# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name _publ_author_address J.Bogojeski ; Departament of Chemistry, Faculty of Science University of Kragujevac R. Domanovica 12 P O Box 60 34000 Kragujevac Serbia ; R.Jelic ; Faculty of Medicine University of Kragujevac S. Markovica 69 34000 Kragujevac Serbia ; D.Petrovic ; Institut f\"ur Anorganische und Analytische Chemie Technische Universit\"at Braunschweig Postfach 3329 38023 Braunschweig Germany ; E.Herdtweck ; Department Chemie Technische Universit\"at M\"unchen Lichtenbergstr. 4 85747 Garching Germany ; P.G.Jones ; Institut f\"ur Anorganische und Analytische Chemie Technische Universit\"at Braunschweig Postfach 3329 38023 Braunschweig Germany ; M.Tamm ; Institut f\"ur Anorganische und Analytische Chemie Technische Universit\"at Braunschweig Postfach 3329 38023 Braunschweig Germany ; ; Z.D.Bugarcic ; ; Departament of Chemistry, Faculty of Science University of Kragujevac R. Domanovica 12 P O Box 60 34000 Kragujevac Serbia ; _publ_contact_author_name 'Peter G. Jones' _publ_contact_author_address ; Institut f\"ur Anorganische und Analytische Chemie Technische Universit\"at Braunschweig Postfach 3329 38023 Braunschweig Germany ; _publ_contact_author_phone '049 531 391-5382' _publ_contact_author_fax '049 531 391-5387' _publ_contact_author_email p.jones@tu-bs.de _publ_section_title ; Equilibrium and kinetic study on the reactions of Pd(II) bis(imidazolin-2- imine) complexes with biologically relevant nucleophiles. ; # Attachment 'Z.Bugarcic.cif' #============================================================================== #TrackingRef 'Z.Bugarcic.cif' #============================================================================== # 3. TITLE AND AUTHOR LIST #============================================================================= # cif data for "jov" (compound 1) #============================================================================= data_jov3 _database_code_depnum_ccdc_archive 'CCDC 808222' #TrackingRef 'Z.Bugarcic.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H53 Cl2 N7 O5 Pd' _chemical_formula_weight 781.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.0962(2) _cell_length_b 13.0994(3) _cell_length_c 29.6124(6) _cell_angle_alpha 90.00 _cell_angle_beta 96.852(2) _cell_angle_gamma 90.00 _cell_volume 3503.26(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 16132 _cell_measurement_theta_min 2.7311 _cell_measurement_theta_max 30.6755 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 0.731 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.95131 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur S' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 16.1057 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60455 _diffrn_reflns_av_R_equivalents 0.0637 _diffrn_reflns_av_sigmaI/netI 0.0659 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 28.28 _reflns_number_total 8568 _reflns_number_gt 5679 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One distorted molecule of ethanol, which could not be refined satisfactorily, was removed using the program SQUEEZE (A.L. Spek, University of Utrecht, Netherlands). The quoted formula and derived parameters are based on one molecule of ethanol per asymmetric unit. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.500 0.000 122.4 11.2 2 0.500 0.000 0.500 122.4 10.7 _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^)+(0.0524P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'rigid methyls, others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8568 _refine_ls_number_parameters 400 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0878 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1055 _refine_ls_wR_factor_gt 0.0960 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.36518(2) 0.24959(2) 0.123822(8) 0.01380(7) Uani 1 1 d . . . Cl1 Cl 0.24520(8) 0.18785(7) 0.18332(3) 0.02125(19) Uani 1 1 d . . . Cl2 Cl 0.83442(10) 0.70638(8) 0.10456(3) 0.0321(2) Uani 1 1 d . . . N1 N 0.4505(2) 0.3082(2) 0.07252(8) 0.0125(5) Uani 1 1 d . . . N2 N 0.2863(2) 0.1473(2) 0.07497(8) 0.0118(5) Uani 1 1 d . . . N3 N 0.4944(3) 0.3588(2) 0.15732(9) 0.0176(6) Uani 1 1 d . . . N4 N 0.0392(3) 0.0715(2) 0.07970(9) 0.0160(6) Uani 1 1 d . . . N5 N 0.2373(3) -0.0225(2) 0.09739(8) 0.0142(6) Uani 1 1 d . . . N6 N 0.3937(3) 0.4515(2) 0.21847(9) 0.0209(6) Uani 1 1 d . . . N7 N 0.5899(3) 0.3561(2) 0.23660(9) 0.0217(7) Uani 1 1 d . . . O1 O 0.8798(4) 0.6911(4) 0.06127(12) 0.0903(14) Uani 1 1 d . . . O2 O 