# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Kresimir Molcanov' _publ_contact_author_email Kresimir.Molcanov@irb.hr loop_ _publ_author_name D.Cincic M.Juribasic D.Babic K.Molcanov P.Sket J.Plavec M.CURIC data_manda-1novi-plocica1 _database_code_depnum_ccdc_archive 'CCDC 831717' #TrackingRef 'AAB-cifdoc.cif' _audit_creation_date 2010-10-15T14:25:06-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_moiety 'C48 H39 Cl2 N3 P2 Pd2' _chemical_formula_sum 'C48 H39 Cl2 N3 P2 Pd2' _chemical_formula_weight 1003.46 #------------------ UNIT CELL INFORMATION -----------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.6854(4) _cell_length_b 10.8731(3) _cell_length_c 42.8266(13) _cell_angle_alpha 90 _cell_angle_beta 96.989(2) _cell_angle_gamma 90 _cell_volume 9098.5(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10717 _cell_measurement_theta_min 3.1163 _cell_measurement_theta_max 76.199 #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.465 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4032 _exptl_absorpt_coefficient_mu 8.397 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.37475 _exptl_absorpt_correction_T_max 1 #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54179 _diffrn_radiation_type CuK\a _diffrn_radiation_probe x-ray _diffrn_measurement_device_type 'Xcalibur, Ruby' _diffrn_measurement_method '\w scans' _diffrn_reflns_number 19815 _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -53 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 4.16 _diffrn_reflns_theta_max 76.39 _diffrn_reflns_theta_full 76.39 _diffrn_measured_fraction_theta_max 0.974 _diffrn_measured_fraction_theta_full 0.974 _reflns_number_total 9302 _reflns_number_gt 8720 _reflns_threshold_expression >2sigma(I) #------------------ COMPUTER PROGRAMS USED ----------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #------------------ REFINEMENT INFORMATION ----------------------------------# _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^)+(0.0728P)^2^+310.2295P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 9302 _refine_ls_number_parameters 514 _refine_ls_number_restraints 12 _refine_ls_R_factor_gt 0.1036 _refine_ls_wR_factor_ref 0.2611 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.118 _refine_ls_shift/su_max 0 _refine_diff_density_max 2.609 _refine_diff_density_min -2.247 #------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group _atom_site_disorder_assembly Cl1 Cl 0.13218(13) 0.3120(3) 0.13239(7) 0.0565(7) Uani 1 d . . . Cl2 Cl 0.27889(16) 0.3528(3) 0.09709(8) 0.0654(8) Uani 1 d . . . P2 P 0.36319(14) 0.2966(3) 0.16990(8) 0.0608(8) Uani 1 d . . . C2 C 0.1794(5) -0.0797(8) 0.1271(3) 0.047(2) Uani 1 d . . . N1 N 0.1946(4) 0.0728(8) 0.1739(2) 0.0456(19) Uani 1 d . . . N2 N 0.2048(6) -0.0398(12) 0.1833(3) 0.070(3) Uani 1 d . . . C31 C 0.4056(7) 0.1847(15) 0.1480(3) 0.073(4) Uani 1 d . . . C3 C 0.1819(6) -0.1676(10) 0.1049(3) 0.060(3) Uani 1 d . . . H3 H 0.1731 -0.1432 0.084 0.071 Uiso 1 calc R . . C7 C 0.2001(6) 0.1626(12) 0.1985(3) 0.056(3) Uani 1 d . . . C1 C 0.1995(7) -0.1231(12) 0.1590(3) 0.062(3) Uani 1 d . . . C8 C 0.2234(6) 0.2776(13) 0.1921(3) 0.058(3) Uani 1 d . . . C4 C 0.1972(8) -0.2968(14) 0.1109(4) 0.082(4) Uani 1 d . . . C37 C 0.3826(6) 0.2375(18) 0.2102(3) 0.078(4) Uani 1 d . . . C6 C 0.2109(9) -0.2460(16) 0.1665(4) 0.091(5) Uani 1 d . . . H6 H 0.2195 -0.2701 0.1874 0.109 Uiso 1 calc R . . C43 C 0.4097(7) 0.4411(16) 0.1687(5) 0.097(6) Uani 1 d . . . C9 C 0.2257(7) 0.3678(16) 0.2154(4) 0.079(4) Uani 1 d . . . H9 H 0.2408 0.4468 0.2116 0.094 Uiso 1 calc R . . C12 C 0.1798(7) 0.1345(16) 0.2278(3) 0.074(4) Uani 1 d . . . H12 H 0.1643 0.056 0.2318 0.089 Uiso 1 calc R . . C32 C 0.4777(8) 0.1842(18) 0.1476(4) 0.090(5) Uani 1 d . . . H32 H 0.5044 0.2483 0.1568 0.108 Uiso 1 calc R . . C15 C 0.2944(8) 0.0602(15) 0.0377(5) 0.093(5) Uani 1 d . . . H15 H 0.3403 0.0483 0.0452 0.111 Uiso 1 calc R . . C36 C 0.3693(8) 0.0872(14) 0.1336(4) 0.080(4) Uani 1 d . . . H36 H 0.322 0.0859 0.1332 0.096 Uiso 1 calc R . . C11 C 0.1830(8) 0.2230(18) 0.2504(4) 0.083(5) Uani 1 d . . . H11 H 0.1697 0.2041 0.27 0.099 Uiso 1 calc R . . N3 N 0.1977(10) -0.3776(12) 0.0876(4) 0.137(8) Uani 1 d . . . H3B H 0.2056 -0.454 0.0918 0.164 Uiso 1 calc R . . H3A H 0.19 -0.3534 0.0684 0.164 Uiso 1 calc R . . C33 C 0.5083(10) 0.085(2) 0.1332(5) 0.113(7) Uani 1 d . . . H33 H 0.5555 0.0836 0.1329 0.136 Uiso 1 calc R . . C10 C 0.2051(8) 0.338(2) 0.2449(4) 0.097(6) Uani 1 d . . . H10 H 0.2066 0.3975 0.2606 0.116 Uiso 1 calc R . . C5 C 0.2096(9) -0.3325(16) 0.1430(4) 0.092(5) Uani 1 d . . . H5 H 0.2168 -0.415 0.1482 0.11 Uiso 1 calc R . . C16 C 0.2760(11) 0.0763(17) 0.0062(5) 0.106(7) Uani 1 d . . . H16 H 0.3093 0.0739 -0.0075 0.128 Uiso 1 calc R . . C17 C 0.2096(11) 0.0959(19) -0.0053(4) 0.107(7) Uani 1 d . . . H17 H 0.1969 0.1048 -0.0269 0.129 Uiso 1 calc R . . C38 C 0.3971(9) 0.1142(18) 0.2166(4) 0.091(5) Uani 1 d . . . H38 H 0.3985 0.059 0.2001 0.109 Uiso 1 calc R . . C42 C 0.3823(9) 0.315(2) 0.2352(5) 0.119(8) Uani 1 d . . . H42 H 0.3717 0.3976 0.2314 0.143 Uiso 1 calc R . . C35 C 0.4007(10) -0.0079(17) 0.1199(4) 0.106(7) Uani 1 d . . . H35 H 0.3751 -0.0731 0.1107 0.128 Uiso 1 calc R . . C34 C 0.4700(11) -0.005(2) 0.1201(4) 0.114(8) Uani 1 d . . . H34 H 0.4911 -0.0694 0.1106 0.137 Uiso 1 calc R . . C40 C 0.4056(11) 0.147(3) 0.2714(5) 0.123(8) Uani 1 d . . . H40 H 0.4085 0.1143 0.2916 0.147 Uiso 1 calc R . . C48 C 0.3832(10) 0.5284(17) 0.1509(6) 0.109(7) Uani 1 d . . . H48 H 0.3414 0.517 0.1386 0.131 Uiso 1 calc R . . C39 C 0.4091(10) 0.074(2) 0.2467(5) 0.111(7) Uani 1 d . . . H39 H 0.4203 -0.0083 0.2503 0.133 Uiso 1 calc R . . C41 C 0.3974(12) 0.275(3) 0.2663(5) 0.140(10) Uani 1 d . . . H41 H 0.4018 0.3303 0.283 0.168 Uiso 1 calc R . . C47 C 0.4186(14) 0.6430(19) 0.1501(7) 0.142(9) Uani 1 d . . . H47 H 0.399 0.7072 0.1378 0.17 Uiso 1 calc R . . C44 C 0.4709(15) 0.456(3) 0.1871(7) 0.153(9) Uani 1 d U . . H44 H 0.4912 0.3901 0.1987 0.183 Uiso 1 calc R . . C46 C 0.4834(14) 0.659(3) 0.1679(8) 0.183(15) Uani 1 d . . . H46 H 0.5107 0.7275 0.1656 0.219 Uiso 1 calc R . . C45 C 0.502(2) 0.571(4) 0.1880(10) 0.207(15) Uani 1 d U . . H45 H 0.5383 0.586 0.2037 0.248 Uiso 1 calc R . . Pd1 Pd 0.15931(4) 0.09754(8) 0.126159(18) 0.0456(2) Uani 1 d . . . Pd2 Pd 0.25226(4) 0.31295(8) 0.14979(2) 0.0502(2) Uani 1 d . . . P1 P 0.11442(13) 0.0938(3) 0.07444(6) 0.0461(6) Uani 1 d . . . C13 C 0.1784(6) 0.0845(11) 0.0468(3) 0.056(3) Uani 1 d . . . C19 C 0.0547(5) -0.0314(10) 0.0661(3) 0.049(2) Uani 1 d . . . C14 C 0.2460(6) 0.0612(14) 0.0588(4) 0.073(4) Uani 1 d . . . H14 H 0.2584 0.0468 0.0802 0.088 Uiso 1 calc R . . C22 C -0.0454(8) -0.2131(17) 0.0545(4) 0.088(5) Uani 1 d . . . H22 H -0.0783 -0.2745 0.0508 0.105 Uiso 1 calc R . . C23 C -0.0435(7) -0.1390(16) 0.0806(4) 0.081(4) Uani 1 d . . . H23 H -0.0764 -0.1485 0.0942 0.098 Uiso 1 calc R . . C20 C 0.0505(7) -0.1053(13) 0.0394(3) 0.066(3) Uani 1 d . . . H20 H 0.0815 -0.0941 0.0249 0.08 Uiso 1 calc R . . C21 C 0.0007(9) -0.1954(15) 0.0343(4) 0.084(4) Uani 1 d . . . H21 H -0.0007 -0.2447 0.0164 0.101 Uiso 1 calc R . . C30 C 0.0963(7) 0.3361(14) 0.0555(3) 0.070(4) Uani 1 d . . . H30 H 0.1438 0.3397 0.0595 0.084 Uiso 1 calc R . . C24 C 0.0070(6) -0.0506(13) 0.0869(3) 0.063(3) Uani 1 d . . . H24 H 0.0089 -0.0039 0.1052 0.075 Uiso 1 calc R . . C29 C 0.0599(8) 0.4391(12) 0.0450(4) 0.073(4) Uani 1 d . . . H29 H 0.083 0.5123 0.0424 0.087 Uiso 1 calc R . . C27 C -0.0425(7) 0.3314(16) 0.0432(4) 0.081(4) Uani 1 d . . . H27 H -0.09 0.3298 0.0395 0.097 Uiso 1 calc R . . C25 C 0.0634(6) 0.2297(10) 0.0600(2) 0.049(2) Uani 1 d . . . C26 C -0.0070(6) 0.2254(14) 0.0539(3) 0.069(3) Uani 1 d . . . H26 H -0.0304 0.1529 0.0569 0.083 Uiso 1 calc R . . C28 C -0.0088(8) 0.4358(14) 0.0383(3) 0.076(4) Uani 1 d . . . H28 H -0.0327 0.5051 0.0303 0.091 Uiso 1 calc R . . C18 C 0.1615(9) 0.1023(15) 0.0150(3) 0.083(4) Uani 1 d . . . H18 H 0.1163 0.119 0.0072 0.099 Uiso 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 Cl1 0.0445(13) 0.0511(15) 0.0723(17) -0.0063(13) 0.0005(11) 0.0143(12) Cl2 0.0563(16) 0.0638(18) 0.0784(19) 0.0068(15) 0.0174(14) 0.0026(14) P2 0.0358(14) 0.067(2) 0.079(2) -0.0085(16) 0.0048(13) -0.0053(13) C2 0.054(6) 0.013(4) 0.073(7) 0.007(4) 0.002(5) 0.000(4) N1 0.043(4) 0.041(5) 0.051(5) 0.006(4) -0.002(4) 0.003(4) N2 0.064(6) 0.078(8) 0.066(6) 0.028(6) 0.002(5) 0.011(6) C31 0.059(7) 0.094(11) 0.066(8) 0.004(8) 0.007(6) 0.020(8) C3 0.068(7) 0.027(5) 0.078(8) 0.001(5) -0.015(6) -0.002(5) C7 0.042(6) 0.066(8) 0.057(6) -0.002(6) 0.002(5) -0.001(5) C1 0.063(7) 0.054(7) 0.066(7) 0.009(6) -0.004(6) -0.006(6) C8 0.041(6) 0.078(9) 0.055(6) -0.017(6) -0.002(5) 0.007(6) C4 0.073(9) 0.059(9) 0.108(12) 0.000(8) -0.015(8) 0.020(7) C37 0.045(7) 0.121(14) 0.065(8) -0.023(9) -0.002(6) 0.005(8) C6 0.096(12) 0.079(11) 0.095(11) 0.045(10) -0.001(9) 0.016(9) C43 0.037(7) 0.066(10) 0.19(2) -0.017(11) 0.005(9) -0.012(7) C9 0.058(8) 0.091(11) 0.087(10) -0.036(8) 0.004(7) -0.009(7) C12 0.065(8) 0.105(12) 0.052(7) -0.005(7) 0.006(6) -0.004(8) C32 0.061(8) 0.110(13) 0.100(11) 0.022(10) 0.017(8) 0.025(9) C15 0.054(8) 0.076(10) 0.156(17) -0.012(11) 0.044(10) -0.006(7) C36 0.077(9) 0.066(9) 0.092(10) -0.014(8) -0.009(8) 0.019(8) C11 0.073(9) 0.111(14) 0.066(8) -0.019(9) 0.010(7) -0.003(9) N3 0.205(19) 0.046(8) 0.140(14) -0.033(8) -0.058(13) 0.033(10) C33 0.073(11) 0.17(2) 0.103(14) 0.012(14) 0.031(10) 0.050(13) C10 0.070(10) 0.145(18) 0.072(10) -0.041(11) -0.004(7) 0.015(11) C5 0.099(12) 0.065(10) 0.108(13) 0.034(10) 0.001(10) 0.008(9) C16 0.119(15) 0.079(12) 0.139(17) 0.025(11) 0.086(14) 0.019(11) C17 0.129(16) 0.116(15) 0.088(11) 0.036(11) 0.057(11) 0.029(13) C38 0.089(11) 0.097(13) 0.084(10) 0.020(9) 0.004(8) 0.011(10) C42 0.076(11) 0.17(2) 0.103(13) -0.043(14) -0.015(9) 0.037(13) C35 0.118(14) 0.089(12) 0.106(13) -0.027(10) -0.009(10) 0.065(11) C34 0.123(16) 0.127(17) 0.086(11) -0.025(11) -0.013(11) 0.082(14) C40 0.089(13) 0.20(3) 0.080(13) -0.003(16) 0.008(10) -0.020(17) C48 0.089(12) 0.067(11) 0.18(2) -0.020(12) 0.032(13) -0.044(10) C39 0.102(14) 0.139(19) 0.087(12) 0.028(13) -0.004(10) -0.002(13) C41 0.112(17) 0.23(3) 0.076(13) -0.042(17) -0.013(11) 0.01(2) C47 0.17(2) 0.063(12) 0.19(3) -0.008(14) 0.02(2) -0.008(14) C44 0.153(9) 0.153(9) 0.153(9) 0.0000(10) 0.0184(15) -0.0001(10) C46 0.12(2) 0.23(4) 0.20(3) -0.03(3) 0.03(2) -0.11(2) C45 0.207(15) 0.207(15) 0.207(15) 0.0000(10) 0.025(2) -0.0001(10) Pd1 0.0402(4) 0.0427(4) 0.0529(4) 0.0023(3) 0.0014(3) 0.0020(3) Pd2 0.0374(4) 0.0459(5) 0.0669(5) -0.0054(4) 0.0056(3) 0.0023(3) P1 0.0402(13) 0.0454(15) 0.0526(14) 0.0036(12) 0.0053(10) 0.0047(11) C13 0.049(6) 0.052(7) 0.067(7) 0.011(5) 0.013(5) -0.004(5) C19 0.044(5) 0.046(6) 0.054(6) 0.006(5) 0.001(4) 0.007(5) C14 0.049(7) 0.082(10) 0.090(10) 0.002(8) 0.018(6) -0.001(7) C22 0.070(10) 0.086(12) 0.104(12) 0.001(10) -0.002(9) -0.020(8) C23 0.048(7) 0.099(12) 0.096(11) 0.016(9) 0.006(7) -0.006(7) C20 0.068(8) 0.067(8) 0.064(7) -0.011(6) 0.009(6) 0.006(7) C21 0.093(11) 0.070(10) 0.083(10) -0.023(8) -0.011(8) -0.019(8) C30 0.054(7) 0.084(10) 0.070(8) 0.009(7) 0.001(6) 0.010(7) C24 0.056(7) 0.070(8) 0.064(7) 0.008(6) 0.015(6) -0.004(6) C29 0.086(10) 0.043(7) 0.090(10) 0.012(6) 0.014(8) 0.008(7) C27 0.051(7) 0.086(11) 0.105(12) -0.002(9) 0.008(7) 0.015(7) C25 0.056(6) 0.046(6) 0.047(5) 0.005(5) 0.008(5) 0.007(5) C26 0.048(7) 0.070(9) 0.087(9) 0.000(7) 0.005(6) 0.014(6) C28 0.084(10) 0.067(9) 0.076(9) 0.006(7) 0.008(7) 0.028(8) C18 0.092(10) 0.091(11) 0.070(8) 0.031(8) 0.029(8) 0.011(9) #------------------ MOLECULAR GEOMETRY --------------------------------------# _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 Cl1 Pd2 2.391(3) . ? Cl1 Pd1 2.414(3) . ? Cl2 Pd2 2.418(3) . ? P2 C31 1.802(15) . ? P2 C43 1.821(16) . ? P2 C37 1.838(16) . ? P2 Pd2 2.255(3) . ? C2 C3 1.355(16) . ? C2 C1 1.454(16) . ? C2 Pd1 1.967(9) . ? N1 N2 1.296(14) . ? N1 C7 1.430(15) . ? N1 Pd1 2.096(8) . ? N2 C1 1.373(18) . ? C31 C36 1.38(2) . ? C31 C32 1.422(19) . ? C3 C4 1.453(18) . ? C3 H3 0.93 . ? C7 C8 1.371(18) . ? C7 C12 1.395(17) . ? C1 C6 1.39(2) . ? C8 C9 1.397(17) . ? C8 Pd2 2.000(13) . ? C4 N3 1.33(2) . ? C4 C5 1.42(2) . ? C37 C42 1.36(2) . ? C37 C38 1.39(2) . ? C6 C5 1.37(2) . ? C6 H6 0.93 . ? C43 C48 1.29(3) . ? C43 C44 1.37(3) . ? C9 C10 1.41(2) . ? C9 H9 0.93 . ? C12 C11 1.36(2) . ? C12 H12 0.93 . ? C32 C33 1.41(3) . ? C32 H32 0.93 . ? C15 C16 1.36(3) . ? C15 C14 1.39(2) . ? C15 H15 0.93 . ? C36 C35 1.37(2) . ? C36 H36 0.93 . ? C11 C10 1.35(3) . ? C11 H11 0.93 . ? N3 H3B 0.86 . ? N3 H3A 0.86 . ? C33 C34 1.32(3) . ? C33 H33 0.93 . ? C10 H10 0.93 . ? C5 H5 0.93 . ? C16 C17 1.36(3) . ? C16 H16 0.93 . ? C17 C18 1.36(2) . ? C17 H17 0.93 . ? C38 C39 1.36(2) . ? C38 H38 0.93 . ? C42 C41 1.40(3) . ? C42 H42 0.93 . ? C35 C34 1.36(3) . ? C35 H35 0.93 . ? C34 H34 0.93 . ? C40 C39 1.33(3) . ? C40 C41 1.42(4) . ? C40 H40 0.93 . ? C48 C47 1.43(3) . ? C48 H48 0.93 . ? C39 H39 0.93 . ? C41 H41 0.93 . ? C47 C46 1.42(3) . ? C47 H47 0.93 . ? C44 C45 1.40(4) . ? C44 H44 0.93 . ? C46 C45 1.31(5) . ? C46 H46 0.93 . ? C45 H45 0.93 . ? Pd1 P1 2.283(3) . ? Pd1 Pd2 3.0673(11) . ? P1 C19 1.806(12) . ? P1 C13 1.832(12) . ? P1 C25 1.851(11) . ? C13 C18 1.377(18) . ? C13 C14 1.390(17) . ? C19 C24 1.388(16) . ? C19 C20 1.389(17) . ? C14 H14 0.93 . ? C22 C21 1.34(2) . ? C22 C23 1.38(2) . ? C22 H22 0.93 . ? C23 C24 1.384(19) . ? C23 H23 0.93 . ? C20 C21 1.38(2) . ? C20 H20 0.93 . ? C21 H21 0.93 . ? C30 C25 1.352(18) . ? C30 C29 1.376(18) . ? C30 H30 0.93 . ? C24 H24 0.93 . ? C29 C28 1.35(2) . ? C29 H29 0.93 . ? C27 C28 1.34(2) . ? C27 C26 1.40(2) . ? C27 H27 0.93 . ? C25 C26 1.378(16) . ? C26 H26 0.93 . ? C28 H28 0.93 . ? C18 H18 0.93 . ? 