# Electronic Supplementary Material (ESI) for Catalysis Science & Technology # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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_miguel010411 _database_code_depnum_ccdc_archive 'CCDC 836429' #TrackingRef 'publimiguel010411.cif' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C15 H29 Cl2 N3 Pd' _chemical_formula_sum 'C15 H29 Cl2 N3 Pd' _chemical_formula_weight 428.71 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.1051(8) _cell_length_b 11.1155(9) _cell_length_c 22.6264(6) _cell_angle_alpha 77.784(5) _cell_angle_beta 89.987(4) _cell_angle_gamma 71.894(3) _cell_volume 1888.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 9500 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 32.5 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description parallelepiped _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.263 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.883 _exptl_absorpt_correction_T_max 0.979 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180(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 'Bruker Kappa APEX II' _diffrn_measurement_method \w-\f _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_av_R_equivalents 0.0177 _diffrn_reflns_av_unetI/netI 0.0118 _diffrn_reflns_number 41896 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 7685 _reflns_number_gt 7222 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0153P)^2^+1.1371P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7685 _refine_ls_number_parameters 385 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0182 _refine_ls_R_factor_gt 0.0161 _refine_ls_wR_factor_ref 0.0409 _refine_ls_wR_factor_gt 0.0393 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.323 _refine_diff_density_min -0.461 _refine_diff_density_rms 0.055 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4879(2) 0.22509(17) 0.53680(8) 0.0302(4) Uani 1 1 d . . . C2 C 0.3734(2) 0.21343(19) 0.49456(8) 0.0371(4) Uani 1 1 d . . . H2 H 0.3445 0.2633 0.4542 0.044 Uiso 1 1 calc R . . C3 C 0.3097(2) 0.11634(18) 0.52207(7) 0.0297(4) Uani 1 1 d . . . C4 C 0.5901(3) 0.3173(2) 0.53030(10) 0.0480(5) Uani 1 1 d . . . H4A H 0.567 0.364 0.5632 0.072 Uiso 1 1 calc R . . H4B H 0.5559 0.3796 0.4912 0.072 Uiso 1 1 calc R . . H4C H 0.7145 0.269 0.5322 0.072 Uiso 1 1 calc R . . C5 C 0.1824(3) 0.0616(2) 0.49951(8) 0.0416(5) Uani 1 1 d . . . H5A H 0.2328 -0.033 0.5068 0.062 Uiso 1 1 calc R . . H5B H 0.1546 0.098 0.4559 0.062 Uiso 1 1 calc R . . H5C H 0.0758 0.0839 0.521 0.062 Uiso 1 1 calc R . . C6 C 0.3503(2) -0.01789(15) 0.62997(7) 0.0247(3) Uani 1 1 d . . . H6A H 0.4589 -0.089 0.6464 0.03 Uiso 1 1 calc R . . H6B H 0.2664 -0.0567 0.6165 0.03 Uiso 1 1 calc R . . C7 C 0.2758(2) 0.05315(17) 0.67879(7) 0.0276(3) Uani 1 1 d . . . H7A H 0.1817 0.134 0.6602 0.033 Uiso 1 1 calc R . . H7B H 0.2239 -0.0017 0.7082 0.033 Uiso 1 1 calc R . . C8 C 0.3360(2) 0.21456(16) 0.72876(8) 0.0299(4) Uani 1 1 d . . . H8A H 0.3012 0.2836 0.6912 0.036 Uiso 1 1 calc R . . H8B H 0.429 0.2304 0.7513 0.036 Uiso 1 1 calc R . . C9 C 0.1802(2) 0.22615(18) 0.76720(8) 0.0341(4) Uani 1 1 d . . . H9A H 0.1329 0.3169 0.7718 0.041 Uiso 1 1 calc R . . H9B H 0.0886 0.2073 0.7454 0.041 Uiso 1 1 calc R . . C10 C 0.2202(2) 0.13651(18) 0.82983(8) 0.0315(4) Uani 1 1 d . . . H10A H 0.322 0.1465 0.85 0.038 Uiso 1 1 calc R . . H10B H 0.2507 0.0454 0.8257 0.038 Uiso 1 1 calc R . . C11 C 0.0657(2) 0.1657(2) 0.86920(8) 0.0379(4) Uani 1 1 d . . . H11A H 0.0218 0.2604 0.8668 0.046 Uiso 1 1 calc R . . H11B H -0.0289 0.141 0.8526 0.046 Uiso 1 1 calc R . . C12 C 0.1092(2) 0.0952(2) 0.93545(8) 0.0363(4) Uani 1 1 d . . . H12A H -0.0005 0.1039 0.9559 0.044 Uiso 1 1 calc R . . H12B H 0.1673 0.0016 0.9375 0.044 Uiso 1 1 calc R . . C13 C 0.2262(2) 0.14514(18) 0.96961(8) 0.0348(4) Uani 1 1 d . . . H13A H 0.1695 0.2392 0.9665 0.042 Uiso 1 1 calc R . . H13B H 0.3371 0.1342 0.9497 0.042 Uiso 1 1 calc R . . C14 C 0.2662(3) 0.0774(2) 1.03629(8) 0.0412(4) Uani 1 1 d . . . H14A H 0.1556 0.0874 1.0562 0.049 Uiso 1 1 calc R . . H14B H 0.3247 -0.0166 1.0395 0.049 Uiso 1 1 calc R . . C15 C 0.3808(3) 0.1301(2) 1.06935(10) 0.0504(5) Uani 1 1 d . . . H15A H 0.4933 0.116 1.0513 0.076 Uiso 1 1 calc R . . H15B H 0.3992 0.0851 1.1122 0.076 Uiso 1 1 calc R . . H15C H 0.3243 0.2232 1.066 0.076 Uiso 1 1 calc R . . C21 C -0.1806(2) 0.44961(15) 0.66568(7) 0.0257(3) Uani 1 1 d . . . C22 C -0.0611(2) 0.43066(17) 0.62155(8) 0.0305(4) Uani 1 1 d . . . H22 H -0.0307 0.3604 0.6017 0.037 Uiso 1 1 calc R . . C23 C 0.0045(2) 0.53263(17) 0.61217(7) 0.0272(3) Uani 1 1 d . . . C24 C -0.2808(3) 0.36391(17) 0.69493(9) 0.0357(4) Uani 1 1 d . . . H24A H -0.2955 0.3711 0.7372 0.054 Uiso 1 1 calc R . . H24B H -0.2174 0.2737 0.6938 0.054 Uiso 1 1 calc R . . H24C H -0.3953 0.3905 0.6731 0.054 Uiso 1 1 calc R . . C25 C 0.1372(3) 0.5620(2) 0.57104(9) 0.0414(5) Uani 1 1 d . . . H25A H 0.0842 0.6447 0.542 0.062 Uiso 1 1 calc R . . H25B H 0.1809 0.4926 0.5491 0.062 Uiso 1 1 calc R . . H25C H 0.2339 0.568 0.595 0.062 Uiso 1 1 calc R . . C26 C -0.0446(2) 0.72321(15) 0.66379(7) 0.0234(3) Uani 1 1 d . . . H26A H -0.151 0.7994 0.6526 0.028 Uiso 1 1 calc R . . H26B H 0.0498 0.743 0.6399 0.028 Uiso 1 1 calc R . . C27 C 0.0060(2) 0.69893(16) 0.73075(7) 0.0247(3) Uani 1 1 d . . . H27A H 0.0954 0.6126 0.7435 0.03 Uiso 1 1 calc R . . H27B H 0.0585 0.7648 0.7373 0.03 Uiso 1 1 calc R . . C28 C -0.0847(2) 0.62876(15) 0.83275(7) 0.0243(3) Uani 1 1 d . . . H28A H -0.0263 0.5365 0.8322 0.029 Uiso 1 1 calc R . . H28B H -0.1875 0.6334 0.8569 0.029 Uiso 1 1 calc R . . C29 C 0.0402(2) 0.67869(17) 0.86339(7) 0.0277(3) Uani 1 1 d . . . H29A H -0.0146 0.7726 0.8613 0.033 Uiso 1 1 calc R . . H29B H 0.1474 0.6676 0.8412 0.033 Uiso 1 1 calc R . . C30 C 0.0884(2) 0.60724(17) 0.92957(7) 0.0296(4) Uani 1 1 d . . . H30A H -0.0193 0.6161 0.9513 0.035 Uiso 1 1 calc R . . H30B H 0.1459 0.5137 0.9314 0.035 Uiso 1 1 calc R . . C31 C 0.2091(2) 0.65851(17) 0.96146(7) 0.0301(4) Uani 1 1 d . . . H31A H 0.1519 0.7523 0.9592 0.036 Uiso 1 1 calc R . . H31B H 0.317 0.6489 0.9399 0.036 Uiso 1 1 calc R . . C32 C 0.2567(2) 0.58862(17) 1.02778(7) 0.0302(4) Uani 1 1 d . . . H32A H 0.1484 0.5967 1.0491 0.036 Uiso 1 1 calc R . . H32B H 0.3156 0.4952 1.0299 0.036 Uiso 1 1 calc R . . C33 C 0.3744(2) 0.64011(17) 1.06066(8) 0.0306(4) Uani 1 1 d . . . H33A H 0.4819 0.6335 1.039 0.037 Uiso 1 1 calc R . . H33B H 0.3147 0.7331 1.0593 0.037 Uiso 1 1 calc R . . C34 C 0.4234(2) 0.56801(18) 1.12631(8) 0.0329(4) Uani 1 1 d . . . H34A H 0.3159 0.5745 1.148 0.039 Uiso 1 1 calc R . . H34B H 0.4834 0.475 1.1277 0.039 Uiso 1 1 calc R . . C35 C 0.5406(3) 0.6201(2) 1.15885(9) 0.0434(5) Uani 1 1 d . . . H35A H 0.6463 0.6156 1.1372 0.065 Uiso 1 1 calc R . . H35B H 0.5721 0.5678 1.2003 0.065 Uiso 1 1 calc R . . H35C H 0.479 0.7105 1.1601 0.065 Uiso 1 1 calc R . . N1 N 0.49649(16) 0.13765(12) 0.58840(6) 0.0222(3) Uani 1 1 d . . . N2 N 0.38696(16) 0.07156(13) 0.57866(6) 0.0221(3) Uani 1 1 d . . . N3 N 0.40897(16) 0.08649(13) 0.71164(6) 0.0222(3) Uani 1 1 d . . . H3 H 0.441 0.0243 0.7478 0.027 Uiso 1 1 calc R . . N4 N -0.18945(16) 0.55995(12) 0.68198(6) 0.0209(3) Uani 1 1 d . . . N5 N -0.07641(16) 0.61044(13) 0.64907(6) 0.0218(3) Uani 1 1 d . . . N6 N -0.14400(16) 0.70382(12) 0.76947(6) 0.0202(3) Uani 1 1 d . . . H6 H -0.1874 0.7899 0.7727 0.024 Uiso 1 1 calc R . . Cl1 Cl 0.77557(5) 0.01728(4) 0.764043(19) 0.03082(9) Uani 1 1 d . . . Cl2 Cl 0.89186(5) 0.06650(4) 0.62422(2) 0.03260(9) Uani 1 1 d . . . Cl3 Cl -0.58686(5) 0.64945(4) 0.68163(2) 0.03240(9) Uani 1 1 d . . . Cl4 Cl -0.52741(5) 0.78809(4) 0.791918(19) 0.02947(9) Uani 1 1 d . . . Pd1 Pd 0.634409(14) 0.080700(11) 0.669487(5) 0.01915(3) Uani 1 1 d . . . Pd2 Pd -0.351073(14) 0.667478(10) 0.732255(5) 0.01811(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0264(8) 0.0317(9) 0.0269(8) 0.0026(7) 0.0051(7) -0.0071(7) C2 0.0306(9) 0.0500(11) 0.0213(8) 0.0046(8) 0.0007(7) -0.0081(8) C3 0.0229(8) 0.0448(10) 0.0187(8) -0.0082(7) 0.0007(6) -0.0063(7) C4 0.0472(12) 0.0418(11) 0.0513(13) 0.0111(9) 0.0069(10) -0.0233(10) C5 0.0345(10) 0.0683(14) 0.0262(9) -0.0158(9) -0.0045(7) -0.0188(9) C6 0.0265(8) 0.0257(8) 0.0238(8) -0.0015(6) -0.0039(6) -0.0136(6) C7 0.0243(8) 0.0418(9) 0.0204(8) -0.0037(7) 0.0008(6) -0.0179(7) C8 0.0322(9) 0.0305(9) 0.0267(8) -0.0073(7) 0.0037(7) -0.0091(7) C9 0.0304(9) 0.0388(10) 0.0294(9) -0.0099(8) 0.0041(7) -0.0040(7) C10 0.0297(9) 0.0373(9) 0.0276(9) -0.0099(7) 0.0052(7) -0.0089(7) C11 0.0313(9) 0.0549(12) 0.0307(9) -0.0137(8) 0.0067(7) -0.0153(9) C12 0.0336(10) 0.0469(11) 0.0316(9) -0.0116(8) 0.0116(8) -0.0153(8) C13 0.0385(10) 0.0383(10) 0.0293(9) -0.0112(8) 0.0074(7) -0.0121(8) C14 0.0447(11) 0.0449(11) 0.0300(10) -0.0093(8) 0.0063(8) -0.0081(9) C15 0.0509(13) 0.0567(13) 0.0379(11) -0.0189(10) -0.0037(9) -0.0035(10) C21 0.0242(8) 0.0236(8) 0.0301(8) -0.0087(6) -0.0016(6) -0.0068(6) C22 0.0299(9) 0.0303(9) 0.0325(9) -0.0153(7) 0.0022(7) -0.0057(7) C23 0.0222(8) 0.0343(9) 0.0240(8) -0.0107(7) 0.0025(6) -0.0046(7) C24 0.0405(10) 0.0261(8) 0.0472(11) -0.0129(8) 0.0073(8) -0.0168(8) C25 0.0355(10) 0.0592(13) 0.0372(10) -0.0220(9) 0.0172(8) -0.0186(9) C26 0.0249(8) 0.0268(8) 0.0222(8) -0.0057(6) 0.0036(6) -0.0131(6) C27 0.0209(7) 0.0349(9) 0.0236(8) -0.0087(7) 0.0028(6) -0.0147(7) C28 0.0258(8) 0.0273(8) 0.0205(7) -0.0039(6) -0.0003(6) -0.0104(6) C29 0.0284(8) 0.0330(9) 0.0233(8) -0.0057(7) -0.0022(6) -0.0124(7) C30 0.0318(9) 0.0343(9) 0.0233(8) -0.0056(7) -0.0031(7) -0.0122(7) C31 0.0324(9) 0.0338(9) 0.0245(8) -0.0053(7) -0.0035(7) -0.0119(7) C32 0.0341(9) 0.0329(9) 0.0243(8) -0.0057(7) -0.0038(7) -0.0124(7) C33 0.0354(9) 0.0326(9) 0.0259(8) -0.0056(7) -0.0026(7) -0.0143(7) C34 0.0393(10) 0.0368(9) 0.0248(8) -0.0060(7) -0.0029(7) -0.0161(8) C35 0.0489(12) 0.0577(13) 0.0301(10) -0.0110(9) -0.0051(8) -0.0253(10) N1 0.0204(6) 0.0251(6) 0.0219(6) -0.0039(5) 0.0024(5) -0.0093(5) N2 0.0201(6) 0.0286(7) 0.0189(6) -0.0057(5) 0.0004(5) -0.0093(5) N3 0.0220(6) 0.0287(7) 0.0170(6) -0.0036(5) -0.0002(5) -0.0105(5) N4 0.0191(6) 0.0224(6) 0.0230(6) -0.0057(5) 0.0020(5) -0.0087(5) N5 0.0192(6) 0.0265(7) 0.0215(6) -0.0066(5) 0.0027(5) -0.0091(5) N6 0.0201(6) 0.0226(6) 0.0199(6) -0.0063(5) 0.0013(5) -0.0085(5) Cl1 0.0341(2) 0.0287(2) 0.0296(2) -0.00320(16) -0.01247(16) -0.01209(16) Cl2 0.01976(18) 0.0433(2) 0.0420(2) -0.02007(19) 0.00730(16) -0.01331(17) Cl3 0.01963(18) 0.0356(2) 0.0438(2) -0.00848(18) -0.00420(16) -0.01159(16) Cl4 0.0286(2) 0.02695(19) 0.0328(2) -0.00946(16) 0.01181(16) -0.00685(16) Pd1 0.01732(6) 0.02066(6) 0.02112(6) -0.00524(4) -0.00084(4) -0.00796(4) Pd2 0.01551(6) 0.01919(6) 0.02022(6) -0.00443(4) 0.00184(4) -0.00630(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.338(2) . ? C1 C2 1.385(3) . ? C1 C4 1.491(3) . ? C2 C3 1.372(3) . ? C2 H2 0.95 . ? C3 N2 1.348(2) . ? C3 C5 1.489(2) . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 N2 1.4558(19) . ? C6 C7 1.510(2) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C7 N3 1.4903(19) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 N3 1.496(2) . ? C8 C9 1.521(2) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C9 C10 1.519(2) . ? C9 H9A 0.99 . ? C9 H9B 0.99 . ? C10 C11 1.529(2) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? C11 C12 1.522(3) . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C12 C13 1.521(3) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 C14 1.522(3) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 C15 1.513(3) . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C21 N4 1.335(2) . ? C21 C22 1.393(2) . ? C21 C24 1.489(2) . ? C22 C23 1.373(2) . ? C22 H22 0.95 . ? C23 N5 1.352(2) . ? C23 C25 1.490(2) . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 N5 1.4580(19) . ? C26 C27 1.515(2) . ? C26 H26A 0.99 . ? C26 H26B 0.99 . ? C27 N6 1.4923(19) . ? C27 H27A 0.99 . ? C27 H27B 0.99 . ? C28 N6 1.4910(19) . ? C28 C29 1.525(2) . ? C28 H28A 0.99 . ? C28 H28B 0.99 . ? C29 C30 1.526(2) . ? C29 H29A 0.99 . ? C29 H29B 0.99 . ? C30 C31 1.524(2) . ? C30 H30A 0.99 . ? C30 H30B 0.99 . ? C31 C32 1.525(2) . ? C31 H31A 0.99 . ? C31 H31B 0.99 . ? C32 C33 1.520(2) . ? C32 H32A 0.99 . ? C32 H32B 0.99 . ? C33 C34 1.518(2) . ? C33 H33A 0.99 . ? C33 H33B 0.99 . ? C34 C35 1.517(2) . ? C34 H34A 0.99 . ? C34 H34B 0.99 . ? C35 H35A 0.98 . ? C35 H35B 0.98 . ? C35 H35C 0.98 . ? N1 N2 1.3603(18) . ? N1 Pd1 2.0214(13) . ? N3 Pd1 2.0505(13) . ? N3 H3 0.93 . ? N4 N5 1.3607(17) . ? N4 Pd2 2.0100(13) . ? N6 Pd2 2.0628(12) . ? N6 H6 0.93 . ? Cl1 Pd1 2.2901(4) . ? Cl2 Pd1 2.3002(4) . ? Cl3 Pd2 2.3109(4) . ? Cl4 Pd2 2.2884(4) . ? 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 N1 C1 C2 109.30(15) . . ? N1 C1 C4 121.93(16) . . ? C2 C1 C4 128.78(17) . . ? C3 C2 C1 107.06(15) . . ? C3 C2 H2 126.5 . . ? C1 C2 H2 126.5 . . ? N2 C3 C2 106.42(15) . . ? N2 C3 C5 122.14(16) . . ? C2 C3 C5 131.44(16) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 C7 110.01(13) . . ? N2 C6 H6A 109.7 . . ? C7 C6 H6A 109.7 . . ? N2 C6 H6B 109.7 . . ? C7 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? N3 C7 C6 112.65(13) . . ? N3 C7 H7A 109.1 . . ? C6 C7 H7A 109.1 . . ? N3 C7 H7B 109.1 . . ? C6 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? N3 C8 C9 114.89(14) . . ? N3 C8 H8A 108.5 . . ? C9 C8 H8A 108.5 . . ? N3 C8 H8B 108.5 . . ? C9 C8 H8B 108.5 . . ? H8A C8 H8B 107.5 . . ? C10 C9 C8 114.37(15) . . ? C10 C9 H9A 108.7 . . ? C8 C9 H9A 108.7 . . ? C10 C9 H9B 108.7 . . ? C8 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? C9 C10 C11 111.80(15) . . ? C9 C10 H10A 109.3 . . ? C11 C10 H10A 109.3 . . ? C9 C10 H10B 109.3 . . ? C11 C10 H10B 109.3 . . ? H10A C10 H10B 107.9 . . ? C12 C11 C10 113.68(16) . . ? C12 C11 H11A 108.8 . . ? C10 C11 H11A 108.8 . . ? C12 C11 H11B 108.8 . . ? C10 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? C13 C12 C11 113.83(16) . . ? C13 C12 H12A 108.8 . . ? C11 C12 H12A 108.8 . . ? C13 C12 H12B 108.8 . . ? C11 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? C12 C13 C14 114.08(16) . . ? C12 C13 H13A 108.7 . . ? C14 C13 H13A 108.7 . . ? C12 C13 H13B 108.7 . . ? C14 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? C15 C14 C13 112.98(18) . . ? C15 C14 H14A 109 . . ? C13 C14 H14A 109 . . ? C15 C14 H14B 109 . . ? C13 C14 H14B 109 . . ? H14A C14 H14B 107.8 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N4 C21 C22 108.75(14) . . ? N4 C21 C24 122.11(15) . . ? C22 C21 C24 129.07(15) . . ? C23 C22 C21 107.15(14) . . ? C23 C22 H22 126.4 . . ? C21 C22 H22 126.4 . . ? N5 C23 C22 106.53(14) . . ? N5 C23 C25 122.75(16) . . ? C22 C23 C25 130.71(16) . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N5 C26 C27 111.05(13) . . ? N5 C26 H26A 109.4 . . ? C27 C26 H26A 109.4 . . ? N5 C26 H26B 109.4 . . ? C27 C26 H26B 109.4 . . ? H26A C26 H26B 108 . . ? N6 C27 C26 113.17(12) . . ? N6 C27 H27A 108.9 . . ? C26 C27 H27A 108.9 . . ? N6 C27 H27B 108.9 . . ? C26 C27 H27B 108.9 . . ? H27A C27 H27B 107.8 . . ? N6 C28 C29 112.86(13) . . ? N6 C28 H28A 109 . . ? C29 C28 H28A 109 . . ? N6 C28 H28B 109 . . ? C29 C28 H28B 109 . . ? H28A C28 H28B 107.8 . . ? C28 C29 C30 111.94(13) . . ? C28 C29 H29A 109.2 . . ? C30 C29 H29A 109.2 . . ? C28 C29 H29B 109.2 . . ? C30 C29 H29B 109.2 . . ? H29A C29 H29B 107.9 . . ? C31 C30 C29 112.68(14) . . ? C31 C30 H30A 109.1 . . ? C29 C30 H30A 109.1 . . ? C31 C30 H30B 109.1 . . ? C29 C30 H30B 109.1 . . ? H30A C30 H30B 107.8 . . ? C30 C31 C32 113.12(14) . . ? C30 C31 H31A 109 . . ? C32 C31 H31A 109 . . ? C30 C31 H31B 109 . . ? C32 C31 H31B 109 . . ? H31A C31 H31B 107.8 . . ? C33 C32 C31 113.88(14) . . ? C33 C32 H32A 108.8 . . ? C31 C32 H32A 108.8 . . ? C33 C32 H32B 108.8 . . ? C31 C32 H32B 108.8 . . ? H32A C32 H32B 107.7 . . ? C34 C33 C32 113.30(14) . . ? C34 C33 H33A 108.9 . . ? C32 C33 H33A 108.9 . . ? C34 C33 H33B 108.9 . . ? C32 C33 H33B 108.9 . . ? H33A C33 H33B 107.7 . . ? C35 C34 C33 112.99(15) . . ? C35 C34 H34A 109 . . ? C33 C34 H34A 109 . . ? C35 C34 H34B 109 . . ? C33 C34 H34B 109 . . ? H34A C34 H34B 107.8 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C1 N1 N2 106.30(13) . . ? C1 N1 Pd1 136.14(11) . . ? N2 N1 Pd1 117.47(9) . . ? C3 N2 N1 110.92(13) . . ? C3 N2 C6 129.82(13) . . ? N1 N2 C6 118.52(12) . . ? C7 N3 C8 112.16(13) . . ? C7 N3 Pd1 116.10(9) . . ? C8 N3 Pd1 109.31(10) . . ? C7 N3 H3 106.2 . . ? C8 N3 H3 106.2 . . ? Pd1 N3 H3 106.2 . . ? C21 N4 N5 107.14(13) . . ? C21 N4 Pd2 133.35(11) . . ? N5 N4 Pd2 118.79(9) . . ? C23 N5 N4 110.42(13) . . ? C23 N5 C26 130.87(13) . . ? N4 N5 C26 118.13(12) . . ? C28 N6 C27 111.32(12) . . ? C28 N6 Pd2 114.50(9) . . ? C27 N6 Pd2 115.40(9) . . ? C28 N6 H6 104.8 . . ? C27 N6 H6 104.8 . . ? Pd2 N6 H6 104.8 . . ? N1 Pd1 N3 89.24(5) . . ? N1 Pd1 Cl1 176.62(4) . . ? N3 Pd1 Cl1 87.39(4) . . ? N1 Pd1 Cl2 92.03(4) . . ? N3 Pd1 Cl2 177.89(4) . . ? Cl1 Pd1 Cl2 91.349(17) . . ? N4 Pd2 N6 90.16(5) . . ? N4 Pd2 Cl4 178.05(4) . . ? N6 Pd2 Cl4 88.13(4) . . ? N4 Pd2 Cl3 89.93(4) . . ? N6 Pd2 Cl3 173.03(4) . . ? Cl4 Pd2 Cl3 91.879(17) . . ? data_miguel070411 _database_code_depnum_ccdc_archive 'CCDC 836430' #TrackingRef 'publimiguel070411.cif' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C15 H28 Cl2 N2 Pd S' _chemical_formula_sum 'C15 H28 Cl2 N2 Pd S' _chemical_formula_weight 445.75 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.1752(8) _cell_length_b 15.2655(6) _cell_length_c 15.4570(10) _cell_angle_alpha 94.321(7) _cell_angle_beta 90.451(5) _cell_angle_gamma 93.185(4) _cell_volume 1920.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 9881 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 33.12 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description parallelepiped _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.349 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.883 _exptl_absorpt_correction_T_max 0.979 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180(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 'Bruker Kappa APEX II' _diffrn_measurement_method \w-\f _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_unetI/netI 0.0177 _diffrn_reflns_number 30197 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 7799 _reflns_number_gt 7010 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0234P)^2^+1.7857P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7799 _refine_ls_number_parameters 385 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0272 _refine_ls_R_factor_gt 0.0225 _refine_ls_wR_factor_ref 0.0585 _refine_ls_wR_factor_gt 0.0548 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.776 _refine_diff_density_min -0.581 _refine_diff_density_rms 0.064 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.1154(3) 0.31383(14) -1.21712(13) 0.0267(4) Uani 1 1 d . . . C2 C -0.0571(3) 0.34892(15) -1.29270(14) 0.0299(5) Uani 1 1 d . . . H2 H -0.0933 0.332 -1.3504 0.036 Uiso 1 1 calc R . . C3 C 0.0627(3) 0.41259(15) -1.26743(13) 0.0271(4) Uani 1 1 d . . . C4 C -0.2428(3) 0.24118(16) -1.20907(15) 0.0363(5) Uani 1 1 d . . . H4A H -0.2714 0.2379 -1.1479 0.054 Uiso 1 1 calc R . . H4B H -0.2001 0.1853 -1.2315 0.054 Uiso 1 1 calc R . . H4C H -0.3406 0.2526 -1.2426 0.054 Uiso 