0.7320(4) 0.6301(3) 0.11256(13) 0.0740(12) Uani 1 1 d . . . O3 O 0.7641(3) 0.8029(2) 0.10423(13) 0.0572(10) Uani 1 1 d . . . O4 O 0.9594(3) 0.7057(3) 0.13821(11) 0.0517(8) Uani 1 1 d . . . C1 C 0.4146(3) 0.2670(2) 0.03092(10) 0.0122(7) Uani 1 1 d . . . C2 C 0.4802(3) 0.3027(3) -0.00581(10) 0.0163(7) Uani 1 1 d . . . H2 H 0.4546 0.2753 -0.0354 0.020 Uiso 1 1 calc R . . C3 C 0.5846(3) 0.3800(3) 0.00189(11) 0.0187(7) Uani 1 1 d . . . H3 H 0.6344 0.4034 -0.0226 0.022 Uiso 1 1 calc R . . C4 C 0.6177(3) 0.4236(3) 0.04429(11) 0.0183(7) Uani 1 1 d . . . H4 H 0.6874 0.4777 0.0490 0.022 Uiso 1 1 calc R . . C5 C 0.5464(3) 0.3863(3) 0.08008(11) 0.0180(7) Uani 1 1 d . . . C6 C 0.2922(3) 0.1885(3) 0.02907(10) 0.0160(7) Uani 1 1 d . . . H6A H 0.1962 0.2205 0.0178 0.019 Uiso 1 1 calc R . . H6B H 0.3113 0.1327 0.0080 0.019 Uiso 1 1 calc R . . C7 C 0.5599(4) 0.4299(3) 0.12710(11) 0.0250(8) Uani 1 1 d . . . H7A H 0.6656 0.4412 0.1383 0.030 Uiso 1 1 calc R . . H7B H 0.5081 0.4964 0.1267 0.030 Uiso 1 1 calc R . . C8 C 0.1925(3) 0.0719(3) 0.08198(10) 0.0137(6) Uani 1 1 d . . . C9 C -0.0042(4) -0.0219(3) 0.09400(12) 0.0232(8) Uani 1 1 d . . . H9 H -0.1037 -0.0422 0.0956 0.028 Uiso 1 1 calc R . . C10 C 0.1157(3) -0.0801(3) 0.10534(11) 0.0216(8) Uani 1 1 d . . . H10 H 0.1168 -0.1480 0.1167 0.026 Uiso 1 1 calc R . . C11 C 0.4911(3) 0.3885(3) 0.20098(11) 0.0177(7) Uani 1 1 d . . . C12 C 0.4326(4) 0.4587(3) 0.26495(11) 0.0265(8) Uani 1 1 d . . . H12 H 0.3834 0.4984 0.2854 0.032 Uiso 1 1 calc R . . C13 C 0.5520(4) 0.3997(3) 0.27592(11) 0.0286(9) Uani 1 1 d . . . H13 H 0.6018 0.3896 0.3057 0.034 Uiso 1 1 calc R . . C14 C -0.0674(3) 0.1548(3) 0.06293(12) 0.0220(8) Uani 1 1 d . . . C15 C -0.2146(3) 0.1338(3) 0.08185(15) 0.0368(10) Uani 1 1 d . . . H15A H -0.2574 0.0700 0.0690 0.055 Uiso 1 1 calc R . . H15B H -0.2834 0.1901 0.0736 0.055 Uiso 1 1 calc R . . H15C H -0.1968 0.1278 0.1150 0.055 Uiso 1 1 calc R . . C16 C -0.0934(3) 0.1497(3) 0.01104(12) 0.0304(9) Uani 1 1 d . . . H16A H 0.0002 0.1618 -0.0014 0.046 Uiso 1 1 calc R . . H16B H -0.1655 0.2020 -0.0004 0.046 Uiso 1 1 calc R . . H16C H -0.1317 0.0821 0.0016 0.046 Uiso 1 1 calc R . . C17 C -0.0128(3) 0.2593(3) 0.08042(12) 0.0236(8) Uani 1 1 d . . . H17A H 0.0094 0.2571 0.1136 0.035 Uiso 1 1 calc R . . H17B H -0.0897 0.3105 0.0719 0.035 Uiso 1 1 calc R . . H17C H 0.0770 0.2775 0.0670 0.035 Uiso 1 1 calc R . . C18 C 0.3942(3) -0.0633(3) 0.10275(10) 0.0157(7) Uani 1 1 d . . . C19 C 0.4877(3) -0.0050(3) 0.14085(11) 0.0222(8) Uani 1 1 d . . . H19A H 0.4915 0.0673 0.1327 0.033 Uiso 1 1 calc R . . H19B H 0.5883 -0.0330 0.1450 0.033 Uiso 1 1 calc R . . H19C H 0.4431 -0.0121 0.1692 0.033 Uiso 1 1 calc R . . C20 C 0.3911(4) -0.1759(3) 0.11519(13) 0.0294(9) Uani 1 1 d . . . H20A H 0.3526 -0.1836 0.1445 0.044 Uiso 1 1 calc R . . H20B H 0.4916 -0.2038 0.1173 0.044 Uiso 1 1 calc R . . H20C H 0.3270 -0.2128 0.0917 0.044 Uiso 1 1 calc R . . C21 C 0.4581(3) -0.0517(3) 0.05764(11) 0.0166(7) Uani 1 1 d . . . H21A H 0.3932 -0.0860 0.0335 0.025 Uiso 1 1 calc R . . H21B H 0.5568 -0.0827 0.0602 0.025 Uiso 1 1 calc R . . H21C H 0.4654 0.0209 0.0503 0.025 Uiso 1 1 calc R . . C22 C 0.2612(4) 0.5098(3) 0.19602(12) 0.0228(8) Uani 1 1 d . . . C23 C 0.2060(4) 0.4723(3) 0.14875(13) 0.0406(11) Uani 1 1 d . . . H23A H 0.2820 0.4844 0.1285 0.061 Uiso 1 1 calc R . . H23B H 0.1154 0.5091 0.1373 0.061 Uiso 1 1 calc R . . H23C H 0.1850 0.3990 0.1498 0.061 Uiso 1 1 calc R . . C24 C 0.1351(4) 0.4928(3) 0.22544(15) 0.0378(10) Uani 1 1 d . . . H24A H 0.0442 0.5245 0.2107 0.057 Uiso 1 1 calc R . . H24B H 0.1618 0.5237 0.2554 0.057 Uiso 1 1 calc R . . H24C H 0.1189 0.4194 0.2289 0.057 Uiso 1 1 calc R . . C25 C 0.3048(4) 0.6220(3) 0.19573(13) 0.0311(9) Uani 1 1 d . . . H25A H 0.3874 0.6308 0.1776 0.047 Uiso 1 1 calc R . . H25B H 0.3351 0.6449 0.2270 0.047 Uiso 1 1 calc R . . H25C H 0.2201 0.6627 0.1824 0.047 Uiso 1 1 calc R . . C26 C 0.7135(4) 0.2795(3) 0.23547(12) 0.0264(9) Uani 1 1 d . . . C27 C 0.8003(4) 0.2993(5) 0.19506(16) 0.0544(14) Uani 1 1 d . . . H27A H 0.8868 0.2541 0.1972 0.082 Uiso 1 1 calc R . . H27B H 0.8331 0.3706 0.1956 0.082 Uiso 1 1 calc R . . H27C H 0.7366 0.2857 0.1666 0.082 Uiso 1 1 calc R . . C28 C 0.8234(5) 0.2938(4) 0.27787(16) 0.0575(14) Uani 1 1 d . . . H28A H 0.7757 0.2766 0.3049 0.086 Uiso 1 1 calc R . . H28B H 0.8565 0.3651 0.2798 0.086 Uiso 1 1 calc R . . H28C H 0.9089 0.2490 0.2762 0.086 Uiso 1 1 calc R . . C29 C 0.6476(4) 0.1765(4) 0.2324(2) 0.0624(16) Uani 1 1 d . . . H29A H 0.5948 0.1644 0.2589 0.094 Uiso 1 1 calc R . . H29B H 0.7261 0.1255 0.2318 0.094 Uiso 1 1 calc R . . H29C H 0.5780 0.1711 0.2046 0.094 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.01391(11) 0.01369(12) 0.01345(11) 0.00045(12) 0.00015(7) -0.00457(11) Cl1 0.0236(4) 0.0232(5) 0.0173(4) 0.0027(3) 0.0043(3) -0.0059(3) Cl2 0.0350(5) 0.0213(5) 0.0363(5) 0.0080(4) -0.0111(4) -0.0060(4) N1 0.0124(12) 0.0099(16) 0.0149(13) 0.0037(11) -0.0001(10) -0.0024(10) N2 0.0134(12) 0.0098(15) 0.0117(13) 0.0015(10) -0.0013(10) -0.0042(10) N3 0.0209(13) 0.0194(17) 0.0128(13) 0.0004(12) 0.0030(10) -0.0097(12) N4 0.0098(12) 0.0145(16) 0.0236(14) -0.0037(12) 0.0013(10) -0.0056(10) N5 0.0132(12) 0.0120(15) 0.0178(14) 0.0003(11) 0.0041(10) -0.0036(10) N6 0.0216(14) 0.0217(18) 0.0184(14) -0.0044(12) -0.0016(11) 0.0018(12) N7 0.0195(14) 0.0290(19) 0.0155(14) -0.0061(12) -0.0025(11) 0.0006(12) O1 0.104(3) 0.115(4) 0.050(2) 0.002(3) 0.004(2) 0.039(3) O2 0.083(2) 0.042(2) 0.088(3) 0.026(2) -0.027(2) -0.0464(19) O3 0.0305(15) 0.0205(19) 0.121(3) 0.0202(19) 0.0105(17) 0.0008(13) O4 0.0443(17) 0.048(2) 0.055(2) 0.0103(17) -0.0268(14) -0.0070(15) C1 0.0118(13) 0.0067(19) 0.0173(15) 0.0006(12) -0.0015(11) 0.0035(11) C2 0.0199(15) 0.0141(19) 0.0144(15) 0.0013(13) 0.0004(12) 0.0026(13) C3 0.0186(16) 0.018(2) 0.0202(17) 0.0092(14) 0.0057(13) 0.0002(13) C4 0.0157(15) 0.0162(19) 0.0232(18) 0.0048(14) 0.0034(13) -0.0049(13) C5 0.0167(15) 0.017(2) 0.0197(17) 0.0025(14) -0.0010(12) -0.0029(13) C6 0.0154(14) 0.016(2) 0.0157(15) -0.0001(13) -0.0024(12) -0.0041(13) C7 0.0332(19) 0.022(2) 0.0193(18) -0.0020(15) 0.0022(14) -0.0122(16) C8 0.0135(14) 0.0158(19) 0.0116(15) -0.0018(13) 0.0004(11) -0.0029(12) C9 0.0197(16) 0.021(2) 0.0299(19) -0.0062(16) 0.0070(14) -0.0110(14) C10 0.0278(18) 0.014(2) 0.0255(18) -0.0025(14) 0.0116(14) -0.0112(14) C11 0.0164(15) 0.018(2) 0.0180(16) -0.0019(14) -0.0019(12) -0.0069(13) C12 0.0299(19) 0.033(2) 0.0169(17) -0.0070(16) 0.0030(14) -0.0019(16) C13 0.0337(19) 0.040(3) 0.0114(16) -0.0066(16) -0.0016(14) 0.0032(17) C14 0.0121(15) 0.023(2) 0.0300(19) -0.0060(15) -0.0003(13) 0.0008(14) C15 0.0140(17) 0.032(3) 0.064(3) -0.007(2) 0.0052(17) -0.0003(16) C16 0.0176(17) 0.032(2) 0.038(2) -0.0064(18) -0.0110(15) 0.0009(15) C17 0.0135(14) 0.020(2) 0.0364(19) -0.0062(17) -0.0014(13) 0.0019(15) C18 0.0174(15) 0.0124(19) 0.0172(17) 0.0008(13) 0.0013(12) 0.0012(12) C19 0.0229(17) 0.022(2) 0.0196(17) 0.0000(15) -0.0038(13) 0.0032(14) C20 0.034(2) 0.017(2) 0.039(2) 0.0076(16) 0.0083(17) 0.0039(16) C21 0.0138(15) 0.0139(19) 0.0218(17) -0.0014(14) 0.0004(12) 0.0000(13) C22 0.0251(17) 0.014(2) 0.0269(19) -0.0073(15) -0.0046(14) 0.0039(14) C23 0.043(2) 0.034(3) 0.038(2) -0.013(2) -0.0214(18) 0.0156(19) C24 0.0233(19) 0.033(3) 0.058(3) 0.001(2) 0.0066(18) -0.0002(17) C25 0.035(2) 0.020(2) 0.037(2) 0.0017(17) 0.0000(17) -0.0022(16) C26 0.0187(16) 0.030(2) 0.0274(19) -0.0047(15) -0.0088(14) 0.0051(14) C27 0.030(2) 0.078(4) 0.057(3) -0.001(3) 0.012(2) 0.017(2) C28 0.039(2) 0.075(4) 0.051(3) -0.024(3) -0.023(2) 0.026(2) C29 0.030(2) 0.031(3) 0.120(5) 0.007(3) -0.015(3) 0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd N1 1.944(2) . ? Pd N3 2.034(3) . ? Pd N2 2.038(2) . ? Pd Cl1 2.3256(8) . ? Cl2 O2 1.405(3) . ? Cl2 O1 1.407(4) . ? Cl2 O3 1.416(3) . ? Cl2 O4 1.419(3) . ? N1 C5 1.346(4) . ? N1 C1 1.349(4) . ? N2 C8 1.339(4) . ? N2 C6 1.469(4) . ? N3 C11 1.354(4) . ? N3 C7 1.466(4) . ? N4 C9 1.368(4) . ? N4 C8 1.387(4) . ? N4 C14 1.504(4) . ? N5 C8 1.364(4) . ? N5 C10 1.382(4) . ? N5 C18 1.514(4) . ? N6 C11 1.358(4) . ? N6 C12 1.383(4) . ? N6 C22 1.513(4) . ? N7 C11 1.369(4) . ? N7 C13 1.377(4) . ? N7 C26 1.510(4) . ? C1 C2 1.383(4) . ? C1 C6 1.511(4) . ? C2 C3 1.388(4) . ? C3 C4 1.379(5) . ? C4 C5 1.395(4) . ? C5 C7 1.496(5) . ? C9 C10 1.340(5) . ? C12 C13 1.342(5) . ? C14 C17 1.526(5) . ? C14 C16 1.528(5) . ? C14 C15 1.537(4) . ? C18 C20 1.521(5) . ? C18 C21 1.527(4) . ? C18 C19 1.533(4) . ? C22 C23 1.512(5) . ? C22 C25 1.523(5) . ? C22 C24 1.537(5) . ? C26 C29 1.476(6) . ? C26 C28 1.521(5) . ? C26 C27 1.533(5) . ? 