# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Chemical Science' _journal_coden_cambridge 1475 #TrackingRef '- 8_photoexps.cif' # Name and address of author for correspondence _publ_contact_author_name 'Hatcher, L.E.' _publ_contact_author_address ; Department of Chemistry University of Bath Bath UK ; _publ_contact_author_email p.r.raithby@bath.ac.uk _publ_contact_author_fax '+44 (0) 1225 383183' _publ_contact_author_phone '+44 (0) 1225 386231' #TrackingRef '- 8_photoexps.cif' _publ_requested_category FM loop_ _publ_author_name 'Somia Bajwa' 'Thomas Storr' 'Lauren Hatcher' 'Thomas Williams' 'Christoph Baumann' 'Adrian Whitwood' 'David Allan' 'Simon Teat' 'Paul Raithby' 'Ian Fairlamb' data_8_GS150K _database_code_depnum_ccdc_archive 'CCDC 858649' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Nitro-(1-(3,4-dimethoxybenzyl)-6,7-dimethoxyisoquinoline)(triphenylphosphine) palladium(II) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H37 Cl2 N2 O6 P Pd' _chemical_formula_sum 'C39 H37 Cl2 N2 O6 P Pd' _chemical_formula_weight 837.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.7223(5) _cell_length_b 21.7779(13) _cell_length_c 16.3387(7) _cell_angle_alpha 90.00 _cell_angle_beta 105.321(4) _cell_angle_gamma 90.00 _cell_volume 3679.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 14061 _cell_measurement_theta_min 1.5461 _cell_measurement_theta_max 29.4767 _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 0.743 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.90004 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.68890 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator synchrotron _diffrn_measurement_device ; CrystalLogic Kappa (3 circle) ; _diffrn_measurement_device_type ; Rigaku Saturn724+ (2x2 bin mode) ; _diffrn_measurement_method '1.0 degree images with \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41375 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_sigmaI/netI 0.1001 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.5461 _diffrn_reflns_theta_max 29.4767 _diffrn_orient_matrix_UB_11 0.0021560000 _diffrn_orient_matrix_UB_12 -0.0108184000 _diffrn_orient_matrix_UB_13 0.0399065000 _diffrn_orient_matrix_UB_21 0.0523788000 _diffrn_orient_matrix_UB_22 -0.0180920000 _diffrn_orient_matrix_UB_23 -0.0008386000 _diffrn_orient_matrix_UB_31 0.0412183000 _diffrn_orient_matrix_UB_32 0.0236126000 _diffrn_orient_matrix_UB_33 0.0176601000 _reflns_number_total 11231 _reflns_number_gt 9607 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009) ; _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-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics WINGX _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+1.8249P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11231 _refine_ls_number_parameters 477 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0429 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0836 _refine_ls_wR_factor_gt 0.0789 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.16270(18) 0.18788(9) 0.78989(11) 0.0252(4) Uani 1 1 d . . . H1 H 1.1579 0.1557 0.8282 0.030 Uiso 1 1 calc R . . C2 C 1.27839(17) 0.21625(9) 0.79770(11) 0.0257(4) Uani 1 1 d . . . H2 H 1.3531 0.2031 0.8396 0.031 Uiso 1 1 calc R . . C3 C 1.28640(16) 0.26543(9) 0.74287(11) 0.0231(3) Uani 1 1 d . . . C4 C 1.40603(17) 0.29554(9) 0.74730(12) 0.0275(4) Uani 1 1 d . . . H4 H 1.4827 0.2824 0.7874 0.033 Uiso 1 1 calc R . . C5 C 1.41049(18) 0.34319(10) 0.69389(14) 0.0313(4) Uani 1 1 d . . . C6 C 1.29498(18) 0.36413(10) 0.63387(13) 0.0294(4) Uani 1 1 d . . . C7 C 1.17944(17) 0.33431(8) 0.62643(12) 0.0244(3) Uani 1 1 d . . . H7 H 1.1041 0.3473 0.5850 0.029 Uiso 1 1 calc R . . C8 C 1.17243(16) 0.28379(8) 0.68095(11) 0.0210(3) Uani 1 1 d . . . C9 C 1.05694(16) 0.24973(8) 0.67513(11) 0.0202(3) Uani 1 1 d . . . C10 C 0.93193(16) 0.25981(8) 0.60636(11) 0.0207(3) Uani 1 1 d . . . H10A H 0.9439 0.2924 0.5669 0.025 Uiso 1 1 calc R . . H10B H 0.8622 0.2726 0.6321 0.025 Uiso 1 1 calc R . . C11 C 0.89616(15) 0.19950(8) 0.55868(10) 0.0194(3) Uani 1 1 d . . . C12 C 0.91522(16) 0.19381(8) 0.47731(10) 0.0206(3) Uani 1 1 d . . . H12 H 0.9381 0.2288 0.4497 0.025 Uiso 1 1 calc R . . C13 C 0.90071(16) 0.13724(8) 0.43716(10) 0.0209(3) Uani 1 1 d . . . C14 C 0.86294(16) 0.08591(8) 0.47711(11) 0.0214(3) Uani 1 1 d . . . C15 C 0.84239(16) 0.09207(8) 0.55721(11) 0.0213(3) Uani 1 1 d . . . H15 H 0.8156 0.0575 0.5836 0.026 Uiso 1 1 calc R . . C16 C 0.86086(16) 0.14889(8) 0.59959(11) 0.0206(3) Uani 1 1 d . A . C17 C 1.6366(2) 0.35751(16) 0.7511(2) 0.0669(9) Uani 1 1 d . . . H17A H 1.6291 0.3627 0.8092 0.100 Uiso 1 1 calc R . . H17B H 1.7074 0.3831 0.7428 0.100 Uiso 1 1 calc R . . H17C H 1.6545 0.3143 0.7417 0.100 Uiso 1 1 calc R . . C18 C 1.2018(3) 0.43923(15) 0.5301(2) 0.0671(10) Uani 1 1 d . . . H18A H 1.1623 0.4082 0.4877 0.101 Uiso 1 1 calc R . . H18B H 1.2275 0.4748 0.5016 0.101 Uiso 1 1 calc R . . H18C H 1.1392 0.4521 0.5608 0.101 Uiso 1 1 calc R . . C19 C 0.9676(2) 0.17634(9) 0.31987(12) 0.0281(4) Uani 1 1 d . . . H19A H 0.9035 0.2095 0.3101 0.042 Uiso 1 1 calc R . . H19B H 0.9811 0.1632 0.2655 0.042 Uiso 1 1 calc R . . H19C H 1.0495 0.1912 0.3569 0.042 Uiso 1 1 calc R . . C20 C 0.8233(2) -0.02202(9) 0.47315(14) 0.0324(4) Uani 1 1 d . . . H20A H 0.8900 -0.0279 0.5266 0.049 Uiso 1 1 calc R . . H20B H 0.8222 -0.0576 0.4363 0.049 Uiso 1 1 calc R . . H20C H 0.7387 -0.0178 0.4848 0.049 Uiso 1 1 calc R . . C21 C 0.53843(16) 0.15443(8) 0.64398(11) 0.0215(3) Uani 1 1 d . . . C22 C 0.55166(19) 0.19439(10) 0.58040(13) 0.0314(4) Uani 1 1 d . . . H22 H 0.6350 0.2030 0.5733 0.038 Uiso 1 1 calc R . . C23 C 0.4424(2) 0.22187(11) 0.52690(14) 0.0386(5) Uani 1 1 d . . . H23 H 0.4524 0.2496 0.4841 0.046 Uiso 1 1 calc R . . C24 C 0.31979(19) 0.20929(10) 0.53536(13) 0.0311(4) Uani 1 1 d . . . H24 H 0.2460 0.2278 0.4982 0.037 Uiso 1 1 calc R . . C25 C 0.30579(18) 0.16963(9) 0.59824(13) 0.0271(4) Uani 1 1 d . . . H25 H 0.2220 0.1608 0.6045 0.033 Uiso 1 1 calc R . . C26 C 0.41394(17) 0.14254(9) 0.65250(12) 0.0255(4) Uani 1 1 d . . . H26 H 0.4033 0.1156 0.6959 0.031 Uiso 1 1 calc R . . C27 C 0.63936(16) 0.11724(9) 0.81633(11) 0.0238(3) Uani 1 1 d . . . C28 C 0.65799(19) 0.17214(10) 0.86229(13) 0.0307(4) Uani 1 1 d . . . H28 H 0.6869 0.2077 0.8391 0.037 Uiso 1 1 calc R . . C29 C 0.6343(2) 0.17483(13) 0.94195(14) 0.0411(5) Uani 1 1 d . . . H29 H 0.6488 0.2120 0.9736 0.049 Uiso 1 1 calc R . . C30 C 0.5894(2) 0.12306(14) 0.97527(14) 0.0487(6) Uani 1 1 d . . . H30 H 0.5730 0.1248 1.0296 0.058 Uiso 1 1 calc R . . C31 C 0.5689(2) 0.06911(13) 0.92919(15) 0.0442(6) Uani 1 1 d . . . H31 H 0.5364 0.0341 0.9516 0.053 Uiso 1 1 calc R . . C32 C 0.5952(2) 0.06539(10) 0.84996(13) 0.0322(4) Uani 1 1 d . . . H32 H 0.5831 0.0278 0.8194 0.039 Uiso 1 1 calc R . . C33 C 0.66266(17) 0.03588(8) 0.68176(11) 0.0225(3) Uani 1 1 d . . . C34 C 0.55606(19) 0.01256(9) 0.62130(13) 0.0311(4) Uani 1 1 d . . . H34 H 0.4853 0.0387 0.5964 0.037 Uiso 1 1 calc R . . C35 C 0.5530(2) -0.04883(10) 0.59730(14) 0.0379(5) Uani 1 1 d . . . H35 H 0.4794 -0.0645 0.5568 0.046 Uiso 1 1 calc R . . C36 C 0.6559(2) -0.08703(10) 0.63177(14) 0.0376(5) Uani 1 1 d . . . H36 H 0.6545 -0.1286 0.6138 0.045 Uiso 1 1 calc R . . C37 C 0.7617(2) -0.06435(10) 0.69298(15) 0.0366(5) Uani 1 1 d . . . H37 H 0.8323 -0.0907 0.7175 0.044 Uiso 1 1 calc R . . C38 C 0.76522(19) -0.00366(9) 0.71856(13) 0.0294(4) Uani 1 1 d . . . H38 H 0.8373 0.0112 0.7611 0.035 Uiso 1 1 calc R . . C40 C 1.1172(2) -0.00285(12) 0.76687(16) 0.0420(5) Uani 1 1 d . . . H40A H 1.0954 -0.0239 0.7112 0.050 Uiso 1 1 calc R . . H40B H 1.0552 0.0313 0.7639 0.050 Uiso 1 1 calc R . . N2 N 1.05319(14) 0.20382(7) 0.72911(9) 0.0218(3) Uani 1 1 d . A . O3 O 1.51779(14) 0.37561(8) 0.69210(11) 0.0470(4) Uani 1 1 d . . . O4 O 1.31328(15) 0.41380(8) 0.58859(11) 0.0429(4) Uani 1 1 d . . . O5 O 0.92238(13) 0.12591(6) 0.35922(8) 0.0258(3) Uani 1 1 d . . . O6 O 0.85115(14) 0.03207(6) 0.43201(8) 0.0287(3) Uani 1 1 d . . . P1 P 0.67880(4) 0.11637(2) 0.71409(3) 0.01976(9) Uani 1 1 d . A . Cl41 Cl 1.27513(7) 0.02687(4) 0.78801(6) 0.0631(2) Uani 1 1 d . . . Cl42 Cl 1.10291(7) -0.05510(3) 0.84640(4) 0.04944(15) Uani 1 1 d . . . Pd1 Pd 0.877120(12) 0.157606(6) 0.724151(8) 0.02103(4) Uani 1 1 d . . . O1 O 0.92291(18) 0.17738(9) 0.85778(12) 0.0268(6) Uani 0.770(6) 1 d P A 1 O2 O 0.9478(7) 0.0822(4) 0.8765(5) 0.0543(18) Uani 0.770(6) 1 d P A 1 N1 N 0.9507(2) 0.13327(12) 0.90857(16) 0.0319(7) Uani 0.770(6) 1 d P A 1 O1A O 0.9749(7) 0.1757(4) 0.9111(5) 0.039(2) Uiso 0.230(6) 1 d P A 2 O2A O 0.9461(14) 0.0800(9) 0.8784(11) 0.020(3) Uiso 0.230(6) 1 d P A 2 N1A N 0.9418(7) 0.1384(4) 0.8595(5) 0.0225(18) Uiso 0.230(6) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0223(8) 0.0305(10) 0.0218(8) 0.0010(7) 0.0037(6) -0.0008(7) C2 0.0195(8) 0.0323(10) 0.0232(8) -0.0013(7) 0.0018(6) 0.0005(7) C3 0.0171(7) 0.0271(9) 0.0243(8) -0.0054(7) 0.0041(6) -0.0013(6) C4 0.0167(8) 0.0329(10) 0.0309(9) -0.0037(7) 0.0026(7) -0.0026(7) C5 0.0203(8) 0.0363(11) 0.0355(10) -0.0020(8) 0.0043(7) -0.0086(8) C6 0.0244(9) 0.0322(10) 0.0297(9) -0.0010(8) 0.0039(7) -0.0085(8) C7 0.0200(8) 0.0265(9) 0.0245(8) -0.0031(7) 0.0021(6) -0.0041(7) C8 0.0175(7) 0.0236(8) 0.0219(8) -0.0058(6) 0.0054(6) -0.0015(6) C9 0.0167(7) 0.0223(8) 0.0216(8) -0.0062(6) 0.0054(6) -0.0010(6) C10 0.0166(7) 0.0217(8) 0.0229(8) -0.0039(6) 0.0036(6) -0.0012(6) C11 0.0149(7) 0.0216(8) 0.0209(7) -0.0027(6) 0.0031(6) -0.0012(6) C12 0.0186(7) 0.0224(8) 0.0201(7) 0.0011(6) 0.0038(6) -0.0020(6) C13 0.0202(7) 0.0239(8) 0.0191(7) -0.0005(6) 0.0058(6) -0.0006(6) C14 0.0215(8) 0.0213(8) 0.0211(8) -0.0025(6) 0.0052(6) -0.0038(6) C15 0.0195(7) 0.0218(8) 0.0230(8) -0.0001(6) 0.0062(6) -0.0039(6) C16 0.0173(7) 0.0261(9) 0.0189(7) -0.0013(6) 0.0059(6) -0.0016(6) C17 0.0220(11) 0.083(2) 0.084(2) 0.0331(18) -0.0066(12) -0.0199(12) C18 0.0435(14) 0.071(2) 0.0672(18) 0.0381(16) -0.0200(13) -0.0276(14) C19 0.0346(10) 0.0264(9) 0.0260(9) -0.0002(7) 0.0128(8) -0.0039(8) C20 0.0383(10) 0.0213(9) 0.0401(11) -0.0038(8) 0.0152(9) -0.0076(8) C21 0.0184(7) 0.0218(8) 0.0230(8) -0.0014(6) 0.0032(6) -0.0003(6) C22 0.0210(8) 0.0389(11) 0.0330(10) 0.0102(8) 0.0045(7) -0.0009(8) C23 0.0299(10) 0.0448(13) 0.0380(11) 0.0173(9) 0.0037(9) 0.0018(9) C24 0.0237(9) 0.0323(10) 0.0325(10) -0.0003(8) -0.0014(7) 0.0051(7) C25 0.0188(8) 0.0269(9) 0.0341(10) -0.0064(7) 0.0042(7) -0.0003(7) C26 0.0215(8) 0.0252(9) 0.0303(9) 0.0010(7) 0.0077(7) 0.0006(7) C27 0.0170(7) 0.0334(10) 0.0209(8) 0.0019(7) 0.0047(6) 0.0024(7) C28 0.0240(9) 0.0380(11) 0.0309(10) -0.0042(8) 0.0086(7) 0.0025(8) C29 0.0279(10) 0.0654(16) 0.0297(10) -0.0146(10) 0.0070(8) 0.0080(10) C30 0.0406(12) 0.083(2) 0.0257(10) 0.0045(11) 0.0147(9) 0.0183(13) C31 0.0446(12) 0.0580(15) 0.0358(11) 0.0176(11) 0.0207(10) 0.0071(11) C32 0.0322(10) 0.0366(11) 0.0310(10) 0.0083(8) 0.0137(8) 0.0025(8) C33 0.0226(8) 0.0222(8) 0.0242(8) 0.0018(6) 0.0087(6) -0.0007(6) C34 0.0278(9) 0.0288(10) 0.0340(10) -0.0019(8) 0.0034(8) -0.0022(8) C35 0.0446(12) 0.0301(11) 0.0362(11) -0.0054(8) 0.0055(9) -0.0084(9) C36 0.0561(14) 0.0224(10) 0.0382(11) -0.0003(8) 0.0194(10) -0.0016(9) C37 0.0416(11) 0.0278(10) 0.0426(12) 0.0058(9) 0.0152(9) 0.0070(9) C38 0.0266(9) 0.0276(10) 0.0334(10) 0.0034(8) 0.0068(8) 0.0015(7) C40 0.0348(11) 0.0428(13) 0.0498(14) -0.0084(10) 0.0139(10) -0.0017(10) N2 0.0179(6) 0.0263(8) 0.0210(7) -0.0031(6) 0.0050(5) -0.0018(5) O3 0.0215(7) 0.0575(11) 0.0558(10) 0.0156(8) -0.0008(7) -0.0172(7) O4 0.0313(8) 0.0457(9) 0.0449(9) 0.0148(7) -0.0020(7) -0.0169(7) O5 0.0348(7) 0.0241(7) 0.0208(6) -0.0028(5) 0.0114(5) -0.0050(5) O6 0.0386(7) 0.0219(6) 0.0278(7) -0.0055(5) 0.0126(6) -0.0075(6) P1 0.01688(18) 0.0222(2) 0.02019(19) 0.00098(16) 0.00492(15) -0.00092(16) Cl41 0.0430(3) 0.0540(4) 0.0970(6) -0.0059(4) 0.0271(4) -0.0113(3) Cl42 0.0547(4) 0.0486(3) 0.0490(3) -0.0111(3) 0.0205(3) -0.0099(3) Pd1 0.01717(6) 0.02734(8) 0.01859(6) -0.00136(5) 0.00477(5) -0.00356(5) O1 0.0263(9) 0.0319(12) 0.0230(10) -0.0063(7) 0.0078(7) -0.0055(7) O2 0.069(3) 0.0366(19) 0.0436(19) 0.0008(11) -0.0099(12) 0.0109(12) N1 0.0222(10) 0.0386(15) 0.0300(13) -0.0068(10) -0.0015(8) 0.0059(9) _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 C1 C2 1.361(3) . ? C1 N2 1.367(2) . ? C1 H1 0.9500 . ? C2 C3 1.414(3) . ? C2 H2 0.9500 . ? C3 C8 1.422(2) . ? C3 C4 1.425(2) . ? C4 C5 1.365(3) . ? C4 H4 0.9500 . ? C5 O3 1.357(2) . ? C5 C6 1.436(3) . ? C6 O4 1.354(2) . ? C6 C7 1.375(2) . ? C7 C8 1.430(3) . ? C7 H7 0.9500 . ? C8 C9 1.425(2) . ? C9 N2 1.341(2) . ? C9 C10 1.520(2) . ? C10 C11 1.523(2) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C16 1.392(2) . ? C11 C12 1.403(2) . ? C12 C13 1.385(2) . ? C12 H12 0.9500 . ? C13 O5 1.376(2) . ? C13 C14 1.407(2) . ? C14 O6 1.373(2) . ? C14 C15 1.390(2) . ? C15 C16 1.406(2) . ? C15 H15 0.9500 . ? C16 Pd1 2.0051(16) . ? C17 O3 1.435(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 O4 1.430(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 O5 1.421(2) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 O6 1.426(2) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.391(3) . ? C21 C26 1.402(2) . ? C21 P1 1.8311(18) . ? C22 C23 1.398(3) . ? C22 H22 0.9500 . ? C23 C24 1.385(3) . ? C23 H23 0.9500 . ? C24 C25 1.380(3) . ? C24 H24 0.9500 . ? C25 C26 1.391(3) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C32 1.392(3) . ? C27 C28 1.398(3) . ? C27 P1 1.8284(17) . ? C28 C29 1.392(3) . ? C28 H28 0.9500 . ? C29 C30 1.392(4) . ? C29 H29 0.9500 . ? C30 C31 1.381(4) . ? C30 H30 0.9500 . ? C31 C32 1.398(3) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.394(3) . ? C33 C38 1.401(3) . ? C33 P1 1.8259(19) . ? C34 C35 1.391(3) . ? C34 H34 0.9500 . ? C35 C36 1.377(3) . ? C35 H35 0.9500 . ? C36 C37 1.390(3) . ? C36 H36 0.9500 . ? C37 C38 1.384(3) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C40 Cl41 1.760(2) . ? C40 Cl42 1.764(3) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? N2 Pd1 2.1219(14) . ? P1 Pd1 2.2739(4) . ? Pd1 O1 2.1511(18) . ? Pd1 N1A 2.177(8) . ? O1 N1 1.253(4) . ? O2 N1 1.227(8) . ? O1A N1A 1.157(14) . ? O2A N1A 1.31(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 N2 122.64(17) . . ? C2 C1 H1 118.7 . . ? N2 C1 H1 118.7 . . ? C1 C2 C3 119.41(17) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C2 C3 C8 118.62(16) . . ? C2 C3 C4 121.40(17) . . ? C8 C3 C4 119.96(17) . . ? C5 C4 C3 120.03(18) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? O3 C5 C4 125.64(19) . . ? O3 C5 C6 113.79(18) . . ? C4 C5 C6 120.56(17) . . ? O4 C6 C7 125.89(18) . . ? O4 C6 C5 113.80(16) . . ? C7 C6 C5 120.31(18) . . ? C6 C7 C8 120.17(17) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C3 C8 C9 117.99(16) . . ? C3 C8 C7 118.85(15) . . ? C9 C8 C7 123.14(16) . . ? N2 C9 C8 121.38(15) . . ? N2 C9 C10 114.83(14) . . ? C8 C9 C10 123.72(16) . . ? C9 C10 C11 107.89(14) . . ? C9 C10 H10A 110.1 . . ? C11 C10 H10A 110.1 . . ? C9 C10 H10B 110.1 . . ? C11 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? C16 C11 C12 120.74(16) . . ? C16 C11 C10 120.03(15) . . ? C12 C11 C10 118.73(15) . . ? C13 C12 C11 120.07(16) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? O5 C13 C12 124.93(16) . . ? O5 C13 C14 115.25(15) . . ? C12 C13 C14 119.81(15) . . ? O6 C14 C15 124.94(16) . . ? O6 C14 C13 115.25(15) . . ? C15 C14 C13 119.80(16) . . ? C14 C15 C16 120.79(16) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C11 C16 C15 118.75(15) . . ? C11 C16 Pd1 116.78(12) . . ? C15 C16 Pd1 123.11(13) . . ? O3 C17 H17A 109.5 . . ? O3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O4 C18 H18A 109.5 . . ? O4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O5 C19 H19A 109.5 . . ? O5 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O5 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O6 C20 H20A 109.5 . . ? O6 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O6 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C26 118.51(17) . . ? C22 C21 P1 121.41(13) . . ? C26 C21 P1 120.06(14) . . ? C21 C22 C23 120.07(18) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C24 C23 C22 120.91(19) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C25 C24 C23 119.39(18) . . ? C25 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? C24 C25 C26 120.22(17) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C25 C26 C21 120.90(17) . . ? C25 C26 H26 119.6 . . ? C21 C26 H26 119.6 . . ? C32 C27 C28 119.79(17) . . ? C32 C27 P1 122.48(15) . . ? C28 C27 P1 117.71(14) . . ? C29 C28 C27 120.2(2) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 C30 119.9(2) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C31 C30 C29 119.9(2) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C30 C31 C32 120.8(2) . . ? C30 C31 H31 119.6 . . ? C32 C31 H31 119.6 . . ? C27 C32 C31 119.4(2) . . ? C27 C32 H32 120.3 . . ? C31 C32 H32 120.3 . . ? C34 C33 C38 118.94(18) . . ? C34 C33 P1 123.50(14) . . ? C38 C33 P1 117.53(14) . . ? C35 C34 C33 120.23(19) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C36 C35 C34 120.6(2) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C35 C36 C37 119.5(2) . . ? C35 C36 H36 120.2 . . ? C37 C36 H36 120.2 . . ? C38 C37 C36 120.6(2) . . ? C38 C37 H37 119.7 . . ? C36 C37 H37 119.7 . . ? C37 C38 C33 120.12(19) . . ? C37 C38 H38 119.9 . . ? C33 C38 H38 119.9 . . ? Cl41 C40 Cl42 111.05(14) . . ? Cl41 C40 H40A 109.4 . . ? Cl42 C40 H40A 109.4 . . ? Cl41 C40 H40B 109.4 . . ? Cl42 C40 H40B 109.4 . . ? H40A C40 H40B 108.0 . . ? C9 N2 C1 119.86(15) . . ? C9 N2 Pd1 120.63(11) . . ? C1 N2 Pd1 119.47(12) . . ? C5 O3 C17 116.73(18) . . ? C6 O4 C18 117.28(17) . . ? C13 O5 C19 116.19(14) . . ? C14 O6 C20 116.97(14) . . ? C33 P1 C27 104.30(8) . . ? C33 P1 C21 104.73(8) . . ? C27 P1 C21 102.50(8) . . ? C33 P1 Pd1 114.55(6) . . ? C27 P1 Pd1 111.56(6) . . ? C21 P1 Pd1 117.70(6) . . ? C16 Pd1 N2 85.50(6) . . ? C16 Pd1 O1 169.88(7) . . ? N2 Pd1 O1 84.50(6) . . ? C16 Pd1 N1A 158.8(2) . . ? N2 Pd1 N1A 90.61(19) . . ? O1 Pd1 N1A 23.2(2) . . ? C16 Pd1 P1 93.46(5) . . ? N2 Pd1 P1 174.65(4) . . ? O1 Pd1 P1 96.36(5) . . ? N1A Pd1 P1 92.22(18) . . ? N1 O1 Pd1 117.98(17) . . ? O2 N1 O1 116.0(4) . . ? O1A N1A O2A 121.8(11) . . ? O1A N1A Pd1 124.0(7) . . ? O2A N1A Pd1 114.1(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 N2 C1 C2 C3 1.9(3) . . . . ? C1 C2 C3 C8 0.0(3) . . . . ? C1 C2 C3 C4 -178.45(18) . . . . ? C2 C3 C4 C5 -179.53(18) . . . . ? C8 C3 C4 C5 2.0(3) . . . . ? C3 C4 C5 O3 179.7(2) . . . . ? C3 C4 C5 C6 1.0(3) . . . . ? O3 C5 C6 O4 -2.3(3) . . . . ? C4 C5 C6 O4 176.53(19) . . . . ? O3 C5 C6 C7 177.78(19) . . . . ? C4 C5 C6 C7 -3.4(3) . . . . ? O4 C6 C7 C8 -177.29(19) . . . . ? C5 C6 C7 C8 2.7(3) . . . . ? C2 C3 C8 C9 -2.6(2) . . . . ? C4 C3 C8 C9 175.87(16) . . . . ? C2 C3 C8 C7 178.78(16) . . . . ? C4 C3 C8 C7 -2.7(2) . . . . ? C6 C7 C8 C3 0.4(3) . . . . ? C6 C7 C8 C9 -178.14(17) . . . . ? C3 C8 C9 N2 3.6(2) . . . . ? C7 C8 C9 N2 -177.92(16) . . . . ? C3 C8 C9 C10 -173.43(15) . . . . ? C7 C8 C9 C10 5.1(3) . . . . ? N2 C9 C10 C11 -56.03(18) . . . . ? C8 C9 C10 C11 121.14(17) . . . . ? C9 C10 C11 C16 66.81(19) . . . . ? C9 C10 C11 C12 -105.23(17) . . . . ? C16 C11 C12 C13 -0.9(2) . . . . ? C10 C11 C12 C13 171.09(15) . . . . ? C11 C12 C13 O5 -177.07(16) . . . . ? C11 C12 C13 C14 2.0(3) . . . . ? O5 C13 C14 O6 -1.0(2) . . . . ? C12 C13 C14 O6 179.91(15) . . . . ? O5 C13 C14 C15 178.09(16) . . . . ? C12 C13 C14 C15 -1.0(3) . . . . ? O6 C14 C15 C16 177.97(16) . . . . ? C13 C14 C15 C16 -1.0(3) . . . . ? C12 C11 C16 C15 -1.1(2) . . . . ? C10 C11 C16 C15 -172.98(15) . . . . ? C12 C11 C16 Pd1 165.99(13) . . . . ? C10 C11 C16 Pd1 -5.9(2) . . . . ? C14 C15 C16 C11 2.0(3) . . . . ? C14 C15 C16 Pd1 -164.19(13) . . . . ? C26 C21 C22 C23 0.2(3) . . . . ? P1 C21 C22 C23 178.83(17) . . . . ? C21 C22 C23 C24 -0.9(4) . . . . ? C22 C23 C24 C25 0.8(3) . . . . ? C23 C24 C25 C26 -0.1(3) . . . . ? C24 C25 C26 C21 -0.6(3) . . . . ? C22 C21 C26 C25 0.5(3) . . . . ? P1 C21 C26 C25 -178.11(14) . . . . ? C32 C27 C28 C29 0.9(3) . . . . ? P1 C27 C28 C29 -177.54(16) . . . . ? C27 C28 C29 C30 -1.3(3) . . . . ? C28 C29 C30 C31 0.2(3) . . . . ? C29 C30 C31 C32 1.4(4) . . . . ? C28 C27 C32 C31 0.6(3) . . . . ? P1 C27 C32 C31 178.98(16) . . . . ? C30 C31 C32 C27 -1.8(3) . . . . ? C38 C33 C34 C35 -0.9(3) . . . . ? P1 C33 C34 C35 177.29(16) . . . . ? C33 C34 C35 C36 -1.1(3) . . . . ? C34 C35 C36 C37 2.0(3) . . . . ? C35 C36 C37 C38 -0.9(3) . . . . ? C36 C37 C38 C33 -1.1(3) . . . . ? C34 C33 C38 C37 2.0(3) . . . . ? P1 C33 C38 C37 -176.30(15) . . . . ? C8 C9 N2 C1 -1.7(2) . . . . ? C10 C9 N2 C1 175.50(15) . . . . ? C8 C9 N2 Pd1 176.03(12) . . . . ? C10 C9 N2 Pd1 -6.73(19) . . . . ? C2 C1 N2 C9 -1.1(3) . . . . ? C2 C1 N2 Pd1 -178.88(14) . . . . ? C4 C5 O3 C17 0.6(4) . . . . ? C6 C5 O3 C17 179.4(2) . . . . ? C7 C6 O4 C18 2.7(3) . . . . ? C5 C6 O4 C18 -177.3(2) . . . . ? C12 C13 O5 C19 2.5(2) . . . . ? C14 C13 O5 C19 -176.59(16) . . . . ? C15 C14 O6 C20 -4.0(3) . . . . ? C13 C14 O6 C20 175.04(16) . . . . ? C34 C33 P1 C27 102.19(16) . . . . ? C38 C33 P1 C27 -79.60(15) . . . . ? C34 C33 P1 C21 -5.15(18) . . . . ? C38 C33 P1 C21 173.05(14) . . . . ? C34 C33 P1 Pd1 -135.57(14) . . . . ? C38 C33 P1 Pd1 42.63(15) . . . . ? C32 C27 P1 C33 -5.73(18) . . . . ? C28 C27 P1 C33 172.67(14) . . . . ? C32 C27 P1 C21 103.25(16) . . . . ? C28 C27 P1 C21 -78.35(15) . . . . ? C32 C27 P1 Pd1 -129.90(14) . . . . ? C28 C27 P1 Pd1 48.49(16) . . . . ? C22 C21 P1 C33 -109.30(17) . . . . ? C26 C21 P1 C33 69.30(16) . . . . ? C22 C21 P1 C27 142.04(17) . . . . ? C26 C21 P1 C27 -39.36(17) . . . . ? C22 C21 P1 Pd1 19.25(18) . . . . ? C26 C21 P1 Pd1 -162.15(13) . . . . ? C11 C16 Pd1 N2 -40.80(13) . . . . ? C15 C16 Pd1 N2 125.69(15) . . . . ? C11 C16 Pd1 O1 -32.1(5) . . . . ? C15 C16 Pd1 O1 134.4(4) . . . . ? C11 C16 Pd1 N1A -120.8(6) . . . . ? C15 C16 Pd1 N1A 45.6(6) . . . . ? C11 C16 Pd1 P1 133.94(12) . . . . ? C15 C16 Pd1 P1 -59.58(14) . . . . ? C9 N2 Pd1 C16 50.34(13) . . . . ? C1 N2 Pd1 C16 -131.88(14) . . . . ? C9 N2 Pd1 O1 -128.13(14) . . . . ? C1 N2 Pd1 O1 49.65(14) . . . . ? C9 N2 Pd1 N1A -150.6(3) . . . . ? C1 N2 Pd1 N1A 27.2(3) . . . . ? C9 N2 Pd1 P1 -28.7(5) . . . . ? C1 N2 Pd1 P1 149.1(4) . . . . ? C33 P1 Pd1 C16 64.86(8) . . . . ? C27 P1 Pd1 C16 -176.94(8) . . . . ? C21 P1 Pd1 C16 -58.88(8) . . . . ? C33 P1 Pd1 N2 143.5(4) . . . . ? C27 P1 Pd1 N2 -98.3(4) . . . . ? C21 P1 Pd1 N2 19.8(4) . . . . ? C33 P1 Pd1 O1 -117.58(9) . . . . ? C27 P1 Pd1 O1 0.61(9) . . . . ? C21 P1 Pd1 O1 118.68(9) . . . . ? C33 P1 Pd1 N1A -94.7(2) . . . . ? C27 P1 Pd1 N1A 23.5(2) . . . . ? C21 P1 Pd1 N1A 141.6(2) . . . . ? C16 Pd1 O1 N1 -120.7(4) . . . . ? N2 Pd1 O1 N1 -112.04(17) . . . . ? N1A Pd1 O1 N1 -7.5(5) . . . . ? P1 Pd1 O1 N1 73.27(16) . . . . ? Pd1 O1 N1 O2 -0.7(4) . . . . ? C16 Pd1 N1A O1A 134.9(7) . . . . ? N2 Pd1 N1A O1A 55.8(7) . . . . ? O1 Pd1 N1A O1A -18.6(5) . . . . ? P1 Pd1 N1A O1A -119.6(7) . . . . ? C16 Pd1 N1A O2A -42.1(10) . . . . ? N2 Pd1 N1A O2A -121.2(8) . . . . ? O1 Pd1 N1A O2A 164.4(10) . . . . ? P1 Pd1 N1A O2A 63.3(8) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 29.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.712 _refine_diff_density_min -0.820 _refine_diff_density_rms 0.073 ### END data_8_UV150K _database_code_depnum_ccdc_archive 'CCDC 858650' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Nitro-(1-(3,4-dimethoxybenzyl)-6,7-dimethoxyisoquinoline)(triphenylphosphine) palladium(II) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H37 Cl2 N2 O6 P Pd' _chemical_formula_sum 'C39 H37 Cl2 N2 O6 P Pd' _chemical_formula_weight 837.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.7119(4) _cell_length_b 21.7420(12) _cell_length_c 16.4105(6) _cell_angle_alpha 90.00 _cell_angle_beta 105.404(4) _cell_angle_gamma 90.00 _cell_volume 3684.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 14733 _cell_measurement_theta_min 1.5429 _cell_measurement_theta_max 29.4767 _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 0.742 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.81579 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.68890 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator synchrotron _diffrn_measurement_device ; CrystalLogic Kappa (3 circle) ; _diffrn_measurement_device_type ; Rigaku Saturn724+ (2x2 bin mode) ; _diffrn_measurement_method '1.0 degree images with \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40979 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0954 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.5429 _diffrn_reflns_theta_max 29.4767 _diffrn_orient_matrix_UB_11 0.0022998000 _diffrn_orient_matrix_UB_12 -0.0107816000 _diffrn_orient_matrix_UB_13 0.0398166000 _diffrn_orient_matrix_UB_21 0.0546163000 _diffrn_orient_matrix_UB_22 -0.0167680000 _diffrn_orient_matrix_UB_23 0.0001655000 _diffrn_orient_matrix_UB_31 0.0382449000 _diffrn_orient_matrix_UB_32 0.0246567000 _diffrn_orient_matrix_UB_33 0.0175440000 _reflns_number_total 11231 _reflns_number_gt 9677 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009) ; _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-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics WINGX _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+1.8208P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11231 _refine_ls_number_parameters 464 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0407 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0814 _refine_ls_wR_factor_gt 0.0771 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.15860(17) 0.19045(9) 0.78852(11) 0.0239(3) Uani 1 1 d . . . H1 H 1.1536 0.1586 0.8271 0.029 Uiso 1 1 calc R . . C2 C 1.27474(16) 0.21885(9) 0.79599(11) 0.0246(3) Uani 1 1 d . . . H2 H 1.3495 0.2058 0.8379 0.030 Uiso 1 1 calc R . . C3 C 1.28329(16) 0.26780(8) 0.74113(11) 0.0220(3) Uani 1 1 d . . . C4 C 1.40284(17) 0.29769(9) 0.74503(12) 0.0272(4) Uani 1 1 d . . . H4 H 1.4797 0.2844 0.7848 0.033 Uiso 1 1 calc R . . C5 C 1.40749(18) 0.34533(10) 0.69196(13) 0.0311(4) Uani 1 1 d . . . C6 C 1.29224(18) 0.36653(9) 0.63219(12) 0.0290(4) Uani 1 1 d . . . C7 C 1.17598(17) 0.33655(8) 0.62447(12) 0.0243(3) Uani 1 1 d . . . H7 H 1.1006 0.3495 0.5830 0.029 Uiso 1 1 calc R . . C8 C 1.16900(15) 0.28597(8) 0.67899(10) 0.0204(3) Uani 1 1 d . . . C9 C 1.05341(15) 0.25188(8) 0.67325(10) 0.0195(3) Uani 1 1 d . . . C10 C 0.92846(15) 0.26143(8) 0.60414(10) 0.0202(3) Uani 1 1 d . . . H10A H 0.9406 0.2938 0.5645 0.024 Uiso 1 1 calc R . . H10B H 0.8582 0.2745 0.6292 0.024 Uiso 1 1 calc R . . C11 C 0.89348(15) 0.20066(8) 0.55763(10) 0.0193(3) Uani 1 1 d . . . C12 C 0.91212(16) 0.19434(8) 0.47641(10) 0.0207(3) Uani 1 1 d . . . H12 H 0.9345 0.2292 0.4484 0.025 Uiso 1 1 calc R . . C13 C 0.89785(16) 0.13725(8) 0.43711(10) 0.0210(3) Uani 1 1 d . . . C14 C 0.86104(16) 0.08607(8) 0.47790(11) 0.0216(3) Uani 1 1 d . . . C15 C 0.84111(16) 0.09289(8) 0.55784(11) 0.0215(3) Uani 1 1 d . . . H15 H 0.8153 0.0583 0.5849 0.026 Uiso 1 1 calc R . . C16 C 0.85859(15) 0.15014(8) 0.59921(10) 0.0195(3) Uani 1 1 d . . . C17 C 1.6341(2) 0.35954(16) 0.7493(2) 0.0654(9) Uani 1 1 d . . . H17A H 1.6255 0.3640 0.8070 0.098 Uiso 1 1 calc R . . H17B H 1.7047 0.3858 0.7421 0.098 Uiso 1 1 calc R . . H17C H 1.6531 0.3165 0.7393 0.098 Uiso 1 1 calc R . . C18 C 1.1987(3) 0.44240(15) 0.5299(2) 0.0695(10) Uani 1 1 d . . . H18A H 1.1600 0.4123 0.4861 0.104 Uiso 1 1 calc R . . H18B H 1.2241 0.4791 0.5036 0.104 Uiso 1 1 calc R . . H18C H 1.1354 0.4538 0.5608 0.104 Uiso 1 1 calc R . . C19 C 0.9649(2) 0.17539(9) 0.31969(12) 0.0284(4) Uani 1 1 d . . . H19A H 0.9011 0.2087 0.3099 0.043 Uiso 1 1 calc R . . H19B H 0.9774 0.1617 0.2655 0.043 Uiso 1 1 calc R . . H19C H 1.0474 0.1902 0.3561 0.043 Uiso 1 1 calc R . . C20 C 0.8242(2) -0.02207(9) 0.47621(13) 0.0314(4) Uani 1 1 d . . . H20A H 0.8926 -0.0276 0.5288 0.047 Uiso 1 1 calc R . . H20B H 0.8217 -0.0580 0.4397 0.047 Uiso 1 1 calc R . . H20C H 0.7405 -0.0177 0.4893 0.047 Uiso 1 1 calc R . . C21 C 0.53481(16) 0.15551(8) 0.64349(11) 0.0214(3) Uani 1 1 d . . . C22 C 0.54730(18) 0.19518(10) 0.57975(13) 0.0308(4) Uani 1 1 d . . . H22 H 0.6306 0.2040 0.5726 0.037 Uiso 1 1 calc R . . C23 C 0.4372(2) 0.22224(11) 0.52609(14) 0.0381(5) Uani 1 1 d . . . H23 H 0.4464 0.2496 0.4830 0.046 Uiso 1 1 calc R . . C24 C 0.31482(18) 0.20945(10) 0.53527(13) 0.0310(4) Uani 1 1 d . . . H24 H 0.2405 0.2277 0.4983 0.037 Uiso 1 1 calc R . . C25 C 0.30173(17) 0.17011(9) 0.59836(13) 0.0269(4) Uani 1 1 d . . . H25 H 0.2181 0.1610 0.6047 0.032 Uiso 1 1 calc R . . C26 C 0.41071(17) 0.14368(9) 0.65271(12) 0.0250(3) Uani 1 1 d . . . H26 H 0.4009 0.1173 0.6967 0.030 Uiso 1 1 calc R . . C27 C 0.63642(16) 0.11830(9) 0.81523(11) 0.0229(3) Uani 1 1 d . . . C28 C 0.65312(18) 0.17348(10) 0.86092(13) 0.0297(4) Uani 1 1 d . . . H28 H 0.6802 0.2095 0.8376 0.036 Uiso 1 1 calc R . . C29 C 0.6302(2) 0.17570(12) 0.94025(14) 0.0397(5) Uani 1 1 d . . . H29 H 0.6440 0.2129 0.9716 0.048 Uiso 1 1 calc R . . C30 C 0.5872(2) 0.12376(14) 0.97395(14) 0.0484(6) Uani 1 1 d . . . H30 H 0.5707 0.1255 1.0280 0.058 Uiso 1 1 calc R . . C31 C 0.5687(2) 0.06959(13) 0.92840(15) 0.0445(6) Uani 1 1 d . . . H31 H 0.5380 0.0342 0.9511 0.053 Uiso 1 1 calc R . . C32 C 0.59445(19) 