2) . . ? C13 P1 Pt1 110.65(19) . . ? C19 P1 Pt1 111.8(2) . . ? C31 P2 C25 105.8(3) . . ? C31 P2 C37 105.0(3) . . ? C25 P2 C37 105.4(3) . . ? C31 P2 Pt1 112.07(19) . . ? C25 P2 Pt1 111.9(2) . . ? C37 P2 Pt1 115.9(2) . . ? C1 S1 Pt1 88.5(2) . . ? C1 S2 Pt1 88.4(2) . . ? P2 Pt1 P1 93.74(6) . . ? P2 Pt1 S2 95.94(5) . . ? P1 Pt1 S2 170.33(5) . . ? P2 Pt1 S1 170.34(5) . . ? P1 Pt1 S1 95.60(5) . . ? S2 Pt1 S1 74.73(5) . . ? P2 Pt1 Ag1 106.31(4) . 2_565 ? P1 Pt1 Ag1 102.60(4) . 2_565 ? S2 Pt1 Ag1 74.64(4) . 2_565 ? S1 Pt1 Ag1 74.03(4) . 2_565 ? Cl2 C40 Cl3 96.8(12) . . ? Cl2 C40 H40A 112.4 . . ? Cl3 C40 H40A 112.4 . . ? Cl2 C40 H40B 112.4 . . ? Cl3 C40 H40B 112.4 . . ? H40A C40 H40B 110.0 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 3.038 _refine_diff_density_min -1.700 _refine_diff_density_rms 0.238 #===END ###Material relevant to compound 11 at 173K ## data_compound11 _database_code_depnum_ccdc_archive 'CCDC 690636' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C78 H64 Ag2 Br2 N4 P4 Pd2 S4, C H2 Br2, H2 O' _chemical_formula_sum 'C79 H68 Ag2 Br4 N4 O P4 Pd2 S4' _chemical_formula_weight 2089.67 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2098(3) _cell_length_b 12.0948(4) _cell_length_c 17.5469(6) _cell_angle_alpha 101.960(2) _cell_angle_beta 95.545(2) _cell_angle_gamma 104.022(2) _cell_volume 2031.83(11) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5457 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27.36 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.708 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1028 _exptl_absorpt_coefficient_mu 3.104 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4273 _exptl_absorpt_correction_T_max 0.8356 _exptl_absorpt_process_details sadabs _exptl_special_details ; One phenyl ring is disordered over two positions, this disorder has been modelled accordingly. The hydrogen atoms on the water molecule have not been introduced but are taken into account in the compoun formula. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26156 _diffrn_reflns_av_R_equivalents 0.0467 _diffrn_reflns_av_sigmaI/netI 0.0681 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.62 _reflns_number_total 9324 _reflns_number_gt 6508 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1264P)^2^+17.7494P] 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 9324 _refine_ls_number_parameters 434 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1168 _refine_ls_R_factor_gt 0.0794 _refine_ls_wR_factor_ref 0.2579 _refine_ls_wR_factor_gt 0.2239 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _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 C1 C 0.4100(9) 0.2390(8) 0.4192(5) 0.0288(18) Uani 1 1 d . A . C2 C 0.4788(8) 0.3162(8) 0.4864(5) 0.0257(17) Uani 1 1 d . . . C3 C 0.6141(9) 0.3973(8) 0.4984(5) 0.0272(18) Uani 1 1 d . . . C4 C 0.7182(9) 0.4217(8) 0.4520(5) 0.0323(19) Uani 1 1 d . . . H4 H 0.7086 0.3781 0.4005 0.039 Uiso 1 1 calc R . . C5 C 0.8338(9) 0.5110(9) 0.4845(6) 0.037(2) Uani 1 1 d . . . H5 H 0.9046 0.5268 0.4554 0.044 Uiso 1 1 calc R . . C6 C 0.8454(9) 0.5775(9) 0.5602(6) 0.039(2) Uani 1 1 d . . . H6 H 0.9239 0.6389 0.5798 0.047 Uiso 1 1 calc R . . C7 C 0.6403(9) 0.4706(8) 0.5745(5) 0.0275(18) Uani 1 1 d . . . C8 C 0.5221(9) 0.4367(8) 0.6131(5) 0.0264(17) Uani 1 1 d . . . C9 C 0.4234(9) 0.3430(7) 0.5604(5) 0.0287(18) Uani 1 1 d . . . C10 C 0.3006(10) 0.3025(8) 0.5863(6) 0.036(2) Uani 1 1 d . . . H10 H 0.2313 0.2403 0.5548 0.044 Uiso 1 1 calc R . . C11 C 0.2852(11) 0.3589(10) 0.6615(6) 0.046(3) Uani 1 1 d . . . H11 H 0.2036 0.3341 0.6802 0.055 Uiso 1 1 calc R . . C12 C 0.3866(11) 0.4493(9) 0.7080(6) 0.042(2) Uani 1 1 d . . . H12 H 0.3715 0.4843 0.7576 0.050 Uiso 1 1 calc R . . C13 C 0.2127(13) -0.0243(10) 0.0667(6) 0.052(3) Uani 1 1 d . A . H13A H 0.1838 0.0434 0.0580 0.062 Uiso 1 1 calc R . . H13B H 0.2529 -0.0534 0.0215 0.062 Uiso 1 1 calc R . . C14 C 0.0859(14) -0.1209(11) 0.0731(8) 0.067(4) Uani 1 1 d . . . H14A H 0.0307 -0.1524 0.0213 0.081 Uiso 1 1 calc R . . H14B H 0.1168 -0.1842 0.0881 0.081 Uiso 1 1 calc R . . C15 C -0.0049(13) -0.0808(11) 0.1319(8) 0.061(4) Uani 1 1 d . A . H15A H -0.0920 -0.1400 0.1210 0.073 Uiso 1 1 calc R . . H15B H -0.0226 -0.0091 0.1224 0.073 Uiso 1 1 calc R . . C16B C 0.389(5) -0.124(3) 0.1583(16) 0.089(10) Uani 0.41(2) 1 d PG A 1 C17B C 0.435(5) -0.178(3) 0.0924(14) 0.089(10) Uani 0.41(2) 1 d PG A 1 H17 H 0.4368 -0.1478 0.0479 0.106 Uiso 0.41(2) 1 calc PR A 1 C18B C 0.479(4) -0.279(3) 0.0931(12) 0.089(10) Uani 0.41(2) 1 d PG A 1 H18B H 0.5093 -0.3152 0.0490 0.106 Uiso 0.41(2) 1 calc PR A 1 C19B C 0.476(4) -0.324(2) 0.1596(12) 0.089(10) Uani 0.41(2) 1 d PG A 1 H19B H 0.5052 -0.3912 0.1600 0.106 Uiso 0.41(2) 1 calc PR A 1 C20B C 0.430(4) -0.269(3) 0.2255(11) 