# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_VR _audit_creation_date 2013-01-22T18:21:40-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C26 H27 N3 O2 Pt S' _chemical_formula_sum 'C26 H27 N3 O2 Pt S' _chemical_formula_weight 640.66 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.5741(3) _cell_length_b 8.17290(10) _cell_length_c 19.7272(3) _cell_angle_alpha 90 _cell_angle_beta 109.1100(10) _cell_angle_gamma 90 _cell_volume 2372.61(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8167 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 27.46 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.794 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 6.031 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.406 _exptl_absorpt_correction_T_max 0.656 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_unetI/netI 0.0395 _diffrn_reflns_number 20808 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 5439 _reflns_number_gt 4683 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2 (Bruker, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2006)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2006)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0170P)^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_number_reflns 5439 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0306 _refine_ls_R_factor_gt 0.0235 _refine_ls_wR_factor_ref 0.0494 _refine_ls_wR_factor_gt 0.0471 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.605 _refine_diff_density_min -0.56 _refine_diff_density_rms 0.109 _iucr_refine_instructions_details ; .res file for SHELXL : job.res ................................................................. TITL import in P 21/n CELL 0.71073 15.5741 8.1729 19.7272 90.000 109.110 90.000 ZERR 4.00 0.0003 0.0001 0.0003 0.000 0.001 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O S PT UNIT 104 108 12 8 4 4 MERG 2 FMAP 2 PLAN 20 ACTA BOND $H CONF LIST 4 WPDB -2 L.S. 4 TEMP -123.00 WGHT 0.017000 FVAR 0.26868 PT1 6 0.366623 0.432737 0.555791 11.00000 0.02355 0.01717 = 0.01593 -0.00202 0.01025 -0.00048 S1 5 0.242336 0.551150 0.568131 11.00000 0.02582 0.03014 = 0.01905 -0.00401 0.01029 0.00345 N1 3 0.471210 0.312622 0.536971 11.00000 0.02439 0.01759 = 0.02225 -0.00210 0.01299 -0.00150 C2 1 0.547098 0.265696 0.588507 11.00000 0.02816 0.03046 = 0.02018 -0.00088 0.01020 0.00281 AFIX 43 H2 2 0.555780 0.296152 0.636772 11.00000 -1.20000 AFIX 0 C3 1 0.612872 0.174508 0.573430 11.00000 0.02594 0.03730 = 0.02629 0.00178 0.00983 0.00318 AFIX 43 H3 2 0.666212 0.142795 0.610949 11.00000 -1.20000 AFIX 0 C4 1 0.601002 0.129377 0.503611 11.00000 0.02472 0.03286 = 0.03422 -0.00357 0.01824 -0.00038 AFIX 43 H4 2 0.645469 0.065110 0.492525 11.00000 -1.20000 AFIX 0 C5 1 0.523158 0.179315 0.449914 11.00000 0.03004 0.03023 = 0.02508 -0.00660 0.01744 -0.00595 AFIX 43 H5 2 0.514235 0.150959 0.401383 11.00000 -1.20000 AFIX 0 C6 1 0.458045 0.271165 0.467269 11.00000 0.02472 0.02133 = 0.02194 -0.00093 0.01398 -0.00531 C7 1 0.370696 0.327605 0.417912 11.00000 0.02499 0.02018 = 0.02032 0.00068 0.01098 -0.00158 C8 1 0.313922 0.405629 0.450486 11.00000 0.02759 0.01518 = 0.01914 -0.00162 0.01197 -0.00332 C9 1 0.228937 0.458530 0.404451 11.00000 0.03058 0.02512 = 0.02139 0.00142 0.01325 0.00236 AFIX 43 H9 2 0.188557 0.512543 0.424197 11.00000 -1.20000 AFIX 0 C10 1 0.202415 0.433640 0.330422 11.00000 0.03450 0.02105 = 0.02070 0.00337 0.01096 -0.00179 C11 1 0.260816 0.357525 0.299981 11.00000 0.03814 0.03827 = 0.01598 -0.00236 0.00941 -0.00314 AFIX 43 H11 2 0.242990 0.341929 0.249542 11.00000 -1.20000 AFIX 0 C12 1 0.344896 0.304823 0.343656 11.00000 0.03600 0.03650 = 0.02196 -0.00504 0.01470 0.00108 AFIX 43 H12 2 0.385300 0.253018 0.323276 11.00000 -1.20000 AFIX 0 C13 1 0.111110 0.487790 0.285821 11.00000 0.03747 0.03012 = 0.02370 0.00123 0.00910 0.00197 AFIX 43 H13 2 0.075405 0.543912 0.309290 11.00000 -1.20000 AFIX 0 O14 4 0.077897 0.466763 0.221925 11.00000 0.04673 0.04942 = 0.02179 0.00098 0.00229 0.00498 O21 4 0.440795 0.454696 0.664260 11.00000 0.02582 0.03043 = 0.01637 -0.00608 0.00697 0.00509 C22 1 0.420048 0.531472 0.712594 11.00000 0.02883 0.01358 = 0.01660 -0.00117 0.00965 -0.00525 C23 1 0.496430 0.561091 0.780736 11.00000 0.02721 0.01768 = 0.01854 -0.00062 0.01215 -0.00450 C24 1 0.579641 0.482598 0.793139 11.00000 0.03018 0.02595 = 0.02639 -0.00580 0.01309 -0.00562 AFIX 43 H24 2 0.587752 0.411455 0.757636 11.00000 -1.20000 AFIX 0 C25 1 0.650637 0.506791 0.856433 11.00000 0.02699 0.03577 = 0.02943 -0.00481 0.00666 -0.00396 AFIX 43 H25 2 0.706613 0.450907 0.864618 11.00000 -1.20000 AFIX 0 C26 1 0.639697 0.612901 0.907811 11.00000 0.03332 0.03225 = 0.02447 -0.00329 0.00383 -0.00785 AFIX 43 H26 2 0.688613 0.631203 0.950952 11.00000 -1.20000 AFIX 0 C27 1 0.558144 0.691752 0.896448 11.00000 0.04102 0.02646 = 0.02258 -0.00722 0.01229 -0.00553 AFIX 43 H27 2 0.551089 0.764714 0.931742 11.00000 -1.20000 AFIX 0 C28 1 0.486094 0.665396 0.833746 11.00000 0.03464 0.02122 = 0.02212 -0.00335 0.01239 -0.00061 AFIX 43 H28 2 0.429566 0.718387 0.826812 11.00000 -1.20000 AFIX 0 N29 3 0.340321 0.583779 0.713542 11.00000 0.02452 0.01796 = 0.01846 -0.00416 0.00971 -0.00308 C30 1 0.260381 0.579923 0.659378 11.00000 0.02915 0.01173 = 0.02575 -0.00260 0.01590 -0.00192 N31 3 0.187362 0.610741 0.678824 11.00000 0.02400 0.01932 = 0.02064 -0.00120 0.01189 0.00015 C32 1 0.195607 0.651637 0.753340 11.00000 0.03281 0.01778 = 0.02365 -0.00159 0.01742 0.00064 AFIX 23 H32A 2 0.142923 0.719339 0.753404 11.00000 -1.20000 H32B 2 0.251283 0.717505 0.774720 11.00000 -1.20000 AFIX 0 C33 1 0.199814 0.500007 0.799465 11.00000 0.05774 0.01698 = 0.03507 0.00225 0.03191 0.00428 AFIX 23 H33A 2 0.144574 0.433200 0.777812 11.00000 -1.20000 H33B 2 0.253091 0.433109 0.800166 11.00000 -1.20000 AFIX 0 C34 1 0.206795 0.543561 0.875193 11.00000 0.10886 0.03133 = 0.04534 0.01539 0.05530 0.02388 AFIX 137 H34A 2 0.260968 0.610958 0.896618 11.00000 -1.50000 H34B 2 0.211361 0.443231 0.903364 11.00000 -1.50000 H34C 2 0.152602 0.604860 0.874920 11.00000 -1.50000 AFIX 0 C35 1 0.094805 0.606138 0.628327 11.00000 0.02646 0.02400 = 0.03093 -0.00736 0.01540 -0.00323 AFIX 23 H35A 2 0.053105 0.572738 0.654418 11.00000 -1.20000 H35B 2 0.091452 0.521804 0.591523 11.00000 -1.20000 AFIX 0 C36 1 0.062123 0.769056 0.590739 11.00000 0.03040 0.02680 = 0.02782 -0.00753 0.01095 0.00120 AFIX 23 H36A 2 0.067881 0.855471 0.627131 11.00000 -1.20000 H36B 2 0.100839 0.799884 0.561742 11.00000 -1.20000 AFIX 0 C37 1 -0.036510 0.757384 0.542277 11.00000 0.02971 0.05188 = 0.04048 -0.00818 0.01350 0.00597 AFIX 137 H37A 2 -0.043003 0.666991 0.508320 11.00000 -1.50000 H37B 2 -0.054402 0.860099 0.515769 11.00000 -1.50000 H37C 2 -0.075570 0.737556 0.571569 11.00000 -1.50000 HKLF 4 REM import in P 21/n REM R1 = 0.0235 for 4683 Fo > 4sig(Fo) and 0.0306 for all 5439 data REM 300 parameters refined using 0 restraints END WGHT 0.0169 0.0000 REM Highest difference peak 0.61, deepest hole -0.56, 1-sigma level 0.11 Q1 1 0.3564 0.3187 0.5438 11.00000 0.05 0.61 Q2 1 0.3552 0.5431 0.5464 11.00000 0.05 0.53 Q3 1 0.4431 0.3653 0.5607 11.00000 0.05 0.51 Q4 1 0.2963 0.5008 0.5536 11.00000 0.05 0.50 Q5 1 0.3754 0.3183 0.5676 11.00000 0.05 0.50 Q6 1 0.0810 0.6964 0.6218 11.00000 0.05 0.49 Q7 1 0.4236 0.4064 0.6091 11.00000 0.05 0.48 Q8 1 0.4315 0.4288 0.5320 11.00000 0.05 0.47 Q9 1 0.2649 0.4394 0.5714 11.00000 0.05 0.45 Q10 1 0.4469 0.5558 0.7486 11.00000 0.05 0.45 Q11 1 0.4153 0.3218 0.4391 11.00000 0.05 0.44 Q12 1 0.3355 0.3270 0.4360 11.00000 0.05 0.43 Q13 1 0.3182 0.4841 0.7714 11.00000 0.05 0.42 Q14 1 0.4033 0.2889 0.4378 11.00000 0.05 0.42 Q15 1 0.6756 -0.0200 0.4885 11.00000 0.05 0.42 Q16 1 0.2984 0.4195 0.5876 11.00000 0.05 0.41 Q17 1 0.2603 0.2738 0.5297 11.00000 0.05 0.41 Q18 1 0.4401 0.3564 0.4437 11.00000 0.05 0.40 Q19 1 0.3136 0.5802 0.6824 11.00000 0.05 0.40 Q20 1 0.2977 0.3992 0.5487 11.00000 0.05 0.40 ; #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' 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 Pt1 Pt 0.366623(8) 0.432737(13) 0.555791(6) 0.01796(4) Uani 1 1 d . . . S1 S 0.24234(6) 0.55115(9) 0.56813(4) 0.02428(17) Uani 1 1 d . . . N1 N 0.47121(16) 0.3126(3) 0.53697(12) 0.0201(5) Uani 1 1 d . . . C2 C 0.5471(2) 0.2657(4) 