# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # 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_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H36 N2 P2 Pd2 S2' _chemical_formula_weight 955.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 18.439(4) _cell_length_b 21.149(4) _cell_length_c 20.707(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.02(3) _cell_angle_gamma 90.00 _cell_volume 7996(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3840 _exptl_absorpt_coefficient_mu 1.120 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 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_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24109 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 24.71 _reflns_number_total 13492 _reflns_number_gt 10413 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect(Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo and Scalepack(Otwinowski & Minor1997)' _computing_data_reduction 'Denzo and Scalepack(Otwinowski & Minor1997)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+9.3353P] 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 13492 _refine_ls_number_parameters 973 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.1015 _refine_ls_wR_factor_gt 0.0868 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.002 _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 0.459737(16) 0.384497(14) 0.727624(15) 0.03072(9) Uani 1 1 d . . . P1 P 0.46233(6) 0.32831(5) 0.82290(5) 0.0338(2) Uani 1 1 d . . . S1 S 0.44358(6) 0.45215(5) 0.63696(6) 0.0440(3) Uani 1 1 d . . . N1 N 0.46625(19) 0.30599(16) 0.66201(17) 0.0382(8) Uani 1 1 d . . . C1 C 0.3736(2) 0.4156(2) 0.5856(2) 0.0429(10) Uani 1 1 d . . . Pd2 Pd 0.313367(16) 0.359627(14) 0.710939(16) 0.03351(9) Uani 1 1 d . . . P2 P 0.29854(5) 0.45999(5) 0.74940(5) 0.0331(2) Uani 1 1 d . . . S2 S 0.33972(7) 0.25359(5) 0.68761(6) 0.0493(3) Uani 1 1 d . . . N2 N 0.32085(19) 0.38120(16) 0.60919(17) 0.0403(8) Uani 1 1 d . . . C2 C 0.3705(3) 0.4241(3) 0.5181(2) 0.0644(15) Uani 1 1 d . . . H2A H 0.4066 0.4476 0.5019 0.077 Uiso 1 1 calc R . . Pd3 Pd 0.941189(16) 0.381449(15) 0.790558(16) 0.03304(9) Uani 1 1 d . . . P3 P 0.94609(5) 0.27731(5) 0.75830(5) 0.0350(2) Uani 1 1 d . . . S3 S 0.92577(6) 0.49045(5) 0.80703(6) 0.0442(3) Uani 1 1 d . . . N3 N 0.93451(19) 0.36728(17) 0.89294(17) 0.0402(8) Uani 1 1 d . . . C3 C 0.3154(4) 0.3984(3) 0.4762(3) 0.0791(18) Uani 1 1 d . . . H3A H 0.3133 0.4049 0.4315 0.095 Uiso 1 1 calc R . . Pd4 Pd 0.793202(16) 0.365162(15) 0.773506(16) 0.03305(9) Uani 1 1 d . . . P4 P 0.79352(5) 0.41835(5) 0.67652(5) 0.0347(2) Uani 1 1 d . . . S4 S 0.80686(6) 0.30309(6) 0.86921(6) 0.0459(3) Uani 1 1 d . . . N4 N 0.79209(17) 0.45044(17) 0.83114(17) 0.0391(8) Uani 1 1 d . . . C4 C 0.2630(3) 0.3632(3) 0.4995(3) 0.0688(16) Uani 1 1 d . . . H4A H 0.2250 0.3451 0.4713 0.083 Uiso 1 1 calc R . . C5 C 0.2677(3) 0.3551(2) 0.5652(3) 0.0553(13) Uani 1 1 d . . . H5A H 0.2325 0.3301 0.5809 0.066 Uiso 1 1 calc R . . C6 C 0.4165(2) 0.2596(2) 0.6476(2) 0.0420(10) Uani 1 1 d . . . C7 C 0.4273(3) 0.2140(2) 0.6003(2) 0.0553(13) Uani 1 1 d . . . H7A H 0.3933 0.1818 0.5906 0.066 Uiso 1 1 calc R . . C8 C 0.4872(3) 0.2168(3) 0.5689(2) 0.0620(15) Uani 1 1 d . . . H8A H 0.4940 0.1866 0.5377 0.074 Uiso 1 1 calc R . . C9 C 0.5375(3) 0.2644(3) 0.5835(3) 0.0606(14) Uani 1 1 d . . . H9A H 0.5790 0.2668 0.5627 0.073 Uiso 1 1 calc R . . C10 C 0.5249(3) 0.3083(2) 0.6296(2) 0.0496(12) Uani 1 1 d . . . H10A H 0.5584 0.3411 0.6389 0.060 Uiso 1 1 calc R . . C11 C 0.3718(2) 0.3234(2) 0.8484(2) 0.0387(10) Uani 1 1 d . . . C12 C 0.3090(2) 0.33221(19) 0.8029(2) 0.0359(9) Uani 1 1 d . . . C13 C 0.2410(2) 0.3200(2) 0.8233(2) 0.0502(12) Uani 1 1 d . . . H13A H 0.1985 0.3249 0.7938 0.060 Uiso 1 1 calc R . . C14 C 0.2358(3) 0.3009(3) 0.8863(3) 0.0602(14) Uani 1 1 d . . . H14A H 0.1900 0.2920 0.8981 0.072 Uiso 1 1 calc R . . C15 C 0.2969(3) 0.2949(3) 0.9314(3) 0.0620(14) Uani 1 1 d . . . H15A H 0.2927 0.2840 0.9742 0.074 Uiso 1 1 calc R . . C16 C 0.3648(3) 0.3053(2) 0.9127(2) 0.0523(12) Uani 1 1 d . . . H16A H 0.4066 0.3002 0.9430 0.063 Uiso 1 1 calc R . . C21 C 0.4922(2) 0.2466(2) 0.8189(2) 0.0394(10) Uani 1 1 d . . . C22 C 0.4643(2) 0.1963(2) 0.8500(3) 0.0516(12) Uani 1 1 d . . . H22A H 0.4241 0.2025 0.8719 0.062 Uiso 1 1 calc R . . C23 C 0.4955(3) 0.1367(2) 0.8491(3) 0.0593(14) Uani 1 1 d . . . H23A H 0.4767 0.1034 0.8711 0.071 Uiso 1 1 calc R . . C24 C 0.5537(3) 0.1264(2) 0.8163(3) 0.0639(15) Uani 1 1 d . . . H24A H 0.5741 0.0863 0.8154 0.077 Uiso 1 1 calc R . . C25 C 0.5822(3) 0.1762(2) 0.7843(3) 0.0588(13) Uani 1 1 d . . . H25A H 0.6219 0.1695 0.7619 0.071 Uiso 1 1 calc R . . C26 C 0.5519(3) 0.2356(2) 0.7858(2) 0.0494(12) Uani 1 1 d . . . H26A H 0.5715 0.2688 0.7645 0.059 Uiso 1 1 calc R . . C31 C 0.5240(2) 0.35677(19) 0.8948(2) 0.0339(9) Uani 1 1 d . . . C32 C 0.5920(2) 0.3304(2) 0.9124(2) 0.0492(12) Uani 1 1 d . . . H32A H 0.6062 0.2963 0.8887 0.059 Uiso 1 1 calc R . . C33 C 0.6401(3) 0.3536(3) 0.9647(3) 0.0598(14) Uani 1 1 d . . . H33A H 0.6857 0.3346 0.9757 0.072 Uiso 1 1 calc R . . C34 C 0.6215(3) 0.4031(2) 0.9996(2) 0.0546(12) Uani 1 1 d . . . H34A H 0.6540 0.4187 1.0344 0.066 Uiso 1 1 calc R . . C35 C 0.5542(3) 0.4302(2) 0.9833(3) 0.0608(14) Uani 1 1 d . . . H35A H 0.5408 0.4642 1.0076 0.073 Uiso 1 1 calc R . . C36 C 0.5057(3) 0.4080(2) 0.9312(2) 0.0506(12) Uani 1 1 d . . . H36A H 0.4604 0.4275 0.9205 0.061 Uiso 1 1 calc R . . C41 C 0.3861(2) 0.49177(19) 0.7876(2) 0.0338(9) Uani 1 1 d . . . C42 C 0.4523(2) 0.46354(19) 0.77898(19) 0.0328(9) Uani 1 1 d . . . C43 C 0.5172(2) 0.4952(2) 0.8037(2) 0.0419(10) Uani 1 1 d . . . H43A H 0.5620 0.4775 0.7976 0.050 Uiso 1 1 calc R . . C44 C 0.5166(2) 0.5514(2) 0.8365(2) 0.0478(11) Uani 1 1 d . . . H44A H 0.5605 0.5718 0.8513 0.057 Uiso 1 1 calc R . . C45 C 0.4513(2) 0.5778(2) 0.8476(2) 0.0472(11) Uani 1 1 d . . . H45A H 0.4508 0.6155 0.8707 0.057 Uiso 1 1 calc R . . C46 C 0.3866(2) 0.5477(2) 0.8242(2) 0.0405(10) Uani 1 1 d . . . H46A H 0.3424 0.5647 0.8327 0.049 Uiso 1 1 calc R . . C51 C 0.2585(2) 0.5163(2) 0.6880(2) 0.0382(10) Uani 1 1 d . . . C52 C 0.2153(3) 0.4933(3) 0.6324(2) 0.0566(13) Uani 1 1 d . . . H52A H 0.2100 0.4498 0.6264 0.068 Uiso 1 1 calc R . . C53 C 0.1806(3) 0.5334(3) 0.5867(3) 0.0696(16) Uani 1 1 d . . . H53A H 0.1527 0.5170 0.5496 0.084 Uiso 1 1 calc R . . C54 C 0.1863(3) 0.5974(3) 0.5948(3) 0.0740(18) Uani 1 1 d . . . H54A H 0.1627 0.6246 0.5633 0.089 Uiso 1 1 calc R . . C55 C 0.2267(3) 0.6209(3) 0.6492(3) 0.0743(18) Uani 1 1 d . . . H55A H 0.2302 0.6644 0.6552 0.089 Uiso 1 1 calc R . . C56 C 0.2628(3) 0.5808(2) 0.6960(3) 0.0625(15) Uani 1 1 d . . . H56A H 0.2902 0.5977 0.7331 0.075 Uiso 1 1 calc R . . C61 C 0.2396(2) 0.4732(2) 0.8127(2) 0.0395(10) Uani 1 1 d . . . C62 C 0.1681(2) 0.4928(2) 0.7974(3) 0.0550(13) Uani 1 1 d . . . H62A H 0.1486 0.4993 0.7541 0.066 Uiso 1 1 calc R . . C63 C 0.1248(3) 0.5028(3) 0.8462(4) 0.0781(19) Uani 1 1 d . . . H63A H 0.0764 0.5157 0.8355 0.094 Uiso 1 1 calc R . . C64 C 0.1530(4) 0.4937(3) 0.9090(4) 0.083(2) Uani 1 1 d . . . H64A H 0.1239 0.5012 0.9414 0.100 Uiso 1 1 calc R . . C65 C 0.2234(3) 0.4737(3) 0.9261(3) 0.0706(16) Uani 1 1 d . . . H65A H 0.2421 0.4674 0.9697 0.085 Uiso 1 1 calc R . . C66 C 0.2664(3) 0.4628(2) 0.8778(2) 0.0567(13) Uani 1 1 d . . . H66A H 0.3141 0.4483 0.8891 0.068 Uiso 1 1 calc R . . C67 C 0.8425(2) 0.4973(2) 0.8374(2) 0.0404(10) Uani 1 1 d . . . C68 C 0.8279(3) 0.5546(2) 0.8668(2) 0.0534(12) Uani 1 1 d . . . H68A H 0.8619 0.5873 0.8692 0.064 Uiso 1 1 calc R . . C69 C 0.7636(3) 0.5627(3) 0.8922(3) 0.0643(15) Uani 1 1 d . . . H69A H 0.7532 0.6010 0.9110 0.077 Uiso 1 1 calc R . . C70 C 0.7141(3) 0.5129(3) 0.8894(3) 0.0581(13) Uani 1 1 d . . . H70A H 0.6711 0.5163 0.9079 0.070 Uiso 1 1 calc R . . C71 C 0.7306(2) 0.4590(2) 0.8587(2) 0.0476(11) Uani 1 1 d . . . H71A H 0.6972 0.4258 0.8565 0.057 Uiso 1 1 calc R . . C72 C 0.8788(2) 0.3398(2) 0.9187(2) 0.0423(10) Uani 1 1 d . . . C73 C 0.8802(3) 0.3396(3) 0.9865(2) 0.0594(13) Uani 1 1 d . . . H73A H 0.8424 0.3200 1.0043 0.071 Uiso 1 1 calc R . . C74 C 0.9354(3) 0.3672(3) 1.0267(3) 0.0680(16) Uani 1 1 d . . . H74A H 0.9356 0.3665 1.0716 0.082 Uiso 1 1 calc R . . C75 C 0.9913(3) 0.3962(3) 1.0002(3) 0.0641(14) Uani 1 1 d . . . H75A H 1.0297 0.4160 1.0266 0.077 Uiso 1 1 calc R . . C76 C 0.9885(3) 0.3950(2) 0.9341(3) 0.0552(13) Uani 1 1 d . . . H76A H 1.0262 0.4146 0.9161 0.066 Uiso 1 1 calc R . . C77 C 0.9470(2) 0.4051(2) 0.6978(2) 0.0364(9) Uani 1 1 d . . . C78 C 0.8852(2) 0.41955(19) 0.6527(2) 0.0337(9) Uani 1 1 d . . . C79 C 0.8944(2) 0.4370(2) 0.5893(2) 0.0437(11) Uani 1 1 d . . . H79A H 0.8531 0.4456 0.5594 0.052 Uiso 1 1 calc R . . C80 C 0.9620(2) 0.4418(2) 0.5695(2) 0.0479(11) Uani 1 1 d . . . H80A H 0.9667 0.4534 0.5270 0.057 Uiso 1 1 calc R . . C81 C 1.0233(2) 0.4288(2) 0.6145(2) 0.0512(12) Uani 1 1 d . . . H81A H 1.0698 0.4319 0.6022 0.061 Uiso 1 1 calc R . . C82 C 1.0155(2) 0.4114(2) 0.6773(2) 0.0437(11) Uani 1 1 d . . . H82A H 1.0573 0.4036 0.7069 0.052 Uiso 1 1 calc R . . C83 C 1.0081(2) 0.25967(19) 0.6985(2) 0.0382(10) Uani 1 1 d . . . C84 C 0.9863(3) 0.2691(2) 0.6326(2) 0.0515(12) Uani 1 1 d . . . H84A H 0.9386 0.2820 0.6182 0.062 Uiso 1 1 calc R . . C85 C 1.0340(3) 0.2597(3) 0.5876(3) 0.0605(14) Uani 1 1 d . . . H85A H 1.0188 0.2663 0.5434 0.073 Uiso 1 1 calc R . . C86 C 1.1046(3) 0.2404(3) 0.6095(3) 0.0655(15) Uani 1 1 d . . . H86A H 1.1372 0.2340 0.5797 0.079 Uiso 1 1 calc R . . C87 C 1.1272(3) 0.2307(3) 0.6734(3) 0.0675(16) Uani 1 1 d . . . H87A H 1.1749 0.2173 0.6871 0.081 Uiso 1 1 calc R . . C88 C 1.0798(2) 0.2404(2) 0.7188(2) 0.0522(12) Uani 1 1 d . . . H88A H 1.0960 0.2340 0.7629 0.063 Uiso 1 1 calc R . . C89 C 0.9787(2) 0.2208(2) 0.8231(2) 0.0443(11) Uani 1 1 d . . . C90 C 1.0306(2) 0.2420(3) 0.8732(2) 0.0522(12) Uani 1 1 d . . . H90A H 1.0435 0.2845 0.8753 0.063 Uiso 1 1 calc R . . C91 C 1.0634(3) 0.2005(3) 0.9201(3) 0.0650(15) Uani 1 1 d . . . H91A H 1.0987 0.2151 0.9533 0.078 Uiso 1 1 calc R . . C92 C 1.0439(3) 0.1379(3) 0.9178(3) 0.078(2) Uani 1 1 d . . . H92A H 1.0661 0.1100 0.9492 0.093 Uiso 1 1 calc R . . C93 C 0.9918(3) 0.1163(3) 0.8694(4) 0.085(2) Uani 1 1 d . . . H93A H 0.9785 0.0739 0.8681 0.102 Uiso 1 1 calc R . . C94 C 0.9586(3) 0.1580(3) 0.8218(3) 0.0664(16) Uani 1 1 d . . . H94A H 0.9228 0.1433 0.7891 0.080 Uiso 1 1 calc R . . C95 C 0.7937(2) 0.28323(19) 0.7242(2) 0.0355(9) Uani 1 1 d . . . C96 C 0.8568(2) 0.24923(19) 0.7183(2) 0.0356(9) Uani 1 1 d . . . C97 C 0.8529(2) 0.1930(2) 0.6826(2) 0.0468(11) Uani 1 1 d . . . H97A H 0.8957 0.1710 0.6783 0.056 Uiso 1 1 calc R . . C98 C 0.7857(3) 0.1696(2) 0.6536(2) 0.0526(12) Uani 1 1 d . . . H98A H 0.7833 0.1322 0.6298 0.063 Uiso 1 1 calc R . . C99 C 0.7231(2) 0.2022(2) 0.6602(2) 0.0485(12) Uani 1 1 d . . . H99A H 0.6779 0.1865 0.6414 0.058 Uiso 1 1 calc R . . C100 C 0.7264(2) 0.2583(2) 0.6946(2) 0.0448(11) Uani 1 1 d . . . H10B H 0.6834 0.2801 0.6984 0.054 Uiso 1 1 calc R . . C101 C 0.7371(2) 0.3903(2) 0.6017(2) 0.0409(10) Uani 1 1 d . . . C102 C 0.7592(3) 0.3372(2) 0.5701(2) 0.0493(11) Uani 1 1 d . . . H10C H 0.8009 0.3154 0.5883 0.059 Uiso 1 1 calc R . . C103 C 0.7205(3) 0.3164(3) 0.5125(2) 0.0592(13) Uani 1 1 d . . . H10D H 0.7365 0.2810 0.4920 0.071 Uiso 1 1 calc R . . C104 C 0.6592(3) 0.3472(3) 0.4853(3) 0.0776(18) Uani 1 1 d . . . H10E H 0.6333 0.3330 0.4462 0.093 Uiso 1 1 calc R . . C105 C 0.6359(3) 0.3989(3) 0.5156(3) 0.087(2) Uani 1 1 d . . . H10F H 0.5936 0.4197 0.4971 0.105 Uiso 1 1 calc R . . C106 C 0.6745(3) 0.4211(3) 0.5738(3) 0.0662(16) Uani 1 1 d . . . H10G H 0.6581 0.4567 0.5939 0.079 Uiso 1 1 calc R . . C107 C 0.7679(2) 0.5017(2) 0.6834(2) 0.0380(10) Uani 1 1 d . . . C108 C 0.8134(3) 0.5510(2) 0.6710(2) 0.0463(11) Uani 1 1 d . . . H10H H 0.8576 0.5425 0.6560 0.056 Uiso 1 1 calc R . . C109 C 0.7932(3) 0.6130(2) 0.6809(3) 0.0548(13) Uani 1 1 d . . . H10I H 0.8239 0.6460 0.6725 0.066 Uiso 1 1 calc R . . C110 C 0.7279(3) 0.6258(3) 0.7031(3) 0.0639(15) Uani 1 1 d . . . H11A H 0.7144 0.6676 0.7092 0.077 Uiso 1 1 calc R . . C111 C 0.6826(3) 0.5779(3) 0.7161(2) 0.0621(15) Uani 1 1 d . . . H11B H 0.6386 0.5870 0.7313 0.074 Uiso 1 1 calc R . . C112 C 0.7023(2) 0.5156(2) 0.7067(2) 0.0503(12) Uani 1 1 d . . . H11C H 0.6716 0.4830 0.7160 0.060 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 0.03363(17) 0.02946(17) 0.02876(18) 0.00017(12) 0.00327(12) 0.00087(12) P1 0.0361(6) 0.0335(6) 0.0311(6) 0.0045(4) 0.0023(4) 0.0023(4) S1 0.0586(7) 0.0368(6) 0.0350(6) 0.0046(5) 0.0011(5) -0.0066(5) N1 0.048(2) 0.0350(19) 0.030(2) 0.0000(15) 0.0032(16) 0.0051(17) C1 0.060(3) 0.034(2) 0.033(3) 0.0004(19) 0.002(2) 0.003(2) Pd2 0.03512(17) 0.03123(17) 0.03269(19) 0.00031(13) -0.00048(13) -0.00279(13) P2 0.0326(5) 0.0328(6) 0.0328(6) -0.0005(4) 0.0009(4) 0.0008(4) S2 0.0584(7) 0.0310(6) 0.0581(8) -0.0012(5) 0.0066(6) -0.0053(5) N2 0.051(2) 0.0351(19) 0.032(2) -0.0016(15) -0.0039(16) -0.0024(16) C2 0.082(4) 0.074(4) 0.035(3) 0.010(3) 0.001(3) -0.017(3) Pd3 0.02985(16) 0.03717(18) 0.03133(19) 0.00317(13) 0.00158(13) -0.00073(13) P3 0.0312(5) 0.0372(6) 0.0359(6) 0.0035(5) 0.0026(4) 0.0009(5) S3 0.0404(6) 0.0384(6) 0.0529(8) 0.0015(5) 0.0039(5) -0.0019(5) N3 0.043(2) 0.044(2) 0.033(2) 0.0062(16) 0.0006(16) 0.0041(17) C3 0.105(5) 0.094(5) 0.032(3) -0.002(3) -0.012(3) -0.020(4) Pd4 0.02935(16) 0.03560(18) 0.03435(19) 0.00499(13) 0.00500(13) -0.00002(13) P4 0.0313(5) 0.0388(6) 0.0335(6) 0.0061(5) 0.0022(4) 0.0001(5) S4 0.0525(7) 0.0440(6) 0.0423(7) 0.0101(5) 0.0099(5) -0.0039(5) N4 0.0343(18) 0.047(2) 0.036(2) 0.0060(16) 0.0045(15) 0.0036(16) C4 0.085(4) 0.076(4) 0.040(3) -0.008(3) -0.014(3) -0.015(3) C5 0.067(3) 0.045(3) 0.048(3) -0.003(2) -0.014(2) -0.009(2) C6 0.058(3) 0.033(2) 0.033(3) 0.0020(18) -0.003(2) 0.009(2) C7 0.072(3) 0.043(3) 0.046(3) -0.006(2) -0.007(3) 0.010(2) C8 0.087(4) 0.057(3) 0.040(3) -0.009(2) 0.002(3) 0.028(3) C9 0.075(3) 0.063(3) 0.046(3) 0.003(3) 0.016(3) 0.024(3) C10 0.058(3) 0.049(3) 0.042(3) 0.003(2) 0.007(2) 0.012(2) C11 0.039(2) 0.042(2) 0.035(2) 0.0078(19) 0.0064(18) -0.0010(19) C12 0.038(2) 0.035(2) 0.036(2) 0.0015(18) 0.0078(18) -0.0073(18) C13 0.041(2) 0.054(3) 0.054(3) 0.006(2) 0.002(2) -0.008(2) C14 0.048(3) 0.073(4) 0.063(4) 0.013(3) 0.019(3) -0.012(3) C15 0.063(3) 0.078(4) 0.049(3) 0.021(3) 0.020(3) -0.011(3) C16 0.051(3) 0.064(3) 0.041(3) 0.015(2) 0.005(2) -0.003(2) C21 0.044(2) 0.035(2) 0.037(3) 0.0023(19) -0.0038(19) 0.0006(19) C22 0.045(3) 0.041(3) 0.067(4) 0.005(2) 0.001(2) -0.004(2) C23 0.066(3) 0.033(3) 0.074(4) 0.009(2) -0.011(3) -0.009(2) C24 0.081(4) 0.034(3) 0.072(4) -0.002(3) -0.008(3) 0.014(3) C25 0.077(4) 0.047(3) 0.053(3) -0.001(2) 0.011(3) 0.017(3) C26 0.065(3) 0.041(3) 0.042(3) 0.000(2) 0.008(2) 0.010(2) C31 0.037(2) 0.034(2) 0.030(2) 0.0069(17) 0.0035(17) -0.0002(18) C32 0.044(3) 0.055(3) 0.047(3) -0.010(2) 0.000(2) 0.005(2) C33 0.041(3) 0.072(4) 0.062(4) -0.005(3) -0.006(2) 0.006(2) C34 0.058(3) 0.059(3) 0.044(3) -0.003(2) -0.006(2) -0.004(3) C35 0.078(4) 0.052(3) 0.047(3) -0.012(2) -0.007(3) 0.011(3) C36 0.058(3) 0.045(3) 0.046(3) -0.002(2) -0.004(2) 0.014(2) C41 0.035(2) 0.033(2) 0.031(2) 0.0019(17) -0.0002(17) 0.0001(17) C42 0.037(2) 0.036(2) 0.025(2) 0.0000(17) 0.0002(16) -0.0016(18) C43 0.036(2) 0.044(3) 0.044(3) -0.001(2) -0.0003(19) -0.0024(19) C44 0.045(3) 0.044(3) 0.051(3) -0.008(2) -0.007(2) -0.012(2) C45 0.061(3) 0.038(2) 0.041(3) -0.011(2) -0.001(2) -0.004(2) C46 0.045(2) 0.037(2) 0.039(3) -0.0081(19) 0.0019(19) 0.0033(19) C51 0.033(2) 0.042(2) 0.040(3) 0.0054(19) 0.0035(18) 0.0002(18) C52 0.058(3) 0.061(3) 0.047(3) 0.001(2) -0.007(2) 0.010(2) C53 0.069(3) 0.085(4) 0.051(4) 0.023(3) -0.007(3) 0.012(3) C54 0.060(3) 0.085(5) 0.074(4) 0.044(4) 0.002(3) 0.011(3) C55 0.074(4) 0.045(3) 0.099(5) 0.027(3) -0.006(3) -0.003(3) C56 0.063(3) 0.043(3) 0.075(4) 0.011(3) -0.012(3) -0.007(2) C61 0.041(2) 0.037(2) 0.043(3) -0.0044(19) 0.0130(19) -0.0050(19) C62 0.036(2) 0.060(3) 0.069(4) -0.009(3) 0.009(2) -0.007(2) C63 0.042(3) 0.083(4) 0.114(6) -0.012(4) 0.027(3) -0.008(3) C64 0.091(5) 0.080(4) 0.091(5) -0.023(4) 0.056(4) -0.027(4) C65 0.085(4) 0.082(4) 0.050(4) -0.006(3) 0.029(3) -0.009(3) C66 0.064(3) 0.065(3) 0.043(3) -0.003(2) 0.015(2) 0.000(3) C67 0.047(2) 0.044(3) 0.029(2) 0.0056(19) -0.0016(18) 0.006(2) C68 0.059(3) 0.047(3) 0.052(3) -0.005(2) 0.002(2) 0.003(2) C69 0.070(3) 0.066(4) 0.057(4) -0.014(3) 0.009(3) 0.018(3) C70 0.052(3) 0.074(4) 0.050(3) -0.005(3) 0.013(2) 0.013(3) C71 0.047(3) 0.057(3) 0.040(3) 0.008(2) 0.008(2) 0.004(2) C72 0.053(3) 0.039(2) 0.035(3) 0.0063(19) 0.006(2) 0.009(2) C73 0.073(3) 0.066(3) 0.041(3) 0.013(3) 0.013(3) 0.003(3) C74 0.093(4) 0.083(4) 0.027(3) 0.004(3) 0.004(3) 0.005(3) C75 0.080(4) 0.066(3) 0.040(3) -0.001(3) -0.013(3) -0.005(3) C76 0.051(3) 0.055(3) 0.057(3) 0.002(2) -0.005(2) -0.001(2) C77 0.035(2) 0.039(2) 0.035(2) 0.0002(19) 0.0039(17) -0.0026(18) C78 0.036(2) 0.035(2) 0.031(2) 0.0036(18) 0.0060(17) -0.0011(18) C79 0.044(2) 0.049(3) 0.036(3) 0.006(2) 0.0018(19) -0.001(2) C80 0.053(3) 0.057(3) 0.038(3) 0.006(2) 0.019(2) -0.008(2) C81 0.043(3) 0.057(3) 0.056(3) 0.003(2) 0.016(2) -0.009(2) C82 0.031(2) 0.051(3) 0.049(3) 0.003(2) 0.0046(19) -0.001(2) C83 0.035(2) 0.036(2) 0.044(3) -0.0006(19) 0.0062(18) 0.0004(18) C84 0.049(3) 0.059(3) 0.047(3) 0.003(2) 0.009(2) 0.001(2) C85 0.071(4) 0.072(4) 0.042(3) -0.006(3) 0.021(3) -0.009(3) C86 0.063(3) 0.072(4) 0.069(4) -0.010(3) 0.036(3) -0.011(3) C87 0.049(3) 0.087(4) 0.071(4) -0.001(3) 0.022(3) 0.008(3) C88 0.048(3) 0.066(3) 0.044(3) 0.000(2) 0.011(2) 0.003(2) C89 0.037(2) 0.050(3) 0.047(3) 0.016(2) 0.011(2) 0.005(2) C90 0.050(3) 0.061(3) 0.046(3) 0.007(2) 0.005(2) 0.016(2) C91 0.058(3) 0.095(5) 0.041(3) 0.014(3) 0.006(2) 0.027(3) C92 0.062(4) 0.094(5) 0.080(5) 0.053(4) 0.019(3) 0.021(3) C93 0.077(4) 0.063(4) 0.114(6) 0.045(4) 0.007(4) -0.004(3) C94 0.052(3) 0.062(3) 0.082(4) 0.025(3) -0.003(3) -0.007(3) C95 0.037(2) 0.039(2) 0.030(2) 0.0066(18) 0.0029(17) -0.0019(18) C96 0.036(2) 0.038(2) 0.033(2) 0.0051(18) 0.0050(17) -0.0007(18) C97 0.047(3) 0.041(3) 0.053(3) 0.000(2) 0.007(2) -0.001(2) C98 0.059(3) 0.041(3) 0.058(3) -0.003(2) 0.007(2) -0.009(2) C99 0.042(2) 0.046(3) 0.055(3) 0.003(2) -0.004(2) -0.015(2) C100 0.034(2) 0.045(3) 0.054(3) 0.008(2) 0.004(2) -0.001(2) C101 0.034(2) 0.049(3) 0.037(3) 0.011(2) -0.0005(18) -0.008(2) C102 0.051(3) 0.051(3) 0.045(3) 0.000(2) 0.003(2) -0.003(2) C103 0.073(3) 0.057(3) 0.046(3) -0.006(2) 0.001(3) -0.017(3) C104 0.082(4) 0.081(4) 0.060(4) 0.003(3) -0.027(3) -0.020(3) C105 0.079(4) 0.076(4) 0.090(5) 0.001(4) -0.046(4) 0.009(3) C106 0.054(3) 0.059(3) 0.078(4) 0.004(3) -0.020(3) 0.005(3) C107 0.039(2) 0.044(2) 0.030(2) 0.0072(19) -0.0012(17) 0.0055(19) C108 0.052(3) 0.043(3) 0.042(3) 0.001(2) 0.000(2) 0.003(2) C109 0.072(3) 0.038(3) 0.052(3) -0.004(2) -0.003(3) -0.006(2) C110 0.087(4) 0.058(3) 0.043(3) -0.005(3) -0.005(3) 0.026(3) C111 0.063(3) 0.079(4) 0.044(3) 0.003(3) 0.005(2) 0.033(3) C112 0.045(3) 0.060(3) 0.046(3) 0.015(2) 0.008(2) 0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C42 1.996(4) . ? Pd1 N1 2.159(3) . ? Pd1 P1 2.2978(11) . ? Pd1 S1 2.3462(12) . ? Pd1 Pd2 2.7240(7) . ? P1 C21 1.820(4) . ? P1 C11 1.823(4) . ? P1 C31 1.844(4) . ? S1 C1 1.735(5) . ? N1 C6 1.348(5) . ? N1 C10 1.351(6) . ? C1 N2 1.358(6) . ? C1 C2 1.404(6) . ? Pd2 C12 2.004(4) . ? Pd2 N2 2.179(4) . ? Pd2 P2 2.2967(12) . ? Pd2 S2 2.3589(13) . ? P2 C51 1.822(4) . ? P2 C41 1.824(4) . ? P2 C61 1.837(4) . ? S2 C6 1.743(5) . ? N2 C5 1.359(6) . ? C2 C3 1.354(7) . ? Pd3 C77 2.001(4) . ? Pd3 N3 2.162(4) . ? Pd3 P3 2.3069(12) . ? Pd3 S3 2.3535(12) . ? Pd3 Pd4 2.7241(7) . ? P3 C89 1.835(4) . ? P3 C96 1.835(4) . ? P3 C83 1.838(4) . ? S3 C67 1.745(4) . ? N3 C76 1.351(6) . ? N3 C72 1.352(6) . ? C3 C4 1.360(8) . ? Pd4 C95 2.011(4) . ? Pd4 N4 2.164(4) . ? Pd4 P4 2.3025(12) . ? Pd4 S4 2.3611(12) . ? P4 C78 1.825(4) . ? P4 C107 1.836(4) . ? P4 C101 1.840(4) . ? S4 C72 1.742(5) . ? N4 C67 1.351(5) . ? N4 C71 1.351(5) . ? C4 C5 1.362(7) . ? C6 C7 1.407(6) . ? C7 C8 1.358(7) . ? C8 C9 1.374(8) . ? C9 C10 1.375(7) . ? C11 C12 1.400(6) . ? C11 C16 1.408(6) . ? C12 C13 1.401(6) . ? C13 C14 1.381(7) . ? C14 C15 1.366(7) . ? C15 C16 1.379(6) . ? C21 C22 1.379(6) . ? C21 C26 1.396(6) . ? C22 C23 1.388(7) . ? C23 C24 1.365(8) . ? C24 C25 1.386(7) . ? C25 C26 1.376(6) . ? C31 C32 1.374(6) . ? C31 C36 1.389(6) . ? C32 C33 1.390(6) . ? C33 C34 1.344(7) . ? C34 C35 1.366(7) . ? C35 C36 1.384(7) . ? C41 C42 1.393(5) . ? C41 C46 1.403(6) . ? C42 C43 1.404(5) . ? C43 C44 1.370(6) . ? C44 C45 1.376(6) . ? C45 C46 1.381(6) . ? C51 C56 1.375(6) . ? C51 C52 1.394(6) . ? C52 C53 1.361(7) . ? C53 C54 1.367(9) . ? C54 C55 1.356(8) . ? C55 C56 1.385(7) . ? C61 C62 1.376(6) . ? C61 C66 1.387(7) . ? C62 C63 1.388(8) . ? C63 C64 1.345(9) . ? C64 C65 1.365(9) . ? C65 C66 1.380(7) . ? C67 C68 1.400(6) . ? C68 C69 1.374(7) . ? C69 C70 1.389(7) . ? C70 C71 1.359(7) . ? C72 C73 1.402(6) . ? C73 C74 1.353(7) . ? C74 C75 1.379(8) . ? C75 C76 1.363(7) . ? C77 C82 1.393(5) . ? C77 C78 1.404(6) . ? C78 C79 1.398(6) . ? C79 C80 1.367(6) . ? C80 C81 1.388(7) . ? C81 C82 1.378(6) . ? C83 C84 1.383(6) . ? C83 C88 1.392(6) . ? C84 C85 1.382(7) . ? C85 C86 1.379(7) . ? C86 C87 1.346(8) . ? C87 C88 1.385(7) . ? C89 C94 1.377(7) . ? C89 C90 1.384(7) . ? C90 C91 1.385(7) . ? C91 C92 1.372(8) . ? C92 C93 1.365(9) . ? C93 C94 1.399(8) . ? C95 C96 1.388(6) . ? C95 C100 1.408(6) . ? C96 C97 1.396(6) . ? C97 C98 1.392(6) . ? C98 C99 1.368(7) . ? C99 C100 1.381(6) . ? C101 C106 1.380(6) . ? C101 C102 1.388(6) . ? C102 C103 1.374(6) . ? C103 C104 1.357(8) . ? C104 C105 1.360(9) . ? C105 C106 1.395(8) . ? C107 C108 1.384(6) . ? C107 C112 1.395(6) . ? C108 C109 1.385(6) . ? C109 C110 1.375(7) . ? C110 C111 1.364(8) . ? C111 C112 1.388(7) . ? 