# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global #=============================================================================== _audit_creation_date 15-10-02 _journal_coden_Cambridge 182 loop_ _publ_author_name 'Djukic, Jean-Pierre' 'Alexsandro, Berger' 'Andre de, Cian' 'Nathalie, Kyritsakas-Gruber' 'Jerome, Lacour' 'Michel, Pfeffer' 'Laurent, Vial' _publ_contact_author_name ; Jean-Pierre Djukic ; _publ_contact_author_address ; Laboratoire de Syntheses Metallo-Induites UMR CNRS 7513 Universite Louis Pasteur 4, rue Blaise Pascal STRASBOURG 67070 FRANCE ; _publ_contact_author_phone +33(0)390241523 _publ_contact_author_fax +33(0)390241526 _publ_contact_author_email djukic@chimie.u-strasbg.fr _publ_requested_journal 'Chemical Communications' _publ_contact_letter ; Please consider this CIF submission for in Chemical Communications. The figures, chemical,structure diagram (scheme), Transfert of Copyright Agreement form and structure factors will be sent on receipt of your acknowledgement letter ; _publ_section_title ; Novel heteroleptic cis-(C-N)2Pd(II) chelates for the preparation of enantiopure planar chiral cyclopalladated 2-[tricarbonyl(eta6-phenyl)chromium]pyridine ; _publ_requested_category FM _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. OpenMoleN, Interactive Intelligent Structure solution (1997) Nonius B.V., Delft, The Netherlands. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. Walker, N. & Stuart, D. (1983). Acta Cryst., A39, 158-166. ; data_5b _database_code_CSD 198824 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C48 H44 Cr2 N4 O6 Pd2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C48 H44 Cr2 N4 O6 Pd2' _chemical_formula_weight 1089.70 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 Cr ? 0.284 0.624 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 Pd ? -1.177 1.007 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' _symmetry_space_group_name_Hall ' P 2yb' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,-z _cell_length_a 11.1217(3) _cell_length_b 17.0324(4) _cell_length_c 11.5570(3) _cell_angle_alpha 90 _cell_angle_beta 102.118(5) _cell_angle_gamma 90 _cell_volume 2140.45(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used 12332 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 30.0 _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.69 _exptl_crystal_density_method none _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 1.377 _exptl_absorpt_correction_type refdelf_(Walker_&_Stuart,_1983) _exptl_absorpt_correction_T_min 0.9609 _exptl_absorpt_correction_T_max 1.0000 #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 12332 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 36. mm. Scan angle = 1.6 deg 1 scans of 60 sec per frame. Data collection was divided into 1 set(s) with the following starting angles and number of frames : Set 1 Theta = 8.80 Omega = 0.00 Kappa = 0.00 90 frames Friedel pairs were averaged. Internal R = 0.05 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12332 _diffrn_reflns_av_R_equivalents 0.050 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 30.03 _reflns_number_total 6364 _reflns_number_gt 4310 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack 0.03(4) _refine_ls_number_reflns 4310 _refine_ls_number_parameters 558 _refine_ls_number_restraints 1 _refine_ls_number_constraints 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_R_factor_all 0.058 _refine_ls_R_factor_gt 0.030 _refine_ls_wR_factor_all 0.153 _refine_ls_wR_factor_ref 0.046 _refine_ls_goodness_of_fit_all 4.048 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_shift/su_max 0.014 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 0.424 _refine_diff_density_min -0.156 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol CR1 0.5659(1) 0.10801(7) 0.45685(9) 0.0172(5) Uani ? ? Cr PD1 0.86745(4) 0.2043 0.38139(4) 0.0193(2) Uani ? ? Pd CR2 0.9203(1) 0.55008(7) 0.04263(9) 0.0179(5) Uani ? ? Cr PD2 0.62165(4) 0.44670(3) 0.11565(4) 0.0201(2) Uani ? ? Pd C1 0.5064(7) 0.1069(4) 0.5928(7) 0.030(4) Uani ? ? C O1 0.4709(6) 0.1076(4) 0.6787(5) 0.047(3) Uani ? ? O C2 0.4060(7) 0.1108(4) 0.3762(6) 0.024(3) Uani ? ? C O2 0.3035(5) 0.1097(4) 0.3265(5) 0.042(3) Uani ? ? O C3 0.5600(6) 0.2167(5) 0.4668(6) 0.028(3) Uani ? ? C O3 0.5555(5) 0.2847(3) 0.4750(4) 0.029(3) Uani ? ? O C4 0.6797(6) 0.0857(4) 0.3180(6) 0.018(3) Uani ? ? C C5 0.7593(6) 0.1205(4) 0.4198(6) 0.017(3) Uani ? ? C C6 0.7641(6) 0.0827(4) 0.5283(7) 0.024(3) Uani ? ? C C7 0.6927(7) 0.0147(4) 0.5396(6) 0.024(3) Uani ? ? C C8 0.6138(7) -0.0167(4) 0.4378(6) 0.024(3) Uani ? ? C C9 0.6071(6) 0.0198(4) 0.3286(6) 0.021(3) Uani ? ? C C10 0.6810(6) 0.1217(4) 0.2013(6) 0.019(3) Uani ? ? C C11 0.6016(7) 0.1017(4) 0.0949(6) 0.023(3) Uani ? ? C C12 0.6108(8) 0.1367(5) -0.0082(7) 0.030(4) Uani ? ? C C13 0.6997(7) 0.1950(5) -0.0046(5) 0.019(3) Uani ? ? C C14 0.7745(7) 0.2136(4) 0.1031(6) 0.025(3) Uani ? ? C N1 0.7705(5) 0.1775(3) 0.2046(5) 0.018(3) Uani ? ? N N2 1.0211(5) 0.2753(3) 0.3496(5) 0.019(3) Uani ? ? N C15 1.0736(6) 0.2418(5) 0.2534(7) 0.028(4) Uani ? ? C C16 0.9893(7) 0.3563(5) 0.3261(6) 0.030(4) Uani ? ? C C17 1.1135(6) 0.2667(5) 0.4662(7) 0.025(3) Uani ? ? C C18 1.2298(8) 0.3153(6) 0.4757(7) 0.043(5) Uani ? ? C C19 1.0445(6) 0.2794(4) 0.5648(6) 0.021(3) Uani ? ? C C20 1.0909(7) 0.3238(4) 0.6635(6) 0.026(4) Uani ? ? C C21 1.0230(7) 0.3327(5) 0.7500(7) 0.029(4) Uani ? ? C C22 0.9076(7) 0.2975(5) 0.7352(6) 0.028(4) Uani ? ? C C23 0.8603(6) 0.2531(4) 0.6360(6) 0.019(3) Uani ? ? C C24 0.9278(6) 0.2441(4) 0.5458(6) 0.016(3) Uani ? ? C C25 0.9860(7) 0.5497(4) -0.0924(6) 0.026(4) Uani ? ? C O4 1.0261(6) 0.5475(4) -0.1770(5) 0.044(3) Uani ? ? O C26 1.0777(7) 0.5559(5) 0.1313(6) 0.030(4) Uani ? ? C O5 1.1788(5) 0.5564(4) 0.1853(5) 0.043(3) Uani ? ? O C27 0.9312(6) 0.4431(5) 0.0380(6) 0.023(3) Uani ? ? C O6 0.9424(5) 0.3758(3) 0.0315(5) 0.036(3) Uani ? ? O C28 0.8036(6) 0.5707(4) 0.1771(6) 0.018(3) Uani ? ? C C29 0.7257(6) 0.5342(4) 0.0765(6) 0.019(3) Uani ? ? C C30 0.7212(6) 0.5712(4) -0.0340(6) 0.018(3) Uani ? ? C C31 0.7867(7) 0.6394(5) -0.0439(6) 0.028(4) Uani ? ? C C32 0.8617(7) 0.6748(4) 0.0535(7) 0.026(3) Uani ? ? C C33 0.8713(7) 0.6396(4) 0.1641(6) 0.026(3) Uani ? ? C C34 0.8046(6) 0.5351(4) 0.2941(6) 0.020(3) Uani ? ? C C35 0.8848(7) 0.5579(5) 0.3975(6) 0.026(3) Uani ? ? C C36 0.8784(7) 0.5195(5) 0.5033(6) 0.024(4) Uani ? ? C C37 0.7935(8) 0.4611(4) 0.5014(7) 0.034(4) Uani ? ? C C38 0.7154(7) 0.4420(5) 0.3958(6) 0.027(3) Uani ? ? C N3 0.7187(5) 0.4791(4) 0.2917(5) 0.021(3) Uani ? ? N N4 0.4736(5) 0.3708(3) 0.1479(5) 0.022(3) Uani ? ? N C39 0.4108(6) 0.4024(5) 0.2391(6) 0.026(3) Uani ? ? C C40 0.5238(7) 0.2908(4) 0.1877(6) 0.021(3) Uani ? ? C C41 0.3852(6) 0.3604(4) 0.0311(6) 0.021(3) Uani ? ? C C42 0.2908(7) 0.4248(5) 0.0038(7) 0.033(4) Uani ? ? C C43 0.4613(6) 0.3555(4) -0.0613(6) 0.020(3) Uani ? ? C C44 0.4246(7) 0.3073(5) -0.1626(7) 0.028(4) Uani ? ? C C45 0.4937(7) 0.3062(5) -0.2493(6) 0.027(4) Uani ? ? C C46 0.5973(6) 0.3513(5) -0.2380(6) 0.024(3) Uani ? ? C C47 0.6356(7) 0.3965(4) -0.1359(7) 0.024(3) Uani ? ? C C48 0.5680(6) 0.4011(4) -0.0473(6) 0.021(3) Uani ? ? C H1 0.8170 0.1032 0.5971 0.0328 Uiso calc C6 H H2 0.6980 -0.0093 0.6147 0.0317 Uiso calc C7 H H3 0.5660 -0.0621 0.4439 0.0325 Uiso calc C8 H H4 0.5525 -0.0002 0.2605 0.0288 Uiso calc C9 H H5 0.5402 0.0629 0.0949 0.0311 Uiso calc C11 H H6 0.5583 0.1221 -0.0808 0.0408 Uiso calc C12 H H7 0.7086 0.2213 -0.0748 0.0349 Uiso calc C13 H H8 0.8326 0.2547 0.1050 0.0328 Uiso calc C14 H H9 1.0161 0.2471 0.1805 0.0374 Uiso calc C15 H H10 1.1472 0.2690 0.2491 0.0374 Uiso calc C15 H H11 1.0915 0.1878 0.2688 0.0374 Uiso calc C15 H H12 0.9316 0.3605 0.2531 0.0385 Uiso calc C16 H H13 0.9541 0.3767 0.3880 0.0385 Uiso calc C16 H H14 1.0612 0.3854 0.3218 0.0385 Uiso calc C16 H H15 1.1469 0.2152 0.4723 0.0341 Uiso calc C17 H H16 1.2824 0.3067 0.5507 0.0645 Uiso calc C18 H H17 1.2709 0.3003 0.4149 0.0645 Uiso calc C18 H H18 1.2088 0.3694 0.4674 0.0645 Uiso calc C18 H H19 1.1692 0.3481 0.6722 0.0356 Uiso calc C20 H H20 1.0547 0.3626 0.8190 0.0416 Uiso calc C21 H H21 0.8606 0.3041 0.7943 0.0375 Uiso calc C22 H H22 0.7823 0.2285 0.6283 0.0254 Uiso calc C23 H H23 0.6720 0.5488 -0.1033 0.0235 Uiso calc C30 H H24 0.7801 0.6626 -0.1197 0.0359 Uiso calc C31 H H25 0.9053 0.7217 0.0450 0.0346 Uiso calc C32 H H26 0.9239 0.6620 0.2315 0.0337 Uiso calc C33 H H27 0.9427 0.5988 0.3966 0.0339 Uiso calc C35 H H28 0.9324 0.5338 0.5754 0.0363 Uiso calc C36 H H29 0.7884 0.4339 0.5721 0.0463 Uiso calc C37 H H30 0.6568 0.4014 0.3955 0.0346 Uiso calc C38 H H31 0.4687 0.4083 0.3117 0.0314 Uiso calc C39 H H32 0.3755 0.4519 0.2142 0.0314 Uiso calc C39 H H33 0.3479 0.3670 0.2498 0.0314 Uiso calc C39 H H34 0.5803 0.2954 0.2614 0.0309 Uiso calc C40 H H35 0.4582 0.2572 0.1962 0.0309 Uiso calc C40 H H36 0.5648 0.2695 0.1304 0.0309 Uiso calc C40 H H37 0.3383 0.3140 0.0333 0.0273 Uiso calc C41 H H38 0.2379 0.4150 -0.0707 0.0450 Uiso calc C42 H H39 0.2439 0.4264 0.0636 0.0450 Uiso calc C42 H H40 0.3311 0.4738 0.0012 0.0450 Uiso calc C42 H H41 0.3528 0.2758 -0.1710 0.0386 Uiso calc C44 H H42 0.4689 0.2740 -0.3172 0.0358 Uiso calc C45 H H43 0.6429 0.3519 -0.2989 0.0312 Uiso calc C46 H H44 0.7103 0.4251 -0.1265 0.0325 Uiso calc C47 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol CR1 0.0185(5) 0.0178(5) 0.0155(5) -0.0036(5) 0.0042(4) 0.0015(4) Cr PD1 0.0192(2) 0.0198(2) 0.0187(2) -0.0024(2) 0.0044(2) -0.0003(2) Pd CR2 0.0175(5) 0.0194(5) 0.0169(5) -0.0011(5) 0.0048(4) 0.0009(4) Cr PD2 0.0211(2) 0.0202(2) 0.0190(2) -0.0005(2) 0.0064(2) 0.0008(2) Pd C1 0.034(4) 0.022(4) 0.035(4) -0.003(3) 0.016(3) 0.003(3) C O1 0.069(3) 0.036(3) 0.042(3) -0.006(3) 0.034(2) -0.002(3) O C2 0.030(3) 0.026(4) 0.017(3) 0.007(3) 0.009(3) 0.002(3) C O2 0.026(3) 0.063(4) 0.045(3) 0.003(3) 0.002(3) 0.002(3) O C3 0.025(3) 0.039(4) 0.021(3) 0.006(3) 0.010(3) 0.012(3) C O3 0.044(3) 0.020(3) 0.027(2) 0.005(2) 0.015(2) 0.002(2) O C4 0.024(3) 0.011(3) 0.020(3) 0.001(3) 0.008(2) -0.002(3) C C5 0.011(3) 0.020(3) 0.024(3) -0.001(3) 0.002(2) -0.000(3) C C6 0.016(3) 0.027(4) 0.033(4) -0.008(3) 0.004(3) 0.000(3) C C7 0.026(3) 0.021(3) 0.026(3) -0.005(3) 0.006(3) 0.013(3) C C8 0.030(4) 0.019(3) 0.023(3) -0.010(3) 0.000(3) 0.002(3) C C9 0.023(3) 0.015(3) 0.026(3) -0.001(3) -0.001(3) 0.001(3) C C10 0.022(3) 0.018(3) 0.017(3) 0.003(3) 0.008(2) 0.002(3) C C11 0.023(3) 0.021(3) 0.025(3) -0.002(3) -0.001(3) -0.012(3) C C12 0.035(4) 0.029(4) 0.026(4) 0.001(4) -0.004(3) -0.001(3) C C13 0.037(3) 0.041(4) 0.004(2) 0.009(4) 0.007(2) 0.007(3) C C14 0.030(3) 0.020(3) 0.026(3) -0.000(3) 0.008(3) 0.010(3) C N1 0.022(3) 0.015(3) 0.017(2) 0.001(2) 0.006(2) 0.000(2) N N2 0.016(2) 0.020(3) 0.022(3) -0.001(2) 0.006(2) 0.005(2) N C15 0.020(3) 0.031(4) 0.036(4) 0.001(3) 0.007(3) -0.009(3) C C16 0.035(4) 0.029(4) 0.027(3) 0.002(3) 0.011(3) 0.013(3) C C17 0.015(3) 0.029(4) 0.034(4) -0.005(3) 0.004(3) 0.005(3) C C18 0.038(4) 0.082(7) 0.025(4) -0.033(4) -0.000(3) 0.002(5) C C19 0.018(3) 0.022(3) 0.023(3) 0.000(3) 0.004(2) 0.003(3) C C20 0.032(4) 0.020(3) 0.028(4) -0.009(3) 0.001(3) 0.003(3) C C21 0.036(4) 0.032(4) 0.021(3) 0.003(4) -0.008(3) -0.005(3) C C22 0.035(4) 0.036(4) 0.018(3) 0.011(3) 0.009(3) -0.002(3) C C23 0.020(3) 0.023(3) 0.016(3) 0.003(3) 0.002(2) 0.005(3) C C24 0.015(3) 0.013(3) 0.023(3) 0.000(3) 0.004(2) 0.003(3) C C25 0.036(4) 0.020(3) 0.024(3) -0.004(3) 0.005(3) 0.002(3) C O4 0.060(3) 0.043(4) 0.034(3) -0.004(3) 0.025(2) 0.001(3) O C26 0.034(4) 0.030(4) 0.026(3) 0.004(3) 0.008(3) -0.012(3) C O5 0.032(3) 0.087(5) 0.029(3) 0.012(3) -0.009(3) -0.022(3) O C27 0.021(3) 0.032(4) 0.018(3) -0.002(3) 0.009(2) 0.004(3) C O6 0.054(3) 0.021(3) 0.040(3) 0.005(3) 0.013(3) 0.008(2) O C28 0.020(3) 0.021(3) 0.014(3) 0.002(3) 0.004(2) 0.002(3) C C29 0.017(3) 0.024(3) 0.017(3) 0.001(3) 0.011(2) 0.001(3) C C30 0.017(3) 0.019(3) 0.019(3) 0.004(3) 0.004(2) 0.006(3) C C31 0.027(3) 0.033(4) 0.023(3) 0.004(3) 0.008(3) 0.004(3) C C32 0.031(4) 0.016(3) 0.033(4) -0.003(3) 0.008(3) 0.007(3) C C33 0.027(3) 0.027(4) 0.025(3) -0.005(3) 0.009(3) -0.012(3) C C34 0.017(3) 0.021(3) 0.022(3) 0.001(3) 0.003(2) -0.006(3) C C35 0.034(4) 0.022(3) 0.022(3) 0.005(3) 0.007(3) 0.005(3) C C36 0.037(4) 0.035(4) 0.011(3) 0.003(4) 0.005(3) -0.004(3) C C37 0.049(4) 0.019(4) 0.041(4) 0.003(4) 0.015(3) 0.004(3) C C38 0.033(3) 0.029(4) 0.022(3) -0.006(3) 0.013(2) -0.011(3) C N3 0.027(3) 0.020(3) 0.017(2) 0.002(3) 0.009(2) 0.002(2) N N4 0.028(3) 0.017(3) 0.021(3) -0.000(2) 0.012(2) -0.003(2) N C39 0.021(3) 0.029(4) 0.029(3) -0.002(3) 0.019(2) -0.005(3) C C40 0.041(4) 0.011(3) 0.020(3) 0.009(3) 0.007(3) 0.002(3) C C41 0.020(3) 0.019(3) 0.026(3) -0.002(3) 0.008(3) -0.001(3) C C42 0.022(3) 0.043(5) 0.038(4) -0.001(4) 0.005(3) 0.001(4) C C43 0.020(3) 0.018(3) 0.020(3) 0.005(3) 0.003(2) 0.004(3) C C44 0.033(4) 0.020(4) 0.032(4) -0.002(3) -0.001(3) -0.002(3) C C45 0.031(4) 0.027(4) 0.022(3) 0.007(3) 0.001(3) -0.008(3) C C46 0.022(3) 0.030(4) 0.021(3) 0.004(3) 0.005(3) -0.002(3) C C47 0.023(3) 0.021(4) 0.030(4) 0.001(3) 0.002(3) -0.003(3) C C48 0.028(3) 0.018(3) 0.017(3) 0.005(3) 0.001(3) -0.002(3) C # 10. 