# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 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_Complex1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18.5 H16 Cl N3 Ni O2 S3' _chemical_formula_weight 502.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 32.8046(13) _cell_length_b 7.5551(7) _cell_length_c 16.8736(14) _cell_angle_alpha 90.000(4) _cell_angle_beta 104.401(3) _cell_angle_gamma 90.000(3) _cell_volume 4050.6(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 27652 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 30.00 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.649 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2056 _exptl_absorpt_coefficient_mu 1.420 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'ABSPACK, Oxford Diffraction Ltd' _exptl_absorpt_correction_T_min 0.884 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_standards_number ? _diffrn_measurement_device 'Oxford Diffaction X-Calibur System' _diffrn_measurement_method '321 frames, counting time 10 s.' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27652 _diffrn_reflns_av_R_equivalents 0.1227 _diffrn_reflns_av_sigmaI/netI 0.1843 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 30.00 _reflns_number_total 11762 _reflns_number_gt 5566 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crysalis, Oxford Diffraction' _computing_cell_refinement 'Crysalis, Oxford Diffraction' _computing_data_reduction 'Crysalis, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics PLATON(Spek,2004) _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 ; _refine_ls_weighting_details w=1/[\s^2^(Fo^2^)+(0.0504P)^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 11762 _refine_ls_number_parameters 516 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1484 _refine_ls_R_factor_gt 0.0658 _refine_ls_wR_factor_ref 0.1484 _refine_ls_wR_factor_gt 0.1271 _refine_ls_goodness_of_fit_ref 0.849 _refine_ls_restrained_S_all 0.849 _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 Ni1 Ni 0.543056(19) 0.89413(8) 0.90983(3) 0.02476(15) Uani 1 1 d . . . Ni2 Ni 0.543510(19) 0.63337(8) 0.65799(3) 0.02318(15) Uani 1 1 d . . . N31A N 0.48475(12) 0.8815(5) 0.8537(2) 0.0252(9) Uani 1 1 d . . . C32A C 0.45348(16) 0.8235(7) 0.8833(3) 0.0329(12) Uani 1 1 d . . . H32A H 0.4599 0.7759 0.9358 0.040 Uiso 1 1 calc R . . C33A C 0.41160(16) 0.8297(7) 0.8403(3) 0.0360(13) Uani 1 1 d . . . H33A H 0.3905 0.7870 0.8633 0.043 Uiso 1 1 calc R . . C34A C 0.40212(15) 0.9006(6) 0.7632(3) 0.0353(12) Uani 1 1 d . . . H34A H 0.3743 0.9084 0.7329 0.042 Uiso 1 1 calc R . . C35A C 0.43477(15) 0.9609(6) 0.7306(3) 0.0283(11) Uani 1 1 d . . . H35A H 0.4291 1.0062 0.6777 0.034 Uiso 1 1 calc R . . C36A C 0.47576(14) 0.9522(6) 0.7780(3) 0.0242(10) Uani 1 1 d . . . C37A C 0.51283(15) 1.0138(6) 0.7520(3) 0.0232(10) Uani 1 1 d . . . C38A C 0.51164(16) 1.0879(6) 0.6766(3) 0.0279(11) Uani 1 1 d . . . H38A H 0.4862 1.0993 0.6377 0.033 Uiso 1 1 calc R . . C39A C 0.54874(17) 1.1455(6) 0.6593(3) 0.0330(12) Uani 1 1 d . . . H39A H 0.5483 1.1966 0.6090 0.040 Uiso 1 1 calc R . . C40A C 0.58625(15) 1.1255(6) 0.7181(3) 0.0293(11) Uani 1 1 d . . . H40A H 0.6116 1.1603 0.7077 0.035 Uiso 1 1 calc R . . C41A C 0.58519(15) 1.0526(6) 0.7926(3) 0.0280(11) Uani 1 1 d . . . H41A H 0.6104 1.0409 0.8323 0.034 Uiso 1 1 calc R . . N42A N 0.54955(12) 0.9974(5) 0.8108(2) 0.0224(8) Uani 1 1 d . . . S11A S 0.54049(4) 0.75621(18) 1.02171(7) 0.0324(3) Uani 1 1 d . . . S12A S 0.60811(4) 0.91223(17) 0.97919(7) 0.0301(3) Uani 1 1 d . . . C13A C 0.59485(15) 0.7755(6) 1.0520(3) 0.0254(10) Uani 1 1 d . . . N14A N 0.61822(12) 0.6948(5) 1.1146(2) 0.0308(10) Uani 1 1 d . . . S15A S 0.66958(4) 0.71840(19) 1.13488(8) 0.0375(3) Uani 1 1 d . . . O16A O 0.68112(12) 0.8955(5) 1.1607(3) 0.0615(12) Uani 1 1 d . . . O17A O 0.68560(12) 0.6480(6) 1.0693(2) 0.0564(12) Uani 1 1 d . . . C21A C 0.68529(14) 0.5775(6) 1.2193(3) 0.0286(11) Uani 1 1 d . . . C22A C 0.69075(15) 0.6420(7) 1.2982(3) 0.0358(13) Uani 1 1 d . . . H22A H 0.6859 0.7608 1.3072 0.043 Uiso 1 1 calc R . . C23A C 0.70356(15) 0.5256(8) 1.3634(3) 0.0409(14) Uani 1 1 d . . . H23A H 0.7066 0.5678 1.4163 0.049 Uiso 1 1 calc R . . C24A C 0.71181(15) 0.3506(8) 1.3522(3) 0.0407(14) Uani 1 1 d . . . C25A C 0.70602(16) 0.2878(7) 1.2728(3) 0.0404(14) Uani 1 1 d . . . H25A H 0.7108 0.1687 1.2642 0.049 Uiso 1 1 calc R . . C26A C 0.69339(15) 0.3992(7) 1.2067(3) 0.0335(12) Uani 1 1 d . . . H26A H 0.6902 0.3562 1.1539 0.040 Uiso 1 1 calc R . . C27A C 0.72853(18) 0.2281(9) 1.4248(4) 0.067(2) Uani 1 1 d . . . H27A H 0.7330 0.2944 1.4747 0.101 Uiso 1 1 calc R . . H27B H 0.7547 0.1770 1.4205 0.101 Uiso 1 1 calc R . . H27C H 0.7085 0.1356 1.4249 0.101 Uiso 1 1 calc R . . S11B S 0.60306(4) 0.70489(17) 0.63425(8) 0.0314(3) Uani 1 1 d . . . S12B S 0.52353(4) 0.73640(17) 0.53395(7) 0.0301(3) Uani 1 1 d . . . C13B C 0.57528(15) 0.7805(6) 0.5385(3) 0.0276(11) Uani 1 1 d . . . N14B N 0.58855(12) 0.8541(5) 0.4796(2) 0.0290(9) Uani 1 1 d . . . S15B S 0.63963(4) 0.87111(17) 0.48665(7) 0.0306(3) Uani 1 1 d . . . O16B O 0.66087(11) 0.7059(4) 0.5113(2) 0.0331(8) Uani 1 1 d . . . O17B O 0.64237(10) 0.9454(5) 0.40984(19) 0.0387(9) Uani 1 1 d . . . C21B C 0.65955(15) 1.0287(6) 0.5632(3) 0.0287(11) Uani 1 1 d . . . C22B C 0.68482(14) 0.9782(6) 0.6392(3) 0.0275(11) Uani 1 1 d . . . H22B H 0.6910 0.8593 0.6505 0.033 Uiso 1 1 calc R . . C23B C 0.70042(15) 1.1038(6) 0.6972(3) 0.0333(12) Uani 1 1 d . . . H23B H 0.7169 1.0690 0.7479 0.040 Uiso 1 1 calc R . . C24B C 0.69214(16) 1.2813(7) 0.6817(3) 0.0347(12) Uani 1 1 d . . . C25B C 0.66698(19) 1.3298(7) 0.6059(4) 0.0458(15) Uani 1 1 d . . . H25B H 0.6609 