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 C42 Pd1 N1 173.26(14) . . ? C42 Pd1 P1 88.31(12) . . ? N1 Pd1 P1 98.41(10) . . ? C42 Pd1 S1 84.55(12) . . ? N1 Pd1 S1 88.71(10) . . ? P1 Pd1 S1 170.93(4) . . ? C42 Pd1 Pd2 95.11(11) . . ? N1 Pd1 Pd2 85.00(9) . . ? P1 Pd1 Pd2 84.88(4) . . ? S1 Pd1 Pd2 90.19(4) . . ? C21 P1 C11 104.7(2) . . ? C21 P1 C31 100.99(18) . . ? C11 P1 C31 105.73(19) . . ? C21 P1 Pd1 114.98(15) . . ? C11 P1 Pd1 111.59(14) . . ? C31 P1 Pd1 117.45(13) . . ? C1 S1 Pd1 102.65(15) . . ? C6 N1 C10 118.9(4) . . ? C6 N1 Pd1 127.1(3) . . ? C10 N1 Pd1 113.8(3) . . ? N2 C1 C2 119.7(4) . . ? N2 C1 S1 121.8(3) . . ? C2 C1 S1 118.5(4) . . ? C12 Pd2 N2 175.10(15) . . ? C12 Pd2 P2 85.14(12) . . ? N2 Pd2 P2 99.70(9) . . ? C12 Pd2 S2 87.49(12) . . ? N2 Pd2 S2 87.62(10) . . ? P2 Pd2 S2 170.94(4) . . ? C12 Pd2 Pd1 96.08(12) . . ? N2 Pd2 Pd1 83.51(10) . . ? P2 Pd2 Pd1 86.64(3) . . ? S2 Pd2 Pd1 88.90(3) . . ? C51 P2 C41 108.03(19) . . ? C51 P2 C61 100.2(2) . . ? C41 P2 C61 102.10(19) . . ? C51 P2 Pd2 114.74(15) . . ? C41 P2 Pd2 110.49(13) . . ? C61 P2 Pd2 119.95(14) . . ? C6 S2 Pd2 103.42(15) . . ? C1 N2 C5 117.5(4) . . ? C1 N2 Pd2 127.2(3) . . ? C5 N2 Pd2 115.2(3) . . ? C3 C2 C1 120.6(5) . . ? C77 Pd3 N3 173.50(15) . . ? C77 Pd3 P3 87.20(12) . . ? N3 Pd3 P3 99.30(10) . . ? C77 Pd3 S3 85.31(12) . . ? N3 Pd3 S3 88.23(10) . . ? P3 Pd3 S3 170.95(4) . . ? C77 Pd3 Pd4 95.41(11) . . ? N3 Pd3 Pd4 85.21(10) . . ? P3 Pd3 Pd4 85.45(3) . . ? S3 Pd3 Pd4 90.20(3) . . ? C89 P3 C96 107.5(2) . . ? C89 P3 C83 100.9(2) . . ? C96 P3 C83 103.52(19) . . ? C89 P3 Pd3 115.62(17) . . ? C96 P3 Pd3 111.76(14) . . ? C83 P3 Pd3 116.25(14) . . ? C67 S3 Pd3 105.26(15) . . ? C76 N3 C72 118.1(4) . . ? C76 N3 Pd3 114.9(3) . . ? C72 N3 Pd3 126.6(3) . . ? C2 C3 C4 119.9(5) . . ? C95 Pd4 N4 176.95(15) . . ? C95 Pd4 P4 88.73(12) . . ? N4 Pd4 P4 94.31(10) . . ? C95 Pd4 S4 86.51(12) . . ? N4 Pd4 S4 90.49(10) . . ? P4 Pd4 S4 172.19(4) . . ? C95 Pd4 Pd3 95.68(11) . . ? N4 Pd4 Pd3 84.81(9) . . ? P4 Pd4 Pd3 85.81(4) . . ? S4 Pd4 Pd3 88.50(4) . . ? C78 P4 C107 105.39(19) . . ? C78 P4 C101 102.31(19) . . ? C107 P4 C101 104.7(2) . . ? C78 P4 Pd4 110.93(13) . . ? C107 P4 Pd4 111.68(14) . . ? C101 P4 Pd4 120.49(14) . . ? C72 S4 Pd4 103.23(15) . . ? C67 N4 C71 117.9(4) . . ? C67 N4 Pd4 127.2(3) . . ? C71 N4 Pd4 114.7(3) . . ? C3 C4 C5 118.3(5) . . ? N2 C5 C4 123.9(5) . . ? N1 C6 C7 119.7(4) . . ? N1 C6 S2 121.4(3) . . ? C7 C6 S2 118.9(4) . . ? C8 C7 C6 120.4(5) . . ? C7 C8 C9 119.7(5) . . ? C8 C9 C10 118.3(5) . . ? N1 C10 C9 123.0(5) . . ? C12 C11 C16 119.7(4) . . ? C12 C11 P1 120.2(3) . . ? C16 C11 P1 119.9(3) . . ? C11 C12 C13 117.6(4) . . ? C11 C12 Pd2 122.6(3) . . ? C13 C12 Pd2 119.7(3) . . ? C14 C13 C12 121.5(4) . . ? C15 C14 C13 120.9(4) . . ? C14 C15 C16 119.2(5) . . ? C15 C16 C11 121.1(4) . . ? C22 C21 C26 118.2(4) . . ? C22 C21 P1 125.2(4) . . ? C26 C21 P1 116.4(3) . . ? C21 C22 C23 120.8(5) . . ? C24 C23 C22 120.5(5) . . ? C23 C24 C25 119.6(5) . . ? C26 C25 C24 120.0(5) . . ? C25 C26 C21 120.9(5) . . ? C32 C31 C36 117.1(4) . . ? C32 C31 P1 121.3(3) . . ? C36 C31 P1 121.5(3) . . ? C31 C32 C33 121.5(4) . . ? C34 C33 C32 120.7(5) . . ? C33 C34 C35 119.0(5) . . ? C34 C35 C36 121.1(5) . . ? C35 C36 C31 120.5(4) . . ? C42 C41 C46 119.4(4) . . ? C42 C41 P2 121.7(3) . . ? C46 C41 P2 118.9(3) . . ? C41 C42 C43 117.8(4) . . ? C41 C42 Pd1 123.6(3) . . ? C43 C42 Pd1 118.4(3) . . ? C44 C43 C42 121.9(4) . . ? C43 C44 C45 120.2(4) . . ? C44 C45 C46 119.2(4) . . ? C45 C46 C41 121.3(4) . . ? C56 C51 C52 117.6(4) . . ? C56 C51 P2 123.6(4) . . ? C52 C51 P2 118.5(3) . . ? C53 C52 C51 121.0(5) . . ? C52 C53 C54 120.8(6) . . ? C55 C54 C53 119.2(5) . . ? C54 C55 C56 120.8(5) . . ? C51 C56 C55 120.6(5) . . ? C62 C61 C66 118.1(4) . . ? C62 C61 P2 121.7(4) . . ? C66 C61 P2 120.2(3) . . ? C61 C62 C63 120.6(5) . . ? C64 C63 C62 119.9(6) . . ? C63 C64 C65 121.3(6) . . ? C64 C65 C66 119.1(6) . . ? C65 C66 C61 121.0(5) . . ? N4 C67 C68 120.4(4) . . ? N4 C67 S3 122.2(3) . . ? C68 C67 S3 117.4(4) . . ? C69 C68 C67 120.1(5) . . ? C68 C69 C70 119.1(5) . . ? C71 C70 C69 117.9(5) . . ? N4 C71 C70 124.4(5) . . ? N3 C72 C73 119.2(4) . . ? N3 C72 S4 121.2(3) . . ? C73 C72 S4 119.6(4) . . ? C74 C73 C72 121.4(5) . . ? C73 C74 C75 119.2(5) . . ? C76 C75 C74 117.7(5) . . ? N3 C76 C75 124.3(5) . . ? C82 C77 C78 117.6(4) . . ? C82 C77 Pd3 119.3(3) . . ? C78 C77 Pd3 123.0(3) . . ? C79 C78 C77 119.2(4) . . ? C79 C78 P4 119.8(3) . . ? C77 C78 P4 121.0(3) . . ? C80 C79 C78 122.4(4) . . ? C79 C80 C81 118.4(4) . . ? C82 C81 C80 120.2(4) . . ? C81 C82 C77 122.1(4) . . ? C84 C83 C88 118.4(4) . . ? C84 C83 P3 120.8(3) . . ? C88 C83 P3 120.7(4) . . ? C85 C84 C83 121.3(5) . . ? C86 C85 C84 118.8(5) . . ? C87 C86 C85 121.2(5) . . ? C86 C87 C88 120.4(5) . . ? C87 C88 C83 120.0(5) . . ? C94 C89 C90 118.9(5) . . ? C94 C89 P3 123.6(4) . . ? C90 C89 P3 117.3(4) . . ? C89 C90 C91 120.6(5) . . ? C92 C91 C90 120.0(6) . . ? C93 C92 C91 120.2(5) . . ? C92 C93 C94 120.0(6) . . ? C89 C94 C93 120.2(6) . . ? C96 C95 C100 117.8(4) . . ? C96 C95 Pd4 123.7(3) . . ? C100 C95 Pd4 118.5(3) . . ? C95 C96 C97 120.4(4) . . ? C95 C96 P3 120.2(3) . . ? C97 C96 P3 119.4(3) . . ? C98 C97 C96 120.5(4) . . ? C99 C98 C97 119.4(5) . . ? C98 C99 C100 120.5(4) . . ? C99 C100 C95 121.3(4) . . ? C106 C101 C102 118.0(5) . . ? C106 C101 P4 122.8(4) . . ? C102 C101 P4 119.2(3) . . ? C103 C102 C101 121.1(5) . . ? C104 C103 C102 120.6(5) . . ? C103 C104 C105 119.5(5) . . ? C104 C105 C106 120.9(5) . . ? C101 C106 C105 119.9(5) . . ? C108 C107 C112 118.9(4) . . ? C108 C107 P4 122.7(3) . . ? C112 C107 P4 118.3(3) . . ? C107 C108 C109 120.2(4) . . ? C110 C109 C108 120.1(5) . . ? C111 C110 C109 120.6(5) . . ? C110 C111 C112 119.9(5) . . ? C111 C112 C107 120.4(5) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.507 _refine_diff_density_min -0.882 _refine_diff_density_rms 0.143 _database_code_depnum_ccdc_archive 'CCDC 941940' ####################################################################### # # 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_2b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H42 Cl2 N2 O3 P2 Pd2 S2' _chemical_formula_weight 1116.61 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 18.2050(5) _cell_length_b 12.9880(4) _cell_length_c 22.1800(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.9870(15) _cell_angle_gamma 90.00 _cell_volume 5066.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.464 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2248 _exptl_absorpt_coefficient_mu 1.002 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 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_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18568 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.0473 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 27.45 _reflns_number_total 11204 _reflns_number_gt 8631 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect(Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo and Scalepack(Otwinowski & Minor1997)' _computing_data_reduction 'Denzo and Scalepack(Otwinowski & Minor1997)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0933P)^2^+7.6603P] 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 11204 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0704 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1702 _refine_ls_wR_factor_gt 0.1546 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.002 _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 O1 O 0.4295(8) 0.0451(12) 0.9909(4) 0.281(9) Uani 1 1 d . . . Pd1 Pd 0.832559(18) 0.07704(3) 0.705824(15) 0.03126(11) Uani 1 1 d . . . P1 P 0.75311(7) 0.17159(9) 0.62760(5) 0.0323(2) Uani 1 1 d . . . S1 S 0.89552(7) -0.03542(11) 0.78706(6) 0.0450(3) Uani 1 1 d . . . Cl1 Cl 0.63759(16) 0.5311(2) 0.76278(13) 0.1151(9) Uani 1 1 d . . . N1 N 0.8775(2) 0.2099(3) 0.76159(17) 0.0376(9) Uani 1 1 d . . . C1 C 0.8608(3) -0.0124(4) 0.8518(2) 0.0437(11) Uani 1 1 d . . . Pd2 Pd 0.713013(19) 0.06892(3) 0.760036(14) 0.03003(11) Uani 1 1 d . . . S2 S 0.73848(7) 0.24518(10) 0.78250(6) 0.0394(3) Uani 1 1 d . . . P2 P 0.69169(7) -0.09544(9) 0.71987(5) 0.0343(3) Uani 1 1 d . . . N2 N 0.7905(2) 0.0243(3) 0.84779(16) 0.0380(9) Uani 1 1 d . . . Cl2 Cl 0.50518(18) 0.4449(2) 0.67700(15) 0.1273(11) Uani 1 1 d . . . C2 C 0.9074(4) -0.0423(6) 0.9102(3) 0.071(2) Uani 1 1 d . . . H2A H 0.9557 -0.0688 0.9130 0.085 Uiso 1 1 calc R . . O2 O 0.9637(5) 0.2198(7) 0.9671(5) 0.177(4) Uani 1 1 d . . . C3 C 0.8824(4) -0.0327(7) 0.9628(3) 0.084(2) Uani 1 1 d . . . H3A H 0.9128 -0.0537 1.0013 0.101 Uiso 1 1 calc R . . O3 O 0.9974(6) 0.3573(12) 0.0474(5) 0.237(6) Uani 1 1 d . . . C4 C 0.8119(4) 0.0083(6) 0.9584(2) 0.0659(18) Uani 1 1 d . . . H4A H 0.7948 0.0181 0.9940 0.079 Uiso 1 1 calc R . . C5 C 0.7658(3) 0.0353(5) 0.8997(2) 0.0463(12) Uani 1 1 d . . . C6 C 0.6874(3) 0.0751(5) 0.8929(3) 0.0536(14) Uani 1 1 d . . . H6A H 0.6641 0.0894 0.8497 0.080 Uiso 1 1 calc R . . H6B H 0.6896 0.1371 0.9168 0.080 Uiso 1 1 calc R . . H6C H 0.6579 0.0243 0.9077 0.080 Uiso 1 1 calc R . . C7 C 0.8334(3) 0.2718(4) 0.7869(2) 0.0394(10) Uani 1 1 d . . . C8 C 0.8621(4) 0.3664(5) 0.8151(3) 0.0610(16) Uani 1 1 d . . . H8A H 0.8313 0.4099 0.8312 0.073 Uiso 1 1 calc R . . C9 C 0.9358(4) 0.3930(6) 0.8184(3) 0.072(2) Uani 1 1 d . . . H9A H 0.9554 0.4552 0.8364 0.086 Uiso 1 1 calc R . . C10 C 0.9807(4) 0.3273(5) 0.7950(3) 0.0622(17) Uani 1 1 d . . . H10A H 1.0311 0.3446 0.7982 0.075 Uiso 1 1 calc R . . C11 C 0.6546(3) 0.1631(4) 0.63199(19) 0.0349(9) Uani 1 1 d . . . C12 C 0.6363(3) 0.1223(3) 0.68444(19) 0.0333(9) Uani 1 1 d . . . C13 C 0.5606(3) 0.1235(4) 0.6868(2) 0.0430(11) Uani 1 1 d . . . H13A H 0.5480 0.0984 0.7221 0.052 Uiso 1 1 calc R . . C14 C 0.5038(3) 0.1611(5) 0.6379(3) 0.0517(13) Uani 1 1 d . . . H14A H 0.4537 0.1616 0.6406 0.062 Uiso 1 1 calc R . . C15 C 0.5211(3) 0.1978(5) 0.5852(3) 0.0551(15) Uani 1 1 d . . . H15A H 0.4828 0.2217 0.5518 0.066 Uiso 1 1 calc R . . C16 C 0.5958(3) 0.1987(4) 0.5823(2) 0.0459(12) Uani 1 1 d . . . H16A H 0.6075 0.2236 0.5465 0.055 Uiso 1 1 calc R . . C17 C 0.9516(3) 0.2353(5) 0.7665(2) 0.0468(12) Uani 1 1 d . . . C18 C 0.9984(3) 0.1663(5) 0.7382(3) 0.0628(16) Uani 1 1 d . . . H18A H 0.9691 0.1069 0.7210 0.094 Uiso 1 1 calc R . . H18B H 1.0427 0.1451 0.7696 0.094 Uiso 1 1 calc R . . H18C H 1.0137 0.2024 0.7057 0.094 Uiso 1 1 calc R . . C19 C 0.5796(5) 0.4240(7) 0.7417(5) 0.106(3) Uani 1 1 d . . . H19A H 0.6100 0.3670 0.7334 0.127 Uiso 1 1 calc R . . H19B H 0.5593 0.4045 0.7765 0.127 Uiso 1 1 calc R . . C21 C 0.7453(3) 0.1399(4) 0.5460(2) 0.0383(10) Uani 1 1 d . . . C22 C 0.7764(3) 0.1993(5) 0.5074(2) 0.0502(13) Uani 1 1 d . . . H22A H 0.8027 0.2590 0.5231 0.060 Uiso 1 1 calc R . . C23 C 0.7694(4) 0.1719(5) 0.4455(2) 0.0581(15) Uani 1 1 d . . . H23A H 0.7918 0.2123 0.4205 0.070 Uiso 1 1 calc R . . C24 C 0.7292(4) 0.0848(5) 0.4216(3) 0.0596(16) Uani 1 1 d . . . H24A H 0.7236 0.0668 0.3800 0.072 Uiso 1 1 calc R . . C25 C 0.6973(3) 0.0242(5) 0.4591(2) 0.0521(13) Uani 1 1 d . . . H25A H 0.6700 -0.0344 0.4427 0.063 Uiso 1 1 calc R . . C26 C 0.7059(3) 0.0505(4) 0.5219(2) 0.0443(12) Uani 1 1 d . . . H26A H 0.6854 0.0085 0.5474 0.053 Uiso 1 1 calc R . . C31 C 0.7774(3) 0.3091(4) 0.6318(2) 0.0394(10) Uani 1 1 d . . . C32 C 0.8519(3) 0.3354(4) 0.6360(2) 0.0485(12) Uani 1 1 d . . . H32A H 0.8869 0.2837 0.6351 0.058 Uiso 1 1 calc R . . C33 C 0.8758(4) 0.4371(5) 0.6414(3) 0.0600(16) Uani 1 1 d . . . H33A H 0.9263 0.4536 0.6443 0.072 Uiso 1 1 calc R . . C34 C 0.8240(5) 0.5125(5) 0.6425(3) 0.075(2) Uani 1 1 d . . . H34A H 0.8394 0.5811 0.6457 0.090 Uiso 1 1 calc R . . C35 C 0.7500(5) 0.4889(5) 0.6390(4) 0.074(2) Uani 1 1 d . . . H35A H 0.7154 0.5411 0.6402 0.089 Uiso 1 1 calc R . . C36 C 0.7262(4) 0.3859(4) 0.6335(3) 0.0560(14) Uani 1 1 d . . . H36A H 0.6758 0.3696 0.6310 0.067 Uiso 1 1 calc R . . C41 C 0.7441(3) -0.1177(4) 0.6606(2) 0.0371(10) Uani 1 1 d . . . C42 C 0.8006(3) -0.0504(4) 0.6540(2) 0.0374(10) Uani 1 1 d . . . C43 C 0.8409(3) -0.0739(4) 0.6102(2) 0.0458(12) Uani 1 1 d . . . H43A H 0.8792 -0.0300 0.6052 0.055 Uiso 1 1 calc R . . C44 C 0.8241(4) -0.1637(5) 0.5735(3) 0.0545(14) Uani 1 1 d . . . H44A H 0.8523 -0.1798 0.5454 0.065 Uiso 1 1 calc R . . C45 C 0.7657(4) -0.2278(5) 0.5793(3) 0.0566(14) Uani 1 1 d . . . H45A H 0.7533 -0.2856 0.5540 0.068 Uiso 1 1 calc R . . C46 C 0.7262(3) -0.2055(4) 0.6226(2) 0.0490(12) Uani 1 1 d . . . H46A H 0.6872 -0.2489 0.6268 0.059 Uiso 1 1 calc R . . C51 C 0.5962(3) -0.1405(4) 0.6787(2) 0.0381(10) Uani 1 1 d . . . C52 C 0.5612(3) -0.0938(4) 0.6211(2) 0.0461(12) Uani 1 1 d . . . H52A H 0.5856 -0.0400 0.6065 0.055 Uiso 1 1 calc R . . C53 C 0.4911(3) -0.1272(5) 0.5862(3) 0.0572(15) Uani 1 1 d . . . H53A H 0.4681 -0.0956 0.5484 0.069 Uiso 1 1 calc R . . C54 C 0.4552(3) -0.2074(5) 0.6075(3) 0.0607(16) Uani 1 1 d . . . H54A H 0.4087 -0.2313 0.5834 0.073 Uiso 1 1 calc R . . C55 C 0.4877(4) -0.2522(5) 0.6641(3) 0.0670(18) Uani 1 1 d . . . H55A H 0.4624 -0.3052 0.6785 0.080 Uiso 1 1 calc R . . C56 C 0.5579(3) -0.2193(4) 0.7001(3) 0.0535(14) Uani 1 1 d . . . H56A H 0.5792 -0.2500 0.7386 0.064 Uiso 1 1 calc R . . C61 C 0.7265(3) -0.1935(4) 0.7795(2) 0.0441(11) Uani 1 1 d . . . C62 C 0.7828(3) -0.2637(5) 0.7767(3) 0.0575(15) Uani 1 1 d . . . H62A H 0.8022 -0.2658 0.7418 0.069 Uiso 1 1 calc R . . C63 C 0.8103(4) -0.3307(6) 0.8261(4) 0.082(2) Uani 1 1 d . . . H63A H 0.8478 -0.3781 0.8239 0.098 Uiso 1 1 calc R . . C64 C 0.7831(4) -0.3280(6) 0.8774(4) 0.080(2) Uani 1 1 d . . . H64A H 0.8025 -0.3731 0.9102 0.096 Uiso 1 1 calc R . . C65 C 0.7268(4) -0.2590(6) 0.8814(3) 0.0710(19) Uani 1 1 d . . . H65A H 0.7082 -0.2576 0.9167 0.085 Uiso 1 1 calc R . . C66 C 0.6988(4) -0.1925(5) 0.8329(2) 0.0544(14) Uani 1 1 d . . . H66A H 0.6609 -0.1461 0.8354 0.065 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 O1 0.320(15) 0.42(2) 0.087(5) -0.056(8) 0.016(7) -0.271(15) Pd1 0.02747(18) 0.0345(2) 0.03103(18) 0.00103(12) 0.00604(13) 0.00155(13) P1 0.0348(6) 0.0319(6) 0.0290(5) 0.0018(4) 0.0063(4) 0.0009(5) S1 0.0382(7) 0.0528(8) 0.0422(6) 0.0085(6) 0.0069(5) 0.0138(6) Cl1 0.1027(18) 0.0842(16) 0.135(2) 0.0181(14) -0.0121(15) -0.0033(14) N1 0.036(2) 0.041(2) 0.0321(18) -0.0026(16) 0.0033(15) -0.0035(17) C1 0.041(3) 0.047(3) 0.038(2) 0.005(2) 0.0012(19) 0.005(2) Pd2 0.02827(18) 0.03225(19) 0.02862(17) 0.00054(12) 0.00566(13) 0.00040(13) S2 0.0397(6) 0.0355(6) 0.0426(6) -0.0064(5) 0.0098(5) -0.0003(5) P2 0.0354(6) 0.0299(6) 0.0354(6) 0.0024(4) 0.0052(5) -0.0005(5) N2 0.038(2) 0.042(2) 0.0298(18) 0.0039(16) 0.0017(15) 0.0003(18) Cl2 0.112(2) 0.104(2) 0.137(2) -0.0164(16) -0.0208(17) 0.0134(16) C2 0.048(3) 0.112(6) 0.045(3) 0.012(3) -0.001(3) 0.029(4) O2 0.134(7) 0.138(8) 0.252(11) 0.070(7) 0.039(7) 0.058(6) C3 0.071(5) 0.131(7) 0.040(3) 0.010(4) -0.005(3) 0.025(5) O3 0.148(10) 0.364(18) 0.184(10) -0.071(11) 0.013(7) -0.026(11) C4 0.072(4) 0.090(5) 0.034(3) 0.003(3) 0.011(3) 0.007(4) C5 0.049(3) 0.053(3) 0.037(2) -0.001(2) 0.012(2) -0.001(2) C6 0.052(3) 0.066(4) 0.046(3) -0.002(3) 0.020(2) 0.002(3) C7 0.045(3) 0.041(3) 0.031(2) -0.0023(19) 0.0071(19) -0.008(2) C8 0.075(4) 0.052(4) 0.060(3) -0.020(3) 0.026(3) -0.022(3) C9 0.077(5) 0.074(5) 0.067(4) -0.022(3) 0.025(3) -0.037(4) C10 0.047(3) 0.077(5) 0.058(3) -0.004(3) 0.007(3) -0.025(3) C11 0.037(2) 0.034(2) 0.031(2) -0.0025(17) 0.0062(17) 0.0011(19) C12 0.034(2) 0.030(2) 0.032(2) -0.0001(17) 0.0025(17) 0.0029(18) C13 0.034(2) 0.049(3) 0.046(3) 0.002(2) 0.011(2) 0.003(2) C14 0.027(2) 0.064(4) 0.060(3) -0.001(3) 0.004(2) 0.008(2) C15 0.040(3) 0.068(4) 0.048(3) 0.001(3) -0.007(2) 0.015(3) C16 0.046(3) 0.051(3) 0.036(2) 0.008(2) 0.003(2) 0.009(2) C17 0.038(3) 0.059(3) 0.040(2) 0.005(2) 0.005(2) -0.012(2) C18 0.041(3) 0.071(4) 0.075(4) 0.005(3) 0.015(3) -0.007(3) C19 0.075(6) 0.081(6) 0.152(9) 0.043(6) 0.011(6) 0.008(4) C21 0.042(3) 0.040(3) 0.032(2) 0.0028(19) 0.0068(18) 0.004(2) C22 0.054(3) 0.056(3) 0.041(3) 0.005(2) 0.013(2) -0.005(3) C23 0.072(4) 0.069(4) 0.038(3) 0.004(3) 0.022(3) 0.002(3) C24 0.073(4) 0.072(4) 0.035(3) -0.003(3) 0.016(3) 0.009(3) C25 0.056(3) 0.052(3) 0.045(3) -0.012(2) 0.006(2) 0.002(3) C26 0.049(3) 0.043(3) 0.039(2) -0.001(2) 0.008(2) 0.001(2) C31 0.049(3) 0.035(2) 0.032(2) -0.0002(18) 0.0069(19) -0.002(2) C32 0.054(3) 0.040(3) 0.049(3) 0.004(2) 0.008(2) -0.005(2) C33 0.069(4) 0.052(4) 0.054(3) 0.005(3) 0.005(3) -0.021(3) C34 0.101(6) 0.037(3) 0.080(4) 0.003(3) 0.010(4) -0.017(4) C35 0.089(5) 0.033(3) 0.095(5) -0.003(3) 0.013(4) 0.005(3) C36 0.061(4) 0.038(3) 0.067(4) 0.003(3) 0.013(3) 0.002(3) C41 0.041(3) 0.030(2) 0.038(2) -0.0011(18) 0.0076(19) 0.004(2) C42 0.034(2) 0.038(3) 0.037(2) 0.0008(19) 0.0039(18) 0.0074(19) C43 0.045(3) 0.046(3) 0.048(3) 0.001(2) 0.014(2) 0.012(2) C44 0.063(4) 0.052(3) 0.050(3) -0.004(2) 0.018(3) 0.016(3) C45 0.071(4) 0.040(3) 0.057(3) -0.011(2) 0.013(3) 0.007(3) C46 0.059(3) 0.033(3) 0.054(3) -0.004(2) 0.014(2) -0.002(2) C51 0.037(2) 0.033(2) 0.041(2) -0.0025(19) 0.0038(19) 0.0011(19) C52 0.046(3) 0.044(3) 0.046(3) 0.000(2) 0.006(2) -0.006(2) C53 0.053(3) 0.058(4) 0.051(3) -0.003(3) -0.003(2) -0.008(3) C54 0.044(3) 0.063(4) 0.065(4) -0.009(3) -0.004(3) -0.017(3) C55 0.060(4) 0.052(4) 0.082(4) 0.003(3) 0.006(3) -0.022(3) C56 0.050(3) 0.045(3) 0.059(3) 0.009(2) 0.002(2) -0.014(3) C61 0.042(3) 0.039(3) 0.047(3) 0.009(2) 0.005(2) -0.003(2) C62 0.050(3) 0.046(3) 0.074(4) 0.018(3) 0.011(3) 0.007(3) C63 0.058(4) 0.065(5) 0.110(6) 0.046(4) 0.002(4) 0.011(3) C64 0.069(5) 0.075(5) 0.081(5) 0.045(4) -0.008(4) -0.014(4) C65 0.083(5) 0.068(4) 0.058(4) 0.013(3) 0.009(3) -0.019(4) C66 0.063(4) 0.052(3) 0.045(3) 0.007(2) 0.009(2) -0.012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C42 2.014(5) . ? Pd1 N1 2.157(4) . ? Pd1 P1 2.3049(11) . ? Pd1 S1 2.3718(12) . ? Pd1 Pd2 2.7471(5) . ? P1 C11 1.825(5) . ? P1 C21 1.825(5) . ? P1 C31 1.836(5) . ? S1 C1 1.738(5) . ? Cl1 C19 1.736(10) . ? N1 C7 1.355(6) . ? N1 C17 1.367(6) . ? C1 N2 1.347(6) . ? C1 C2 1.408(7) . ? Pd2 C12 2.008(4) . ? Pd2 N2 2.166(4) . ? Pd2 P2 