0.06598(10) 0.84914(13) 0.0321(4) Uani 1 1 d . . . H32 H 0.5834 0.0282 0.8189 0.038 Uiso 1 1 calc R . . C33 C 0.66054(17) 0.03717(8) 0.68118(11) 0.0218(3) Uani 1 1 d . . . C34 C 0.55334(19) 0.01383(9) 0.62128(13) 0.0304(4) Uani 1 1 d . . . H34 H 0.4823 0.0400 0.5968 0.036 Uiso 1 1 calc R . . C35 C 0.5500(2) -0.04769(10) 0.59723(14) 0.0366(5) Uani 1 1 d . . . H35 H 0.4760 -0.0634 0.5570 0.044 Uiso 1 1 calc R . . C36 C 0.6534(2) -0.08604(9) 0.63146(14) 0.0356(5) Uani 1 1 d . . . H36 H 0.6518 -0.1277 0.6136 0.043 Uiso 1 1 calc R . . C37 C 0.7594(2) -0.06349(10) 0.69199(14) 0.0350(4) Uani 1 1 d . . . H37 H 0.8301 -0.0900 0.7162 0.042 Uiso 1 1 calc R . . C38 C 0.76336(19) -0.00245(9) 0.71765(13) 0.0288(4) Uani 1 1 d . . . H38 H 0.8358 0.0124 0.7599 0.035 Uiso 1 1 calc R . . C40 C 1.1158(2) -0.00131(12) 0.76446(16) 0.0428(5) Uani 1 1 d . . . H40A H 1.0957 -0.0226 0.7092 0.051 Uiso 1 1 calc R . . H40B H 1.0527 0.0326 0.7605 0.051 Uiso 1 1 calc R . . N2 N 1.04914(13) 0.20626(7) 0.72747(9) 0.0203(3) Uani 1 1 d . . . O3 O 1.51519(14) 0.37758(8) 0.69009(11) 0.0463(4) Uani 1 1 d . . . O4 O 1.31040(15) 0.41619(8) 0.58721(10) 0.0425(4) Uani 1 1 d . . . O5 O 0.91953(13) 0.12529(6) 0.35976(8) 0.0259(3) Uani 1 1 d . . . O6 O 0.84977(14) 0.03173(6) 0.43389(8) 0.0286(3) Uani 1 1 d . . . P1 P 0.67599(4) 0.11780(2) 0.71343(3) 0.01923(8) Uani 1 1 d . . . Cl41 Cl 1.27335(7) 0.02920(4) 0.78713(6) 0.0640(2) Uani 1 1 d . . . Cl42 Cl 1.10067(6) -0.05361(3) 0.84363(4) 0.04909(15) Uani 1 1 d . . . Pd1 Pd 0.873498(12) 0.160138(6) 0.723002(8) 0.01884(4) Uani 1 1 d . . . O1 O 0.92072(13) 0.17801(7) 0.85640(8) 0.0288(3) Uani 1 1 d . . . O2 O 0.94514(18) 0.08211(7) 0.87469(10) 0.0463(4) Uani 1 1 d . . . N1 N 0.94915(16) 0.13394(9) 0.90660(11) 0.0338(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0219(8) 0.0274(9) 0.0218(8) 0.0014(7) 0.0045(6) 0.0005(7) C2 0.0184(7) 0.0292(9) 0.0243(8) -0.0011(7) 0.0024(6) 0.0005(7) C3 0.0172(7) 0.0254(9) 0.0235(8) -0.0051(6) 0.0053(6) -0.0005(6) C4 0.0169(7) 0.0315(10) 0.0313(9) -0.0029(7) 0.0028(6) -0.0021(7) C5 0.0206(8) 0.0360(11) 0.0354(10) -0.0030(8) 0.0056(7) -0.0090(7) C6 0.0257(9) 0.0307(10) 0.0286(9) -0.0002(7) 0.0036(7) -0.0079(7) C7 0.0215(8) 0.0244(9) 0.0253(8) -0.0021(7) 0.0032(6) -0.0032(7) C8 0.0176(7) 0.0226(8) 0.0208(7) -0.0046(6) 0.0048(6) 0.0004(6) C9 0.0170(7) 0.0214(8) 0.0202(7) -0.0043(6) 0.0054(6) 0.0001(6) C10 0.0169(7) 0.0207(8) 0.0218(7) -0.0027(6) 0.0034(6) -0.0007(6) C11 0.0156(7) 0.0201(8) 0.0209(7) -0.0018(6) 0.0029(6) -0.0007(6) C12 0.0200(7) 0.0213(8) 0.0206(7) 0.0010(6) 0.0050(6) -0.0013(6) C13 0.0206(7) 0.0234(8) 0.0188(7) -0.0016(6) 0.0052(6) -0.0014(6) C14 0.0217(7) 0.0200(8) 0.0232(8) -0.0036(6) 0.0061(6) -0.0032(6) C15 0.0214(7) 0.0207(8) 0.0232(8) 0.0004(6) 0.0072(6) -0.0033(6) C16 0.0169(7) 0.0232(8) 0.0185(7) -0.0014(6) 0.0050(6) -0.0014(6) C17 0.0215(10) 0.082(2) 0.082(2) 0.0303(17) -0.0044(12) -0.0197(12) C18 0.0489(15) 0.0691(19) 0.0677(18) 0.0411(16) -0.0246(13) -0.0322(14) C19 0.0363(10) 0.0268(9) 0.0254(9) -0.0015(7) 0.0142(8) -0.0052(8) C20 0.0371(10) 0.0214(9) 0.0384(10) -0.0042(8) 0.0144(8) -0.0067(8) C21 0.0192(7) 0.0210(8) 0.0238(8) -0.0005(6) 0.0050(6) 0.0003(6) C22 0.0207(8) 0.0366(11) 0.0343(10) 0.0100(8) 0.0057(7) -0.0014(7) C23 0.0286(10) 0.0454(13) 0.0372(11) 0.0183(9) 0.0033(8) 0.0009(9) C24 0.0231(8) 0.0326(10) 0.0327(10) 0.0000(8) -0.0007(7) 0.0037(7) C25 0.0191(8) 0.0260(9) 0.0342(9) -0.0070(7) 0.0047(7) 0.0005(7) C26 0.0227(8) 0.0229(9) 0.0306(9) -0.0002(7) 0.0093(7) 0.0006(7) C27 0.0179(7) 0.0296(9) 0.0213(8) 0.0022(7) 0.0053(6) 0.0035(6) C28 0.0225(8) 0.0366(11) 0.0310(9) -0.0052(8) 0.0089(7) 0.0040(7) C29 0.0287(10) 0.0604(15) 0.0301(10) -0.0148(10) 0.0079(8) 0.0075(10) C30 0.0404(12) 0.083(2) 0.0246(10) 0.0030(11) 0.0138(9) 0.0167(12) C31 0.0454(12) 0.0576(15) 0.0366(11) 0.0176(11) 0.0219(10) 0.0082(11) C32 0.0319(9) 0.0347(11) 0.0333(10) 0.0072(8) 0.0151(8) 0.0020(8) C33 0.0233(8) 0.0203(8) 0.0232(8) 0.0011(6) 0.0084(6) -0.0013(6) C34 0.0294(9) 0.0261(10) 0.0327(10) -0.0021(7) 0.0034(7) -0.0015(7) C35 0.0438(12) 0.0272(10) 0.0362(11) -0.0060(8) 0.0057(9) -0.0087(9) C36 0.0535(13) 0.0203(9) 0.0363(11) -0.0016(8) 0.0175(10) -0.0031(9) C37 0.0409(11) 0.0257(10) 0.0406(11) 0.0047(8) 0.0147(9) 0.0077(8) C38 0.0266(9) 0.0263(9) 0.0329(9) 0.0035(7) 0.0070(7) 0.0022(7) C40 0.0372(11) 0.0402(13) 0.0532(14) -0.0093(10) 0.0157(10) -0.0028(10) N2 0.0172(6) 0.0229(7) 0.0209(6) -0.0018(5) 0.0053(5) -0.0008(5) O3 0.0223(7) 0.0566(11) 0.0547(10) 0.0137(8) 0.0008(7) -0.0162(7) O4 0.0336(8) 0.0436(9) 0.0437(9) 0.0142(7) -0.0013(7) -0.0173(7) O5 0.0361(7) 0.0232(6) 0.0212(6) -0.0033(5) 0.0124(5) -0.0051(5) O6 0.0390(7) 0.0207(6) 0.0289(7) -0.0059(5) 0.0139(6) -0.0066(5) P1 0.01741(18) 0.0201(2) 0.02044(19) 0.00086(15) 0.00555(15) -0.00045(15) Cl41 0.0439(3) 0.0527(4) 0.1003(6) -0.0039(4) 0.0279(4) -0.0117(3) Cl42 0.0554(3) 0.0467(3) 0.0498(3) -0.0116(3) 0.0221(3) -0.0108(3) Pd1 0.01732(6) 0.02088(7) 0.01858(6) -0.00114(4) 0.00519(4) -0.00184(5) O1 0.0287(7) 0.0344(7) 0.0245(6) -0.0047(5) 0.0093(5) -0.0057(6) O2 0.0552(10) 0.0336(9) 0.0395(9) -0.0006(7) -0.0059(7) 0.0086(8) N1 0.0255(8) 0.0378(10) 0.0339(9) -0.0082(7) 0.0008(7) 0.0048(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.365(2) . ? C1 N2 1.368(2) . ? C1 H1 0.9500 . ? C2 C3 1.412(3) . ? C2 H2 0.9500 . ? C3 C4 1.422(2) . ? C3 C8 1.425(2) . ? C4 C5 1.363(3) . ? C4 H4 0.9500 . ? C5 O3 1.357(2) . ? C5 C6 1.434(3) . ? C6 O4 1.351(2) . ? C6 C7 1.381(2) . ? C7 C8 1.432(2) . ? C7 H7 0.9500 . ? C8 C9 1.425(2) . ? C9 N2 1.341(2) . ? C9 C10 1.521(2) . ? C10 C11 1.522(2) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C16 1.395(2) . ? C11 C12 1.406(2) . ? C12 C13 1.388(2) . ? C12 H12 0.9500 . ? C13 O5 1.3746(19) . ? C13 C14 1.408(2) . ? C14 O6 1.373(2) . ? C14 C15 1.392(2) . ? C15 C16 1.406(2) . ? C15 H15 0.9500 . ? C16 Pd1 2.0069(16) . ? C17 O3 1.436(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 O4 1.429(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 O5 1.423(2) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 O6 1.424(2) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.389(3) . ? C21 C26 1.401(2) . ? C21 P1 1.8314(18) . ? C22 C23 1.400(3) . ? C22 H22 0.9500 . ? C23 C24 1.387(3) . ? C23 H23 0.9500 . ? C24 C25 1.378(3) . ? C24 H24 0.9500 . ? C25 C26 1.391(3) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C32 1.392(3) . ? C27 C28 1.401(3) . ? C27 P1 1.8295(17) . ? C28 C29 1.388(3) . ? C28 H28 0.9500 . ? C29 C30 1.389(4) . ? C29 H29 0.9500 . ? C30 C31 1.381(4) . ? C30 H30 0.9500 . ? C31 C32 1.402(3) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.394(3) . ? C33 C38 1.401(3) . ? C33 P1 1.8260(18) . ? C34 C35 1.393(3) . ? C34 H34 0.9500 . ? C35 C36 1.381(3) . ? C35 H35 0.9500 . ? C36 C37 1.385(3) . ? C36 H36 0.9500 . ? C37 C38 1.390(3) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C40 Cl41 1.759(2) . ? C40 Cl42 1.766(3) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? N2 Pd1 2.1160(14) . ? P1 Pd1 2.2741(4) . ? Pd1 O1 2.1472(13) . ? O1 N1 1.248(2) . ? O2 N1 1.239(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 N2 122.37(17) . . ? C2 C1 H1 118.8 . . ? N2 C1 H1 118.8 . . ? C1 C2 C3 119.70(16) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C2 C3 C4 121.70(16) . . ? C2 C3 C8 118.43(15) . . ? C4 C3 C8 119.84(16) . . ? C5 C4 C3 120.26(17) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? O3 C5 C4 125.64(18) . . ? O3 C5 C6 113.64(18) . . ? C4 C5 C6 120.70(17) . . ? O4 C6 C7 125.74(18) . . ? O4 C6 C5 114.08(16) . . ? C7 C6 C5 120.18(18) . . ? C6 C7 C8 120.02(17) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C9 C8 C3 118.00(16) . . ? C9 C8 C7 123.15(15) . . ? C3 C8 C7 118.84(15) . . ? N2 C9 C8 121.53(15) . . ? N2 C9 C10 114.66(14) . . ? C8 C9 C10 123.74(15) . . ? C9 C10 C11 107.82(14) . . ? C9 C10 H10A 110.1 . . ? C11 C10 H10A 110.1 . . ? C9 C10 H10B 110.1 . . ? C11 C10 H10B 110.1 . . ? H10A C10 H10B 108.5 . . ? C16 C11 C12 120.70(15) . . ? C16 C11 C10 120.02(14) . . ? C12 C11 C10 118.83(15) . . ? C13 C12 C11 120.13(16) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? O5 C13 C12 124.99(15) . . ? O5 C13 C14 115.26(15) . . ? C12 C13 C14 119.74(15) . . ? O6 C14 C15 124.98(16) . . ? O6 C14 C13 115.25(14) . . ? C15 C14 C13 119.76(16) . . ? C14 C15 C16 121.01(16) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C11 C16 C15 118.64(15) . . ? C11 C16 Pd1 116.75(12) . . ? C15 C16 Pd1 123.30(12) . . ? O3 C17 H17A 109.5 . . ? O3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O4 C18 H18A 109.5 . . ? O4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O5 C19 H19A 109.5 . . ? O5 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O5 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O6 C20 H20A 109.5 . . ? O6 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O6 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C26 118.62(16) . . ? C22 C21 P1 121.41(13) . . ? C26 C21 P1 119.96(13) . . ? C21 C22 C23 120.06(17) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C24 C23 C22 120.65(19) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C25 C24 C23 119.59(18) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C24 C25 C26 120.15(17) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C25 C26 C21 120.91(17) . . ? C25 C26 H26 119.5 . . ? C21 C26 H26 119.5 . . ? C32 C27 C28 119.65(17) . . ? C32 C27 P1 122.54(15) . . ? C28 C27 P1 117.79(14) . . ? C29 C28 C27 120.2(2) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 C30 120.3(2) . . ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? C31 C30 C29 119.6(2) . . ? C31 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C30 C31 C32 121.0(2) . . ? C30 C31 H31 119.5 . . ? C32 C31 H31 119.5 . . ? C27 C32 C31 119.3(2) . . ? C27 C32 H32 120.4 . . ? C31 C32 H32 120.4 . . ? C34 C33 C38 118.97(17) . . ? C34 C33 P1 123.24(14) . . ? C38 C33 P1 117.78(14) . . ? C35 C34 C33 120.26(19) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C36 C35 C34 120.5(2) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C35 C36 C37 119.64(19) . . ? C35 C36 H36 120.2 . . ? C37 C36 H36 120.2 . . ? C36 C37 C38 120.6(2) . . ? C36 C37 H37 119.7 . . ? C38 C37 H37 119.7 . . ? C37 C38 C33 120.05(19) . . ? C37 C38 H38 120.0 . . ? C33 C38 H38 120.0 . . ? Cl41 C40 Cl42 110.95(14) . . ? Cl41 C40 H40A 109.4 . . ? Cl42 C40 H40A 109.4 . . ? Cl41 C40 H40B 109.4 . . ? Cl42 C40 H40B 109.4 . . ? H40A C40 H40B 108.0 . . ? C9 N2 C1 119.85(14) . . ? C9 N2 Pd1 120.94(11) . . ? C1 N2 Pd1 119.17(12) . . ? C5 O3 C17 116.72(18) . . ? C6 O4 C18 117.47(17) . . ? C13 O5 C19 116.36(14) . . ? C14 O6 C20 116.86(14) . . ? C33 P1 C27 104.19(8) . . ? C33 P1 C21 104.59(8) . . ? C27 P1 C21 102.51(8) . . ? C33 P1 Pd1 114.81(6) . . ? C27 P1 Pd1 111.81(6) . . ? C21 P1 Pd1 117.41(6) . . ? C16 Pd1 N2 85.26(6) . . ? C16 Pd1 O1 170.22(6) . . ? N2 Pd1 O1 84.98(5) . . ? C16 Pd1 P1 93.66(5) . . ? N2 Pd1 P1 175.24(4) . . ? O1 Pd1 P1 96.12(4) . . ? N1 O1 Pd1 118.97(12) . . ? O2 N1 O1 116.40(17) . . ? 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 N2 C1 C2 C3 2.2(3) . . . . ? C1 C2 C3 C4 -178.29(17) . . . . ? C1 C2 C3 C8 -0.1(3) . . . . ? C2 C3 C4 C5 -179.10(18) . . . . ? C8 C3 C4 C5 2.8(3) . . . . ? C3 C4 C5 O3 179.55(19) . . . . ? C3 C4 C5 C6 0.7(3) . . . . ? O3 C5 C6 O4 -2.5(3) . . . . ? C4 C5 C6 O4 176.45(19) . . . . ? O3 C5 C6 C7 177.40(19) . . . . ? C4 C5 C6 C7 -3.6(3) . . . . ? O4 C6 C7 C8 -177.13(18) . . . . ? C5 C6 C7 C8 3.0(3) . . . . ? C2 C3 C8 C9 -2.7(2) . . . . ? C4 C3 C8 C9 175.49(16) . . . . ? C2 C3 C8 C7 178.45(16) . . . . ? C4 C3 C8 C7 -3.4(2) . . . . ? C6 C7 C8 C9 -178.31(17) . . . . ? C6 C7 C8 C3 0.5(3) . . . . ? C3 C8 C9 N2 3.8(2) . . . . ? C7 C8 C9 N2 -177.41(16) . . . . ? C3 C8 C9 C10 -173.06(15) . . . . ? C7 C8 C9 C10 5.7(3) . . . . ? N2 C9 C10 C11 -55.97(18) . . . . ? C8 C9 C10 C11 121.08(17) . . . . ? C9 C10 C11 C16 66.54(19) . . . . ? C9 C10 C11 C12 -105.83(17) . . . . ? C16 C11 C12 C13 -1.0(2) . . . . ? C10 C11 C12 C13 171.32(15) . . . . ? C11 C12 C13 O5 -176.84(16) . . . . ? C11 C12 C13 C14 1.8(2) . . . . ? O5 C13 C14 O6 -1.1(2) . . . . ? C12 C13 C14 O6 -179.90(15) . . . . ? O5 C13 C14 C15 177.82(15) . . . . ? C12 C13 C14 C15 -1.0(3) . . . . ? O6 C14 C15 C16 178.11(16) . . . . ? C13 C14 C15 C16 -0.7(3) . . . . ? C12 C11 C16 C15 -0.7(2) . . . . ? C10 C11 C16 C15 -172.89(15) . . . . ? C12 C11 C16 Pd1 166.72(12) . . . . ? C10 C11 C16 Pd1 -5.5(2) . . . . ? C14 C15 C16 C11 1.5(2) . . . . ? C14 C15 C16 Pd1 -164.99(13) . . . . ? C26 C21 C22 C23 -0.3(3) . . . . ? P1 C21 C22 C23 178.57(17) . . . . ? C21 C22 C23 C24 -0.6(3) . . . . ? C22 C23 C24 C25 0.6(3) . . . . ? C23 C24 C25 C26 0.3(3) . . . . ? C24 C25 C26 C21 -1.2(3) . . . . ? C22 C21 C26 C25 1.2(3) . . . . ? P1 C21 C26 C25 -177.69(14) . . . . ? C32 C27 C28 C29 1.2(3) . . . . ? P1 C27 C28 C29 -177.06(15) . . . . ? C27 C28 C29 C30 -1.7(3) . . . . ? C28 C29 C30 C31 0.7(3) . . . . ? C29 C30 C31 C32 1.0(4) . . . . ? C28 C27 C32 C31 0.5(3) . . . . ? P1 C27 C32 C31 178.60(16) . . . . ? C30 C31 C32 C27 -1.5(3) . . . . ? C38 C33 C34 C35 -1.1(3) . . . . ? P1 C33 C34 C35 177.54(16) . . . . ? C33 C34 C35 C36 -0.9(3) . . . . ? C34 C35 C36 C37 1.9(3) . . . . ? C35 C36 C37 C38 -0.9(3) . . . . ? C36 C37 C38 C33 -1.1(3) . . . . ? C34 C33 C38 C37 2.1(3) . . . . ? P1 C33 C38 C37 -176.59(15) . . . . ? C8 C9 N2 C1 -1.9(2) . . . . ? C10 C9 N2 C1 175.23(14) . . . . ? C8 C9 N2 Pd1 175.89(11) . . . . ? C10 C9 N2 Pd1 -6.99(19) . . . . ? C2 C1 N2 C9 -1.2(3) . . . . ? C2 C1 N2 Pd1 -178.99(14) . . . . ? C4 C5 O3 C17 0.1(4) . . . . ? C6 C5 O3 C17 179.0(2) . . . . ? C7 C6 O4 C18 3.8(3) . . . . ? C5 C6 O4 C18 -176.3(2) . . . . ? C12 C13 O5 C19 2.6(2) . . . . ? C14 C13 O5 C19 -176.10(16) . . . . ? C15 C14 O6 C20 -4.4(3) . . . . ? C13 C14 O6 C20 174.51(16) . . . . ? C34 C33 P1 C27 101.71(16) . . . . ? C38 C33 P1 C27 -79.65(15) . . . . ? C34 C33 P1 C21 -5.55(17) . . . . ? C38 C33 P1 C21 173.09(14) . . . . ? C34 C33 P1 Pd1 -135.68(14) . . . . ? C38 C33 P1 Pd1 42.97(15) . . . . ? C32 C27 P1 C33 -4.80(17) . . . . ? C28 C27 P1 C33 173.37(14) . . . . ? C32 C27 P1 C21 104.00(16) . . . . ? C28 C27 P1 C21 -77.83(15) . . . . ? C32 C27 P1 Pd1 -129.37(14) . . . . ? C28 C27 P1 Pd1 48.80(15) . . . . ? C22 C21 P1 C33 -108.79(17) . . . . ? C26 C21 P1 C33 70.04(16) . . . . ? C22 C21 P1 C27 142.71(16) . . . . ? C26 C21 P1 C27 -38.46(16) . . . . ? C22 C21 P1 Pd1 19.78(18) . . . . ? C26 C21 P1 Pd1 -161.39(13) . . . . ? C11 C16 Pd1 N2 -41.15(13) . . . . ? C15 C16 Pd1 N2 125.59(14) . . . . ? C11 C16 Pd1 O1 -44.3(4) . . . . ? C15 C16 Pd1 O1 122.5(3) . . . . ? C11 C16 Pd1 P1 134.20(12) . . . . ? C15 C16 Pd1 P1 -59.06(14) . . . . ? C9 N2 Pd1 C16 50.71(13) . . . . ? C1 N2 Pd1 C16 -131.49(14) . . . . ? C9 N2 Pd1 O1 -129.82(13) . . . . ? C1 N2 Pd1 O1 47.98(13) . . . . ? C9 N2 Pd1 P1 -26.3(6) . . . . ? C1 N2 Pd1 P1 151.5(4) . . . . ? C33 P1 Pd1 C16 63.74(8) . . . . ? C27 P1 Pd1 C16 -177.85(8) . . . . ? C21 P1 Pd1 C16 -59.79(8) . . . . ? C33 P1 Pd1 N2 140.4(5) . . . . ? C27 P1 Pd1 N2 -101.2(5) . . . . ? C21 P1 Pd1 N2 16.9(5) . . . . ? C33 P1 Pd1 O1 -116.53(7) . . . . ? C27 P1 Pd1 O1 1.89(8) . . . . ? C21 P1 Pd1 O1 119.94(8) . . . . ? C16 Pd1 O1 N1 -108.8(4) . . . . ? N2 Pd1 O1 N1 -111.88(13) . . . . ? P1 Pd1 O1 N1 72.78(13) . . . . ? Pd1 O1 N1 O2 -1.5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 29.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.803 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.072 ### END data_8_VT200K _database_code_depnum_ccdc_archive 'CCDC 858651' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Nitro-(1-(3,4-dimethoxybenzyl)-6,7-dimethoxyisoquinoline)(triphenylphosphine) palladium(II) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H37 Cl2 N2 O6 P Pd' _chemical_formula_sum 'C39 H37 Cl2 N2 O6 P Pd' _chemical_formula_weight 837.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.7245(5) _cell_length_b 21.8948(15) _cell_length_c 16.3488(8) _cell_angle_alpha 90.00 _cell_angle_beta 105.251(5) _cell_angle_gamma 90.00 _cell_volume 3703.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 190(2) _cell_measurement_reflns_used 11256 _cell_measurement_theta_min 1.5423 _cell_measurement_theta_max 29.4767 _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 0.738 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.81204 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ? _diffrn_ambient_temperature 190(2) _diffrn_radiation_wavelength 0.68890 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator synchrotron _diffrn_measurement_device ; CrystalLogic Kappa (3 circle) ; _diffrn_measurement_device_type ; Rigaku Saturn724+ (2x2 bin mode) ; _diffrn_measurement_method '1.0 degree images with \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41224 _diffrn_reflns_av_R_equivalents 0.0526 _diffrn_reflns_av_sigmaI/netI 0.1338 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.5423 _diffrn_reflns_theta_max 29.4767 _diffrn_orient_matrix_UB_11 0.0037677000 _diffrn_orient_matrix_UB_12 -0.0101450000 _diffrn_orient_matrix_UB_13 0.0404480000 _diffrn_orient_matrix_UB_21 0.0552871000 _diffrn_orient_matrix_UB_22 -0.0160578000 _diffrn_orient_matrix_UB_23 0.0001142000 _diffrn_orient_matrix_UB_31 0.0369836000 _diffrn_orient_matrix_UB_32 0.0250789000 _diffrn_orient_matrix_UB_33 0.0164366000 _reflns_number_total 11279 _reflns_number_gt 9129 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009) ; _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-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics WINGX _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0509P)^2^+2.6267P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11279 _refine_ls_number_parameters 477 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0546 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.1092 _refine_ls_wR_factor_gt 0.1001 _refine_ls_goodness_of_fit_ref 0.949 _refine_ls_restrained_S_all 0.949 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.1613(2) 0.18837(12) 0.78958(15) 0.0368(5) Uani 1 1 d . . . H1 H 1.1562 0.1564 0.8279 0.044 Uiso 1 1 calc R . . C2 C 1.2772(2) 0.21675(12) 0.79751(15) 0.0375(5) Uani 1 1 d . . . H2 H 1.3518 0.2038 0.8395 0.045 Uiso 1 1 calc R . . C3 C 1.2851(2) 0.26531(11) 0.74287(14) 0.0339(5) Uani 1 1 d . . . C4 C 1.4038(2) 0.29537(13) 0.74707(17) 0.0411(5) Uani 1 1 d . . . H4 H 1.4804 0.2825 0.7873 0.049 Uiso 1 1 calc R . . C5 C 1.4088(2) 0.34250(13) 0.69381(19) 0.0465(6) Uani 1 1 d . . . C6 C 1.2940(2) 0.36342(13) 0.63395(17) 0.0439(6) Uani 1 1 d . . . C7 C 1.1785(2) 0.33345(11) 0.62626(15) 0.0368(5) Uani 1 1 d . . . H7 H 1.1034 0.3463 0.5847 0.044 Uiso 1 1 calc R . . C8 C 1.1714(2) 0.28339(10) 0.68036(13) 0.0308(4) Uani 1 1 d . . . C9 C 1.0560(2) 0.24941(10) 0.67464(13) 0.0299(4) Uani 1 1 d . . . C10 C 0.9320(2) 0.25909(10) 0.60572(14) 0.0308(4) Uani 1 1 d . . . H10A H 0.9444 0.2914 0.5662 0.037 Uiso 1 1 calc R . . H10B H 0.8620 0.2720 0.6311 0.037 Uiso 1 1 calc R . . C11 C 0.89628(19) 0.19941(10) 0.55842(13) 0.0289(4) Uani 1 1 d . . . C12 C 0.9148(2) 0.19348(10) 0.47720(13) 0.0303(4) Uani 1 1 d . . . H12 H 0.9379 0.2282 0.4496 0.036 Uiso 1 1 calc R . . C13 C 0.8996(2) 0.13727(11) 0.43677(13) 0.0313(4) Uani 1 1 d . . . C14 C 0.8629(2) 0.08644(10) 0.47729(14) 0.0325(4) Uani 1 1 d . . . C15 C 0.8431(2) 0.09258(11) 0.55750(14) 0.0326(4) Uani 1 1 d . . . H15 H 0.8169 0.0581 0.5842 0.039 Uiso 1 1 calc R . . C16 C 0.8612(2) 0.14910(10) 0.59970(14) 0.0301(4) Uani 1 1 d . A . C17 C 1.6338(3) 0.3569(2) 0.7519(3) 0.1021(17) Uani 1 1 d . . . H17A H 1.6246 0.3615 0.8096 0.153 Uiso 1 1 calc R . . H17B H 1.7048 0.3827 0.7448 0.153 Uiso 1 1 calc R . . H17C H 1.6527 0.3141 0.7421 0.153 Uiso 1 1 calc R . . C18 C 1.2010(4) 0.4388(2) 0.5316(3) 0.0969(17) Uani 1 1 d . . . H18A H 1.1620 0.4088 0.4878 0.145 Uiso 1 1 calc R . . H18B H 1.2266 0.4751 0.5049 0.145 Uiso 1 1 calc R . . H18C H 1.1380 0.4504 0.5627 0.145 Uiso 1 1 calc R . . C19 C 0.9666(3) 0.17588(12) 0.31947(16) 0.0415(5) Uani 1 1 d . . . H19A H 0.9040 0.2094 0.3111 0.062 Uiso 1 1 calc R . . H19B H 0.9773 0.1628 0.2644 0.062 Uiso 1 1 calc R . . H19C H 1.0499 0.1898 0.3555 0.062 Uiso 1 1 calc R . . C20 C 0.8230(3) -0.02070(12) 0.47312(19) 0.0471(6) Uani 1 1 d . . . H20A H 0.8907 -0.0270 0.5259 0.071 Uiso 1 1 calc R . . H20B H 0.8202 -0.0559 0.4357 0.071 Uiso 1 1 calc R . . H20C H 0.7393 -0.0162 0.4860 0.071 Uiso 1 1 calc R . . C21 C 0.5384(2) 0.15388(10) 0.64370(14) 0.0317(4) Uani 1 1 d . . . C22 C 0.5508(2) 0.19287(13) 0.58003(18) 0.0464(6) Uani 1 1 d . . . H22 H 0.6341 0.2015 0.5728 0.056 Uiso 1 1 calc R . . C23 C 0.4416(3) 0.21981(15) 0.5260(2) 0.0561(8) Uani 1 1 d . . . H23 H 0.4513 0.2469 0.4828 0.067 Uiso 1 1 calc R . . C24 C 0.3196(2) 0.20726(13) 0.53514(17) 0.0456(6) Uani 1 1 d . . . H24 H 0.2456 0.2255 0.4981 0.055 Uiso 1 1 calc R . . C25 C 0.3061(2) 0.16848(12) 0.59772(17) 0.0402(5) Uani 1 1 d . . . H25 H 0.2224 0.1593 0.6038 0.048 Uiso 1 1 calc R . . C26 C 0.4144(2) 0.14244(11) 0.65243(16) 0.0373(5) Uani 1 1 d . . . H26 H 0.4040 0.1164 0.6966 0.045 Uiso 1 1 calc R . . C27 C 0.6390(2) 0.11770(12) 0.81597(14) 0.0345(5) Uani 1 1 d . . . C28 C 0.6557(3) 0.17231(14) 0.86131(18) 0.0454(6) Uani 1 1 d . . . H28 H 0.6837 0.2078 0.8378 0.054 Uiso 1 1 calc R . . C29 C 0.6317(3) 0.17521(18) 0.94095(19) 0.0588(8) Uani 1 1 d . . . H29 H 0.6454 0.2123 0.9723 0.071 Uiso 1 1 calc R . . C30 C 0.5878(3) 0.1239(2) 0.9742(2) 0.0703(11) Uani 1 1 d . . . H30 H 0.5707 0.1258 1.0283 0.084 Uiso 1 1 calc R . . C31 C 0.5690(3) 0.07016(19) 0.9291(2) 0.0676(10) Uani 1 1 d . . . H31 H 0.5372 0.0354 0.9519 0.081 Uiso 1 1 calc R . . C32 C 0.5959(3) 0.06607(14) 0.85004(18) 0.0483(6) Uani 1 1 d . . . H32 H 0.5849 0.0285 0.8200 0.058 Uiso 1 1 calc R . . C33 C 0.6646(2) 0.03669(11) 0.68214(14) 0.0334(4) Uani 1 1 d . . . C34 C 0.5590(3) 0.01307(13) 0.62239(18) 0.0459(6) Uani 1 1 d . . . H34 H 0.4877 0.0387 0.5974 0.055 Uiso 1 1 calc R . . C35 C 0.5570(3) -0.04803(14) 0.5989(2) 0.0557(7) Uani 1 1 d . . . H35 H 0.4840 -0.0639 0.5582 0.067 Uiso 1 1 calc R . . C36 C 0.6591(3) -0.08542(13) 0.6338(2) 0.0553(7) Uani 1 1 d . . . H36 H 0.6582 -0.1269 0.6165 0.066 Uiso 1 1 calc R . . C37 C 0.7635(3) -0.06251(14) 0.6943(2) 0.0558(7) Uani 1 1 d . . . H37 H 0.8342 -0.0885 0.7189 0.067 Uiso 1 1 calc R . . C38 C 0.7665(3) -0.00227(12) 0.71945(18) 0.0443(6) Uani 1 1 d . . . H38 H 0.8380 0.0127 0.7622 0.053 Uiso 1 1 calc R . . C40 C 1.1197(3) -0.00356(17) 0.7675(2) 0.0653(9) Uani 1 1 d . . . H40A H 1.0987 -0.0251 0.7124 0.078 Uiso 1 1 calc R . . H40B H 1.0563 0.0299 0.7638 0.078 Uiso 1 1 calc R . . N2 N 1.05245(17) 0.20416(9) 0.72869(12) 0.0325(4) Uani 1 1 d . A . O3 O 1.51587(19) 0.37483(12) 0.69212(16) 0.0714(7) Uani 1 1 d . . . O4 O 1.3120(2) 0.41270(11) 0.58879(15) 0.0637(6) Uani 1 1 d . . . O5 O 0.92088(17) 0.12611(8) 0.35916(10) 0.0383(4) Uani 1 1 d . . . O6 O 0.85060(18) 0.03291(8) 0.43236(11) 0.0420(4) Uani 1 1 d . . . P1 P 0.67901(5) 0.11672(3) 0.71410(4) 0.02970(12) Uani 1 1 d . A . Cl41 Cl 1.27473(10) 0.02714(5) 0.78752(9) 0.0951(4) Uani 1 1 d . . . Cl42 Cl 1.10712(10) -0.05467(5) 0.84758(6) 0.0770(3) Uani 1 1 d . . . Pd1 Pd 0.876643(15) 0.158152(8) 0.723953(10) 0.03076(6) Uani 1 1 d . . . O1 O 0.9214(3) 0.17818(15) 0.85712(17) 0.0359(9) Uani 0.762(10) 1 d P A 1 O2 O 0.9483(4) 0.08293(19) 0.8773(3) 0.0515(10) Uani 0.762(10) 1 d P A 1 N1 N 0.9509(3) 0.1346(2) 0.9086(2) 0.0433(10) Uani 0.762(10) 1 d P A 1 O1A O 0.9690(13) 0.1736(7) 0.9053(10) 0.068(4) Uiso 0.238(10) 1 d P A 2 N1A N 0.9438(10) 0.1431(7) 0.8636(8) 0.039(3) Uiso 0.238(10) 1 d P A 2 O2A O 0.951(4) 0.0869(19) 0.874(3) 0.174(14) Uiso 0.238(10) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0337(10) 0.0442(14) 0.0312(11) 0.0013(9) 0.0064(9) -0.0013(10) C2 0.0276(10) 0.0474(14) 0.0340(11) -0.0031(10) 0.0018(8) 0.0010(9) C3 0.0265(9) 0.0402(12) 0.0347(11) -0.0082(9) 0.0074(8) -0.0022(9) C4 0.0261(10) 0.0499(15) 0.0447(13) -0.0058(11) 0.0048(9) -0.0043(10) C5 0.0310(11) 0.0564(17) 0.0503(15) -0.0027(12) 0.0072(11) -0.0131(11) C6 0.0373(12) 0.0480(15) 0.0442(14) 0.0004(11) 0.0069(10) -0.0108(11) C7 0.0303(10) 0.0420(13) 0.0357(11) -0.0053(9) 0.0045(9) -0.0055(9) C8 0.0267(9) 0.0347(11) 0.0308(10) -0.0083(8) 0.0073(8) -0.0024(8) C9 0.0262(9) 0.0340(11) 0.0295(10) -0.0080(8) 0.0074(8) -0.0003(8) C10 0.0252(9) 0.0336(11) 0.0324(10) -0.0051(8) 0.0057(8) -0.0017(8) C11 0.0246(9) 0.0318(11) 0.0293(10) -0.0030(8) 0.0055(7) -0.0021(8) C12 0.0286(9) 0.0321(11) 0.0290(10) 0.0010(8) 0.0052(8) -0.0027(8) C13 0.0319(10) 0.0353(11) 0.0274(10) -0.0007(8) 0.0089(8) -0.0024(9) C14 0.0331(10) 0.0307(11) 0.0338(11) -0.0035(8) 0.0087(8) -0.0034(8) C15 0.0321(10) 0.0345(12) 0.0324(10) -0.0001(8) 0.0107(8) -0.0044(9) C16 0.0267(9) 0.0356(12) 0.0285(10) -0.0027(8) 0.0083(8) -0.0020(8) C17 0.0330(16) 0.135(4) 0.122(4) 0.044(3) -0.0078(19) -0.031(2) C18 0.070(2) 0.099(3) 0.095(3) 0.053(3) -0.023(2) -0.039(2) C19 0.0532(14) 0.0413(13) 0.0342(12) -0.0006(10) 0.0189(11) -0.0067(11) C20 0.0543(15) 0.0324(13) 0.0588(16) -0.0090(11) 0.0221(13) -0.0122(11) C21 0.0289(10) 0.0328(11) 0.0321(10) -0.0015(8) 0.0057(8) -0.0012(8) C22 0.0317(11) 0.0563(17) 0.0488(15) 0.0165(12) 0.0061(10) -0.0017(11) C23 0.0440(14) 0.065(2) 0.0559(17) 0.0256(14) 0.0067(13) 0.0024(13) C24 0.0354(12) 0.0480(15) 0.0465(14) 0.0009(11) -0.0014(10) 0.0054(11) C25 0.0301(10) 0.0403(13) 0.0485(14) -0.0093(10) 0.0074(10) 0.0010(9) C26 0.0336(11) 0.0354(12) 0.0444(13) 0.0007(10) 0.0127(10) 0.0012(9) C27 0.0267(9) 0.0474(14) 0.0292(10) 0.0030(9) 0.0068(8) 0.0036(9) C28 0.0370(12) 0.0566(16) 0.0434(14) -0.0066(12) 0.0120(10) 0.0061(11) C29 0.0432(14) 0.090(2) 0.0429(15) -0.0175(15) 0.0116(12) 0.0143(15) C30 0.0580(18) 0.119(3) 0.0367(15) 0.0040(18) 0.0184(14) 0.026(2) C31 0.069(2) 0.090(3) 0.0532(18) 0.0271(18) 0.0316(16) 0.0113(19) C32 0.0482(14) 0.0579(17) 0.0432(14) 0.0115(12) 0.0197(12) 0.0035(12) C33 0.0369(11) 0.0315(11) 0.0339(11) 0.0022(8) 0.0132(9) -0.0021(9) C34 0.0443(13) 0.0402(14) 0.0491(15) -0.0022(11) 0.0053(11) -0.0035(11) C35 0.0671(19) 0.0422(16) 0.0547(17) -0.0077(13) 0.0105(14) -0.0118(14) C36 0.080(2) 0.0351(14) 0.0552(17) -0.0006(12) 0.0261(16) -0.0028(14) C37 0.0651(18) 0.0405(15) 0.0649(19) 0.0101(13) 0.0225(15) 0.0132(14) C38 0.0439(13) 0.0389(14) 0.0503(15) 0.0043(11) 0.0128(11) 0.0040(11) C40 0.0571(18) 0.063(2) 0.079(2) -0.0151(17) 0.0248(17) -0.0013(15) N2 0.0281(8) 0.0392(11) 0.0298(9) -0.0037(7) 0.0070(7) -0.0010(7) O3 0.0348(10) 0.0900(18) 0.0820(17) 0.0196(13) 0.0023(10) -0.0260(11) O4 0.0509(11) 0.0686(14) 0.0630(13) 0.0173(11) -0.0004(10) -0.0270(10) O5 0.0509(10) 0.0364(9) 0.0311(8) -0.0041(6) 0.0168(7) -0.0068(7) O6 0.0556(10) 0.0330(9) 0.0411(9) -0.0083(7) 0.0194(8) -0.0097(8) P1 0.0270(2) 0.0329(3) 0.0295(3) 0.0016(2) 0.0079(2) -0.0007(2) Cl41 0.0690(6) 0.0842(7) 0.1391(11) -0.0127(7) 0.0399(6) -0.0199(5) Cl42 0.0879(6) 0.0764(6) 0.0729(6) -0.0177(5) 0.0323(5) -0.0161(5) Pd1 0.02731(8) 0.03804(11) 0.02714(9) -0.00183(6) 0.00754(6) -0.00370(6) O1 0.0382(13) 0.0408(18) 0.0297(14) -0.0056(10) 0.0106(10) -0.0030(10) O2 0.0619(18) 0.0375(15) 0.0418(15) 0.0040(10) -0.0099(12) 0.0090(12) N1 0.0373(14) 0.048(2) 0.0398(19) -0.0080(14) 0.0020(12) 0.0034(13) _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 C1 C2 1.365(3) . ? C1 N2 1.364(3) . ? C1 H1 0.9500 . ? C2 C3 1.406(3) . ? C2 H2 0.9500 . ? C3 C4 1.419(3) . ? C3 C8 1.426(3) . ? C4 C5 1.360(4) . ? C4 H4 0.9500 . ? C5 O3 1.356(3) . ? C5 C6 1.431(4) . ? C6 O4 1.350(3) . ? C6 C7 1.378(3) . ? C7 C8 1.423(3) . ? C7 H7 0.9500 . ? C8 C9 1.426(3) . ? C9 N2 1.335(3) . ? C9 C10 1.515(3) . ? C10 C11 1.515(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C16 1.394(3) . ? C11 C12 1.399(3) . ? C12 C13 1.386(3) . ? C12 H12 0.9500 . ? C13 O5 1.369(3) . ? C13 C14 1.404(3) . ? C14 O6 1.371(3) . ? C14 C15 1.389(3) . ? C15 C16 1.405(3) . ? C15 H15 0.9500 . ? C16 Pd1 2.004(2) . ? C17 O3 1.435(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 O4 1.426(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 O5 1.420(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 O6 1.419(3) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.379(3) . ? C21 C26 1.397(3) . ? C21 P1 1.830(2) . ? C22 C23 1.398(4) . ? C22 H22 0.9500 . ? C23 C24 1.383(4) . ? C23 H23 0.9500 . ? C24 C25 1.366(4) . ? C24 H24 0.9500 . ? C25 C26 1.388(3) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C32 1.392(4) . ? C27 C28 1.393(4) . ? C27 P1 1.826(2) . ? C28 C29 1.394(4) . ? C28 H28 0.9500 . ? C29 C30 1.383(6) . ? C29 H29 0.9500 . ? C30 C31 1.375(6) . ? C30 H30 0.9500 . ? C31 C32 1.399(4) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.386(3) . ? C33 C38 1.394(3) . ? C33 P1 1.823(2) . ? C34 C35 1.390(4) . ? C34 H34 0.9500 . ? C35 C36 1.366(5) . ? C35 H35 0.9500 . ? C36 C37 1.378(5) . ? C36 H36 0.9500 . ? C37 C38 1.380(4) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C40 Cl41 1.743(3) . ? C40 Cl42 1.754(4) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? N2 Pd1 2.1210(18) . ? P1 Pd1 2.2719(6) . ? Pd1 O1 2.148(3) . ? Pd1 N1A 2.231(13) . ? O1 N1 1.256(7) . ? O2 N1 1.239(6) . ? O1A N1A 0.94(2) . ? N1A O2A 1.24(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 N2 122.5(2) . . ? C2 C1 H1 118.8 . . ? N2 C1 H1 