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 CR1 C1 1.83(1) . . ? CR1 C2 1.83(1) . . ? CR1 C3 1.86(1) . . ? CR1 C4 2.28(1) . . ? CR1 C5 2.290(9) . . ? CR1 C6 2.23(1) . . ? CR1 C7 2.20(1) . . ? CR1 C8 2.21(1) . . ? CR1 C9 2.22(1) . . ? PD1 C5 1.98(1) . . ? PD1 N1 2.149(9) . . ? PD1 N2 2.187(8) . . ? PD1 C24 2.00(1) . . ? CR2 C25 1.86(1) . . ? CR2 C26 1.84(1) . . ? CR2 C27 1.83(1) . . ? CR2 C28 2.25(1) . . ? CR2 C29 2.295(9) . . ? CR2 C30 2.235(9) . . ? CR2 C31 2.21(1) . . ? CR2 C32 2.23(1) . . ? CR2 C33 2.22(1) . . ? PD2 C29 2.00(1) . . ? PD2 N3 2.165(9) . . ? PD2 N4 2.186(8) . . ? PD2 C48 2.01(1) . . ? C1 O1 1.14(1) . . ? C2 O2 1.16(1) . . ? C3 O3 1.16(2) . . ? C4 C5 1.44(1) . . ? C4 C9 1.40(1) . . ? C4 C10 1.48(1) . . ? C5 C6 1.40(2) . . ? C6 C7 1.43(1) . . ? C7 C8 1.42(2) . . ? C8 C9 1.40(2) . . ? C10 C11 1.40(1) . . ? C10 N1 1.37(1) . . ? C11 C12 1.36(2) . . ? C12 C13 1.39(2) . . ? C13 C14 1.38(1) . . ? C14 N1 1.33(1) . . ? N2 C15 1.47(1) . . ? N2 C16 1.44(2) . . ? N2 C17 1.52(1) . . ? C17 C18 1.52(1) . . ? C17 C19 1.52(1) . . ? C19 C20 1.38(2) . . ? C19 C24 1.40(1) . . ? C20 C21 1.38(2) . . ? C21 C22 1.39(2) . . ? C22 C23 1.38(2) . . ? C23 C24 1.41(1) . . ? C25 O4 1.16(1) . . ? C26 O5 1.17(1) . . ? C27 O6 1.16(2) . . ? C28 C29 1.44(1) . . ? C28 C33 1.42(2) . . ? C28 C34 1.48(1) . . ? C29 C30 1.42(1) . . ? C30 C31 1.39(2) . . ? C31 C32 1.39(2) . . ? C32 C33 1.39(2) . . ? C34 C35 1.39(1) . . ? C34 N3 1.35(1) . . ? C35 C36 1.40(2) . . ? C36 C37 1.37(2) . . ? C37 C38 1.38(2) . . ? C38 N3 1.36(1) . . ? N4 C39 1.48(1) . . ? N4 C40 1.51(1) . . ? N4 C41 1.50(1) . . ? C41 C42 1.51(1) . . ? C41 C43 1.50(1) . . ? C43 C44 1.42(2) . . ? C43 C48 1.40(1) . . ? C44 C45 1.38(2) . . ? C45 C46 1.37(2) . . ? C46 C47 1.40(2) . . ? C47 C48 1.39(2) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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 C1 CR1 C2 87.1(5) . . . ? C1 CR1 C3 86.2(5) . . . ? C1 CR1 C4 163.7(5) . . . ? C1 CR1 C5 133.2(4) . . . ? C1 CR1 C6 100.8(5) . . . ? C1 CR1 C7 86.2(5) . . . ? C1 CR1 C8 102.3(5) . . . ? C1 CR1 C9 136.7(5) . . . ? C2 CR1 C3 87.9(5) . . . ? C2 CR1 C4 105.7(4) . . . ? C2 CR1 C5 139.0(4) . . . ? C2 CR1 C6 167.3(5) . . . ? C2 CR1 C7 134.9(4) . . . ? C2 CR1 C8 101.7(4) . . . ? C2 CR1 C9 89.6(4) . . . ? C3 CR1 C4 104.0(4) . . . ? C3 CR1 C5 88.0(4) . . . ? C3 CR1 C6 102.4(4) . . . ? C3 CR1 C7 136.0(4) . . . ? C3 CR1 C8 167.4(4) . . . ? C3 CR1 C9 136.8(5) . . . ? C4 CR1 C5 36.8(4) . . . ? C4 CR1 C6 64.9(4) . . . ? C4 CR1 C7 77.6(4) . . . ? C4 CR1 C8 65.7(4) . . . ? C4 CR1 C9 36.3(4) . . . ? C5 CR1 C6 36.1(4) . . . ? C5 CR1 C7 66.9(4) . . . ? C5 CR1 C8 79.3(4) . . . ? C5 CR1 C9 66.7(4) . . . ? C6 CR1 C7 37.5(4) . . . ? C6 CR1 C8 67.1(4) . . . ? C6 CR1 C9 77.9(4) . . . ? C7 CR1 C8 37.4(4) . . . ? C7 CR1 C9 66.4(4) . . . ? C8 CR1 C9 36.7(4) . . . ? C5 PD1 N1 81.5(4) . . . ? C5 PD1 N2 166.2(3) . . . ? C5 PD1 C24 97.5(4) . . . ? N1 PD1 N2 102.2(3) . . . ? N1 PD1 C24 168.0(3) . . . ? N2 PD1 C24 81.6(4) . . . ? C25 CR2 C26 88.4(5) . . . ? C25 CR2 C27 86.1(5) . . . ? C25 CR2 C28 165.0(5) . . . ? C25 CR2 C29 134.0(4) . . . ? C25 CR2 C30 101.5(4) . . . ? C25 CR2 C31 88.2(5) . . . ? C25 CR2 C32 102.8(5) . . . ? C25 CR2 C33 136.6(5) . . . ? C26 CR2 C27 90.5(5) . . . ? C26 CR2 C28 103.1(5) . . . ? C26 CR2 C29 137.2(5) . . . ? C26 CR2 C30 164.1(5) . . . ? C26 CR2 C31 133.3(5) . . . ? C26 CR2 C32 99.9(5) . . . ? C26 CR2 C33 86.7(4) . . . ? C27 CR2 C28 103.2(4) . . . ? C27 CR2 C29 87.6(4) . . . ? C27 CR2 C30 102.4(4) . . . ? C27 CR2 C31 135.6(4) . . . ? C27 CR2 C32 166.4(4) . . . ? C27 CR2 C33 137.0(5) . . . ? C28 CR2 C29 36.8(4) . . . ? C28 CR2 C30 65.3(4) . . . ? C28 CR2 C31 77.0(4) . . . ? C28 CR2 C32 66.1(4) . . . ? C28 CR2 C33 37.0(4) . . . ? C29 CR2 C30 36.4(4) . . . ? C29 CR2 C31 65.8(4) . . . ? C29 CR2 C32 78.8(4) . . . ? C29 CR2 C33 66.8(4) . . . ? C30 CR2 C31 36.4(4) . . . ? C30 CR2 C32 66.0(4) . . . ? C30 CR2 C33 77.6(4) . . . ? C31 CR2 C32 36.4(4) . . . ? C31 CR2 C33 65.3(4) . . . ? C32 CR2 C33 36.5(4) . . . ? C29 PD2 N3 79.9(4) . . . ? C29 PD2 N4 166.7(4) . . . ? C29 PD2 C48 98.6(4) . . . ? N3 PD2 N4 103.6(3) . . . ? N3 PD2 C48 166.2(3) . . . ? N4 PD2 C48 81.1(4) . . . ? C5 C4 C9 121(1) . . . ? C5 C4 C10 116.8(9) . . . ? C9 C4 C10 121.7(9) . . . ? C4 C5 C6 116.3(9) . . . ? C5 C6 C7 122(1) . . . ? C6 C7 C8 119(1) . . . ? C7 C8 C9 119.3(9) . . . ? C4 C9 C8 120(1) . . . ? C4 C10 C11 125(1) . . . ? C4 C10 N1 113.9(9) . . . ? C11 C10 N1 121(1) . . . ? C10 C11 C12 121(1) . . . ? C11 C12 C13 118(1) . . . ? C12 C13 C14 118(1) . . . ? C13 C14 N1 124(1) . . . ? C10 N1 C14 116.9(9) . . . ? C15 N2 C16 110(1) . . . ? C15 N2 C17 109.3(8) . . . ? C16 N2 C17 110.7(9) . . . ? N2 C17 C18 114.7(8) . . . ? N2 C17 C19 107.3(7) . . . ? C18 C17 C19 115.2(9) . . . ? C17 C19 C20 122.7(9) . . . ? C17 C19 C24 114(1) . . . ? C20 C19 C24 122(1) . . . ? C19 C20 C21 119.6(9) . . . ? C20 C21 C22 119(1) . . . ? C21 C22 C23 121(1) . . . ? C22 C23 C24 120.1(9) . . . ? C19 C24 C23 117(1) . . . ? C29 C28 C33 120(1) . . . ? C29 C28 C34 116.7(9) . . . ? C33 C28 C34 122.3(9) . . . ? C28 C29 C30 116.0(9) . . . ? C29 C30 C31 121(1) . . . ? C30 C31 C32 122(1) . . . ? C31 C32 C33 118(1) . . . ? C28 C33 C32 120(1) . . . ? C28 C34 C35 123(1) . . . ? C28 C34 N3 113.8(9) . . . ? C35 C34 N3 122(1) . . . ? C34 C35 C36 118(1) . . . ? C35 C36 C37 119(1) . . . ? C36 C37 C38 119(1) . . . ? C37 C38 N3 122(1) . . . ? C34 N3 C38 117.4(9) . . . ? C39 N4 C40 108.1(9) . . . ? C39 N4 C41 111.3(7) . . . ? C40 N4 C41 107.3(8) . . . ? N4 C41 C42 113.5(8) . . . ? N4 C41 C43 106.5(7) . . . ? C42 C41 C43 111.4(8) . . . ? C41 C43 C44 120.8(9) . . . ? C41 C43 C48 118(1) . . . ? C44 C43 C48 120(1) . . . ? C43 C44 C45 119(1) . . . ? C44 C45 C46 120(1) . . . ? C45 C46 C47 119(1) . . . ? C46 C47 C48 122(1) . . . ? C43 C48 C47 117(1) . . . ? #-----------------END data_5c _database_code_CSD 198825 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C48 H44 Cr2 N4 O6 Pd2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C48 H44 Cr2 N4 O6 Pd2' _chemical_formula_weight 1089.70 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 Cr ? 0.284 0.624 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 Pd ? -1.177 1.007 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' _symmetry_space_group_name_Hall ' P 2yb' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,-z _cell_length_a 11.1267(2) _cell_length_b 17.0317(3) _cell_length_c 11.5572(2) _cell_angle_alpha 90 _cell_angle_beta 102.140(5) _cell_angle_gamma 90 _cell_volume 2141.19(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.69 _exptl_crystal_density_method none _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 1.376 _exptl_absorpt_correction_type refdelf_(Walker_&_Stuart,_1983) _exptl_absorpt_correction_T_min 0.9783 _exptl_absorpt_correction_T_max 1.1570 #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 10295 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 36. mm. Scan angle = 1.6 deg 1 scans of 60 sec per frame. Data collection was divided into 2 set(s) with the following starting angles and number of frames : Set 1 Theta = 8.80 Omega = 0.00 Kappa = 0.00 90 frames Set 2 Theta = -8.50 Kappa = -80.00 Phi = 0.00 27 frames Friedel pairs were averaged. Internal R = 0.03 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10295 _diffrn_reflns_av_R_equivalents 0.030 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 30.02 _reflns_number_total 6443 _reflns_number_gt 5557 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack 0.01(2) _refine_ls_number_reflns 5557 _refine_ls_number_parameters 558 _refine_ls_number_restraints 1 _refine_ls_number_constraints 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_R_factor_all 0.032 _refine_ls_R_factor_gt 0.023 _refine_ls_wR_factor_all 0.279 _refine_ls_wR_factor_ref 0.028 _refine_ls_goodness_of_fit_all 9.351 _refine_ls_goodness_of_fit_ref 0.941 _refine_ls_shift/su_max 0.005 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 0.372 _refine_diff_density_min -0.117 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol PD1 0.63257(2) 0.5538 0.61860(2) 0.01598(9) Uani ? ? Pd CR1 0.93412(4) 0.64951(2) 0.54315(4) 0.0195(2) Uani ? ? Cr C1 0.9389(3) 0.5428(2) 0.5340(3) 0.024(1) Uani ? ? C O1 0.9447(2) 0.4755(1) 0.5253(2) 0.034(1) Uani ? ? O C2 1.0950(3) 0.6497(2) 0.6249(3) 0.030(2) Uani ? ? C O2 1.1965(2) 0.6497(2) 0.6744(2) 0.043(1) Uani ? ? O C3 0.9925(3) 0.6521(2) 0.4062(3) 0.029(1) Uani ? ? C O3 1.0301(2) 0.6517(1) 0.3199(2) 0.048(1) Uani ? ? O C4 0.8201(2) 0.6733(2) 0.6808(3) 0.020(1) Uani ? ? C C5 0.7406(2) 0.6394(1) 0.5809(3) 0.017(1) Uani ? ? C C6 0.7359(3) 0.6770(2) 0.4713(3) 0.022(1) Uani ? ? C C7 0.8068(3) 0.7440(2) 0.4609(3) 0.027(1) Uani ? ? C C8 0.8854(3) 0.7759(2) 0.5614(3) 0.025(1) Uani ? ? C C9 0.8929(3) 0.7400(2) 0.6711(3) 0.023(1) Uani ? ? C C10 0.8192(2) 0.6380(1) 0.7980(3) 0.018(1) Uani ? ? C C11 0.8997(3) 0.6577(2) 0.9036(3) 0.023(1) Uani ? ? C C12 0.8902(3) 0.6214(2) 1.0084(3) 0.029(2) Uani ? ? C C13 0.8002(3) 0.5644(2) 1.0042(3) 0.027(1) Uani ? ? C C14 0.7249(3) 0.5466(2) 0.8973(3) 0.026(1) Uani ? ? C N1 0.7302(2) 0.5827(1) 0.7953(2) 0.019(1) Uani ? ? N C15 0.5727(2) 0.5153(1) 0.4534(3) 0.018(1) Uani ? ? C C16 0.6399(3) 0.5054(2) 0.3650(3) 0.021(1) Uani ? ? C C17 0.5923(3) 0.4621(2) 0.2635(3) 0.026(1) Uani ? ? C C18 0.4793(3) 0.4266(2) 0.2491(3) 0.031(2) Uani ? ? C C19 0.4110(3) 0.4354(2) 0.3345(3) 0.029(2) Uani ? ? C C20 0.4561(3) 0.4801(2) 0.4358(3) 0.022(1) Uani ? ? C C21 0.3866(3) 0.4931(2) 0.5334(3) 0.024(1) Uani ? ? C C22 0.2699(3) 0.4449(3) 0.5235(3) 0.045(2) Uani ? ? C N2 0.4784(2) 0.4844(1) 0.6498(2) 0.019(1) Uani ? ? N C23 0.4261(3) 0.5170(2) 0.7467(3) 0.028(1) Uani ? ? C C24 0.5119(3) 0.4010(2) 0.6750(3) 0.027(1) Uani ? ? C PD2 0.87817(2) 0.31142(1) 0.88417(2) 0.01695(9) Uani ? ? Pd CR2 0.57978(4) 0.20748(3) 0.95723(4) 0.0189(2) Uani ? ? Cr C25 0.5665(3) 0.3154(2) 0.9612(3) 0.026(1) Uani ? ? C O4 0.5562(2) 0.3838(1) 0.9684(2) 0.036(1) Uani ? ? O C26 0.4224(3) 0.2053(2) 0.8700(3) 0.029(2) Uani ? ? C O5 0.3227(2) 0.2034(2) 0.8154(2) 0.046(2) Uani ? ? O C27 0.5139(3) 0.2093(2) 1.0916(3) 0.026(1) Uani ? ? C O6 0.4743(2) 0.2120(1) 1.1750(2) 0.047(1) Uani ? ? O C28 0.6971(3) 0.1891(1) 0.8221(3) 0.020(1) Uani ? ? C C29 0.7739(2) 0.2257(2) 0.9235(3) 0.020(1) Uani ? ? C C30 0.7791(3) 0.1881(2) 1.0338(3) 0.021(1) Uani ? ? C C31 0.7115(3) 0.1186(2) 1.0435(3) 0.026(1) Uani ? ? C C32 0.6379(3) 0.0846(2) 0.9460(3) 0.025(1) Uani ? ? C C33 0.6283(3) 0.1198(2) 0.8354(3) 0.024(1) Uani ? ? C C34 0.6960(3) 0.2243(2) 0.7054(3) 0.020(1) Uani ? ? C C35 0.6169(3) 0.2022(2) 0.6018(3) 0.023(1) Uani ? ? C C36 0.6220(3) 0.2389(2) 0.4963(3) 0.025(1) Uani ? ? C C37 0.7077(3) 0.2979(2) 0.4987(3) 0.031(2) Uani ? ? C C38 0.7837(3) 0.3178(2) 0.6043(3) 0.027(1) Uani ? ? C N3 0.7816(2) 0.2814(1) 0.7077(2) 0.021(1) Uani ? ? N C39 0.9316(2) 0.3581(1) 1.0459(3) 0.018(1) Uani ? ? C C40 0.8652(3) 0.3621(2) 1.1360(3) 0.024(1) Uani ? ? C C41 0.9016(3) 0.4083(2) 1.2365(3) 0.026(1) Uani ? ? C C42 1.0070(3) 0.4533(2) 1.2487(3) 0.026(1) Uani ? ? C C43 1.0755(3) 0.4515(2) 1.1608(3) 0.027(1) Uani ? ? C C44 1.0390(3) 0.4033(2) 1.0619(3) 0.020(1) Uani ? ? C C45 1.1142(3) 0.3997(2) 0.9692(3) 0.022(1) Uani ? ? C C46 1.2107(3) 0.3340(2) 0.9968(3) 0.034(2) Uani ? ? C N4 1.0255(2) 0.3889(1) 0.8508(2) 0.020(1) Uani ? ? N C47 1.0889(3) 0.3575(2) 0.7611(3) 0.030(2) Uani ? ? C C48 0.9752(3) 0.4674(2) 0.8132(3) 0.029(2) Uani ? ? C H1 0.6833 0.6564 0.4024 0.0299 Uiso calc C6 H H2 0.8015 0.7680 0.3857 0.0354 Uiso calc C7 H H3 0.9329 0.8213 0.5546 0.0346 Uiso calc C8 H H4 0.9470 0.7603 0.7392 0.0300 Uiso calc C9 H H5 0.9613 0.6963 0.9037 0.0303 Uiso calc C11 H H6 0.9437 0.6350 1.0810 0.0395 Uiso calc C12 H H7 0.7909 0.5381 1.0743 0.0374 Uiso calc C13 H H8 0.6654 0.5064 0.8955 0.0336 Uiso calc C14 H H9 0.7191 0.5284 0.3743 0.0290 Uiso calc C16 H H10 0.6385 0.4570 0.2035 0.0362 Uiso calc C17 H H11 0.4484 0.3961 0.1805 0.0430 Uiso calc C18 H H12 0.3328 0.4109 0.3247 0.0396 Uiso calc C19 H H13 0.3533 0.5447 0.5271 0.0324 Uiso calc C21 H H14 0.2325 0.4567 0.5881 0.0698 Uiso calc C22 H H15 0.2145 0.4571 0.4513 0.0698 Uiso calc C22 H H16 0.2897 0.3906 0.5248 0.0698 Uiso calc C22 H H17 0.4839 0.5114 0.8195 0.0350 Uiso calc C23 H H18 0.4079 0.5710 0.7321 0.0350 Uiso calc C23 H H19 0.3529 0.4895 0.7509 0.0350 Uiso calc C23 H H20 0.5694 0.3973 0.7483 0.0349 Uiso calc C24 H H21 0.4403 0.3718 0.6793 0.0349 Uiso calc C24 H H22 0.5476 0.3805 0.6136 0.0349 Uiso calc C24 H H23 0.8292 0.2099 1.1031 0.0280 Uiso calc C30 H H24 0.7174 0.0950 1.1190 0.0338 Uiso calc C31 H H25 0.5940 0.0377 0.9538 0.0330 Uiso calc C32 H H26 0.5755 0.0976 0.7681 0.0316 Uiso calc C33 H H27 0.5587 0.1616 0.6031 0.0307 Uiso calc C35 H H28 0.5684 0.2240 0.4245 0.0359 Uiso calc C36 H H29 0.7141 0.3244 0.4279 0.0410 Uiso calc C37 H H30 0.8407 0.3594 0.6047 0.0343 Uiso calc C38 H H31 0.7922 0.3320 1.1282 0.0315 Uiso calc C40 H H32 0.8544 0.4090 1.2961 0.0344 Uiso calc C41 H H33 1.0327 0.4853 1.3168 0.0363 Uiso calc C42 H H34 1.1470 0.4831 1.1682 0.0360 Uiso calc C43 H H35 1.1597 0.4467 0.9670 0.0284 Uiso calc C45 H H36 1.2576 0.3326 0.9370 0.0447 Uiso calc C46 H H37 1.2636 0.3438 1.0713 0.0447 Uiso calc C46 H H38 1.1705 0.2850 0.9992 0.0447 Uiso calc C46 H H39 1.0315 0.3513 0.6882 0.0384 Uiso calc C47 H H40 1.1517 0.3930 0.7507 0.0384 Uiso calc C47 H H41 1.1244 0.3081 0.7865 0.0384 Uiso calc C47 H H42 0.9191 0.4632 0.7392 0.0379 Uiso calc C48 H H43 0.9339 0.4877 0.8707 0.0379 Uiso calc C48 H H44 1.0405 0.5016 0.8056 0.0379 Uiso calc C48 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol PD1 0.01548(9) 0.01806(8) 0.0146(1) -0.00225(7) 0.00366(8) -0.00020(8) Pd CR1 0.0200(2) 0.0206(2) 0.0179(2) -0.0029(2) 0.0049(2) 0.0013(2) Cr C1 0.026(1) 0.027(1) 0.020(2) -0.002(1) 0.008(1) 0.004(1) C O1 0.048(1) 0.0262(9) 0.031(1) 0.004(1) 0.012(1) 0.000(1) O C2 0.025(1) 0.036(1) 0.029(2) 0.000(1) 0.006(1) 0.002(2) C O2 0.027(1) 0.079(2) 0.036(1) 0.006(1) -0.000(1) 0.005(2) O C3 0.034(2) 0.024(1) 0.029(2) -0.007(1) 0.010(1) 0.003(1) C O3 0.078(2) 0.047(1) 0.031(1) -0.018(1) 0.034(1) -0.004(1) O C4 0.019(1) 0.019(1) 0.021(2) 0.001(1) 0.003(1) 0.000(1) C C5 0.014(1) 0.020(1) 0.018(1) -0.002(1) 0.003(1) 0.004(1) C C6 0.017(1) 0.029(1) 0.022(2) -0.003(1) 0.000(1) -0.001(1) C C7 0.031(2) 0.021(1) 0.030(2) 0.001(1) 0.007(1) 0.013(1) C C8 0.025(1) 0.019(1) 0.034(2) -0.009(1) 0.002(1) -0.002(1) C C9 0.025(1) 0.021(1) 0.022(2) -0.002(1) 0.003(1) 0.000(1) C C10 0.021(1) 0.016(1) 0.017(1) 0.004(1) 0.007(1) 0.001(1) C C11 0.020(1) 0.027(1) 0.022(2) -0.004(1) 0.003(1) -0.009(1) C C12 0.036(2) 0.030(1) 0.021(2) 0.003(1) -0.002(1) -0.004(1) C C13 0.038(2) 0.030(1) 0.017(2) 0.002(1) 0.004(1) 0.007(1) C C14 0.025(1) 0.030(1) 0.022(2) -0.000(1) 0.005(1) 0.013(1) C N1 0.019(1) 0.0215(9) 0.015(1) 0.0007(9) 0.0045(9) 0.001(1) N C15 0.018(1) 0.018(1) 0.019(1) 0.002(1) 0.003(1) 0.000(1) C C16 0.020(1) 0.025(1) 0.020(2) 0.001(1) -0.001(1) -0.000(1) C C17 0.035(2) 0.030(1) 0.017(1) 0.010(1) 0.002(1) -0.002(1) C C18 0.042(2) 0.029(1) 0.024(2) -0.002(1) -0.004(2) -0.006(1) C