1 1 calc R . . C5 C 0.1675(3) 0.47215(17) -1.31863(15) 0.0366(5) Uani 1 1 d . . . H5A H 0.1576 0.5332 -1.2957 0.055 Uiso 1 1 calc R . . H5B H 0.1317 0.4656 -1.3796 0.055 Uiso 1 1 calc R . . H5C H 0.2819 0.4568 -1.3143 0.055 Uiso 1 1 calc R . . C6 C 0.1854(3) 0.46709(14) -1.12117(14) 0.0271(4) Uani 1 1 d . . . H6A H 0.1238 0.4923 -1.0712 0.033 Uiso 1 1 calc R . . H6B H 0.2361 0.5165 -1.1514 0.033 Uiso 1 1 calc R . . C7 C 0.3191(3) 0.41263(15) -1.08820(15) 0.0307(5) Uani 1 1 d . . . H7A H 0.4025 0.4524 -1.0563 0.037 Uiso 1 1 calc R . . H7B H 0.3734 0.3829 -1.1384 0.037 Uiso 1 1 calc R . . C8 C 0.3009(3) 0.22753(16) -1.07375(16) 0.0352(5) Uani 1 1 d . . . H8A H 0.4217 0.2299 -1.0782 0.042 Uiso 1 1 calc R . . H8B H 0.2691 0.179 -1.0372 0.042 Uiso 1 1 calc R . . C9 C 0.2300(3) 0.20426(16) -1.16311(16) 0.0378(5) Uani 1 1 d . . . H9A H 0.2538 0.2539 -1.1996 0.045 Uiso 1 1 calc R . . H9B H 0.1095 0.1952 -1.1592 0.045 Uiso 1 1 calc R . . C10 C 0.2994(3) 0.12118(17) -1.20626(18) 0.0410(6) Uani 1 1 d . . . H10A H 0.4202 0.1295 -1.2082 0.049 Uiso 1 1 calc R . . H10B H 0.2723 0.0712 -1.1707 0.049 Uiso 1 1 calc R . . C11 C 0.2334(4) 0.09887(17) -1.29736(18) 0.0441(6) Uani 1 1 d . . . H11A H 0.2614 0.1489 -1.3327 0.053 Uiso 1 1 calc R . . H11B H 0.1124 0.0916 -1.2952 0.053 Uiso 1 1 calc R . . C12 C 0.2984(4) 0.01604(18) -1.34197(18) 0.0475(7) Uani 1 1 d . . . H12A H 0.4196 0.0222 -1.3417 0.057 Uiso 1 1 calc R . . H12B H 0.2659 -0.0345 -1.3081 0.057 Uiso 1 1 calc R . . C13 C 0.2385(4) -0.00389(19) -1.43409(18) 0.0499(7) Uani 1 1 d . . . H13A H 0.2731 0.0462 -1.4681 0.06 Uiso 1 1 calc R . . H13B H 0.1172 -0.0084 -1.4343 0.06 Uiso 1 1 calc R . . C14 C 0.2987(5) -0.0872(2) -1.47899(19) 0.0596(8) Uani 1 1 d . . . H14A H 0.42 -0.0829 -1.4782 0.071 Uiso 1 1 calc R . . H14B H 0.2632 -0.1374 -1.4452 0.071 Uiso 1 1 calc R . . C15 C 0.2403(5) -0.1068(2) -1.5712(2) 0.0730(11) Uani 1 1 d . . . H15A H 0.1204 -0.1137 -1.5727 0.11 Uiso 1 1 calc R . . H15B H 0.2859 -0.1614 -1.5953 0.11 Uiso 1 1 calc R . . H15C H 0.2766 -0.0582 -1.6057 0.11 Uiso 1 1 calc R . . C21 C 0.5737(3) 0.31774(14) -0.72050(13) 0.0259(4) Uani 1 1 d . . . C22 C 0.5221(3) 0.35537(15) -0.79439(14) 0.0300(5) Uani 1 1 d . . . H22 H 0.5524 0.3394 -0.8524 0.036 Uiso 1 1 calc R . . C23 C 0.4187(3) 0.42026(14) -0.76774(13) 0.0265(4) Uani 1 1 d . . . C24 C 0.6811(3) 0.24283(16) -0.71428(15) 0.0358(5) Uani 1 1 d . . . H24A H 0.7012 0.2338 -0.6531 0.054 Uiso 1 1 calc R . . H24B H 0.7856 0.256 -0.7425 0.054 Uiso 1 1 calc R . . H24C H 0.6273 0.1894 -0.7432 0.054 Uiso 1 1 calc R . . C25 C 0.3264(3) 0.48179(16) -0.81717(15) 0.0346(5) Uani 1 1 d . . . H25A H 0.2085 0.4678 -0.8122 0.052 Uiso 1 1 calc R . . H25B H 0.3573 0.4758 -0.8784 0.052 Uiso 1 1 calc R . . H25C H 0.3524 0.5424 -0.7935 0.052 Uiso 1 1 calc R . . C26 C 0.3102(3) 0.47064(14) -0.62062(14) 0.0274(5) Uani 1 1 d . . . H26A H 0.2692 0.521 -0.6495 0.033 Uiso 1 1 calc R . . H26B H 0.3768 0.4944 -0.5695 0.033 Uiso 1 1 calc R . . C27 C 0.1659(3) 0.41409(16) -0.59083(16) 0.0350(5) Uani 1 1 d . . . H27A H 0.1064 0.3857 -0.6425 0.042 Uiso 1 1 calc R . . H27B H 0.0897 0.4525 -0.5587 0.042 Uiso 1 1 calc R . . C28 C 0.1444(3) 0.22746(18) -0.57934(18) 0.0432(6) Uani 1 1 d . . . H28A H 0.1556 0.1793 -0.5406 0.052 Uiso 1 1 calc R . . H28B H 0.0259 0.2322 -0.5904 0.052 Uiso 1 1 calc R . . C29 C 0.2237(3) 0.20224(19) -0.6634(2) 0.0501(7) Uani 1 1 d . . . H29A H 0.3401 0.1917 -0.6524 0.06 Uiso 1 1 calc R . . H29B H 0.2203 0.2517 -0.7012 0.06 Uiso 1 1 calc R . . C30 C 0.1402(4) 0.11948(19) -0.7110(2) 0.0530(7) Uani 1 1 d . . . H30A H 0.136 0.0708 -0.672 0.064 Uiso 1 1 calc R . . H30B H 0.0264 0.1313 -0.7267 0.064 Uiso 1 1 calc R . . C31 C 0.2318(4) 0.0926(2) -0.7915(2) 0.0663(9) Uani 1 1 d . . . H31A H 0.3447 0.0802 -0.7745 0.08 Uiso 1 1 calc R . . H31B H 0.2397 0.1429 -0.8284 0.08 Uiso 1 1 calc R . . C32 C 0.1578(4) 0.0139(2) -0.8445(2) 0.0609(8) Uani 1 1 d . . . H32A H 0.0462 0.0268 -0.8632 0.073 Uiso 1 1 calc R . . H32B H 0.1471 -0.0362 -0.8074 0.073 Uiso 1 1 calc R . . C33 C 0.2548(5) -0.0135(2) -0.9239(2) 0.0672(9) Uani 1 1 d . . . H33A H 0.2709 0.0381 -0.9587 0.081 Uiso 1 1 calc R . . H33B H 0.3644 -0.029 -0.9044 0.081 Uiso 1 1 calc R . . C34 C 0.1828(6) -0.0885(2) -0.9818(2) 0.0781(12) Uani 1 1 d . . . H34A H 0.0744 -0.0729 -1.003 0.094 Uiso 1 1 calc R . . H34B H 0.1651 -0.1403 -0.9474 0.094 Uiso 1 1 calc R . . C35 C 0.2883(6) -0.1140(2) -1.0599(2) 0.0844(13) Uani 1 1 d . . . H35A H 0.3087 -0.0629 -1.0938 0.127 Uiso 1 1 calc R . . H35B H 0.231 -0.1617 -1.0963 0.127 Uiso 1 1 calc R . . H35C H 0.393 -0.1339 -1.0397 0.127 Uiso 1 1 calc R . . N1 N -0.0350(2) 0.35477(11) -1.14874(11) 0.0229(4) Uani 1 1 d . . . N2 N 0.0727(2) 0.41522(12) -1.18019(11) 0.0241(4) Uani 1 1 d . . . N3 N 0.5061(2) 0.35793(11) -0.65077(11) 0.0225(3) Uani 1 1 d . . . N4 N 0.4123(2) 0.42058(11) -0.68045(11) 0.0230(4) Uani 1 1 d . . . S1 S 0.24334(6) 0.33006(4) -1.01720(3) 0.02758(12) Uani 1 1 d . . . S2 S 0.22393(6) 0.32959(4) -0.52211(4) 0.02803(12) Uani 1 1 d . . . Cl1 Cl -0.02249(7) 0.31703(4) -0.87443(4) 0.03890(14) Uani 1 1 d . . . Cl2 Cl -0.31386(6) 0.35486(4) -1.01435(3) 0.02914(11) Uani 1 1 d . . . Cl3 Cl 0.49037(7) 0.30931(4) -0.37966(4) 0.03672(13) Uani 1 1 d . . . Cl4 Cl 0.78675(6) 0.35285(4) -0.51692(3) 0.02956(12) Uani 1 1 d . . . Pd1 Pd -0.034519(19) 0.336394(10) -1.019993(9) 0.02244(5) Uani 1 1 d . . . Pd2 Pd 0.503426(19) 0.335051(10) -0.523508(9) 0.02154(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0248(11) 0.0323(11) 0.0227(10) -0.0037(8) -0.0052(8) 0.0067(9) C2 0.0314(12) 0.0394(13) 0.0184(10) -0.0039(9) -0.0038(9) 0.0070(9) C3 0.0279(11) 0.0354(12) 0.0187(10) 0.0005(8) -0.0003(8) 0.0094(9) C4 0.0389(14) 0.0384(13) 0.0300(12) -0.0031(10) -0.0099(10) -0.0035(10) C5 0.0375(13) 0.0469(14) 0.0266(12) 0.0080(10) 0.0040(10) 0.0058(11) C6 0.0280(11) 0.0290(11) 0.0235(10) -0.0015(8) -0.0027(9) -0.0005(9) C7 0.0242(11) 0.0358(12) 0.0312(12) 0.0011(9) -0.0041(9) -0.0033(9) C8 0.0305(12) 0.0324(12) 0.0430(14) 0.0025(10) -0.0020(10) 0.0064(9) C9 0.0358(13) 0.0351(13) 0.0422(14) -0.0020(10) -0.0017(11) 0.0068(10) C10 0.0375(14) 0.0341(13) 0.0510(16) -0.0044(11) 0.0000(12) 0.0077(10) C11 0.0493(16) 0.0333(13) 0.0488(16) -0.0051(11) 0.0032(12) 0.0057(11) C12 0.0548(17) 0.0373(14) 0.0498(16) -0.0057(12) 0.0013(13) 0.0093(12) C13 0.0587(18) 0.0433(16) 0.0482(16) -0.0006(12) 0.0076(14) 0.0124(13) C14 0.086(2) 0.0453(17) 0.0480(17) -0.0063(13) -0.0019(16) 0.0218(16) C15 0.106(3) 0.068(2) 0.0466(18) -0.0104(16) -0.0019(18) 0.035(2) C21 0.0249(11) 0.0320(11) 0.0203(10) -0.0014(8) 0.0051(8) 0.0016(8) C22 0.0331(12) 0.0377(12) 0.0186(10) -0.0011(9) 0.0046(9) 0.0022(9) C23 0.0265(11) 0.0326(11) 0.0198(10) 0.0018(8) 0.0001(8) -0.0032(9) C24 0.0417(14) 0.0398(13) 0.0270(12) -0.0004(10) 0.0092(10) 0.0138(11) C25 0.0358(13) 0.0431(14) 0.0260(11) 0.0086(10) -0.0016(10) 0.0031(10) C26 0.0298(11) 0.0293(11) 0.0235(10) -0.0008(8) 0.0027(9) 0.0079(9) C27 0.0266(12) 0.0447(14) 0.0356(13) 0.0087(10) 0.0061(10) 0.0116(10) C28 0.0322(13) 0.0418(14) 0.0546(17) 0.0004(12) 0.0002(12) -0.0016(11) C29 0.0407(15) 0.0467(16) 0.0601(18) -0.0096(13) 0.0030(13) -0.0046(12) C30 0.0481(17) 0.0425(16) 0.0654(19) -0.0101(13) -0.0102(14) -0.0031(12) C31 0.057(2) 0.0478(18) 0.089(3) -0.0234(17) 0.0025(18) -0.0059(14) C32 0.081(2) 0.0432(17) 0.0568(19) -0.0025(14) -0.0159(17) -0.0038(15) C33 0.078(2) 0.0477(18) 0.074(2) -0.0063(16) -0.0048(19) 0.0039(16) C34 0.133(4) 0.051(2) 0.0484(19) 0.0009(15) -0.012(2) -0.007(2) C35 0.138(4) 0.053(2) 0.060(2) -0.0024(17) 0.006(2) -0.005(2) N1 0.0198(8) 0.0280(9) 0.0205(8) -0.0007(7) -0.0015(7) 0.0017(7) N2 0.0220(9) 0.0303(9) 0.0199(8) 0.0003(7) -0.0010(7) 0.0024(7) N3 0.0197(8) 0.0275(9) 0.0203(8) 0.0008(7) 0.0021(7) 0.0028(7) N4 0.0214(9) 0.0280(9) 0.0196(8) 0.0007(7) 0.0001(7) 0.0032(7) S1 0.0231(3) 0.0366(3) 0.0230(3) 0.0012(2) -0.0040(2) 0.0031(2) S2 0.0212(3) 0.0356(3) 0.0272(3) 0.0016(2) 0.0035(2) 0.0021(2) Cl1 0.0360(3) 0.0591(4) 0.0226(3) 0.0124(2) -0.0026(2) -0.0002(3) Cl2 0.0219(2) 0.0422(3) 0.0229(2) -0.0002(2) -0.00058(19) 0.0024(2) Cl3 0.0347(3) 0.0551(4) 0.0222(3) 0.0119(2) 0.0033(2) 0.0068(3) Cl4 0.0205(2) 0.0441(3) 0.0239(3) -0.0002(2) 0.00046(19) 0.0039(2) Pd1 0.02108(9) 0.02923(9) 0.01685(8) 0.00082(6) -0.00249(6) 0.00155(6) Pd2 0.01986(8) 0.02820(9) 0.01664(8) 0.00095(6) 0.00160(6) 0.00280(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.336(3) . ? C1 C2 1.398(3) . ? C1 C4 1.491(3) . ? C2 C3 1.374(3) . ? C2 H2 0.95 . ? C3 N2 1.348(3) . ? C3 C5 1.490(3) . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 N2 1.451(3) . ? C6 C7 1.517(3) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C7 S1 1.819(2) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 C9 1.503(3) . ? C8 S1 1.821(2) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C9 C10 1.528(3) . ? C9 H9A 0.99 . ? C9 H9B 0.99 . ? C10 C11 1.512(4) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? C11 C12 1.518(3) . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C12 C13 1.506(4) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 C14 1.512(4) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 C15 1.502(4) . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C21 N3 1.338(3) . ? C21 C22 1.390(3) . ? C21 C24 1.488(3) . ? C22 C23 1.380(3) . ? C22 H22 0.95 . ? C23 N4 1.350(3) . ? C23 C25 1.488(3) . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 N4 1.453(3) . ? C26 C27 1.518(3) . ? C26 H26A 0.99 . ? C26 H26B 0.99 . ? C27 S2 1.812(2) . ? C27 H27A 0.99 . ? C27 H27B 0.99 . ? C28 C29 1.491(4) . ? C28 S2 1.818(3) . ? C28 H28A 0.99 . ? C28 H28B 0.99 . ? C29 C30 1.536(4) . ? C29 H29A 0.99 . ? C29 H29B 0.99 . ? C30 C31 1.499(4) . ? C30 H30A 0.99 . ? C30 H30B 0.99 . ? C31 C32 1.499(4) . ? C31 H31A 0.99 . ? C31 H31B 0.99 . ? C32 C33 1.511(5) . ? C32 H32A 0.99 . ? C32 H32B 0.99 . ? C33 C34 1.490(5) . ? C33 H33A 0.99 . ? C33 H33B 0.99 . ? C34 C35 1.529(5) . ? C34 H34A 0.99 . ? C34 H34B 0.99 . ? C35 H35A 0.98 . ? C35 H35B 0.98 . ? C35 H35C 0.98 . ? N1 N2 1.359(2) . ? N1 Pd1 2.0305(17) . ? N3 N4 1.362(2) . ? N3 Pd2 2.0236(17) . ? S1 Pd1 2.2792(6) . ? S2 Pd2 2.2822(6) . ? Cl1 Pd1 2.2934(6) . ? Cl2 Pd1 2.3180(6) . ? Cl3 Pd2 2.2892(6) . ? Cl4 Pd2 2.3176(6) . ? 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 N1 C1 C2 109.0(2) . . ? N1 C1 C4 122.8(2) . . ? C2 C1 C4 128.2(2) . . ? C3 C2 C1 106.76(19) . . ? C3 C2 H2 126.6 . . ? C1 C2 H2 126.6 . . ? N2 C3 C2 106.59(19) . . ? N2 C3 C5 122.1(2) . . ? C2 C3 C5 131.4(2) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 C7 111.96(18) . . ? N2 C6 H6A 109.2 . . ? C7 C6 H6A 109.2 . . ? N2 C6 H6B 109.2 . . ? C7 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C6 C7 S1 113.22(15) . . ? C6 C7 H7A 108.9 . . ? S1 C7 H7A 108.9 . . ? C6 C7 H7B 108.9 . . ? S1 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? C9 C8 S1 117.50(16) . . ? C9 C8 H8A 107.9 . . ? S1 C8 H8A 107.9 . . ? C9 C8 H8B 107.9 . . ? S1 C8 H8B 107.9 . . ? H8A C8 H8B 107.2 . . ? C8 C9 C10 112.2(2) . . ? C8 C9 H9A 109.2 . . ? C10 C9 H9A 109.2 . . ? C8 C9 H9B 109.2 . . ? C10 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C11 C10 C9 112.6(2) . . ? C11 C10 H10A 109.1 . . ? C9 C10 H10A 109.1 . . ? C11 C10 H10B 109.1 . . ? C9 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? C10 C11 C12 114.1(2) . . ? C10 C11 H11A 108.7 . . ? C12 C11 H11A 108.7 . . ? C10 C11 H11B 108.7 . . ? C12 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? C13 C12 C11 114.1(2) . . ? C13 C12 H12A 108.7 . . ? C11 C12 H12A 108.7 . . ? C13 C12 H12B 108.7 . . ? C11 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? C12 C13 C14 114.9(2) . . ? C12 C13 H13A 108.5 . . ? C14 C13 H13A 108.5 . . ? C12 C13 H13B 108.5 . . ? C14 C13 H13B 108.5 . . ? H13A C13 H13B 107.5 . . ? C15 C14 C13 115.0(3) . . ? C15 C14 H14A 108.5 . . ? C13 C14 H14A 108.5 . . ? C15 C14 H14B 108.5 . . ? C13 C14 H14B 108.5 . . ? H14A C14 H14B 107.5 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C21 C22 109.10(19) . . ? N3 C21 C24 122.40(19) . . ? C22 C21 C24 128.47(19) . . ? C23 C22 C21 107.20(18) . . ? C23 C22 H22 126.4 . . ? C21 C22 H22 126.4 . . ? N4 C23 C22 106.08(19) . . ? N4 C23 C25 122.23(19) . . ? C22 C23 C25 131.7(2) . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N4 C26 C27 111.44(18) . . ? N4 C26 H26A 109.3 . . ? C27 C26 H26A 109.3 . . ? N4 C26 H26B 109.3 . . ? C27 C26 H26B 109.3 . . ? H26A C26 H26B 108 . . ? C26 C27 S2 113.63(16) . . ? C26 C27 H27A 108.8 . . ? S2 C27 H27A 108.8 . . ? C26 C27 H27B 108.8 . . ? S2 C27 H27B 108.8 . . ? H27A C27 H27B 107.7 . . ? C29 C28 S2 116.04(19) . . ? C29 C28 H28A 108.3 . . ? S2 C28 H28A 108.3 . . ? C29 C28 H28B 108.3 . . ? S2 C28 H28B 108.3 . . ? H28A C28 H28B 107.4 . . ? C28 C29 C30 112.7(2) . . ? C28 C29 H29A 109.1 . . ? C30 C29 H29A 109.1 . . ? C28 C29 H29B 109.1 . . ? C30 C29 H29B 109.1 . . ? H29A C29 H29B 107.8 . . ? C31 C30 C29 110.7(3) . . ? C31 C30 H30A 109.5 . . ? C29 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 108.1 . . ? C30 C31 C32 115.2(3) . . ? C30 C31 H31A 108.5 . . ? C32 C31 H31A 108.5 . . ? C30 C31 H31B 108.5 . . ? C32 C31 H31B 108.5 . . ? H31A C31 H31B 107.5 . . ? C31 C32 C33 114.2(3) . . ? C31 C32 H32A 108.7 . . ? C33 C32 H32A 108.7 . . ? C31 C32 H32B 108.7 . . ? C33 C32 H32B 108.7 . . ? H32A C32 H32B 107.6 . . ? C34 C33 C32 116.7(3) . . ? C34 C33 H33A 108.1 . . ? C32 C33 H33A 108.1 . . ? C34 C33 H33B 108.1 . . ? C32 C33 H33B 108.1 . . ? H33A C33 H33B 107.3 . . ? C33 C34 C35 114.1(4) . . ? C33 C34 H34A 108.7 . . ? C35 C34 H34A 108.7 . . ? C33 C34 H34B 108.7 . . ? C35 C34 H34B 108.7 . . ? H34A C34 H34B 107.6 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C1 N1 N2 106.71(17) . . ? C1 N1 Pd1 133.28(15) . . ? N2 N1 Pd1 119.80(12) . . ? C3 N2 N1 110.92(17) . . ? C3 N2 C6 129.29(19) . . ? N1 N2 C6 119.64(16) . . ? C21 N3 N4 106.57(16) . . ? C21 N3 Pd2 133.20(15) . . ? N4 N3 Pd2 119.94(12) . . ? C23 N4 N3 111.05(16) . . ? C23 N4 C26 128.75(18) . . ? N3 N4 C26 119.87(16) . . ? C7 S1 C8 102.90(11) . . ? C7 S1 Pd1 105.24(7) . . ? C8 S1 Pd1 109.65(8) . . ? C27 S2 C28 104.14(13) . . ? C27 S2 Pd2 105.25(8) . . ? C28 S2 Pd2 109.37(9) . . ? N1 Pd1 S1 91.71(5) . . ? N1 Pd1 Cl1 177.63(5) . . ? S1 Pd1 Cl1 86.01(2) . . ? N1 Pd1 Cl2 90.54(5) . . ? S1 Pd1 Cl2 174.62(2) . . ? Cl1 Pd1 Cl2 91.68(2) . . ? N3 Pd2 S2 91.55(5) . . ? N3 Pd2 Cl3 177.94(5) . . ? S2 Pd2 Cl3 86.39(2) . . ? N3 Pd2 Cl4 90.33(5) . . ? S2 Pd2 Cl4 174.64(2) . . ? Cl3 Pd2 Cl4 91.71(2) . . ? data_miguel100511 _database_code_depnum_ccdc_archive 'CCDC 836431' #TrackingRef 'publimiguel100511.cif' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C30 H56 Cl2 N4 O2 Pd' _chemical_formula_sum 'C30 H56 Cl2 N4 O2 Pd' _chemical_formula_weight 682.09 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 1' _symmetry_space_group_name_Hall 'P 1' _symmetry_Int_Tables_number 1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 8.1693(8) _cell_length_b 9.1162(10) _cell_length_c 22.9935(7) _cell_angle_alpha 93.592(3) _cell_angle_beta 91.806(5) _cell_angle_gamma 89.939(6) _cell_volume 1708.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 6109 _cell_measurement_theta_min 3.3443 _cell_measurement_theta_max 29.1639 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description platelet _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.326 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.731 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.9286 _exptl_absorpt_correction_T_max 0.9987 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1978 _diffrn_orient_matrix_ub_11 -0.0227471 _diffrn_orient_matrix_ub_12 -0.0233469 _diffrn_orient_matrix_ub_13 -0.0291444 _diffrn_orient_matrix_ub_21 -0.0473555 _diffrn_orient_matrix_ub_22 -0.057626 _diffrn_orient_matrix_ub_23 0.0102714 _diffrn_orient_matrix_ub_31 -0.0691875 _diffrn_orient_matrix_ub_32 0.0470283 _diffrn_orient_matrix_ub_33 0.0013259 _diffrn_reflns_av_R_equivalents 0.0838 _diffrn_reflns_av_unetI/netI 0.1495 _diffrn_reflns_number 19788 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.35 _diffrn_reflns_theta_max 25.35 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 11748 _reflns_number_gt 8928 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0755P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 11748 _refine_ls_number_parameters 686 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1022 _refine_ls_R_factor_gt 0.0759 _refine_ls_wR_factor_ref 0.182 _refine_ls_wR_factor_gt 0.1632 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(5) _refine_diff_density_max 3.986 _refine_diff_density_min -1.075 _refine_diff_density_rms 0.144 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.7013(14) -0.9006(12) 1.5530(6) 0.036(3) Uani 1 1 d . . . H1A H 1.6255 -0.8513 1.58 0.054 Uiso 1 1 calc R . . H1B H 1.7353 -0.9947 1.5678 0.054 Uiso 1 1 calc R . . H1C H 1.6465 -0.9181 1.5146 0.054 Uiso 1 1 calc R . . C2 C 1.8451(11) -0.8078(11) 1.5477(4) 0.018(2) Uani 1 1 d . . . C3 C 2.0082(12) -0.8325(12) 1.5613(5) 0.021(2) Uani 1 1 d . . . H3 H 2.0552 -0.9196 1.5751 0.025 Uiso 1 1 calc R . . C4 C 2.0892(15) -0.7040(12) 1.5506(5) 0.022(3) Uani 1 1 d . . . C5 C 2.2679(12) -0.6781(13) 1.5555(5) 0.023(3) Uani 1 1 d . . . H5A H 2.3123 -0.6768 1.5165 0.034 Uiso 1 1 calc R . . H5B H 2.3203 -0.7569 1.5764 0.034 Uiso 1 1 calc R . . H5C H 2.2897 -0.5834 1.5769 0.034 Uiso 1 1 calc R . . C6 C 2.0514(19) 0.1147(15) 1.3987(7) 0.046(4) Uani 1 1 d . . . H6A H 2.1328 0.1913 1.3935 0.069 Uiso 1 1 calc R . . H6B H 1.9579 0.1579 1.4193 0.069 Uiso 1 1 calc R . . H6C H 2.014 0.0716 1.3605 0.069 Uiso 1 1 calc R . . C7 C 2.1261(14) -0.0011(11) 1.4333(5) 0.029(3) Uani 1 1 d . . . C8 C 2.2778(13) -0.0217(12) 1.4568(5) 0.027(3) Uani 1 1 d . . . H8 H 2.3702 0.0403 1.4539 0.032 Uiso 1 1 calc R . . C9 C 2.2729(13) -0.1509(12) 1.4860(5) 0.026(3) Uani 1 1 d . . . C10 C 2.4032(13) -0.2245(12) 1.5190(6) 0.035(3) Uani 1 1 d . . . H10A H 2.3572 -0.2651 1.5534 0.052 Uiso 1 1 calc R . . H10B H 2.4892 -0.1533 1.5314 0.052 Uiso 1 1 calc R . . H10C H 2.45 -0.3042 1.4942 0.052 Uiso 1 1 calc R . . C11 C 1.6910(11) -0.5939(11) 1.5096(5) 0.025(3) Uani 1 1 d . . . H11A H 1.6978 -0.4901 1.525 0.03 Uiso 1 1 calc R . . H11B H 1.594 -0.6383 1.5264 0.03 Uiso 1 1 calc R . . C12 C 1.6665(14) -0.5977(11) 1.4445(5) 0.029(3) Uani 1 1 d . . . H12A H 1.5727 -0.5346 1.4341 0.035 Uiso 1 1 calc R . . H12B H 1.7655 -0.5599 1.4267 0.035 Uiso 1 1 calc R . . C13 C 1.573(3) -0.7606(18) 1.3669(6) 0.082(6) Uani 1 1 d . . . H13A H 1.4575 -0.7276 1.3675 0.098 Uiso 1 1 calc R . . H13B H 1.5712 -0.8675 1.3561 0.098 Uiso 1 1 calc R . . C14 C 1.650(3) -0.690(2) 1.3205(7) 0.082(6) Uani 1 1 d . . . H14A H 1.7691 -0.7092 1.3238 0.098 Uiso 1 1 calc R . . H14B H 1.6352 -0.5822 1.3277 0.098 Uiso 1 1 calc R . . C15 C 1.595(2) -0.7292(17) 1.2590(6) 0.056(4) Uani 1 1 d . . . H15A H 1.6323 -0.8312 1.2497 0.068 Uiso 1 1 calc R . . H15B H 1.4742 -0.7317 1.2582 0.068 Uiso 1 1 calc R . . C16 C 1.643(3) -0.643(2) 1.2110(8) 0.082(6) Uani 1 1 d . . . H16A H 1.7633 -0.6347 1.2134 0.098 Uiso 1 1 calc R . . H16B H 1.5984 -0.5432 1.2188 0.098 Uiso 1 1 calc R . . C17 C 1.597(2) -0.6887(18) 1.1503(7) 