0.58851(16) 0.0257(7) Uani 1 1 d . . . H2 H 0.5558 0.2962 0.6368 0.031 Uiso 1 1 calc R . . C3 C 0.6129(2) 0.1745(4) 0.57343(16) 0.0295(7) Uani 1 1 d . . . H3 H 0.6662 0.1428 0.6109 0.035 Uiso 1 1 calc R . . C4 C 0.6010(2) 0.1294(4) 0.50361(17) 0.0285(7) Uani 1 1 d . . . H4 H 0.6455 0.0651 0.4925 0.034 Uiso 1 1 calc R . . C5 C 0.5232(2) 0.1793(4) 0.44991(16) 0.0264(7) Uani 1 1 d . . . H5 H 0.5142 0.151 0.4014 0.032 Uiso 1 1 calc R . . C6 C 0.4580(2) 0.2712(3) 0.46727(15) 0.0211(7) Uani 1 1 d . . . C7 C 0.3707(2) 0.3276(3) 0.41791(15) 0.0210(6) Uani 1 1 d . . . C8 C 0.3139(2) 0.4056(3) 0.45049(15) 0.0196(6) Uani 1 1 d . . . C9 C 0.2289(2) 0.4585(3) 0.40445(16) 0.0245(7) Uani 1 1 d . . . H9 H 0.1886 0.5125 0.4242 0.029 Uiso 1 1 calc R . . C10 C 0.2024(2) 0.4336(3) 0.33042(16) 0.0249(7) Uani 1 1 d . . . C11 C 0.2608(2) 0.3575(4) 0.29998(16) 0.0307(8) Uani 1 1 d . . . H11 H 0.243 0.3419 0.2495 0.037 Uiso 1 1 calc R . . C12 C 0.3449(2) 0.3048(4) 0.34366(15) 0.0302(7) Uani 1 1 d . . . H12 H 0.3853 0.253 0.3233 0.036 Uiso 1 1 calc R . . C13 C 0.1111(2) 0.4878(4) 0.28582(17) 0.0307(8) Uani 1 1 d . . . H13 H 0.0754 0.5439 0.3093 0.037 Uiso 1 1 calc R . . O14 O 0.07790(17) 0.4668(3) 0.22193(12) 0.0415(6) Uani 1 1 d . . . O21 O 0.44079(15) 0.4547(2) 0.66426(11) 0.0242(5) Uani 1 1 d . . . C22 C 0.4200(2) 0.5315(3) 0.71259(15) 0.0191(6) Uani 1 1 d . . . C23 C 0.4964(2) 0.5611(3) 0.78074(15) 0.0200(6) Uani 1 1 d . . . C24 C 0.5796(2) 0.4826(4) 0.79314(17) 0.0266(7) Uani 1 1 d . . . H24 H 0.5878 0.4115 0.7576 0.032 Uiso 1 1 calc R . . C25 C 0.6506(2) 0.5068(4) 0.85643(17) 0.0314(8) Uani 1 1 d . . . H25 H 0.7066 0.4509 0.8646 0.038 Uiso 1 1 calc R . . C26 C 0.6397(2) 0.6129(4) 0.90781(17) 0.0314(8) Uani 1 1 d . . . H26 H 0.6886 0.6312 0.951 0.038 Uiso 1 1 calc R . . C27 C 0.5581(2) 0.6918(4) 0.89645(16) 0.0296(7) Uani 1 1 d . . . H27 H 0.5511 0.7647 0.9317 0.035 Uiso 1 1 calc R . . C28 C 0.4861(2) 0.6654(3) 0.83375(15) 0.0252(7) Uani 1 1 d . . . H28 H 0.4296 0.7184 0.8268 0.03 Uiso 1 1 calc R . . N29 N 0.34032(17) 0.5838(3) 0.71354(13) 0.0197(5) Uani 1 1 d . . . C30 C 0.2604(2) 0.5799(3) 0.65938(16) 0.0205(7) Uani 1 1 d . . . N31 N 0.18736(17) 0.6107(3) 0.67882(13) 0.0202(5) Uani 1 1 d . . . C32 C 0.1956(2) 0.6516(3) 0.75334(14) 0.0227(7) Uani 1 1 d . . . H32A H 0.1429 0.7193 0.7534 0.027 Uiso 1 1 calc R . . H32B H 0.2513 0.7175 0.7747 0.027 Uiso 1 1 calc R . . C33 C 0.1998(3) 0.5000(4) 0.79946(17) 0.0325(8) Uani 1 1 d . . . H33A H 0.1446 0.4332 0.7778 0.039 Uiso 1 1 calc R . . H33B H 0.2531 0.4331 0.8002 0.039 Uiso 1 1 calc R . . C34 C 0.2068(3) 0.5436(4) 0.8752(2) 0.0545(13) Uani 1 1 d . . . H34A H 0.261 0.611 0.8966 0.082 Uiso 1 1 calc R . . H34B H 0.2114 0.4432 0.9034 0.082 Uiso 1 1 calc R . . H34C H 0.1526 0.6049 0.8749 0.082 Uiso 1 1 calc R . . C35 C 0.0948(2) 0.6061(3) 0.62833(17) 0.0257(7) Uani 1 1 d . . . H35A H 0.0531 0.5727 0.6544 0.031 Uiso 1 1 calc R . . H35B H 0.0915 0.5218 0.5915 0.031 Uiso 1 1 calc R . . C36 C 0.0621(2) 0.7691(4) 0.59074(16) 0.0280(7) Uani 1 1 d . . . H36A H 0.0679 0.8555 0.6271 0.034 Uiso 1 1 calc R . . H36B H 0.1008 0.7999 0.5617 0.034 Uiso 1 1 calc R . . C37 C -0.0365(2) 0.7574(4) 0.54228(18) 0.0402(9) Uani 1 1 d . . . H37A H -0.043 0.667 0.5083 0.06 Uiso 1 1 calc R . . H37B H -0.0544 0.8601 0.5158 0.06 Uiso 1 1 calc R . . H37C H -0.0756 0.7376 0.5716 0.06 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02355(7) 0.01717(7) 0.01593(7) -0.00202(5) 0.01025(5) -0.00048(5) S1 0.0258(4) 0.0301(4) 0.0190(4) -0.0040(3) 0.0103(3) 0.0035(3) N1 0.0244(14) 0.0176(12) 0.0222(13) -0.0021(11) 0.0130(11) -0.0015(11) C2 0.0282(18) 0.0305(17) 0.0202(15) -0.0009(14) 0.0102(14) 0.0028(14) C3 0.0259(18) 0.0373(19) 0.0263(17) 0.0018(15) 0.0098(14) 0.0032(15) C4 0.0247(18) 0.0329(17) 0.0342(18) -0.0036(16) 0.0182(15) -0.0004(14) C5 0.0300(18) 0.0302(17) 0.0251(16) -0.0066(14) 0.0174(15) -0.0059(14) C6 0.0247(17) 0.0213(15) 0.0219(15) -0.0009(13) 0.0140(13) -0.0053(13) C7 0.0250(17) 0.0202(15) 0.0203(15) 0.0007(13) 0.0110(13) -0.0016(13) C8 0.0276(17) 0.0152(14) 0.0191(15) -0.0016(12) 0.0120(13) -0.0033(12) C9 0.0306(19) 0.0251(16) 0.0214(16) 0.0014(13) 0.0132(14) 0.0024(13) C10 0.0345(19) 0.0210(16) 0.0207(16) 0.0034(13) 0.0110(14) -0.0018(14) C11 0.038(2) 0.0383(19) 0.0160(15) -0.0024(15) 0.0094(15) -0.0031(16) C12 0.036(2) 0.0365(18) 0.0220(16) -0.0050(15) 0.0147(15) 0.0011(16) C13 0.037(2) 0.0301(17) 0.0237(18) 0.0012(15) 0.0091(16) 0.0020(15) O14 0.0467(17) 0.0494(15) 0.0218(13) 0.0010(12) 0.0023(12) 0.0050(12) O21 0.0258(12) 0.0304(12) 0.0164(11) -0.0061(9) 0.0070(9) 0.0051(9) C22 0.0288(18) 0.0136(13) 0.0166(15) -0.0012(12) 0.0096(13) -0.0052(12) C23 0.0272(17) 0.0177(14) 0.0185(15) -0.0006(12) 0.0121(13) -0.0045(13) C24 0.0302(19) 0.0260(16) 0.0264(18) -0.0058(14) 0.0131(15) -0.0056(14) C25 0.0270(19) 0.0358(18) 0.0294(19) -0.0048(16) 0.0067(15) -0.0040(15) C26 0.033(2) 0.0323(18) 0.0245(18) -0.0033(15) 0.0038(15) -0.0079(15) C27 0.041(2) 0.0265(17) 0.0226(16) -0.0072(14) 0.0123(15) -0.0055(15) C28 0.0346(19) 0.0212(16) 0.0221(16) -0.0034(13) 0.0124(14) -0.0006(14) N29 0.0245(14) 0.0180(12) 0.0185(13) -0.0042(10) 0.0097(11) -0.0031(10) C30 0.0292(18) 0.0117(14) 0.0258(16) -0.0026(12) 0.0159(14) -0.0019(12) N31 0.0240(14) 0.0193(12) 0.0206(13) -0.0012(11) 0.0119(11) 0.0001(10) C32 0.0328(18) 0.0178(15) 0.0237(16) -0.0016(13) 0.0174(14) 0.0006(13) C33 0.058(3) 0.0170(15) 0.0351(19) 0.0023(15) 0.0319(18) 0.0043(16) C34 0.109(4) 0.031(2) 0.045(2) 0.0154(17) 0.055(3) 0.024(2) C35 0.0265(18) 0.0240(16) 0.0309(18) -0.0074(14) 0.0154(15) -0.0032(13) C36 0.0304(19) 0.0268(17) 0.0278(17) -0.0075(14) 0.0109(15) 0.0012(14) C37 0.030(2) 0.052(2) 0.040(2) -0.0082(18) 0.0135(17) 0.0060(17) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C8 1.980(3) . ? Pt1 N1 2.037(2) . ? Pt1 O21 2.080(2) . ? Pt1 S1 2.2475(8) . ? S1 C30 1.744(3) . ? N1 C2 1.338(4) . ? N1 C6 1.365(3) . ? C2 C3 1.376(4) . ? C2 H2 0.95 . ? C3 C4 1.379(4) . ? C3 H3 0.95 . ? C4 C5 1.385(4) . ? C4 H4 0.95 . ? C5 C6 1.392(4) . ? C5 H5 0.95 . ? C6 C7 1.464(4) . ? C7 C12 1.399(4) . ? C7 C8 1.405(4) . ? C8 C9 1.406(4) . ? C9 C10 1.396(4) . ? C9 H9 0.95 . ? C10 C11 1.390(4) . ? C10 C13 1.474(4) . ? C11 C12 1.380(4) . ? C11 H11 0.95 . ? C12 H12 0.95 . ? C13 O14 1.208(4) . ? C13 H13 0.95 . ? O21 C22 1.268(3) . ? C22 N29 1.319(4) . ? C22 C23 1.495(4) . ? C23 C24 1.394(4) . ? C23 C28 1.399(4) . ? C24 C25 1.384(4) . ? C24 H24 0.95 . ? C25 C26 1.386(5) . ? C25 H25 0.95 . ? C26 C27 1.376(4) . ? C26 H26 0.95 . ? C27 C28 1.388(4) . ? C27 H27 0.95 . ? C28 H28 0.95 . ? N29 C30 1.350(4) . ? C30 N31 1.338(4) . ? N31 C35 1.460(4) . ? N31 C32 1.472(3) . ? C32 C33 1.526(4) . ? C32 H32A 0.99 . ? C32 H32B 0.99 . ? C33 C34 1.505(4) . ? C33 H33A 0.99 . ? C33 H33B 0.99 . ? C34 H34A 0.98 . ? C34 H34B 0.98 . ? C34 H34C 0.98 . ? C35 C36 1.528(4) . ? C35 H35A 0.99 . ? C35 H35B 0.99 . ? C36 C37 1.524(4) . ? C36 H36A 0.99 . ? C36 H36B 0.99 . ? C37 H37A 0.98 . ? C37 H37B 0.98 . ? C37 H37C 0.98 . ? 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 C8 Pt1 N1 80.59(11) . . ? C8 Pt1 O21 171.34(10) . . ? N1 Pt1 O21 91.21(9) . . ? C8 Pt1 S1 94.93(9) . . ? N1 Pt1 S1 174.59(7) . . ? O21 Pt1 S1 93.40(6) . . ? C30 S1 Pt1 108.44(11) . . ? C2 N1 C6 119.9(3) . . ? C2 N1 Pt1 124.03(19) . . ? C6 N1 Pt1 115.97(19) . . ? N1 C2 C3 121.7(3) . . ? N1 C2 H2 119.1 . . ? C3 C2 H2 119.1 . . ? C2 C3 C4 119.7(3) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C3 C4 C5 118.9(3) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C4 C5 C6 119.8(3) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? N1 C6 C5 120.0(3) . . ? N1 C6 C7 113.1(3) . . ? C5 C6 C7 126.8(3) . . ? C12 C7 C8 122.1(3) . . ? C12 C7 C6 122.7(3) . . ? C8 C7 C6 115.2(3) . . ? C7 C8 C9 116.4(3) . . ? C7 C8 Pt1 115.1(2) . . ? C9 C8 Pt1 128.5(2) . . ? C10 C9 C8 121.6(3) . . ? C10 C9 H9 119.2 . . ? C8 C9 H9 119.2 . . ? C11 C10 C9 120.4(3) . . ? C11 C10 C13 121.1(3) . . ? C9 C10 C13 118.5(3) . . ? C12 C11 C10 119.4(3) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C11 C12 C7 120.1(3) . . ? C11 C12 H12 120 . . ? C7 C12 H12 120 . . ? O14 C13 C10 125.5(3) . . ? O14 C13 H13 117.3 . . ? C10 C13 H13 117.3 . . ? C22 O21 Pt1 128.6(2) . . ? O21 C22 N29 130.1(3) . . ? O21 C22 C23 115.6(3) . . ? N29 