C19 0.030(2) 0.029(1) 0.027(2) -0.009(1) -0.006(1) 0.003(1) C C20 0.021(1) 0.026(1) 0.019(2) -0.002(1) 0.002(1) 0.003(1) C C21 0.019(1) 0.031(1) 0.025(2) -0.001(1) 0.004(1) 0.005(1) C C22 0.027(2) 0.095(3) 0.035(2) -0.035(2) -0.002(2) 0.010(2) C N2 0.016(1) 0.0201(9) 0.023(1) 0.0010(9) 0.0062(9) 0.005(1) N C23 0.025(1) 0.030(1) 0.030(2) -0.002(1) 0.014(1) -0.007(1) C C24 0.035(2) 0.021(1) 0.027(2) 0.001(1) 0.015(1) 0.005(1) C PD2 0.01715(9) 0.01856(8) 0.0153(1) -0.00031(7) 0.00573(8) 0.00125(8) Pd CR2 0.0199(2) 0.0216(2) 0.0156(2) -0.0012(2) 0.0050(2) 0.0016(2) Cr C25 0.031(1) 0.034(1) 0.017(2) 0.001(1) 0.008(1) 0.003(1) C O4 0.055(1) 0.0236(9) 0.036(1) 0.004(1) 0.015(1) 0.006(1) O C26 0.036(2) 0.044(2) 0.016(2) 0.007(1) 0.004(1) -0.009(1) C O5 0.026(1) 0.091(2) 0.039(2) 0.013(1) -0.009(1) -0.023(2) O C27 0.032(1) 0.022(1) 0.024(2) -0.002(1) 0.008(1) 0.001(1) C O6 0.061(1) 0.044(1) 0.038(1) 0.007(1) 0.031(1) 0.007(1) O C28 0.020(1) 0.021(1) 0.019(1) 0.003(1) 0.007(1) 0.002(1) C C29 0.018(1) 0.021(1) 0.020(1) 0.001(1) 0.008(1) -0.003(1) C C30 0.020(1) 0.024(1) 0.020(2) -0.001(1) 0.004(1) 0.006(1) C C31 0.027(1) 0.028(1) 0.023(2) 0.004(1) 0.006(1) 0.006(1) C C32 0.032(2) 0.018(1) 0.028(2) -0.001(1) 0.010(1) 0.010(1) C C33 0.027(1) 0.020(1) 0.028(2) -0.002(1) 0.008(1) -0.005(1) C C34 0.020(1) 0.025(1) 0.017(1) 0.001(1) 0.004(1) -0.005(1) C C35 0.029(2) 0.022(1) 0.020(2) 0.001(1) 0.004(1) 0.001(1) C C36 0.035(2) 0.035(1) 0.012(1) 0.001(1) 0.004(1) -0.005(1) C C37 0.045(2) 0.034(1) 0.019(2) 0.002(1) 0.015(1) 0.002(1) C C38 0.031(1) 0.026(1) 0.024(2) -0.003(1) 0.011(1) -0.004(1) C N3 0.025(1) 0.023(1) 0.016(1) 0.002(1) 0.007(1) -0.000(1) N C39 0.022(1) 0.019(1) 0.015(1) 0.002(1) 0.003(1) 0.003(1) C C40 0.022(1) 0.031(1) 0.020(2) 0.003(1) 0.005(1) 0.006(1) C C41 0.028(1) 0.035(1) 0.017(1) 0.007(1) 0.006(1) 0.000(1) C C42 0.033(2) 0.031(1) 0.018(2) 0.009(1) -0.000(1) -0.005(1) C C43 0.031(2) 0.026(1) 0.024(2) -0.002(1) -0.000(1) -0.003(1) C C44 0.021(1) 0.022(1) 0.018(1) 0.003(1) 0.001(1) 0.003(1) C C45 0.019(1) 0.022(1) 0.024(2) -0.003(1) 0.006(1) 0.000(1) C C46 0.026(2) 0.039(2) 0.038(2) 0.004(1) 0.005(1) -0.001(2) C N4 0.024(1) 0.0171(9) 0.020(1) -0.0015(9) 0.0100(9) -0.003(1) N C47 0.025(1) 0.037(1) 0.029(2) 0.001(1) 0.014(1) -0.005(1) C C48 0.038(2) 0.026(1) 0.025(2) 0.005(1) 0.009(1) 0.004(1) C # 10. 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 PD1 C5 1.994(4) . . ? PD1 N1 2.158(4) . . ? PD1 C15 1.995(4) . . ? PD1 N2 2.176(3) . . ? CR1 C1 1.822(4) . . ? CR1 C2 1.840(4) . . ? CR1 C3 1.834(5) . . ? CR1 C4 2.270(4) . . ? CR1 C5 2.292(4) . . ? CR1 C6 2.237(4) . . ? CR1 C7 2.222(4) . . ? CR1 C8 2.240(4) . . ? CR1 C9 2.248(4) . . ? PD2 C29 1.977(4) . . ? PD2 N3 2.157(4) . . ? PD2 C39 2.003(4) . . ? PD2 N4 2.200(3) . . ? CR2 C25 1.845(5) . . ? CR2 C26 1.828(4) . . ? CR2 C27 1.851(5) . . ? CR2 C28 2.258(4) . . ? CR2 C29 2.295(4) . . ? CR2 C30 2.233(4) . . ? CR2 C31 2.196(4) . . ? CR2 C32 2.203(4) . . ? CR2 C33 2.196(4) . . ? PD1 C5 1.994(4) . . ? PD1 C15 1.995(4) . . ? CR1 C1 1.822(4) . . ? CR1 C2 1.840(4) . . ? CR1 C3 1.834(5) . . ? C1 O1 1.155(5) . . ? C2 O2 1.153(5) . . ? C3 O3 1.160(5) . . ? C4 C5 1.421(6) . . ? C4 C9 1.413(5) . . ? C4 C10 1.484(6) . . ? C5 C6 1.411(6) . . ? C6 C7 1.408(6) . . ? C7 C8 1.408(6) . . ? C8 C9 1.394(6) . . ? C10 C11 1.395(6) . . ? C10 N1 1.363(5) . . ? C11 C12 1.383(7) . . ? C12 C13 1.388(6) . . ? C13 C14 1.373(6) . . ? C14 N1 1.342(5) . . ? C15 C16 1.398(6) . . ? C15 C20 1.405(5) . . ? C16 C17 1.392(6) . . ? C17 C18 1.373(6) . . ? C18 C19 1.374(7) . . ? C19 C20 1.399(6) . . ? C20 C21 1.513(6) . . ? C21 C22 1.520(5) . . ? C21 N2 1.515(6) . . ? N2 C23 1.474(6) . . ? N2 C24 1.481(5) . . ? PD2 C29 1.977(4) . . ? CR2 C25 1.845(5) . . ? CR2 C26 1.828(4) . . ? CR2 C27 1.851(5) . . ? C25 O4 1.175(6) . . ? C26 O5 1.156(5) . . ? C27 O6 1.142(5) . . ? C28 C29 1.439(6) . . ? C28 C33 1.431(5) . . ? C28 C34 1.473(6) . . ? C29 C30 1.418(6) . . ? C30 C31 1.420(6) . . ? C31 C32 1.374(6) . . ? C32 C33 1.396(6) . . ? C34 C35 1.380(6) . . ? C34 N3 1.358(5) . . ? C35 C36 1.382(6) . . ? C36 C37 1.382(6) . . ? C37 C38 1.373(6) . . ? C38 N3 1.352(6) . . ? C39 C40 1.399(6) . . ? C39 C44 1.401(5) . . ? C40 C41 1.391(6) . . ? C41 C42 1.383(6) . . ? C42 C43 1.392(6) . . ? C43 C44 1.397(6) . . ? C44 C45 1.492(6) . . ? C45 C46 1.538(5) . . ? C45 N4 1.521(6) . . ? N4 C47 1.471(6) . . ? N4 C48 1.479(5) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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 C5 PD1 N1 80.4(2) . . . ? C5 PD1 C15 97.3(2) . . . ? C5 PD1 N2 165.0(1) . . . ? N1 PD1 C15 168.6(1) . . . ? N1 PD1 N2 103.0(1) . . . ? C15 PD1 N2 82.2(2) . . . ? C1 CR1 C2 89.7(2) . . . ? C1 CR1 C3 87.4(2) . . . ? C1 CR1 C4 104.3(2) . . . ? C1 CR1 C5 88.6(2) . . . ? C1 CR1 C6 103.0(2) . . . ? C1 CR1 C7 136.2(2) . . . ? C1 CR1 C8 167.0(2) . . . ? C1 CR1 C9 137.3(2) . . . ? C2 CR1 C3 87.7(2) . . . ? C2 CR1 C4 105.5(2) . . . ? C2 CR1 C5 138.9(2) . . . ? C2 CR1 C6 165.3(2) . . . ? C2 CR1 C7 133.1(2) . . . ? C2 CR1 C8 100.3(2) . . . ? C2 CR1 C9 88.4(2) . . . ? C3 CR1 C4 162.2(2) . . . ? C3 CR1 C5 133.1(2) . . . ? C3 CR1 C6 100.1(2) . . . ? C3 CR1 C7 85.6(2) . . . ? C3 CR1 C8 101.2(2) . . . ? C3 CR1 C9 135.2(2) . . . ? C4 CR1 C5 36.3(1) . . . ? C4 CR1 C6 64.5(2) . . . ? C4 CR1 C7 76.7(2) . . . ? C4 CR1 C8 65.2(2) . . . ? C4 CR1 C9 36.4(1) . . . ? C5 CR1 C6 36.3(2) . . . ? C5 CR1 C7 66.2(1) . . . ? C5 CR1 C8 78.4(1) . . . ? C5 CR1 C9 66.2(1) . . . ? C6 CR1 C7 36.8(1) . . . ? C6 CR1 C8 66.1(2) . . . ? C6 CR1 C9 77.3(2) . . . ? C7 CR1 C8 36.8(2) . . . ? C7 CR1 C9 65.5(2) . . . ? C8 CR1 C9 36.2(2) . . . ? C29 PD2 N3 80.9(2) . . . ? C29 PD2 C39 98.7(2) . . . ? C29 PD2 N4 168.0(1) . . . ? N3 PD2 C39 165.3(1) . . . ? N3 PD2 N4 102.6(1) . . . ? C39 PD2 N4 80.8(1) . . . ? C25 CR2 C26 87.8(2) . . . ? C25 CR2 C27 85.1(2) . . . ? C25 CR2 C28 102.5(2) . . . ? C25 CR2 C29 87.3(2) . . . ? C25 CR2 C30 102.4(2) . . . ? C25 CR2 C31 136.4(2) . . . ? C25 CR2 C32 166.9(2) . . . ? C25 CR2 C33 136.5(2) . . . ? C26 CR2 C27 87.7(2) . . . ? C26 CR2 C28 104.0(2) . . . ? C26 CR2 C29 137.4(2) . . . ? C26 CR2 C30 166.4(2) . . . ? C26 CR2 C31 135.0(2) . . . ? C26 CR2 C32 101.9(2) . . . ? C26 CR2 C33 88.2(2) . . . ? C27 CR2 C28 166.1(2) . . . ? C27 CR2 C29 133.9(2) . . . ? C27 CR2 C30 101.9(2) . . . ? C27 CR2 C31 88.6(2) . . . ? C27 CR2 C32 103.8(2) . . . ? C27 CR2 C33 138.0(2) . . . ? C28 CR2 C29 36.8(1) . . . ? C28 CR2 C30 65.4(2) . . . ? C28 CR2 C31 77.9(2) . . . ? C28 CR2 C32 66.9(1) . . . ? C28 CR2 C33 37.5(1) . . . ? C29 CR2 C30 36.5(2) . . . ? C29 CR2 C31 66.9(1) . . . ? C29 CR2 C32 79.6(1) . . . ? C29 CR2 C33 67.4(1) . . . ? C30 CR2 C31 37.4(2) . . . ? C30 CR2 C32 66.6(2) . . . ? C30 CR2 C33 78.2(2) . . . ? C31 CR2 C32 36.4(2) . . . ? C31 CR2 C33 65.9(2) . . . ? C32 CR2 C33 37.0(2) . . . ? C5 PD1 C15 97.3(2) . . . ? C1 CR1 C2 89.7(2) . . . ? C1 CR1 C3 87.4(2) . . . ? C2 CR1 C3 87.7(2) . . . ? CR1 C1 O1 177.5(4) . . . ? CR1 C2 O2 178.9(4) . . . ? CR1 C3 O3 178.2(4) . . . ? C5 C4 C9 122.1(4) . . . ? C5 C4 C10 