0.065(5) Uani 1 1 d . . . H17A H 1.6464 -0.7868 1.1421 0.078 Uiso 1 1 calc R . . H17B H 1.477 -0.7029 1.1486 0.078 Uiso 1 1 calc R . . C18 C 1.636(2) -0.6006(18) 1.1013(7) 0.072(5) Uani 1 1 d . . . H18A H 1.5783 -0.5056 1.1067 0.086 Uiso 1 1 calc R . . H18B H 1.755 -0.5791 1.104 0.086 Uiso 1 1 calc R . . C19 C 1.598(3) -0.660(2) 1.0433(7) 0.086(6) Uani 1 1 d . . . H19A H 1.4802 -0.6836 1.0403 0.104 Uiso 1 1 calc R . . H19B H 1.6593 -0.7531 1.0369 0.104 Uiso 1 1 calc R . . C20 C 1.638(2) -0.560(2) 0.9942(8) 0.085(6) Uani 1 1 d . . . H20A H 1.5537 -0.4839 0.9915 0.128 Uiso 1 1 calc R . . H20B H 1.6421 -0.6184 0.9571 0.128 Uiso 1 1 calc R . . H20C H 1.7451 -0.5125 1.0028 0.128 Uiso 1 1 calc R . . C21 C 1.8594(15) -0.1475(14) 1.4341(5) 0.037(3) Uani 1 1 d . . . H21A H 1.802 -0.0528 1.4299 0.044 Uiso 1 1 calc R . . H21B H 1.8119 -0.1949 1.4673 0.044 Uiso 1 1 calc R . . C22 C 1.8291(16) -0.2438(13) 1.3798(5) 0.039(3) Uani 1 1 d . . . H22A H 1.9013 -0.331 1.3801 0.047 Uiso 1 1 calc R . . H22B H 1.7139 -0.2779 1.3777 0.047 Uiso 1 1 calc R . . C23 C 1.8547(17) -0.2456(15) 1.2777(5) 0.043(3) Uani 1 1 d . . . H23A H 1.7497 -0.2999 1.2733 0.052 Uiso 1 1 calc R . . H23B H 1.945 -0.3181 1.2765 0.052 Uiso 1 1 calc R . . C24 C 1.8692(17) -0.1468(15) 1.2292(5) 0.041(3) Uani 1 1 d . . . H24A H 1.7753 -0.078 1.2307 0.049 Uiso 1 1 calc R . . H24B H 1.9698 -0.0873 1.2367 0.049 Uiso 1 1 calc R . . C25 C 1.875(2) -0.2149(15) 1.1694(6) 0.058(4) Uani 1 1 d . . . H25A H 1.7772 -0.2784 1.1622 0.07 Uiso 1 1 calc R . . H25B H 1.9725 -0.279 1.1669 0.07 Uiso 1 1 calc R . . C26 C 1.881(2) -0.1072(15) 1.1209(6) 0.063(5) Uani 1 1 d . . . H26A H 1.7799 -0.0467 1.1222 0.076 Uiso 1 1 calc R . . H26B H 1.9747 -0.04 1.1295 0.076 Uiso 1 1 calc R . . C27 C 1.895(2) -0.1725(16) 1.0616(5) 0.056(4) Uani 1 1 d . . . H27A H 1.8038 -0.2429 1.0533 0.067 Uiso 1 1 calc R . . H27B H 1.9985 -0.2289 1.0595 0.067 Uiso 1 1 calc R . . C28 C 1.8927(19) -0.0629(14) 1.0142(6) 0.047(4) Uani 1 1 d . . . H28A H 1.7899 -0.0057 1.0173 0.057 Uiso 1 1 calc R . . H28B H 1.9843 0.0068 1.0229 0.057 Uiso 1 1 calc R . . C29 C 1.905(2) -0.1202(15) 0.9538(6) 0.055(4) Uani 1 1 d . . . H29A H 1.8165 -0.1933 0.9449 0.066 Uiso 1 1 calc R . . H29B H 2.0107 -0.1716 0.9494 0.066 Uiso 1 1 calc R . . C30 C 1.892(2) -0.0010(16) 0.9093(6) 0.058(4) Uani 1 1 d . . . H30A H 1.7806 0.04 0.909 0.087 Uiso 1 1 calc R . . H30B H 1.9149 -0.0445 0.8704 0.087 Uiso 1 1 calc R . . H30C H 1.9708 0.0774 0.9201 0.087 Uiso 1 1 calc R . . C31 C 1.2071(14) -0.3712(13) 0.6839(5) 0.035(3) Uani 1 1 d . . . H31A H 1.1271 -0.4201 0.6566 0.053 Uiso 1 1 calc R . . H31B H 1.2355 -0.2751 0.6701 0.053 Uiso 1 1 calc R . . H31C H 1.16 -0.3576 0.7226 0.053 Uiso 1 1 calc R . . C32 C 1.3550(11) -0.4618(11) 0.6876(4) 0.0176(14) Uani 1 1 d . . . C33 C 1.5168(12) -0.4399(12) 0.6741(4) 0.0176(14) Uani 1 1 d . . . H33 H 1.56 -0.3537 0.6591 0.021 Uiso 1 1 calc R . . C34 C 1.6050(13) -0.5651(12) 0.6860(5) 0.0176(14) Uani 1 1 d . . . C35 C 1.7820(13) -0.5909(14) 0.6805(6) 0.028(3) Uani 1 1 d . . . H35A H 1.8383 -0.5655 0.7181 0.041 Uiso 1 1 calc R . . H35B H 1.8243 -0.5296 0.6508 0.041 Uiso 1 1 calc R . . H35C H 1.8011 -0.6947 0.6691 0.041 Uiso 1 1 calc R . . C36 C 1.606(2) -1.3895(15) 0.8363(7) 0.050(4) Uani 1 1 d . . . H36A H 1.537 -1.348 0.8674 0.074 Uiso 1 1 calc R . . H36B H 1.7009 -1.4382 0.8536 0.074 Uiso 1 1 calc R . . H36C H 1.5421 -1.4613 0.8114 0.074 Uiso 1 1 calc R . . C37 C 1.6628(14) -1.2686(12) 0.8004(5) 0.0300(16) Uani 1 1 d . . . C38 C 1.8115(14) -1.2467(12) 0.7764(5) 0.0300(16) Uani 1 1 d . . . H38 H 1.9044 -1.309 0.7786 0.036 Uiso 1 1 calc R . . C39 C 1.8014(14) -1.1156(12) 0.7479(5) 0.0300(16) Uani 1 1 d . . . C40 C 1.9217(14) -1.0365(13) 0.7142(6) 0.042(3) Uani 1 1 d . . . H40A H 1.8718 -0.9465 0.7007 0.063 Uiso 1 1 calc R . . H40B H 1.9544 -1.0997 0.6805 0.063 Uiso 1 1 calc R . . H40C H 2.0184 -1.0113 0.7391 0.063 Uiso 1 1 calc R . . C41 C 1.2110(13) -0.6800(12) 0.7282(5) 0.030(2) Uani 1 1 d . . . H41A H 1.2174 -0.7839 0.7132 0.035 Uiso 1 1 calc R . . H41B H 1.1095 -0.6379 0.7115 0.035 Uiso 1 1 calc R . . C42 C 1.1995(13) -0.6750(12) 0.7932(5) 0.030(2) Uani 1 1 d . . . H42A H 1.1123 -0.7425 0.8041 0.035 Uiso 1 1 calc R . . H42B H 1.3045 -0.7069 0.811 0.035 Uiso 1 1 calc R . . C43 C 1.186(3) -0.4959(16) 0.8754(7) 0.077(6) Uani 1 1 d . . . H43A H 1.1415 -0.3965 0.885 0.093 Uiso 1 1 calc R . . H43B H 1.3054 -0.4914 0.8842 0.093 Uiso 1 1 calc R . . C44 C 1.114(2) -0.5971(17) 0.9150(6) 0.066(5) Uani 1 1 d . . . H44A H 1.1672 -0.6943 0.9096 0.079 Uiso 1 1 calc R . . H44B H 0.9959 -0.6099 0.9047 0.079 Uiso 1 1 calc R . . C45 C 1.133(2) -0.5425(17) 0.9782(6) 0.057(4) Uani 1 1 d . . . H45A H 1.2457 -0.5049 0.985 0.069 Uiso 1 1 calc R . . H45B H 1.0576 -0.4581 0.9848 0.069 Uiso 1 1 calc R . . C46 C 1.101(2) -0.6498(17) 1.0228(6) 0.061(4) Uani 1 1 d . . . H46A H 1.1749 -0.735 1.0167 0.073 Uiso 1 1 calc R . . H46B H 0.9869 -0.6862 1.0172 0.073 Uiso 1 1 calc R . . C47 C 1.125(2) -0.5862(16) 1.0852(6) 0.058(4) Uani 1 1 d . . . H47A H 1.0487 -0.5025 1.0911 0.069 Uiso 1 1 calc R . . H47B H 1.2376 -0.5464 1.0898 0.069 Uiso 1 1 calc R . . C48 C 1.0995(18) -0.6910(15) 1.1336(6) 0.047(3) Uani 1 1 d . . . H48A H 0.9871 -0.7313 1.1289 0.056 Uiso 1 1 calc R . . H48B H 1.1763 -0.7744 1.128 0.056 Uiso 1 1 calc R . . C49 C 1.123(2) -0.6272(19) 1.1943(7) 0.071(5) Uani 1 1 d . . . H49A H 1.0432 -0.5458 1.2 0.085 Uiso 1 1 calc R . . H49B H 1.2336 -0.5837 1.1983 0.085 Uiso 1 1 calc R . . C50 C 1.104(2) -0.7284(17) 1.2427(7) 0.068(5) Uani 1 1 d . . . H50A H 0.9886 -0.7571 1.2447 0.101 Uiso 1 1 calc R . . H50B H 1.1395 -0.6778 1.2798 0.101 Uiso 1 1 calc R . . H50C H 1.1709 -0.8163 1.2353 0.101 Uiso 1 1 calc R . . C51 C 1.3969(13) -1.1290(13) 0.7985(5) 0.026(3) Uani 1 1 d . . . H51A H 1.3401 -1.2235 0.8026 0.031 Uiso 1 1 calc R . . H51B H 1.3456 -1.0823 0.7648 0.031 Uiso 1 1 calc R . . C52 C 1.3741(15) -1.0313(13) 0.8524(5) 0.033(3) Uani 1 1 d . . . H52A H 1.4515 -0.9477 0.8535 0.039 Uiso 1 1 calc R . . H52B H 1.2612 -0.9919 0.8527 0.039 Uiso 1 1 calc R . . C53 C 1.3972(18) -1.0336(14) 0.9559(5) 0.043(3) Uani 1 1 d . . . H53A H 1.2944 -0.9761 0.9578 0.052 Uiso 1 1 calc R . . H53B H 1.4907 -0.9644 0.9605 0.052 Uiso 1 1 calc R . . C54 C 1.405(2) -1.1411(15) 1.0040(6) 0.051(4) Uani 1 1 d . . . H54A H 1.314 -1.2128 0.9974 0.061 Uiso 1 1 calc R . . H54B H 1.509 -1.1963 1.0019 0.061 Uiso 1 1 calc R . . C55 C 1.392(2) -1.0657(15) 1.0645(6) 0.057(4) Uani 1 1 d . . . H55A H 1.2906 -1.0068 1.0662 0.068 Uiso 1 1 calc R . . H55B H 1.4862 -0.9978 1.072 0.068 Uiso 1 1 calc R . . C56 C 1.392(2) -1.1758(16) 1.1116(5) 0.057(4) Uani 1 1 d . . . H56A H 1.2989 -1.2445 1.1033 0.068 Uiso 1 1 calc R . . H56B H 1.4939 -1.2341 1.1096 0.068 Uiso 1 1 calc R . . C57 C 1.378(2) -1.1085(15) 1.1729(6) 0.056(4) Uani 1 1 d . . . H57A H 1.473 -1.0427 1.1817 0.067 Uiso 1 1 calc R . . H57B H 1.2781 -1.047 1.1745 0.067 Uiso 1 1 calc R . . C58 C 1.3709(19) -1.2160(15) 1.2198(6) 0.050(4) Uani 1 1 d . . . H58A H 1.271 -1.2764 1.2122 0.06 Uiso 1 1 calc R . . H58B H 1.4659 -1.2829 1.2154 0.06 Uiso 1 1 calc R . . C59 C 1.3703(18) -1.1583(16) 1.2813(6) 0.050(4) Uani 1 1 d . . . H59A H 1.278 -1.0886 1.2861 0.06 Uiso 1 1 calc R . . H59B H 1.4729 -1.1026 1.2904 0.06 Uiso 1 1 calc R . . C60 C 1.355(2) -1.2750(18) 1.3247(6) 0.060(4) Uani 1 1 d . . . H60A H 1.2546 -1.3316 1.3159 0.09 Uiso 1 1 calc R . . H60B H 1.3514 -1.2282 1.3642 0.09 Uiso 1 1 calc R . . H60C H 1.4499 -1.3409 1.3222 0.09 Uiso 1 1 calc R . . N1 N 1.9872(9) -0.6071(10) 1.5305(4) 0.020(2) Uani 1 1 d . . . N2 N 1.8331(11) -0.6688(11) 1.5285(4) 0.023(2) Uani 1 1 d . . . N3 N 2.1184(10) -0.2069(9) 1.4803(4) 0.022(2) Uani 1 1 d . . . N4 N 2.0299(14) -0.1187(13) 1.4471(6) 0.031(3) Uani 1 1 d . . . N5 N 1.5034(10) -0.6633(9) 0.7056(3) 0.0136(18) Uani 1 1 d . . . N6 N 1.3498(9) -0.6016(9) 0.7080(4) 0.0140(19) Uani 1 1 d . . . N7 N 1.6464(10) -1.0606(9) 0.7541(4) 0.0177(19) Uani 1 1 d . . . N8 N 1.5671(12) -1.1575(11) 0.7873(4) 0.018(2) Uani 1 1 d . . . O1 O 1.6365(10) -0.7421(9) 1.4233(3) 0.037(2) Uani 1 1 d . . . O2 O 1.8612(11) -0.1632(9) 1.3314(3) 0.039(2) Uani 1 1 d . . . O3 O 1.1628(11) -0.5269(9) 0.8143(4) 0.044(2) Uani 1 1 d . . . O4 O 1.4038(10) -1.1163(9) 0.9018(3) 0.039(2) Uani 1 1 d . . . Cl1 Cl 1.8975(3) -0.2897(3) 1.57768(12) 0.0237(6) Uani 1 1 d . . . Cl2 Cl 2.1789(4) -0.5117(3) 1.42586(13) 0.0330(7) Uani 1 1 d . . . Cl3 Cl 1.7142(4) -0.7600(3) 0.80893(14) 0.0365(7) Uani 1 1 d . . . Cl4 Cl 1.4056(3) -0.9816(3) 0.65707(11) 0.0241(6) Uani 1 1 d . . . Pd1 Pd 2.04288(7) -0.40478(7) 1.50388(4) 0.0180(2) Uani 1 1 d . . . Pd2 Pd 1.56512(7) -0.86592(7) 0.73113(4) 0.0192(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.039(7) 0.014(6) 0.056(8) 0.004(6) 0.015(6) -0.013(5) C2 0.013(5) 0.018(6) 0.024(6) -0.001(4) 0.011(4) -0.005(4) C3 0.011(5) 0.015(6) 0.037(7) 0.003(5) -0.001(5) 0.000(4) C4 0.035(7) 0.006(6) 0.025(6) -0.002(5) 0.004(5) -0.005(5) C5 0.007(5) 0.037(7) 0.024(6) 0.010(5) 0.001(5) 0.013(5) C6 0.078(11) 0.014(7) 0.046(9) 0.002(6) 0.002(8) -0.005(7) C7 0.045(7) 0.007(5) 0.035(7) 0.006(5) 0.014(6) -0.008(5) C8 0.024(6) 0.012(6) 0.044(7) -0.005(5) 0.005(5) 0.000(5) C9 0.024(6) 0.017(6) 0.035(7) -0.009(5) 0.008(5) -0.004(5) C10 0.020(6) 0.014(6) 0.070(9) -0.001(6) 0.009(6) -0.002(5) C11 0.006(5) 0.011(5) 0.057(8) -0.003(5) -0.007(5) 0.007(4) C12 0.029(6) 0.011(6) 0.047(7) 0.007(5) -0.010(5) -0.002(5) C13 0.16(2) 0.045(10) 0.036(9) -0.003(8) -0.017(11) -0.028(11) C14 0.137(18) 0.064(12) 0.045(10) 0.009(9) -0.015(11) 0.007(12) C15 0.085(12) 0.045(9) 