2.3070(13) . ? Pd2 S2 2.3632(13) . ? S2 C7 1.741(5) . ? P2 C61 1.828(5) . ? P2 C41 1.837(5) . ? P2 C51 1.838(5) . ? N2 C5 1.348(6) . ? Cl2 C19 1.721(9) . ? C2 C3 1.364(9) . ? C2 H2A 0.9300 . ? C3 C4 1.369(10) . ? C3 H3A 0.9300 . ? C4 C5 1.398(8) . ? C4 H4A 0.9300 . ? C5 C6 1.488(8) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.417(7) . ? C8 C9 1.370(9) . ? C8 H8A 0.9300 . ? C9 C10 1.372(10) . ? C9 H9A 0.9300 . ? C10 C17 1.391(8) . ? C10 H10A 0.9300 . ? C11 C12 1.395(6) . ? C11 C16 1.402(6) . ? C12 C13 1.393(7) . ? C13 C14 1.380(7) . ? C13 H13A 0.9300 . ? C14 C15 1.371(8) . ? C14 H14A 0.9300 . ? C15 C16 1.379(8) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? C17 C18 1.482(8) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C21 C22 1.378(7) . ? C21 C26 1.396(7) . ? C22 C23 1.392(7) . ? C22 H22A 0.9300 . ? C23 C24 1.378(9) . ? C23 H23A 0.9300 . ? C24 C25 1.377(9) . ? C24 H24A 0.9300 . ? C25 C26 1.404(7) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C31 C36 1.373(8) . ? C31 C32 1.377(7) . ? C32 C33 1.386(8) . ? C32 H32A 0.9300 . ? C33 C34 1.365(10) . ? C33 H33A 0.9300 . ? C34 C35 1.364(11) . ? C34 H34A 0.9300 . ? C35 C36 1.402(9) . ? C35 H35A 0.9300 . ? C36 H36A 0.9300 . ? C41 C42 1.385(7) . ? C41 C46 1.405(7) . ? C42 C43 1.394(7) . ? C43 C44 1.409(8) . ? C43 H43A 0.9300 . ? C44 C45 1.382(9) . ? C44 H44A 0.9300 . ? C45 C46 1.370(8) . ? C45 H45A 0.9300 . ? C46 H46A 0.9300 . ? C51 C56 1.389(7) . ? C51 C52 1.410(7) . ? C52 C53 1.381(7) . ? C52 H52A 0.9300 . ? C53 C54 1.376(9) . ? C53 H53A 0.9300 . ? C54 C55 1.371(9) . ? C54 H54A 0.9300 . ? C55 C56 1.387(8) . ? C55 H55A 0.9300 . ? C56 H56A 0.9300 . ? C61 C62 1.385(8) . ? C61 C66 1.400(8) . ? C62 C63 1.387(8) . ? C62 H62A 0.9300 . ? C63 C64 1.353(12) . ? C63 H63A 0.9300 . ? C64 C65 1.382(11) . ? C64 H64A 0.9300 . ? C65 C66 1.372(8) . ? C65 H65A 0.9300 . ? C66 H66A 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 C42 Pd1 N1 174.73(17) . . ? C42 Pd1 P1 88.59(13) . . ? N1 Pd1 P1 94.39(11) . . ? C42 Pd1 S1 86.52(13) . . ? N1 Pd1 S1 91.14(11) . . ? P1 Pd1 S1 170.36(5) . . ? C42 Pd1 Pd2 94.22(14) . . ? N1 Pd1 Pd2 90.31(11) . . ? P1 Pd1 Pd2 86.33(3) . . ? S1 Pd1 Pd2 85.74(3) . . ? C11 P1 C21 102.3(2) . . ? C11 P1 C31 106.5(2) . . ? C21 P1 C31 103.1(2) . . ? C11 P1 Pd1 111.21(15) . . ? C21 P1 Pd1 119.93(16) . . ? C31 P1 Pd1 112.54(16) . . ? C1 S1 Pd1 108.30(17) . . ? C7 N1 C17 120.1(4) . . ? C7 N1 Pd1 122.3(3) . . ? C17 N1 Pd1 117.3(3) . . ? N2 C1 C2 119.7(5) . . ? N2 C1 S1 123.3(3) . . ? C2 C1 S1 116.8(4) . . ? C12 Pd2 N2 173.33(17) . . ? C12 Pd2 P2 89.17(13) . . ? N2 Pd2 P2 96.03(12) . . ? C12 Pd2 S2 84.14(13) . . ? N2 Pd2 S2 91.31(12) . . ? P2 Pd2 S2 169.12(4) . . ? C12 Pd2 Pd1 94.59(13) . . ? N2 Pd2 Pd1 89.89(11) . . ? P2 Pd2 Pd1 86.54(3) . . ? S2 Pd2 Pd1 85.45(3) . . ? C7 S2 Pd2 109.99(18) . . ? C61 P2 C41 105.2(2) . . ? C61 P2 C51 104.1(2) . . ? C41 P2 C51 101.2(2) . . ? C61 P2 Pd2 111.90(18) . . ? C41 P2 Pd2 110.83(16) . . ? C51 P2 Pd2 121.97(16) . . ? C1 N2 C5 120.2(4) . . ? C1 N2 Pd2 122.7(3) . . ? C5 N2 Pd2 117.1(3) . . ? C3 C2 C1 120.5(6) . . ? C3 C2 H2A 119.8 . . ? C1 C2 H2A 119.8 . . ? C2 C3 C4 119.2(6) . . ? C2 C3 H3A 120.4 . . ? C4 C3 H3A 120.4 . . ? C3 C4 C5 119.4(5) . . ? C3 C4 H4A 120.3 . . ? C5 C4 H4A 120.3 . . ? N2 C5 C4 121.1(5) . . ? N2 C5 C6 118.2(5) . . ? C4 C5 C6 120.7(5) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N1 C7 C8 120.5(5) . . ? N1 C7 S2 123.0(4) . . ? C8 C7 S2 116.3(4) . . ? C9 C8 C7 119.0(6) . . ? C9 C8 H8A 120.5 . . ? C7 C8 H8A 120.5 . . ? C8 C9 C10 119.6(6) . . ? C8 C9 H9A 120.2 . . ? C10 C9 H9A 120.2 . . ? C9 C10 C17 120.8(6) . . ? C9 C10 H10A 119.6 . . ? C17 C10 H10A 119.6 . . ? C12 C11 C16 118.9(4) . . ? C12 C11 P1 121.1(3) . . ? C16 C11 P1 119.9(4) . . ? C13 C12 C11 118.6(4) . . ? C13 C12 Pd2 117.0(3) . . ? C11 C12 Pd2 124.3(3) . . ? C14 C13 C12 121.4(5) . . ? C14 C13 H13A 119.3 . . ? C12 C13 H13A 119.3 . . ? C15 C14 C13 120.2(5) . . ? C15 C14 H14A 119.9 . . ? C13 C14 H14A 119.9 . . ? C14 C15 C16 119.3(5) . . ? C14 C15 H15A 120.4 . . ? C16 C15 H15A 120.4 . . ? C15 C16 C11 121.4(5) . . ? C15 C16 H16A 119.3 . . ? C11 C16 H16A 119.3 . . ? N1 C17 C10 119.7(6) . . ? N1 C17 C18 118.9(5) . . ? C10 C17 C18 121.3(5) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Cl2 C19 Cl1 113.0(5) . . ? Cl2 C19 H19A 109.0 . . ? Cl1 C19 H19A 109.0 . . ? Cl2 C19 H19B 109.0 . . ? Cl1 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? C22 C21 C26 118.7(5) . . ? C22 C21 P1 123.4(4) . . ? C26 C21 P1 117.9(4) . . ? C21 C22 C23 121.5(6) . . ? C21 C22 H22A 119.2 . . ? C23 C22 H22A 119.2 . . ? C24 C23 C22 119.6(6) . . ? C24 C23 H23A 120.2 . . ? C22 C23 H23A 120.2 . . ? C25 C24 C23 120.1(5) . . ? C25 C24 H24A 120.0 . . ? C23 C24 H24A 120.0 . . ? C24 C25 C26 120.3(6) . . ? C24 C25 H25A 119.8 . . ? C26 C25 H25A 119.8 . . ? C21 C26 C25 119.7(5) . . ? C21 C26 H26A 120.1 . . ? C25 C26 H26A 120.1 . . ? C36 C31 C32 118.8(5) . . ? C36 C31 P1 123.5(4) . . ? C32 C31 P1 117.7(4) . . ? C31 C32 C33 121.6(6) . . ? C31 C32 H32A 119.2 . . ? C33 C32 H32A 119.2 . . ? C34 C33 C32 118.8(7) . . ? C34 C33 H33A 120.6 . . ? C32 C33 H33A 120.6 . . ? C35 C34 C33 121.0(6) . . ? C35 C34 H34A 119.5 . . ? C33 C34 H34A 119.5 . . ? C34 C35 C36 119.8(7) . . ? C34 C35 H35A 120.1 . . ? C36 C35 H35A 120.1 . . ? C31 C36 C35 120.0(6) . . ? C31 C36 H36A 120.0 . . ? C35 C36 H36A 120.0 . . ? C42 C41 C46 120.8(5) . . ? C42 C41 P2 120.9(4) . . ? C46 C41 P2 118.3(4) . . ? C41 C42 C43 118.3(5) . . ? C41 C42 Pd1 124.8(4) . . ? C43 C42 Pd1 116.8(4) . . ? C42 C43 C44 120.5(5) . . ? C42 C43 H43A 119.7 . . ? C44 C43 H43A 119.7 . . ? C45 C44 C43 120.2(5) . . ? C45 C44 H44A 119.9 . . ? C43 C44 H44A 119.9 . . ? C46 C45 C44 119.5(5) . . ? C46 C45 H45A 120.2 . . ? C44 C45 H45A 120.2 . . ? C45 C46 C41 120.6(5) . . ? C45 C46 H46A 119.7 . . ? C41 C46 H46A 119.7 . . ? C56 C51 C52 118.6(5) . . ? C56 C51 P2 124.0(4) . . ? C52 C51 P2 117.4(4) . . ? C53 C52 C51 120.6(5) . . ? C53 C52 H52A 119.7 . . ? C51 C52 H52A 119.7 . . ? C54 C53 C52 119.8(6) . . ? C54 C53 H53A 120.1 . . ? C52 C53 H53A 120.1 . . ? C55 C54 C53 120.3(5) . . ? C55 C54 H54A 119.8 . . ? C53 C54 H54A 119.8 . . ? C54 C55 C56 120.8(6) . . ? C54 C55 H55A 119.6 . . ? C56 C55 H55A 119.6 . . ? C55 C56 C51 119.9(5) . . ? C55 C56 H56A 120.0 . . ? C51 C56 H56A 120.0 . . ? C62 C61 C66 118.4(5) . . ? C62 C61 P2 123.2(4) . . ? C66 C61 P2 118.2(4) . . ? C61 C62 C63 119.8(7) . . ? C61 C62 H62A 120.1 . . ? C63 C62 H62A 120.1 . . ? C64 C63 C62 120.8(7) . . ? C64 C63 H63A 119.6 . . ? C62 C63 H63A 119.6 . . ? C63 C64 C65 120.7(6) . . ? C63 C64 H64A 119.7 . . ? C65 C64 H64A 119.7 . . ? C66 C65 C64 119.2(7) . . ? C66 C65 H65A 120.4 . . ? C64 C65 H65A 120.4 . . ? C65 C66 C61 121.1(7) . . ? C65 C66 H66A 119.5 . . ? C61 C66 H66A 119.5 . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.625 _refine_diff_density_min -1.080 _refine_diff_density_rms 0.212 _database_code_depnum_ccdc_archive 'CCDC 941941' ####################################################################### # # 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_2c _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H40 N2 P2 Pd2 S2' _chemical_formula_weight 1055.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 14.032(3) _cell_length_b 20.200(4) _cell_length_c 18.761(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.03(3) _cell_angle_gamma 90.00 _cell_volume 5265.7(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.332 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2128 _exptl_absorpt_coefficient_mu 0.858 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 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_type none _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16149 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0490 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 24.71 _reflns_number_total 8859 _reflns_number_gt 6306 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect(Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo and Scalepack(Otwinowski & Minor1997)' _computing_data_reduction 'Denzo and Scalepack(Otwinowski & Minor1997)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+5.3285P] 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 8859 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.1248 _refine_ls_wR_factor_gt 0.1112 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 Pd1 Pd 0.21156(3) 0.154714(19) 0.286192(18) 0.04780(12) Uani 1 1 d . . . Pd2 Pd 0.29045(3) 0.03247(2) 0.270901(19) 0.04996(13) Uani 1 1 d . . . P1 P 0.07129(9) 0.11435(7) 0.22287(7) 0.0533(3) Uani 1 1 d . . . P2 P 0.35216(10) 0.07813(7) 0.17442(7) 0.0547(3) Uani 1 1 d . . . S1 S 0.36685(10) 0.18917(8) 0.33736(8) 0.0633(4) Uani 1 1 d . . . S2 S 0.20325(11) -0.00724(8) 0.36134(8) 0.0684(4) Uani 1 1 d . . . N2 N 0.4124(3) 0.0585(2) 0.3494(2) 0.0531(10) Uani 1 1 d . . . N1 N 0.1753(3) 0.1228(2) 0.3885(2) 0.0553(10) Uani 1 1 d . . . C36 C -0.0457(4) 0.1454(4) 0.3245(3) 0.0764(18) Uani 1 1 d . . . H36 H -0.0195 0.1876 0.3223 0.092 Uiso 1 1 calc R . . C41 C 0.3010(4) 0.1587(3) 0.1490(2) 0.0592(13) Uani 1 1 d . . . C12 C 0.1801(4) 0.0016(3) 0.1999(3) 0.0635(14) Uani 1 1 d . . . C42 C 0.2461(4) 0.1933(3) 0.1949(3) 0.0563(12) Uani 1 1 d . . . C21 C 0.0021(4) 0.1608(3) 0.1498(3) 0.0578(13) Uani 1 1 d . . . C67 C 0.4739(3) 0.0082(3) 0.3776(3) 0.0570(13) Uani 1 1 d . . . C52 C 0.5402(4) 0.0398(3) 0.2213(3) 0.0686(15) Uani 1 1 d . . . H52 H 0.5122 -0.0011 0.2279 0.082 Uiso 1 1 calc R . . C51 C 0.4818(4) 0.0920(3) 0.1941(2) 0.0582(13) Uani 1 1 d . . . C11 C 0.0959(4) 0.0362(3) 0.1796(3) 0.0628(14) Uani 1 1 d . . . C75 C 0.4350(4) 0.1214(3) 0.3687(2) 0.0551(13) Uani 1 1 d . . . C72 C 0.5583(4) 0.0211(3) 0.4250(3) 0.0652(15) Uani 1 1 d . . . C76 C 0.1459(4) 0.1735(3) 0.4323(3) 0.0619(14) Uani 1 1 d . . . C61 C 0.3382(4) 0.0334(3) 0.0890(3) 0.0651(14) Uani 1 1 d . . . C46 C 0.3215(5) 0.1893(4) 0.0859(3) 0.0772(17) Uani 1 1 d . . . H46 H 0.3556 0.1664 0.0546 0.093 Uiso 1 1 calc R . . C74 C 0.5209(4) 0.1355(4) 0.4155(3) 0.0745(17) Uani 1 1 d . . . H74 H 0.5359 0.1792 0.4276 0.089 Uiso 1 1 calc R . . C31 C -0.0177(4) 0.0952(3) 0.2821(3) 0.0642(15) Uani 1 1 d . . . C83 C 0.1223(4) 0.0436(4) 0.4709(3) 0.080(2) Uani 1 1 d . . . H83 H 0.1153 -0.0004 0.4837 0.096 Uiso 1 1 calc R . . C77 C 0.1572(5) 0.2376(4) 0.4137(3) 0.0727(16) Uani 1 1 d . . . H77 H 0.1859 0.2471 0.3731 0.087 Uiso 1 1 calc R . . C73 C 0.5800(4) 0.0881(4) 0.4422(3) 0.0768(18) Uani 1 1 d . . . H73 H 0.6362 0.0988 0.4725 0.092 Uiso 1 1 calc R . . C56 C 0.5244(5) 0.1529(3) 0.1858(3) 0.0727(16) Uani 1 1 d . . . H56 H 0.4869 0.1889 0.1684 0.087 Uiso 1 1 calc R . . C53 C 0.6373(5) 0.0466(4) 0.2386(3) 0.0799(19) Uani 1 1 d . . . H53 H 0.6750 0.0107 0.2563 0.096 Uiso 1 1 calc R . . C22 C 0.0421(5) 0.1709(3) 0.0865(3) 0.0710(16) Uani 1 1 d . . . H22 H 0.1040 0.1559 0.0831 0.085 Uiso 1 1 calc R . . C43 C 0.2182(5) 0.2573(3) 0.1761(3) 0.0721(16) Uani 1 1 d . . . H43 H 0.1823 0.2805 0.2059 0.087 Uiso 1 1 calc R . . C68 C 0.4517(4) -0.0574(3) 0.3588(3) 0.0670(15) Uani 1 1 d . . . H68 H 0.3954 -0.0666 0.3279 0.080 Uiso 1 1 calc R . . C84 C 0.1672(4) 0.0599(3) 0.4078(3) 0.0636(15) Uani 1 1 d . . . C16 C 0.0255(5) 0.0103(4) 0.1249(4) 0.089(2) Uani 1 1 d . . . H16 H -0.0298 0.0347 0.1099 0.107 Uiso 1 1 calc R . . C62 C 0.2527(6) 0.0362(5) 0.0441(4) 0.111(3) Uani 1 1 d . . . H62 H 0.2032 0.0624 0.0567 0.134 Uiso 1 1 calc R . . C13 C 0.1891(5) -0.0607(4) 0.1681(4) 0.090(2) Uani 1 1 d . . . H13 H 0.2441 -0.0856 0.1831 0.108 Uiso 1 1 calc R . . C71 C 0.6180(4) -0.0317(5) 0.4520(3) 0.085(2) Uani 1 1 d . . . H71 H 0.6739 -0.0231 0.4835 0.103 Uiso 1 1 calc R . . C55 C 0.6247(5) 0.1602(5) 0.2038(4) 0.093(2) Uani 1 1 d . . . H55 H 0.6538 0.2009 0.1982 0.111 Uiso 1 1 calc R . . C32 C -0.0552(5) 0.0334(4) 0.2889(4) 0.091(2) Uani 1 1 d . . . H32 H -0.0356 -0.0014 0.2618 0.110 Uiso 1 1 calc R . . C26 C -0.0892(4) 0.1836(3) 0.1519(3) 0.0738(17) Uani 1 1 d . . . H26 H -0.1171 0.1781 0.1937 0.089 Uiso 1 1 calc R . . C81 C 0.1036(5) 0.1590(4) 0.4941(3) 0.0800(19) Uani 1 1 d . . . C65 C 0.3930(6) -0.0424(4) 0.0049(4) 0.091(2) Uani 1 1 d . . . H65 H 0.4423 -0.0681 -0.0089 0.109 Uiso 1 1 calc R . . C44 C 0.2409(6) 0.2882(4) 0.1154(4) 0.093(2) Uani 1 1 d . . . H44 H 0.2225 0.3318 0.1051 0.111 Uiso 1 1 calc R . . C66 C 0.4068(5) -0.0078(3) 0.0691(3) 0.0739(16) Uani 1 1 d . . . H66 H 0.4646 -0.0127 0.0996 0.089 Uiso 1 1 calc R . . C33 C -0.1216(6) 0.0215(6) 0.3351(6) 0.126(4) Uani 1 1 d . . . H33 H -0.1469 -0.0208 0.3380 0.151 Uiso 1 1 calc R . . C23 C -0.0102(5) 0.2035(3) 0.0285(3) 0.0804(19) Uani 1 1 d . . . H23 H 0.0180 0.2107 -0.0128 0.096 Uiso 1 1 calc R . . C24 C -0.1010(5) 0.2249(4) 0.0306(3) 0.0787(18) Uani 1 1 d . . . H24 H -0.1352 0.2459 -0.0091 0.094 Uiso 1 1 calc R . . C69 C 0.5100(5) -0.1086(4) 0.3845(4) 0.088(2) Uani 1 1 d . . . H69 H 0.4941 -0.1518 0.3706 0.105 Uiso 1 1 calc R . . C82 C 0.0909(5) 0.0922(5) 0.5108(3) 0.089(2) Uani 1 1 d . . . H82 H 0.0603 0.0813 0.5501 0.107 Uiso 1 1 calc R . . C25 C -0.1420(5) 0.2153(4) 0.0921(4) 0.092(2) Uani 1 1 d . . . H25 H -0.2046 0.2296 0.0942 0.111 Uiso 1 1 calc R . . C64 C 0.3060(8) -0.0385(5) -0.0382(4) 0.110(3) Uani 1 1 d . . . H64 H 0.2945 -0.0636 -0.0801 0.132 Uiso 1 1 calc R . . C45 C 0.2917(6) 0.2529(4) 0.0702(4) 0.095(2) Uani 1 1 d . . . H45 H 0.3059 0.2726 0.0282 0.113 Uiso 1 1 calc R . . C54 C 0.6790(5) 0.1070(5) 0.2295(3) 0.094(2) Uani 1 1 d . . . H54 H 0.7453 0.1117 0.2411 0.113 Uiso 1 1 calc R . . C14 C 0.1211(6) -0.0867(4) 0.1162(5) 0.113(3) Uani 1 1 d . . . H14 H 0.1301 -0.1279 0.0962 0.135 Uiso 1 1 calc R . . C15 C 0.0377(6) -0.0500(4) 0.0940(5) 0.113(3) Uani 1 1 d . . . H15 H -0.0092 -0.0664 0.0584 0.135 Uiso 1 1 calc R . . C80 C 0.0729(5) 0.2129(5) 0.5340(4) 0.097(3) Uani 1 1 d . . . H80 H 0.0451 0.2042 0.5752 0.117 Uiso 1 1 calc R . . C35 C -0.1137(5) 0.1328(6) 0.3708(4) 0.105(3) Uani 1 1 d . . . H35 H -0.1346 0.1668 0.3983 0.126 Uiso 1 1 calc R . . C78 C 0.1270(6) 0.2890(4) 0.4535(4) 0.095(2) Uani 1 1 d . . . H78 H 0.1361 0.3326 0.4399 0.114 Uiso 1 1 calc R . . C70 C 0.5950(5) -0.0952(4) 0.4324(4) 0.092(2) Uani 1 1 d . . . H70 H 0.6350 -0.1297 0.4505 0.110 Uiso 1 1 calc R . . C34 C -0.1496(6) 0.0694(8) 0.3751(5) 0.134(5) Uani 1 1 d . . . H34 H -0.1939 0.0604 0.4064 0.161 Uiso 1 1 calc R . . C79 C 0.0828(7) 0.2755(5) 0.5143(4) 0.109(3) Uani 1 1 d . . . H79 H 0.0606 0.3099 0.5406 0.130 Uiso 1 1 calc R . . C63 C 0.2383(7) 0.0010(6) -0.0198(4) 0.130(4) Uani 1 1 d . . . H63 H 0.1803 0.0052 -0.0502 0.156 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 0.0456(2) 0.0557(2) 0.04079(19) -0.00179(16) 0.00173(14) -0.00189(17) Pd2 0.0448(2) 0.0543(2) 0.0472(2) -0.00243(16) -0.00613(15) -0.00251(17) P1 0.0461(7) 0.0586(8) 0.0514(7) 0.0065(6) -0.0068(5) -0.0025(6) P2 0.0533(8) 0.0674(9) 0.0423(7) -0.0062(6) 0.0022(5) 0.0023(6) S1 0.0532(8) 0.0674(9) 0.0668(8) -0.0123(7) -0.0007(6) -0.0084(7) S2 0.0600(8) 0.0699(10) 0.0734(9) 0.0148(7) 0.0025(7) -0.0075(7) N2 0.045(2) 0.071(3) 0.042(2) -0.0006(19) 0.0024(16) -0.003(2) N1 0.048(2) 0.072(3) 0.044(2) 0.001(2) -0.0019(17) -0.001(2) C36 0.054(3) 0.116(6) 0.056(3) 0.016(3) -0.005(2) -0.004(3) C41 0.063(3) 0.075(4) 0.038(2) 0.001(2) 0.004(2) 0.004(3) C12 0.062(3) 0.060(3) 0.063(3) 0.001(3) -0.011(2) -0.003(3) C42 0.054(3) 0.068(4) 0.046(3) -0.002(2) 0.002(2) -0.001(3) C21 0.053(3) 0.065(3) 0.051(3) 0.008(2) -0.008(2) 0.001(3) C67 0.042(3) 0.081(4) 0.047(3) 0.008(2) 0.002(2) -0.001(3) C52 0.057(3) 0.086(4) 0.064(3) 0.009(3) 0.011(3) 0.003(3) C51 0.058(3) 0.078(4) 0.038(2) -0.007(2) 0.008(2) -0.001(3) C11 0.057(3) 0.056(3) 0.068(3) -0.004(3) -0.016(3) -0.005(3) C75 0.046(3) 0.075(4) 0.044(3) -0.009(2) 0.003(2) -0.006(3) C72 0.047(3) 0.095(5) 0.051(3) -0.003(3) 0.000(2) -0.001(3) C76 0.048(3) 0.091(5) 0.044(3) -0.007(3) -0.001(2) 0.002(3) C61 0.069(4) 0.072(4) 0.053(3) -0.012(3) 0.002(3) 0.004(3) C46 0.092(5) 0.086(5) 0.056(3) 0.016(3) 0.021(3) 0.012(4) C74 0.053(3) 0.095(5) 0.072(4) -0.026(3) -0.005(3) -0.012(3) C31 0.044(3) 0.082(4) 0.063(3) 0.019(3) -0.007(2) -0.001(3) C83 0.067(4) 0.110(6) 0.062(4) 0.038(4) 0.004(3) 0.007(4) C77 0.075(4) 0.088(5) 0.056(3) -0.019(3) 0.011(3) 0.005(3) C73 0.046(3) 0.118(6) 0.062(3) -0.016(3) -0.008(2) -0.006(4) C56 0.079(4) 0.075(4) 0.063(3) -0.002(3) 0.005(3) -0.011(3) C53 0.057(4) 0.114(6) 0.068(4) 0.009(4) 0.005(3) -0.001(4) C22 0.073(4) 0.082(4) 0.055(3) 0.007(3) -0.002(3) 0.014(3) C43 0.089(4) 0.068(4) 0.062(3) 0.012(3) 0.019(3) 0.013(3) C68 0.056(3) 0.077(4) 0.063(3) 0.012(3) -0.010(2) -0.001(3) C84 0.041(3) 0.093(4) 0.053(3) 0.012(3) -0.006(2) -0.001(3) C16 0.080(4) 0.074(5) 0.098(5) -0.010(4) -0.039(4) -0.001(4) C62 0.090(5) 0.167(9) 0.069(4) -0.048(5) -0.017(4) 0.032(5) C13 0.080(4) 0.075(4) 0.103(5) -0.029(4) -0.035(4) 0.006(4) C71 0.049(3) 0.137(7) 0.065(4) 0.017(4) -0.007(3) 0.009(4) C55 0.071(4) 0.128(7) 0.078(4) 0.004(4) 0.007(3) -0.036(5) C32 0.058(4) 0.095(5) 0.116(5) 0.051(4) -0.006(4) -0.005(4) C26 0.056(3) 0.098(5) 0.064(3) 0.020(3) -0.005(3) 0.002(3) C81 0.071(4) 0.121(6) 0.048(3) 0.008(3) 0.005(3) 0.012(4) C65 0.107(6) 0.080(5) 0.096(5) -0.031(4) 0.048(5) -0.020(4) C44 0.114(6) 0.083(5) 0.089(5) 0.023(4) 0.039(4) 0.015(4) C66 0.079(4) 0.075(4) 0.070(4) -0.015(3) 0.018(3) -0.014(3) C33 0.070(5) 0.156(10) 0.149(9) 0.102(8) 0.009(5) 0.004(6) C23 0.102(5) 0.085(5) 0.049(3) 0.012(3) -0.006(3) -0.001(4) C24 0.076(4) 0.089(5) 0.063(4) 0.014(3) -0.018(3) 0.007(4) C69 0.067(4) 0.089(5) 0.102(5) 0.014(4) -0.006(3) 0.003(4) C82 0.076(4) 0.141(7) 0.054(3) 0.026(4) 0.018(3) 0.023(5) C25 0.064(4) 0.120(6) 0.087(5) 0.031(4) -0.010(3) 0.018(4) C64 0.151(8) 0.118(7) 0.062(4) -0.027(4) 0.021(5) -0.034(6) C45 0.113(6) 0.099(6) 0.075(4) 0.034(4) 0.027(4) 0.010(5) C54 0.059(4) 0.155(8) 0.065(4) 0.014(4) -0.001(3) -0.006(5) C14 0.111(6) 0.079(5) 0.130(6) -0.037(5) -0.048(5) 0.003(5) C15 0.104(6) 0.094(6) 0.120(6) -0.032(5) -0.056(5) 0.001(5) C80 0.088(5) 0.151(8) 0.056(4) -0.005(4) 0.020(3) 0.027(5) C35 0.050(4) 0.200(10) 0.066(4) 0.023(5) 0.008(3) 0.005(5) C78 0.107(6) 0.104(6) 0.077(4) -0.025(4) 0.024(4) -0.001(4) C70 0.068(4) 0.098(6) 0.103(5) 0.030(4) -0.011(4) 0.006(4) C34 0.052(5) 0.248(15) 0.101(7) 0.090(8) 0.007(4) -0.005(7) C79 0.134(7) 0.122(7) 0.072(5) -0.017(5) 0.023(4) 0.024(6) C63 0.115(7) 0.191(10) 0.073(5) -0.061(6) -0.020(4) 0.011(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C42 2.002(5) . ? Pd1 N1 2.151(4) . ? Pd1 P1 2.3014(15) . ? Pd1 S1 2.3600(15) . ? Pd1 Pd2 2.7375(7) . ? Pd2 C12 1.996(5) . ? Pd2 N2 2.160(4) . ? Pd2 P2 2.3054(15) . ? Pd2 S2 2.3663(16) . ? P1 C21 1.825(5) . ? P1 C31 1.825(6) . ? P1 C11 1.830(6) . ? P2 C41 1.815(6) . ? P2 C51 1.826(5) . ? P2 C61 1.827(5) . ? S1 C75 1.726(6) . ? S2 C84 1.726(7) . ? N2 C75 1.347(7) . ? N2 C67 1.388(7) . ? N1 C84 1.331(8) . ? N1 C76 1.410(7) . ? C36 C31 1.381(9) . ? C36 C35 1.400(9) . ? C41 C46 1.401(7) . ? C41 C42 1.417(7) . ? C12 C11 1.381(8) . ? C12 C13 1.406(9) . ? C42 C43 1.383(8) . ? C21 C26 1.369(8) . ? C21 C22 1.398(8) . ? C67 C68 1.397(8) . ? C67 C72 1.403(7) . ? C52 C53 1.363(8) . ? C52 C51 1.388(8) . ? C51 C56 1.386(8) . ? C11 C16 1.420(7) . ? C75 C74 1.417(7) . ? C72 C71 1.406(9) . ? C72 C73 1.415(9) . ? C76 C77 1.356(9) . ? C76 C81 1.405(8) . ? C61 C66 1.364(8) . ? C61 C62 1.367(9) . ? C46 C45 1.370(10) . ? C74 C73 1.319(9) . ? C31 C32 1.368(9) . ? C83 C82 1.346(10) . ? C83 C84 1.454(8) . ? C77 C78 1.380(9) . ? C56 C55 1.408(9) . ? C53 C54 1.374(11) . ? C22 C23 1.390(8) . ? C43 C44 1.374(8) . ? C68 C69 1.363(9) . ? C16 C15 1.370(10) . ? C62 C63 1.384(10) . ? C13 C14 1.369(9) . ? C71 C70 1.360(11) . ? C55 C54 1.365(11) . ? C32 C33 1.379(12) . ? C26 C25 1.409(8) . ? C81 C82 1.402(11) . ? C81 C80 1.423(11) . ? C65 C64 1.369(12) . ? C65 C66 1.383(9) . ? C44 C45 1.380(10) . ? C33 C34 1.317(16) . ? C23 C24 1.351(9) . ? C24 C25 1.373(9) . ? C69 C70 1.415(10) . ? C64 C63 1.322(12) . ? C14 C15 1.399(11) . ? C80 C79 1.330(12) . ? C35 C34 1.384(16) . ? C78 C79 1.400(11) . ? 