0.089(10) Uani 0.41(2) 1 d PG A 1 H20B H 0.4285 -0.3000 0.2700 0.106 Uiso 0.41(2) 1 calc PR A 1 C21B C 0.387(5) -0.169(3) 0.2248(13) 0.089(10) Uani 0.41(2) 1 d PG A 1 H21B H 0.3560 -0.1326 0.2689 0.106 Uiso 0.41(2) 1 calc PR A 1 C16A C 0.432(2) -0.0823(17) 0.1558(9) 0.039(5) Uani 0.59(2) 1 d P A 2 C17A C 0.485(2) -0.1376(17) 0.0906(10) 0.040(4) Uani 0.59(2) 1 d P A 2 H17A H 0.4619 -0.1260 0.0409 0.048 Uiso 0.59(2) 1 calc PR A 2 C18A C 0.570(2) -0.2088(18) 0.1005(10) 0.045(5) Uani 0.59(2) 1 d P A 2 H18A H 0.6071 -0.2413 0.0578 0.054 Uiso 0.59(2) 1 calc PR A 2 C19A C 0.600(2) -0.2317(18) 0.1729(11) 0.048(5) Uani 0.59(2) 1 d P A 2 H19A H 0.6540 -0.2827 0.1781 0.057 Uiso 0.59(2) 1 calc PR A 2 C20A C 0.553(2) -0.181(2) 0.2358(10) 0.051(6) Uani 0.59(2) 1 d P A 2 H20A H 0.5765 -0.1935 0.2852 0.062 Uiso 0.59(2) 1 calc PR A 2 C21A C 0.466(3) -0.107(2) 0.2263(10) 0.059(7) Uani 0.59(2) 1 d P A 2 H21A H 0.4315 -0.0737 0.2699 0.070 Uiso 0.59(2) 1 calc PR A 2 C22 C 0.4768(11) 0.1389(13) 0.1343(6) 0.055(3) Uani 1 1 d . A . C23 C 0.4467(11) 0.2307(12) 0.1117(7) 0.054(3) Uani 1 1 d . . . H23 H 0.3560 0.2324 0.1030 0.065 Uiso 1 1 calc R . . C24 C 0.5496(14) 0.3236(17) 0.1009(8) 0.084(3) Uani 1 1 d . . . H24 H 0.5252 0.3862 0.0859 0.100 Uiso 1 1 calc R . . C25 C 0.6833(14) 0.3257(18) 0.1116(8) 0.084(3) Uani 1 1 d . . . H25 H 0.7496 0.3886 0.1041 0.100 Uiso 1 1 calc R . . C26 C 0.7175(15) 0.2378(17) 0.1325(8) 0.084(3) Uani 1 1 d . . . H26 H 0.8090 0.2378 0.1384 0.100 Uiso 1 1 calc R . . C27 C 0.6187(14) 0.1424(18) 0.1466(8) 0.087(6) Uani 1 1 d . . . H27 H 0.6459 0.0824 0.1637 0.104 Uiso 1 1 calc R . . C28 C 0.0577(12) -0.1981(9) 0.2529(7) 0.051(3) Uani 1 1 d . A . C29 C -0.0163(14) -0.3028(10) 0.2008(7) 0.058(3) Uani 1 1 d . . . H29 H -0.0709 -0.3012 0.1556 0.070 Uiso 1 1 calc R . . C30 C -0.0092(16) -0.4095(10) 0.2158(8) 0.065(4) Uani 1 1 d . . . H30 H -0.0578 -0.4788 0.1799 0.078 Uiso 1 1 calc R . . C31 C 0.0680(18) -0.4146(12) 0.2824(10) 0.078(5) Uani 1 1 d . . . H31 H 0.0754 -0.4867 0.2903 0.094 Uiso 1 1 calc R . . C32 C 0.1357(18) -0.3113(13) 0.3386(11) 0.088(5) Uani 1 1 d . . . H32 H 0.1842 -0.3142 0.3855 0.105 Uiso 1 1 calc R . . C33 C 0.1297(16) -0.2034(11) 0.3234(8) 0.069(4) Uani 1 1 d . . . H33 H 0.1742 -0.1343 0.3606 0.083 Uiso 1 1 calc R . . C34 C -0.0569(8) 0.0010(7) 0.2982(5) 0.056(3) Uani 1 1 d G A . C35 C -0.0932(11) -0.0384(8) 0.3642(6) 0.086(5) Uani 1 1 d G . . H35 H -0.0652 -0.1013 0.3763 0.103 Uiso 1 1 calc R . . C36 C -0.1714(13) 0.0160(10) 0.4121(6) 0.098(4) Uani 1 1 d G . . H36 H -0.1957 -0.0104 0.4563 0.117 Uiso 1 1 calc R . . C37 C -0.2133(11) 0.1099(9) 0.3940(5) 0.098(4) Uani 1 1 d G . . H37 H -0.2657 0.1463 0.4260 0.117 Uiso 1 1 calc R . . C38 C -0.1771(9) 0.1493(7) 0.3280(5) 0.050(3) Uani 1 1 d G . . H38 H -0.2051 0.2121 0.3159 0.061 Uiso 1 1 calc R . . C39 C -0.0989(8) 0.0949(7) 0.2801(4) 0.049(3) Uani 1 1 d G . . H39 H -0.0746 0.1213 0.2360 0.059 Uiso 1 1 calc R . . N1 N 0.7504(8) 0.5587(7) 0.6071(5) 0.0368(18) Uani 1 1 d . . . N2 N 0.5069(9) 0.4901(7) 0.6856(4) 0.0378(19) Uani 1 1 d . . . P1 P 0.3422(3) 0.0213(3) 0.15508(14) 0.0433(7) Uani 1 1 d . . . P2 P 0.0623(3) -0.0544(2) 0.23457(18) 0.0417(6) Uani 1 1 d . . . S1 S 0.4725(2) 0.2212(2) 0.32751(12) 0.0305(5) Uani 1 1 d . . . S2 S 0.2456(2) 0.1452(2) 0.40398(14) 0.0346(5) Uani 1 1 d . . . Br1 Br 0.89714(9) 0.73291(9) 0.84887(6) 0.0379(3) Uani 1 1 d . . . Pd1 Pd 0.27113(7) 0.07740(6) 0.27251(4) 0.0313(2) Uani 1 1 d . . . Ag1 Ag 0.70645(9) 0.66786(7) 0.72970(4) 0.0452(3) Uani 1 1 d . . . C40 C 0.1668(19) 0.516(5) 0.056(2) 0.1529(17) Uani 0.50 1 d PD B -1 H40A H 0.2078 0.5993 0.0635 0.183 Uiso 0.50 1 calc PR B -1 H40B H 0.1665 0.4986 0.1080 0.183 Uiso 0.50 1 calc PR B -1 Br2 Br 0.2789(6) 0.4174(6) -0.0121(4) 0.1529(17) Uani 0.50 1 d P B -1 Br3 Br -0.0430(5) 0.4659(7) -0.0075(5) 0.1529(17) Uani 0.50 1 d PD B -1 O1 O 0.465(4) -0.064(3) 0.458(2) 0.1529(17) Uani 0.50 1 d P C -1 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 C1 0.023(4) 0.028(4) 0.030(4) -0.003(3) 0.000(3) 0.006(3) C2 0.023(4) 0.025(4) 0.029(4) 0.005(3) 0.001(3) 0.009(3) C3 0.030(4) 0.026(4) 0.024(4) -0.001(3) -0.001(3) 0.012(4) C4 0.026(4) 0.037(5) 0.033(4) 0.001(4) 0.000(4) 0.014(4) C5 0.023(4) 0.034(5) 0.049(6) 0.000(4) 0.003(4) 0.009(4) C6 0.020(4) 0.034(5) 0.052(6) -0.010(4) -0.003(4) 0.006(4) C7 0.026(4) 0.028(4) 0.026(4) -0.001(3) -0.004(3) 0.012(4) C8 0.027(4) 0.027(4) 0.024(4) 0.001(3) 0.000(3) 0.010(3) C9 0.035(5) 0.020(4) 0.028(4) 0.000(3) 0.000(4) 0.007(4) C10 0.039(5) 0.028(5) 0.038(5) 0.000(4) 0.011(4) 0.005(4) C11 0.040(6) 0.051(7) 0.046(6) 0.003(5) 0.023(5) 0.013(5) C12 0.049(6) 0.038(6) 0.032(5) -0.005(4) 0.014(4) 0.007(5) C13 0.064(7) 0.040(6) 0.041(6) -0.010(5) -0.019(5) 0.024(6) C14 0.078(9) 0.036(6) 0.062(8) -0.006(6) -0.043(7) 