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 Pd N3 80.90(10) . . ? N1 Pd N2 81.05(10) . . ? N3 Pd N2 160.51(9) . . ? N1 Pd Cl1 175.08(7) . . ? N3 Pd Cl1 99.86(7) . . ? N2 Pd Cl1 98.74(7) . . ? O2 Cl2 O1 109.0(3) . . ? O2 Cl2 O3 109.1(2) . . ? O1 Cl2 O3 107.6(2) . . ? O2 Cl2 O4 111.6(2) . . ? O1 Cl2 O4 110.0(2) . . ? O3 Cl2 O4 109.5(2) . . ? C5 N1 C1 122.5(3) . . ? C5 N1 Pd 118.8(2) . . ? C1 N1 Pd 118.7(2) . . ? C8 N2 C6 120.6(2) . . ? C8 N2 Pd 123.52(19) . . ? C6 N2 Pd 111.52(19) . . ? C11 N3 C7 117.2(3) . . ? C11 N3 Pd 126.2(2) . . ? C7 N3 Pd 113.7(2) . . ? C9 N4 C8 108.3(3) . . ? C9 N4 C14 123.5(3) . . ? C8 N4 C14 128.2(3) . . ? C8 N5 C10 109.8(3) . . ? C8 N5 C18 126.6(2) . . ? C10 N5 C18 123.6(3) . . ? C11 N6 C12 108.7(3) . . ? C11 N6 C22 131.4(3) . . ? C12 N6 C22 119.9(3) . . ? C11 N7 C13 108.4(3) . . ? C11 N7 C26 127.6(3) . . ? C13 N7 C26 123.8(3) . . ? N1 C1 C2 120.1(3) . . ? N1 C1 C6 113.7(3) . . ? C2 C1 C6 125.9(3) . . ? C1 C2 C3 118.0(3) . . ? C4 C3 C2 121.5(3) . . ? C3 C4 C5 118.4(3) . . ? N1 C5 C4 119.4(3) . . ? N1 C5 C7 115.1(3) . . ? C4 C5 C7 125.4(3) . . ? N2 C6 C1 108.9(2) . . ? N3 C7 C5 109.4(3) . . ? N2 C8 N5 123.4(3) . . ? N2 C8 N4 130.6(3) . . ? N5 C8 N4 105.8(3) . . ? C10 C9 N4 109.3(3) . . ? C9 C10 N5 106.9(3) . . ? N3 C11 N6 128.9(3) . . ? N3 C11 N7 124.0(3) . . ? N6 C11 N7 107.0(3) . . ? C13 C12 N6 107.8(3) . . ? C12 C13 N7 108.1(3) . . ? N4 C14 C17 111.6(3) . . ? N4 C14 C16 108.5(3) . . ? C17 C14 C16 112.7(3) . . ? N4 C14 C15 107.8(3) . . ? C17 C14 C15 107.4(3) . . ? C16 C14 C15 108.8(3) . . ? N5 C18 C20 108.8(2) . . ? N5 C18 C21 109.0(2) . . ? C20 C18 C21 109.2(3) . . ? N5 C18 C19 109.5(3) . . ? C20 C18 C19 109.3(3) . . ? C21 C18 C19 111.0(3) . . ? C23 C22 N6 113.7(3) . . ? C23 C22 C25 111.5(3) . . ? N6 C22 C25 107.2(3) . . ? C23 C22 C24 106.9(3) . . ? N6 C22 C24 106.7(3) . . ? C25 C22 C24 110.8(3) . . ? C29 C26 N7 108.1(3) . . ? C29 C26 C28 112.7(4) . . ? N7 C26 C28 108.5(3) . . ? C29 C26 C27 110.5(4) . . ? N7 C26 C27 111.1(3) . . ? C28 C26 C27 105.9(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Pd N1 C5 -0.1(2) . . . . ? N2 Pd N1 C5 -172.7(2) . . . . ? Cl1 Pd N1 C5 99.3(9) . . . . ? N3 Pd N1 C1 177.9(2) . . . . ? N2 Pd N1 C1 5.3(2) . . . . ? Cl1 Pd N1 C1 -82.7(10) . . . . ? N1 Pd N2 C8 -174.8(2) . . . . ? N3 Pd N2 C8 162.8(3) . . . . ? Cl1 Pd N2 C8 0.2(2) . . . . ? N1 Pd N2 C6 -18.28(19) . . . . ? N3 Pd N2 C6 -40.6(4) . . . . ? Cl1 Pd N2 C6 156.75(17) . . . . ? N1 Pd N3 C11 169.1(3) . . . . ? N2 Pd N3 C11 -168.5(3) . . . . ? Cl1 Pd N3 C11 -6.0(3) . . . . ? N1 Pd N3 C7 8.9(2) . . . . ? N2 Pd N3 C7 31.3(4) . . . . ? Cl1 Pd N3 C7 -166.2(2) . . . . ? C5 N1 C1 C2 1.9(4) . . . . ? Pd N1 C1 C2 -176.0(2) . . . . ? C5 N1 C1 C6 -173.4(3) . . . . ? Pd N1 C1 C6 8.7(3) . . . . ? N1 C1 C2 C3 1.2(4) . . . . ? C6 C1 C2 C3 175.8(3) . . . . ? C1 C2 C3 C4 -3.0(5) . . . . ? C2 C3 C4 C5 1.7(5) . . . . ? C1 N1 C5 C4 -3.2(5) . . . . ? Pd N1 C5 C4 174.8(2) . . . . ? C1 N1 C5 C7 173.4(3) . . . . ? Pd N1 C5 C7 -8.7(4) . . . . ? C3 C4 C5 N1 1.3(5) . . . . ? C3 C4 C5 C7 -174.9(3) . . . . ? C8 N2 C6 C1 -176.0(3) . . . . ? Pd N2 C6 C1 26.6(3) . . . . ? N1 C1 C6 N2 -23.1(4) . . . . ? C2 C1 C6 N2 161.9(3) . . . . ? C11 N3 C7 C5 -177.1(3) . . . . ? Pd N3 C7 C5 -15.0(3) . . . . ? N1 C5 C7 N3 15.2(4) . . . . ? C4 C5 C7 N3 -168.5(3) . . . . ? C6 N2 C8 N5 116.5(3) . . . . ? Pd N2 C8 N5 -89.0(3) . . . . ? C6 N2 C8 N4 -69.6(4) . . . . ? Pd N2 C8 N4 84.9(4) . . . . ? C10 N5 C8 N2 174.2(3) . . . . ? C18 N5 C8 N2 -9.2(5) . . . . ? C10 N5 C8 N4 -1.0(3) . . . . ? C18 N5 C8 N4 175.5(3) . . . . ? C9 N4 C8 N2 -174.3(3) . . . . ? C14 N4 C8 N2 8.1(5) . . . . ? C9 N4 C8 N5 0.5(3) . . . . ? C14 N4 C8 N5 -177.1(3) . . . . ? C8 N4 C9 C10 0.2(4) . . . . ? C14 N4 C9 C10 177.9(3) . . . . ? N4 C9 C10 N5 -0.8(4) . . . . ? C8 N5 C10 C9 1.1(4) . . . . ? C18 N5 C10 C9 -175.5(3) . . . . ? C7 N3 C11 N6 80.9(4) . . . . ? Pd N3 C11 N6 -78.7(4) . . . . ? C7 N3 C11 N7 -100.5(4) . . . . ? Pd N3 C11 N7 99.9(3) . . . . ? C12 N6 C11 N3 179.2(3) . . . . ? C22 N6 C11 N3 -1.1(6) . . . . ? C12 N6 C11 N7 0.3(4) . . . . ? C22 N6 C11 N7 -179.9(3) . . . . ? C13 N7 C11 N3 -178.8(3) . . . . ? C26 N7 C11 N3 -3.4(5) . . . . ? C13 N7 C11 N6 0.1(4) . . . . ? C26 N7 C11 N6 175.5(3) . . . . ? C11 N6 C12 C13 -0.6(4) . . . . ? C22 N6 C12 C13 179.6(3) . . . . ? N6 C12 C13 N7 0.7(4) . . . . ? C11 N7 C13 C12 -0.5(4) . . . . ? C26 N7 C13 C12 -176.1(3) . . . . ? C9 N4 C14 C17 139.4(3) . . . . ? C8 N4 C14 C17 -43.4(4) . . . . ? C9 N4 C14 C16 -95.9(4) . . . . ? C8 N4 C14 C16 81.3(4) . . . . ? C9 N4 C14 C15 21.7(4) . . . . ? C8 N4 C14 C15 -161.1(3) . . . . ? C8 N5 C18 C20 -172.9(3) . . . . ? C10 N5 C18 C20 3.2(4) . . . . ? C8 N5 C18 C21 -53.9(4) . . . . ? C10 N5 C18 C21 122.2(3) . . . . ? C8 N5 C18 C19 67.7(4) . . . . ? C10 N5 C18 C19 -116.2(3) . . . . ? C11 N6 C22 C23 16.9(5) . . . . ? C12 N6 C22 C23 -163.4(3) . . . . ? C11 N6 C22 C25 -106.8(4) . . . . ? C12 N6 C22 C25 72.9(4) . . . . ? C11 N6 C22 C24 134.5(4) . . . . ? C12 N6 C22 C24 -45.8(4) . . . . ? C11 N7 C26 C29 -76.3(5) . . . . ? C13 N7 C26 C29 98.5(4) . . . . ? C11 N7 C26 C28 161.2(4) . . . . ? C13 N7 C26 C28 -24.0(5) . . . . ? C11 N7 C26 C27 45.1(5) . . . . ? C13 N7 C26 C27 -140.