0.039(8) -0.007(7) 0.005(8) -0.001(8) C16 0.097(14) 0.083(14) 0.066(12) 0.024(11) -0.024(11) -0.015(12) C17 0.084(12) 0.049(10) 0.059(11) -0.026(8) 0.004(9) -0.010(9) C18 0.098(14) 0.043(10) 0.076(13) 0.024(9) -0.011(11) -0.001(9) C19 0.16(2) 0.050(11) 0.050(11) -0.006(9) 0.002(12) -0.018(12) C20 0.112(16) 0.058(12) 0.087(14) 0.027(10) -0.021(12) 0.016(11) C21 0.046(8) 0.038(8) 0.028(7) 0.004(6) 0.001(6) 0.010(6) C22 0.054(8) 0.026(7) 0.040(8) 0.018(6) 0.004(6) -0.018(6) C23 0.053(8) 0.042(8) 0.032(7) -0.010(6) 0.001(6) -0.011(7) C24 0.052(8) 0.042(8) 0.029(7) 0.006(6) 0.002(6) 0.002(6) C25 0.095(12) 0.037(8) 0.042(8) -0.002(7) -0.012(8) -0.014(8) C26 0.128(15) 0.026(8) 0.035(8) 0.012(6) -0.020(9) -0.011(8) C27 0.096(12) 0.048(9) 0.023(7) -0.010(6) 0.014(7) 0.015(8) C28 0.080(10) 0.022(7) 0.040(8) 0.006(6) 0.001(7) -0.007(7) C29 0.097(12) 0.032(8) 0.036(8) 0.001(6) 0.012(8) -0.001(8) C30 0.087(12) 0.048(9) 0.040(8) 0.013(7) -0.012(8) -0.011(8) C31 0.030(6) 0.032(7) 0.043(7) 0.007(6) -0.012(6) 0.020(5) C32 0.013(3) 0.017(3) 0.023(3) 0.000(3) -0.006(3) -0.003(2) C33 0.013(3) 0.017(3) 0.023(3) 0.000(3) -0.006(3) -0.003(2) C34 0.013(3) 0.017(3) 0.023(3) 0.000(3) -0.006(3) -0.003(2) C35 0.017(6) 0.023(7) 0.043(8) -0.001(6) 0.000(5) 0.009(5) C36 0.091(12) 0.014(7) 0.044(9) 0.002(6) 0.003(8) 0.012(7) C37 0.034(4) 0.011(3) 0.045(4) -0.001(3) -0.003(3) 0.011(3) C38 0.034(4) 0.011(3) 0.045(4) -0.001(3) -0.003(3) 0.011(3) C39 0.034(4) 0.011(3) 0.045(4) -0.001(3) -0.003(3) 0.011(3) C40 0.019(6) 0.027(7) 0.081(10) 0.004(7) 0.006(6) 0.008(5) C41 0.018(4) 0.020(4) 0.052(5) 0.004(4) 0.018(4) -0.009(3) C42 0.018(4) 0.020(4) 0.052(5) 0.004(4) 0.018(4) -0.009(3) C43 0.134(17) 0.026(9) 0.073(12) -0.006(8) 0.044(12) 0.003(10) C44 0.116(15) 0.041(9) 0.041(9) -0.001(7) 0.019(9) -0.013(9) C45 0.075(11) 0.045(10) 0.054(10) 0.009(8) 0.019(9) -0.004(8) C46 0.103(14) 0.039(9) 0.040(9) 0.000(7) 0.011(9) 0.009(9) C47 0.088(12) 0.028(8) 0.058(10) -0.001(7) 0.019(9) 0.008(8) C48 0.062(9) 0.035(8) 0.044(9) 0.007(6) 0.011(7) -0.003(7) C49 0.108(14) 0.055(11) 0.052(10) 0.020(8) 0.010(10) 0.029(10) C50 0.104(14) 0.045(10) 0.057(10) 0.023(8) 0.018(10) 0.005(9) C51 0.025(6) 0.031(7) 0.024(6) 0.018(5) 0.006(5) 0.002(5) C52 0.035(7) 0.024(6) 0.040(7) 0.010(5) 0.010(5) 0.018(5) C53 0.061(9) 0.035(8) 0.034(7) 0.008(6) 0.004(6) 0.018(7) C54 0.076(10) 0.036(8) 0.040(8) 0.006(6) -0.002(7) 0.008(7) C55 0.106(13) 0.028(8) 0.038(8) 0.011(6) 0.008(8) 0.002(8) C56 0.097(12) 0.047(9) 0.025(7) 0.002(6) 0.004(7) -0.003(8) C57 0.097(12) 0.031(8) 0.039(8) 0.005(6) -0.003(8) -0.004(8) C58 0.074(10) 0.034(8) 0.042(8) -0.002(6) 0.006(7) -0.014(7) C59 0.058(9) 0.053(9) 0.041(8) 0.018(7) 0.000(7) -0.008(7) C60 0.076(11) 0.066(11) 0.041(8) 0.012(8) 0.019(8) 0.002(9) N1 0.003(4) 0.019(5) 0.036(6) -0.004(4) 0.001(4) 0.004(4) N2 0.014(5) 0.021(5) 0.034(6) -0.001(5) -0.003(4) -0.009(4) N3 0.021(5) 0.003(4) 0.041(6) 0.001(4) -0.003(4) 0.000(4) N4 0.034(7) 0.014(6) 0.044(8) 0.009(6) 0.003(6) 0.001(5) N5 0.014(5) 0.010(5) 0.016(4) -0.004(4) -0.002(4) 0.004(3) N6 0.012(4) 0.016(5) 0.015(5) 0.001(4) 0.005(4) 0.001(3) N7 0.020(5) 0.009(4) 0.023(5) -0.007(4) 0.001(4) 0.004(4) N8 0.029(6) 0.020(6) 0.005(5) -0.004(4) -0.004(4) -0.004(5) O1 0.047(5) 0.026(5) 0.038(5) 0.005(4) -0.012(4) -0.006(4) O2 0.065(6) 0.034(5) 0.017(4) -0.001(4) -0.006(4) -0.006(4) O3 0.054(6) 0.026(5) 0.053(6) 0.003(4) 0.019(5) 0.012(4) O4 0.059(6) 0.025(5) 0.033(5) 0.010(4) 0.006(4) 0.016(4) Cl1 0.0256(14) 0.0194(14) 0.0262(15) 0.0012(11) 0.0027(11) 0.0058(11) Cl2 0.0464(18) 0.0208(15) 0.0328(17) 0.0035(13) 0.0158(14) -0.0043(13) Cl3 0.0447(18) 0.0220(16) 0.0413(18) -0.0016(13) -0.0147(15) 0.0021(13) Cl4 0.0280(14) 0.0207(14) 0.0236(14) 0.0014(11) -0.0006(11) -0.0056(11) Pd1 0.0174(4) 0.0117(4) 0.0252(5) 0.0030(3) 0.0031(3) -0.0016(3) Pd2 0.0195(4) 0.0126(4) 0.0253(5) 0.0013(3) -0.0005(3) 0.0035(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.462(14) . ? C1 H1A 0.98 . ? C1 H1B 0.98 . ? C1 H1C 0.98 . ? C2 N2 1.370(14) . ? C2 C3 1.380(14) . ? C3 C4 1.385(15) . ? C3 H3 0.95 . ? C4 N1 1.308(14) . ? C4 C5 1.479(15) . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 C7 1.480(17) . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 C8 1.353(15) . ? C7 N4 1.389(16) . ? C8 C9 1.393(16) . ? C8 H8 0.95 . ? C9 N3 1.361(14) . ? C9 C10 1.473(16) . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 N2 1.417(13) . ? C11 C12 1.503(16) . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C12 O1 1.393(13) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 O1 1.383(16) . ? C13 C14 1.44(2) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 C15 1.49(2) . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C15 C16 1.45(2) . ? C15 H15A 0.99 . ? C15 H15B 0.99 . ? C16 C17 1.47(2) . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? C17 C18 1.47(2) . ? C17 H17A 0.99 . ? C17 H17B 0.99 . ? C18 C19 1.43(2) . ? C18 H18A 0.99 . ? C18 H18B 0.99 . ? C19 C20 1.54(2) . ? C19 H19A 0.99 . ? C19 H19B 0.99 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 N4 1.437(17) . ? C21 C22 1.494(16) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C22 O2 1.403(13) . ? C22 H22A 0.99 . ? C22 H22B 0.99 . ? C23 O2 1.404(13) . ? C23 C24 1.484(17) . ? C23 H23A 0.99 . ? C23 H23B 0.99 . ? C24 C25 1.475(17) . ? C24 H24A 0.99 . ? C24 H24B 0.99 . ? C25 C26 1.534(18) . ? C25 H25A 0.99 . ? C25 H25B 0.99 . ? C26 C27 1.462(18) . ? C26 H26A 0.99 . ? C26 H26B 0.99 . ? C27 C28 1.523(18) . ? C27 H27A 0.99 . ? C27 H27B 0.99 . ? C28 C29 1.459(17) . ? C28 H28A 0.99 . ? C28 H28B 0.99 . ? C29 C30 1.541(18) . ? C29 H29A 0.99 . ? C29 H29B 0.99 . ? C30 H30A 0.98 . ? C30 H30B 0.98 . ? C30 H30C 0.98 . ? C31 C32 1.466(13) . ? C31 H31A 0.98 . ? C31 H31B 0.98 . ? C31 H31C 0.98 . ? C32 C33 1.385(14) . ? C32 N6 1.387(13) . ? C33 C34 1.386(15) . ? C33 H33 0.95 . ? C34 N5 1.330(14) . ? C34 C35 1.473(15) . ? C35 H35A 0.98 . ? C35 H35B 0.98 . ? C35 H35C 0.98 . ? C36 C37 1.502(19) . ? C36 H36A 0.98 . ? C36 H36B 0.98 . ? C36 H36C 0.98 . ? C37 N8 1.322(14) . ? C37 C38 1.370(16) . ? C38 C39 1.399(16) . ? C38 H38 0.95 . ? C39 N7 1.370(13) . ? C39 C40 1.485(17) . ? C40 H40A 0.98 . ? C40 H40B 0.98 . ? C40 H40C 0.98 . ? C41 N6 1.444(12) . ? C41 C42 1.499(16) . ? C41 H41A 0.99 . ? C41 H41B 0.99 . ? C42 O3 1.440(13) . ? C42 H42A 0.99 . ? C42 H42B 0.99 . ? C43 O3 1.423(18) . ? C43 C44 1.47(2) . ? C43 H43A 0.99 . ? C43 H43B 0.99 . ? C44 C45 1.51(2) . ? C44 H44A 0.99 . ? C44 H44B 0.99 . ? C45 C46 1.49(2) . ? C45 H45A 0.99 . ? C45 H45B 0.99 . ? C46 C47 1.52(2) . ? C46 H46A 0.99 . ? C46 H46B 0.99 . ? C47 C48 1.531(18) . ? C47 H47A 0.99 . ? C47 H47B 0.99 . ? C48 C49 1.48(2) . ? C48 H48A 0.99 . ? C48 H48B 0.99 . ? C49 C50 1.50(2) . ? C49 H49A 0.99 . ? C49 H49B 0.99 . ? C50 H50A 0.98 . ? C50 H50B 0.98 . ? C50 H50C 0.98 . ? C51 N8 1.442(14) . ? C51 C52 1.495(16) . ? C51 H51A 0.99 . ? C51 H51B 0.99 . ? C52 O4 1.428(13) . ? C52 H52A 0.99 . ? C52 H52B 0.99 . ? C53 O4 1.416(14) . ? C53 C54 1.524(17) . ? C53 H53A 0.99 . ? C53 H53B 0.99 . ? C54 C55 1.518(18) . ? C54 H54A 0.99 . ? C54 H54B 0.99 . ? C55 C56 1.523(18) . ? C55 H55A 0.99 . ? C55 H55B 0.99 . ? C56 C57 1.508(18) . ? C56 H56A 0.99 . ? C56 H56B 0.99 . ? C57 C58 1.504(18) . ? C57 H57A 0.99 . ? C57 H57B 0.99 . ? C58 C59 1.477(18) . ? C58 H58A 0.99 . ? C58 H58B 0.99 . ? C59 C60 1.512(18) . ? C59 H59A 0.99 . ? C59 H59B 0.99 . ? C60 H60A 0.98 . ? C60 H60B 0.98 . ? C60 H60C 0.98 . ? N1 N2 1.377(12) . ? N1 Pd1 2.036(9) . ? N3 N4 1.339(14) . ? N3 Pd1 2.019(8) . ? N5 N6 1.376(11) . ? N5 Pd2 2.031(8) . ? N7 N8 1.379(13) . ? N7 Pd2 1.991(8) . ? Cl1 Pd1 2.300(3) . ? Cl2 Pd1 2.304(3) . ? Cl3 Pd2 2.294(3) . ? Cl4 Pd2 2.313(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N2 C2 C3 107.3(9) . . ? N2 C2 C1 122.0(10) . . ? C3 C2 C1 130.6(10) . . ? C2 C3 C4 105.8(10) . . ? C2 C3 H3 127.1 . . ? C4 C3 H3 127.1 . . ? N1 C4 C3 110.9(10) . . ? N1 C4 C5 122.3(10) . . ? C3 C4 C5 126.6(10) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 N4 107.4(10) . . ? C8 C7 C6 133.8(11) . . ? N4 C7 C6 118.9(12) . . ? C7 C8 C9 107.1(10) . . ? C7 C8 H8 126.4 . . ? C9 C8 H8 126.4 . . ? N3 C9 C8 108.5(10) . . ? N3 C9 C10 121.5(10) . . ? C8 C9 C10 130.0(10) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 C12 113.9(9) . . ? N2 C11 H11A 108.8 . . ? C12 C11 H11A 108.8 . . ? N2 C11 H11B 108.8 . . ? C12 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? O1 C12 C11 109.0(9) . . ? O1 C12 H12A 109.9 . . ? C11 C12 H12A 109.9 . . ? O1 C12 H12B 109.9 . . ? C11 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? O1 C13 C14 120.0(15) . . ? O1 C13 H13A 107.3 . . ? C14 C13 H13A 107.3 . . ? O1 C13 H13B 107.3 . . ? C14 C13 H13B 107.3 . . ? H13A C13 H13B 106.9 . . ? C13 C14 C15 118.8(17) . . ? C13 C14 H14A 107.6 . . ? C15 C14 H14A 107.6 . . ? C13 C14 H14B 107.6 . . ? C15 C14 H14B 107.6 . . ? H14A C14 H14B 107 . . ? C16 C15 C14 122.0(16) . . ? C16 C15 H15A 106.8 . . ? C14 C15 H15A 106.8 . . ? C16 C15 H15B 106.8 . . ? C14 C15 H15B 106.8 . . ? H15A C15 H15B 106.7 . . ? C15 C16 C17 121.6(16) . . ? C15 C16 H16A 106.9 . . ? C17 C16 H16A 106.9 . . ? C15 C16 H16B 106.9 . . ? C17 C16 H16B 106.9 . . ? H16A C16 H16B 106.7 . . ? C18 C17 C16 122.8(15) . . ? C18 C17 H17A 106.6 . . ? C16 C17 H17A 106.6 . . ? C18 C17 H17B 106.6 . . ? C16 C17 H17B 106.6 . . ? H17A C17 H17B 106.6 . . ? C19 C18 C17 118.5(15) . . ? C19 C18 H18A 107.7 . . ? C17 C18 H18A 107.7 . . ? C19 C18 H18B 107.7 . . ? C17 C18 H18B 107.7 . . ? H18A C18 H18B 107.1 . . ? C18 C19 C20 115.6(16) . . ? C18 C19 H19A 108.4 . . ? C20 C19 H19A 108.4 . . ? C18 C19 