0.003(6) C15 0.049(7) 0.046(7) 0.070(8) 0.001(6) -0.032(6) 0.003(6) C16B 0.18(3) 0.080(15) 0.040(8) 0.010(8) 0.030(11) 0.091(18) C17B 0.18(3) 0.080(15) 0.040(8) 0.010(8) 0.030(11) 0.091(18) C18B 0.18(3) 0.080(15) 0.040(8) 0.010(8) 0.030(11) 0.091(18) C19B 0.18(3) 0.080(15) 0.040(8) 0.010(8) 0.030(11) 0.091(18) C20B 0.18(3) 0.080(15) 0.040(8) 0.010(8) 0.030(11) 0.091(18) C21B 0.18(3) 0.080(15) 0.040(8) 0.010(8) 0.030(11) 0.091(18) C16A 0.062(12) 0.047(11) 0.012(6) -0.007(6) -0.002(7) 0.036(9) C17A 0.059(12) 0.049(11) 0.017(7) -0.003(7) 0.004(7) 0.032(9) C18A 0.061(12) 0.047(12) 0.036(9) 0.007(8) 0.019(8) 0.031(10) C19A 0.056(12) 0.050(12) 0.041(9) 0.005(8) 0.000(8) 0.031(10) C20A 0.069(14) 0.067(14) 0.028(8) 0.005(8) 0.006(8) 0.042(12) C21A 0.094(17) 0.085(16) 0.019(8) 0.010(9) 0.015(9) 0.063(14) C22 0.033(5) 0.097(10) 0.021(4) -0.021(5) -0.003(4) 0.025(6) C23 0.030(5) 0.076(9) 0.043(6) -0.013(6) 0.009(4) 0.010(6) C24 0.041(4) 0.132(10) 0.050(4) -0.015(5) 0.004(3) 0.005(5) C25 0.041(4) 0.132(10) 0.050(4) -0.015(5) 0.004(3) 0.005(5) C26 0.041(4) 0.132(10) 0.050(4) -0.015(5) 0.004(3) 0.005(5) C27 0.053(8) 0.164(17) 0.040(7) -0.008(8) -0.010(6) 0.057(10) C28 0.045(6) 0.028(5) 0.068(7) -0.007(5) -0.013(5) 0.011(5) C29 0.070(8) 0.035(6) 0.052(7) -0.007(5) -0.008(6) 0.002(6) C30 0.101(11) 0.029(6) 0.056(7) -0.006(5) 0.014(7) 0.012(6) C31 0.114(13) 0.037(7) 0.095(12) 0.017(7) 0.022(10) 0.039(8) C32 0.098(12) 0.054(9) 0.108(13) 0.020(9) -0.035(10) 0.032(8) C33 0.090(10) 0.040(7) 0.066(8) -0.005(6) -0.027(7) 0.029(7) C34 0.027(5) 0.034(6) 0.115(11) 0.029(6) 0.014(6) 0.011(4) C35 0.103(13) 0.083(12) 0.101(13) 0.046(10) 0.041(10) 0.049(10) C36 0.108(10) 0.107(10) 0.121(11) 0.060(9) 0.071(9) 0.059(8) C37 0.108(10) 0.107(10) 0.121(11) 0.060(9) 0.071(9) 0.059(8) C38 0.041(6) 0.075(8) 0.050(6) 0.026(6) 0.015(5) 0.030(6) C39 0.065(8) 0.050(7) 0.045(6) 0.023(5) 0.020(5) 0.023(6) N1 0.028(4) 0.033(4) 0.042(4) -0.003(3) -0.006(3) 0.010(3) N2 0.045(5) 0.037(5) 0.027(4) -0.006(3) -0.001(3) 0.018(4) P1 0.0404(14) 0.0594(18) 0.0248(11) -0.0142(11) -0.0091(10) 0.0297(13) P2 0.0298(13) 0.0232(12) 0.0596(17) -0.0043(11) -0.0164(11) 0.0045(10) S1 0.0231(10) 0.0358(12) 0.0256(10) -0.0061(8) 0.0014(8) 0.0075(9) S2 0.0260(11) 0.0307(12) 0.0366(12) -0.0081(9) 0.0057(9) 0.0019(9) Br1 0.0264(5) 0.0461(6) 0.0358(5) 0.0046(4) -0.0018(4) 0.0069(4) Pd1 0.0214(3) 0.0315(4) 0.0317(4) -0.0114(3) -0.0037(3) 0.0089(3) Ag1 0.0466(5) 0.0433(5) 0.0342(4) -0.0118(3) -0.0107(3) 0.0154(4) C40 0.117(3) 0.181(5) 0.170(4) 0.027(3) 0.047(3) 0.059(3) Br2 0.117(3) 0.181(5) 0.170(4) 0.027(3) 0.047(3) 0.059(3) Br3 0.117(3) 0.181(5) 0.170(4) 0.027(3) 0.047(3) 0.059(3) O1 0.117(3) 0.181(5) 0.170(4) 0.027(3) 0.047(3) 0.059(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.349(12) . ? C1 S2 1.744(9) . ? C1 S1 1.778(9) . ? C2 C3 1.455(12) . ? C2 C9 1.473(12) . ? C3 C7 1.401(11) . ? C3 C4 1.413(13) . ? C4 C5 1.371(13) . ? C4 H4 0.9300 . ? C5 C6 1.381(14) . ? C5 H5 0.9300 . ? C6 N1 1.339(13) . ? C6 H6 0.9300 . ? C7 N1 1.331(12) . ? C7 C8 1.455(12) . ? C8 N2 1.344(11) . ? C8 C9 1.410(12) . ? C9 C10 1.386(13) . ? C10 C11 1.397(13) . ? C10 H10 0.9300 . ? C11 C12 1.361(15) . ? C11 H11 0.9300 . ? C12 N2 1.337(13) . ? C12 H12 0.9300 . ? C13 C14 1.550(19) . ? C13 P1 1.831(10) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.54(2) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 P2 1.799(13) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16B C17B 1.3900 . ? C16B C21B 1.3900 . ? C16B P1 1.937(17) . ? C17B C18B 1.3900 . ? C17B H17 0.9300 . ? C18B C19B 1.3900 . ? C18B H18B 0.9300 . ? C19B C20B 1.3900 . ? C19B H19B 0.9300 . ? C20B C21B 1.3900 . ? C20B H20B 0.9300 . ? C21B H21B 0.9300 . ? C16A C21A 1.36(2) . ? C16A C17A 1.422(19) . ? C16A P1 1.725(18) . ? C17A C18A 1.39(2) . ? C17A H17A 0.9300 . ? C18A C19A 1.38(3) . ? C18A H18A 0.9300 . ? C19A C20A 1.34(2) . ? C19A H19A 0.9300 . ? C20A C21A 1.43(3) . ? C20A H20A 0.9300 . ? C21A H21A 0.9300 . ? C22 C23 1.345(19) . ? C22 C27 1.433(16) . ? C22 P1 1.846(15) . ? C23 C24 1.40(2) . ? C23 H23 0.9300 . ? C24 C25 1.35(2) . ? C24 H24 0.9300 . ? C25 C26 1.30(2) . ? C25 H25 0.9300 . ? C26 C27 1.42(3) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.390(15) . ? C28 C33 1.397(17) . ? C28 P2 1.822(12) . ? C29 C30 1.387(18) . ? C29 H29 0.9300 . ? C30 C31 1.37(2) . ? C30 H30 0.9300 . ? C31 C32 1.40(2) . ? C31 H31 0.9300 . ? C32 C33 1.400(18) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C35 1.3900 . ? C34 C39 1.3900 . ? C34 P2 1.878(7) . ? C35 C36 1.3900 . ? C35 H35 0.9300 . ? C36 C37 1.3900 . ? C36 H36 0.9300 . ? C37 C38 1.3900 . ? C37 H37 0.9300 . ? C38 C39 1.3900 . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? N1 Ag1 2.423(8) . ? N2 Ag1 2.501(9) . ? P1 Pd1 2.276(3) . ? P2 Pd1 2.274(3) . ? S1 Pd1 2.318(2) . ? S1 Ag1 2.746(2) 2_666 ? S2 Pd1 2.345(2) . ? Br1 Ag1 2.5634(12) . ? Pd1 Ag1 3.0424(11) 2_666 ? Ag1 S1 2.746(2) 2_666 ? Ag1 Pd1 3.0424(11) 2_666 ? C40 Br2 2.12(5) . ? C40 Br3 2.2002(10) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? 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 C2 C1 S2 127.8(7) . . ? C2 C1 S1 124.4(7) . . ? S2 C1 S1 107.7(5) . . ? C1 C2 C3 127.8(8) . . ? C1 C2 C9 125.6(8) . . ? C3 C2 C9 106.3(7) . . ? C7 C3 C4 115.0(8) . . ? C7 C3 C2 109.1(8) . . ? C4 C3 C2 135.8(8) . . ? C5 C4 C3 118.6(8) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? C4 C5 C6 120.3(9) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? N1 C6 C5 123.9(9) . . ? N1 C6 H6 118.1 . . ? C5 C6 H6 118.1 . . ? N1 C7 C3 127.7(9) . . ? N1 C7 C8 124.3(8) . . ? C3 C7 C8 108.0(8) . . ? N2 C8 C9 125.6(9) . . ? N2 C8 C7 125.5(8) . . ? C9 C8 C7 108.8(7) . . ? C10 C9 C8 116.8(8) . . ? C10 C9 C2 135.5(8) . . ? C8 C9 C2 107.7(8) . . ? C9 C10 C11 117.3(9) . . ? C9 C10 H10 121.4 . . ? C11 C10 H10 121.4 . . ? C12 C11 C10 121.6(9) . . ? C12 C11 H11 119.2 . . ? C10 C11 H11 119.2 . . ? N2 C12 C11 122.9(9) . . ? N2 C12 H12 118.5 . . ? C11 C12 H12 118.5 . . ? C14 C13 P1 112.7(8) . . ? C14 C13 H13A 109.1 . . ? P1 C13 H13A 109.1 . . ? C14 C13 H13B 109.1 . . ? P1 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? C15 C14 C13 115.3(10) . . ? C15 C14 H14A 108.5 . . ? C13 C14 H14A 108.5 . . ? C15 C14 H14B 108.5 . . ? C13 C14 H14B 108.5 . . ? H14A C14 H14B 107.5 . . ? C14 C15 P2 116.0(8) . . ? C14 C15 H15A 108.3 . . ? P2 C15 H15A 108.3 . . ? C14 C15 H15B 108.3 . . ? P2 C15 H15B 108.3 . . ? H15A C15 H15B 107.4 . . ? C17B C16B C21B 120.0 . . ? C17B C16B P1 117.3(14) . . ? C21B C16B P1 122.6(13) . . ? C18B C17B C16B 120.0 . . ? C18B C17B H17 120.0 . . ? C16B C17B H17 120.0 . . ? C17B C18B C19B 120.0 . . ? C17B C18B H18B 120.0 . . ? C19B C18B H18B 120.0 . . ? C18B C19B C20B 120.0 . . ? C18B C19B H19B 120.0 . . ? C20B C19B H19B 120.0 . . ? C21B C20B C19B 120.0 . . ? C21B C20B H20B 120.0 . . ? C19B C20B H20B 120.0 . . ? C20B C21B C16B 120.0 . . ? C20B C21B H21B 120.0 . . ? C16B C21B H21B 120.0 . . ? C21A C16A C17A 116.3(15) . . ? C21A C16A P1 117.6(12) . . ? C17A C16A P1 125.8(13) . . ? C18A C17A C16A 120.7(15) . . ? C18A C17A H17A 119.6 . . ? C16A C17A H17A 119.6 . . ? C19A C18A C17A 120.7(15) . . ? C19A C18A H18A 119.6 . . ? C17A C18A H18A 119.6 . . ? C20A C19A C18A 120.2(17) . . ? C20A C19A H19A 119.9 . . ? C18A C19A H19A 119.9 . . ? C19A C20A C21A 119.3(16) . . ? C19A C20A H20A 120.3 . . ? C21A C20A H20A 120.3 . . ? C16A C21A C20A 122.6(15) . . ? C16A C21A H21A 118.7 . . ? C20A C21A H21A 118.7 . . ? C23 C22 C27 116.3(14) . . ? C23 C22 P1 121.0(8) . . ? C27 C22 P1 122.5(13) . . ? C22 C23 C24 121.1(12) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C25 C24 C23 122.3(19) . . ? C25 C24 H24 118.8 . . ? C23 C24 H24 118.8 . . ? C26 C25 C24 118.9(18) . . ? C26 C25 H25 120.6 . . ? C24 C25 H25 120.6 . . ? C25 C26 C27 121.7(15) . . ? C25 C26 H26 119.1 . . ? C27 C26 H26 119.1 . . ? C26 C27 C22 119.6(17) . . ? C26 C27 H27 120.2 . . ? C22 C27 H27 120.2 . . ? C29 C28 C33 118.4(11) . . ? C29 C28 P2 123.1(10) . . ? C33 C28 P2 118.5(8) . . ? C30 C29 C28 120.4(12) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C31 C30 C29 121.1(12) . . ? C31 C30 H30 119.4 . . ? C29 C30 H30 119.4 . . ? C30 C31 C32 119.8(12) . . ? C30 C31 H31 120.1 . . ? C32 C31 H31 120.1 . . ? C31 C32 C33 119.1(14) . . ? C31 C32 H32 120.4 . . ? C33 C32 H32 120.4 . . ? C28 C33 C32 120.9(12) . . ? C28 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C35 C34 C39 120.0 . . ? C35 C34 P2 124.3(4) . . ? C39 C34 P2 115.5(4) . . ? C34 C35 C36 120.0 . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C35 C36 C37 120.0 . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? C36 C37 C38 120.0 . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C39 C38 C37 120.0 . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 C34 120.0 . . ? C38 C39 H39 120.0 . . ? C34 C39 H39 120.0 . . ? C7 N1 C6 114.5(8) . . ? C7 N1 Ag1 109.0(6) . . ? C6 N1 Ag1 135.3(6) . . ? C12 N2 C8 115.8(8) . . ? C12 N2 Ag1 137.3(6) . . ? C8 N2 Ag1 105.7(6) . . ? C16A P1 C13 110.1(7) . . ? C16A P1 C22 98.9(8) . . ? C13 P1 C22 104.1(6) . . ? C16A P1 C16B 17.4(17) . . ? C13 P1 C16B 101.9(13) . . ? C22 P1 C16B 116.1(15) . . ? C16A P1 Pd1 112.6(6) . . ? C13 P1 Pd1 116.8(4) . . ? C22 P1 Pd1 112.6(3) . . ? C16B P1 Pd1 105.2(8) . . ? C15 P2 C28 106.0(6) . . ? C15 P2 C34 110.6(5) . . ? C28 P2 C34 104.4(5) . . ? C15 P2 Pd1 114.4(5) . . ? C28 P2 Pd1 113.8(4) . . ? C34 P2 Pd1 107.3(3) . . ? C1 S1 Pd1 88.5(3) . . ? C1 S1 Ag1 90.4(3) . 2_666 ? Pd1 S1 Ag1 73.31(6) . 