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 C42 Pd1 N1 174.5(2) . . ? C42 Pd1 P1 89.32(15) . . ? N1 Pd1 P1 93.59(12) . . ? C42 Pd1 S1 85.01(15) . . ? N1 Pd1 S1 92.60(11) . . ? P1 Pd1 S1 171.46(5) . . ? C42 Pd1 Pd2 96.41(16) . . ? N1 Pd1 Pd2 88.45(13) . . ? P1 Pd1 Pd2 87.45(4) . . ? S1 Pd1 Pd2 86.84(4) . . ? C12 Pd2 N2 175.9(2) . . ? C12 Pd2 P2 86.69(17) . . ? N2 Pd2 P2 95.11(11) . . ? C12 Pd2 S2 86.69(18) . . ? N2 Pd2 S2 91.92(11) . . ? P2 Pd2 S2 170.81(5) . . ? C12 Pd2 Pd1 93.71(17) . . ? N2 Pd2 Pd1 90.16(12) . . ? P2 Pd2 Pd1 85.59(4) . . ? S2 Pd2 Pd1 88.48(5) . . ? C21 P1 C31 103.3(2) . . ? C21 P1 C11 102.9(2) . . ? C31 P1 C11 105.9(3) . . ? C21 P1 Pd1 122.18(19) . . ? C31 P1 Pd1 111.69(18) . . ? C11 P1 Pd1 109.51(18) . . ? C41 P2 C51 105.2(3) . . ? C41 P2 C61 102.8(2) . . ? C51 P2 C61 103.6(3) . . ? C41 P2 Pd2 112.75(17) . . ? C51 P2 Pd2 112.06(17) . . ? C61 P2 Pd2 119.0(2) . . ? C75 S1 Pd1 109.92(18) . . ? C84 S2 Pd2 108.2(2) . . ? C75 N2 C67 118.5(4) . . ? C75 N2 Pd2 123.2(3) . . ? C67 N2 Pd2 118.2(4) . . ? C84 N1 C76 119.4(5) . . ? C84 N1 Pd1 124.7(4) . . ? C76 N1 Pd1 115.3(4) . . ? C31 C36 C35 119.8(8) . . ? C46 C41 C42 119.2(5) . . ? C46 C41 P2 119.8(4) . . ? C42 C41 P2 120.8(4) . . ? C11 C12 C13 117.4(5) . . ? C11 C12 Pd2 125.4(4) . . ? C13 C12 Pd2 117.1(4) . . ? C43 C42 C41 117.7(5) . . ? C43 C42 Pd1 119.3(4) . . ? C41 C42 Pd1 123.0(4) . . ? C26 C21 C22 117.7(5) . . ? C26 C21 P1 123.6(4) . . ? C22 C21 P1 118.7(4) . . ? N2 C67 C68 119.6(5) . . ? N2 C67 C72 122.1(6) . . ? C68 C67 C72 118.3(5) . . ? C53 C52 C51 122.0(6) . . ? C56 C51 C52 118.2(5) . . ? C56 C51 P2 123.1(5) . . ? C52 C51 P2 118.6(5) . . ? C12 C11 C16 119.6(6) . . ? C12 C11 P1 121.5(4) . . ? C16 C11 P1 118.9(5) . . ? N2 C75 C74 120.3(5) . . ? N2 C75 S1 123.9(4) . . ? C74 C75 S1 115.7(5) . . ? C67 C72 C71 119.8(6) . . ? C67 C72 C73 117.2(6) . . ? C71 C72 C73 123.0(6) . . ? C77 C76 C81 119.3(6) . . ? C77 C76 N1 119.3(5) . . ? C81 C76 N1 121.4(6) . . ? C66 C61 C62 116.6(6) . . ? C66 C61 P2 123.2(5) . . ? C62 C61 P2 119.9(5) . . ? C45 C46 C41 120.2(6) . . ? C73 C74 C75 121.7(6) . . ? C32 C31 C36 118.2(6) . . ? C32 C31 P1 123.8(6) . . ? C36 C31 P1 118.0(5) . . ? C82 C83 C84 120.1(7) . . ? C76 C77 C78 121.6(6) . . ? C74 C73 C72 120.2(5) . . ? C51 C56 C55 119.9(7) . . ? C52 C53 C54 119.3(7) . . ? C23 C22 C21 120.2(6) . . ? C44 C43 C42 123.1(6) . . ? C69 C68 C67 121.9(6) . . ? N1 C84 C83 120.1(6) . . ? N1 C84 S2 124.8(4) . . ? C83 C84 S2 115.1(5) . . ? C15 C16 C11 121.2(6) . . ? C61 C62 C63 121.5(8) . . ? C14 C13 C12 123.3(7) . . ? C70 C71 C72 120.7(6) . . ? C54 C55 C56 119.4(7) . . ? C31 C32 C33 121.4(9) . . ? C21 C26 C25 121.3(6) . . ? C82 C81 C76 117.8(6) . . ? C82 C81 C80 124.2(7) . . ? C76 C81 C80 117.9(7) . . ? C64 C65 C66 119.3(7) . . ? C43 C44 C45 118.2(7) . . ? C61 C66 C65 121.9(7) . . ? C34 C33 C32 120.8(10) . . ? C24 C23 C22 121.7(6) . . ? C23 C24 C25 119.2(6) . . ? C68 C69 C70 119.4(7) . . ? C83 C82 C81 121.0(6) . . ? C24 C25 C26 119.9(6) . . ? C63 C64 C65 119.7(7) . . ? C46 C45 C44 121.4(6) . . ? C55 C54 C53 121.1(7) . . ? C13 C14 C15 118.7(7) . . ? C16 C15 C14 119.5(6) . . ? C79 C80 C81 122.1(7) . . ? C34 C35 C36 119.3(9) . . ? C77 C78 C79 119.9(8) . . ? C71 C70 C69 120.0(7) . . ? C33 C34 C35 120.4(9) . . ? C80 C79 C78 119.2(8) . . ? C64 C63 C62 120.8(8) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.373 _refine_diff_density_min -0.459 _refine_diff_density_rms 0.077 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.225 0.840 0.207 286 21 ' ' 2 -0.275 0.340 0.293 286 21 ' ' 3 0.275 0.660 0.707 286 21 ' ' 4 0.225 0.160 0.793 286 21 ' ' _platon_squeeze_details ; ; #=========================================== _database_code_depnum_ccdc_archive 'CCDC 941942' ####################################################################### # # 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_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H38 Cl4 N4 P2 Pd2 S2' _chemical_formula_weight 1127.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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 P2(1)/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 10.2320(4) _cell_length_b 12.8480(4) _cell_length_c 35.2620(11) _cell_angle_alpha 90.00 _cell_angle_beta 94.4200(13) _cell_angle_gamma 90.00 _cell_volume 4621.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour ? _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.620 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2256 _exptl_absorpt_coefficient_mu 1.207 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 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_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14381 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_sigmaI/netI 0.1017 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 27.47 _reflns_number_total 10531 _reflns_number_gt 5914 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect(Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo and Scalepack(Otwinowski & Minor1997)' _computing_data_reduction 'Denzo and Scalepack(Otwinowski & Minor1997)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0810P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0042(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10531 _refine_ls_number_parameters 542 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1215 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1678 _refine_ls_wR_factor_gt 0.1248 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 Pd1 Pd 0.60145(5) 0.78578(4) 0.155816(13) 0.02992(15) Uani 1 1 d . . . P1 P 0.67472(17) 0.95115(12) 0.14410(5) 0.0324(4) Uani 1 1 d . . . N3 N 0.6503(7) 0.4431(5) 0.1848(2) 0.0641(19) Uani 1 1 d . . . C1 C 0.6743(7) 0.5406(5) 0.17327(19) 0.0416(16) Uani 1 1 d . . . S1 S 0.53350(17) 0.61228(13) 0.16020(5) 0.0387(4) Uani 1 1 d . . . Cl1 Cl 0.2837(3) 0.8745(2) 0.18441(7) 0.0844(7) Uani 1 1 d . . . Pd2 Pd 0.84897(5) 0.72303(4) 0.143899(13) 0.02967(15) Uani 1 1 d . . . P2 P 0.76423(17) 0.67440(13) 0.08442(5) 0.0327(4) Uani 1 1 d . . . S2 S 0.92783(16) 0.79352(13) 0.20269(5) 0.0383(4) Uani 1 1 d . . . N2 N 0.7965(5) 0.5815(4) 0.17215(14) 0.0387(13) Uani 1 1 d . . . C2 C 0.8960(7) 0.5227(5) 0.18647(18) 0.0442(17) Uani 1 1 d . . . H2A H 0.9804 0.5499 0.1874 0.053 Uiso 1 1 calc R . . Cl2 Cl 0.2507(4) 1.0753(3) 0.21692(15) 0.193(2) Uani 1 1 d . . . N1 N 0.6700(5) 0.7885(4) 0.21588(14) 0.0344(12) Uani 1 1 d . . . C3 C 0.8788(9) 0.4237(6) 0.1998(2) 0.065(2) Uani 1 1 d . . . H3A H 0.9484 0.3841 0.2104 0.078 Uiso 1 1 calc R . . Cl3 Cl 0.1765(3) 0.5813(3) 0.12704(9) 0.1229(11) Uani 1 1 d . . . N4 N 0.8276(6) 0.8263(5) 0.26697(16) 0.0519(16) Uani 1 1 d . . . C4 C 0.7537(9) 0.3871(7) 0.1965(3) 0.076(3) Uani 1 1 d . . . H4B H 0.7402 0.3180 0.2030 0.091 Uiso 1 1 calc R . . Cl4 Cl 0.2142(4) 0.4306(3) 0.06726(15) 0.196(2) Uani 1 1 d . . . C5 C 0.7950(7) 0.8026(5) 0.22995(18) 0.0371(15) Uani 1 1 d . . . C6 C 0.7302(8) 0.8347(7) 0.2896(2) 0.057(2) Uani 1 1 d . . . H6A H 0.7504 0.8558 0.3146 0.068 Uiso 1 1 calc R . . C7 C 0.6022(8) 0.8142(6) 0.27824(19) 0.0517(19) Uani 1 1 d . . . H7A H 0.5367 0.8160 0.2951 0.062 Uiso 1 1 calc R . . C8 C 0.5758(7) 0.7908(5) 0.24053(19) 0.0445(17) Uani 1 1 d . . . H8A H 0.4899 0.7760 0.2316 0.053 Uiso 1 1 calc R . . C9 C 0.2786(11) 0.5284(10) 0.0959(3) 0.115(4) Uani 1 1 d . . . H9A H 0.3073 0.5837 0.0797 0.138 Uiso 1 1 calc R . . H9B H 0.3557 0.5016 0.1104 0.138 Uiso 1 1 calc R . . C10 C 0.1771(10) 0.9722(7) 0.1952(3) 0.089(3) Uani 1 1 d . . . H10A H 0.1297 0.9955 0.1718 0.106 Uiso 1 1 calc R . . H10B H 0.1136 0.9440 0.2114 0.106 Uiso 1 1 calc R . . C11 C 0.8281(6) 0.9490(5) 0.12018(17) 0.0362(15) Uani 1 1 d . . . C12 C 0.9044(6) 0.8586(4) 0.12084(16) 0.0295(13) Uani 1 1 d . . . C13 C 1.0266(7) 0.8651(5) 0.10635(19) 0.0401(16) Uani 1 1 d . . . H13A H 1.0781 0.8056 0.1058 0.048 Uiso 1 1 calc R . . C14 C 1.0738(7) 0.9577(5) 0.09272(19) 0.0448(17) Uani 1 1 d . . . H14A H 1.1578 0.9608 0.0845 0.054 Uiso 1 1 calc R . . C15 C 0.9956(8) 1.0455(5) 0.0914(2) 0.0487(18) Uani 1 1 d . . . H15A H 1.0257 1.1075 0.0816 0.058 Uiso 1 1 calc R . . C16 C 0.8723(7) 1.0405(5) 0.10485(19) 0.0419(16) Uani 1 1 d . . . H16A H 0.8187 1.0991 0.1036 0.050 Uiso 1 1 calc R . . C21 C 0.5643(7) 1.0363(5) 0.11454(19) 0.0390(16) Uani 1 1 d . . . C22 C 0.5512(8) 1.0228(5) 0.0756(2) 0.052(2) Uani 1 1 d . . . H22A H 0.6043 0.9747 0.0644 0.063 Uiso 1 1 calc R . . C23 C 0.4611(8) 1.0792(6) 0.0528(2) 0.060(2) Uani 1 1 d . . . H23A H 0.4557 1.0706 0.0265 0.072 Uiso 1 1 calc R . . C24 C 0.3791(9) 1.1482(7) 0.0692(3) 0.070(3) Uani 1 1 d . . . H24A H 0.3168 1.1851 0.0540 0.084 Uiso 1 1 calc R . . C25 C 0.3891(9) 1.1624(7) 0.1078(3) 0.075(3) Uani 1 1 d . . . H25A H 0.3339 1.2092 0.1188 0.090 Uiso 1 1 calc R . . C26 C 0.4832(8) 1.1062(6) 0.1308(2) 0.056(2) Uani 1 1 d . . . H26A H 0.4906 1.1163 0.1569 0.067 Uiso 1 1 calc R . . C31 C 0.7155(7) 1.0269(5) 0.18752(18) 0.0366(15) Uani 1 1 d . . . C32 C 0.6252(7) 1.0295(5) 0.21494(19) 0.0444(17) Uani 1 1 d . . . H32A H 0.5447 0.9966 0.2100 0.053 Uiso 1 1 calc R . . C33 C 0.6512(9) 1.0794(6) 0.2494(2) 0.057(2) Uani 1 1 d . . . H33A H 0.5893 1.0803 0.2673 0.068 Uiso 1 1 calc R . . C34 C 0.7711(9) 1.1279(6) 0.2566(2) 0.058(2) Uani 1 1 d . . . H34A H 0.7898 1.1618 0.2797 0.069 Uiso 1 1 calc R . . C35 C 0.8634(9) 1.1267(6) 0.2300(2) 0.061(2) Uani 1 1 d . . . H35A H 0.9434 1.1603 0.2349 0.074 Uiso 1 1 calc R . . C36 C 0.8347(7) 1.0744(5) 0.1957(2) 0.0458(17) Uani 1 1 d . . . H36A H 0.8975 1.0717 0.1780 0.055 Uiso 1 1 calc R . . C41 C 0.6060(6) 0.7329(5) 0.07236(17) 0.0335(14) Uani 1 1 d . . . C42 C 0.5344(6) 0.7768(5) 0.10092(17) 0.0323(14) Uani 1 1 d . . . C43 C 0.4064(7) 0.8090(5) 0.09062(18) 0.0398(16) Uani 1 1 d . . . H43A H 0.3569 0.8370 0.1092 0.048 Uiso 1 1 calc R . . C44 C 0.3500(7) 0.8005(5) 0.0534(2) 0.0490(19) Uani 1 1 d . . . H44A H 0.2636 0.8212 0.0477 0.059 Uiso 1 1 calc R . . C45 C 0.4219(8) 0.7616(6) 0.0253(2) 0.0507(19) Uani 1 1 d . . . H45A H 0.3856 0.7574 0.0003 0.061 Uiso 1 1 calc R . . C46 C 0.5480(7) 0.7291(5) 0.03457(18) 0.0450(17) Uani 1 1 d . . . H46A H 0.5971 0.7037 0.0154 0.054 Uiso 1 1 calc R . . C51 C 0.8635(6) 0.7063(5) 0.04490(17) 0.0356(15) Uani 1 1 d . . . C52 C 0.8565(8) 0.8050(5) 0.02902(19) 0.0476(18) Uani 1 1 d . . . H52A H 0.7954 0.8522 0.0370 0.057 Uiso 1 1 calc R . . C53 C 0.9393(8) 0.8349(6) 0.0014(2) 0.056(2) Uani 1 1 d . . . H53A H 0.9335 0.9013 -0.0091 0.067 Uiso 1 1 calc R . . C54 C 1.0296(8) 0.7650(7) -0.0101(2) 0.059(2) Uani 1 1 d . . . H54A H 1.0857 0.7846 -0.0284 0.071 Uiso 1 1 calc R . . C55 C 1.0386(8) 0.6668(7) 0.0050(2) 0.062(2) Uani 1 1 d . . . H55A H 1.0996 0.6198 -0.0032 0.075 Uiso 1 1 calc R . . C56 C 0.9558(7) 0.6379(6) 0.0325(2) 0.0497(19) Uani 1 1 d . . . H56A H 0.9625 0.5714 0.0428 0.060 Uiso 1 1 calc R . . C61 C 0.7340(7) 0.5327(5) 0.08043(18) 0.0356(15) Uani 1 1 d . . . C62 C 0.8322(7) 0.4652(5) 0.09468(19) 0.0437(17) Uani 1 1 d . . . H62A H 0.9125 0.4916 0.1044 0.052 Uiso 1 1 calc R . . C63 C 0.8111(9) 0.3609(6) 0.0944(2) 0.057(2) Uani 1 1 d . . . H63A H 0.8776 0.3166 0.1039 0.069 Uiso 1 1 calc R . . C64 C 0.6931(9) 0.3194(6) 0.0802(2) 0.063(2) Uani 1 1 d . . . H64A H 0.6794 0.2478 0.0802 0.075 Uiso 1 1 calc R . . C65 C 0.5961(8) 0.3861(6) 0.0661(2) 0.060(2) Uani 1 1 d . . . H65A H 0.5161 0.3589 0.0564 0.072 Uiso 1 1 calc R . . C66 C 0.6147(7) 0.4926(5) 0.0660(2) 0.0457(17) Uani 1 1 d . . . H66A H 0.5480 0.5367 0.0565 0.055 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 0.0265(3) 0.0355(3) 0.0277(3) 0.0006(2) 0.00133(19) 0.0014(2) P1 0.0323(9) 0.0337(8) 0.0310(9) 0.0003(7) 0.0024(7) 0.0024(7) N3 0.049(4) 0.051(4) 0.093(5) 0.036(4) 0.007(4) -0.005(3) C1 0.036(4) 0.047(4) 0.042(4) 0.011(3) 0.005(3) -0.002(3) S1 0.0313(9) 0.0404(9) 0.0441(10) 0.0054(7) 0.0001(7) -0.0021(8) Cl1 0.0736(17) 0.0905(17) 0.0875(18) -0.0081(13) -0.0042(13) 0.0224(14) Pd2 0.0260(3) 0.0332(3) 0.0297(3) 0.0018(2) 0.00187(19) 0.0009(2) P2 0.0327(9) 0.0355(9) 0.0301(8) -0.0026(7) 0.0039(7) 0.0013(8) S2 0.0308(9) 0.0502(10) 0.0334(9) -0.0005(7) -0.0013(7) -0.0032(8) N2 0.037(3) 0.043(3) 0.037(3) 0.007(2) 0.006(2) -0.002(3) C2 0.039(4) 0.053(4) 0.040(4) 0.010(3) 0.001(3) 0.008(4) Cl2 0.153(4) 0.122(3) 0.322(6) -0.124(3) 0.122(4) -0.067(3) N1 0.033(3) 0.041(3) 0.029(3) 0.000(2) 0.003(2) -0.003(3) C3 0.055(6) 0.065(6) 0.073(6) 0.024(4) 0.003(4) 0.013(5) Cl3 0.071(2) 0.178(3) 0.120(3) -0.022(2) 0.0137(17) -0.011(2) N4 0.044(4) 0.076(4) 0.036(3) -0.006(3) 0.003(3) -0.007(3) C4 0.062(6) 0.058(5) 0.106(8) 0.033(5) 0.004(5) 0.012(5) Cl4 0.120(3) 0.135(3) 0.315(6) -0.121(4) -0.095(4) 0.050(3) C5 0.037(4) 0.041(4) 0.033(4) 0.002(3) 0.001(3) 0.003(3) C6 0.053(5) 0.088(6) 0.030(4) -0.010(4) 0.004(3) 0.003(5) C7 0.050(5) 0.073(5) 0.034(4) 0.006(4) 0.014(3) 0.005(4) C8 0.036(4) 0.059(5) 0.039(4) 0.007(3) 0.007(3) 0.002(4) C9 0.081(8) 0.143(11) 0.120(10) -0.059(8) 0.008(7) -0.015(8) C10 0.075(7) 0.076(7) 0.116(9) -0.015(6) 0.015(6) -0.003(6) C11 0.034(4) 0.041(4) 0.034(4) 0.003(3) 0.006(3) -0.003(3) C12 0.031(3) 0.027(3) 0.031(3) 0.002(2) 0.003(3) -0.007(3) C13 0.036(4) 0.036(4) 0.048(4) 0.002(3) 0.006(3) -0.001(3) C14 0.038(4) 0.051(4) 0.047(4) -0.001(3) 0.009(3) -0.004(4) C15 0.053(5) 0.042(4) 0.053(5) 0.003(3) 0.012(4) -0.015(4) C16 0.040(4) 0.037(4) 0.049(4) 0.012(3) 0.003(3) 0.000(3) C21 0.035(4) 0.041(4) 0.040(4) 0.004(3) 0.000(3) 0.003(3) C22 0.063(5) 0.043(4) 0.049(5) 0.004(3) -0.003(4) 0.013(4) C23 0.065(6) 0.048(4) 0.063(5) 0.013(4) -0.021(4) 0.003(4) C24 0.051(5) 0.067(6) 0.089(7) 0.027(5) -0.019(5) 0.007(5) C25 0.061(6) 0.077(6) 0.087(7) 0.014(5) 0.008(5) 0.043(5) C26 0.052(5) 0.062(5) 0.053(5) 0.005(4) 0.000(4) 0.020(4) C31 0.038(4) 0.037(3) 0.035(4) -0.002(3) -0.001(3) 0.006(3) C32 0.046(4) 0.046(4) 0.041(4) -0.004(3) 0.000(3) 0.005(3) C33 0.072(6) 0.063(5) 0.035(4) -0.007(4) 0.011(4) 0.020(5) C34 0.077(6) 0.050(5) 0.042(5) -0.016(4) -0.019(4) 0.009(4) C35 0.060(6) 0.057(5) 0.063(6) -0.007(4) -0.020(5) 0.001(4) C36 0.040(4) 0.049(4) 0.047(4) -0.004(3) -0.005(3) 0.003(4) C41 0.036(4) 0.032(3) 0.033(3) -0.006(3) 0.002(3) 0.004(3) C42 0.032(3) 0.036(3) 0.029(3) 0.005(3) 0.003(3) 0.002(3) C43 0.036(4) 0.049(4) 0.034(4) -0.002(3) -0.001(3) 0.008(3) C44 0.038(4) 0.059(5) 0.047(4) 0.002(4) -0.011(3) 0.012(4) C45 0.049(5) 0.066(5) 0.034(4) -0.002(3) -0.014(3) 0.009(4) C46 0.050(4) 0.054(4) 0.031(4) -0.002(3) 0.002(3) 0.013(4) C51 0.027(3) 0.047(4) 0.032(3) -0.002(3) -0.005(3) 0.003(3) C52 0.055(5) 0.053(4) 0.036(4) 0.005(3) 0.010(3) 0.005(4) C53 0.067(6) 0.062(5) 0.039(4) 0.001(4) 0.008(4) -0.004(4) C54 0.049(5) 0.084(6) 0.045(5) -0.002(4) 0.013(4) -0.011(5) C55 0.056(5) 0.078(6) 0.057(5) -0.004(4) 0.029(4) 0.012(5) C56 0.052(5) 0.053(4) 0.046(4) 0.001(3) 0.012(4) -0.001(4) C61 0.038(4) 0.035(3) 0.034(4) -0.007(3) 0.007(3) 0.001(3) C62 0.042(4) 0.035(4) 0.054(5) -0.006(3) 0.001(3) 0.003(3) C63 0.061(6) 0.044(4) 0.068(6) 0.004(4) 0.003(4) 0.010(4) C64 0.072(6) 0.037(4) 0.078(6) -0.009(4) 0.008(5) -0.006(4) C65 0.051(5) 0.052(5) 0.075(6) -0.013(4) 0.000(4) -0.015(4) C66 0.043(4) 0.037(4) 0.057(5) 0.000(3) 0.002(4) -0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C42 2.007(6) . ? Pd1 N1 2.180(5) . ? Pd1 P1 2.3009(17) . ? Pd1 S1 2.3438(17) . ? Pd1 Pd2 2.7212(7) . ? P1 C31 1.835(6) . ? P1 C21 1.838(7) . ? P1 C11 1.838(7) . ? N3 C4 1.319(10) . ? N3 C1 1.346(8) . ? C1 N2 1.360(8) . ? C1 S1 1.741(7) . ? Cl1 C10 1.725(9) . ? Pd2 C12 2.022(6) . ? Pd2 N2 2.161(5) . ? Pd2 P2 2.2936(17) . ? Pd2 S2 2.3474(17) . ? P2 C41 1.806(7) . ? P2 C51 1.833(7) . ? P2 C61 1.850(6) . ? S2 C5 1.728(7) . ? N2 C2 1.336(8) . ? C2 C3 1.371(10) . ? C2 H2A 0.9300 . ? Cl2 C10 1.680(9) . ? N1 C5 1.348(8) . ? N1 C8 1.347(8) . ? C3 C4 1.360(12) . ? C3 H3A 0.9300 . ? Cl3 C9 1.714(11) . ? N4 C6 1.329(9) . ? N4 C5 1.357(8) . ? C4 H4B 0.9300 . ? Cl4 C9 1.711(10) . ? C6 C7 1.366(10) . ? C6 H6A 0.9300 . ? C7 C8 1.370(9) . ? C7 H7A 0.9300 . ? C8 H8A 0.9300 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C16 1.385(8) . ? C11 C12 1.399(8) . ? C12 C13 1.388(9) . ? C13 C14 1.383(9) . ? C13 H13A 0.9300 . ? C14 C15 1.382(10) . ? C14 H14A 0.9300 . ? C15 C16 1.382(10) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? C21 C26 1.377(9) . ? C21 C22 1.381(9) . ? C22 C23 1.380(10) . ? C22 H22A 0.9300 . ? C23 C24 1.378(11) . ? C23 H23A 0.9300 . ? C24 C25 1.370(12) . ? C24 H24A 0.9300 . ? C25 C26 1.409(10) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C31 C36 1.375(9) . ? C31 C32 1.388(9) . ? C32 C33 1.381(9) . ? C32 H32A 0.9300 . ? C33 C34 1.382(11) . ? C33 H33A 0.9300 . ? C34 C35 1.381(12) . ? C34 H34A 0.9300 . ? C35 C36 1.396(10) . ? C35 H35A 0.9300 . ? C36 H36A 0.9300 . ? C41 C42 1.408(8) . ? C41 C46 1.417(9) . ? C42 C43 1.394(9) . ? C43 C44 1.395(9) . ? C43 H43A 0.9300 . ? C44 C45 1.375(10) . ? C44 H44A 0.9300 . ? C45 C46 1.372(10) . ? C45 H45A 0.9300 . ? C46 H46A 0.9300 . ? C51 C56 1.385(9) . ? C51 C52 1.386(9) . ? C52 C53 1.393(10) . ? C52 H52A 0.9300 . ? C53 C54 1.372(11) . ? C53 H53A 0.9300 . ? C54 C55 1.370(11) . ? C54 H54A 0.9300 . ? C55 C56 1.386(10) . ? C55 H55A 0.9300 . ? C56 H56A 0.9300 . ? C61 C66 1.385(9) . ? C61 C62 1.391(9) . ? C62 C63 1.357(9) . ? C62 H62A 0.9300 . ? C63 C64 1.378(11) . ? C63 H63A 0.9300 . ? C64 C65 1.375(11) . ? C64 H64A 0.9300 . ? C65 C66 1.381(9) . ? C65 H65A 0.9300 . ? C66 H66A 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 C42 Pd1 N1 177.3(2) . . ? C42 Pd1 P1 88.40(17) . . ? N1 Pd1 P1 94.30(14) . . ? C42 Pd1 S1 85.85(17) . . ? N1 Pd1 S1 91.48(14) . . ? P1 Pd1 S1 172.97(6) . . ? C42 Pd1 Pd2 95.00(18) . . ? N1 Pd1 Pd2 85.47(14) . . ? P1 Pd1 Pd2 85.75(5) . . ? S1 Pd1 Pd2 90.73(5) . . ? C31 P1 C21 104.3(3) . . ? C31 P1 C11 104.1(3) . . ? C21 P1 C11 104.9(3) . . ? C31 P1 Pd1 113.3(2) . . ? C21 P1 Pd1 117.2(2) . . ? C11 P1 Pd1 111.7(2) . . ? C4 N3 C1 116.2(7) . . ? N3 C1 N2 123.9(6) . . ? N3 C1 S1 113.9(5) . . ? N2 C1 S1 122.1(5) . . ? C1 S1 Pd1 106.1(2) . . ? C12 Pd2 N2 176.1(2) . . ? C12 Pd2 P2 87.99(17) . . ? N2 Pd2 P2 95.88(15) . . ? C12 Pd2 S2 86.26(17) . . ? N2 Pd2 S2 89.90(15) . . ? P2 Pd2 S2 173.01(6) . . ? C12 Pd2 Pd1 95.76(18) . . ? N2 Pd2 Pd1 84.88(15) . . ? P2 Pd2 Pd1 86.05(5) . . ? S2 Pd2 Pd1 90.57(5) . . ? C41 P2 C51 105.5(3) . . ? C41 P2 C61 104.5(3) . . ? C51 P2 C61 105.1(3) . . ? C41 P2 Pd2 111.8(2) . . ? C51 P2 Pd2 116.2(2) . . ? C61 P2 Pd2 112.8(2) . . ? C5 S2 Pd2 106.6(2) . . ? C2 N2 C1 116.5(6) . . ? C2 N2 Pd2 116.2(5) . . ? C1 N2 Pd2 126.9(4) . . ? N2 C2 C3 122.7(7) . . ? N2 C2 H2A 118.7 . . ? C3 C2 H2A 118.7 . . ? C5 N1 C8 117.7(6) . . ? C5 N1 Pd1 125.8(4) . . ? C8 N1 Pd1 115.8(4) . . ? C4 C3 C2 115.9(8) . . ? C4 C3 H3A 122.1 . . ? C2 C3 H3A 122.1 . . ? C6 N4 C5 117.2(6) . . ? N3 C4 C3 124.4(8) . . ? N3 C4 H4B 117.8 . . ? C3 C4 H4B 117.8 . . ? N1 C5 N4 122.7(6) . . ? N1 C5 S2 123.4(5) . . ? N4 C5 S2 113.9(5) . . ? N4 C6 C7 123.6(7) . . ? N4 C6 H6A 118.2 . . ? C7 C6 H6A 118.2 . . ? C6 C7 C8 116.2(7) . . ? C6 C7 H7A 121.9 . . ? C8 C7 H7A 121.9 . . ? N1 C8 C7 122.3(7) . . ? N1 C8 H8A 118.9 . . ? C7 C8 H8A 118.9 . . ? Cl4 C9 Cl3 116.3(7) . . ? Cl4 C9 H9A 108.2 . . ? Cl3 C9 H9A 108.2 . . ? Cl4 C9 H9B 108.2 . . ? Cl3 C9 H9B 108.2 . . ? H9A C9 H9B 107.4 . . ? Cl2 C10 Cl1 114.0(6) . . ? Cl2 C10 H10A 108.8 . . ? Cl1 C10 H10A 108.8 . . ? Cl2 C10 H10B 108.8 . . ? Cl1 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? C16 C11 C12 120.8(6) . . ? C16 C11 P1 118.8(5) . . ? C12 C11 P1 120.0(5) . . ? C13 C12 C11 117.4(6) . . ? C13 C12 Pd2 119.3(5) . . ? C11 C12 Pd2 123.2(5) . . ? C14 C13 C12 121.9(6) . . ? C14 C13 H13A 119.1 . . ? C12 C13 H13A 119.1 . . ? C15 C14 C13 119.8(7) . . ? C15 C14 H14A 120.1 . . ? C13 C14 H14A 120.1 . . ? C16 C15 C14 119.5(6) . . ? C16 C15 H15A 120.3 . . ? C14 C15 H15A 120.3 . . ? C15 C16 C11 120.5(6) . . ? C15 C16 H16A 119.8 . . ? C11 C16 H16A 119.8 . . ? C26 C21 C22 118.7(6) . . ? C26 C21 P1 121.1(5) . . ? C22 C21 P1 119.8(5) . . ? C23 C22 C21 121.4(7) . . ? C23 C22 H22A 119.3 . . ? C21 C22 H22A 119.3 . . ? C24 C23 C22 119.7(8) . . ? C24 C23 H23A 120.2 . . ? C22 C23 H23A 120.2 . . ? C25 C24 C23 120.1(7) . . ? C25 C24 H24A 119.9 . . ? C23 C24 H24A 119.9 . . ? C24 C25 C26 119.9(8) . . ? C24 C25 H25A 120.1 . . ? C26 C25 H25A 120.1 . . ? C21 C26 C25 120.2(8) . . ? C21 C26 H26A 119.9 . . ? C25 C26 H26A 119.9 . . ? C36 C31 C32 118.1(6) . . ? C36 C31 P1 123.5(5) . . ? C32 C31 P1 118.2(5) . . ? C33 C32 C31 122.0(7) . . ? C33 C32 H32A 119.0 . . ? C31 C32 H32A 119.0 . . ? C32 C33 C34 118.7(8) . . ? C32 C33 H33A 120.6 . . ? C34 C33 H33A 120.6 . . ? C35 C34 C33 120.8(7) . . ? C35 C34 H34A 119.6 . . ? C33 C34 H34A 119.6 . . ? C34 C35 C36 119.1(8) . . ? C34 C35 H35A 120.5 . . ? C36 C35 H35A 120.5 . . ? C31 C36 C35 121.3(7) . . ? C31 C36 H36A 119.4 . . ? C35 C36 H36A 119.4 . . ? C42 C41 C46 118.9(6) . . ? C42 C41 P2 120.3(5) . . ? C46 C41 P2 120.6(5) . . ? C43 C42 C41 117.5(6) . . ? C43 C42 Pd1 118.6(5) . . ? C41 C42 Pd1 123.7(5) . . ? C42 C43 C44 122.3(6) . . ? C42 C43 H43A 118.9 . . ? C44 C43 H43A 118.9 . . ? C45 C44 C43 120.1(7) . . ? C45 C44 H44A 120.0 . . ? C43 C44 H44A 120.0 . . ? C46 C45 C44 119.0(7) . . ? C46 C45 H45A 120.5 . . ? C44 C45 H45A 120.5 . . ? C45 C46 C41 122.1(7) . . ? C45 C46 H46A 119.0 . . ? C41 C46 H46A 119.0 . . ? C56 C51 C52 117.9(7) . . ? C56 C51 P2 122.0(5) . . ? C52 C51 P2 119.8(5) . . ? C51 C52 C53 121.3(7) . . ? C51 C52 H52A 119.3 . . ? C53 C52 H52A 119.3 . . ? C54 C53 C52 119.0(7) . . ? C54 C53 H53A 120.5 . . ? C52 C53 H53A 120.5 . . ? C53 C54 C55 121.0(8) . . ? C53 C54 H54A 119.5 . . ? C55 C54 H54A 119.5 . . ? C54 C55 C56 119.4(8) . . ? C54 C55 H55A 120.3 . . ? C56 C55 H55A 120.3 . . ? C51 C56 C55 121.3(7) . . ? C51 C56 H56A 119.3 . . ? C55 C56 H56A 119.3 . . ? C66 C61 C62 119.5(6) . . ? C66 C61 P2 122.1(5) . . ? C62 C61 P2 118.3(5) . . ? C63 C62 C61 120.2(7) . . ? C63 C62 H62A 119.9 . . ? C61 C62 H62A 119.9 . . ? C62 C63 C64 121.3(8) . . ? C62 C63 H63A 119.3 . . ? C64 C63 H63A 119.3 . . ? C65 C64 C63 118.5(7) . . ? C65 C64 H64A 120.7 . . ? C63 C64 H64A 120.7 . . ? C64 C65 C66 121.5(8) . . ? C64 C65 H65A 119.3 . . ? C66 C65 H65A 119.3 . . ? C61 C66 C65 119.1(7) . . ? C61 C66 H66A 120.5 . . ? C65 C66 H66A 120.