118.8 . . ? C1 C2 C3 119.3(2) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C2 C3 C4 121.6(2) . . ? C2 C3 C8 118.8(2) . . ? C4 C3 C8 119.6(2) . . ? C5 C4 C3 120.4(2) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? O3 C5 C4 125.8(3) . . ? O3 C5 C6 113.6(2) . . ? C4 C5 C6 120.6(2) . . ? O4 C6 C7 125.8(2) . . ? O4 C6 C5 114.1(2) . . ? C7 C6 C5 120.0(2) . . ? C6 C7 C8 120.3(2) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C7 C8 C9 123.3(2) . . ? C7 C8 C3 118.9(2) . . ? C9 C8 C3 117.8(2) . . ? N2 C9 C8 121.3(2) . . ? N2 C9 C10 115.07(18) . . ? C8 C9 C10 123.6(2) . . ? C9 C10 C11 108.27(18) . . ? C9 C10 H10A 110.0 . . ? C11 C10 H10A 110.0 . . ? C9 C10 H10B 110.0 . . ? C11 C10 H10B 110.0 . . ? H10A C10 H10B 108.4 . . ? C16 C11 C12 120.6(2) . . ? C16 C11 C10 119.89(19) . . ? C12 C11 C10 118.97(19) . . ? C13 C12 C11 120.4(2) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? O5 C13 C12 125.0(2) . . ? O5 C13 C14 115.6(2) . . ? C12 C13 C14 119.42(19) . . ? O6 C14 C15 124.9(2) . . ? O6 C14 C13 115.10(19) . . ? C15 C14 C13 120.0(2) . . ? C14 C15 C16 120.9(2) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C11 C16 C15 118.58(19) . . ? C11 C16 Pd1 116.86(16) . . ? C15 C16 Pd1 123.27(16) . . ? O3 C17 H17A 109.5 . . ? O3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O4 C18 H18A 109.5 . . ? O4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O5 C19 H19A 109.5 . . ? O5 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O5 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O6 C20 H20A 109.5 . . ? O6 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O6 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C26 118.1(2) . . ? C22 C21 P1 121.51(18) . . ? C26 C21 P1 120.35(18) . . ? C21 C22 C23 120.4(2) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C24 C23 C22 120.5(3) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C25 C24 C23 119.6(2) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C24 C25 C26 120.1(2) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C25 C26 C21 121.2(2) . . ? C25 C26 H26 119.4 . . ? C21 C26 H26 119.4 . . ? C32 C27 C28 119.6(2) . . ? C32 C27 P1 122.5(2) . . ? C28 C27 P1 117.83(19) . . ? C29 C28 C27 120.4(3) . . ? C29 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? C30 C29 C28 119.7(3) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? C31 C30 C29 120.1(3) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C30 C31 C32 120.9(3) . . ? C30 C31 H31 119.6 . . ? C32 C31 H31 119.6 . . ? C27 C32 C31 119.2(3) . . ? C27 C32 H32 120.4 . . ? C31 C32 H32 120.4 . . ? C34 C33 C38 118.8(2) . . ? C34 C33 P1 123.54(19) . . ? C38 C33 P1 117.70(19) . . ? C33 C34 C35 120.3(3) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C36 C35 C34 120.6(3) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C35 C36 C37 119.5(3) . . ? C35 C36 H36 120.3 . . ? C37 C36 H36 120.3 . . ? C38 C37 C36 120.9(3) . . ? C38 C37 H37 119.6 . . ? C36 C37 H37 119.6 . . ? C37 C38 C33 120.0(3) . . ? C37 C38 H38 120.0 . . ? C33 C38 H38 120.0 . . ? Cl41 C40 Cl42 111.3(2) . . ? Cl41 C40 H40A 109.4 . . ? Cl42 C40 H40A 109.4 . . ? Cl41 C40 H40B 109.4 . . ? Cl42 C40 H40B 109.4 . . ? H40A C40 H40B 108.0 . . ? C9 N2 C1 120.21(19) . . ? C9 N2 Pd1 120.55(14) . . ? C1 N2 Pd1 119.20(16) . . ? C5 O3 C17 116.3(3) . . ? C6 O4 C18 117.7(2) . . ? C13 O5 C19 116.64(18) . . ? C14 O6 C20 117.27(19) . . ? C33 P1 C27 104.48(11) . . ? C33 P1 C21 104.66(11) . . ? C27 P1 C21 102.47(10) . . ? C33 P1 Pd1 114.29(7) . . ? C27 P1 Pd1 111.67(8) . . ? C21 P1 Pd1 117.80(7) . . ? C16 Pd1 N2 85.38(8) . . ? C16 Pd1 O1 169.91(9) . . ? N2 Pd1 O1 84.65(8) . . ? C16 Pd1 N1A 160.3(4) . . ? N2 Pd1 N1A 89.3(3) . . ? O1 Pd1 N1A 21.1(3) . . ? C16 Pd1 P1 93.56(6) . . ? N2 Pd1 P1 174.86(6) . . ? O1 Pd1 P1 96.24(6) . . ? N1A Pd1 P1 93.3(3) . . ? N1 O1 Pd1 118.3(3) . . ? O1 N1 O2 116.3(4) . . ? O1A N1A O2A 128(3) . . ? O1A N1A Pd1 126.2(16) . . ? O2A N1A Pd1 106(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 N2 C1 C2 C3 1.9(4) . . . . ? C1 C2 C3 C4 -178.5(2) . . . . ? C1 C2 C3 C8 -0.2(3) . . . . ? C2 C3 C4 C5 -179.6(2) . . . . ? C8 C3 C4 C5 2.2(4) . . . . ? C3 C4 C5 O3 179.6(3) . . . . ? C3 C4 C5 C6 1.4(4) . . . . ? O3 C5 C6 O4 -2.2(4) . . . . ? C4 C5 C6 O4 176.3(3) . . . . ? O3 C5 C6 C7 177.6(3) . . . . ? C4 C5 C6 C7 -4.0(4) . . . . ? O4 C6 C7 C8 -177.3(3) . . . . ? C5 C6 C7 C8 2.9(4) . . . . ? C6 C7 C8 C9 -178.5(2) . . . . ? C6 C7 C8 C3 0.6(3) . . . . ? C2 C3 C8 C7 178.6(2) . . . . ? C4 C3 C8 C7 -3.2(3) . . . . ? C2 C3 C8 C9 -2.3(3) . . . . ? C4 C3 C8 C9 176.0(2) . . . . ? C7 C8 C9 N2 -177.5(2) . . . . ? C3 C8 C9 N2 3.4(3) . . . . ? C7 C8 C9 C10 5.7(3) . . . . ? C3 C8 C9 C10 -173.42(19) . . . . ? N2 C9 C10 C11 -55.9(2) . . . . ? C8 C9 C10 C11 121.1(2) . . . . ? C9 C10 C11 C16 66.3(2) . . . . ? C9 C10 C11 C12 -105.7(2) . . . . ? C16 C11 C12 C13 -0.6(3) . . . . ? C10 C11 C12 C13 171.37(19) . . . . ? C11 C12 C13 O5 -177.0(2) . . . . ? C11 C12 C13 C14 1.3(3) . . . . ? O5 C13 C14 O6 -1.4(3) . . . . ? C12 C13 C14 O6 -179.9(2) . . . . ? O5 C13 C14 C15 177.9(2) . . . . ? C12 C13 C14 C15 -0.6(3) . . . . ? O6 C14 C15 C16 178.3(2) . . . . ? C13 C14 C15 C16 -1.0(3) . . . . ? C12 C11 C16 C15 -0.9(3) . . . . ? C10 C11 C16 C15 -172.80(19) . . . . ? C12 C11 C16 Pd1 166.49(16) . . . . ? C10 C11 C16 Pd1 -5.4(3) . . . . ? C14 C15 C16 C11 1.7(3) . . . . ? C14 C15 C16 Pd1 -164.87(17) . . . . ? C26 C21 C22 C23 -0.1(4) . . . . ? P1 C21 C22 C23 178.8(2) . . . . ? C21 C22 C23 C24 -0.7(5) . . . . ? C22 C23 C24 C25 0.3(5) . . . . ? C23 C24 C25 C26 0.8(4) . . . . ? C24 C25 C26 C21 -1.6(4) . . . . ? C22 C21 C26 C25 1.3(4) . . . . ? P1 C21 C26 C25 -177.68(19) . . . . ? C32 C27 C28 C29 1.1(4) . . . . ? P1 C27 C28 C29 -177.4(2) . . . . ? C27 C28 C29 C30 -1.6(4) . . . . ? C28 C29 C30 C31 0.5(5) . . . . ? C29 C30 C31 C32 1.2(5) . . . . ? C28 C27 C32 C31 0.6(4) . . . . ? P1 C27 C32 C31 179.1(2) . . . . ? C30 C31 C32 C27 -1.7(5) . . . . ? C38 C33 C34 C35 -1.6(4) . . . . ? P1 C33 C34 C35 177.5(2) . . . . ? C33 C34 C35 C36 -0.4(5) . . . . ? C34 C35 C36 C37 1.5(5) . . . . ? C35 C36 C37 C38 -0.5(5) . . . . ? C36 C37 C38 C33 -1.6(4) . . . . ? C34 C33 C38 C37 2.6(4) . . . . ? P1 C33 C38 C37 -176.6(2) . . . . ? C8 C9 N2 C1 -1.8(3) . . . . ? C10 C9 N2 C1 175.24(19) . . . . ? C8 C9 N2 Pd1 175.98(15) . . . . ? C10 C9 N2 Pd1 -7.0(2) . . . . ? C2 C1 N2 C9 -0.9(3) . . . . ? C2 C1 N2 Pd1 -178.73(18) . . . . ? C4 C5 O3 C17 0.4(5) . . . . ? C6 C5 O3 C17 178.8(4) . . . . ? C7 C6 O4 C18 4.1(5) . . . . ? C5 C6 O4 C18 -176.1(3) . . . . ? C12 C13 O5 C19 2.5(3) . . . . ? C14 C13 O5 C19 -175.9(2) . . . . ? C15 C14 O6 C20 -3.9(3) . . . . ? C13 C14 O6 C20 175.4(2) . . . . ? C34 C33 P1 C27 101.8(2) . . . . ? C38 C33 P1 C27 -79.1(2) . . . . ? C34 C33 P1 C21 -5.6(2) . . . . ? C38 C33 P1 C21 173.61(19) . . . . ? C34 C33 P1 Pd1 -135.89(19) . . . . ? C38 C33 P1 Pd1 43.3(2) . . . . ? C32 C27 P1 C33 -5.5(2) . . . . ? C28 C27 P1 C33 172.95(19) . . . . ? C32 C27 P1 C21 103.4(2) . . . . ? C28 C27 P1 C21 -78.1(2) . . . . ? C32 C27 P1 Pd1 -129.58(19) . . . . ? C28 C27 P1 Pd1 48.9(2) . . . . ? C22 C21 P1 C33 -108.7(2) . . . . ? C26 C21 P1 C33 70.2(2) . . . . ? C22 C21 P1 C27 142.5(2) . . . . ? C26 C21 P1 C27 -38.6(2) . . . . ? C22 C21 P1 Pd1 19.5(2) . . . . ? C26 C21 P1 Pd1 -161.55(17) . . . . ? C11 C16 Pd1 N2 -40.97(16) . . . . ? C15 C16 Pd1 N2 125.81(19) . . . . ? C11 C16 Pd1 O1 -32.3(7) . . . . ? C15 C16 Pd1 O1 134.5(6) . . . . ? C11 C16 Pd1 N1A -115.9(9) . . . . ? C15 C16 Pd1 N1A 50.9(9) . . . . ? C11 C16 Pd1 P1 133.98(16) . . . . ? C15 C16 Pd1 P1 -59.24(18) . . . . ? C9 N2 Pd1 C16 50.35(17) . . . . ? C1 N2 Pd1 C16 -131.84(18) . . . . ? C9 N2 Pd1 O1 -128.13(19) . . . . ? C1 N2 Pd1 O1 49.68(19) . . . . ? C9 N2 Pd1 N1A -148.7(4) . . . . ? C1 N2 Pd1 N1A 29.1(4) . . . . ? C9 N2 Pd1 P1 -27.9(7) . . . . ? C1 N2 Pd1 P1 149.9(5) . . . . ? C33 P1 Pd1 C16 64.68(10) . . . . ? C27 P1 Pd1 C16 -177.00(11) . . . . ? C21 P1 Pd1 C16 -58.82(11) . . . . ? C33 P1 Pd1 N2 142.6(6) . . . . ? C27 P1 Pd1 N2 -99.1(6) . . . . ? C21 P1 Pd1 N2 19.1(6) . . . . ? C33 P1 Pd1 O1 -117.72(13) . . . . ? C27 P1 Pd1 O1 0.61(13) . . . . ? C21 P1 Pd1 O1 118.79(13) . . . . ? C33 P1 Pd1 N1A -96.8(4) . . . . ? C27 P1 Pd1 N1A 21.5(4) . . . . ? C21 P1 Pd1 N1A 139.7(4) . . . . ? C16 Pd1 O1 N1 -119.7(6) . . . . ? N2 Pd1 O1 N1 -111.1(2) . . . . ? N1A Pd1 O1 N1 -8.9(8) . . . . ? P1 Pd1 O1 N1 74.0(2) . . . . ? Pd1 O1 N1 O2 -1.8(4) . . . . ? C16 Pd1 N1A O1A 131.3(13) . . . . ? N2 Pd1 N1A O1A 57.0(13) . . . . ? O1 Pd1 N1A O1A -19.7(10) . . . . ? P1 Pd1 N1A O1A -118.6(13) . . . . ? C16 Pd1 N1A O2A -43(2) . . . . ? N2 Pd1 N1A O2A -117(2) . . . . ? O1 Pd1 N1A O2A 166(2) . . . . ? P1 Pd1 N1A O2A 67(2) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 29.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.831 _refine_diff_density_min -0.613 _refine_diff_density_rms 0.077 ### END # Attachment '- 8_slowcool.cif' data_298K _database_code_depnum_ccdc_archive 'CCDC 858652' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Nitro-(1-(3,4-dimethoxybenzyl)-6,7-dimethoxyisoquinoline)(triphenylphosphine) palladium(II) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H37 Cl2 N2 O6 P Pd' _chemical_formula_sum 'C39 H37 Cl2 N2 O6 P Pd' _chemical_formula_weight 837.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.786(8) _cell_length_b 22.362(17) _cell_length_c 16.405(12) _cell_angle_alpha 90.00 _cell_angle_beta 104.945(9) _cell_angle_gamma 90.00 _cell_volume 3823(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 9888 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 30.33 _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.456 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 0.715 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9320 _exptl_absorpt_correction_T_max 0.9858 _exptl_absorpt_process_details ; SADABS V2008-1, Bruker AXS.: Madison, WI, USA, 2008 ; _exptl_special_details ? _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.7749 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator synchrotron _diffrn_measurement_device_type ? _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38082 _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_sigmaI/netI 0.0570 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 34.54 _reflns_number_total 11705 _reflns_number_gt 8664 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics WINGX _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0895P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11705 _refine_ls_number_parameters 477 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0618 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.1521 _refine_ls_wR_factor_gt 0.1399 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.1597(3) 0.18733(14) 0.71038(18) 0.0532(6) Uani 1 1 d . . . H1 H -0.1549 0.1564 0.6734 0.064 Uiso 1 1 calc R . . C2 C -0.2741(3) 0.21564(14) 0.70204(17) 0.0547(6) Uani 1 1 d . . . H2 H -0.3461 0.2034 0.6608 0.066 Uiso 1 1 calc R . . C3 C -0.2828(2) 0.26361(12) 0.75624(17) 0.0477(5) Uani 1 1 d . . . C4 C -0.4014(3) 0.29339(15) 0.7521(2) 0.0597(7) Uani 1 1 d . . . H4 H -0.4756 0.2812 0.7129 0.072 Uiso 1 1 calc R . . C5 C -0.4065(3) 0.33957(16) 0.8054(2) 0.0685(9) Uani 1 1 d . . . C6 C -0.2925(3) 0.35991(16) 0.8650(2) 0.0630(7) Uani 1 1 d . . . C7 C -0.1783(3) 0.33027(13) 0.87326(19) 0.0521(6) Uani 1 1 d . . . H7 H -0.1059 0.3423 0.9143 0.062 Uiso 1 1 calc R . . C8 C -0.1701(2) 0.28102(11) 0.81928(15) 0.0427(5) Uani 1 1 d . . . C9 C -0.0560(2) 0.24742(11) 0.82451(15) 0.0419(5) Uani 1 1 d . . . C10 C 0.0672(2) 0.25689(10) 0.89361(15) 0.0420(5) Uani 1 1 d . . . H10A H 0.0547 0.2879 0.9320 0.050 Uiso 1 1 calc R . . H10B H 0.1357 0.2694 0.8689 0.050 Uiso 1 1 calc R . . C11 C 0.1031(2) 0.19813(10) 0.94130(15) 0.0410(5) Uani 1 1 d . . . C12 C 0.0849(2) 0.19287(11) 1.02256(15) 0.0428(5) Uani 1 1 d . . . H12 H 0.0621 0.2263 1.0492 0.051 Uiso 1 1 calc R . . C13 C 0.1010(2) 0.13755(12) 1.06358(15) 0.0444(5) Uani 1 1 d . . . C14 C 0.1376(2) 0.08740(11) 1.02337(16) 0.0456(5) Uani 1 1 d . . . C15 C 0.1563(2) 0.09318(12) 0.94334(16) 0.0463(5) Uani 1 1 d . . . H15 H 0.1809 0.0599 0.9173 0.056 Uiso 1 1 calc R . . C16 C 0.1388(2) 0.14876(11) 0.90032(15) 0.0418(5) Uani 1 1 d . A . C17 C -0.6297(4) 0.3550(3) 0.7437(4) 0.152(3) Uani 1 1 d . . . H17A H -0.6186 0.3621 0.6883 0.228 Uiso 1 1 calc R . . H17B H -0.6999 0.3787 0.7517 0.228 Uiso 1 1 calc R . . H17C H -0.6478 0.3134 0.7496 0.228 Uiso 1 1 calc R . . C18 C -0.2017(5) 0.4345(2) 0.9667(3) 0.136(3) Uani 1 1 d . . . H18A H -0.1672 0.4072 1.0121 0.203 Uiso 1 1 calc R . . H18B H -0.2263 0.4710 0.9890 0.203 Uiso 1 1 calc R . . H18C H -0.1378 0.4429 0.9369 0.203 Uiso 1 1 calc R . . C19 C 0.0338(3) 0.17564(14) 1.1811(2) 0.0628(8) Uani 1 1 d . . . H19A H 0.0936 0.2082 1.1887 0.094 Uiso 1 1 calc R . . H19B H 0.0237 0.1631 1.2350 0.094 Uiso 1 1 calc R . . H19C H -0.0476 0.1884 1.1462 0.094 Uiso 1 1 calc R . . C20 C 0.1788(4) -0.01833(13) 1.0292(2) 0.0708(9) Uani 1 1 d . . . H20A H 0.1160 -0.0241 0.9764 0.106 Uiso 1 1 calc R . . H20B H 0.1778 -0.0520 1.0653 0.106 Uiso 1 1 calc R . . H20C H 0.2623 -0.0146 1.0192 0.106 Uiso 1 1 calc R . . C21 C 0.3621(2) 0.11768(13) 0.68440(16) 0.0512(6) Uani 1 1 d . . . C22 C 0.4033(3) 0.06743(17) 0.6495(2) 0.0719(9) Uani 1 1 d . . . H22 H 0.4121 0.0310 0.6779 0.086 Uiso 1 1 calc R . . C23 C 0.4316(5) 0.0721(3) 0.5703(3) 0.1008(15) Uani 1 1 d . . . H23 H 0.4623 0.0389 0.5474 0.121 Uiso 1 1 calc R . . C24 C 0.4142(4) 0.1251(3) 0.5272(3) 0.1101(19) Uani 1 1 d . . . H24 H 0.4316 0.1276 0.4746 0.132 Uiso 1 1 calc R . . C25 C 0.3713(4) 0.1745(2) 0.5611(2) 0.0874(12) Uani 1 1 d . . . H25 H 0.3591 0.2103 0.5314 0.105 Uiso 1 1 calc R . . C26 C 0.3461(3) 0.17131(17) 0.6392(2) 0.0655(8) Uani 1 1 d . . . H26 H 0.3180 0.2052 0.6620 0.079 Uiso 1 1 calc R . . C27 C 0.4604(3) 0.15229(10) 0.85644(17) 0.0453(5) Uani 1 1 d . . . C28 C 0.4486(3) 0.18986(15) 0.9209(2) 0.0662(8) Uani 1 1 d . . . H28 H 0.3679 0.1982 0.9284 0.079 Uiso 1 1 calc R . . C29 C 0.5574(3) 0.21532(18) 0.9746(2) 0.0824(11) Uani 1 1 d . . . H29 H 0.5480 0.2409 1.0174 0.099 Uiso 1 1 calc R . . C30 C 0.6782(3) 0.20338(15) 0.9656(2) 0.0658(8) Uani 1 1 d . . . H30 H 0.7500 0.2206 1.0020 0.079 Uiso 1 1 calc R . . C31 C 0.6915(3) 0.16598(13) 0.9026(2) 0.0587(7) Uani 1 1 d . . . H31 H 0.7730 0.1574 0.8964 0.070 Uiso 1 1 calc R . . C32 C 0.5841(3) 0.14050(13) 0.8474(2) 0.0538(6) Uani 1 1 d . . . H32 H 0.5945 0.1155 0.8043 0.065 Uiso 1 1 calc R . . C33 C 0.3324(3) 0.03696(11) 0.81667(17) 0.0477(5) Uani 1 1 d . . . C34 C 0.4355(3) 0.01311(14) 0.8754(2) 0.0654(8) Uani 1 1 d . . . H34 H 0.5056 0.0370 0.9003 0.079 Uiso 1 1 calc R . . C35 C 0.4342(4) -0.04736(16) 0.8977(3) 0.0827(11) Uani 1 1 d . . . H35 H 0.5040 -0.0632 0.9375 0.099 Uiso 1 1 calc R . . C36 C 0.3349(5) -0.08276(16) 0.8629(3) 0.0831(11) Uani 1 1 d . . . H36 H 0.3350 -0.1226 0.8792 0.100 Uiso 1 1 calc R . . C37 C 0.2322(4) -0.05990(15) 0.8026(3) 0.0835(11) Uani 1 1 d . . . H37 H 0.1632 -0.0845 0.7779 0.100 Uiso 1 1 calc R . . C38 C 0.2310(3) -0.00014(13) 0.7783(2) 0.0649(8) Uani 1 1 d . . . H38 H 0.1625 0.0148 0.7366 0.078 Uiso 1 1 calc R . . C40 C -0.1259(4) -0.0060(2) 0.7280(3) 0.0974(14) Uani 1 1 d . . . H40A H -0.1061 -0.0272 0.7813 0.117 Uiso 1 1 calc R . . H40B H -0.0620 0.0252 0.7318 0.117 Uiso 1 1 calc R . . N2 N -0.0518(2) 0.20271(10) 0.77104(13) 0.0456(4) Uani 1 1 d . A . O3 O -0.5124(2) 0.37139(16) 0.8069(2) 0.1071(11) Uani 1 1 d . . . O4 O -0.3113(3) 0.40822(13) 0.91021(18) 0.0924(9) Uani 1 1 d . . . O5 O 0.0807(2) 0.12705(8) 1.14179(12) 0.0556(5) Uani 1 1 d . . . O6 O 0.1493(2) 0.03493(8) 1.06883(13) 0.0623(5) Uani 1 1 d . . . P1 P 0.32023(6) 0.11632(3) 0.78565(4) 0.04194(14) Uani 1 1 d . A . Cl41 Cl -0.11652(16) -0.05549(7) 0.64783(9) 0.1237(5) Uani 1 1 d . . . Cl42 Cl -0.27402(16) 0.02623(8) 0.71164(14) 0.1529(7) Uani 1 1 d . . . Pd1 Pd 0.123609(17) 0.157304(9) 0.776016(11) 0.04240(8) Uani 1 1 d . . . N1 N 0.0496(4) 0.1366(2) 0.5907(3) 0.0702(13) Uani 0.760(8) 1 d P A 1 O1 O 0.0806(3) 0.17853(15) 0.6428(2) 0.0566(10) Uani 0.760(8) 1 d P A 1 O2 O 0.0492(8) 0.08559(19) 0.6205(4) 0.080(2) Uani 0.760(8) 1 d P A 1 O1A O 0.0315(11) 0.1783(5) 0.5899(8) 0.068(3) Uiso 0.240(8) 1 d PD A 2 O2A O 0.051(5) 0.0874(11) 0.625(3) 0.154(14) Uiso 0.240(8) 1 d PD A 2 N1A N 0.0613(9) 0.1401(5) 0.6410(7) 0.044(3) Uiso 0.240(8) 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0476(14) 0.0646(17) 0.0452(14) -0.0044(12) 0.0080(11) 0.0019(12) C2 0.0404(13) 0.0723(18) 0.0466(14) 0.0045(12) 0.0024(10) 0.0000(12) C3 0.0372(11) 0.0567(14) 0.0471(13) 0.0099(11) 0.0072(10) 0.0028(10) C4 0.0362(13) 0.0774(19) 0.0606(17) 0.0080(15) 0.0034(11) 0.0068(12) C5 0.0412(15) 0.087(2) 0.073(2) -0.0019(16) 0.0079(14) 0.0184(14) C6 0.0526(16) 0.0727(18) 0.0602(18) -0.0008(15) 0.0080(13) 0.0187(14) C7 0.0450(13) 0.0556(14) 0.0535(16) 0.0063(12) 0.0088(11) 0.0097(11) C8 0.0365(11) 0.0487(12) 0.0416(12) 0.0093(10) 0.0080(9) 0.0025(9) C9 0.0357(11) 0.0483(12) 0.0415(12) 0.0105(9) 0.0093(9) 0.0029(9) C10 0.0366(11) 0.0432(11) 0.0446(12) 0.0063(9) 0.0072(9) 0.0024(8) C11 0.0372(11) 0.0445(11) 0.0397(11) 0.0029(9) 0.0072(9) 0.0036(9) C12 0.0430(12) 0.0450(12) 0.0389(12) -0.0019(9) 0.0078(9) 0.0041(9) C13 0.0461(13) 0.0498(12) 0.0372(12) 0.0028(10) 0.0102(10) 0.0046(10) C14 0.0493(13) 0.0438(12) 0.0440(13) 0.0053(10) 0.0127(10) 0.0063(10) C15 0.0482(13) 0.0471(12) 0.0450(13) -0.0005(10) 0.0144(10) 0.0081(10) C16 0.0389(11) 0.0492(12) 0.0368(12) 0.0015(9) 0.0085(9) 0.0042(9) C17 0.046(2) 0.204(7) 0.179(6) -0.074(5) -0.017(3) 0.044(3) C18 0.102(4) 0.151(5) 0.118(4) -0.078(4) -0.035(3) 0.059(3) C19 0.081(2) 0.0628(16) 0.0526(16) 0.0011(13) 0.0307(15) 0.0115(15) C20 0.087(2) 0.0448(14) 0.086(2) 0.0097(15) 0.0314(19) 0.0161(14) C21 0.0420(13) 0.0700(17) 0.0415(13) -0.0064(12) 0.0106(10) -0.0049(11) C22 0.075(2) 0.086(2) 0.0596(19) -0.0183(17) 0.0271(16) -0.0031(17) C23 0.097(3) 0.145(4) 0.071(3) -0.037(3) 0.040(2) -0.013(3) C24 0.087(3) 0.199(6) 0.049(2) 0.000(3) 0.026(2) -0.048(3) C25 0.069(2) 0.136(4) 0.057(2) 0.020(2) 0.0172(17) -0.023(2) C26 0.0556(17) 0.086(2) 0.0547(17) 0.0073(15) 0.0139(14) -0.0132(15) C27 0.0415(12) 0.0459(12) 0.0462(13) 0.0000(10) 0.0072(10) 0.0011(9) C28 0.0476(15) 0.076(2) 0.071(2) -0.0258(16) 0.0084(14) 0.0027(14) C29 0.062(2) 0.097(3) 0.079(2) -0.040(2) 0.0019(17) -0.0002(18) C30 0.0514(16) 0.0680(18) 0.068(2) -0.0044(15) -0.0026(14) -0.0075(13) C31 0.0438(14) 0.0600(16) 0.0687(19) 0.0141(13) 0.0079(13) 0.0005(11) C32 0.0469(14) 0.0551(14) 0.0594(17) -0.0001(13) 0.0138(12) -0.0019(11) C33 0.0494(13) 0.0464(12) 0.0499(14) -0.0030(10) 0.0174(11) 0.0025(10) C34 0.0657(18) 0.0548(16) 0.070(2) 0.0028(14) 0.0069(15) 0.0075(13) C35 0.102(3) 0.0571(19) 0.084(3) 0.0081(17) 0.014(2) 0.0221(19) C36 0.120(3) 0.0489(17) 0.085(3) -0.0025(17) 0.034(2) 0.0046(19) C37 0.100(3) 0.0520(17) 0.100(3) -0.0126(18) 0.028(2) -0.0168(18) C38 0.0638(18) 0.0539(16) 0.076(2) -0.0080(14) 0.0155(15) -0.0052(14) C40 0.086(3) 0.097(3) 0.112(4) 0.022(2) 0.030(3) 0.002(2) N2 0.0386(10) 0.0570(12) 0.0400(10) 0.0034(9) 0.0081(8) 0.0051(8) O3 0.0489(13) 0.137(3) 0.122(2) -0.034(2) -0.0014(14) 0.0407(16) O4 0.0683(15) 0.108(2) 0.0885(18) -0.0318(16) -0.0020(13) 0.0395(14) O5 0.0769(13) 0.0516(10) 0.0422(10) 0.0049(8) 0.0221(9) 0.0107(9) O6 0.0888(15) 0.0474(10) 0.0561(12) 0.0120(9) 0.0282(11) 0.0161(10) P1 0.0396(3) 0.0465(3) 0.0399(3) -0.0033(2) 0.0106(2) 0.0009(2) Cl41 0.1434(12) 0.1239(10) 0.1097(10) 0.0260(8) 0.0433(9) 0.0227(9) Cl42 0.1168(11) 0.1419(13) 0.2104(19) 0.0316(12) 0.0606(12) 0.0420(10) Pd1 0.03864(11) 0.05235(13) 0.03580(11) 0.00137(7) 0.00886(7) 0.00501(7) N1 0.057(2) 0.091(3) 0.056(3) 0.005(2) 0.0016(16) -0.004(2) O1 0.0589(17) 0.064(2) 0.0480(18) 0.0057(12) 0.0159(13) 0.0065(13) O2 0.104(3) 0.0561(19) 0.061(2) -0.0094(14) -0.0151(18) -0.0108(16) _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 C1 C2 1.362(4) . ? C1 N2 1.366(4) . ? C1 H1 0.9300 . ? C2 C3 1.412(4) . ? C2 H2 0.9300 . ? C3 C4 1.428(4) . ? C3 C8 1.432(3) . ? C4 C5 1.363(5) . ? C4 H4 0.9300 . ? C5 O3 1.351(4) . ? C5 C6 1.434(5) . ? C6 O4 1.354(4) . ? C6 C7 1.374(4) . ? C7 C8 1.430(4) . ? C7 H7 0.9300 . ? C8 C9 1.425(3) . ? C9 N2 1.338(3) . ? C9 C10 1.523(3) . ? C10 C11 1.527(3) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C16 1.397(3) . ? C11 C12 1.401(3) . ? C12 C13 1.398(4) . ? C12 H12 0.9300 . ? C13 O5 1.376(3) . ? C13 C14 1.408(4) . ? C14 O6 1.378(3) . ? C14 C15 1.385(4) . ? C15 C16 1.418(4) . ? C15 H15 0.9300 . ? C16 Pd1 2.012(3) . ? C17 O3 1.461(5) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 O4 1.426(5) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 O5 1.422(4) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 O6 1.432(4) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.385(4) . ? C21 C26 1.397(5) . ? C21 P1 1.831(3) . ? C22 C23 1.413(5) . ? C22 H22 0.9300 . ? C23 C24 1.369(8) . ? C23 H23 0.9300 . ? C24 C25 1.370(8) . ? C24 H24 0.9300 . ? C25 C26 1.378(5) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.381(4) . ? C27 C32 1.405(4) . ? C27 P1 1.837(3) . ? C28 C29 1.395(4) . ? C28 H28 0.9300 . ? C29 C30 1.375(5) . ? C29 H29 0.9300 . ? C30 C31 1.366(5) . ? C30 H30 0.9300 . ? C31 C32 1.395(4) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.378(4) . ? C33 C38 1.388(4) . ? C33 P1 1.842(3) . ? C34 C35 1.402(5) . ? C34 H34 0.9300 . ? C35 C36 1.336(6) . ? C35 H35 0.9300 . ? C36 C37 1.379(6) . ? C36 H36 0.9300 . ? C37 C38 1.393(5) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C40 Cl42 1.710(4) . ? C40 Cl41 1.742(5) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? N2 Pd1 2.130(2) . ? P1 Pd1 2.2780(16) . ? Pd1 O1 2.167(3) . ? Pd1 N1A 2.177(12) . ? N1 O2 1.243(8) . ? N1 O1 1.254(7) . ? O1A N1A 1.182(15) . ? O2A N1A 1.206(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 N2 122.4(3) . . ? C2 C1 H1 118.8 . . ? N2 C1 H1 118.8 . . ? C1 C2 C3 119.7(3) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C2 C3 C4 122.0(2) . . ? C2 C3 C8 118.6(2) . . ? C4 C3 C8 119.4(3) . . ? C5 C4 C3 120.5(3) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? O3 C5 C4 125.8(3) . . ? O3 C5 C6 113.6(3) . . ? C4 C5 C6 120.6(3) . . ? O4 C6 C7 126.0(3) . . ? O4 C6 C5 113.8(3) . . ? C7 C6 C5 120.2(3) . . ? C6 C7 C8 120.5(3) . . ? C6 C7 H7 119.7 . . ? C8 C7 H7 119.7 . . ? C9 C8 C7 124.0(2) . . ? C9 C8 C3 117.3(2) . . ? C7 C8 C3 118.6(2) . . ? N2 C9 C8 122.0(2) . . ? N2 C9 C10 114.9(2) . . ? C8 C9 C10 123.1(2) . . ? C9 C10 C11 108.58(19) . . ? C9 C10 H10A 110.0 . . ? C11 C10 H10A 110.0 . . ? C9 C10 H10B 110.0 . . ? C11 C10 H10B 110.0 . . ? H10A C10 H10B 108.4 . . ? C16 C11 C12 121.0(2) . . ? C16 C11 C10 119.9(2) . . ? C12 C11 C10 118.7(2) . . ? C13 C12 C11 120.1(2) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? O5 C13 C12 124.8(2) . . ? O5 C13 C14 115.6(2) . . ? C12 C13 C14 119.6(2) . . ? O6 C14 C15 125.2(2) . . ? O6 C14 C13 115.0(2) . . ? C15 C14 C13 119.8(2) . . ? C14 C15 C16 121.3(2) . . ? C14 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? C11 C16 C15 118.1(2) . . ? C11 C16 Pd1 116.88(17) . . ? C15 C16 Pd1 123.58(18) . . ? O3 C17 H17A 109.5 . . ? O3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O4 C18 H18A 109.5 . . ? O4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O5 C19 H19A 109.5 . . ? O5 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O5 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O6 C20 H20A 109.5 . . ? O6 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O6 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C26 119.1(3) . . ? C22 C21 P1 122.8(3) . . ? C26 C21 P1 118.0(2) . . ? C21 C22 C23 119.2(4) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? C24 C23 C22 120.4(4) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 120.2(4) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C24 C25 C26 120.4(4) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C25 C26 C21 120.7(4) . . ? C25 C26 H26 119.7 . . ? C21 C26 H26 119.7 . . ? C28 C27 C32 118.2(3) . . ? C28 C27 P1 121.8(2) . . ? C32 C27 P1 120.0(2) . . ? C27 C28 C29 120.3(3) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C30 C29 C28 121.2(3) . . ? C30 C29 H29 119.4 . . ? C28 C29 H29 119.4 . . ? C31 C30 C29 119.2(3) . . ? C31 C30 H30 120.4 . . ? C29 C30 H30 120.4 . . ? C30 C31 C32 120.7(3) . . ? C30 C31 H31 119.7 . . ? C32 C31 H31 119.7 . . ? C31 C32 C27 120.5(3) . . ? C31 C32 H32 119.8 . . ? C27 C32 H32 119.8 . . ? C34 C33 C38 119.0(3) . . ? C34 C33 P1 123.6(2) . . ? C38 C33 P1 117.4(2) . . ? C33 C34 C35 119.7(3) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C36 C35 C34 121.4(4) . . ? C36 C35 H35 119.3 . . ? C34 C35 H35 119.3 . . ? C35 C36 C37 119.6(3) . . ? C35 C36 H36 120.2 . . ? C37 C36 H36 120.2 . . ? C36 C37 C38 120.4(4) . . ? C36 C37 H37 119.8 . . ? C38 C37 H37 119.8 . . ? C33 C38 C37 119.7(3) . . ? C33 C38 H38 120.1 . . ? C37 C38 H38 120.1 . . ? Cl42 C40 Cl41 112.5(3) . . ? Cl42 C40 H40A 109.1 . . ? Cl41 C40 H40A 109.1 . . ? Cl42 C40 H40B 109.1 . . ? Cl41 C40 H40B 109.1 . . ? H40A C40 H40B 107.8 . . ? C9 N2 C1 119.9(2) . . ? C9 N2 Pd1 120.73(16) . . ? C1 N2 Pd1 119.29(19) . . ? C5 O3 C17 115.9(3) . . ? C6 O4 C18 117.9(3) . . ? C13 O5 C19 117.0(2) . . ? C14 O6 C20 117.5(2) . . ? C21 P1 C27 102.18(13) . . ? C21 P1 C33 104.48(13) . . ? C27 P1 C33 105.01(12) . . ? C21 P1 Pd1 111.94(9) . . ? C27 P1 Pd1 117.86(10) . . ? C33 P1 Pd1 113.92(9) . . ? C16 Pd1 N2 85.61(9) . . ? C16 Pd1 O1 169.52(10) . . ? N2 Pd1 O1 84.25(9) . . ? C16 Pd1 N1A 159.6(3) . . ? N2 Pd1 N1A 90.4(3) . . ? O1 Pd1 N1A 23.5(3) . . ? C16 Pd1 P1 93.46(7) . . ? N2 Pd1 P1 174.99(6) . . ? O1 Pd1 P1 96.40(8) . . ? N1A Pd1 P1 92.1(2) . . ? O2 N1 O1 116.4(5) . . ? N1 O1 Pd1 118.3(3) . . ? O1A N1A O2A 124(2) . . ? O1A N1A Pd1 123.4(11) . . ? O2A N1A Pd1 112(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 N2 C1 C2 C3 1.4(4) . . . . ? C1 C2 C3 C4 -177.7(3) . . . . ? C1 C2 C3 C8 -0.3(4) . . . . ? C2 C3 C4 C5 -180.0(3) . . . . ? C8 C3 C4 C5 2.6(4) . . . . ? C3 C4 C5 O3 179.3(4) . . . . ? C3 C4 C5 C6 1.4(5) . . . . ? O3 C5 C6 O4 -1.7(5) . . . . ? C4 C5 C6 O4 176.4(4) . . . . ? O3 C5 C6 C7 177.2(3) . . . . ? C4 C5 C6 C7 -4.6(6) . . . . ? O4 C6 C7 C8 -177.6(3) . . . . ? C5 C6 C7 C8 3.6(5) . . . . ? C6 C7 C8 C9 -179.0(3) . . . . ? C6 C7 C8 C3 0.5(4) . . . . ? C2 C3 C8 C9 -1.5(3) . . . . ? C4 C3 C8 C9 175.9(2) . . . . ? C2 C3 C8 C7 178.9(2) . . . . ? C4 C3 C8 C7 -3.6(4) . . . . ? C7 C8 C9 N2 -178.1(2) . . . . ? C3 C8 C9 N2 2.4(3) . . . . ? C7 C8 C9 C10 5.6(4) . . . . ? C3 C8 C9 C10 -173.9(2) . . . . ? N2 C9 C10 C11 -55.4(3) . . . . ? C8 C9 C10 C11 121.2(2) . . . . ? C9 C10 C11 C16 66.3(3) . . . . ? C9 C10 C11 C12 -106.3(3) . . . . ? C16 C11 C12 C13 -0.8(4) . . . . ? C10 C11 C12 C13 171.8(2) . . . . ? C11 C12 C13 O5 -177.4(2) . . . . ? C11 C12 C13 C14 1.1(4) . . . . ? O5 C13 C14 O6 -0.7(3) . . . . ? C12 C13 C14 O6 -179.3(2) . . . . ? O5 C13 C14 C15 178.1(2) . . . . ? C12 C13 C14 C15 -0.5(4) . . . . ? O6 C14 C15 C16 178.3(3) . . . . ? C13 C14 C15 C16 -0.3(4) . . . . ? C12 C11 C16 C15 -0.1(4) . . . . ? C10 C11 C16 C15 -172.5(2) . . . . ? C12 C11 C16 Pd1 166.75(18) . . . . ? C10 C11 C16 Pd1 -5.7(3) . . . . ? C14 C15 C16 C11 0.6(4) . . . . ? C14 C15 C16 Pd1 -165.3(2) . . . . ? C26 C21 C22 C23 1.9(5) . . . . ? P1 C21 C22 C23 178.9(3) . . . . ? C21 C22 C23 C24 -2.3(6) . . . . ? C22 C23 C24 C25 1.2(7) . . . . ? C23 C24 C25 C26 0.4(7) . . . . ? C24 C25 C26 C21 -0.9(6) . . . . ? C22 C21 C26 C25 -0.3(5) . . . . ? P1 C21 C26 C25 -177.5(3) . . . . ? C32 C27 C28 C29 0.4(5) . . . . ? P1 C27 C28 C29 178.5(3) . . . . ? C27 C28 C29 C30 -0.7(6) . . . . ? C28 C29 C30 C31 0.2(6) . . . . ? C29 C30 C31 C32 0.6(5) . . . . ? C30 C31 C32 C27 -0.8(5) . . . . ? C28 C27 C32 C31 0.4(4) . . . . ? P1 C27 C32 C31 -177.8(2) . . . . ? C38 C33 C34 C35 -2.3(5) . . . . ? P1 C33 C34 C35 177.4(3) . . . . ? C33 C34 C35 C36 0.2(6) . . . . ? C34 C35 C36 C37 1.2(7) . . . . ? C35 C36 C37 C38 -0.5(6) . . . . ? C34 C33 C38 C37 3.0(5) . . . . ? P1 C33 C38 C37 -176.8(3) . . . . ? C36 C37 C38 C33 -1.6(6) . . . . ? C8 C9 N2 C1 -1.4(4) . . . . ? C10 C9 N2 C1 175.2(2) . . . . ? C8 C9 N2 Pd1 176.03(17) . . . . ? C10 C9 N2 Pd1 -7.3(3) . . . . ? C2 C1 N2 C9 -0.6(4) . . . . ? C2 C1 N2 Pd1 -178.1(2) . . . . ? C4 C5 O3 C17 -1.8(7) . . . . ? C6 C5 O3 C17 176.3(5) . . . . ? C7 C6 O4 C18 5.7(6) . . . . ? C5 C6 O4 C18 -175.4(4) . . . . ? C12 C13 O5 C19 3.4(4) . . . . ? C14 C13 O5 C19 -175.1(3) . . . . ? C15 C14 O6 C20 -2.3(4) . . . . ? C13 C14 O6 C20 176.3(3) . . . . ? C22 C21 P1 C27 104.3(3) . . . . ? C26 C21 P1 C27 -78.6(2) . . . . ? C22 C21 P1 C33 -4.9(3) . . . . ? C26 C21 P1 C33 172.1(2) . . . . ? C22 C21 P1 Pd1 -128.7(2) . . . . ? C26 C21 P1 Pd1 48.4(2) . . . . ? C28 C27 P1 C21 143.3(3) . . . . ? C32 C27 P1 C21 -38.6(3) . . . . ? C28 C27 P1 C33 -107.9(3) . . . . ? C32 C27 P1 C33 70.2(2) . . . . ? C28 C27 P1 Pd1 20.2(3) . . . . ? C32 C27 P1 Pd1 -161.72(19) . . . . ? C34 C33 P1 C21 101.4(3) . . . . ? C38 C33 P1 C21 -78.9(2) . . . . ? C34 C33 P1 C27 -5.7(3) . . . . ? C38 C33 P1 C27 174.0(2) . . . . ? C34 C33 P1 Pd1 -136.1(2) . . . . ? C38 C33 P1 Pd1 43.6(2) . . . . ? C11 C16 Pd1 N2 -40.53(19) . . . . ? C15 C16 Pd1 N2 125.5(2) . . . . ? C11 C16 Pd1 O1 -25.8(7) . . . . ? C15 C16 Pd1 O1 140.3(6) . . . . ? C11 C16 Pd1 N1A -119.8(8) . . . . ? C15 C16 Pd1 N1A 46.2(8) . . . . ? C11 C16 Pd1 P1 134.53(19) . . . . ? C15 C16 Pd1 P1 -59.4(2) . . . . ? C9 N2 Pd1 C16 50.39(19) . . . . ? C1 N2 Pd1 C16 -132.1(2) . . . . ? C9 N2 Pd1 O1 -126.9(2) . . . . ? C1 N2 Pd1 O1 50.5(2) . . . . ? C9 N2 Pd1 N1A -149.6(3) . . . . ? C1 N2 Pd1 N1A 27.9(4) . . . . ? C9 N2 Pd1 P1 -29.1(8) . . . . ? C1 N2 Pd1 P1 148.3(6) . . . . ? C21 P1 Pd1 C16 -176.16(12) . . . . ? C27 P1 Pd1 C16 -58.13(13) . . . . ? C33 P1 Pd1 C16 65.57(12) . . . . ? C21 P1 Pd1 N2 -97.0(7) . . . . ? C27 P1 Pd1 N2 21.1(7) . . . . ? C33 P1 Pd1 N2 144.8(7) . . . . ? C21 P1 Pd1 O1 0.30(14) . . . . ? C27 P1 Pd1 O1 118.33(14) . . . . ? C33 P1 Pd1 O1 -117.97(13) . . . . ? C21 P1 Pd1 N1A 23.4(3) . . . . ? C27 P1 Pd1 N1A 141.5(3) . . . . ? C33 P1 Pd1 N1A -94.8(3) . . . . ? O2 N1 O1 Pd1 -1.6(6) . . . . ? C16 Pd1 O1 N1 -124.8(6) . . . . ? N2 Pd1 O1 N1 -110.0(3) . . . . ? N1A Pd1 O1 N1 -5.5(7) . . . . ? P1 Pd1 O1 N1 75.0(3) . . . . ? C16 Pd1 N1A O1A 135.7(9) . . . . ? N2 Pd1 N1A O1A 57.2(9) . . . . ? O1 Pd1 N1A O1A -17.2(7) . . . . ? P1 Pd1 N1A O1A -118.5(9) . . . . ? C16 Pd1 N1A O2A -39(3) . . . . ? N2 Pd1 N1A O2A -117(3) . . . . ? O1 Pd1 N1A O2A 168(3) . . . . ? P1 Pd1 N1A O2A 67(3) . . . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 34.54 _diffrn_measured_fraction_theta_full 0.933 _refine_diff_density_max 0.871 _refine_diff_density_min -0.641 _refine_diff_density_rms 0.097 ### END data_250K _database_code_depnum_ccdc_archive 'CCDC 858653' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Nitro-(1-(3,4-dimethoxybenzyl)-6,7-dimethoxyisoquinoline)(triphenylphosphine) palladium(II) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H37 Cl2 N2 O6 P Pd' _chemical_formula_sum 'C39 H37 Cl2 N2 O6 P Pd' _chemical_formula_weight 837.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.7248(5) _cell_length_b 22.0346(11) _cell_length_c 16.3099(8) _cell_angle_alpha 90.00 _cell_angle_beta 105.1660(10) _cell_angle_gamma 90.00 _cell_volume 3720.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 250(2) _cell_measurement_reflns_used 9487 _cell_measurement_theta_min 2.94 _cell_measurement_theta_max 31.31 _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.496 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 0.735 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9302 _exptl_absorpt_correction_T_max 0.9855 _exptl_absorpt_process_details ; SADABS V2008-1, Bruker AXS.: Madison, WI, USA, 2008 ; _exptl_special_details ? _diffrn_ambient_temperature 250(2) _diffrn_radiation_wavelength 0.77490 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator synchrotron _diffrn_measurement_device_type ? _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39374 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0576 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 33.66 _reflns_number_total 11236 _reflns_number_gt 8411 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics WINGX _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0814P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11236 _refine_ls_number_parameters 477 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1408 _refine_ls_wR_factor_gt 0.1312 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.1611(3) 0.18735(14) 0.71025(17) 0.0427(6) Uani 1 1 d . . . H1 H -0.1558 0.1559 0.6724 0.051 Uiso 1 1 calc R . . C2 C -0.2761(3) 0.21536(14) 0.70203(17) 0.0435(6) Uani 1 1 d . . . H2 H -0.3497 0.2025 0.6604 0.052 Uiso 1 1 calc R . . C3 C -0.2845(2) 0.26410(12) 0.75648(17) 0.0378(5) Uani 1 1 d . . . C4 C -0.4028(3) 0.29402(15) 0.75227(19) 0.0465(6) Uani 1 1 d . . . H4 H -0.4785 0.2814 0.7123 0.056 Uiso 1 1 calc R . . C5 C -0.4077(3) 0.34108(15) 0.8059(2) 0.0538(8) Uani 1 1 d . . . C6 C -0.2936(3) 0.36178(15) 0.8653(2) 0.0501(7) Uani 1 1 d . . . C7 C -0.1790(3) 0.33189(13) 0.87336(18) 0.0419(6) Uani 1 1 d . . . H7 H -0.1049 0.3443 0.9149 0.050 Uiso 1 1 calc R . . C8 C -0.1714(2) 0.28223(12) 0.81925(15) 0.0343(5) Uani 1 1 d . . . C9 C -0.0567(2) 0.24804(11) 0.82526(15) 0.0330(5) Uani 1 1 d . . . C10 C 0.0670(2) 0.25789(11) 0.89370(16) 0.0347(5) Uani 1 1 d . . . H10A H 0.0550 0.2900 0.9326 0.042 Uiso 1 1 calc R . . H10B H 0.1363 0.2702 0.8682 0.042 Uiso 1 1 calc R . . C11 C 0.1020(2) 0.19859(11) 0.94161(15) 0.0327(5) Uani 1 1 d . . . C12 C 0.0845(2) 0.19333(12) 1.02293(15) 0.0345(5) Uani 1 1 d . . . H12 H 0.0626 0.2277 1.0503 0.041 Uiso 1 1 calc R . . C13 C 0.0996(3) 0.13733(12) 1.06372(15) 0.0363(5) Uani 1 1 d . . . C14 C 0.1368(3) 0.08686(11) 1.02350(16) 0.0371(5) Uani 1 1 d . . . C15 C 0.1566(3) 0.09275(12) 0.94323(16) 0.0369(5) Uani 1 1 d . . . H15 H 0.1827 0.0588 0.9169 0.044 Uiso 1 1 calc R . . C16 C 0.1381(2) 0.14872(11) 0.90075(16) 0.0335(5) Uani 1 1 d . A . C17 C -0.6324(4) 0.3558(3) 0.7455(4) 0.119(2) Uani 1 1 d . . . H17A H -0.6230 0.3618 0.6885 0.178 Uiso 1 1 calc R . . H17B H -0.7035 0.3803 0.7534 0.178 Uiso 1 1 calc R . . H17C H -0.6499 0.3133 0.7535 0.178 Uiso 1 1 calc R . . C18 C -0.2025(5) 0.4365(2) 0.9678(3) 0.110(2) Uani 1 1 d . . . H18A H -0.1654 0.4074 1.0122 0.165 Uiso 1 1 calc R . . H18B H -0.2281 0.4727 0.9931 0.165 Uiso 1 1 calc R . . H18C H -0.1388 0.4471 0.9376 0.165 Uiso 1 1 calc R . . C19 C 0.0334(3) 0.17610(14) 1.18141(19) 0.0490(7) Uani 1 1 d . . . H19A H 0.0967 0.2085 1.1918 0.074 Uiso 1 1 calc R . . H19B H 0.0189 0.1629 1.2349 0.074 Uiso 1 1 calc R . . H19C H -0.0472 0.1907 1.1444 0.074 Uiso 1 1 calc R . . C20 C 0.1783(4) -0.01941(13) 1.0290(2) 0.0568(8) Uani 1 1 d . . . H20A H 0.1143 -0.0252 0.9752 0.085 Uiso 1 1 calc R . . H20B H 0.1776 -0.0541 1.0654 0.085 Uiso 1 1 calc R . . H20C H 0.2632 -0.0154 1.0189 0.085 Uiso 1 1 calc R . . C21 C 0.3611(3) 0.11762(13) 0.68390(16) 0.0400(6) Uani 1 1 d . . . C22 C 0.4033(3) 0.06692(17) 0.6489(2) 0.0555(8) Uani 1 1 d . . . H22 H 0.4135 0.0298 0.6782 0.067 Uiso 1 1 calc R . . C23 C 0.4304(4) 0.0710(2) 0.5707(2) 0.0779(12) Uani 1 1 d . . . H23 H 0.4613 0.0368 0.5477 0.094 Uiso 1 1 calc R . . C24 C 0.4125(4) 0.1249(3) 0.5264(2) 0.0850(15) Uani 1 1 d . . . H24 H 0.4301 0.1272 0.4730 0.102 Uiso 1 1 calc R . . C25 C 0.3692(4) 0.1751(2) 0.5600(2) 0.0697(11) Uani 1 1 d . . . H25 H 0.3563 0.2117 0.5293 0.084 Uiso 1 1 calc R . . C26 C 0.3443(3) 0.17219(17) 0.6390(2) 0.0521(7) Uani 1 1 d . . . H26 H 0.3162 0.2069 0.6624 0.062 Uiso 1 1 calc R . . C27 C 0.4607(3) 0.15297(11) 0.85699(17) 0.0359(5) Uani 1 1 d . . . C28 C 0.4487(3) 0.19139(16) 0.9209(2) 0.0536(8) Uani 1 1 d . . . H28 H 0.3664 0.1999 0.9283 0.064 Uiso 1 1 calc R . . C29 C 0.5573(3) 0.21761(18) 0.9747(2) 0.0656(10) Uani 1 1 d . . . H29 H 0.5479 0.2441 1.0178 0.079 Uiso 1 1 calc R . . C30 C 0.6782(3) 0.20521(15) 0.9655(2) 0.0540(8) Uani 1 1 d . . . H30 H 0.7514 0.2229 1.0025 0.065 Uiso 1 1 calc R . . C31 C 0.6921(3) 0.16725(13) 0.9024(2) 0.0450(6) Uani 1 1 d . . . H31 H 0.7748 0.1586 0.8960 0.054 Uiso 1 1 calc R . . C32 C 0.5842(3) 0.14153(13) 0.84796(19) 0.0438(6) Uani 1 1 d . . . H32 H 0.5944 0.1159 0.8041 0.053 Uiso 1 1 calc R . . C33 C 0.3333(3) 0.03668(12) 0.81728(16) 0.0379(5) Uani 1 1 d . . . C34 C 0.4378(3) 0.01285(14) 0.8769(2) 0.0537(7) Uani 1 1 d . . . H34 H 0.5088 0.0377 0.9020 0.064 Uiso 1 1 calc R . . C35 C 0.4376(4) -0.04781(16) 0.8997(2) 0.0668(10) Uani 1 1 d . . . H35 H 0.5091 -0.0637 0.9404 0.080 Uiso 1 1 calc R . . C36 C 0.3369(4) -0.08452(15) 0.8646(2) 0.0647(10) Uani 1 1 d . . . H36 H 0.3376 -0.1254 0.8812 0.078 Uiso 1 1 calc R . . C37 C 0.2326(4) -0.06125(15) 0.8038(3) 0.0653(9) Uani 1 1 d . . . H37 H 0.1622 -0.0864 0.7788 0.078 Uiso 1 1 calc R . . C38 C 0.2319(3) -0.00139(14) 0.7800(2) 0.0505(7) Uani 1 1 d . . . H38 H 0.1615 0.0139 0.7378 0.061 Uiso 1 1 calc R . . C40 C -0.1226(4) -0.0049(2) 0.7296(3) 0.0760(12) Uani 1 1 d . . . H40A H -0.1014 -0.0263 0.7842 0.091 Uiso 1 1 calc R . . H40B H -0.0592 0.0276 0.7329 0.091 Uiso 1 1 calc R . . N2 N -0.0522(2) 0.20316(10) 0.77156(13) 0.0363(4) Uani 1 1 d . A . O3 O -0.5142(2) 0.37360(15) 0.80694(19) 0.0830(9) Uani 1 1 d . . . O4 O -0.3126(3) 0.41041(13) 0.91011(17) 0.0730(8) Uani 1 1 d . . . O5 O 0.0797(2) 0.12662(9) 1.14201(12) 0.0442(4) Uani 1 1 d . . . O6 O 0.1489(2) 0.03400(9) 1.06900(13) 0.0498(5) Uani 1 1 d . . . P1 P 0.32017(6) 0.11646(3) 0.78588(4) 0.03331(14) Uani 1 1 d . A . Cl41 Cl -0.11205(13) -0.05542(6) 0.64951(8) 0.0942(4) Uani 1 1 d . . . Cl42 Cl -0.27531(14) 0.02628(7) 0.71148(12) 0.1148(5) Uani 1 1 d . . . Pd1 Pd 0.123082(18) 0.157521(9) 0.776268(11) 0.03398(7) Uani 1 1 d . . . N1 N 0.0491(3) 0.1358(2) 0.5913(3) 0.0541(11) Uani 0.780(8) 1 d P A 1 O1 O 0.0795(3) 0.17819(15) 0.64301(18) 0.0454(9) Uani 0.780(8) 1 d P A 1 O2 O 0.0494(6) 0.08444(15) 0.6218(3) 0.0604(12) Uani 0.780(8) 1 d P A 1 O1A O 0.0273(12) 0.1774(6) 0.5909(8) 0.059(4) Uiso 0.220(8) 1 d PD A 2 O2A O 0.057(5) 0.0860(11) 0.628(3) 0.183(17) Uiso 0.220(8) 1 d PD A 2 N1A N 0.0612(11) 0.1397(6) 0.6424(8) 0.037(3) Uiso 0.220(8) 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0386(14) 0.0506(16) 0.0360(13) -0.0022(11) 0.0046(10) 0.0031(12) C2 0.0310(13) 0.0589(17) 0.0358(13) 0.0032(12) 0.0003(10) -0.0024(11) C3 0.0307(12) 0.0419(14) 0.0398(13) 0.0087(10) 0.0076(10) 0.0021(10) C4 0.0283(13) 0.0574(18) 0.0496(15) 0.0054(13) 0.0030(11) 0.0026(11) C5 0.0361(15) 0.061(2) 0.061(2) 0.0019(15) 0.0078(14) 0.0140(13) C6 0.0417(16) 0.0553(17) 0.0504(17) 0.0017(14) 0.0066(13) 0.0135(13) C7 0.0357(14) 0.0453(15) 0.0419(14) 0.0053(11) 0.0050(11) 0.0083(11) C8 0.0300(12) 0.0383(13) 0.0331(11) 0.0079(9) 0.0056(9) 0.0033(9) C9 0.0286(11) 0.0366(12) 0.0332(11) 0.0068(9) 0.0073(9) 0.0014(9) C10 0.0299(11) 0.0345(12) 0.0380(12) 0.0069(10) 0.0055(9) 0.0012(9) C11 0.0292(11) 0.0346(12) 0.0326(11) 0.0028(9) 0.0052(9) 0.0022(9) C12 0.0330(12) 0.0376(12) 0.0314(11) -0.0015(9) 0.0058(9) 0.0041(9) C13 0.0390(13) 0.0395(13) 0.0301(11) 0.0003(10) 0.0086(10) 0.0032(10) C14 0.0408(14) 0.0343(12) 0.0364(12) 0.0045(10) 0.0105(10) 0.0037(10) C15 0.0384(13) 0.0365(13) 0.0363(12) 0.0000(10) 0.0105(10) 0.0075(10) C16 0.0296(11) 0.0400(13) 0.0308(11) 0.0022(9) 0.0075(9) 0.0032(9) C17 0.038(2) 0.155(5) 0.140(5) -0.058(4) -0.016(3) 0.031(3) C18 0.081(3) 0.122(4) 0.097(3) -0.062(3) -0.028(3) 0.048(3) C19 0.064(2) 0.0480(16) 0.0398(14) 0.0003(12) 0.0212(14) 0.0087(14) C20 0.067(2) 0.0367(15) 0.070(2) 0.0056(14) 0.0239(17) 0.0154(14) C21 0.0340(13) 0.0533(16) 0.0337(12) -0.0024(11) 0.0109(10) -0.0040(11) C22 0.0576(19) 0.063(2) 0.0487(17) -0.0142(15) 0.0198(14) -0.0022(15) C23 0.077(3) 0.109(4) 0.055(2) -0.030(2) 0.0302(19) -0.010(2) C24 0.069(3) 0.150(5) 0.0420(18) -0.003(2) 0.0241(18) -0.032(3) C25 0.056(2) 0.103(3) 0.0495(19) 0.021(2) 0.0131(16) -0.017(2) C26 0.0414(16) 0.0659(19) 0.0491(17) 0.0066(14) 0.0123(13) -0.0086(14) C27 0.0333(13) 0.0368(13) 0.0356(12) 0.0004(9) 0.0052(10) -0.0010(9) C28 0.0387(15) 0.063(2) 0.0564(18) -0.0205(15) 0.0074(13) 0.0045(14) C29 0.0481(18) 0.077(2) 0.064(2) -0.0328(18) 0.0001(16) -0.0017(16) C30 0.0414(16) 0.0574(19) 0.0537(18) -0.0012(14) -0.0042(13) -0.0051(13) C31 0.0338(14) 0.0470(15) 0.0513(16) 0.0078(12) 0.0062(12) -0.0020(11) C32 0.0394(14) 0.0417(14) 0.0502(16) -0.0019(12) 0.0118(12) -0.0047(11) C33 0.0402(14) 0.0365(13) 0.0402(13) -0.0016(10) 0.0164(11) 0.0025(10) C34 0.0559(19) 0.0441(16) 0.0564(18) 0.0045(13) 0.0065(15) 0.0045(13) C35 0.082(3) 0.0477(18) 0.064(2) 0.0090(16) 0.0076(19) 0.0148(18) C36 0.097(3) 0.0356(16) 0.068(2) 0.0004(15) 0.032(2) 0.0025(17) C37 0.077(2) 0.0424(17) 0.079(2) -0.0079(16) 0.024(2) -0.0148(16) C38 0.0470(17) 0.0436(15) 0.0595(18) -0.0041(13) 0.0115(14) -0.0043(13) C40 0.067(3) 0.073(3) 0.090(3) 0.018(2) 0.024(2) 0.0033(19) N2 0.0314(10) 0.0445(12) 0.0322(10) 0.0053(9) 0.0066(8) 0.0034(9) O3 0.0386(13) 0.103(2) 0.098(2) -0.0270(17) 0.0002(13) 0.0300(14) O4 0.0580(15) 0.0797(18) 0.0708(16) -0.0234(13) -0.0021(12) 0.0311(13) O5 0.0606(13) 0.0421(11) 0.0332(9) 0.0038(8) 0.0182(9) 0.0071(9) O6 0.0680(14) 0.0376(10) 0.0472(11) 0.0104(8) 0.0212(10) 0.0132(9) P1 0.0317(3) 0.0360(3) 0.0324(3) -0.0022(2) 0.0085(2) 0.0012(2) Cl41 0.1092(10) 0.0934(8) 0.0860(8) 0.0213(6) 0.0364(7) 0.0198(7) Cl42 0.0847(9) 0.1052(10) 0.1621(14) 0.0213(9) 0.0458(9) 0.0272(7) Pd1 0.03086(11) 0.04152(12) 0.02939(11) 0.00151(7) 0.00758(7) 0.00451(7) N1 0.0445(19) 0.067(3) 0.045(2) 0.0066(17) 0.0003(15) -0.0037(17) O1 0.0477(16) 0.0512(19) 0.0371(15) 0.0066(11) 0.0109(12) 0.0071(12) O2 0.077(2) 0.0418(16) 0.0465(17) -0.0039(12) -0.0117(15) -0.0125(14) _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 C1 C2 1.354(4) . ? C1 N2 1.369(3) . ? C1 H1 0.9400 . ? C2 C3 1.411(4) . ? C2 H2 0.9400 . ? C3 C4 1.415(4) . ? C3 C8 1.425(4) . ? C4 C5 1.366(5) . ? C4 H4 0.9400 . ? C5 O3 1.352(4) . ? C5 C6 1.423(5) . ? C6 O4 1.343(4) . ? C6 C7 1.370(4) . ? C7 C8 1.421(4) . ? C7 H7 0.9400 . ? C8 C9 1.424(3) . ? C9 N2 1.330(3) . ? C9 C10 1.509(3) . ? C10 C11 1.518(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 C16 1.391(3) . ? C11 C12 1.392(3) . ? C12 C13 1.391(4) . ? C12 H12 0.9400 . ? C13 O5 1.369(3) . ? C13 C14 1.401(4) . ? C14 O6 1.369(3) . ? C14 C15 1.386(3) . ? C15 C16 1.403(3) . ? C15 H15 0.9400 . ? C16 Pd1 2.004(2) . ? C17 O3 1.449(5) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 O4 1.425(5) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 O5 1.420(3) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 O6 1.421(4) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 C22 1.383(4) . ? C21 C26 1.395(4) . ? C21 P1 1.828(3) . ? C22 C23 1.384(5) . ? C22 H22 0.9400 . ? C23 C24 1.377(7) . ? C23 H23 0.9400 . ? C24 C25 1.370(7) . ? C24 H24 0.9400 . ? C25 C26 1.384(5) . ? C25 H25 0.9400 . ? C26 H26 0.9400 . ? C27 C28 1.375(4) . ? C27 C32 1.394(4) . ? C27 P1 1.830(3) . ? C28 C29 1.388(4) . ? C28 H28 0.9400 . ? C29 C30 1.372(5) . ? C29 H29 0.9400 . ? C30 C31 1.363(5) . ? C30 H30 0.9400 . ? C31 C32 1.382(4) . ? C31 H31 0.9400 . ? C32 H32 0.9400 . ? C33 C34 1.381(4) . ? C33 C38 1.382(4) . ? C33 P1 1.826(3) . ? C34 C35 1.387(5) . ? C34 H34 0.9400 . ? C35 C36 1.351(6) . ? C35 H35 0.9400 . ? C36 C37 1.384(6) . ? C36 H36 0.9400 . ? C37 C38 1.374(4) . ? C37 H37 0.9400 . ? C38 H38 0.9400 . ? C40 Cl42 1.729(4) . ? C40 Cl41 1.741(5) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? N2 Pd1 2.116(2) . ? P1 Pd1 2.2666(7) . ? Pd1 N1A 2.146(12) . ? Pd1 O1 2.149(3) . ? N1 O2 1.235(6) . ? N1 O1 1.243(6) . ? O1A N1A 1.170(16) . ? O2A N1A 1.205(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 N2 122.5(3) . . ? C2 C1 H1 118.8 . . ? N2 C1 H1 118.8 . . ? C1 C2 C3 119.4(3) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C2 C3 C4 121.9(3) . . ? C2 C3 C8 118.9(2) . . ? C4 C3 C8 119.2(3) . . ? C5 C4 C3 120.4(3) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? O3 C5 C4 125.8(3) . . ? O3 C5 C6 113.6(3) . . ? C4 C5 C6 120.6(3) . . ? O4 C6 C7 126.3(3) . . ? O4 C6 C5 113.6(3) . . ? C7 C6 C5 120.1(3) . . ? C6 C7 C8 120.4(3) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C7 C8 C9 123.6(2) . . ? C7 C8 C3 119.1(2) . . ? C9 C8 C3 117.3(2) . . ? N2 C9 C8 121.8(2) . . ? N2 C9 C10 114.7(2) . . ? C8 C9 C10 123.4(2) . . ? C9 C10 C11 107.9(2) . . ? C9 C10 H10A 110.1 . . ? C11 C10 H10A 110.1 . . ? C9 C10 H10B 110.1 . . ? C11 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? C16 C11 C12 120.9(2) . . ? C16 C11 C10 119.7(2) . . ? C12 C11 C10 119.0(2) . . ? C13 C12 C11 120.1(2) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? O5 C13 C12 124.9(2) . . ? O5 C13 C14 115.6(2) . . ? C12 C13 C14 119.4(2) . . ? O6 C14 C15 125.1(2) . . ? O6 C14 C13 114.8(2) . . ? C15 C14 C13 120.0(2) . . ? C14 C15 C16 120.8(2) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C11 C16 C15 118.6(2) . . ? C11 C16 Pd1 116.75(18) . . ? C15 C16 Pd1 123.29(19) . . ? O3 C17 H17A 109.5 . . ? O3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O4 C18 H18A 109.5 . . ? O4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O5 C19 H19A 109.5 . . ? O5 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O5 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O6 C20 H20A 109.5 . . ? O6 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O6 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C26 119.4(3) . . ? C22 C21 P1 123.1(2) . . ? C26 C21 P1 117.5(2) . . ? C21 C22 C23 119.9(4) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C24 C23 C22 120.4(4) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C25 C24 C23 120.2(3) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 120.2(4) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C25 C26 C21 120.0(4) . . ? C25 C26 H26 120.0 . . ? C21 C26 H26 120.0 . . ? C28 C27 C32 118.2(3) . . ? C28 C27 P1 121.7(2) . . ? C32 C27 P1 120.1(2) . . ? C27 C28 C29 120.4(3) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C30 C29 C28 120.6(3) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C31 C30 C29 119.8(3) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C30 C31 C32 119.9(3) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C31 C32 C27 121.1(3) . . ? C31 C32 H32 119.4 . . ? C27 C32 H32 119.4 . . ? C34 C33 C38 118.6(3) . . ? C34 C33 P1 123.5(2) . . ? C38 C33 P1 117.8(2) . . ? C33 C34 C35 119.8(3) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C36 C35 C34 121.3(4) . . ? C36 C35 H35 119.3 . . ? C34 C35 H35 119.3 . . ? C35 C36 C37 119.2(3) . . ? C35 C36 H36 120.4 . . ? C37 C36 H36 120.4 . . ? C38 C37 C36 120.1(3) . . ? C38 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C37 C38 C33 120.8(3) . . ? C37 C38 H38 119.6 . . ? C33 C38 H38 119.6 . . ? Cl42 C40 Cl41 111.8(3) . . ? Cl42 C40 H40A 109.3 . . ? Cl41 C40 H40A 109.3 . . ? Cl42 C40 H40B 109.3 . . ? Cl41 C40 H40B 109.3 . . ? H40A C40 H40B 107.9 . . ? C9 N2 C1 120.0(2) . . ? C9 N2 Pd1 120.95(17) . . ? C1 N2 Pd1 119.06(18) . . ? C5 O3 C17 115.9(3) . . ? C6 O4 C18 117.6(3) . . ? C13 O5 C19 116.6(2) . . ? C14 O6 C20 117.2(2) . . ? C33 P1 C21 104.43(12) . . ? C33 P1 C27 104.77(12) . . ? C21 P1 C27 102.50(12) . . ? C33 P1 Pd1 113.96(9) . . ? C21 P1 Pd1 111.90(9) . . ? C27 P1 Pd1 117.83(9) . . ? C16 Pd1 N2 85.28(9) . . ? C16 Pd1 N1A 159.2(3) . . ? N2 Pd1 N1A 90.9(3) . . ? C16 Pd1 O1 169.69(10) . . ? N2 Pd1 O1 84.63(9) . . ? N1A Pd1 O1 23.4(3) . . ? C16 Pd1 P1 93.73(7) . . ? N2 Pd1 P1 174.86(6) . . ? N1A Pd1 P1 91.8(3) . . ? O1 Pd1 P1 96.13(7) . . ? O2 N1 O1 116.3(4) . . ? N1 O1 Pd1 118.4(3) . . ? O1A N1A O2A 124(3) . . ? O1A N1A Pd1 123.7(12) . . ? O2A N1A Pd1 112(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 N2 C1 C2 C3 2.2(4) . . . . ? C1 C2 C3 C4 -178.3(3) . . . . ? C1 C2 C3 C8 -0.5(4) . . . . ? C2 C3 C4 C5 -180.0(3) . . . . ? C8 C3 C4 C5 2.2(4) . . . . ? C3 C4 C5 O3 178.9(3) . . . . ? C3 C4 C5 C6 1.6(5) . . . . ? O3 C5 C6 O4 -1.2(5) . . . . ? C4 C5 C6 O4 176.4(3) . . . . ? O3 C5 C6 C7 177.8(3) . . . . ? C4 C5 C6 C7 -4.6(5) . . . . ? O4 C6 C7 C8 -177.5(3) . . . . ? C5 C6 C7 C8 3.6(5) . . . . ? C6 C7 C8 C9 -178.3(3) . . . . ? C6 C7 C8 C3 0.1(4) . . . . ? C2 C3 C8 C7 179.1(2) . . . . ? C4 C3 C8 C7 -3.0(4) . . . . ? C2 C3 C8 C9 -2.4(4) . . . . ? C4 C3 C8 C9 175.5(2) . . . . ? C7 C8 C9 N2 -177.7(2) . . . . ? C3 C8 C9 N2 3.9(4) . . . . ? C7 C8 C9 C10 4.5(4) . . . . ? C3 C8 C9 C10 -174.0(2) . . . . ? N2 C9 C10 C11 -56.6(3) . . . . ? C8 C9 C10 C11 121.4(2) . . . . ? C9 C10 C11 C16 67.3(3) . . . . ? C9 C10 C11 C12 -106.2(3) . . . . ? C16 C11 C12 C13 -1.8(4) . . . . ? C10 C11 C12 C13 171.6(2) . . . . ? C11 C12 C13 O5 -177.3(2) . . . . ? C11 C12 C13 C14 2.2(4) . . . . ? O5 C13 C14 O6 -0.5(4) . . . . ? C12 C13 C14 O6 180.0(2) . . . . ? O5 C13 C14 C15 178.6(2) . . . . ? C12 C13 C14 C15 -0.9(4) . . . . ? O6 C14 C15 C16 178.2(3) . . . . ? C13 C14 C15 C16 -0.9(4) . . . . ? C12 C11 C16 C15 0.0(4) . . . . ? C10 C11 C16 C15 -173.3(2) . . . . ? C12 C11 C16 Pd1 167.24(19) . . . . ? C10 C11 C16 Pd1 -6.1(3) . . . . ? C14 C15 C16 C11 1.3(4) . . . . ? C14 C15 C16 Pd1 -165.0(2) . . . . ? C26 C21 C22 C23 1.1(5) . . . . ? P1 C21 C22 C23 178.9(3) . . . . ? C21 C22 C23 C24 -1.7(6) . . . . ? C22 C23 C24 C25 0.8(6) . . . . ? C23 C24 C25 C26 0.6(6) . . . . ? C24 C25 C26 C21 -1.2(5) . . . . ? C22 C21 C26 C25 0.4(5) . . . . ? P1 C21 C26 C25 -177.6(3) . . . . ? C32 C27 C28 C29 -0.2(5) . . . . ? P1 C27 C28 C29 178.9(3) . . . . ? C27 C28 C29 C30 -0.6(6) . . . . ? C28 C29 C30 C31 0.6(6) . . . . ? C29 C30 C31 C32 0.2(5) . . . . ? C30 C31 C32 C27 -1.0(5) . . . . ? C28 C27 C32 C31 1.0(4) . . . . ? P1 C27 C32 C31 -178.2(2) . . . . ? C38 C33 C34 C35 -1.6(5) . . . . ? P1 C33 C34 C35 177.3(3) . . . . ? C33 C34 C35 C36 0.0(6) . . . . ? C34 C35 C36 C37 0.9(6) . . . . ? C35 C36 C37 C38 -0.3(6) . . . . ? C36 C37 C38 C33 -1.3(5) . . . . ? C34 C33 C38 C37 2.3(5) . . . . ? P1 C33 C38 C37 -176.7(3) . . . . ? C8 C9 N2 C1 -2.3(4) . . . . ? C10 C9 N2 C1 175.7(2) . . . . ? C8 C9 N2 Pd1 175.37(17) . . . . ? C10 C9 N2 Pd1 -6.6(3) . . . . ? C2 C1 N2 C9 -0.8(4) . . . . ? C2 C1 N2 Pd1 -178.5(2) . . . . ? C4 C5 O3 C17 0.4(6) . . . . ? C6 C5 O3 C17 177.9(4) . . . . ? C7 C6 O4 C18 4.5(6) . . . . ? C5 C6 O4 C18 -176.5(4) . . . . ? C12 C13 O5 C19 3.7(4) . . . . ? C14 C13 O5 C19 -175.8(3) . . . . ? C15 C14 O6 C20 -3.0(4) . . . . ? C13 C14 O6 C20 176.1(3) . . . . ? C34 C33 P1 C21 101.8(3) . . . . ? C38 C33 P1 C21 -79.3(2) . . . . ? C34 C33 P1 C27 -5.6(3) . . . . ? C38 C33 P1 C27 173.3(2) . . . . ? C34 C33 P1 Pd1 -135.8(2) . . . . ? C38 C33 P1 Pd1 43.1(2) . . . . ? C22 C21 P1 C33 -5.3(3) . . . . ? C26 C21 P1 C33 172.5(2) . . . . ? C22 C21 P1 C27 103.7(3) . . . . ? C26 C21 P1 C27 -78.4(2) . . . . ? C22 C21 P1 Pd1 -129.1(2) . . . . ? C26 C21 P1 Pd1 48.8(2) . . . . ? C28 C27 P1 C33 -108.5(3) . . . . ? C32 C27 P1 C33 70.6(2) . . . . ? C28 C27 P1 C21 142.6(3) . . . . ? C32 C27 P1 C21 -38.2(3) . . . . ? C28 C27 P1 Pd1 19.3(3) . . . . ? C32 C27 P1 Pd1 -161.55(19) . . . . ? C11 C16 Pd1 N2 -40.5(2) . . . . ? C15 C16 Pd1 N2 126.1(2) . . . . ? C11 C16 Pd1 N1A -120.4(9) . . . . ? C15 C16 Pd1 N1A 46.1(9) . . . . ? C11 C16 Pd1 O1 -28.7(7) . . . . ? C15 C16 Pd1 O1 137.8(6) . . . . ? C11 C16 Pd1 P1 134.45(19) . . . . ? C15 C16 Pd1 P1 -59.0(2) . . . . ? C9 N2 Pd1 C16 50.3(2) . . . . ? C1 N2 Pd1 C16 -132.0(2) . . . . ? C9 N2 Pd1 N1A -150.1(4) . . . . ? C1 N2 Pd1 N1A 27.6(4) . . . . ? C9 N2 Pd1 O1 -127.6(2) . . . . ? C1 N2 Pd1 O1 50.1(2) . . . . ? C9 N2 Pd1 P1 -28.8(8) . . . . ? C1 N2 Pd1 P1 148.9(6) . . . . ? C33 P1 Pd1 C16 65.13(12) . . . . ? C21 P1 Pd1 C16 -176.67(12) . . . . ? C27 P1 Pd1 C16 -58.25(12) . . . . ? C33 P1 Pd1 N2 143.9(6) . . . . ? C21 P1 Pd1 N2 -97.9(7) . . . . ? C27 P1 Pd1 N2 20.5(7) . . . . ? C33 P1 Pd1 N1A -94.8(4) . . . . ? C21 P1 Pd1 N1A 23.4(4) . . . . ? C27 P1 Pd1 N1A 141.8(4) . . . . ? C33 P1 Pd1 O1 -117.86(13) . . . . ? C21 P1 Pd1 O1 0.34(14) . . . . ? C27 P1 Pd1 O1 118.77(13) . . . . ? O2 N1 O1 Pd1 -1.5(5) . . . . ? C16 Pd1 O1 N1 -122.2(6) . . . . ? N2 Pd1 O1 N1 -110.4(3) . . . . ? N1A Pd1 O1 N1 -5.6(8) . . . . ? P1 Pd1 O1 N1 74.7(3) . . . . ? C16 Pd1 N1A O1A 133.8(11) . . . . ? N2 Pd1 N1A O1A 54.9(11) . . . . ? O1 Pd1 N1A O1A -19.4(8) . . . . ? P1 Pd1 N1A O1A -120.8(11) . . . . ? C16 Pd1 N1A O2A -41(3) . . . . ? N2 Pd1 N1A O2A -120(3) . . . . ? O1 Pd1 N1A O2A 166(3) . . . . ? P1 Pd1 N1A O2A 64(3) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 33.66 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.552 _refine_diff_density_min -0.744 _refine_diff_density_rms 0.094 ### END data_200K _database_code_depnum_ccdc_archive 'CCDC 858654' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Nitro-(1-(3,4-dimethoxybenzyl)-6,7-dimethoxyisoquinoline)(triphenylphosphine) palladium(II) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H37 Cl2 N2 O6 P Pd' _chemical_formula_sum 'C39 H37 Cl2 N2 O6 P Pd' _chemical_formula_weight 837.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.7075(7) _cell_length_b 21.8698(14) _cell_length_c 16.3273(10) _cell_angle_alpha 90.00 _cell_angle_beta 105.3090(10) _cell_angle_gamma 90.00 _cell_volume 3687.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9897 _cell_measurement_theta_min 2.96 _cell_measurement_theta_max 33.37 _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 0.741 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9296 _exptl_absorpt_correction_T_max 0.9853 _exptl_absorpt_process_details ; SADABS V2008-1, Bruker AXS.: Madison, WI, USA, 2008 ; _exptl_special_details ? _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.77490 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator synchrotron _diffrn_measurement_device_type ? _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38982 _diffrn_reflns_av_R_equivalents 0.0576 _diffrn_reflns_av_sigmaI/netI 0.0590 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 33.64 _reflns_number_total 11142 _reflns_number_gt 8822 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics WINGX _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0868P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11142 _refine_ls_number_parameters 477 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0572 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1422 _refine_ls_wR_factor_gt 0.1341 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.1614(3) 0.18809(13) 0.71065(16) 0.0338(5) Uani 1 1 d . . . H1 H -0.1567 0.1559 0.6725 0.041 Uiso 1 1 calc R . . C2 C -0.2756(3) 0.21642(13) 0.70271(16) 0.0347(5) Uani 1 1 d . . . H2 H -0.3502 0.2034 0.6605 0.042 Uiso 1 1 calc R . . C3 C -0.2846(2) 0.26540(12) 0.75712(16) 0.0306(5) Uani 1 1 d . . . C4 C -0.4036(2) 0.29548(13) 0.75295(18) 0.0364(6) Uani 1 1 d . . . H4 H -0.4804 0.2824 0.7128 0.044 Uiso 1 1 calc R . . C5 C -0.4087(3) 0.34303(14) 0.8061(2) 0.0424(7) Uani 1 1 d . . . C6 C -0.2939(3) 0.36367(14) 0.86579(18) 0.0390(6) Uani 1 1 d . . . C7 C -0.1784(3) 0.33393(11) 0.87373(17) 0.0315(5) Uani 1 1 d . . . H7 H -0.1031 0.3469 0.9153 0.038 Uiso 1 1 calc R . . C8 C -0.1713(2) 0.28340(11) 0.81959(15) 0.0282(5) Uani 1 1 d . . . C9 C -0.0560(2) 0.24930(11) 0.82553(14) 0.0271(4) Uani 1 1 d . . . C10 C 0.0683(2) 0.25929(11) 0.89429(15) 0.0277(4) Uani 1 1 d . . . H10A H 0.0561 0.2917 0.9337 0.033 Uiso 1 1 calc R . . H10B H 0.1384 0.2721 0.8688 0.033 Uiso 1 1 calc R . . C11 C 0.1037(2) 0.19924(11) 0.94189(14) 0.0263(4) Uani 1 1 d . . . C12 C 0.0850(2) 0.19367(11) 1.02263(15) 0.0287(5) Uani 1 1 d . . . H12 H 0.0620 0.2285 1.0501 0.034 Uiso 1 1 calc R . . C13 C 0.0997(2) 0.13723(12) 1.06327(15) 0.0291(5) Uani 1 1 d . . . C14 C 0.1375(2) 0.08616(11) 1.02301(16) 0.0297(5) Uani 1 1 d . . . C15 C 0.1575(2) 0.09269(11) 0.94305(15) 0.0295(5) Uani 1 1 d . . . H15 H 0.1845 0.0583 0.9165 0.035 Uiso 1 1 calc R . . C16 C 0.1387(2) 0.14895(11) 0.90068(15) 0.0275(5) Uani 1 1 d . A . C17 C -0.6345(4) 0.3574(3) 0.7467(4) 0.0910(17) Uani 1 1 d . . . H17A H -0.6240 0.3609 0.6891 0.137 Uiso 1 1 calc R . . H17B H -0.7050 0.3842 0.7526 0.137 Uiso 1 1 calc R . . H17C H -0.6552 0.3150 0.7574 0.137 Uiso 1 1 calc R . . C18 C -0.2015(4) 0.4388(2) 0.9692(3) 0.0918(18) Uani 1 1 d . . . H18A H -0.1628 0.4085 1.0126 0.138 Uiso 1 1 calc R . . H18B H -0.2278 0.4748 0.9963 0.138 Uiso 1 1 calc R . . H18C H -0.1379 0.4509 0.9387 0.138 Uiso 1 1 calc R . . C19 C 0.0335(3) 0.17605(14) 1.18077(18) 0.0393(6) Uani 1 1 d . . . H19A H 0.0972 0.2092 1.1901 0.059 Uiso 1 1 calc R . . H19B H 0.0207 0.1630 1.2354 0.059 Uiso 1 1 calc R . . H19C H -0.0489 0.1905 1.1439 0.059 Uiso 1 1 calc R . . C20 C 0.1776(3) -0.02068(13) 1.0271(2) 0.0439(7) Uani 1 1 d . . . H20A H 0.1129 -0.0258 0.9726 0.066 Uiso 1 1 calc R . . H20B H 0.1758 -0.0563 1.0632 0.066 Uiso 1 1 calc R . . H20C H 0.2638 -0.0168 1.0175 0.066 Uiso 1 1 calc R . . C21 C 0.3610(2) 0.11759(12) 0.68384(16) 0.0317(5) Uani 1 1 d . . . C22 C 0.4043(3) 0.06625(15) 0.6500(2) 0.0447(7) Uani 1 1 d . . . H22 H 0.4165 0.0288 0.6805 0.054 Uiso 1 1 calc R . . C23 C 0.4297(4) 0.0700(2) 0.5707(2) 0.0611(10) Uani 1 1 d . . . H23 H 0.4599 0.0349 0.5474 0.073 Uiso 1 1 calc R . . C24 C 0.4115(4) 0.1240(2) 0.5258(2) 0.0676(12) Uani 1 1 d . . . H24 H 0.4288 0.1260 0.4717 0.081 Uiso 1 1 calc R . . C25 C 0.3682(3) 0.1752(2) 0.5593(2) 0.0560(9) Uani 1 1 d . . . H25 H 0.3545 0.2123 0.5281 0.067 Uiso 1 1 calc R . . C26 C 0.3446(3) 0.17229(15) 0.6387(2) 0.0414(6) Uani 1 1 d . . . H26 H 0.3170 0.2079 0.6624 0.050 Uiso 1 1 calc R . . C27 C 0.4621(2) 0.15404(11) 0.85654(16) 0.0284(5) Uani 1 1 d . . . C28 C 0.4494(3) 0.19336(14) 0.92022(19) 0.0424(6) Uani 1 1 d . . . H28 H 0.3660 0.2022 0.9272 0.051 Uiso 1 1 calc R . . C29 C 0.5587(3) 0.21991(17) 0.9741(2) 0.0524(8) Uani 1 1 d . . . H29 H 0.5492 0.2467 1.0179 0.063 Uiso 1 1 calc R . . C30 C 0.6805(3) 0.20780(14) 0.96463(19) 0.0426(6) Uani 1 1 d . . . H30 H 0.7546 0.2264 1.0013 0.051 Uiso 1 1 calc R . . C31 C 0.6939(3) 0.16877(13) 0.90200(19) 0.0367(6) Uani 1 1 d . . . H31 H 0.7777 0.1597 0.8959 0.044 Uiso 1 1 calc R . . C32 C 0.5859(3) 0.14251(12) 0.84760(18) 0.0345(5) Uani 1 1 d . . . H32 H 0.5962 0.1162 0.8035 0.041 Uiso 1 1 calc R . . C33 C 0.3356(2) 0.03654(11) 0.81813(16) 0.0306(5) Uani 1 1 d . . . C34 C 0.4413(3) 0.01307(13) 0.87790(19) 0.0419(6) Uani 1 1 d . . . H34 H 0.5128 0.0387 0.9031 0.050 Uiso 1 1 calc R . . C35 C 0.4424(4) -0.04816(15) 0.9008(2) 0.0517(8) Uani 1 1 d . . . H35 H 0.5158 -0.0641 0.9413 0.062 Uiso 1 1 calc R . . C36 C 0.3412(4) -0.08577(14) 0.8667(2) 0.0520(8) Uani 1 1 d . . . H36 H 0.3426 -0.1273 0.8841 0.062 Uiso 1 1 calc R . . C37 C 0.2361(4) -0.06272(14) 