2_666 ? C1 S2 Pd1 88.5(3) . . ? P2 Pd1 P1 93.49(11) . . ? P2 Pd1 S1 171.86(10) . . ? P1 Pd1 S1 94.62(9) . . ? P2 Pd1 S2 96.80(10) . . ? P1 Pd1 S2 168.25(9) . . ? S1 Pd1 S2 75.19(8) . . ? P2 Pd1 Ag1 118.27(7) . 2_666 ? P1 Pd1 Ag1 98.22(9) . 2_666 ? S1 Pd1 Ag1 59.83(6) . 2_666 ? S2 Pd1 Ag1 81.87(7) . 2_666 ? N1 Ag1 N2 74.6(3) . . ? N1 Ag1 Br1 117.73(19) . . ? N2 Ag1 Br1 131.62(19) . . ? N1 Ag1 S1 100.17(19) . 2_666 ? N2 Ag1 S1 83.66(19) . 2_666 ? Br1 Ag1 S1 132.39(6) . 2_666 ? N1 Ag1 Pd1 111.7(2) . 2_666 ? N2 Ag1 Pd1 130.43(19) . 2_666 ? Br1 Ag1 Pd1 90.56(4) . 2_666 ? S1 Ag1 Pd1 46.87(5) 2_666 2_666 ? Br2 C40 Br3 107.2(17) . . ? Br2 C40 H40A 110.3 . . ? Br3 C40 H40A 110.3 . . ? Br2 C40 H40B 110.3 . . ? Br3 C40 H40B 110.3 . . ? H40A C40 H40B 108.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.62 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 3.521 _refine_diff_density_min -2.822 _refine_diff_density_rms 0.343 #===END ###Material relevant to compound 12 at 173K ## data_compound12 _database_code_depnum_ccdc_archive 'CCDC 690637' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C82 H64 Ag2 Cl2 N4 P4 Pt2 S8, 2(C2 H3 N), 2(C H2 Cl2)' _chemical_formula_sum 'C88 H74 Ag2 Cl6 N6 P4 Pt2 S8' _chemical_formula_weight 2414.51 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' 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' _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 9.8721(2) _cell_length_b 16.2902(4) _cell_length_c 27.9170(7) _cell_angle_alpha 90.00 _cell_angle_beta 100.0700(10) _cell_angle_gamma 90.00 _cell_volume 4420.41(18) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3958 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 23.54 _exptl_crystal_description platelet _exptl_crystal_colour orange _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.814 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2368 _exptl_absorpt_coefficient_mu 4.084 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6188 _exptl_absorpt_correction_T_max 0.8537 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34440 _diffrn_reflns_av_R_equivalents 0.0600 _diffrn_reflns_av_sigmaI/netI 0.0682 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 27.55 _reflns_number_total 10142 _reflns_number_gt 6990 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1106P)^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 10142 _refine_ls_number_parameters 512 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0905 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1798 _refine_ls_wR_factor_gt 0.1507 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.047 _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 C1 C 0.6097(8) 0.8975(5) 0.3742(3) 0.0275(17) Uani 1 1 d . . . C2 C 0.4918(8) 0.9339(5) 0.3566(3) 0.0272(17) Uani 1 1 d . . . C3 C 0.5935(8) 1.0156(6) 0.4355(3) 0.0290(18) Uani 1 1 d . . . C4 C 0.6126(8) 1.0669(5) 0.4754(3) 0.0290(18) Uani 1 1 d . . . C5 C 0.7281(9) 1.0651(6) 0.5168(3) 0.0313(19) Uani 1 1 d . . . C6 C 0.8400(9) 1.0132(6) 0.5310(3) 0.038(2) Uani 1 1 d . . . H6 H 0.8584 0.9697 0.5115 0.046 Uiso 1 1 calc R . . C7 C 0.9229(9) 1.0291(6) 0.5754(3) 0.041(2) Uani 1 1 d . . . H7 H 0.9983 0.9954 0.5857 0.049 Uiso 1 1 calc R . . C8 C 0.8975(10) 1.0932(7) 0.6049(3) 0.042(2) Uani 1 1 d . . . H8 H 0.9568 1.1017 0.6343 0.050 Uiso 1 1 calc R . . C9 C 0.7046(8) 1.1277(5) 0.5490(3) 0.0290(18) Uani 1 1 d . . . C10 C 0.5806(9) 1.1693(6) 0.5299(3) 0.0317(19) Uani 1 1 d . . . C11 C 0.5230(9) 1.1329(5) 0.4851(3) 0.0309(19) Uani 1 1 d . . . C12 C 0.4013(9) 1.1656(5) 0.4615(3) 0.0340(19) Uani 1 1 d . . . H12 H 0.3584 1.1442 0.4318 0.041 Uiso 1 1 calc R . . C13 C 0.3430(11) 1.2313(6) 0.4826(3) 0.039(2) Uani 1 1 d . . . H13 H 0.2617 1.2551 0.4667 0.046 Uiso 1 1 calc R . . C14 C 0.4077(12) 1.2612(6) 0.5277(4) 0.045(2) Uani 1 1 d . . . H14 H 0.3655 1.3036 0.5419 0.054 Uiso 1 1 calc R . . C15 C 0.1502(8) 0.8190(6) 0.2299(3) 0.0318(19) Uani 1 1 d . . . C16 C 0.1151(10) 0.8907(6) 0.2034(4) 0.042(2) Uani 1 1 d . . . H16 H 0.1681 0.9094 0.1812 0.050 Uiso 1 1 calc R . . C17 C -0.0015(10) 0.9336(7) 0.2109(4) 0.049(3) Uani 1 1 d . . . H17 H -0.0272 0.9811 0.1932 0.058 Uiso 1 1 calc R . . C18 C -0.0794(10) 0.9065(7) 0.2445(4) 0.048(3) Uani 1 1 d . . . H18 H -0.1564 0.9361 0.2493 0.057 Uiso 1 1 calc R . . C19 C -0.0426(9) 0.8351(7) 0.2709(3) 0.039(2) Uani 1 1 d . . . H19 H -0.0959 0.8169 0.2932 0.047 Uiso 1 1 calc R . . C20 C 0.0743(10) 0.7902(6) 0.2643(3) 0.040(2) Uani 1 1 d . . . H20 H 0.1004 0.7429 0.2822 0.048 Uiso 1 1 calc R . . C21 C 0.3526(9) 0.7999(6) 0.1668(3) 0.036(2) Uani 1 1 d . . . C22 C 0.4433(10) 0.8637(6) 0.1682(3) 0.041(2) Uani 1 1 d . . . H22 H 0.4774 0.8885 0.1979 0.049 Uiso 1 1 calc R . . C23 C 0.4857(12) 0.8923(7) 0.1264(4) 0.056(3) Uani 1 1 d . . . H23 H 0.5467 0.9361 0.1276 0.067 Uiso 1 1 calc R . . C24 C 0.4350(13) 0.8544(9) 