1.4488 0.5947 0.055 Uiso 1 1 calc R . . C26B C 0.65091(18) 1.2062(7) 0.5473(4) 0.0424(14) Uani 1 1 d . . . H26B H 0.6342 1.2415 0.4968 0.051 Uiso 1 1 calc R . . C27B C 0.70957(18) 1.4183(7) 0.7458(4) 0.0530(16) Uani 1 1 d . . . H27D H 0.6941 1.4156 0.7872 0.080 Uiso 1 1 calc R . . H27E H 0.7070 1.5334 0.7209 0.080 Uiso 1 1 calc R . . H27F H 0.7387 1.3935 0.7701 0.080 Uiso 1 1 calc R . . N31B N 0.56479(12) 0.5556(5) 0.7684(2) 0.0252(9) Uani 1 1 d . . . C32B C 0.60497(15) 0.5625(6) 0.8133(3) 0.0269(11) Uani 1 1 d . . . H32B H 0.6253 0.6131 0.7905 0.032 Uiso 1 1 calc R . . C33B C 0.61695(15) 0.4972(6) 0.8918(3) 0.0310(11) Uani 1 1 d . . . H33B H 0.6448 0.5070 0.9219 0.037 Uiso 1 1 calc R . . C34B C 0.58758(17) 0.4174(6) 0.9255(3) 0.0332(12) Uani 1 1 d . . . H34B H 0.5954 0.3687 0.9777 0.040 Uiso 1 1 calc R . . C35B C 0.54590(16) 0.4108(6) 0.8801(3) 0.0294(11) Uani 1 1 d . . . H35B H 0.5254 0.3584 0.9016 0.035 Uiso 1 1 calc R . . C36B C 0.53554(14) 0.4837(6) 0.8022(3) 0.0217(10) Uani 1 1 d . . . C37B C 0.49245(15) 0.4878(6) 0.7484(3) 0.0230(10) Uani 1 1 d . . . C38B C 0.45711(14) 0.4267(6) 0.7703(3) 0.0266(11) Uani 1 1 d . . . H38B H 0.4593 0.3798 0.8221 0.032 Uiso 1 1 calc R . . C39B C 0.41862(16) 0.4360(6) 0.7144(3) 0.0358(13) Uani 1 1 d . . . H39B H 0.3945 0.3956 0.7281 0.043 Uiso 1 1 calc R . . C40B C 0.41628(15) 0.5057(6) 0.6378(3) 0.0308(11) Uani 1 1 d . . . H40B H 0.3907 0.5124 0.5989 0.037 Uiso 1 1 calc R . . C41B C 0.45299(15) 0.5655(6) 0.6203(3) 0.0273(11) Uani 1 1 d . . . H41B H 0.4514 0.6116 0.5685 0.033 Uiso 1 1 calc R . . N42B N 0.49050(12) 0.5605(4) 0.6738(2) 0.0214(8) Uani 1 1 d . . . C2 C 0.72284(19) -0.0401(7) 0.9620(3) 0.0504(16) Uani 1 1 d . . . H2A H 0.7529 -0.0173 0.9783 0.061 Uiso 1 1 calc R . . H2B H 0.7143 -0.0839 1.0095 0.061 Uiso 1 1 calc R . . Cl1 Cl 0.69615(6) 0.1592(2) 0.92928(12) 0.0698(5) Uani 1 1 d . . . Cl2 Cl 0.71256(6) -0.2024(2) 0.88532(10) 0.0646(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 Ni1 0.0177(3) 0.0358(3) 0.0200(3) 0.0017(3) 0.0034(2) 0.0009(3) Ni2 0.0192(3) 0.0293(3) 0.0212(3) 0.0029(3) 0.0054(2) -0.0013(3) N31A 0.023(2) 0.035(2) 0.022(2) -0.0007(18) 0.0122(17) 0.0011(19) C32A 0.021(3) 0.051(3) 0.027(3) 0.007(2) 0.007(2) 0.001(3) C33A 0.021(3) 0.055(3) 0.032(3) 0.003(3) 0.008(2) -0.006(3) C34A 0.016(2) 0.048(3) 0.038(3) 0.001(3) -0.001(2) -0.001(2) C35A 0.022(3) 0.039(3) 0.022(2) 0.000(2) 0.002(2) -0.002(2) C36A 0.013(2) 0.027(2) 0.028(3) -0.008(2) -0.0024(19) 0.001(2) C37A 0.020(2) 0.024(2) 0.026(2) -0.006(2) 0.007(2) 0.000(2) C38A 0.027(3) 0.032(3) 0.023(2) 0.000(2) 0.002(2) 0.001(2) C39A 0.033(3) 0.041(3) 0.025(3) 0.006(2) 0.007(2) 0.000(3) C40A 0.020(2) 0.038(3) 0.032(3) 0.007(2) 0.008(2) 0.001(2) C41A 0.022(3) 0.035(3) 0.026(3) 0.004(2) 0.003(2) 0.005(2) N42A 0.0124(19) 0.028(2) 0.025(2) -0.0018(17) 0.0017(16) 0.0022(17) S11A 0.0154(6) 0.0575(8) 0.0238(6) 0.0074(6) 0.0038(5) -0.0011(6) S12A 0.0214(6) 0.0438(8) 0.0246(6) 0.0069(6) 0.0049(5) -0.0019(6) C13A 0.019(2) 0.033(3) 0.023(2) -0.002(2) 0.0047(19) 0.004(2) N14A 0.018(2) 0.047(2) 0.028(2) 0.006(2) 0.0072(18) 0.002(2) S15A 0.0180(6) 0.0585(9) 0.0334(7) 0.0137(7) 0.0013(5) -0.0013(7) O16A 0.033(2) 0.052(3) 0.082(3) 0.024(2) -0.018(2) -0.013(2) O17A 0.024(2) 0.113(3) 0.036(2) 0.021(2) 0.0130(17) 0.018(2) C21A 0.016(2) 0.046(3) 0.023(2) 0.001(2) 0.0037(19) 0.003(2) C22A 0.016(2) 0.054(3) 0.036(3) -0.002(3) 0.004(2) 0.004(3) C23A 0.014(2) 0.085(4) 0.024(3) 0.000(3) 0.004(2) -0.004(3) C24A 0.009(2) 0.070(4) 0.042(3) 0.025(3) 0.005(2) 0.000(3) C25A 0.022(3) 0.040(3) 0.058(4) 0.009(3) 0.007(3) -0.002(3) C26A 0.019(2) 0.048(3) 0.032(3) -0.011(3) 0.004(2) -0.006(2) C27A 0.024(3) 0.114(5) 0.064(4) 0.048(4) 0.010(3) -0.002(4) S11B 0.0187(6) 0.0462(7) 0.0293(7) 0.0122(6) 0.0058(5) -0.0008(6) S12B 0.0181(6) 0.0471(8) 0.0251(6) 0.0063(6) 0.0052(5) -0.0044(6) C13B 0.026(3) 0.023(2) 0.031(3) 0.004(2) 0.002(2) -0.001(2) N14B 0.019(2) 0.043(2) 0.025(2) 0.0081(19) 0.0061(17) 0.0033(19) S15B 0.0215(6) 0.0446(8) 0.0267(6) 0.0075(6) 0.0077(5) -0.0001(6) O16B 0.029(2) 0.0346(19) 0.039(2) 0.0018(16) 0.0136(17) 0.0039(17) O17B 0.0177(18) 0.070(2) 0.0282(18) 0.0168(18) 0.0061(15) 0.0003(18) C21B 0.021(3) 0.038(3) 0.028(3) 0.010(2) 0.008(2) -0.003(2) C22B 0.016(2) 0.027(3) 0.038(3) 0.004(2) 0.005(2) 0.002(2) C23B 0.020(3) 0.038(3) 0.042(3) 0.002(3) 0.009(2) -0.004(2) C24B 0.019(3) 0.036(3) 0.050(3) -0.001(3) 0.011(2) -0.001(2) C25B 0.050(4) 0.032(3) 0.059(4) 0.016(3) 0.022(3) 0.015(3) C26B 0.043(4) 0.036(3) 0.051(4) 0.023(3) 0.016(3) 0.014(3) C27B 0.035(4) 0.049(4) 0.071(4) -0.006(3) 0.006(3) -0.004(3) N31B 0.023(2) 0.027(2) 0.024(2) -0.0011(17) 0.0052(17) -0.0013(19) C32B 0.021(3) 0.030(3) 0.031(3) 0.000(2) 0.008(2) -0.004(2) C33B 0.020(3) 0.042(3) 0.026(3) -0.002(2) -0.003(2) -0.004(2) C34B 0.038(3) 0.039(3) 0.023(2) 0.003(2) 0.008(2) 0.004(3) C35B 0.024(3) 0.040(3) 0.024(2) 0.010(2) 0.005(2) 0.001(2) C36B 0.016(2) 0.026(2) 0.024(2) 0.000(2) 0.0081(19) 0.001(2) C37B 0.022(3) 0.025(2) 0.024(2) -0.002(2) 0.010(2) -0.001(2) C38B 0.017(2) 0.044(3) 0.021(2) 0.005(2) 0.0090(19) -0.002(2) C39B 0.022(3) 0.041(3) 0.046(3) 0.007(3) 0.011(2) -0.004(2) C40B 0.017(2) 0.041(3) 0.033(3) 0.004(2) 0.003(2) 0.000(2) C41B 0.021(3) 0.040(3) 0.018(2) 0.003(2) 0.0011(19) -0.003(2) N42B 0.022(2) 0.024(2) 0.0179(19) 0.0013(16) 0.0040(16) 0.0011(17) C2 0.042(4) 0.053(4) 0.058(4) 0.003(3) 0.014(3) -0.003(3) Cl1 0.0439(10) 0.0591(10) 0.0976(14) 0.0148(10) 0.0011(9) -0.0003(8) Cl2 0.0720(13) 0.0656(10) 0.0577(10) -0.0050(9) 0.0189(9) -0.0176(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N42A 1.904(4) . ? Ni1 N31A 1.914(4) . ? Ni1 S12A 2.1680(14) . ? Ni1 S11A 2.1762(13) . ? Ni2 