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 Pd2 Cl1 Pd1 79.35(8) . . ? C31 P2 C43 107.6(8) . . ? C31 P2 C37 101.3(7) . . ? C43 P2 C37 106.3(9) . . ? C31 P2 Pd2 110.0(5) . . ? C43 P2 Pd2 112.8(6) . . ? C37 P2 Pd2 117.9(4) . . ? C3 C2 C1 113.7(10) . . ? C3 C2 Pd1 134.5(9) . . ? C1 C2 Pd1 111.6(8) . . ? N2 N1 C7 114.9(10) . . ? N2 N1 Pd1 116.4(8) . . ? C7 N1 Pd1 128.1(7) . . ? N1 N2 C1 113.1(10) . . ? C36 C31 C32 117.0(15) . . ? C36 C31 P2 120.3(11) . . ? C32 C31 P2 122.3(13) . . ? C2 C3 C4 125.6(13) . . ? C2 C3 H3 117.2 . . ? C4 C3 H3 117.2 . . ? C8 C7 C12 121.2(13) . . ? C8 C7 N1 118.2(10) . . ? C12 C7 N1 120.5(12) . . ? N2 C1 C6 117.9(13) . . ? N2 C1 C2 119.0(11) . . ? C6 C1 C2 123.1(13) . . ? C7 C8 C9 118.6(13) . . ? C7 C8 Pd2 119.7(9) . . ? C9 C8 Pd2 121.7(12) . . ? N3 C4 C5 122.0(16) . . ? N3 C4 C3 121.7(15) . . ? C5 C4 C3 116.3(15) . . ? C42 C37 C38 117.6(18) . . ? C42 C37 P2 120.0(16) . . ? C38 C37 P2 122.4(12) . . ? C5 C6 C1 120.3(15) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? C48 C43 C44 121(2) . . ? C48 C43 P2 118.9(13) . . ? C44 C43 P2 120(2) . . ? C8 C9 C10 119.5(16) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C11 C12 C7 119.4(16) . . ? C11 C12 H12 120.3 . . ? C7 C12 H12 120.3 . . ? C33 C32 C31 119.2(19) . . ? C33 C32 H32 120.4 . . ? C31 C32 H32 120.4 . . ? C16 C15 C14 121.5(16) . . ? C16 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? C35 C36 C31 122.3(16) . . ? C35 C36 H36 118.8 . . ? C31 C36 H36 118.8 . . ? C10 C11 C12 121.2(16) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C4 N3 H3B 120 . . ? C4 N3 H3A 120 . . ? H3B N3 H3A 120 . . ? C34 C33 C32 120.1(17) . . ? C34 C33 H33 120 . . ? C32 C33 H33 120 . . ? C11 C10 C9 120.0(16) . . ? C11 C10 H10 120 . . ? C9 C10 H10 120 . . ? C6 C5 C4 120.4(15) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C17 C16 C15 120.5(15) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C18 119.2(17) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? C39 C38 C37 120(2) . . ? C39 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? C37 C42 C41 122(2) . . ? C37 C42 H42 118.9 . . ? C41 C42 H42 118.9 . . ? C34 C35 C36 119.0(19) . . ? C34 C35 H35 120.5 . . ? C36 C35 H35 120.5 . . ? C33 C34 C35 122.4(17) . . ? C33 C34 H34 118.8 . . ? C35 C34 H34 118.8 . . ? C39 C40 C41 119(2) . . ? C39 C40 H40 120.6 . . ? C41 C40 H40 120.6 . . ? C43 C48 C47 120(2) . . ? C43 C48 H48 120.2 . . ? C47 C48 H48 120.2 . . ? C40 C39 C38 123(2) . . ? C40 C39 H39 118.5 . . ? C38 C39 H39 118.5 . . ? C42 C41 C40 117(2) . . ? C42 C41 H41 121.3 . . ? C40 C41 H41 121.3 . . ? C46 C47 C48 120(3) . . ? C46 C47 H47 119.8 . . ? C48 C47 H47 119.8 . . ? C43 C44 C45 118(3) . . ? C43 C44 H44 120.8 . . ? C45 C44 H44 120.8 . . ? C45 C46 C47 115(3) . . ? C45 C46 H46 122.3 . . ? C47 C46 H46 122.3 . . ? C46 C45 C44 123(4) . . ? C46 C45 H45 118.4 . . ? C44 C45 H45 118.4 . . ? C2 Pd1 N1 79.1(4) . . ? C2 Pd1 P1 93.2(3) . . ? N1 Pd1 P1 171.0(3) . . ? C2 Pd1 Cl1 172.2(4) . . ? N1 Pd1 Cl1 93.9(3) . . ? P1 Pd1 Cl1 93.42(10) . . ? C2 Pd1 Pd2 129.1(3) . . ? N1 Pd1 Pd2 70.3(2) . . ? P1 Pd1 Pd2 118.59(8) . . ? Cl1 Pd1 Pd2 49.99(7) . . ? C8 Pd2 P2 90.4(3) . . ? C8 Pd2 Cl1 84.4(3) . . ? P2 Pd2 Cl1 173.57(13) . . ? C8 Pd2 Cl2 175.9(3) . . ? P2 Pd2 Cl2 93.48(12) . . ? Cl1 Pd2 Cl2 91.62(11) . . ? C8 Pd2 Pd1 85.9(4) . . ? P2 Pd2 Pd1 125.25(10) . . ? Cl1 Pd2 Pd1 50.66(7) . . ? Cl2 Pd2 Pd1 90.98(9) . . ? C19 P1 C13 108.2(5) . . ? C19 P1 C25 102.8(5) . . ? C13 P1 C25 102.5(5) . . ? C19 P1 Pd1 111.8(4) . . ? C13 P1 Pd1 114.3(4) . . ? C25 P1 Pd1 116.1(4) . . ? C18 C13 C14 119.7(12) . . ? C18 C13 P1 122.0(10) . . ? C14 C13 P1 118.3(10) . . ? C24 C19 C20 117.6(12) . . ? C24 C19 P1 117.5(9) . . ? C20 C19 P1 124.8(9) . . ? C13 C14 C15 117.5(15) . . ? C13 C14 H14 121.3 . . ? C15 C14 H14 121.3 . . ? C21 C22 C23 119.1(15) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? C22 C23 C24 120.9(14) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C21 C20 C19 120.8(13) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C22 C21 C20 121.3(15) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C25 C30 C29 120.2(13) . . ? C25 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C23 C24 C19 120.3(13) . . ? C23 C24 H24 119.8 . . ? C19 C24 H24 119.8 . . ? C28 C29 C30 121.2(14) . . ? C28 C29 H29 119.4 . . ? C30 C29 H29 119.4 . . ? C28 C27 C26 120.8(13) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C30 C25 C26 119.4(12) . . ? C30 C25 P1 118.7(9) . . ? C26 C25 P1 121.9(10) . . ? C25 C26 C27 119.1(14) . . ? C25 C26 H26 120.5 . . ? C27 C26 H26 120.5 . . ? C27 C28 C29 119.3(13) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? C17 C18 C13 121.6(16) . . ? C17 C18 H18 119.2 . . ? C13 C18 H18 119.2 . . ? 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 C7 N1 N2 C1 -179.6(10) . . . . ? Pd1 N1 N2 C1 8.6(13) . . . . ? C43 P2 C31 C36 -152.7(13) . . . . ? C37 P2 C31 C36 96.0(13) . . . . ? Pd2 P2 C31 C36 -29.4(14) . . . . ? C43 P2 C31 C32 34.5(16) . . . . ? C37 P2 C31 C32 -76.8(14) . . . . ? Pd2 P2 C31 C32 157.8(11) . . . . ? C1 C2 C3 C4 5.0(19) . . . . ? Pd1 C2 C3 C4 -179.1(11) . . . . ? N2 N1 C7 C8 148.5(11) . . . . ? Pd1 N1 C7 C8 -40.9(14) . . . . ? N2 N1 C7 C12 -33.7(15) . . . . ? Pd1 N1 C7 C12 136.9(10) . . . . ? N1 N2 C1 C6 178.6(13) . . . . ? N1 N2 C1 C2 -4.1(17) . . . . ? C3 C2 C1 N2 174.3(12) . . . . ? Pd1 C2 C1 N2 -2.6(15) . . . . ? C3 C2 C1 C6 -8.6(19) . . . . ? Pd1 C2 C1 C6 174.6(12) . . . . ? C12 C7 C8 C9 -0.9(18) . . . . ? N1 C7 C8 C9 176.9(10) . . . . ? C12 C7 C8 Pd2 179.7(9) . . . . ? N1 C7 C8 Pd2 -2.5(14) . . . . ? C2 C3 C4 N3 179.0(16) . . . . ? C2 C3 C4 C5 1(2) . . . . ? C31 P2 C37 C42 155.9(14) . . . . ? C43 P2 C37 C42 43.6(15) . . . . ? Pd2 P2 C37 C42 -84.1(14) . . . . ? C31 P2 C37 C38 -25.0(15) . . . . ? C43 P2 C37 C38 -137.3(14) . . . . ? Pd2 P2 C37 C38 95.0(13) . . . . ? N2 C1 C6 C5 -176.8(15) . . . . ? C2 C1 C6 C5 6(2) . . . . ? C31 P2 C43 C48 105.5(18) . . . . ? C37 P2 C43 C48 -146.7(18) . . . . ? Pd2 P2 C43 C48 -16(2) . . . . ? C31 P2 C43 C44 -76(2) . . . . ? C37 P2 C43 C44 32(2) . . . . ? Pd2 P2 C43 C44 162.7(17) . . . . ? C7 C8 C9 C10 0.8(19) . . . . ? Pd2 C8 C9 C10 -179.7(11) . . . . ? C8 C7 C12 C11 0(2) . . . . ? N1 C7 C12 C11 -177.4(12) . . . . ? C36 C31 C32 C33 -1(2) . . . . ? P2 C31 C32 C33 172.2(13) . . . . ? C32 C31 C36 C35 1(2) . . . . ? P2 C31 C36 C35 -172.0(14) . . . . ? C7 C12 C11 C10 0(2) . . . . ? C31 C32 C33 C34 0(3) . . . . ? C12 C11 C10 C9 0(3) . . . . ? C8 C9 C10 C11 0(2) . . . . ? C1 C6 C5 C4 1(3) . . . . ? N3 C4 C5 C6 177.9(18) . . . . ? C3 C4 C5 C6 -4(2) . . . . ? C14 C15 C16 C17 1(3) . . . . ? C15 C16 C17 C18 2(3) . . . . ? C42 C37 C38 C39 1(3) . . . . ? P2 C37 C38 C39 -178.0(14) . . . . ? C38 C37 C42 C41 1(3) . . . . ? P2 C37 C42 C41 -179.4(16) . . . . ? C31 C36 C35 C34 -1(3) . . . . ? C32 C33 C34 C35 0(3) . . . . ? C36 C35 C34 C33 1(3) . . . . ? C44 C43 C48 C47 0(4) . . . . ? P2 C43 C48 C47 179.0(17) . . . . ? C41 C40 C39 C38 -8(3) . . . . ? C37 C38 C39 C40 2(3) . . . . ? C37 C42 C41 C40 -7(3) . . . . ? C39 C40 C41 C42 10(4) . . . . ? C43 C48 C47 C46 2(4) . . . . ? C48 C43 C44 C45 5(4) . . . . ? P2 C43 C44 C45 -174(3) . . . . ? C48 C47 C46 C45 -10(5) . . . . ? C47 C46 C45 C44 16(6) . . . . ? C43 C44 C45 C46 -14(6) . . . . ? C3 C2 Pd1 N1 -170.8(13) . . . . ? C1 C2 Pd1 N1 5.1(8) . . . . ? C3 C2 Pd1 P1 13.9(12) . . . . ? C1 C2 Pd1 P1 -170.1(8) . . . . ? C3 C2 Pd1 Pd2 -117.7(12) . . . . ? C1 C2 Pd1 Pd2 58.3(10) . . . . ? N2 N1 Pd1 C2 -8.0(8) . . . . ? C7 N1 Pd1 C2 -178.6(9) . . . . ? N2 N1 Pd1 Cl1 168.4(8) . . . . ? C7 N1 Pd1 Cl1 -2.1(9) . . . . ? N2 N1 Pd1 Pd2 -146.8(9) . . . . ? C7 N1 Pd1 Pd2 42.7(8) . . . . ? Pd2 Cl1 Pd1 N1 60.1(2) . . . . ? Pd2 Cl1 Pd1 P1 -125.16(9) . . . . ? C7 C8 Pd2 P2 -102.0(9) . . . . ? C9 C8 Pd2 P2 78.6(10) . . . . ? C7 C8 Pd2 Cl1 74.2(9) . . . . ? C9 C8 Pd2 Cl1 -105.2(10) . . . . ? C7 C8 Pd2 Pd1 23.3(9) . . . . ? C9 C8 Pd2 Pd1 -156.1(10) . . . . ? C43 P2 Pd2 C8 -114.8(9) . . . . ? C37 P2 Pd2 C8 9.7(8) . . . . ? C31 P2 Pd2 Cl1 88.4(12) . . . . ? C31 P2 Pd2 Cl2 -53.9(6) . . . . ? C43 P2 Pd2 Cl2 66.2(8) . . . . ? C37 P2 Pd2 Cl2 -169.3(7) . . . . ? C31 P2 Pd2 Pd1 39.8(6) . . . . ? C43 P2 Pd2 Pd1 159.9(8) . . . . ? C37 P2 Pd2 Pd1 -75.6(7) . . . . ? Pd1 Cl1 Pd2 C8 -89.3(4) . . . . ? Pd1 Cl1 Pd2 Cl2 89.94(10) . . . . ? C2 Pd1 Pd2 C8 -83.8(6) . . . . ? N1 Pd1 Pd2 C8 -27.2(4) . . . . ? P1 Pd1 Pd2 C8 154.5(4) . . . . ? Cl1 Pd1 Pd2 C8 86.1(4) . . . . ? C2 Pd1 Pd2 P2 3.9(5) . . . . ? N1 Pd1 Pd2 P2 60.5(3) . . . . ? P1 Pd1 Pd2 P2 -117.89(14) . . . . ? Cl1 Pd1 Pd2 P2 173.76(15) . . . . ? C2 Pd1 Pd2 Cl1 -169.9(5) . . . . ? N1 Pd1 Pd2 Cl1 -113.3(3) . . . . ? P1 Pd1 Pd2 Cl1 68.36(13) . . . . ? C2 Pd1 Pd2 Cl2 98.8(4) . . . . ? N1 Pd1 Pd2 Cl2 155.4(3) . . . . ? P1 Pd1 Pd2 Cl2 -22.94(11) . . . . ? Cl1 Pd1 Pd2 Cl2 -91.29(12) . . . . ? C2 Pd1 P1 C19 47.1(5) . . . . ? Cl1 Pd1 P1 C19 -128.8(4) . . . . ? Pd2 Pd1 P1 C19 -174.3(4) . . . . ? C2 Pd1 P1 C13 -76.3(5) . . . . ? Cl1 Pd1 P1 C13 107.9(4) . . . . ? Pd2 Pd1 P1 C13 62.4(4) . . . . ? C2 Pd1 P1 C25 164.6(5) . . . . ? Cl1 Pd1 P1 C25 -11.3(4) . . . . ? Pd2 Pd1 P1 C25 -56.8(4) . . . . ? C19 P1 C13 C18 66.0(13) . . . . ? C25 P1 C13 C18 -42.2(13) . . . . ? Pd1 P1 C13 C18 -168.8(11) . . . . ? C19 P1 C13 C14 -115.4(11) . . . . ? C25 P1 C13 C14 136.4(11) . . . . ? Pd1 P1 C13 C14 9.9(12) . . . . ? C13 P1 C19 C24 172.0(9) . . . . ? C25 P1 C19 C24 -80.0(10) . . . . ? Pd1 P1 C19 C24 45.3(10) . . . . ? C13 P1 C19 C20 -11.9(12) . . . . ? C25 P1 C19 C20 96.1(11) . . . . ? Pd1 P1 C19 C20 -138.6(10) . . . . ? C18 C13 C14 C15 2(2) . . . . ? P1 C13 C14 C15 -177.0(11) . . . . ? C16 C15 C14 C13 -3(2) . . . . ? C21 C22 C23 C24 -3(3) . . . . ? C24 C19 C20 C21 -0.6(19) . . . . ? P1 C19 C20 C21 -176.8(11) . . . . ? C23 C22 C21 C20 1(3) . . . . ? C19 C20 C21 C22 1(2) . . . . ? C22 C23 C24 C19 3(2) . . . . ? C20 C19 C24 C23 -1.3(19) . . . . ? P1 C19 C24 C23 175.2(11) . . . . ? C25 C30 C29 C28 -1(2) . . . . ? C29 C30 C25 C26 0(2) . . . . ? C29 C30 C25 P1 -179.6(11) . . . . ? C19 P1 C25 C30 -164.1(10) . . . . ? C13 P1 C25 C30 -51.9(11) . . . . ? Pd1 P1 C25 C30 73.5(10) . . . . ? C19 P1 C25 C26 16.2(11) . . . . ? C13 P1 C25 C26 128.4(11) . . . . ? Pd1 P1 C25 C26 -106.2(10) . . . . ? C30 C25 C26 C27 0(2) . . . . ? P1 C25 C26 C27 179.7(11) . . . . ? C28 C27 C26 C25 1(2) . . . . ? C26 C27 C28 C29 -3(2) . . . . ? C30 C29 C28 C27 3(2) . . . . ? C16 C17 C18 C13 -3(3) . . . . ? C14 C13 C18 C17 1(2) . . . . ? P1 C13 C18 C17 179.6(14) . . . . ? # Attachment 'AZB-cifdoc.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-10-14 at 17:35:48 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\program files\wingx\files\cifdoc.dat # CIF files read : manda-c2abtpp manda-c2abtpp-info struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_manda-c2abtpp _database_code_depnum_ccdc_archive 'CCDC 831718' #TrackingRef 'AZB-cifdoc.cif' _audit_creation_date 2010-10-14T17:35:48-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_moiety 'C48 H38 Cl2 N2 P2 Pd2, C2 H6 O' _chemical_formula_sum 'C50 H44 Cl2 N2 O P2 Pd2' _chemical_formula_weight 1034.51 #------------------ UNIT CELL INFORMATION -----------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' 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 11.62710(10) _cell_length_b 9.02440(10) _cell_length_c 43.0468(4) _cell_angle_alpha 90 _cell_angle_beta 95.9830(10) _cell_angle_gamma 90 _cell_volume 4492.19(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 16686 _cell_measurement_theta_min 3.0933 _cell_measurement_theta_max 76.0964 #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.53 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2088 _exptl_absorpt_coefficient_mu 8.532 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.40374 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type CuK\a _diffrn_measurement_device_type 'Oxford Xcalibur Nova' _diffrn_measurement_method ; CCD detector ; _diffrn_radiation_probe x-ray _diffrn_reflns_number 22989 _diffrn_reflns_av_R_equivalents 0.0461 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -54 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_theta_min 3.85 _diffrn_reflns_theta_max 76.21 _diffrn_reflns_theta_full 76.21 _diffrn_measured_fraction_theta_max 0.979 _diffrn_measured_fraction_theta_full 0.979 _reflns_number_total 9219 _reflns_number_gt 8513 _reflns_threshold_expression >2sigma(I) #------------------ COMPUTER PROGRAMS USED ----------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #------------------ REFINEMENT INFORMATION ----------------------------------# _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^)+(0.0312P)^2^+51.5395P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 9219 _refine_ls_number_parameters 561 _refine_ls_number_restraints 7 _refine_ls_R_factor_gt 0.064 _refine_ls_wR_factor_ref 0.1804 _refine_ls_goodness_of_fit_ref 1.201 _refine_ls_restrained_S_all 1.206 _refine_ls_shift/su_max 0.001 _refine_diff_density_max 1.271 _refine_diff_density_min -0.996 #------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group _atom_site_disorder_assembly Pd1 Pd 0.77816(5) 0.05941(6) 0.126600(13) 0.03364(15) Uani 1 d . . . Pd2 Pd 1.02167(5) 0.18415(6) 0.146607(13) 0.03450(15) Uani 1 d . . . P1 P 0.71713(18) 0.0442(2) 0.07459(5) 0.0371(4) Uani 1 d . . . P2 P 1.15603(17) 0.0441(2) 0.17369(5) 0.0373(4) Uani 1 d . . . Cl1 Cl 0.85364(18) 0.3061(2) 0.12167(5) 0.0441(4) Uani 1 d . . . Cl2 Cl 1.0957(2) 0.1246(3) 0.09820(5) 0.0557(5) Uani 1 d . . . N1 N 0.8136(5) 0.0571(7) 0.17574(14) 0.0327(13) Uani 1 d . . . N2 N 0.7793(6) -0.0544(8) 0.18999(16) 0.0425(15) Uani 1 d . . . C1 C 0.7353(8) -0.1651(9) 0.1694(2) 0.0442(19) Uani 1 d . . . C2 C 0.7260(6) -0.1440(8) 0.13651(19) 0.0364(16) Uani 1 d . . . C3 C 0.6875(8) -0.2642(9) 0.1188(2) 0.0458(19) Uani 1 d . . . H3 H 0.6797 -0.2553 0.0972 0.055 Uiso 1 calc R . . C4 C 0.6597(9) -0.3983(11) 0.1319(3) 0.060(3) Uani 1 d . . . H4 H 0.6353 -0.4774 0.119 0.072 Uiso 1 calc R . . C5 C 0.6682(12) -0.4145(11) 0.1638(3) 0.075(3) Uani 1 d . . . H5 H 0.6484 -0.504 0.1725 0.09 Uiso 1 calc R . . C6 C 0.7059(11) -0.2988(11) 0.1827(2) 0.067(3) Uani 1 d . . . H6 H 0.7118 -0.3094 0.2043 0.08 Uiso 1 calc R . . C7 C 0.8604(7) 0.1786(9) 0.19457(17) 0.0373(16) Uani 1 d . . . C8 C 0.9571(7) 0.2464(9) 0.18566(18) 0.0378(17) Uani 1 d . . . C9 C 1.0020(8) 0.3676(10) 0.2032(2) 0.048(2) Uani 1 d . . . H9 H 1.0688 0.4142 0.1981 0.058 Uiso 1 calc R . . C10 C 0.9473(10) 0.4181(11) 0.2281(2) 0.059(3) Uani 1 d . . . H10 H 0.9766 0.5002 0.2393 0.071 Uiso 1 calc R . . C11 C 0.8502(10) 0.3488(12) 0.2365(2) 0.058(3) Uani 1 d . . . H11 H 0.8136 0.3846 0.2532 0.07 Uiso 1 calc R . . C12 C 0.8073(8) 0.2264(11) 0.2203(2) 0.050(2) Uani 1 d . . . H12 H 0.7435 0.1761 0.2264 0.06 Uiso 1 calc R . . C13 C 0.5707(7) -0.0289(9) 0.06618(19) 0.0410(18) Uani 1 d . . . C14 C 0.4917(8) 0.0019(12) 0.0869(2) 0.055(2) Uani 1 d . . . H14 H 0.515 0.0543 0.1051 0.066 Uiso 1 calc R . . C15 C 0.3776(10) -0.0442(15) 0.0811(3) 0.072(3) Uani 1 d . . . H15 H 0.3244 -0.02 0.095 0.086 Uiso 1 calc R . . C16 C 0.3438(9) -0.1242(14) 0.0552(3) 0.073(3) Uani 1 d . . . H16 H 0.2674 -0.1555 0.0513 0.087 Uiso 1 calc R . . C17 C 0.4230(10) -0.1596(14) 0.0344(3) 0.071(3) Uani 1 d . . . H17 H 0.3999 -0.2167 0.0169 0.086 Uiso 1 calc R . . C18 C 0.5363(9) -0.1109(12) 0.0395(2) 0.055(2) Uani 1 d . . . H18 H 0.5887 -0.1328 0.0253 0.066 Uiso 1 calc R . . C19 C 0.8134(8) -0.0613(9) 0.0527(2) 0.0439(19) Uani 1 d . . . C20 C 0.8098(10) -0.0514(11) 0.0205(2) 0.057(2) Uani 1 d . . . H20 H 0.7543 0.0078 0.0094 0.069 Uiso 1 calc R . . C21 C 0.8879(12) -0.1286(13) 0.0047(3) 0.073(3) Uani 1 d . . . H21 H 0.885 -0.121 -0.0169 0.087 Uiso 1 calc R . . C22 C 0.9695(11) -0.2160(14) 0.0207(3) 0.076(3) Uani 1 d . . . H22 H 1.0213 -0.2692 0.0099 0.091 Uiso 1 calc R . . C23 C 0.9753(10) -0.2257(13) 0.0525(3) 0.070(3) Uani 1 d . . . H23 H 1.0319 -0.2843 0.0633 0.084 Uiso 1 calc R . . C24 C 0.8988(8) -0.1501(10) 0.0685(2) 0.052(2) Uani 1 d . . . H24 H 0.9035 -0.1577 0.0902 0.063 Uiso 1 calc R . . C25 C 0.7115(8) 0.2257(9) 0.05558(19) 0.0450(19) Uani 1 d . . . C26 C 0.6117(11) 0.3085(12) 0.0521(3) 0.066(3) Uani 1 d . . . H26 H 0.5431 0.2682 0.0576 0.079 Uiso 1 calc R . . C27 C 0.6127(12) 0.4521(14) 0.0404(3) 0.083(4) Uani 1 d . . . H27 H 0.5448 0.5074 0.0381 0.099 Uiso 1 calc R . . C28 C 0.7117(14) 0.5107(13) 0.0324(3) 0.082(4) Uani 1 d . . . H28 H 0.7121 0.6072 0.0249 0.099 Uiso 1 calc R . . C29 C 0.8109(12) 0.4306(13) 0.0353(3) 0.073(3) Uani 1 d . . . H29 H 0.8785 0.4716 0.0293 0.088 Uiso 1 calc R . . C30 C 0.8119(9) 0.2865(11) 0.0472(2) 0.055(2) Uani 1 d . . . H30 H 0.8802 0.2321 0.0495 0.066 Uiso 1 calc R . . C31 C 1.1489(8) -0.1431(9) 0.1576(2) 0.0440(19) Uani 1 d . . . C32 C 1.0413(9) -0.2085(10) 0.1520(3) 0.058(3) Uani 1 d . . . H32 H 0.9757 -0.1559 0.156 0.07 Uiso 1 calc R . . C33 C 1.0300(11) -0.3522(11) 0.1403(3) 0.067(3) Uani 1 d . . . H33 H 0.9572 -0.396 0.1374 0.08 Uiso 1 calc R . . C34 C 1.1226(11) -0.4282(11) 0.1333(3) 0.069(3) Uani 1 d . . . H34 H 1.1148 -0.5237 0.1252 0.082 Uiso 1 calc R . . C35 C 1.2281(12) -0.3633(12) 0.1382(3) 0.072(3) Uani 1 d . . . H35 H 1.2922 -0.4166 0.1332 0.087 Uiso 1 calc R . . C36 C 1.2456(8) -0.2222(11) 0.1503(2) 0.053(2) Uani 1 d . . . H36 H 1.3193 -0.1814 0.1534 0.063 Uiso 1 calc R . . C37 C 1.1447(8) 0.0221(10) 0.2157(2) 0.048(2) Uani 1 d . . . C38 C 1.0729(10) -0.0826(13) 0.2267(3) 0.064(3) Uani 1 d . . . H38 H 1.0351 -0.1504 0.2129 0.077 Uiso 1 calc R . . C39 C 1.0566(12) -0.0879(17) 0.2582(3) 0.087(4) Uani 1 d . . . H39 H 1.0057 -0.156 0.2655 0.104 Uiso 1 calc R . . C40 C 1.1174(13) 0.0102(17) 0.2786(3) 0.084(4) Uani 1 d . . . H40 H 1.1086 0.0061 0.2999 0.101 Uiso 1 calc R . . C41 C 1.1893(12) 0.1116(15) 0.2679(3) 0.078(3) Uani 1 d . . . H41 H 1.2311 0.1755 0.2818 0.094 Uiso 1 calc R . . C42 C 1.2006(10) 0.1200(13) 0.2367(2) 0.064(3) Uani 1 d . . . H42 H 1.247 0.1935 0.2294 0.077 Uiso 1 calc R . . C43 C 1.3041(6) 0.1061(9) 0.17250(19) 0.0392(17) Uani 1 d . . . C44 C 1.3288(7) 0.2221(10) 0.1531(2) 0.046(2) Uani 1 d . . . H44 H 1.2688 0.2705 0.1412 0.055 Uiso 1 calc R . . C45 C 1.4410(8) 0.2661(11) 0.1513(2) 0.052(2) Uani 1 