0.8062(2) 0.0502(8) Uani 1 1 d . . . H37 H 0.1650 -0.0887 0.7817 0.060 Uiso 1 1 calc R . . C38 C 0.2332(3) -0.00229(13) 0.78096(19) 0.0406(6) Uani 1 1 d . . . H38 H 0.1614 0.0127 0.7383 0.049 Uiso 1 1 calc R . . C40 C -0.1199(3) -0.00350(18) 0.7313(2) 0.0577(9) Uani 1 1 d . . . H40A H -0.0981 -0.0247 0.7868 0.069 Uiso 1 1 calc R . . H40B H -0.0568 0.0301 0.7344 0.069 Uiso 1 1 calc R . . N2 N -0.05125(19) 0.20407(10) 0.77192(13) 0.0291(4) Uani 1 1 d . A . O3 O -0.5151(2) 0.37529(13) 0.80766(18) 0.0649(7) Uani 1 1 d . . . O4 O -0.3124(2) 0.41292(12) 0.91061(16) 0.0580(6) Uani 1 1 d . . . O5 O 0.0791(2) 0.12593(8) 1.14145(11) 0.0359(4) Uani 1 1 d . . . O6 O 0.1490(2) 0.03276(8) 1.06788(12) 0.0389(4) Uani 1 1 d . . . P1 P 0.32133(6) 0.11681(3) 0.78612(4) 0.02673(13) Uani 1 1 d . A . Cl41 Cl -0.10723(11) -0.05491(5) 0.65215(7) 0.0707(3) Uani 1 1 d . . . Cl42 Cl -0.27524(11) 0.02713(6) 0.71194(10) 0.0874(4) Uani 1 1 d . . . Pd1 Pd 0.123783(17) 0.158222(9) 0.776381(11) 0.02716(7) Uani 1 1 d . . . N1 N 0.0494(3) 0.13442(16) 0.5921(2) 0.0432(9) Uani 0.844(7) 1 d P A 1 O1 O 0.0788(2) 0.17808(12) 0.64287(15) 0.0363(7) Uani 0.844(7) 1 d P A 1 O2 O 0.0515(5) 0.08279(13) 0.6232(3) 0.0515(11) Uani 0.844(7) 1 d P A 1 O1A O 0.0269(15) 0.1774(7) 0.5887(10) 0.046(4) Uiso 0.156(7) 1 d PD A 2 O2A O 0.055(7) 0.0855(13) 0.626(4) 0.15(2) Uiso 0.156(7) 1 d PD A 2 N1A N 0.0584(13) 0.1397(7) 0.6406(9) 0.025(3) Uiso 0.156(7) 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0306(12) 0.0392(14) 0.0303(12) -0.0021(10) 0.0055(9) 0.0019(10) C2 0.0275(12) 0.0420(14) 0.0313(12) 0.0025(10) 0.0021(9) 0.0006(10) C3 0.0234(11) 0.0352(12) 0.0322(12) 0.0065(9) 0.0055(9) 0.0025(9) C4 0.0226(11) 0.0442(15) 0.0400(13) 0.0010(11) 0.0038(10) 0.0025(10) C5 0.0290(13) 0.0503(17) 0.0458(16) 0.0027(12) 0.0063(12) 0.0124(11) C6 0.0340(14) 0.0410(14) 0.0399(14) 0.0017(11) 0.0059(11) 0.0113(11) C7 0.0266(12) 0.0327(12) 0.0326(12) 0.0036(9) 0.0035(10) 0.0054(9) C8 0.0227(10) 0.0322(12) 0.0290(11) 0.0072(9) 0.0055(8) 0.0027(8) C9 0.0238(10) 0.0304(11) 0.0274(10) 0.0067(9) 0.0071(8) 0.0010(8) C10 0.0238(10) 0.0270(11) 0.0304(11) 0.0038(9) 0.0037(9) 0.0004(8) C11 0.0229(10) 0.0279(11) 0.0269(10) 0.0027(8) 0.0044(8) 0.0022(8) C12 0.0271(11) 0.0292(11) 0.0278(11) -0.0001(9) 0.0040(9) 0.0023(9) C13 0.0298(12) 0.0313(11) 0.0267(11) -0.0001(9) 0.0084(9) 0.0031(9) C14 0.0306(12) 0.0271(11) 0.0314(11) 0.0034(9) 0.0081(9) 0.0030(9) C15 0.0310(12) 0.0293(11) 0.0296(11) 0.0013(9) 0.0101(9) 0.0060(9) C16 0.0234(11) 0.0330(12) 0.0259(11) 0.0009(9) 0.0064(8) 0.0025(8) C17 0.0321(19) 0.110(4) 0.115(4) -0.039(3) -0.009(2) 0.026(2) C18 0.060(2) 0.094(3) 0.094(3) -0.052(3) -0.029(2) 0.039(2) C19 0.0505(17) 0.0388(14) 0.0324(13) -0.0006(11) 0.0176(12) 0.0065(12) C20 0.0508(17) 0.0295(13) 0.0548(17) 0.0074(12) 0.0197(14) 0.0134(12) C21 0.0269(11) 0.0404(13) 0.0279(11) -0.0028(10) 0.0078(9) -0.0027(10) C22 0.0458(16) 0.0500(17) 0.0425(15) -0.0111(13) 0.0190(13) -0.0038(13) C23 0.063(2) 0.082(3) 0.0459(18) -0.0230(18) 0.0280(16) -0.0093(19) C24 0.053(2) 0.119(4) 0.0350(16) -0.0034(19) 0.0177(15) -0.026(2) C25 0.0399(17) 0.088(3) 0.0396(16) 0.0186(17) 0.0096(13) -0.0131(17) C26 0.0347(14) 0.0493(16) 0.0410(15) 0.0091(12) 0.0116(12) -0.0049(12) C27 0.0253(11) 0.0282(11) 0.0303(12) -0.0001(9) 0.0050(9) -0.0004(8) C28 0.0295(13) 0.0491(16) 0.0469(16) -0.0169(13) 0.0070(11) 0.0016(11) C29 0.0388(16) 0.064(2) 0.0494(17) -0.0245(15) 0.0029(13) -0.0022(14) C30 0.0352(14) 0.0441(16) 0.0421(15) -0.0009(12) -0.0012(11) -0.0040(11) C31 0.0263(12) 0.0379(13) 0.0444(15) 0.0067(11) 0.0067(11) -0.0010(10) C32 0.0316(13) 0.0331(12) 0.0405(14) 0.0002(10) 0.0123(11) -0.0005(10) C33 0.0315(12) 0.0270(11) 0.0350(12) -0.0013(9) 0.0121(10) 0.0022(9) C34 0.0437(15) 0.0335(14) 0.0445(15) 0.0032(11) 0.0046(12) 0.0033(11) C35 0.063(2) 0.0372(15) 0.0495(17) 0.0082(13) 0.0058(15) 0.0104(14) C36 0.077(2) 0.0314(14) 0.0511(18) 0.0010(13) 0.0236(17) 0.0032(14) C37 0.061(2) 0.0337(15) 0.0581(19) -0.0068(13) 0.0186(16) -0.0109(13) C38 0.0403(15) 0.0365(14) 0.0445(15) -0.0027(11) 0.0104(12) -0.0032(11) C40 0.051(2) 0.053(2) 0.072(2) 0.0126(17) 0.0211(18) 0.0030(15) N2 0.0251(10) 0.0355(11) 0.0258(9) 0.0035(8) 0.0050(8) 0.0019(8) O3 0.0295(11) 0.0799(18) 0.0771(17) -0.0220(14) -0.0007(11) 0.0221(11) O4 0.0459(13) 0.0611(15) 0.0583(14) -0.0190(11) -0.0013(11) 0.0231(11) O5 0.0492(11) 0.0335(9) 0.0281(8) 0.0043(7) 0.0155(8) 0.0074(8) O6 0.0534(12) 0.0291(9) 0.0378(10) 0.0072(7) 0.0186(9) 0.0102(8) P1 0.0252(3) 0.0287(3) 0.0265(3) -0.0015(2) 0.0072(2) 0.0013(2) Cl41 0.0804(7) 0.0688(6) 0.0683(6) 0.0163(5) 0.0291(5) 0.0156(5) Cl42 0.0623(6) 0.0758(7) 0.1306(11) 0.0122(7) 0.0367(7) 0.0175(5) Pd1 0.02455(11) 0.03279(11) 0.02423(10) 0.00148(6) 0.00662(7) 0.00365(6) N1 0.0373(16) 0.049(2) 0.0385(18) 0.0079(13) 0.0013(12) -0.0037(13) O1 0.0376(13) 0.0417(15) 0.0307(13) 0.0045(9) 0.0108(10) 0.0042(10) O2 0.067(2) 0.0341(14) 0.0423(15) -0.0015(10) -0.0060(13) -0.0104(12) _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 C1 C2 1.346(4) . ? C1 N2 1.375(3) . ? C1 H1 0.9500 . ? C2 C3 1.411(4) . ? C2 H2 0.9500 . ? C3 C8 1.419(3) . ? C3 C4 1.420(3) . ? C4 C5 1.365(4) . ? C4 H4 0.9500 . ? C5 O3 1.346(3) . ? C5 C6 1.426(4) . ? C6 O4 1.346(4) . ? C6 C7 1.373(4) . ? C7 C8 1.430(4) . ? C7 H7 0.9500 . ? C8 C9 1.423(3) . ? C9 N2 1.331(3) . ? C9 C10 1.514(3) . ? C10 C11 1.522(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.390(3) . ? C11 C16 1.391(3) . ? C12 C13 1.390(3) . ? C12 H12 0.9500 . ? C13 O5 1.374(3) . ? C13 C14 1.408(3) . ? C14 O6 1.367(3) . ? C14 C15 1.385(3) . ? C15 C16 1.400(3) . ? C15 H15 0.9500 . ? C16 Pd1 2.003(2) . ? C17 O3 1.451(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 O4 1.430(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 O5 1.421(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 O6 1.418(3) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.384(4) . ? C21 C26 1.392(4) . ? C21 P1 1.828(3) . ? C22 C23 1.394(4) . ? C22 H22 0.9500 . ? C23 C24 1.377(6) . ? C23 H23 0.9500 . ? C24 C25 1.379(6) . ? C24 H24 0.9500 . ? C25 C26 1.385(4) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.383(4) . ? C27 C32 1.395(4) . ? C27 P1 1.828(3) . ? C28 C29 1.392(4) . ? C28 H28 0.9500 . ? C29 C30 1.380(4) . ? C29 H29 0.9500 . ? C30 C31 1.368(4) . ? C30 H30 0.9500 . ? C31 C32 1.383(4) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.384(4) . ? C33 C38 1.393(4) . ? C33 P1 1.827(3) . ? C34 C35 1.389(4) . ? C34 H34 0.9500 . ? C35 C36 1.358(5) . ? C35 H35 0.9500 . ? C36 C37 1.381(5) . ? C36 H36 0.9500 . ? C37 C38 1.382(4) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C40 Cl42 1.743(4) . ? C40 Cl41 1.745(4) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? N2 Pd1 2.110(2) . ? P1 Pd1 2.2676(6) . ? Pd1 O1 2.149(2) . ? Pd1 N1A 2.179(15) . ? N1 O2 1.236(5) . ? N1 O1 1.249(5) . ? O1A N1A 1.168(16) . ? O2A N1A 1.209(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 N2 122.4(2) . . ? C2 C1 H1 118.8 . . ? N2 C1 H1 118.8 . . ? C1 C2 C3 120.0(2) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C2 C3 C8 118.4(2) . . ? C2 C3 C4 122.1(2) . . ? C8 C3 C4 119.5(2) . . ? C5 C4 C3 120.6(3) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? O3 C5 C4 126.0(3) . . ? O3 C5 C6 113.8(3) . . ? C4 C5 C6 120.3(3) . . ? O4 C6 C7 125.9(3) . . ? O4 C6 C5 113.6(2) . . ? C7 C6 C5 120.5(3) . . ? C6 C7 C8 120.1(2) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C3 C8 C9 117.7(2) . . ? C3 C8 C7 118.9(2) . . ? C9 C8 C7 123.4(2) . . ? N2 C9 C8 121.9(2) . . ? N2 C9 C10 114.6(2) . . ? C8 C9 C10 123.5(2) . . ? C9 C10 C11 107.82(19) . . ? C9 C10 H10A 110.1 . . ? C11 C10 H10A 110.1 . . ? C9 C10 H10B 110.1 . . ? C11 C10 H10B 110.1 . . ? H10A C10 H10B 108.5 . . ? C12 C11 C16 120.9(2) . . ? C12 C11 C10 118.7(2) . . ? C16 C11 C10 119.8(2) . . ? C11 C12 C13 120.2(2) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? O5 C13 C12 125.2(2) . . ? O5 C13 C14 115.3(2) . . ? C12 C13 C14 119.5(2) . . ? O6 C14 C15 125.4(2) . . ? O6 C14 C13 115.1(2) . . ? C15 C14 C13 119.5(2) . . ? C14 C15 C16 121.2(2) . . ? C14 C15 H15 119.4 . . ? C16 C15 H15 119.4 . . ? C11 C16 C15 118.5(2) . . ? C11 C16 Pd1 116.77(17) . . ? C15 C16 Pd1 123.52(18) . . ? O3 C17 H17A 109.5 . . ? O3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O4 C18 H18A 109.5 . . ? O4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O5 C19 H19A 109.5 . . ? O5 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O5 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O6 C20 H20A 109.5 . . ? O6 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O6 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C26 119.6(3) . . ? C22 C21 P1 122.7(2) . . ? C26 C21 P1 117.7(2) . . ? C21 C22 C23 119.5(3) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? C24 C23 C22 120.6(4) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 120.0(3) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C24 C25 C26 119.9(4) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C25 C26 C21 120.4(3) . . ? C25 C26 H26 119.8 . . ? C21 C26 H26 119.8 . . ? C28 C27 C32 118.4(2) . . ? C28 C27 P1 121.4(2) . . ? C32 C27 P1 120.2(2) . . ? C27 C28 C29 120.1(3) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C30 C29 C28 120.7(3) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C31 C30 C29 119.5(3) . . ? C31 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C30 C31 C32 120.2(3) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C31 C32 C27 121.0(3) . . ? C31 C32 H32 119.5 . . ? C27 C32 H32 119.5 . . ? C34 C33 C38 119.0(3) . . ? C34 C33 P1 123.3(2) . . ? C38 C33 P1 117.7(2) . . ? C33 C34 C35 119.6(3) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C36 C35 C34 121.6(3) . . ? C36 C35 H35 119.2 . . ? C34 C35 H35 119.2 . . ? C35 C36 C37 118.9(3) . . ? C35 C36 H36 120.5 . . ? C37 C36 H36 120.5 . . ? C36 C37 C38 120.8(3) . . ? C36 C37 H37 119.6 . . ? C38 C37 H37 119.6 . . ? C37 C38 C33 120.0(3) . . ? C37 C38 H38 120.0 . . ? C33 C38 H38 120.0 . . ? Cl42 C40 Cl41 111.7(2) . . ? Cl42 C40 H40A 109.3 . . ? Cl41 C40 H40A 109.3 . . ? Cl42 C40 H40B 109.3 . . ? Cl41 C40 H40B 109.3 . . ? H40A C40 H40B 107.9 . . ? C9 N2 C1 119.5(2) . . ? C9 N2 Pd1 121.25(16) . . ? C1 N2 Pd1 119.19(17) . . ? C5 O3 C17 116.3(3) . . ? C6 O4 C18 117.7(3) . . ? C13 O5 C19 116.1(2) . . ? C14 O6 C20 116.9(2) . . ? C33 P1 C27 104.79(11) . . ? C33 P1 C21 104.37(12) . . ? C27 P1 C21 102.63(12) . . ? C33 P1 Pd1 114.20(8) . . ? C27 P1 Pd1 117.72(8) . . ? C21 P1 Pd1 111.68(9) . . ? C16 Pd1 N2 85.15(9) . . ? C16 Pd1 O1 169.92(9) . . ? N2 Pd1 O1 84.83(8) . . ? C16 Pd1 N1A 158.4(4) . . ? N2 Pd1 N1A 90.5(3) . . ? O1 Pd1 N1A 23.1(4) . . ? C16 Pd1 P1 93.74(7) . . ? N2 Pd1 P1 174.82(6) . . ? O1 Pd1 P1 96.13(6) . . ? N1A Pd1 P1 92.3(3) . . ? O2 N1 O1 116.8(4) . . ? N1 O1 Pd1 118.0(2) . . ? O1A N1A O2A 124(4) . . ? O1A N1A Pd1 124.2(14) . . ? O2A N1A Pd1 112(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C1 C2 C3 1.6(4) . . . . ? C1 C2 C3 C8 -0.2(4) . . . . ? C1 C2 C3 C4 -178.0(3) . . . . ? C2 C3 C4 C5 -179.5(3) . . . . ? C8 C3 C4 C5 2.7(4) . . . . ? C3 C4 C5 O3 179.4(3) . . . . ? C3 C4 C5 C6 0.9(5) . . . . ? O3 C5 C6 O4 -2.2(4) . . . . ? C4 C5 C6 O4 176.5(3) . . . . ? O3 C5 C6 C7 177.7(3) . . . . ? C4 C5 C6 C7 -3.6(5) . . . . ? O4 C6 C7 C8 -177.5(3) . . . . ? C5 C6 C7 C8 2.6(4) . . . . ? C2 C3 C8 C9 -2.2(3) . . . . ? C4 C3 C8 C9 175.7(2) . . . . ? C2 C3 C8 C7 178.5(2) . . . . ? C4 C3 C8 C7 -3.6(4) . . . . ? C6 C7 C8 C3 1.0(4) . . . . ? C6 C7 C8 C9 -178.2(3) . . . . ? C3 C8 C9 N2 3.6(3) . . . . ? C7 C8 C9 N2 -177.2(2) . . . . ? C3 C8 C9 C10 -173.9(2) . . . . ? C7 C8 C9 C10 5.3(4) . . . . ? N2 C9 C10 C11 -56.3(3) . . . . ? C8 C9 C10 C11 121.3(2) . . . . ? C9 C10 C11 C12 -105.6(2) . . . . ? C9 C10 C11 C16 66.5(3) . . . . ? C16 C11 C12 C13 -0.6(4) . . . . ? C10 C11 C12 C13 171.4(2) . . . . ? C11 C12 C13 O5 -177.5(2) . . . . ? C11 C12 C13 C14 1.8(4) . . . . ? O5 C13 C14 O6 -0.4(3) . . . . ? C12 C13 C14 O6 -179.8(2) . . . . ? O5 C13 C14 C15 178.5(2) . . . . ? C12 C13 C14 C15 -0.9(4) . . . . ? O6 C14 C15 C16 177.6(2) . . . . ? C13 C14 C15 C16 -1.2(4) . . . . ? C12 C11 C16 C15 -1.4(4) . . . . ? C10 C11 C16 C15 -173.4(2) . . . . ? C12 C11 C16 Pd1 166.60(18) . . . . ? C10 C11 C16 Pd1 -5.4(3) . . . . ? C14 C15 C16 C11 2.3(4) . . . . ? C14 C15 C16 Pd1 -164.8(2) . . . . ? C26 C21 C22 C23 -0.6(4) . . . . ? P1 C21 C22 C23 178.5(2) . . . . ? C21 C22 C23 C24 -0.4(5) . . . . ? C22 C23 C24 C25 0.3(6) . . . . ? C23 C24 C25 C26 0.8(5) . . . . ? C24 C25 C26 C21 -1.8(5) . . . . ? C22 C21 C26 C25 1.6(4) . . . . ? P1 C21 C26 C25 -177.5(2) . . . . ? C32 C27 C28 C29 -0.7(5) . . . . ? P1 C27 C28 C29 178.5(3) . . . . ? C27 C28 C29 C30 0.4(5) . . . . ? C28 C29 C30 C31 -0.6(5) . . . . ? C29 C30 C31 C32 1.2(5) . . . . ? C30 C31 C32 C27 -1.5(4) . . . . ? C28 C27 C32 C31 1.2(4) . . . . ? P1 C27 C32 C31 -178.0(2) . . . . ? C38 C33 C34 C35 -1.2(4) . . . . ? P1 C33 C34 C35 177.7(2) . . . . ? C33 C34 C35 C36 -0.8(5) . . . . ? C34 C35 C36 C37 1.6(5) . . . . ? C35 C36 C37 C38 -0.4(5) . . . . ? C36 C37 C38 C33 -1.6(5) . . . . ? C34 C33 C38 C37 2.4(4) . . . . ? P1 C33 C38 C37 -176.6(2) . . . . ? C8 C9 N2 C1 -2.3(3) . . . . ? C10 C9 N2 C1 175.4(2) . . . . ? C8 C9 N2 Pd1 175.63(17) . . . . ? C10 C9 N2 Pd1 -6.7(3) . . . . ? C2 C1 N2 C9 -0.3(4) . . . . ? C2 C1 N2 Pd1 -178.3(2) . . . . ? C4 C5 O3 C17 -0.1(6) . . . . ? C6 C5 O3 C17 178.5(4) . . . . ? C7 C6 O4 C18 3.1(5) . . . . ? C5 C6 O4 C18 -177.0(4) . . . . ? C12 C13 O5 C19 3.0(4) . . . . ? C14 C13 O5 C19 -176.3(2) . . . . ? C15 C14 O6 C20 -3.3(4) . . . . ? C13 C14 O6 C20 175.5(2) . . . . ? C34 C33 P1 C27 -5.6(3) . . . . ? C38 C33 P1 C27 173.3(2) . . . . ? C34 C33 P1 C21 101.9(2) . . . . ? C38 C33 P1 C21 -79.1(2) . . . . ? C34 C33 P1 Pd1 -135.9(2) . . . . ? C38 C33 P1 Pd1 43.1(2) . . . . ? C28 C27 P1 C33 -108.9(2) . . . . ? C32 C27 P1 C33 70.3(2) . . . . ? C28 C27 P1 C21 142.3(2) . . . . ? C32 C27 P1 C21 -38.5(2) . . . . ? C28 C27 P1 Pd1 19.3(3) . . . . ? C32 C27 P1 Pd1 -161.57(18) . . . . ? C22 C21 P1 C33 -6.0(3) . . . . ? C26 C21 P1 C33 173.1(2) . . . . ? C22 C21 P1 C27 103.1(2) . . . . ? C26 C21 P1 C27 -77.7(2) . . . . ? C22 C21 P1 Pd1 -129.8(2) . . . . ? C26 C21 P1 Pd1 49.3(2) . . . . ? C11 C16 Pd1 N2 -41.04(19) . . . . ? C15 C16 Pd1 N2 126.3(2) . . . . ? C11 C16 Pd1 O1 -34.2(7) . . . . ? C15 C16 Pd1 O1 133.1(5) . . . . ? C11 C16 Pd1 N1A -120.1(10) . . . . ? C15 C16 Pd1 N1A 47.2(10) . . . . ? C11 C16 Pd1 P1 133.89(18) . . . . ? C15 C16 Pd1 P1 -58.8(2) . . . . ? C9 N2 Pd1 C16 50.61(19) . . . . ? C1 N2 Pd1 C16 -131.5(2) . . . . ? C9 N2 Pd1 O1 -128.2(2) . . . . ? C1 N2 Pd1 O1 49.7(2) . . . . ? C9 N2 Pd1 N1A -150.6(4) . . . . ? C1 N2 Pd1 N1A 27.3(4) . . . . ? C9 N2 Pd1 P1 -27.2(7) . . . . ? C1 N2 Pd1 P1 150.7(5) . . . . ? C33 P1 Pd1 C16 64.48(12) . . . . ? C27 P1 Pd1 C16 -59.04(12) . . . . ? C21 P1 Pd1 C16 -177.39(12) . . . . ? C33 P1 Pd1 N2 142.0(6) . . . . ? C27 P1 Pd1 N2 18.4(6) . . . . ? C21 P1 Pd1 N2 -99.9(6) . . . . ? C33 P1 Pd1 O1 -117.59(12) . . . . ? C27 P1 Pd1 O1 118.88(12) . . . . ? C21 P1 Pd1 O1 0.53(12) . . . . ? C33 P1 Pd1 N1A -94.8(4) . . . . ? C27 P1 Pd1 N1A 141.7(4) . . . . ? C21 P1 Pd1 N1A 23.3(4) . . . . ? O2 N1 O1 Pd1 -1.6(5) . . . . ? C16 Pd1 O1 N1 -117.9(6) . . . . ? N2 Pd1 O1 N1 -111.1(2) . . . . ? N1A Pd1 O1 N1 -7.4(9) . . . . ? P1 Pd1 O1 N1 74.0(2) . . . . ? C16 Pd1 N1A O1A 135.2(12) . . . . ? N2 Pd1 N1A O1A 57.1(14) . . . . ? O1 Pd1 N1A O1A -18.3(10) . . . . ? P1 Pd1 N1A O1A -118.6(13) . . . . ? C16 Pd1 N1A O2A -43(4) . . . . ? N2 Pd1 N1A O2A -121(4) . . . . ? O1 Pd1 N1A O2A 164(4) . . . . ? P1 Pd1 N1A O2A 64(4) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 33.64 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.617 _refine_diff_density_min -0.962 _refine_diff_density_rms 0.144 ### END data_150K _database_code_depnum_ccdc_archive 'CCDC 858655' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Nitro-(1-(3,4-dimethoxybenzyl)-6,7-dimethoxyisoquinoline)(triphenylphosphine) palladium(II) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H37 Cl2 N2 O6 P Pd' _chemical_formula_sum 'C39 H37 Cl2 N2 O6 P Pd' _chemical_formula_weight 837.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.6878(7) _cell_length_b 21.7334(14) _cell_length_c 16.3349(10) _cell_angle_alpha 90.00 _cell_angle_beta 105.4190(10) _cell_angle_gamma 90.00 _cell_volume 3657.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9928 _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 33.58 _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 0.747 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9290 _exptl_absorpt_correction_T_max 0.9852 _exptl_absorpt_process_details ; SADABS V2008-1, Bruker AXS.: Madison, WI, USA, 2008 ; _exptl_special_details ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.7749 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator synchrotron _diffrn_measurement_device_type ? _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39140 _diffrn_reflns_av_R_equivalents 0.0793 _diffrn_reflns_av_sigmaI/netI 0.0755 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 33.64 _reflns_number_total 11046 _reflns_number_gt 9181 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics WINGX _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+0.7884P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11046 _refine_ls_number_parameters 477 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0563 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1262 _refine_ls_wR_factor_gt 0.1207 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.1615(2) 0.18866(12) 0.71055(15) 0.0267(4) Uani 1 1 d . . . H1 H -0.1567 0.1564 0.6723 0.032 Uiso 1 1 calc R . . C2 C -0.2770(2) 0.21706(12) 0.70255(15) 0.0273(5) Uani 1 1 d . . . H2 H -0.3517 0.2040 0.6602 0.033 Uiso 1 1 calc R . . C3 C -0.2858(2) 0.26620(11) 0.75742(14) 0.0240(4) Uani 1 1 d . . . C4 C -0.4049(2) 0.29648(12) 0.75327(16) 0.0288(5) Uani 1 1 d . . . H4 H -0.4819 0.2834 0.7130 0.035 Uiso 1 1 calc R . . C5 C -0.4097(3) 0.34399(12) 0.80644(18) 0.0338(6) Uani 1 1 d . . . C6 C -0.2937(2) 0.36494(12) 0.86672(16) 0.0306(5) Uani 1 1 d . . . C7 C -0.1778(2) 0.33496(11) 0.87420(15) 0.0268(5) Uani 1 1 d . . . H7 H -0.1020 0.3479 0.9157 0.032 Uiso 1 1 calc R . . C8 C -0.1712(2) 0.28467(10) 0.81998(13) 0.0222(4) Uani 1 1 d . . . C9 C -0.0559(2) 0.25052(10) 0.82534(13) 0.0212(4) Uani 1 1 d . . . C10 C 0.0690(2) 0.26029(10) 0.89429(14) 0.0225(4) Uani 1 1 d . . . H10A H 0.0569 0.2928 0.9340 0.027 Uiso 1 1 calc R . . H10B H 0.1391 0.2733 0.8689 0.027 Uiso 1 1 calc R . . C11 C 0.1044(2) 0.19978(10) 0.94133(13) 0.0209(4) Uani 1 1 d . . . C12 C 0.0852(2) 0.19398(10) 1.02276(14) 0.0229(4) Uani 1 1 d . . . H12 H 0.0621 0.2290 1.0504 0.028 Uiso 1 1 calc R . . C13 C 0.1000(2) 0.13730(11) 1.06276(13) 0.0222(4) Uani 1 1 d . . . C14 C 0.1378(2) 0.08590(10) 1.02256(14) 0.0232(4) Uani 1 1 d . . . C15 C 0.1581(2) 0.09236(10) 0.94253(14) 0.0232(4) Uani 1 1 d . . . H15 H 0.1845 0.0577 0.9158 0.028 Uiso 1 1 calc R . . C16 C 0.1401(2) 0.14918(10) 0.90067(14) 0.0217(4) Uani 1 1 d . A . C17 C -0.6360(3) 0.3583(2) 0.7488(3) 0.0672(12) Uani 1 1 d . . . H17A H -0.6268 0.3619 0.6909 0.101 Uiso 1 1 calc R . . H17B H -0.7066 0.3850 0.7553 0.101 Uiso 1 1 calc R . . H17C H -0.6558 0.3155 0.7597 0.101 Uiso 1 1 calc R . . C18 C -0.2013(3) 0.44002(19) 0.9702(3) 0.0729(14) Uani 1 1 d . . . H18A H -0.1610 0.4086 1.0120 0.109 Uiso 1 1 calc R . . H18B H -0.2273 0.4752 0.9995 0.109 Uiso 1 1 calc R . . H18C H -0.1389 0.4536 0.9395 0.109 Uiso 1 1 calc R . . C19 C 0.0328(3) 0.17598(12) 1.18017(16) 0.0307(5) Uani 1 1 d . . . H19A H 0.0973 0.2091 1.1907 0.046 Uiso 1 1 calc R . . H19B H 0.0185 0.1625 1.2342 0.046 Uiso 1 1 calc R . . H19C H -0.0490 0.1910 1.1428 0.046 Uiso 1 1 calc R . . C20 C 0.1768(3) -0.02200(11) 1.02601(18) 0.0340(5) Uani 1 1 d . . . H20A H 0.1104 -0.0274 0.9721 0.051 Uiso 1 1 calc R . . H20B H 0.1768 -0.0578 1.0624 0.051 Uiso 1 1 calc R . . H20C H 0.2621 -0.0179 1.0150 0.051 Uiso 1 1 calc R . . C21 C 0.3617(2) 0.11767(11) 0.68422(14) 0.0244(4) Uani 1 1 d . . . C22 C 0.4057(3) 0.06529(13) 0.65048(17) 0.0344(5) Uani 1 1 d . . . H22 H 0.4179 0.0276 0.6811 0.041 Uiso 1 1 calc R . . C23 C 0.4314(3) 0.06920(16) 0.57093(19) 0.0466(7) Uani 1 1 d . . . H23 H 0.4630 0.0341 0.5481 0.056 Uiso 1 1 calc R . . C24 C 0.4117(3) 0.12330(19) 0.52526(18) 0.0501(8) Uani 1 1 d . . . H24 H 0.4284 0.1251 0.4710 0.060 Uiso 1 1 calc R . . C25 C 0.3671(3) 0.17521(17) 0.55875(18) 0.0432(7) Uani 1 1 d . . . H25 H 0.3528 0.2125 0.5273 0.052 Uiso 1 1 calc R . . C26 C 0.3438(2) 0.17234(13) 0.63801(16) 0.0313(5) Uani 1 1 d . . . H26 H 0.3153 0.2081 0.6612 0.038 Uiso 1 1 calc R . . C27 C 0.4624(2) 0.15479(10) 0.85601(15) 0.0233(4) Uani 1 1 d . . . C28 C 0.4498(2) 0.19465(12) 0.91991(16) 0.0321(5) Uani 1 1 d . . . H28 H 0.3662 0.2034 0.9270 0.038 Uiso 1 1 calc R . . C29 C 0.5592(3) 0.22183(14) 0.97350(18) 0.0404(6) Uani 1 1 d . . . H29 H 0.5496 0.2492 1.0168 0.048 Uiso 1 1 calc R . . C30 C 0.6816(2) 0.20937(12) 0.96440(17) 0.0326(5) Uani 1 1 d . . . H30 H 0.7558 0.2281 1.0012 0.039 Uiso 1 1 calc R . . C31 C 0.6954(2) 0.16963(11) 0.90168(17) 0.0283(5) Uani 1 1 d . . . H31 H 0.7794 0.1606 0.8956 0.034 Uiso 1 1 calc R . . C32 C 0.5871(2) 0.14289(11) 0.84753(16) 0.0277(5) Uani 1 1 d . . . H32 H 0.5975 0.1160 0.8039 0.033 Uiso 1 1 calc R . . C33 C 0.3378(2) 0.03627(10) 0.81844(14) 0.0234(4) Uani 1 1 d . . . C34 C 0.4443(3) 0.01303(12) 0.87846(17) 0.0328(5) Uani 1 1 d . . . H34 H 0.5154 0.0392 0.9032 0.039 Uiso 1 1 calc R . . C35 C 0.4478(3) -0.04849(13) 0.90272(18) 0.0401(6) Uani 1 1 d . . . H35 H 0.5218 -0.0641 0.9434 0.048 Uiso 1 1 calc R . . C36 C 0.3453(3) -0.08681(13) 0.86839(18) 0.0396(6) Uani 1 1 d . . . H36 H 0.3473 -0.1285 0.8861 0.047 Uiso 1 1 calc R . . C37 C 0.2381(3) -0.06401(12) 0.80727(19) 0.0376(6) Uani 1 1 d . . . H37 H 0.1668 -0.0903 0.7831 0.045 Uiso 1 1 calc R . . C38 C 0.2353(3) -0.00346(11) 0.78186(16) 0.0301(5) Uani 1 1 d . . . H38 H 0.1631 0.0114 0.7391 0.036 Uiso 1 1 calc R . . C40 C -0.1165(3) -0.00269(15) 0.7335(2) 0.0445(7) Uani 1 1 d . . . H40A H -0.0538 0.0313 0.7368 0.053 Uiso 1 1 calc R . . H40B H -0.0949 -0.0239 0.7891 0.053 Uiso 1 1 calc R . . N2 N -0.05156(18) 0.20458(9) 0.77162(12) 0.0229(4) Uani 1 1 d . A . O3 O -0.51706(19) 0.37643(11) 0.80828(15) 0.0489(6) Uani 1 1 d . . . O4 O -0.3130(2) 0.41468(10) 0.91144(13) 0.0440(5) Uani 1 1 d . . . O5 O 0.07887(18) 0.12556(8) 1.14066(10) 0.0275(3) Uani 1 1 d . . . O6 O 0.14907(18) 0.03190(8) 1.06733(11) 0.0302(4) Uani 1 1 d . . . P1 P 0.32218(5) 0.11684(3) 0.78611(3) 0.02073(11) Uani 1 1 d . A . Cl41 Cl -0.10248(9) -0.05467(4) 0.65433(5) 0.05092(19) Uani 1 1 d . . . Cl42 Cl -0.27454(9) 0.02763(4) 0.71237(8) 0.0648(3) Uani 1 1 d . . . Pd1 Pd 0.124065(16) 0.158454(8) 0.776170(10) 0.02143(6) Uani 1 1 d . . . N1 N 0.0505(3) 0.13351(14) 0.59185(19) 0.0353(7) Uani 0.857(6) 1 d P A 1 O1 O 0.0775(2) 0.17758(11) 0.64265(14) 0.0296(6) Uani 0.857(6) 1 d P A 1 O2 O 0.0544(5) 0.08135(13) 0.6237(3) 0.0400(10) Uani 0.857(6) 1 d P A 1 O1A O 0.0251(13) 0.1759(6) 0.5873(9) 0.034(4) Uiso 0.143(6) 1 d PD A 2 O2A O 0.044(6) 0.0852(13) 0.622(4) 0.109(17) Uiso 0.143(6) 1 d PD A 2 N1A N 0.0566(12) 0.1388(6) 0.6410(8) 0.016(3) Uiso 0.143(6) 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0238(11) 0.0321(12) 0.0224(10) -0.0014(9) 0.0031(8) 0.0004(9) C2 0.0228(11) 0.0329(12) 0.0236(10) 0.0015(9) 0.0015(8) 0.0014(9) C3 0.0196(10) 0.0275(11) 0.0245(10) 0.0047(8) 0.0048(8) 0.0002(8) C4 0.0185(10) 0.0343(12) 0.0316(11) 0.0026(9) 0.0033(9) 0.0034(8) C5 0.0224(12) 0.0410(14) 0.0356(13) 0.0006(10) 0.0033(10) 0.0084(9) C6 0.0259(12) 0.0319(12) 0.0325(12) 0.0019(10) 0.0050(9) 0.0076(9) C7 0.0230(11) 0.0292(11) 0.0257(11) 0.0038(9) 0.0020(9) 0.0044(8) C8 0.0191(10) 0.0241(10) 0.0228(10) 0.0061(8) 0.0042(8) 0.0020(7) C9 0.0192(9) 0.0230(10) 0.0220(9) 0.0052(8) 0.0065(7) 0.0005(7) C10 0.0193(10) 0.0227(10) 0.0248(10) 0.0037(8) 0.0045(8) 0.0015(7) C11 0.0181(9) 0.0213(10) 0.0222(9) 0.0007(8) 0.0033(7) 0.0010(7) C12 0.0227(10) 0.0239(10) 0.0207(9) 0.0001(8) 0.0032(8) 0.0030(8) C13 0.0220(10) 0.0258(10) 0.0188(9) 0.0010(8) 0.0054(8) 0.0030(8) C14 0.0238(10) 0.0228(10) 0.0235(10) 0.0036(8) 0.0072(8) 0.0031(8) C15 0.0226(10) 0.0246(10) 0.0236(10) -0.0004(8) 0.0082(8) 0.0030(8) C16 0.0207(10) 0.0249(10) 0.0202(10) 0.0023(8) 0.0067(8) 0.0014(7) C17 0.0220(14) 0.086(3) 0.083(3) -0.029(2) -0.0049(16) 0.0204(16) C18 0.0459(19) 0.078(3) 0.072(2) -0.046(2) -0.0244(17) 0.0310(18) C19 0.0384(14) 0.0302(12) 0.0273(11) 0.0001(9) 0.0155(10) 0.0050(10) C20 0.0405(14) 0.0229(11) 0.0421(14) 0.0027(10) 0.0170(11) 0.0079(10) C21 0.0190(10) 0.0327(12) 0.0216(10) -0.0021(8) 0.0060(8) -0.0034(8) C22 0.0348(13) 0.0371(14) 0.0348(13) -0.0092(10) 0.0155(11) -0.0045(10) C23 0.0482(17) 0.059(2) 0.0380(15) -0.0178(14) 0.0216(13) -0.0070(15) C24 0.0416(17) 0.084(3) 0.0273(13) -0.0035(14) 0.0140(12) -0.0191(16) C25 0.0320(14) 0.066(2) 0.0313(13) 0.0132(13) 0.0078(11) -0.0101(13) C26 0.0249(12) 0.0398(13) 0.0295(12) 0.0050(10) 0.0076(9) -0.0036(10) C27 0.0211(10) 0.0236(10) 0.0238(10) 0.0015(8) 0.0034(8) -0.0001(7) C28 0.0230(11) 0.0383(13) 0.0325(12) -0.0106(10) 0.0032(9) 0.0027(9) C29 0.0305(13) 0.0482(16) 0.0386(14) -0.0172(12) 0.0025(11) 0.0011(11) C30 0.0259(12) 0.0340(13) 0.0333(12) -0.0003(10) -0.0003(10) -0.0049(9) C31 0.0224(11) 0.0273(11) 0.0340(12) 0.0060(9) 0.0057(9) 0.0003(8) C32 0.0262(11) 0.0251(11) 0.0330(12) 0.0012(9) 0.0101(9) 0.0013(8) C33 0.0236(10) 0.0226(10) 0.0253(10) -0.0003(8) 0.0092(8) 0.0009(8) C34 0.0331(13) 0.0277(12) 0.0349(13) 0.0026(10) 0.0045(10) 0.0025(9) C35 0.0486(17) 0.0306(13) 0.0374(14) 0.0047(11) 0.0054(12) 0.0079(11) C36 0.0581(18) 0.0265(12) 0.0388(14) 0.0008(11) 0.0209(13) 0.0037(12) C37 0.0424(15) 0.0284(12) 0.0425(14) -0.0048(11) 0.0123(12) -0.0076(11) C38 0.0295(12) 0.0260(11) 0.0339(12) -0.0023(9) 0.0072(10) -0.0028(9) C40 0.0425(16) 0.0409(16) 0.0527(18) 0.0090(13) 0.0172(14) 0.0024(12) N2 0.0198(9) 0.0273(9) 0.0212(8) 0.0021(7) 0.0048(7) 0.0015(7) O3 0.0231(9) 0.0617(14) 0.0556(13) -0.0148(11) -0.0004(9) 0.0182(9) O4 0.0351(10) 0.0449(11) 0.0454(11) -0.0150(9) -0.0008(9) 0.0163(9) O5 0.0382(9) 0.0247(8) 0.0220(7) 0.0023(6) 0.0121(7) 0.0044(7) O6 0.0411(10) 0.0228(8) 0.0286(8) 0.0052(6) 0.0130(7) 0.0074(7) P1 0.0190(3) 0.0225(3) 0.0207(2) -0.00105(19) 0.0052(2) 0.00073(19) Cl41 0.0582(5) 0.0485(4) 0.0505(4) 0.0107(3) 0.0223(4) 0.0102(4) Cl42 0.0457(5) 0.0542(5) 0.0991(8) 0.0055(5) 0.0274(5) 0.0114(4) Pd1 0.01919(9) 0.02618(10) 0.01901(9) 0.00137(6) 0.00521(6) 0.00301(6) N1 0.0270(13) 0.0419(17) 0.0331(16) 0.0080(11) 0.0013(10) -0.0044(11) O1 0.0310(11) 0.0334(13) 0.0262(11) 0.0046(8) 0.0108(9) 0.0052(8) O2 0.0510(17) 0.0259(12) 0.0324(13) -0.0008(9) -0.0076(11) -0.0076(10) _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 C1 C2 1.355(3) . ? C1 N2 1.368(3) . ? C1 H1 0.9500 . ? C2 C3 1.413(3) . ? C2 H2 0.9500 . ? C3 C4 1.419(3) . ? C3 C8 1.428(3) . ? C4 C5 1.359(4) . ? C4 H4 0.9500 . ? C5 O3 1.354(3) . ? C5 C6 1.437(4) . ? C6 O4 1.351(3) . ? C6 C7 1.376(3) . ? C7 C8 1.420(3) . ? C7 H7 0.9500 . ? C8 C9 1.421(3) . ? C9 N2 1.338(3) . ? C9 C10 1.515(3) . ? C10 C11 1.520(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C16 1.389(3) . ? C11 C12 1.404(3) . ? C12 C13 1.384(3) . ? C12 H12 0.9500 . ? C13 O5 1.374(3) . ? C13 C14 1.408(3) . ? C14 O6 1.371(3) . ? C14 C15 1.388(3) . ? C15 C16 1.400(3) . ? C15 H15 0.9500 . ? C16 Pd1 2.005(2) . ? C17 O3 1.434(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 O4 1.428(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 O5 1.424(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 O6 1.422(3) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C26 1.393(3) . ? C21 C22 1.400(3) . ? C21 P1 1.823(2) . ? C22 C23 1.401(4) . ? C22 H22 0.9500 . ? C23 C24 1.378(5) . ? C23 H23 0.9500 . ? C24 C25 1.392(5) . ? C24 H24 0.9500 . ? C25 C26 1.383(4) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.390(3) . ? C27 C32 1.401(3) . ? C27 P1 1.822(2) . ? C28 C29 1.392(4) . ? C28 H28 0.9500 . ? C29 C30 1.383(4) . ? C29 H29 0.9500 . ? C30 C31 1.378(4) . ? C30 H30 0.9500 . ? C31 C32 1.384(3) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.385(3) . ? C33 C38 1.398(3) . ? C33 P1 1.824(2) . ? C34 C35 1.392(4) . ? C34 H34 0.9500 . ? C35 C36 1.372(4) . ? C35 H35 0.9500 . ? C36 C37 1.395(4) . ? C36 H36 0.9500 . ? C37 C38 1.378(4) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C40 Cl41 1.753(3) . ? C40 Cl42 1.759(3) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? N2 Pd1 2.1118(19) . ? P1 Pd1 2.2682(6) . ? Pd1 O1 2.145(2) . ? Pd1 N1A 2.175(13) . ? N1 O2 1.243(5) . ? N1 O1 1.250(4) . ? O1A N1A 1.174(15) . ? O2A N1A 1.205(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 N2 122.6(2) . . ? C2 C1 H1 118.7 . . ? N2 C1 H1 118.7 . . ? C1 C2 C3 119.7(2) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C2 C3 C4 122.0(2) . . ? C2 C3 C8 118.5(2) . . ? C4 C3 C8 119.5(2) . . ? C5 C4 C3 120.5(2) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? O3 C5 C4 125.9(2) . . ? O3 C5 C6 113.7(2) . . ? C4 C5 C6 120.4(2) . . ? O4 C6 C7 126.4(2) . . ? O4 C6 C5 113.3(2) . . ? C7 C6 C5 120.2(2) . . ? C6 C7 C8 