117.0(3) . . . ? C9 C4 C10 120.8(4) . . . ? PD1 C5 C4 114.9(3) . . . ? PD1 C5 C6 128.1(3) . . . ? C4 C5 C6 116.4(3) . . . ? C5 C6 C7 121.9(4) . . . ? C6 C7 C8 120.3(4) . . . ? C7 C8 C9 119.3(3) . . . ? C4 C9 C8 119.9(4) . . . ? C4 C10 C11 125.1(3) . . . ? C4 C10 N1 113.8(3) . . . ? C11 C10 N1 121.1(4) . . . ? C10 C11 C12 120.4(4) . . . ? C11 C12 C13 118.0(4) . . . ? C12 C13 C14 119.0(4) . . . ? C13 C14 N1 124.0(4) . . . ? C10 N1 C14 117.5(4) . . . ? PD1 C15 C16 128.1(3) . . . ? PD1 C15 C20 113.0(3) . . . ? C16 C15 C20 117.5(4) . . . ? C15 C16 C17 120.8(4) . . . ? C16 C17 C18 120.8(5) . . . ? C17 C18 C19 119.7(4) . . . ? C18 C19 C20 120.3(4) . . . ? C15 C20 C19 120.8(4) . . . ? C15 C20 C21 115.5(4) . . . ? C19 C20 C21 123.7(4) . . . ? C20 C21 C22 115.3(4) . . . ? C20 C21 N2 107.0(3) . . . ? C22 C21 N2 114.8(4) . . . ? C21 N2 C23 109.7(3) . . . ? C21 N2 C24 111.3(3) . . . ? C23 N2 C24 109.6(4) . . . ? C25 CR2 C26 87.8(2) . . . ? C25 CR2 C27 85.1(2) . . . ? C26 CR2 C27 87.7(2) . . . ? CR2 C25 O4 177.0(5) . . . ? CR2 C26 O5 179.5(5) . . . ? CR2 C27 O6 178.5(4) . . . ? C29 C28 C33 120.6(4) . . . ? C29 C28 C34 117.3(3) . . . ? C33 C28 C34 122.2(4) . . . ? PD2 C29 C28 114.2(3) . . . ? PD2 C29 C30 128.7(3) . . . ? C28 C29 C30 116.2(3) . . . ? C29 C30 C31 121.7(4) . . . ? C30 C31 C32 121.4(4) . . . ? C31 C32 C33 119.1(4) . . . ? C28 C33 C32 120.9(4) . . . ? C28 C34 C35 124.3(4) . . . ? C28 C34 N3 113.8(3) . . . ? C35 C34 N3 121.9(4) . . . ? C34 C35 C36 120.3(4) . . . ? C35 C36 C37 117.9(4) . . . ? C36 C37 C38 119.4(5) . . . ? C37 C38 N3 123.4(4) . . . ? C34 N3 C38 117.0(4) . . . ? C40 C39 C44 116.4(4) . . . ? C39 C40 C41 122.9(4) . . . ? C40 C41 C42 119.3(4) . . . ? C41 C42 C43 119.7(4) . . . ? C42 C43 C44 120.1(4) . . . ? C39 C44 C43 121.5(4) . . . ? C39 C44 C45 118.3(4) . . . ? C43 C44 C45 120.1(4) . . . ? C44 C45 C46 110.7(3) . . . ? C44 C45 N4 107.1(3) . . . ? C46 C45 N4 113.0(3) . . . ? C45 N4 C47 111.2(3) . . . ? C45 N4 C48 106.7(3) . . . ? C47 N4 C48 109.2(4) . . . ? #-----------------END data_pR3 _database_code_CSD 198826 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C20 H15 Cl3 Cr N2 O3 Pd' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C20 H15 Cl3 Cr N2 O3 Pd' _chemical_formula_weight 596.11 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1 Cr ? 0.284 0.624 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 Pd ? -1.177 1.007 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' _symmetry_space_group_name_Hall ' P 2yb' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,-z _cell_length_a 6.4747(2) _cell_length_b 12.4324(3) _cell_length_c 14.0935(5) _cell_angle_alpha 90 _cell_angle_beta 96.103(5) _cell_angle_gamma 90 _cell_volume 1128.04(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.75 _exptl_crystal_density_method none _exptl_crystal_F_000 588 _exptl_absorpt_coefficient_mu 1.658 _exptl_absorpt_correction_type refdelf_(Walker_&_Stuart,_1983) _exptl_absorpt_correction_T_min 0.9592 _exptl_absorpt_correction_T_max 1.0000 #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 6353 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 36. mm. Scan angle = 2.0 deg 1 scans of 50 sec per frame. Data collection was divided into 2 set(s) with the following starting angles and number of frames : Set 1 Theta = 8.80 Omega = 0.00 Kappa = 0.00 90 frames Set 2 Theta = -8.50 Kappa = -165.00 Phi = 0.00 15 frames Friedel pairs were averaged. Internal R = 0.04 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6353 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 30.04 _reflns_number_total 3451 _reflns_number_gt 2879 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack -0.04(5) _refine_ls_number_reflns 2879 _refine_ls_number_parameters 255 _refine_ls_number_restraints 1 _refine_ls_number_constraints 12 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_R_factor_all 0.049 _refine_ls_R_factor_gt 0.040 _refine_ls_wR_factor_all 0.663 _refine_ls_wR_factor_ref 0.057 _refine_ls_goodness_of_fit_all 13.275 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_shift/su_max 0.012 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 1.137 _refine_diff_density_min -0.866 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol PD 0.14400(5) 0.2750 0.17214(2) 0.0297(1) 1.000 Uani ? ? Pd CR -0.1062(1) 0.55527(9) 0.18650(7) 0.0348(4) 1.000 Uani ? ? Cr CL1 0.4170(3) 0.1457(1) 0.1815(1) 0.0511(8) 1.000 Uani ? ? Cl C1 0.108(1) 0.5397(6) 0.2834(5) 0.048(3) 1.000 Uani ? ? C O1 0.2317(8) 0.5280(5) 0.3463(3) 0.061(3) 1.000 Uani ? ? O C2 0.0569(9) 0.6520(5) 0.1269(5) 0.037(3) 1.000 Uani ? ? C O2 0.1638(7) 0.7091(5) 0.0907(4) 0.057(3) 1.000 Uani ? ? O C3 -0.203(1) 0.6686(6) 0.2552(4) 0.051(3) 1.000 Uani ? ? C O3 -0.270(1) 0.7353(5) 0.2978(4) 0.083(3) 1.000 Uani ? ? O N1 0.2021(7) 0.3381(4) 0.0442(3) 0.030(2) 1.000 Uani ? ? N C4 0.3596(9) 0.3118(5) -0.0047(4) 0.039(3) 1.000 Uani ? ? C C5 0.391(1) 0.3567(6) -0.0911(5) 0.045(3) 1.000 Uani ? ? C C6 0.250(1) 0.4338(5) -0.1289(5) 0.046(3) 1.000 Uani ? ? C C7 0.083(1) 0.4636(5) -0.0798(4) 0.037(3) 1.000 Uani ? ? C C8 0.0628(8) 0.4133(4) 0.0075(4) 0.029(2) 1.000 Uani ? ? C C9 -0.1010(9) 0.4373(5) 0.0699(4) 0.032(2) 1.000 Uani ? ? C C10 -0.2639(9) 0.5126(6) 0.0446(4) 0.039(3) 1.000 Uani ? ? C C11 -0.420(1) 0.5299(6) 0.1046(6) 0.050(4) 1.000 Uani ? ? C C12 -0.406(1) 0.4743(6) 0.1914(7) 0.057(4) 1.000 Uani ? ? C C13 -0.246(1) 0.3971(6) 0.2163(5) 0.049(3) 1.000 Uani ? ? C C14 -0.0883(8) 0.3778(5) 0.1566(4) 0.036(3) 1.000 Uani ? ? C N2 0.0808(9) 0.2241(5) 0.3033(4) 0.047(3) 1.000 Uani ? ? N C15 -0.093(1) 0.1675(7) 0.3140(6) 0.062(4) 1.000 Uani ? ? C C16 -0.116(1) 0.124(1) 0.4001(8) 0.101(6) 1.000 Uani ? ? C C17 0.000(4) 0.152(2) 0.4791(7) 0.13(1) 1.000 Uani ? ? C C18 0.185(2) 0.203(1) 0.4647(6) 0.100(7) 1.000 Uani ? ? C C19 0.213(2) 0.2443(9) 0.3775(6) 0.075(5) 1.000 Uani ? ? C C20 0.2721(7) 0.8249(5) 0.3865(4) 0.109(8) 0.500 Uiso ? ? C CL2 0.3045 0.9372 0.3093 0.095(2) 0.500 Uiso ? ? Cl CL3 0.3398 0.8882 0.5087 0.132(3) 0.500 Uiso ? ? Cl C21 0.373(1) 0.8832(6) 0.3566(4) 0.13(1) 0.500 Uiso ? ? C CL5 0.4280 0.9354 0.4804 0.115(2) 0.500 Uiso ? ? Cl Cl4 0.1703 0.8563 0.3159 0.188(4) 0.500 Uiso ? ? Cl H1 0.4554 0.2591 0.0215 0.0508 1.000 Uiso calc C4 H H2 0.5058 0.3358 -0.1238 0.0586 1.000 Uiso calc C5 H H3 0.2673 0.4663 -0.1886 0.0607 1.000 Uiso calc C6 H H4 -0.0137 0.5165 -0.1048 0.0517 1.000 Uiso calc C7 H H5 -0.2666 0.5515 -0.0135 0.0529 1.000 Uiso calc C10 H H6 -0.5317 0.5778 0.0869 0.0675 1.000 Uiso calc C11 H H7 -0.5056 0.4882 0.2349 0.0809 1.000 Uiso calc C12 H H8 -0.2453 0.3580 0.2742 0.0628 1.000 Uiso calc C13 H H9 -0.1979 0.1586 0.2620 0.0798 1.000 Uiso calc C15 H H10 -0.2198 0.0707 0.4040 0.1336 1.000 Uiso calc C16 H H11 -0.0400 0.1380 0.5409 0.2368 1.000 Uiso calc C17 H H12 0.2925 0.2085 0.5158 0.1505 1.000 Uiso calc C18 H H13 0.3302 0.2886 0.3707 0.1102 1.000 Uiso calc C19 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol PD 0.0333(1) 0.0270(1) 0.0290(1) 0.0008(2) 0.0014(1) 0.0011(2) Pd CR 0.0314(4) 0.0366(4) 0.0368(4) 0.0063(3) 0.0100(3) -0.0009(4) Cr