C22 C23 114.2(3) . . ? C24 C23 C28 118.5(3) . . ? C24 C23 C22 120.3(3) . . ? C28 C23 C22 121.2(3) . . ? C25 C24 C23 121.0(3) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C24 C25 C26 119.7(3) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C27 C26 C25 120.1(3) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C26 C27 C28 120.4(3) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C27 C28 C23 120.2(3) . . ? C27 C28 H28 119.9 . . ? C23 C28 H28 119.9 . . ? C22 N29 C30 127.6(3) . . ? N31 C30 N29 114.8(3) . . ? N31 C30 S1 117.2(2) . . ? N29 C30 S1 128.0(2) . . ? C30 N31 C35 122.8(3) . . ? C30 N31 C32 121.7(3) . . ? C35 N31 C32 115.5(2) . . ? N31 C32 C33 112.6(2) . . ? N31 C32 H32A 109.1 . . ? C33 C32 H32A 109.1 . . ? N31 C32 H32B 109.1 . . ? C33 C32 H32B 109.1 . . ? H32A C32 H32B 107.8 . . ? C34 C33 C32 112.0(3) . . ? C34 C33 H33A 109.2 . . ? C32 C33 H33A 109.2 . . ? C34 C33 H33B 109.2 . . ? C32 C33 H33B 109.2 . . ? H33A C33 H33B 107.9 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N31 C35 C36 114.0(2) . . ? N31 C35 H35A 108.8 . . ? C36 C35 H35A 108.8 . . ? N31 C35 H35B 108.8 . . ? C36 C35 H35B 108.8 . . ? H35A C35 H35B 107.7 . . ? C37 C36 C35 110.9(3) . . ? C37 C36 H36A 109.5 . . ? C35 C36 H36A 109.5 . . ? C37 C36 H36B 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 108 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C8 Pt1 S1 C30 175.13(12) . . . . ? O21 Pt1 S1 C30 -7.22(11) . . . . ? C8 Pt1 N1 C2 -176.5(2) . . . . ? O21 Pt1 N1 C2 6.3(2) . . . . ? C8 Pt1 N1 C6 -0.5(2) . . . . ? O21 Pt1 N1 C6 -177.7(2) . . . . ? C6 N1 C2 C3 -0.6(4) . . . . ? Pt1 N1 C2 C3 175.2(2) . . . . ? N1 C2 C3 C4 -0.1(5) . . . . ? C2 C3 C4 C5 0.9(5) . . . . ? C3 C4 C5 C6 -1.0(5) . . . . ? C2 N1 C6 C5 0.4(4) . . . . ? Pt1 N1 C6 C5 -175.7(2) . . . . ? C2 N1 C6 C7 178.3(2) . . . . ? Pt1 N1 C6 C7 2.2(3) . . . . ? C4 C5 C6 N1 0.4(4) . . . . ? C4 C5 C6 C7 -177.2(3) . . . . ? N1 C6 C7 C12 177.1(3) . . . . ? C5 C6 C7 C12 -5.2(5) . . . . ? N1 C6 C7 C8 -3.3(4) . . . . ? C5 C6 C7 C8 174.4(3) . . . . ? C12 C7 C8 C9 0.6(4) . . . . ? C6 C7 C8 C9 -178.9(2) . . . . ? C12 C7 C8 Pt1 -177.5(2) . . . . ? C6 C7 C8 Pt1 3.0(3) . . . . ? N1 Pt1 C8 C7 -1.4(2) . . . . ? S1 Pt1 C8 C7 -178.3(2) . . . . ? N1 Pt1 C8 C9 -179.2(3) . . . . ? S1 Pt1 C8 C9 3.8(3) . . . . ? C7 C8 C9 C10 0.4(4) . . . . ? Pt1 C8 C9 C10 178.2(2) . . . . ? C8 C9 C10 C11 -1.1(5) . . . . ? C8 C9 C10 C13 178.1(3) . . . . ? C9 C10 C11 C12 0.8(5) . . . . ? C13 C10 C11 C12 -178.4(3) . . . . ? C10 C11 C12 C7 0.2(5) . . . . ? C8 C7 C12 C11 -0.9(5) . . . . ? C6 C7 C12 C11 178.6(3) . . . . ? C11 C10 C13 O14 3.0(5) . . . . ? C9 C10 C13 O14 -176.2(3) . . . . ? N1 Pt1 O21 C22 174.3(2) . . . . ? S1 Pt1 O21 C22 -8.5(2) . . . . ? Pt1 O21 C22 N29 18.6(4) . . . . ? Pt1 O21 C22 C23 -164.72(18) . . . . ? O21 C22 C23 C24 -11.0(4) . . . . ? N29 C22 C23 C24 166.3(3) . . . . ? O21 C22 C23 C28 170.0(3) . . . . ? N29 C22 C23 C28 -12.8(4) . . . . ? C28 C23 C24 C25 0.1(5) . . . . ? C22 C23 C24 C25 -179.0(3) . . . . ? C23 C24 C25 C26 -1.2(5) . . . . ? C24 C25 C26 C27 1.1(5) . . . . ? C25 C26 C27 C28 0.3(5) . . . . ? C26 C27 C28 C23 -1.5(5) . . . . ? C24 C23 C28 C27 1.3(4) . . . . ? C22 C23 C28 C27 -179.7(3) . . . . ? O21 C22 N29 C30 -6.1(5) . . . . ? C23 C22 N29 C30 177.1(2) . . . . ? C22 N29 C30 N31 167.3(3) . . . . ? C22 N29 C30 S1 -16.5(4) . . . . ? Pt1 S1 C30 N31 -163.89(18) . . . . ? Pt1 S1 C30 N29 20.0(3) . . . . ? N29 C30 N31 C35 -177.7(2) . . . . ? S1 C30 N31 C35 5.7(3) . . . . ? N29 C30 N31 C32 2.2(4) . . . . ? S1 C30 N31 C32 -174.38(19) . . . . ? C30 N31 C32 C33 -85.8(3) . . . . ? C35 N31 C32 C33 94.2(3) . . . . ? N31 C32 C33 C34 -179.1(3) . . . . ? C30 N31 C35 C36 -88.8(3) . . . . ? C32 N31 C35 C36 91.2(3) . . . . ? N31 C35 C36 C37 -176.8(3) . . . . ? _database_code_depnum_ccdc_archive 'CCDC 948666' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_job _audit_creation_date 2011-04-26T10:20:03-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C28 H36 Cl2 N2 O2 Pt S, C H2 Cl2' _chemical_formula_sum 'C29 H38 Cl4 N2 O2 Pt S' _chemical_formula_weight 815.56 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.4355(9) _cell_length_b 8.2355(10) _cell_length_c 26.969(3) _cell_angle_alpha 94.842(5) _cell_angle_beta 92.304(5) _cell_angle_gamma 104.881(5) _cell_volume 1587.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6659 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 27.15 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.707 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.852 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.751 _exptl_absorpt_correction_T_max 0.908 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0499 _diffrn_reflns_av_unetI/netI 0.0675 _diffrn_reflns_number 21012 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.978 _diffrn_measured_fraction_theta_max 0.97 _reflns_number_total 7079 _reflns_number_gt 6006 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2 (Bruker, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2006)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2006)' _computing_structure_solution 'SIR97 (Altomare et al., 1999))' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0000P)^2^+6.1116P] 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_number_reflns 7079 _refine_ls_number_parameters 355 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0554 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.0726 _refine_ls_wR_factor_gt 0.0688 _refine_ls_goodness_of_fit_ref 1.04 _refine_ls_restrained_S_all 1.04 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.299 _refine_diff_density_min -1.976 _refine_diff_density_rms 0.167 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Pt1 Pt 0.40924(3) 0.34676(3) 0.382879(8) 0.01418(6) Uani 1 1 d . . . Cl1 Cl 0.20885(18) 0.44994(17) 0.43187(5) 0.0224(3) Uani 1 1 d . . . Cl2 Cl 0.60691(18) 0.25079(16) 0.33127(5) 0.0221(3) Uani 1 1 d . . . O1 O 0.4446(5) 0.0093(4) 0.42604(14) 0.0257(9) Uani 1 1 d . . . S1 S 0.48588(18) 0.19267(16) 0.43973(5) 0.0167(3) Uani 1 1 d . . . C2 C 0.7281(7) 0.2706(7) 0.4556(2) 0.0260(13) Uani 1 1 d . . . H2A H 0.764 0.2097 0.4824 0.039 Uiso 1 1 calc R . . H2B H 0.7567 0.3913 0.4669 0.039 Uiso 1 1 calc R . . H2C H 0.7976 0.254 0.4263 0.039 Uiso 1 1 calc R . . C3 C 0.3923(8) 0.2242(7) 0.49818(19) 0.0233(12) Uani 1 1 d . . . H3A H 0.2559 0.1859 0.4944 0.035 Uiso 1 1 calc R . . H3B H 0.4303 0.3445 0.5101 0.035 Uiso 1 1 calc R . . H3C H 0.439 0.1597 0.5223 0.035 Uiso 1 1 calc R . . N4 N 0.3688(6) 0.5054(5) 0.32996(16) 0.0171(9) Uani 1 1 d . . . C5 C 0.4445(7) 0.6708(7) 0.3437(2) 0.0216(12) Uani 1 1 d . . . H5 H 0.4913 0.7052 0.3773 0.026 Uiso 1 1 calc R . . C6 C 0.4567(7) 0.7927(7) 0.3105(2) 0.0244(12) Uani 1 1 d . . . H6 H 0.5077 0.9088 0.3215 0.029 Uiso 1 1 calc R . . C7 C 0.3935(7) 0.7424(7) 0.2614(2) 0.0250(13) Uani 1 1 d . . . H7 H 0.405 0.8227 0.2376 0.03 Uiso 1 1 calc R . . C8 C 0.3131(7) 0.5726(6) 0.2474(2) 0.0207(12) Uani 1 1 d . . . H8 H 0.2675 0.5365 0.2138 0.025 Uiso 1 1 calc R . . C9 C 0.2980(7) 0.4533(6) 0.28230(19) 0.0176(11) Uani 1 1 d . . . C10 C 0.2011(7) 0.2728(6) 0.26715(19) 0.0170(11) Uani 1 1 d . . . C11 C 0.0657(7) 0.1838(6) 0.2955(2) 0.0187(11) Uani 1 1 d . . . H11 H 0.0383 0.2359 0.3261 0.022 Uiso 1 1 calc R . . C12 C -0.0304(7) 0.0179(7) 0.27942(19) 0.0207(12) Uani 1 1 d . . . H12 H -0.125 -0.0414 0.2988 0.025 Uiso 1 1 calc R . . C13 C 0.0100(7) -0.0625(6) 0.23527(19) 0.0194(11) Uani 1 1 d . . . C14 C 0.1450(7) 0.0300(7) 0.20635(19) 0.0207(12) Uani 1 1 d . . . H14 H 0.1729 -0.0217 0.1758 0.025 Uiso 1 1 calc R . . C15 C 0.2375(7) 0.1955(7) 0.22185(19) 0.0211(12) Uani 1 1 d . . . H15 H 0.3267 0.2575 0.2016 0.025 Uiso 1 1 calc R . . C16 C -0.0861(7) -0.2402(7) 0.2210(2) 0.0226(12) Uani 1 1 d . . . H16 H -0.1903 -0.291 0.2388 0.027 Uiso 1 1 calc R . . N17 N -0.0366(6) -0.3306(5) 0.18572(16) 0.0223(10) Uani 1 1 d . . . C18 C -0.1266(7) -0.5071(7) 0.1792(2) 0.0207(12) Uani 1 1 d . . . C19 C -0.1188(8) -0.5955(7) 0.1329(2) 0.0241(12) Uani 1 1 d . . . H19 H -0.0562 -0.536 0.1073 0.029 Uiso 1 1 calc R . . C20 C -0.2004(7) -0.7692(7) 0.1235(2) 0.0247(13) Uani 1 1 d . . . H20 H -0.1964 -0.8265 0.0916 0.03 Uiso 1 1 calc R . . C21 C -0.2874(7) -0.8558(7) 0.1616(2) 0.0209(12) Uani 1 1 d . . . C22 C -0.2927(8) -0.7694(7) 0.2078(2) 0.0236(12) Uani 1 1 d . . . H22 H -0.3527 -0.8295 0.2338 0.028 Uiso 1 1 calc R . . C23 C -0.2130(8) -0.5994(7) 0.2168(2) 0.0254(13) Uani 1 1 d . . . H23 H -0.2165 -0.5436 0.2489 0.03 Uiso 1 1 calc R . . O24 O -0.3771(5) -1.0259(5) 0.15819(14) 0.0266(9) Uani 1 1 d . . . C25 C -0.3651(8) -1.1323(7) 0.1146(2) 0.0257(13) Uani 1 1 d . . . H25A H -0.2342 -1.1346 0.1102 0.031 Uiso 1 1 calc R . . H25B H -0.4136 -1.0918 0.0846 0.031 Uiso 1 1 calc R . . C26 C -0.4831(8) -1.3056(6) 0.1228(2) 0.0242(12) Uani 1 1 d . . . H26A H -0.6101 -1.297 0.1298 0.029 Uiso 1 1 calc R . . H26B H -0.4302 -1.3427 0.1528 0.029 Uiso 1 1 calc R . . C27 C -0.4983(8) -1.4409(7) 0.0795(2) 0.0253(13) Uani 1 1 d . . . H27A H -0.3717 -1.4466 0.0709 0.03 Uiso 1 1 calc R . . H27B H -0.5603 -1.4098 0.0499 0.03 Uiso 1 1 calc R . . C28 C -0.6093(8) -1.6142(7) 0.0924(2) 0.0237(12) Uani 1 1 d . . . H28A H -0.5436 -1.6456 0.1213 0.028 Uiso 1 1 calc R . . H28B H -0.7329 -1.6053 0.1028 0.028 Uiso 1 1 calc R . . C29 C -0.6382(8) -1.7550(7) 0.0501(2) 0.0264(13) Uani 1 1 d . . . H29A H -0.5149 -1.7641 0.0396 0.032 Uiso 1 1 calc R . . H29B H -0.7053 -1.7248 0.0213 0.032 Uiso 1 1 calc R . . C30 C -0.7478(8) -1.9264(7) 0.0643(2) 0.0257(13) Uani 1 1 d . . . H30A H -0.6784 -1.9583 0.0923 0.031 Uiso 1 1 calc R . . H30B H -0.8692 -1.9161 0.076 0.031 Uiso 1 1 calc R . . C31 C -0.7831(8) -2.0667(7) 0.0216(2) 0.0299(14) Uani 1 1 d . . . H31A H -0.6616 -2.0797 0.0106 0.036 Uiso 1 1 calc R . . H31B H -0.8483 -2.0328 -0.007 0.036 Uiso 1 1 calc R . . C32 C -0.8992(9) -2.2376(7) 0.0351(3) 0.0397(16) Uani 1 1 d . . . H32A H -0.8332 -2.2748 0.0624 0.06 Uiso 1 1 calc R . . H32B H -0.9182 -2.321 0.0059 0.06 Uiso 1 1 calc R . . H32C H -1.0203 -2.2264 0.0457 0.06 Uiso 1 1 calc R . . C101 C 0.0685(8) 0.8129(7) 0.3830(2) 0.0304(14) Uani 1 1 d . . . H10A H 0.1432 0.8766 0.358 0.037 Uiso 1 1 calc R . . H10B H 0.1549 0.7788 0.4064 0.037 Uiso 1 1 calc R . . Cl11 Cl -0.0910(2) 0.63043(19) 0.35260(7) 0.0430(4) Uani 1 1 d . . . Cl12 Cl -0.0500(3) 0.9442(2) 0.41615(7) 0.0505(5) 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 Pt1 0.01554(10) 0.00956(9) 0.01702(10) 0.00108(7) 0.00084(7) 0.00262(7) Cl1 0.0232(7) 0.0255(7) 0.0225(7) 0.0031(5) 0.0046(5) 0.0127(6) Cl2 0.0271(7) 0.0184(7) 0.0223(7) 0.0002(5) 0.0076(6) 0.0084(6) O1 0.035(2) 0.0136(19) 0.029(2) 0.0026(16) -0.0039(18) 0.0069(17) S1 0.0183(7) 0.0122(6) 0.0195(7) 0.0025(5) -0.0014(5) 0.0037(5) C2 0.018(3) 0.030(3) 0.030(3) -0.005(3) -0.007(2) 0.009(2) C3 0.028(3) 0.025(3) 0.018(3) 0.005(2) 0.002(2) 0.009(2) N4 0.017(2) 0.012(2) 0.023(2) 0.0022(18) 0.0019(19) 0.0038(18) C5 0.022(3) 0.017(3) 0.026(3) 0.003(2) 0.003(2) 0.005(2) C6 0.024(3) 0.014(3) 0.037(3) 0.006(2) 0.005(3) 0.006(2) C7 0.022(3) 0.021(3) 0.035(3) 0.013(2) 0.008(3) 0.007(2) C8 0.021(3) 0.019(3) 0.023(3) 0.005(2) -0.001(2) 0.006(2) C9 0.016(3) 0.020(3) 0.016(3) 0.004(2) 0.003(2) 0.003(2) C10 0.019(3) 0.016(3) 0.017(3) 0.006(2) 0.001(2) 0.005(2) C11 0.018(3) 0.016(3) 0.022(3) 0.005(2) 0.002(2) 0.004(2) C12 0.017(3) 0.022(3) 0.022(3) 0.006(2) 0.002(2) 0.002(2) C13 0.021(3) 0.017(3) 0.021(3) 0.004(2) -0.001(2) 0.006(2) C14 0.024(3) 0.019(3) 0.017(3) -0.001(2) 0.000(2) 0.003(2) C15 0.023(3) 0.018(3) 0.019(3) 0.003(2) 0.003(2) 0.000(2) C16 0.016(3) 0.023(3) 0.027(3) 0.003(2) -0.001(2) 0.002(2) N17 0.024(2) 0.018(2) 0.024(3) 0.0022(19) -0.001(2) 0.005(2) C18 0.020(3) 0.017(3) 0.025(3) 0.000(2) -0.001(2) 0.005(2) C19 0.028(3) 0.025(3) 0.023(3) 0.005(2) 0.006(2) 0.012(2) C20 0.023(3) 0.021(3) 0.030(3) -0.005(2) 0.004(2) 0.007(2) C21 0.023(3) 0.016(3) 0.024(3) 0.001(2) 0.005(2) 0.004(2) C22 0.027(3) 0.022(3) 0.022(3) 0.003(2) 0.005(2) 0.005(2) C23 0.034(3) 0.018(3) 0.021(3) -0.004(2) -0.001(2) 0.004(2) O24 0.036(2) 0.018(2) 0.024(2) -0.0006(16) 0.0086(18) 0.0022(17) C25 0.035(3) 0.021(3) 0.019(3) -0.005(2) 0.004(2) 0.006(3) C26 0.032(3) 0.017(3) 0.022(3) 0.000(2) 0.000(2) 0.005(2) C27 0.032(3) 0.019(3) 0.024(3) -0.005(2) 0.002(2) 0.008(2) C28 0.025(3) 0.021(3) 0.023(3) -0.001(2) 0.004(2) 0.004(2) C29 0.029(3) 0.023(3) 0.026(3) -0.002(2) 0.003(3) 0.006(3) C30 0.028(3) 0.022(3) 0.026(3) 0.001(2) 0.003(2) 0.006(2) C31 0.027(3) 0.022(3) 0.038(4) -0.005(3) 0.004(3) 0.004(3) C32 0.036(4) 0.023(3) 0.057(5) 0.001(3) 0.003(3) 0.003(3) C101 0.026(3) 0.027(3) 0.038(4) -0.002(3) 0.001(3) 0.009(3) Cl11 0.0389(9) 0.0256(8) 0.0593(11) -0.0048(7) -0.0207(8) 0.0055(7) Cl12 0.0518(11) 0.0440(11) 0.0579(12) -0.0053(8) 0.0234(9) 0.0166(9) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N4 2.078(4) . ? Pt1 S1 2.2170(13) . ? Pt1 Cl2 2.3016(13) . ? Pt1 Cl1 2.3037(13) . ? O1 S1 1.473(4) . ? S1 C2 1.771(5) . ? S1 C3 1.775(5) . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C3 H3C 0.98 . ? N4 C5 1.346(6) . ? N4 C9 1.360(6) . ? C5 C6 1.388(7) . ? C5 H5 0.95 . ? C6 C7 1.381(8) . ? C6 H6 0.95 . ? C7 C8 1.385(7) . ? C7 H7 0.95 . ? C8 C9 1.405(7) . ? C8 H8 0.95 . ? C9 C10 1.490(7) . ? C10 C11 1.383(7) . ? C10 C15 1.398(7) . ? C11 C12 1.393(7) . ? C11 H11 0.95 . ? C12 C13 1.394(7) . ? C12 H12 0.95 . ? C13 C14 1.402(7) . ? C13 C16 1.465(7) . ? C14 C15 1.380(7) . ? C14 H14 0.95 . ? C15 H15 0.95 . ? C16 N17 1.282(7) . ? C16 H16 0.95 . ? N17 C18 1.428(6) . ? C18 C23 1.396(7) . ? C18 C19 1.401(7) . ? C19 C20 1.400(7) . ? C19 H19 0.95 . ? C20 C21 1.386(7) . ? C20 H20 0.95 . ? C21 O24 1.382(6) . ? C21 C22 1.391(7) . ? C22 C23 1.369(7) . ? C22 H22 0.95 . ? C23 H23 0.95 . ? O24 C25 1.427(6) . ? C25 C26 1.511(7) . ? C25 H25A 0.99 . ? C25 H25B 0.99 . ? C26 C27 1.525(7) . ? C26 H26A 0.99 . ? C26 H26B 0.99 . ? C27 C28 1.530(7) . ? C27 H27A 0.99 . ? C27 H27B 0.99 . ? C28 C29 1.523(7) . ? C28 H28A 0.99 . ? C28 H28B 0.99 . ? C29 C30 1.525(7) . ? C29 H29A 0.99 . ? C29 H29B 0.99 . ? C30 C31 1.526(7) . ? C30 H30A 0.99 . ? C30 H30B 0.99 . ? C31 C32 1.533(8) . ? C31 H31A 0.99 . ? C31 H31B 0.99 . ? C32 H32A 0.98 . ? C32 H32B 0.98 . ? C32 H32C 0.98 . ? C101 Cl11 1.770(6) . ? C101 Cl12 1.771(6) . ? C101 H10A 0.99 . ? C101 H10B 0.99 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Pt1 S1 173.60(12) . . ? N4 Pt1 Cl2 89.01(12) . . ? S1 Pt1 Cl2 87.80(5) . . ? N4 Pt1 Cl1 88.49(12) . . ? S1 Pt1 Cl1 94.70(5) . . ? Cl2 Pt1 Cl1 177.50(5) . . ? O1 S1 C2 108.4(2) . . ? O1 S1 C3 107.6(2) . . ? C2 S1 C3 101.3(3) . . ? O1 S1 Pt1 116.95(16) . . ? C2 S1 Pt1 107.8(2) . . ? C3 S1 Pt1 113.49(19) . . ? S1 C2 H2A 109.5 . . ? S1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? S1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? S1 C3 H3A 109.5 . . ? S1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? S1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 N4 C9 119.9(4) . . ? C5 N4 Pt1 114.4(4) . . ? C9 N4 Pt1 125.0(3) . . ? N4 C5 C6 122.4(5) . . ? N4 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? C7 C6 C5 118.9(5) . . ? C7 C6 H6 120.6 . . ? C5 C6 H6 120.6 . . ? C6 C7 C8 118.7(5) . . ? C6 C7 H7 120.6 . . ? C8 C7 H7 120.6 . . ? C7 C8 C9 120.8(5) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? N4 C9 C8 119.2(5) . . ? N4 C9 C10 120.9(4) . . ? C8 C9 C10 119.9(5) . . ? C11 C10 C15 119.3(5) . . ? C11 C10 C9 120.9(5) . . ? C15 C10 C9 119.6(4) . . ? C10 C11 C12 120.1(5) . . ? C10 C11 H11 120 . . ? C12 C11 H11 120 . . ? C11 C12 C13 121.0(5) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C12 C13 C14 118.3(5) . . ? C12 C13 C16 119.5(5) . . ? C14 C13 C16 122.2(5) . . ? C15 C14 C13 120.6(5) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C10 120.6(5) . . ? C14 C15 H15 119.7 . . ? C10 C15 H15 119.7 . . ? N17 C16 C13 123.3(5) . . ? N17 C16 H16 118.3 . . ? C13 C16 H16 118.3 . . ? C16 N17 C18 118.1(5) . . ? C23 C18 C19 117.7(5) . . ? C23 C18 N17 124.2(5) . . ? C19 C18 N17 118.0(5) . . ? C20 C19 C18 121.9(5) . . ? C20 C19 H19 119.1 . . ? C18 C19 H19 119.1 . . ? C21 C20 C19 118.6(5) . . ? C21 C20 H20 120.7 . . ? C19 C20 H20 120.7 . . ? O24 C21 C20 125.9(5) . . ? O24 C21 C22 114.2(4) . . ? C20 C21 C22 119.8(5) . . ? C23 C22 C21 121.2(5) . . ? C23 C22 H22 119.4 . . ? C21 C22 H22 119.4 . . ? C22 C23 C18 120.7(5) . . ? C22 C23 H23 119.6 . . ? C18 C23 H23 119.6 . . ? C21 O24 C25 119.8(4) . . ? O24 C25 C26 105.5(4) . . ? O24 C25 H25A 110.6 . . ? C26 C25 H25A 110.6 . . ? O24 C25 H25B 110.6 . . ? C26 C25 H25B 110.6 . . ? H25A C25 H25B 108.8 . . ? C25 C26 C27 115.1(4) . . ? C25 C26 H26A 108.5 . . ? C27 C26 H26A 108.5 . . ? C25 C26 H26B 108.5 . . ? C27 C26 H26B 108.5 . . ? H26A C26 H26B 107.5 . . ? C26 C27 C28 111.4(4) . . ? C26 C27 H27A 109.3 . . ? C28 C27 H27A 109.3 . . ? C26 C27 H27B 109.3 . . ? C28 C27 H27B 109.3 . . ? H27A C27 H27B 108 . . ? C29 C28 C27 114.7(4) . . ? C29 C28 H28A 108.6 . . ? C27 C28 H28A 108.6 . . ? C29 C28 H28B 108.6 . . ? C27 C28 H28B 108.6 . . ? H28A C28 H28B 107.6 . . ? C28 C29 C30 113.4(5) . . ? C28 C29 H29A 108.9 . . ? C30 C29 H29A 108.9 . . ? C28 C29 H29B 108.9 . . ? C30 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? C31 C30 C29 113.7(5) . . ? C31 C30 H30A 108.8 . . ? C29 C30 H30A 108.8 . . ? C31 C30 H30B 108.8 . . ? C29 C30 H30B 108.8 . . ? H30A C30 H30B 107.7 . . ? C30 C31 C32 113.8(5) . . ? C30 C31 H31A 108.8 . . ? C32 C31 H31A 108.8 . . ? C30 C31 H31B 108.8 . . ? C32 C31 H31B 108.8 . . ? H31A C31 H31B 107.7 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Cl11 C101 Cl12 111.0(3) . . ? Cl11 C101 H10A 109.4 . . ? Cl12 C101 H10A 109.4 . . ? Cl11 C101 H10B 109.4 . . ? Cl12 C101 H10B 109.4 . . ? H10A C101 H10B 108 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl2 Pt1 S1 O1 -60.04(19) . . . . ? Cl1 Pt1 S1 O1 120.06(19) . . . . ? Cl2 Pt1 S1 C2 62.4(2) . . . . ? Cl1 Pt1 S1 C2 -117.5(2) . . . . ? Cl2 Pt1 S1 C3 173.7(2) . . . . ? Cl1 Pt1 S1 C3 -6.2(2) . . . . ? Cl2 Pt1 N4 C5 -110.6(4) . . . . ? Cl1 Pt1 N4 C5 69.6(3) . . . . ? Cl2 Pt1 N4 C9 59.8(4) . . . . ? Cl1 Pt1 N4 C9 -120.0(4) . . . . ? C9 N4 C5 C6 -1.1(8) . . . . ? Pt1 N4 C5 C6 169.8(4) . . . . ? N4 C5 C6 C7 -1.8(8) . . . . ? C5 C6 C7 C8 2.7(8) . . . . ? C6 C7 C8 C9 -0.8(8) . . . . ? C5 N4 C9 C8 3.0(7) . . . . ? Pt1 N4 C9 C8 -166.9(4) . . . . ? C5 N4 C9 C10 -175.5(5) . . . . ? Pt1 N4 C9 C10 14.6(7) . . . . ? C7 C8 C9 N4 -2.1(8) . . . . ? C7 C8 C9 C10 176.5(5) . . . . ? N4 C9 C10 C11 47.7(7) . . . . ? C8 C9 C10 C11 -130.8(5) . . . . ? N4 C9 C10 C15 -137.0(5) . . . . ? C8 C9 C10 C15 44.6(7) . . . . ? C15 C10 C11 C12 1.2(8) . . . . ? C9 C10 C11 C12 176.6(5) . . . . ? C10 C11 C12 C13 1.3(8) . . . . ? C11 C12 C13 C14 -2.5(8) . . . . ? C11 C12 C13 C16 176.4(5) . . . . ? C12 C13 C14 C15 1.2(8) . . . . ? C16 C13 C14 C15 -177.7(5) . . . . ? C13 C14 C15 C10 1.3(8) . . . . ? C11 C10 C15 C14 -2.5(8) . . . . ? C9 C10 C15 C14 -177.9(5) . . . . ? C12 C13 C16 N17 -168.4(5) . . . . ? C14 C13 C16 N17 10.4(8) . . . . ? C13 C16 N17 C18 172.6(5) . . . . ? C16 N17 C18 C23 -23.6(8) . . . . ? C16 N17 C18 C19 160.2(5) . . . . ? C23 C18 C19 C20 2.5(8) . . . . ? N17 C18 C19 C20 179.0(5) . . . . ? C18 C19 C20 C21 -1.6(8) . . . . ? C19 C20 C21 O24 178.8(5) . . . . ? C19 C20 C21 C22 0.3(8) . . . . ? O24 C21 C22 C23 -178.8(5) . . . . ? C20 C21 C22 C23 -0.1(9) . . . . ? C21 C22 C23 C18 1.1(9) . . . . ? C19 C18 C23 C22 -2.3(8) . . . . ? N17 C18 C23 C22 -178.5(5) . . . . ? C20 C21 O24 C25 8.1(8) . . . . ? C22 C21 O24 C25 -173.4(5) . . . . ? C21 O24 C25 C26 -178.1(5) . . . . ? O24 C25 C26 C27 177.4(5) . . . . ? C25 C26 C27 C28 176.3(5) . . . . ? C26 C27 C28 C29 177.4(5) . . . . ? C27 C28 C29 C30 179.5(5) . . . . ? C28 C29 C30 C31 178.0(5) . . . . ? C29 C30 C31 C32 -177.9(5) . . . . ? _database_code_depnum_ccdc_archive 'CCDC 948667' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_job _audit_creation_date 2011-07-13T16:05:43-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C54 H66 N6 O3 Pd2 S2' _chemical_formula_sum 'C54 H66 N6 O3 Pd2 S2' _chemical_formula_weight 1124.05 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2638(10) _cell_length_b 14.4107(14) _cell_length_c 19.1385(16) _cell_angle_alpha 73.808(3) _cell_angle_beta 89.864(4) _cell_angle_gamma 73.765(4) _cell_volume 2601.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9917 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 27.25 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.435 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.820 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.787 _exptl_absorpt_correction_T_max 0.921 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0494 _diffrn_reflns_av_unetI/netI 0.0522 _diffrn_reflns_number 39191 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.981 _diffrn_measured_fraction_theta_max 0.981 _reflns_number_total 11705 _reflns_number_gt 8808 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2 (Bruker, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2006)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2006)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0804P)^2^+4.6956P] 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_number_reflns 11705 _refine_ls_number_parameters 596 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0766 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1609 _refine_ls_wR_factor_gt 0.1388 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.062 _refine_diff_density_min -1.462 _refine_diff_density_rms 0.234 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' 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 Pd1 Pd 0.52090(3) 0.24668(2) 0.630622(16) 0.03056(11) Uani 1 1 d . . . S1 S 0.62519(14) 0.09655(9) 0.61252(7) 0.0450(3) Uani 1 1 d . . . O1 O 0.3981(3) 0.2948(2) 0.53432(16) 0.0361(7) Uani 1 1 d . . . C2 C 0.4271(4) 0.2703(3) 0.4764(2) 0.0298(9) Uani 1 1 d . . . C3 C 0.3477(4) 0.3433(3) 0.4074(2) 0.0307(9) Uani 1 1 d . . . C4 C 0.2588(4) 0.4342(3) 0.4099(2) 0.0356(10) Uani 1 1 d . . . H4 H 0.2474 0.449 0.4552 0.043 Uiso 1 1 calc R . . C5 C 0.1864(5) 0.5038(4) 0.3473(3) 0.0442(11) Uani 1 1 d . . . H5 H 0.1269 0.5664 0.3496 0.053 Uiso 1 1 calc R . . C6 C 0.2012(6) 0.4817(4) 0.2812(3) 0.0508(13) Uani 1 1 d . . . H6 H 0.1497 0.5282 0.2383 0.061 Uiso 1 1 calc R . . C7 C 0.2908(7) 0.3921(4) 0.2781(3) 0.0591(15) Uani 1 1 d . . . H7 H 0.3025 0.3775 0.2326 0.071 Uiso 1 1 calc R . . C8 C 0.3640(6) 0.3230(4) 0.3411(3) 0.0470(12) Uani 1 1 d . . . H8 H 0.4258 0.2614 0.3385 0.056 Uiso 1 1 calc R . . N9 N 0.5180(4) 0.1895(3) 0.4672(2) 0.0346(8) Uani 1 1 d . . . C10 C 0.5968(5) 0.1117(4) 0.5197(3) 0.0450(12) Uani 1 1 d . A . N11 N 0.6666(6) 0.0344(4) 0.4956(3) 0.089(2) Uani 1 1 d . . . C12 C 0.6564(7) 0.0426(5) 0.4168(3) 0.069(2) Uani 1 1 d . A . H12A H 0.6832 -0.0257 0.4101 0.082 Uiso 1 1 calc R . . H12B H 0.5611 0.0769 0.3961 0.082 Uiso 1 1 calc R . . C13 C 0.7465(7) 0.1008(6) 0.3785(4) 0.085(2) Uani 1 1 d . . . H13A H 0.727 0.1651 0.3911 0.102 Uiso 1 1 calc R A . H13B H 0.8423 0.062 0.3959 0.102 Uiso 1 1 calc R . . C14 C 0.7304(8) 0.1230(7) 0.2986(4) 0.094(3) Uani 1 1 d . A . H14A H 0.756 0.0597 0.2854 0.141 Uiso 1 1 calc R . . H14B H 0.7892 0.1643 0.2761 0.141 Uiso 1 1 calc R . . H14C H 0.6353 0.1599 0.281 0.141 Uiso 1 1 calc R . . C15A C 0.7310(8) -0.0729(7) 0.5502(5) 0.0416(9) Uani 0.588(6) 1 d P A 1 H15A H 0.6915 -0.0775 0.5979 0.05 Uiso 0.588(6) 1 calc PR A 1 H15B H 0.7132 -0.1254 0.5307 0.05 Uiso 0.588(6) 1 calc PR A 1 C16A C 0.8803(8) -0.0874(6) 0.5590(5) 0.0416(9) Uani 0.588(6) 1 d P A 1 H16A H 0.8965 -0.0327 0.5764 0.05 Uiso 0.588(6) 1 calc PR A 1 H16B H 0.9187 -0.0835 0.5111 0.05 Uiso 0.588(6) 1 calc PR A 1 C17A C 0.9519(9) -0.1890(7) 0.6131(5) 0.0416(9) Uani 0.588(6) 1 d P A 1 H17A H 0.9325 -0.1865 0.6628 0.062 Uiso 0.588(6) 1 calc PR A 1 H17B H 1.0504 -0.2044 0.6089 0.062 Uiso 0.588(6) 1 calc PR A 1 H17C H 0.9191 -0.2416 0.6024 0.062 Uiso 0.588(6) 1 calc PR A 1 C15B C 0.8166(12) -0.0287(9) 0.5274(7) 0.0416(9) Uani 0.412(6) 1 d P A 2 H15C H 0.8806 -0.0309 0.4887 0.05 Uiso 0.412(6) 1 calc PR A 2 H15D H 0.8503 -0.004 0.565 0.05 Uiso 0.412(6) 1 calc PR A 2 C16B C 0.7884(12) -0.1304(9) 0.5599(7) 0.0416(9) Uani 0.412(6) 1 d P A 2 H16C H 0.7102 -0.1212 0.5903 0.05 Uiso 0.412(6) 1 calc PR A 2 H16D H 0.7638 -0.1552 0.52 0.05 Uiso 0.412(6) 1 calc PR A 2 C17B C 0.9119(14) -0.2080(10) 0.6063(8) 0.0416(9) Uani 0.412(6) 1 d P A 2 H17D H 0.9853 -0.2244 0.575 0.062 Uiso 0.412(6) 1 calc PR A 2 H17E H 0.8876 -0.2693 0.6315 0.062 Uiso 0.412(6) 1 calc PR A 2 H17F H 0.9427 -0.1803 0.6424 0.062 Uiso 0.412(6) 1 calc PR A 2 N21 N 0.4426(4) 0.3844(3) 0.65106(18) 0.0305(7) Uani 1 1 d . . . C22 C 0.5104(4) 0.3938(3) 0.7049(2) 0.0331(9) Uani 1 1 d . . . H22 H 0.4896 0.4554 0.7174 0.04 Uiso 1 1 calc R . . C23 C 0.6181(5) 0.3067(3) 0.7446(2) 0.0335(9) Uani 1 1 d . . . C24 