d . . . H45 H 1.4569 0.3443 0.1383 0.062 Uiso 1 calc R . . C46 C 1.5289(7) 0.1942(11) 0.1686(2) 0.053(2) Uani 1 d . . . H46 H 1.6047 0.224 0.1672 0.064 Uiso 1 calc R . . C47 C 1.5084(7) 0.0801(12) 0.1881(2) 0.053(2) Uani 1 d . . . H47 H 1.5695 0.0327 0.1997 0.064 Uiso 1 calc R . . C48 C 1.3968(7) 0.0363(11) 0.1901(2) 0.049(2) Uani 1 d . . . H48 H 1.3822 -0.0409 0.2035 0.059 Uiso 1 calc R . . C49B C 0.297(3) 0.401(5) 0.0527(7) 0.089(13) Uani 0.41(3) d PD 2 A H49C H 0.2942 0.3213 0.0376 0.107 Uiso 0.41(3) calc PR 2 A H49D H 0.3608 0.4661 0.0489 0.107 Uiso 0.41(3) calc PR 2 A C50B C 0.183(6) 0.489(9) 0.0486(18) 0.18(5) Uani 0.41(3) d PD 2 A H50D H 0.1629 0.5097 0.0269 0.263 Uiso 0.41(3) calc PR 2 A H50E H 0.1923 0.5801 0.06 0.263 Uiso 0.41(3) calc PR 2 A H50F H 0.1229 0.4311 0.0564 0.263 Uiso 0.41(3) calc PR 2 A O1B O 0.317(3) 0.342(4) 0.0834(6) 0.114(13) Uani 0.41(3) d PD 2 A H1B H 0.2555 0.3401 0.0913 0.172 Uiso 0.41(3) calc PR 2 A C49A C 0.243(3) 0.362(5) 0.0513(13) 0.29(6) Uani 0.59(3) d PD 1 A H49A H 0.2636 0.3571 0.0301 0.354 Uiso 0.59(3) calc PR 1 A H49B H 0.2416 0.2626 0.0597 0.354 Uiso 0.59(3) calc PR 1 A O1A O 0.132(4) 0.430(5) 0.0517(10) 0.170(19) Uani 0.59(3) d PD 1 A H1A H 0.0962 0.3882 0.0646 0.255 Uiso 0.59(3) calc PRD 1 A C50A C 0.331(4) 0.457(5) 0.0715(10) 0.19(3) Uani 0.59(3) d PD 1 A H50A H 0.3702 0.5212 0.0583 0.288 Uiso 0.59(3) calc PR 1 A H50B H 0.3855 0.3941 0.0832 0.288 Uiso 0.59(3) calc PR 1 A H50C H 0.2909 0.5162 0.0856 0.288 Uiso 0.59(3) calc PR 1 A loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0335(3) 0.0286(3) 0.0383(3) -0.0020(2) 0.0015(2) -0.0010(2) Pd2 0.0303(3) 0.0318(3) 0.0411(3) 0.0002(2) 0.0022(2) -0.0025(2) P1 0.0402(10) 0.0331(10) 0.0375(10) -0.0024(8) 0.0020(8) 0.0011(8) P2 0.0307(9) 0.0348(10) 0.0460(11) 0.0019(8) 0.0018(8) -0.0022(8) Cl1 0.0470(11) 0.0305(9) 0.0520(11) 0.0029(8) -0.0076(8) -0.0010(8) Cl2 0.0476(12) 0.0699(15) 0.0508(11) -0.0044(11) 0.0109(9) 0.0015(11) N1 0.025(3) 0.034(3) 0.040(3) -0.001(3) 0.004(2) 0.000(3) N2 0.042(4) 0.039(4) 0.047(4) 0.000(3) 0.008(3) -0.004(3) C1 0.052(5) 0.034(4) 0.047(4) -0.002(4) 0.009(4) -0.004(4) C2 0.027(4) 0.032(4) 0.051(4) -0.004(3) 0.004(3) 0.004(3) C3 0.044(5) 0.037(4) 0.056(5) -0.002(4) -0.001(4) -0.004(4) C4 0.066(7) 0.043(5) 0.071(7) -0.007(5) 0.002(5) -0.015(5) C5 0.109(10) 0.037(5) 0.081(8) 0.006(5) 0.018(7) -0.025(6) C6 0.104(9) 0.041(5) 0.055(6) 0.005(4) 0.011(6) -0.014(6) C7 0.042(4) 0.033(4) 0.036(4) -0.002(3) -0.002(3) 0.000(3) C8 0.035(4) 0.037(4) 0.041(4) -0.001(3) 0.000(3) 0.005(3) C9 0.045(5) 0.044(5) 0.055(5) -0.008(4) 0.003(4) -0.007(4) C10 0.074(7) 0.051(6) 0.051(5) -0.015(4) 0.000(5) -0.009(5) C11 0.074(7) 0.057(6) 0.046(5) -0.015(4) 0.011(4) 0.003(5) C12 0.046(5) 0.055(5) 0.050(5) -0.005(4) 0.007(4) -0.006(4) C13 0.038(4) 0.040(4) 0.045(4) 0.001(3) 0.001(3) 0.005(3) C14 0.045(5) 0.068(6) 0.053(5) -0.006(5) 0.008(4) 0.003(5) C15 0.051(6) 0.092(9) 0.073(7) 0.009(6) 0.011(5) 0.010(6) C16 0.033(5) 0.084(8) 0.098(9) 0.009(7) -0.005(5) -0.008(5) C17 0.056(6) 0.078(8) 0.074(7) -0.010(6) -0.020(5) -0.006(6) C18 0.052(5) 0.063(6) 0.048(5) -0.006(4) -0.002(4) 0.001(5) C19 0.044(5) 0.036(4) 0.052(5) -0.007(4) 0.009(4) -0.001(4) C20 0.070(7) 0.051(5) 0.052(5) 0.000(4) 0.014(5) 0.005(5) C21 0.097(9) 0.064(7) 0.063(6) -0.011(6) 0.037(6) -0.010(7) C22 0.075(8) 0.064(7) 0.096(9) -0.018(7) 0.044(7) 0.005(6) C23 0.053(6) 0.062(7) 0.097(9) -0.010(6) 0.017(6) 0.011(5) C24 0.049(5) 0.045(5) 0.063(6) -0.005(4) 0.007(4) 0.004(4) C25 0.059(5) 0.033(4) 0.042(4) -0.001(3) 0.000(4) 0.000(4) C26 0.075(7) 0.050(6) 0.072(7) 0.008(5) 0.005(5) 0.007(5) C27 0.085(9) 0.057(7) 0.106(10) 0.017(7) 0.010(7) 0.030(7) C28 0.114(11) 0.049(6) 0.085(8) 0.018(6) 0.015(8) 0.009(7) C29 0.094(9) 0.054(6) 0.074(7) 0.010(5) 0.022(6) -0.012(6) C30 0.066(6) 0.043(5) 0.058(6) 0.004(4) 0.011(5) -0.004(5) C31 0.047(5) 0.037(4) 0.047(4) 0.007(4) -0.001(4) -0.004(4) C32 0.048(5) 0.038(5) 0.086(7) -0.002(5) -0.005(5) -0.015(4) C33 0.072(7) 0.033(5) 0.092(8) -0.001(5) -0.006(6) -0.007(5) C34 0.093(9) 0.030(5) 0.082(7) -0.003(5) 0.003(6) -0.008(5) C35 0.088(9) 0.044(6) 0.088(8) -0.010(5) 0.021(6) 0.017(6) C36 0.042(5) 0.050(5) 0.067(6) -0.002(4) 0.011(4) 0.004(4) C37 0.051(5) 0.047(5) 0.046(5) 0.008(4) 0.006(4) 0.006(4) C38 0.064(7) 0.067(7) 0.064(6) 0.017(5) 0.009(5) -0.005(6) C39 0.091(10) 0.092(10) 0.081(8) 0.037(8) 0.027(7) 0.001(8) C40 0.098(10) 0.097(10) 0.060(7) 0.017(7) 0.017(7) 0.020(8) C41 0.098(10) 0.085(9) 0.052(6) -0.006(6) 0.008(6) 0.004(8) C42 0.073(7) 0.068(7) 0.051(5) -0.002(5) 0.006(5) -0.007(6) C43 0.026(4) 0.040(4) 0.051(4) 0.000(4) 0.005(3) -0.001(3) C44 0.033(4) 0.038(4) 0.066(5) 0.002(4) 0.001(4) 0.000(4) C45 0.037(5) 0.044(5) 0.076(6) -0.002(4) 0.011(4) -0.011(4) C46 0.026(4) 0.061(6) 0.074(6) -0.018(5) 0.010(4) -0.004(4) C47 0.030(4) 0.065(6) 0.064(6) -0.003(5) -0.001(4) 0.010(4) C48 0.036(4) 0.053(5) 0.058(5) 0.003(4) -0.001(4) 0.006(4) C49B 0.08(2) 0.11(3) 0.09(3) -0.02(2) 0.02(2) -0.02(2) C50B 0.33(11) 0.12(6) 0.10(4) 0.06(4) 0.11(6) 0.14(7) O1B 0.12(2) 0.12(3) 0.10(2) 0.009(19) -0.004(16) 0.03(2) C49A 0.31(9) 0.41(11) 0.19(6) -0.07(7) 0.11(6) -0.28(9) O1A 0.26(4) 0.12(3) 0.12(3) -0.003(18) -0.01(3) 0.12(3) C50A 0.28(7) 0.17(5) 0.15(4) 0.04(4) 0.14(5) 0.08(5) #------------------ MOLECULAR GEOMETRY --------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C2 1.993(8) . ? Pd1 N1 2.113(6) . ? Pd1 P1 2.281(2) . ? Pd1 Cl1 2.411(2) . ? Pd1 Pd2 3.0849(8) . ? Pd2 C8 1.992(8) . ? Pd2 P2 2.240(2) . ? Pd2 Cl1 2.397(2) . ? Pd2 Cl2 2.397(2) . ? P1 C19 1.808(9) . ? P1 C13 1.826(9) . ? P1 C25 1.829(9) . ? P2 C43 1.816(8) . ? P2 C31 1.825(9) . ? P2 C37 1.839(9) . ? N1 N2 1.264(9) . ? N1 C7 1.436(10) . ? N2 C1 1.396(11) . ? C1 C6 1.392(12) . ? C1 C2 1.423(11) . ? C2 C3 1.373(11) . ? C3 C4 1.386(13) . ? C3 H3 0.93 . ? C4 C5 1.375(15) . ? C4 H4 0.93 . ? C5 C6 1.367(15) . ? C5 H5 0.93 . ? C6 H6 0.93 . ? C7 C8 1.370(11) . ? C7 C12 1.391(12) . ? C8 C9 1.399(11) . ? C9 C10 1.379(13) . ? C9 H9 0.93 . ? C10 C11 1.372(15) . ? C10 H10 0.93 . ? C11 C12 1.373(13) . ? C11 H11 0.93 . ? C12 H12 0.93 . ? C13 C14 1.375(12) . ? C13 C18 1.388(12) . ? C14 C15 1.388(15) . ? C14 H14 0.93 . ? C15 C16 1.352(17) . ? C15 H15 0.93 . ? C16 C17 1.385(17) . ? C16 H16 0.93 . ? C17 C18 1.384(14) . ? C17 H17 0.93 . ? C18 H18 0.93 . ? C19 C20 1.386(13) . ? C19 C24 1.398(13) . ? C20 C21 1.378(15) . ? C20 H20 0.93 . ? C21 C22 1.364(18) . ? C21 H21 0.93 . ? C22 C23 1.368(17) . ? C22 H22 0.93 . ? C23 C24 1.364(14) . ? C23 H23 0.93 . ? C24 H24 0.93 . ? C25 C30 1.371(13) . ? C25 C26 1.375(14) . ? C26 C27 1.390(16) . ? C26 H26 0.93 . ? C27 C28 1.343(18) . ? C27 H27 0.93 . ? C28 C29 1.357(18) . ? C28 H28 0.93 . ? C29 C30 1.398(14) . ? C29 H29 0.93 . ? C30 H30 0.93 . ? C31 C32 1.382(12) . ? C31 C36 1.395(13) . ? C32 C33 1.392(13) . ? C32 H32 0.93 . ? C33 C34 1.338(16) . ? C33 H33 0.93 . ? C34 C35 1.356(17) . ? C34 H34 0.93 . ? C35 C36 1.382(14) . ? C35 H35 0.93 . ? C36 H36 0.93 . ? C37 C42 1.376(14) . ? C37 C38 1.376(14) . ? C38 C39 1.392(16) . ? C38 H38 0.93 . ? C39 C40 1.39(2) . ? C39 H39 0.93 . ? C40 C41 1.353(18) . ? C40 H40 0.93 . ? C41 C42 1.368(14) . ? C41 H41 0.93 . ? C42 H42 0.93 . ? C43 C44 1.387(12) . ? C43 C48 1.402(11) . ? C44 C45 1.373(11) . ? C44 H44 0.93 . ? C45 C46 1.365(14) . ? C45 H45 0.93 . ? C46 C47 1.362(14) . ? C46 H46 0.93 . ? C47 C48 1.369(12) . ? C47 H47 0.93 . ? C48 H48 0.93 . ? C49B O1B 1.423(10) . ? C49B C50B 1.539(10) . ? C49B H49C 0.97 . ? C49B H49D 0.97 . ? C50B H50D 0.96 . ? C50B H50E 0.96 . ? C50B H50F 0.96 . ? O1B H1B 0.82 . ? C49A O1A 1.427(10) . ? C49A C50A 1.531(10) . ? C49A H49A 0.97 . ? C49A H49B 0.97 . ? O1A H1A 0.82 . ? C50A H50A 0.96 . ? C50A H50B 0.96 . ? C50A H50C 0.96 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Pd1 N1 79.0(3) . . ? C2 Pd1 P1 94.8(2) . . ? N1 Pd1 P1 172.05(17) . . ? C2 Pd1 Cl1 172.3(2) . . ? N1 Pd1 Cl1 93.58(18) . . ? P1 Pd1 Cl1 92.75(7) . . ? C2 Pd1 Pd2 124.6(2) . . ? N1 Pd1 Pd2 69.30(16) . . ? P1 Pd1 Pd2 118.59(6) . . ? Cl1 Pd1 Pd2 49.88(5) . . ? C8 Pd2 P2 91.3(2) . . ? C8 Pd2 Cl1 83.5(2) . . ? P2 Pd2 Cl1 169.76(8) . . ? C8 Pd2 Cl2 176.3(2) . . ? P2 Pd2 Cl2 91.81(8) . . ? Cl1 Pd2 Cl2 93.65(8) . . ? C8 Pd2 Pd1 85.6(2) . . ? P2 Pd2 Pd1 120.63(6) . . ? Cl1 Pd2 Pd1 50.28(5) . . ? Cl2 Pd2 Pd1 94.47(6) . . ? C19 P1 C13 108.7(4) . . ? C19 P1 C25 103.5(4) . . ? C13 P1 C25 104.2(4) . . ? C19 P1 Pd1 113.4(3) . . ? C13 P1 Pd1 113.9(3) . . ? C25 P1 Pd1 112.2(3) . . ? C43 P2 C31 106.3(4) . . ? C43 P2 C37 103.1(4) . . ? C31 P2 C37 105.6(4) . . ? C43 P2 Pd2 115.0(3) . . ? C31 P2 Pd2 108.9(3) . . ? C37 P2 Pd2 117.1(3) . . ? Pd2 Cl1 Pd1 79.83(6) . . ? N2 N1 C7 117.0(6) . . ? N2 N1 Pd1 117.1(5) . . ? C7 N1 Pd1 125.5(5) . . ? N1 N2 C1 112.0(7) . . ? C6 C1 N2 116.8(8) . . ? C6 C1 C2 121.8(8) . . ? N2 C1 C2 121.4(7) . . ? C3 C2 C1 115.7(8) . . ? C3 C2 Pd1 134.2(7) . . ? C1 C2 Pd1 110.1(6) . . ? C2 C3 C4 122.7(9) . . ? C2 C3 H3 118.6 . . ? C4 C3 H3 118.6 . . ? C5 C4 C3 120.2(9) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C6 C5 C4 119.9(9) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C1 119.7(10) . . ? C5 C6 H6 120.1 . . ? C1 C6 H6 120.1 . . ? C8 C7 C12 122.0(8) . . ? C8 C7 N1 117.2(7) . . ? C12 C7 N1 120.8(7) . . ? C7 C8 C9 117.9(8) . . ? C7 C8 Pd2 120.2(6) . . ? C9 C8 Pd2 121.6(6) . . ? C10 C9 C8 120.1(9) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C11 C10 C9 120.9(9) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C10 C11 C12 119.8(9) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C11 C12 C7 119.1(9) . . ? C11 C12 H12 120.4 . . ? C7 C12 H12 120.4 . . ? C14 C13 C18 119.3(9) . . ? C14 C13 P1 118.1(7) . . ? C18 C13 P1 122.6(7) . . ? C13 C14 C15 120.9(10) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C16 C15 C14 120.0(11) . . ? C16 C15 H15 120 . . ? C14 C15 H15 120 . . ? C15 C16 C17 119.9(10) . . ? C15 C16 H16 120 . . ? C17 C16 H16 120 . . ? C18 C17 C16 120.7(10) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C18 C13 119.2(10) . . ? C17 C18 H18 120.4 . . ? C13 C18 H18 120.4 . . ? C20 C19 C24 118.1(8) . . ? C20 C19 P1 122.2(7) . . ? C24 C19 P1 119.6(7) . . ? C21 C20 C19 120.5(10) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C22 C21 C20 120.2(11) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 120.1(10) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C24 C23 C22 120.6(11) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C19 120.5(10) . . ? C23 C24 H24 119.8 . . ? C19 C24 H24 119.8 . . ? C30 C25 C26 119.1(9) . . ? C30 C25 P1 118.9(7) . . ? C26 C25 P1 121.7(8) . . ? C25 C26 C27 120.5(12) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C28 C27 C26 119.9(12) . . ? C28 C27 H27 120 . . ? C26 C27 H27 120 . . ? C27 C28 C29 120.7(11) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? C28 C29 C30 120.2(12) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C25 C30 C29 119.6(11) . . ? C25 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C32 C31 C36 118.5(9) . . ? C32 C31 P2 117.8(7) . . ? C36 C31 P2 123.7(7) . . ? C31 C32 C33 120.7(10) . . ? C31 C32 H32 119.6 . . ? C33 C32 H32 119.6 . . ? C34 C33 C32 120.7(11) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C33 C34 C35 118.7(10) . . ? C33 C34 H34 120.7 . . ? C35 C34 H34 120.7 . . ? C34 C35 C36 123.5(11) . . ? C34 C35 H35 118.3 . . ? C36 C35 H35 118.3 . . ? C35 C36 C31 117.8(10) . . ? C35 C36 H36 121.1 . . ? C31 C36 H36 121.1 . . ? C42 C37 C38 118.6(9) . . ? C42 C37 P2 119.8(8) . . ? C38 C37 P2 121.3(8) . . ? C37 C38 C39 120.5(12) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C40 C39 C38 118.9(12) . . ? C40 C39 H39 120.5 . . ? C38 C39 H39 120.5 . . ? C41 C40 C39 120.5(12) . . ? C41 C40 H40 119.7 . . ? C39 C40 H40 119.7 . . ? C40 C41 C42 119.9(13) . . ? C40 C41 H41 120 . . ? C42 C41 H41 120 . . ? C41 C42 C37 121.4(11) . . ? C41 C42 H42 119.3 . . ? C37 C42 H42 119.3 . . ? C44 C43 C48 118.0(8) . . ? C44 C43 P2 120.4(6) . . ? C48 C43 P2 121.6(7) . . ? C45 C44 C43 120.7(8) . . ? C45 C44 H44 119.7 . . ? C43 C44 H44 119.7 . . ? C46 C45 C44 119.5(9) . . ? C46 C45 H45 120.2 . . ? C44 C45 H45 120.2 . . ? C47 C46 C45 121.7(8) . . ? C47 C46 H46 119.1 . . ? C45 C46 H46 119.1 . . ? C46 C47 C48 119.1(9) . . ? C46 C47 H47 120.5 . . ? C48 C47 H47 120.5 . . ? C47 C48 C43 121.0(9) . . ? C47 C48 H48 119.5 . . ? C43 C48 H48 119.5 . . ? O1B C49B C50B 111(3) . . ? O1B C49B H49C 109.5 . . ? C50B C49B H49C 109.5 . . ? O1B C49B H49D 109.5 . . ? C50B C49B H49D 109.5 . . ? H49C C49B H49D 108.1 . . ? C49B C50B H50D 109.5 . . ? C49B C50B H50E 109.5 . . ? H50D C50B H50E 109.5 . . ? C49B C50B H50F 109.5 . . ? H50D C50B H50F 109.5 . . ? H50E C50B H50F 109.5 . . ? O1A C49A C50A 108(4) . . ? O1A C49A H49A 110.2 . . ? C50A C49A H49A 110.2 . . ? O1A C49A H49B 110.2 . . ? C50A C49A H49B 110.2 . . ? H49A C49A H49B 108.5 . . ? C49A O1A H1A 109.5 . . ? C49A C50A H50A 109.5 . . ? C49A C50A H50B 109.5 . . ? H50A C50A H50B 109.5 . . ? C49A C50A H50C 109.5 . . ? H50A C50A H50C 109.5 . . ? H50B C50A H50C 109.5 . . ? 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 C2 Pd1 Pd2 C8 -88.1(4) . . . . ? N1 Pd1 Pd2 C8 -28.7(3) . . . . ? P1 Pd1 Pd2 C8 152.4(2) . . . . ? Cl1 Pd1 Pd2 C8 85.2(2) . . . . ? C2 Pd1 Pd2 P2 0.8(3) . . . . ? N1 Pd1 Pd2 P2 60.26(19) . . . . ? P1 Pd1 Pd2 P2 -118.62(9) . . . . ? Cl1 Pd1 Pd2 P2 174.20(10) . . . . ? C2 Pd1 Pd2 Cl1 -173.4(3) . . . . ? N1 Pd1 Pd2 Cl1 -113.93(19) . . . . ? P1 Pd1 Pd2 Cl1 67.18(9) . . . . ? C2 Pd1 Pd2 Cl2 95.6(3) . . . . ? N1 Pd1 Pd2 Cl2 155.03(19) . . . . ? P1 Pd1 Pd2 Cl2 -23.86(9) . . . . ? Cl1 Pd1 Pd2 Cl2 -91.04(9) . . . . ? C2 Pd1 P1 C19 -78.1(4) . . . . ? Cl1 Pd1 P1 C19 100.7(3) . . . . ? Pd2 Pd1 P1 C19 55.9(3) . . . . ? C2 Pd1 P1 C13 46.9(4) . . . . ? Cl1 Pd1 P1 C13 -134.2(3) . . . . ? Pd2 Pd1 P1 C13 -179.1(3) . . . . ? C2 Pd1 P1 C25 165.0(4) . . . . ? Cl1 Pd1 P1 C25 -16.1(3) . . . . ? Pd2 Pd1 P1 C25 -61.0(3) . . . . ? C8 Pd2 P2 C43 -114.0(4) . . . . ? Cl1 Pd2 P2 C43 -173.7(5) . . . . ? Cl2 Pd2 P2 C43 64.0(3) . . . . ? Pd1 Pd2 P2 C43 160.3(3) . . . . ? C8 Pd2 P2 C31 126.9(4) . . . . ? Cl1 Pd2 P2 C31 67.2(6) . . . . ? Cl2 Pd2 P2 C31 -55.1(3) . . . . ? Pd1 Pd2 P2 C31 41.2(3) . . . . ? C8 Pd2 P2 C37 7.3(4) . . . . ? Cl1 Pd2 P2 C37 -52.4(6) . . . . ? Cl2 Pd2 P2 C37 -174.6(4) . . . . ? Pd1 Pd2 P2 C37 -78.4(4) . . . . ? C8 Pd2 Cl1 Pd1 -89.6(2) . . . . ? P2 Pd2 Cl1 Pd1 -29.3(5) . . . . ? Cl2 Pd2 Cl1 Pd1 92.78(8) . . . . ? N1 Pd1 Cl1 Pd2 58.94(17) . . . . ? P1 Pd1 Cl1 Pd2 -125.88(7) . . . . ? C2 Pd1 N1 N2 -6.7(5) . . . . ? Cl1 Pd1 N1 N2 175.1(5) . . . . ? Pd2 Pd1 N1 N2 -140.5(6) . . . . ? C2 Pd1 N1 C7 -178.6(6) . . . . ? Cl1 Pd1 N1 C7 3.2(6) . . . . ? Pd2 Pd1 N1 C7 47.6(5) . . . . ? C7 N1 N2 C1 179.8(7) . . . . ? Pd1 N1 N2 C1 7.2(9) . . . . ? N1 N2 C1 C6 173.7(9) . . . . ? N1 N2 C1 C2 -3.6(11) . . . . ? C6 C1 C2 C3 -0.6(13) . . . . ? N2 C1 C2 C3 176.5(8) . . . . ? C6 C1 C2 Pd1 -179.0(8) . . . . ? N2 C1 C2 Pd1 -1.9(10) . . . . ? N1 Pd1 C2 C3 -173.9(9) . . . . ? P1 Pd1 C2 C3 11.1(8) . . . . ? Pd2 Pd1 C2 C3 -118.8(8) . . . . ? N1 Pd1 C2 C1 4.1(5) . . . . ? P1 Pd1 C2 C1 -170.9(5) . . . . ? Pd2 Pd1 C2 C1 59.2(6) . . . . ? C1 C2 C3 C4 -0.3(13) . . . . ? Pd1 C2 C3 C4 177.6(7) . . . . ? C2 C3 C4 C5 1.2(16) . . . . ? C3 C4 C5 C6 -1.0(19) . . . . ? C4 C5 C6 C1 0(2) . . . . ? N2 C1 C6 C5 -176.4(11) . . . . ? C2 C1 C6 C5 0.8(17) . . . . ? N2 N1 C7 C8 138.5(7) . . . . ? Pd1 N1 C7 C8 -49.6(9) . . . . ? N2 N1 C7 C12 -42.9(11) . . . . ? Pd1 N1 C7 C12 129.0(7) . . . . ? C12 C7 C8 C9 -0.4(12) . . . . ? N1 C7 C8 C9 178.3(7) . . . . ? C12 C7 C8 Pd2 -174.8(7) . . . . ? N1 C7 C8 Pd2 3.8(10) . . . . ? P2 Pd2 C8 C7 -99.3(6) . . . . ? Cl1 Pd2 C8 C7 71.8(6) . . . . ? Pd1 Pd2 C8 C7 21.3(6) . . . . ? P2 Pd2 C8 C9 86.4(7) . . . . ? Cl1 Pd2 C8 C9 -102.4(7) . . . . ? Pd1 Pd2 C8 C9 -152.9(7) . . . . ? C7 C8 C9 C10 -1.7(13) . . . . ? Pd2 C8 C9 C10 172.7(7) . . . . ? C8 C9 C10 C11 1.5(16) . . . . ? C9 C10 C11 C12 0.8(16) . . . . ? C10 C11 C12 C7 -2.8(15) . . . . ? C8 C7 C12 C11 