CL1 0.0530(8) 0.0437(8) 0.0576(9) 0.0177(6) -0.0092(7) -0.0044(7) Cl C1 0.047(3) 0.054(4) 0.043(3) 0.011(3) 0.013(2) -0.006(3) C O1 0.068(3) 0.098(4) 0.035(2) 0.037(3) -0.004(2) -0.006(3) O C2 0.033(3) 0.037(3) 0.042(3) 0.004(2) 0.002(2) -0.001(2) C O2 0.053(3) 0.046(2) 0.075(3) -0.006(2) -0.001(2) 0.008(3) O C3 0.079(4) 0.052(4) 0.032(3) 0.020(3) 0.019(3) 0.002(3) C O3 0.117(4) 0.092(3) 0.054(3) 0.067(3) 0.003(3) -0.015(3) O N1 0.033(2) 0.029(2) 0.027(2) -0.004(2) 0.001(2) -0.005(2) N C4 0.045(3) 0.032(3) 0.040(3) 0.002(2) 0.009(2) -0.007(2) C C5 0.054(3) 0.046(3) 0.038(3) -0.004(3) 0.016(2) -0.007(3) C C6 0.068(4) 0.038(3) 0.037(3) -0.013(3) 0.017(3) -0.004(3) C C7 0.060(3) 0.037(3) 0.023(2) -0.004(3) 0.005(2) 0.000(2) C C8 0.033(2) 0.027(2) 0.027(2) 0.001(2) 0.004(2) -0.003(2) C C9 0.035(2) 0.031(2) 0.031(2) -0.002(2) 0.003(2) 0.000(2) C C10 0.030(2) 0.042(3) 0.049(3) -0.003(2) -0.004(2) -0.002(3) C C11 0.039(3) 0.045(3) 0.072(5) 0.006(3) 0.005(3) -0.005(3) C C12 0.033(2) 0.051(4) 0.109(5) 0.002(3) 0.035(3) -0.001(4) C C13 0.048(3) 0.050(4) 0.050(3) 0.000(3) 0.020(3) 0.003(3) C C14 0.034(2) 0.030(2) 0.045(3) -0.001(2) 0.008(2) 0.004(2) C N2 0.066(3) 0.043(3) 0.036(2) -0.001(3) 0.006(2) 0.015(2) N C15 0.057(3) 0.066(4) 0.065(4) -0.007(4) 0.021(3) 0.021(4) C C16 0.079(5) 0.119(6) 0.111(7) -0.037(4) 0.013(4) 0.058(5) C C17 0.30(2) 0.21(1) 0.037(5) -0.08(1) 0.014(8) 0.047(6) C C18 0.139(9) 0.16(1) 0.045(4) -0.055(8) 0.003(5) 0.031(6) C C19 0.117(7) 0.095(6) 0.039(4) -0.040(5) -0.010(4) 0.022(4) C # 10. 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 2.382(2) . . ? PD N1 2.039(5) . . ? PD C14 1.969(6) . . ? PD N2 2.036(6) . . ? CR C1 1.851(8) . . ? CR C2 1.859(7) . . ? CR C3 1.856(8) . . ? CR C9 2.206(6) . . ? CR C10 2.211(7) . . ? CR C11 2.250(8) . . ? CR C12 2.195(8) . . ? CR C13 2.223(8) . . ? CR C14 2.251(7) . . ? C1 O1 1.139(9) . . ? C2 O2 1.148(9) . . ? C3 O3 1.14(1) . . ? N1 C4 1.330(8) . . ? N1 C8 1.362(8) . . ? C4 C5 1.37(1) . . ? C5 C6 1.39(1) . . ? C6 C7 1.39(1) . . ? C7 C8 1.399(9) . . ? C8 C9 1.478(8) . . ? C9 C10 1.427(9) . . ? C9 C14 1.424(9) . . ? C10 C11 1.40(1) . . ? C11 C12 1.40(1) . . ? C12 C13 1.43(1) . . ? C13 C14 1.409(9) . . ? N2 C15 1.35(1) . . ? N2 C19 1.30(1) . . ? C15 C16 1.35(1) . . ? C16 C17 1.32(2) . . ? C17 C18 1.39(3) . . ? C18 C19 1.36(1) . . ? C20 CL2 1.796(7) . . ? C20 CL3 1.901(6) . . ? C20 C21 1.089(9) . . ? C20 Cl4 1.199(6) . . ? CL2 C21 1.013(8) . . ? CL2 Cl4 1.3386 . . ? C21 CL5 1.860(8) . . ? C21 Cl4 1.414(8) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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 N1 95.9(2) . . . ? CL1 PD C14 176.4(2) . . . ? CL1 PD N2 87.7(2) . . . ? N1 PD C14 82.1(2) . . . ? N1 PD N2 175.4(3) . . . ? C14 PD N2 94.5(3) . . . ? C1 CR C2 89.0(3) . . . ? C1 CR C3 87.9(3) . . . ? C1 CR C9 114.2(3) . . . ? C1 CR C10 151.7(3) . . . ? C1 CR C11 158.3(3) . . . ? C1 CR C12 121.7(4) . . . ? C1 CR C13 93.2(3) . . . ? C1 CR C14 89.2(3) . . . ? C2 CR C3 89.1(3) . . . ? C2 CR C9 92.2(3) . . . ? C2 CR C10 88.7(3) . . . ? C2 CR C11 112.6(3) . . . ? C2 CR C12 149.1(4) . . . ? C2 CR C13 156.9(3) . . . ? C2 CR C14 120.4(3) . . . ? C3 CR C9 157.9(3) . . . ? C3 CR C10 120.3(3) . . . ? C3 CR C11 92.2(4) . . . ? C3 CR C12 89.0(4) . . . ? C3 CR C13 114.0(3) . . . ? C3 CR C14 150.3(3) . . . ? C9 CR C10 37.7(2) . . . ? C9 CR C11 67.0(3) . . . ? C9 CR C12 78.6(3) . . . ? C9 CR C13 65.9(3) . . . ? C9 CR C14 37.2(2) . . . ? C10 CR C11 36.6(3) . . . ? C10 CR C12 66.0(3) . . . ? C10 CR C13 78.5(3) . . . ? C10 CR C14 67.9(3) . . . ? C11 CR C12 36.7(4) . . . ? C11 CR C13 67.0(3) . . . ? C11 CR C14 80.1(3) . . . ? C12 CR C13 37.8(3) . . . ? C12 CR C14 67.7(3) . . . ? C13 CR C14 36.7(2) . . . ? C4 N1 C8 119.0(5) . . . ? N1 C4 C5 123.7(7) . . . ? C4 C5 C6 117.7(6) . . . ? C5 C6 C7 120.4(7) . . . ? C6 C7 C8 118.0(7) . . . ? N1 C8 C7 121.3(6) . . . ? N1 C8 C9 113.7(5) . . . ? C7 C8 C9 125.0(6) . . . ? C8 C9 C10 122.9(6) . . . ? C8 C9 C14 115.2(5) . . . ? C10 C9 C14 121.9(6) . . . ? C9 C10 C11 120.8(6) . . . ? C10 C11 C12 117.9(7) . . . ? C11 C12 C13 121.5(7) . . . ? C12 C13 C14 121.4(7) . . . ? C9 C14 C13 116.4(6) . . . ? C15 N2 C19 119.8(8) . . . ? N2 C15 C16 118(1) . . . ? C15 C16 C17 123(1) . . . ? C16 C17 C18 114(1) . . . ? C17 C18 C19 120(1) . . . ? N2 C19 C18 120(1) . . . ? CL2 C20 CL3 101.3(3) . . . ? CL2 C20 C21 30.1(4) . . . ? CL2 C20 Cl4 48.2(2) . . . ? CL3 C20 C21 89.2(6) . . . ? CL3 C20 Cl4 132.1(5) . . . ? C21 C20 Cl4 76.1(6) . . . ? C20 CL2 C21 32.6(5) . . . ? C20 CL2 Cl4 41.9(2) . . . ? C21 CL2 Cl4 72.4(5) . . . ? C20 C21 CL2 117.3(8) . . . ? C20 C21 CL5 86.1(6) . . . ? C20 C21 Cl4 55.5(5) . . . ? CL2 C21 CL5 114.4(7) . . . ? CL2 C21 Cl4 64.5(4) . . . ? CL5 C21 Cl4 122.8(5) . . . ? C20 Cl4 CL2 89.9(3) . . . ? C20 Cl4 C21 48.4(4) . . . ? CL2 Cl4 C21 43.1(3) . . . ? #-----------------END data_pS3 _database_code_CSD 198827 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C20 H15 Cl3 Cr N2 O3 Pd' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C20 H15 Cl3 Cr N2 O3 Pd' _chemical_formula_weight 596.11 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 Cl ? 0.132 0.159 International_Tables_Vol_IV_Table_2.3.1 Cr ? 0.284 0.624 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 Pd ? -1.177 1.007 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall ' P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,-y,1/2+z -x,1/2+y,1/2-z 1/2+x,1/2-y,-z _cell_length_a 18.0316(3) _cell_length_b 18.0653(3) _cell_length_c 6.6008(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2150.19(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.84 _exptl_crystal_density_method none _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 1.739 _exptl_absorpt_correction_type refdelf_(Walker_&_Stuart,_1983) _exptl_absorpt_correction_T_min 0.9449 _exptl_absorpt_correction_T_max 1.0000 #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 6317 reflections were collected using program Collect ("Collect" Data collection software, Nonius B.V., 1998) The conditions were as follow : crystal to detector distance = 36. mm. Scan angle = 2.0 deg 1 scans of 70 sec per frame. Data collection was divided into 2 set(s) with the following starting angles and number of frames : Set 1 Theta = 8.80 Omega = 0.00 Kappa = 0.00 93 frames Set 2 Theta = -8.50 Kappa = -135.00 Phi = 0.00 53 frames Friedel pairs were averaged. Internal R = 0.04 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6317 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 30.03 _reflns_number_total 6317 _reflns_number_gt 5347 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack -0.05(5) _refine_ls_number_reflns 5347 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_R_factor_all 0.041 _refine_ls_R_factor_gt 0.030 _refine_ls_wR_factor_all 0.154 _refine_ls_wR_factor_ref 0.036 _refine_ls_goodness_of_fit_all 4.521 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_shift/su_max 0.003 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 0.893 _refine_diff_density_min -0.321 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol PD 0.59166(1) 0.85213(1) 0.44461(3) 0.01584(7) Uani ? ? Pd CR 0.40251(2) 0.88822(2) 0.69528(7) 0.0181(2) Uani ? ? Cr CL1 0.71882(4) 0.81290(4) 0.4400(1) 0.0263(3) Uani ? ? Cl C1 0.3776(2) 0.8084(2) 0.8571(5) 0.028(1) Uani ? ? C O1 0.3630(1) 0.7583(1) 0.9587(4) 0.040(1) Uani ? ? O C2 0.4806(2) 0.9068(2) 0.8671(5) 0.025(1) Uani ? ? C O2 0.5302(1) 0.9187(1) 0.9740(4) 0.039(1) Uani ? ? O C3 0.3433(2) 0.9460(2) 0.8562(5) 0.026(1) Uani ? ? C O3 0.3055(1) 0.9818(1) 0.9587(4) 0.041(1) Uani ? ? O N1 0.5485(1) 0.7486(1) 0.4489(4) 0.018(1) Uani ? ? N C4 0.5881(2) 0.6848(1) 0.4502(4) 0.023(1) Uani ? ? C C5 0.5546(2) 0.6163(2) 0.4505(5) 0.029(1) Uani ? ? C C6 0.4780(2) 0.6127(2) 0.4466(5) 0.031(1) Uani ? ? C C7 0.4372(2) 0.6767(2) 0.4450(5) 0.026(1) Uani ? ? C C8 0.4729(1) 0.7443(1) 0.4447(4) 0.018(1) Uani ? ? C C9 0.4371(1) 0.8168(1) 0.4378(4) 0.018(1) Uani ? ? C C10 0.3590(2) 0.8266(2) 0.4299(5) 0.025(1) Uani ? ? C C11 0.3285(2) 0.8974(2) 0.4269(5) 0.027(1) Uani ? ? C C12 0.3754(2) 0.9599(2) 0.4342(5) 0.026(1) Uani ? ? C C13 0.4526(1) 0.9506(1) 0.4392(5) 0.023(1) Uani ? ? C C14 0.4856(1) 0.8794(1) 0.4397(4) 0.018(1) Uani ? ? C N2 0.6283(1) 0.9584(1) 0.4288(4) 0.020(1) Uani ? ? N C15 0.6667(2) 0.9791(2) 0.2627(5) 0.025(1) Uani ? ? C C16 0.6989(2) 1.0484(2) 0.2450(5) 0.030(2) Uani ? ? C C17 0.6927(2) 1.0976(2) 0.4007(6) 0.030(2) Uani ? ? C C18 0.6550(2) 1.0771(2) 0.5740(6) 0.033(2) Uani ? ? C C19 0.6234(2) 1.0072(2) 0.5817(5) 0.029(1) Uani ? ? C C20 0.6308(2) 0.7378(2) -0.0540(6) 0.043(2) Uani ? ? C CL2 0.69022(6) 0.66115(7) -0.0585(2) 0.0616(6) Uani ? ? Cl CL3 0.53767(5) 0.71108(7) -0.0485(2) 0.0498(5) Uani ? ? Cl H1 0.6407 0.6875 0.4509 0.0305 Uiso calc C4 H H2 0.5836 0.5724 0.4533 0.0383 Uiso calc C5 H H3 0.4537 0.5660 0.4451 0.0408 Uiso calc C6 H H4 0.3846 0.6746 0.4440 0.0337 Uiso calc C7 H H5 0.3274 0.7845 0.4267 0.0325 Uiso calc C10 H H6 0.2762 0.9037 0.4200 0.0368 Uiso calc C11 H H7 0.3547 1.0083 0.4357 0.0340 Uiso calc C12 H H8 0.4836 0.9932 0.4422 0.0301 Uiso calc C13 H H9 0.6718 0.9449 0.1542 0.0323 Uiso calc C15 H H10 0.7251 1.0615 0.1255 0.0407 Uiso calc C16 H H11 0.7141 1.1455 0.3901 0.0445 Uiso calc C17 H H12 0.6507 1.1101 0.6854 0.0440 Uiso calc C18 H H13 0.5972 0.9932 0.7005 0.0374 Uiso calc C19 H H14 0.6393 0.7668 -0.1717 0.0620 Uiso calc C20 H H15 0.6413 0.7664 0.0633 0.0620 Uiso calc C20 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol PD 0.01417(8) 0.01597(8) 0.01757(7) -0.00053(8) 0.00061(9) -0.00050(8) Pd CR 0.0155(2) 0.0175(2) 0.0219(2) 0.0007(2) 0.0017(2) 0.0003(2) Cr CL1 0.0167(3) 0.0246(3) 0.0443(4) 0.0016(3) -0.0032(4) -0.0042(4) Cl C1 0.027(1) 0.028(1) 0.028(1) -0.001(1) 0.004(1) -0.007(1) C O1 0.051(1) 0.030(1) 0.043(1) -0.008(1) 0.011(1) 0.011(1) O C2 0.025(1) 0.028(1) 0.023(1) -0.003(1) 0.006(1) 0.003(1) C O2 0.034(1) 0.060(1) 0.030(1) -0.017(1) -0.006(1) 0.005(1) O C3 0.023(1) 0.022(1) 0.034(2) 0.000(1) 0.002(1) -0.001(1) C O3 0.038(1) 0.041(1) 0.045(1) 0.014(1) 0.013(1) -0.009(1) O N1 0.021(1) 0.017(1) 0.0158(9) -0.0013(9) 0.002(1) -0.000(1) N C4 0.024(1) 0.023(1) 0.023(1) 0.004(1) 0.002(1) -0.001(1) C C5 0.037(2) 0.020(1) 0.032(1) 0.003(1) -0.001(2) 0.001(2) C C6 0.036(2) 0.023(1) 0.035(1) -0.010(1) -0.001(2) 0.001(2) C C7 0.025(1) 0.025(1) 0.028(1) -0.006(1) -0.000(1) 0.000(1) C C8 0.019(1) 0.022(1) 0.015(1) -0.000(1) 0.000(1) -0.001(1) C C9 0.017(1) 0.021(1) 0.017(1) -0.002(1) -0.001(1) 0.001(1) C C10 0.020(1) 0.029(1) 0.026(1) -0.003(1) -0.001(1) -0.002(1) C C11 0.019(1) 0.035(1) 0.031(1) 0.007(1) -0.004(1) -0.003(1) C C12 0.024(1) 0.023(1) 0.031(1) 0.006(1) -0.003(1) 0.004(1) C C13 0.021(1) 0.024(1) 0.024(1) -0.002(1) 0.004(1) 0.006(1) C C14 0.016(1) 0.021(1) 0.016(1) 0.001(1) -0.001(1) 0.002(1) C N2 0.017(1) 0.019(1) 0.025(1) 0.0023(9) 0.000(1) 0.002(1) N C15 0.021(1) 0.025(1) 0.029(1) 0.003(1) 0.004(1) 0.004(1) C C16 0.024(1) 0.028(2) 0.042(2) -0.000(1) 0.007(1) 0.012(1) C C17 0.027(2) 0.017(1) 0.058(2) -0.003(1) 0.002(2) 0.005(1) C C18 0.036(2) 0.023(1) 0.042(2) -0.002(1) 0.000(2) -0.007(2) C C19 0.029(1) 0.026(1) 0.031(2) -0.004(1) 0.005(1) -0.001(1) C C20 0.073(2) 0.046(2) 0.023(1) -0.014(2) -0.006(2) -0.000(2) C CL2 0.0383(5) 0.0852(7) 0.0717(6) 0.0196(5) 0.0032(5) 0.0026(7) Cl CL3 0.0429(5) 0.1057(8) 0.0273(4) 0.0235(5) 0.0007(4) 0.0021(6) Cl # 10. 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 2.4001(7) . . ? PD N1 2.026(2) . . ? PD C14 1.975(3) . . ? PD N2 2.034(2) . . ? CR C1 1.850(4) . . ? CR C2 1.839(3) . . ? CR C3 1.833(3) . . ? CR C9 2.223(3) . . ? CR C10 2.219(3) . . ? CR C11 2.224(3) . . ? CR C12 2.211(4) . . ? CR C13 2.224(3) . . ? CR C14 2.262(3) . . ? C1 O1 1.157(4) . . ? C2 O2 1.160(4) . . ? C3 O3 1.157(4) . . ? N1 C4 1.355(4) . . ? N1 C8 1.365(3) . . ? C4 C5 1.376(4) . . ? C5 C6 1.384(5) . . ? C6 C7 1.371(5) . . ? C7 C8 1.380(4) . . ? C8 C9 1.462(4) . . ? C9 C10 1.419(4) . . ? C9 C14 1.430(4) . . ? C10 C11 1.394(4) . . ? C11 C12 1.412(4) . . ? C12 C13 1.402(4) . . ? C13 C14 1.417(4) . . ? N2 C15 1.349(4) . . ? N2 C19 1.343(4) . . ? C15 C16 1.386(5) . . ? C16 C17 1.363(5) . . ? C17 C18 1.382(5) . . ? C18 C19 1.385(5) . . ? C20 CL2 1.750(4) . . ? C20 CL3 1.748(5) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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 N1 95.43(7) . . . ? CL1 PD C14 176.83(9) . . . ? CL1 PD N2 88.16(7) . . . ? N1 PD C14 81.9(1) . . . ? N1 PD N2 175.8(1) . . . ? C14 PD N2 94.5(1) . . . ? C1 CR C2 88.4(1) . . . ? C1 CR C3 88.2(1) . . . ? C1 CR C9 93.3(1) . . . ? C1 CR C10 88.8(1) . . . ? C1 CR C11 111.9(1) . . . ? C1 CR C12 148.6(1) . . . ? C1 CR C13 158.9(1) . . . ? C1 CR C14 122.5(1) . . . ? C2 CR C3 89.1(1) . . . ? C2 CR C9 111.3(1) . . . ? C2 CR C10 148.1(1) . . . ? C2 CR C11 159.5(1) . . . ? C2 CR C12 122.9(1) . . . ? C2 CR C13 93.7(1) . . . ? C2 CR C14 88.0(1) . . . ? C3 CR C9 159.5(1) . . . ? C3 CR C10 122.5(1) . . . ? C3 CR C11 94.0(1) . . . ? C3 CR C12 89.4(1) . . . ? C3 CR C13 112.9(1) . . . ? C3 CR C14 149.1(1) . . . ? C9 CR C10 37.3(1) . . . ? C9 CR C11 66.6(1) . . . ? C9 CR C12 78.8(1) . . . ? C9 CR C13 66.4(1) . . . ? C9 CR C14 37.2(1) . . . ? C10 CR C11 36.6(1) . . . ? C10 CR C12 66.5(1) . . . ? C10 CR C13 78.3(1) . . . ? C10 CR C14 67.1(1) . . . ? C11 CR C12 37.1(1) . . . ? C11 CR C13 66.5(1) . . . ? C11 CR C14 79.0(1) . . . ? C12 CR C13 36.9(1) . . . ? C12 CR C14 66.8(1) . . . ? C13 CR C14 36.8(1) . . . ? C4 N1 C8 118.5(2) . . . ? N1 C4 C5 122.2(3) . . . ? C4 C5 C6 118.7(3) . . . ? C5 C6 C7 119.7(3) . . . ? C6 C7 C8 119.8(3) . . . ? N1 C8 C7 121.1(3) . . . ? N1 C8 C9 113.1(2) . . . ? C7 C8 C9 125.9(3) . . . ? C8 C9 C10 123.4(3) . . . ? C8 C9 C14 116.0(2) . . . ? C10 C9 C14 120.6(3) . . . ? C9 C10 C11 120.4(3) . . . ? C10 C11 C12 119.8(3) . . . ? C11 C12 C13 120.0(3) . . . ? C12 C13 C14 121.7(3) . . . ? C9 C14 C13 117.4(2) . . . ? C15 N2 C19 117.6(3) . . . ? N2 C15 C16 122.2(3) . . . ? C15 C16 C17 119.4(3) . . . ? C16 C17 C18 119.3(3) . . . ? C17 C18 C19 118.5(3) . . . ? N2 C19 C18 122.9(3) . . . ? CL2 C20 CL3 111.7(2) . . . ? #-----------------END