120.1(2) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C7 C8 C9 123.3(2) . . ? C7 C8 C3 119.2(2) . . ? C9 C8 C3 117.5(2) . . ? N2 C9 C8 122.0(2) . . ? N2 C9 C10 114.49(18) . . ? C8 C9 C10 123.4(2) . . ? C9 C10 C11 107.85(18) . . ? C9 C10 H10A 110.1 . . ? C11 C10 H10A 110.1 . . ? C9 C10 H10B 110.1 . . ? C11 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? C16 C11 C12 120.6(2) . . ? C16 C11 C10 120.43(19) . . ? C12 C11 C10 118.49(19) . . ? C13 C12 C11 120.0(2) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? O5 C13 C12 125.2(2) . . ? O5 C13 C14 115.00(19) . . ? C12 C13 C14 119.8(2) . . ? O6 C14 C15 125.1(2) . . ? O6 C14 C13 115.19(19) . . ? C15 C14 C13 119.7(2) . . ? C14 C15 C16 120.9(2) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C11 C16 C15 119.0(2) . . ? C11 C16 Pd1 116.43(16) . . ? C15 C16 Pd1 123.21(16) . . ? O3 C17 H17A 109.5 . . ? O3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O4 C18 H18A 109.5 . . ? O4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O5 C19 H19A 109.5 . . ? O5 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O5 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O6 C20 H20A 109.5 . . ? O6 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O6 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C26 C21 C22 119.5(2) . . ? C26 C21 P1 118.15(18) . . ? C22 C21 P1 122.35(19) . . ? C21 C22 C23 119.0(3) . . ? C21 C22 H22 120.5 . . ? C23 C22 H22 120.5 . . ? C24 C23 C22 121.0(3) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C23 C24 C25 119.9(3) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C26 C25 C24 119.8(3) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C21 120.9(3) . . ? C25 C26 H26 119.6 . . ? C21 C26 H26 119.6 . . ? C28 C27 C32 118.3(2) . . ? C28 C27 P1 121.69(18) . . ? C32 C27 P1 120.01(18) . . ? C27 C28 C29 120.3(2) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C30 C29 C28 120.7(2) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C31 C30 C29 119.6(2) . . ? C31 C30 H30 120.2 . . ? C29 C30 H30 120.2 . . ? C30 C31 C32 120.1(2) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C31 C32 C27 121.0(2) . . ? C31 C32 H32 119.5 . . ? C27 C32 H32 119.5 . . ? C34 C33 C38 118.7(2) . . ? C34 C33 P1 123.37(19) . . ? C38 C33 P1 117.90(18) . . ? C33 C34 C35 120.4(3) . . ? C33 C34 H34 119.8 . . ? C35 C34 H34 119.8 . . ? C36 C35 C34 120.6(3) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C35 C36 C37 119.4(3) . . ? C35 C36 H36 120.3 . . ? C37 C36 H36 120.3 . . ? C38 C37 C36 120.2(3) . . ? C38 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C37 C38 C33 120.6(2) . . ? C37 C38 H38 119.7 . . ? C33 C38 H38 119.7 . . ? Cl41 C40 Cl42 111.26(19) . . ? Cl41 C40 H40A 109.4 . . ? Cl42 C40 H40A 109.4 . . ? Cl41 C40 H40B 109.4 . . ? Cl42 C40 H40B 109.4 . . ? H40A C40 H40B 108.0 . . ? C9 N2 C1 119.59(19) . . ? C9 N2 Pd1 121.12(15) . . ? C1 N2 Pd1 119.25(15) . . ? C5 O3 C17 116.4(2) . . ? C6 O4 C18 116.9(2) . . ? C13 O5 C19 116.00(18) . . ? C14 O6 C20 116.86(19) . . ? C27 P1 C21 102.50(11) . . ? C27 P1 C33 104.85(10) . . ? C21 P1 C33 104.38(11) . . ? C27 P1 Pd1 117.43(8) . . ? C21 P1 Pd1 111.66(8) . . ? C33 P1 Pd1 114.56(7) . . ? C16 Pd1 N2 85.35(8) . . ? C16 Pd1 O1 170.06(8) . . ? N2 Pd1 O1 84.74(7) . . ? C16 Pd1 N1A 157.8(3) . . ? N2 Pd1 N1A 90.3(3) . . ? O1 Pd1 N1A 23.3(3) . . ? C16 Pd1 P1 93.50(7) . . ? N2 Pd1 P1 174.80(6) . . ? O1 Pd1 P1 96.31(6) . . ? N1A Pd1 P1 92.6(3) . . ? O2 N1 O1 116.4(3) . . ? N1 O1 Pd1 118.48(19) . . ? O1A N1A O2A 119(3) . . ? O1A N1A Pd1 125.1(12) . . ? O2A N1A Pd1 116(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C1 C2 C3 1.6(4) . . . . ? C1 C2 C3 C4 -178.3(2) . . . . ? C1 C2 C3 C8 0.3(3) . . . . ? C2 C3 C4 C5 -179.3(2) . . . . ? C8 C3 C4 C5 2.1(4) . . . . ? C3 C4 C5 O3 179.8(3) . . . . ? C3 C4 C5 C6 1.1(4) . . . . ? O3 C5 C6 O4 -2.5(4) . . . . ? C4 C5 C6 O4 176.3(3) . . . . ? O3 C5 C6 C7 177.7(3) . . . . ? C4 C5 C6 C7 -3.4(4) . . . . ? O4 C6 C7 C8 -177.2(2) . . . . ? C5 C6 C7 C8 2.6(4) . . . . ? C6 C7 C8 C9 -178.4(2) . . . . ? C6 C7 C8 C3 0.6(3) . . . . ? C2 C3 C8 C7 178.5(2) . . . . ? C4 C3 C8 C7 -2.9(3) . . . . ? C2 C3 C8 C9 -2.5(3) . . . . ? C4 C3 C8 C9 176.1(2) . . . . ? C7 C8 C9 N2 -177.8(2) . . . . ? C3 C8 C9 N2 3.2(3) . . . . ? C7 C8 C9 C10 5.7(3) . . . . ? C3 C8 C9 C10 -173.26(19) . . . . ? N2 C9 C10 C11 -55.7(2) . . . . ? C8 C9 C10 C11 121.1(2) . . . . ? C9 C10 C11 C16 66.9(3) . . . . ? C9 C10 C11 C12 -105.5(2) . . . . ? C16 C11 C12 C13 -1.0(3) . . . . ? C10 C11 C12 C13 171.4(2) . . . . ? C11 C12 C13 O5 -177.3(2) . . . . ? C11 C12 C13 C14 1.8(3) . . . . ? O5 C13 C14 O6 -0.5(3) . . . . ? C12 C13 C14 O6 -179.7(2) . . . . ? O5 C13 C14 C15 178.2(2) . . . . ? C12 C13 C14 C15 -1.0(3) . . . . ? O6 C14 C15 C16 177.9(2) . . . . ? C13 C14 C15 C16 -0.7(3) . . . . ? C12 C11 C16 C15 -0.7(3) . . . . ? C10 C11 C16 C15 -172.9(2) . . . . ? C12 C11 C16 Pd1 166.19(16) . . . . ? C10 C11 C16 Pd1 -6.0(3) . . . . ? C14 C15 C16 C11 1.5(3) . . . . ? C14 C15 C16 Pd1 -164.43(18) . . . . ? C26 C21 C22 C23 0.3(4) . . . . ? P1 C21 C22 C23 178.7(2) . . . . ? C21 C22 C23 C24 -1.2(4) . . . . ? C22 C23 C24 C25 0.9(5) . . . . ? C23 C24 C25 C26 0.5(5) . . . . ? C24 C25 C26 C21 -1.4(4) . . . . ? C22 C21 C26 C25 1.0(4) . . . . ? P1 C21 C26 C25 -177.4(2) . . . . ? C32 C27 C28 C29 0.1(4) . . . . ? P1 C27 C28 C29 178.5(2) . . . . ? C27 C28 C29 C30 -0.4(5) . . . . ? C28 C29 C30 C31 0.0(4) . . . . ? C29 C30 C31 C32 0.7(4) . . . . ? C30 C31 C32 C27 -1.0(4) . . . . ? C28 C27 C32 C31 0.5(4) . . . . ? P1 C27 C32 C31 -177.88(18) . . . . ? C38 C33 C34 C35 -1.0(4) . . . . ? P1 C33 C34 C35 177.4(2) . . . . ? C33 C34 C35 C36 -0.8(4) . . . . ? C34 C35 C36 C37 1.4(4) . . . . ? C35 C36 C37 C38 -0.1(4) . . . . ? C36 C37 C38 C33 -1.8(4) . . . . ? C34 C33 C38 C37 2.3(4) . . . . ? P1 C33 C38 C37 -176.2(2) . . . . ? C8 C9 N2 C1 -1.5(3) . . . . ? C10 C9 N2 C1 175.29(19) . . . . ? C8 C9 N2 Pd1 176.01(15) . . . . ? C10 C9 N2 Pd1 -7.2(2) . . . . ? C2 C1 N2 C9 -1.0(3) . . . . ? C2 C1 N2 Pd1 -178.56(19) . . . . ? C4 C5 O3 C17 0.5(5) . . . . ? C6 C5 O3 C17 179.3(3) . . . . ? C7 C6 O4 C18 2.4(5) . . . . ? C5 C6 O4 C18 -177.4(3) . . . . ? C12 C13 O5 C19 2.9(3) . . . . ? C14 C13 O5 C19 -176.3(2) . . . . ? C15 C14 O6 C20 -3.6(3) . . . . ? C13 C14 O6 C20 175.0(2) . . . . ? C28 C27 P1 C21 142.3(2) . . . . ? C32 C27 P1 C21 -39.3(2) . . . . ? C28 C27 P1 C33 -108.9(2) . . . . ? C32 C27 P1 C33 69.5(2) . . . . ? C28 C27 P1 Pd1 19.6(2) . . . . ? C32 C27 P1 Pd1 -162.04(16) . . . . ? C26 C21 P1 C27 -78.1(2) . . . . ? C22 C21 P1 C27 103.5(2) . . . . ? C26 C21 P1 C33 172.76(19) . . . . ? C22 C21 P1 C33 -5.6(2) . . . . ? C26 C21 P1 Pd1 48.5(2) . . . . ? C22 C21 P1 Pd1 -129.91(19) . . . . ? C34 C33 P1 C27 -5.5(2) . . . . ? C38 C33 P1 C27 173.02(18) . . . . ? C34 C33 P1 C21 101.9(2) . . . . ? C38 C33 P1 C21 -79.6(2) . . . . ? C34 C33 P1 Pd1 -135.64(19) . . . . ? C38 C33 P1 Pd1 42.8(2) . . . . ? C11 C16 Pd1 N2 -40.66(17) . . . . ? C15 C16 Pd1 N2 125.6(2) . . . . ? C11 C16 Pd1 O1 -36.3(6) . . . . ? C15 C16 Pd1 O1 130.0(5) . . . . ? C11 C16 Pd1 N1A -120.1(9) . . . . ? C15 C16 Pd1 N1A 46.2(9) . . . . ? C11 C16 Pd1 P1 134.27(17) . . . . ? C15 C16 Pd1 P1 -59.45(19) . . . . ? C9 N2 Pd1 C16 50.76(17) . . . . ? C1 N2 Pd1 C16 -131.73(18) . . . . ? C9 N2 Pd1 O1 -128.48(18) . . . . ? C1 N2 Pd1 O1 49.03(18) . . . . ? C9 N2 Pd1 N1A -151.1(4) . . . . ? C1 N2 Pd1 N1A 26.4(4) . . . . ? C9 N2 Pd1 P1 -26.5(7) . . . . ? C1 N2 Pd1 P1 151.0(5) . . . . ? C27 P1 Pd1 C16 -59.28(11) . . . . ? C21 P1 Pd1 C16 -177.21(10) . . . . ? C33 P1 Pd1 C16 64.42(10) . . . . ? C27 P1 Pd1 N2 17.7(6) . . . . ? C21 P1 Pd1 N2 -100.3(6) . . . . ? C33 P1 Pd1 N2 141.4(6) . . . . ? C27 P1 Pd1 O1 119.08(11) . . . . ? C21 P1 Pd1 O1 1.15(11) . . . . ? C33 P1 Pd1 O1 -117.22(10) . . . . ? C27 P1 Pd1 N1A 142.1(3) . . . . ? C21 P1 Pd1 N1A 24.2(3) . . . . ? C33 P1 Pd1 N1A -94.2(3) . . . . ? O2 N1 O1 Pd1 -0.7(4) . . . . ? C16 Pd1 O1 N1 -117.1(5) . . . . ? N2 Pd1 O1 N1 -112.7(2) . . . . ? N1A Pd1 O1 N1 -9.5(8) . . . . ? P1 Pd1 O1 N1 72.4(2) . . . . ? C16 Pd1 N1A O1A 136.6(11) . . . . ? N2 Pd1 N1A O1A 58.1(12) . . . . ? O1 Pd1 N1A O1A -17.6(9) . . . . ? P1 Pd1 N1A O1A -117.6(12) . . . . ? C16 Pd1 N1A O2A -39(4) . . . . ? N2 Pd1 N1A O2A -117(4) . . . . ? O1 Pd1 N1A O2A 167(4) . . . . ? P1 Pd1 N1A O2A 67(4) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 33.64 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.622 _refine_diff_density_min -1.240 _refine_diff_density_rms 0.154 ### END # Attachment '- Complex 6_ijf1020m.cif' data_ijf1020m _database_code_depnum_ccdc_archive 'CCDC 858656' #TrackingRef '- Complex 6_ijf1020m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H46 N2 O12 Pd2, 3(C2 H3 N)' _chemical_formula_sum 'C50 H55 N5 O12 Pd2' _chemical_formula_weight 1130.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1250(17) _cell_length_b 15.392(2) _cell_length_c 15.758(2) _cell_angle_alpha 74.695(3) _cell_angle_beta 77.903(3) _cell_angle_gamma 70.463(3) _cell_volume 2430.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9094 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.545 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1156 _exptl_absorpt_coefficient_mu 0.808 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.755 _exptl_absorpt_correction_T_max 0.931 _exptl_absorpt_process_details 'SADABS v2.10 (Sheldrick)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24776 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0483 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 28.31 _reflns_number_total 11912 _reflns_number_gt 9784 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+1.1704P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11912 _refine_ls_number_parameters 635 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0507 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.0993 _refine_ls_wR_factor_gt 0.0932 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8468(3) 0.0728(2) 0.47930(18) 0.0213(6) Uani 1 1 d . . . H1 H 0.8001 0.0280 0.4945 0.026 Uiso 1 1 calc R . . C2 C 0.8663(3) 0.1068(2) 0.54523(18) 0.0218(6) Uani 1 1 d . . . H2 H 0.8351 0.0850 0.6053 0.026 Uiso 1 1 calc R . . C3 C 0.9334(3) 0.1747(2) 0.52330(18) 0.0207(5) Uani 1 1 d . . . C4 C 0.9547(3) 0.2145(2) 0.58893(19) 0.0251(6) Uani 1 1 d . . . H4 H 0.9262 0.1932 0.6497 0.030 Uiso 1 1 calc R . . C5 C 1.0158(3) 0.2832(2) 0.56536(19) 0.0276(6) Uani 1 1 d . . . C6 C 1.0602(3) 0.3148(2) 0.4733(2) 0.0264(6) Uani 1 1 d . . . C7 C 1.0433(3) 0.2768(2) 0.40907(18) 0.0233(6) Uani 1 1 d . . . H7 H 1.0741 0.2979 0.3487 0.028 Uiso 1 1 calc R . . C8 C 0.9793(3) 0.2049(2) 0.43243(18) 0.0201(5) Uani 1 1 d . . . C9 C 0.9586(3) 0.16381(19) 0.36821(17) 0.0185(5) Uani 1 1 d . . . C10 C 1.0071(3) 0.1890(2) 0.27075(17) 0.0208(6) Uani 1 1 d . . . H10A H 1.0620 0.2304 0.2624 0.025 Uiso 1 1 calc R . . H10B H 0.9329 0.2247 0.2377 0.025 Uiso 1 1 calc R . . C11 C 1.0838(3) 0.10277(19) 0.23259(17) 0.0192(5) Uani 1 1 d . . . C12 C 1.0303(3) 0.0309(2) 0.23963(17) 0.0188(5) Uani 1 1 d . . . C13 C 1.0993(3) -0.04308(19) 0.19618(17) 0.0200(5) Uani 1 1 d . . . H13 H 1.0633 -0.0922 0.2003 0.024 Uiso 1 1 calc R . . C14 C 1.2197(3) -0.0460(2) 0.14716(18) 0.0211(6) Uani 1 1 d . . . C15 C 1.2733(3) 0.0270(2) 0.14111(18) 0.0221(6) Uani 1 1 d . . . C16 C 1.2054(3) 0.1000(2) 0.18399(17) 0.0211(6) Uani 1 1 d . . . H16 H 1.2416 0.1489 0.1805 0.025 Uiso 1 1 calc R . . C17 C 1.0099(4) 0.2917(3) 0.7146(2) 0.0420(9) Uani 1 1 d . . . H17A H 0.9165 0.3045 0.7302 0.063 Uiso 1 1 calc R . . H17B H 1.0411 0.3234 0.7481 0.063 Uiso 1 1 calc R . . H17C H 1.0518 0.2236 0.7293 0.063 Uiso 1 1 calc R . . C18 C 1.1634(5) 0.4202(3) 0.3685(2) 0.0515(11) Uani 1 1 d . . . H18A H 1.2348 0.3702 0.3464 0.077 Uiso 1 1 calc R . . H18B H 1.1936 0.4740 0.3658 0.077 Uiso 1 1 calc R . . H18C H 1.0940 0.4404 0.3317 0.077 Uiso 1 1 calc R . . C19 C 1.2355(3) -0.1827(2) 0.0965(2) 0.0273(6) Uani 1 1 d . . . H19A H 1.2166 -0.2189 0.1563 0.041 Uiso 1 1 calc R . . H19B H 1.2950 -0.2255 0.0595 0.041 Uiso 1 1 calc R . . H19C H 1.1555 -0.1507 0.0702 0.041 Uiso 1 1 calc R . . C20 C 1.4611(3) 0.0793(3) 0.0944(2) 0.0327(7) Uani 1 1 d . . . H20A H 1.4103 0.1453 0.0767 0.049 Uiso 1 1 calc R . . H20B H 1.5425 0.0669 0.0546 0.049 Uiso 1 1 calc R . . H20C H 1.4788 0.0672 0.1555 0.049 Uiso 1 1 calc R . . C21 C 0.9319(3) 0.2332(2) 0.06321(17) 0.0204(5) Uani 1 1 d . . . H21 H 0.9671 0.1687 0.0897 0.024 Uiso 1 1 calc R . . C22 C 1.0117(3) 0.2804(2) 0.00719(18) 0.0220(6) Uani 1 1 d . . . H22 H 1.1014 0.2496 -0.0024 0.026 Uiso 1 1 calc R . . C23 C 0.9608(3) 0.37527(19) -0.03683(17) 0.0192(5) Uani 1 1 d . . . C24 C 1.0396(3) 0.4276(2) -0.09575(18) 0.0214(6) Uani 1 1 d . . . H24 H 1.1302 0.4000 -0.1046 0.026 Uiso 1 1 calc R . . C25 C 0.9853(3) 0.5179(2) -0.14010(18) 0.0211(6) Uani 1 1 d . . . C26 C 0.8485(3) 0.5601(2) -0.12723(18) 0.0218(6) Uani 1 1 d . . . C27 C 0.7718(3) 0.5113(2) -0.06886(18) 0.0205(5) Uani 1 1 d . . . H27 H 0.6814 0.5402 -0.0600 0.025 Uiso 1 1 calc R . . C28 C 0.8255(3) 0.41750(19) -0.02102(17) 0.0174(5) Uani 1 1 d . . . C29 C 0.7507(3) 0.36526(19) 0.04332(17) 0.0187(5) Uani 1 1 d . . . C30 C 0.6090(3) 0.4077(2) 0.07190(17) 0.0200(6) Uani 1 1 d . . . H30A H 0.5588 0.3766 0.0514 0.024 Uiso 1 1 calc R . . H30B H 0.5828 0.4756 0.0436 0.024 Uiso 1 1 calc R . . C31 C 0.5784(3) 0.3963(2) 0.17246(18) 0.0197(5) Uani 1 1 d . . . C32 C 0.6183(3) 0.3082(2) 0.22703(18) 0.0205(5) Uani 1 1 d . . . C33 C 0.5950(3) 0.2997(2) 0.31949(19) 0.0236(6) Uani 1 1 d . . . H33 H 0.6239 0.2397 0.3572 0.028 Uiso 1 1 calc R . . C34 C 0.5305(3) 0.3777(2) 0.35631(19) 0.0269(6) Uani 1 1 d . . . C35 C 0.4852(3) 0.4667(2) 0.3011(2) 0.0263(6) Uani 1 1 d . . . C36 C 0.5112(3) 0.4753(2) 0.2095(2) 0.0237(6) Uani 1 1 d . . . H36 H 0.4831 0.5354 0.1716 0.028 Uiso 1 1 calc R . . C37 C 1.1879(3) 0.5404(2) -0.2062(2) 0.0254(6) Uani 1 1 d . . . H37A H 1.2157 0.5256 -0.1476 0.038 Uiso 1 1 calc R . . H37B H 1.2242 0.5889 -0.2459 0.038 Uiso 1 1 calc R . . H37C H 1.2180 0.4834 -0.2307 0.038 Uiso 1 1 calc R . . C38 C 0.6717(3) 0.6888(2) -0.1776(2) 0.0272(6) Uani 1 1 d . . . H38A H 0.6383 0.6475 -0.1980 0.041 Uiso 1 1 calc R . . H38B H 0.6536 0.7510 -0.2177 0.041 Uiso 1 1 calc R . . H38C H 0.6299 0.6954 -0.1174 0.041 Uiso 1 1 calc R . . C39 C 0.5669(4) 0.2915(3) 0.5020(2) 0.0486(10) Uani 1 1 d . . . H39A H 0.5353 0.2405 0.4981 0.073 Uiso 1 1 calc R . . H39B H 0.5483 0.3000 0.5634 0.073 Uiso 1 1 calc R . . H39C H 0.6600 0.2754 0.4833 0.073 Uiso 1 1 calc R . . C40 C 0.3798(4) 0.6301(3) 0.2903(3) 0.0501(10) Uani 1 1 d . . . H40A H 0.4563 0.6484 0.2585 0.075 Uiso 1 1 calc R . . H40B H 0.3292 0.6751 0.3277 0.075 Uiso 1 1 calc R . . H40C H 0.3274 0.6303 0.2474 0.075 Uiso 1 1 calc R . . C41 C 0.8108(3) -0.0009(2) 0.14201(19) 0.0222(6) Uani 1 1 d . . . C42 C 0.8337(3) -0.0716(2) 0.0855(2) 0.0319(7) Uani 1 1 d . . . H42A H 0.7610 -0.0538 0.0520 0.048 Uiso 1 1 calc R . . H42B H 0.8418 -0.1344 0.1237 0.048 Uiso 1 1 calc R . . H42C H 0.9130 -0.0727 0.0440 0.048 Uiso 1 1 calc R . . C43 C 0.5653(3) 0.0898(2) 0.3325(2) 0.0264(6) Uani 1 1 d . . . C44 C 0.4347(3) 0.0840(3) 0.3812(2) 0.0450(10) Uani 1 1 d . . . H44A H 0.4459 0.0337 0.4348 0.068 Uiso 1 1 calc R . . H44B H 0.3882 0.0701 0.3425 0.068 Uiso 1 1 calc R . . H44C H 0.3854 0.1443 0.3980 0.068 Uiso 1 1 calc R . . N1 N 0.8924(2) 0.10079(16) 0.39163(14) 0.0192(5) Uani 1 1 d . . . N2 N 0.8032(2) 0.27543(16) 0.08268(14) 0.0186(5) Uani 1 1 d . . . O1 O 1.1159(2) 0.38495(17) 0.45914(14) 0.0351(5) Uani 1 1 d . . . O2 O 1.0398(2) 0.32655(16) 0.62120(14) 0.0343(5) Uani 1 1 d . . . O3 O 1.3909(2) 0.01923(16) 0.08915(14) 0.0271(5) Uani 1 1 d . . . O4 O 1.2928(2) -0.11461(15) 0.10156(14) 0.0271(5) Uani 1 1 d . . . O5 O 1.05019(19) 0.57463(15) -0.19781(14) 0.0263(5) Uani 1 1 d . . . O6 O 0.80800(19) 0.64866(14) -0.17721(14) 0.0250(4) Uani 1 1 d . . . O7 O 0.4181(2) 0.53894(17) 0.34392(16) 0.0370(5) Uani 1 1 d . . . O8 O 0.5046(2) 0.37644(18) 0.44565(14) 0.0391(6) Uani 1 1 d . . . O9 O 0.82739(19) -0.03452(14) 0.22330(13) 0.0218(4) Uani 1 1 d . . . O10 O 0.7805(2) 0.08428(14) 0.10470(13) 0.0246(4) Uani 1 1 d . . . O11 O 0.66198(19) 0.05302(15) 0.37363(13) 0.0241(4) Uani 1 1 d . . . O12 O 0.56536(19) 0.13562(15) 0.25262(13) 0.0241(4) Uani 1 1 d . . . Pd1 Pd 0.854256(19) 0.041401(15) 0.303273(13) 0.01814(6) Uani 1 1 d . . . Pd2 Pd 0.69817(2) 0.198186(14) 0.172528(13) 0.01802(6) Uani 1 1 d . . . C45 C 0.5842(4) 0.7229(3) 0.0903(3) 0.0420(9) Uani 1 1 d . . . C46 C 0.5928(4) 0.7949(3) 0.1311(3) 0.0560(11) Uani 1 1 d . . . H46A H 0.6493 0.8297 0.0910 0.084 Uiso 1 1 calc R . . H46B H 0.6282 0.7648 0.1872 0.084 Uiso 1 1 calc R . . H46C H 0.5068 0.8386 0.1424 0.084 Uiso 1 1 calc R . . C47 C 0.2771(4) 0.4245(3) 0.6195(3) 0.0461(9) Uani 1 1 d . . . C48 C 0.2439(5) 0.5086(3) 0.5488(3) 0.0584(12) Uani 1 1 d . . . H48A H 0.1686 0.5098 0.5250 0.088 Uiso 1 1 calc R . . H48B H 0.3168 0.5071 0.5013 0.088 Uiso 1 1 calc R . . H48C H 0.2241 0.5651 0.5729 0.088 Uiso 1 1 calc R . . C49 C 0.4480(7) 0.1344(4) 0.6570(4) 0.0799(18) Uani 1 1 d . . . C50 C 0.3301(5) 0.1621(4) 0.6157(4) 0.0753(16) Uani 1 1 d . . . H50A H 0.3061 0.2299 0.5904 0.113 Uiso 1 1 calc R . . H50B H 0.2602 0.1473 0.6607 0.113 Uiso 1 1 calc R . . H50C H 0.3453 0.1274 0.5686 0.113 Uiso 1 1 calc R . . N3 N 0.5742(4) 0.6681(2) 0.0586(2) 0.0535(9) Uani 1 1 d . . . N4 N 0.3016(4) 0.3608(3) 0.6739(3) 0.0629(10) Uani 1 1 d . . . N5 N 0.5418(7) 0.1138(4) 0.6880(4) 0.128(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0177(13) 0.0225(14) 0.0200(13) -0.0004(11) -0.0024(11) -0.0044(11) C2 0.0199(14) 0.0228(14) 0.0179(13) -0.0015(11) -0.0022(11) -0.0024(11) C3 0.0196(14) 0.0199(13) 0.0193(13) -0.0025(11) -0.0043(11) -0.0020(11) C4 0.0283(16) 0.0278(15) 0.0177(13) -0.0012(11) -0.0039(11) -0.0084(13) C5 0.0329(17) 0.0286(16) 0.0224(14) -0.0058(12) -0.0073(12) -0.0082(13) C6 0.0295(16) 0.0243(15) 0.0269(15) -0.0054(12) -0.0037(12) -0.0100(13) C7 0.0256(15) 0.0247(15) 0.0181(13) -0.0020(11) -0.0020(11) -0.0082(12) C8 0.0186(13) 0.0198(13) 0.0187(12) -0.0030(10) -0.0044(10) -0.0013(11) C9 0.0174(13) 0.0165(13) 0.0186(12) -0.0008(10) -0.0046(10) -0.0021(10) C10 0.0217(14) 0.0206(14) 0.0189(13) -0.0022(10) -0.0044(11) -0.0053(11) C11 0.0219(14) 0.0207(13) 0.0140(12) -0.0012(10) -0.0055(10) -0.0050(11) C12 0.0181(13) 0.0216(13) 0.0145(12) -0.0009(10) -0.0036(10) -0.0046(11) C13 0.0223(14) 0.0187(13) 0.0186(12) -0.0012(10) -0.0053(11) -0.0059(11) C14 0.0214(14) 0.0235(14) 0.0177(12) -0.0054(11) -0.0051(11) -0.0033(12) C15 0.0199(14) 0.0285(15) 0.0177(12) -0.0047(11) -0.0017(11) -0.0074(12) C16 0.0222(14) 0.0252(14) 0.0181(12) -0.0036(11) -0.0044(11) -0.0094(12) C17 0.065(3) 0.051(2) 0.0207(15) -0.0096(15) -0.0034(16) -0.032(2) C18 0.081(3) 0.062(3) 0.0302(18) -0.0118(18) 0.0101(19) -0.054(3) C19 0.0280(16) 0.0247(15) 0.0284(15) -0.0084(12) 0.0006(12) -0.0071(13) C20 0.0262(16) 0.0399(19) 0.0364(17) -0.0139(15) 0.0055(13) -0.0166(15) C21 0.0212(14) 0.0201(13) 0.0172(12) -0.0034(10) -0.0059(11) -0.0011(11) C22 0.0177(14) 0.0237(14) 0.0203(13) -0.0048(11) -0.0034(11) 0.0002(11) C23 0.0179(13) 0.0196(13) 0.0186(12) -0.0056(10) -0.0031(10) -0.0020(11) C24 0.0131(13) 0.0256(14) 0.0222(13) -0.0046(11) -0.0018(10) -0.0022(11) C25 0.0183(13) 0.0262(14) 0.0194(13) -0.0029(11) -0.0029(11) -0.0087(12) C26 0.0210(14) 0.0201(14) 0.0226(13) 0.0003(11) -0.0072(11) -0.0049(11) C27 0.0149(13) 0.0220(14) 0.0217(13) -0.0024(11) -0.0022(10) -0.0036(11) C28 0.0160(13) 0.0172(13) 0.0187(12) -0.0038(10) -0.0039(10) -0.0034(10) C29 0.0165(13) 0.0207(13) 0.0176(12) -0.0051(10) -0.0037(10) -0.0021(11) C30 0.0151(13) 0.0195(13) 0.0214(13) 0.0019(11) -0.0038(10) -0.0039(11) C31 0.0124(12) 0.0241(14) 0.0222(13) -0.0047(11) -0.0021(10) -0.0049(11) C32 0.0147(13) 0.0245(14) 0.0227(13) -0.0058(11) -0.0027(10) -0.0056(11) C33 0.0202(14) 0.0256(15) 0.0216(13) -0.0041(11) -0.0033(11) -0.0029(12) C34 0.0228(15) 0.0330(17) 0.0218(14) -0.0085(12) -0.0025(12) -0.0024(13) C35 0.0197(14) 0.0252(15) 0.0317(15) -0.0118(12) -0.0005(12) -0.0011(12) C36 0.0162(13) 0.0237(14) 0.0288(14) -0.0047(12) -0.0027(11) -0.0036(11) C37 0.0174(14) 0.0318(16) 0.0270(14) -0.0057(12) 0.0008(11) -0.0098(12) C38 0.0173(14) 0.0241(15) 0.0353(16) 0.0007(12) -0.0061(12) -0.0036(12) C39 0.058(3) 0.049(2) 0.0249(17) -0.0093(16) -0.0069(17) 0.003(2) C40 0.058(3) 0.032(2) 0.046(2) -0.0135(17) -0.0069(19) 0.0097(18) C41 0.0183(14) 0.0243(14) 0.0248(14) -0.0058(11) -0.0038(11) -0.0063(11) C42 0.0394(19) 0.0263(16) 0.0340(17) -0.0108(13) -0.0148(14) -0.0053(14) C43 0.0218(15) 0.0322(16) 0.0261(14) -0.0020(12) -0.0045(12) -0.0114(13) C44 0.0265(18) 0.067(3) 0.0344(18) 0.0067(18) -0.0022(15) -0.0187(18) N1 0.0165(11) 0.0210(12) 0.0172(11) -0.0009(9) -0.0046(9) -0.0029(9) N2 0.0180(11) 0.0204(12) 0.0170(10) -0.0054(9) -0.0028(9) -0.0035(9) O1 0.0522(15) 0.0384(13) 0.0245(11) -0.0079(10) 0.0024(10) -0.0297(12) O2 0.0533(15) 0.0360(13) 0.0218(10) -0.0083(9) -0.0041(10) -0.0226(12) O3 0.0199(10) 0.0348(12) 0.0310(11) -0.0148(9) 0.0034(9) -0.0116(9) O4 0.0213(11) 0.0302(11) 0.0325(11) -0.0151(9) 0.0004(9) -0.0070(9) O5 0.0160(10) 0.0270(11) 0.0314(11) 0.0027(9) -0.0028(8) -0.0077(9) O6 0.0171(10) 0.0210(10) 0.0316(11) 0.0045(8) -0.0062(8) -0.0047(8) O7 0.0375(13) 0.0304(12) 0.0351(12) -0.0141(10) 0.0007(10) 0.0026(10) O8 0.0413(14) 0.0422(14) 0.0223(11) -0.0106(10) -0.0045(10) 0.0056(11) O9 0.0221(10) 0.0210(10) 0.0226(10) -0.0026(8) -0.0053(8) -0.0068(8) O10 0.0322(12) 0.0212(10) 0.0202(9) -0.0037(8) -0.0060(8) -0.0065(9) O11 0.0194(10) 0.0300(11) 0.0212(9) -0.0006(8) -0.0043(8) -0.0077(9) O12 0.0219(10) 0.0260(11) 0.0232(10) 0.0019(8) -0.0070(8) -0.0085(9) Pd1 0.01669(11) 0.02024(11) 0.01668(10) -0.00096(8) -0.00391(8) -0.00568(8) Pd2 0.01829(11) 0.01758(11) 0.01690(10) -0.00167(8) -0.00366(8) -0.00436(8) C45 0.0333(19) 0.037(2) 0.047(2) -0.0001(17) -0.0009(16) -0.0092(16) C46 0.041(2) 0.052(3) 0.078(3) -0.008(2) -0.024(2) -0.013(2) C47 0.052(2) 0.040(2) 0.047(2) -0.0266(19) -0.0110(19) 0.0009(18) C48 0.071(3) 0.051(3) 0.038(2) -0.0165(19) -0.005(2) 0.006(2) C49 0.126(6) 0.040(3) 0.051(3) -0.001(2) -0.003(3) -0.006(3) C50 0.079(4) 0.054(3) 0.090(4) -0.018(3) 0.013(3) -0.029(3) N3 0.066(2) 0.0380(19) 0.049(2) -0.0060(16) 0.0046(17) -0.0150(18) N4 0.085(3) 0.049(2) 0.056(2) -0.0195(19) -0.021(2) -0.008(2) N5 0.170(7) 0.087(4) 0.092(4) -0.004(3) -0.061(4) 0.020(4) _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 C1 C2 1.364(4) . ? C1 N1 1.375(3) . ? C1 H1 0.9500 . ? C2 C3 1.412(4) . ? C2 H2 0.9500 . ? C3 C8 1.424(4) . ? C3 C4 1.426(4) . ? C4 C5 1.374(4) . ? C4 H4 0.9500 . ? C5 O2 1.348(4) . ? C5 C6 1.440(4) . ? C6 O1 1.365(3) . ? C6 C7 1.366(4) . ? C7 C8 1.438(4) . ? C7 H7 0.9500 . ? C8 C9 1.418(4) . ? C9 N1 1.339(3) . ? C9 C10 1.510(4) . ? C10 C11 1.517(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.391(4) . ? C11 C16 1.402(4) . ? C12 C13 1.401(4) . ? C12 Pd1 1.980(3) . ? C13 C14 1.391(4) . ? C13 H13 0.9500 . ? C14 O4 1.370(3) . ? C14 C15 1.413(4) . ? C15 O3 1.376(3) . ? C15 C16 1.381(4) . ? C16 H16 0.9500 . ? C17 O2 1.436(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 O1 1.442(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 O4 1.423(4) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 O3 1.423(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.363(4) . ? C21 N2 1.366(4) . ? C21 H21 0.9500 . ? C22 C23 1.418(4) . ? C22 H22 0.9500 . ? C23 C24 1.419(4) . ? C23 C28 1.422(4) . ? C24 C25 1.374(4) . ? C24 H24 0.9500 . ? C25 O5 1.355(3) . ? C25 C26 1.435(4) . ? C26 O6 1.361(3) . ? C26 C27 1.369(4) . ? C27 C28 1.431(4) . ? C27 H27 0.9500 . ? C28 C29 1.425(4) . ? C29 N2 1.340(3) . ? C29 C30 1.511(4) . ? C30 C31 1.525(4) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.385(4) . ? C31 C36 1.400(4) . ? C32 C33 1.404(4) . ? C32 Pd2 1.959(3) . ? C33 C34 1.381(4) . ? C33 H33 0.9500 . ? C34 O8 1.373(4) . ? C34 C35 1.407(4) . ? C35 O7 1.371(4) . ? C35 C36 1.392(4) . ? C36 H36 0.9500 . ? C37 O5 1.433(3) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 O6 1.434(3) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 O8 1.420(4) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 O7 1.411(4) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 O10 1.248(3) . ? C41 O9 1.276(3) . ? C41 C42 1.508(4) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 O11 1.261(3) . ? C43 O12 1.270(3) . ? C43 C44 1.514(4) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? N1 Pd1 2.033(2) . ? N2 Pd2 2.032(2) . ? O9 Pd1 2.0523(19) . ? O10 Pd2 2.135(2) . ? O11 Pd1 2.166(2) . ? O12 Pd2 2.0571(19) . ? Pd1 Pd2 3.0258(4) . ? C45 N3 1.132(5) . ? C45 C46 1.457(6) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 N4 1.116(5) . ? C47 C48 1.464(6) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 N5 1.158(9) . ? C49 C50 1.470(9) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 N1 122.4(3) . . ? C2 C1 H1 118.8 . . ? N1 C1 H1 118.8 . . ? C1 C2 C3 119.3(3) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C2 C3 C8 118.4(3) . . ? C2 C3 C4 122.1(3) . . ? C8 C3 C4 119.5(3) . . ? C5 C4 C3 120.8(3) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? O2 C5 C4 126.1(3) . . ? O2 C5 C6 114.4(3) . . ? C4 C5 C6 119.6(3) . . ? O1 C6 C7 125.7(3) . . ? O1 C6 C5 113.4(3) . . ? C7 C6 C5 120.9(3) . . ? C6 C7 C8 120.3(3) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C9 C8 C3 118.7(2) . . ? C9 C8 C7 122.5(2) . . ? C3 C8 C7 118.8(2) . . ? N1 C9 C8 120.9(2) . . ? N1 C9 C10 116.5(2) . . ? C8 C9 C10 122.6(2) . . ? C9 C10 C11 112.5(2) . . ? C9 C10 H10A 109.1 . . ? C11 C10 H10A 109.1 . . ? C9 C10 H10B 109.1 . . ? C11 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? C12 C11 C16 120.4(3) . . ? C12 C11 C10 120.6(2) . . ? C16 C11 C10 118.9(2) . . ? C11 C12 C13 118.8(2) . . ? C11 C12 Pd1 118.9(2) . . ? C13 C12 Pd1 122.1(2) . . ? C14 C13 C12 121.2(3) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? O4 C14 C13 125.1(3) . . ? O4 C14 C15 115.4(2) . . ? C13 C14 C15 119.4(3) . . ? O3 C15 C16 125.5(3) . . ? O3 C15 C14 115.0(3) . . ? C16 C15 C14 119.4(3) . . ? C15 C16 C11 120.8(3) . . ? C15 C16 H16 119.6 . . ? C11 C16 H16 119.6 . . ? O2 C17 H17A 109.5 . . ? O2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O1 C18 H18A 109.5 . . ? O1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O4 C19 H19A 109.5 . . ? O4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O3 C20 H20A 109.5 . . ? O3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 N2 122.3(3) . . ? C22 C21 H21 118.8 . . ? N2 C21 H21 118.8 . . ? C21 C22 C23 120.1(3) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C22 C23 C24 122.3(3) . . ? C22 C23 C28 117.7(2) . . ? C24 C23 C28 120.0(2) . . ? C25 C24 C23 120.3(3) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? O5 C25 C24 125.8(3) . . ? O5 C25 C26 114.0(2) . . ? C24 C25 C26 120.2(2) . . ? O6 C26 C27 126.1(3) . . ? O6 C26 C25 113.8(2) . . ? C27 C26 C25 120.0(3) . . ? C26 C27 C28 121.0(3) . . ? C26 C27 H27 119.5 . . ? C28 C27 H27 119.5 . . ? C23 C28 C29 118.4(2) . . ? C23 C28 C27 118.3(2) . . ? C29 C28 C27 123.2(2) . . ? N2 C29 C28 121.5(2) . . ? N2 C29 C30 116.2(2) . . ? C28 C29 C30 122.3(2) . . ? C29 C30 C31 111.7(2) . . ? C29 C30 H30A 109.3 . . ? C31 C30 H30A 109.3 . . ? C29 C30 H30B 109.3 . . ? C31 C30 H30B 109.3 . . ? H30A C30 H30B 107.9 . . ? C32 C31 C36 120.1(3) . . ? C32 C31 C30 120.0(3) . . ? C36 C31 C30 119.9(2) . . ? C31 C32 C33 119.3(3) . . ? C31 C32 Pd2 118.7(2) . . ? C33 C32 Pd2 122.0(2) . . ? C34 C33 C32 120.8(3) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? O8 C34 C33 124.9(3) . . ? O8 C34 C35 115.0(3) . . ? C33 C34 C35 120.0(3) . . ? O7 C35 C36 125.2(3) . . ? O7 C35 C34 115.7(3) . . ? C36 C35 C34 119.0(3) . . ? C35 C36 C31 120.6(3) . . ? C35 C36 H36 119.7 . . ? C31 C36 H36 119.7 . . ? O5 C37 H37A 109.5 . . ? O5 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? O5 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O6 C38 H38A 109.5 . . ? O6 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? O6 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O8 C39 H39A 109.5 . . ? O8 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? O8 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O7 C40 H40A 109.5 . . ? O7 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? O7 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O10 C41 O9 126.4(3) . . ? O10 C41 C42 117.3(3) . . ? O9 C41 C42 116.4(3) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O11 C43 O12 125.8(3) . . ? O11 C43 C44 119.0(3) . . ? O12 C43 C44 115.2(3) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C9 N1 C1 120.1(2) . . ? C9 N1 Pd1 123.35(18) . . ? C1 N1 Pd1 116.52(18) . . ? C29 N2 C21 119.8(2) . . ? C29 N2 Pd2 122.36(19) . . ? C21 N2 Pd2 117.85(18) . . ? C6 O1 C18 116.8(2) . . ? C5 O2 C17 117.1(2) . . ? C15 O3 C20 117.4(2) . . ? C14 O4 C19 117.2(2) . . ? C25 O5 C37 116.6(2) . . ? C26 O6 C38 116.3(2) . . ? C35 O7 C40 116.9(3) . . ? C34 O8 C39 116.1(3) . . ? C41 O9 Pd1 123.29(18) . . ? C41 O10 Pd2 124.62(18) . . ? C43 O11 Pd1 120.61(18) . . ? C43 O12 Pd2 129.82(18) . . ? C12 Pd1 N1 89.38(10) . . ? C12 Pd1 O9 89.63(10) . . ? N1 Pd1 O9 172.82(8) . . ? C12 Pd1 O11 179.64(9) . . ? N1 Pd1 O11 90.27(8) . . ? O9 Pd1 O11 90.70(8) . . ? C12 Pd1 Pd2 100.41(7) . . ? N1 Pd1 Pd2 107.87(6) . . ? O9 Pd1 Pd2 79.30(6) . . ? O11 Pd1 Pd2 79.80(5) . . ? C32 Pd2 N2 87.44(10) . . ? C32 Pd2 O12 89.13(10) . . ? N2 Pd2 O12 170.10(8) . . ? C32 Pd2 O10 176.00(9) . . ? N2 Pd2 O10 90.48(9) . . ? O12 Pd2 O10 92.36(8) . . ? C32 Pd2 Pd1 108.26(8) . . ? N2 Pd2 Pd1 113.71(6) . . ? O12 Pd2 Pd1 76.19(6) . . ? O10 Pd2 Pd1 75.71(5) . . ? N3 C45 C46 178.2(4) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N4 C47 C48 179.4(5) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N5 C49 C50 178.6(7) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? 