C 0.6424(4) 0.2212(3) 0.7195(2) 0.0310(9) Uani 1 1 d . . . C25 C 0.7503(5) 0.1377(3) 0.7549(2) 0.0329(9) Uani 1 1 d . . . H25 H 0.7691 0.0781 0.7398 0.039 Uiso 1 1 calc R . . C26 C 0.8321(4) 0.1406(3) 0.8132(2) 0.0306(9) Uani 1 1 d . . . C27 C 0.8043(5) 0.2258(3) 0.8393(2) 0.0461(10) Uani 1 1 d . . . C28 C 0.6954(5) 0.3084(3) 0.8041(2) 0.0332(9) Uani 1 1 d . . . H28 H 0.6732 0.3668 0.8207 0.04 Uiso 1 1 calc R . . C29 C 0.9530(4) 0.0570(3) 0.8482(2) 0.0308(9) Uani 1 1 d . . . C30 C 1.0033(5) -0.0324(3) 0.8304(2) 0.0361(10) Uani 1 1 d . . . H30 H 0.957 -0.0452 0.7928 0.043 Uiso 1 1 calc R . . C31 C 1.1214(5) -0.1033(3) 0.8675(2) 0.0406(11) Uani 1 1 d . . . H31 H 1.1571 -0.1645 0.8552 0.049 Uiso 1 1 calc R . . C32 C 1.1872(5) -0.0839(4) 0.9231(2) 0.0399(10) Uani 1 1 d . . . H32 H 1.2677 -0.1313 0.9497 0.048 Uiso 1 1 calc R . . C33 C 1.1314(5) 0.0067(3) 0.9381(2) 0.0361(10) Uani 1 1 d . . . H33 H 1.1752 0.0205 0.9761 0.043 Uiso 1 1 calc R . . N34 N 1.0200(4) 0.0751(3) 0.90226(17) 0.0192(7) Uani 1 1 d . . . C41 C 0.3419(4) 0.4698(3) 0.6049(2) 0.0284(8) Uani 1 1 d . . . C42 C 0.2090(4) 0.4665(3) 0.5988(2) 0.0347(9) Uani 1 1 d . . . H42 H 0.1849 0.4085 0.626 0.042 Uiso 1 1 calc R . . C43 C 0.1111(4) 0.5474(4) 0.5533(2) 0.0355(10) Uani 1 1 d . . . H43 H 0.0194 0.5458 0.5505 0.043 Uiso 1 1 calc R . . C44 C 0.1467(4) 0.6307(3) 0.5115(2) 0.0322(9) Uani 1 1 d . . . C45 C 0.2796(5) 0.6347(4) 0.5172(3) 0.0432(11) Uani 1 1 d . . . H45 H 0.304 0.692 0.4891 0.052 Uiso 1 1 calc R . . C46 C 0.3773(5) 0.5533(3) 0.5647(3) 0.0392(10) Uani 1 1 d . . . H46 H 0.4685 0.5556 0.5692 0.047 Uiso 1 1 calc R . . O47 O 0.0441(3) 0.7038(2) 0.46565(17) 0.0405(7) Uani 1 1 d . . . C48 C 0.0789(5) 0.7850(4) 0.4137(3) 0.0423(11) Uani 1 1 d . . . H48A H 0.1599 0.758 0.3892 0.051 Uiso 1 1 calc R . . H48B H 0.0998 0.8315 0.4386 0.051 Uiso 1 1 calc R . . C49 C -0.0429(5) 0.8401(3) 0.3583(3) 0.0404(10) Uani 1 1 d . . . H49A H -0.0271 0.902 0.3257 0.049 Uiso 1 1 calc R . . H49B H -0.1245 0.861 0.3842 0.049 Uiso 1 1 calc R . . C50 C -0.0696(5) 0.7753(3) 0.3123(2) 0.0363(10) Uani 1 1 d . . . H50A H 0.0099 0.7585 0.2839 0.044 Uiso 1 1 calc R . . H50B H -0.078 0.7111 0.3453 0.044 Uiso 1 1 calc R . . C51 C -0.1966(5) 0.8252(3) 0.2599(2) 0.0361(10) Uani 1 1 d . . . H51A H -0.19 0.8906 0.2281 0.043 Uiso 1 1 calc R . . H51B H -0.2768 0.8394 0.2883 0.043 Uiso 1 1 calc R . . C52 C -0.2185(5) 0.7612(3) 0.2124(2) 0.0365(10) Uani 1 1 d . . . H52A H -0.137 0.7452 0.1852 0.044 Uiso 1 1 calc R . . H52B H -0.2278 0.6966 0.2443 0.044 Uiso 1 1 calc R . . C53 C -0.3426(5) 0.8116(3) 0.1583(2) 0.0374(10) Uani 1 1 d . . . H53A H -0.3323 0.8759 0.1265 0.045 Uiso 1 1 calc R . . H53B H -0.4234 0.8286 0.1858 0.045 Uiso 1 1 calc R . . C54 C -0.3698(5) 0.7502(4) 0.1102(3) 0.0486(12) Uani 1 1 d . . . H54A H -0.3803 0.6857 0.1414 0.058 Uiso 1 1 calc R . . H54B H -0.2906 0.7342 0.0815 0.058 Uiso 1 1 calc R . . C55 C -0.4972(6) 0.8062(5) 0.0583(3) 0.0649(16) Uani 1 1 d . . . H55A H -0.577 0.8171 0.0866 0.097 Uiso 1 1 calc R . . H55B H -0.5078 0.7659 0.0262 0.097 Uiso 1 1 calc R . . H55C H -0.4889 0.8715 0.0288 0.097 Uiso 1 1 calc R . . Pd2 Pd 0.93378(3) 0.21266(2) 0.920584(16) 0.03220(11) Uani 1 1 d . . . S2 S 0.82134(15) 0.36420(10) 0.93347(7) 0.0525(4) Uani 1 1 d . . . O61 O 1.0813(3) 0.1847(2) 1.00345(16) 0.0386(7) Uani 1 1 d . . . C62 C 1.0821(4) 0.2303(3) 1.0516(2) 0.0299(9) Uani 1 1 d . . . C63 C 1.1963(4) 0.1810(3) 1.1103(2) 0.0295(8) Uani 1 1 d . . . C64 C 1.3073(5) 0.1056(4) 1.1009(3) 0.0422(11) Uani 1 1 d . . . H64 H 1.3098 0.0858 1.0574 0.051 Uiso 1 1 calc R . . C65 C 1.4139(6) 0.0593(4) 1.1543(3) 0.0571(15) Uani 1 1 d . . . H65 H 1.4917 0.0103 1.1464 0.068 Uiso 1 1 calc R . . C66 C 1.4079(6) 0.0841(4) 1.2198(3) 0.0561(15) Uani 1 1 d . . . H66 H 1.4792 0.0502 1.2575 0.067 Uiso 1 1 calc R . . C67 C 1.2975(6) 0.1582(4) 1.2290(3) 0.0476(12) Uani 1 1 d . . . H67 H 1.2931 0.1756 1.2734 0.057 Uiso 1 1 calc R . . C68 C 1.1926(5) 0.2079(3) 1.1746(2) 0.0357(10) Uani 1 1 d . . . H68 H 1.1182 0.2604 1.1813 0.043 Uiso 1 1 calc R . . N69 N 0.9955(4) 0.3139(3) 1.05898(19) 0.0364(8) Uani 1 1 d . . . C70 C 0.8857(6) 0.3744(4) 1.0141(3) 0.0520(14) Uani 1 1 d . . . N71 N 0.8168(6) 0.4536(4) 1.0359(3) 0.087(2) Uani 1 1 d . . . C72 C 0.8626(7) 0.4719(5) 1.1035(4) 0.078(2) Uani 1 1 d . . . H72A H 0.9634 0.449 1.1097 0.093 Uiso 1 1 calc R . . H72B H 0.8328 0.5454 1.0976 0.093 Uiso 1 1 calc R . . C73 C 0.8093(7) 0.4197(6) 1.1697(4) 0.079(2) Uani 1 1 d . . . H73A H 0.8404 0.346 1.1764 0.095 Uiso 1 1 calc R . . H73B H 0.7086 0.4417 1.1636 0.095 Uiso 1 1 calc R . . C74 C 0.8560(8) 0.4410(5) 1.2372(4) 0.084(2) Uani 1 1 d . . . H74A H 0.9522 0.4035 1.2512 0.126 Uiso 1 1 calc R . . H74B H 0.8014 0.4199 1.2773 0.126 Uiso 1 1 calc R . . H74C H 0.8446 0.5135 1.2267 0.126 Uiso 1 1 calc R . . C75 C 0.6697(7) 0.5160(5) 1.0042(3) 0.0649(9) Uani 1 1 d . . . H75A H 0.6252 0.4758 0.9834 0.078 Uiso 1 1 calc R . . H75B H 0.6149 0.5373 1.0427 0.078 Uiso 1 1 calc R . . C76 C 0.6828(7) 0.6032(5) 0.9477(3) 0.0649(9) Uani 1 1 d . . . H76A H 0.7469 0.5818 0.9125 0.078 Uiso 1 1 calc R . . H76B H 0.7171 0.6477 0.9693 0.078 Uiso 1 1 calc R . . C77 C 0.5335(7) 0.6612(5) 0.9078(3) 0.0649(9) Uani 1 1 d . . . H77A H 0.5108 0.624 0.8761 0.097 Uiso 1 1 calc R . . H77B H 0.5311 0.7293 0.8783 0.097 Uiso 1 1 calc R . . H77C H 0.4672 0.6657 0.9445 0.097 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.03296(19) 0.03521(19) 0.02646(17) -0.01034(14) -0.00465(13) -0.01307(14) S1 0.0541(7) 0.0370(6) 0.0424(6) -0.0153(5) -0.0162(6) -0.0068(5) O1 0.0332(16) 0.0465(18) 0.0306(15) -0.0176(14) -0.0059(12) -0.0080(14) C2 0.028(2) 0.037(2) 0.032(2) -0.0153(18) -0.0014(16) -0.0173(17) C3 0.028(2) 0.039(2) 0.029(2) -0.0109(18) -0.0014(16) -0.0161(18) C4 0.028(2) 0.044(2) 0.035(2) -0.014(2) 0.0003(18) -0.0089(19) C5 0.037(3) 0.048(3) 0.042(3) -0.009(2) 0.001(2) -0.006(2) C6 0.064(4) 0.049(3) 0.033(2) 0.000(2) -0.012(2) -0.018(3) C7 0.094(5) 0.052(3) 0.030(2) -0.013(2) -0.007(3) -0.017(3) C8 0.066(3) 0.043(3) 0.031(2) -0.013(2) -0.001(2) -0.013(2) N9 0.0328(19) 0.038(2) 0.0369(19) -0.0180(16) -0.0045(15) -0.0086(16) C10 0.043(3) 0.046(3) 0.045(3) -0.022(2) -0.015(2) -0.003(2) N11 0.094(4) 0.082(4) 0.067(3) -0.054(3) -0.043(3) 0.045(3) C12 0.066(4) 0.071(4) 0.059(4) -0.042(3) -0.025(3) 0.017(3) C13 0.052(4) 0.108(6) 0.088(5) -0.051(5) -0.020(4) 0.007(4) C14 0.081(5) 0.110(6) 0.088(6) -0.053(5) 0.007(4) 0.000(5) C15A 0.036(3) 0.041(2) 0.048(2) -0.0120(18) -0.0032(18) -0.0130(16) C16A 0.036(3) 0.041(2) 0.048(2) -0.0120(18) -0.0032(18) -0.0130(16) C17A 0.036(3) 0.041(2) 0.048(2) -0.0120(18) -0.0032(18) -0.0130(16) C15B 0.036(3) 0.041(2) 0.048(2) -0.0120(18) -0.0032(18) -0.0130(16) C16B 0.036(3) 0.041(2) 0.048(2) -0.0120(18) -0.0032(18) -0.0130(16) C17B 0.036(3) 0.041(2) 0.048(2) -0.0120(18) -0.0032(18) -0.0130(16) N21 0.0337(19) 0.0369(19) 0.0249(17) -0.0095(15) 0.0032(14) -0.0161(15) C22 0.036(2) 0.040(2) 0.026(2) -0.0119(18) -0.0009(17) -0.0116(19) C23 0.036(2) 0.040(2) 0.0243(19) -0.0073(18) -0.0009(17) -0.0131(19) C24 0.035(2) 0.037(2) 0.0232(19) -0.0079(17) -0.0014(16) -0.0159(18) C25 0.039(2) 0.036(2) 0.028(2) -0.0098(18) -0.0009(18) -0.0157(19) C26 0.037(2) 0.034(2) 0.0219(18) -0.0057(16) 0.0019(17) -0.0140(18) C27 0.056(3) 0.054(2) 0.0289(19) -0.0114(18) -0.0011(18) -0.018(2) C28 0.038(2) 0.037(2) 0.026(2) -0.0104(17) -0.0033(17) -0.0116(19) C29 0.036(2) 0.035(2) 0.0218(18) -0.0030(16) 0.0013(17) -0.0164(18) C30 0.046(3) 0.034(2) 0.029(2) -0.0054(18) -0.0016(19) -0.018(2) C31 0.053(3) 0.034(2) 0.036(2) -0.0065(19) -0.002(2) -0.017(2) C32 0.041(3) 0.041(2) 0.035(2) -0.006(2) -0.005(2) -0.011(2) C33 0.038(2) 0.046(3) 0.026(2) -0.0108(19) 0.0002(18) -0.015(2) N34 0.0254(18) 0.0235(17) 0.0101(15) -0.0034(13) 0.0027(13) -0.0110(14) C41 0.030(2) 0.034(2) 0.0239(18) -0.0123(16) -0.0037(16) -0.0093(17) C42 0.034(2) 0.045(2) 0.028(2) -0.0060(18) 0.0021(18) -0.021(2) C43 0.026(2) 0.053(3) 0.032(2) -0.013(2) 0.0039(17) -0.0162(19) C44 0.028(2) 0.040(2) 0.027(2) -0.0107(18) 0.0002(16) -0.0071(18) C45 0.035(2) 0.044(3) 0.049(3) -0.004(2) -0.008(2) -0.018(2) C46 0.031(2) 0.043(2) 0.043(2) -0.004(2) -0.0069(19) -0.0178(19) O47 0.0325(17) 0.0494(19) 0.0336(16) -0.0045(14) -0.0003(13) -0.0098(14) C48 0.046(3) 