N42B 1.905(4) . ? Ni2 N31B 1.912(4) . ? Ni2 S11B 2.1582(13) . ? Ni2 S12B 2.1758(13) . ? N31A C32A 1.322(6) . ? N31A C36A 1.349(6) . ? C32A C33A 1.385(6) . ? C32A H32A 0.9300 . ? C33A C34A 1.370(7) . ? C33A H33A 0.9300 . ? C34A C35A 1.397(6) . ? C34A H34A 0.9300 . ? C35A C36A 1.385(6) . ? C35A H35A 0.9300 . ? C36A C37A 1.467(6) . ? C37A N42A 1.363(5) . ? C37A C38A 1.381(6) . ? C38A C39A 1.390(6) . ? C38A H38A 0.9300 . ? C39A C40A 1.384(6) . ? C39A H39A 0.9300 . ? C40A C41A 1.381(6) . ? C40A H40A 0.9300 . ? C41A N42A 1.347(6) . ? C41A H41A 0.9300 . ? S11A C13A 1.735(5) . ? S12A C13A 1.741(5) . ? C13A N14A 1.294(5) . ? N14A S15A 1.643(4) . ? S15A O16A 1.429(4) . ? S15A O17A 1.439(4) . ? S15A C21A 1.750(5) . ? C21A C22A 1.386(6) . ? C21A C26A 1.399(6) . ? C22A C23A 1.390(7) . ? C22A H22A 0.9300 . ? C23A C24A 1.372(7) . ? C23A H23A 0.9300 . ? C24A C25A 1.390(7) . ? C24A C27A 1.524(7) . ? C25A C26A 1.377(7) . ? C25A H25A 0.9300 . ? C26A H26A 0.9300 . ? C27A H27A 0.9600 . ? C27A H27B 0.9600 . ? C27A H27C 0.9600 . ? S11B C13B 1.743(5) . ? S12B C13B 1.713(5) . ? C13B N14B 1.303(5) . ? N14B S15B 1.655(4) . ? S15B O17B 1.436(3) . ? S15B O16B 1.439(3) . ? S15B C21B 1.759(5) . ? C21B C26B 1.383(6) . ? C21B C22B 1.396(6) . ? C22B C23B 1.367(6) . ? C22B H22B 0.9300 . ? C23B C24B 1.381(7) . ? C23B H23B 0.9300 . ? C24B C25B 1.388(8) . ? C24B C27B 1.503(7) . ? C25B C26B 1.366(7) . ? C25B H25B 0.9300 . ? C26B H26B 0.9300 . ? C27B H27D 0.9600 . ? C27B H27E 0.9600 . ? C27B H27F 0.9600 . ? N31B C32B 1.348(6) . ? N31B C36B 1.346(5) . ? C32B C33B 1.376(6) . ? C32B H32B 0.9300 . ? C33B C34B 1.373(6) . ? C33B H33B 0.9300 . ? C34B C35B 1.392(7) . ? C34B H34B 0.9300 . ? C35B C36B 1.387(6) . ? C35B H35B 0.9300 . ? C36B C37B 1.478(6) . ? C37B N42B 1.361(5) . ? C37B C38B 1.380(6) . ? C38B C39B 1.377(6) . ? C38B H38B 0.9300 . ? C39B C40B 1.379(6) . ? C39B H39B 0.9300 . ? C40B C41B 1.386(6) . ? C40B H40B 0.9300 . ? C41B N42B 1.334(5) . ? C41B H41B 0.9300 . ? C2 Cl2 1.754(6) . ? C2 Cl1 1.760(6) . ? C2 H2A 0.9700 . ? C2 H2B 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 N42A Ni1 N31A 84.40(15) . . ? N42A Ni1 S12A 97.93(12) . . ? N31A Ni1 S12A 176.99(11) . . ? N42A Ni1 S11A 174.10(12) . . ? N31A Ni1 S11A 98.96(11) . . ? S12A Ni1 S11A 78.89(5) . . ? N42B Ni2 N31B 84.22(16) . . ? N42B Ni2 S11B 176.63(11) . . ? N31B Ni2 S11B 97.47(12) . . ? N42B Ni2 S12B 99.85(11) . . ? N31B Ni2 S12B 175.43(12) . . ? S11B Ni2 S12B 78.57(5) . . ? C32A N31A C36A 118.8(4) . . ? C32A N31A Ni1 127.1(3) . . ? C36A N31A Ni1 113.9(3) . . ? N31A C32A C33A 123.6(5) . . ? N31A C32A H32A 118.2 . . ? C33A C32A H32A 118.2 . . ? C34A C33A C32A 118.1(5) . . ? C34A C33A H33A 120.9 . . ? C32A C33A H33A 120.9 . . ? C33A C34A C35A 119.1(5) . . ? C33A C34A H34A 120.4 . . ? C35A C34A H34A 120.4 . . ? C36A C35A C34A 119.1(5) . . ? C36A C35A H35A 120.4 . . ? C34A C35A H35A 120.4 . . ? N31A C36A C35A 121.2(4) . . ? N31A C36A C37A 114.0(4) . . ? C35A C36A C37A 124.8(4) . . ? N42A C37A C38A 121.7(4) . . ? N42A C37A C36A 113.7(4) . . ? C38A C37A C36A 124.6(4) . . ? C37A C38A C39A 119.6(5) . . ? C37A C38A H38A 120.2 . . ? C39A C38A H38A 120.2 . . ? C40A C39A C38A 119.0(4) . . ? C40A C39A H39A 120.5 . . ? C38A C39A H39A 120.5 . . ? C39A C40A C41A 118.5(4) . . ? C39A C40A H40A 120.8 . . ? C41A C40A H40A 120.8 . . ? N42A C41A C40A 123.4(4) . . ? N42A C41A H41A 118.3 . . ? C40A C41A H41A 118.3 . . ? C41A N42A C37A 117.8(4) . . ? C41A N42A Ni1 128.3(3) . . ? C37A N42A Ni1 113.9(3) . . ? C13A S11A Ni1 87.49(16) . . ? C13A S12A Ni1 87.60(16) . . ? N14A C13A S11A 123.9(4) . . ? N14A C13A S12A 130.9(4) . . ? S11A C13A S12A 105.2(2) . . ? C13A N14A S15A 119.2(3) . . ? O16A S15A O17A 117.5(3) . . ? O16A S15A N14A 110.2(2) . . ? O17A S15A N14A 110.6(2) . . ? O16A S15A C21A 108.6(2) . . ? O17A S15A C21A 108.1(2) . . ? N14A S15A C21A 100.5(2) . . ? C22A C21A C26A 120.0(5) . . ? C22A C21A S15A 120.6(4) . . ? C26A C21A S15A 119.4(4) . . ? C23A C22A C21A 118.6(5) . . ? C23A C22A H22A 120.7 . . ? C21A C22A H22A 120.7 . . ? C24A C23A C22A 122.1(5) . . ? C24A C23A H23A 118.9 . . ? C22A C23A H23A 118.9 . . ? C23A C24A C25A 118.5(5) . . ? C23A C24A C27A 121.3(6) . . ? C25A C24A C27A 120.2(6) . . ? C26A C25A C24A 120.9(5) . . ? C26A C25A H25A 119.5 . . ? C24A C25A H25A 119.5 . . ? C25A C26A C21A 119.7(5) . . ? C25A C26A H26A 120.1 . . ? C21A C26A H26A 120.1 . . ? C24A C27A H27A 109.5 . . ? C24A C27A H27B 109.5 . . ? H27A C27A H27B 109.5 . . ? C24A C27A H27C 109.5 . . ? H27A C27A H27C 109.5 . . ? H27B C27A H27C 109.5 . . ? C13B S11B Ni2 88.03(17) . . ? C13B S12B Ni2 88.21(16) . . ? N14B C13B S12B 124.3(4) . . ? N14B C13B S11B 130.5(4) . . ? S12B C13B S11B 105.1(3) . . ? C13B N14B S15B 120.2(3) . . ? O17B S15B O16B 117.7(2) . . ? O17B S15B N14B 104.80(19) . . ? O16B S15B N14B 111.2(2) . . ? O17B S15B C21B 107.7(2) . . ? O16B S15B C21B 108.1(2) . . ? N14B S15B C21B 106.8(2) . . ? C26B C21B C22B 119.3(5) . . ? C26B C21B S15B 119.5(4) . . ? C22B C21B S15B 121.1(4) . . ? C23B C22B C21B 119.9(4) . . ? C23B C22B H22B 120.1 . . ? C21B C22B H22B 120.1 . . ? C22B C23B C24B 121.2(5) . . ? C22B C23B H23B 119.4 . . ? C24B C23B H23B 119.4 . . ? C23B C24B C25B 118.3(5) . . ? C23B C24B C27B 120.7(5) . . ? C25B C24B C27B 120.9(5) . . ? C26B C25B C24B 121.4(5) . . ? C26B C25B H25B 119.3 . . ? C24B C25B H25B 119.3 . . ? C25B C26B C21B 119.9(5) . . ? C25B C26B H26B 120.1 . . ? C21B C26B H26B 120.1 . . ? C24B C27B H27D 109.5 . . ? C24B C27B H27E 109.5 . . ? H27D C27B H27E 109.5 . . ? C24B C27B H27F 109.5 . . ? H27D C27B H27F 109.5 . . ? H27E C27B H27F 109.5 . . ? C32B N31B C36B 118.5(4) . . ? C32B N31B Ni2 127.2(3) . . ? C36B N31B Ni2 114.3(3) . . ? N31B