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.734 _refine_diff_density_min -1.118 _refine_diff_density_rms 0.089 #============================================================================= # end of cif data for "jov3" (compound 1) #============================================================================= #============================================================================= # cif data for "pete" (compound 2) #============================================================================= data_pete _database_code_depnum_ccdc_archive 'CCDC 808223' #TrackingRef 'Z.Bugarcic.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_formula_moiety 'C24 H44 Cl2 N6 Pd' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H44 Cl2 N6 Pd' _chemical_formula_weight 593.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=================================================================== # CRYSTAL DATA #=================================================================== _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 8.9184(1) _cell_length_b 10.6686(2) _cell_length_c 15.6865(2) _cell_angle_alpha 102.2305(7) _cell_angle_beta 95.6647(8) _cell_angle_gamma 104.1218(7) _cell_volume 1396.64(3) _cell_formula_units_Z 2 _cell_measurement_temperature 143(1) _cell_measurement_reflns_used 4777 _cell_measurement_theta_min 2.92 _cell_measurement_theta_max 25.33 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.412 _exptl_crystal_density_method none _exptl_crystal_F_000 620 _exptl_absorpt_coefficient_mu 0.879 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.579 _exptl_absorpt_correction_T_max 0.926 _exptl_absorpt_process_details ; applied during scaling procedure source: (Otwinowsky, 1997) ; _exptl_special_details ; Diffractometer operator E. Herdtweck exposure_time 300 s per image exposure_phi_range 1-360 exposure_delta_phi 2.0 exposure_sum_images 180 ; _publ_section_exptl_prep ; The crystal was fixed in a capillary with perfluorinated ether and transferred to the diffractometer. ; _publ_section_exptl_refinement ; straight forward after integration and scaling source: (Otwinowsky, 1997) Hydrogen atoms calculated in ideal positions (riding model). ; #=================================================================== # EXPERIMENTAL DATA #=================================================================== _diffrn_ambient_temperature 143(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'NONIUS FR 590 sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'one-circle diffractometer' _diffrn_measurement_device_type 'DIP2020 (Nonius)' _diffrn_measurement_method 'phi-rotation ' _diffrn_detector 'image plate' _diffrn_detector_area_resol_mean 67 _diffrn_standards_decay_% 0 # number of measured reflections (redundant set) _diffrn_reflns_number 18974 _diffrn_reflns_av_R_equivalents 0.029 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 25.33 _reflns_number_total 4786 _reflns_number_gt 4762 # number of observed reflections (> n sig(I)) _reflns_threshold_expression I>2\s(I) _computing_data_collection 'DIP2020 (Nonius, 1997)' _computing_cell_refinement 'DIP2020 (Otwinowsky, 1997)' _computing_data_reduction 'DIP2020 (Otwinowsky, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2010)' _computing_publication_material 'PLATON (Spek, 2010)' #=================================================================== # REFINEMENT DATA #=================================================================== _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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 sigma _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0491P)^2^+1.0609P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 4786 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0309 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0806 _refine_ls_wR_factor_gt 0.0805 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 25.33 _diffrn_measured_fraction_theta_full 0.936 _refine_diff_density_max 0.386 _refine_diff_density_min -0.865 _refine_diff_density_rms 0.081 #=================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS #=================================================================== loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Pd Pd Uani 0.21573(2) 0.02897(1) 0.24430(1) 1.000 0.0189(1) . . Cl1 Cl Uani 