0.041(2) 0.039(2) -0.010(2) -0.005(2) -0.014(2) C49 0.040(3) 0.037(2) 0.039(2) -0.008(2) -0.002(2) -0.007(2) C50 0.038(2) 0.033(2) 0.034(2) -0.0054(18) -0.0003(19) -0.0082(19) C51 0.033(2) 0.039(2) 0.035(2) -0.0099(19) 0.0031(18) -0.0086(19) C52 0.036(2) 0.035(2) 0.037(2) -0.0103(19) 0.0041(19) -0.0095(19) C53 0.033(2) 0.041(2) 0.033(2) -0.0080(19) 0.0043(18) -0.0062(19) C54 0.043(3) 0.062(3) 0.042(3) -0.022(2) 0.003(2) -0.009(2) C55 0.051(3) 0.096(5) 0.046(3) -0.020(3) -0.004(3) -0.019(3) Pd2 0.0362(2) 0.0396(2) 0.02052(16) -0.01081(14) -0.00388(13) -0.00850(15) S2 0.0609(8) 0.0486(7) 0.0382(6) -0.0212(6) -0.0254(6) 0.0081(6) O61 0.0384(17) 0.0472(18) 0.0297(15) -0.0189(14) -0.0067(13) -0.0038(14) C62 0.033(2) 0.038(2) 0.0200(18) -0.0079(17) 0.0006(16) -0.0128(18) C63 0.032(2) 0.030(2) 0.027(2) -0.0062(16) -0.0015(16) -0.0128(17) C64 0.041(3) 0.039(2) 0.048(3) -0.020(2) -0.009(2) -0.007(2) C65 0.048(3) 0.046(3) 0.074(4) -0.023(3) -0.018(3) -0.002(2) C66 0.063(4) 0.037(3) 0.059(3) -0.006(2) -0.032(3) -0.008(2) C67 0.062(3) 0.046(3) 0.033(2) -0.011(2) -0.018(2) -0.012(2) C68 0.036(2) 0.041(2) 0.030(2) -0.0097(19) -0.0042(18) -0.0114(19) N69 0.037(2) 0.040(2) 0.0293(18) -0.0124(16) -0.0085(15) -0.0052(16) C70 0.056(3) 0.050(3) 0.043(3) -0.024(2) -0.019(2) 0.006(2) N71 0.088(4) 0.077(4) 0.075(4) -0.056(3) -0.056(3) 0.041(3) C72 0.083(5) 0.060(4) 0.077(4) -0.048(3) -0.054(4) 0.029(3) C73 0.055(4) 0.107(5) 0.081(5) -0.066(5) -0.024(3) 0.008(4) C74 0.093(5) 0.081(5) 0.072(4) -0.050(4) -0.035(4) 0.012(4) C75 0.074(2) 0.069(2) 0.057(2) -0.0203(17) -0.0008(18) -0.0267(19) C76 0.074(2) 0.069(2) 0.057(2) -0.0203(17) -0.0008(18) -0.0267(19) C77 0.074(2) 0.069(2) 0.057(2) -0.0203(17) -0.0008(18) -0.0267(19) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C24 1.996(4) . ? Pd1 O1 2.068(3) . ? Pd1 N21 2.069(3) . ? Pd1 S1 2.2512(12) . ? S1 C10 1.743(5) . ? O1 C2 1.265(5) . ? C2 N9 1.328(5) . ? C2 C3 1.505(6) . ? C3 C8 1.380(6) . ? C3 C4 1.384(6) . ? C4 C5 1.381(6) . ? C4 H4 0.95 . ? C5 C6 1.386(7) . ? C5 H5 0.95 . ? C6 C7 1.376(8) . ? C6 H6 0.95 . ? C7 C8 1.388(7) . ? C7 H7 0.95 . ? C8 H8 0.95 . ? N9 C10 1.337(6) . ? C10 N11 1.344(6) . ? N11 C12 1.482(7) . ? N11 C15A 1.565(10) . ? N11 C15B 1.574(13) . ? C12 C13 1.478(11) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 C14 1.472(10) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15A C16A 1.491(11) . ? C15A H15A 0.99 . ? C15A H15B 0.99 . ? C16A C17A 1.520(12) . ? C16A H16A 0.99 . ? C16A H16B 0.99 . ? C17A H17A 0.98 . ? C17A H17B 0.98 . ? C17A H17C 0.98 . ? C15B C16B 1.531(17) . ? C15B H15C 0.99 . ? C15B H15D 0.99 . ? C16B C17B 1.519(18) . ? C16B H16C 0.99 . ? C16B H16D 0.99 . ? C17B H17D 0.98 . ? C17B H17E 0.98 . ? C17B H17F 0.98 . ? N21 C22 1.303(5) . ? N21 C41 1.431(5) . ? C22 C23 1.439(6) . ? C22 H22 0.95 . ? C23 C28 1.401(6) . ? C23 C24 1.404(6) . ? C24 C25 1.392(6) . ? C25 C26 1.415(6) . ? C25 H25 0.95 . ? C26 C27 1.409(6) . ? C26 C29 1.469(6) . ? C27 C28 1.390(6) . ? C27 Pd2 1.982(4) . ? C28 H28 0.95 . ? C29 N34 1.365(5) . ? C29 C30 1.383(6) . ? C30 C31 1.388(7) . ? C30 H30 0.95 . ? C31 C32 1.393(6) . ? C31 H31 0.95 . ? C32 C33 1.380(6) . ? C32 H32 0.95 . ? C33 N34 1.322(6) . ? C33 H33 0.95 . ? N34 Pd2 2.059(4) . ? C41 C46 1.379(6) . ? C41 C42 1.385(6) . ? C42 C43 1.382(6) . ? C42 H42 0.95 . ? C43 C44 1.386(6) . ? C43 H43 0.95 . ? C44 O47 1.363(5) . ? C44 C45 1.387(6) . ? C45 C46 1.400(6) . ? C45 H45 0.95 . ? C46 H46 0.95 . ? O47 C48 1.439(6) . ? C48 C49 1.516(6) . ? C48 H48A 0.99 . ? C48 H48B 0.99 . ? C49 C50 1.526(6) . ? C49 H49A 0.99 . ? C49 H49B 0.99 . ? C50 C51 1.517(6) . ? C50 H50A 0.99 . ? C50 H50B 0.99 . ? C51 C52 1.522(6) . ? C51 H51A 0.99 . ? C51 H51B 0.99 . ? C52 C53 1.513(6) . ? C52 H52A 0.99 . ? C52 H52B 0.99 . ? C53 C54 1.518(7) . ? C53 H53A 0.99 . ? C53 H53B 0.99 . ? C54 C55 1.522(7) . ? C54 H54A 0.99 . ? C54 H54B 0.99 . ? C55 H55A 0.98 . ? C55 H55B 0.98 . ? C55 H55C 0.98 . ? Pd2 O61 2.070(3) . ? Pd2 S2 2.2475(13) . ? S2 C70 1.739(5) . ? O61 C62 1.273(5) . ? C62 N69 1.326(6) . ? C62 C63 1.497(6) . ? C63 C68 1.387(6) . ? C63 C64 1.387(6) . ? C64 C65 1.380(7) . ? C64 H64 0.95 . ? C65 C66 1.392(8) . ? C65 H65 0.95 . ? C66 C67 1.371(8) . ? C66 H66 0.95 . ? C67 C68 1.383(6) . ? C67 H67 0.95 . ? C68 H68 0.95 . ? N69 C70 1.343(6) . ? C70 N71 1.337(7) . ? N71 C72 1.493(6) . ? N71 C75 1.548(8) . ? C72 C73 1.472(11) . ? C72 H72A 0.99 . ? C72 H72B 0.99 . ? C73 C74 1.517(7) . ? C73 H73A 0.99 . ? C73 H73B 0.99 . ? C74 H74A 0.98 . ? C74 H74B 0.98 . ? C74 H74C 0.98 . ? C75 C76 1.451(9) . ? C75 H75A 0.99 . ? C75 H75B 0.99 . ? C76 C77 1.601(9) . ? C76 H76A 0.99 . ? C76 H76B 0.99 . ? C77 H77A 0.98 . ? C77 H77B 0.98 . ? C77 H77C 0.98 . ? 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 C24 Pd1 O1 171.37(15) . . ? C24 Pd1 N21 81.54(16) . . ? O1 Pd1 N21 91.73(12) . . ? C24 Pd1 S1 93.97(13) . . ? O1 Pd1 S1 92.46(9) . . ? N21 Pd1 S1 174.64(10) . . ? C10 S1 Pd1 106.55(17) . . ? C2 O1 Pd1 127.0(3) . . ? O1 C2 N9 129.6(4) . . ? O1 C2 C3 115.6(4) . . ? N9 C2 C3 114.8(4) . . ? C8 C3 C4 118.9(4) . . ? C8 C3 C2 121.5(4) . . ? C4 C3 C2 119.6(4) . . ? C5 C4 C3 121.1(4) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C4 C5 C6 119.5(5) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C7 C6 C5 119.8(5) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C6 C7 C8 120.2(5) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C3 C8 C7 120.4(5) . . ? C3 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C2 N9 C10 126.5(4) . . ? N9 C10 N11 113.6(4) . . ? N9 C10 S1 130.5(4) . . ? N11 C10 S1 115.9(4) . . ? C10 N11 C12 120.0(5) . . ? C10 N11 C15A 120.7(6) . . ? C12 N11 C15A 117.7(5) . . ? C10 N11 C15B 121.5(6) . . ? C12 N11 C15B 107.7(6) . . ? C15A N11 C15B 46.3(5) . . ? C13 C12 N11 109.6(6) . . ? C13 C12 H12A 109.8 . . ? N11 C12 H12A 109.8 . . ? C13 C12 H12B 109.8 . . ? N11 C12 H12B 109.8 . . ? H12A C12 H12B 108.2 . . ? C14 C13 C12 113.2(6) . . ? C14 C13 H13A 108.9 . . ? C12 C13 H13A 108.9 . . ? C14 C13 H13B 108.9 . . ? C12 C13 H13B 108.9 . . ? H13A C13 H13B 107.8 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16A C15A N11 107.0(7) . . ? C16A C15A H15A 110.3 . . ? N11 C15A H15A 110.3 . . ? C16A C15A H15B 110.3 . . ? N11 C15A H15B 110.3 . . ? H15A C15A H15B 108.6 . . ? C15A C16A C17A 111.0(7) . . ? C15A C16A H16A 109.4 . . ? C17A C16A H16A 109.4 . . ? C15A C16A H16B 109.4 . . ? C17A C16A H16B 109.4 . . ? H16A C16A H16B 108 . . ? C16B C15B N11 97.3(8) . . ? C16B C15B H15C 112.3 . . ? N11 C15B H15C 112.3 . . ? C16B C15B H15D 112.3 . . ? N11 C15B H15D 112.3 . . ? H15C C15B H15D 109.9 . . ? C17B C16B C15B 111.2(10) . . ? C17B C16B H16C 109.4 . . ? C15B C16B H16C 109.4 . . ? C17B C16B H16D 109.4 . . ? C15B C16B H16D 109.4 . . ? H16C C16B H16D 108 . . ? C16B C17B H17D 109.5 . . ? C16B C17B H17E 109.5 . . ? H17D C17B H17E 109.5 . . ? C16B C17B H17F 109.5 . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? C22 N21 C41 120.5(4) . . ? C22 N21 Pd1 113.0(3) . . ? C41 N21 Pd1 125.6(3) . . ? N21 C22 C23 117.0(4) . . ? N21 C22 H22 121.5 . . ? C23 C22 H22 121.5 . . ? C28 C23 C24 122.2(4) . . ? C28 C23 C22 121.5(4) . . ? C24 C23 C22 116.3(4) . . ? C25 C24 C23 117.3(4) . . ? C25 C24 Pd1 130.6(3) . . ? C23 C24 Pd1 111.9(3) . . ? C24 C25 C26 120.6(4) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C27 C26 C25 121.6(4) . . ? C27 C26 C29 116.1(4) . . ? C25 C26 C29 122.3(4) . . ? C28 C27 C26 117.4(4) . . ? C28 C27 Pd2 128.3(3) . . ? C26 C27 Pd2 114.2(3) . . ? C27 C28 C23 120.8(4) . . ? C27 C28 H28 119.6 . . ? C23 C28 H28 119.6 . . ? N34 C29 C30 119.8(4) . . ? N34 C29 C26 113.4(4) . . ? C30 C29 C26 126.7(4) . . ? C29 C30 C31 120.0(4) . . ? C29 C30 H30 120 . . ? C31 C30 H30 120 . . ? C30 C31 C32 119.3(4) . . ? C30 C31 H31 120.4 . . ? C32 C31 H31 120.4 . . ? C33 C32 C31 117.8(4) . . ? C33 C32 H32 121.1 . . ? C31 C32 H32 121.1 . . ? N34 C33 C32 123.2(4) . . ? C34 C33 H33 118.4 . . ? C32 C33 H33 118.4 . . ? C33 N34 C29 120.0(4) . . ? C33 N34 Pd2 125.1(3) . . ? C29 N34 Pd2 114.9(3) . . ? C46 C41 C42 120.0(4) . . ? C46 C41 N21 120.5(4) . . ? C42 C41 N21 119.5(4) . . ? C43 C42 C41 120.2(4) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C42 C43 C44 120.1(4) . . ? C42 C43 H43 120 . . ? C44 C43 H43 120 . . ? O47 C44 C43 115.3(4) . . ? O47 