C32B C33B 122.1(4) . . ? N31B C32B H32B 118.9 . . ? C33B C32B H32B 118.9 . . ? C34B C33B C32B 119.6(5) . . ? C34B C33B H33B 120.2 . . ? C32B C33B H33B 120.2 . . ? C33B C34B C35B 118.8(5) . . ? C33B C34B H34B 120.6 . . ? C35B C34B H34B 120.6 . . ? C36B C35B C34B 118.9(4) . . ? C36B C35B H35B 120.6 . . ? C34B C35B H35B 120.6 . . ? N31B C36B C35B 121.9(4) . . ? N31B C36B C37B 113.9(4) . . ? C35B C36B C37B 124.2(4) . . ? N42B C37B C38B 122.2(4) . . ? N42B C37B C36B 113.2(4) . . ? C38B C37B C36B 124.6(4) . . ? C39B C38B C37B 119.2(4) . . ? C39B C38B H38B 120.4 . . ? C37B C38B H38B 120.4 . . ? C38B C39B C40B 119.3(5) . . ? C38B C39B H39B 120.4 . . ? C40B C39B H39B 120.4 . . ? C39B C40B C41B 118.4(5) . . ? C39B C40B H40B 120.8 . . ? C41B C40B H40B 120.8 . . ? N42B C41B C40B 123.4(4) . . ? N42B C41B H41B 118.3 . . ? C40B C41B H41B 118.3 . . ? C41B N42B C37B 117.5(4) . . ? C41B N42B Ni2 128.1(3) . . ? C37B N42B Ni2 114.3(3) . . ? Cl2 C2 Cl1 112.2(3) . . ? Cl2 C2 H2A 109.2 . . ? Cl1 C2 H2A 109.2 . . ? Cl2 C2 H2B 109.2 . . ? Cl1 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.835 _refine_diff_density_min -0.662 _refine_diff_density_rms 0.125 _database_code_depnum_ccdc_archive 'CCDC 791742' ####################################################################### # # 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_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H15 N3 O2 Pd S3' _chemical_formula_weight 507.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' 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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.1369(5) _cell_length_b 31.497(2) _cell_length_c 15.4964(13) _cell_angle_alpha 90.00 _cell_angle_beta 99.381(6) _cell_angle_gamma 90.00 _cell_volume 3918.5(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 17419 _cell_measurement_theta_min 2.96 _cell_measurement_theta_max 25.00 _exptl_crystal_description bloxk _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.722 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 1.285 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.906 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'ABSPACK, Oxford Diffraction Ltd' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Oxford Diffaction X-Calibur System' _diffrn_measurement_method '321 frames, counting time 10 s.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17419 _diffrn_reflns_av_R_equivalents 0.1067 _diffrn_reflns_av_sigmaI/netI 0.2502 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6463 _reflns_number_gt 2495 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crysalis, Oxford Diffraction' _computing_cell_refinement 'Crysalis, Oxford Diffraction' _computing_data_reduction 'Crysalis, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics PLATON(Spek,2004) _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. some atoms with unreasonable anisotropic thermal parameters were refined using ISOR constraints. ; _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^)+(0.0546P)^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 6463 _refine_ls_number_parameters 489 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.2011 _refine_ls_R_factor_gt 0.0901 _refine_ls_wR_factor_ref 0.1688 _refine_ls_wR_factor_gt 0.1508 _refine_ls_goodness_of_fit_ref 0.919 _refine_ls_restrained_S_all 0.919 _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 Pd1 Pd 0.49828(11) 0.20730(4) 0.51981(7) 0.0399(4) Uani 1 1 d . . . Pd2 Pd 0.86568(12) 0.19525(4) 0.66208(8) 0.0428(4) Uani 1 1 d . . . S11A S 0.5863(4) 0.21305(12) 0.3895(3) 0.0447(10) Uani 1 1 d . . . S12A S 0.5529(4) 0.13951(12) 0.4831(3) 0.0450(10) Uani 1 1 d . . . C13A C 0.6169(14) 0.1592(4) 0.3895(9) 0.037(4) Uani 1 1 d . . . N14A N 0.6834(11) 0.1407(4) 0.3289(7) 0.037(3) Uani 1 1 d . . . S15A S 0.7133(4) 0.08959(13) 0.3236(3) 0.0492(11) Uani 1 1 d . . . O16A O 0.7268(11) 0.0696(3) 0.4065(7) 0.062(3) Uani 1 1 d . . . O17A O 0.8528(10) 0.0843(3) 0.2771(7) 0.068(3) Uani 1 1 d . . . C21A C 0.5309(17) 0.0715(4) 0.2554(10) 0.047(4) Uani 1 1 d . . . C22A C 0.5361(19) 0.0593(4) 0.1725(11) 0.056(4) Uani 1 1 d . . . H22A H 0.6381 0.0588 0.1527 0.067 Uiso 1 1 calc R . . C23A C 0.394(3) 0.0477(5) 0.1163(12) 0.073(5) Uani 1 1 d . . . H23A H 0.3995 0.0406 0.0586 0.087 Uiso 1 1 calc R . . C24A C 0.243(2) 0.0469(5) 0.1465(14) 0.065(5) Uani 1 1 d . . . C25A C 0.2362(19) 0.0595(5) 0.2320(14) 0.073(6) Uani 1 1 d . . . H25A H 0.1347 0.0599 0.2523 0.087 Uiso 1 1 calc R . . C26A C 0.3829(17) 0.0718(5) 0.2877(11) 0.064(5) Uani 1 1 d . . . H26A H 0.3800 0.0799 0.3452 0.077 Uiso 1 1 calc R . . C27A C 0.084(2) 0.0354(5) 0.0893(14) 0.104(7) Uani 1 1 d . . . H27A H 0.0757 0.0051 0.0836 0.156 Uiso 1 1 calc R . . H27B H 0.0805 0.0480 0.0327 0.156 Uiso 1 1 calc R . . H27C H -0.0084 0.0458 0.1150 0.156 Uiso 1 1 calc R . . S11B S 0.7630(4) 0.20613(12) 0.7884(2) 0.0435(10) Uani 1 1 d . . . S12B S 0.8278(5) 0.12913(12) 0.7139(3) 0.0531(11) Uani 1 1 d . . . C13B C 0.7509(14) 0.1509(4) 0.8017(10) 0.044(4) Uani 1 1 d . . . N14B N 0.6891(12) 0.1350(4) 0.8676(8) 0.045(3) Uani 1 1 d . . . S15B S 0.6892(5) 0.08358(14) 0.8833(3) 0.0547(12) Uani 1 1 d . . . O16B O 0.6660(11) 0.0791(3) 0.9727(7) 0.073(3) Uani 1 1 d . . . O17B O 0.8322(10) 0.0641(3) 0.8571(7) 0.068(3) Uani 1 1 d . . . C21B C 0.5069(16) 0.0641(5) 0.8154(12) 0.057(5) Uani 1 1 d . . . C22B C 0.363(2) 0.0630(5) 0.8504(13) 0.073(5) Uani 1 1 d . . . H22B H 0.3610 0.0712 0.9079 0.088 Uiso 1 1 calc R . . C23B C 0.217(2) 0.0489(6) 0.796(2) 0.095(8) Uani 1 1 d . . . H23B H 0.1182 0.0471 0.8180 0.114 Uiso 1 1 calc R . . C24B C 0.217(3) 0.0375(6) 0.709(2) 0.093(7) Uani 1 1 d . . . C25B C 0.367(3) 0.0381(5) 