2.7(14) . . . . ? N1 C7 C12 C11 -175.9(8) . . . . ? C19 P1 C13 C14 160.2(7) . . . . ? C25 P1 C13 C14 -89.9(8) . . . . ? Pd1 P1 C13 C14 32.7(8) . . . . ? C19 P1 C13 C18 -21.2(9) . . . . ? C25 P1 C13 C18 88.7(8) . . . . ? Pd1 P1 C13 C18 -148.7(7) . . . . ? C18 C13 C14 C15 -1.9(15) . . . . ? P1 C13 C14 C15 176.8(9) . . . . ? C13 C14 C15 C16 2.0(18) . . . . ? C14 C15 C16 C17 -0.2(19) . . . . ? C15 C16 C17 C18 -1.5(19) . . . . ? C16 C17 C18 C13 1.6(17) . . . . ? C14 C13 C18 C17 0.1(15) . . . . ? P1 C13 C18 C17 -178.5(8) . . . . ? C13 P1 C19 C20 69.9(9) . . . . ? C25 P1 C19 C20 -40.5(9) . . . . ? Pd1 P1 C19 C20 -162.4(7) . . . . ? C13 P1 C19 C24 -113.7(7) . . . . ? C25 P1 C19 C24 135.9(7) . . . . ? Pd1 P1 C19 C24 14.0(8) . . . . ? C24 C19 C20 C21 0.7(15) . . . . ? P1 C19 C20 C21 177.1(8) . . . . ? C19 C20 C21 C22 0.2(17) . . . . ? C20 C21 C22 C23 -1.0(19) . . . . ? C21 C22 C23 C24 1.0(19) . . . . ? C22 C23 C24 C19 -0.1(17) . . . . ? C20 C19 C24 C23 -0.7(14) . . . . ? P1 C19 C24 C23 -177.2(8) . . . . ? C19 P1 C25 C30 -42.3(8) . . . . ? C13 P1 C25 C30 -156.0(7) . . . . ? Pd1 P1 C25 C30 80.4(8) . . . . ? C19 P1 C25 C26 143.9(8) . . . . ? C13 P1 C25 C26 30.2(9) . . . . ? Pd1 P1 C25 C26 -93.5(8) . . . . ? C30 C25 C26 C27 -0.2(16) . . . . ? P1 C25 C26 C27 173.6(9) . . . . ? C25 C26 C27 C28 0(2) . . . . ? C26 C27 C28 C29 1(2) . . . . ? C27 C28 C29 C30 -1(2) . . . . ? C26 C25 C30 C29 -0.3(15) . . . . ? P1 C25 C30 C29 -174.2(8) . . . . ? C28 C29 C30 C25 1.0(17) . . . . ? C43 P2 C31 C32 -171.4(7) . . . . ? C37 P2 C31 C32 79.5(8) . . . . ? Pd2 P2 C31 C32 -47.0(8) . . . . ? C43 P2 C31 C36 7.5(9) . . . . ? C37 P2 C31 C36 -101.6(8) . . . . ? Pd2 P2 C31 C36 131.9(7) . . . . ? C36 C31 C32 C33 2.4(15) . . . . ? P2 C31 C32 C33 -178.6(8) . . . . ? C31 C32 C33 C34 -2.4(18) . . . . ? C32 C33 C34 C35 1.1(18) . . . . ? C33 C34 C35 C36 0.2(19) . . . . ? C34 C35 C36 C31 -0.2(17) . . . . ? C32 C31 C36 C35 -1.1(14) . . . . ? P2 C31 C36 C35 180.0(8) . . . . ? C43 P2 C37 C42 36.8(9) . . . . ? C31 P2 C37 C42 148.1(8) . . . . ? Pd2 P2 C37 C42 -90.6(9) . . . . ? C43 P2 C37 C38 -149.1(8) . . . . ? C31 P2 C37 C38 -37.8(9) . . . . ? Pd2 P2 C37 C38 83.5(9) . . . . ? C42 C37 C38 C39 0.7(17) . . . . ? P2 C37 C38 C39 -173.5(9) . . . . ? C37 C38 C39 C40 -2.6(19) . . . . ? C38 C39 C40 C41 2(2) . . . . ? C39 C40 C41 C42 1(2) . . . . ? C40 C41 C42 C37 -3(2) . . . . ? C38 C37 C42 C41 2.3(17) . . . . ? P2 C37 C42 C41 176.6(10) . . . . ? C31 P2 C43 C44 113.7(7) . . . . ? C37 P2 C43 C44 -135.5(7) . . . . ? Pd2 P2 C43 C44 -6.9(8) . . . . ? C31 P2 C43 C48 -64.2(8) . . . . ? C37 P2 C43 C48 46.6(8) . . . . ? Pd2 P2 C43 C48 175.2(6) . . . . ? C48 C43 C44 C45 0.3(13) . . . . ? P2 C43 C44 C45 -177.7(7) . . . . ? C43 C44 C45 C46 0.3(14) . . . . ? C44 C45 C46 C47 -0.5(15) . . . . ? C45 C46 C47 C48 0.1(15) . . . . ? C46 C47 C48 C43 0.5(15) . . . . ? C44 C43 C48 C47 -0.7(14) . . . . ? P2 C43 C48 C47 177.2(7) . . . . ? # Attachment 'DMANAB-cifdoc.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-10-28 at 16:43:55 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\program files\wingx\files\cifdoc.dat # CIF files read : manda-4a-d12-ponovo manda-4a-d12-ponovo-teh struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_manda-4a-d12-ponovo _database_code_depnum_ccdc_archive 'CCDC 831719' #TrackingRef 'DMANAB-cifdoc.cif' _audit_creation_date 2010-10-28T16:43:55-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_moiety '2(C50 H42 Cl2 N4 O2 P2 Pd2), C2 H6 O, H2 O' _chemical_formula_sum 'C102 H92 Cl4 N8 O6 P4 Pd4' _chemical_formula_weight 2217.12 #------------------ UNIT CELL INFORMATION -----------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0943(3) _cell_length_b 20.0688(7) _cell_length_c 25.3224(6) _cell_angle_alpha 110.178(3) _cell_angle_beta 90.883(2) _cell_angle_gamma 90.024(3) _cell_volume 4814.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 13321 _cell_measurement_theta_min 3.4576 _cell_measurement_theta_max 75.9554 #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.529 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 8.048 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.33114 _exptl_absorpt_correction_T_max 1 #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54179 _diffrn_radiation_type CuK\a _diffrn_radiation_probe x-ray _diffrn_measurement_device_type 'Xcalibur, Ruby' _diffrn_measurement_method '\w scans' _diffrn_reflns_number 43140 _diffrn_reflns_av_R_equivalents 0.0509 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 76.14 _diffrn_reflns_theta_full 76.14 _diffrn_measured_fraction_theta_max 0.968 _diffrn_measured_fraction_theta_full 0.968 _reflns_number_total 19491 _reflns_number_gt 9835 _reflns_threshold_expression >2sigma(I) #------------------ COMPUTER PROGRAMS USED ----------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #------------------ REFINEMENT INFORMATION ----------------------------------# _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^)+(0.0351P)^2^+60.5558P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 19491 _refine_ls_number_parameters 987 _refine_ls_number_restraints 86 _refine_ls_R_factor_gt 0.0905 _refine_ls_wR_factor_ref 0.2358 _refine_ls_goodness_of_fit_ref 1.203 _refine_ls_restrained_S_all 1.201 _refine_ls_shift/su_max 0.007 _refine_diff_density_max 1.224 _refine_diff_density_min -0.91 #------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group _atom_site_disorder_assembly Pd2A Pd 0.93452(11) 0.25177(6) 0.22757(4) 0.0429(2) Uani 1 d . . . Pd1A Pd 0.80240(10) 0.28297(6) 0.12599(4) 0.0414(2) Uani 1 d . . . Pd2B Pd 0.56536(12) 0.74841(7) 0.27230(5) 0.0530(3) Uani 1 d . . . Pd1B Pd 0.69770(12) 0.71706(7) 0.37382(5) 0.0513(3) Uani 1 d . . . P2A P 1.1498(3) 0.27125(19) 0.25272(13) 0.0410(8) Uani 1 d . . . P1A P 0.7076(3) 0.19077(19) 0.05504(13) 0.0403(7) Uani 1 d . . . Cl1A Cl 0.7071(3) 0.2441(2) 0.19828(13) 0.0491(8) Uani 1 d . . . P2B P 0.3509(4) 0.7282(2) 0.24694(16) 0.0550(10) Uani 1 d . . . P1B P 0.7922(5) 0.8092(2) 0.44492(16) 0.0573(10) Uani 1 d . . . Cl1B Cl 0.7927(4) 0.7551(3) 0.30148(17) 0.0668(11) Uani 1 d . . . Cl2A Cl 0.9830(5) 0.1322(2) 0.17093(18) 0.0747(13) Uani 1 d . . . Cl2B Cl 0.5164(6) 0.8674(2) 0.3286(2) 0.0908(17) Uani 1 d . . . C18A C 0.9601(10) 0.1354(5) 0.0296(3) 0.063(4) Uani 1 d G . . H18A H 0.9826 0.1654 0.0658 0.076 Uiso 1 calc R . . C17A C 1.0557(8) 0.0921(6) -0.0042(5) 0.090(7) Uani 1 d G . . H17A H 1.1421 0.0931 0.0093 0.108 Uiso 1 calc R . . C16A C 1.0220(11) 0.0472(6) -0.0582(4) 0.078(6) Uani 1 d GU . . H16A H 1.086 0.0182 -0.0808 0.094 Uiso 1 calc R . . C15A C 0.8928(12) 0.0457(6) -0.0784(3) 0.090(7) Uani 1 d G . . H15A H 0.8703 0.0157 -0.1145 0.108 Uiso 1 calc R . . C14A C 0.7973(9) 0.0890(6) -0.0446(4) 0.078(6) Uani 1 d G . . H14A H 0.7108 0.088 -0.0581 0.093 Uiso 1 calc R . . C13A C 0.8309(8) 0.1339(5) 0.0094(4) 0.046(3) Uani 1 d G . . C25A C 0.5880(8) 0.2156(5) 0.0091(4) 0.047(3) Uani 1 d G . . C26A C 0.4997(11) 0.1650(4) -0.0247(5) 0.065(5) Uani 1 d G . . H26A H 0.5034 0.1185 -0.0252 0.078 Uiso 1 calc R . . C27A C 0.4060(10) 0.1840(6) -0.0576(5) 0.097(8) Uani 1 d G . . H27A H 0.347 0.1501 -0.0803 0.117 Uiso 1 calc R . . C28A C 0.4005(10) 0.2535(7) -0.0568(4) 0.091(7) Uani 1 d G . . H28A H 0.3378 0.2662 -0.0789 0.11 Uiso 1 calc R . . C29A C 0.4887(10) 0.3041(5) -0.0230(5) 0.063(4) Uani 1 d G . . H29A H 0.485 0.3507 -0.0225 0.075 Uiso 1 calc R . . C30A C 0.5824(8) 0.2852(5) 0.0099(4) 0.052(4) Uani 1 d G . . H30A H 0.6415 0.319 0.0325 0.063 Uiso 1 calc R . . C19A C 0.6101(9) 0.1295(5) 0.0780(4) 0.043(3) Uani 1 d G . . C20A C 0.6708(9) 0.0708(6) 0.0849(5) 0.068(5) Uani 1 d GU . . H20A H 0.7596 0.0618 0.0761 0.082 Uiso 1 calc R . . C21A C 0.5988(15) 0.0257(5) 0.1049(5) 0.096(7) Uani 1 d G . . H21A H 0.6394 -0.0135 0.1095 0.115 Uiso 1 calc R . . C22A C 0.4660(14) 0.0393(6) 0.1181(5) 0.095(8) Uani 1 d G . . H22A H 0.4178 0.0091 0.1315 0.114 Uiso 1 calc R . . C23A C 0.4053(9) 0.0980(7) 0.1112(5) 0.081(6) Uani 1 d G . . H23A H 0.3165 0.1071 0.12 0.097 Uiso 1 calc R . . C24A C 0.4773(10) 0.1431(5) 0.0912(4) 0.064(4) Uani 1 d G . . H24A H 0.4367 0.1824 0.0866 0.076 Uiso 1 calc R . . C37A C 1.2430(9) 0.2908(5) 0.1988(3) 0.049(4) Uani 1 d G . . C38A C 1.3684(9) 0.3214(6) 0.2106(4) 0.070(5) Uani 1 d G . . H38A H 1.4097 0.3274 0.245 0.083 Uiso 1 calc R . . C39A C 1.4322(9) 0.3431(6) 0.1709(5) 0.084(6) Uani 1 d G . . H39A H 1.5161 0.3636 0.1788 0.1 Uiso 1 calc R . . C40A C 1.3705(12) 0.3341(6) 0.1194(5) 0.088(7) Uani 1 d G . . H40A H 1.4131 0.3486 0.0929 0.106 Uiso 1 calc R . . C41A C 1.2450(12) 0.3035(7) 0.1076(3) 0.079(6) Uani 1 d G . . H41A H 1.2037 0.2975 0.0732 0.095 Uiso 1 calc R . . C42A C 1.1813(8) 0.2818(6) 0.1473(4) 0.062(5) Uani 1 d G . . H42A H 1.0973 0.2613 0.1394 0.075 Uiso 1 calc R . . C31A C 1.2285(11) 0.1979(5) 0.2666(4) 0.058(4) Uani 1 d G . . C36A C 1.3575(11) 0.1783(7) 0.2500(4) 0.079(6) Uani 1 d G . . H36 H 1.4051 0.2031 0.2315 0.095 Uiso 1 calc R . . C35A C 1.4155(12) 0.1215(8) 0.2609(6) 0.110(9) Uani 1 d GU . . H35A H 1.5018 0.1083 0.2498 0.132 Uiso 1 calc R . . C34A C 1.3444(18) 0.0844(6) 0.2885(6) 0.120(11) Uani 1 d G . . H34A H 1.3832 0.0464 0.2959 0.144 Uiso 1 calc R . . C33A C 1.2154(16) 0.1040(7) 0.3052(6) 0.113(10) Uani 1 d G . . H33A H 1.1678 0.0792 0.3236 0.135 Uiso 1 calc R . . C32A C 1.1574(10) 0.1608(8) 0.2942(5) 0.086(6) Uani 1 d G . . H32A H 1.0711 0.174 0.3053 0.104 Uiso 1 calc R . . C43A C 1.1856(10) 0.3481(4) 0.3157(3) 0.048(3) Uani 1 d G . . C44A C 1.1882(10) 0.3411(5) 0.3685(4) 0.059(4) Uani 1 d G . . H44A H 1.1827 0.2964 0.3715 0.071 Uiso 1 calc R . . C45A C 1.1989(11) 0.4011(7) 0.4166(3) 0.078(6) Uani 1 d G . . H45A H 1.2006 0.3965 0.4519 0.094 Uiso 1 calc R . . C46A C 1.2071(11) 0.4681(5) 0.4120(4) 0.075(6) Uani 1 d G . . H46A H 1.2143 0.5082 0.4443 0.09 Uiso 1 calc R . . C47A C 1.2046(11) 0.4750(4) 0.3593(5) 0.067(5) Uani 1 d G . . H47A H 1.2101 0.5198 0.3562 0.08 Uiso 1 calc R . . C48A C 1.1938(10) 0.4150(5) 0.3111(3) 0.056(4) Uani 1 d G . . H48A H 1.1921 0.4196 0.2758 0.067 Uiso 1 calc R . . C25B C 0.9105(10) 0.7844(6) 0.4904(4) 0.058(4) Uani 1 d G . . C30B C 0.9160(10) 0.7145(5) 0.4888(4) 0.070(5) Uani 1 d GU . . H30B H 0.8575 0.6808 0.4656 0.085 Uiso 1 calc R . . C29B C 1.0090(12) 0.6950(5) 0.5217(5) 0.075(5) Uani 1 d G . . H29B H 1.0126 0.6482 0.5206 0.09 Uiso 1 calc R . . C28B C 1.0964(11) 0.7453(7) 0.5563(5) 0.091(7) Uani 1 d GU . . H28B H 1.1586 0.7322 0.5784 0.11 Uiso 1 calc R . . C27B C 1.0909(12) 0.8152(7) 0.5580(5) 0.101(8) Uani 1 d G . . H27B H 1.1494 0.8489 0.5811 0.122 Uiso 1 calc R . . C26B C 0.9979(13) 0.8348(5) 0.5250(5) 0.079(6) Uani 1 d G . . H26B H 0.9942 0.8815 0.5261 0.094 Uiso 1 calc R . . C13B C 0.8900(12) 0.8696(6) 0.4211(5) 0.064(5) Uani 1 d G . . C18B C 1.0229(13) 0.8563(6) 0.4081(5) 0.077(5) Uani 1 d G . . H18B H 1.0635 0.8168 0.4123 0.092 Uiso 1 calc R . . C17B C 1.0951(11) 0.9020(8) 0.3888(5) 0.089(7) Uani 1 d G . . H17B H 1.184 0.8931 0.3801 0.106 Uiso 1 calc R . . C16B C 1.0343(17) 0.9610(7) 0.3825(5) 0.101(8) Uani 1 d G . . H16B H 1.0826 0.9916 0.3695 0.121 Uiso 1 calc R . . C15B C 0.9014(17) 0.9743(6) 0.3954(6) 0.112(9) Uani 1 d G . . H15B H 0.8608 1.0138 0.3912 0.135 Uiso 1 calc R . . C14B C 0.8293(11) 0.9286(7) 0.4148(6) 0.089(6) Uani 1 d G . . H14B H 0.7404 0.9374 0.4235 0.107 Uiso 1 calc R . . C19B C 0.6692(12) 0.8655(6) 0.4910(4) 0.070(5) Uani 1 d G . . C24B C 0.7028(11) 0.9103(7) 0.5450(5) 0.092(7) Uani 1 d G . . H24B H 0.7891 0.9111 0.5586 0.111 Uiso 1 calc R . . C23B C 0.6073(15) 0.9538(6) 0.5787(4) 0.108(9) Uani 1 d G . . H23B H 0.6298 0.9837 0.6149 0.13 Uiso 1 calc R . . C22B C 0.4783(14) 0.9525(6) 0.5584(5) 0.094(8) Uani 1 d G . . H22B H 0.4144 0.9817 0.581 0.112 Uiso 1 calc R . . C21B C 0.4448(11) 0.9078(8) 0.5044(6) 0.094(7) Uani 1 d G . . H21B H 0.3585 0.9069 0.4908 0.113 Uiso 1 calc R . . C20B C 0.5402(13) 0.8642(6) 0.4706(4) 0.087(6) Uani 1 d GU . . H20B H 0.5178 0.8343 0.4345 0.104 Uiso 1 calc R . . C31B C 0.2693(12) 0.8021(6) 0.2331(5) 0.067(5) Uani 1 d G . . C36B C 0.3429(12) 0.8388(8) 0.2060(6) 0.089(7) Uani 1 d G . . H36B H 0.429 0.8249 0.1951 0.107 Uiso 1 calc R . . C35B C 0.2877(19) 0.8963(7) 0.1951(6) 0.130(11) Uani 1 d G . . H35B H 0.3369 0.9209 0.1769 0.156 Uiso 1 calc R . . C34B C 0.159(2) 0.9171(6) 0.2114(7) 0.145(15) Uani 1 d G . . H34B H 0.122 0.9556 0.2041 0.174 Uiso 1 calc R . . C33B C 0.0853(13) 0.8804(8) 0.2385(6) 0.129(13) Uani 1 d G . . H33B H -0.0009 0.8943 0.2494 0.155 Uiso 1 calc R . . C32B C 0.1405(12) 0.8229(7) 0.2494(5) 0.078(6) Uani 1 d G . . H32B H 0.0912 0.7983 0.2676 0.094 Uiso 1 calc R . . C43B C 0.2569(11) 0.7098(6) 0.3014(4) 0.063(4) Uani 1 d GU . . C48B C 0.3185(10) 0.7188(6) 0.3529(5) 0.074(5) Uani 1 d G . . H48B H 0.4022 0.7396 0.3609 0.089 Uiso 1 calc R . . C47B C 0.2551(15) 0.6967(7) 0.3923(4) 0.095(8) Uani 1 d G . . H47B H 0.2963 0.7026 0.4268 0.114 Uiso 1 calc R . . C46B C 0.1300(15) 0.6656(7) 0.3803(6) 0.100(8) Uani 1 d G . . H46B H 0.0875 0.6508 0.4067 0.12 Uiso 1 calc R . . C45B C 0.0684(10) 0.6566(6) 0.3288(6) 0.085(6) Uani 1 d G . . H45B H -0.0153 0.6358 0.3208 0.102 Uiso 1 calc R . . C44B C 0.1319(11) 0.6788(6) 0.2893(4) 0.077(5) Uani 1 d G . . H44B H 0.0906 0.6728 0.2549 0.092 Uiso 1 calc R . . C37B C 0.3144(10) 0.6511(5) 0.1841(3) 0.055(4) Uani 1 d G . . C42B C 0.3060(11) 0.5839(6) 0.1881(4) 0.063(4) Uani 1 d G . . H42B H 0.3076 0.5788 0.2233 0.076 Uiso 1 calc R . . C41B C 0.2952(11) 0.5243(5) 0.1397(5) 0.080(6) Uani 1 d G . . H41B H 0.2896 0.4793 0.1424 0.096 Uiso 1 calc R . . C40B C 0.2928(11) 0.5319(6) 0.0871(4) 0.086(7) Uani 1 d G . . H40B H 0.2856 0.492 0.0547 0.103 Uiso 1 calc R . . C39B C 0.3012(11) 0.5991(7) 0.0831(3) 0.072(6) Uani 1 d G . . H39B H 0.2996 0.6042 0.048 0.086 Uiso 1 calc R . . C38B C 0.3120(11) 0.6587(5) 0.1316(4) 0.069(5) Uani 1 d GU . . H38B H 0.3176 0.7036 0.1289 0.083 Uiso 1 calc R . . N1A N 0.8905(10) 0.3762(6) 0.1840(4) 0.041(3) Uani 1 d . . . N2A N 0.9396(12) 0.4204(6) 0.1613(5) 0.048(3) Uani 1 d . . . C2B C 0.6119(15) 0.6757(9) 0.4262(6) 0.054(4) Uani 1 d U . . C7A C 0.8862(12) 0.4024(7) 0.2429(5) 0.036(3) Uani 1 d . . . C2A C 0.8901(12) 0.3236(7) 0.0730(6) 0.039(3) Uani 1 d U . . C9A C 0.8842(12) 0.3789(8) 0.3299(5) 0.042(3) Uani 1 d U . . H9A H 0.8868 0.3479 0.3501 0.051 Uiso 1 calc R . . C8A C 0.8960(12) 0.3532(7) 0.2721(5) 0.038(3) Uani 1 d . . . O2A O 0.8605(16) 0.5402(7) 0.4438(5) 0.095(5) Uani 1 d . . . N3A N 0.8537(14) 0.4770(8) 0.4187(5) 0.061(4) Uani 1 d . . . O1A O 0.8395(13) 0.4337(7) 0.4428(4) 0.074(4) Uani 1 d . . . C3A C 0.9118(14) 0.2979(8) 0.0164(5) 0.051(4) Uani 1 d . . . H3A H 0.8826 0.2522 -0.0041 0.062 Uiso 1 calc R . . C11A C 0.8667(14) 0.4990(8) 0.3303(5) 0.049(4) Uani 1 d . . . H11A H 0.8572 0.5471 0.3505 0.059 Uiso 1 calc R . . C3B C 0.5915(16) 0.7018(9) 0.4825(6) 0.056(4) Uani 1 d . . . H3B H 0.6219 0.7474 0.5027 0.067 Uiso 1 calc R . . C10A C 0.8686(13) 0.4505(8) 0.3575(5) 0.044(3) Uani 1 d U . . C12A C 0.8792(13) 0.4754(7) 0.2726(6) 0.044(3) Uani 1 d . . . H12A H 0.8829 0.5077 0.2536 0.053 Uiso 1 calc R . . N4A N 0.9982(16) 0.3066(9) -0.0682(5) 0.070(4) Uani 1 d . . . N4B N 0.5039(15) 0.6927(9) 0.5680(6) 0.072(4) Uani 1 d . . . C1A C 0.9389(14) 0.3930(7) 0.1040(5) 0.044(3) Uani 1 d . . . C1B C 0.5609(18) 0.6058(9) 0.3955(7) 0.063(4) Uani 1 d . . . C4A C 0.9761(15) 0.3370(9) -0.0126(6) 0.052(4) Uani 1 d . . . C4B C 0.5264(17) 0.6634(10) 0.5121(7) 0.063(5) Uani 1 d . . . C5A C 1.0148(16) 0.4076(9) 0.0185(6) 0.060(4) Uani 1 d . . . H5A H 1.053 0.436 0.0005 0.072 Uiso 1 calc R . . C5B C 0.4866(19) 0.5926(10) 0.4810(7) 0.073(5) Uani 1 d . . . H5B H 0.4489 0.5647 0.4995 0.087 Uiso 1 calc R . . C6A C 0.9957(16) 0.4339(8) 0.0754(6) 0.055(4) Uani 1 d . . . H6A H 1.0211 0.4804 0.0955 0.066 Uiso 1 calc R . . C6B C 0.5032(18) 0.5653(10) 0.4243(7) 0.067(5) Uani 1 d . . . H6B H 0.4758 0.519 0.4045 0.08 Uiso 1 calc R . . C50A C 1.0507(19) 0.3478(11) -0.1012(7) 0.084(6) Uani 1 d . . . H50A H 1.0757 0.3161 -0.1376 0.126 Uiso 1 calc R . . H50C H 1.1268 0.3745 -0.0821 0.126 Uiso 1 calc R . . H50B H 0.9839 0.3796 -0.1055 0.126 Uiso 1 calc R . . C50B C 0.451(2) 0.6531(11) 0.6011(8) 0.090(7) Uani 1 d . . . H50F H 0.4585 0.6809 0.6404 0.135 Uiso 1 calc R . . H50E H 0.499 0.6097 0.5937 0.135 Uiso 1 calc R . . H50D H 0.3589 0.6423 0.5912 0.135 Uiso 1 calc R . . C49B C 0.530(2) 0.7663(11) 0.5981(8) 0.097(7) Uani 1 d . . . H49D H 0.5704 0.7873 0.5735 0.145 Uiso 1 calc R . . H49F H 0.5889 0.7709 0.6293 0.145 Uiso 1 calc R . . H49E H 0.4484 0.7901 0.6118 0.145 Uiso 1 calc R . . N1B N 0.6125(12) 0.6230(7) 0.3166(5) 0.052(3) Uani 1 d . . . N3B N 0.6450(14) 0.5237(8) 0.0805(5) 0.064(4) Uani 1 d . . . N2B N 0.5628(12) 0.5802(7) 0.3386(5) 0.055(3) Uani 1 d . . . C8B C 0.6030(16) 0.6465(8) 0.2288(6) 0.059(4) Uani 1 d . . . C7B C 0.6102(15) 0.5976(9) 0.2560(6) 0.054(4) Uani 1 d . . . C11B C 0.6329(15) 0.4993(8) 0.1694(6) 0.058(4) Uani 1 d . . . H11B H 0.6406 0.451 0.1494 0.069 Uiso 1 calc R . . C9B C 0.6167(14) 0.6213(8) 0.1703(6) 0.053(4) Uani 1 d . . . H9B H 0.6153 0.6526 0.1504 0.063 Uiso 1 calc R . . C10B C 0.6324(15) 0.5498(9) 0.1427(6) 0.059(4) Uani 1 d . . . C12B C 0.6214(15) 0.5253(9) 0.2268(6) 0.058(4) Uani 1 d . . . H12B H 0.6211 0.4939 0.2466 0.069 Uiso 1 calc R . . O1B O 0.6586(14) 0.5665(7) 0.0570(5) 0.081(4) Uani 1 d . . . O2B O 0.6400(17) 0.4595(7) 0.0563(5) 0.097(5) Uani 1 d . . . C49A C 0.968(2) 0.2334(10) -0.0981(7) 0.091(7) Uani 1 d . . . H49C H 1.0085 0.219 -0.1344 0.136 Uiso 1 calc R . . H49B H 0.8742 0.227 -0.1026 0.136 Uiso 1 calc R . . H49A H 1.0028 0.2051 -0.0773 0.136 Uiso 1 calc R . . C51 C 0.282 0.105 -0.1976 0.182(12) Uani 1 d DU . . H51C H 0.3603 0.1336 -0.1851 0.274 Uiso 1 calc R . . H51A H 0.2478 0.0924 -0.1671 0.274 Uiso 1 calc R . . H51B H 0.2164 0.1313 -0.2099 0.274 Uiso 1 calc R . . O3 O 0.2207 -0.0149 -0.2701 0.275(17) Uani 1 d D . . H3 H 0.2552 -0.0496 -0.2931 0.412 Uiso 1 calc RD . . C52 C 0.3164 0.0372 -0.2467 0.30(3) Uiso 1 d D . . H52A H 0.3493 0.0519 -0.2768 0.362 Uiso 1 calc R . . H52B H 0.3897 0.0148 -0.2341 0.362 Uiso 1 calc R . . O4 O 0.2351 -0.1517 -0.309 0.236(12) Uiso 1 d D . . H4D H 0.1779 -0.1445 -0.3367 0.5 Uiso 1 d D . . H4C H 0.1894 -0.1308 -0.2748 0.742 Uiso 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd2A 0.0509(6) 0.0397(6) 0.0328(4) 0.0059(4) -0.0034(4) -0.0026(4) Pd1A 0.0461(5) 0.0413(6) 0.0342(4) 0.0100(4) -0.0039(4) -0.0040(4) Pd2B 0.0623(7) 0.0471(7) 0.0449(5) 0.0100(5) -0.0057(5) -0.0022(5) Pd1B 0.0592(6) 0.0483(7) 0.0438(5) 0.0130(5) -0.0063(5) -0.0031(5) P2A 0.0479(18) 0.0396(19) 0.0303(14) 0.0054(13) -0.0004(13) 0.0035(15) P1A 0.0434(18) 0.0379(19) 0.0378(16) 0.0108(14) -0.0023(13) -0.0015(15) Cl1A 0.0486(18) 0.056(2) 0.0389(15) 0.0123(15) 0.0007(13) -0.0091(15) P2B 0.060(2) 0.056(3) 0.0463(19) 0.0136(18) -0.0024(17) 0.0009(19) P1B 0.075(3) 0.045(2) 0.047(2) 0.0103(17) -0.0092(18) -0.003(2) Cl1B 0.065(2) 0.080(3) 0.058(2) 0.027(2) -0.0102(18) -0.018(2) Cl2A 0.086(3) 0.052(2) 0.065(2) -0.0065(19) -0.020(2) 0.008(2) Cl2B 0.123(4) 0.049(3) 0.081(3) -0.001(2) -0.023(3) 0.008(3) C18A 0.059(9) 0.069(11) 0.059(9) 0.020(8) -0.012(7) 0.018(8) C17A 0.080(14) 0.097(17) 0.090(14) 0.028(13) 0.011(11) 0.039(12) C16A 0.085(13) 0.073(13) 0.071(11) 0.017(10) 0.022(10) 0.028(11) C15A 0.104(16) 0.089(16) 0.056(10) -0.004(10) -0.009(10) 0.035(13) C14A 0.074(12) 0.083(14) 0.053(9) -0.007(9) -0.021(8) 0.010(10) C13A 0.048(8) 0.040(8) 0.047(7) 0.008(6) 0.001(6) 0.005(6) C25A 0.055(8) 0.046(9) 0.046(7) 0.022(6) -0.008(6) -0.003(7) C26A 0.067(11) 0.058(11) 0.068(10) 0.019(8) -0.024(8) 0.003(8) C27A 0.096(16) 0.103(19) 0.086(14) 0.026(13) -0.049(12) -0.001(14) C28A 0.075(13) 0.13(2) 0.077(12) 0.040(13) -0.034(10) 0.011(13) C29A 0.058(10) 0.072(12) 0.070(10) 0.040(9) 0.004(8) 0.007(9) C30A 0.032(6) 0.062(10) 0.061(8) 0.020(7) -0.018(6) -0.024(6) C19A 0.062(9) 0.032(7) 0.032(6) 0.006(5) -0.007(6) -0.005(6) C20A 0.059(10) 0.065(12) 0.088(12) 0.038(10) 0.003(9) -0.006(8) C21A 0.14(2) 0.050(12) 0.109(17) 0.042(12) -0.009(15) -0.013(13) C22A 0.15(2) 0.061(13) 0.076(13) 0.024(11) 0.001(14) -0.041(14) C23A 0.091(14) 0.083(15) 0.063(11) 0.017(10) 0.010(10) -0.033(12) C24A 0.075(11) 0.049(10) 0.061(9) 0.011(8) 0.015(8) 0.001(8) C37A 0.051(8) 0.049(9) 0.042(7) 0.008(6) 0.007(6) 0.010(7) C38A 0.041(8) 0.095(15) 0.065(10) 0.017(10) 0.006(7) 0.000(9) C39A 0.079(13) 0.076(14) 0.092(14) 0.024(12) 0.040(11) -0.002(11) C40A 0.091(15) 0.089(16) 0.099(15) 0.048(13) 0.049(12) 0.041(12) C41A 0.079(13) 0.115(18) 0.052(9) 0.041(10) 0.022(9) 0.043(12) C42A 0.069(10) 0.079(13) 0.040(7) 0.021(8) 0.007(7) 0.020(9) C31A 0.079(11) 0.053(10) 0.034(7) 0.007(6) -0.017(7) 0.011(8) C36A 0.089(13) 0.085(14) 0.052(9) 0.010(9) -0.002(9) 0.052(11) C35A 0.13(2) 0.12(2) 0.072(13) 0.023(13) -0.009(13) 0.053(16) C34A 0.19(3) 0.055(13) 0.107(18) 0.015(12) -0.065(19) 0.039(16) C33A 0.17(3) 0.075(16) 0.105(17) 0.047(14) -0.082(17) -0.025(16) C32A 0.083(14) 0.100(18) 0.078(13) 0.035(12) -0.023(11) -0.015(13) C43A 0.049(8) 0.051(9) 0.037(7) 0.007(6) -0.001(6) 0.000(7) C44A 0.049(8) 0.070(12) 0.053(8) 0.014(8) 0.006(7) 0.008(8) C45A 0.068(11) 0.102(16) 0.049(9) 0.005(10) 0.010(8) 0.010(11) C46A 0.053(9) 0.084(14) 0.059(10) -0.012(9) -0.009(7) -0.010(9) C47A 0.065(11) 0.054(11) 0.070(11) 0.008(8) 0.006(8) -0.005(8) C48A 0.047(8) 0.057(10) 0.052(8) 0.003(7) 0.000(6) -0.004(7) C25B 0.069(10) 0.048(10) 0.054(8) 0.013(7) -0.001(7) 0.003(8) C30B 0.085(12) 0.064(11) 0.065(10) 0.026(9) 0.014(9) 0.025(9) C29B 0.078(13) 0.083(15) 0.071(11) 0.036(11) -0.005(9) 0.003(11) C28B 0.104(16) 0.103(17) 0.074(12) 0.040(12) -0.022(11) 0.011(13) C27B 0.12(2) 0.074(15) 0.100(16) 0.025(13) -0.043(14) -0.025(14) C26B 0.088(14) 0.070(13) 0.070(11) 0.015(10) -0.033(10) -0.007(11) C13B 0.089(13) 0.048(10) 0.053(9) 0.014(7) -0.013(8) -0.017(9) C18B 0.087(14) 0.067(13) 0.079(12) 0.029(10) -0.004(10) -0.014(10) C17B 0.079(14) 0.086(16) 0.090(14) 0.015(12) 0.010(11) -0.025(12) C16B 0.15(2) 0.081(17) 0.067(12) 0.023(12) 0.000(14) -0.050(16) C15B 0.14(2) 0.087(18) 0.13(2) 0.059(16) -0.023(18) -0.037(17) C14B 0.108(17) 0.066(14) 0.104(16) 0.044(12) -0.017(13) -0.018(12) C19B 0.110(15) 0.045(10) 0.057(9) 0.018(8) -0.003(9) -0.005(10) C24B 0.096(15) 0.071(14) 0.079(13) -0.014(11) 0.011(11) 0.000(11) C23B 0.17(3) 0.066(14) 0.073(14) 0.003(11) 0.026(15) 0.008(16) C22B 0.14(2) 0.072(14) 0.075(13) 0.027(11) 0.028(13) 0.043(15) C21B 0.077(14) 0.102(19) 0.094(15) 0.022(13) -0.007(11) 0.017(13) C20B 0.112(16) 0.096(16) 0.048(9) 0.020(10) -0.003(10) 0.025(13) C31B 0.085(13) 0.052(10) 0.060(9) 0.017(8) -0.009(9) 0.002(9) C36B 0.113(18) 0.062(13) 0.102(15) 0.040(12) -0.018(13) -0.008(12) C35B 0.21(4) 0.082(19) 0.11(2) 0.057(17) -0.01(2) 0.00(2) C34B 0.27(5) 0.075(18) 0.085(18) 0.017(14) -0.05(2) 0.03(2) C33B 0.20(3) 0.095(18) 0.068(13) -0.002(12) -0.024(15) 0.10(2) C32B 0.089(14) 0.089(15) 0.050(9) 0.017(9) -0.009(9) 0.016(11) C43B 0.071(11) 0.060(11) 0.055(9) 0.016(8) 0.010(8) 0.009(8) C48B 0.079(12) 0.084(14) 0.056(9) 0.020(9) 0.000(9) 0.012(11) C47B 0.121(19) 0.113(19) 0.070(12) 0.053(13) 0.026(12) 0.046(16) C46B 0.13(2) 0.078(15) 0.107(18) 0.043(14) 0.067(16) 0.031(14) C45B 0.074(13) 0.075(15) 0.110(17) 0.034(13) 0.030(12) 0.001(11) C44B 0.082(13) 0.065(12) 0.079(12) 0.019(10) 0.005(10) 0.004(10) C37B 0.042(8) 0.058(10) 0.056(8) 0.009(7) -0.006(6) 0.004(7) C42B 0.066(10) 0.054(10) 0.063(10) 0.012(8) 0.002(8) 0.002(8) C41B 0.058(11) 0.064(12) 0.097(14) -0.001(11) 0.001(10) -0.010(9) C40B 0.065(11) 0.081(15) 0.072(12) -0.022(11) 0.002(9) -0.020(10) C39B 0.054(9) 0.107(16) 0.042(8) 0.009(9) -0.012(7) -0.017(10) C38B 0.060(10) 0.081(13) 0.057(9) 0.013(9) -0.009(8) -0.011(9) N1A 0.042(6) 0.033(6) 0.043(6) 0.008(5) 0.010(4) -0.003(5) N2A 0.059(7) 0.046(7) 0.039(6) 0.013(5) -0.003(5) -0.003(6) C2B 0.056(9) 0.063(11) 0.041(7) 0.016(7) 0.001(6) 0.005(8) C7A 0.034(6) 0.040(8) 0.032(6) 0.007(5) 0.006(5) 0.002(5) C2A 0.032(6) 0.038(7) 0.053(7) 0.022(6) -0.008(5) -0.010(5) C9A 0.031(6) 0.064(10) 0.035(6) 0.021(6) -0.002(5) 0.000(6) C8A 0.035(6) 0.045(8) 0.033(6) 0.012(5) -0.014(5) -0.009(5) O2A 0.150(14) 0.065(9) 0.047(6) -0.011(6) 0.008(7) 0.003(9) N3A 0.073(9) 0.058(9) 0.045(7) 0.009(6) 0.010(6) 0.001(7) O1A 0.106(10) 0.072(9) 0.040(6) 0.013(6) 0.012(6) 0.003(7) C3A 0.059(9) 0.054(10) 0.038(7) 0.012(6) -0.007(6) -0.016(7) C11A 0.057(8) 0.043(8) 0.036(6) 0.000(6) -0.004(6) 0.011(7) C3B 0.070(10) 0.053(10) 0.044(8) 0.016(7) 0.000(7) -0.003(8) C10A 0.043(7) 0.051(9) 0.025(6) -0.001(5) 0.003(5) 0.005(6) C12A 0.052(8) 0.027(7) 0.054(8) 0.014(6) -0.001(6) 0.003(6) N4A 0.090(11) 0.077(11) 0.042(7) 0.018(7) 0.001(7) -0.015(9) N4B 0.080(10) 0.085(12) 0.052(8) 0.026(8) 0.002(7) -0.016(9) C1A 0.050(8) 0.040(8) 0.038(6) 0.009(6) -0.001(6) 0.000(6) C1B 0.076(11) 0.058(11) 0.053(9) 0.017(8) -0.003(8) -0.013(9) C4A 0.051(8) 0.058(10) 0.045(7) 0.013(7) 0.001(6) 0.003(7) C4B 0.060(10) 0.079(13) 0.051(8) 0.025(8) -0.011(7) -0.013(9) C5A 0.069(10) 0.062(11) 0.053(8) 0.026(8) 0.001(7) -0.012(8) C5B 0.083(13) 0.071(13) 0.071(11) 0.033(10) 0.002(9) -0.023(10) C6A 0.069(10) 0.046(9) 0.049(8) 0.014(7) -0.010(7) -0.016(7) C6B 0.075(12) 0.061(11) 0.063(10) 0.020(9) 0.004(8) -0.013(9) C50A 0.084(13) 0.124(19) 0.057(10) 0.047(11) 0.009(9) -0.021(12) C50B 0.090(15) 0.110(19) 0.071(12) 0.033(12) 0.005(10) -0.020(13) C49B 0.13(2) 0.099(18) 0.054(10) 0.018(11) 0.009(11) -0.017(15) N1B 0.061(8) 0.048(8) 0.041(6) 0.009(5) -0.021(5) 0.002(6) N3B 0.066(9) 0.067(10) 0.047(7) 0.004(7) -0.005(6) 0.012(8) N2B 0.052(7) 0.048(8) 0.058(7) 0.009(6) -0.007(6) -0.013(6) C8B 0.066(10) 0.043(9) 0.053(8) -0.002(7) -0.001(7) 0.006(7) C7B 0.055(9) 0.054(10) 0.046(8) 0.008(7) -0.011(6) -0.001(7) C11B 0.055(9) 0.046(9) 0.059(9) 0.002(7) -0.013(7) 0.003(7) C9B 0.048(8) 0.050(9) 0.057(8) 0.014(7) 0.003(6) 0.003(7) C10B 0.052(9) 0.060(11) 0.053(8) 0.005(7) -0.004(7) -0.001(8) C12B 0.052(9) 0.071(12) 0.052(8) 0.024(8) -0.012(7) 0.001(8) O1B 0.103(11) 0.082(10) 0.054(7) 0.020(7) 0.004(7) -0.004(8) O2B 0.162(15) 0.063(9) 0.050(7) 0.000(6) -0.001(8) 0.013(9) C49A 0.14(2) 0.086(16) 0.043(9) 0.014(9) 0.005(10) -0.016(14) C51 0.182(12) 0.183(12) 0.182(12) 0.063(4) 0.0030(10) 0.0010(10) O3 0.26(3) 0.28(3) 0.38(5) 0.24(4) -0.03(3) 0.07(3) #------------------ MOLECULAR GEOMETRY --------------------------------------# _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 Pd2A C8A 1.999(13) . ? Pd2A P2A 2.251(4) . ? Pd2A Cl2A 2.388(4) . ? Pd2A Cl1A 2.390(4) . ? Pd2A Pd1A 3.1294(14) . ? Pd1A C2A 2.010(13) . ? Pd1A N1A 2.124(11) . ? Pd1A P1A 2.285(3) . ? Pd1A Cl1A 2.434(3) . ? Pd2B C8B 2.000(15) . ? Pd2B P2B 2.245(4) . ? Pd2B Cl2B 2.378(5) . ? Pd2B Cl1B 2.389(4) . ? Pd2B Pd1B 3.1306(16) . ? Pd1B C2B 1.998(16) . ? Pd1B N1B 2.116(12) . ? Pd1B P1B 2.285(4) . ? Pd1B Cl1B 2.424(4) . ? P2A C31A 1.808(9) . ? P2A C37A 1.821(8) . ? P2A C43A 1.827(7) . ? P1A C13A 1.823(7) . ? P1A C19A 1.824(8) . ? P1A C25A 1.848(7) . ? P2B C43B 1.824(9) . ? P2B C31B 1.830(10) . ? P2B C37B 1.830(8) . ? P1B C19B 1.820(9) . ? P1B C13B 1.824(10) . ? P1B C25B 1.832(9) . ? C18A C17A 1.39 . ? C18A C13A 1.39 . ? C18A H18A 0.93 . ? C17A C16A 1.39 . ? C17A H17A 0.93 . ? C16A C15A 1.39 . ? C16A H16A 0.93 . ? C15A C14A 1.39 . ? C15A H15A 0.93 . ? C14A C13A 1.39 . ? C14A H14A 0.93 . ? C25A C26A 1.39 . ? C25A C30A 1.39 . ? C26A C27A 1.39 . ? C26A H26A 0.93 . ? C27A C28A 1.39 . ? C27A H27A 0.93 . ? C28A C29A 1.39 . ? C28A H28A 0.93 . ? C29A C30A 1.39 . ? C29A H29A 0.93 . ? C30A H30A 0.93 . ? C19A C20A 1.39 . ? C19A C24A 1.39 . ? C20A C21A 1.39 . ? C20A H20A 0.93 . ? C21A C22A 1.39 . ? C21A H21A 0.93 . ? C22A C23A 1.39 . ? C22A H22A 0.93 . ? C23A C24A 1.39 . ? C23A H23A 0.93 . ? C24A H24A 0.93 . ? C37A C38A 1.39 . ? C37A C42A 1.39 . ? C38A C39A 1.39 . ? C38A H38A 0.93 . ? C39A C40A 1.39 . ? C39A H39A 0.93 . ? C40A C41A 1.39 . ? C40A H40A 0.93 . ? C41A C42A 1.39 . ? C41A H41A 0.93 . ? C42A H42A 0.93 . ? C31A C36A 1.39 . ? C31A C32A 1.39 . ? C36A C35A 1.39 . ? C36A H36 0.93 . ? C35A C34A 1.39 . ? C35A H35A 0.93 . ? C34A C33A 1.39 . ? C34A H34A 0.93 . ? C33A C32A 1.39 . ? C33A H33A 0.93 . ? C32A H32A 0.93 . ? C43A C44A 1.39 . ? C43A C48A 1.39 . ? C44A C45A 1.39 . ? C44A H44A 0.93 . ? C45A C46A 1.39 . ? C45A H45A 0.93 . ? C46A C47A 1.39 . ? C46A H46A 0.93 . ? C47A C48A 1.39 . ? C47A H47A 0.93 . ? C48A H48A 0.93 . ? C25B C30B 1.39 . ? C25B C26B 1.39 . ? C30B C29B 1.39 . ? C30B H30B 0.93 . ? C29B C28B 1.39 . ? C29B H29B 0.93 . ? C28B C27B 1.39 . ? C28B H28B 0.93 . ? C27B C26B 1.39 . ? C27B H27B 0.93 . ? C26B H26B 0.93 . ? C13B C18B 1.39 . ? C13B C14B 1.39 . ? C18B C17B 1.39 . ? C18B H18B 0.93 . ? C17B C16B 1.39 . ? C17B H17B 0.93 . ? C16B C15B 1.39 . ? C16B H16B 0.93 . ? C15B C14B 1.39 . ? C15B H15B 0.93 . ? C14B H14B 0.93 . ? C19B C24B 1.39 . ? C19B C20B 1.39 . ? C24B C23B 1.39 . ? C24B H24B 0.93 . ? C23B C22B 1.39 . ? C23B H23B 0.93 . ? C22B C21B 1.39 . ? C22B H22B 0.93 . ? C21B C20B 1.39 . ? C21B H21B 0.93 . ? C20B H20B 0.93 . ? C31B C36B 1.39 . ? C31B C32B 1.39 . ? C36B C35B 1.39 . ? C36B H36B 0.93 . ? C35B C34B 1.39 . ? C35B H35B 0.93 . ? C34B C33B 1.39 . ? C34B H34B 0.93 . ? C33B C32B 1.39 . ? C33B H33B 0.93 . ? C32B H32B 0.93 . ? C43B C48B 1.39 . ? C43B C44B 1.39 . ? C48B C47B 1.39 . ? C48B H48B 0.93 . ? C47B C46B 1.39 . ? C47B H47B 0.93 . ? C46B C45B 1.39 . ? C46B H46B 0.93 . ? C45B C44B 1.39 . ? C45B H45B 0.93 . ? C44B H44B 0.93 . ? C37B C42B 1.39 . ? C37B C38B 1.39 . ? C42B C41B 1.39 . ? C42B H42B 0.93 . ? C41B C40B 1.39 . ? C41B H41B 0.93 . ? C40B C39B 1.39 . ? C40B H40B 0.93 . ? C39B C38B 1.39 . ? C39B H39B 0.93 . ? C38B H38B 0.93 . ? N1A N2A 1.312(15) . ? N1A C7A 1.401(15) . ? N2A C1A 1.362(16) . ? C2B C3B 1.357(19) . ? C2B C1B 1.44(2) . ? C7A C12A 1.400(16) . ? C7A C8A 1.427(17) . ? C2A C3A 1.367(18) . ? C2A C1A 1.427(18) . ? C9A C10A 1.375(18) . ? C9A C8A 1.381(16) . ? C9A H9A 0.93 . ? O2A N3A 1.209(17) . ? N3A O1A 1.231(17) . ? N3A C10A 1.465(16) . ? C3A C4A 1.41(2) . ? C3A H3A 0.93 . ? C11A C10A 1.373(19) . ? C11A C12A 1.380(18) . ? C11A H11A 0.93 . ? C3B C4B 1.41(2) . ? C3B H3B 0.93 . ? C12A H12A 0.93 . ? N4A C4A 1.350(18) . ? N4A C49A 1.43(2) . ? N4A C50A 1.46(2) . ? N4B C4B 1.35(2) . ? N4B C49B 1.43(2) . ? N4B C50B 1.45(2) . ? C1A C6A 1.40(2) . ? C1B N2B 1.351(19) . ? C1B C6B 1.40(2) . ? C4A C5A 1.41(2) . ? C4B C5B 1.42(2) . ? C5A C6A 1.37(2) . ? C5A H5A 0.93 . ? C5B C6B 1.36(2) . ? C5B H5B 0.93 . ? C6A H6A 0.93 . ? C6B H6B 0.93 . ? C50A H50A 0.96 . ? C50A H50C 0.96 . ? C50A H50B 0.96 . ? C50B H50F 0.96 . ? C50B H50E 0.96 . ? C50B H50D 0.96 . ? C49B H49D 0.96 . ? C49B H49F 0.96 . ? C49B H49E 0.96 . ? N1B N2B 1.280(17) . ? N1B C7B 1.439(17) . ? N3B O1B 1.212(18) . ? N3B O2B 1.222(18) . ? N3B C10B 1.485(19) . ? C8B C7B 1.38(2) . ? C8B C9B 1.40(2) . ? C7B C12B 1.39(2) . ? C11B C12B 1.37(2) . ? C11B C10B 1.40(2) . ? C11B H11B 0.93 . ? C9B C10B 1.37(2) . ? C9B H9B 0.93 . ? C12B H12B 0.93 . ? C49A H49C 0.96 . ? C49A H49B 0.96 . ? C49A H49A 0.96 . ? C51 C52 1.5378 . ? C51 H51C 0.96 . ? C51 H51A 0.96 . ? C51 H51B 0.96 . ? O3 C52 1.3898 . ? O3 H3 0.82 . ? C52 H52A 0.97 . ? C52 H52B 0.97 . ? O4 H4D 0.95 . ? O4 H4C 0.9501 . ? 