0.0836(4) 0.063(3) Uani 1 1 d . . . H24 H 0.4645 0.8721 0.0554 0.076 Uiso 1 1 calc R . . C25 C 0.3429(14) 0.7917(8) 0.0803(4) 0.061(4) Uani 1 1 d . . . H25 H 0.3087 0.7671 0.0506 0.074 Uiso 1 1 calc R . . C26 C 0.3027(12) 0.7661(7) 0.1221(4) 0.049(3) Uani 1 1 d . . . H26 H 0.2385 0.7239 0.1203 0.059 Uiso 1 1 calc R . . C27 C 0.6935(9) 0.6206(5) 0.3252(3) 0.035(2) Uani 1 1 d . . . C28 C 0.8364(9) 0.6258(7) 0.3338(3) 0.040(2) Uani 1 1 d . . . H28 H 0.8809 0.6491 0.3104 0.048 Uiso 1 1 calc R . . C29 C 0.9132(10) 0.5968(8) 0.3767(4) 0.053(3) Uani 1 1 d . . . H29 H 1.0088 0.5989 0.3815 0.063 Uiso 1 1 calc R . . C30 C 0.8476(11) 0.5647(7) 0.4125(3) 0.051(3) Uani 1 1 d . . . H30 H 0.8993 0.5465 0.4416 0.061 Uiso 1 1 calc R . . C31 C 0.7075(10) 0.5598(6) 0.4053(3) 0.039(2) Uani 1 1 d . . . H31 H 0.6639 0.5370 0.4291 0.047 Uiso 1 1 calc R . . C32 C 0.6291(10) 0.5892(6) 0.3616(3) 0.038(2) Uani 1 1 d . . . H32 H 0.5335 0.5875 0.3571 0.045 Uiso 1 1 calc R . . C33 C 0.6996(9) 0.6638(6) 0.2256(3) 0.0319(19) Uani 1 1 d . . . C34 C 0.7721(8) 0.5934(6) 0.2162(3) 0.0333(19) Uani 1 1 d . . . H34 H 0.7644 0.5452 0.2334 0.040 Uiso 1 1 calc R . . C35 C 0.8556(10) 0.5964(7) 0.1811(3) 0.046(2) Uani 1 1 d . . . H35 H 0.9066 0.5504 0.1756 0.055 Uiso 1 1 calc R . . C36 C 0.8638(9) 0.6646(7) 0.1549(3) 0.044(3) Uani 1 1 d . . . H36 H 0.9166 0.6646 0.1304 0.053 Uiso 1 1 calc R . . C37 C 0.7956(10) 0.7340(7) 0.1638(3) 0.047(3) Uani 1 1 d . . . H37 H 0.8050 0.7813 0.1461 0.056 Uiso 1 1 calc R . . C38 C 0.7127(10) 0.7353(7) 0.1988(3) 0.039(2) Uani 1 1 d . . . H38 H 0.6661 0.7829 0.2045 0.047 Uiso 1 1 calc R . . C39 C 0.2497(9) 0.6574(6) 0.2122(4) 0.038(2) Uani 1 1 d . . . H39A H 0.2101 0.6385 0.2397 0.046 Uiso 1 1 calc R . . H39B H 0.1776 0.6563 0.1837 0.046 Uiso 1 1 calc R . . C40 C 0.3631(9) 0.5977(6) 0.2042(3) 0.037(2) Uani 1 1 d . . . H40A H 0.4120 0.6206 0.1800 0.044 Uiso 1 1 calc R . . H40B H 0.3210 0.5467 0.1912 0.044 Uiso 1 1 calc R . . C41 C 0.4684(8) 0.5784(6) 0.2510(3) 0.0341(19) Uani 1 1 d . . . H41A H 0.5208 0.5302 0.2452 0.041 Uiso 1 1 calc R . . H41B H 0.4185 0.5653 0.2770 0.041 Uiso 1 1 calc R . . N1 N 0.7889(8) 1.1441(5) 0.5924(3) 0.0407(19) Uani 1 1 d . . . N2 N 0.5259(9) 1.2323(5) 0.5513(3) 0.0365(18) Uani 1 1 d . . . P1 P 0.3079(2) 0.76336(15) 0.22344(8) 0.0303(5) Uani 1 1 d . . . P2 P 0.5875(2) 0.66176(14) 0.27093(8) 0.0279(5) Uani 1 1 d . . . S1 S 0.3712(2) 0.89508(13) 0.30979(7) 0.0287(4) Uani 1 1 d . . . S2 S 0.6669(2) 0.80697(15) 0.35015(8) 0.0326(5) Uani 1 1 d . . . S3 S 0.7106(2) 0.93899(14) 0.42656(7) 0.0322(5) Uani 1 1 d . . . S4 S 0.4488(2) 1.01921(14) 0.38992(7) 0.0292(4) Uani 1 1 d . . . Cl1 Cl 0.7552(2) 1.39014(13) 0.65787(8) 0.0323(4) Uani 1 1 d . . . Ag1 Ag 0.66826(9) 1.24981(5) 0.63302(3) 0.0484(2) Uani 1 1 d . . . Pt1 Pt 0.48404(3) 0.78066(2) 0.287177(11) 0.02517(12) Uani 1 1 d . . . C42 C 0.2148(18) 0.4476(10) 0.4402(7) 0.186(2) Uani 1 1 d D . . H42A H 0.2327 0.4621 0.4082 0.223 Uiso 1 1 calc R . . H42B H 0.2889 0.4116 0.4548 0.223 Uiso 1 1 calc R . . Cl2 Cl 0.0700(9) 0.3918(5) 0.4319(2) 0.186(2) Uani 1 1 d D . . Cl3 Cl 0.2284(8) 0.5346(5) 0.4736(2) 0.186(2) Uani 1 1 d D . . C43 C 0.9869(17) 0.7504(9) -0.0312(6) 0.087(5) Uani 1 1 d . . . H43A H 1.0122 0.8063 -0.0232 0.130 Uiso 1 1 calc R . . H43B H 0.8907 0.7478 -0.0448 0.130 Uiso 1 1 calc R . . H43C H 1.0398 0.7301 -0.0544 0.130 Uiso 1 1 calc R . . C44 C 1.0142(13) 0.7000(9) 0.0130(5) 0.061(3) Uani 1 1 d . . . N3 N 1.0367(11) 0.6640(7) 0.0464(5) 0.073(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.030(4) 0.029(5) 0.025(4) -0.003(3) 0.010(3) -0.004(3) C2 0.030(4) 0.027(4) 0.027(4) -0.003(3) 0.010(3) 0.004(3) C3 0.029(4) 0.037(5) 0.022(4) 0.006(3) 0.008(3) 0.004(4) C4 0.030(4) 0.031(5) 0.028(4) 0.005(3) 0.009(3) -0.004(4) C5 0.034(5) 0.035(5) 0.025(4) 0.001(3) 0.007(3) -0.006(4) C6 0.033(5) 0.051(6) 0.032(4) 0.005(4) 0.010(4) -0.002(4) C7 0.033(5) 0.048(6) 0.038(5) 0.012(4) 0.000(4) -0.006(4) C8 0.039(5) 0.053(6) 0.031(4) 0.005(4) 0.004(4) -0.009(5) C9 0.030(4) 0.029(5) 0.027(4) -0.002(3) 0.003(3) -0.005(4) C10 0.034(5) 0.034(5) 0.028(4) -0.005(3) 0.008(3) -0.013(4) C11 0.044(5) 0.028(5) 0.022(4) -0.004(3) 0.009(3) -0.006(4) C12 0.041(5) 0.030(5) 0.033(4) 0.000(4) 0.011(4) 0.002(4) C13 0.044(6) 0.035(5) 0.037(5) -0.003(4) 0.010(4) 0.003(4) C14 0.057(7) 0.037(6) 0.044(5) -0.010(4) 0.015(5) -0.005(5) C15 0.027(4) 0.033(5) 0.035(4) -0.012(4) 0.003(3) -0.001(4) C16 0.039(5) 0.038(6) 0.047(5) -0.002(4) 0.003(4) 0.005(4) C17 0.047(6) 0.038(6) 0.060(6) 0.007(5) 0.007(5) 0.010(5) C18 0.028(5) 0.058(7) 0.056(6) -0.020(5) 0.005(4) 0.004(5) C19 0.026(4) 0.055(7) 0.038(5) -0.010(4) 0.009(4) -0.006(4) C20 0.037(5) 0.040(6) 0.042(5) -0.006(4) 0.006(4) 0.001(4) C21 0.035(5) 0.044(6) 0.029(4) -0.005(4) 0.005(4) 0.009(4) C22 