0.6803(14) 0.092(6) Uani 1 1 d . . . H25B H 0.3712 0.0291 0.6236 0.110 Uiso 1 1 calc R . . C26B C 0.512(2) 0.0516(5) 0.7315(13) 0.064(5) Uani 1 1 d . . . H26B H 0.6118 0.0521 0.7094 0.077 Uiso 1 1 calc R . . C27B C 0.056(2) 0.0233(6) 0.6519(16) 0.132(9) Uani 1 1 d . . . H27D H 0.0643 0.0278 0.5915 0.197 Uiso 1 1 calc R . . H27E H -0.0350 0.0395 0.6668 0.197 Uiso 1 1 calc R . . H27F H 0.0383 -0.0063 0.6618 0.197 Uiso 1 1 calc R . . N31A N 0.4662(11) 0.2687(3) 0.5501(7) 0.034(3) Uani 1 1 d U . . C32A C 0.4952(15) 0.3036(4) 0.5123(11) 0.051(4) Uani 1 1 d . . . H32A H 0.5297 0.3000 0.4584 0.061 Uiso 1 1 calc R . . C33A C 0.4847(18) 0.3447(5) 0.5366(13) 0.064(5) Uani 1 1 d . . . H33A H 0.5120 0.3673 0.5029 0.077 Uiso 1 1 calc R . . C34A C 0.4299(19) 0.3503(5) 0.6157(15) 0.073(6) Uani 1 1 d . . . H34A H 0.4173 0.3773 0.6377 0.088 Uiso 1 1 calc R . . C35A C 0.3952(14) 0.3156(6) 0.6601(10) 0.051(5) Uani 1 1 d . . . H35A H 0.3593 0.3196 0.7135 0.061 Uiso 1 1 calc R . . C36A C 0.4094(16) 0.2749(5) 0.6318(11) 0.045(4) Uani 1 1 d U . . C37A C 0.3703(15) 0.2359(5) 0.6708(10) 0.040(4) Uani 1 1 d U . . C38A C 0.3012(16) 0.2366(6) 0.7474(9) 0.049(4) Uani 1 1 d . . . H38A H 0.2823 0.2619 0.7751 0.059 Uiso 1 1 calc R . . C39A C 0.2631(16) 0.1986(7) 0.7793(12) 0.070(5) Uani 1 1 d . . . H39A H 0.2132 0.1981 0.8292 0.084 Uiso 1 1 calc R . . C40A C 0.2944(17) 0.1611(5) 0.7419(11) 0.052(4) Uani 1 1 d U . . H40A H 0.2669 0.1353 0.7650 0.063 Uiso 1 1 calc R . . C41A C 0.3691(15) 0.1630(5) 0.6674(10) 0.047(4) Uani 1 1 d . . . H41A H 0.3956 0.1380 0.6407 0.057 Uiso 1 1 calc R . . N42A N 0.4018(11) 0.1992(4) 0.6354(7) 0.034(3) Uani 1 1 d . . . N31B N 0.9051(12) 0.2557(3) 0.6197(8) 0.038(3) Uani 1 1 d . . . C32B C 0.8769(15) 0.2912(5) 0.6558(10) 0.047(4) Uani 1 1 d U . . H32B H 0.8295 0.2900 0.7064 0.057 Uiso 1 1 calc R . . N42B N 0.9699(11) 0.1821(4) 0.5499(7) 0.040(3) Uani 1 1 d . . . C33B C 0.911(2) 0.3308(5) 0.6256(14) 0.076(6) Uani 1 1 d . . . H33B H 0.8901 0.3557 0.6544 0.092 Uiso 1 1 calc R . . C34B C 0.979(2) 0.3309(6) 0.5493(14) 0.075(6) Uani 1 1 d . . . H34B H 1.0009 0.3570 0.5256 0.089 Uiso 1 1 calc R . . C35B C 1.0145(16) 0.2957(6) 0.5072(10) 0.056(5) Uani 1 1 d . . . H35B H 1.0635 0.2973 0.4571 0.068 Uiso 1 1 calc R . . C36B C 0.9755(15) 0.2565(5) 0.5410(10) 0.046(4) Uani 1 1 d . . . C37B C 1.0096(16) 0.2168(5) 0.5068(10) 0.040(4) Uani 1 1 d U . . C38B C 1.0892(16) 0.2102(6) 0.4274(15) 0.092(7) Uani 1 1 d . . . H38B H 1.1207 0.2330 0.3958 0.110 Uiso 1 1 calc R . . C39B C 1.1133(17) 0.1706(6) 0.4037(11) 0.059(5) Uani 1 1 d U . . H39B H 1.1612 0.1664 0.3538 0.071 Uiso 1 1 calc R . . C40B C 1.0728(15) 0.1359(5) 0.4471(11) 0.055(5) Uani 1 1 d . . . H40B H 1.0904 0.1086 0.4281 0.066 Uiso 1 1 calc R . . C41B C 1.0019(16) 0.1437(6) 0.5231(11) 0.053(4) Uani 1 1 d . . . H41B H 0.9767 0.1206 0.5558 0.064 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 0.0317(6) 0.0560(8) 0.0319(7) -0.0046(6) 0.0048(5) 0.0008(6) Pd2 0.0327(6) 0.0598(9) 0.0361(8) 0.0036(6) 0.0064(5) -0.0024(6) S11A 0.052(2) 0.048(3) 0.036(2) 0.002(2) 0.0143(19) -0.0053(19) S12A 0.044(2) 0.052(3) 0.040(3) 0.003(2) 0.010(2) 0.0035(18) C13A 0.028(8) 0.055(11) 0.027(9) 0.000(8) 0.003(7) -0.009(7) N14A 0.020(6) 0.058(9) 0.030(8) 0.001(6) -0.001(5) 0.008(5) S15A 0.040(2) 0.055(3) 0.053(3) -0.004(2) 0.008(2) 0.0039(19) O16A 0.076(7) 0.071(8) 0.040(7) -0.001(6) 0.013(6) 0.006(6) O17A 0.049(6) 0.086(8) 0.077(9) -0.009(6) 0.036(6) 0.010(5) C21A 0.060(10) 0.035(10) 0.045(11) -0.019(8) 0.007(8) 0.003(7) C22A 0.061(11) 0.051(11) 0.059(12) -0.011(10) 0.020(10) 0.004(8) C23A 0.108(16) 0.055(13) 0.052(13) -0.005(10) 0.003(12) -0.003(11) C24A 0.062(12) 0.045(12) 0.079(16) 0.013(11) -0.013(11) -0.012(9) C25A 0.042(10) 0.068(13) 0.106(18) -0.023(12) 0.005(11) -0.006(9) C26A 0.045(10) 0.080(13) 0.075(14) -0.006(10) 0.034(10) 0.006(8) C27A 0.078(13) 0.078(15) 0.14(2) -0.002(13) -0.038(13) -0.004(10) S11B 0.040(2) 0.055(3) 0.035(2) -0.003(2) 0.0056(17) -0.0003(19) S12B 0.063(2) 0.045(3) 0.057(3) -0.001(2) 0.028(2) 0.002(2) C13B 0.017(7) 0.062(12) 0.046(11) -0.011(9) -0.014(7) 0.004(7) N14B 0.045(7) 0.057(9) 0.037(8) 0.001(7) 0.022(6) 0.003(6) S15B 0.053(3) 0.067(3) 0.048(3) 0.014(2) 0.020(2) 0.005(2) O16B 0.077(7) 0.085(8) 0.062(9) 0.023(7) 0.027(6) 0.005(6) O17B 0.044(6) 0.069(7) 0.094(9) 0.019(7) 0.021(6) 0.008(5) C21B 0.040(9) 0.069(12) 0.070(14) 0.027(10) 0.034(9) 0.010(8) C22B 0.071(12) 0.050(11) 0.110(17) 0.010(11) 0.050(12) 0.008(10) C23B 0.049(13) 0.071(16) 0.17(3) 0.013(17) 0.038(17) -0.007(10) C24B 0.059(14) 0.066(15) 0.15(2) 0.009(16) -0.003(16) -0.006(10) C25B 0.078(14) 0.093(16) 0.105(19) -0.010(13) 0.018(14) 0.003(12) C26B 0.055(11) 0.066(12) 0.076(15) 0.008(11) 0.026(11) 0.000(9) C27B 0.078(14) 0.097(16) 0.20(3) -0.022(16) -0.023(16) -0.005(12) N31A 0.028(4) 0.036(5) 0.033(5) 0.012(4) -0.012(4) -0.005(4) C32A 0.046(8) 0.022(9) 0.074(12) -0.015(9) -0.024(8) 0.002(8) C33A 0.057(10) 0.054(13) 0.078(15) 0.005(11) 0.001(10) 0.004(9) C34A 0.069(12) 0.039(12) 0.111(19) -0.009(13) 0.014(12) 0.004(9) C35A 0.021(8) 0.096(15) 0.037(10) -0.007(10) 0.009(7) 0.010(8) C36A 0.042(5) 0.045(6) 0.048(6) -0.006(5) 0.007(4) 0.008(4) C37A 0.033(5) 0.044(6) 0.038(6) -0.001(4) -0.004(4) 0.000(4) C38A 0.050(9) 0.081(14) 0.019(9) -0.005(9) 0.015(7) -0.001(9) C39A 0.041(9) 0.111(17) 0.056(13) -0.005(13) -0.003(9) 0.018(10) C40A 0.048(6) 0.058(6) 0.051(6) 0.007(5) 0.010(4) 0.003(4) C41A 0.034(8) 0.051(11) 0.047(11) 0.004(9) -0.022(8) 0.007(8) N42A 0.026(6) 0.043(8) 0.031(7) 0.012(7) -0.004(5) 0.004(6) N31B 0.038(7) 0.029(8) 0.038(8) -0.005(6) -0.020(6) 0.010(6) C32B 0.052(5) 0.043(6) 0.045(6) 0.005(5) 0.002(4) -0.002(5) N42B 