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.178 _refine_diff_density_min -0.955 _refine_diff_density_rms 0.298 _database_code_depnum_ccdc_archive 'CCDC 941943' ####################################################################### # # 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_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H40 Cl2 N4 P2 Pd2 S2' _chemical_formula_weight 1046.57 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0150(4) _cell_length_b 11.7990(5) _cell_length_c 18.9040(7) _cell_angle_alpha 84.0930(17) _cell_angle_beta 74.7700(18) _cell_angle_gamma 64.9740(19) _cell_volume 2147.93(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.631 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1060 _exptl_absorpt_coefficient_mu 1.174 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 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_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13427 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.0751 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.12 _diffrn_reflns_theta_max 27.47 _reflns_number_total 9381 _reflns_number_gt 7214 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect(Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo and Scalepack(Otwinowski & Minor1997)' _computing_data_reduction 'Denzo and Scalepack(Otwinowski & Minor1997)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0975P)^2^+2.8207P] 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 9381 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0841 _refine_ls_R_factor_gt 0.0610 _refine_ls_wR_factor_ref 0.1699 _refine_ls_wR_factor_gt 0.1559 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.002 _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 0.21501(4) 0.30899(3) 0.762343(19) 0.03659(12) Uani 1 1 d . . . P1 P 0.32476(13) 0.16243(12) 0.66917(7) 0.0396(3) Uani 1 1 d . . . S1 S 0.09223(16) 0.45079(14) 0.86425(8) 0.0520(3) Uani 1 1 d . . . N2 N -0.1269(5) 0.4659(4) 0.8130(2) 0.0425(9) Uani 1 1 d . . . C3 C -0.0745(6) 0.5035(5) 0.8578(3) 0.0435(11) Uani 1 1 d . . . Cl1 Cl 0.6571(4) 0.4025(6) 0.6804(3) 0.197(2) Uani 1 1 d . . . Pd2 Pd -0.02670(4) 0.30750(3) 0.740995(19) 0.03648(12) Uani 1 1 d . . . P2 P -0.00826(14) 0.16923(12) 0.83617(7) 0.0417(3) Uani 1 1 d . . . S2 S -0.02689(16) 0.43901(14) 0.63597(7) 0.0506(3) Uani 1 1 d . . . C8 C -0.2649(5) 0.5377(4) 0.8286(3) 0.0406(10) Uani 1 1 d . . . H8A H -0.3258 0.5315 0.8048 0.049 Uiso 1 1 calc R . . C4 C -0.1847(9) 0.6645(8) 0.9598(4) 0.097(3) Uani 1 1 d . . . H4A H -0.0922 0.6386 0.9648 0.145 Uiso 1 1 calc R . . H4B H -0.2403 0.6477 1.0043 0.145 Uiso 1 1 calc R . . H4C H -0.2230 0.7526 0.9500 0.145 Uiso 1 1 calc R . . Cl2 Cl 0.4580(5) 0.3967(6) 0.8070(3) 0.207(2) Uani 1 1 d . . . C1 C 0.0910(5) 0.4942(5) 0.6421(3) 0.0410(10) Uani 1 1 d . . . C9 C -0.2992(5) 0.6139(5) 0.8797(3) 0.0486(12) Uani 1 1 d . . . H9A H -0.3881 0.6717 0.9003 0.058 Uiso 1 1 calc R . . N6 N -0.1826(5) 0.5959(4) 0.8993(2) 0.0567(12) Uani 1 1 d . . . C2 C 0.0644(9) 0.6426(7) 0.5356(4) 0.076(2) Uani 1 1 d . . . H2A H 0.1012 0.7030 0.5160 0.114 Uiso 1 1 calc R . . H2B H -0.0346 0.6836 0.5500 0.114 Uiso 1 1 calc R . . H2C H 0.0916 0.5802 0.4989 0.114 Uiso 1 1 calc R . . N1 N 0.1739(4) 0.4620(4) 0.6879(2) 0.0398(9) Uani 1 1 d . . . C5 C 0.5157(12) 0.4887(14) 0.7461(6) 0.134(4) Uani 1 1 d . . . H5A H 0.5391 0.5407 0.7718 0.160 Uiso 1 1 calc R . . H5B H 0.4427 0.5433 0.7230 0.160 Uiso 1 1 calc R . . C6 C 0.2474(5) 0.5323(4) 0.6713(3) 0.0402(10) Uani 1 1 d . . . H6A H 0.3130 0.5283 0.6952 0.048 Uiso 1 1 calc R . . C7 C 0.2142(6) 0.6051(5) 0.6181(3) 0.0456(12) Uani 1 1 d . . . H7A H 0.2505 0.6622 0.5967 0.055 Uiso 1 1 calc R . . N5 N 0.1171(5) 0.5835(4) 0.5988(2) 0.0524(11) Uani 1 1 d . . . C11 C 0.2127(6) 0.1008(5) 0.6470(3) 0.0453(11) Uani 1 1 d . . . C12 C 0.0697(5) 0.1590(5) 0.6725(3) 0.0406(10) Uani 1 1 d . . . C13 C -0.0100(6) 0.1144(6) 0.6477(3) 0.0561(14) Uani 1 1 d . . . H13A H -0.1056 0.1523 0.6645 0.067 Uiso 1 1 calc R . . C14 C 0.0480(7) 0.0157(7) 0.5991(4) 0.0688(18) Uani 1 1 d . . . H14A H -0.0081 -0.0097 0.5816 0.083 Uiso 1 1 calc R . . C15 C 0.1902(8) -0.0456(7) 0.5762(4) 0.0728(19) Uani 1 1 d . . . H15A H 0.2304 -0.1149 0.5451 0.087 Uiso 1 1 calc R . . C16 C 0.2718(7) -0.0028(6) 0.6001(4) 0.0609(15) Uani 1 1 d . . . H16A H 0.3674 -0.0436 0.5846 0.073 Uiso 1 1 calc R . . C21 C 0.3834(5) 0.2342(5) 0.5843(3) 0.0466(12) Uani 1 1 d . . . C22 C 0.4740(7) 0.2878(6) 0.5841(3) 0.0569(14) Uani 1 1 d . . . H22A H 0.5010 0.2875 0.6268 0.068 Uiso 1 1 calc R . . C23 C 0.5241(7) 0.3405(6) 0.5228(4) 0.0682(18) Uani 1 1 d . . . H23A H 0.5870 0.3735 0.5233 0.082 Uiso 1 1 calc R . . C24 C 0.4819(9) 0.3452(7) 0.4600(4) 0.079(2) Uani 1 1 d . . . H24A H 0.5171 0.3806 0.4179 0.094 Uiso 1 1 calc R . . C25 C 0.3873(9) 0.2975(8) 0.4592(4) 0.080(2) Uani 1 1 d . . . H25A H 0.3558 0.3040 0.4172 0.096 Uiso 1 1 calc R . . C26 C 0.3391(7) 0.2397(6) 0.5213(3) 0.0630(16) Uani 1 1 d . . . H26A H 0.2776 0.2051 0.5205 0.076 Uiso 1 1 calc R . . C31 C 0.4799(6) 0.0197(5) 0.6782(3) 0.0516(13) Uani 1 1 d . . . C32 C 0.4647(7) -0.0701(6) 0.7265(4) 0.0678(17) Uani 1 1 d . . . H32A H 0.3767 -0.0583 0.7540 0.081 Uiso 1 1 calc R . . C33 C 0.5757(8) -0.1777(7) 0.7355(5) 0.079(2) Uani 1 1 d . . . H33A H 0.5617 -0.2366 0.7694 0.095 Uiso 1 1 calc R . . C34 C 0.7018(10) -0.1984(8) 0.6968(6) 0.100(3) Uani 1 1 d . . . H34A H 0.7765 -0.2712 0.7034 0.119 Uiso 1 1 calc R . . C35 C 0.7216(9) -0.1091(10) 0.6456(8) 0.134(5) Uani 1 1 d . . . H35A H 0.8099 -0.1223 0.6180 0.161 Uiso 1 1 calc R . . C36 C 0.6080(7) -0.0002(7) 0.6361(5) 0.086(2) Uani 1 1 d . . . H36A H 0.6201 0.0583 0.6013 0.103 Uiso 1 1 calc R . . C41 C 0.1551(6) 0.1136(5) 0.8619(3) 0.0459(11) Uani 1 1 d . . . C42 C 0.2479(6) 0.1689(5) 0.8341(3) 0.0453(11) Uani 1 1 d . . . C43 C 0.3659(7) 0.1287(6) 0.8615(4) 0.0625(15) Uani 1 1 d . . . H43A H 0.4277 0.1658 0.8447 0.075 Uiso 1 1 calc R . . C44 C 0.3920(8) 0.0353(7) 0.9130(4) 0.0726(19) Uani 1 1 d . . . H44A H 0.4703 0.0109 0.9310 0.087 Uiso 1 1 calc R . . C45 C 0.3035(8) -0.0215(7) 0.9378(4) 0.0746(19) Uani 1 1 d . . . H45A H 0.3241 -0.0878 0.9703 0.089 Uiso 1 1 calc R . . C46 C 0.1842(8) 0.0197(6) 0.9144(4) 0.0649(16) Uani 1 1 d . . . H46A H 0.1214 -0.0156 0.9338 0.078 Uiso 1 1 calc R . . C51 C -0.0260(6) 0.0244(5) 0.8225(3) 0.0527(13) Uani 1 1 d . . . C52 C 0.0883(8) -0.0774(6) 0.7917(4) 0.0729(18) Uani 1 1 d . . . H52A H 0.1751 -0.0765 0.7820 0.088 Uiso 1 1 calc R . . C53 C 0.0755(9) -0.1838(6) 0.7746(4) 0.078(2) Uani 1 1 d . . . H53A H 0.1540 -0.2518 0.7518 0.093 Uiso 1 1 calc R . . C54 C -0.0460(12) -0.1895(8) 0.7901(5) 0.099(3) Uani 1 1 d . . . H54A H -0.0520 -0.2626 0.7807 0.119 Uiso 1 1 calc R . . C55 C -0.1609(13) -0.0893(11) 0.8194(7) 0.137(5) Uani 1 1 d . . . H55A H -0.2467 -0.0918 0.8277 0.164 Uiso 1 1 calc R . . C56 C -0.1525(8) 0.0209(8) 0.8380(5) 0.094(3) Uani 1 1 d . . . H56A H -0.2316 0.0889 0.8603 0.113 Uiso 1 1 calc R . . C61 C -0.1401(6) 0.2425(5) 0.9196(3) 0.0486(12) Uani 1 1 d . . . C62 C -0.2781(6) 0.2930(6) 0.9180(3) 0.0581(14) Uani 1 1 d . . . H62A H -0.3013 0.2911 0.8744 0.070 Uiso 1 1 calc R . . C63 C -0.3810(8) 0.3457(7) 0.9792(4) 0.080(2) Uani 1 1 d . . . H63A H -0.4731 0.3763 0.9777 0.096 Uiso 1 1 calc R . . C64 C -0.3467(9) 0.3530(7) 1.0437(4) 0.084(2) Uani 1 1 d . . . H64A H -0.4158 0.3875 1.0858 0.101 Uiso 1 1 calc R . . C65 C -0.2110(10) 0.3094(8) 1.0451(4) 0.083(2) Uani 1 1 d . . . H65A H -0.1889 0.3186 1.0878 0.100 Uiso 1 1 calc R . . C66 C -0.1051(8) 0.2516(6) 0.9841(3) 0.0628(15) Uani 1 1 d . . . H66B H -0.0131 0.2197 0.9862 0.075 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 0.0383(2) 0.0368(2) 0.0347(2) -0.00025(14) -0.01045(15) -0.01441(15) P1 0.0396(7) 0.0374(6) 0.0388(6) -0.0025(5) -0.0067(5) -0.0140(5) S1 0.0543(8) 0.0557(8) 0.0440(7) -0.0103(6) -0.0174(6) -0.0153(6) N2 0.047(2) 0.040(2) 0.041(2) 0.0023(17) -0.0139(18) -0.0166(18) C3 0.053(3) 0.039(3) 0.032(2) -0.0006(19) -0.007(2) -0.015(2) Cl1 0.099(2) 0.300(6) 0.201(4) -0.066(4) -0.032(2) -0.079(3) Pd2 0.0384(2) 0.0368(2) 0.0345(2) -0.00040(14) -0.00873(15) -0.01572(15) P2 0.0484(7) 0.0357(6) 0.0390(6) 0.0007(5) -0.0059(5) -0.0183(5) S2 0.0615(8) 0.0578(8) 0.0433(7) 0.0113(6) -0.0241(6) -0.0305(7) C8 0.032(2) 0.036(2) 0.047(3) -0.002(2) -0.013(2) -0.0052(19) C4 0.097(6) 0.088(6) 0.070(5) -0.047(4) -0.032(4) 0.012(4) Cl2 0.205(4) 0.320(7) 0.196(4) 0.084(4) -0.103(4) -0.191(5) C1 0.048(3) 0.039(2) 0.032(2) -0.0005(18) -0.007(2) -0.016(2) C9 0.034(3) 0.044(3) 0.050(3) -0.006(2) -0.009(2) 0.001(2) N6 0.068(3) 0.044(2) 0.042(2) -0.0091(19) -0.011(2) -0.007(2) C2 0.104(6) 0.072(4) 0.059(4) 0.029(3) -0.036(4) -0.039(4) N1 0.044(2) 0.037(2) 0.041(2) 0.0023(16) -0.0141(18) -0.0178(18) C5 0.118(9) 0.218(14) 0.113(8) 0.006(9) -0.058(7) -0.098(10) C6 0.047(3) 0.037(2) 0.044(3) -0.0035(19) -0.011(2) -0.022(2) C7 0.059(3) 0.043(3) 0.046(3) 0.006(2) -0.015(2) -0.032(2) N5 0.070(3) 0.048(3) 0.039(2) 0.0057(19) -0.011(2) -0.026(2) C11 0.049(3) 0.046(3) 0.043(3) -0.003(2) -0.007(2) -0.023(2) C12 0.043(3) 0.037(2) 0.040(2) -0.0069(19) -0.008(2) -0.015(2) C13 0.052(3) 0.063(4) 0.055(3) -0.014(3) -0.007(3) -0.026(3) C14 0.072(4) 0.080(5) 0.066(4) -0.027(3) -0.011(3) -0.039(4) C15 0.076(5) 0.070(4) 0.075(4) -0.036(4) -0.003(3) -0.033(4) C16 0.053(3) 0.056(3) 0.067(4) -0.019(3) -0.005(3) -0.018(3) C21 0.045(3) 0.047(3) 0.039(3) -0.008(2) 0.003(2) -0.017(2) C22 0.064(4) 0.050(3) 0.054(3) -0.004(3) -0.002(3) -0.027(3) C23 0.071(4) 0.059(4) 0.070(4) -0.013(3) 0.011(3) -0.035(3) C24 0.105(6) 0.065(4) 0.059(4) 0.003(3) 0.007(4) -0.044(4) C25 0.102(6) 0.091(5) 0.043(3) 0.006(3) -0.015(3) -0.040(5) C26 0.073(4) 0.071(4) 0.046(3) 0.000(3) -0.009(3) -0.033(3) C31 0.049(3) 0.041(3) 0.057(3) -0.007(2) -0.012(3) -0.010(2) C32 0.061(4) 0.055(4) 0.069(4) 0.008(3) -0.011(3) -0.012(3) C33 0.078(5) 0.056(4) 0.085(5) 0.002(3) -0.035(4) -0.002(4) C34 0.089(6) 0.053(4) 0.148(9) -0.009(5) -0.062(6) 0.000(4) C35 0.047(4) 0.081(6) 0.252(15) -0.006(8) -0.026(6) -0.009(4) C36 0.046(4) 0.059(4) 0.133(7) -0.003(4) -0.003(4) -0.014(3) C41 0.058(3) 0.037(2) 0.038(3) 0.004(2) -0.013(2) -0.015(2) C42 0.048(3) 0.040(3) 0.043(3) 0.003(2) -0.016(2) -0.011(2) C43 0.060(4) 0.063(4) 0.064(4) 0.009(3) -0.028(3) -0.019(3) C44 0.079(5) 0.065(4) 0.069(4) 0.011(3) -0.042(4) -0.013(4) C45 0.095(5) 0.058(4) 0.064(4) 0.021(3) -0.040(4) -0.018(4) C46 0.082(5) 0.056(4) 0.057(4) 0.016(3) -0.020(3) -0.032(3) C51 0.069(4) 0.042(3) 0.044(3) -0.003(2) 0.000(3) -0.027(3) C52 0.075(4) 0.050(4) 0.091(5) -0.015(3) -0.018(4) -0.021(3) C53 0.099(6) 0.046(4) 0.083(5) -0.013(3) -0.029(4) -0.018(4) C54 0.139(8) 0.061(5) 0.113(7) -0.011(5) -0.018(6) -0.062(5) C55 0.128(9) 0.119(9) 0.180(11) -0.061(8) 0.033(8) -0.094(8) C56 0.071(5) 0.070(5) 0.140(8) -0.035(5) 0.013(5) -0.042(4) C61 0.061(3) 0.039(3) 0.041(3) 0.002(2) -0.002(2) -0.023(2) C62 0.058(4) 0.052(3) 0.052(3) -0.003(3) -0.003(3) -0.016(3) C63 0.071(5) 0.057(4) 0.084(5) 0.001(4) 0.008(4) -0.017(3) C64 0.097(6) 0.062(4) 0.061(4) -0.010(3) 0.006(4) -0.015(4) C65 0.109(7) 0.080(5) 0.051(4) -0.010(3) -0.008(4) -0.035(5) C66 0.074(4) 0.059(4) 0.050(3) -0.006(3) -0.006(3) -0.027(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C42 1.999(5) . ? Pd1 N1 2.136(4) . ? Pd1 P1 2.3008(13) . ? Pd1 S1 2.3915(14) . ? Pd1 Pd2 2.8031(5) . ? P1 C11 1.822(5) . ? P1 C21 1.829(5) . ? P1 C31 1.856(6) . ? S1 C3 1.706(6) . ? N2 C3 1.340(6) . ? N2 C8 1.357(6) . ? N2 Pd2 2.134(4) . ? C3 N6 1.345(7) . ? Cl1 C5 1.706(13) . ? Pd2 C12 2.010(5) . ? Pd2 P2 2.2907(13) . ? Pd2 S2 2.3906(13) . ? P2 C41 1.817(6) . ? P2 C61 1.833(5) . ? P2 C51 1.850(5) . ? S2 C1 1.713(5) . ? C8 C9 1.259(7) . ? C8 H8A 0.9300 . ? C4 N6 1.457(8) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? Cl2 C5 1.687(12) . ? C1 N1 1.336(6) . ? C1 N5 1.348(6) . ? C9 N6 1.354(7) . ? C9 H9A 0.9300 . ? C2 N5 1.450(7) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? N1 C6 1.350(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.279(7) . ? C6 H6A 0.9300 . ? C7 N5 1.340(7) . ? C7 H7A 0.9300 . ? C11 C12 1.392(7) . ? C11 C16 1.397(8) . ? C12 C13 1.388(7) . ? C13 C14 1.376(8) . ? C13 H13A 0.9300 . ? C14 C15 1.383(10) . ? C14 H14A 0.9300 . ? C15 C16 1.382(9) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? C21 C26 1.387(8) . ? C21 C22 1.389(8) . ? C22 C23 1.357(8) . ? C22 H22A 0.9300 . ? C23 C24 1.372(11) . ? C23 H23A 0.9300 . ? C24 C25 1.383(11) . ? C24 H24A 0.9300 . ? C25 C26 1.393(9) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C31 C36 1.359(9) . ? C31 C32 1.362(9) . ? C32 C33 1.374(9) . ? C32 H32A 0.9300 . ? C33 C34 1.319(12) . ? C33 H33A 0.9300 . ? C34 C35 1.404(14) . ? C34 H34A 0.9300 . ? C35 C36 1.399(11) . ? C35 H35A 0.9300 . ? C36 H36A 0.9300 . ? C41 C46 1.399(7) . ? C41 C42 1.399(8) . ? C42 C43 1.401(8) . ? C43 C44 1.379(9) . ? C43 H43A 0.9300 . ? C44 C45 1.367(10) . ? C44 H44A 0.9300 . ? C45 C46 1.371(10) . ? C45 H45A 0.9300 . ? C46 H46A 0.9300 . ? C51 C52 1.359(9) . ? C51 C56 1.365(9) . ? C52 C53 1.399(9) . ? C52 H52A 0.9300 . ? C53 C54 1.322(11) . ? C53 H53A 0.9300 . ? C54 C55 1.345(14) . ? C54 H54A 0.9300 . ? C55 C56 1.426(11) . ? C55 H55A 0.9300 . ? C56 H56A 0.9300 . ? C61 C62 1.386(8) . ? C61 C66 1.399(8) . ? C62 C63 1.369(9) . ? C62 H62A 0.9300 . ? C63 C64 1.388(12) . ? C63 H63A 0.9300 . ? C64 C65 1.366(12) . ? C64 H64A 0.9300 . ? C65 C66 1.393(10) . ? C65 H65A 0.9300 . ? C66 H66B 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 C42 Pd1 N1 178.22(19) . . ? C42 Pd1 P1 88.54(16) . . ? N1 Pd1 P1 92.95(12) . . ? C42 Pd1 S1 87.98(16) . . ? N1 Pd1 S1 90.48(12) . . ? P1 Pd1 S1 175.41(5) . . ? C42 Pd1 Pd2 95.60(16) . . ? N1 Pd1 Pd2 83.58(11) . . ? P1 Pd1 Pd2 84.30(3) . . ? S1 Pd1 Pd2 93.06(4) . . ? C11 P1 C21 104.7(2) . . ? C11 P1 C31 103.5(3) . . ? C21 P1 C31 104.4(3) . . ? C11 P1 Pd1 113.60(18) . . ? C21 P1 Pd1 109.81(17) . . ? C31 P1 Pd1 119.50(19) . . ? C3 S1 Pd1 102.01(17) . . ? C3 N2 C8 107.1(4) . . ? C3 N2 Pd2 128.5(4) . . ? C8 N2 Pd2 123.8(3) . . ? N2 C3 N6 105.8(5) . . ? N2 C3 S1 129.6(4) . . ? N6 C3 S1 124.6(4) . . ? C12 Pd2 N2 179.21(18) . . ? C12 Pd2 P2 87.67(15) . . ? N2 Pd2 P2 92.76(11) . . ? C12 Pd2 S2 88.26(15) . . ? N2 Pd2 S2 91.28(11) . . ? P2 Pd2 S2 175.02(5) . . ? C12 Pd2 Pd1 95.68(14) . . ? N2 Pd2 Pd1 83.70(12) . . ? P2 Pd2 Pd1 84.48(4) . . ? S2 Pd2 Pd1 93.08(4) . . ? C41 P2 C61 104.9(3) . . ? C41 P2 C51 104.1(3) . . ? C61 P2 C51 105.5(2) . . ? C41 P2 Pd2 113.90(17) . . ? C61 P2 Pd2 110.96(17) . . ? C51 P2 Pd2 116.52(19) . . ? C1 S2 Pd2 101.81(17) . . ? C9 C8 N2 110.7(5) . . ? C9 C8 H8A 124.7 . . ? N2 C8 H8A 124.7 . . ? N6 C4 H4A 109.5 . . ? N6 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N6 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C1 N5 105.8(4) . . ? N1 C1 S2 129.6(4) . . ? N5 C1 S2 124.6(4) . . ? C8 C9 N6 107.3(5) . . ? C8 C9 H9A 126.4 . . ? N6 C9 H9A 126.4 . . ? C3 N6 C9 109.1(5) . . ? C3 N6 C4 128.5(6) . . ? C9 N6 C4 122.2(5) . . ? N5 C2 H2A 109.5 . . ? N5 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N5 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 N1 C6 107.4(4) . . ? C1 N1 Pd1 128.4(3) . . ? C6 N1 Pd1 123.5(3) . . ? Cl2 C5 Cl1 111.6(9) . . ? Cl2 C5 H5A 109.3 . . ? Cl1 C5 H5A 109.3 . . ? Cl2 C5 H5B 109.3 . . ? Cl1 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? C7 C6 N1 110.3(4) . . ? C7 C6 H6A 124.8 . . ? N1 C6 H6A 124.8 . . ? C6 C7 N5 107.0(4) . . ? C6 C7 H7A 126.5 . . ? N5 C7 H7A 126.5 . . ? C7 N5 C1 109.4(4) . . ? C7 N5 C2 121.7(5) . . ? C1 N5 C2 128.5(5) . . ? C12 C11 C16 119.7(5) . . ? C12 C11 P1 121.3(4) . . ? C16 C11 P1 118.9(4) . . ? C13 C12 C11 118.2(5) . . ? C13 C12 Pd2 118.6(4) . . ? C11 C12 Pd2 123.2(4) . . ? C14 C13 C12 122.1(6) . . ? C14 C13 H13A 119.0 . . ? C12 C13 H13A 119.0 . . ? C13 C14 C15 119.7(6) . . ? C13 C14 H14A 120.2 . . ? C15 C14 H14A 120.2 . . ? C16 C15 C14 119.3(6) . . ? C16 C15 H15A 120.4 . . ? C14 C15 H15A 120.4 . . ? C15 C16 C11 121.0(6) . . ? C15 C16 H16A 119.5 . . ? C11 C16 H16A 119.5 . . ? C26 C21 C22 119.0(5) . . ? C26 C21 P1 123.1(4) . . ? C22 C21 P1 117.9(4) . . ? C23 C22 C21 121.3(6) . . ? C23 C22 H22A 119.4 . . ? C21 C22 H22A 119.4 . . ? C22 C23 C24 120.1(6) . . ? C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? C23 C24 C25 120.1(6) . . ? C23 C24 H24A 119.9 . . ? C25 C24 H24A 119.9 . . ? C24 C25 C26 119.9(7) . . ? C24 C25 H25A 120.0 . . ? C26 C25 H25A 120.0 . . ? C21 C26 C25 119.5(6) . . ? C21 C26 H26A 120.2 . . ? C25 C26 H26A 120.2 . . ? C36 C31 C32 118.8(6) . . ? C36 C31 P1 122.0(5) . . ? C32 C31 P1 119.2(5) . . ? C31 C32 C33 121.8(7) . . ? C31 C32 H32A 119.1 . . ? C33 C32 H32A 119.1 . . ? C34 C33 C32 120.9(8) . . ? C34 C33 H33A 119.6 . . ? C32 C33 H33A 119.6 . . ? C33 C34 C35 119.1(8) . . ? C33 C34 H34A 120.4 . . ? C35 C34 H34A 120.4 . . ? C36 C35 C34 119.8(9) . . ? C36 C35 H35A 120.1 . . ? C34 C35 H35A 120.1 . . ? C31 C36 C35 119.6(8) . . ? C31 C36 H36A 120.2 . . ? C35 C36 H36A 120.2 . . ? C46 C41 C42 119.4(5) . . ? C46 C41 P2 119.2(5) . . ? C42 C41 P2 121.3(4) . . ? C41 C42 C43 118.0(5) . . ? C41 C42 Pd1 123.4(4) . . ? C43 C42 Pd1 118.4(4) . . ? C44 C43 C42 121.2(6) . . ? C44 C43 H43A 119.4 . . ? C42 C43 H43A 119.4 . . ? C45 C44 C43 120.4(6) . . ? C45 C44 H44A 119.8 . . ? C43 C44 H44A 119.8 . . ? C44 C45 C46 119.6(6) . . ? C44 C45 H45A 120.2 . . ? C46 C45 H45A 120.2 . . ? C45 C46 C41 121.3(6) . . ? C45 C46 H46A 119.4 . . ? C41 C46 H46A 119.4 . . ? C52 C51 C56 119.5(6) . . ? C52 C51 P2 119.2(5) . . ? C56 C51 P2 121.2(5) . . ? C51 C52 C53 120.0(7) . . ? C51 C52 H52A 120.0 . . ? C53 C52 H52A 120.0 . . ? C54 C53 C52 121.3(7) . . ? C54 C53 H53A 119.4 . . ? C52 C53 H53A 119.4 . . ? C53 C54 C55 119.8(7) . . ? C53 C54 H54A 120.1 . . ? C55 C54 H54A 120.1 . . ? C54 C55 C56 120.7(9) . . ? C54 C55 H55A 119.6 . . ? C56 C55 H55A 119.6 . . ? C51 C56 C55 118.6(8) . . ? C51 C56 H56A 120.7 . . ? C55 C56 H56A 120.7 . . ? C62 C61 C66 119.2(5) . . ? C62 C61 P2 118.9(4) . . ? C66 C61 P2 121.8(5) . . ? C63 C62 C61 121.4(7) . . ? C63 C62 H62A 119.3 . . ? C61 C62 H62A 119.3 . . ? C62 C63 C64 119.5(8) . . ? C62 C63 H63A 120.3 . . ? C64 C63 H63A 120.3 . . ? C65 C64 C63 119.8(7) . . ? C65 C64 H64A 120.1 . . ? C63 C64 H64A 120.1 . . ? C64 C65 C66 121.5(7) . . ? C64 C65 H65A 119.3 . . ? C66 C65 H65A 119.3 . . ? C65 C66 C61 118.5(7) . . ? C65 C66 H66B 120.7 . . ? C61 C66 H66B 120.7 . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 1.879 _refine_diff_density_min -1.150 _refine_diff_density_rms 0.159 _database_code_depnum_ccdc_archive 'CCDC 941944' ####################################################################### # # 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_2f _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H42 N4 P2 Pd2 S2' _chemical_formula_weight 1061.76 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4700(4) _cell_length_b 11.1020(4) _cell_length_c 20.3260(6) _cell_angle_alpha 104.6680(19) _cell_angle_beta 90.2450(18) _cell_angle_gamma 97.2770(15) _cell_volume 2265.61(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour ? _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 0.998 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 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_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13805 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0433 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.04 _diffrn_reflns_theta_max 27.55 _reflns_number_total 9841 _reflns_number_gt 7921 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect(Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo and Scalepack(Otwinowski & Minor1997)' _computing_data_reduction 'Denzo and Scalepack(Otwinowski & Minor1997)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0746P)^2^+0.6421P] 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 9841 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0538 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.1200 _refine_ls_wR_factor_gt 0.1078 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 Pd1 Pd 0.74588(2) -0.05610(2) 0.712051(11) 0.02867(8) Uani 1 1 d . . . S1 S 0.92292(9) 0.01247(9) 0.65223(5) 0.0414(2) Uani 1 1 d . . . P1 P 0.58009(9) -0.11270(8) 0.77627(4) 0.03283(19) Uani 1 1 d . . . N1 N 0.9461(3) 0.2165(3) 0.60183(16) 0.0429(7) Uani 1 1 d . . . C1 C 0.8831(3) 0.1549(3) 0.64563(17) 0.0359(7) Uani 1 1 d . . . Pd2 Pd 0.68351(2) 0.18425(2) 0.761563(11) 0.02980(8) Uani 1 1 d . . . P2 P 0.85669(9) 0.20868(9) 0.83514(4) 0.0367(2) Uani 1 1 d . . . S2 S 0.49389(9) 0.14648(10) 0.69175(5) 0.0430(2) Uani 1 1 d . . . N2 N 0.7980(3) 0.2224(3) 0.68026(13) 0.0332(6) Uani 1 1 d . . . C2 C 1.0495(5) 0.1757(5) 0.5574(3) 0.0748(16) Uani 1 1 d . . . H2A H 1.0647 0.0936 0.5603 0.112 Uiso 1 1 calc R . . H2B H 1.1266 0.2338 0.5714 0.112 Uiso 1 1 calc R . . H2C H 1.0254 0.1727 0.5114 0.112 Uiso 1 1 calc R . . N3 N 0.6167(3) -0.0546(3) 0.63124(13) 0.0345(6) Uani 1 1 d . . . C3 C 0.8989(4) 0.3303(4) 0.61004(19) 0.0426(8) Uani 1 1 d . . . N4 N 0.4386(3) -0.0376(3) 0.57601(16) 0.0474(8) Uani 1 1 d . . . C4 C 0.9311(5) 0.4305(5) 0.5815(2) 0.0614(12) Uani 1 1 d . . . H4A H 0.9931 0.4281 0.5488 0.074 Uiso 1 1 calc R . . C5 C 0.8678(5) 0.5333(5) 0.6037(3) 0.0683(14) Uani 1 1 d . . . H5A H 0.8880 0.6022 0.5857 0.082 Uiso 1 1 calc R . . C6 C 0.7738(4) 0.5376(4) 0.6525(2) 0.0560(11) Uani 1 1 d . . . H6A H 0.7322 0.6086 0.6661 0.067 Uiso 1 1 calc R . . C7 C 0.7423(4) 0.4375(4) 0.6807(2) 0.0448(9) Uani 1 1 d . . . H7A H 0.6800 0.4404 0.7133 0.054 Uiso 1 1 calc R . . C8 C 0.8049(3) 0.3333(3) 0.65947(17) 0.0351(7) Uani 1 1 d . . . C9 C 0.5205(3) 0.0132(3) 0.63150(17) 0.0371(8) Uani 1 1 d . . . C10 C 0.3180(4) 0.0056(5) 0.5624(2) 0.0648(13) Uani 1 1 d . . . H10A H 0.3080 0.0814 0.5962 0.097 Uiso 1 1 calc R . . H10B H 0.2474 -0.0578 0.5638 0.097 Uiso 1 1 calc R . . H10C H 0.3191 0.0217 0.5181 0.097 Uiso 1 1 calc R . . C11 C 0.5405(3) 0.0205(3) 0.84198(17) 0.0365(7) Uani 1 1 d . . . C12 C 0.5715(3) 0.1426(3) 0.83472(16) 0.0342(7) Uani 1 1 d . . . C13 C 0.5208(4) 0.2394(4) 0.8809(2) 0.0487(10) Uani 1 1 d . . . H13A H 0.5389 0.3212 0.8767 0.058 Uiso 1 1 calc R . . C14 C 0.4442(5) 0.2161(4) 0.9328(2) 0.0572(12) Uani 1 1 d . . . H14A H 0.4100 0.2818 0.9622 0.069 Uiso 1 1 calc R . . C15 C 0.4182(5) 0.0951(4) 0.9412(2) 0.0576(12) Uani 1 1 d . . . H15A H 0.3692 0.0796 0.9769 0.069 Uiso 1 1 calc R . . C16 C 0.4657(4) -0.0009(4) 0.8960(2) 0.0491(10) Uani 1 1 d . . . H16A H 0.4480 -0.0822 0.9012 0.059 Uiso 1 1 calc R . . C21 C 0.5965(4) -0.2335(3) 0.82216(18) 0.0382(8) Uani 1 1 d . . . C22 C 0.5203(4) -0.3482(4) 0.8058(2) 0.0548(11) Uani 1 1 d . . . H22A H 0.4562 -0.3657 0.7716 0.066 Uiso 1 1 calc R . . C23 C 0.5397(5) -0.4381(4) 0.8406(3) 0.0675(14) Uani 1 1 d . . . H23A H 0.4888 -0.5160 0.8292 0.081 Uiso 1 1 calc R . . C24 C 0.6329(5) -0.4126(4) 0.8911(2) 0.0619(12) Uani 1 1 d . . . H24A H 0.6464 -0.4734 0.9137 0.074 Uiso 1 1 calc R . . C25 C 0.7069(5) -0.2970(4) 0.9088(2) 0.0550(11) Uani 1 1 d . . . H25A H 0.7697 -0.2793 0.9436 0.066 Uiso 1 1 calc R . . C26 C 0.6880(4) -0.2074(4) 0.87484(18) 0.0464(9) Uani 1 1 d . . . H26A H 0.7372 -0.1287 0.8875 0.056 Uiso 1 1 calc R . . C31 C 0.4297(4) -0.1726(3) 0.72565(18) 0.0398(8) Uani 1 1 d . . . C32 C 0.3193(4) -0.1147(5) 0.7392(2) 0.0570(11) Uani 1 1 d . . . H32A H 0.3189 -0.0453 0.7761 0.068 Uiso 1 1 calc R . . C33 C 0.2104(5) -0.1606(7) 0.6978(3) 0.0798(17) Uani 1 1 d . . . H33A H 0.1370 -0.1210 0.7071 0.096 Uiso 1 1 calc R . . C34 C 0.2074(5) -0.2627(7) 0.6435(3) 0.0885(19) Uani 1 1 d . . . H34A H 0.1330 -0.2925 0.6162 0.106 Uiso 1 1 calc R . . C35 C 0.3171(6) -0.3211(5) 0.6298(3) 0.0813(17) Uani 1 1 d . . . H35A H 0.3162 -0.3910 0.5931 0.098 Uiso 1 1 calc R . . C36 C 0.4278(5) -0.2762(4) 0.6703(2) 0.0543(10) Uani 1 1 d . . . H36A H 0.5013 -0.3155 0.6605 0.065 Uiso 1 1 calc R . . C41 C 0.9098(4) 0.0605(4) 0.83875(19) 0.0439(9) Uani 1 1 d . . . C42 C 0.8730(3) -0.0492(3) 0.78813(17) 0.0356(7) Uani 1 1 d . . . C43 C 0.9262(4) -0.1570(4) 0.7910(2) 0.0472(9) Uani 1 1 d . . . H43A H 0.9025 -0.2310 0.7575 0.057 Uiso 1 1 calc R . . C44 C 1.0131(5) -0.1566(5) 0.8423(2) 0.0590(11) Uani 1 1 d . . . H44A H 1.0492 -0.2289 0.8424 0.071 Uiso 1 1 calc R . . C45 C 1.0465(5) -0.0476(5) 0.8940(3) 0.0719(14) Uani 1 1 d . . . H45A H 1.1016 -0.0476 0.9300 0.086 Uiso 1 1 calc R . . C46 C 0.9973(5) 0.0598(4) 0.8914(2) 0.0619(12) Uani 1 1 d . . . H46A H 1.0221 0.1335 0.9250 0.074 Uiso 1 1 calc R . . C51 C 0.8327(4) 0.2883(4) 0.92447(18) 0.0468(9) Uani 1 1 d . . . C52 C 0.7779(5) 0.2208(5) 0.9680(2) 0.0722(15) Uani 1 1 d . . . H52A H 0.7602 0.1337 0.9534 0.087 Uiso 1 1 calc R . . C53 C 0.7491(6) 0.2823(7) 1.0335(2) 0.0872(19) Uani 1 1 d . . . H53A H 0.7125 0.2357 1.0624 0.105 Uiso 1 1 calc R . . C54 C 0.7733(5) 0.4094(6) 1.0564(2) 0.0794(17) Uani 1 1 d . . . H54A H 0.7522 0.4496 1.1001 0.095 Uiso 1 1 calc R . . C55 C 0.8295(5) 0.4777(5) 1.0139(2) 0.0676(13) Uani 1 1 d . . . H55A H 0.8476 0.5646 1.0291 0.081 Uiso 1 1 calc R . . C56 C 0.8593(4) 0.4175(4) 0.9482(2) 0.0519(10) Uani 1 1 d . . . H56A H 0.8976 0.4645 0.9199 0.062 Uiso 1 1 calc R . . C61 C 0.9977(4) 0.2986(4) 0.80837(18) 0.0436(9) Uani 1 1 d . . . C62 C 1.1134(4) 0.2510(5) 0.7948(3) 0.0635(12) Uani 1 1 d . . . H62A H 1.1265 0.1764 0.8050 0.076 Uiso 1 1 calc R . . C63 C 1.2099(5) 0.3166(6) 0.7655(3) 0.0846(19) Uani 1 1 d . . . H63A H 1.2878 0.2849 0.7563 0.102 Uiso 1 1 calc R . . C64 C 1.1924(5) 0.4273(6) 0.7500(3) 0.0791(17) Uani 1 1 d . . . H64A H 1.2573 0.4690 0.7298 0.095 Uiso 1 1 calc R . . C65 C 1.0806(5) 0.4748(5) 0.7644(2) 0.0659(13) Uani 1 1 d . . . H65A H 1.0694 0.5505 0.7550 0.079 Uiso 1 1 calc R . . C66 C 0.9815(4) 0.4115(4) 0.79339(19) 0.0489(9) Uani 1 1 d . . . H66A H 0.9045 0.4447 0.8027 0.059 Uiso 1 1 calc R . . C71 C 0.5985(4) -0.1526(4) 0.57241(17) 0.0403(8) Uani 1 1 d . . . C72 C 0.4858(4) -0.1439(4) 0.53789(19) 0.0474(9) Uani 1 1 d . . . C73 C 0.4420(5) -0.2316(5) 0.4774(2) 0.0675(14) Uani 1 1 d . . . H73A H 0.3681 -0.2247 0.4537 0.081 Uiso 1 1 calc R . . C74 C 0.5135(6) -0.3289(5) 0.4544(2) 0.0810(17) Uani 1 1 d . . . H74A H 0.4859 -0.3904 0.4149 0.097 Uiso 1 1 calc R . . C75 C 0.6247(6) -0.3375(5) 0.4883(3) 0.0741(15) Uani 1 1 d . . . H75A H 0.6709 -0.4040 0.4707 0.089 Uiso 1 1 calc R . . C76 C 0.6696(5) -0.2501(4) 0.5477(2) 0.0531(10) Uani 1 1 d . . . H76A H 0.7449 -0.2566 0.5702 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 0.02904(14) 0.02800(13) 0.02928(13) 0.00700(9) 0.00054(9) 0.00557(10) S1 0.0369(5) 0.0426(5) 0.0488(5) 0.0154(4) 0.0125(4) 0.0128(4) P1 0.0353(5) 0.0279(4) 0.0356(4) 0.0089(3) 0.0039(3) 0.0035(4) N1 0.0379(18) 0.0486(18) 0.0465(17) 0.0179(14) 0.0146(13) 0.0092(15) C1 0.0330(18) 0.0413(19) 0.0331(16) 0.0096(14) 0.0038(13) 0.0035(15) Pd2 0.03268(15) 0.02740(13) 0.03026(13) 0.00829(10) 0.00451(10) 0.00545(10) P2 0.0395(5) 0.0349(5) 0.0335(4) 0.0064(3) -0.0024(4) 0.0011(4) S2 0.0354(5) 0.0512(5) 0.0456(5) 0.0132(4) 0.0022(4) 0.0162(4) N2 0.0338(16) 0.0359(15) 0.0313(13) 0.0107(11) 0.0066(11) 0.0051(12) C2 0.078(4) 0.078(3) 0.088(3) 0.043(3) 0.054(3) 0.035(3) N3 0.0347(16) 0.0392(16) 0.0304(13) 0.0101(11) -0.0031(11) 0.0057(13) C3 0.039(2) 0.050(2) 0.045(2) 0.0208(17) 0.0063(15) 0.0082(17) N4 0.0379(18) 0.058(2) 0.0489(18) 0.0190(16) -0.0104(13) 0.0079(16) C4 0.056(3) 0.068(3) 0.077(3) 0.045(3) 0.023(2) 0.015(2) C5 0.060(3) 0.061(3) 0.103(4) 0.053(3) 0.013(3) 0.009(2) C6 0.050(3) 0.047(2) 0.078(3) 0.026(2) 0.001(2) 0.013(2) C7 0.040(2) 0.050(2) 0.048(2) 0.0156(17) 0.0007(16) 0.0109(18) C8 0.0305(18) 0.0406(18) 0.0364(17) 0.0140(14) 0.0003(13) 0.0040(15) C9 0.0332(19) 0.0427(19) 0.0377(17) 0.0146(15) -0.0023(13) 0.0057(16) C10 0.041(2) 0.085(4) 0.074(3) 0.032(3) -0.016(2) 0.005(2) C11 0.0383(19) 0.0351(18) 0.0358(17) 0.0085(14) 0.0082(14) 0.0049(15) C12 0.041(2) 0.0301(16) 0.0322(16) 0.0084(13) 0.0037(13) 0.0071(15) C13 0.062(3) 0.0341(19) 0.053(2) 0.0131(16) 0.0214(19) 0.0142(18) C14 0.073(3) 0.046(2) 0.053(2) 0.0075(19) 0.026(2) 0.018(2) C15 0.074(3) 0.050(2) 0.051(2) 0.0156(19) 0.031(2) 0.010(2) C16 0.061(3) 0.038(2) 0.051(2) 0.0160(17) 0.0200(19) 0.0057(19) C21 0.044(2) 0.0325(17) 0.0403(18) 0.0134(14) 0.0095(15) 0.0054(16) C22 0.057(3) 0.040(2) 0.069(3) 0.024(2) -0.004(2) -0.005(2) C23 0.080(4) 0.039(2) 0.090(4) 0.034(2) -0.007(3) -0.004(2) C24 0.076(3) 0.048(2) 0.072(3) 0.033(2) 0.006(2) 0.014(2) C25 0.067(3) 0.057(3) 0.045(2) 0.0189(19) 0.0027(19) 0.008(2) C26 0.055(2) 0.043(2) 0.0409(19) 0.0126(16) 0.0030(17) -0.0004(18) C31 0.037(2) 0.0361(18) 0.047(2) 0.0168(15) 0.0018(15) -0.0047(15) C32 0.037(2) 0.073(3) 0.064(3) 0.023(2) 0.0070(19) 0.008(2) C33 0.037(3) 0.120(5) 0.092(4) 0.047(4) 0.002(2) 0.005(3) C34 0.052(3) 0.105(5) 0.100(4) 0.034(4) -0.027(3) -0.032(3) C35 0.089(4) 0.058(3) 0.083(4) 0.010(3) -0.026(3) -0.025(3) C36 0.058(3) 0.042(2) 0.057(2) 0.0095(18) -0.0069(19) -0.008(2) C41 0.045(2) 0.044(2) 0.044(2) 0.0138(16) -0.0077(16) 0.0032(18) C42 0.0341(18) 0.0389(18) 0.0360(17) 0.0140(14) -0.0050(13) 0.0039(15) C43 0.045(2) 0.048(2) 0.052(2) 0.0141(18) -0.0014(17) 0.0142(18) C44 0.062(3) 0.059(3) 0.061(3) 0.021(2) -0.010(2) 0.020(2) C45 0.074(3) 0.077(3) 0.068(3) 0.022(3) -0.032(2) 0.018(3) C46 0.070(3) 0.052(2) 0.058(3) 0.006(2) -0.033(2) 0.004(2) C51 0.045(2) 0.058(2) 0.0319(18) 0.0042(16) -0.0033(15) -0.0011(19) C52 0.084(4) 0.078(3) 0.046(2) 0.014(2) 0.001(2) -0.020(3) C53 0.098(4) 0.117(5) 0.036(2) 0.016(3) 0.007(2) -0.015(4) C54 0.070(3) 0.120(5) 0.034(2) -0.007(3) 0.001(2) 0.012(3) C55 0.069(3) 0.071(3) 0.050(3) -0.011(2) -0.003(2) 0.011(3) C56 0.051(3) 0.053(2) 0.045(2) -0.0012(18) -0.0018(17) 0.007(2) C61 0.040(2) 0.044(2) 0.0397(19) 0.0018(15) -0.0005(15) -0.0058(17) C62 0.044(3) 0.056(3) 0.083(3) 0.004(2) 0.008(2) 0.004(2) C63 0.042(3) 0.095(4) 0.095(4) -0.008(3) 0.018(3) -0.007(3) C64 0.063(3) 0.090(4) 0.067(3) 0.008(3) 0.014(2) -0.033(3) C65 0.070(3) 0.060(3) 0.055(3) 0.010(2) -0.008(2) -0.029(3) C66 0.047(2) 0.052(2) 0.044(2) 0.0126(17) -0.0016(16) -0.0074(19) C71 0.047(2) 0.0398(19) 0.0327(17) 0.0100(14) -0.0077(14) 0.0001(17) C72 0.050(2) 0.049(2) 0.043(2) 0.0153(17) -0.0101(16) -0.0005(19) C73 0.071(3) 0.070(3) 0.052(2) 0.009(2) -0.029(2) -0.010(3) C74 0.111(5) 0.062(3) 0.053(3) -0.009(2) -0.025(3) -0.003(3) C75 0.101(4) 0.049(3) 0.060(3) -0.010(2) -0.011(3) 0.012(3) C76 0.069(3) 0.044(2) 0.045(2) 0.0056(17) -0.0058(19) 0.014(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C42 2.017(3) . ? Pd1 N3 2.128(3) . ? Pd1 P1 2.2957(9) . ? Pd1 S1 2.3717(9) . ? Pd1 Pd2 2.7653(3) . ? S1 C1 1.722(4) . ? P1 C11 1.817(3) . ? P1 C31 1.832(4) . ? P1 C21 1.841(3) . ? N1 C1 1.376(4) . ? N1 C3 1.386(5) . ? N1 C2 1.455(5) . ? C1 N2 1.326(4) . ? Pd2 C12 2.006(3) . ? Pd2 N2 2.143(2) . ? Pd2 P2 2.2901(10) . ? Pd2 S2 2.3654(10) . ? P2 C41 1.820(4) . ? P2 C61 1.839(4) . ? P2 C51 1.841(4) . ? S2 C9 1.719(4) . ? N2 C8 1.393(4) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? N3 C9 1.330(5) . ? N3 C71 1.392(4) . ? C3 C4 1.386(5) . ? C3 C8 1.407(5) . ? N4 C9 1.369(5) . ? N4 C72 1.387(5) . ? N4 C10 1.456(5) . ? C4 C5 1.371(7) . ? C4 H4A 0.9300 . ? C5 C6 1.396(6) . ? C5 H5A 0.9300 . ? C6 C7 1.380(5) . ? C6 H6A 0.9300 . ? C7 C8 1.377(5) . ? C7 H7A 0.9300 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.399(5) . ? C11 C16 1.403(5) . ? C12 C13 1.399(5) . ? C13 C14 1.382(5) . ? C13 H13A 0.9300 . ? C14 C15 1.390(6) . ? C14 H14A 0.9300 . ? C15 C16 1.367(6) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? C21 C22 1.376(5) . ? C21 C26 1.383(5) . ? C22 C23 1.395(6) . ? C22 H22A 0.9300 . ? C23 C24 1.365(7) . ? C23 H23A 0.9300 . ? C24 C25 1.374(6) . ? C24 H24A 0.9300 . ? C25 C26 1.379(5) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C31 C32 1.387(6) . ? C31 C36 1.388(6) . ? C32 C33 1.377(7) . ? C32 H32A 0.9300 . ? C33 C34 1.364(9) . ? C33 H33A 0.9300 . ? C34 C35 1.384(8) . ? C34 H34A 0.9300 . ? C35 C36 1.381(7) . ? C35 H35A 0.9300 . ? C36 H36A 0.9300 . ? C41 C42 1.390(5) . ? C41 C46 1.407(5) . ? C42 C43 1.397(5) . ? C43 C44 1.380(6) . ? C43 H43A 0.9300 . ? C44 C45 1.392(7) . ? C44 H44A 0.9300 . ? C45 C46 1.370(7) . ? C45 H45A 0.9300 . ? C46 H46A 0.9300 . ? C51 C52 1.381(6) . ? C51 C56 1.384(6) . ? C52 C53 1.387(7) . ? C52 H52A 0.9300 . ? C53 C54 1.359(9) . ? C53 H53A 0.9300 . ? C54 C55 1.375(7) . ? C54 H54A 0.9300 . ? C55 C56 1.390(6) . ? C55 H55A 0.9300 . ? C56 H56A 0.9300 . ? C61 C62 1.383(6) . ? C61 C66 1.392(6) . ? C62 C63 1.394(7) . ? C62 H62A 0.9300 . ? C63 C64 1.377(8) . ? C63 H63A 0.9300 . ? C64 C65 1.347(8) . ? C64 H64A 0.9300 . ? C65 C66 1.395(6) . ? C65 H65A 0.9300 . ? C66 H66A 0.9300 . ? C71 C76 1.382(6) . ? C71 C72 1.396(5) . ? C72 C73 1.395(6) . ? C73 C74 1.378(7) . ? C73 H73A 0.9300 . ? C74 C75 1.376(8) . ? C74 H74A 0.9300 . ? C75 C76 1.380(6) . ? C75 H75A 0.9300 . ? C76 H76A 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 C42 Pd1 N3 177.09(12) . . ? C42 Pd1 P1 89.91(10) . . ? N3 Pd1 P1 92.14(8) . . ? C42 Pd1 S1 87.37(10) . . ? N3 Pd1 S1 90.49(8) . . ? P1 Pd1 S1 176.22(3) . . ? C42 Pd1 Pd2 96.36(10) . . ? N3 Pd1 Pd2 81.79(8) . . ? P1 Pd1 Pd2 84.63(2) . . ? S1 Pd1 Pd2 93.06(2) . . ? C1 S1 Pd1 100.93(12) . . ? C11 P1 C31 104.39(17) . . ? C11 P1 C21 103.93(15) . . ? C31 P1 C21 103.32(17) . . ? C11 P1 Pd1 111.99(11) . . ? C31 P1 Pd1 112.27(11) . . ? C21 P1 Pd1 119.47(12) . . ? C1 N1 C3 107.7(3) . . ? C1 N1 C2 127.3(3) . . ? C3 N1 C2 124.9(3) . . ? N2 C1 N1 110.7(3) . . ? N2 C1 S1 128.6(3) . . ? N1 C1 S1 120.6(3) . . ? C12 Pd2 N2 177.51(12) . . ? C12 Pd2 P2 87.66(11) . . ? N2 Pd2 P2 94.24(8) . . ? C12 Pd2 S2 87.21(11) . . ? N2 Pd2 S2 90.82(8) . . ? P2 Pd2 S2 174.43(3) . . ? C12 Pd2 Pd1 95.26(9) . . ? N2 Pd2 Pd1 83.34(8) . . ? P2 Pd2 Pd1 84.30(3) . . ? S2 Pd2 Pd1 94.00(3) . . ? C41 P2 C61 105.03(19) . . ? C41 P2 C51 104.51(18) . . ? C61 P2 C51 106.45(17) . . ? C41 P2 Pd2 113.24(13) . . ? C61 P2 Pd2 110.99(13) . . ? C51 P2 Pd2 115.78(14) . . ? C9 S2 Pd2 101.01(13) . . ? C1 N2 C8 107.4(3) . . ? C1 N2 Pd2 128.1(2) . . ? C8 N2 Pd2 124.2(2) . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C9 N3 C71 106.6(3) . . ? C9 N3 Pd1 129.6(2) . . ? C71 N3 Pd1 121.8(2) . . ? C4 C3 N1 132.4(4) . . ? C4 C3 C8 121.6(4) . . ? N1 C3 C8 105.9(3) . . ? C9 N4 C72 107.6(3) . . ? C9 N4 C10 126.2(4) . . ? C72 N4 C10 126.0(4) . . ? C5 C4 C3 117.2(4) . . ? C5 C4 H4A 121.4 . . ? C3 C4 H4A 121.4 . . ? C4 C5 C6 121.9(4) . . ? C4 C5 H5A 119.0 . . ? C6 C5 H5A 119.0 . . ? C7 C6 C5 120.6(4) . . ? C7 C6 H6A 119.7 . . ? C5 C6 H6A 119.7 . . ? C8 C7 C6 118.6(4) . . ? C8 C7 H7A 120.7 . . ? C6 C7 H7A 120.7 . . ? C7 C8 N2 131.7(3) . . ? C7 C8 C3 120.1(3) . . ? N2 C8 C3 108.2(3) . . ? N3 C9 N4 111.0(3) . . ? N3 C9 S2 127.3(3) . . ? N4 C9 S2 121.7(3) . . ? N4 C10 H10A 109.5 . . ? N4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C16 120.0(3) . . ? C12 C11 P1 120.2(2) . . ? C16 C11 P1 119.4(3) . . ? C11 C12 C13 117.7(3) . . ? C11 C12 Pd2 123.2(2) . . ? C13 C12 Pd2 119.1(2) . . ? C14 C13 C12 121.5(4) . . ? C14 C13 H13A 119.3 . . ? C12 C13 H13A 119.3 . . ? C13 C14 C15 120.4(4) . . ? C13 C14 H14A 119.8 . . ? C15 C14 H14A 119.8 . . ? C16 C15 C14 118.9(3) . . ? C16 C15 H15A 120.5 . . ? C14 C15 H15A 120.5 . . ? C15 C16 C11 121.4(4) . . ? C15 C16 H16A 119.3 . . ? C11 C16 H16A 119.3 . . ? C22 C21 C26 119.3(3) . . ? C22 C21 P1 122.0(3) . . ? C26 C21 P1 118.7(3) . . ? C21 C22 C23 119.8(4) . . ? C21 C22 H22A 120.1 . . ? C23 C22 H22A 120.1 . . ? C24 C23 C22 120.4(4) . . ? C24 C23 H23A 119.8 . . ? C22 C23 H23A 119.8 . . ? C23 C24 C25 120.0(4) . . ? C23 C24 H24A 120.0 . . ? C25 C24 H24A 120.0 . . ? C24 C25 C26 120.0(4) . . ? C24 C25 H25A 120.0 . . ? C26 C25 H25A 120.0 . . ? C25 C26 C21 120.5(4) . . ? C25 C26 H26A 119.7 . . ? C21 C26 H26A 119.7 . . ? C32 C31 C36 119.1(4) . . ? C32 C31 P1 122.1(3) . . ? C36 C31 P1 118.8(3) . . ? C33 C32 C31 119.7(5) . . ? C33 C32 H32A 120.1 . . ? C31 C32 H32A 120.1 . . ? C34 C33 C32 121.6(6) . . ? C34 C33 H33A 119.2 . . ? C32 C33 H33A 119.2 . . ? C33 C34 C35 118.9(5) . . ? C33 C34 H34A 120.5 . . ? C35 C34 H34A 120.5 . . ? C36 C35 C34 120.4(5) . . ? C36 C35 H35A 119.8 . . ? C34 C35 H35A 119.8 . . ? C35 C36 C31 120.2(5) . . ? C35 C36 H36A 119.9 . . ? C31 C36 H36A 119.9 . . ? C42 C41 C46 119.7(4) . . ? C42 C41 P2 121.3(3) . . ? C46 C41 P2 118.8(3) . . ? C41 C42 C43 118.2(3) . . ? C41 C42 Pd1 121.9(3) . . ? C43 C42 Pd1 119.8(3) . . ? C44 C43 C42 121.7(4) . . ? C44 C43 H43A 119.1 . . ? C42 C43 H43A 119.1 . . ? C43 C44 C45 119.7(4) . . ? C43 C44 H44A 120.1 . . ? C45 C44 H44A 120.1 . . ? C46 C45 C44 119.4(4) . . ? C46 C45 H45A 120.3 . . ? C44 C45 H45A 120.3 . . ? C45 C46 C41 121.2(4) . . ? C45 C46 H46A 119.4 . . ? C41 C46 H46A 119.4 . . ? C52 C51 C56 118.4(4) . . ? C52 C51 P2 120.3(3) . . ? C56 C51 P2 121.2(3) . . ? C51 C52 C53 120.2(5) . . ? C51 C52 H52A 119.9 . . ? C53 C52 H52A 119.9 . . ? C54 C53 C52 121.4(5) . . ? C54 C53 H53A 119.3 . . ? C52 C53 H53A 119.3 . . ? C53 C54 C55 119.0(4) . . ? C53 C54 H54A 120.5 . . ? C55 C54 H54A 120.5 . . ? C54 C55 C56 120.3(5) . . ? C54 C55 H55A 119.8 . . ? C56 C55 H55A 119.8 . . ? C51 C56 C55 120.7(4) . . ? C51 C56 H56A 119.7 . . ? C55 C56 H56A 119.7 . . ? C62 C61 C66 119.2(4) . . ? C62 C61 P2 122.3(3) . . ? C66 C61 P2 118.1(3) . . ? C61 C62 C63 119.0(5) . . ? C61 C62 H62A 120.5 . . ? C63 C62 H62A 120.5 . . ? C64 C63 C62 121.4(5) . . ? C64 C63 H63A 119.3 . . ? C62 C63 H63A 119.3 . . ? C65 C64 C63 119.5(5) . . ? C65 C64 H64A 120.2 . . ? C63 C64 H64A 120.2 . . ? C64 C65 C66 120.7(5) . . ? C64 C65 H65A 119.6 . . ? C66 C65 H65A 119.6 . . ? C61 C66 C65 120.2(4) . . ? C61 C66 H66A 119.9 . . ? C65 C66 H66A 119.9 . . ? C76 C71 N3 130.5(3) . . ? C76 C71 C72 120.6(4) . . ? N3 C71 C72 108.8(3) . . ? N4 C72 C73 132.6(4) . . ? N4 C72 C71 105.9(3) . . ? C73 C72 C71 121.5(4) . . ? C74 C73 C72 116.7(4) . . ? C74 C73 H73A 121.7 . . ? C72 C73 H73A 121.7 . . ? C75 C74 C73 121.8(4) . . ? C75 C74 H74A 119.1 . . ? C73 C74 H74A 119.1 . . ? C74 C75 C76 121.8(5) . . ? C74 C75 H75A 119.1 . . ? C76 C75 H75A 119.1 . . ? C75 C76 C71 117.5(4) . . ? C75 C76 H76A 121.2 . . ? C71 C76 H76A 121.2 . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 0.613 _refine_diff_density_min -0.958 _refine_diff_density_rms 0.123 _database_code_depnum_ccdc_archive 'CCDC 941945' ####################################################################### # # 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_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H42 Cl4 N8 P2 Pd2 S2' _chemical_formula_weight 1139.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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 P2(1)/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 10.2310(5) _cell_length_b 12.5690(6) _cell_length_c 35.9450(16) _cell_angle_alpha 90.00 _cell_angle_beta 94.4590(18) _cell_angle_gamma 90.00 _cell_volume 4608.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour 0.26 _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2288 _exptl_absorpt_coefficient_mu 1.214 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 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_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15507 _diffrn_reflns_av_R_equivalents 0.0701 _diffrn_reflns_av_sigmaI/netI 0.1110 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 27.52 _reflns_number_total 9800 _reflns_number_gt 5271 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect(Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo and Scalepack(Otwinowski & Minor1997)' _computing_data_reduction 'Denzo and Scalepack(Otwinowski & Minor1997)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1293P)^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 costr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0063(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9800 _refine_ls_number_parameters 542 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1372 _refine_ls_R_factor_gt 0.0674 _refine_ls_wR_factor_ref 0.2299 _refine_ls_wR_factor_gt 0.1709 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.990 _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 Pd1 Pd 0.15148(6) 0.22176(5) 0.358992(17) 0.0316(2) Uani 1 1 d . . . P1 P 0.2414(2) 0.18210(17) 0.41771(6) 0.0338(5) Uani 1 1 d . . . S1 S 0.0679(2) 0.28055(19) 0.29889(6) 0.0450(6) Uani 1 1 d . . . N2 N 0.3324(7) 0.2726(5) 0.28907(19) 0.0376(16) Uani 1 1 d . . . C2 C 0.2075(8) 0.2825(7) 0.2757(2) 0.0392(19) Uani 1 1 d . . . Cl1 Cl 0.7925(6) 0.9366(5) 0.4398(2) 0.237(4) Uani 1 1 d . . . Pd2 Pd 0.40833(6) 0.27693(5) 0.346179(16) 0.0317(2) Uani 1 1 d . . . P2 P 0.3357(2) 0.44772(17) 0.35455(6) 0.0362(5) Uani 1 1 d . . . S2 S 0.4740(2) 0.09519(18) 0.34311(7) 0.0412(5) Uani 1 1 d . . . N1 N 0.2056(6) 0.0744(5) 0.33545(19) 0.0359(16) Uani 1 1 d . . . N4 N 0.2115(7) 0.2964(6) 0.23896(19) 0.048(2) Uani 1 1 d . . . Cl2 Cl 0.8310(5) 1.0646(7) 0.37477(18) 0.227(4) Uani 1 1 d . . . C3 C 0.1056(10) 0.3142(11) 0.2103(3) 0.075(4) Uani 1 1 d . . . H3A H 0.0233 0.3139 0.2214 0.112 Uiso 1 1 calc R . . H3B H 0.1059 0.2586 0.1920 0.112 Uiso 1 1 calc R . . H3C H 0.1177 0.3817 0.1986 0.112 Uiso 1 1 calc R . . Cl3 Cl 0.7579(5) 0.5389(5) 0.27042(19) 0.175(3) Uani 1 1 d . . . N5 N 0.3369(8) 0.2940(7) 0.2297(2) 0.060(2) Uani 1 1 d . . . H4A H 0.3640 0.3006 0.2077 0.072 Uiso 1 1 calc R . . Cl4 Cl 0.7184(4) 0.3560(3) 0.31546(12) 0.1122(13) Uani 1 1 d . . . N6 N 0.4075(7) 0.2796(6) 0.2605(2) 0.0475(19) Uani 1 1 d . . . H5A H 0.4916 0.2752 0.2624 0.057 Uiso 1 1 calc R . . N10 N 0.1182(8) -0.0016(6) 0.3242(2) 0.060(2) Uani 1 1 d . . . H6A H 0.0344 0.0061 0.3226 0.072 Uiso 1 1 calc R . . N9 N 0.1785(8) -0.0871(7) 0.3162(3) 0.078(3) Uani 1 1 d . . . H7A H 0.1435 -0.1464 0.3089 0.094 Uiso 1 1 calc R . . N8 N 0.3084(7) -0.0656(6) 0.3217(3) 0.059(2) Uani 1 1 d . . . C9 C 0.4058(12) -0.1470(9) 0.3145(4) 0.107(6) Uani 1 1 d . . . H9A H 0.4923 -0.1186 0.3200 0.160 Uiso 1 1 calc R . . H9B H 0.3951 -0.1679 0.2888 0.160 Uiso 1 1 calc R . . H9C H 0.3938 -0.2077 0.3301 0.160 Uiso 1 1 calc R . . C1 C 0.3233(9) 0.0358(7) 0.3331(2) 0.043(2) Uani 1 1 d . . . C11 C 0.4002(8) 0.2426(6) 0.4286(2) 0.038(2) Uani 1 1 d . . . C12 C 0.4766(8) 0.2763(7) 0.4003(2) 0.0369(18) Uani 1 1 d . . . C13 C 0.6060(8) 0.3097(7) 0.4093(2) 0.040(2) Uani 1 1 d . . . H13A H 0.6570 0.3328 0.3906 0.048 Uiso 1 1 calc R . . C14 C 0.6572(9) 0.3082(8) 0.4453(3) 0.051(2) Uani 1 1 d . . . H14A H 0.7441 0.3287 0.4505 0.062 Uiso 1 1 calc R . . C15 C 0.5860(10) 0.2777(8) 0.4743(3) 0.055(3) Uani 1 1 d . . . H15A H 0.6226 0.2787 0.4988 0.065 Uiso 1 1 calc R . . C16 C 0.4563(10) 0.2452(7) 0.4658(3) 0.049(2) Uani 1 1 d . . . H16A H 0.4058 0.2247 0.4850 0.058 Uiso 1 1 calc R . . C20 C 0.780(3) 0.417(2) 0.2861(8) 0.34(2) Uani 1 1 d . . . H20A H 0.7661 0.3728 0.2640 0.412 Uiso 1 1 calc R . . H20B H 0.8732 0.4130 0.2933 0.412 Uiso 1 1 calc R . . C21 C 0.1435(8) 0.2205(7) 0.4565(2) 0.040(2) Uani 1 1 d . . . C22 C 0.0495(9) 0.1508(9) 0.4688(3) 0.054(3) Uani 1 1 d . . . H22A H 0.0422 0.0821 0.4593 0.065 Uiso 1 1 calc R . . C23 C -0.0324(10) 0.1848(10) 0.4951(3) 0.069(3) Uani 1 1 d . . . H23A H -0.0962 0.1387 0.5027 0.082 Uiso 1 1 calc R . . C24 C -0.0223(12) 0.2854(10) 0.5104(3) 0.072(3) Uani 1 1 d . . . H24A H -0.0783 0.3071 0.5281 0.086 Uiso 1 1 calc R . . C25 C 0.0718(11) 0.3526(9) 0.4989(3) 0.064(3) Uani 1 1 d . . . H25A H 0.0835 0.4193 0.5098 0.076 Uiso 1 1 calc R . . C26 C 0.1504(10) 0.3208(8) 0.4708(3) 0.058(3) Uani 1 1 d . . . H26A H 0.2086 0.3692 0.4616 0.070 Uiso 1 1 calc R . . C30 C 0.7335(17) 1.0256(17) 0.4084(5) 0.163(9) Uani 1 1 d . . . H30A H 0.7091 1.0886 0.4218 0.195 Uiso 1 1 calc R . . H30B H 0.6536 0.9965 0.3961 0.195 Uiso 1 1 calc R . . C31 C 0.2695(8) 0.0393(7) 0.4238(2) 0.039(2) Uani 1 1 d . . . C32 C 0.1703(10) -0.0302(7) 0.4107(3) 0.052(2) Uani 1 1 d . . . H32A H 0.0903 -0.0025 0.4012 0.062 Uiso 1 1 calc R . . C33 C 0.1880(11) -0.1407(7) 0.4116(3) 0.062(3) Uani 1 1 d . . . H33A H 0.1209 -0.1865 0.4030 0.074 Uiso 1 1 calc R . . C34 C 0.3095(12) -0.1803(8) 0.4259(3) 0.069(3) Uani 1 1 d . . . H34A H 0.3239 -0.2533 0.4267 0.082 Uiso 1 1 calc R . . C35 C 0.4104(11) -0.1103(8) 0.4390(3) 0.065(3) Uani 1 1 d . . . H35A H 0.4913 -0.1369 0.4482 0.078 Uiso 1 1 calc R . . C36 C 0.3882(9) -0.0016(7) 0.4380(3) 0.047(2) Uani 1 1 d . . . H36A H 0.4543 0.0446 0.4471 0.056 Uiso 1 1 calc R . . C41 C 0.1825(8) 0.4541(6) 0.3776(2) 0.0371(19) Uani 1 1 d . . . C42 C 0.1018(8) 0.3631(6) 0.3786(2) 0.0363(19) Uani 1 1 d . . . C43 C -0.0206(8) 0.3759(7) 0.3922(2) 0.042(2) Uani 1 1 d . . . H43A H -0.0742 0.3167 0.3939 0.050 Uiso 1 1 calc R . . C44 C -0.0653(9) 0.4733(7) 0.4033(3) 0.050(2) Uani 1 1 d . . . H44A H -0.1484 0.4792 0.4120 0.061 Uiso 1 1 calc R . . C45 C 0.0140(10) 0.5629(7) 0.4017(3) 0.055(3) Uani 1 1 d . . . H45A H -0.0166 0.6293 0.4085 0.066 Uiso 1 1 calc R . . C46 C 0.1385(9) 0.5523(7) 0.3897(3) 0.047(2) Uani 1 1 d . . . H46A H 0.1936 0.6112 0.3898 0.056 Uiso 1 1 calc R . . C51 C 0.2996(9) 0.5160(7) 0.3102(3) 0.045(2) Uani 1 1 d . . . C52 C 0.1746(9) 0.5532(7) 0.2985(3) 0.055(3) Uani 1 1 d . . . H52A H 0.1081 0.5491 0.3147 0.066 Uiso 1 1 calc R . . C53 C 0.1484(13) 0.5947(9) 0.2643(3) 0.076(3) Uani 1 1 d . . . H53A H 0.0635 0.6168 0.2570 0.091 Uiso 1 1 calc R . . C54 C 0.2453(15) 0.6053(10) 0.2397(3) 0.087(4) Uani 1 1 d . . . H54A H 0.2272 0.6377 0.2166 0.105 Uiso 1 1 calc R . . C55 C 0.3683(14) 0.5674(9) 0.2500(3) 0.074(4) Uani 1 1 d . . . H55A H 0.4339 0.5722 0.2335 0.089 Uiso 1 1 calc R . . C56 C 0.3953(11) 0.5217(8) 0.2849(3) 0.059(3) Uani 1 1 d . . . H56A H 0.4784 0.4945 0.2914 0.071 Uiso 1 1 calc R . . C61 C 0.4477(9) 0.5364(7) 0.3824(3) 0.047(2) Uani 1 1 d . . . C62 C 0.4534(10) 0.5283(7) 0.4208(3) 0.056(3) Uani 1 1 d . . . H62A H 0.3952 0.4844 0.4322 0.067 Uiso 1 1 calc R . . C63 C 0.5483(12) 0.5872(9) 0.4424(3) 0.070(3) Uani 1 1 d . . . H63A H 0.5529 0.5799 0.4683 0.085 Uiso 1 1 calc R . . C64 C 0.6315(11) 0.6525(10) 0.4276(4) 0.076(4) Uani 1 1 d . . . H64A H 0.6921 0.6913 0.4427 0.091 Uiso 1 1 calc R . . C65 C 0.6267(11) 0.6618(10) 0.3895(4) 0.081(4) Uani 1 1 d . . . H65A H 0.6854 0.7063 0.3786 0.097 Uiso 1 1 calc R . . C66 C 0.5323(10) 0.6037(7) 0.3667(3) 0.060(3) Uani 1 1 d . . . H66A H 0.5281 0.6115 0.3409 0.071 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 0.0281(3) 0.0321(3) 0.0349(4) -0.0023(3) 0.0050(3) 0.0013(3) P1 0.0332(11) 0.0331(10) 0.0357(11) 0.0009(9) 0.0062(9) 0.0010(9) S1 0.0349(11) 0.0593(15) 0.0404(12) 0.0018(11) 0.0004(9) 0.0029(11) N2 0.037(4) 0.045(4) 0.032(4) -0.001(3) 0.005(3) 0.005(3) C2 0.036(5) 0.047(5) 0.035(4) 0.002(4) 0.003(4) 0.003(4) Cl1 0.148(5) 0.162(5) 0.378(10) 0.147(6) -0.132(6) -0.062(4) Pd2 0.0284(3) 0.0348(4) 0.0321(3) 0.0004(3) 0.0040(2) 0.0010(3) P2 0.0343(12) 0.0324(11) 0.0421(13) 0.0021(10) 0.0041(10) 0.0004(9) S2 0.0332(11) 0.0414(12) 0.0492(13) -0.0021(10) 0.0045(10) 0.0074(9) N1 0.031(4) 0.035(4) 0.042(4) -0.010(3) 0.002(3) 0.003(3) N4 0.046(5) 0.070(6) 0.027(4) 0.005(4) -0.007(3) -0.001(4) Cl2 0.084(3) 0.443(12) 0.152(5) 0.065(6) 0.002(3) 0.036(5) C3 0.057(7) 0.127(11) 0.038(6) 0.007(6) -0.015(5) 0.005(7) Cl3 0.136(4) 0.152(5) 0.239(7) 0.101(5) 0.028(4) 0.000(4) N5 0.048(5) 0.102(7) 0.031(4) 0.012(4) 0.008(4) 0.000(5) Cl4 0.113(3) 0.111(3) 0.117(3) 0.014(2) 0.036(3) 0.000(2) N6 0.037(4) 0.065(5) 0.042(4) 0.008(4) 0.008(3) 0.004(4) N10 0.037(4) 0.057(5) 0.085(7) -0.019(5) 0.007(4) 0.001(4) N9 0.047(5) 0.056(5) 0.134(9) -0.049(6) 0.017(6) -0.007(4) N8 0.036(4) 0.042(4) 0.101(7) -0.020(5) 0.010(4) 0.004(4) C9 0.070(8) 0.053(7) 0.200(17) -0.052(9) 0.030(10) 0.009(6) C1 0.044(5) 0.042(5) 0.044(5) -0.010(4) 0.014(4) -0.002(4) C11 0.038(5) 0.032(4) 0.045(5) 0.003(4) 0.003(4) 0.006(4) C12 0.037(4) 0.044(5) 0.030(4) 0.008(4) 0.000(3) -0.002(4) C13 0.032(4) 0.048(5) 0.040(5) -0.005(4) -0.002(4) -0.009(4) C14 0.039(5) 0.051(6) 0.064(7) 0.002(5) 0.006(5) 0.001(4) C15 0.061(6) 0.065(7) 0.036(5) -0.004(5) -0.004(5) -0.002(5) C16 0.053(6) 0.057(6) 0.035(5) 0.001(4) -0.006(4) -0.003(5) C20 0.31(3) 0.34(4) 0.42(4) 0.32(3) 0.27(3) 0.28(3) C21 0.033(4) 0.051(5) 0.035(4) 0.002(4) 0.005(4) 0.012(4) C22 0.038(5) 0.080(7) 0.046(5) 0.009(5) 0.009(4) -0.003(5) C23 0.054(7) 0.104(9) 0.052(6) 0.005(6) 0.024(5) -0.002(6) C24 0.069(8) 0.098(10) 0.050(6) -0.016(6) 0.017(6) 0.014(7) C25 0.075(7) 0.068(7) 0.050(6) -0.018(5) 0.015(6) 0.018(6) C26 0.064(7) 0.058(6) 0.054(6) -0.008(5) 0.015(5) 0.008(5) C30 0.127(15) 0.26(3) 0.102(14) 0.059(15) 0.004(12) 0.045(16) C31 0.045(5) 0.038(4) 0.035(5) 0.005(4) 0.007(4) 0.006(4) C32 0.046(5) 0.045(5) 0.064(7) -0.006(5) 0.009(5) -0.004(5) C33 0.074(7) 0.035(5) 0.074(7) 0.012(5) -0.005(6) -0.008(5) C34 0.096(9) 0.032(5) 0.075(8) -0.001(5) -0.010(7) 0.003(6) C35 0.065(7) 0.049(6) 0.080(8) 0.011(6) -0.005(6) 0.015(5) C36 0.045(5) 0.045(5) 0.051(6) 0.013(4) 0.004(4) 0.007(4) C41 0.036(4) 0.035(4) 0.042(5) -0.003(4) 0.010(4) -0.001(4) C42 0.039(5) 0.034(4) 0.038(5) 0.001(4) 0.011(4) 0.006(4) C43 0.033(4) 0.038(5) 0.055(6) -0.001(4) 0.007(4) 0.005(4) C44 0.041(5) 0.041(5) 0.070(7) -0.013(5) 0.011(5) 0.002(4) C45 0.059(6) 0.038(5) 0.069(7) -0.004(5) 0.008(5) 0.017(5) C46 0.046(5) 0.042(5) 0.053(6) -0.006(4) 0.006(4) 0.002(4) C51 0.048(5) 0.036(5) 0.051(6) 0.009(4) 0.000(4) 0.002(4) C52 0.045(5) 0.052(6) 0.067(7) 0.003(5) 0.005(5) 0.013(5) C53 0.091(9) 0.071(8) 0.062(8) 0.010(6) -0.010(7) 0.031(7) C54 0.128(12) 0.074(8) 0.056(8) 0.028(7) -0.017(8) -0.001(9) C55 0.119(11) 0.064(7) 0.044(6) 0.005(5) 0.027(7) -0.010(7) C56 0.062(7) 0.053(6) 0.065(7) 0.010(5) 0.020(6) -0.009(5) C61 0.044(5) 0.032(5) 0.066(7) 0.001(4) 0.015(5) 0.002(4) C62 0.069(7) 0.041(5) 0.056(6) -0.008(5) -0.002(5) -0.005(5) C63 0.085(9) 0.058(7) 0.064(7) -0.020(6) -0.024(6) 0.002(6) C64 0.057(7) 0.068(8) 0.097(10) -0.032(7) -0.035(7) 0.003(6) C65 0.050(7) 0.071(8) 0.121(12) -0.013(8) 0.006(7) -0.014(6) C66 0.065(7) 0.038(5) 0.076(7) -0.005(5) 0.008(6) -0.008(5) _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 C42 1.992(8) . ? Pd1 N1 2.128(6) . ? Pd1 P1 2.291(2) . ? Pd1 S1 2.378(2) . ? Pd1 Pd2 2.7905(8) . ? P1 C11 1.810(9) . ? P1 C31 1.829(8) . ? P1 C21 1.844(8) . ? S1 C2 1.710(9) . ? N2 N6 1.333(9) . ? N2 C2 1.336(11) . ? N2 Pd2 2.138(7) . ? C2 N4 1.335(10) . ? Cl1 C30 1.669(16) . ? Pd2 C12 2.017(8) . ? Pd2 P2 2.299(2) . ? Pd2 S2 2.386(2) . ? P2 C51 1.823(9) . ? P2 C41 1.831(8) . ? P2 C61 1.839(10) . ? S2 C1 1.726(9) . ? N1 C1 1.307(10) . ? N1 N10 1.348(9) . ? N4 N5 1.352(10) . ? N4 C3 1.453(11) . ? Cl2 C30 1.698(17) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? Cl3 C20 1.642(19) . ? N5 N6 1.287(10) . ? N5 H4A 0.8600 . ? Cl4 C20 1.484(18) . ? N6 H5A 0.8600 . ? N10 N9 1.283(10) . ? N10 H6A 0.8600 . ? N9 N8 1.355(11) . ? N9 H7A 0.8600 . ? N8 C1 1.344(11) . ? N8 C9 1.465(12) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C11 C12 1.394(11) . ? C11 C16 1.413(12) . ? C12 C13 1.403(11) . ? C13 C14 1.358(12) . ? C13 H13A 0.9300 . ? C14 C15 1.372(13) . ? C14 H14A 0.9300 . ? C15 C16 1.400(13) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C26 1.360(13) . ? C21 C22 1.397(12) . ? C22 C23 1.379(13) . ? C22 H22A 0.9300 . ? C23 C24 1.380(16) . ? C23 H23A 0.9300 . ? C24 C25 1.368(15) . ? C24 H24A 0.9300 . ? C25 C26 1.400(12) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C36 1.379(12) . ? C31 C32 1.393(12) . ? C32 C33 1.401(12) . ? C32 H32A 0.9300 . ? C33 C34 1.398(15) . ? C33 H33A 0.9300 . ? C34 C35 1.409(15) . ? C34 H34A 0.9300 . ? C35 C36 1.386(13) . ? C35 H35A 0.9300 . ? C36 H36A 0.9300 . ? C41 C46 1.394(11) . ? C41 C42 1.413(11) . ? C42 C43 1.388(11) . ? C43 C44 1.376(11) . ? C43 H43A 0.9300 . ? C44 C45 1.392(13) . ? C44 H44A 0.9300 . ? C45 C46 1.382(12) . ? C45 H45A 0.9300 . ? C46 H46A 0.9300 . ? C51 C56 1.389(12) . ? C51 C52 1.395(12) . ? C52 C53 1.343(14) . ? C52 H52A 0.9300 . ? C53 C54 1.385(17) . ? C53 H53A 0.9300 . ? C54 C55 1.370(17) . ? C54 H54A 0.9300 . ? C55 C56 1.388(14) . ? C55 H55A 0.9300 . ? C56 H56A 0.9300 . ? C61 C66 1.364(12) . ? C61 C62 1.378(13) . ? C62 C63 1.407(14) . ? C62 H62A 0.9300 . ? C63 C64 1.325(16) . ? C63 H63A 0.9300 . ? C64 C65 1.370(17) . ? C64 H64A 0.9300 . ? C65 C66 1.419(15) . ? C65 H65A 0.9300 . ? C66 H66A 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 C42 Pd1 N1 177.2(3) . . ? C42 Pd1 P1 87.9(2) . . ? N1 Pd1 P1 94.52(19) . . ? C42 Pd1 S1 87.8(2) . . ? N1 Pd1 S1 89.75(19) . . ? P1 Pd1 S1 174.13(8) . . ? C42 Pd1 Pd2 96.1(2) . . ? N1 Pd1 Pd2 82.73(18) . . ? P1 Pd1 Pd2 83.71(6) . . ? S1 Pd1 Pd2 92.85(6) . . ? C11 P1 C31 104.9(4) . . ? C11 P1 C21 105.0(4) . . ? C31 P1 C21 104.8(4) . . ? C11 P1 Pd1 113.4(3) . . ? C31 P1 Pd1 111.8(3) . . ? C21 P1 Pd1 115.9(3) . . ? C2 S1 Pd1 101.1(3) . . ? N6 N2 C2 108.0(7) . . ? N6 N2 Pd2 123.4(6) . . ? C2 N2 Pd2 127.6(6) . . ? N4 C2 N2 105.5(7) . . ? N4 C2 S1 125.1(7) . . ? N2 C2 S1 129.4(7) . . ? C12 Pd2 N2 178.0(3) . . ? C12 Pd2 P2 88.2(2) . . ? N2 Pd2 P2 93.01(19) . . ? C12 Pd2 S2 87.9(2) . . ? N2 Pd2 S2 90.79(19) . . ? P2 Pd2 S2 174.26(8) . . ? C12 Pd2 Pd1 95.7(2) . . ? N2 Pd2 Pd1 82.86(19) . . ? P2 Pd2 Pd1 83.81(6) . . ? S2 Pd2 Pd1 92.41(6) . . ? C51 P2 C41 104.7(4) . . ? C51 P2 C61 105.5(4) . . ? C41 P2 C61 104.2(4) . . ? C51 P2 Pd2 111.7(3) . . ? C41 P2 Pd2 113.4(3) . . ? C61 P2 Pd2 116.3(3) . . ? C1 S2 Pd2 100.0(3) . . ? C1 N1 N10 108.1(7) . . ? C1 N1 Pd1 128.2(6) . . ? N10 N1 Pd1 123.3(5) . . ? C2 N4 N5 110.1(7) . . ? C2 N4 C3 130.0(8) . . ? N5 N4 C3 119.9(7) . . ? N4 C3 H3A 109.5 . . ? N4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N6 N5 N4 105.7(7) . . ? N6 N5 H4A 127.2 . . ? N4 N5 H4A 127.2 . . ? N5 N6 N2 110.8(7) . . ? N5 N6 H5A 124.6 . . ? N2 N6 H5A 124.6 . . ? N9 N10 N1 109.9(7) . . ? N9 N10 H6A 125.0 . . ? N1 N10 H6A 125.0 . . ? N10 N9 N8 106.5(8) . . ? N10 N9 H7A 126.8 . . ? N8 N9 H7A 126.8 . . ? C1 N8 N9 108.7(7) . . ? C1 N8 C9 130.8(9) . . ? N9 N8 C9 120.5(8) . . ? N8 C9 H9A 109.5 . . ? N8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C1 N8 106.7(8) . . ? N1 C1 S2 129.7(7) . . ? N8 C1 S2 123.5(7) . . ? C12 C11 C16 118.2(8) . . ? C12 C11 P1 121.0(7) . . ? C16 C11 P1 120.3(7) . . ? C11 C12 C13 119.7(8) . . ? C11 C12 Pd2 122.2(6) . . ? C13 C12 Pd2 118.1(6) . . ? C14 C13 C12 120.2(8) . . ? C14 C13 H13A 119.9 . . ? C12 C13 H13A 119.9 . . ? C13 C14 C15 122.7(9) . . ? C13 C14 H14A 118.7 . . ? C15 C14 H14A 118.7 . . ? C14 C15 C16 117.7(9) . . ? C14 C15 H15A 121.1 . . ? C16 C15 H15A 121.1 . . ? C15 C16 C11 121.5(9) . . ? C15 C16 H16A 119.2 . . ? C11 C16 H16A 119.2 . . ? Cl4 C20 Cl3 132.1(14) . . ? Cl4 C20 H20A 104.2 . . ? Cl3 C20 H20A 104.2 . . ? Cl4 C20 H20B 104.2 . . ? Cl3 C20 H20B 104.2 . . ? H20A C20 H20B 105.5 . . ? C26 C21 C22 118.6(9) . . ? C26 C21 P1 120.8(7) . . ? C22 C21 P1 120.2(7) . . ? C23 C22 C21 119.5(10) . . ? C23 C22 H22A 120.3 . . ? C21 C22 H22A 120.3 . . ? C22 C23 C24 121.8(11) . . ? C22 C23 H23A 119.1 . . ? C24 C23 H23A 119.1 . . ? C25 C24 C23 118.5(10) . . ? C25 C24 H24A 120.7 . . ? C23 C24 H24A 120.7 . . ? C24 C25 C26 119.9(10) . . ? C24 C25 H25A 120.0 . . ? C26 C25 H25A 120.0 . . ? C21 C26 C25 121.4(10) . . ? C21 C26 H26A 119.3 . . ? C25 C26 H26A 119.3 . . ? Cl1 C30 Cl2 118.3(11) . . ? Cl1 C30 H30A 107.7 . . ? Cl2 C30 H30A 107.7 . . ? Cl1 C30 H30B 107.7 . . ? Cl2 C30 H30B 107.7 . . ? H30A C30 H30B 107.1 . . ? C36 C31 C32 119.3(8) . . ? C36 C31 P1 122.4(7) . . ? C32 C31 P1 118.1(7) . . ? C31 C32 C33 121.6(9) . . ? C31 C32 H32A 119.2 . . ? C33 C32 H32A 119.2 . . ? C34 C33 C32 118.1(10) . . ? C34 C33 H33A 121.0 . . ? C32 C33 H33A 121.0 . . ? C33 C34 C35 120.5(9) . . ? C33 C34 H34A 119.7 . . ? C35 C34 H34A 119.7 . . ? C36 C35 C34 119.5(10) . . ? C36 C35 H35A 120.2 . . ? C34 C35 H35A 120.2 . . ? C31 C36 C35 120.9(9) . . ? C31 C36 H36A 119.5 . . ? C35 C36 H36A 119.5 . . ? C46 C41 C42 120.3(7) . . ? C46 C41 P2 119.2(6) . . ? C42 C41 P2 119.9(6) . . ? C43 C42 C41 117.4(7) . . ? C43 C42 Pd1 119.4(6) . . ? C41 C42 Pd1 123.2(6) . . ? C44 C43 C42 122.3(8) . . ? C44 C43 H43A 118.8 . . ? C42 C43 H43A 118.8 . . ? C43 C44 C45 119.9(8) . . ? C43 C44 H44A 120.0 . . ? C45 C44 H44A 120.0 . . ? C46 C45 C44 119.3(8) . . ? C46 C45 H45A 120.4 . . ? C44 C45 H45A 120.4 . . ? C45 C46 C41 120.7(9) . . ? C45 C46 H46A 119.7 . . ? C41 C46 H46A 119.7 . . ? C56 C51 C52 117.5(9) . . ? C56 C51 P2 119.4(7) . . ? C52 C51 P2 122.7(8) . . ? C53 C52 C51 121.3(10) . . ? C53 C52 H52A 119.4 . . ? C51 C52 H52A 119.4 . . ? C52 C53 C54 121.3(11) . . ? C52 C53 H53A 119.3 . . ? C54 C53 H53A 119.3 . . ? C55 C54 C53 118.9(11) . . ? C55 C54 H54A 120.6 . . ? C53 C54 H54A 120.6 . . ? C54 C55 C56 120.1(11) . . ? C54 C55 H55A 119.9 . . ? C56 C55 H55A 119.9 . . ? C55 C56 C51 120.8(11) . . ? C55 C56 H56A 119.6 . . ? C51 C56 H56A 119.6 . . ? C66 C61 C62 118.8(10) . . ? C66 C61 P2 122.6(8) . . ? C62 C61 P2 118.4(7) . . ? C61 C62 C63 119.2(10) . . ? C61 C62 H62A 120.4 . . ? C63 C62 H62A 120.4 . . ? C64 C63 C62 122.7(12) . . ? C64 C63 H63A 118.7 . . ? C62 C63 H63A 118.7 . . ? C63 C64 C65 118.8(11) . . ? C63 C64 H64A 120.6 . . ? C65 C64 H64A 120.6 . . ? C64 C65 C66 120.1(12) . . ? C64 C65 H65A 119.9 . . ? C66 C65 H65A 119.9 . . ? C61 C66 C65 120.4(11) . . ? C61 C66 H66A 119.8 . . ? C65 C66 H66A 119.8 . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 1.349 _refine_diff_density_min -1.563 _refine_diff_density_rms 0.312 _database_code_depnum_ccdc_archive 'CCDC 941946' ####################################################################### # # 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_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H44 Cl8 N8 P2 Pd2 S2' _chemical_formula_weight 1295.