0.19197(7) -0.13079(6) 0.32707(4) 1.000 0.0311(2) . . Cl2 Cl Uani -0.05058(6) 0.01830(6) 0.23058(4) 1.000 0.0301(2) . . N1 N Uani 0.4510(2) 0.06123(19) 0.25052(13) 1.000 0.0229(5) . . N2 N Uani 0.2532(2) 0.17039(18) 0.17282(13) 1.000 0.0220(5) . . N3 N Uani 0.5352(2) -0.14416(18) 0.23180(12) 1.000 0.0222(5) . . N4 N Uani 0.6286(2) 0.00956(19) 0.35354(13) 1.000 0.0232(5) . . N5 N Uani 0.1820(2) 0.35205(18) 0.26969(12) 1.000 0.0239(5) . . N6 N Uani 0.0593(2) 0.27877(17) 0.13423(12) 1.000 0.0217(5) . . C1 C Uani 0.4965(3) 0.1113(2) 0.17367(16) 1.000 0.0253(7) . . C2 C Uani 0.4209(3) 0.2239(2) 0.17174(16) 1.000 0.0248(6) . . C3 C Uani 0.5309(3) -0.0212(2) 0.27595(15) 1.000 0.0217(6) . . C4 C Uani 0.6398(3) -0.1888(2) 0.28210(16) 1.000 0.0245(6) . . C5 C Uani 0.6971(3) -0.0930(2) 0.35739(16) 1.000 0.0248(6) . . C6 C Uani 0.6993(3) -0.3069(3) 0.24875(19) 1.000 0.0340(8) . . C7 C Uani 0.8274(3) -0.0821(3) 0.42853(17) 1.000 0.0338(8) . . C8 C Uani 0.4301(3) -0.2181(2) 0.14811(15) 1.000 0.0273(7) . . C9 C Uani 0.3239(3) -0.3489(3) 0.15712(19) 1.000 0.0369(8) . . C10 C Uani 0.5208(3) -0.2355(3) 0.07192(18) 1.000 0.0405(9) . . C11 C Uani 0.6665(3) 0.1368(2) 0.42221(17) 1.000 0.0317(7) . . C12 C Uani 0.5236(3) 0.1582(3) 0.46118(17) 1.000 0.0366(8) . . C13 C Uani 0.7501(3) 0.2521(3) 0.3865(2) 1.000 0.0421(8) . . C14 C Uani 0.1721(3) 0.2627(2) 0.19161(14) 1.000 0.0214(6) . . C15 C Uani 0.0719(3) 0.4234(2) 0.26086(16) 1.000 0.0268(7) . . C16 C Uani -0.0046(3) 0.3777(2) 0.17635(16) 1.000 0.0252(7) . . C17 C Uani 0.0485(4) 0.5312(2) 0.33221(18) 1.000 0.0372(8) . . C18 C Uani -0.1330(3) 0.4232(3) 0.13458(18) 1.000 0.0350(8) . . C19 C Uani 0.2885(3) 0.3586(2) 0.34998(15) 1.000 0.0282(7) . . C20 C Uani 0.2006(3) 0.3287(3) 0.42435(17) 1.000 0.0380(8) . . C21 C Uani 0.4185(4) 0.4889(3) 0.3754(2) 1.000 0.0476(9) . . C22 C Uani 0.0150(3) 0.1964(2) 0.04217(15) 1.000 0.0261(7) . . C23 C Uani -0.1559(3) 0.1178(3) 0.02241(17) 1.000 0.0338(8) . . C24 C Uani 0.0624(3) 0.2792(3) -0.02384(17) 1.000 0.0376(8) . . H11 H Uiso 0.45830 0.03980 0.11860 1.000 0.0300 calc R H12 H Uiso 0.61180 0.14440 0.18010 1.000 0.0300 calc R H21 H Uiso 0.46790 0.29930 0.22390 1.000 0.0300 calc R H22 H Uiso 0.43660 0.25610 0.11770 1.000 0.0300 calc R H61 H Uiso 0.61130 -0.38250 0.21670 1.000 0.0510 calc R H62 H Uiso 0.75100 -0.33050 0.29880 1.000 0.0510 calc R H63 H Uiso 0.77440 -0.28500 0.20900 1.000 0.0510 calc R H71 H Uiso 0.79460 -0.05950 0.48630 1.000 0.0510 calc R H72 H Uiso 0.91950 -0.01220 0.42510 1.000 0.0510 calc R H73 H Uiso 0.85360 -0.16740 0.42080 1.000 0.0510 calc R H81 H Uiso 0.36030 -0.16170 0.13530 1.000 0.0330 calc R H91 H Uiso 0.27480 -0.33210 0.21010 1.000 0.0550 calc R H92 H Uiso 0.38610 -0.41180 0.16220 1.000 0.0550 calc R H93 H Uiso 0.24250 -0.38670 0.10490 1.000 0.0550 calc R H101 H Uiso 0.58780 -0.14870 0.07020 1.000 0.0610 calc R H102 H Uiso 0.44740 -0.27390 0.01640 1.000 0.0610 calc R H103 H Uiso 0.58590 -0.29540 0.07980 1.000 0.0610 calc R H111 H Uiso 0.74200 0.12950 0.47120 1.000 0.0380 calc R H121 H Uiso 0.46930 0.07710 0.47730 1.000 0.0550 calc R H122 H Uiso 0.45300 0.17890 0.41750 1.000 0.0550 calc R H123 H Uiso 0.55600 0.23260 0.51390 1.000 0.0550 calc R H131 H Uiso 0.83260 0.22730 0.35540 1.000 0.0630 calc R H132 H Uiso 0.79680 0.33050 0.43560 1.000 0.0630 calc R H133 H Uiso 0.67480 0.27270 0.34540 1.000 0.0630 calc R H171 H Uiso 0.15050 0.59130 0.36180 1.000 0.0560 calc R H172 H Uiso -0.00620 0.49130 0.37530 1.000 0.0560 calc R H173 H Uiso -0.01430 0.58150 0.30630 1.000 0.0560 calc R H181 H Uiso -0.11950 0.42460 0.07350 1.000 0.0530 calc R H182 H Uiso -0.12920 0.51300 0.16790 1.000 0.0530 calc R H183 H Uiso -0.23430 0.36180 0.13500 1.000 0.0530 calc R H191 H Uiso 0.34070 0.28580 0.33370 1.000 0.0340 calc R H201 H Uiso 0.12160 0.24240 0.40350 1.000 0.0570 calc R H202 H Uiso 0.14890 0.39860 0.44360 1.000 0.0570 calc R H203 H Uiso 0.27420 0.32560 0.47410 1.000 0.0570 calc R H211 H Uiso 0.46250 0.50560 0.32270 1.000 0.0710 calc R H212 H Uiso 0.50090 0.48270 0.41920 1.000 0.0710 calc R H213 H Uiso 0.37550 0.56230 0.40050 1.000 0.0710 calc R H221 H Uiso 0.07720 0.12960 0.03680 1.000 0.0310 calc R H231 H Uiso -0.17890 0.06700 0.06700 1.000 0.0510 calc R H232 H Uiso -0.17750 0.05620 -0.03620 1.000 0.0510 calc R H233 H Uiso -0.22180 0.17920 0.02360 1.000 0.0510 calc R H241 H Uiso 0.17270 0.33000 -0.00630 1.000 0.0560 calc R H242 H Uiso -0.00280 0.34090 -0.02490 1.000 0.0560 calc R H243 H Uiso 0.04780 0.22000 -0.08280 1.000 0.0560 calc R loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.0191(1) 0.0172(1) 0.0209(1) 0.0053(1) 0.0032(1) 0.0054(1) Cl1 0.0350(3) 0.0275(3) 0.0390(3) 0.0186(2) 0.0128(3) 0.0117(2) Cl2 0.0199(3) 0.0333(3) 0.0403(3) 0.0147(2) 0.0069(2) 0.0075(2) N1 0.0247(9) 0.0233(9) 0.0236(10) 0.0091(7) 0.0056(8) 0.0085(7) N2 0.0206(9) 0.0210(9) 0.0247(10) 0.0064(7) 0.0018(8) 0.0065(7) N3 0.0208(9) 0.0248(9) 0.0217(9) 0.0054(7) 0.0017(8) 0.0086(7) N4 0.0200(9) 0.0270(10) 0.0224(9) 0.0055(8) 0.0015(8) 0.0070(7) N5 0.0309(10) 0.0172(9) 0.0207(9) 0.0030(7) -0.0012(8) 0.0045(7) N6 0.0248(9) 0.0186(9) 0.0222(9) 0.0048(7) 0.0015(8) 0.0080(7) C1 0.0226(11) 0.0291(12) 0.0274(12) 0.0116(9) 0.0060(10) 0.0081(9) C2 0.0248(11) 0.0264(11) 0.0256(11) 0.0112(9) 0.0053(10) 0.0066(9) C3 0.0197(10) 0.0243(11) 0.0224(11) 0.0070(8) 0.0056(9) 0.0064(8) C4 0.0212(10) 0.0282(11) 0.0289(12) 0.0107(9) 0.0063(10) 0.0114(9) C5 0.0201(10) 0.0322(12) 0.0264(11) 0.0123(9) 0.0057(10) 0.0097(9) C6 0.0339(13) 0.0325(13) 0.0422(15) 0.0111(11) 0.0093(12) 0.0184(11) C7 0.0273(12) 0.0499(15) 0.0288(13) 0.0150(11) 0.0006(11) 0.0160(11) C8 0.0260(11) 0.0299(12) 0.0229(11) 0.0021(9) -0.0012(10) 0.0079(9) C9 0.0369(14) 0.0271(13) 0.0389(14) 0.0013(11) -0.0008(12) 0.0027(10) C10 0.0399(15) 0.0529(17) 0.0271(13) 0.0022(12) 0.0070(12) 0.0154(12) C11 0.0311(12) 0.0321(13) 0.0259(12) -0.0007(10) -0.0027(10) 0.0069(10) C12 0.0435(15) 0.0368(14) 0.0288(13) 0.0015(10) 0.0084(12) 0.0144(11) C13 0.0364(14) 0.0327(14) 0.0471(16) 0.0003(12) 0.0062(13) -0.0010(11) C14 0.0228(10) 0.0189(10) 0.0211(11) 0.0057(8) 0.0022(9) 0.0029(8) C15 0.0361(13) 0.0175(10) 0.0275(12) 0.0047(9) 0.0071(10) 0.0085(9) C16 0.0311(12) 0.0190(10) 0.0283(12) 0.0064(9) 0.0058(10) 0.0109(9) C17 0.0557(17) 0.0220(12) 0.0344(13) 0.0021(10) 0.0088(13) 0.0152(11) C18 0.0425(14) 0.0311(13) 0.0371(14) 0.0075(10) 0.0047(12) 0.0217(11) C19 0.0317(12) 0.0262(12) 0.0214(11) 0.0028(9) -0.0036(10) 0.0036(9) C20 0.0415(15) 0.0489(16) 0.0267(13) 0.0121(11) 0.0050(12) 0.0155(12) C21 0.0522(18) 0.0352(15) 0.0376(15) 0.0016(12) -0.0095(14) -0.0083(13) C22 0.0308(12) 0.0256(11) 0.0218(11) 0.0016(9) -0.0015(10) 0.0134(9) C23 0.0333(13) 0.0316(13) 0.0311(13) 0.0002(10) -0.0050(11) 0.0091(10) C24 0.0439(15) 0.0441(15) 0.0273(13) 0.0104(11) 0.0055(12) 0.0152(12) #================================================================== # MOLECULAR GEOMETRY #=================================================================== loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd Cl1 2.3348(6) . . yes Pd Cl2 2.3360(6) . . yes Pd N1 2.0306(19) . . yes Pd N2 2.0469(19) . . yes N1 C1 1.472(3) . . yes N1 C3 1.356(3) . . yes N2 C2 1.468(3) . . yes N2 C14 1.359(3) . . yes N3 C3 1.359(3) . . yes N3 C4 1.397(3) . . yes N3 C8 1.477(3) . . yes N4 C3 1.353(3) . . yes N4 C5 1.386(3) . . yes N4 C11 1.484(3) . . yes N5 C14 1.364(3) . . yes N5 C15 1.395(3) . . yes N5 C19 1.479(3) . . yes N6 C14 1.350(3) . . yes N6 C16 1.396(3) . . yes N6 C22 1.481(3) . . yes C1 C2 1.518(3) . . no C4 C5 1.347(3) . . no C4 C6 1.498(4) . . no C5 C7 1.494(4) . . no C8 C9 1.526(4) . . no C8 C10 1.512(4) . . no C11 C12 1.512(4) . . no C11 C13 1.520(4) . . no C15 C16 1.359(3) . . no C15 C17 1.496(4) . . no C16 C18 1.495(4) . . no C19 C20 1.514(4) . . no C19 C21 1.524(4) . . no C22 C23 1.515(4) . . no C22 C24 1.524(4) . . no C1 H11 0.9900 . . no C1 H12 0.9897 . . no C2 H21 0.9905 . . no C2 H22 0.9897 . . no C6 H61 0.9801 . . no C6 H62 0.9805 . . no C6 H63 0.9797 . . no C7 H71 0.9793 . . no C7 H72 0.9801 . . no C7 H73 0.9798 . . no C8 H81 0.9996 . . no C9 H91 0.9806 . . no C9 H92 0.9798 . . no C9 H93 0.9800 . . no C10 H101 0.9793 . . no C10 H102 0.9799 . . no C10 H103 0.9804 . . no C11 H111 0.9994 . . no C12 H121 0.9795 . . no C12 H122 0.9806 . . no C12 H123 0.9799 . . no C13 H131 0.9801 . . no C13 H132 0.9798 . . no C13 H133 0.9806 . . no C17 H171 0.9798 . . no C17 H172 0.9807 . . no C17 H173 0.9803 . . no C18 H181 0.9801 . . no C18 H182 0.9801 . . no C18 H183 0.9796 . . no C19 H191 1.0005 . . no C20 H201 0.9805 . . no C20 H202 0.9797 . . no C20 H203 0.9805 . . no C21 H211 0.9805 . . no C21 H212 0.9797 . . no C21 H213 0.9803 . . no C22 H221 0.9997 . . no C23 H231 0.9797 . . no C23 H232 0.9806 . . no C23 H233 0.9796 . . no C24 H241 0.9800 . . no C24 H242 0.9804 . . no C24 H243 0.9797 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Pd Cl2 93.39(2) . . . yes Cl1 Pd N1 94.12(6) . . . yes Cl1 Pd N2 175.96(6) . . . yes Cl2 Pd N1 172.26(6) . . . yes Cl2 Pd N2 90.65(5) . . . yes N1 Pd N2 81.84(8) . . . yes Pd N1 C1 108.18(15) . . . yes Pd N1 C3 123.54(16) . . . yes C1 N1 C3 115.78(19) . . . yes Pd N2 C2 111.27(14) . . . yes Pd N2 C14 114.41(15) . . . yes C2 N2 C14 115.53(19) . . . yes C3 N3 C4 109.30(19) . . . yes C3 N3 C8 122.41(19) . . . yes C4 N3 C8 128.02(19) . . . yes C3 N4 C5 109.6(2) . . . yes C3 N4 C11 125.9(2) . . . yes C5 N4 C11 124.4(2) . . . yes C14 N5 C15 109.40(19) . . . yes C14 N5 C19 122.12(19) . . . yes C15 N5 C19 128.34(19) . . . yes C14 N6 C16 109.69(19) . . . yes C14 N6 C22 121.80(19) . . . yes C16 N6 C22 128.49(19) . . . yes N1 C1 C2 105.7(2) . . . yes N2 C2 C1 107.09(18) . . . yes N1 C3 N3 129.4(2) . . . yes N1 C3 N4 124.0(2) . . . yes N3 C3 N4 106.5(2) . . . yes N3 C4 C5 106.9(2) . . . yes N3 C4 C6 124.8(2) . . . yes C5 C4 C6 127.1(2) . . . no N4 C5 C4 107.6(2) . . . yes N4 C5 C7 122.9(2) . . . yes C4 C5 C7 128.9(2) . . . no N3 C8 C9 111.53(19) . . . yes N3 C8 C10 111.4(2) . . . yes C9 C8 C10 113.3(2) . . . no N4 C11 C12 111.7(2) . . . yes N4 C11 C13 110.5(2) . . . yes C12 C11 C13 113.6(2) . . . no N2 C14 N5 128.5(2) . . . yes N2 C14 N6 124.7(2) . . . yes N5 C14 N6 106.8(2) . . . yes N5 C15 C16 107.0(2) . . . yes N5 C15 C17 125.1(2) . . . yes C16 C15 C17 127.9(2) . . . no N6 C16 C15 107.2(2) . . . yes N6 C16 C18 125.5(2) . . . yes C15 C16 C18 127.4(2) . . . no N5 C19 C20 112.2(2) . . . yes N5 C19 C21 110.8(2) . . . yes C20 C19 C21 114.3(2) . . . no N6 C22 C23 111.9(2) . . . yes N6 C22 C24 111.44(19) . . . yes C23 C22 C24 113.4(2) . . . no N1 C1 H11 110.59 . . . no N1 C1 H12 110.59 . . . no C2 C1 H11 110.63 . . . no C2 C1 H12 110.62 . . . no H11 C1 H12 108.70 . . . no N2 C2 H21 110.29 . . . no N2 C2 H22 110.30 . . . no C1 C2 H21 110.27 . . . no C1 C2 H22 110.30 . . . no H21 C2 H22 108.59 . . . no C4 C6 H61 109.42 . . . no C4 C6 H62 109.48 . . . no C4 C6 H63 109.48 . . . no H61 C6 H62 109.45 . . . no H61 C6 H63 109.52 . . . no H62 C6 H63 109.48 . . . no C5 C7 H71 109.49 . . . no C5 C7 H72 109.43 . . . no C5 C7 H73 109.47 . . . no H71 C7 H72 109.46 . . . no H71 C7 H73 109.47 . . . no H72 C7 H73 109.50 . . . no N3 C8 H81 106.73 . . . no C9 C8 H81 106.72 . . . no C10 C8 H81 106.72 . . . no C8 C9 H91 109.46 . . . no C8 C9 H92 109.51 . . . no C8 C9 H93 109.43 . . . no H91 C9 H92 109.45 . . . no H91 C9 H93 109.47 . . . no H92 C9 H93 109.51 . . . no C8 C10 H101 109.48 . . . no C8 C10 H102 109.43 . . . no C8 C10 H103 109.49 . . . no H101 C10 H102 109.56 . . . no H101 C10 H103 109.46 . . . no H102 C10 H103 109.41 . . . no N4 C11 H111 106.96 . . . no C12 C11 H111 106.88 . . . no C13 C11 H111 106.88 . . . no C11 C12 H121 109.44 . . . no C11 C12 H122 109.46 . . . no C11 C12 H123 109.43 . . . no H121 C12 H122 109.51 . . . no H121 C12 H123 109.56 . . . no H122 C12 H123 109.42 . . . no C11 C13 H131 109.45 . . . no C11 C13 H132 109.44 . . . no C11 C13 H133 109.47 . . . no H131 C13 H132 109.47 . . . no H131 C13 H133 109.42 . . . no H132 C13 H133 109.57 . . . no C15 C17 H171 109.47 . . . no C15 C17 H172 109.44 . . . no C15 C17 H173 109.48 . . . no H171 C17 H172 109.48 . . . no H171 C17 H173 109.52 . . . no H172 C17 H173 109.44 . . . no C16 C18 H181 109.42 . . . no C16 C18 H182 109.45 . . . no C16 C18 H183 109.43 . . . no H181 C18 H182 109.51 . . . no H181 C18 H183 109.52 . . . no H182 C18 H183 109.49 . . . no N5 C19 H191 106.30 . . . no C20 C19 H191 106.33 . . . no C21 C19 H191 106.31 . . . no C19 C20 H201 109.46 . . . no C19 C20 H202 109.50 . . . no C19 C20 H203 109.55 . . . no H201 C20 H202 109.41 . . . no H201 C20 H203 109.45 . . . no H202 C20 H203 109.46 . . . no C19 C21 H211 109.43 . . . no C19 C21 H212 109.53 . . . no C19 C21 H213 109.45 . . . no H211 C21 H212 109.53 . . . no H211 C21 H213 109.38 . . . no H212 C21 H213 109.51 . . . no N6 C22 H221 106.52 . . . no C23 C22 H221 106.52 . . . no C24 C22 H221 106.56 . . . no C22 C23 H231 109.46 . . . no C22 C23 H232 109.47 . . . no C22 C23 H233 109.49 . . . no H231 C23 H232 109.41 . . . no H231 C23 H233 109.50 . . . no H232 C23 H233 109.50 . . . no C22 C24 H241 109.49 . . . no C22 C24 H242 109.51 . . . no C22 C24 H243 109.47 . . . no H241 C24 H242 109.45 . . . no H241 C24 H243 109.45 . . . no H242 C24 H243 109.45 . . . no #============================================================================= # end of cif data for "pete" (compound 2) #============================================================================= #============================================================================= # end of cif file #=============================================================================