C44 C45 124.5(4) . . ? C43 C44 C45 120.1(4) . . ? C44 C45 C46 119.3(4) . . ? C44 C45 H45 120.3 . . ? C46 C45 H45 120.3 . . ? C41 C46 C45 120.2(4) . . ? C41 C46 H46 119.9 . . ? C45 C46 H46 119.9 . . ? C44 O47 C48 117.7(4) . . ? O47 C48 C49 107.1(4) . . ? O47 C48 H48A 110.3 . . ? C49 C48 H48A 110.3 . . ? O47 C48 H48B 110.3 . . ? C49 C48 H48B 110.3 . . ? H48A C48 H48B 108.5 . . ? C48 C49 C50 112.4(4) . . ? C48 C49 H49A 109.1 . . ? C50 C49 H49A 109.1 . . ? C48 C49 H49B 109.1 . . ? C50 C49 H49B 109.1 . . ? H49A C49 H49B 107.8 . . ? C51 C50 C49 114.0(4) . . ? C51 C50 H50A 108.8 . . ? C49 C50 H50A 108.8 . . ? C51 C50 H50B 108.8 . . ? C49 C50 H50B 108.8 . . ? H50A C50 H50B 107.7 . . ? C50 C51 C52 113.2(4) . . ? C50 C51 H51A 108.9 . . ? C52 C51 H51A 108.9 . . ? C50 C51 H51B 108.9 . . ? C52 C51 H51B 108.9 . . ? H51A C51 H51B 107.7 . . ? C53 C52 C51 113.7(4) . . ? C53 C52 H52A 108.8 . . ? C51 C52 H52A 108.8 . . ? C53 C52 H52B 108.8 . . ? C51 C52 H52B 108.8 . . ? H52A C52 H52B 107.7 . . ? C52 C53 C54 115.7(4) . . ? C52 C53 H53A 108.4 . . ? C54 C53 H53A 108.4 . . ? C52 C53 H53B 108.4 . . ? C54 C53 H53B 108.4 . . ? H53A C53 H53B 107.4 . . ? C53 C54 C55 112.1(5) . . ? C53 C54 H54A 109.2 . . ? C55 C54 H54A 109.2 . . ? C53 C54 H54B 109.2 . . ? C55 C54 H54B 109.2 . . ? H54A C54 H54B 107.9 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C27 Pd2 C34 81.28(16) . . ? C27 Pd2 O61 173.82(15) . . ? N34 Pd2 O61 92.58(13) . . ? C27 Pd2 S2 93.10(13) . . ? N34 Pd2 S2 174.24(10) . . ? O61 Pd2 S2 93.05(9) . . ? C70 S2 Pd2 108.51(17) . . ? C62 O61 Pd2 129.5(3) . . ? O61 C62 N69 130.2(4) . . ? O61 C62 C63 115.4(4) . . ? N69 C62 C63 114.4(3) . . ? C68 C63 C64 119.3(4) . . ? C68 C63 C62 121.3(4) . . ? C64 C63 C62 119.4(4) . . ? C65 C64 C63 120.3(5) . . ? C65 C64 H64 119.8 . . ? C63 C64 H64 119.8 . . ? C64 C65 C66 120.2(5) . . ? C64 C65 H65 119.9 . . ? C66 C65 H65 119.9 . . ? C67 C66 C65 119.1(5) . . ? C67 C66 H66 120.5 . . ? C65 C66 H66 120.5 . . ? C66 C67 C68 121.2(5) . . ? C66 C67 H67 119.4 . . ? C68 C67 H67 119.4 . . ? C67 C68 C63 119.8(4) . . ? C67 C68 H68 120.1 . . ? C63 C68 H68 120.1 . . ? C62 N69 C70 127.4(4) . . ? N71 C70 N69 114.0(4) . . ? N71 C70 S2 116.3(4) . . ? N69 C70 S2 129.7(4) . . ? C70 N71 C72 121.6(4) . . ? C70 N71 C75 121.9(4) . . ? C72 N71 C75 115.0(5) . . ? C73 C72 N71 113.2(6) . . ? C73 C72 H72A 108.9 . . ? N71 C72 H72A 108.9 . . ? C73 C72 H72B 108.9 . . ? N71 C72 H72B 108.9 . . ? H72A C72 H72B 107.8 . . ? C72 C73 C74 111.9(6) . . ? C72 C73 H73A 109.2 . . ? C74 C73 H73A 109.2 . . ? C72 C73 H73B 109.2 . . ? C74 C73 H73B 109.2 . . ? H73A C73 H73B 107.9 . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C76 C75 N71 105.7(6) . . ? C76 C75 H75A 110.6 . . ? N71 C75 H75A 110.6 . . ? C76 C75 H75B 110.6 . . ? N71 C75 H75B 110.6 . . ? H75A C75 H75B 108.7 . . ? C75 C76 C77 106.1(5) . . ? C75 C76 H76A 110.5 . . ? C77 C76 H76A 110.5 . . ? C75 C76 H76B 110.5 . . ? C77 C76 H76B 110.5 . . ? H76A C76 H76B 108.7 . . ? C76 C77 H77A 109.5 . . ? C76 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C76 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C24 Pd1 S1 C10 -154.8(2) . . . . ? O1 Pd1 S1 C10 19.5(2) . . . . ? N21 Pd1 O1 C2 146.0(3) . . . . ? S1 Pd1 O1 C2 -30.7(3) . . . . ? Pd1 O1 C2 N9 22.8(6) . . . . ? Pd1 O1 C2 C3 -157.0(3) . . . . ? O1 C2 C3 C8 -176.4(4) . . . . ? N9 C2 C3 C8 3.7(6) . . . . ? O1 C2 C3 C4 5.4(6) . . . . ? N9 C2 C3 C4 -174.4(4) . . . . ? C8 C3 C4 C5 0.5(7) . . . . ? C2 C3 C4 C5 178.7(4) . . . . ? C3 C4 C5 C6 1.0(7) . . . . ? C4 C5 C6 C7 -2.0(8) . . . . ? C5 C6 C7 C8 1.4(9) . . . . ? C4 C3 C8 C7 -1.1(8) . . . . ? C2 C3 C8 C7 -179.2(5) . . . . ? C6 C7 C8 C3 0.2(9) . . . . ? O1 C2 N9 C10 3.4(7) . . . . ? C3 C2 N9 C10 -176.9(4) . . . . ? C2 N9 C10 N11 171.9(5) . . . . ? C2 N9 C10 S1 -9.7(8) . . . . ? Pd1 S1 C10 N9 -7.2(6) . . . . ? Pd1 S1 C10 N11 171.1(5) . . . . ? N9 C10 N11 C12 2.5(9) . . . . ? S1 C10 N11 C12 -176.1(5) . . . . ? N9 C10 N11 C15A -162.8(6) . . . . ? S1 C10 N11 C15A 18.5(9) . . . . ? N9 C10 N11 C15B 142.5(7) . . . . ? S1 C10 N11 C15B -36.1(10) . . . . ? C10 N11 C12 C13 80.5(8) . . . . ? C15A N11 C12 C13 -113.6(7) . . . . ? C15B N11 C12 C13 -64.3(8) . . . . ? N11 C12 C13 C14 -173.1(5) . . . . ? C10 N11 C15A C16A -104.4(8) . . . . ? C12 N11 C15A C16A 89.8(8) . . . . ? C15B N11 C15A C16A 1.3(8) . . . . ? N11 C15A C16A C17A 178.4(6) . . . . ? C10 N11 C15B C16B 117.1(9) . . . . ? C12 N11 C15B C16B -98.7(9) . . . . ? C15A N11 C15B C16B 13.0(7) . . . . ? N11 C15B C16B C17B -171.3(9) . . . . ? C24 Pd1 N21 C22 4.9(3) . . . . ? O1 Pd1 N21 C22 -169.7(3) . . . . ? C24 Pd1 N21 C41 173.7(3) . . . . ? O1 Pd1 N21 C41 -0.9(3) . . . . ? C41 N21 C22 C23 -174.6(4) . . . . ? Pd1 N21 C22 C23 -5.1(5) . . . . ? N21 C22 C23 C28 -178.9(4) . . . . ? N21 C22 C23 C24 2.2(6) . . . . ? C28 C23 C24 C25 -1.9(7) . . . . ? C22 C23 C24 C25 177.0(4) . . . . ? C28 C23 C24 Pd1 -176.9(3) . . . . ? C22 C23 C24 Pd1 2.0(5) . . . . ? N21 Pd1 C24 C25 -177.7(4) . . . . ? S1 Pd1 C24 C25 -0.7(4) . . . . ? N21 Pd1 C24 C23 -3.5(3) . . . . ? S1 Pd1 C24 C23 173.5(3) . . . . ? C23 C24 C25 C26 -0.8(6) . . . . ? Pd1 C24 C25 C26 173.2(3) . . . . ? C24 C25 C26 N27 2.7(7) . . . . ? C24 C25 C26 C29 -175.2(4) . . . . ? C25 C26 C27 C28 -1.9(6) . . . . ? C29 C26 C27 C28 176.1(4) . . . . ? C25 C26 C27 Pd2 -179.5(3) . . . . ? C29 C26 C27 Pd2 -1.5(5) . . . . ? C26 C27 C28 C23 -0.7(7) . . . . ? Pd2 C27 C28 C23 176.5(3) . . . . ? C24 C23 C28 C27 2.7(7) . . . . ? C22 C23 C28 C27 -176.2(4) . . . . ? C27 C26 C29 N34 0.7(5) . . . . ? C25 C26 C29 N34 178.7(4) . . . . ? C27 C26 C29 C30 -177.7(4) . . . . ? C25 C26 C29 C30 0.3(7) . . . . ? N34 C29 C30 C31 0.0(6) . . . . ? C26 C29 C30 C31 178.3(4) . . . . ? C29 C30 C31 C32 0.7(7) . . . . ? C30 C31 C32 C33 -0.6(7) . . . . ? C31 C32 C33 N34 -0.4(7) . . . . ? C32 C33 N34 C29 1.2(7) . . . . ? C32 C33 N34 Pd2 -178.7(3) . . . . ? C30 C29 N34 C33 -1.0(6) . . . . ? C26 C29 N34 C33 -179.4(4) . . . . ? C30 C29 C34 Pd2 178.9(3) . . . . ? C26 C29 C34 Pd2 0.4(4) . . . . ? C22 N21 C41 C46 60.9(6) . . . . ? Pd1 N21 C41 C46 -107.2(4) . . . . ? C22 N21 C41 C42 -121.5(4) . . . . ? Pd1 N21 C41 C42 70.4(5) . . . . ? C46 C41 C42 C43 -0.9(6) . . . . ? N21 C41 C42 C43 -178.5(4) . . . . ? C41 C42 C43 C44 2.3(6) . . . . ? C42 C43 C44 O47 176.7(4) . . . . ? C42 C43 C44 C45 -2.2(6) . . . . ? O47 C44 C45 C46 -177.9(4) . . . . ? C43 C44 C45 C46 0.8(7) . . . . ? C42 C41 C46 C45 -0.4(7) . . . . ? N21 C41 C46 C45 177.1(4) . . . . ? C44 C45 C46 C41 0.5(7) . . . . ? C43 C44 O47 C48 -171.3(4) . . . . ? C45 C44 O47 C48 7.5(6) . . . . ? C44 O47 C48 C49 166.3(4) . . . . ? O47 C48 C49 C50 -66.4(5) . . . . ? C48 C49 C50 C51 175.9(4) . . . . ? C49 C50 C51 C52 177.7(4) . . . . ? C50 C51 C52 C53 -178.2(4) . . . . ? C51 C52 C53 C54 -179.3(4) . . . . ? C52 C53 C54 C55 179.3(4) . . . . ? C28 C27 Pd2 N34 -176.0(4) . . . . ? C26 C27 Pd2 N34 1.3(3) . . . . ? C28 N27 Pd2 S2 5.3(4) . . . . ? C26 C27 Pd2 S2 -177.4(3) . . . . ? C33 N34 Pd2 C27 178.9(4) . . . . ? C29 N34 Pd2 C27 -1.0(3) . . . . ? C33 N34 Pd2 O61 -0.4(4) . . . . ? C29 N34 Pd2 O61 179.8(3) . . . . ? N27 Pd2 S2 C70 168.8(3) . . . . ? N34 Pd2 O61 C62 -165.5(4) . . . . ? S2 Pd2 O61 C62 13.3(4) . . . . ? Pd2 O61 C62 N69 -6.8(7) . . . . ? Pd2 O61 C62 C63 171.4(3) . . . . ? O61 C62 C63 C68 -164.5(4) . . . . ? N69 C62 C63 C68 14.0(6) . . . . ? O61 C62 C63 C64 14.4(6) . . . . ? N69 C62 C63 C64 -167.1(4) . . . . ? C68 C63 C64 C65 -1.2(7) . . . . ? C62 C63 C64 C65 179.9(5) . . . . ? C63 C64 C65 C66 3.3(8) . . . . ? C64 C65 C66 C67 -2.9(9) . . . . ? C65 C66 C67 C68 0.3(9) . . . . ? C66 C67 C68 C63 1.9(8) . . . . ? C64 C63 C68 C67 -1.4(7) . . . . ? C62 C63 C68 C67 177.5(4) . . . . ? O61 C62 N69 C70 -3.1(8) . . . . ? C63 C62 N69 C70 178.7(5) . . . . ? C62 N69 C70 N71 179.7(6) . . . . ? C62 N69 C70 S2 0.1(9) . . . . ? Pd2 S2 C70 N71 -170.3(5) . . . . ? Pd2 S2 C70 N69 9.3(7) . . . . ? N69 C70 N71 C72 1.3(10) . . . . ? S2 C70 N71 C72 -179.0(6) . . . . ? N69 C70 N71 C75 -163.8(6) . . . . ? S2 C70 N71 C75 15.8(9) . . . . ? C70 N71 C72 C73 -87.7(9) . . . . ? C75 N71 C72 C73 78.4(7) . . . . ? N71 C72 C73 C74 -179.2(5) . . . . ? C70 N71 C75 C76 -97.6(8) . . . . ? C72 N71 C75 C76 96.3(7) . . . . ? N71 C75 C76 C77 173.1(4) . . . . ? _database_code_depnum_ccdc_archive 'CCDC 948668'