0.049(6) 0.042(6) 0.032(4) 0.010(4) 0.010(4) 0.016(5) C23 0.068(7) 0.057(7) 0.050(6) 0.020(5) 0.027(6) 0.019(6) C24 0.070(8) 0.084(10) 0.041(6) 0.019(6) 0.025(6) 0.021(7) C25 0.073(8) 0.075(9) 0.037(6) -0.008(5) 0.012(5) 0.031(7) C26 0.048(6) 0.064(8) 0.036(5) -0.009(5) 0.006(5) 0.013(5) C27 0.044(5) 0.027(5) 0.035(4) 0.000(4) 0.008(4) 0.008(4) C28 0.031(5) 0.056(6) 0.035(5) -0.006(4) 0.010(4) -0.004(4) C29 0.035(5) 0.081(9) 0.043(5) 0.004(5) 0.008(4) 0.013(5) C30 0.061(7) 0.057(7) 0.031(5) 0.007(4) 0.000(5) 0.018(6) C31 0.045(5) 0.040(6) 0.034(5) 0.009(4) 0.013(4) -0.007(4) C32 0.038(5) 0.036(5) 0.040(5) 0.003(4) 0.011(4) -0.003(4) C33 0.029(4) 0.038(5) 0.030(4) -0.004(4) 0.008(3) -0.003(4) C34 0.030(4) 0.033(5) 0.038(5) -0.008(4) 0.009(4) 0.003(4) C35 0.037(5) 0.061(7) 0.040(5) -0.015(5) 0.010(4) 0.005(5) C36 0.028(5) 0.076(8) 0.031(4) -0.008(5) 0.012(4) -0.001(5) C37 0.037(5) 0.070(8) 0.033(5) 0.005(5) 0.004(4) -0.010(5) C38 0.029(5) 0.059(7) 0.027(4) 0.001(4) 0.001(4) 0.003(4) C39 0.025(4) 0.042(6) 0.049(5) -0.011(4) 0.008(4) -0.004(4) C40 0.037(5) 0.027(5) 0.045(5) -0.010(4) 0.004(4) -0.004(4) C41 0.034(5) 0.030(5) 0.043(5) 0.001(4) 0.017(4) 0.009(4) N1 0.052(5) 0.040(5) 0.032(4) 0.000(3) 0.010(4) -0.015(4) N2 0.045(5) 0.031(4) 0.033(4) -0.005(3) 0.006(3) -0.001(3) P1 0.0270(11) 0.0359(13) 0.0278(10) -0.0046(9) 0.0045(9) 0.0024(9) P2 0.0262(11) 0.0280(12) 0.0305(10) -0.0016(8) 0.0079(9) 0.0029(9) S1 0.0286(10) 0.0264(11) 0.0304(10) -0.0042(8) 0.0034(8) 0.0026(8) S2 0.0269(10) 0.0389(12) 0.0320(10) -0.0067(9) 0.0049(9) 0.0071(9) S3 0.0271(10) 0.0379(13) 0.0311(10) -0.0074(9) 0.0035(8) 0.0029(9) S4 0.0287(10) 0.0310(11) 0.0278(10) -0.0044(8) 0.0044(8) 0.0014(9) Cl1 0.0310(10) 0.0269(11) 0.0416(11) -0.0026(8) 0.0136(9) -0.0077(8) Ag1 0.0641(5) 0.0473(5) 0.0384(4) -0.0124(3) 0.0219(4) -0.0221(4) Pt1 0.02468(18) 0.02603(19) 0.02570(17) -0.00171(12) 0.00687(12) 0.00132(13) C42 0.211(5) 0.209(6) 0.138(4) 0.075(4) 0.033(4) 0.052(5) Cl2 0.211(5) 0.209(6) 0.138(4) 0.075(4) 0.033(4) 0.052(5) Cl3 0.211(5) 0.209(6) 0.138(4) 0.075(4) 0.033(4) 0.052(5) C43 0.083(10) 0.092(11) 0.093(11) -0.013(10) 0.037(9) 0.011(9) C44 0.055(7) 0.055(8) 0.077(9) -0.008(7) 0.026(7) 0.003(6) N3 0.064(7) 0.059(7) 0.098(9) -0.013(7) 0.022(7) -0.001(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.322(11) . ? C1 S2 1.754(9) . ? C1 S3 1.754(8) . ? C2 S1 1.727(8) . ? C2 S4 1.765(8) . ? C3 C4 1.378(11) . ? C3 S4 1.741(8) . ? C3 S3 1.748(9) . ? C4 C11 1.449(12) . ? C4 C5 1.474(11) . ? C5 C6 1.393(13) . ? C5 C9 1.406(12) . ? C6 C7 1.386(12) . ? C6 H6 0.9300 . ? C7 C8 1.380(14) . ? C7 H7 0.9300 . ? C8 N1 1.352(13) . ? C8 H8 0.9300 . ? C9 N1 1.371(10) . ? C9 C10 1.418(12) . ? C10 N2 1.348(12) . ? C10 C11 1.410(11) . ? C11 C12 1.373(12) . ? C12 C13 1.394(12) . ? C12 H12 0.9300 . ? C13 C14 1.396(13) . ? C13 H13 0.9300 . ? C14 N2 1.322(14) . ? C14 H14 0.9300 . ? C15 C16 1.393(13) . ? C15 C20 1.399(13) . ? C15 P1 1.837(9) . ? C16 C17 1.394(13) . ? C16 H16 0.9300 . ? C17 C18 1.383(15) . ? C17 H17 0.9300 . ? C18 C19 1.392(15) . ? C18 H18 0.9300 . ? C19 C20 1.407(13) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.368(14) . ? C21 C26 1.374(13) . ? C21 P1 1.813(9) . ? C22 C23 1.387(13) . ? C22 H22 0.9300 . ? C23 C24 1.361(16) . ? C23 H23 0.9300 . ? C24 C25 1.361(18) . ? C24 H24 0.9300 . ? C25 C26 1.362(16) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C32 1.386(12) . ? C27 C28 1.391(12) . ? C27 P2 1.813(9) . ? C28 C29 1.385(13) . ? C28 H28 0.9300 . ? C29 C30 1.384(14) . ? C29 H29 0.9300 . ? C30 C31 1.365(14) . ? C30 H30 0.9300 . ? C31 C32 1.410(12) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.400(12) . ? C33 C38 1.402(13) . ? C33 P2 1.822(8) . ? C34 C35 1.389(12) . ? C34 H34 0.9300 . ? C35 C36 1.341(15) . ? C35 H35 0.9300 . ? C36 C37 1.360(15) . ? C36 H36 0.9300 . ? C37 C38 1.379(13) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C40 1.528(12) . ? C39 P1 1.829(10) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C41 1.552(12) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 P2 1.818(9) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? N1 Ag1 2.479(9) . ? N2 Ag1 2.478(8) . ? P1 Pt1 2.278(2) . ? P2 Pt1 2.272(2) . ? S1 Pt1 2.315(2) . ? S1 Ag1 2.914(2) 3_676 ? S2 Pt1 2.329(2) . ? Cl1 Ag1 2.497(2) . ? Ag1 S1 2.914(2) 3_676 ? Ag1 Pt1 2.9396(8) 3_676 ? Pt1 Ag1 2.9396(8) 3_676 ? C42 Cl2 1.674(9) . ? C42 Cl3 1.690(10) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.47(2) . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 N3 1.089(16) . ? 