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 C8A Pd2A P2A 89.6(3) . . ? C8A Pd2A Cl2A 177.5(4) . . ? P2A Pd2A Cl2A 90.23(14) . . ? C8A Pd2A Cl1A 85.7(3) . . ? P2A Pd2A Cl1A 173.02(15) . . ? Cl2A Pd2A Cl1A 94.31(14) . . ? C8A Pd2A Pd1A 85.8(3) . . ? P2A Pd2A Pd1A 124.44(10) . . ? Cl2A Pd2A Pd1A 92.28(11) . . ? Cl1A Pd2A Pd1A 50.16(9) . . ? C2A Pd1A N1A 79.3(5) . . ? C2A Pd1A P1A 93.6(4) . . ? N1A Pd1A P1A 172.1(3) . . ? C2A Pd1A Cl1A 173.9(4) . . ? N1A Pd1A Cl1A 94.6(3) . . ? P1A Pd1A Cl1A 92.48(12) . . ? C2A Pd1A Pd2A 127.2(3) . . ? N1A Pd1A Pd2A 69.0(3) . . ? P1A Pd1A Pd2A 118.49(10) . . ? Cl1A Pd1A Pd2A 48.95(8) . . ? C8B Pd2B P2B 89.1(5) . . ? C8B Pd2B Cl2B 176.5(5) . . ? P2B Pd2B Cl2B 90.44(18) . . ? C8B Pd2B Cl1B 85.3(5) . . ? P2B Pd2B Cl1B 172.28(18) . . ? Cl2B Pd2B Cl1B 94.88(19) . . ? C8B Pd2B Pd1B 85.0(5) . . ? P2B Pd2B Pd1B 124.38(12) . . ? Cl2B Pd2B Pd1B 92.45(13) . . ? Cl1B Pd2B Pd1B 49.90(11) . . ? C2B Pd1B N1B 78.6(6) . . ? C2B Pd1B P1B 93.8(5) . . ? N1B Pd1B P1B 171.2(4) . . ? C2B Pd1B Cl1B 173.3(5) . . ? N1B Pd1B Cl1B 94.7(4) . . ? P1B Pd1B Cl1B 92.88(16) . . ? C2B Pd1B Pd2B 127.5(4) . . ? N1B Pd1B Pd2B 70.0(3) . . ? P1B Pd1B Pd2B 118.50(13) . . ? Cl1B Pd1B Pd2B 48.95(10) . . ? C31A P2A C37A 108.4(5) . . ? C31A P2A C43A 104.4(5) . . ? C37A P2A C43A 102.8(5) . . ? C31A P2A Pd2A 113.7(4) . . ? C37A P2A Pd2A 110.9(3) . . ? C43A P2A Pd2A 115.8(3) . . ? C13A P1A C19A 103.6(5) . . ? C13A P1A C25A 107.0(5) . . ? C19A P1A C25A 102.0(5) . . ? C13A P1A Pd1A 112.1(3) . . ? C19A P1A Pd1A 115.0(3) . . ? C25A P1A Pd1A 115.8(4) . . ? Pd2A Cl1A Pd1A 80.88(11) . . ? C43B P2B C31B 107.1(6) . . ? C43B P2B C37B 103.1(5) . . ? C31B P2B C37B 104.4(5) . . ? C43B P2B Pd2B 111.0(4) . . ? C31B P2B Pd2B 114.0(5) . . ? C37B P2B Pd2B 116.3(4) . . ? C19B P1B C13B 104.7(6) . . ? C19B P1B C25B 106.5(6) . . ? C13B P1B C25B 102.3(6) . . ? C19B P1B Pd1B 112.3(5) . . ? C13B P1B Pd1B 114.2(4) . . ? C25B P1B Pd1B 115.7(4) . . ? Pd2B Cl1B Pd1B 81.15(14) . . ? C17A C18A C13A 120 . . ? C17A C18A H18A 120 . . ? C13A C18A H18A 120 . . ? C16A C17A C18A 120 . . ? C16A C17A H17A 120 . . ? C18A C17A H17A 120 . . ? C17A C16A C15A 120 . . ? C17A C16A H16A 120 . . ? C15A C16A H16A 120 . . ? C14A C15A C16A 120 . . ? C14A C15A H15A 120 . . ? C16A C15A H15A 120 . . ? C15A C14A C13A 120 . . ? C15A C14A H14A 120 . . ? C13A C14A H14A 120 . . ? C14A C13A C18A 120 . . ? C14A C13A P1A 121.1(6) . . ? C18A C13A P1A 118.9(6) . . ? C26A C25A C30A 120 . . ? C26A C25A P1A 119.7(6) . . ? C30A C25A P1A 120.3(6) . . ? C25A C26A C27A 120 . . ? C25A C26A H26A 120 . . ? C27A C26A H26A 120 . . ? C28A C27A C26A 120 . . ? C28A C27A H27A 120 . . ? C26A C27A H27A 120 . . ? C27A C28A C29A 120 . . ? C27A C28A H28A 120 . . ? C29A C28A H28A 120 . . ? C30A C29A C28A 120 . . ? C30A C29A H29A 120 . . ? C28A C29A H29A 120 . . ? C29A C30A C25A 120 . . ? C29A C30A H30A 120 . . ? C25A C30A H30A 120 . . ? C20A C19A C24A 120 . . ? C20A C19A P1A 119.6(7) . . ? C24A C19A P1A 120.3(7) . . ? C21A C20A C19A 120 . . ? C21A C20A H20A 120 . . ? C19A C20A H20A 120 . . ? C22A C21A C20A 120 . . ? C22A C21A H21A 120 . . ? C20A C21A H21A 120 . . ? C21A C22A C23A 120 . . ? C21A C22A H22A 120 . . ? C23A C22A H22A 120 . . ? C22A C23A C24A 120 . . ? C22A C23A H23A 120 . . ? C24A C23A H23A 120 . . ? C23A C24A C19A 120 . . ? C23A C24A H24A 120 . . ? C19A C24A H24A 120 . . ? C38A C37A C42A 120 . . ? C38A C37A P2A 120.8(6) . . ? C42A C37A P2A 118.9(6) . . ? C37A C38A C39A 120 . . ? C37A C38A H38A 120 . . ? C39A C38A H38A 120 . . ? C40A C39A C38A 120 . . ? C40A C39A H39A 120 . . ? C38A C39A H39A 120 . . ? C39A C40A C41A 120 . . ? C39A C40A H40A 120 . . ? C41A C40A H40A 120 . . ? C42A C41A C40A 120 . . ? C42A C41A H41A 120 . . ? C40A C41A H41A 120 . . ? C41A C42A C37A 120 . . ? C41A C42A H42A 120 . . ? C37A C42A H42A 120 . . ? C36A C31A C32A 120 . . ? C36A C31A P2A 121.2(8) . . ? C32A C31A P2A 118.8(8) . . ? C35A C36A C31A 120 . . ? C35A C36A H36 120 . . ? C31A C36A H36 120 . . ? C34A C35A C36A 120 . . ? C34A C35A H35A 120 . . ? C36A C35A H35A 120 . . ? C35A C34A C33A 120 . . ? C35A C34A H34A 120 . . ? C33A C34A H34A 120 . . ? C32A C33A C34A 120 . . ? C32A C33A H33A 120 . . ? C34A C33A H33A 120 . . ? C33A C32A C31A 120 . . ? C33A C32A H32A 120 . . ? C31A C32A H32A 120 . . ? C44A C43A C48A 120 . . ? C44A C43A P2A 120.4(6) . . ? C48A C43A P2A 119.2(6) . . ? C43A C44A C45A 120 . . ? C43A C44A H44A 120 . . ? C45A C44A H44A 120 . . ? C44A C45A C46A 120 . . ? C44A C45A H45A 120 . . ? C46A C45A H45A 120 . . ? C47A C46A C45A 120 . . ? C47A C46A H46A 120 . . ? C45A C46A H46A 120 . . ? C48A C47A C46A 120 . . ? C48A C47A H47A 120 . . ? C46A C47A H47A 120 . . ? C47A C48A C43A 120 . . ? C47A C48A H48A 120 . . ? C43A C48A H48A 120 . . ? C30B C25B C26B 120 . . ? C30B C25B P1B 119.9(7) . . ? C26B C25B P1B 120.1(7) . . ? C29B C30B C25B 120 . . ? C29B C30B H30B 120 . . ? C25B C30B H30B 120 . . ? C30B C29B C28B 120 . . ? C30B C29B H29B 120 . . ? C28B C29B H29B 120 . . ? C27B C28B C29B 120 . . ? C27B C28B H28B 120 . . ? C29B C28B H28B 120 . . ? C28B C27B C26B 120 . . ? C28B C27B H27B 120 . . ? C26B C27B H27B 120 . . ? C27B C26B C25B 120 . . ? C27B C26B H26B 120 . . ? C25B C26B H26B 120 . . ? C18B C13B C14B 120 . . ? C18B C13B P1B 120.8(9) . . ? C14B C13B P1B 119.2(9) . . ? C17B C18B C13B 120 . . ? C17B C18B H18B 120 . . ? C13B C18B H18B 120 . . ? C18B C17B C16B 120 . . ? C18B C17B H17B 120 . . ? C16B C17B H17B 120 . . ? C15B C16B C17B 120 . . ? C15B C16B H16B 120 . . ? C17B C16B H16B 120 . . ? C16B C15B C14B 120 . . ? C16B C15B H15B 120 . . ? C14B C15B H15B 120 . . ? C15B C14B C13B 120 . . ? C15B C14B H14B 120 . . ? C13B C14B H14B 120 . . ? C24B C19B C20B 120 . . ? C24B C19B P1B 121.3(8) . . ? C20B C19B P1B 118.6(8) . . ? C19B C24B C23B 120 . . ? C19B C24B H24B 120 . . ? C23B C24B H24B 120 . . ? C22B C23B C24B 120 . . ? C22B C23B H23B 120 . . ? C24B C23B H23B 120 . . ? C21B C22B C23B 120 . . ? C21B C22B H22B 120 . . ? C23B C22B H22B 120 . . ? C22B C21B C20B 120 . . ? C22B C21B H21B 120 . . ? C20B C21B H21B 120 . . ? C21B C20B C19B 120 . . ? C21B C20B H20B 120 . . ? C19B C20B H20B 120 . . ? C36B C31B C32B 120 . . ? C36B C31B P2B 117.0(9) . . ? C32B C31B P2B 123.0(9) . . ? C35B C36B C31B 120 . . ? C35B C36B H36B 120 . . ? C31B C36B H36B 120 . . ? C36B C35B C34B 120 . . ? C36B C35B H35B 120 . . ? C34B C35B H35B 120 . . ? C33B C34B C35B 120 . . ? C33B C34B H34B 120 . . ? C35B C34B H34B 120 . . ? C34B C33B C32B 120 . . ? C34B C33B H33B 120 . . ? C32B C33B H33B 120 . . ? C33B C32B C31B 120 . . ? C33B C32B H32B 120 . . ? C31B C32B H32B 120 . . ? C48B C43B C44B 120 . . ? C48B C43B P2B 119.0(7) . . ? C44B C43B P2B 120.5(7) . . ? C43B C48B C47B 120 . . ? C43B C48B H48B 120 . . ? C47B C48B H48B 120 . . ? C46B C47B C48B 120 . . ? C46B C47B H47B 120 . . ? C48B C47B H47B 120 . . ? C45B C46B C47B 120 . . ? C45B C46B H46B 120 . . ? C47B C46B H46B 120 . . ? C46B C45B C44B 120 . . ? C46B C45B H45B 120 . . ? C44B C45B H45B 120 . . ? C45B C44B C43B 120 . . ? C45B C44B H44B 120 . . ? C43B C44B H44B 120 . . ? C42B C37B C38B 120 . . ? C42B C37B P2B 119.9(7) . . ? C38B C37B P2B 119.5(7) . . ? C41B C42B C37B 120 . . ? C41B C42B H42B 120 . . ? C37B C42B H42B 120 . . ? C42B C41B C40B 120 . . ? C42B C41B H41B 120 . . ? C40B C41B H41B 120 . . ? C41B C40B C39B 120 . . ? C41B C40B H40B 120 . . ? C39B C40B H40B 120 . . ? C38B C39B C40B 120 . . ? C38B C39B H39B 120 . . ? C40B C39B H39B 120 . . ? C39B C38B C37B 120 . . ? C39B C38B H38B 120 . . ? C37B C38B H38B 120 . . ? N2A N1A C7A 115.0(11) . . ? N2A N1A Pd1A 114.9(8) . . ? C7A N1A Pd1A 129.3(9) . . ? N1A N2A C1A 112.7(12) . . ? C3B C2B C1B 117.4(16) . . ? C3B C2B Pd1B 132.3(14) . . ? C1B C2B Pd1B 110.3(11) . . ? C12A C7A N1A 120.9(12) . . ? C12A C7A C8A 120.5(11) . . ? N1A C7A C8A 118.5(11) . . ? C3A C2A C1A 117.5(13) . . ? C3A C2A Pd1A 133.4(11) . . ? C1A C2A Pd1A 109.1(10) . . ? C10A C9A C8A 119.6(13) . . ? C10A C9A H9A 120.2 . . ? C8A C9A H9A 120.2 . . ? C9A C8A C7A 118.1(12) . . ? C9A C8A Pd2A 123.7(11) . . ? C7A C8A Pd2A 118.1(9) . . ? O2A N3A O1A 122.5(14) . . ? O2A N3A C10A 118.8(15) . . ? O1A N3A C10A 118.6(14) . . ? C2A C3A C4A 123.6(14) . . ? C2A C3A H3A 118.2 . . ? C4A C3A H3A 118.2 . . ? C10A C11A C12A 119.2(13) . . ? C10A C11A H11A 120.4 . . ? C12A C11A H11A 120.4 . . ? C2B C3B C4B 123.6(16) . . ? C2B C3B H3B 118.2 . . ? C4B C3B H3B 118.2 . . ? C11A C10A C9A 122.9(11) . . ? C11A C10A N3A 118.0(13) . . ? C9A C10A N3A 119.1(13) . . ? C11A C12A C7A 119.2(13) . . ? C11A C12A H12A 120.4 . . ? C7A C12A H12A 120.4 . . ? C4A N4A C49A 121.8(16) . . ? C4A N4A C50A 121.4(16) . . ? C49A N4A C50A 116.8(14) . . ? C4B N4B C49B 121.3(17) . . ? C4B N4B C50B 123.2(18) . . ? C49B N4B C50B 115.5(15) . . ? N2A C1A C6A 117.7(13) . . ? N2A C1A C2A 122.8(13) . . ? C6A C1A C2A 119.4(12) . . ? N2B C1B C6B 119.6(16) . . ? N2B C1B C2B 120.4(15) . . ? C6B C1B C2B 120.0(15) . . ? N4A C4A C3A 119.7(15) . . ? N4A C4A C5A 122.6(16) . . ? C3A C4A C5A 117.7(13) . . ? N4B C4B C3B 121.5(17) . . ? N4B C4B C5B 121.2(17) . . ? C3B C4B C5B 117.3(15) . . ? C6A C5A C4A 119.6(15) . . ? C6A C5A H5A 120.2 . . ? C4A C5A H5A 120.2 . . ? C6B C5B C4B 120.5(17) . . ? C6B C5B H5B 119.7 . . ? C4B C5B H5B 119.7 . . ? C5A C6A C1A 122.0(15) . . ? C5A C6A H6A 119 . . ? C1A C6A H6A 119 . . ? C5B C6B C1B 121.0(18) . . ? C5B C6B H6B 119.5 . . ? C1B C6B H6B 119.5 . . ? N4A C50A H50A 109.5 . . ? N4A C50A H50C 109.5 . . ? H50A C50A H50C 109.5 . . ? N4A C50A H50B 109.5 . . ? H50A C50A H50B 109.5 . . ? H50C C50A H50B 109.5 . . ? N4B C50B H50F 109.5 . . ? N4B C50B H50E 109.5 . . ? H50F C50B H50E 109.5 . . ? N4B C50B H50D 109.5 . . ? H50F C50B H50D 109.5 . . ? H50E C50B H50D 109.5 . . ? N4B C49B H49D 109.5 . . ? N4B C49B H49F 109.5 . . ? H49D C49B H49F 109.5 . . ? N4B C49B H49E 109.5 . . ? H49D C49B H49E 109.5 . . ? H49F C49B H49E 109.5 . . ? N2B N1B C7B 114.9(13) . . ? N2B N1B Pd1B 115.7(9) . . ? C7B N1B Pd1B 129.3(11) . . ? O1B N3B O2B 124.1(15) . . ? O1B N3B C10B 118.8(15) . . ? O2B N3B C10B 117.1(16) . . ? N1B N2B C1B 114.3(13) . . ? C7B C8B C9B 117.6(14) . . ? C7B C8B Pd2B 120.1(11) . . ? C9B C8B Pd2B 122.2(13) . . ? C8B C7B C12B 122.0(14) . . ? C8B C7B N1B 118.7(14) . . ? C12B C7B N1B 119.2(15) . . ? C12B C11B C10B 116.0(15) . . ? C12B C11B H11B 122 . . ? C10B C11B H11B 122 . . ? C10B C9B C8B 119.1(16) . . ? C10B C9B H9B 120.5 . . ? C8B C9B H9B 120.5 . . ? C9B C10B C11B 123.9(15) . . ? C9B C10B N3B 118.5(16) . . ? C11B C10B N3B 117.5(15) . . ? C11B C12B C7B 121.3(16) . . ? C11B C12B H12B 119.3 . . ? C7B C12B H12B 119.3 . . ? N4A C49A H49C 109.5 . . ? N4A C49A H49B 109.5 . . ? H49C C49A H49B 109.5 . . ? N4A C49A H49A 109.5 . . ? H49C C49A H49A 109.5 . . ? H49B C49A H49A 109.5 . . ? C52 C51 H51C 109.5 . . ? C52 C51 H51A 109.5 . . ? H51C C51 H51A 109.5 . . ? C52 C51 H51B 109.5 . . ? H51C C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C52 O3 H3 109.5 . . ? O3 C52 H52A 107.2 . . ? C51 C52 H52A 107.2 . . ? O3 C52 H52B 107.2 . . ? C51 C52 H52B 107.2 . . ? H52A C52 H52B 106.9 . . ? 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 C8A Pd2A Pd1A C2A 86.0(6) . . . . ? P2A Pd2A Pd1A C2A -0.5(5) . . . . ? Cl2A Pd2A Pd1A C2A -92.4(5) . . . . ? Cl1A Pd2A Pd1A C2A 173.9(5) . . . . ? C8A Pd2A Pd1A N1A 28.7(5) . . . . ? P2A Pd2A Pd1A N1A -57.8(3) . . . . ? Cl2A Pd2A Pd1A N1A -149.7(3) . . . . ? Cl1A Pd2A Pd1A N1A 116.6(3) . . . . ? C8A Pd2A Pd1A P1A -153.9(4) . . . . ? P2A Pd2A Pd1A P1A 119.59(15) . . . . ? Cl2A Pd2A Pd1A P1A 27.75(17) . . . . ? Cl1A Pd2A Pd1A P1A -65.96(15) . . . . ? C8A Pd2A Pd1A Cl1A -87.9(4) . . . . ? P2A Pd2A Pd1A Cl1A -174.44(17) . . . . ? Cl2A Pd2A Pd1A Cl1A 93.71(17) . . . . ? C8B Pd2B Pd1B C2B -84.7(8) . . . . ? P2B Pd2B Pd1B C2B 0.8(6) . . . . ? Cl2B Pd2B Pd1B C2B 93.0(6) . . . . ? Cl1B Pd2B Pd1B C2B -172.7(6) . . . . ? C8B Pd2B Pd1B N1B -27.6(6) . . . . ? P2B Pd2B Pd1B N1B 57.8(4) . . . . ? Cl2B Pd2B Pd1B N1B 150.0(4) . . . . ? Cl1B Pd2B Pd1B N1B -115.6(4) . . . . ? C8B Pd2B Pd1B P1B 154.6(5) . . . . ? P2B Pd2B Pd1B P1B -119.9(2) . . . . ? Cl2B Pd2B Pd1B P1B -27.7(2) . . . . ? Cl1B Pd2B Pd1B P1B 66.6(2) . . . . ? C8B Pd2B Pd1B Cl1B 88.0(5) . . . . ? P2B Pd2B Pd1B Cl1B 173.5(2) . . . . ? Cl2B Pd2B Pd1B Cl1B -94.3(2) . . . . ? C8A Pd2A P2A C31A 141.9(5) . . . . ? Cl2A Pd2A P2A C31A -40.6(4) . . . . ? Pd1A Pd2A P2A C31A -133.6(4) . . . . ? C8A Pd2A P2A C37A -95.7(5) . . . . ? Cl2A Pd2A P2A C37A 81.8(4) . . . . ? Pd1A Pd2A P2A C37A -11.1(4) . . . . ? C8A Pd2A P2A C43A 21.0(5) . . . . ? Cl2A Pd2A P2A C43A -161.5(4) . . . . ? Pd1A Pd2A P2A C43A 105.6(4) . . . . ? C2A Pd1A P1A C13A 60.9(5) . . . . ? Cl1A Pd1A P1A C13A -119.0(4) . . . . ? Pd2A Pd1A P1A C13A -75.5(4) . . . . ? C2A Pd1A P1A C19A 178.9(5) . . . . ? Cl1A Pd1A P1A C19A -1.0(4) . . . . ? Pd2A Pd1A P1A C19A 42.6(4) . . . . ? C2A Pd1A P1A C25A -62.3(5) . . . . ? Cl1A Pd1A P1A C25A 117.7(4) . . . . ? Pd2A Pd1A P1A C25A 161.3(4) . . . . ? C8A Pd2A Cl1A Pd1A 88.1(4) . . . . ? Cl2A Pd2A Cl1A Pd1A -89.37(15) . . . . ? N1A Pd1A Cl1A Pd2A -56.9(3) . . . . ? P1A Pd1A Cl1A Pd2A 126.54(12) . . . . ? C8B Pd2B P2B C43B 95.7(7) . . . . ? Cl2B Pd2B P2B C43B -80.9(4) . . . . ? Pd1B Pd2B P2B C43B 12.4(5) . . . . ? C8B Pd2B P2B C31B -143.3(7) . . . . ? Cl2B Pd2B P2B C31B 40.2(5) . . . . ? Pd1B Pd2B P2B C31B 133.4(4) . . . . ? C8B Pd2B P2B C37B -21.7(7) . . . . ? Cl2B Pd2B P2B C37B 161.7(5) . . . . ? Pd1B Pd2B P2B C37B -105.0(4) . . . . ? C2B Pd1B P1B C19B -60.9(6) . . . . ? Cl1B Pd1B P1B C19B 119.8(5) . . . . ? Pd2B Pd1B P1B C19B 76.0(5) . . . . ? C2B Pd1B P1B C13B -179.9(7) . . . . ? Cl1B Pd1B P1B C13B 0.8(5) . . . . ? Pd2B Pd1B P1B C13B -43.1(5) . . . . ? C2B Pd1B P1B C25B 61.7(6) . . . . ? Cl1B Pd1B P1B C25B -117.6(5) . . . . ? Pd2B Pd1B P1B C25B -161.5(4) . . . . ? C8B Pd2B Cl1B Pd1B -87.4(5) . . . . ? Cl2B Pd2B Cl1B Pd1B 89.10(18) . . . . ? N1B Pd1B Cl1B Pd2B 58.2(3) . . . . ? P1B Pd1B Cl1B Pd2B -126.14(16) . . . . ? C13A C18A C17A C16A 0 . . . . ? C18A C17A C16A C15A 0 . . . . ? C17A C16A C15A C14A 0 . . . . ? C16A C15A C14A C13A 0 . . . . ? C15A C14A C13A C18A 0 . . . . ? C15A C14A C13A P1A -179.4(8) . . . . ? C17A C18A C13A C14A 0 . . . . ? C17A C18A C13A P1A 179.4(8) . . . . ? C19A P1A C13A C14A 75.3(7) . . . . ? C25A P1A C13A C14A -32.1(8) . . . . ? Pd1A P1A C13A C14A -160.1(5) . . . . ? C19A P1A C13A C18A -104.1(7) . . . . ? C25A P1A C13A C18A 148.5(6) . . . . ? Pd1A P1A C13A C18A 20.5(7) . . . . ? C13A P1A C25A C26A 71.6(7) . . . . ? C19A P1A C25A C26A -36.9(7) . . . . ? Pd1A P1A C25A C26A -162.6(5) . . . . ? C13A P1A C25A C30A -111.0(7) . . . . ? C19A P1A C25A C30A 140.5(6) . . . . ? Pd1A P1A C25A C30A 14.9(7) . . . . ? C30A C25A C26A C27A 0 . . . . ? P1A C25A C26A C27A 177.4(8) . . . . ? C25A C26A C27A C28A 0 . . . . ? C26A C27A C28A C29A 0 . . . . ? C27A C28A C29A C30A 0 . . . . ? C28A C29A C30A C25A 0 . . . . ? C26A C25A C30A C29A 0 . . . . ? P1A C25A C30A C29A -177.4(8) . . . . ? C13A P1A C19A C20A 32.3(7) . . . . ? C25A P1A C19A C20A 143.4(6) . . . . ? Pd1A P1A C19A C20A -90.4(6) . . . . ? C13A P1A C19A C24A -150.7(6) . . . . ? C25A P1A C19A C24A -39.6(7) . . . . ? Pd1A P1A C19A C24A 86.6(6) . . . . ? C24A C19A C20A C21A 0 . . . . ? P1A C19A C20A C21A 177.0(7) . . . . ? C19A C20A C21A C22A 0 . . . . ? C20A C21A C22A C23A 0 . . . . ? C21A C22A C23A C24A 0 . . . . ? C22A C23A C24A C19A 0 . . . . ? C20A C19A C24A C23A 0 . . . . ? P1A C19A C24A C23A -177.0(7) . . . . ? C31A P2A C37A C38A -70.6(7) . . . . ? C43A P2A C37A C38A 39.5(7) . . . . ? Pd2A P2A C37A C38A 164.0(5) . . . . ? C31A P2A C37A C42A 116.3(6) . . . . ? C43A P2A C37A C42A -133.5(6) . . . . ? Pd2A P2A C37A C42A -9.1(7) . . . . ? C42A C37A C38A C39A 0 . . . . ? P2A C37A C38A C39A -173.0(7) . . . . ? C37A C38A C39A C40A 0 . . . . ? C38A C39A C40A C41A 0 . . . . ? C39A C40A C41A C42A 0 . . . . ? C40A C41A C42A C37A 0 . . . . ? C38A C37A C42A C41A 0 . . . . ? P2A C37A C42A C41A 173.1(7) . . . . ? C37A P2A C31A C36A 17.1(8) . . . . ? C43A P2A C31A C36A -92.0(7) . . . . ? Pd2A P2A C31A C36A 140.9(6) . . . . ? C37A P2A C31A C32A -162.6(6) . . . . ? C43A P2A C31A C32A 88.3(7) . . . . ? Pd2A P2A C31A C32A -38.8(7) . . . . ? C32A C31A C36A C35A 0 . . . . ? P2A C31A C36A C35A -179.7(8) . . . . ? C31A C36A C35A C34A 0 . . . . ? C36A C35A C34A C33A 0 . . . . ? C35A C34A C33A C32A 0 . . . . ? C34A C33A C32A C31A 0 . . . . ? C36A C31A C32A C33A 0 . . . . ? P2A C31A C32A C33A 179.7(8) . . . . ? C31A P2A C43A C44A -36.5(7) . . . . ? C37A P2A C43A C44A -149.6(6) . . . . ? Pd2A P2A C43A C44A 89.3(6) . . . . ? C31A P2A C43A C48A 151.5(6) . . . . ? C37A P2A C43A C48A 38.4(6) . . . . ? Pd2A P2A C43A C48A -82.7(6) . . . . ? C48A C43A C44A C45A 0 . . . . ? P2A C43A C44A C45A -171.9(7) . . . . ? C43A C44A C45A C46A 0 . . . . ? C44A C45A C46A C47A 0 . . . . ? C45A C46A