0.030(6) 0.045(8) 0.041(8) -0.007(7) -0.011(6) -0.012(6) C33B 0.085(13) 0.051(13) 0.082(16) -0.023(12) -0.022(12) 0.006(10) C34B 0.060(12) 0.084(16) 0.065(15) 0.011(13) -0.033(11) -0.006(11) C35B 0.049(9) 0.084(14) 0.043(11) 0.015(11) 0.027(8) 0.001(10) C36B 0.026(8) 0.078(13) 0.027(10) 0.021(10) -0.017(7) -0.018(8) C37B 0.031(5) 0.041(6) 0.044(6) -0.002(5) -0.003(4) -0.001(4) C38B 0.021(8) 0.084(15) 0.17(2) 0.022(15) 0.000(11) -0.018(9) C39B 0.056(6) 0.067(6) 0.056(6) -0.002(5) 0.015(5) 0.002(5) C40B 0.026(8) 0.071(13) 0.063(13) -0.009(11) -0.009(8) 0.003(8) C41B 0.032(8) 0.078(14) 0.041(11) -0.015(10) -0.015(8) -0.004(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N31A 2.017(11) . ? Pd1 N42A 2.085(11) . ? Pd1 S11A 2.257(4) . ? Pd1 S12A 2.272(4) . ? Pd2 N31B 2.055(11) . ? Pd2 N42B 2.096(12) . ? Pd2 S12B 2.271(4) . ? Pd2 S11B 2.276(4) . ? S11A C13A 1.714(14) . ? S12A C13A 1.734(14) . ? C13A N14A 1.294(15) . ? N14A S15A 1.633(11) . ? S15A O16A 1.418(10) . ? S15A O17A 1.450(9) . ? S15A C21A 1.770(14) . ? C21A C22A 1.349(19) . ? C21A C26A 1.377(17) . ? C22A C23A 1.38(2) . ? C22A H22A 0.9300 . ? C23A C24A 1.38(2) . ? C23A H23A 0.9300 . ? C24A C25A 1.39(2) . ? C24A C27A 1.49(2) . ? C25A C26A 1.41(2) . ? C25A H25A 0.9300 . ? C26A H26A 0.9300 . ? C27A H27A 0.9600 . ? C27A H27B 0.9600 . ? C27A H27C 0.9600 . ? S11B C13B 1.758(14) . ? S12B C13B 1.729(15) . ? C13B N14B 1.310(16) . ? N14B S15B 1.637(11) . ? S15B O17B 1.432(9) . ? S15B O16B 1.435(11) . ? S15B C21B 1.781(17) . ? C21B C26B 1.37(2) . ? C21B C22B 1.370(17) . ? C22B C23B 1.41(3) . ? C22B H22B 0.9300 . ? C23B C24B 1.39(3) . ? C23B H23B 0.9300 . ? C24B C25B 1.36(2) . ? C24B C27B 1.52(3) . ? C25B C26B 1.38(2) . ? C25B H25B 0.9300 . ? C26B H26B 0.9300 . ? C27B H27D 0.9600 . ? C27B H27E 0.9600 . ? C27B H27F 0.9600 . ? N31A C32A 1.286(15) . ? N31A C36A 1.431(17) . ? C32A C33A 1.356(17) . ? C32A H32A 0.9300 . ? C33A C34A 1.38(2) . ? C33A H33A 0.9300 . ? C34A C35A 1.345(19) . ? C34A H34A 0.9300 . ? C35A C36A 1.365(18) . ? C35A H35A 0.9300 . ? C36A C37A 1.429(18) . ? C37A N42A 1.323(15) . ? C37A C38A 1.395(18) . ? C38A C39A 1.348(19) . ? C38A H38A 0.9300 . ? C39A C40A 1.359(19) . ? C39A H39A 0.9300 . ? C40A C41A 1.390(18) . ? C40A H40A 0.9300 . ? C41A N42A 1.289(15) . ? C41A H41A 0.9300 . ? N31B C32B 1.289(15) . ? N31B C36B 1.429(16) . ? C32B C33B 1.377(19) . ? C32B H32B 0.9300 . ? N42B C41B 1.318(16) . ? N42B C37B 1.348(16) . ? C33B C34B 1.38(2) . ? C33B H33B 0.9300 . ? C34B C35B 1.34(2) . ? C34B H34B 0.9300 . ? C35B C36B 1.398(18) . ? C35B H35B 0.9300 . ? C36B C37B 1.402(18) . ? C37B C38B 1.50(2) . ? C38B C39B 1.321(19) . ? C38B H38B 0.9300 . ? C39B C40B 1.353(19) . ? C39B H39B 0.9300 . ? C40B C41B 1.414(18) . ? C40B H40B 0.9300 . ? C41B H41B 0.9300 . ? 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 N31A Pd1 N42A 80.6(5) . . ? N31A Pd1 S11A 101.7(3) . . ? N42A Pd1 S11A 175.6(3) . . ? N31A Pd1 S12A 175.8(3) . . ? N42A Pd1 S12A 102.5(4) . . ? S11A Pd1 S12A 75.38(14) . . ? N31B Pd2 N42B 79.2(5) . . ? N31B Pd2 S12B 177.9(3) . . ? N42B Pd2 S12B 102.0(4) . . ? N31B Pd2 S11B 103.5(4) . . ? N42B Pd2 S11B 176.3(4) . . ? S12B Pd2 S11B 75.17(14) . . ? C13A S11A Pd1 89.3(5) . . ? C13A S12A Pd1 88.4(5) . . ? N14A C13A S11A 121.5(11) . . ? N14A C13A S12A 131.6(11) . . ? S11A C13A S12A 106.9(8) . . ? C13A N14A S15A 124.3(10) . . ? O16A S15A O17A 116.6(6) . . ? O16A S15A N14A 112.4(6) . . ? O17A S15A N14A 105.8(6) . . ? O16A S15A C21A 109.4(7) . . ? O17A S15A C21A 108.4(7) . . ? N14A S15A C21A 103.3(6) . . ? C22A C21A C26A 120.9(14) . . ? C22A C21A S15A 120.4(12) . . ? C26A C21A S15A 118.6(12) . . ? C21A C22A C23A 121.6(14) . . ? C21A C22A H22A 119.2 . . ? C23A C22A H22A 119.2 . . ? C22A C23A C24A 119.4(17) . . ? C22A C23A H23A 120.3 . . ? C24A C23A H23A 120.3 . . ? C23A C24A C25A 119.5(16) . . ? C23A C24A C27A 123(2) . . ? C25A C24A C27A 117.8(18) . . ? C24A C25A C26A 119.9(15) . . ? C24A C25A H25A 120.0 . . ? C26A C25A H25A 120.0 . . ? C21A C26A C25A 118.7(16) . . ? C21A C26A H26A 120.7 . . ? C25A C26A H26A 120.7 . . ? C24A C27A H27A 109.5 . . ? C24A C27A H27B 109.5 . . ? H27A C27A H27B 109.5 . . ? C24A C27A H27C 109.5 . . ? H27A C27A H27C 109.5 . . ? H27B C27A H27C 109.5 . . ? C13B S11B Pd2 89.3(5) . . ? C13B S12B Pd2 90.1(5) . . ? N14B C13B S12B 134.2(11) . . ? N14B C13B S11B 120.4(11) . . ? S12B C13B S11B 105.4(8) . . ? C13B N14B S15B 120.2(10) . . ? O17B S15B O16B 118.2(6) . . ? O17B S15B N14B 111.2(5) . . ? O16B S15B N14B 104.1(6) . . ? O17B S15B C21B 108.8(7) . . ? O16B S15B C21B 107.9(7) . . ? N14B S15B C21B 105.8(6) . . ? C26B C21B C22B 122.1(17) . . ? C26B C21B S15B 120.6(12) . . ? C22B C21B S15B 117.3(16) . . ? C21B C22B C23B 117.2(19) . . ? C21B C22B H22B 121.4 . . ? C23B C22B H22B 121.4 . . ? C24B C23B C22B 122.0(19) . . ? C24B C23B H23B 119.0 . . ? C22B C23B H23B 119.0 . . ? C25B C24B C23B 117(2) . . ? C25B C24B C27B 123(3) . . ? C23B C24B C27B 120(2) . . ? C24B C25B C26B 123(2) . . ? C24B C25B H25B 118.4 . . ? C26B C25B H25B 118.4 . . ? C21B C26B C25B 118.6(15) . . ? C21B C26B H26B 120.7 . . ? C25B C26B H26B 120.7 . . ? C24B C27B H27D 109.5 . . ? C24B C27B H27E 109.5 . . ? H27D C27B H27E 109.5 . . ? C24B C27B H27F 109.5 . . ? H27D C27B H27F 109.5 . . ? H27E C27B H27F 109.5 . . ? C32A N31A C36A 113.3(13) . . ? C32A N31A Pd1 132.4(11) . . ? C36A N31A Pd1 114.2(9) . . ? N31A C32A C33A 131.8(17) . . ? N31A C32A H32A 114.1 . . ? C33A C32A H32A 114.1 . . ? C32A C33A C34A 114.2(17) . . ? C32A C33A H33A 122.9 . . ? C34A C33A H33A 122.9 . . ? C35A C34A C33A 118.4(16) . . ? C35A C34A H34A 120.8 . . ? C33A C34A H34A 120.8 . . ? C34A C35A C36A 124.2(16) . . ? C34A C35A H35A 117.9 . . ? C36A C35A