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3750(6) _cell_length_b 13.1110(5) _cell_length_c 16.1830(7) _cell_angle_alpha 82.393(2) _cell_angle_beta 87.808(2) _cell_angle_gamma 73.407(3) _cell_volume 2494.19(19) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour ? _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.725 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 1.340 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21524 _diffrn_reflns_av_R_equivalents 0.0603 _diffrn_reflns_av_sigmaI/netI 0.0997 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 27.52 _reflns_number_total 11396 _reflns_number_gt 6815 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect(Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo and Scalepack(Otwinowski & Minor1997)' _computing_data_reduction 'Denzo and Scalepack(Otwinowski & Minor1997)' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0751P)^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 11396 _refine_ls_number_parameters 586 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1046 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1566 _refine_ls_wR_factor_gt 0.1214 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 Pd1 Pd -0.04194(4) 0.73439(3) 0.18100(3) 0.02519(13) Uani 1 1 d . . . S1 S -0.20485(13) 0.88673(12) 0.16368(9) 0.0313(3) Uani 1 1 d . . . Cl1 Cl -0.09139(13) 0.69403(11) 0.04615(9) 0.0329(3) Uani 1 1 d . . . P1 P 0.12200(13) 0.59645(11) 0.19160(9) 0.0271(3) Uani 1 1 d . . . N1 N -0.1406(4) 0.6327(3) 0.2410(3) 0.0290(11) Uani 1 1 d . . . C1 C -0.2437(5) 0.8901(4) 0.2656(4) 0.0290(13) Uani 1 1 d . . . Pd2 Pd -0.00598(4) 0.75919(3) 0.33546(3) 0.02548(13) Uani 1 1 d . . . Cl2 Cl -0.00093(13) 0.80067(11) 0.47749(9) 0.0333(3) Uani 1 1 d . . . P2 P 0.03872(13) 0.91355(11) 0.28157(9) 0.0267(3) Uani 1 1 d . . . S2 S -0.03856(14) 0.59406(12) 0.39573(9) 0.0343(4) Uani 1 1 d . . . N2 N -0.1853(4) 0.8391(4) 0.3335(3) 0.0273(11) Uani 1 1 d . . . C2 C -0.1203(5) 0.5780(4) 0.3183(4) 0.0301(13) Uani 1 1 d . . . N3 N -0.2113(4) 0.5923(4) 0.2052(3) 0.0357(12) Uani 1 1 d . . . H3A H -0.2387 0.6153 0.1560 0.043 Uiso 1 1 calc R . . C3 C -0.1817(7) 0.4211(5) 0.3922(4) 0.0503(19) Uani 1 1 d . . . H3B H -0.1361 0.4248 0.4377 0.075 Uiso 1 1 calc R . . H3C H -0.1541 0.3519 0.3732 0.075 Uiso 1 1 calc R . . H3D H -0.2584 0.4317 0.4104 0.075 Uiso 1 1 calc R . . Cl3 Cl 0.3228(2) 0.13055(16) 0.1457(2) 0.1170(12) Uani 1 1 d . . . N4 N -0.2336(5) 0.5155(4) 0.2527(3) 0.0399(13) Uani 1 1 d . . . H4A H -0.2768 0.4783 0.2412 0.048 Uiso 1 1 calc R . . C4 C -0.4388(6) 1.0213(5) 0.2456(4) 0.0462(17) Uani 1 1 d . . . H4B H -0.4219 1.0230 0.1871 0.069 Uiso 1 1 calc R . . H4C H -0.4516 1.0919 0.2613 0.069 Uiso 1 1 calc R . . H4D H -0.5052 0.9979 0.2570 0.069 Uiso 1 1 calc R . . Cl4 Cl 0.42413(17) 0.30540(15) 0.13727(14) 0.0611(5) Uani 1 1 d . . . N5 N -0.1763(4) 0.5034(4) 0.3249(3) 0.0373(13) Uani 1 1 d . . . C5 C 0.3035(6) 0.2646(5) 0.1191(5) 0.0536(19) Uani 1 1 d . . . H5A H 0.2408 0.3036 0.1509 0.064 Uiso 1 1 calc R . . H5B H 0.2838 0.2834 0.0605 0.064 Uiso 1 1 calc R . . Cl5 Cl 0.51192(19) 0.7125(2) 0.19810(16) 0.0931(8) Uani 1 1 d . . . N6 N -0.2508(4) 0.8634(4) 0.3995(3) 0.0361(12) Uani 1 1 d . . . H6A H -0.2313 0.8387 0.4504 0.043 Uiso 1 1 calc R . . Cl6 Cl 0.4913(3) 0.8723(2) 0.0542(2) 0.1137(11) Uani 1 1 d . . . C6 C 0.5767(7) 0.7566(6) 0.1065(5) 0.059(2) Uani 1 1 d . . . H6B H 0.6467 0.7692 0.1211 0.071 Uiso 1 1 calc R . . H6C H 0.5947 0.7009 0.0702 0.071 Uiso 1 1 calc R . . N7 N -0.3461(5) 0.9283(4) 0.3772(3) 0.0398(13) Uani 1 1 d . . . H7A H -0.4008 0.9547 0.4096 0.048 Uiso 1 1 calc R . . Cl7 Cl 0.61459(17) 0.66537(16) 0.42617(13) 0.0627(5) Uani 1 1 d . . . C7 C 0.6733(7) 0.6762(6) 0.5194(4) 0.058(2) Uani 1 1 d . . . H7B H 0.7058 0.6049 0.5484 0.070 Uiso 1 1 calc R . . H7C H 0.7338 0.7094 0.5071 0.070 Uiso 1 1 calc R . . N8 N -0.3453(4) 0.9480(4) 0.2926(3) 0.0348(12) Uani 1 1 d . . . Cl8 Cl 0.5763(3) 0.7510(2) 0.58446(17) 0.0986(9) Uani 1 1 d . . . C11 C 0.2100(5) 0.6096(4) 0.2736(4) 0.0285(13) Uani 1 1 d . . . C12 C 0.1618(5) 0.6756(4) 0.3348(3) 0.0270(13) Uani 1 1 d . . . C13 C 0.2305(5) 0.6785(5) 0.4002(3) 0.0317(14) Uani 1 1 d . . . H13A H 0.2009 0.7224 0.4410 0.038 Uiso 1 1 calc R . . C14 C 0.3423(5) 0.6171(5) 0.4054(4) 0.0363(15) Uani 1 1 d . . . H14A H 0.3862 0.6206 0.4497 0.044 Uiso 1 1 calc R . . C15 C 0.3898(5) 0.5508(5) 0.3460(4) 0.0386(15) Uani 1 1 d . . . H15A H 0.4643 0.5085 0.3506 0.046 Uiso 1 1 calc R . . C16 C 0.3232(5) 0.5489(5) 0.2788(4) 0.0367(15) Uani 1 1 d . . . H16A H 0.3545 0.5069 0.2371 0.044 Uiso 1 1 calc R . . C21 C 0.0939(5) 0.4666(4) 0.2170(4) 0.0297(13) Uani 1 1 d . . . C22 C 0.1441(6) 0.3976(5) 0.2876(4) 0.0416(16) Uani 1 1 d . . . H22A H 0.1915 0.4184 0.3210 0.050 Uiso 1 1 calc R . . C23 C 0.1233(6) 0.2986(5) 0.3081(4) 0.0478(18) Uani 1 1 d . . . H23A H 0.1567 0.2531 0.3549 0.057 Uiso 1 1 calc R . . C24 C 0.0527(6) 0.2681(5) 0.2581(4) 0.0472(18) Uani 1 1 d . . . H24A H 0.0384 0.2020 0.2716 0.057 Uiso 1 1 calc R . . C25 C 0.0029(6) 0.3360(5) 0.1877(4) 0.0404(16) Uani 1 1 d . . . H25A H -0.0433 0.3145 0.1538 0.048 Uiso 1 1 calc R . . C26 C 0.0221(5) 0.4358(5) 0.1681(4) 0.0337(14) Uani 1 1 d . . . H26A H -0.0132 0.4820 0.1222 0.040 Uiso 1 1 calc R . . C31 C 0.2090(5) 0.5862(4) 0.0969(3) 0.0300(13) Uani 1 1 d . . . C32 C 0.1898(5) 0.5291(4) 0.0350(4) 0.0315(14) Uani 1 1 d . . . H32A H 0.1320 0.4963 0.0407 0.038 Uiso 1 1 calc R . . C33 C 0.2575(5) 0.5218(5) -0.0347(4) 0.0362(15) Uani 1 1 d . . . H33A H 0.2459 0.4825 -0.0757 0.043 Uiso 1 1 calc R . . C34 C 0.3418(6) 0.5714(5) -0.0448(4) 0.0426(16) Uani 1 1 d . . . H34A H 0.3869 0.5662 -0.0923 0.051 Uiso 1 1 calc R . . C35 C 0.3588(6) 0.6292(5) 0.0164(4) 0.0415(16) Uani 1 1 d . . . H35A H 0.4162 0.6625 0.0105 0.050 Uiso 1 1 calc R . . C36 C 0.2920(5) 0.6377(5) 0.0854(4) 0.0343(14) Uani 1 1 d . . . H36A H 0.3025 0.6789 0.1253 0.041 Uiso 1 1 calc R . . C41 C 0.0762(5) 0.9089(4) 0.1725(3) 0.0265(13) Uani 1 1 d . . . C42 C 0.0513(5) 0.8334(4) 0.1288(3) 0.0276(13) Uani 1 1 d . . . C43 C 0.0839(5) 0.8336(5) 0.0456(4) 0.0302(13) Uani 1 1 d . . . H43A H 0.0666 0.7861 0.0140 0.036 Uiso 1 1 calc R . . C44 C 0.1421(5) 0.9042(5) 0.0096(4) 0.0347(14) Uani 1 1 d . . . H44A H 0.1666 0.9006 -0.0452 0.042 Uiso 1 1 calc R . . C45 C 0.1646(5) 0.9795(5) 0.0529(4) 0.0345(14) Uani 1 1 d . . . H45A H 0.2010 1.0282 0.0271 0.041 Uiso 1 1 calc R . . C46 C 0.1329(5) 0.9812(5) 0.1334(4) 0.0332(14) Uani 1 1 d . . . H46A H 0.1488 1.0309 0.1636 0.040 Uiso 1 1 calc R . . C51 C 0.1590(5) 0.9352(4) 0.3303(3) 0.0283(13) Uani 1 1 d . . . C52 C 0.1439(5) 1.0031(4) 0.3919(3) 0.0304(14) Uani 1 1 d . . . H52A H 0.0717 1.0383 0.4088 0.036 Uiso 1 1 calc R . . C53 C 0.2379(5) 1.0178(5) 0.4281(4) 0.0353(15) Uani 1 1 d . . . H53A H 0.2281 1.0648 0.4679 0.042 Uiso 1 1 calc R . . C54 C 0.3445(6) 0.9636(5) 0.4056(4) 0.0390(15) Uani 1 1 d . . . H54A H 0.4070 0.9715 0.4315 0.047 Uiso 1 1 calc R . . C55 C 0.3585(5) 0.8969(5) 0.3442(4) 0.0407(16) Uani 1 1 d . . . H55A H 0.4309 0.8609 0.3282 0.049 Uiso 1 1 calc R . . C56 C 0.2681(5) 0.8831(5) 0.3068(4) 0.0337(14) Uani 1 1 d . . . H56A H 0.2792 0.8385 0.2652 0.040 Uiso 1 1 calc R . . C61 C -0.0799(5) 1.0334(4) 0.2874(4) 0.0302(13) Uani 1 1 d . . . C62 C -0.1180(5) 1.1047(5) 0.2164(4) 0.0344(14) Uani 1 1 d . . . H62A H -0.0813 1.0936 0.1657 0.041 Uiso 1 1 calc R . . C63 C -0.2112(6) 1.1929(5) 0.2212(4) 0.0450(17) Uani 1 1 d . . . H63A H -0.2367 1.2404 0.1734 0.054 Uiso 1 1 calc R . . C64 C -0.2665(6) 1.2110(5) 0.2956(4) 0.0448(17) Uani 1 1 d . . . H64A H -0.3298 1.2696 0.2977 0.054 Uiso 1 1 calc R . . C65 C -0.2276(6) 1.1416(5) 0.3678(4) 0.0424(16) Uani 1 1 d . . . H65A H -0.2631 1.1545 0.4186 0.051 Uiso 1 1 calc R . . C66 C -0.1356(5) 1.0530(5) 0.3632(4) 0.0340(14) Uani 1 1 d . . . H66A H -0.1103 1.0058 0.4112 0.041 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 0.0323(3) 0.0240(2) 0.0212(2) -0.00122(17) -0.00090(18) -0.01175(19) S1 0.0347(9) 0.0330(8) 0.0261(8) -0.0009(6) -0.0013(7) -0.0105(7) Cl1 0.0422(9) 0.0340(8) 0.0260(8) -0.0041(6) -0.0031(7) -0.0161(7) P1 0.0338(9) 0.0239(7) 0.0254(8) -0.0028(6) -0.0005(7) -0.0113(7) N1 0.039(3) 0.027(3) 0.024(3) -0.002(2) 0.001(2) -0.015(2) C1 0.032(3) 0.027(3) 0.033(3) -0.005(3) -0.001(3) -0.017(3) Pd2 0.0333(3) 0.0248(2) 0.0206(2) -0.00089(17) -0.00017(19) -0.0127(2) Cl2 0.0453(9) 0.0342(8) 0.0216(7) -0.0034(6) -0.0006(6) -0.0130(7) P2 0.0343(9) 0.0263(8) 0.0221(8) -0.0019(6) -0.0002(7) -0.0131(7) S2 0.0477(10) 0.0331(8) 0.0268(8) 0.0013(6) -0.0023(7) -0.0208(7) N2 0.034(3) 0.027(2) 0.022(3) 0.000(2) 0.000(2) -0.011(2) C2 0.032(3) 0.029(3) 0.030(3) -0.004(3) -0.004(3) -0.010(3) N3 0.042(3) 0.041(3) 0.027(3) 0.000(2) -0.005(2) -0.017(3) C3 0.074(5) 0.042(4) 0.043(4) 0.010(3) -0.002(4) -0.034(4) Cl3 0.0647(15) 0.0401(12) 0.246(4) 0.0095(16) -0.060(2) -0.0191(11) N4 0.051(4) 0.044(3) 0.035(3) -0.001(3) -0.003(3) -0.031(3) C4 0.041(4) 0.046(4) 0.046(4) 0.002(3) -0.005(3) -0.008(3) Cl4 0.0559(12) 0.0483(11) 0.0848(15) -0.0081(10) 0.0019(11) -0.0241(9) N5 0.046(3) 0.035(3) 0.036(3) 0.002(2) -0.004(3) -0.022(3) C5 0.047(4) 0.042(4) 0.071(5) -0.005(4) -0.008(4) -0.011(3) Cl5 0.0508(14) 0.151(2) 0.0716(16) -0.0168(16) 0.0081(12) -0.0181(15) N6 0.041(3) 0.038(3) 0.031(3) 0.000(2) -0.004(3) -0.016(3) Cl6 0.123(2) 0.0609(15) 0.139(3) -0.0031(15) -0.060(2) 0.0053(15) C6 0.061(5) 0.050(4) 0.068(5) -0.008(4) -0.009(4) -0.018(4) N7 0.037(3) 0.045(3) 0.040(3) -0.016(3) 0.009(3) -0.013(3) Cl7 0.0555(12) 0.0650(12) 0.0709(14) -0.0075(10) -0.0152(10) -0.0209(10) C7 0.068(5) 0.057(5) 0.051(5) 0.011(4) -0.006(4) -0.027(4) N8 0.038(3) 0.040(3) 0.027(3) -0.005(2) 0.000(2) -0.012(3) Cl8 0.125(2) 0.0884(18) 0.0798(18) -0.0207(14) 0.0240(16) -0.0251(17) C11 0.031(3) 0.026(3) 0.028(3) 0.003(2) -0.002(3) -0.012(3) C12 0.032(3) 0.027(3) 0.022(3) 0.005(2) 0.002(2) -0.012(3) C13 0.043(4) 0.034(3) 0.022(3) 0.002(3) -0.006(3) -0.018(3) C14 0.041(4) 0.040(4) 0.028(3) 0.005(3) -0.007(3) -0.015(3) C15 0.034(4) 0.042(4) 0.039(4) -0.002(3) -0.002(3) -0.010(3) C16 0.036(4) 0.038(4) 0.035(4) -0.007(3) 0.000(3) -0.007(3) C21 0.040(4) 0.024(3) 0.027(3) -0.006(2) 0.003(3) -0.011(3) C22 0.054(4) 0.032(3) 0.040(4) 0.003(3) -0.009(3) -0.017(3) C23 0.068(5) 0.030(3) 0.044(4) 0.015(3) -0.013(4) -0.019(3) C24 0.061(5) 0.034(4) 0.052(4) 0.005(3) -0.003(4) -0.026(3) C25 0.056(4) 0.035(3) 0.038(4) -0.008(3) 0.001(3) -0.023(3) C26 0.039(4) 0.031(3) 0.032(3) -0.004(3) 0.000(3) -0.012(3) C31 0.034(4) 0.030(3) 0.023(3) 0.000(2) -0.002(3) -0.005(3) C32 0.036(4) 0.029(3) 0.029(3) -0.002(3) -0.002(3) -0.009(3) C33 0.044(4) 0.035(3) 0.027(3) -0.009(3) 0.000(3) -0.005(3) C34 0.042(4) 0.045(4) 0.036(4) -0.001(3) 0.004(3) -0.006(3) C35 0.037(4) 0.052(4) 0.036(4) -0.004(3) 0.004(3) -0.015(3) C36 0.041(4) 0.035(3) 0.030(3) -0.007(3) 0.002(3) -0.015(3) C41 0.031(3) 0.028(3) 0.023(3) -0.001(2) -0.003(2) -0.014(3) C42 0.033(3) 0.025(3) 0.026(3) 0.002(2) -0.001(3) -0.011(3) C43 0.032(3) 0.033(3) 0.026(3) -0.004(3) 0.002(3) -0.011(3) C44 0.039(4) 0.041(4) 0.023(3) 0.002(3) 0.002(3) -0.012(3) C45 0.048(4) 0.037(3) 0.024(3) 0.001(3) 0.000(3) -0.023(3) C46 0.045(4) 0.033(3) 0.027(3) -0.002(3) 0.000(3) -0.021(3) C51 0.035(4) 0.029(3) 0.022(3) 0.001(2) 0.002(3) -0.013(3) C52 0.040(4) 0.026(3) 0.026(3) -0.001(2) 0.001(3) -0.013(3) C53 0.047(4) 0.039(3) 0.027(3) -0.004(3) -0.001(3) -0.023(3) C54 0.038(4) 0.050(4) 0.033(4) 0.003(3) -0.009(3) -0.020(3) C55 0.028(4) 0.048(4) 0.050(4) -0.004(3) 0.003(3) -0.019(3) C56 0.044(4) 0.028(3) 0.034(4) -0.005(3) 0.004(3) -0.017(3) C61 0.036(4) 0.027(3) 0.032(3) -0.003(3) -0.005(3) -0.015(3) C62 0.045(4) 0.032(3) 0.028(3) 0.001(3) -0.007(3) -0.016(3) C63 0.059(5) 0.032(4) 0.042(4) 0.005(3) -0.015(4) -0.012(3) C64 0.043(4) 0.034(4) 0.054(5) -0.008(3) -0.004(4) -0.005(3) C65 0.052(4) 0.033(3) 0.045(4) -0.005(3) 0.008(3) -0.017(3) C66 0.039(4) 0.034(3) 0.032(4) -0.002(3) -0.003(3) -0.016(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C42 2.055(5) . ? Pd1 N1 2.169(4) . ? Pd1 P1 2.2946(16) . ? Pd1 S1 2.3931(16) . ? Pd1 Cl1 2.4514(14) . ? Pd1 Pd2 2.6334(6) . ? S1 C1 1.704(6) . ? P1 C11 1.804(6) . ? P1 C21 1.825(5) . ? P1 C31 1.836(6) . ? N1 N3 1.329(6) . ? N1 C2 1.352(7) . ? C1 N2 1.329(7) . ? C1 N8 1.358(8) . ? Pd2 C12 2.053(6) . ? Pd2 N2 2.166(5) . ? Pd2 P2 2.3016(15) . ? Pd2 S2 2.3896(15) . ? Pd2 Cl2 2.4380(14) . ? P2 C41 1.812(6) . ? P2 C51 1.818(6) . ? P2 C61 1.828(6) . ? S2 C2 1.711(6) . ? N2 N6 1.332(7) . ? C2 N5 1.343(7) . ? N3 N4 1.271(7) . ? N3 H3A 0.8600 . ? C3 N5 1.442(7) . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C3 H3D 0.9600 . ? Cl3 C5 1.703(7) . ? N4 N5 1.357(7) . ? N4 H4A 0.8600 . ? C4 N8 1.443(8) . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C4 H4D 0.9600 . ? Cl4 C5 1.769(7) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? Cl5 C6 1.766(8) . ? N6 N7 1.274(7) . ? N6 H6A 0.8600 . ? Cl6 C6 1.717(8) . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? N7 N8 1.360(7) . ? N7 H7A 0.8600 . ? Cl7 C7 1.738(7) . ? C7 Cl8 1.736(8) . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C11 C16 1.399(8) . ? C11 C12 1.406(8) . ? C12 C13 1.393(7) . ? C13 C14 1.387(9) . ? C13 H13A 0.9300 . ? C14 C15 1.383(8) . ? C14 H14A 0.9300 . ? C15 C16 1.396(8) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? C21 C26 1.385(8) . ? C21 C22 1.403(8) . ? C22 C23 1.390(8) . ? C22 H22A 0.9300 . ? C23 C24 1.384(9) . ? C23 H23A 0.9300 . ? C24 C25 1.394(9) . ? C24 H24A 0.9300 . ? C25 C26 1.390(8) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C31 C36 1.377(8) . ? C31 C32 1.391(8) . ? C32 C33 1.376(8) . ? C32 H32A 0.9300 . ? C33 C34 1.373(9) . ? C33 H33A 0.9300 . ? C34 C35 1.380(9) . ? C34 H34A 0.9300 . ? C35 C36 1.361(8) . ? C35 H35A 0.9300 . ? C36 H36A 0.9300 . ? C41 C42 1.396(7) . ? C41 C46 1.407(8) . ? C42 C43 1.390(8) . ? C43 C44 1.386(8) . ? C43 H43A 0.9300 . ? C44 C45 1.378(8) . ? C44 H44A 0.9300 . ? C45 C46 1.347(8) . ? C45 H45A 0.9300 . ? C46 H46A 0.9300 . ? C51 C56 1.392(8) . ? C51 C52 1.396(8) . ? C52 C53 1.393(8) . ? C52 H52A 0.9300 . ? C53 C54 1.369(9) . ? C53 H53A 0.9300 . ? C54 C55 1.384(9) . ? C54 H54A 0.9300 . ? C55 C56 1.359(8) . ? C55 H55A 0.9300 . ? C56 H56A 0.9300 . ? C61 C62 1.387(8) . ? C61 C66 1.401(8) . ? C62 C63 1.389(9) . ? C62 H62A 0.9300 . ? C63 C64 1.376(9) . ? C63 H63A 0.9300 . ? C64 C65 1.391(9) . ? C64 H64A 0.9300 . ? C65 C66 1.382(9) . ? C65 H65A 0.9300 . ? C66 H66A 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 C42 Pd1 N1 177.60(19) . . ? C42 Pd1 P1 87.83(16) . . ? N1 Pd1 P1 92.70(13) . . ? C42 Pd1 S1 87.72(16) . . ? N1 Pd1 S1 91.76(13) . . ? P1 Pd1 S1 175.51(6) . . ? C42 Pd1 Cl1 93.92(16) . . ? N1 Pd1 Cl1 88.39(12) . . ? P1 Pd1 Cl1 93.18(5) . . ? S1 Pd1 Cl1 86.47(5) . . ? C42 Pd1 Pd2 94.39(15) . . ? N1 Pd1 Pd2 83.31(12) . . ? P1 Pd1 Pd2 87.08(4) . . ? S1 Pd1 Pd2 93.92(4) . . ? Cl1 Pd1 Pd2 171.69(4) . . ? C1 S1 Pd1 98.6(2) . . ? C11 P1 C21 107.0(3) . . ? C11 P1 C31 106.5(3) . . ? C21 P1 C31 105.7(3) . . ? C11 P1 Pd1 110.7(2) . . ? C21 P1 Pd1 111.4(2) . . ? C31 P1 Pd1 115.02(19) . . ? N3 N1 C2 106.3(4) . . ? N3 N1 Pd1 127.6(4) . . ? C2 N1 Pd1 124.4(4) . . ? N2 C1 N8 106.4(5) . . ? N2 C1 S1 128.9(5) . . ? N8 C1 S1 124.7(5) . . ? C12 Pd2 N2 176.53(19) . . ? C12 Pd2 P2 89.73(15) . . ? N2 Pd2 P2 92.91(12) . . ? C12 Pd2 S2 86.43(15) . . ? N2 Pd2 S2 91.01(12) . . ? P2 Pd2 S2 175.73(6) . . ? C12 Pd2 Cl2 93.88(16) . . ? N2 Pd2 Cl2 88.32(13) . . ? P2 Pd2 Cl2 91.51(5) . . ? S2 Pd2 Cl2 86.89(5) . . ? C12 Pd2 Pd1 94.58(15) . . ? N2 Pd2 Pd1 83.31(12) . . ? P2 Pd2 Pd1 87.19(4) . . ? S2 Pd2 Pd1 94.98(4) . . ? Cl2 Pd2 Pd1 171.44(4) . . ? C41 P2 C51 105.3(3) . . ? C41 P2 C61 107.1(3) . . ? C51 P2 C61 107.3(3) . . ? C41 P2 Pd2 109.79(18) . . ? C51 P2 Pd2 114.88(19) . . ? C61 P2 Pd2 112.05(19) . . ? C2 S2 Pd2 98.5(2) . . ? C1 N2 N6 107.8(5) . . ? C1 N2 Pd2 124.7(4) . . ? N6 N2 Pd2 126.4(4) . . ? N5 C2 N1 106.9(5) . . ? N5 C2 S2 124.1(5) . . ? N1 C2 S2 129.0(4) . . ? N4 N3 N1 111.8(5) . . ? N4 N3 H3A 124.1 . . ? N1 N3 H3A 124.1 . . ? N5 C3 H3B 109.5 . . ? N5 C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N5 C3 H3D 109.5 . . ? H3B C3 H3D 109.5 . . ? H3C C3 H3D 109.5 . . ? N3 N4 N5 107.1(5) . . ? N3 N4 H4A 126.4 . . ? N5 N4 H4A 126.4 . . ? N8 C4 H4B 109.5 . . ? N8 C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N8 C4 H4D 109.5 . . ? H4B C4 H4D 109.5 . . ? H4C C4 H4D 109.5 . . ? C2 N5 N4 107.9(5) . . ? C2 N5 C3 130.7(5) . . ? N4 N5 C3 121.4(5) . . ? Cl3 C5 Cl4 113.1(4) . . ? Cl3 C5 H5A 109.0 . . ? Cl4 C5 H5A 109.0 . . ? Cl3 C5 H5B 109.0 . . ? Cl4 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? N7 N6 N2 110.8(5) . . ? N7 N6 H6A 124.6 . . ? N2 N6 H6A 124.6 . . ? Cl6 C6 Cl5 111.8(5) . . ? Cl6 C6 H6B 109.2 . . ? Cl5 C6 H6B 109.2 . . ? Cl6 C6 H6C 109.2 . . ? Cl5 C6 H6C 109.2 . . ? H6B C6 H6C 107.9 . . ? N6 N7 N8 107.2(5) . . ? N6 N7 H7A 126.4 . . ? N8 N7 H7A 126.4 . . ? Cl8 C7 Cl7 113.2(5) . . ? Cl8 C7 H7B 108.9 . . ? Cl7 C7 H7B 108.9 . . ? Cl8 C7 H7C 108.9 . . ? Cl7 C7 H7C 108.9 . . ? H7B C7 H7C 107.8 . . ? C1 N8 N7 107.7(5) . . ? C1 N8 C4 129.8(5) . . ? N7 N8 C4 122.6(5) . . ? C16 C11 C12 120.6(5) . . ? C16 C11 P1 119.9(4) . . ? C12 C11 P1 119.3(4) . . ? C13 C12 C11 117.8(5) . . ? C13 C12 Pd2 119.3(4) . . ? C11 C12 Pd2 122.8(4) . . ? C14 C13 C12 121.2(6) . . ? C14 C13 H13A 119.4 . . ? C12 C13 H13A 119.4 . . ? C15 C14 C13 121.3(6) . . ? C15 C14 H14A 119.3 . . ? C13 C14 H14A 119.3 . . ? C14 C15 C16 118.4(6) . . ? C14 C15 H15A 120.8 . . ? C16 C15 H15A 120.8 . . ? C15 C16 C11 120.7(6) . . ? C15 C16 H16A 119.7 . . ? C11 C16 H16A 119.7 . . ? C26 C21 C22 119.5(5) . . ? C26 C21 P1 120.8(4) . . ? C22 C21 P1 119.7(4) . . ? C23 C22 C21 120.5(6) . . ? C23 C22 H22A 119.8 . . ? C21 C22 H22A 119.8 . . ? C24 C23 C22 119.5(6) . . ? C24 C23 H23A 120.3 . . ? C22 C23 H23A 120.3 . . ? C23 C24 C25 120.3(6) . . ? C23 C24 H24A 119.8 . . ? C25 C24 H24A 119.8 . . ? C26 C25 C24 120.1(6) . . ? C26 C25 H25A 119.9 . . ? C24 C25 H25A 119.9 . . ? C21 C26 C25 120.1(6) . . ? C21 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? C36 C31 C32 119.3(6) . . ? C36 C31 P1 120.0(4) . . ? C32 C31 P1 120.6(5) . . ? C33 C32 C31 119.2(6) . . ? C33 C32 H32A 120.4 . . ? C31 C32 H32A 120.4 . . ? C34 C33 C32 121.2(6) . . ? C34 C33 H33A 119.4 . . ? C32 C33 H33A 119.4 . . ? C33 C34 C35 119.1(6) . . ? C33 C34 H34A 120.5 . . ? C35 C34 H34A 120.5 . . ? C36 C35 C34 120.4(6) . . ? C36 C35 H35A 119.8 . . ? C34 C35 H35A 119.8 . . ? C35 C36 C31 120.9(6) . . ? C35 C36 H36A 119.6 . . ? C31 C36 H36A 119.6 . . ? C42 C41 C46 120.8(5) . . ? C42 C41 P2 120.6(4) . . ? C46 C41 P2 118.6(4) . . ? C43 C42 C41 117.4(5) . . ? C43 C42 Pd1 120.5(4) . . ? C41 C42 Pd1 121.8(4) . . ? C44 C43 C42 120.3(5) . . ? C44 C43 H43A 119.9 . . ? C42 C43 H43A 119.9 . . ? C45 C44 C43 121.8(6) . . ? C45 C44 H44A 119.1 . . ? C43 C44 H44A 119.1 . . ? C46 C45 C44 118.8(6) . . ? C46 C45 H45A 120.6 . . ? C44 C45 H45A 120.6 . . ? C45 C46 C41 120.9(5) . . ? C45 C46 H46A 119.6 . . ? C41 C46 H46A 119.6 . . ? C56 C51 C52 118.9(5) . . ? C56 C51 P2 120.1(4) . . ? C52 C51 P2 121.0(5) . . ? C53 C52 C51 119.5(6) . . ? C53 C52 H52A 120.2 . . ? C51 C52 H52A 120.2 . . ? C54 C53 C52 120.6(6) . . ? C54 C53 H53A 119.7 . . ? C52 C53 H53A 119.7 . . ? C53 C54 C55 119.4(6) . . ? C53 C54 H54A 120.3 . . ? C55 C54 H54A 120.3 . . ? C56 C55 C54 121.0(6) . . ? C56 C55 H55A 119.5 . . ? C54 C55 H55A 119.5 . . ? C55 C56 C51 120.4(6) . . ? C55 C56 H56A 119.8 . . ? C51 C56 H56A 119.8 . . ? C62 C61 C66 119.0(6) . . ? C62 C61 P2 120.4(5) . . ? C66 C61 P2 120.5(4) . . ? C61 C62 C63 119.7(6) . . ? C61 C62 H62A 120.2 . . ? C63 C62 H62A 120.2 . . ? C64 C63 C62 121.1(6) . . ? C64 C63 H63A 119.5 . . ? C62 C63 H63A 119.5 . . ? C63 C64 C65 119.8(6) . . ? C63 C64 H64A 120.1 . . ? C65 C64 H64A 120.1 . . ? C66 C65 C64 119.3(6) . . ? C66 C65 H65A 120.3 . . ? C64 C65 H65A 120.3 . . ? C65 C66 C61 121.0(6) . . ? C65 C66 H66A 119.5 . . ? C61 C66 H66A 119.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.938 _refine_diff_density_min -1.746 _refine_diff_density_rms 0.301 _database_code_depnum_ccdc_archive 'CCDC 941947'