C47A C48A 0 . . . . ? C46A C47A C48A C43A 0 . . . . ? C44A C43A C48A C47A 0 . . . . ? P2A C43A C48A C47A 172.0(7) . . . . ? C19B P1B C25B C30B 111.3(7) . . . . ? C13B P1B C25B C30B -139.0(7) . . . . ? Pd1B P1B C25B C30B -14.2(8) . . . . ? C19B P1B C25B C26B -71.1(8) . . . . ? C13B P1B C25B C26B 38.6(8) . . . . ? Pd1B P1B C25B C26B 163.4(5) . . . . ? C26B C25B C30B C29B 0 . . . . ? P1B C25B C30B C29B 177.6(8) . . . . ? C25B C30B C29B C28B 0 . . . . ? C30B C29B C28B C27B 0 . . . . ? C29B C28B C27B C26B 0 . . . . ? C28B C27B C26B C25B 0 . . . . ? C30B C25B C26B C27B 0 . . . . ? P1B C25B C26B C27B -177.6(8) . . . . ? C19B P1B C13B C18B 149.8(7) . . . . ? C25B P1B C13B C18B 38.8(8) . . . . ? Pd1B P1B C13B C18B -87.0(7) . . . . ? C19B P1B C13B C14B -31.6(8) . . . . ? C25B P1B C13B C14B -142.7(7) . . . . ? Pd1B P1B C13B C14B 91.6(7) . . . . ? C14B C13B C18B C17B 0 . . . . ? P1B C13B C18B C17B 178.6(8) . . . . ? C13B C18B C17B C16B 0 . . . . ? C18B C17B C16B C15B 0 . . . . ? C17B C16B C15B C14B 0 . . . . ? C16B C15B C14B C13B 0 . . . . ? C18B C13B C14B C15B 0 . . . . ? P1B C13B C14B C15B -178.6(8) . . . . ? C13B P1B C19B C24B -75.4(8) . . . . ? C25B P1B C19B C24B 32.5(9) . . . . ? Pd1B P1B C19B C24B 160.2(6) . . . . ? C13B P1B C19B C20B 103.2(8) . . . . ? C25B P1B C19B C20B -148.9(7) . . . . ? Pd1B P1B C19B C20B -21.3(8) . . . . ? C20B C19B C24B C23B 0 . . . . ? P1B C19B C24B C23B 178.5(9) . . . . ? C19B C24B C23B C22B 0 . . . . ? C24B C23B C22B C21B 0 . . . . ? C23B C22B C21B C20B 0 . . . . ? C22B C21B C20B C19B 0 . . . . ? C24B C19B C20B C21B 0 . . . . ? P1B C19B C20B C21B -178.6(9) . . . . ? C43B P2B C31B C36B 161.6(7) . . . . ? C37B P2B C31B C36B -89.5(7) . . . . ? Pd2B P2B C31B C36B 38.4(7) . . . . ? C43B P2B C31B C32B -17.2(9) . . . . ? C37B P2B C31B C32B 91.7(8) . . . . ? Pd2B P2B C31B C32B -140.3(7) . . . . ? C32B C31B C36B C35B 0 . . . . ? P2B C31B C36B C35B -178.8(9) . . . . ? C31B C36B C35B C34B 0 . . . . ? C36B C35B C34B C33B 0 . . . . ? C35B C34B C33B C32B 0 . . . . ? C34B C33B C32B C31B 0 . . . . ? C36B C31B C32B C33B 0 . . . . ? P2B C31B C32B C33B 178.7(9) . . . . ? C31B P2B C43B C48B -117.0(7) . . . . ? C37B P2B C43B C48B 133.3(7) . . . . ? Pd2B P2B C43B C48B 8.0(7) . . . . ? C31B P2B C43B C44B 71.2(8) . . . . ? C37B P2B C43B C44B -38.5(8) . . . . ? Pd2B P2B C43B C44B -163.8(5) . . . . ? C44B C43B C48B C47B 0 . . . . ? P2B C43B C48B C47B -171.8(8) . . . . ? C43B C48B C47B C46B 0 . . . . ? C48B C47B C46B C45B 0 . . . . ? C47B C46B C45B C44B 0 . . . . ? C46B C45B C44B C43B 0 . . . . ? C48B C43B C44B C45B 0 . . . . ? P2B C43B C44B C45B 171.7(8) . . . . ? C43B P2B C37B C42B -39.0(7) . . . . ? C31B P2B C37B C42B -150.9(7) . . . . ? Pd2B P2B C37B C42B 82.6(6) . . . . ? C43B P2B C37B C38B 149.2(6) . . . . ? C31B P2B C37B C38B 37.3(7) . . . . ? Pd2B P2B C37B C38B -89.2(6) . . . . ? C38B C37B C42B C41B 0 . . . . ? P2B C37B C42B C41B -171.8(8) . . . . ? C37B C42B C41B C40B 0 . . . . ? C42B C41B C40B C39B 0 . . . . ? C41B C40B C39B C38B 0 . . . . ? C40B C39B C38B C37B 0 . . . . ? C42B C37B C38B C39B 0 . . . . ? P2B C37B C38B C39B 171.8(8) . . . . ? C2A Pd1A N1A N2A 9.8(9) . . . . ? Cl1A Pd1A N1A N2A -170.6(9) . . . . ? Pd2A Pd1A N1A N2A 146.8(10) . . . . ? C2A Pd1A N1A C7A 179.1(12) . . . . ? Cl1A Pd1A N1A C7A -1.4(11) . . . . ? Pd2A Pd1A N1A C7A -43.9(10) . . . . ? C7A N1A N2A C1A -178.7(11) . . . . ? Pd1A N1A N2A C1A -7.8(15) . . . . ? N1B Pd1B C2B C3B -170.8(17) . . . . ? P1B Pd1B C2B C3B 13.5(16) . . . . ? Pd2B Pd1B C2B C3B -117.2(15) . . . . ? N1B Pd1B C2B C1B 7.1(12) . . . . ? P1B Pd1B C2B C1B -168.6(12) . . . . ? Pd2B Pd1B C2B C1B 60.7(14) . . . . ? N2A N1A C7A C12A 26.1(17) . . . . ? Pd1A N1A C7A C12A -143.2(11) . . . . ? N2A N1A C7A C8A -150.7(12) . . . . ? Pd1A N1A C7A C8A 40.0(16) . . . . ? N1A Pd1A C2A C3A 170.1(15) . . . . ? P1A Pd1A C2A C3A -13.3(14) . . . . ? Pd2A Pd1A C2A C3A 117.1(13) . . . . ? N1A Pd1A C2A C1A -8.7(9) . . . . ? P1A Pd1A C2A C1A 167.8(9) . . . . ? Pd2A Pd1A C2A C1A -61.8(11) . . . . ? C10A C9A C8A C7A -2.4(18) . . . . ? C10A C9A C8A Pd2A 174.6(9) . . . . ? C12A C7A C8A C9A 6.8(18) . . . . ? N1A C7A C8A C9A -176.4(11) . . . . ? C12A C7A C8A Pd2A -170.4(9) . . . . ? N1A C7A C8A Pd2A 6.4(15) . . . . ? P2A Pd2A C8A C9A -78.8(10) . . . . ? Cl1A Pd2A C8A C9A 106.3(10) . . . . ? Pd1A Pd2A C8A C9A 156.6(10) . . . . ? P2A Pd2A C8A C7A 98.2(9) . . . . ? Cl1A Pd2A C8A C7A -76.7(9) . . . . ? Pd1A Pd2A C8A C7A -26.3(9) . . . . ? C1A C2A C3A C4A -2(2) . . . . ? Pd1A C2A C3A C4A 179.5(11) . . . . ? C1B C2B C3B C4B 2(3) . . . . ? Pd1B C2B C3B C4B 179.4(13) . . . . ? C12A C11A C10A C9A 1(2) . . . . ? C12A C11A C10A N3A -179.4(13) . . . . ? C8A C9A C10A C11A -1(2) . . . . ? C8A C9A C10A N3A 178.9(12) . . . . ? O2A N3A C10A C11A -11(2) . . . . ? O1A N3A C10A C11A 171.5(14) . . . . ? O2A N3A C10A C9A 168.7(15) . . . . ? O1A N3A C10A C9A -9(2) . . . . ? C10A C11A C12A C7A 3(2) . . . . ? N1A C7A C12A C11A 176.0(12) . . . . ? C8A C7A C12A C11A -7.3(19) . . . . ? N1A N2A C1A C6A -176.6(13) . . . . ? N1A N2A C1A C2A -0.2(19) . . . . ? C3A C2A C1A N2A -170.8(13) . . . . ? Pd1A C2A C1A N2A 8.3(17) . . . . ? C3A C2A C1A C6A 6(2) . . . . ? Pd1A C2A C1A C6A -175.4(11) . . . . ? C3B C2B C1B N2B 171.6(16) . . . . ? Pd1B C2B C1B N2B -7(2) . . . . ? C3B C2B C1B C6B -5(3) . . . . ? Pd1B C2B C1B C6B 176.4(14) . . . . ? C49A N4A C4A C3A -6(3) . . . . ? C50A N4A C4A C3A 172.9(15) . . . . ? C49A N4A C4A C5A 174.7(17) . . . . ? C50A N4A C4A C5A -7(3) . . . . ? C2A C3A C4A N4A 177.4(15) . . . . ? C2A C3A C4A C5A -3(2) . . . . ? C49B N4B C4B C3B 8(3) . . . . ? C50B N4B C4B C3B -173.2(17) . . . . ? C49B N4B C4B C5B -172.8(19) . . . . ? C50B N4B C4B C5B 6(3) . . . . ? C2B C3B C4B N4B -177.5(17) . . . . ? C2B C3B C4B C5B 3(3) . . . . ? N4A C4A C5A C6A -176.6(16) . . . . ? C3A C4A C5A C6A 4(2) . . . . ? N4B C4B C5B C6B 176.3(18) . . . . ? C3B C4B C5B C6B -4(3) . . . . ? C4A C5A C6A C1A 0(3) . . . . ? N2A C1A C6A C5A 171.6(15) . . . . ? C2A C1A C6A C5A -5(2) . . . . ? C4B C5B C6B C1B 1(3) . . . . ? N2B C1B C6B C5B -172.7(18) . . . . ? C2B C1B C6B C5B 4(3) . . . . ? C2B Pd1B N1B N2B -8.0(11) . . . . ? Cl1B Pd1B N1B N2B 171.8(10) . . . . ? Pd2B Pd1B N1B N2B -145.2(11) . . . . ? C2B Pd1B N1B C7B 176.8(13) . . . . ? Cl1B Pd1B N1B C7B -3.5(12) . . . . ? Pd2B Pd1B N1B C7B 39.5(11) . . . . ? C7B N1B N2B C1B -177.6(14) . . . . ? Pd1B N1B N2B C1B 6.5(18) . . . . ? C6B C1B N2B N1B 177.0(15) . . . . ? C2B C1B N2B N1B 0(2) . . . . ? P2B Pd2B C8B C7B -97.0(13) . . . . ? Cl1B Pd2B C8B C7B 77.7(13) . . . . ? Pd1B Pd2B C8B C7B 27.6(13) . . . . ? P2B Pd2B C8B C9B 80.0(13) . . . . ? Cl1B Pd2B C8B C9B -105.3(14) . . . . ? Pd1B Pd2B C8B C9B -155.4(14) . . . . ? C9B C8B C7B C12B -4(2) . . . . ? Pd2B C8B C7B C12B 172.7(12) . . . . ? C9B C8B C7B N1B 172.6(14) . . . . ? Pd2B C8B C7B N1B -10(2) . . . . ? N2B N1B C7B C8B 151.0(15) . . . . ? Pd1B N1B C7B C8B -34(2) . . . . ? N2B N1B C7B C12B -32(2) . . . . ? Pd1B N1B C7B C12B 143.3(12) . . . . ? C7B C8B C9B C10B 2(2) . . . . ? Pd2B C8B C9B C10B -175.0(12) . . . . ? C8B C9B C10B C11B 1(2) . . . . ? C8B C9B C10B N3B 179.2(14) . . . . ? C12B C11B C10B C9B -2(2) . . . . ? C12B C11B C10B N3B 179.8(13) . . . . ? O1B N3B C10B C9B 10(2) . . . . ? O2B N3B C10B C9B -170.0(16) . . . . ? O1B N3B C10B C11B -172.4(15) . . . . ? O2B N3B C10B C11B 8(2) . . . . ? C10B C11B C12B C7B 0(2) . . . . ? C8B C7B C12B C11B 4(2) . . . . ? N1B C7B C12B C11B -173.5(14) . . . . ? # Attachment 'MAB_cifdoc.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2011-05-12 at 16:16:45 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\program files\wingx\files\cifdoc.dat # CIF files read : manda-mab manda-mab-teh struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_manda-mab _database_code_depnum_ccdc_archive 'CCDC 831720' #TrackingRef 'MAB_cifdoc.cif' _audit_creation_date 2011-05-12T16:16:45-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_moiety 'C49 H40 Cl2 N2 P2 Pd2' _chemical_formula_sum 'C49 H40 Cl2 N2 P2 Pd2' _chemical_formula_weight 1002.47 #------------------ UNIT CELL INFORMATION -----------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' 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 13.36700(10) _cell_length_b 18.4303(2) _cell_length_c 18.4227(2) _cell_angle_alpha 90 _cell_angle_beta 109.3200(10) _cell_angle_gamma 90 _cell_volume 4282.99(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12070 _cell_measurement_theta_min 2.5394 _cell_measurement_theta_max 75.9142 #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 8.911 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.35712 _exptl_absorpt_correction_T_max 1 #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54179 _diffrn_radiation_type CuK\a _diffrn_radiation_probe x-ray _diffrn_measurement_device_type 'Xcalibur, Ruby' _diffrn_measurement_method '\w scans' _diffrn_reflns_number 23737 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 76.1 _diffrn_reflns_theta_full 76.1 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measured_fraction_theta_full 0.989 _reflns_number_total 8856 _reflns_number_gt 7544 _reflns_threshold_expression >2sigma(I) #------------------ COMPUTER PROGRAMS USED ----------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #------------------ REFINEMENT INFORMATION ----------------------------------# _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^)+(0.0478P)^2^+14.8687P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 8856 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1369 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.001 _refine_diff_density_max 2.274 _refine_diff_density_min -2.388 #------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group _atom_site_disorder_assembly Pd2 Pd 0.68849(3) 0.72677(2) 0.48715(2) 0.04697(11) Uani 1 d . . . Pd1 Pd 0.78237(3) 0.87948(2) 0.55894(3) 0.05588(13) Uani 1 d . . . P2 P 0.79928(10) 0.63222(7) 0.49966(7) 0.0446(3) Uani 1 d . . . Cl1 Cl 0.60466(12) 0.84337(9) 0.47947(8) 0.0605(3) Uani 1 d . . . Cl2 Cl 0.61160(12) 0.67878(9) 0.57754(8) 0.0623(4) Uani 1 d . . . P1 P 0.72649(11) 0.92797(8) 0.65195(8) 0.0504(3) Uani 1 d . . . N1 N 0.8542(5) 0.8513(3) 0.4775(4) 0.0711(16) Uani 1 d . . . C37 C 0.8827(5) 0.6164(3) 0.5998(3) 0.0537(13) Uani 1 d . . . C31 C 0.7333(4) 0.5468(3) 0.4626(3) 0.0500(12) Uani 1 d . . . C13 C 0.5862(4) 0.9135(3) 0.6388(3) 0.0520(12) Uani 1 d . . . N2 N 0.9487(5) 0.8762(4) 0.4906(5) 0.091(2) Uani 1 d . . . C8 C 0.7311(6) 0.7623(4) 0.3984(3) 0.0653(18) Uani 1 d . . . C14 C 0.5557(5) 0.8431(4) 0.6481(4) 0.0637(15) Uani 1 d . . . H14 H 0.6053 0.8058 0.6595 0.076 Uiso 1 calc R . . C30 C 0.8636(5) 0.8422(4) 0.7688(4) 0.0664(16) Uani 1 d . . . H30 H 0.8861 0.8217 0.7307 0.08 Uiso 1 calc R . . C43 C 0.8986(4) 0.6432(3) 0.4517(4) 0.0553(13) Uani 1 d . . . C16 C 0.3784(5) 0.8835(5) 0.6233(5) 0.084(2) Uani 1 d . . . H16 H 0.3085 0.8732 0.6188 0.101 Uiso 1 calc R . . C9 C 0.6833(7) 0.7312(5) 0.3270(4) 0.085(2) Uani 1 d . . . H9 H 0.6339 0.6941 0.3204 0.102 Uiso 1 calc R . . C15 C 0.4524(6) 0.8287(5) 0.6404(4) 0.078(2) Uani 1 d . . . H15 H 0.432 0.7816 0.6468 0.094 Uiso 1 calc R . . C25 C 0.7868(4) 0.8949(4) 0.7504(3) 0.0577(14) Uani 1 d . . . C1 C 0.9923(6) 0.9112(4) 0.5614(6) 0.081(2) Uani 1 d . . . C6 C 1.0984(6) 0.9402(5) 0.5818(6) 0.093(3) Uani 1 d . . . H6 H 1.1355 0.938 0.5471 0.111 Uiso 1 calc R . . C2 C 0.9336(5) 0.9181(4) 0.6117(5) 0.075(2) Uani 1 d . . . C7 C 0.8071(6) 0.8181(4) 0.4073(5) 0.077(2) Uani 1 d . . . C19 C 0.7451(5) 1.0259(3) 0.6552(3) 0.0565(13) Uani 1 d . . . C18 C 0.5109(5) 0.9681(4) 0.6205(4) 0.0647(15) Uani 1 d . . . H18 H 0.5305 1.0153 0.6135 0.078 Uiso 1 calc R . . C44 C 0.8821(7) 0.6189(4) 0.3788(4) 0.080(2) Uani 1 d . . . H44 H 0.822 0.5914 0.3541 0.096 Uiso 1 calc R . . C32 C 0.6246(5) 0.5411(4) 0.4465(3) 0.0616(15) Uani 1 d . . . H32 H 0.5865 0.5808 0.4542 0.074 Uiso 1 calc R . . C36 C 0.7869(6) 0.4864(4) 0.4490(4) 0.0710(17) Uani 1 d . . . H36 H 0.8596 0.489 0.4585 0.085 Uiso 1 calc R . . C33 C 0.5727(6) 0.4772(4) 0.4192(4) 0.0746(18) Uani 1 d . . . H33 H 0.5 0.4741 0.4092 0.09 Uiso 1 calc R . . C34 C 0.6265(7) 0.4182(4) 0.4064(4) 0.079(2) Uani 1 d . . . H34 H 0.5906 0.3752 0.3877 0.095 Uiso 1 calc R . . C29 C 0.9080(6) 0.8196(4) 0.8452(4) 0.077(2) Uani 1 d . . . H29 H 0.9606 0.7843 0.858 0.093 Uiso 1 calc R . . C28 C 0.8743(6) 0.8491(5) 0.9008(4) 0.082(2) Uani 1 d . . . H28 H 0.9048 0.834 0.9516 0.098 Uiso 1 calc R . . C26 C 0.7519(6) 0.9226(4) 0.8082(4) 0.0724(18) Uani 1 d . . . H26 H 0.6975 0.9567 0.796 0.087 Uiso 1 calc R . . C12 C 0.8380(9) 0.8394(5) 0.3441(5) 0.100(3) Uani 1 d . . . H12 H 0.8917 0.8733 0.3504 0.12 Uiso 1 calc R . . C10 C 0.7132(8) 0.7586(5) 0.2612(4) 0.092(3) Uani 1 d . . . C27 C 0.7969(6) 0.9002(5) 0.8831(4) 0.082(2) Uani 1 d . . . H27 H 0.7743 0.9199 0.9215 0.098 Uiso 1 calc R . . C35 C 0.7333(7) 0.4228(4) 0.4215(5) 0.082(2) Uani 1 d . . . H35 H 0.7704 0.3828 0.4131 0.099 Uiso 1 calc R . . C11 C 0.7899(8) 0.8107(5) 0.2765(6) 0.097(3) Uani 1 d . . . H11 H 0.8097 0.8273 0.2355 0.116 Uiso 1 calc R . . C42 C 0.8772(7) 0.6608(5) 0.6570(4) 0.092(3) Uani 1 d . . . H42 H 0.8271 0.6978 0.6458 0.11 Uiso 1 calc R . . C3 C 0.9836(5) 0.9505(4) 0.6800(5) 0.080(2) Uani 1 d . . . H3 H 0.9468 0.9555 0.7147 0.096 Uiso 1 calc R . . C17 C 0.4067(5) 0.9527(5) 0.6127(4) 0.077(2) Uani 1 d . . . H17 H 0.3561 0.9894 0.6004 0.093 Uiso 1 calc R . . C20 C 0.7027(7) 1.0630(4) 0.5868(4) 0.084(2) Uani 1 d . . . H20 H 0.6667 1.0381 0.5418 0.101 Uiso 1 calc R . . C40 C 1.0200(6) 0.6011(4) 0.7491(4) 0.077(2) Uani 1 d . . . H40 H 1.0683 0.5973 0.7986 0.092 Uiso 1 calc R . . C24 C 0.7981(7) 1.0648(4) 0.7205(4) 0.081(2) Uani 1 d . . . H24 H 0.8258 1.0408 0.7673 0.097 Uiso 1 calc R . . C48 C 0.9864(6) 0.6844(5) 0.4866(5) 0.088(2) Uani 1 d . . . H48 H 0.9986 0.7016 0.5362 0.105 Uiso 1 calc R . . C23 C 0.8103(8) 1.1390(5) 0.7175(5) 0.097(3) Uani 1 d . . . H23 H 0.8473 1.1643 0.7619 0.116 Uiso 1 calc R . . C4 C 1.0919(7) 0.9780(5) 0.7026(8) 0.116(4) Uani 1 d . . . H4 H 1.1241 0.9998 0.7502 0.139 Uiso 1 calc R . . C22 C 0.7690(8) 1.1752(5) 0.6503(6) 0.094(3) Uani 1 d . . . H22 H 0.778 1.2251 0.6482 0.113 Uiso 1 calc R . . C5 C 1.1426(8) 0.9703(5) 0.6512(7) 0.107(3) Uani 1 d . . . H5 H 1.2121 0.9867 0.6645 0.129 Uiso 1 calc R . . C41 C 0.9450(7) 0.6519(6) 0.7320(5) 0.100(3) Uani 1 d . . . H41 H 0.9379 0.6817 0.7707 0.119 Uiso 1 calc R . . C38 C 0.9558(9) 0.5632(6) 0.6194(5) 0.129(5) Uani 1 d . . . H38 H 0.9602 0.5307 0.582 0.155 Uiso 1 calc R . . C46 C 1.0402(9) 0.6733(6) 0.3752(7) 0.112(4) Uani 1 d . . . H46 H 1.0889 0.682 0.35 0.135 Uiso 1 calc R . . C47 C 1.0582(7) 0.7008(6) 0.4481(7) 0.113(3) Uani 1 d . . . H47 H 1.117 0.7297 0.4713 0.136 Uiso 1 calc R . . C45 C 0.9534(9) 0.6344(6) 0.3407(6) 0.109(3) Uani 1 d . . . H45 H 0.9407 0.6175 0.2909 0.13 Uiso 1 calc R . . C49 C 0.6581(10) 0.7290(6) 0.1873(5) 0.123(4) Uani 1 d . . . H49A H 0.6083 0.6933 0.1919 0.184 Uiso 1 calc R . . H49B H 0.708 0.7067 0.1668 0.184 Uiso 1 calc R . . H49C H 0.6211 0.767 0.1534 0.184 Uiso 1 calc R . . C39 C 1.0242(10) 0.5559(6) 0.6937(5) 0.140(5) Uani 1 d . . . H39 H 1.0742 0.5188 0.7054 0.168 Uiso 1 calc R . . C21 C 0.7140(9) 1.1374(5) 0.5857(6) 0.107(3) Uani 1 d . . . H21 H 0.6835 1.1624 0.5398 0.129 Uiso 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 Pd2 0.0497(2) 0.0547(2) 0.03854(18) 0.00320(15) 0.01723(15) 0.00877(17) Pd1 0.0542(2) 0.0545(2) 0.0707(3) 0.0125(2) 0.0364(2) 0.01084(18) P2 0.0458(6) 0.0460(7) 0.0441(6) 0.0014(5) 0.0178(5) 0.0026(5) Cl1 0.0613(8) 0.0690(9) 0.0529(7) 0.0061(6) 0.0212(6) 0.0231(7) Cl2 0.0683(8) 0.0697(9) 0.0565(7) -0.0025(6) 0.0311(7) -0.0078(7) P1 0.0412(6) 0.0595(8) 0.0515(7) 0.0030(6) 0.0167(5) 0.0043(6) N1 0.099(4) 0.055(3) 0.084(4) 0.014(3) 0.064(3) 0.019(3) C37 0.055(3) 0.056(3) 0.049(3) 0.004(2) 0.017(2) -0.004(3) C31 0.055(3) 0.048(3) 0.048(3) 0.002(2) 0.018(2) 0.000(2) C13 0.045(3) 0.066(3) 0.048(3) -0.004(2) 0.019(2) 0.004(2) N2 