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 C2 C1 S2 123.8(6) . . ? C2 C1 S3 118.1(6) . . ? S2 C1 S3 118.0(5) . . ? C1 C2 S1 124.3(6) . . ? C1 C2 S4 115.8(6) . . ? S1 C2 S4 119.3(5) . . ? C4 C3 S4 123.3(7) . . ? C4 C3 S3 123.2(6) . . ? S4 C3 S3 113.5(5) . . ? C3 C4 C11 126.9(8) . . ? C3 C4 C5 126.8(8) . . ? C11 C4 C5 106.4(7) . . ? C6 C5 C9 118.0(8) . . ? C6 C5 C4 134.6(8) . . ? C9 C5 C4 107.2(8) . . ? C7 C6 C5 117.1(9) . . ? C7 C6 H6 121.4 . . ? C5 C6 H6 121.4 . . ? C8 C7 C6 122.4(9) . . ? C8 C7 H7 118.8 . . ? C6 C7 H7 118.8 . . ? N1 C8 C7 121.8(8) . . ? N1 C8 H8 119.1 . . ? C7 C8 H8 119.1 . . ? N1 C9 C5 124.3(8) . . ? N1 C9 C10 126.1(8) . . ? C5 C9 C10 109.6(7) . . ? N2 C10 C11 125.5(8) . . ? N2 C10 C9 125.8(8) . . ? C11 C10 C9 108.7(8) . . ? C12 C11 C10 116.6(8) . . ? C12 C11 C4 135.2(8) . . ? C10 C11 C4 108.2(8) . . ? C11 C12 C13 119.1(8) . . ? C11 C12 H12 120.4 . . ? C13 C12 H12 120.4 . . ? C12 C13 C14 119.4(9) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? N2 C14 C13 123.4(10) . . ? N2 C14 H14 118.3 . . ? C13 C14 H14 118.3 . . ? C16 C15 C20 122.2(9) . . ? C16 C15 P1 119.9(7) . . ? C20 C15 P1 117.8(7) . . ? C15 C16 C17 118.4(9) . . ? C15 C16 H16 120.8 . . ? C17 C16 H16 120.8 . . ? C18 C17 C16 120.9(10) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C17 C18 C19 120.1(9) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C18 C19 C20 120.6(9) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C15 C20 C19 117.8(9) . . ? C15 C20 H20 121.1 . . ? C19 C20 H20 121.1 . . ? C22 C21 C26 117.3(9) . . ? C22 C21 P1 118.9(7) . . ? C26 C21 P1 123.8(8) . . ? C21 C22 C23 121.6(10) . . ? C21 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? C24 C23 C22 117.9(12) . . ? C24 C23 H23 121.0 . . ? C22 C23 H23 121.0 . . ? C23 C24 C25 122.5(10) . . ? C23 C24 H24 118.7 . . ? C25 C24 H24 118.7 . . ? C24 C25 C26 117.7(11) . . ? C24 C25 H25 121.2 . . ? C26 C25 H25 121.2 . . ? C25 C26 C21 123.0(12) . . ? C25 C26 H26 118.5 . . ? C21 C26 H26 118.5 . . ? C32 C27 C28 118.5(8) . . ? C32 C27 P2 118.5(7) . . ? C28 C27 P2 122.8(7) . . ? C29 C28 C27 120.9(9) . . ? C29 C28 H28 119.5 . . ? C27 C28 H28 119.5 . . ? C30 C29 C28 119.9(9) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? C31 C30 C29 120.4(9) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C30 C31 C32 119.8(8) . . ? C30 C31 H31 120.1 . . ? C32 C31 H31 120.1 . . ? C27 C32 C31 120.4(8) . . ? C27 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C34 C33 C38 118.9(8) . . ? C34 C33 P2 120.4(7) . . ? C38 C33 P2 120.6(7) . . ? C35 C34 C33 119.3(9) . . ? C35 C34 H34 120.4 . . ? C33 C34 H34 120.4 . . ? C36 C35 C34 120.9(10) . . ? C36 C35 H35 119.6 . . ? C34 C35 H35 119.6 . . ? C35 C36 C37 120.7(9) . . ? C35 C36 H36 119.6 . . ? C37 C36 H36 119.6 . . ? C36 C37 C38 121.1(10) . . ? C36 C37 H37 119.5 . . ? C38 C37 H37 119.5 . . ? C37 C38 C33 119.1(10) . . ? C37 C38 H38 120.5 . . ? C33 C38 H38 120.5 . . ? C40 C39 P1 114.2(6) . . ? C40 C39 H39A 108.7 . . ? P1 C39 H39A 108.7 . . ? C40 C39 H39B 108.7 . . ? P1 C39 H39B 108.7 . . ? H39A C39 H39B 107.6 . . ? C39 C40 C41 113.9(7) . . ? C39 C40 H40A 108.8 . . ? C41 C40 H40A 108.8 . . ? C39 C40 H40B 108.8 . . ? C41 C40 H40B 108.8 . . ? H40A C40 H40B 107.7 . . ? C40 C41 P2 114.1(6) . . ? C40 C41 H41A 108.7 . . ? P2 C41 H41A 108.7 . . ? C40 C41 H41B 108.7 . . ? P2 C41 H41B 108.7 . . ? H41A C41 H41B 107.6 . . ? C8 N1 C9 116.2(8) . . ? C8 N1 Ag1 136.9(6) . . ? C9 N1 Ag1 105.9(6) . . ? C14 N2 C10 116.0(8) . . ? C14 N2 Ag1 136.6(7) . . ? C10 N2 Ag1 106.8(6) . . ? C21 P1 C39 106.1(4) . . ? C21 P1 C15 105.2(4) . . ? C39 P1 C15 103.7(4) . . ? C21 P1 Pt1 111.8(3) . . ? C39 P1 Pt1 115.1(3) . . ? C15 P1 Pt1 114.0(3) . . ? C27 P2 C41 103.2(4) . . ? C27 P2 C33 104.8(4) . . ? C41 P2 C33 103.9(4) . . ? C27 P2 Pt1 111.3(3) . . ? C41 P2 Pt1 114.1(3) . . ? C33 P2 Pt1 118.2(3) . . ? C2 S1 Pt1 101.5(3) . . ? C2 S1 Ag1 91.3(3) . 3_676 ? Pt1 S1 Ag1 67.29(6) . 3_676 ? C1 S2 Pt1 100.7(3) . . ? C3 S3 C1 95.8(4) . . ? C3 S4 C2 96.6(4) . . ? N2 Ag1 N1 74.9(3) . . ? N2 Ag1 Cl1 118.25(19) . . ? N1 Ag1 Cl1 126.43(19) . . ? N2 Ag1 S1 107.61(19) . 3_676 ? N1 Ag1 S1 78.98(18) . 3_676 ? Cl1 Ag1 S1 131.44(7) . 3_676 ? N2 Ag1 Pt1 113.3(2) . 3_676 ? N1 Ag1 Pt1 125.44(18) . 3_676 ? Cl1 Ag1 Pt1 98.09(5) . 3_676 ? S1 Ag1 Pt1 46.60(4) 3_676 3_676 ? P2 Pt1 P1 92.69(8) . . ? P2 Pt1 S1 174.44(8) . . ? P1 Pt1 S1 88.55(8) . . ? P2 Pt1 S2 89.51(8) . . ? P1 Pt1 S2 176.12(9) . . ? S1 Pt1 S2 89.56(7) . . ? P2 Pt1 Ag1 108.34(6) . 3_676 ? P1 Pt1 Ag1 98.59(6) . 3_676 ? S1 Pt1 Ag1 66.11(6) . 3_676 ? S2 Pt1 Ag1 83.72(6) . 3_676 ? Cl2 C42 Cl3 121.0(12) . . ? Cl2 C42 H42A 107.1 . . ? Cl3 C42 H42A 107.1 . . ? Cl2 C42 H42B 107.1 . . ? Cl3 C42 H42B 107.1 . . ? H42A C42 H42B 106.8 . . ? C44 C43 H43A 109.5 . . ? C44 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C44 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N3 C44 C43 178.2(17) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 3.565 _refine_diff_density_min -2.465 _refine_diff_density_rms 0.458 #===END