H19B 108.4 . . ? C20 C19 H19B 108.4 . . ? H19A C19 H19B 107.4 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N4 C21 C22 113.5(11) . . ? N4 C21 H21A 108.9 . . ? C22 C21 H21A 108.9 . . ? N4 C21 H21B 108.9 . . ? C22 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? O2 C22 C21 108.8(10) . . ? O2 C22 H22A 109.9 . . ? C21 C22 H22A 109.9 . . ? O2 C22 H22B 109.9 . . ? C21 C22 H22B 109.9 . . ? H22A C22 H22B 108.3 . . ? O2 C23 C24 110.0(11) . . ? O2 C23 H23A 109.7 . . ? C24 C23 H23A 109.7 . . ? O2 C23 H23B 109.7 . . ? C24 C23 H23B 109.7 . . ? H23A C23 H23B 108.2 . . ? C25 C24 C23 117.7(11) . . ? C25 C24 H24A 107.9 . . ? C23 C24 H24A 107.9 . . ? C25 C24 H24B 107.9 . . ? C23 C24 H24B 107.9 . . ? H24A C24 H24B 107.2 . . ? C24 C25 C26 115.4(12) . . ? C24 C25 H25A 108.4 . . ? C26 C25 H25A 108.4 . . ? C24 C25 H25B 108.4 . . ? C26 C25 H25B 108.4 . . ? H25A C25 H25B 107.5 . . ? C27 C26 C25 116.2(12) . . ? C27 C26 H26A 108.2 . . ? C25 C26 H26A 108.2 . . ? C27 C26 H26B 108.2 . . ? C25 C26 H26B 108.2 . . ? H26A C26 H26B 107.4 . . ? C26 C27 C28 114.9(12) . . ? C26 C27 H27A 108.6 . . ? C28 C27 H27A 108.6 . . ? C26 C27 H27B 108.6 . . ? C28 C27 H27B 108.6 . . ? H27A C27 H27B 107.5 . . ? C29 C28 C27 118.0(11) . . ? C29 C28 H28A 107.8 . . ? C27 C28 H28A 107.8 . . ? C29 C28 H28B 107.8 . . ? C27 C28 H28B 107.8 . . ? H28A C28 H28B 107.1 . . ? C28 C29 C30 113.7(12) . . ? C28 C29 H29A 108.8 . . ? C30 C29 H29A 108.8 . . ? C28 C29 H29B 108.8 . . ? C30 C29 H29B 108.8 . . ? H29A C29 H29B 107.7 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C32 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 N6 105.4(9) . . ? C33 C32 C31 133.4(10) . . ? N6 C32 C31 121.2(9) . . ? C32 C33 C34 108.5(10) . . ? C32 C33 H33 125.8 . . ? C34 C33 H33 125.8 . . ? N5 C34 C33 108.7(9) . . ? N5 C34 C35 123.2(10) . . ? C33 C34 C35 128.1(10) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 H36A 109.5 . . ? C37 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C37 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N8 C37 C38 107.5(11) . . ? N8 C37 C36 122.1(11) . . ? C38 C37 C36 130.4(11) . . ? C37 C38 C39 107.5(10) . . ? C37 C38 H38 126.3 . . ? C39 C38 H38 126.3 . . ? N7 C39 C38 107.9(10) . . ? N7 C39 C40 119.9(10) . . ? C38 C39 C40 132.2(10) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N6 C41 C42 114.2(9) . . ? N6 C41 H41A 108.7 . . ? C42 C41 H41A 108.7 . . ? N6 C41 H41B 108.7 . . ? C42 C41 H41B 108.7 . . ? H41A C41 H41B 107.6 . . ? O3 C42 C41 108.9(10) . . ? O3 C42 H42A 109.9 . . ? C41 C42 H42A 109.9 . . ? O3 C42 H42B 109.9 . . ? C41 C42 H42B 109.9 . . ? H42A C42 H42B 108.3 . . ? O3 C43 C44 118.3(14) . . ? O3 C43 H43A 107.7 . . ? C44 C43 H43A 107.7 . . ? O3 C43 H43B 107.7 . . ? C44 C43 H43B 107.7 . . ? H43A C43 H43B 107.1 . . ? C43 C44 C45 112.5(13) . . ? C43 C44 H44A 109.1 . . ? C45 C44 H44A 109.1 . . ? C43 C44 H44B 109.1 . . ? C45 C44 H44B 109.1 . . ? H44A C44 H44B 107.8 . . ? C46 C45 C44 117.2(13) . . ? C46 C45 H45A 108 . . ? C44 C45 H45A 108 . . ? C46 C45 H45B 108 . . ? C44 C45 H45B 108 . . ? H45A C45 H45B 107.2 . . ? C45 C46 C47 113.6(13) . . ? C45 C46 H46A 108.8 . . ? C47 C46 H46A 108.8 . . ? C45 C46 H46B 108.8 . . ? C47 C46 H46B 108.8 . . ? H46A C46 H46B 107.7 . . ? C46 C47 C48 116.8(13) . . ? C46 C47 H47A 108.1 . . ? C48 C47 H47A 108.1 . . ? C46 C47 H47B 108.1 . . ? C48 C47 H47B 108.1 . . ? H47A C47 H47B 107.3 . . ? C49 C48 C47 116.3(13) . . ? C49 C48 H48A 108.2 . . ? C47 C48 H48A 108.2 . . ? C49 C48 H48B 108.2 . . ? C47 C48 H48B 108.2 . . ? H48A C48 H48B 107.4 . . ? C48 C49 C50 117.5(15) . . ? C48 C49 H49A 107.9 . . ? C50 C49 H49A 107.9 . . ? C48 C49 H49B 107.9 . . ? C50 C49 H49B 107.9 . . ? H49A C49 H49B 107.2 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N8 C51 C52 112.6(10) . . ? N8 C51 H51A 109.1 . . ? C52 C51 H51A 109.1 . . ? N8 C51 H51B 109.1 . . ? C52 C51 H51B 109.1 . . ? H51A C51 H51B 107.8 . . ? O4 C52 C51 108.2(9) . . ? O4 C52 H52A 110.1 . . ? C51 C52 H52A 110.1 . . ? O4 C52 H52B 110.1 . . ? C51 C52 H52B 110.1 . . ? H52A C52 H52B 108.4 . . ? O4 C53 C54 107.7(10) . . ? O4 C53 H53A 110.2 . . ? C54 C53 H53A 110.2 . . ? O4 C53 H53B 110.2 . . ? C54 C53 H53B 110.2 . . ? H53A C53 H53B 108.5 . . ? C55 C54 C53 112.8(11) . . ? C55 C54 H54A 109 . . ? C53 C54 H54A 109 . . ? C55 C54 H54B 109 . . ? C53 C54 H54B 109 . . ? H54A C54 H54B 107.8 . . ? C54 C55 C56 111.9(11) . . ? C54 C55 H55A 109.2 . . ? C56 C55 H55A 109.2 . . ? C54 C55 H55B 109.2 . . ? C56 C55 H55B 109.2 . . ? H55A C55 H55B 107.9 . . ? C57 C56 C55 114.8(12) . . ? C57 C56 H56A 108.6 . . ? C55 C56 H56A 108.6 . . ? C57 C56 H56B 108.6 . . ? C55 C56 H56B 108.6 . . ? H56A C56 H56B 107.5 . . ? C58 C57 C56 115.5(11) . . ? C58 C57 H57A 108.4 . . ? C56 C57 H57A 108.4 . . ? C58 C57 H57B 108.4 . . ? C56 C57 H57B 108.4 . . ? H57A C57 H57B 107.5 . . ? C59 C58 C57 118.6(12) . . ? C59 C58 H58A 107.7 . . ? C57 C58 H58A 107.7 . . ? C59 C58 H58B 107.7 . . ? C57 C58 H58B 107.7 . . ? H58A C58 H58B 107.1 . . ? C58 C59 C60 114.3(13) . . ? C58 C59 H59A 108.7 . . ? C60 C59 H59A 108.7 . . ? C58 C59 H59B 108.7 . . ? C60 C59 H59B 108.7 . . ? H59A C59 H59B 107.6 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C4 N1 N2 107.4(9) . . ? C4 N1 Pd1 127.2(8) . . ? N2 N1 Pd1 125.4(7) . . ? C2 N2 N1 108.5(9) . . ? C2 N2 C11 128.4(9) . . ? N1 N2 C11 123.1(9) . . ? N4 N3 C9 107.6(10) . . ? N4 N3 Pd1 124.6(7) . . ? C9 N3 Pd1 127.0(7) . . ? N3 N4 C7 109.3(10) . . ? N3 N4 C21 120.9(11) . . ? C7 N4 C21 129.7(11) . . ? C34 N5 N6 108.2(8) . . ? C34 N5 Pd2 126.2(7) . . ? N6 N5 Pd2 125.6(6) . . ? N5 N6 C32 109.3(8) . . ? N5 N6 C41 122.0(9) . . ? C32 N6 C41 128.7(9) . . ? C39 N7 N8 105.5(9) . . ? C39 N7 Pd2 126.8(7) . . ? N8 N7 Pd2 127.0(7) . . ? C37 N8 N7 111.5(10) . . ? C37 N8 C51 131.1(11) . . ? N7 N8 C51 117.2(9) . . ? C13 O1 C12 116.2(10) . . ? C22 O2 C23 114.6(9) . . ? C43 O3 C42 115.7(10) . . ? C53 O4 C52 113.8(9) . . ? N3 Pd1 N1 174.9(4) . . ? N3 Pd1 Cl1 89.7(3) . . ? N1 Pd1 Cl1 91.8(2) . . ? N3 Pd1 Cl2 88.5(3) . . ? N1 Pd1 Cl2 90.3(2) . . ? Cl1 Pd1 Cl2 176.38(12) . . ? N7 Pd2 N5 174.8(4) . . ? N7 Pd2 Cl3 88.1(2) . . ? N5 Pd2 Cl3 90.0(2) . . ? N7 Pd2 Cl4 89.9(2) . . ? N5 Pd2 Cl4 92.3(2) . . ? Cl3 Pd2 Cl4 176.17(12) . . ? data_miguel140411 _database_code_depnum_ccdc_archive 'CCDC 836432' #TrackingRef 'publimiguel140411.cif' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C23 H45 Cl2 N3 Pd1' _chemical_formula_sum 'C23 H45 Cl2 N3 Pd' _chemical_formula_weight 540.92 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.7877(10) _cell_length_b 21.0937(13) _cell_length_c 8.1090(5) _cell_angle_alpha 90 _cell_angle_beta 102.061(3) _cell_angle_gamma 90 _cell_volume 2640.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 9582 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 34.92 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.36 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.919 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.912 _exptl_absorpt_correction_T_max 0.991 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180(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 'Bruker Kappa APEX II' _diffrn_measurement_method \w-\f _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_av_unetI/netI 0.0292 _diffrn_reflns_number 124677 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 36.96 _diffrn_reflns_theta_full 36.96 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 13366 _reflns_number_gt 10115 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0224P)^2^+1.4003P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 13366 _refine_ls_number_parameters 266 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0553 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0682 _refine_ls_wR_factor_gt 0.0593 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.781 _refine_diff_density_min -0.612 _refine_diff_density_rms 0.086 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.17805(11) 0.49441(8) 0.0224(2) 0.0356(3) Uani 1 1 d . . . H1A H 0.19 0.45 0.0541 0.053 Uiso 1 1 calc R . . H1B H 0.1178 0.4986 -0.0387 0.053 Uiso 1 1 calc R . . H1C H 0.1873 0.5207 0.1243 0.053 Uiso 1 1 calc R . . C2 C 0.23728(9) 0.51565(6) -0.08752(17) 0.0247(2) Uani 1 1 d . . . C3 C 0.22343(10) 0.56423(7) -0.20662(19) 0.0279(3) Uani 1 1 d . . . H3 H 0.1755 0.5925 -0.2289 0.033 Uiso 1 1 calc R . . C4 C 0.29266(9) 0.56341(6) -0.28594(16) 0.0239(2) Uani 1 1 d . . . C5 C 0.31078(11) 0.60256(7) -0.42688(18) 0.0309(3) Uani 1 1 d . . . H5A H 0.3689 0.6209 -0.3945 0.046 Uiso 1 1 calc R . . H5B H 0.2679 0.6367 -0.4521 0.046 Uiso 1 1 calc R . . H5C H 0.3075 0.5759 -0.5271 0.046 Uiso 1 1 calc R . . C6 C 0.41906(9) 0.48832(6) -0.26734(16) 0.0215(2) Uani 1 1 d . . . H6A H 0.4723 0.4952 -0.1801 0.026 Uiso 1 1 calc R . . H6B H 0.427 0.5087 -0.373 0.026 Uiso 1 1 calc R . . C7 C 0.40401(9) 0.41768(6) -0.29639(15) 0.0219(2) Uani 1 1 d . . . H7A H 0.3421 0.4104 -0.3471 0.026 Uiso 1 1 calc R . . H7B H 0.4384 0.4027 -0.3778 0.026 Uiso 1 1 calc R . . C8 C 0.52577(8) 0.37320(6) -0.09447(16) 0.0218(2) Uani 1 1 d . . . H8A H 0.5427 0.3572 0.0226 0.026 Uiso 1 1 calc R . . H8B H 0.5514 0.4159 -0.0967 0.026 Uiso 1 1 calc R . . C9 C 0.56588(9) 0.32974(7) -0.20825(19) 0.0279(3) Uani 1 1 d . . . H9A H 0.5422 0.2864 -0.2059 0.033 Uiso 1 1 calc R . . H9B H 0.551 0.3454 -0.3259 0.033 Uiso 1 1 calc R . . C10 C 0.66388(9) 0.32811(7) -0.14834(18) 0.0256(2) Uani 1 1 d . . . H10A H 0.6783 0.3207 -0.0251 0.031 Uiso 1 1 calc R . . H10B H 0.6883 0.3697 -0.1707 0.031 Uiso 1 1 calc R . . C11 C 0.70496(10) 0.27616(7) -0.23664(19) 0.0279(3) Uani 1 1 d . . . H11A H 0.675 