0.089(4) 0.076(4) 0.144(6) 0.039(4) 0.089(5) 0.023(3) C8 0.083(4) 0.079(4) 0.042(3) 0.017(3) 0.031(3) 0.038(4) C14 0.055(3) 0.070(4) 0.072(4) -0.007(3) 0.028(3) 0.002(3) C30 0.062(4) 0.068(4) 0.065(4) 0.006(3) 0.016(3) -0.002(3) C43 0.048(3) 0.057(3) 0.067(3) 0.010(3) 0.027(3) 0.005(2) C16 0.048(3) 0.121(7) 0.087(5) -0.019(5) 0.026(3) -0.002(4) C9 0.096(5) 0.112(6) 0.048(3) 0.019(4) 0.028(3) 0.051(5) C15 0.063(4) 0.086(5) 0.092(5) -0.015(4) 0.033(4) -0.017(4) C25 0.041(3) 0.071(4) 0.056(3) 0.012(3) 0.010(2) -0.001(3) C1 0.083(5) 0.058(4) 0.123(7) 0.005(4) 0.064(5) 0.010(4) C6 0.068(5) 0.089(6) 0.146(8) 0.026(6) 0.070(5) 0.020(4) C2 0.055(3) 0.061(4) 0.127(6) 0.029(4) 0.055(4) 0.013(3) C7 0.096(5) 0.064(4) 0.098(5) 0.040(4) 0.070(5) 0.029(4) C19 0.051(3) 0.060(3) 0.061(3) 0.001(3) 0.021(3) 0.001(3) C18 0.056(3) 0.072(4) 0.069(4) 0.000(3) 0.024(3) 0.009(3) C44 0.092(5) 0.091(5) 0.076(4) -0.001(4) 0.051(4) -0.002(4) C32 0.058(3) 0.066(4) 0.061(3) -0.014(3) 0.020(3) -0.008(3) C36 0.065(4) 0.065(4) 0.083(4) -0.008(3) 0.024(3) 0.005(3) C33 0.068(4) 0.082(5) 0.075(4) -0.013(4) 0.025(3) -0.017(4) C34 0.097(6) 0.065(4) 0.072(4) -0.013(3) 0.023(4) -0.023(4) C29 0.059(4) 0.079(5) 0.078(5) 0.016(4) 0.001(3) 0.004(3) C28 0.076(5) 0.104(6) 0.055(4) 0.007(4) 0.007(3) -0.023(4) C26 0.064(4) 0.092(5) 0.063(4) 0.003(4) 0.024(3) 0.003(4) C12 0.162(9) 0.078(5) 0.092(6) 0.021(4) 0.087(6) 0.029(6) C10 0.112(6) 0.113(7) 0.045(3) -0.006(4) 0.016(4) 0.058(6) C27 0.074(5) 0.109(6) 0.059(4) 0.003(4) 0.018(3) -0.006(4) C35 0.093(6) 0.054(4) 0.101(6) -0.014(4) 0.033(5) 0.002(4) C11 0.113(7) 0.089(6) 0.093(6) 0.024(5) 0.040(5) 0.008(5) C42 0.081(5) 0.115(7) 0.065(4) -0.021(4) 0.005(4) 0.029(5) C3 0.050(3) 0.071(4) 0.116(6) 0.002(4) 0.026(4) -0.004(3) C17 0.049(3) 0.101(6) 0.080(4) -0.007(4) 0.020(3) 0.015(4) C20 0.108(6) 0.074(5) 0.062(4) 0.006(3) 0.018(4) -0.002(4) C40 0.083(5) 0.074(4) 0.056(4) 0.008(3) 0.000(3) -0.007(4) C24 0.096(6) 0.077(5) 0.064(4) -0.002(4) 0.018(4) -0.006(4) C48 0.068(4) 0.099(6) 0.104(6) 0.000(5) 0.038(4) -0.012(4) C23 0.129(8) 0.076(5) 0.078(5) -0.016(4) 0.025(5) -0.019(5) C4 0.085(5) 0.073(5) 0.223(12) 0.051(6) 0.097(7) 0.028(4) C22 0.117(7) 0.065(5) 0.111(7) 0.001(5) 0.052(6) -0.006(5) C5 0.077(5) 0.075(5) 0.178(11) -0.015(6) 0.052(6) -0.007(4) C41 0.084(5) 0.129(8) 0.067(4) -0.027(5) 0.001(4) 0.024(5) C38 0.164(10) 0.124(8) 0.065(5) -0.016(5) -0.008(5) 0.092(8) C46 0.108(7) 0.116(8) 0.149(10) 0.031(7) 0.091(7) 0.020(6) C47 0.070(5) 0.110(7) 0.169(11) 0.019(7) 0.052(6) -0.015(5) C45 0.129(8) 0.124(8) 0.107(7) 0.001(6) 0.086(7) -0.002(7) C49 0.146(10) 0.130(9) 0.083(6) -0.016(6) 0.027(6) 0.000(8) C39 0.175(11) 0.122(8) 0.078(6) -0.001(5) -0.019(6) 0.090(8) C21 0.151(9) 0.077(5) 0.090(6) 0.018(5) 0.034(6) -0.003(6) #------------------ MOLECULAR GEOMETRY --------------------------------------# _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 Pd2 C8 2.011(6) . ? Pd2 P2 2.2488(14) . ? Pd2 Cl2 2.3967(14) . ? Pd2 Cl1 2.4059(15) . ? Pd2 Pd1 3.1855(6) . ? Pd1 C2 2.058(8) . ? Pd1 N1 2.097(5) . ? Pd1 P1 2.2670(15) . ? Pd1 Cl1 2.4348(17) . ? P2 C31 1.823(6) . ? P2 C43 1.833(6) . ? P2 C37 1.836(6) . ? P1 C19 1.821(6) . ? P1 C25 1.829(6) . ? P1 C13 1.829(6) . ? N1 N2 1.289(9) . ? N1 C7 1.380(10) . ? C37 C38 1.347(10) . ? C37 C42 1.354(9) . ? C31 C32 1.387(8) . ? C31 C36 1.390(8) . ? C13 C18 1.384(8) . ? C13 C14 1.388(9) . ? N2 C1 1.397(11) . ? C8 C9 1.382(10) . ? C8 C7 1.417(11) . ? C14 C15 1.366(9) . ? C14 H14 0.93 . ? C30 C25 1.372(9) . ? C30 C29 1.397(9) . ? C30 H30 0.93 . ? C43 C44 1.363(9) . ? C43 C48 1.366(10) . ? C16 C17 1.363(11) . ? C16 C15 1.374(11) . ? C16 H16 0.93 . ? C9 C10 1.486(11) . ? C9 H9 0.93 . ? C15 H15 0.93 . ? C25 C26 1.393(9) . ? C1 C2 1.405(10) . ? C1 C6 1.444(11) . ? C6 C5 1.339(13) . ? C6 H6 0.93 . ? C2 C3 1.354(11) . ? C7 C12 1.413(9) . ? C19 C20 1.379(9) . ? C19 C24 1.379(9) . ? C18 C17 1.381(9) . ? C18 H18 0.93 . ? C44 C45 1.388(10) . ? C44 H44 0.93 . ? C32 C33 1.375(9) . ? C32 H32 0.93 . ? C36 C35 1.379(10) . ? C36 H36 0.93 . ? C33 C34 1.366(11) . ? C33 H33 0.93 . ? C34 C35 1.365(11) . ? C34 H34 0.93 . ? C29 C28 1.361(11) . ? C29 H29 0.93 . ? C28 C27 1.357(12) . ? C28 H28 0.93 . ? C26 C27 1.374(10) . ? C26 H26 0.93 . ? C12 C11 1.308(13) . ? C12 H12 0.93 . ? C10 C11 1.365(13) . ? C10 C49 1.424(11) . ? C27 H27 0.93 . ? C35 H35 0.93 . ? C11 H11 0.93 . ? C42 C41 1.390(10) . ? C42 H42 0.93 . ? C3 C4 1.458(11) . ? C3 H3 0.93 . ? C17 H17 0.93 . ? C20 C21 1.381(11) . ? C20 H20 0.93 . ? C40 C41 1.330(11) . ? C40 C39 1.333(12) . ? C40 H40 0.93 . ? C24 C23 1.380(11) . ? C24 H24 0.93 . ? C48 C47 1.402(12) . ? C48 H48 0.93 . ? C23 C22 1.351(12) . ? C23 H23 0.93 . ? C4 C5 1.342(14) . ? C4 H4 0.93 . ? C22 C21 1.365(13) . ? C22 H22 0.93 . ? C5 H5 0.93 . ? C41 H41 0.93 . ? C38 C39 1.378(11) . ? C38 H38 0.93 . ? C46 C45 1.332(15) . ? C46 C47 1.379(15) . ? C46 H46 0.93 . ? C47 H47 0.93 . ? C45 H45 0.93 . ? C49 H49A 0.96 . ? C49 H49B 0.96 . ? C49 H49C 0.96 . ? C39 H39 0.93 . ? C21 H21 0.93 . ? 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 C8 Pd2 P2 88.96(17) . . ? C8 Pd2 Cl2 170.8(2) . . ? P2 Pd2 Cl2 93.56(5) . . ? C8 Pd2 Cl1 84.99(17) . . ? P2 Pd2 Cl1 167.49(6) . . ? Cl2 Pd2 Cl1 94.13(5) . . ? C8 Pd2 Pd1 82.6(2) . . ? P2 Pd2 Pd1 119.11(4) . . ? Cl2 Pd2 Pd1 103.78(4) . . ? Cl1 Pd2 Pd1 49.24(4) . . ? C2 Pd1 N1 79.2(3) . . ? C2 Pd1 P1 91.4(2) . . ? N1 Pd1 P1 169.11(18) . . ? C2 Pd1 Cl1 171.4(2) . . ? N1 Pd1 Cl1 95.1(2) . . ? P1 Pd1 Cl1 93.58(5) . . ? C2 Pd1 Pd2 133.79(19) . . ? N1 Pd1 Pd2 72.21(17) . . ? P1 Pd1 Pd2 118.62(4) . . ? Cl1 Pd1 Pd2 48.46(4) . . ? C31 P2 C43 104.6(3) . . ? C31 P2 C37 107.3(3) . . ? C43 P2 C37 101.9(3) . . ? C31 P2 Pd2 114.21(19) . . ? C43 P2 Pd2 115.00(19) . . ? C37 P2 Pd2 112.7(2) . . ? Pd2 Cl1 Pd1 82.30(4) . . ? C19 P1 C25 106.7(3) . . ? C19 P1 C13 105.8(3) . . ? C25 P1 C13 100.3(3) . . ? C19 P1 Pd1 109.8(2) . . ? C25 P1 Pd1 118.1(2) . . ? C13 P1 Pd1 114.97(18) . . ? N2 N1 C7 116.6(6) . . ? N2 N1 Pd1 115.5(5) . . ? C7 N1 Pd1 127.3(5) . . ? C38 C37 C42 116.9(6) . . ? C38 C37 P2 122.0(5) . . ? C42 C37 P2 121.0(5) . . ? C32 C31 C36 117.8(6) . . ? C32 C31 P2 119.3(5) . . ? C36 C31 P2 123.0(5) . . ? C18 C13 C14 119.3(6) . . ? C18 C13 P1 123.9(5) . . ? C14 C13 P1 116.8(4) . . ? N1 N2 C1 114.8(6) . . ? C9 C8 C7 119.9(6) . . ? C9 C8 Pd2 118.2(6) . . ? C7 C8 Pd2 121.9(5) . . ? C15 C14 C13 119.8(7) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C25 C30 C29 119.6(7) . . ? C25 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C44 C43 C48 118.7(7) . . ? C44 C43 P2 122.1(5) . . ? C48 C43 P2 118.7(5) . . ? C17 C16 C15 120.5(7) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C8 C9 C10 118.1(9) . . ? C8 C9 H9 121 . . ? C10 C9 H9 121 . . ? C14 C15 C16 120.4(8) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C30 C25 C26 118.9(6) . . ? C30 C25 P1 121.9(5) . . ? C26 C25 P1 119.2(5) . . ? N2 C1 C2 120.4(7) . . ? N2 C1 C6 119.0(7) . . ? C2 C1 C6 120.6(9) . . ? C5 C6 C1 119.2(8) . . ? C5 C6 H6 120.4 . . ? C1 C6 H6 120.4 . . ? C3 C2 C1 116.2(7) . . ? C3 C2 Pd1 134.3(5) . . ? C1 C2 Pd1 109.4(7) . . ? N1 C7 C12 118.9(8) . . ? N1 C7 C8 121.1(5) . . ? C12 C7 C8 120.0(8) . . ? C20 C19 C24 118.5(7) . . ? C20 C19 P1 116.8(5) . . ? C24 C19 P1 124.7(5) . . ? C17 C18 C13 120.2(7) . . ? C17 C18 H18 119.9 . . ? C13 C18 H18 119.9 . . ? C43 C44 C45 121.1(9) . . ? C43 C44 H44 119.5 . . ? C45 C44 H44 119.5 . . ? C33 C32 C31 120.6(6) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C35 C36 C31 120.7(7) . . ? C35 C36 H36 119.6 . . ? C31 C36 H36 119.6 . . ? C34 C33 C32 121.0(7) . . ? C34 C33 H33 119.5 . . ? C32 C33 H33 119.5 . . ? C35 C34 C33 119.3(7) . . ? C35 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? C28 C29 C30 120.2(7) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C27 C28 C29 120.8(7) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? C27 C26 C25 120.7(7) . . ? C27 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C11 C12 C7 119.1(10) . . ? C11 C12 H12 120.4 . . ? C7 C12 H12 120.4 . . ? C11 C10 C49 125.7(10) . . ? C11 C10 C9 117.2(7) . . ? C49 C10 C9 117.1(10) . . ? C28 C27 C26 119.7(8) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C34 C35 C36 120.6(7) . . ? C34 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? C12 C11 C10 125.4(9) . . ? C12 C11 H11 117.3 . . ? C10 C11 H11 117.3 . . ? C37 C42 C41 121.1(8) . . ? C37 C42 H42 119.4 . . ? C41 C42 H42 119.4 . . ? C2 C3 C4 123.9(9) . . ? C2 C3 H3 118.1 . . ? C4 C3 H3 118.1 . . ? C16 C17 C18 119.6(7) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C19 C20 C21 119.4(8) . . ? C19 C20 H20 120.3 . . ? C21 C20 H20 120.3 . . ? C41 C40 C39 118.5(7) . . ? C41 C40 H40 120.7 . . ? C39 C40 H40 120.7 . . ? C19 C24 C23 120.8(7) . . ? C19 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C43 C48 C47 120.4(9) . . ? C43 C48 H48 119.8 . . ? C47 C48 H48 119.8 . . ? C22 C23 C24 120.5(8) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C5 C4 C3 116.5(11) . . ? C5 C4 H4 121.7 . . ? C3 C4 H4 121.7 . . ? C23 C22 C21 119.0(8) . . ? C23 C22 H22 120.5 . . ? C21 C22 H22 120.5 . . ? C6 C5 C4 123.5(10) . . ? C6 C5 H5 118.3 . . ? C4 C5 H5 118.3 . . ? C40 C41 C42 120.7(8) . . ? C40 C41 H41 119.6 . . ? C42 C41 H41 119.6 . . ? C37 C38 C39 121.4(8) . . ? C37 C38 H38 119.3 . . ? C39 C38 H38 119.3 . . ? C45 C46 C47 120.4(8) . . ? C45 C46 H46 119.8 . . ? C47 C46 H46 119.8 . . ? C46 C47 C48 119.0(9) . . ? C46 C47 H47 120.5 . . ? C48 C47 H47 120.5 . . ? C46 C45 C44 120.3(9) . . ? C46 C45 H45 119.8 . . ? C44 C45 H45 119.8 . . ? C10 C49 H49A 109.5 . . ? C10 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C10 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C40 C39 C38 121.1(8) . . ? C40 C39 H39 119.4 . . ? C38 C39 H39 119.4 . . ? C22 C21 C20 121.6(8) . . ? C22 C21 H21 119.2 . . ? C20 C21 H21 119.2 . . ? 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 C8 Pd2 Pd1 C2 -78.9(3) . . . . ? P2 Pd2 Pd1 C2 5.7(3) . . . . ? Cl2 Pd2 Pd1 C2 107.8(3) . . . . ? Cl1 Pd2 Pd1 C2 -168.7(3) . . . . ? C8 Pd2 Pd1 N1 -24.3(2) . . . . ? P2 Pd2 Pd1 N1 60.30(18) . . . . ? Cl2 Pd2 Pd1 N1 162.41(18) . . . . ? Cl1 Pd2 Pd1 N1 -114.10(18) . . . . ? C8 Pd2 Pd1 P1 156.89(18) . . . . ? P2 Pd2 Pd1 P1 -118.46(6) . . . . ? Cl2 Pd2 Pd1 P1 -16.35(6) . . . . ? Cl1 Pd2 Pd1 P1 67.14(6) . . . . ? C8 Pd2 Pd1 Cl1 89.76(18) . . . . ? P2 Pd2 Pd1 Cl1 174.40(6) . . . . ? Cl2 Pd2 Pd1 Cl1 -83.49(6) . . . . ? C8 Pd2 P2 C31 -103.8(3) . . . . ? Cl2 Pd2 P2 C31 67.39(19) . . . . ? Cl1 Pd2 P2 C31 -164.7(3) . . . . ? Pd1 Pd2 P2 C31 175.32(19) . . . . ? C8 Pd2 P2 C43 17.3(3) . . . . ? Cl2 Pd2 P2 C43 -171.6(2) . . . . ? Cl1 Pd2 P2 C43 -43.7(3) . . . . ? Pd1 Pd2 P2 C43 -63.6(2) . . . . ? C8 Pd2 P2 C37 133.5(3) . . . . ? Cl2 Pd2 P2 C37 -55.4(2) . . . . ? Cl1 Pd2 P2 C37 72.5(3) . . . . ? Pd1 Pd2 P2 C37 52.5(2) . . . . ? C8 Pd2 Cl1 Pd1 -84.5(2) . . . . ? P2 Pd2 Cl1 Pd1 -23.2(2) . . . . ? Cl2 Pd2 Cl1 Pd1 104.66(5) . . . . ? N1 Pd1 Cl1 Pd2 60.76(15) . . . . ? P1 Pd1 Cl1 Pd2 -125.86(5) . . . . ? C2 Pd1 P1 C19 60.1(3) . . . . ? N1 Pd1 P1 C19 29.7(9) . . . . ? Cl1 Pd1 P1 C19 -112.9(2) . . . . ? Pd2 Pd1 P1 C19 -156.6(2) . . . . ? C2 Pd1 P1 C25 -62.6(3) . . . . ? N1 Pd1 P1 C25 -93.0(9) . . . . ? Cl1 Pd1 P1 C25 124.5(2) . . . . ? Pd2 Pd1 P1 C25 80.8(2) . . . . ? C2 Pd1 P1 C13 179.2(3) . . . . ? N1 Pd1 P1 C13 148.8(9) . . . . ? Cl1 Pd1 P1 C13 6.3(2) . . . . ? Pd2 Pd1 P1 C13 -37.5(2) . . . . ? C2 Pd1 N1 N2 -7.6(5) . . . . ? P1 Pd1 N1 N2 23.4(12) . . . . ? Cl1 Pd1 N1 N2 165.9(4) . . . . ? Pd2 Pd1 N1 N2 -150.8(5) . . . . ? C2 Pd1 N1 C7 -178.0(5) . . . . ? P1 Pd1 N1 C7 -146.9(7) . . . . ? Cl1 Pd1 N1 C7 -4.5(5) . . . . ? Pd2 Pd1 N1 C7 38.8(5) . . . . ? C31 P2 C37 C38 54.7(9) . . . . ? C43 P2 C37 C38 -55.0(9) . . . . ? Pd2 P2 C37 C38 -178.8(8) . . . . ? C31 P2 C37 C42 -129.0(6) . . . . ? C43 P2 C37 C42 121.4(7) . . . . ? Pd2 P2 C37 C42 -2.4(7) . . . . ? C43 P2 C31 C32 -140.9(5) . . . . ? C37 P2 C31 C32 111.4(5) . . . . ? Pd2 P2 C31 C32 -14.3(5) . . . . ? C43 P2 C31 C36 38.5(6) . . . . ? C37 P2 C31 C36 -69.2(6) . . . . ? Pd2 P2 C31 C36 165.1(5) . . . . ? C19 P1 C13 C18 10.9(6) . . . . ? C25 P1 C13 C18 121.7(5) . . . . ? Pd1 P1 C13 C18 -110.4(5) . . . . ? C19 P1 C13 C14 -169.0(5) . . . . ? C25 P1 C13 C14 -58.2(5) . . . . ? Pd1 P1 C13 C14 69.6(5) . . . . ? C7 N1 N2 C1 178.2(6) . . . . ? Pd1 N1 N2 C1 6.8(8) . . . . ? P2 Pd2 C8 C9 81.2(5) . . . . ? Cl1 Pd2 C8 C9 -109.8(5) . . . . ? Pd1 Pd2 C8 C9 -159.3(5) . . . . ? P2 Pd2 C8 C7 -99.3(5) . . . . ? Cl1 Pd2 C8 C7 69.8(5) . . . . ? Pd1 Pd2 C8 C7 20.3(5) . . . . ? C18 C13 C14 C15 -1.1(9) . . . . ? P1 C13 C14 C15 178.9(5) . . . . ? C31 P2 C43 C44 33.0(6) . . . . ? C37 P2 C43 C44 144.6(6) . . . . ? Pd2 P2 C43 C44 -93.2(6) . . . . ? C31 P2 C43 C48 -154.9(6) . . . . ? C37 P2 C43 C48 -43.2(6) . . . . ? Pd2 P2 C43 C48 79.0(6) . . . . ? C7 C8 C9 C10 -0.8(9) . . . . ? Pd2 C8 C9 C10 178.7(5) . . . . ? C13 C14 C15 C16 0.2(11) . . . . ? C17 C16 C15 C14 0.8(12) . . . . ? C29 C30 C25 C26 -2.4(10) . . . . ? C29 C30 C25 P1 179.2(5) . . . . ? C19 P1 C25 C30 -124.3(6) . . . . ? C13 P1 C25 C30 125.6(6) . . . . ? Pd1 P1 C25 C30 -0.1(6) . . . . ? C19 P1 C25 C26 57.4(6) . . . . ? C13 P1 C25 C26 -52.7(6) . . . . ? Pd1 P1 C25 C26 -178.4(5) . . . . ? N1 N2 C1 C2 -1.0(10) . . . . ? N1 N2 C1 C6 179.3(6) . . . . ? N2 C1 C6 C5 -176.5(8) . . . . ? C2 C1 C6 C5 3.8(12) . . . . ? N2 C1 C2 C3 177.7(7) . . . . ? C6 C1 C2 C3 -2.5(11) . . . . ? N2 C1 C2 Pd1 -5.3(9) . . . . ? C6 C1 C2 Pd1 174.5(6) . . . . ? N1 Pd1 C2 C3 -177.4(8) . . . . ? P1 Pd1 C2 C3 8.1(7) . . . . ? Pd2 Pd1 C2 C3 -125.3(7) . . . . ? N1 Pd1 C2 C1 6.3(5) . . . . ? P1 Pd1 C2 C1 -168.1(5) . . . . ? Pd2 Pd1 C2 C1 58.5(6) . . . . ? N2 N1 C7 C12 -27.4(9) . . . . ? Pd1 N1 C7 C12 142.9(6) . . . . ? N2 N1 C7 C8 151.0(6) . . . . ? Pd1 N1 C7 C8 -38.7(8) . . . . ? C9 C8 C7 N1 178.5(6) . . . . ? Pd2 C8 C7 N1 -1.0(8) . . . . ? C9 C8 C7 C12 -3.1(10) . . . . ? Pd2 C8 C7 C12 177.4(6) . . . . ? C25 P1 C19 C20 -178.2(6) . . . . ? C13 P1 C19 C20 -72.0(6) . . . . ? Pd1 P1 C19 C20 52.7(6) . . . . ? C25 P1 C19 C24 1.7(7) . . . . ? C13 P1 C19 C24 107.9(6) . . . . ? Pd1 P1 C19 C24 -127.4(6) . . . . ? C14 C13 C18 C17 0.9(9) . . . . ? P1 C13 C18 C17 -179.0(5) . . . . ? C48 C43 C44 C45 1.0(12) . . . . ? P2 C43 C44 C45 173.2(7) . . . . ? C36 C31 C32 C33 1.1(9) . . . . ? P2 C31 C32 C33 -179.4(5) . . . . ? C32 C31 C36 C35 -1.0(10) . . . . ? P2 C31 C36 C35 179.5(6) . . . . ? C31 C32 C33 C34 -0.8(11) . . . . ? C32 C33 C34 C35 0.3(12) . . . . ? C25 C30 C29 C28 0.7(11) . . . . ? C30 C29 C28 C27 0.7(12) . . . . ? C30 C25 C26 C27 3.0(11) . . . . ? P1 C25 C26 C27 -178.7(6) . . . . ? N1 C7 C12 C11 -176.7(8) . . . . ? C8 C7 C12 C11 4.9(12) . . . . ? C8 C9 C10 C11 3.0(10) . . . . ? C8 C9 C10 C49 -176.1(8) . . . . ? C29 C28 C27 C26 -0.2(12) . . . . ? C25 C26 C27 C28 -1.7(12) . . . . ? C33 C34 C35 C36 -0.2(13) . . . . ? C31 C36 C35 C34 0.6(12) . . . . ? C7 C12 C11 C10 -2.7(15) . . . . ? C49 C10 C11 C12 177.8(10) . . . . ? C9 C10 C11 C12 -1.3(14) . . . . ? C38 C37 C42 C41 0.8(14) . . . . ? P2 C37 C42 C41 -175.8(8) . . . . ? C1 C2 C3 C4 0.5(11) . . . . ? Pd1 C2 C3 C4 -175.5(6) . . . . ? C15 C16 C17 C18 -1.0(12) . . . . ? C13 C18 C17 C16 0.1(11) . . . . ? C24 C19 C20 C21 -0.1(13) . . . . ? P1 C19 C20 C21 179.8(8) . . . . ? C20 C19 C24 C23 -1.4(13) . . . . ? P1 C19 C24 C23 178.7(7) . . . . ? C44 C43 C48 C47 -0.4(12) . . . . ? P2 C43 C48 C47 -172.9(7) . . . . ? C19 C24 C23 C22 1.2(15) . . . . ? C2 C3 C4 C5 0.3(12) . . . . ? C24 C23 C22 C21 0.6(16) . . . . ? C1 C6 C5 C4 -3.0(15) . . . . ? C3 C4 C5 C6 1.0(14) . . . . ? C39 C40 C41 C42 -4.3(16) . . . . ? C37 C42 C41 C40 2.5(16) . . . . ? C42 C37 C38 C39 -2.2(18) . . . . ? P2 C37 C38 C39 174.3(11) . . . . ? C45 C46 C47 C48 2.9(17) . . . . ? C43 C48 C47 C46 -1.5(15) . . . . ? C47 C46 C45 C44 -2.3(17) . . . . ? C43 C44 C45 C46 0.3(15) . . . . ? C41 C40 C39 C38 3(2) . . . . ? C37 C38 C39 C40 0(2) . . . . ? C23 C22 C21 C20 -2.2(17) . . . . ? C19 C20 C21 C22 1.9(16) . . . . ?