H35A 117.9 . . ? C35A C36A N31A 118.0(14) . . ? C35A C36A C37A 129.5(16) . . ? N31A C36A C37A 112.4(14) . . ? N42A C37A C38A 120.0(14) . . ? N42A C37A C36A 120.4(15) . . ? C38A C37A C36A 119.6(15) . . ? C39A C38A C37A 116.5(16) . . ? C39A C38A H38A 121.7 . . ? C37A C38A H38A 121.7 . . ? C38A C39A C40A 123.0(18) . . ? C38A C39A H39A 118.5 . . ? C40A C39A H39A 118.5 . . ? C39A C40A C41A 117.0(16) . . ? C39A C40A H40A 121.5 . . ? C41A C40A H40A 121.5 . . ? N42A C41A C40A 120.2(15) . . ? N42A C41A H41A 119.9 . . ? C40A C41A H41A 119.9 . . ? C41A N42A C37A 123.2(13) . . ? C41A N42A Pd1 124.8(11) . . ? C37A N42A Pd1 112.0(10) . . ? C32B N31B C36B 118.6(13) . . ? C32B N31B Pd2 128.1(11) . . ? C36B N31B Pd2 113.3(9) . . ? N31B C32B C33B 125.5(16) . . ? N31B C32B H32B 117.3 . . ? C33B C32B H32B 117.3 . . ? C41B N42B C37B 120.8(14) . . ? C41B N42B Pd2 124.8(11) . . ? C37B N42B Pd2 114.3(10) . . ? C32B C33B C34B 114.9(17) . . ? C32B C33B H33B 122.6 . . ? C34B C33B H33B 122.6 . . ? C35B C34B C33B 124.3(18) . . ? C35B C34B H34B 117.9 . . ? C33B C34B H34B 117.9 . . ? C34B C35B C36B 117.8(16) . . ? C34B C35B H35B 121.1 . . ? C36B C35B H35B 121.1 . . ? C35B C36B C37B 125.1(17) . . ? C35B C36B N31B 118.9(15) . . ? C37B C36B N31B 115.9(14) . . ? N42B C37B C36B 117.3(15) . . ? N42B C37B C38B 117.7(14) . . ? C36B C37B C38B 125.0(16) . . ? C39B C38B C37B 117.7(17) . . ? C39B C38B H38B 121.2 . . ? C37B C38B H38B 121.2 . . ? C38B C39B C40B 124.3(18) . . ? C38B C39B H39B 117.8 . . ? C40B C39B H39B 117.8 . . ? C39B C40B C41B 116.1(16) . . ? C39B C40B H40B 122.0 . . ? C41B C40B H40B 122.0 . . ? N42B C41B C40B 123.4(16) . . ? N42B C41B H41B 118.3 . . ? C40B C41B H41B 118.3 . . ? _diffrn_measured_fraction_theta_max 0.96 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.96 _refine_diff_density_max 1.266 _refine_diff_density_min -1.789 _refine_diff_density_rms 0.138 _database_code_depnum_ccdc_archive 'CCDC 791743' ####################################################################### # # 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_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H23 N3 O2 Pd S3' _chemical_formula_weight 467.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c 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 12.4574(13) _cell_length_b 15.6410(15) _cell_length_c 9.7801(10) _cell_angle_alpha 90.00 _cell_angle_beta 94.840(10) _cell_angle_gamma 90.00 _cell_volume 1898.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 13839 _cell_measurement_theta_min 3.06 _cell_measurement_theta_max 25.00 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.637 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 1.318 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'ABSPACK, Oxford Diffraction Ltd' _exptl_absorpt_correction_T_min 0.330 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_standards_number ? _diffrn_measurement_device 'Oxford Diffaction X-Calibur System' _diffrn_measurement_method '321 frames, counting time 10 s.' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13839 _diffrn_reflns_av_R_equivalents 0.3291 _diffrn_reflns_av_sigmaI/netI 0.1908 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3321 _reflns_number_gt 2283 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crysalis, Oxford Diffraction' _computing_cell_refinement 'Crysalis, Oxford Diffraction' _computing_data_reduction 'Crysalis, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics PLATON(Spek,2004) _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 ; _refine_ls_weighting_details w=1/[\s^2^(Fo^2^)+(0.2000P)^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 3321 _refine_ls_number_parameters 212 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1595 _refine_ls_R_factor_gt 0.1000 _refine_ls_wR_factor_ref 0.3099 _refine_ls_wR_factor_gt 0.2635 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 Pd1 Pd 0.69405(7) 0.74043(6) 0.14491(8) 0.0276(4) Uani 1 1 d . . . S11 S 0.5806(2) 0.8474(2) 0.1951(3) 0.0371(8) Uani 1 1 d . . . S12 S 0.7900(2) 0.8624(2) 0.1151(3) 0.0347(8) Uani 1 1 d . . . C13 C 0.6854(9) 0.9188(8) 0.1781(11) 0.031(3) Uani 1 1 d . . . N14 N 0.6763(8) 0.9977(7) 0.2132(10) 0.037(2) Uani 1 1 d . . . S15 S 0.7755(3) 1.0652(2) 0.2132(3) 0.0428(9) Uani 1 1 d . . . O16 O 0.8736(8) 1.0289(7) 0.2739(10) 0.060(3) Uani 1 1 d . . . O17 O 0.7359(10) 1.1414(7) 0.2743(11) 0.066(3) Uani 1 1 d . . . C21 C 0.7902(10) 1.0890(7) 0.0411(12) 0.034(3) Uani 1 1 d . . . C22 C 0.8893(10) 1.0783(9) -0.0115(13) 0.046(3) Uani 1 1 d . . . H22 H 0.9459 1.0528 0.0418 0.055 Uiso 1 1 calc R . . C23 C 0.9036(12) 1.1048(10) -0.1407(18) 0.058(4) Uani 1 1 d . . . H23 H 0.9713 1.0984 -0.1728 0.070 Uiso 1 1 calc R . . C24 C 0.8227(10) 1.1409(7) -0.2267(13) 0.036(3) Uani 1 1 d . . . C25 C 0.7224(12) 1.1505(10) -0.1708(16) 0.053(4) Uani 1 1 d . . . H25 H 0.6650 1.1752 -0.2237 0.064 Uiso 1 1 calc R . . C26 C 0.7083(10) 1.1244(9) -0.0416(14) 0.046(3) Uani 1 1 d . . . H26 H 0.6410 1.1307 -0.0082 0.055 Uiso 1 1 calc R . . C27 C 0.8358(14) 1.1719(12) -0.3705(17) 0.071(5) Uani 1 1 d . . . H27C H 0.8132 1.2305 -0.3790 0.107 Uiso 1 1 calc R . . H27A H 0.7925 1.1375 -0.4351 0.107 Uiso 1 1 calc R . . H27B H 0.9101 1.1675 -0.3889 0.107 Uiso 1 1 calc R . . N31 N 0.5945(9) 0.6344(7) 0.1756(11) 0.043(3) Uani 1 1 d . . . C32 C 0.6625(18) 0.5595(11) 0.172(3) 0.111(9) Uani 1 1 d . . . H32B H 0.6896 0.5457 0.2656 0.134 Uiso 1 1 calc R . . H32A H 0.6186 0.5118 0.1374 0.134 Uiso 1 1 calc R . . C33 C 0.749(2) 0.5676(11) 0.094(2) 0.100(8) Uani 1 1 d . . . H33A H 0.7227 0.5614 -0.0019 0.120 Uiso 1 1 calc R . . H33B H 0.7981 0.5206 0.1163 0.120 Uiso 1 1 calc R . . N34 N 0.8114(9) 0.6495(8) 0.1094(10) 0.044(3) Uani 1 1 d . . . C35 C 0.5023(12) 0.6321(12) 0.0735(14) 0.064(5) Uani 1 1 d . . . H35A H 0.5272 0.6290 -0.0166 0.095 Uiso 1 1 calc R . . H35B H 0.4600 0.6829 0.0810 0.095 Uiso 1 1 calc R . . H35C H 0.4590 0.5829 0.0889 0.095 Uiso 1 1 calc R . . C36 C 0.5513(13) 0.6374(12) 0.3115(15) 0.068(5) Uani 1 1 d . . . H36A H 0.5244 0.5820 0.3333 0.103 Uiso 1 1 calc R . . H36B H 0.4939 0.6784 0.3098 0.103 Uiso 1 1 calc R . . H36C H 0.6076 0.6537 0.3796 0.103 Uiso 1 1 calc R . . C37 C 0.8620(15) 0.6620(12) -0.0164(17) 0.072(5) Uani 1 1 d . . . H37A H 0.9059 0.7125 -0.0089 0.109 Uiso 1 1 calc R . . H37B H 0.8076 0.6684 -0.0912 0.109 Uiso 1 1 calc R . . H37C H 0.9062 0.6134 -0.0328 0.109 Uiso 1 1 calc R . . C38 C 0.8928(15) 0.6454(14) 0.2245(19) 0.094(7) Uani 1 1 d . . . H38A H 0.9225 0.5887 0.2310 0.141 Uiso 1 1 calc R . . H38B H 0.8607 0.6589 0.3077 0.141 Uiso 1 1 calc R . . H38C H 0.9491 0.6856 0.2109 0.141 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 0.0295(6) 0.0259(7) 0.0273(6) -0.0002(3) 0.0023(4) -0.0021(4) S11 0.0245(15) 0.040(2) 0.0478(19) 0.0014(14) 0.0106(14) -0.0015(13) S12 0.0249(15) 0.034(2) 0.0465(19) -0.0009(13) 0.0104(14) 0.0010(13) C13 0.040(7) 0.029(8) 0.025(6) 0.002(5) 0.015(5) -0.003(5) N14 0.041(6) 0.034(7) 0.039(6) -0.005(5) 0.013(5) -0.004(5) S15 0.052(2) 0.033(2) 0.0433(19) -0.0040(13) 0.0030(16) -0.0076(15) O16 0.049(6) 0.072(8) 0.054(6) 0.010(5) -0.017(5) -0.017(5) O17 0.098(9) 0.051(7) 0.054(6) -0.014(5) 0.027(6) -0.010(6) C21 0.039(7) 0.022(7) 0.043(7) -0.006(5) 0.010(6) -0.004(5) C22 0.032(7) 0.063(10) 0.042(8) -0.004(6) -0.001(6) 0.012(6) C23 0.040(8) 0.054(10) 0.084(12) -0.016(8) 0.023(8) 0.001(7) C24 0.037(7) 0.018(7) 0.051(8) 0.001(5) 0.001(6) 0.003(5) C25 0.041(8) 0.054(10) 0.065(10) 0.023(7) 0.014(7) 0.011(7) C26 0.026(7) 0.057(10) 0.053(9) 0.005(7) 0.004(6) 0.013(6) C27 0.079(12) 0.068(12) 0.069(11) 0.011(8) 0.022(10) -0.003(9) N31 0.043(6) 0.036(7) 0.050(7) -0.002(5) -0.007(5) -0.012(5) C32 0.095(15) 0.007(9) 0.24(3) 0.001(12) 0.047(18) -0.009(9) C33 0.15(2) 0.026(10) 0.136(19) -0.021(10) 0.079(16) 0.010(11) N34 0.053(7) 0.044(7) 0.035(6) -0.005(4) -0.001(5) 0.013(5) C35 0.063(10) 0.091(14) 0.037(8) -0.019(7) 0.004(7) -0.042(9) C36 0.065(11) 0.096(15) 0.044(9) 0.006(8) 0.002(8) -0.042(10) C37 0.090(13) 0.069(12) 0.064(11) 0.008(8) 0.034(10) 0.032(10) C38 0.075(12) 0.128(19) 0.074(12) -0.004(11) -0.028(10) 0.067(13) _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 N34 2.089(11) . ? Pd1 N31 2.107(11) . ? Pd1 S11 2.270(3) . ? Pd1 S12 2.282(3) . ? S11 C13 1.736(12) . ? S12 C13 1.729(12) . ? C13 N14 1.289(16) . ? N14 S15 1.626(10) . ? S15 O16 1.430(10) . ? S15 O17 1.439(11) . ? S15 C21 1.749(12) . ? C21 C26 1.364(16) . ? C21 C22 1.387(17) . ? C22 C23 1.36(2) . ? C22 H22 0.9300 . ? C23 C24 1.38(2) . ? C23 H23 0.9300 . ? C24 C25 1.414(18) . ? C24 C27 1.510(19) . ? C25 C26 1.35(2) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 H27C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? N31 C32 1.45(2) . ? N31 C35 1.457(17) . ? N31 C36 1.476(18) . ? C32 C33 1.38(3) . ? C32 H32B 0.9700 . ? C32 H32A 0.9700 . ? C33 N34 1.50(2) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? N34 C37 1.442(18) . ? N34 C38 1.451(19) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N34 Pd1 N31 85.2(5) . . ? N34 Pd1 S11 174.0(3) . . ? N31 Pd1 S11 99.5(3) . . ? N34 Pd1 S12 99.6(4) . . ? N31 Pd1 S12 175.2(3) . . ? S11 Pd1 S12 75.75(12) . . ? C13 S11 Pd1 88.1(4) . . ? C13 S12 Pd1 87.8(4) . . ? N14 C13 S12 132.0(9) . . ? N14 C13 S11 120.4(9) . . ? S12 C13 S11 107.5(7) . . ? C13 N14 S15 122.5(9) . . ? O16 S15 O17 117.9(7) . . ? O16 S15 N14 111.4(6) . . ? O17 S15 N14 104.5(6) . . ? O16 S15 C21 109.2(6) . . ? O17 S15 C21 106.9(6) . . ? N14 S15 C21 106.2(5) . . ? C26 C21 C22 118.3(12) . . ? C26 C21 S15 121.5(10) . . ? C22 C21 S15 120.0(10) . . ? C23 C22 C21 119.9(12) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 123.2(13) . . ? C22 C23 H23 118.4 . . ? C24 C23 H23 118.4 . . ? C23 C24 C25 115.6(13) . . ? C23 C24 C27 124.7(13) . . ? C25 C24 C27 119.7(12) . . ? C26 C25 C24 121.1(13) . . ? C26 C25 H25 119.4 . . ? C24 C25 H25 119.4 . . ? C25 C26 C21 121.8(13) . . ? C25 C26 H26 119.1 . . ? C21 C26 H26 119.1 . . ? C24 C27 H27C 109.5 . . ? C24 C27 H27A 109.5 . . ? H27C C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27C C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C32 N31 C35 113.1(14) . . ? C32 N31 C36 107.7(15) . . ? C35 N31 C36 106.9(11) . . ? C32 N31 Pd1 106.4(10) . . ? C35 N31 Pd1 111.2(9) . . ? C36 N31 Pd1 111.6(9) . . ? C33 C32 N31 115.1(16) . . ? C33 C32 H32B 108.5 . . ? N31 C32 H32B 108.5 . . ? C33 C32 H32A 108.5 . . ? N31 C32 H32A 108.5 . . ? H32B C32 H32A 107.5 . . ? C32 C33 N34 116.3(14) . . ? C32 C33 H33A 108.2 . . ? N34 C33 H33A 108.2 . . ? C32 C33 H33B 108.2 . . ? N34 C33 H33B 108.2 . . ? H33A C33 H33B 107.4 . . ? C37 N34 C38 109.9(14) . . ? C37 N34 C33 106.8(12) . . ? C38 N34 C33 111.2(16) . . ? C37 N34 Pd1 114.3(9) . . ? C38 N34 Pd1 110.8(10) . . ? C33 N34 Pd1 103.5(10) . . ? N31 C35 H35A 109.5 . . ? N31 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N31 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N31 C36 H36A 109.5 . . ? N31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N34 C37 H37A 109.5 . . ? N34 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N34 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N34 C38 H38A 109.5 . . ? N34 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N34 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.357 _refine_diff_density_min -1.696 _refine_diff_density_rms 0.316 _database_code_depnum_ccdc_archive 'CCDC 809581'