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 N1 C1 C2 C3 1.3(4) . . . . ? C1 C2 C3 C8 -0.4(4) . . . . ? C1 C2 C3 C4 178.7(3) . . . . ? C2 C3 C4 C5 -177.4(3) . . . . ? C8 C3 C4 C5 1.7(4) . . . . ? C3 C4 C5 O2 179.2(3) . . . . ? C3 C4 C5 C6 -0.7(5) . . . . ? O2 C5 C6 O1 -1.5(4) . . . . ? C4 C5 C6 O1 178.3(3) . . . . ? O2 C5 C6 C7 179.6(3) . . . . ? C4 C5 C6 C7 -0.6(5) . . . . ? O1 C6 C7 C8 -178.1(3) . . . . ? C5 C6 C7 C8 0.7(5) . . . . ? C2 C3 C8 C9 -1.6(4) . . . . ? C4 C3 C8 C9 179.3(3) . . . . ? C2 C3 C8 C7 177.6(3) . . . . ? C4 C3 C8 C7 -1.6(4) . . . . ? C6 C7 C8 C9 179.5(3) . . . . ? C6 C7 C8 C3 0.4(4) . . . . ? C3 C8 C9 N1 2.8(4) . . . . ? C7 C8 C9 N1 -176.3(3) . . . . ? C3 C8 C9 C10 -178.1(3) . . . . ? C7 C8 C9 C10 2.8(4) . . . . ? N1 C9 C10 C11 -52.8(3) . . . . ? C8 C9 C10 C11 128.1(3) . . . . ? C9 C10 C11 C12 55.7(3) . . . . ? C9 C10 C11 C16 -129.3(3) . . . . ? C16 C11 C12 C13 -1.0(4) . . . . ? C10 C11 C12 C13 173.9(2) . . . . ? C16 C11 C12 Pd1 -176.62(19) . . . . ? C10 C11 C12 Pd1 -1.7(3) . . . . ? C11 C12 C13 C14 0.5(4) . . . . ? Pd1 C12 C13 C14 175.9(2) . . . . ? C12 C13 C14 O4 -178.9(2) . . . . ? C12 C13 C14 C15 0.0(4) . . . . ? O4 C14 C15 O3 0.8(4) . . . . ? C13 C14 C15 O3 -178.2(2) . . . . ? O4 C14 C15 C16 179.1(2) . . . . ? C13 C14 C15 C16 0.0(4) . . . . ? O3 C15 C16 C11 177.5(3) . . . . ? C14 C15 C16 C11 -0.6(4) . . . . ? C12 C11 C16 C15 1.1(4) . . . . ? C10 C11 C16 C15 -173.9(2) . . . . ? N2 C21 C22 C23 -3.3(4) . . . . ? C21 C22 C23 C24 180.0(3) . . . . ? C21 C22 C23 C28 -0.8(4) . . . . ? C22 C23 C24 C25 177.0(3) . . . . ? C28 C23 C24 C25 -2.2(4) . . . . ? C23 C24 C25 O5 -180.0(3) . . . . ? C23 C24 C25 C26 -0.1(4) . . . . ? O5 C25 C26 O6 1.7(4) . . . . ? C24 C25 C26 O6 -178.2(3) . . . . ? O5 C25 C26 C27 -178.3(3) . . . . ? C24 C25 C26 C27 1.8(4) . . . . ? O6 C26 C27 C28 178.9(3) . . . . ? C25 C26 C27 C28 -1.1(4) . . . . ? C22 C23 C28 C29 5.2(4) . . . . ? C24 C23 C28 C29 -175.6(2) . . . . ? C22 C23 C28 C27 -176.4(2) . . . . ? C24 C23 C28 C27 2.9(4) . . . . ? C26 C27 C28 C23 -1.2(4) . . . . ? C26 C27 C28 C29 177.1(3) . . . . ? C23 C28 C29 N2 -6.0(4) . . . . ? C27 C28 C29 N2 175.7(2) . . . . ? C23 C28 C29 C30 173.3(2) . . . . ? C27 C28 C29 C30 -5.0(4) . . . . ? N2 C29 C30 C31 53.0(3) . . . . ? C28 C29 C30 C31 -126.3(3) . . . . ? C29 C30 C31 C32 -52.4(3) . . . . ? C29 C30 C31 C36 126.9(3) . . . . ? C36 C31 C32 C33 -2.5(4) . . . . ? C30 C31 C32 C33 176.8(2) . . . . ? C36 C31 C32 Pd2 174.6(2) . . . . ? C30 C31 C32 Pd2 -6.1(3) . . . . ? C31 C32 C33 C34 1.5(4) . . . . ? Pd2 C32 C33 C34 -175.5(2) . . . . ? C32 C33 C34 O8 -179.3(3) . . . . ? C32 C33 C34 C35 1.2(4) . . . . ? O8 C34 C35 O7 -2.0(4) . . . . ? C33 C34 C35 O7 177.6(3) . . . . ? O8 C34 C35 C36 177.6(3) . . . . ? C33 C34 C35 C36 -2.8(5) . . . . ? O7 C35 C36 C31 -178.6(3) . . . . ? C34 C35 C36 C31 1.8(4) . . . . ? C32 C31 C36 C35 0.9(4) . . . . ? C30 C31 C36 C35 -178.5(3) . . . . ? C8 C9 N1 C1 -2.0(4) . . . . ? C10 C9 N1 C1 178.8(2) . . . . ? C8 C9 N1 Pd1 178.3(2) . . . . ? C10 C9 N1 Pd1 -0.9(3) . . . . ? C2 C1 N1 C9 0.0(4) . . . . ? C2 C1 N1 Pd1 179.7(2) . . . . ? C28 C29 N2 C21 2.0(4) . . . . ? C30 C29 N2 C21 -177.3(2) . . . . ? C28 C29 N2 Pd2 -178.56(19) . . . . ? C30 C29 N2 Pd2 2.1(3) . . . . ? C22 C21 N2 C29 2.7(4) . . . . ? C22 C21 N2 Pd2 -176.7(2) . . . . ? C7 C6 O1 C18 -1.4(5) . . . . ? C5 C6 O1 C18 179.8(3) . . . . ? C4 C5 O2 C17 6.3(5) . . . . ? C6 C5 O2 C17 -173.8(3) . . . . ? C16 C15 O3 C20 14.0(4) . . . . ? C14 C15 O3 C20 -167.9(3) . . . . ? C13 C14 O4 C19 6.8(4) . . . . ? C15 C14 O4 C19 -172.2(2) . . . . ? C24 C25 O5 C37 -6.6(4) . . . . ? C26 C25 O5 C37 173.5(2) . . . . ? C27 C26 O6 C38 -9.2(4) . . . . ? C25 C26 O6 C38 170.8(3) . . . . ? C36 C35 O7 C40 -4.2(5) . . . . ? C34 C35 O7 C40 175.4(3) . . . . ? C33 C34 O8 C39 10.3(5) . . . . ? C35 C34 O8 C39 -170.1(3) . . . . ? O10 C41 O9 Pd1 -16.7(4) . . . . ? C42 C41 O9 Pd1 161.5(2) . . . . ? O9 C41 O10 Pd2 -17.8(4) . . . . ? C42 C41 O10 Pd2 164.0(2) . . . . ? O12 C43 O11 Pd1 -11.6(4) . . . . ? C44 C43 O11 Pd1 171.2(3) . . . . ? O11 C43 O12 Pd2 -18.5(5) . . . . ? C44 C43 O12 Pd2 158.9(2) . . . . ? C11 C12 Pd1 N1 -37.1(2) . . . . ? C13 C12 Pd1 N1 147.5(2) . . . . ? C11 C12 Pd1 O9 150.0(2) . . . . ? C13 C12 Pd1 O9 -25.4(2) . . . . ? C11 C12 Pd1 O11 -54(17) . . . . ? C13 C12 Pd1 O11 131(17) . . . . ? C11 C12 Pd1 Pd2 71.0(2) . . . . ? C13 C12 Pd1 Pd2 -104.5(2) . . . . ? C9 N1 Pd1 C12 40.3(2) . . . . ? C1 N1 Pd1 C12 -139.4(2) . . . . ? C9 N1 Pd1 O9 122.4(6) . . . . ? C1 N1 Pd1 O9 -57.3(7) . . . . ? C9 N1 Pd1 O11 -139.8(2) . . . . ? C1 N1 Pd1 O11 40.5(2) . . . . ? C9 N1 Pd1 Pd2 -60.4(2) . . . . ? C1 N1 Pd1 Pd2 119.90(19) . . . . ? C41 O9 Pd1 C12 -73.2(2) . . . . ? C41 O9 Pd1 N1 -155.3(6) . . . . ? C41 O9 Pd1 O11 106.9(2) . . . . ? C41 O9 Pd1 Pd2 27.4(2) . . . . ? C43 O11 Pd1 C12 146(26) . . . . ? C43 O11 Pd1 N1 129.5(2) . . . . ? C43 O11 Pd1 O9 -57.6(2) . . . . ? C43 O11 Pd1 Pd2 21.4(2) . . . . ? C31 C32 Pd2 N2 44.8(2) . . . . ? C33 C32 Pd2 N2 -138.2(2) . . . . ? C31 C32 Pd2 O12 -125.9(2) . . . . ? C33 C32 Pd2 O12 51.1(2) . . . . ? C31 C32 Pd2 O10 -13.9(15) . . . . ? C33 C32 Pd2 O10 163.1(12) . . . . ? C31 C32 Pd2 Pd1 158.95(19) . . . . ? C33 C32 Pd2 Pd1 -24.1(2) . . . . ? C29 N2 Pd2 C32 -44.9(2) . . . . ? C21 N2 Pd2 C32 134.5(2) . . . . ? C29 N2 Pd2 O12 25.0(6) . . . . ? C21 N2 Pd2 O12 -155.6(4) . . . . ? C29 N2 Pd2 O10 131.7(2) . . . . ? C21 N2 Pd2 O10 -48.87(19) . . . . ? C29 N2 Pd2 Pd1 -153.71(18) . . . . ? C21 N2 Pd2 Pd1 25.7(2) . . . . ? C43 O12 Pd2 C32 -82.8(3) . . . . ? C43 O12 Pd2 N2 -152.5(5) . . . . ? C43 O12 Pd2 O10 100.9(3) . . . . ? C43 O12 Pd2 Pd1 26.3(3) . . . . ? C41 O10 Pd2 C32 -159.4(13) . . . . ? C41 O10 Pd2 N2 142.0(2) . . . . ? C41 O10 Pd2 O12 -47.5(2) . . . . ? C41 O10 Pd2 Pd1 27.6(2) . . . . ? C12 Pd1 Pd2 C32 -113.51(12) . . . . ? N1 Pd1 Pd2 C32 -20.78(11) . . . . ? O9 Pd1 Pd2 C32 158.86(10) . . . . ? O11 Pd1 Pd2 C32 66.19(10) . . . . ? C12 Pd1 Pd2 N2 -18.14(11) . . . . ? N1 Pd1 Pd2 N2 74.59(10) . . . . ? O9 Pd1 Pd2 N2 -105.76(9) . . . . ? O11 Pd1 Pd2 N2 161.56(9) . . . . ? C12 Pd1 Pd2 O12 162.09(10) . . . . ? N1 Pd1 Pd2 O12 -105.18(9) . . . . ? O9 Pd1 Pd2 O12 74.46(8) . . . . ? O11 Pd1 Pd2 O12 -18.22(8) . . . . ? C12 Pd1 Pd2 O10 65.98(10) . . . . ? N1 Pd1 Pd2 O10 158.71(9) . . . . ? O9 Pd1 Pd2 O10 -21.65(8) . . . . ? O11 Pd1 Pd2 O10 -114.33(8) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.691 _refine_diff_density_min -0.774 _refine_diff_density_rms 0.102 ### END # Attachment '- Pd(NO2)2(N-Hpap)2_ijsf1110.cif' data_ijsf1110 _database_code_depnum_ccdc_archive 'CCDC 858658' #TrackingRef '- Pd(NO2)2(N-Hpap)2_ijsf1110.cif' _audit_creation_date 2011-08-16 _audit_creation_method ; Olex2 1.1 (compiled 2011.08.12 svn.r1921, GUI svn.r3809) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C38 H42 N6 O12 Pd, 2(C2 H3 N)' _chemical_formula_sum 'C42 H48 N8 O12 Pd' _chemical_formula_weight 963.28 _chemical_melting_point ? _chemical_oxdiff_formula 'C22 H23 N3 O6 Pd1' _chemical_oxdiff_usercomment "Somia's Hpap-new 2 - NO2" loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 8.4350(6) _cell_length_b 10.2678(5) _cell_length_c 13.5105(7) _cell_angle_alpha 77.953(4) _cell_angle_beta 76.502(5) _cell_angle_gamma 72.666(5) _cell_volume 1073.86(11) _cell_formula_units_Z 1 _cell_measurement_reflns_used 8352 _cell_measurement_temperature 109.9 _cell_measurement_theta_max 32.0420 _cell_measurement_theta_min 3.1330 _exptl_absorpt_coefficient_mu 0.505 _exptl_absorpt_correction_T_max 0.981 _exptl_absorpt_correction_T_min 0.942 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_crystal_colour 'clear light orange' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 498 _exptl_crystal_size_max 0.1827 _exptl_crystal_size_mid 0.1176 _exptl_crystal_size_min 0.042 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_unetI/netI 0.0418 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 16540 _diffrn_reflns_theta_full 30.01 _diffrn_reflns_theta_max 32.08 _diffrn_reflns_theta_min 3.14 _diffrn_ambient_temperature 109.9 _diffrn_detector_area_resol_mean 16.1450 _diffrn_measured_fraction_theta_full 0.9952 _diffrn_measured_fraction_theta_max 0.906 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -54.00 45.00 1.0000 45.0000 omega____ theta____ kappa____ phi______ frames - -25.1672 77.0000 -180.0000 99 #__ type_ start__ end____ width___ exp.time_ 2 omega -44.00 55.00 1.0000 45.0000 omega____ theta____ kappa____ phi______ frames - 26.4172 -77.0000 -120.0000 99 #__ type_ start__ end____ width___ exp.time_ 3 omega 0.00 92.00 1.0000 45.0000 omega____ theta____ kappa____ phi______ frames - 26.4172 77.0000 90.0000 92 #__ type_ start__ end____ width___ exp.time_ 4 omega -40.00 56.00 1.0000 45.0000 omega____ theta____ kappa____ phi______ frames - 26.4172 -77.0000 -30.0000 96 #__ type_ start__ end____ width___ exp.time_ 5 omega -74.00 10.00 1.0000 45.0000 omega____ theta____ kappa____ phi______ frames - -25.1672 111.0000 37.0000 84 #__ type_ start__ end____ width___ exp.time_ 6 omega -98.00 -45.00 1.0000 45.0000 omega____ theta____ kappa____ phi______ frames - -25.1672 -37.0000 150.0000 53 #__ type_ start__ end____ width___ exp.time_ 7 omega -4.00 97.00 1.0000 45.0000 omega____ theta____ kappa____ phi______ frames - 26.4172 77.0000 -90.0000 101 ; _diffrn_measurement_device_type 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0022528000 _diffrn_orient_matrix_UB_12 -0.0008090000 _diffrn_orient_matrix_UB_13 -0.0527330000 _diffrn_orient_matrix_UB_21 -0.0894833000 _diffrn_orient_matrix_UB_22 0.0148682000 _diffrn_orient_matrix_UB_23 0.0093407000 _diffrn_orient_matrix_UB_31 -0.0051940000 _diffrn_orient_matrix_UB_32 0.0717086000 _diffrn_orient_matrix_UB_33 -0.0109120000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'SuperNova (Mo) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 6462 _reflns_number_total 6809 _reflns_odcompleteness_completeness 99.52 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 30.01 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; XS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.749 _refine_diff_density_min -0.981 _refine_diff_density_rms 0.091 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 291 _refine_ls_number_reflns 6809 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0399 _refine_ls_R_factor_gt 0.0367 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0445P)^2^+0.6314P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0919 _refine_ls_wR_factor_ref 0.0942 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The acetonitrile shows considerable uncertainty in the position of the CN group particularly the nitrogen. This is apparent from the large prolate adp for these atoms (C20 & N4). Using a two site model for each of these atoms did not give a sensible improvement in the structure. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5477(2) 0.6348(2) 0.29018(15) 0.0219(4) Uani 1 1 d . . . H1 H 0.4297 0.6706 0.3118 0.026 Uiso 1 1 calc R . . C2 C 0.6227(3) 0.6829(2) 0.19433(16) 0.0242(4) Uani 1 1 d . . . H2 H 0.5574 0.7519 0.1503 0.029 Uiso 1 1 calc R . . C3 C 0.7974(2) 0.62979(19) 0.16077(14) 0.0200(3) Uani 1 1 d . . . C4 C 0.8817(3) 0.6819(2) 0.06387(15) 0.0235(4) Uani 1 1 d . . . H4 H 0.8195 0.7515 0.0187 0.028 Uiso 1 1 calc R . . C5 C 1.0525(3) 0.6321(2) 0.03526(14) 0.0237(4) Uani 1 1 d . . . C6 C 1.1466(2) 0.5262(2) 0.10305(15) 0.0222(4) Uani 1 1 d . . . C7 C 1.0670(2) 0.47453(19) 0.19653(14) 0.0189(3) Uani 1 1 d . . . H7 H 1.1303 0.4040 0.2406 0.023 Uiso 1 1 calc R . . C8 C 0.8890(2) 0.52615(17) 0.22835(13) 0.0160(3) Uani 1 1 d . . . C9 C 0.8037(2) 0.48214(17) 0.32814(13) 0.0143(3) Uani 1 1 d . . . C10 C 1.0635(4) 0.7913(3) -0.12002(18) 0.0392(6) Uani 1 1 d . . . H10A H 1.1456 0.8159 -0.1802 0.059 Uiso 1 1 calc R . . H10B H 1.0118 0.8702 -0.0826 0.059 Uiso 1 1 calc R . . H10C H 0.9756 0.7664 -0.1427 0.059 Uiso 1 1 calc R . . C11 C 1.4173(3) 0.3820(3) 0.12861(18) 0.0366(5) Uani 1 1 d . . . H11A H 1.5359 0.3651 0.0941 0.055 Uiso 1 1 calc R . . H11B H 1.3812 0.2970 0.1399 0.055 Uiso 1 1 calc R . . H11C H 1.4050 0.4118 0.1950 0.055 Uiso 1 1 calc R . . C12 C 0.8969(2) 0.37914(17) 0.40652(13) 0.0147(3) Uani 1 1 d . . . H12A H 0.8241 0.3844 0.4754 0.018 Uiso 1 1 calc R . . H12B H 0.9996 0.4060 0.4080 0.018 Uiso 1 1 calc R . . C13 C 0.9489(2) 0.23024(17) 0.38670(13) 0.0145(3) Uani 1 1 d . . . C14 C 1.1199(2) 0.15968(18) 0.36521(13) 0.0160(3) Uani 1 1 d . . . H14 H 1.2040 0.2061 0.3606 0.019 Uiso 1 1 calc R . . C15 C 1.1676(2) 0.02246(18) 0.35063(14) 0.0166(3) Uani 1 1 d . . . C16 C 1.0436(2) -0.04755(18) 0.35890(13) 0.0167(3) Uani 1 1 d . . . C17 C 0.8746(2) 0.02253(18) 0.38108(14) 0.0185(3) Uani 1 1 d . . . H17 H 0.7900 -0.0239 0.3868 0.022 Uiso 1 1 calc R . . C18 C 1.4610(2) 0.0032(2) 0.33331(19) 0.0282(4) Uani 1 1 d . . . H18A H 1.4599 0.0843 0.2800 0.042 Uiso 1 1 calc R . . H18B H 1.5704 -0.0649 0.3213 0.042 Uiso 1 1 calc R . . H18C H 1.4426 0.0308 0.4011 0.042 Uiso 1 1 calc R . . C19 C 0.9814(3) -0.2547(2) 0.34955(18) 0.0273(4) Uani 1 1 d . . . H19A H 0.9175 -0.2112 0.2940 0.041 Uiso 1 1 calc R . . H19B H 0.9041 -0.2512 0.4161 0.041 Uiso 1 1 calc R . . H19C H 1.0383 -0.3511 0.3413 0.041 Uiso 1 1 calc R . . N1 N 0.63723(18) 0.53663(15) 0.35611(11) 0.0157(3) Uani 1 1 d . . . N2 N 0.8275(2) 0.16057(18) 0.39511(14) 0.0261(3) Uani 1 1 d . . . H2A H 0.7197 0.2039 0.4094 0.031 Uiso 1 1 calc R . . N3 N 0.38467(19) 0.38502(17) 0.44922(13) 0.0210(3) Uani 1 1 d . . . O1 O 1.1473(2) 0.67649(18) -0.05380(11) 0.0326(3) Uani 1 1 d . . . O2 O 1.31476(19) 0.48763(17) 0.06552(12) 0.0299(3) Uani 1 1 d . . . O3 O 1.33003(17) -0.05594(14) 0.32966(12) 0.0250(3) Uani 1 1 d . . . O4 O 1.10411(17) -0.18314(13) 0.34567(11) 0.0219(3) Uani 1 1 d . . . O5 O 0.3012(2) 0.43816(18) 0.38164(13) 0.0335(3) Uani 1 1 d . . . O6 O 0.3980(2) 0.26340(15) 0.48981(14) 0.0314(3) Uani 1 1 d . . . Pd1 Pd 0.5000 0.5000 0.5000 0.01379(6) Uani 1 2 d S . . C20 C 0.3033(8) 0.9203(4) 0.0074(4) 0.106(2) Uani 1 1 d . . . C21 C 0.2375(4) 0.8505(4) 0.1020(3) 0.0567(8) Uani 1 1 d . . . H21A H 0.2917 0.7514 0.1055 0.085 Uiso 1 1 calc R . . H21B H 0.1154 0.8668 0.1077 0.085 Uiso 1 1 calc R . . H21C H 0.2596 0.8848 0.1586 0.085 Uiso 1 1 calc R . . N4 N 0.3526(14) 0.9779(5) -0.0695(5) 0.278(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0172(8) 0.0195(8) 0.0252(9) -0.0007(7) -0.0038(7) -0.0011(7) C2 0.0225(9) 0.0213(9) 0.0242(9) 0.0032(7) -0.0049(7) -0.0029(7) C3 0.0238(9) 0.0176(8) 0.0184(8) -0.0017(6) -0.0022(7) -0.0070(7) C4 0.0294(10) 0.0214(9) 0.0175(8) 0.0029(7) -0.0035(7) -0.0079(8) C5 0.0298(10) 0.0261(9) 0.0148(8) -0.0010(7) 0.0021(7) -0.0132(8) C6 0.0207(8) 0.0247(9) 0.0194(8) -0.0034(7) 0.0027(7) -0.0080(7) C7 0.0178(8) 0.0188(8) 0.0176(8) -0.0019(6) 0.0012(6) -0.0051(6) C8 0.0171(7) 0.0135(7) 0.0168(8) -0.0029(6) 0.0004(6) -0.0055(6) C9 0.0138(7) 0.0125(7) 0.0160(7) -0.0026(6) -0.0006(6) -0.0041(6) C10 0.0539(15) 0.0374(13) 0.0220(10) 0.0077(9) -0.0035(10) -0.0167(11) C11 0.0214(10) 0.0417(13) 0.0315(11) 0.0042(10) 0.0074(8) -0.0020(9) C12 0.0136(7) 0.0146(7) 0.0142(7) -0.0022(6) 0.0000(6) -0.0030(6) C13 0.0146(7) 0.0124(7) 0.0136(7) 0.0000(6) -0.0012(6) -0.0020(6) C14 0.0133(7) 0.0158(7) 0.0186(8) -0.0029(6) -0.0016(6) -0.0044(6) C15 0.0138(7) 0.0154(7) 0.0201(8) -0.0043(6) -0.0027(6) -0.0020(6) C16 0.0181(8) 0.0135(7) 0.0178(8) -0.0022(6) -0.0026(6) -0.0037(6) C17 0.0157(7) 0.0167(8) 0.0233(8) -0.0011(6) -0.0027(6) -0.0064(6) C18 0.0149(8) 0.0243(9) 0.0466(13) -0.0119(9) -0.0047(8) -0.0033(7) C19 0.0282(10) 0.0195(9) 0.0396(11) -0.0072(8) -0.0097(9) -0.0098(8) N1 0.0138(6) 0.0137(6) 0.0179(7) -0.0026(5) -0.0007(5) -0.0027(5) N2 0.0206(8) 0.0239(8) 0.0312(9) -0.0030(7) -0.0024(7) -0.0047(6) N3 0.0144(7) 0.0226(8) 0.0258(8) -0.0105(6) 0.0037(6) -0.0055(6) O1 0.0372(9) 0.0374(9) 0.0173(7) 0.0051(6) 0.0039(6) -0.0140(7) O2 0.0213(7) 0.0366(8) 0.0235(7) 0.0010(6) 0.0074(6) -0.0080(6) O3 0.0135(6) 0.0191(6) 0.0429(8) -0.0128(6) -0.0030(6) -0.0010(5) O4 0.0208(6) 0.0138(6) 0.0327(7) -0.0066(5) -0.0048(5) -0.0047(5) O5 0.0327(8) 0.0402(9) 0.0348(8) -0.0092(7) -0.0109(7) -0.0141(7) O6 0.0303(8) 0.0210(7) 0.0462(9) -0.0085(6) -0.0036(7) -0.0119(6) Pd1 0.01060(8) 0.01347(9) 0.01697(9) -0.00469(6) 0.00113(6) -0.00385(6) C20 0.154(5) 0.048(2) 0.088(3) -0.022(2) 0.051(3) -0.030(3) C21 0.0490(17) 0.060(2) 0.0614(19) -0.0103(16) -0.0118(15) -0.0134(15) N4 0.480(15) 0.069(3) 0.159(6) -0.025(3) 0.190(8) -0.070(6) _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 C1 H1 0.9500 . ? C1 C2 1.363(3) . ? C1 N1 1.366(2) . ? C2 H2 0.9500 . ? C2 C3 1.410(3) . ? C3 C4 1.416(3) . ? C3 C8 1.413(3) . ? C4 H4 0.9500 . ? C4 C5 1.368(3) . ? C5 C6 1.436(3) . ? C5 O1 1.354(2) . ? C6 C7 1.365(2) . ? C6 O2 1.356(2) . ? C7 H7 0.9500 . ? C7 C8 1.429(2) . ? C8 C9 1.423(2) . ? C9 C12 1.511(2) . ? C9 N1 1.341(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C10 O1 1.431(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C11 O2 1.432(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C12 C13 1.522(2) . ? C13 C14 1.400(2) . ? C13 N2 1.386(2) . ? C14 H14 0.9500 . ? C14 C15 1.388(2) . ? C15 C16 1.408(2) . ? C15 O3 1.364(2) . ? C16 C17 1.386(2) . ? C16 O4 1.367(2) . ? C17 H17 0.9500 . ? C17 N2 1.394(2) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C18 O3 1.424(2) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C19 O4 1.424(2) . ? N1 Pd1 2.0406(15) . ? N2 H2A 0.8800 . ? N3 O5 1.221(2) . ? N3 O6 1.238(2) . ? N3 Pd1 2.0359(16) . ? Pd1 N1 2.0406(15) 2_666 ? Pd1 N3 2.0359(16) 2_666 ? C20 C21 1.406(5) . ? C20 N4 1.135(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1 119.0 . . ? C2 C1 N1 121.97(17) . . ? N1 C1 H1 119.0 . . ? C1 C2 H2 120.2 . . ? C1 C2 C3 119.69(18) . . ? C3 C2 H2 120.2 . . ? C2 C3 C4 121.46(18) . . ? C2 C3 C8 118.19(17) . . ? C8 C3 C4 120.31(17) . . ? C3 C4 H4 120.0 . . ? C5 C4 C3 120.07(18) . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 120.09(17) . . ? O1 C5 C4 125.40(19) . . ? O1 C5 C6 114.50(18) . . ? C7 C6 C5 120.52(18) . . ? O2 C6 C5 113.85(16) . . ? O2 C6 C7 125.61(19) . . ? C6 C7 H7 119.9 . . ? C6 C7 C8 120.28(18) . . ? C8 C7 H7 119.9 . . ? C3 C8 C7 118.73(16) . . ? C3 C8 C9 119.31(16) . . ? C9 C8 C7 121.85(16) . . ? C8 C9 C12 121.77(15) . . ? N1 C9 C8 119.92(16) . . ? N1 C9 C12 118.25(15) . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O1 C10 H10A 109.5 . . ? O1 C10 H10B 109.5 . . ? O1 C10 H10C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O2 C11 H11A 109.5 . . ? O2 C11 H11B 109.5 . . ? O2 C11 H11C 109.5 . . ? C9 C12 H12A 108.6 . . ? C9 C12 H12B 108.6 . . ? C9 C12 C13 114.71(14) . . ? H12A C12 H12B 107.6 . . ? C13 C12 H12A 108.6 . . ? C13 C12 H12B 108.6 . . ? C14 C13 C12 120.43(15) . . ? N2 C13 C12 120.36(15) . . ? N2 C13 C14 119.13(15) . . ? C13 C14 H14 119.7 . . ? C15 C14 C13 120.55(15) . . ? C15 C14 H14 119.7 . . ? C14 C15 C16 120.02(16) . . ? O3 C15 C14 125.38(16) . . ? O3 C15 C16 114.59(15) . . ? C17 C16 C15 119.15(16) . . ? O4 C16 C15 115.31(15) . . ? O4 C16 C17 125.52(16) . . ? C16 C17 H17 119.7 . . ? C16 C17 N2 120.54(16) . . ? N2 C17 H17 119.7 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O3 C18 H18A 109.5 . . ? O3 C18 H18B 109.5 . . ? O3 C18 H18C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O4 C19 H19A 109.5 . . ? O4 C19 H19B 109.5 . . ? O4 C19 H19C 109.5 . . ? C1 N1 Pd1 113.76(12) . . ? C9 N1 C1 120.89(15) . . ? C9 N1 Pd1 125.05(12) . . ? C13 N2 C17 120.61(16) . . ? C13 N2 H2A 119.7 . . ? C17 N2 H2A 119.7 . . ? O5 N3 O6 121.74(17) . . ? O5 N3 Pd1 119.50(13) . . ? O6 N3 Pd1 118.74(14) . . ? C5 O1 C10 117.13(19) . . ? C6 O2 C11 117.21(16) . . ? C15 O3 C18 117.31(14) . . ? C16 O4 C19 116.41(15) . . ? N1 Pd1 N1 179.999(2) . 2_666 ? N3 Pd1 N1 90.98(6) . . ? N3 Pd1 N1 89.02(6) 2_666 . ? N3 Pd1 N1 90.98(6) 2_666 2_666 ? N3 Pd1 N1 89.02(6) . 2_666 ? N3 Pd1 N3 179.999(1) . 2_666 ? N4 C20 C21 178.3(9) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 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 C1 C2 C3 C4 -176.75(19) . . . . ? C1 C2 C3 C8 0.7(3) . . . . ? C1 N1 Pd1 N3 -102.41(13) . . . 2_666 ? C1 N1 Pd1 N3 77.59(13) . . . . ? C2 C1 N1 C9 -0.8(3) . . . . ? C2 C1 N1 Pd1 173.18(16) . . . . ? C2 C3 C4 C5 177.35(19) . . . . ? C2 C3 C8 C7 -178.09(17) . . . . ? C2 C3 C8 C9 -1.8(3) . . . . ? C3 C4 C5 C6 0.5(3) . . . . ? C3 C4 C5 O1 -178.00(19) . . . . ? C3 C8 C9 C12 -175.59(15) . . . . ? C3 C8 C9 N1 1.6(2) . . . . ? C4 C3 C8 C7 -0.6(3) . . . . ? C4 C3 C8 C9 175.69(17) . . . . ? C4 C5 C6 C7 -0.2(3) . . . . ? C4 C5 C6 O2 -179.31(18) . . . . ? C4 C5 O1 C10 4.6(3) . . . . ? C5 C6 C7 C8 -0.5(3) . . . . ? C5 C6 O2 C11 -179.84(19) . . . . ? C6 C5 O1 C10 -173.97(19) . . . . ? C6 C7 C8 C3 0.8(3) . . . . ? C6 C7 C8 C9 -175.32(17) . . . . ? C7 C6 O2 C11 1.1(3) . . . . ? C7 C8 C9 C12 0.6(3) . . . . ? C7 C8 C9 N1 177.78(16) . . . . ? C8 C3 C4 C5 -0.1(3) . . . . ? C8 C9 C12 C13 -75.6(2) . . . . ? C8 C9 N1 C1 -0.3(2) . . . . ? C8 C9 N1 Pd1 -173.61(12) . . . . ? C9 C12 C13 C14 116.07(17) . . . . ? C9 C12 C13 N2 -67.4(2) . . . . ? C9 N1 Pd1 N3 -108.69(14) . . . . ? C9 N1 Pd1 N3 71.31(14) . . . 2_666 ? C12 C9 N1 C1 177.02(16) . . . . ? C12 C9 N1 Pd1 3.7(2) . . . . ? C12 C13 C14 C15 177.75(16) . . . . ? C12 C13 N2 C17 -177.43(16) . . . . ? C13 C14 C15 C16 -0.9(3) . . . . ? C13 C14 C15 O3 -179.83(17) . . . . ? C14 C13 N2 C17 -0.8(3) . . . . ? C14 C15 C16 C17 0.4(3) . . . . ? C14 C15 C16 O4 -178.45(16) . . . . ? C14 C15 O3 C18 6.8(3) . . . . ? C15 C16 C17 N2 0.0(3) . . . . ? C15 C16 O4 C19 -177.56(17) . . . . ? C16 C15 O3 C18 -172.19(18) . . . . ? C16 C17 N2 C13 0.3(3) . . . . ? C17 C16 O4 C19 3.7(3) . . . . ? N1 C1 C2 C3 0.6(3) . . . . ? N1 C9 C12 C13 107.11(17) . . . . ? N2 C13 C14 C15 1.2(3) . . . . ? O1 C5 C6 C7 178.43(18) . . . . ? O1 C5 C6 O2 -0.7(3) . . . . ? O2 C6 C7 C8 178.52(18) . . . . ? O3 C15 C16 C17 179.37(16) . . . . ? O3 C15 C16 O4 0.6(2) . . . . ? O4 C16 C17 N2 178.65(17) . . . . ? O5 N3 Pd1 N1 -60.28(15) . . . . ? O5 N3 Pd1 N1 119.72(15) . . . 2_666 ? O6 N3 Pd1 N1 -58.54(14) . . . 2_666 ? O6 N3 Pd1 N1 121.46(14) . . . . ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0 1 0 0.0550 0.0000 1.0000 0.0000 -0.0008 0.0149 0.0717 0 -1 0 0.0550 -0.0000 -1.0000 -0.0000 0.0008 -0.0149 -0.0717 1 0 0 0.0669 1.0000 0.0000 -0.0000 0.0023 -0.0895 -0.0052 -1 0 0 0.0629 -1.0000 -0.0000 0.0000 -0.0023 0.0895 0.0052 0 0 -1 0.0190 -0.0000 0.0000 -1.0000 0.0527 -0.0093 0.0109 0 0 1 0.0230 0.0000 -0.0000 1.0000 -0.0527 0.0093 -0.0109 # Attachment '- Pd(OAc)(C^N)PPh3_ijf1042.cif' data_ijf1042 _database_code_depnum_ccdc_archive 'CCDC 858659' #TrackingRef '- Pd(OAc)(C^N)PPh3_ijf1042.cif' _audit_creation_date 2011-01-24 _audit_creation_method ; Olex2 1.1 (compiled 2011.01.21 svn.r1625, GUI svn.r3464) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C40 H38 N O6 P Pd, C H2 Cl2' _chemical_formula_sum 'C41 H40 Cl2 N O6 P Pd' _chemical_formula_weight 851.01 _chemical_melting_point ? _chemical_oxdiff_formula 'C40 H38 N O6 P Pd' _chemical_oxdiff_usercomment "Somia's B-19(a)" loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y, -z+1/2' 3 'x+1/2, y+1/2, z' 4 '-x+1/2, y+1/2, -z+1/2' 5 '-x, -y, -z' 6 'x, -y, z-1/2' 7 '-x+1/2, -y+1/2, -z' 8 'x+1/2, -y+1/2, z-1/2' _cell_length_a 47.4181(14) _cell_length_b 11.0136(3) _cell_length_c 17.7382(6) _cell_angle_alpha 90.00 _cell_angle_beta 107.608(3) _cell_angle_gamma 90.00 _cell_volume 8829.7(5) _cell_formula_units_Z 8 _cell_measurement_reflns_used 23218 _cell_measurement_temperature 110.15 _cell_measurement_theta_max 24.9737 _cell_measurement_theta_min 2.9037 _exptl_absorpt_coefficient_mu 0.619 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.83682 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour ? _exptl_crystal_density_diffrn 1.280 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description ? _exptl_crystal_F_000 3488 _exptl_crystal_size_max 0.336 _exptl_crystal_size_mid 0.2842 _exptl_crystal_size_min 0.2773 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_unetI/netI 0.0240 _diffrn_reflns_limit_h_max 56 _diffrn_reflns_limit_h_min -56 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 42881 _diffrn_reflns_theta_full 25.11 _diffrn_reflns_theta_max 25.11 _diffrn_reflns_theta_min 2.92 _diffrn_ambient_temperature 110.15 _diffrn_detector_area_resol_mean 16.1450 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -87.00 4.50 0.7500 5.0000 omega____ theta____ kappa____ phi______ frames - -17.6138 -37.0000 60.0000 122 #__ type_ start__ end____ width___ exp.time_ 2 omega -38.00 -11.00 0.7500 5.0000 omega____ theta____ kappa____ phi______ frames - -17.6138 142.0000 -133.0000 36 #__ type_ start__ end____ width___ exp.time_ 3 omega -88.00 5.00 0.7500 5.0000 omega____ theta____ kappa____ phi______ frames - -17.6138 -77.0000 -180.0000 124 #__ type_ start__ end____ width___ exp.time_ 4 omega -88.00 -7.00 0.7500 5.0000 omega____ theta____ kappa____ phi______ frames - -17.6138 -77.0000 -30.0000 108 #__ type_ start__ end____ width___ exp.time_ 5 omega -77.00 -5.00 0.7500 5.0000 omega____ theta____ kappa____ phi______ frames - -17.6138 128.0000 -124.0000 96 #__ type_ start__ end____ width___ exp.time_ 6 omega -51.00 48.00 0.7500 5.0000 omega____ theta____ kappa____ phi______ frames - 18.8638 -77.0000 60.0000 132 #__ type_ start__ end____ width___ exp.time_ 7 omega -54.00 45.00 0.7500 5.0000 omega____ theta____ kappa____ phi______ frames - 18.8638 -37.0000 120.0000 132 ; _diffrn_measurement_device_type 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0148643000 _diffrn_orient_matrix_UB_12 -0.0122507000 _diffrn_orient_matrix_UB_13 0.0220963000 _diffrn_orient_matrix_UB_21 -0.0049201000 _diffrn_orient_matrix_UB_22 -0.0281738000 _diffrn_orient_matrix_UB_23 0.0296381000 _diffrn_orient_matrix_UB_31 -0.0007814000 _diffrn_orient_matrix_UB_32 -0.0563894000 _diffrn_orient_matrix_UB_33 -0.0196742000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'SuperNova (Mo) X-ray Source' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 7088 _reflns_number_total 7832 _reflns_odcompleteness_completeness 99.73 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 24.97 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'A short history of SHELX (Sheldrick, 2007)/Bruker' _refine_diff_density_max 1.292 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.082 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 474 _refine_ls_number_reflns 7832 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0407 _refine_ls_R_factor_gt 0.0373 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+29.4470P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1018 _refine_ls_wR_factor_ref 0.1038 _refine_special_details ; During refinement it was observed that there are three DCM molecules present in the UC, of which 2 show disorder over more than 3 positions. Attempts to model this disorder were unsatisfactory, thus the SQUEEZE algorithm was used to remove the contribution of these molecules from the hkl file. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.68513(7) -0.1782(3) 0.58546(18) 0.0227(6) Uani 1 1 d . . . H1 H 0.6749 -0.2379 0.6058 0.027 Uiso 1 1 calc R . . C2 C 0.71459(7) -0.1932(3) 0.59532(19) 0.0240(6) Uani 1 1 d . . . H2 H 0.7249 -0.2601 0.6250 0.029 Uiso 1 1 calc R . . C3 C 0.72962(6) -0.1099(3) 0.56160(18) 0.0214(6) Uani 1 1 d . . . C4 C 0.75999(7) -0.1225(3) 0.56820(19) 0.0246(7) Uani 1 1 d . . . H4 H 0.7711 -0.1870 0.5987 0.030 Uiso 1 1 calc R . . C5 C 0.77346(6) -0.0433(3) 0.53140(19) 0.0237(7) Uani 1 1 d . . . C6 C 0.75655(7) 0.0527(3) 0.48427(18) 0.0226(6) Uani 1 1 d . . . C7 C 0.72774(6) 0.0695(3) 0.47930(18) 0.0201(6) Uani 1 1 d . . . H7 H 0.7170 0.1354 0.4493 0.024 Uiso 1 1 calc R . . C8 C 0.71339(6) -0.0113(3) 0.51888(17) 0.0188(6) Uani 1 1 d . . . C9 C 0.68349(6) 0.0028(3) 0.51653(16) 0.0172(6) Uani 1 1 d . . . C10 C 0.66496(6) 0.1141(3) 0.48317(17) 0.0187(6) Uani 1 1 d . . . H10A H 0.6772 0.1749 0.4662 0.022 Uiso 1 1 calc R . . H10B H 0.6482 0.0911 0.4366 0.022 Uiso 1 1 calc R . . C11 C 0.65331(6) 0.1680(3) 0.54672(16) 0.0157(6) Uani 1 1 d . . . C12 C 0.66342(6) 0.2821(3) 0.57857(17) 0.0182(6) Uani 1 1 d . . . H12 H 0.6759 0.3283 0.5566 0.022 Uiso 1 1 calc R . . C13 C 0.65537(6) 0.3278(3) 0.64157(18) 0.0200(6) Uani 1 1 d . . . C14 C 0.63679(6) 0.2601(3) 0.67353(17) 0.0205(6) Uani 1 1 d . . . C15 C 0.62639(6) 0.1486(3) 0.64052(17) 0.0196(6) Uani 1 1 d . . . H15 H 0.6135 0.1033 0.6618 0.024 Uiso 1 1 calc R . . C16 C 0.63428(6) 0.1010(3) 0.57686(16) 0.0166(6) Uani 1 1 d . . . C17 C 0.82050(7) -0.1358(4) 0.5843(2) 0.0383(9) Uani 1 1 d . . . H17A H 0.8202 -0.1237 0.6388 0.057 Uiso 1 1 calc R . . H17B H 0.8408 -0.1284 0.5822 0.057 Uiso 1 1 calc R . . H17C H 0.8129 -0.2169 0.5663 0.057 Uiso 1 1 calc R . . C18 C 0.75555(7) 0.2021(3) 0.3873(2) 0.0294(7) Uani 1 1 d . . . H18A H 0.7457 0.2634 0.4103 0.044 Uiso 1 1 calc R . . H18B H 0.7407 0.1550 0.3476 0.044 Uiso 1 1 calc R . . H18C H 0.7688 0.2423 0.3621 0.044 Uiso 1 1 calc R . . C19 C 0.61387(8) 0.2389(4) 0.7757(2) 0.0356(8) Uani 1 1 d . . . H19A H 0.6123 0.2818 0.8227 0.053 Uiso 1 1 calc R . . H19B H 0.6238 0.1608 0.7915 0.053 Uiso 1 1 calc R . . H19C H 0.5940 0.2248 0.7392 0.053 Uiso 1 1 calc R . . C20 C 0.68425(8) 0.5049(3) 0.6475(2) 0.0361(8) Uani 1 1 d . . . H20A H 0.6894 0.5807 0.6774 0.054 Uiso 1 1 calc R . . H20B H 0.6747 0.5236 0.5915 0.054 Uiso 1 1 calc R . . H20C H 0.7022 0.4575 0.6529 0.054 Uiso 1 1 calc R . . C21 C 0.61534(6) -0.3239(3) 0.52831(18) 0.0212(6) Uani 1 1 d . . . C22 C 0.60696(8) -0.4471(3) 0.4902(2) 0.0321(8) Uani 1 1 d . . . H22A H 0.6142 -0.4544 0.4442 0.048 Uiso 1 1 calc R . . H22B H 0.5854 -0.4559 0.4733 0.048 Uiso 1 1 calc R . . H22C H 0.6159 -0.5109 0.5285 0.048 Uiso 1 1 calc R . . C23 C 0.55423(6) -0.1669(3) 0.46314(17) 0.0188(6) Uani 1 1 d . . . C24 C 0.55680(7) -0.2023(3) 0.39021(18) 0.0236(6) Uani 1 1 d . . . H24 H 0.5705 -0.1618 0.3693 0.028 Uiso 1 1 calc R . . C25 C 0.53968(8) -0.2958(3) 0.3477(2) 0.0327(8) Uani 1 1 d . . . H25 H 0.5414 -0.3183 0.2976 0.039 Uiso 1 1 calc R . . C26 C 0.52017(8) -0.3560(3) 0.3786(2) 0.0393(9) Uani 1 1 d . . . H26 H 0.5082 -0.4194 0.3492 0.047 Uiso 1 1 calc R . . C27 C 0.51801(8) -0.3245(3) 0.4524(2) 0.0375(8) Uani 1 1 d . . . H27 H 0.5050 -0.3678 0.4742 0.045 Uiso 1 1 calc R . . C28 C 0.53492(7) -0.2296(3) 0.4945(2) 0.0291(7) Uani 1 1 d . . . H28 H 0.5333 -0.2075 0.5448 0.035 Uiso 1 1 calc R . . C29 C 0.56609(6) -0.0225(3) 0.60369(17) 0.0191(6) Uani 1 1 d . . . C30 C 0.57942(7) -0.1018(3) 0.66508(19) 0.0258(7) Uani 1 1 d . . . H30 H 0.5936 -0.1588 0.6592 0.031 Uiso 1 1 calc R . . C31 C 0.57203(8) -0.0977(3) 0.7347(2) 0.0332(8) Uani 1 1 d . . . H31 H 0.5809 -0.1528 0.7763 0.040 Uiso 1 1 calc R . . C32 C 0.55179(8) -0.0140(3) 0.7438(2) 0.0358(8) Uani 1 1 d . . . H32 H 0.5466 -0.0121 0.7916 0.043 Uiso 1 1 calc R . . C33 C 0.53892(7) 0.0670(3) 0.6842(2) 0.0302(8) Uani 1 1 d . . . H33 H 0.5252 0.1254 0.6912 0.036 Uiso 1 1 calc R . . C34 C 0.54609(7) 0.0631(3) 0.61361(18) 0.0220(6) Uani 1 1 d . . . H34 H 0.5373 0.1190 0.5724 0.026 Uiso 1 1 calc R . . C35 C 0.55786(6) 0.0892(3) 0.45218(16) 0.0169(6) Uani 1 1 d . . . C36 C 0.52720(6) 0.0875(3) 0.41713(18) 0.0214(6) Uani 1 1 d . . . H36 H 0.5161 0.0192 0.4245 0.026 Uiso 1 1 calc R . . C37 C 0.51295(7) 0.1838(3) 0.37198(18) 0.0238(6) Uani 1 1 d . . . H37 H 0.4921 0.1814 0.3483 0.029 Uiso 1 1 calc R . . C38 C 0.52884(7) 0.2838(3) 0.36105(18) 0.0240(7) Uani 1 1 d . . . H38 H 0.5189 0.3503 0.3302 0.029 Uiso 1 1 calc R . . C39 C 0.55927(7) 0.2867(3) 0.39528(18) 0.0233(6) Uani 1 1 d . . . H39 H 0.5702 0.3555 0.3877 0.028 Uiso 1 1 calc R . . C40 C 0.57381(6) 0.1900(3) 0.44040(16) 0.0192(6) Uani 1 1 d . . . H40 H 0.5947 0.1923 0.4634 0.023 Uiso 1 1 calc R . . C41 C 0.57568(8) 0.5088(3) 0.6621(2) 0.0381(9) Uani 1 1 d . . . H41A H 0.5838 0.5715 0.6343 0.046 Uiso 1 1 calc R . . H41B H 0.5921 0.4785 0.7071 0.046 Uiso 1 1 calc R . . Cl1 Cl 0.56141(2) 0.38871(9) 0.59708(7) 0.0494(3) Uani 1 1 d . . . Cl2 Cl 0.54869(2) 0.57494(9) 0.69848(7) 0.0501(3) Uani 1 1 d . . . N1 N 0.67002(5) -0.0804(2) 0.54753(15) 0.0186(5) Uani 1 1 d . . . O1 O 0.80221(5) -0.0456(2) 0.53387(15) 0.0328(5) Uani 1 1 d . . . O2 O 0.77220(5) 0.1232(2) 0.44771(14) 0.0298(5) Uani 1 1 d . . . O3 O 0.66450(5) 0.43669(18) 0.67732(14) 0.0265(5) Uani 1 1 d . . . O4 O 0.63055(5) 0.3107(2) 0.73720(12) 0.0255(5) Uani 1 1 d . . . O5 O 0.61992(4) -0.24169(18) 0.48387(12) 0.0217(4) Uani 1 1 d . . . O6 O 0.61672(5) -0.3100(2) 0.59882(13) 0.0308(5) Uani 1 1 d . . . P1 P 0.576123(15) -0.03818(7) 0.51305(4) 0.01494(15) Uani 1 1 d . . . Pd1 Pd 0.624710(4) -0.065377(19) 0.532731(12) 0.01540(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0208(15) 0.0185(15) 0.0290(16) 0.0044(13) 0.0081(13) 0.0010(12) C2 0.0203(15) 0.0216(15) 0.0295(16) 0.0032(13) 0.0065(13) 0.0038(12) C3 0.0177(14) 0.0212(15) 0.0250(16) -0.0052(12) 0.0061(12) 0.0009(12) C4 0.0183(15) 0.0266(16) 0.0274(16) -0.0006(13) 0.0046(13) 0.0029(12) C5 0.0133(14) 0.0319(17) 0.0258(16) -0.0057(13) 0.0058(12) 0.0011(12) C6 0.0200(15) 0.0250(16) 0.0248(16) -0.0034(12) 0.0097(12) -0.0026(12) C7 0.0181(14) 0.0212(15) 0.0228(15) -0.0015(12) 0.0090(12) 0.0001(11) C8 0.0164(14) 0.0206(15) 0.0195(14) -0.0044(12) 0.0059(11) -0.0012(11) C9 0.0154(13) 0.0202(14) 0.0165(13) -0.0029(11) 0.0054(11) -0.0022(11) C10 0.0146(13) 0.0225(15) 0.0204(14) 0.0040(12) 0.0073(11) 0.0018(11) C11 0.0115(12) 0.0195(14) 0.0141(13) 0.0036(11) 0.0009(10) 0.0032(11) C12 0.0120(13) 0.0185(14) 0.0248(15) 0.0062(12) 0.0067(11) 0.0028(11) C13 0.0161(14) 0.0166(14) 0.0275(16) -0.0016(12) 0.0066(12) -0.0009(11) C14 0.0175(14) 0.0250(15) 0.0198(14) -0.0039(12) 0.0070(12) -0.0012(12) C15 0.0150(14) 0.0246(15) 0.0186(14) 0.0018(12) 0.0043(11) -0.0038(11) C16 0.0131(13) 0.0198(14) 0.0157(14) 0.0010(11) 0.0027(11) -0.0001(11) C17 0.0179(16) 0.055(2) 0.043(2) 0.0068(18) 0.0099(15) 0.0090(16) C18 0.0274(16) 0.0273(17) 0.0391(19) 0.0013(15) 0.0188(15) -0.0030(13) C19 0.0367(19) 0.047(2) 0.0298(18) -0.0141(16) 0.0207(15) -0.0175(16) C20 0.0376(19) 0.0221(17) 0.059(2) -0.0101(16) 0.0302(18) -0.0119(15) C21 0.0147(13) 0.0232(15) 0.0266(16) -0.0010(13) 0.0076(12) 0.0009(12) C22 0.0367(19) 0.0223(17) 0.038(2) -0.0047(14) 0.0129(16) -0.0039(14) C23 0.0153(13) 0.0160(14) 0.0242(15) 0.0003(12) 0.0045(12) 0.0004(11) C24 0.0226(15) 0.0241(16) 0.0228(15) -0.0022(13) 0.0049(12) 0.0000(12) C25 0.0336(18) 0.0265(17) 0.0324(18) -0.0082(14) 0.0014(15) 0.0011(14) C26 0.0279(18) 0.0226(17) 0.056(2) -0.0104(16) -0.0045(17) -0.0040(14) C27 0.0269(17) 0.0300(19) 0.056(2) -0.0005(17) 0.0124(17) -0.0122(14) C28 0.0259(16) 0.0279(17) 0.0343(18) -0.0012(14) 0.0106(14) -0.0063(13) C29 0.0179(14) 0.0228(15) 0.0187(14) -0.0039(12) 0.0084(12) -0.0080(12) C30 0.0300(17) 0.0241(16) 0.0248(16) 0.0011(13) 0.0103(13) -0.0034(13) C31 0.044(2) 0.0360(19) 0.0218(16) 0.0047(14) 0.0123(15) -0.0118(16) C32 0.044(2) 0.045(2) 0.0250(17) -0.0116(16) 0.0199(16) -0.0222(17) C33 0.0264(17) 0.0367(19) 0.0330(18) -0.0129(15) 0.0175(15) -0.0087(14) C34 0.0185(15) 0.0251(16) 0.0233(15) -0.0072(12) 0.0077(12) -0.0056(12) C35 0.0188(14) 0.0203(14) 0.0127(13) -0.0036(11) 0.0066(11) -0.0003(11) C36 0.0159(14) 0.0248(15) 0.0247(16) -0.0011(13) 0.0081(12) -0.0014(12) C37 0.0183(14) 0.0282(16) 0.0246(16) -0.0003(13) 0.0062(12) 0.0027(12) C38 0.0265(16) 0.0215(15) 0.0239(16) 0.0013(12) 0.0074(13) 0.0079(12) C39 0.0254(16) 0.0211(15) 0.0248(16) -0.0020(12) 0.0096(13) -0.0045(12) C40 0.0198(14) 0.0209(15) 0.0167(14) -0.0033(12) 0.0050(11) -0.0027(12) C41 0.0316(18) 0.035(2) 0.051(2) -0.0159(17) 0.0179(17) -0.0115(15) Cl1 0.0430(5) 0.0422(5) 0.0643(7) -0.0225(5) 0.0181(5) -0.0139(4) Cl2 0.0444(6) 0.0448(6) 0.0694(7) -0.0144(5) 0.0299(5) -0.0044(4) N1 0.0143(12) 0.0205(12) 0.0211(12) 0.0000(10) 0.0056(10) 0.0007(9) O1 0.0144(11) 0.0448(14) 0.0405(14) 0.0053(11) 0.0104(10) 0.0033(10) O2 0.0195(11) 0.0332(13) 0.0407(13) 0.0058(11) 0.0151(10) 0.0000(9) O3 0.0259(11) 0.0187(11) 0.0387(13) -0.0081(9) 0.0156(10) -0.0065(9) O4 0.0260(11) 0.0314(12) 0.0237(11) -0.0124(9) 0.0142(9) -0.0108(9) O5 0.0200(10) 0.0206(11) 0.0263(11) -0.0025(9) 0.0097(9) -0.0012(8) O6 0.0389(13) 0.0264(12) 0.0270(12) 0.0019(10) 0.0099(10) -0.0025(10) P1 0.0132(3) 0.0171(3) 0.0158(3) -0.0013(3) 0.0064(3) -0.0024(3) Pd1 0.01266(12) 0.01730(13) 0.01717(13) -0.00119(8) 0.00590(9) -0.00167(8) _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 C1 H1 0.9500 . ? C1 C2 1.364(4) . ? C1 N1 1.354(4) . ? C2 H2 0.9500 . ? C2 C3 1.402(4) . ? C3 C4 1.416(4) . ? C3 C8 1.412(4) . ? C4 H4 0.9500 . ? C4 C5 1.359(5) . ? C5 C6 1.434(4) . ? C5 O1 1.351(4) . ? C6 C7 1.355(4) . ? C6 O2 1.366(4) . ? C7 H7 0.9500 . ? C7 C8 1.427(4) . ? C8 C9 1.414(4) . ? C9 C10 1.521(4) . ? C9 N1 1.328(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 C11 1.518(4) . ? C11 C12 1.401(4) . ? C11 C16 1.391(4) . ? C12 H12 0.9500 . ? C12 C13 1.381(4) . ? C13 C14 1.398(4) . ? C13 O3 1.365(4) . ? C14 C15 1.385(4) . ? C14 O4 1.370(3) . ? C15 H15 0.9500 . ? C15 C16 1.395(4) . ? C16 Pd1 1.990(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C17 O1 1.439(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C18 O2 1.420(4) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C19 O4 1.430(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C20 O3 1.422(4) . ? C21 C22 1.515(4) . ? C21 O5 1.261(4) . ? C21 O6 1.242(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.391(4) . ? C23 C28 1.390(4) . ? C23 P1 1.821(3) . ? C24 H24 0.9500 . ? C24 C25 1.384(4) . ? C25 H25 0.9500 . ? C25 C26 1.379(5) . ? C26 H26 0.9500 . ? C26 C27 1.389(6) . ? C27 H27 0.9500 . ? C27 C28 1.390(5) . ? C28 H28 0.9500 . ? C29 C30 1.389(4) . ? C29 C34 1.386(4) . ? C29 P1 1.818(3) . ? C30 H30 0.9500 . ? C30 C31 1.383(5) . ? C31 H31 0.9500 . ? C31 C32 1.375(5) . ? C32 H32 0.9500 . ? C32 C33 1.377(5) . ? C33 H33 0.9500 . ? C33 C34 1.394(4) . ? C34 H34 0.9500 . ? C35 C36 1.397(4) . ? C35 C40 1.394(4) . ? C35 P1 1.822(3) . ? C36 H36 0.9500 . ? C36 C37 1.377(4) . ? C37 H37 0.9500 . ? C37 C38 1.381(4) . ? C38 H38 0.9500 . ? C38 C39 1.386(4) . ? C39 H39 0.9500 . ? C39 C40 1.384(4) . ? C40 H40 0.9500 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C41 Cl1 1.752(4) . ? C41 Cl2 1.756(4) . ? N1 Pd1 2.091(2) . ? O5 Pd1 2.111(2) . ? P1 Pd1 2.2434(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1 119.1 . . ? N1 C1 H1 119.1 . . ? N1 C1 C2 121.9(3) . . ? C1 C2 H2 120.0 . . ? C1 C2 C3 119.9(3) . . ? C3 C2 H2 120.0 . . ? C2 C3 C4 122.4(3) . . ? C2 C3 C8 117.9(3) . . ? C8 C3 C4 119.7(3) . . ? C3 C4 H4 119.6 . . ? C5 C4 C3 120.8(3) . . ? C5 C4 H4 119.6 . . ? C4 C5 C6 119.5(3) . . ? O1 C5 C4 126.1(3) . . ? O1 C5 C6 114.4(3) . . ? C7 C6 C5 120.9(3) . . ? C7 C6 O2 125.0(3) . . ? O2 C6 C5 114.1(3) . . ? C6 C7 H7 119.9 . . ? C6 C7 C8 120.3(3) . . ? C8 C7 H7 119.9 . . ? C3 C8 C7 118.7(3) . . ? C3 C8 C9 118.6(3) . . ? C9 C8 C7 122.7(3) . . ? C8 C9 C10 123.8(3) . . ? N1 C9 C8 121.1(3) . . ? N1 C9 C10 115.1(2) . . ? C9 C10 H10A 109.9 . . ? C9 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? C11 C10 C9 108.9(2) . . ? C11 C10 H10A 109.9 . . ? C11 C10 H10B 109.9 . . ? C12 C11 C10 119.5(2) . . ? C16 C11 C10 120.2(3) . . ? C16 C11 C12 120.2(3) . . ? C11 C12 H12 119.7 . . ? C13 C12 C11 120.6(3) . . ? C13 C12 H12 119.7 . . ? C12 C13 C14 119.7(3) . . ? O3 C13 C12 124.7(3) . . ? O3 C13 C14 115.5(3) . . ? C15 C14 C13 119.2(3) . . ? O4 C14 C13 115.9(3) . . ? O4 C14 C15 124.8(3) . . ? C14 C15 H15 119.1 . . ? C14 C15 C16 121.8(3) . . ? C16 C15 H15 119.1 . . ? C11 C16 C15 118.4(3) . . ? C11 C16 Pd1 115.7(2) . . ? C15 C16 Pd1 125.4(2) . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O1 C17 H17A 109.5 . . ? O1 C17 H17B 109.5 . . ? O1 C17 H17C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O2 C18 H18A 109.5 . . ? O2 C18 H18B 109.5 . . ? O2 C18 H18C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O4 C19 H19A 109.5 . . ? O4 C19 H19B 109.5 . . ? O4 C19 H19C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O3 C20 H20A 109.5 . . ? O3 C20 H20B 109.5 . . ? O3 C20 H20C 109.5 . . ? O5 C21 C22 115.8(3) . . ? O6 C21 C22 119.1(3) . . ? O6 C21 O5 125.1(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 P1 118.2(2) . . ? C28 C23 C24 119.1(3) . . ? C28 C23 P1 122.6(2) . . ? C23 C24 H24 119.6 . . ? C25 C24 C23 120.8(3) . . ? C25 C24 H24 119.6 . . ? C24 C25 H25 120.2 . . ? C26 C25 C24 119.7(3) . . ? C26 C25 H25 120.2 . . ? C25 C26 H26 119.9 . . ? C25 C26 C27 120.2(3) . . ? C27 C26 H26 119.9 . . ? C26 C27 H27 120.0 . . ? C26 C27 C28 120.0(3) . . ? C28 C27 H27 120.0 . . ? C23 C28 H28 120.0 . . ? C27 C28 C23 120.1(3) . . ? C27 C28 H28 120.0 . . ? C30 C29 P1 117.1(2) . . ? C34 C29 C30 119.6(3) . . ? C34 C29 P1 123.3(2) . . ? C29 C30 H30 119.9 . . ? C31 C30 C29 120.1(3) . . ? C31 C30 H30 119.9 . . ? C30 C31 H31 120.0 . . ? C32 C31 C30 120.1(3) . . ? C32 C31 H31 120.0 . . ? C31 C32 H32 119.8 . . ? C31 C32 C33 120.5(3) . . ? C33 C32 H32 119.8 . . ? C32 C33 H33 120.1 . . ? C32 C33 C34 119.9(3) . . ? C34 C33 H33 120.1 . . ? C29 C34 C33 119.8(3) . . ? C29 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C36 C35 P1 119.8(2) . . ? C40 C35 C36 118.9(3) . . ? C40 C35 P1 121.3(2) . . ? C35 C36 H36 119.7 . . ? C37 C36 C35 120.6(3) . . ? C37 C36 H36 119.7 . . ? C36 C37 H37 119.9 . . ? C36 C37 C38 120.2(3) . . ? C38 C37 H37 119.9 . . ? C37 C38 H38 120.1 . . ? C37 C38 C39 119.8(3) . . ? C39 C38 H38 120.1 . . ? C38 C39 H39 119.8 . . ? C40 C39 C38 120.4(3) . . ? C40 C39 H39 119.8 . . ? C35 C40 H40 120.0 . . ? C39 C40 C35 120.1(3) . . ? C39 C40 H40 120.0 . . ? H41A C41 H41B 107.9 . . ? Cl1 C41 H41A 109.2 . . ? Cl1 C41 H41B 109.2 . . ? Cl1 C41 Cl2 112.07(19) . . ? Cl2 C41 H41A 109.2 . . ? Cl2 C41 H41B 109.2 . . ? C1 N1 Pd1 119.67(19) . . ? C9 N1 C1 120.4(2) . . ? C9 N1 Pd1 119.89(19) . . ? C5 O1 C17 116.5(3) . . ? C6 O2 C18 116.6(2) . . ? C13 O3 C20 116.3(2) . . ? C14 O4 C19 117.2(2) . . ? C21 O5 Pd1 114.90(18) . . ? C23 P1 C35 102.28(13) . . ? C23 P1 Pd1 112.29(9) . . ? C29 P1 C23 103.92(13) . . ? C29 P1 C35 104.27(13) . . ? C29 P1 Pd1 113.98(10) . . ? C35 P1 Pd1 118.48(9) . . ? C16 Pd1 N1 85.43(10) . . ? C16 Pd1 O5 172.74(9) . . ? C16 Pd1 P1 92.26(8) . . ? N1 Pd1 O5 87.56(8) . . ? N1 Pd1 P1 176.44(7) . . ? O5 Pd1 P1 94.65(6) . . ? 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 C1 C2 C3 C4 -178.4(3) . . . . ? C1 C2 C3 C8 0.8(4) . . . . ? C1 N1 Pd1 C16 129.6(2) . . . . ? C1 N1 Pd1 O5 -52.3(2) . . . . ? C1 N1 Pd1 P1 179(100) . . . . ? C2 C1 N1 C9 1.9(4) . . . . ? C2 C1 N1 Pd1 178.8(2) . . . . ? C2 C3 C4 C5 176.7(3) . . . . ? C2 C3 C8 C7 -175.5(3) . . . . ? C2 C3 C8 C9 3.9(4) . . . . ? C3 C4 C5 C6 -1.1(5) . . . . ? C3 C4 C5 O1 179.5(3) . . . . ? C3 C8 C9 C10 170.7(3) . . . . ? C3 C8 C9 N1 -6.0(4) . . . . ? C4 C3 C8 C7 3.7(4) . . . . ? C4 C3 C8 C9 -176.8(3) . . . . ? C4 C5 C6 C7 3.5(5) . . . . ? C4 C5 C6 O2 -177.4(3) . . . . ? C4 C5 O1 C17 -4.2(5) . . . . ? C5 C6 C7 C8 -2.2(5) . . . . ? C5 C6 O2 C18 166.7(3) . . . . ? C6 C5 O1 C17 176.3(3) . . . . ? C6 C7 C8 C3 -1.4(4) . . . . ? C6 C7 C8 C9 179.2(3) . . . . ? C7 C6 O2 C18 -14.3(4) . . . . ? C7 C8 C9 C10 -9.8(4) . . . . ? C7 C8 C9 N1 173.4(3) . . . . ? C8 C3 C4 C5 -2.5(5) . . . . ? C8 C9 C10 C11 -123.0(3) . . . . ? C8 C9 N1 C1 3.1(4) . . . . ? C8 C9 N1 Pd1 -173.7(2) . . . . ? C9 C10 C11 C12 112.9(3) . . . . ? C9 C10 C11 C16 -62.8(3) . . . . ? C9 N1 Pd1 C16 -53.5(2) . . . . ? C9 N1 Pd1 O5 124.6(2) . . . . ? C9 N1 Pd1 P1 -3.9(13) . . . . ? C10 C9 N1 C1 -173.9(3) . . . . ? C10 C9 N1 Pd1 9.2(3) . . . . ? C10 C11 C12 C13 -173.8(3) . . . . ? C10 C11 C16 C15 173.7(2) . . . . ? C10 C11 C16 Pd1 1.1(3) . . . . ? C11 C12 C13 C14 -0.4(4) . . . . ? C11 C12 C13 O3 178.8(3) . . . . ? C11 C16 Pd1 N1 44.9(2) . . . . ? C11 C16 Pd1 O5 29.7(9) . . . . ? C11 C16 Pd1 P1 -132.4(2) . . . . ? C12 C11 C16 C15 -1.9(4) . . . . ? C12 C11 C16 Pd1 -174.6(2) . . . . ? C12 C13 C14 C15 -1.0(4) . . . . ? C12 C13 C14 O4 178.3(3) . . . . ? C12 C13 O3 C20 -1.5(4) . . . . ? C13 C14 C15 C16 0.9(4) . . . . ? C13 C14 O4 C19 -174.4(3) . . . . ? C14 C13 O3 C20 177.8(3) . . . . ? C14 C15 C16 C11 0.5(4) . . . . ? C14 C15 C16 Pd1 172.4(2) . . . . ? C15 C14 O4 C19 4.8(4) . . . . ? C15 C16 Pd1 N1 -127.2(3) . . . . ? C15 C16 Pd1 O5 -142.4(7) . . . . ? C15 C16 Pd1 P1 55.5(2) . . . . ? C16 C11 C12 C13 1.9(4) . . . . ? C21 O5 Pd1 C16 121.0(7) . . . . ? C21 O5 Pd1 N1 105.8(2) . . . . ? C21 O5 Pd1 P1 -76.98(19) . . . . ? C22 C21 O5 Pd1 170.5(2) . . . . ? C23 C24 C25 C26 -1.1(5) . . . . ? C23 P1 Pd1 C16 175.50(13) . . . . ? C23 P1 Pd1 N1 126.1(11) . . . . ? C23 P1 Pd1 O5 -2.26(12) . . . . ? C24 C23 C28 C27 -1.4(5) . . . . ? C24 C23 P1 C29 179.6(2) . . . . ? C24 C23 P1 C35 71.3(2) . . . . ? C24 C23 P1 Pd1 -56.8(2) . . . . ? C24 C25 C26 C27 -1.0(5) . . . . ? C25 C26 C27 C28 1.8(5) . . . . ? C26 C27 C28 C23 -0.6(5) . . . . ? C28 C23 C24 C25 2.3(5) . . . . ? C28 C23 P1 C29 0.4(3) . . . . ? C28 C23 P1 C35 -107.9(3) . . . . ? C28 C23 P1 Pd1 124.1(2) . . . . ? C29 C30 C31 C32 -1.0(5) . . . . ? C29 P1 Pd1 C16 -66.67(13) . . . . ? C29 P1 Pd1 N1 -116.1(11) . . . . ? C29 P1 Pd1 O5 115.56(12) . . . . ? C30 C29 C34 C33 -1.7(4) . . . . ? C30 C29 P1 C23 79.3(2) . . . . ? C30 C29 P1 C35 -173.9(2) . . . . ? C30 C29 P1 Pd1 -43.2(3) . . . . ? C30 C31 C32 C33 -0.6(5) . . . . ? C31 C32 C33 C34 1.0(5) . . . . ? C32 C33 C34 C29 0.2(5) . . . . ? C34 C29 C30 C31 2.1(5) . . . . ? C34 C29 P1 C23 -100.5(3) . . . . ? C34 C29 P1 C35 6.3(3) . . . . ? C34 C29 P1 Pd1 136.9(2) . . . . ? C35 C36 C37 C38 -0.3(5) . . . . ? C35 P1 Pd1 C16 56.57(13) . . . . ? C35 P1 Pd1 N1 7.1(11) . . . . ? C35 P1 Pd1 O5 -121.20(12) . . . . ? C36 C35 C40 C39 0.6(4) . . . . ? C36 C35 P1 C23 34.8(3) . . . . ? C36 C35 P1 C29 -73.2(2) . . . . ? C36 C35 P1 Pd1 158.85(19) . . . . ? C36 C37 C38 C39 0.4(5) . . . . ? C37 C38 C39 C40 0.0(5) . . . . ? C38 C39 C40 C35 -0.5(4) . . . . ? C40 C35 C36 C37 -0.3(4) . . . . ? C40 C35 P1 C23 -146.0(2) . . . . ? C40 C35 P1 C29 106.0(2) . . . . ? C40 C35 P1 Pd1 -21.9(3) . . . . ? N1 C1 C2 C3 -3.9(5) . . . . ? N1 C9 C10 C11 54.0(3) . . . . ? O1 C5 C6 C7 -177.0(3) . . . . ? O1 C5 C6 O2 2.1(4) . . . . ? O2 C6 C7 C8 178.8(3) . . . . ? O3 C13 C14 C15 179.7(3) . . . . ? O3 C13 C14 O4 -1.0(4) . . . . ? O4 C14 C15 C16 -178.3(3) . . . . ? O6 C21 O5 Pd1 -8.1(4) . . . . ? P1 C23 C24 C25 -176.9(2) . . . . ? P1 C23 C28 C27 177.7(3) . . . . ? P1 C29 C30 C31 -177.8(2) . . . . ? P1 C29 C34 C33 178.2(2) . . . . ? P1 C35 C36 C37 179.0(2) . . . . ? P1 C35 C40 C39 -178.6(2) . . . . ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -1 1 1 0.1477 -1.0000 1.0000 1.0000 -0.0051 0.0063 -0.0752 2 0 -1 0.1541 2.0000 -0.0000 -1.0000 0.0077 -0.0395 0.0181 -1 0 1 0.1387 -1.0000 0.0000 1.0000 0.0072 0.0346 -0.0189 1 0 -1 0.1387 1.0000 0.0000 -1.0000 -0.0072 -0.0346 0.0189 1 2 0 0.1534 1.0000 2.0000 0.0000 -0.0096 -0.0614 -0.1135 -1 -2 0 0.1437 -1.0000 -2.0000 0.0000 0.0096 0.0614 0.1135 1 0 0 0.1451 1.0000 0.0000 0.0000 0.0149 -0.0049 -0.0008 -1 -1 -1 0.1090 -1.0000 -1.0000 -1.0000 -0.0247 0.0034 0.0768 -2 0 -1 0.1410 -2.0000 0.0000 -1.0000 -0.0517 -0.0200 0.0212 2 0 1 0.1495 2.0000 -0.0000 1.0000 0.0517 0.0200 -0.0212 -67 -1 8 0.1427 -67.0000 -1.0000 8.0000 -0.8068 0.5924 -0.0487 -3 1 -1 0.1327 -3.0000 1.0000 -1.0000 -0.0788 -0.0434 -0.0343 52 -7 4 0.1234 52.0000 -7.0000 4.0000 0.9462 0.0634 0.2752 -2 -1 2 0.1581 -2.0000 -1.0000 2.0000 0.0266 0.0974 0.0186 2 1 -2 0.1578 2.0000 1.0000 -2.0000 -0.0266 -0.0974 -0.0186 -11 15 9 0.1283 -11.0000 15.0000 9.0000 -0.1485 -0.1029 -1.0136 -5 -1 0 0.1319 -5.0000 -1.0000 0.0000 -0.0620 0.0526 0.0603 _platon_squeeze_details ; ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.250 -0.115 0.250 410 128 ' ' 2 0.250 0.115 0.750 410 128 ' ' 3 0.750 0.075 0.250 410 128 ' ' 4 0.750 -0.107 0.750 410 128 ' ' # Attachment '- Pd(OAc)(NO2)(pip)2_ijf0916m.cif' data_ijf0916m _database_code_depnum_ccdc_archive 'CCDC 858660' #TrackingRef '- Pd(OAc)(NO2)(pip)2_ijf0916m.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H25 N3 O4 Pd' _chemical_formula_sum 'C12 H25 N3 O4 Pd' _chemical_formula_weight 381.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _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 10.5351(7) _cell_length_b 9.7782(6) _cell_length_c 15.3104(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.5550(10) _cell_angle_gamma 90.00 _cell_volume 1577.12(18) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 5113 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 29.30 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 1.193 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS v2.10 (Sheldrick)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17456 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 30.00 _reflns_number_total 4560 _reflns_number_gt 3834 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Inspection of the Fobs electron density map at the nitro group showed a continuum of electron density at the positions of O3 and O4 therefore the group was not modelled in two discrete positions. ; _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^)+(0.0265P)^2^+0.7825P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4560 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0371 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0626 _refine_ls_wR_factor_gt 0.0595 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7152(2) 0.2688(2) -0.04488(14) 0.0263(5) Uani 1 1 d . . . H1A H 0.7900 0.3217 -0.0246 0.032 Uiso 1 1 calc R . . H1B H 0.6389 0.3101 -0.0184 0.032 Uiso 1 1 calc R . . C2 C 0.7046(2) 0.2797(2) -0.14416(14) 0.0295(5) Uani 1 1 d . . . H2A H 0.6248 0.2360 -0.1644 0.035 Uiso 1 1 calc R . . H2B H 0.7021 0.3772 -0.1615 0.035 Uiso 1 1 calc R . . C3 C 0.8168(2) 0.2101(3) -0.18693(15) 0.0345(5) Uani 1 1 d . . . H3A H 0.8963 0.2581 -0.1705 0.041 Uiso 1 1 calc R . . H3B H 0.8071 0.2142 -0.2513 0.041 Uiso 1 1 calc R . . C4 C 0.8239(2) 0.0617(3) -0.15742(14) 0.0331(5) Uani 1 1 d . . . H4A H 0.7474 0.0122 -0.1782 0.040 Uiso 1 1 calc R . . H4B H 0.8991 0.0175 -0.1835 0.040 Uiso 1 1 calc R . . C5 C 0.8330(2) 0.0522(2) -0.05834(14) 0.0274(5) Uani 1 1 d . . . H5A H 0.8317 -0.0453 -0.0409 0.033 Uiso 1 1 calc R . . H5B H 0.9149 0.0916 -0.0386 0.033 Uiso 1 1 calc R . . C6 C 0.8747(2) 0.0963(2) 0.29566(14) 0.0261(5) Uani 1 1 d . . . H6A H 0.9311 0.1725 0.2787 0.031 Uiso 1 1 calc R . . H6B H 0.9111 0.0106 0.2724 0.031 Uiso 1 1 calc R . . C7 C 0.8702(2) 0.0877(3) 0.39510(15) 0.0339(6) Uani 1 1 d . . . H7A H 0.8210 0.0060 0.4125 0.041 Uiso 1 1 calc R . . H7B H 0.9574 0.0781 0.4189 0.041 Uiso 1 1 calc R . . C8 C 0.8086(2) 0.2157(3) 0.43277(15) 0.0398(6) Uani 1 1 d . . . H8A H 0.8001 0.2057 0.4968 0.048 Uiso 1 1 calc R . . H8B H 0.8630 0.2961 0.4213 0.048 Uiso 1 1 calc R . . C9 C 0.6787(2) 0.2375(3) 0.39152(15) 0.0346(5) Uani 1 1 d . . . H9A H 0.6216 0.1617 0.4084 0.041 Uiso 1 1 calc R . . H9B H 0.6419 0.3240 0.4134 0.041 Uiso 1 1 calc R . . C10 C 0.6879(2) 0.2435(2) 0.29280(14) 0.0261(5) Uani 1 1 d . . . H10A H 0.6018 0.2548 0.2674 0.031 Uiso 1 1 calc R . . H10B H 0.7390 0.3241 0.2761 0.031 Uiso 1 1 calc R . . C11 C 0.9470(2) 0.3051(2) 0.12492(13) 0.0226(4) Uani 1 1 d . . . C12 C 1.0843(2) 0.3493(2) 0.12292(16) 0.0306(5) Uani 1 1 d . . . H12A H 1.0985 0.4066 0.0714 0.046 Uiso 1 1 calc R . . H12B H 1.1390 0.2684 0.1202 0.046 Uiso 1 1 calc R . . H12C H 1.1045 0.4016 0.1758 0.046 Uiso 1 1 calc R . . N1 N 0.72776(17) 0.12505(18) -0.01430(11) 0.0195(3) Uani 1 1 d . . . H1 H 0.666(2) 0.084(2) -0.0287(16) 0.023(6) Uiso 1 1 d . . . N2 N 0.74687(16) 0.11822(18) 0.25604(11) 0.0183(3) Uani 1 1 d . . . H2 H 0.701(2) 0.056(3) 0.2696(16) 0.026(7) Uiso 1 1 d . . . N3 N 0.55742(17) 0.06532(19) 0.12629(11) 0.0241(4) Uani 1 1 d . . . O1 O 0.86367(15) 0.39010(16) 0.13788(11) 0.0291(3) Uani 1 1 d . . . O2 O 0.92582(13) 0.17641(15) 0.11256(9) 0.0224(3) Uani 1 1 d . . . Pd1 Pd 0.739374(14) 0.121315(15) 0.120651(9) 0.01752(5) Uani 1 1 d . . . O3 O 0.48224(16) 0.1028(2) 0.06906(12) 0.0474(5) Uani 1 1 d . . . O4 O 0.51832(17) -0.0046(2) 0.18656(12) 0.0476(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0301(12) 0.0244(11) 0.0243(11) 0.0002(8) -0.0052(9) 0.0053(9) C2 0.0300(12) 0.0326(12) 0.0257(11) 0.0060(9) -0.0071(9) 0.0002(10) C3 0.0259(12) 0.0554(16) 0.0222(11) 0.0077(11) -0.0002(9) -0.0010(11) C4 0.0300(12) 0.0482(15) 0.0212(11) -0.0036(10) 0.0033(9) 0.0109(11) C5 0.0267(11) 0.0328(12) 0.0228(11) -0.0027(9) 0.0013(9) 0.0091(9) C6 0.0216(10) 0.0320(12) 0.0245(11) 0.0037(9) -0.0049(8) -0.0043(8) C7 0.0301(12) 0.0463(14) 0.0250(11) 0.0135(10) -0.0101(9) -0.0167(10) C8 0.0453(15) 0.0527(16) 0.0213(11) -0.0043(11) -0.0008(10) -0.0222(13) C9 0.0432(14) 0.0369(13) 0.0238(11) -0.0074(10) 0.0066(10) -0.0070(11) C10 0.0320(12) 0.0213(10) 0.0250(11) -0.0019(8) 0.0046(9) 0.0001(9) C11 0.0238(10) 0.0283(11) 0.0158(9) 0.0004(8) -0.0022(8) -0.0036(8) C12 0.0249(11) 0.0353(13) 0.0318(12) -0.0050(10) 0.0019(9) -0.0054(9) N1 0.0187(8) 0.0208(8) 0.0192(8) -0.0016(7) -0.0011(6) -0.0006(7) N2 0.0186(8) 0.0176(8) 0.0185(8) 0.0002(6) -0.0009(6) -0.0030(6) N3 0.0231(9) 0.0283(9) 0.0207(9) 0.0002(7) -0.0009(7) -0.0043(7) O1 0.0284(8) 0.0252(8) 0.0339(9) -0.0029(6) -0.0017(7) 0.0025(6) O2 0.0191(7) 0.0248(7) 0.0232(7) -0.0013(6) 0.0002(6) 0.0002(6) Pd1 0.01732(8) 0.01865(8) 0.01658(8) -0.00069(6) -0.00085(5) -0.00007(6) O3 0.0227(9) 0.0776(15) 0.0416(11) 0.0251(10) -0.0090(8) -0.0069(9) O4 0.0337(10) 0.0703(14) 0.0387(10) 0.0229(10) -0.0049(8) -0.0206(9) _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 C1 N1 1.487(3) . ? C1 C2 1.527(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.517(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.522(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.522(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 N1 1.485(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N2 1.487(3) . ? C6 C7 1.526(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.526(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.517(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.517(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N2 1.486(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 O1 1.226(3) . ? C11 O2 1.291(3) . ? C11 C12 1.511(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? N1 Pd1 2.0690(17) . ? N1 H1 0.80(3) . ? N2 Pd1 2.0738(17) . ? N2 H2 0.80(3) . ? N3 O4 1.223(2) . ? N3 O3 1.231(2) . ? N3 Pd1 1.9962(18) . ? O2 Pd1 2.0417(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 112.60(18) . . ? N1 C1 H1A 109.1 . . ? C2 C1 H1A 109.1 . . ? N1 C1 H1B 109.1 . . ? C2 C1 H1B 109.1 . . ? H1A C1 H1B 107.8 . . ? C3 C2 C1 110.41(18) . . ? C3 C2 H2A 109.6 . . ? C1 C2 H2A 109.6 . . ? C3 C2 H2B 109.6 . . ? C1 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? C2 C3 C4 109.60(19) . . ? C2 C3 H3A 109.8 . . ? C4 C3 H3A 109.8 . . ? C2 C3 H3B 109.8 . . ? C4 C3 H3B 109.8 . . ? H3A C3 H3B 108.2 . . ? C5 C4 C3 110.9(2) . . ? C5 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.0 . . ? N1 C5 C4 112.53(18) . . ? N1 C5 H5A 109.1 . . ? C4 C5 H5A 109.1 . . ? N1 C5 H5B 109.1 . . ? C4 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? N2 C6 C7 112.23(18) . . ? N2 C6 H6A 109.2 . . ? C7 C6 H6A 109.2 . . ? N2 C6 H6B 109.2 . . ? C7 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C8 C7 C6 110.4(2) . . ? C8 C7 H7A 109.6 . . ? C6 C7 H7A 109.6 . . ? C8 C7 H7B 109.6 . . ? C6 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? C9 C8 C7 110.08(19) . . ? C9 C8 H8A 109.6 . . ? C7 C8 H8A 109.6 . . ? C9 C8 H8B 109.6 . . ? C7 C8 H8B 109.6 . . ? H8A C8 H8B 108.2 . . ? C10 C9 C8 110.74(19) . . ? C10 C9 H9A 109.5 . . ? C8 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? N2 C10 C9 112.13(18) . . ? N2 C10 H10A 109.2 . . ? C9 C10 H10A 109.2 . . ? N2 C10 H10B 109.2 . . ? C9 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? O1 C11 O2 124.2(2) . . ? O1 C11 C12 119.7(2) . . ? O2 C11 C12 116.09(19) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C5 N1 C1 112.02(17) . . ? C5 N1 Pd1 114.06(13) . . ? C1 N1 Pd1 109.58(13) . . ? C5 N1 H1 104.4(18) . . ? C1 N1 H1 108.5(18) . . ? Pd1 N1 H1 108.0(18) . . ? C10 N2 C6 110.14(17) . . ? C10 N2 Pd1 110.76(13) . . ? C6 N2 Pd1 115.81(13) . . ? C10 N2 H2 106.0(18) . . ? C6 N2 H2 108.9(17) . . ? Pd1 N2 H2 104.6(17) . . ? O4 N3 O3 118.96(19) . . ? O4 N3 Pd1 121.10(15) . . ? O3 N3 Pd1 119.93(15) . . ? C11 O2 Pd1 114.38(13) . . ? N3 Pd1 O2 178.83(6) . . ? N3 Pd1 N1 90.03(7) . . ? O2 Pd1 N1 88.99(6) . . ? N3 Pd1 N2 88.86(7) . . ? O2 Pd1 N2 92.13(6) . . ? N1 Pd1 N2 178.78(7) . . ? 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 N1 C1 C2 C3 -55.6(3) . . . . ? C1 C2 C3 C4 56.9(3) . . . . ? C2 C3 C4 C5 -56.9(3) . . . . ? C3 C4 C5 N1 55.1(3) . . . . ? N2 C6 C7 C8 -56.2(2) . . . . ? C6 C7 C8 C9 54.9(3) . . . . ? C7 C8 C9 C10 -55.4(3) . . . . ? C8 C9 C10 N2 57.1(3) . . . . ? C4 C5 N1 C1 -52.6(3) . . . . ? C4 C5 N1 Pd1 -177.85(16) . . . . ? C2 C1 N1 C5 53.0(2) . . . . ? C2 C1 N1 Pd1 -179.36(14) . . . . ? C9 C10 N2 C6 -56.9(2) . . . . ? C9 C10 N2 Pd1 173.71(15) . . . . ? C7 C6 N2 C10 56.5(2) . . . . ? C7 C6 N2 Pd1 -176.85(15) . . . . ? O1 C11 O2 Pd1 -2.2(3) . . . . ? C12 C11 O2 Pd1 177.74(14) . . . . ? O4 N3 Pd1 N1 150.58(19) . . . . ? O3 N3 Pd1 N1 -30.38(18) . . . . ? O4 N3 Pd1 N2 -29.92(19) . . . . ? O3 N3 Pd1 N2 149.12(19) . . . . ? C11 O2 Pd1 N1 99.15(14) . . . . ? C11 O2 Pd1 N2 -80.36(14) . . . . ? C5 N1 Pd1 N3 -131.85(15) . . . . ? C1 N1 Pd1 N3 101.66(14) . . . . ? C5 N1 Pd1 O2 47.52(15) . . . . ? C1 N1 Pd1 O2 -78.97(14) . . . . ? C10 N2 Pd1 N3 -78.39(14) . . . . ? C6 N2 Pd1 N3 155.29(15) . . . . ? C10 N2 Pd1 O2 102.24(14) . . . . ? C6 N2 Pd1 O2 -24.09(15) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O3 0.80(3) 2.46(2) 2.904(3) 116(2) . N1 H1 O3 0.80(3) 2.48(3) 3.244(3) 162(2) 3_655 N2 H2 O1 0.80(3) 2.26(3) 3.001(2) 153(2) 2_645 N2 H2 O4 0.80(3) 2.38(2) 2.885(2) 122(2) . _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.784 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.085