0.2356 -0.2254 0.034 Uiso 1 1 calc R . . H11B H 0.6952 0.2864 -0.3583 0.034 Uiso 1 1 calc R . . C12 C 0.80182(11) 0.26683(7) -0.1696(2) 0.0332(3) Uani 1 1 d . . . H12A H 0.8116 0.2559 -0.0484 0.04 Uiso 1 1 calc R . . H12B H 0.8216 0.2305 -0.229 0.04 Uiso 1 1 calc R . . C13 C 0.85641(10) 0.32420(8) -0.1903(2) 0.0359(3) Uani 1 1 d . . . H13A H 0.8409 0.3385 -0.3092 0.043 Uiso 1 1 calc R . . H13B H 0.8418 0.359 -0.1191 0.043 Uiso 1 1 calc R . . C14 C 0.95276(12) 0.31279(11) -0.1445(3) 0.0514(5) Uani 1 1 d . . . H14A H 0.9678 0.2785 -0.2167 0.062 Uiso 1 1 calc R . . H14B H 0.9685 0.2982 -0.026 0.062 Uiso 1 1 calc R . . C15 C 1.00560(14) 0.37102(11) -0.1643(3) 0.0577(6) Uani 1 1 d . . . H15A H 0.9917 0.3851 -0.2821 0.087 Uiso 1 1 calc R . . H15B H 1.0674 0.3608 -0.1321 0.087 Uiso 1 1 calc R . . H15C H 0.9919 0.405 -0.0915 0.087 Uiso 1 1 calc R . . C16 C 0.38853(9) 0.31525(6) -0.16346(17) 0.0222(2) Uani 1 1 d . . . H16A H 0.4194 0.2872 -0.0726 0.027 Uiso 1 1 calc R . . H16B H 0.3982 0.2982 -0.2718 0.027 Uiso 1 1 calc R . . C17 C 0.29218(9) 0.31207(6) -0.16502(18) 0.0249(2) Uani 1 1 d . . . H17A H 0.2593 0.3367 -0.2614 0.03 Uiso 1 1 calc R . . H17B H 0.2805 0.3304 -0.0596 0.03 Uiso 1 1 calc R . . C18 C 0.26416(10) 0.24290(7) -0.18042(19) 0.0279(3) Uani 1 1 d . . . H18A H 0.2732 0.2265 -0.2898 0.033 Uiso 1 1 calc R . . H18B H 0.3025 0.2185 -0.0903 0.033 Uiso 1 1 calc R . . C19 C 0.17120(10) 0.23017(7) -0.1692(2) 0.0311(3) Uani 1 1 d . . . H19A H 0.1318 0.2533 -0.2604 0.037 Uiso 1 1 calc R . . H19B H 0.1611 0.2458 -0.0599 0.037 Uiso 1 1 calc R . . C20 C 0.15152(11) 0.15917(8) -0.1851(2) 0.0380(4) Uani 1 1 d . . . H20A H 0.1527 0.1457 -0.3015 0.046 Uiso 1 1 calc R . . H20B H 0.1982 0.136 -0.1079 0.046 Uiso 1 1 calc R . . C21 C 0.06553(12) 0.13991(9) -0.1463(3) 0.0425(4) Uani 1 1 d . . . H21A H 0.0185 0.1628 -0.2232 0.051 Uiso 1 1 calc R . . H21B H 0.0642 0.1528 -0.0295 0.051 Uiso 1 1 calc R . . C22 C 0.04880(13) 0.06900(9) -0.1646(3) 0.0471(4) Uani 1 1 d . . . H22A H -0.01 0.0602 -0.1456 0.056 Uiso 1 1 calc R . . H22B H 0.0498 0.0564 -0.2818 0.056 Uiso 1 1 calc R . . C23 C 0.11313(15) 0.02837(10) -0.0452(3) 0.0545(5) Uani 1 1 d . . . H23A H 0.1706 0.0328 -0.0719 0.082 Uiso 1 1 calc R . . H23B H 0.0949 -0.0161 -0.0575 0.082 Uiso 1 1 calc R . . H23C H 0.1155 0.0421 0.0711 0.082 Uiso 1 1 calc R . . N1 N 0.31263(7) 0.48714(5) -0.09183(13) 0.02058(19) Uani 1 1 d . . . N2 N 0.34571(7) 0.51670(5) -0.21319(13) 0.02089(19) Uani 1 1 d . . . N3 N 0.42809(7) 0.37977(5) -0.13817(13) 0.01877(18) Uani 1 1 d . . . Cl1 Cl 0.35822(3) 0.479903(18) 0.29196(4) 0.03184(7) Uani 1 1 d . . . Cl2 Cl 0.45880(2) 0.350955(17) 0.25456(4) 0.02861(7) Uani 1 1 d . . . Pd1 Pd 0.387293(6) 0.424506(4) 0.066691(11) 0.01810(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0295(7) 0.0393(8) 0.0410(8) 0.0043(7) 0.0144(6) 0.0011(6) C2 0.0247(6) 0.0247(6) 0.0247(6) -0.0017(5) 0.0051(5) -0.0004(5) C3 0.0288(7) 0.0238(6) 0.0295(6) 0.0007(5) 0.0027(5) 0.0043(5) C4 0.0318(7) 0.0179(5) 0.0200(5) 0.0002(4) 0.0011(5) 0.0006(5) C5 0.0439(9) 0.0226(6) 0.0254(6) 0.0056(5) 0.0055(6) 0.0037(6) C6 0.0266(6) 0.0201(5) 0.0189(5) 0.0016(4) 0.0070(4) -0.0005(4) C7 0.0289(6) 0.0211(5) 0.0156(4) -0.0009(4) 0.0046(4) 0.0004(5) C8 0.0223(6) 0.0222(5) 0.0216(5) -0.0021(4) 0.0060(4) -0.0012(4) C9 0.0262(6) 0.0289(6) 0.0301(6) -0.0070(5) 0.0095(5) 0.0001(5) C10 0.0277(7) 0.0244(6) 0.0265(6) 0.0002(5) 0.0094(5) 0.0015(5) C11 0.0323(7) 0.0229(6) 0.0312(6) 0.0018(5) 0.0126(5) 0.0023(5) C12 0.0353(8) 0.0304(7) 0.0363(7) 0.0061(6) 0.0127(6) 0.0098(6) C13 0.0304(8) 0.0337(8) 0.0435(9) 0.0005(7) 0.0074(6) 0.0057(6) C14 0.0322(9) 0.0568(12) 0.0619(13) 0.0023(10) 0.0022(8) 0.0058(8) C15 0.0367(10) 0.0611(13) 0.0750(15) -0.0128(12) 0.0109(10) -0.0064(9) C16 0.0257(6) 0.0167(5) 0.0242(5) -0.0029(4) 0.0051(5) -0.0029(4) C17 0.0262(6) 0.0217(5) 0.0275(6) -0.0029(5) 0.0072(5) -0.0031(5) C18 0.0280(7) 0.0241(6) 0.0323(7) -0.0041(5) 0.0080(5) -0.0057(5) C19 0.0307(7) 0.0325(7) 0.0318(7) -0.0035(6) 0.0107(6) -0.0067(6) C20 0.0332(8) 0.0332(8) 0.0498(10) -0.0054(7) 0.0134(7) -0.0085(6) C21 0.0360(9) 0.0428(9) 0.0516(10) 0.0065(8) 0.0159(8) -0.0055(7) C22 0.0438(10) 0.0455(10) 0.0526(11) 0.0075(8) 0.0118(8) -0.0142(8) C23 0.0593(13) 0.0440(10) 0.0607(13) 0.0148(9) 0.0140(10) -0.0081(9) N1 0.0236(5) 0.0200(4) 0.0186(4) 0.0001(4) 0.0054(4) 0.0003(4) N2 0.0271(5) 0.0189(4) 0.0170(4) 0.0014(3) 0.0054(4) 0.0001(4) N3 0.0219(5) 0.0174(4) 0.0175(4) -0.0006(3) 0.0051(4) -0.0004(4) Cl1 0.0416(2) 0.03680(17) 0.01867(13) -0.00581(12) 0.00974(13) 0.00417(15) Cl2 0.03344(17) 0.02921(15) 0.02291(13) 0.00779(12) 0.00528(12) 0.00314(13) Pd1 0.02329(4) 0.01718(4) 0.01428(4) -0.00025(3) 0.00498(3) -0.00152(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.490(2) . ? C1 H1A 0.98 . ? C1 H1B 0.98 . ? C1 H1C 0.98 . ? C2 N1 1.3400(18) . ? C2 C3 1.3936(19) . ? C3 C4 1.379(2) . ? C3 H3 0.95 . ? C4 N2 1.3467(17) . ? C4 C5 1.4856(19) . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 N2 1.4506(17) . ? C6 C7 1.5196(17) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C7 N3 1.4920(16) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 N3 1.5149(17) . ? C8 C9 1.5286(18) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C9 C10 1.522(2) . ? C9 H9A 0.99 . ? C9 H9B 0.99 . ? C10 C11 1.5259(19) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? C11 C12 1.525(2) . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C12 C13 1.515(2) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 C14 1.508(2) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 C15 1.512(3) . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 N3 1.4937(16) . ? C16 C17 1.5199(19) . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? C17 C18 1.5221(19) . ? C17 H17A 0.99 . ? C17 H17B 0.99 . ? C18 C19 1.513(2) . ? C18 H18A 0.99 . ? C18 H18B 0.99 . ? C19 C20 1.529(2) . ? C19 H19A 0.99 . ? C19 H19B 0.99 . ? C20 C21 1.512(2) . ? C20 H20A 0.99 . ? C20 H20B 0.99 . ? C21 C22 1.521(3) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C22 C23 1.514(3) . ? C22 H22A 0.99 . ? C22 H22B 0.99 . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? N1 N2 1.3582(15) . ? N1 Pd1 2.0382(11) . ? N3 Pd1 2.1241(10) . ? Cl1 Pd1 2.2942(3) . ? Cl2 Pd1 2.2987(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 108.88(12) . . ? N1 C2 C1 123.54(13) . . ? C3 C2 C1 127.50(14) . . ? C4 C3 C2 106.80(12) . . ? C4 C3 H3 126.6 . . ? C2 C3 H3 126.6 . . ? N2 C4 C3 106.61(12) . . ? N2 C4 C5 122.79(13) . . ? C3 C4 C5 130.59(13) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 C7 110.05(11) . . ? N2 C6 H6A 109.7 . . ? C7 C6 H6A 109.7 . . ? N2 C6 H6B 109.7 . . ? C7 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? N3 C7 C6 112.87(10) . . ? N3 C7 H7A 109 . . ? C6 C7 H7A 109 . . ? N3 C7 H7B 109 . . ? C6 C7 H7B 109 . . ? H7A C7 H7B 107.8 . . ? N3 C8 C9 116.33(10) . . ? N3 C8 H8A 108.2 . . ? C9 C8 H8A 108.2 . . ? N3 C8 H8B 108.2 . . ? C9 C8 H8B 108.2 . . ? H8A C8 H8B 107.4 . . ? C10 C9 C8 110.03(11) . . ? C10 C9 H9A 109.7 . . ? C8 C9 H9A 109.7 . . ? C10 C9 H9B 109.7 . . ? C8 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? C9 C10 C11 111.71(12) . . ? C9 C10 H10A 109.3 . . ? C11 C10 H10A 109.3 . . ? C9 C10 H10B 109.3 . . ? C11 C10 H10B 109.3 . . ? H10A C10 H10B 107.9 . . ? C12 C11 C10 114.74(13) . . ? C12 C11 H11A 108.6 . . ? C10 C11 H11A 108.6 . . ? C12 C11 H11B 108.6 . . ? C10 C11 H11B 108.6 . . ? H11A C11 H11B 107.6 . . ? C13 C12 C11 114.12(12) . . ? C13 C12 H12A 108.7 . . ? C11 C12 H12A 108.7 . . ? C13 C12 H12B 108.7 . . ? C11 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? C14 C13 C12 114.39(15) . . ? C14 C13 H13A 108.7 . . ? C12 C13 H13A 108.7 . . ? C14 C13 H13B 108.7 . . ? C12 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? C13 C14 C15 113.24(17) . . ? C13 C14 H14A 108.9 . . ? C15 C14 H14A 108.9 . . ? C13 C14 H14B 108.9 . . ? C15 C14 H14B 108.9 . . ? H14A C14 H14B 107.7 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C16 C17 115.49(10) . . ? N3 C16 H16A 108.4 . . ? C17 C16 H16A 108.4 . . ? N3 C16 H16B 108.4 . . ? C17 C16 H16B 108.4 . . ? H16A C16 H16B 107.5 . . ? C16 C17 C18 108.43(11) . . ? C16 C17 H17A 110 . . ? C18 C17 H17A 110 . . ? C16 C17 H17B 110 . . ? C18 C17 H17B 110 . . ? H17A C17 H17B 108.4 . . ? C19 C18 C17 115.73(12) . . ? C19 C18 H18A 108.3 . . ? C17 C18 H18A 108.3 . . ? C19 C18 H18B 108.3 . . ? C17 C18 H18B 108.3 . . ? H18A C18 H18B 107.4 . . ? C18 C19 C20 110.57(13) . . ? C18 C19 H19A 109.5 . . ? C20 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? C21 C20 C19 114.91(15) . . ? C21 C20 H20A 108.5 . . ? C19 C20 H20A 108.5 . . ? C21 C20 H20B 108.5 . . ? C19 C20 H20B 108.5 . . ? H20A C20 H20B 107.5 . . ? C20 C21 C22 112.91(16) . . ? C20 C21 H21A 109 . . ? C22 C21 H21A 109 . . ? C20 C21 H21B 109 . . ? C22 C21 H21B 109 . . ? H21A C21 H21B 107.8 . . ? C23 C22 C21 114.51(17) . . ? C23 C22 H22A 108.6 . . ? C21 C22 H22A 108.6 . . ? C23 C22 H22B 108.6 . . ? C21 C22 H22B 108.6 . . ? H22A C22 H22B 107.6 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C2 N1 N2 106.90(10) . . ? C2 N1 Pd1 132.38(9) . . ? N2 N1 Pd1 119.69(8) . . ? C4 N2 N1 110.80(11) . . ? C4 N2 C6 129.20(11) . . ? N1 N2 C6 118.81(10) . . ? C7 N3 C16 110.25(10) . . ? C7 N3 C8 108.32(10) . . ? C16 N3 C8 108.95(10) . . ? C7 N3 Pd1 111.72(7) . . ? C16 N3 Pd1 109.01(7) . . ? C8 N3 Pd1 108.54(7) . . ? N1 Pd1 N3 91.41(4) . . ? N1 Pd1 Cl1 89.22(3) . . ? N3 Pd1 Cl1 173.10(3) . . ? N1 Pd1 Cl2 174.12(3) . . ? N3 Pd1 Cl2 91.79(3) . . ? Cl1 Pd1 Cl2 88.186(14) . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF