# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Mark Stradiotto' _publ_contact_author_email mark.stradiotto@dal.ca loop_ _publ_author_name B.Tardiff K.Hesp M.Ferguson M.Stradiotto data_dal09p0 _database_code_depnum_ccdc_archive 'CCDC 847279' #TrackingRef 'BTNHC_Combined-CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H67 Cl2 N2 P Pd' _chemical_formula_weight 868.30 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' 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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.2112(16) _cell_length_b 12.1097(12) _cell_length_c 22.836(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.2460(10) _cell_angle_gamma 90.00 _cell_volume 4304.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9992 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 27.35 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.340 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1832 _exptl_absorpt_coefficient_mu 0.627 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8671 _exptl_absorpt_correction_T_max 0.9102 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 37222 _diffrn_reflns_av_R_equivalents 0.0667 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 27.52 _reflns_number_total 9881 _reflns_number_gt 8010 _reflns_threshold_expression I>2\s(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 '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^)+(0.0611P)^2^+2.4260P] 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 9881 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0559 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1139 _refine_ls_wR_factor_gt 0.1034 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 Pd Pd 0.483999(11) 0.486357(16) 0.215776(8) 0.02005(7) Uani 1 1 d . . . Cl1 Cl 0.50321(4) 0.35725(6) 0.14675(3) 0.02979(15) Uani 1 1 d . . . Cl2 Cl 0.47677(5) 0.62346(6) 0.28430(3) 0.03569(17) Uani 1 1 d . . . P P 0.39322(4) 0.59276(5) 0.13969(3) 0.02133(14) Uani 1 1 d . . . H1P H 0.3735 0.6507 0.1639 0.026 Uiso 1 1 calc R . . N1 N 0.63992(12) 0.36913(17) 0.30658(9) 0.0209(4) Uani 1 1 d . . . N2 N 0.51924(13) 0.28821(18) 0.29817(9) 0.0218(4) Uani 1 1 d . . . C1 C 0.55380(15) 0.3807(2) 0.28074(10) 0.0195(5) Uani 1 1 d . . . C2 C 0.65800(16) 0.2709(2) 0.33880(12) 0.0263(5) Uani 1 1 d . . . H2 H 0.7133 0.2444 0.3604 0.032 Uiso 1 1 calc R . . C3 C 0.58262(17) 0.2201(2) 0.33367(12) 0.0274(6) Uani 1 1 d . . . H3 H 0.5743 0.1510 0.3509 0.033 Uiso 1 1 calc R . . C11 C 0.70467(15) 0.4546(2) 0.31224(11) 0.0218(5) Uani 1 1 d . . . C12 C 0.75243(16) 0.4617(2) 0.26974(12) 0.0250(5) Uani 1 1 d . . . C13 C 0.81832(17) 0.5395(2) 0.28070(13) 0.0289(6) Uani 1 1 d . . . H13 H 0.8508 0.5473 0.2522 0.035 Uiso 1 1 calc R . . C14 C 0.83755(18) 0.6057(2) 0.33229(14) 0.0332(6) Uani 1 1 d . . . H14 H 0.8833 0.6575 0.3393 0.040 Uiso 1 1 calc R . . C15 C 0.78947(18) 0.5958(2) 0.37363(13) 0.0314(6) Uani 1 1 d . . . H15 H 0.8030 0.6413 0.4090 0.038 Uiso 1 1 calc R . . C16 C 0.72216(17) 0.5214(2) 0.36474(13) 0.0261(5) Uani 1 1 d . . . C17 C 0.73708(17) 0.3868(2) 0.21430(12) 0.0281(6) Uani 1 1 d . . . H17 H 0.6865 0.3386 0.2131 0.034 Uiso 1 1 calc R . . C18 C 0.8158(2) 0.3120(3) 0.21978(16) 0.0465(8) Uani 1 1 d . . . H18A H 0.8275 0.2693 0.2577 0.056 Uiso 1 1 calc R . . H18B H 0.8658 0.3578 0.2203 0.056 Uiso 1 1 calc R . . H18C H 0.8041 0.2615 0.1849 0.056 Uiso 1 1 calc R . . C19 C 0.7170(2) 0.4538(3) 0.15509(15) 0.0511(9) Uani 1 1 d . . . H19A H 0.6664 0.5002 0.1521 0.061 Uiso 1 1 calc R . . H19B H 0.7053 0.4034 0.1202 0.061 Uiso 1 1 calc R . . H19C H 0.7663 0.5007 0.1552 0.061 Uiso 1 1 calc R . . C20 C 0.67113(19) 0.5133(2) 0.41168(14) 0.0320(6) Uani 1 1 d . . . H20 H 0.6178 0.4700 0.3929 0.038 Uiso 1 1 calc R . . C21 C 0.6440(2) 0.6265(3) 0.42933(15) 0.0438(8) Uani 1 1 d . . . H21A H 0.6114 0.6655 0.3926 0.053 Uiso 1 1 calc R . . H21B H 0.6953 0.6694 0.4497 0.053 Uiso 1 1 calc R . . H21C H 0.6081 0.6171 0.4571 0.053 Uiso 1 1 calc R . . C22 C 0.7223(2) 0.4511(3) 0.46845(15) 0.0454(8) Uani 1 1 d . . . H22A H 0.7392 0.3786 0.4565 0.055 Uiso 1 1 calc R . . H22B H 0.6868 0.4413 0.4964 0.055 Uiso 1 1 calc R . . H22C H 0.7739 0.4935 0.4888 0.055 Uiso 1 1 calc R . . C31 C 0.42742(15) 0.2704(2) 0.28635(12) 0.0245(5) Uani 1 1 d . . . C32 C 0.38396(16) 0.3324(2) 0.32096(12) 0.0269(5) Uani 1 1 d . . . C33 C 0.29496(18) 0.3195(3) 0.30642(13) 0.0330(6) Uani 1 1 d . . . H33 H 0.2632 0.3618 0.3277 0.040 Uiso 1 1 calc R . . C34 C 0.25195(17) 0.2463(3) 0.26161(14) 0.0366(7) Uani 1 1 d . . . H34 H 0.1912 0.2401 0.2518 0.044 Uiso 1 1 calc R . . C35 C 0.29727(18) 0.1823(3) 0.23127(14) 0.0358(7) Uani 1 1 d . . . H35 H 0.2673 0.1300 0.2020 0.043 Uiso 1 1 calc R . . C36 C 0.38639(16) 0.1925(2) 0.24262(12) 0.0281(6) Uani 1 1 d . . . C37 C 0.43198(18) 0.4053(2) 0.37370(13) 0.0304(6) Uani 1 1 d . . . H37 H 0.4811 0.4398 0.3619 0.036 Uiso 1 1 calc R . . C38 C 0.4699(2) 0.3351(3) 0.43069(14) 0.0427(7) Uani 1 1 d . . . H38A H 0.5043 0.2752 0.4207 0.051 Uiso 1 1 calc R . . H38B H 0.4233 0.3039 0.4450 0.051 Uiso 1 1 calc R . . H38C H 0.5065 0.3815 0.4628 0.051 Uiso 1 1 calc R . . C39 C 0.3779(2) 0.4988(3) 0.38865(18) 0.0479(9) Uani 1 1 d . . . H39A H 0.3540 0.5434 0.3520 0.057 Uiso 1 1 calc R . . H39B H 0.4141 0.5453 0.4208 0.057 Uiso 1 1 calc R . . H39C H 0.3310 0.4675 0.4027 0.057 Uiso 1 1 calc R . . C40 C 0.43401(18) 0.1179(2) 0.20962(13) 0.0329(6) Uani 1 1 d . . . H40 H 0.4922 0.1503 0.2141 0.039 Uiso 1 1 calc R . . C41 C 0.4458(3) 0.0032(3) 0.23933(18) 0.0463(8) Uani 1 1 d . . . H41A H 0.4755 0.0103 0.2829 0.056 Uiso 1 1 calc R . . H41B H 0.4800 -0.0432 0.2198 0.056 Uiso 1 1 calc R . . H41C H 0.3894 -0.0310 0.2343 0.056 Uiso 1 1 calc R . . C42 C 0.3877(2) 0.1083(3) 0.14123(14) 0.0417(7) Uani 1 1 d . . . H42A H 0.3808 0.1820 0.1227 0.050 Uiso 1 1 calc R . . H42B H 0.3310 0.0749 0.1359 0.050 Uiso 1 1 calc R . . H42C H 0.4216 0.0619 0.1215 0.050 Uiso 1 1 calc R . . C51 C 0.44834(15) 0.6765(2) 0.09359(11) 0.0226(5) Uani 1 1 d . . . C52 C 0.39583(18) 0.7783(2) 0.06346(14) 0.0316(6) Uani 1 1 d . . . H52A H 0.3423 0.7539 0.0334 0.038 Uiso 1 1 calc R . . H52B H 0.3800 0.8232 0.0949 0.038 Uiso 1 1 calc R . . C53 C 0.44937(19) 0.8484(2) 0.03146(14) 0.0342(6) Uani 1 1 d . . . H53 H 0.4147 0.9135 0.0117 0.041 Uiso 1 1 calc R . . C54 C 0.5313(2) 0.8892(2) 0.07821(15) 0.0367(7) Uani 1 1 d . . . H54A H 0.5652 0.9357 0.0577 0.044 Uiso 1 1 calc R . . H54B H 0.5160 0.9345 0.1097 0.044 Uiso 1 1 calc R . . C55 C 0.58460(18) 0.7895(2) 0.10795(13) 0.0310(6) Uani 1 1 d . . . H55 H 0.6381 0.8155 0.1385 0.037 Uiso 1 1 calc R . . C56 C 0.53136(17) 0.7181(2) 0.14030(12) 0.0285(6) Uani 1 1 d . . . H56A H 0.5161 0.7624 0.1722 0.034 Uiso 1 1 calc R . . H56B H 0.5661 0.6542 0.1603 0.034 Uiso 1 1 calc R . . C57 C 0.47386(17) 0.6080(2) 0.04454(12) 0.0259(5) Uani 1 1 d . . . H57A H 0.4215 0.5813 0.0140 0.031 Uiso 1 1 calc R . . H57B H 0.5078 0.5429 0.0637 0.031 Uiso 1 1 calc R . . C58 C 0.52745(18) 0.6795(2) 0.01294(12) 0.0279(6) Uani 1 1 d . . . H58 H 0.5433 0.6348 -0.0191 0.033 Uiso 1 1 calc R . . C59 C 0.47305(19) 0.7794(2) -0.01705(13) 0.0334(6) Uani 1 1 d . . . H59A H 0.5060 0.8250 -0.0386 0.040 Uiso 1 1 calc R . . H59B H 0.4202 0.7534 -0.0473 0.040 Uiso 1 1 calc R . . C60 C 0.60877(17) 0.7192(2) 0.05942(13) 0.0303(6) Uani 1 1 d . . . H60A H 0.6437 0.7635 0.0388 0.036 Uiso 1 1 calc R . . H60B H 0.6434 0.6549 0.0790 0.036 Uiso 1 1 calc R . . C61 C 0.28949(16) 0.5252(2) 0.09777(12) 0.0249(5) Uani 1 1 d . . . C62 C 0.22142(17) 0.6104(2) 0.06449(14) 0.0330(6) Uani 1 1 d . . . H62A H 0.2156 0.6687 0.0934 0.040 Uiso 1 1 calc R . . H62B H 0.2400 0.6457 0.0312 0.040 Uiso 1 1 calc R . . C63 C 0.13394(18) 0.5527(3) 0.03787(14) 0.0376(7) Uani 1 1 d . . . H63 H 0.0904 0.6085 0.0166 0.045 Uiso 1 1 calc R . . C64 C 0.10469(19) 0.4993(3) 0.08918(17) 0.0435(8) Uani 1 1 d . . . H64A H 0.0983 0.5565 0.1185 0.052 Uiso 1 1 calc R . . H64B H 0.0482 0.4633 0.0722 0.052 Uiso 1 1 calc R . . C65 C 0.17049(19) 0.4138(3) 0.12173(16) 0.0421(8) Uani 1 1 d . . . H65 H 0.1509 0.3786 0.1551 0.050 Uiso 1 1 calc R . . C66 C 0.25830(18) 0.4701(3) 0.14907(14) 0.0344(6) Uani 1 1 d . . . H66A H 0.3009 0.4145 0.1705 0.041 Uiso 1 1 calc R . . H66B H 0.2530 0.5266 0.1791 0.041 Uiso 1 1 calc R . . C67 C 0.29775(17) 0.4362(3) 0.05189(14) 0.0333(6) Uani 1 1 d . . . H67A H 0.3412 0.3810 0.0725 0.040 Uiso 1 1 calc R . . H67B H 0.3170 0.4704 0.0186 0.040 Uiso 1 1 calc R . . C68 C 0.20988(18) 0.3786(3) 0.02504(15) 0.0401(7) Uani 1 1 d . . . H68 H 0.2159 0.3205 -0.0046 0.048 Uiso 1 1 calc R . . C69 C 0.14350(19) 0.4646(3) -0.00794(15) 0.0411(7) Uani 1 1 d . . . H69A H 0.1625 0.4994 -0.0412 0.049 Uiso 1 1 calc R . . H69B H 0.0875 0.4282 -0.0261 0.049 Uiso 1 1 calc R . . C70 C 0.1799(2) 0.3252(3) 0.07614(17) 0.0466(8) Uani 1 1 d . . . H70A H 0.2223 0.2690 0.0972 0.056 Uiso 1 1 calc R . . H70B H 0.1241 0.2878 0.0588 0.056 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.01431(10) 0.02162(11) 0.02150(11) 0.00115(7) 0.00053(7) 0.00082(7) Cl1 0.0298(3) 0.0316(3) 0.0247(3) -0.0018(3) 0.0021(3) 0.0080(3) Cl2 0.0413(4) 0.0315(4) 0.0289(3) -0.0048(3) 0.0010(3) 0.0078(3) P 0.0158(3) 0.0217(3) 0.0237(3) -0.0011(2) 0.0009(2) 0.0023(2) N1 0.0141(9) 0.0227(11) 0.0226(10) 0.0007(8) -0.0005(8) 0.0010(8) N2 0.0143(9) 0.0245(11) 0.0248(10) 0.0020(8) 0.0025(8) 0.0000(8) C1 0.0164(11) 0.0231(12) 0.0171(11) -0.0024(9) 0.0015(9) 0.0009(9) C2 0.0192(12) 0.0239(13) 0.0324(14) 0.0063(11) 0.0018(10) 0.0031(10) C3 0.0227(13) 0.0243(13) 0.0327(14) 0.0052(11) 0.0038(11) 0.0019(10) C11 0.0138(11) 0.0217(12) 0.0266(12) 0.0036(10) 0.0003(9) 0.0004(9) C12 0.0190(12) 0.0261(13) 0.0273(13) 0.0044(10) 0.0022(10) 0.0032(10) C13 0.0216(13) 0.0301(14) 0.0349(15) 0.0056(12) 0.0079(11) -0.0011(11) C14 0.0230(13) 0.0266(14) 0.0464(17) 0.0021(12) 0.0038(12) -0.0057(11) C15 0.0256(13) 0.0276(14) 0.0371(15) -0.0052(12) 0.0024(12) -0.0017(11) C16 0.0195(12) 0.0261(13) 0.0299(14) 0.0014(11) 0.0026(11) 0.0022(10) C17 0.0203(12) 0.0350(15) 0.0276(13) 0.0000(11) 0.0044(11) -0.0003(11) C18 0.0285(15) 0.055(2) 0.052(2) -0.0231(17) 0.0042(14) 0.0060(15) C19 0.051(2) 0.067(2) 0.0333(17) 0.0099(16) 0.0069(15) -0.0095(19) C20 0.0246(14) 0.0376(16) 0.0331(15) -0.0077(12) 0.0069(12) -0.0045(12) C21 0.0372(17) 0.053(2) 0.0400(17) -0.0111(15) 0.0094(14) 0.0074(15) C22 0.049(2) 0.049(2) 0.0427(18) 0.0061(15) 0.0194(16) 0.0045(16) C31 0.0156(11) 0.0277(13) 0.0282(13) 0.0054(10) 0.0031(10) -0.0030(10) C32 0.0200(12) 0.0320(14) 0.0285(13) 0.0049(11) 0.0063(10) 0.0000(11) C33 0.0245(13) 0.0431(17) 0.0333(15) 0.0050(13) 0.0110(11) 0.0002(12) C34 0.0176(13) 0.0521(19) 0.0388(16) 0.0083(14) 0.0055(12) -0.0077(13) C35 0.0251(14) 0.0432(18) 0.0364(16) -0.0004(13) 0.0042(12) -0.0134(13) C36 0.0206(12) 0.0316(14) 0.0309(14) 0.0018(11) 0.0052(11) -0.0054(11) C37 0.0240(13) 0.0367(16) 0.0305(14) -0.0015(12) 0.0077(11) 0.0044(11) C38 0.0467(19) 0.0484(19) 0.0301(16) -0.0019(14) 0.0060(14) 0.0008(15) C39 0.0365(18) 0.055(2) 0.051(2) -0.0162(16) 0.0107(16) 0.0077(15) C40 0.0274(14) 0.0301(15) 0.0394(16) -0.0055(12) 0.0064(12) -0.0051(12) C41 0.047(2) 0.0335(18) 0.055(2) -0.0022(14) 0.0097(17) 0.0003(14) C42 0.0396(17) 0.0427(18) 0.0424(18) -0.0125(14) 0.0108(14) -0.0040(14) C51 0.0179(11) 0.0212(12) 0.0257(12) 0.0012(10) 0.0012(10) 0.0001(10) C52 0.0264(13) 0.0263(14) 0.0404(16) 0.0051(12) 0.0065(12) 0.0059(11) C53 0.0344(15) 0.0262(14) 0.0413(16) 0.0101(12) 0.0096(13) 0.0081(12) C54 0.0436(17) 0.0220(14) 0.0474(18) -0.0049(12) 0.0173(14) -0.0071(12) C55 0.0258(13) 0.0317(15) 0.0325(14) -0.0011(12) 0.0033(11) -0.0084(11) C56 0.0245(13) 0.0294(14) 0.0288(14) -0.0030(11) 0.0028(11) -0.0037(11) C57 0.0241(13) 0.0232(13) 0.0280(13) -0.0012(10) 0.0035(11) -0.0002(10) C58 0.0301(14) 0.0259(14) 0.0274(13) -0.0002(11) 0.0076(11) 0.0012(11) C59 0.0322(15) 0.0322(15) 0.0325(15) 0.0081(12) 0.0035(12) 0.0019(12) C60 0.0231(13) 0.0306(14) 0.0363(15) 0.0044(12) 0.0071(11) -0.0006(11) C61 0.0141(11) 0.0272(13) 0.0293(13) -0.0013(11) -0.0005(10) 0.0019(10) C62 0.0205(13) 0.0311(15) 0.0391(16) -0.0027(12) -0.0054(12) 0.0032(11) C63 0.0186(13) 0.0391(17) 0.0453(17) -0.0038(14) -0.0070(12) 0.0035(12) C64 0.0182(13) 0.049(2) 0.060(2) -0.0106(16) 0.0065(14) -0.0019(13) C65 0.0217(14) 0.050(2) 0.0509(19) 0.0048(15) 0.0048(13) -0.0074(13) C66 0.0217(13) 0.0409(17) 0.0378(16) 0.0042(13) 0.0038(12) -0.0064(12) C67 0.0184(12) 0.0346(16) 0.0428(16) -0.0110(13) 0.0017(12) 0.0005(11) C68 0.0225(14) 0.0382(17) 0.0535(19) -0.0183(14) 0.0008(13) -0.0016(12) C69 0.0231(14) 0.0479(19) 0.0438(18) -0.0096(15) -0.0048(13) -0.0057(13) C70 0.0223(14) 0.0356(17) 0.073(2) -0.0002(16) -0.0008(15) -0.0073(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 Pd C1 2.045(2) . ? Pd Cl1 2.3024(7) . ? Pd Cl2 2.3070(7) . ? Pd P 2.3268(7) . ? P C51 1.861(3) . ? P C61 1.874(3) . ? N1 C1 1.362(3) . ? N1 C2 1.387(3) . ? N1 C11 1.454(3) . ? N2 C1 1.360(3) . ? N2 C3 1.388(3) . ? N2 C31 1.453(3) . ? C2 C3 1.344(4) . ? C11 C12 1.403(4) . ? C11 C16 1.408(4) . ? C12 C13 1.393(4) . ? C12 C17 1.521(4) . ? C13 C14 1.387(4) . ? C14 C15 1.387(4) . ? C15 C16 1.386(4) . ? C16 C20 1.529(4) . ? C17 C19 1.532(4) . ? C17 C18 1.540(4) . ? C20 C21 1.528(4) . ? C20 C22 1.528(4) . ? C31 C36 1.399(4) . ? C31 C32 1.413(4) . ? C32 C33 1.396(4) . ? C32 C37 1.520(4) . ? C33 C34 1.386(4) . ? C34 C35 1.380(4) . ? C35 C36 1.400(4) . ? C36 C40 1.518(4) . ? C37 C39 1.527(4) . ? C37 C38 1.531(4) . ? C40 C41 1.535(4) . ? C40 C42 1.536(4) . ? C51 C57 1.541(4) . ? C51 C52 1.546(4) . ? C51 C56 1.549(3) . ? C52 C53 1.537(4) . ? C53 C59 1.520(4) . ? C53 C54 1.535(4) . ? C54 C55 1.529(4) . ? C55 C60 1.533(4) . ? C55 C56 1.548(4) . ? C57 C58 1.542(4) . ? C58 C60 1.521(4) . ? C58 C59 1.540(4) . ? C61 C67 1.535(4) . ? C61 C62 1.546(4) . ? C61 C66 1.551(4) . ? C62 C63 1.545(4) . ? C63 C64 1.525(5) . ? C63 C69 1.532(5) . ? C64 C65 1.523(5) . ? C65 C70 1.532(5) . ? C65 C66 1.544(4) . ? C67 C68 1.550(4) . ? C68 C70 1.527(5) . ? C68 C69 1.535(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd Cl1 85.31(7) . . ? C1 Pd Cl2 94.66(7) . . ? Cl1 Pd Cl2 174.53(3) . . ? C1 Pd P 173.99(7) . . ? Cl1 Pd P 92.48(2) . . ? Cl2 Pd P 88.08(3) . . ? C51 P C61 116.95(12) . . ? C51 P Pd 114.89(8) . . ? C61 P Pd 115.44(9) . . ? C1 N1 C2 110.9(2) . . ? C1 N1 C11 126.3(2) . . ? C2 N1 C11 121.6(2) . . ? C1 N2 C3 111.2(2) . . ? C1 N2 C31 123.5(2) . . ? C3 N2 C31 125.0(2) . . ? N2 C1 N1 104.2(2) . . ? N2 C1 Pd 122.53(17) . . ? N1 C1 Pd 132.10(18) . . ? C3 C2 N1 107.1(2) . . ? C2 C3 N2 106.6(2) . . ? C12 C11 C16 122.3(2) . . ? C12 C11 N1 120.4(2) . . ? C16 C11 N1 117.0(2) . . ? C13 C12 C11 117.4(2) . . ? C13 C12 C17 119.5(2) . . ? C11 C12 C17 123.1(2) . . ? C14 C13 C12 121.5(3) . . ? C13 C14 C15 119.5(3) . . ? C16 C15 C14 121.7(3) . . ? C15 C16 C11 117.5(2) . . ? C15 C16 C20 119.8(3) . . ? C11 C16 C20 122.7(2) . . ? C12 C17 C19 111.3(3) . . ? C12 C17 C18 110.1(2) . . ? C19 C17 C18 110.5(3) . . ? C21 C20 C22 110.3(3) . . ? C21 C20 C16 112.3(3) . . ? C22 C20 C16 110.8(2) . . ? C36 C31 C32 123.1(2) . . ? C36 C31 N2 119.4(2) . . ? C32 C31 N2 117.6(2) . . ? C33 C32 C31 116.9(3) . . ? C33 C32 C37 121.3(2) . . ? C31 C32 C37 121.8(2) . . ? C34 C33 C32 121.3(3) . . ? C35 C34 C33 120.1(3) . . ? C34 C35 C36 121.6(3) . . ? C31 C36 C35 116.9(3) . . ? C31 C36 C40 123.3(2) . . ? C35 C36 C40 119.8(3) . . ? C32 C37 C39 114.1(2) . . ? C32 C37 C38 110.3(2) . . ? C39 C37 C38 109.9(3) . . ? C36 C40 C41 109.7(3) . . ? C36 C40 C42 112.2(2) . . ? C41 C40 C42 110.2(3) . . ? C57 C51 C52 109.4(2) . . ? C57 C51 C56 108.5(2) . . ? C52 C51 C56 108.2(2) . . ? C57 C51 P 112.76(18) . . ? C52 C51 P 113.25(18) . . ? C56 C51 P 104.47(17) . . ? C53 C52 C51 109.8(2) . . ? C59 C53 C54 109.8(2) . . ? C59 C53 C52 109.5(2) . . ? C54 C53 C52 109.9(2) . . ? C55 C54 C53 109.0(2) . . ? C54 C55 C60 110.1(2) . . ? C54 C55 C56 109.4(2) . . ? C60 C55 C56 108.9(2) . . ? C55 C56 C51 110.2(2) . . ? C51 C57 C58 109.8(2) . . ? C60 C58 C59 109.8(2) . . ? C60 C58 C57 110.0(2) . . ? C59 C58 C57 108.8(2) . . ? C53 C59 C58 109.7(2) . . ? C58 C60 C55 109.5(2) . . ? C67 C61 C62 108.6(2) . . ? C67 C61 C66 108.8(2) . . ? C62 C61 C66 108.7(2) . . ? C67 C61 P 114.70(18) . . ? C62 C61 P 112.04(19) . . ? C66 C61 P 103.74(18) . . ? C63 C62 C61 110.0(2) . . ? C64 C63 C69 110.0(3) . . ? C64 C63 C62 109.7(2) . . ? C69 C63 C62 109.1(2) . . ? C65 C64 C63 109.7(3) . . ? C64 C65 C70 109.5(3) . . ? C64 C65 C66 109.7(3) . . ? C70 C65 C66 109.1(3) . . ? C65 C66 C61 110.1(2) . . ? C61 C67 C68 109.9(2) . . ? C70 C68 C69 109.5(3) . . ? C70 C68 C67 110.0(3) . . ? C69 C68 C67 109.2(3) . . ? C63 C69 C68 109.2(3) . . ? C68 C70 C65 109.6(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 C1 Pd P C51 -144.6(6) . . . . ? Cl1 Pd P C51 -76.36(9) . . . . ? Cl2 Pd P C51 98.19(9) . . . . ? C1 Pd P C61 -3.9(7) . . . . ? Cl1 Pd P C61 64.34(10) . . . . ? Cl2 Pd P C61 -121.11(10) . . . . ? C3 N2 C1 N1 -0.5(3) . . . . ? C31 N2 C1 N1 173.2(2) . . . . ? C3 N2 C1 Pd 168.46(18) . . . . ? C31 N2 C1 Pd -17.8(3) . . . . ? C2 N1 C1 N2 0.6(3) . . . . ? C11 N1 C1 N2 -167.0(2) . . . . ? C2 N1 C1 Pd -166.90(19) . . . . ? C11 N1 C1 Pd 25.6(4) . . . . ? Cl1 Pd C1 N2 -78.40(19) . . . . ? Cl2 Pd C1 N2 107.09(19) . . . . ? P Pd C1 N2 -9.8(8) . . . . ? Cl1 Pd C1 N1 87.1(2) . . . . ? Cl2 Pd C1 N1 -87.4(2) . . . . ? P Pd C1 N1 155.8(5) . . . . ? C1 N1 C2 C3 -0.4(3) . . . . ? C11 N1 C2 C3 167.8(2) . . . . ? N1 C2 C3 N2 0.1(3) . . . . ? C1 N2 C3 C2 0.3(3) . . . . ? C31 N2 C3 C2 -173.4(2) . . . . ? C1 N1 C11 C12 -97.5(3) . . . . ? C2 N1 C11 C12 96.2(3) . . . . ? C1 N1 C11 C16 88.4(3) . . . . ? C2 N1 C11 C16 -77.9(3) . . . . ? C16 C11 C12 C13 -0.9(4) . . . . ? N1 C11 C12 C13 -174.7(2) . . . . ? C16 C11 C12 C17 177.2(2) . . . . ? N1 C11 C12 C17 3.4(4) . . . . ? C11 C12 C13 C14 1.5(4) . . . . ? C17 C12 C13 C14 -176.7(3) . . . . ? C12 C13 C14 C15 -1.0(4) . . . . ? C13 C14 C15 C16 -0.2(4) . . . . ? C14 C15 C16 C11 0.7(4) . . . . ? C14 C15 C16 C20 179.8(3) . . . . ? C12 C11 C16 C15 -0.2(4) . . . . ? N1 C11 C16 C15 173.8(2) . . . . ? C12 C11 C16 C20 -179.3(2) . . . . ? N1 C11 C16 C20 -5.3(4) . . . . ? C13 C12 C17 C19 -59.2(3) . . . . ? C11 C12 C17 C19 122.7(3) . . . . ? C13 C12 C17 C18 63.7(3) . . . . ? C11 C12 C17 C18 -114.4(3) . . . . ? C15 C16 C20 C21 47.9(4) . . . . ? C11 C16 C20 C21 -133.0(3) . . . . ? C15 C16 C20 C22 -75.8(3) . . . . ? C11 C16 C20 C22 103.2(3) . . . . ? C1 N2 C31 C36 108.3(3) . . . . ? C3 N2 C31 C36 -78.8(3) . . . . ? C1 N2 C31 C32 -72.8(3) . . . . ? C3 N2 C31 C32 100.1(3) . . . . ? C36 C31 C32 C33 -5.0(4) . . . . ? N2 C31 C32 C33 176.1(2) . . . . ? C36 C31 C32 C37 171.9(3) . . . . ? N2 C31 C32 C37 -7.0(4) . . . . ? C31 C32 C33 C34 2.3(4) . . . . ? C37 C32 C33 C34 -174.7(3) . . . . ? C32 C33 C34 C35 1.5(5) . . . . ? C33 C34 C35 C36 -2.8(5) . . . . ? C32 C31 C36 C35 3.8(4) . . . . ? N2 C31 C36 C35 -177.3(2) . . . . ? C32 C31 C36 C40 -174.0(2) . . . . ? N2 C31 C36 C40 4.9(4) . . . . ? C34 C35 C36 C31 0.2(4) . . . . ? C34 C35 C36 C40 178.1(3) . . . . ? C33 C32 C37 C39 -26.9(4) . . . . ? C31 C32 C37 C39 156.3(3) . . . . ? C33 C32 C37 C38 97.4(3) . . . . ? C31 C32 C37 C38 -79.4(3) . . . . ? C31 C36 C40 C41 99.8(3) . . . . ? C35 C36 C40 C41 -77.9(3) . . . . ? C31 C36 C40 C42 -137.3(3) . . . . ? C35 C36 C40 C42 45.0(4) . . . . ? C61 P C51 C57 -61.2(2) . . . . ? Pd P C51 C57 78.94(18) . . . . ? C61 P C51 C52 63.8(2) . . . . ? Pd P C51 C52 -156.15(16) . . . . ? C61 P C51 C56 -178.78(17) . . . . ? Pd P C51 C56 -38.70(19) . . . . ? C57 C51 C52 C53 -58.6(3) . . . . ? C56 C51 C52 C53 59.4(3) . . . . ? P C51 C52 C53 174.71(19) . . . . ? C51 C52 C53 C59 59.7(3) . . . . ? C51 C52 C53 C54 -60.9(3) . . . . ? C59 C53 C54 C55 -59.8(3) . . . . ? C52 C53 C54 C55 60.7(3) . . . . ? C53 C54 C55 C60 59.7(3) . . . . ? C53 C54 C55 C56 -60.0(3) . . . . ? C54 C55 C56 C51 60.3(3) . . . . ? C60 C55 C56 C51 -60.1(3) . . . . ? C57 C51 C56 C55 59.2(3) . . . . ? C52 C51 C56 C55 -59.3(3) . . . . ? P C51 C56 C55 179.76(18) . . . . ? C52 C51 C57 C58 59.0(3) . . . . ? C56 C51 C57 C58 -58.8(3) . . . . ? P C51 C57 C58 -173.99(17) . . . . ? C51 C57 C58 C60 60.4(3) . . . . ? C51 C57 C58 C59 -60.0(3) . . . . ? C54 C53 C59 C58 59.7(3) . . . . ? C52 C53 C59 C58 -61.1(3) . . . . ? C60 C58 C59 C53 -59.4(3) . . . . ? C57 C58 C59 C53 61.1(3) . . . . ? C59 C58 C60 C55 58.9(3) . . . . ? C57 C58 C60 C55 -60.8(3) . . . . ? C54 C55 C60 C58 -59.7(3) . . . . ? C56 C55 C60 C58 60.3(3) . . . . ? C51 P C61 C67 65.2(2) . . . . ? Pd P C61 C67 -74.7(2) . . . . ? C51 P C61 C62 -59.3(2) . . . . ? Pd P C61 C62 160.85(17) . . . . ? C51 P C61 C66 -176.29(17) . . . . ? Pd P C61 C66 43.84(19) . . . . ? C67 C61 C62 C63 59.7(3) . . . . ? C66 C61 C62 C63 -58.6(3) . . . . ? P C61 C62 C63 -172.6(2) . . . . ? C61 C62 C63 C64 59.9(3) . . . . ? C61 C62 C63 C69 -60.6(3) . . . . ? C69 C63 C64 C65 59.7(3) . . . . ? C62 C63 C64 C65 -60.3(3) . . . . ? C63 C64 C65 C70 -59.6(3) . . . . ? C63 C64 C65 C66 60.2(3) . . . . ? C64 C65 C66 C61 -59.7(3) . . . . ? C70 C65 C66 C61 60.3(3) . . . . ? C67 C61 C66 C65 -59.6(3) . . . . ? C62 C61 C66 C65 58.5(3) . . . . ? P C61 C66 C65 177.9(2) . . . . ? C62 C61 C67 C68 -59.4(3) . . . . ? C66 C61 C67 C68 58.7(3) . . . . ? P C61 C67 C68 174.4(2) . . . . ? C61 C67 C68 C70 -59.6(3) . . . . ? C61 C67 C68 C69 60.6(3) . . . . ? C64 C63 C69 C68 -59.5(3) . . . . ? C62 C63 C69 C68 60.9(3) . . . . ? C70 C68 C69 C63 59.6(3) . . . . ? C67 C68 C69 C63 -60.8(3) . . . . ? C69 C68 C70 C65 -60.1(3) . . . . ? C67 C68 C70 C65 59.9(3) . . . . ? C64 C65 C70 C68 60.0(3) . . . . ? C66 C65 C70 C68 -60.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.551 _refine_diff_density_min -1.537 _refine_diff_density_rms 0.096 #===END data_dal09p1 _database_code_depnum_ccdc_archive 'CCDC 847280' #TrackingRef 'BTNHC_Combined-CIF.CIF' _vrf_DIFMX02_dal09p1 ; RESPONSE: The highest peak in the difference fourier map is located 0.9 angstroms from Pd ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H66 Cl N2 P Pd, 0.5(C5 H12)' _chemical_formula_sum 'C49.50 H72 Cl N2 P Pd' _chemical_formula_weight 867.91 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' 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 C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.4934(7) _cell_length_b 13.5722(5) _cell_length_c 31.6794(11) _cell_angle_alpha 90.00 _cell_angle_beta 95.8069(4) _cell_angle_gamma 90.00 _cell_volume 9193.9(6) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9792 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 28.48 _exptl_crystal_description ? _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.254 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3688 _exptl_absorpt_coefficient_mu 0.531 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7768 _exptl_absorpt_correction_T_max 0.8691 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 33027 _diffrn_reflns_av_R_equivalents 0.0156 _diffrn_reflns_av_sigmaI/netI 0.0122 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.49 _reflns_number_total 8574 _reflns_number_gt 8131 _reflns_threshold_expression I>2\s(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 '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^)+(0.0680P)^2^+37.3343P] 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 8574 _refine_ls_number_parameters 492 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1267 _refine_ls_wR_factor_gt 0.1252 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 Pd Pd 0.128783(10) 0.694717(16) 0.105056(7) 0.02673(10) Uani 1 1 d . . . Cl Cl 0.04283(4) 0.80191(6) 0.01115(2) 0.0400(2) Uani 1 1 d . . . P P 0.06442(4) 0.80766(5) 0.07725(2) 0.02579(17) Uani 1 1 d . . . N1 N 0.17527(11) 0.49097(17) 0.13312(7) 0.0242(5) Uani 1 1 d . . . N2 N 0.24353(11) 0.59841(18) 0.15485(7) 0.0246(5) Uani 1 1 d . . . C1 C 0.18533(12) 0.5898(2) 0.13381(8) 0.0229(5) Uani 1 1 d . . . C2 C 0.22622(14) 0.4396(2) 0.15227(10) 0.0317(6) Uani 1 1 d . . . H2 H 0.2301 0.3702 0.1550 0.038 Uiso 1 1 calc R . . C3 C 0.26895(14) 0.5074(2) 0.16614(10) 0.0318(6) Uani 1 1 d . . . H3 H 0.3089 0.4952 0.1809 0.038 Uiso 1 1 calc R . . C11 C 0.11716(13) 0.4491(2) 0.11409(10) 0.0260(6) Uani 1 1 d . . . C12 C 0.07359(14) 0.4176(2) 0.14093(10) 0.0310(6) Uani 1 1 d . . . C13 C 0.01644(15) 0.3828(3) 0.12194(12) 0.0393(8) Uani 1 1 d . . . H13 H -0.0145 0.3614 0.1393 0.047 Uiso 1 1 calc R . . C14 C 0.00418(16) 0.3790(3) 0.07855(12) 0.0447(8) Uani 1 1 d . . . H14 H -0.0351 0.3554 0.0662 0.054 Uiso 1 1 calc R . . C15 C 0.04855(17) 0.4094(3) 0.05270(11) 0.0416(8) Uani 1 1 d . . . H15 H 0.0395 0.4058 0.0228 0.050 Uiso 1 1 calc R . . C16 C 0.10666(15) 0.4455(2) 0.07001(10) 0.0314(6) Uani 1 1 d . . . C17 C 0.08629(15) 0.4245(3) 0.18895(10) 0.0372(7) Uani 1 1 d . . . H17 H 0.1327 0.4284 0.1957 0.045 Uiso 1 1 calc R . . C18 C 0.0645(3) 0.3334(4) 0.21113(15) 0.0700(14) Uani 1 1 d . . . H18A H 0.0827 0.2745 0.1994 0.105 Uiso 1 1 calc R . . H18B H 0.0188 0.3292 0.2068 0.105 Uiso 1 1 calc R . . H18C H 0.0779 0.3376 0.2416 0.105 Uiso 1 1 calc R . . C19 C 0.0590(3) 0.5194(4) 0.20501(14) 0.0763(15) Uani 1 1 d . . . H19A H 0.0738 0.5756 0.1893 0.115 Uiso 1 1 calc R . . H19B H 0.0725 0.5272 0.2353 0.115 Uiso 1 1 calc R . . H19C H 0.0133 0.5164 0.2007 0.115 Uiso 1 1 calc R . . C20 C 0.15592(17) 0.4767(2) 0.04136(10) 0.0366(7) Uani 1 1 d . . . H20 H 0.1866 0.5201 0.0584 0.044 Uiso 1 1 calc R . . C21 C 0.1286(2) 0.5355(3) 0.00305(13) 0.0584(11) Uani 1 1 d . . . H21A H 0.1058 0.5926 0.0126 0.088 Uiso 1 1 calc R . . H21B H 0.0998 0.4937 -0.0150 0.088 Uiso 1 1 calc R . . H21C H 0.1624 0.5581 -0.0131 0.088 Uiso 1 1 calc R . . C22 C 0.1913(2) 0.3867(3) 0.02782(14) 0.0580(11) Uani 1 1 d . . . H22A H 0.2087 0.3504 0.0530 0.087 Uiso 1 1 calc R . . H22B H 0.2254 0.4079 0.0115 0.087 Uiso 1 1 calc R . . H22C H 0.1627 0.3439 0.0102 0.087 Uiso 1 1 calc R . . C31 C 0.27448(14) 0.6921(2) 0.16107(10) 0.0294(6) Uani 1 1 d . . . C32 C 0.31160(14) 0.7244(2) 0.12999(11) 0.0360(7) Uani 1 1 d . . . C33 C 0.34046(18) 0.8164(3) 0.13642(15) 0.0511(10) Uani 1 1 d . . . H33 H 0.3660 0.8409 0.1160 0.061 Uiso 1 1 calc R . . C34 C 0.33253(19) 0.8717(3) 0.17166(16) 0.0582(11) Uani 1 1 d . . . H34 H 0.3530 0.9335 0.1756 0.070 Uiso 1 1 calc R . . C35 C 0.2952(2) 0.8386(3) 0.20133(14) 0.0551(10) Uani 1 1 d . . . H35 H 0.2899 0.8785 0.2253 0.066 Uiso 1 1 calc R . . C36 C 0.26475(16) 0.7473(3) 0.19708(11) 0.0402(8) Uani 1 1 d . . . C37 C 0.31981(17) 0.6642(3) 0.09064(12) 0.0435(8) Uani 1 1 d . . . H37 H 0.2977 0.6002 0.0937 0.052 Uiso 1 1 calc R . . C38 C 0.3883(2) 0.6403(4) 0.08690(17) 0.0655(13) Uani 1 1 d . . . H38A H 0.3917 0.6015 0.0611 0.098 Uiso 1 1 calc R . . H38B H 0.4052 0.6024 0.1118 0.098 Uiso 1 1 calc R . . H38C H 0.4120 0.7017 0.0854 0.098 Uiso 1 1 calc R . . C39 C 0.2893(3) 0.7136(4) 0.05078(15) 0.0774(16) Uani 1 1 d . . . H39A H 0.2958 0.6731 0.0260 0.116 Uiso 1 1 calc R . . H39B H 0.3079 0.7788 0.0477 0.116 Uiso 1 1 calc R . . H39C H 0.2443 0.7208 0.0529 0.116 Uiso 1 1 calc R . . C40 C 0.2221(2) 0.7116(3) 0.22908(12) 0.0547(10) Uani 1 1 d . . . H40 H 0.2033 0.6478 0.2184 0.066 Uiso 1 1 calc R . . C41 C 0.2588(3) 0.6917(5) 0.27218(17) 0.100(2) Uani 1 1 d . . . H41A H 0.2926 0.6450 0.2687 0.150 Uiso 1 1 calc R . . H41B H 0.2307 0.6639 0.2916 0.150 Uiso 1 1 calc R . . H41C H 0.2766 0.7536 0.2839 0.150 Uiso 1 1 calc R . . C42 C 0.1693(3) 0.7828(5) 0.2338(2) 0.101(2) Uani 1 1 d . . . H42A H 0.1456 0.7934 0.2061 0.152 Uiso 1 1 calc R . . H42B H 0.1864 0.8457 0.2448 0.152 Uiso 1 1 calc R . . H42C H 0.1415 0.7554 0.2536 0.152 Uiso 1 1 calc R . . C51 C -0.01581(14) 0.7933(2) 0.09488(10) 0.0293(6) Uani 1 1 d . . . C52 C -0.06286(14) 0.8773(2) 0.08440(11) 0.0347(7) Uani 1 1 d . . . H52A H -0.0695 0.8870 0.0533 0.042 Uiso 1 1 calc R . . H52B H -0.0462 0.9394 0.0974 0.042 Uiso 1 1 calc R . . C53 C -0.12547(15) 0.8515(3) 0.10161(12) 0.0410(8) Uani 1 1 d . . . H53 H -0.1558 0.9066 0.0950 0.049 Uiso 1 1 calc R . . C54 C -0.15213(16) 0.7574(3) 0.08101(13) 0.0477(9) Uani 1 1 d . . . H54A H -0.1591 0.7662 0.0499 0.057 Uiso 1 1 calc R . . H54B H -0.1928 0.7421 0.0916 0.057 Uiso 1 1 calc R . . C55 C -0.10612(17) 0.6722(3) 0.09169(13) 0.0463(9) Uani 1 1 d . . . H55 H -0.1235 0.6101 0.0782 0.056 Uiso 1 1 calc R . . C56 C -0.04329(16) 0.6968(2) 0.07460(12) 0.0393(8) Uani 1 1 d . . . H56A H -0.0497 0.7045 0.0434 0.047 Uiso 1 1 calc R . . H56B H -0.0134 0.6421 0.0812 0.047 Uiso 1 1 calc R . . C57 C -0.00643(15) 0.7783(3) 0.14343(10) 0.0357(7) Uani 1 1 d . . . H57A H 0.0111 0.8390 0.1573 0.043 Uiso 1 1 calc R . . H57B H 0.0236 0.7239 0.1504 0.043 Uiso 1 1 calc R . . C58 C -0.06955(17) 0.7534(3) 0.16035(12) 0.0446(8) Uani 1 1 d . . . H58 H -0.0631 0.7447 0.1918 0.053 Uiso 1 1 calc R . . C59 C -0.09587(18) 0.6587(3) 0.13979(14) 0.0512(10) Uani 1 1 d . . . H59A H -0.1360 0.6422 0.1509 0.061 Uiso 1 1 calc R . . H59B H -0.0663 0.6038 0.1468 0.061 Uiso 1 1 calc R . . C60 C -0.11490(17) 0.8377(3) 0.14960(12) 0.0455(8) Uani 1 1 d . . . H60A H -0.0978 0.8992 0.1630 0.055 Uiso 1 1 calc R . . H60B H -0.1552 0.8234 0.1609 0.055 Uiso 1 1 calc R . . C61 C 0.09537(14) 0.9373(2) 0.08181(10) 0.0292(6) Uani 1 1 d . . . C62 C 0.06163(17) 1.0171(3) 0.05366(12) 0.0420(8) Uani 1 1 d . . . H62A H 0.0596 0.9970 0.0235 0.050 Uiso 1 1 calc R . . H62B H 0.0183 1.0252 0.0612 0.050 Uiso 1 1 calc R . . C63 C 0.09699(18) 1.1152(3) 0.05993(14) 0.0519(10) Uani 1 1 d . . . H63 H 0.0743 1.1667 0.0418 0.062 Uiso 1 1 calc R . . C64 C 0.16316(19) 1.1038(3) 0.04675(14) 0.0541(10) Uani 1 1 d . . . H64A H 0.1612 1.0831 0.0167 0.065 Uiso 1 1 calc R . . H64B H 0.1855 1.1676 0.0498 0.065 Uiso 1 1 calc R . . C65 C 0.19768(16) 1.0268(3) 0.07494(12) 0.0432(8) Uani 1 1 d . . . H65 H 0.2411 1.0193 0.0666 0.052 Uiso 1 1 calc R . . C66 C 0.16340(15) 0.9278(2) 0.06897(11) 0.0376(7) Uani 1 1 d . . . H66A H 0.1864 0.8769 0.0867 0.045 Uiso 1 1 calc R . . H66B H 0.1620 0.9070 0.0389 0.045 Uiso 1 1 calc R . . C67 C 0.09997(16) 0.9701(2) 0.12841(11) 0.0377(7) Uani 1 1 d . . . H67A H 0.1225 0.9194 0.1465 0.045 Uiso 1 1 calc R . . H67B H 0.0574 0.9771 0.1375 0.045 Uiso 1 1 calc R . . C68 C 0.13485(19) 1.0691(3) 0.13406(13) 0.0488(9) Uani 1 1 d . . . H68 H 0.1369 1.0902 0.1644 0.059 Uiso 1 1 calc R . . C69 C 0.0997(2) 1.1465(3) 0.10601(16) 0.0583(11) Uani 1 1 d . . . H69A H 0.0567 1.1541 0.1143 0.070 Uiso 1 1 calc R . . H69B H 0.1212 1.2109 0.1099 0.070 Uiso 1 1 calc R . . C70 C 0.20117(18) 1.0575(3) 0.12110(13) 0.0486(9) Uani 1 1 d . . . H70A H 0.2240 1.1207 0.1252 0.058 Uiso 1 1 calc R . . H70B H 0.2241 1.0070 0.1391 0.058 Uiso 1 1 calc R . . C1S C 0.0654(4) 1.1070(5) 0.2885(3) 0.124(3) Uani 1 1 d . . . H1SA H 0.1044 1.1444 0.2886 0.187 Uiso 1 1 calc R . . H1SB H 0.0654 1.0707 0.3153 0.187 Uiso 1 1 calc R . . H1SC H 0.0298 1.1525 0.2855 0.187 Uiso 1 1 calc R . . C2S C 0.0602(4) 1.0364(6) 0.2525(2) 0.110(2) Uani 1 1 d . . . H2SA H 0.0965 0.9911 0.2556 0.133 Uiso 1 1 calc R . . H2SB H 0.0616 1.0733 0.2256 0.133 Uiso 1 1 calc R . . C3S C 0.0000 0.9759(6) 0.2500 0.094(3) Uani 1 2 d S . . H3SA H 0.0015 0.9328 0.2753 0.113 Uiso 0.50 1 calc PR . . H3SB H -0.0015 0.9328 0.2247 0.113 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.02406(14) 0.02165(14) 0.03403(15) 0.00223(8) 0.00074(9) 0.00462(8) Cl 0.0471(5) 0.0449(5) 0.0272(4) -0.0029(3) 0.0003(3) 0.0036(3) P 0.0270(4) 0.0237(4) 0.0265(4) -0.0002(3) 0.0017(3) 0.0059(3) N1 0.0234(11) 0.0232(12) 0.0264(12) 0.0028(9) 0.0040(9) 0.0001(9) N2 0.0231(11) 0.0269(12) 0.0241(11) 0.0007(9) 0.0032(9) -0.0008(9) C1 0.0226(13) 0.0237(14) 0.0232(13) -0.0009(10) 0.0066(10) -0.0004(11) C2 0.0305(15) 0.0262(15) 0.0381(17) 0.0091(12) 0.0028(12) 0.0050(12) C3 0.0257(14) 0.0338(16) 0.0353(16) 0.0084(13) 0.0001(12) 0.0052(12) C11 0.0244(13) 0.0196(13) 0.0339(15) -0.0004(11) 0.0014(11) 0.0000(11) C12 0.0301(15) 0.0260(15) 0.0374(16) 0.0044(12) 0.0056(12) 0.0000(12) C13 0.0289(16) 0.0389(18) 0.050(2) 0.0070(15) 0.0047(14) -0.0061(13) C14 0.0331(17) 0.043(2) 0.056(2) 0.0013(17) -0.0070(15) -0.0107(15) C15 0.048(2) 0.0378(18) 0.0370(17) -0.0033(14) -0.0055(15) -0.0060(15) C16 0.0381(16) 0.0228(14) 0.0335(16) -0.0014(12) 0.0050(13) -0.0016(12) C17 0.0314(16) 0.047(2) 0.0339(16) 0.0095(14) 0.0083(13) -0.0019(14) C18 0.078(3) 0.077(3) 0.053(3) 0.031(2) 0.001(2) -0.021(3) C19 0.109(4) 0.079(3) 0.042(2) -0.006(2) 0.014(2) 0.028(3) C20 0.0476(19) 0.0333(17) 0.0298(16) -0.0035(13) 0.0085(14) -0.0056(14) C21 0.079(3) 0.049(2) 0.050(2) 0.0165(18) 0.019(2) 0.012(2) C22 0.063(3) 0.056(2) 0.058(2) 0.012(2) 0.024(2) 0.018(2) C31 0.0236(14) 0.0288(16) 0.0346(16) -0.0016(12) -0.0032(12) -0.0015(11) C32 0.0253(15) 0.0316(16) 0.051(2) 0.0043(14) 0.0051(13) -0.0016(13) C33 0.0333(18) 0.039(2) 0.081(3) 0.0091(19) 0.0068(18) -0.0075(15) C34 0.045(2) 0.035(2) 0.090(3) -0.007(2) -0.013(2) -0.0096(17) C35 0.058(2) 0.044(2) 0.058(2) -0.0209(19) -0.016(2) -0.0001(19) C36 0.0408(18) 0.0433(19) 0.0344(17) -0.0089(14) -0.0076(14) 0.0006(15) C37 0.0421(19) 0.0417(19) 0.051(2) 0.0056(16) 0.0243(16) -0.0003(16) C38 0.057(3) 0.058(3) 0.088(3) 0.012(2) 0.035(2) 0.017(2) C39 0.095(4) 0.090(4) 0.049(3) 0.006(2) 0.017(3) 0.042(3) C40 0.068(3) 0.066(3) 0.0306(18) -0.0132(17) 0.0090(17) 0.001(2) C41 0.113(5) 0.138(6) 0.049(3) 0.017(3) 0.003(3) 0.021(4) C42 0.095(4) 0.135(6) 0.081(4) 0.031(4) 0.042(3) 0.046(4) C51 0.0264(15) 0.0261(15) 0.0359(16) -0.0022(12) 0.0049(12) 0.0041(12) C52 0.0303(16) 0.0322(16) 0.0411(17) 0.0000(13) 0.0010(13) 0.0092(13) C53 0.0277(16) 0.044(2) 0.051(2) -0.0002(16) 0.0043(14) 0.0125(14) C54 0.0287(17) 0.060(2) 0.054(2) -0.0034(18) 0.0016(15) -0.0008(16) C55 0.0347(18) 0.0409(19) 0.064(2) -0.0090(17) 0.0094(17) -0.0064(15) C56 0.0351(18) 0.0334(18) 0.050(2) -0.0097(14) 0.0076(15) -0.0003(13) C57 0.0301(16) 0.0441(18) 0.0330(16) 0.0044(14) 0.0031(13) 0.0037(14) C58 0.0378(18) 0.058(2) 0.0395(18) 0.0055(16) 0.0110(15) 0.0043(16) C59 0.0372(19) 0.045(2) 0.074(3) 0.0145(19) 0.0148(18) 0.0008(16) C60 0.0363(18) 0.051(2) 0.051(2) -0.0070(17) 0.0130(15) 0.0043(16) C61 0.0293(15) 0.0246(14) 0.0336(16) 0.0000(12) 0.0033(12) 0.0028(12) C62 0.0402(18) 0.0308(17) 0.053(2) 0.0080(15) -0.0039(15) 0.0033(14) C63 0.048(2) 0.0297(18) 0.075(3) 0.0163(18) -0.0093(19) 0.0022(15) C64 0.056(2) 0.042(2) 0.064(3) 0.0188(19) 0.0012(19) -0.0087(18) C65 0.0339(17) 0.0375(19) 0.059(2) 0.0087(16) 0.0072(15) -0.0028(14) C66 0.0344(17) 0.0349(17) 0.0450(19) 0.0027(14) 0.0108(14) 0.0029(14) C67 0.0403(18) 0.0350(17) 0.0379(17) -0.0024(14) 0.0052(14) -0.0016(14) C68 0.053(2) 0.045(2) 0.048(2) -0.0140(17) 0.0019(17) -0.0089(17) C69 0.051(2) 0.0265(18) 0.098(3) -0.0100(19) 0.009(2) -0.0015(16) C70 0.042(2) 0.041(2) 0.060(2) 0.0044(17) -0.0091(17) -0.0094(16) C1S 0.114(6) 0.086(5) 0.157(7) 0.000(5) -0.065(5) 0.003(4) C2S 0.112(5) 0.132(6) 0.086(4) 0.013(4) 0.005(4) 0.039(5) C3S 0.130(8) 0.069(5) 0.073(5) 0.000 -0.035(5) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd C1 2.027(3) . ? Pd P 2.1893(7) . ? Cl P 2.0998(11) . ? P C51 1.876(3) . ? P C61 1.881(3) . ? N1 C1 1.359(4) . ? N1 C2 1.385(4) . ? N1 C11 1.447(4) . ? N2 C1 1.361(4) . ? N2 C3 1.383(4) . ? N2 C31 1.439(4) . ? C2 C3 1.342(5) . ? C11 C16 1.393(4) . ? C11 C12 1.394(4) . ? C12 C13 1.394(4) . ? C12 C17 1.521(5) . ? C13 C14 1.374(5) . ? C14 C15 1.381(5) . ? C15 C16 1.400(5) . ? C16 C20 1.523(4) . ? C17 C18 1.520(5) . ? C17 C19 1.524(6) . ? C20 C21 1.520(5) . ? C20 C22 1.525(5) . ? C31 C36 1.399(5) . ? C31 C32 1.399(5) . ? C32 C33 1.399(5) . ? C32 C37 1.516(5) . ? C33 C34 1.370(6) . ? C34 C35 1.372(7) . ? C35 C36 1.401(6) . ? C36 C40 1.513(6) . ? C37 C39 1.519(6) . ? C37 C38 1.523(5) . ? C40 C42 1.511(7) . ? C40 C41 1.530(7) . ? C51 C52 1.538(4) . ? C51 C57 1.544(4) . ? C51 C56 1.549(4) . ? C52 C53 1.543(5) . ? C53 C54 1.520(5) . ? C53 C60 1.526(5) . ? C54 C55 1.537(5) . ? C55 C59 1.528(6) . ? C55 C56 1.542(5) . ? C57 C58 1.546(5) . ? C58 C60 1.519(5) . ? C58 C59 1.524(6) . ? C61 C67 1.535(4) . ? C61 C62 1.538(4) . ? C61 C66 1.562(4) . ? C62 C63 1.536(5) . ? C63 C69 1.516(7) . ? C63 C64 1.530(6) . ? C64 C65 1.519(5) . ? C65 C70 1.515(6) . ? C65 C66 1.535(5) . ? C67 C68 1.541(5) . ? C68 C69 1.526(6) . ? C68 C70 1.531(6) . ? C1S C2S 1.486(10) . ? C2S C3S 1.528(9) . ? C3S C2S 1.528(9) 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 C1 Pd P 176.58(8) . . ? C51 P C61 113.77(13) . . ? C51 P Cl 100.14(11) . . ? C61 P Cl 98.75(10) . . ? C51 P Pd 111.70(10) . . ? C61 P Pd 114.81(10) . . ? Cl P Pd 116.24(4) . . ? C1 N1 C2 111.8(2) . . ? C1 N1 C11 121.6(2) . . ? C2 N1 C11 126.6(2) . . ? C1 N2 C3 111.7(2) . . ? C1 N2 C31 122.1(2) . . ? C3 N2 C31 126.0(2) . . ? N1 C1 N2 103.3(2) . . ? N1 C1 Pd 126.8(2) . . ? N2 C1 Pd 129.7(2) . . ? C3 C2 N1 106.5(3) . . ? C2 C3 N2 106.7(3) . . ? C16 C11 C12 123.4(3) . . ? C16 C11 N1 118.5(3) . . ? C12 C11 N1 118.1(3) . . ? C11 C12 C13 117.2(3) . . ? C11 C12 C17 121.8(3) . . ? C13 C12 C17 120.9(3) . . ? C14 C13 C12 121.0(3) . . ? C13 C14 C15 120.5(3) . . ? C14 C15 C16 120.9(3) . . ? C11 C16 C15 116.9(3) . . ? C11 C16 C20 122.4(3) . . ? C15 C16 C20 120.7(3) . . ? C18 C17 C12 112.3(3) . . ? C18 C17 C19 112.7(4) . . ? C12 C17 C19 110.5(3) . . ? C21 C20 C16 112.7(3) . . ? C21 C20 C22 111.1(3) . . ? C16 C20 C22 110.0(3) . . ? C36 C31 C32 123.3(3) . . ? C36 C31 N2 118.7(3) . . ? C32 C31 N2 118.0(3) . . ? C33 C32 C31 117.0(3) . . ? C33 C32 C37 120.9(3) . . ? C31 C32 C37 122.1(3) . . ? C34 C33 C32 121.2(4) . . ? C33 C34 C35 120.5(4) . . ? C34 C35 C36 121.6(4) . . ? C31 C36 C35 116.4(3) . . ? C31 C36 C40 121.7(3) . . ? C35 C36 C40 121.9(3) . . ? C32 C37 C39 111.7(3) . . ? C32 C37 C38 111.9(3) . . ? C39 C37 C38 111.7(4) . . ? C42 C40 C36 111.9(4) . . ? C42 C40 C41 110.4(4) . . ? C36 C40 C41 111.2(4) . . ? C52 C51 C57 109.3(3) . . ? C52 C51 C56 108.8(3) . . ? C57 C51 C56 107.9(3) . . ? C52 C51 P 117.6(2) . . ? C57 C51 P 106.2(2) . . ? C56 C51 P 106.7(2) . . ? C51 C52 C53 109.4(3) . . ? C54 C53 C60 109.7(3) . . ? C54 C53 C52 110.1(3) . . ? C60 C53 C52 109.4(3) . . ? C53 C54 C55 109.4(3) . . ? C59 C55 C54 109.5(3) . . ? C59 C55 C56 109.4(3) . . ? C54 C55 C56 109.0(3) . . ? C55 C56 C51 110.4(3) . . ? C51 C57 C58 110.1(3) . . ? C60 C58 C59 109.7(3) . . ? C60 C58 C57 108.9(3) . . ? C59 C58 C57 109.7(3) . . ? C58 C59 C55 109.6(3) . . ? C58 C60 C53 110.0(3) . . ? C67 C61 C62 109.5(3) . . ? C67 C61 C66 107.7(3) . . ? C62 C61 C66 107.8(3) . . ? C67 C61 P 109.5(2) . . ? C62 C61 P 118.2(2) . . ? C66 C61 P 103.7(2) . . ? C63 C62 C61 109.8(3) . . ? C69 C63 C64 110.2(3) . . ? C69 C63 C62 109.7(3) . . ? C64 C63 C62 109.8(3) . . ? C65 C64 C63 108.7(3) . . ? C70 C65 C64 110.6(3) . . ? C70 C65 C66 109.6(3) . . ? C64 C65 C66 109.3(3) . . ? C65 C66 C61 110.3(3) . . ? C61 C67 C68 110.4(3) . . ? C69 C68 C70 109.5(3) . . ? C69 C68 C67 109.0(3) . . ? C70 C68 C67 109.5(3) . . ? C63 C69 C68 109.6(3) . . ? C65 C70 C68 109.3(3) . . ? C1S C2S C3S 112.6(6) . . ? C2S C3S C2S 115.0(8) . 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 C1 Pd P C51 -28.8(14) . . . . ? C1 Pd P C61 102.7(14) . . . . ? C1 Pd P Cl -142.8(14) . . . . ? C2 N1 C1 N2 -1.3(3) . . . . ? C11 N1 C1 N2 178.7(2) . . . . ? C2 N1 C1 Pd 173.7(2) . . . . ? C11 N1 C1 Pd -6.3(4) . . . . ? C3 N2 C1 N1 1.0(3) . . . . ? C31 N2 C1 N1 176.9(2) . . . . ? C3 N2 C1 Pd -173.8(2) . . . . ? C31 N2 C1 Pd 2.1(4) . . . . ? P Pd C1 N1 82.8(14) . . . . ? P Pd C1 N2 -103.6(13) . . . . ? C1 N1 C2 C3 1.2(3) . . . . ? C11 N1 C2 C3 -178.8(3) . . . . ? N1 C2 C3 N2 -0.6(3) . . . . ? C1 N2 C3 C2 -0.3(3) . . . . ? C31 N2 C3 C2 -176.0(3) . . . . ? C1 N1 C11 C16 75.3(4) . . . . ? C2 N1 C11 C16 -104.6(3) . . . . ? C1 N1 C11 C12 -102.4(3) . . . . ? C2 N1 C11 C12 77.6(4) . . . . ? C16 C11 C12 C13 -1.3(5) . . . . ? N1 C11 C12 C13 176.3(3) . . . . ? C16 C11 C12 C17 -178.8(3) . . . . ? N1 C11 C12 C17 -1.2(4) . . . . ? C11 C12 C13 C14 0.6(5) . . . . ? C17 C12 C13 C14 178.2(3) . . . . ? C12 C13 C14 C15 0.3(6) . . . . ? C13 C14 C15 C16 -0.6(6) . . . . ? C12 C11 C16 C15 1.0(5) . . . . ? N1 C11 C16 C15 -176.6(3) . . . . ? C12 C11 C16 C20 -177.7(3) . . . . ? N1 C11 C16 C20 4.7(4) . . . . ? C14 C15 C16 C11 0.0(5) . . . . ? C14 C15 C16 C20 178.7(3) . . . . ? C11 C12 C17 C18 -138.5(4) . . . . ? C13 C12 C17 C18 44.1(5) . . . . ? C11 C12 C17 C19 94.7(4) . . . . ? C13 C12 C17 C19 -82.8(4) . . . . ? C11 C16 C20 C21 -138.8(3) . . . . ? C15 C16 C20 C21 42.6(4) . . . . ? C11 C16 C20 C22 96.7(4) . . . . ? C15 C16 C20 C22 -81.9(4) . . . . ? C1 N2 C31 C36 88.8(4) . . . . ? C3 N2 C31 C36 -95.9(4) . . . . ? C1 N2 C31 C32 -89.5(3) . . . . ? C3 N2 C31 C32 85.8(4) . . . . ? C36 C31 C32 C33 0.8(5) . . . . ? N2 C31 C32 C33 179.1(3) . . . . ? C36 C31 C32 C37 -178.2(3) . . . . ? N2 C31 C32 C37 0.0(5) . . . . ? C31 C32 C33 C34 0.1(5) . . . . ? C37 C32 C33 C34 179.1(4) . . . . ? C32 C33 C34 C35 -0.9(6) . . . . ? C33 C34 C35 C36 0.8(6) . . . . ? C32 C31 C36 C35 -0.9(5) . . . . ? N2 C31 C36 C35 -179.1(3) . . . . ? C32 C31 C36 C40 177.5(3) . . . . ? N2 C31 C36 C40 -0.7(5) . . . . ? C34 C35 C36 C31 0.0(6) . . . . ? C34 C35 C36 C40 -178.3(4) . . . . ? C33 C32 C37 C39 -66.8(5) . . . . ? C31 C32 C37 C39 112.2(4) . . . . ? C33 C32 C37 C38 59.2(5) . . . . ? C31 C32 C37 C38 -121.8(4) . . . . ? C31 C36 C40 C42 -120.8(5) . . . . ? C35 C36 C40 C42 57.5(6) . . . . ? C31 C36 C40 C41 115.2(5) . . . . ? C35 C36 C40 C41 -66.5(5) . . . . ? C61 P C51 C52 37.5(3) . . . . ? Cl P C51 C52 -66.8(2) . . . . ? Pd P C51 C52 169.5(2) . . . . ? C61 P C51 C57 -85.1(2) . . . . ? Cl P C51 C57 170.56(19) . . . . ? Pd P C51 C57 46.9(2) . . . . ? C61 P C51 C56 160.0(2) . . . . ? Cl P C51 C56 55.6(2) . . . . ? Pd P C51 C56 -68.1(2) . . . . ? C57 C51 C52 C53 -58.8(3) . . . . ? C56 C51 C52 C53 58.8(3) . . . . ? P C51 C52 C53 -179.8(2) . . . . ? C51 C52 C53 C54 -60.7(4) . . . . ? C51 C52 C53 C60 60.0(4) . . . . ? C60 C53 C54 C55 -59.5(4) . . . . ? C52 C53 C54 C55 61.0(4) . . . . ? C53 C54 C55 C59 59.7(4) . . . . ? C53 C54 C55 C56 -60.0(4) . . . . ? C59 C55 C56 C51 -60.2(4) . . . . ? C54 C55 C56 C51 59.6(4) . . . . ? C52 C51 C56 C55 -59.1(4) . . . . ? C57 C51 C56 C55 59.3(4) . . . . ? P C51 C56 C55 173.1(3) . . . . ? C52 C51 C57 C58 58.9(4) . . . . ? C56 C51 C57 C58 -59.2(3) . . . . ? P C51 C57 C58 -173.4(2) . . . . ? C51 C57 C58 C60 -59.6(4) . . . . ? C51 C57 C58 C59 60.5(4) . . . . ? C60 C58 C59 C55 59.4(4) . . . . ? C57 C58 C59 C55 -60.2(4) . . . . ? C54 C55 C59 C58 -59.6(4) . . . . ? C56 C55 C59 C58 59.9(4) . . . . ? C59 C58 C60 C53 -59.4(4) . . . . ? C57 C58 C60 C53 60.6(4) . . . . ? C54 C53 C60 C58 59.7(4) . . . . ? C52 C53 C60 C58 -61.2(4) . . . . ? C51 P C61 C67 61.0(2) . . . . ? Cl P C61 C67 166.2(2) . . . . ? Pd P C61 C67 -69.5(2) . . . . ? C51 P C61 C62 -65.2(3) . . . . ? Cl P C61 C62 40.0(3) . . . . ? Pd P C61 C62 164.3(2) . . . . ? C51 P C61 C66 175.6(2) . . . . ? Cl P C61 C66 -79.2(2) . . . . ? Pd P C61 C66 45.2(2) . . . . ? C67 C61 C62 C63 57.9(4) . . . . ? C66 C61 C62 C63 -58.9(4) . . . . ? P C61 C62 C63 -175.9(3) . . . . ? C61 C62 C63 C69 -59.9(4) . . . . ? C61 C62 C63 C64 61.4(4) . . . . ? C69 C63 C64 C65 59.4(4) . . . . ? C62 C63 C64 C65 -61.6(4) . . . . ? C63 C64 C65 C70 -59.7(4) . . . . ? C63 C64 C65 C66 61.1(4) . . . . ? C70 C65 C66 C61 60.6(4) . . . . ? C64 C65 C66 C61 -60.8(4) . . . . ? C67 C61 C66 C65 -59.0(3) . . . . ? C62 C61 C66 C65 59.1(4) . . . . ? P C61 C66 C65 -174.9(2) . . . . ? C62 C61 C67 C68 -58.0(4) . . . . ? C66 C61 C67 C68 58.9(3) . . . . ? P C61 C67 C68 171.0(2) . . . . ? C61 C67 C68 C69 59.2(4) . . . . ? C61 C67 C68 C70 -60.7(4) . . . . ? C64 C63 C69 C68 -59.7(4) . . . . ? C62 C63 C69 C68 61.3(4) . . . . ? C70 C68 C69 C63 59.2(4) . . . . ? C67 C68 C69 C63 -60.6(4) . . . . ? C64 C65 C70 C68 59.9(4) . . . . ? C66 C65 C70 C68 -60.6(4) . . . . ? C69 C68 C70 C65 -59.1(4) . . . . ? C67 C68 C70 C65 60.5(4) . . . . ? C1S C2S C3S C2S 55.7(5) . . . 2 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.996 _refine_diff_density_min -0.642 _refine_diff_density_rms 0.081 #===END data_dal1155 _database_code_depnum_ccdc_archive 'CCDC 847281' #TrackingRef 'BTNHC_Combined-CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H54 Cl N2 P Pd' _chemical_formula_weight 675.62 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' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.2945(11) _cell_length_b 18.0530(10) _cell_length_c 22.0271(13) _cell_angle_alpha 90.00 _cell_angle_beta 96.3508(7) _cell_angle_gamma 90.00 _cell_volume 7230.3(7) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9993 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 25.86 _exptl_crystal_description fragment _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.241 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2848 _exptl_absorpt_coefficient_mu 0.655 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8031 _exptl_absorpt_correction_T_max 0.9350 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 28604 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 26.42 _reflns_number_total 7417 _reflns_number_gt 6018 _reflns_threshold_expression I>2\s(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 '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^)+(0.0312P)^2^+8.1267P] 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 7417 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0426 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0745 _refine_ls_wR_factor_gt 0.0679 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 Pd Pd 0.271682(9) 0.029611(10) 0.065948(7) 0.03008(6) Uani 1 1 d . . . Cl Cl 0.25832(4) 0.11118(5) -0.08898(3) 0.0581(2) Uani 1 1 d . . . P P 0.20885(3) 0.05013(4) -0.02322(3) 0.03208(14) Uani 1 1 d . . . N1 N 0.37993(9) -0.02069(10) 0.17736(8) 0.0275(4) Uani 1 1 d . . . N2 N 0.27444(9) 0.00492(10) 0.20500(8) 0.0259(4) Uani 1 1 d . . . C1 C 0.31172(11) 0.00315(12) 0.15441(9) 0.0257(4) Uani 1 1 d . . . C2 C 0.38443(12) -0.03339(13) 0.23980(10) 0.0339(5) Uani 1 1 d . . . H2 H 0.4264 -0.0503 0.2653 0.041 Uiso 1 1 calc R . . C3 C 0.31836(12) -0.01737(13) 0.25736(10) 0.0335(5) Uani 1 1 d . . . H3 H 0.3044 -0.0206 0.2975 0.040 Uiso 1 1 calc R . . C11 C 0.43942(11) -0.03184(13) 0.14037(10) 0.0318(5) Uani 1 1 d . . . C12 C 0.45383(13) -0.10380(15) 0.12201(11) 0.0397(6) Uani 1 1 d . . . C13 C 0.51139(15) -0.11303(18) 0.08561(13) 0.0537(7) Uani 1 1 d . . . H13 H 0.5230 -0.1613 0.0725 0.064 Uiso 1 1 calc R . . C14 C 0.55112(15) -0.0536(2) 0.06863(13) 0.0575(8) Uani 1 1 d . . . H14 H 0.5898 -0.0611 0.0439 0.069 Uiso 1 1 calc R . . C15 C 0.53538(14) 0.01647(18) 0.08706(12) 0.0518(7) Uani 1 1 d . . . H15 H 0.5632 0.0570 0.0745 0.062 Uiso 1 1 calc R . . C16 C 0.47922(12) 0.02970(15) 0.12402(11) 0.0381(6) Uani 1 1 d . . . C17 C 0.40629(15) -0.16909(14) 0.13617(13) 0.0459(6) Uani 1 1 d . . . H17 H 0.3787 -0.1541 0.1710 0.055 Uiso 1 1 calc R . . C18 C 0.34949(18) -0.18617(18) 0.08200(16) 0.0694(9) Uani 1 1 d . . . H18A H 0.3218 -0.1411 0.0698 0.083 Uiso 1 1 calc R . . H18B H 0.3156 -0.2244 0.0936 0.083 Uiso 1 1 calc R . . H18C H 0.3745 -0.2040 0.0477 0.083 Uiso 1 1 calc R . . C19 C 0.45013(19) -0.23837(18) 0.15599(16) 0.0703(9) Uani 1 1 d . . . H19A H 0.4866 -0.2264 0.1906 0.084 Uiso 1 1 calc R . . H19B H 0.4753 -0.2566 0.1219 0.084 Uiso 1 1 calc R . . H19C H 0.4167 -0.2767 0.1682 0.084 Uiso 1 1 calc R . . C20 C 0.46337(14) 0.10821(15) 0.14303(12) 0.0443(6) Uani 1 1 d . . . H20 H 0.4264 0.1057 0.1732 0.053 Uiso 1 1 calc R . . C21 C 0.42973(17) 0.15320(18) 0.08825(14) 0.0606(8) Uani 1 1 d . . . H21A H 0.3860 0.1277 0.0688 0.073 Uiso 1 1 calc R . . H21B H 0.4658 0.1585 0.0588 0.073 Uiso 1 1 calc R . . H21C H 0.4158 0.2023 0.1020 0.073 Uiso 1 1 calc R . . C22 C 0.53230(17) 0.14678(19) 0.17436(14) 0.0647(9) Uani 1 1 d . . . H22A H 0.5532 0.1170 0.2092 0.078 Uiso 1 1 calc R . . H22B H 0.5190 0.1958 0.1887 0.078 Uiso 1 1 calc R . . H22C H 0.5687 0.1521 0.1452 0.078 Uiso 1 1 calc R . . C31 C 0.20019(11) 0.03287(12) 0.20365(9) 0.0278(5) Uani 1 1 d . . . C32 C 0.14169(12) -0.01711(12) 0.19879(9) 0.0289(5) Uani 1 1 d . . . C33 C 0.07085(13) 0.01252(14) 0.19417(11) 0.0374(6) Uani 1 1 d . . . H33 H 0.0297 -0.0200 0.1908 0.045 Uiso 1 1 calc R . . C34 C 0.05936(14) 0.08787(15) 0.19441(11) 0.0428(6) Uani 1 1 d . . . H34 H 0.0106 0.1069 0.1897 0.051 Uiso 1 1 calc R . . C35 C 0.11816(14) 0.13564(15) 0.20140(11) 0.0413(6) Uani 1 1 d . . . H35 H 0.1095 0.1875 0.2024 0.050 Uiso 1 1 calc R . . C36 C 0.19034(13) 0.10949(13) 0.20704(10) 0.0337(5) Uani 1 1 d . . . C37 C 0.15329(12) -0.10026(13) 0.19726(10) 0.0331(5) Uani 1 1 d . . . H37 H 0.2035 -0.1111 0.2181 0.040 Uiso 1 1 calc R . . C38 C 0.09761(15) -0.14241(16) 0.23113(13) 0.0498(7) Uani 1 1 d . . . H38A H 0.1007 -0.1251 0.2735 0.060 Uiso 1 1 calc R . . H38B H 0.1085 -0.1955 0.2306 0.060 Uiso 1 1 calc R . . H38C H 0.0479 -0.1336 0.2110 0.060 Uiso 1 1 calc R . . C39 C 0.15059(16) -0.12687(15) 0.13144(12) 0.0479(6) Uani 1 1 d . . . H39A H 0.1871 -0.0997 0.1107 0.057 Uiso 1 1 calc R . . H39B H 0.1014 -0.1180 0.1102 0.057 Uiso 1 1 calc R . . H39C H 0.1616 -0.1800 0.1310 0.057 Uiso 1 1 calc R . . C40 C 0.25443(15) 0.16333(14) 0.21840(12) 0.0420(6) Uani 1 1 d . . . H40 H 0.3003 0.1329 0.2237 0.050 Uiso 1 1 calc R . . C41 C 0.2511(3) 0.2051(2) 0.27690(15) 0.1047(17) Uani 1 1 d . . . H41A H 0.2475 0.1700 0.3104 0.126 Uiso 1 1 calc R . . H41B H 0.2079 0.2376 0.2730 0.126 Uiso 1 1 calc R . . H41C H 0.2957 0.2350 0.2856 0.126 Uiso 1 1 calc R . . C42 C 0.2612(2) 0.2142(2) 0.16649(16) 0.0990(15) Uani 1 1 d . . . H42A H 0.3033 0.2473 0.1766 0.119 Uiso 1 1 calc R . . H42B H 0.2162 0.2436 0.1585 0.119 Uiso 1 1 calc R . . H42C H 0.2687 0.1853 0.1300 0.119 Uiso 1 1 calc R . . C51 C 0.18601(14) -0.03526(15) -0.07093(11) 0.0421(6) Uani 1 1 d . . . C52 C 0.26043(17) -0.07349(18) -0.07381(13) 0.0594(8) Uani 1 1 d . . . H52A H 0.2533 -0.1188 -0.0983 0.071 Uiso 1 1 calc R . . H52B H 0.2820 -0.0861 -0.0324 0.071 Uiso 1 1 calc R . . H52C H 0.2936 -0.0400 -0.0926 0.071 Uiso 1 1 calc R . . C53 C 0.14975(16) -0.02366(18) -0.13639(12) 0.0563(8) Uani 1 1 d . . . H53A H 0.1399 -0.0719 -0.1560 0.068 Uiso 1 1 calc R . . H53B H 0.1828 0.0050 -0.1595 0.068 Uiso 1 1 calc R . . H53C H 0.1034 0.0033 -0.1354 0.068 Uiso 1 1 calc R . . C54 C 0.1376(2) -0.08505(19) -0.03645(15) 0.0734(10) Uani 1 1 d . . . H54A H 0.1244 -0.1295 -0.0608 0.088 Uiso 1 1 calc R . . H54B H 0.0929 -0.0582 -0.0291 0.088 Uiso 1 1 calc R . . H54C H 0.1645 -0.0995 0.0027 0.088 Uiso 1 1 calc R . . C61 C 0.12613(14) 0.11006(16) -0.01734(11) 0.0440(6) Uani 1 1 d . . . C62 C 0.07304(15) 0.12050(18) -0.07526(13) 0.0589(8) Uani 1 1 d . . . H62A H 0.0326 0.1529 -0.0665 0.071 Uiso 1 1 calc R . . H62B H 0.0533 0.0723 -0.0894 0.071 Uiso 1 1 calc R . . H62C H 0.0992 0.1430 -0.1071 0.071 Uiso 1 1 calc R . . C63 C 0.08558(16) 0.0774(2) 0.03391(14) 0.0631(9) Uani 1 1 d . . . H63A H 0.0421 0.1075 0.0389 0.076 Uiso 1 1 calc R . . H63B H 0.1185 0.0772 0.0722 0.076 Uiso 1 1 calc R . . H63C H 0.0703 0.0265 0.0233 0.076 Uiso 1 1 calc R . . C64 C 0.15612(17) 0.18614(17) 0.00427(14) 0.0633(9) Uani 1 1 d . . . H64A H 0.1150 0.2199 0.0085 0.076 Uiso 1 1 calc R . . H64B H 0.1866 0.2063 -0.0257 0.076 Uiso 1 1 calc R . . H64C H 0.1859 0.1809 0.0438 0.076 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.02591(9) 0.03694(11) 0.02605(9) 0.00243(7) -0.00313(6) 0.00166(7) Cl 0.0480(4) 0.0727(5) 0.0536(4) 0.0266(4) 0.0061(3) -0.0056(4) P 0.0260(3) 0.0420(4) 0.0271(3) 0.0041(2) -0.0019(2) -0.0012(2) N1 0.0218(9) 0.0327(10) 0.0270(9) 0.0008(8) -0.0015(7) 0.0002(7) N2 0.0215(9) 0.0305(10) 0.0249(9) 0.0005(7) -0.0008(7) 0.0002(7) C1 0.0235(10) 0.0240(10) 0.0288(11) -0.0014(9) -0.0005(8) -0.0009(8) C2 0.0275(11) 0.0441(14) 0.0282(11) 0.0035(10) -0.0051(9) 0.0020(10) C3 0.0311(12) 0.0418(14) 0.0266(11) 0.0026(10) -0.0012(9) -0.0005(10) C11 0.0205(10) 0.0452(14) 0.0290(11) 0.0021(10) -0.0013(8) 0.0033(10) C12 0.0294(12) 0.0490(16) 0.0396(13) 0.0009(11) -0.0008(10) 0.0111(11) C13 0.0414(15) 0.068(2) 0.0524(16) -0.0039(14) 0.0087(13) 0.0191(14) C14 0.0313(14) 0.091(2) 0.0523(17) 0.0011(16) 0.0124(12) 0.0115(15) C15 0.0289(13) 0.080(2) 0.0470(15) 0.0085(15) 0.0063(11) -0.0052(13) C16 0.0247(11) 0.0536(16) 0.0349(12) 0.0057(11) -0.0025(9) -0.0019(11) C17 0.0483(15) 0.0352(14) 0.0543(16) -0.0001(12) 0.0067(12) 0.0112(12) C18 0.062(2) 0.055(2) 0.086(2) 0.0045(17) -0.0125(18) -0.0066(16) C19 0.075(2) 0.058(2) 0.076(2) 0.0118(17) 0.0000(18) 0.0211(17) C20 0.0392(14) 0.0476(16) 0.0452(15) 0.0045(12) 0.0011(11) -0.0109(12) C21 0.0588(19) 0.0542(19) 0.066(2) 0.0134(15) -0.0041(15) -0.0073(15) C22 0.0565(19) 0.070(2) 0.064(2) -0.0013(16) -0.0059(15) -0.0233(16) C31 0.0239(10) 0.0343(12) 0.0251(10) 0.0007(9) 0.0029(8) 0.0034(9) C32 0.0241(11) 0.0364(13) 0.0265(10) 0.0019(9) 0.0037(8) 0.0025(9) C33 0.0281(12) 0.0484(16) 0.0357(12) 0.0037(11) 0.0039(10) 0.0001(10) C34 0.0348(13) 0.0547(17) 0.0397(13) 0.0039(12) 0.0082(10) 0.0192(12) C35 0.0468(15) 0.0365(14) 0.0412(14) 0.0003(11) 0.0081(11) 0.0127(12) C36 0.0378(13) 0.0352(13) 0.0284(11) -0.0011(9) 0.0053(9) 0.0016(10) C37 0.0270(11) 0.0329(13) 0.0389(12) 0.0029(10) 0.0011(9) -0.0015(9) C38 0.0491(16) 0.0444(16) 0.0579(17) 0.0040(13) 0.0151(13) -0.0094(13) C39 0.0565(17) 0.0432(16) 0.0442(15) -0.0043(12) 0.0064(13) -0.0012(13) C40 0.0469(15) 0.0324(13) 0.0469(14) -0.0019(11) 0.0067(12) -0.0045(11) C41 0.140(4) 0.127(4) 0.0495(19) -0.029(2) 0.021(2) -0.089(3) C42 0.125(3) 0.108(3) 0.058(2) 0.027(2) -0.015(2) -0.067(3) C51 0.0401(14) 0.0548(17) 0.0306(12) -0.0055(11) 0.0010(10) -0.0007(12) C52 0.0640(19) 0.063(2) 0.0479(16) -0.0081(14) -0.0073(14) 0.0218(16) C53 0.0474(16) 0.081(2) 0.0377(14) -0.0185(14) -0.0088(12) 0.0124(15) C54 0.096(3) 0.067(2) 0.0597(19) -0.0189(17) 0.0221(18) -0.038(2) C61 0.0357(13) 0.0550(17) 0.0385(13) -0.0041(12) -0.0082(11) 0.0079(12) C62 0.0453(16) 0.074(2) 0.0520(17) -0.0128(15) -0.0178(13) 0.0206(15) C63 0.0409(16) 0.093(3) 0.0577(18) -0.0059(17) 0.0137(14) 0.0143(16) C64 0.063(2) 0.0556(19) 0.066(2) -0.0128(15) -0.0205(16) 0.0162(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd C1 2.061(2) . ? Pd P 2.1947(6) . ? Cl P 2.1029(9) . ? P C61 1.876(3) . ? P C51 1.886(3) . ? N1 C1 1.363(3) . ? N1 C2 1.388(3) . ? N1 C11 1.444(3) . ? N2 C1 1.370(3) . ? N2 C3 1.390(3) . ? N2 C31 1.446(3) . ? C2 C3 1.341(3) . ? C11 C12 1.394(3) . ? C11 C16 1.397(3) . ? C12 C13 1.402(3) . ? C12 C17 1.518(4) . ? C13 C14 1.371(4) . ? C14 C15 1.369(4) . ? C15 C16 1.400(4) . ? C16 C20 1.515(4) . ? C17 C19 1.523(4) . ? C17 C18 1.525(4) . ? C20 C21 1.527(4) . ? C20 C22 1.536(4) . ? C31 C32 1.395(3) . ? C31 C36 1.398(3) . ? C32 C33 1.395(3) . ? C32 C37 1.517(3) . ? C33 C34 1.377(4) . ? C34 C35 1.374(4) . ? C35 C36 1.395(3) . ? C36 C40 1.522(3) . ? C37 C39 1.523(3) . ? C37 C38 1.530(3) . ? C40 C42 1.483(4) . ? C40 C41 1.500(4) . ? C51 C54 1.522(4) . ? C51 C53 1.533(3) . ? C51 C52 1.534(4) . ? C61 C62 1.527(3) . ? C61 C64 1.535(4) . ? C61 C63 1.536(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 C1 Pd P 169.00(6) . . ? C61 P C51 112.27(11) . . ? C61 P Cl 99.04(9) . . ? C51 P Cl 97.48(9) . . ? C61 P Pd 112.47(8) . . ? C51 P Pd 114.99(8) . . ? Cl P Pd 118.83(3) . . ? C1 N1 C2 111.78(18) . . ? C1 N1 C11 123.43(17) . . ? C2 N1 C11 124.79(17) . . ? C1 N2 C3 111.97(17) . . ? C1 N2 C31 122.85(17) . . ? C3 N2 C31 124.99(18) . . ? N1 C1 N2 102.91(17) . . ? N1 C1 Pd 129.71(15) . . ? N2 C1 Pd 127.37(15) . . ? C3 C2 N1 107.08(19) . . ? C2 C3 N2 106.25(19) . . ? C12 C11 C16 123.1(2) . . ? C12 C11 N1 118.2(2) . . ? C16 C11 N1 118.8(2) . . ? C11 C12 C13 117.0(3) . . ? C11 C12 C17 122.2(2) . . ? C13 C12 C17 120.6(2) . . ? C14 C13 C12 121.2(3) . . ? C15 C14 C13 120.5(3) . . ? C14 C15 C16 121.5(3) . . ? C11 C16 C15 116.8(2) . . ? C11 C16 C20 123.5(2) . . ? C15 C16 C20 119.7(2) . . ? C12 C17 C19 113.6(2) . . ? C12 C17 C18 110.6(2) . . ? C19 C17 C18 110.5(2) . . ? C16 C20 C21 110.6(2) . . ? C16 C20 C22 112.1(2) . . ? C21 C20 C22 110.7(2) . . ? C32 C31 C36 122.8(2) . . ? C32 C31 N2 119.14(19) . . ? C36 C31 N2 118.06(19) . . ? C31 C32 C33 117.1(2) . . ? C31 C32 C37 122.26(19) . . ? C33 C32 C37 120.6(2) . . ? C34 C33 C32 121.3(2) . . ? C35 C34 C33 120.2(2) . . ? C34 C35 C36 121.3(2) . . ? C35 C36 C31 117.2(2) . . ? C35 C36 C40 120.2(2) . . ? C31 C36 C40 122.6(2) . . ? C32 C37 C39 110.08(19) . . ? C32 C37 C38 112.3(2) . . ? C39 C37 C38 110.7(2) . . ? C42 C40 C41 111.5(3) . . ? C42 C40 C36 113.4(2) . . ? C41 C40 C36 111.0(2) . . ? C54 C51 C53 109.6(2) . . ? C54 C51 C52 108.8(3) . . ? C53 C51 C52 108.4(2) . . ? C54 C51 P 108.04(18) . . ? C53 C51 P 117.3(2) . . ? C52 C51 P 104.34(18) . . ? C62 C61 C64 108.7(2) . . ? C62 C61 C63 110.3(2) . . ? C64 C61 C63 107.5(2) . . ? C62 C61 P 117.18(19) . . ? C64 C61 P 105.91(18) . . ? C63 C61 P 106.73(19) . . ? 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 Pd P C61 54.8(3) . . . . ? C1 Pd P C51 -75.4(3) . . . . ? C1 Pd P Cl 169.8(3) . . . . ? C2 N1 C1 N2 0.2(2) . . . . ? C11 N1 C1 N2 179.58(19) . . . . ? C2 N1 C1 Pd -179.25(16) . . . . ? C11 N1 C1 Pd 0.1(3) . . . . ? C3 N2 C1 N1 -0.2(2) . . . . ? C31 N2 C1 N1 174.99(18) . . . . ? C3 N2 C1 Pd 179.28(16) . . . . ? C31 N2 C1 Pd -5.5(3) . . . . ? P Pd C1 N1 148.6(2) . . . . ? P Pd C1 N2 -30.7(5) . . . . ? C1 N1 C2 C3 -0.1(3) . . . . ? C11 N1 C2 C3 -179.5(2) . . . . ? N1 C2 C3 N2 0.0(3) . . . . ? C1 N2 C3 C2 0.1(3) . . . . ? C31 N2 C3 C2 -174.9(2) . . . . ? C1 N1 C11 C12 -99.5(3) . . . . ? C2 N1 C11 C12 79.8(3) . . . . ? C1 N1 C11 C16 79.8(3) . . . . ? C2 N1 C11 C16 -100.9(3) . . . . ? C16 C11 C12 C13 0.2(3) . . . . ? N1 C11 C12 C13 179.4(2) . . . . ? C16 C11 C12 C17 -175.2(2) . . . . ? N1 C11 C12 C17 4.0(3) . . . . ? C11 C12 C13 C14 -0.5(4) . . . . ? C17 C12 C13 C14 175.0(2) . . . . ? C12 C13 C14 C15 0.1(4) . . . . ? C13 C14 C15 C16 0.6(4) . . . . ? C12 C11 C16 C15 0.5(3) . . . . ? N1 C11 C16 C15 -178.7(2) . . . . ? C12 C11 C16 C20 179.2(2) . . . . ? N1 C11 C16 C20 0.0(3) . . . . ? C14 C15 C16 C11 -0.9(4) . . . . ? C14 C15 C16 C20 -179.6(2) . . . . ? C11 C12 C17 C19 -138.3(3) . . . . ? C13 C12 C17 C19 46.5(3) . . . . ? C11 C12 C17 C18 96.8(3) . . . . ? C13 C12 C17 C18 -78.5(3) . . . . ? C11 C16 C20 C21 -109.2(3) . . . . ? C15 C16 C20 C21 69.4(3) . . . . ? C11 C16 C20 C22 126.8(3) . . . . ? C15 C16 C20 C22 -54.6(3) . . . . ? C1 N2 C31 C32 98.2(3) . . . . ? C3 N2 C31 C32 -87.2(3) . . . . ? C1 N2 C31 C36 -81.5(3) . . . . ? C3 N2 C31 C36 93.1(3) . . . . ? C36 C31 C32 C33 3.2(3) . . . . ? N2 C31 C32 C33 -176.48(19) . . . . ? C36 C31 C32 C37 -177.9(2) . . . . ? N2 C31 C32 C37 2.4(3) . . . . ? C31 C32 C33 C34 0.0(3) . . . . ? C37 C32 C33 C34 -178.8(2) . . . . ? C32 C33 C34 C35 -2.3(4) . . . . ? C33 C34 C35 C36 1.4(4) . . . . ? C34 C35 C36 C31 1.6(3) . . . . ? C34 C35 C36 C40 -176.5(2) . . . . ? C32 C31 C36 C35 -4.0(3) . . . . ? N2 C31 C36 C35 175.67(19) . . . . ? C32 C31 C36 C40 174.0(2) . . . . ? N2 C31 C36 C40 -6.3(3) . . . . ? C31 C32 C37 C39 -92.7(3) . . . . ? C33 C32 C37 C39 86.1(3) . . . . ? C31 C32 C37 C38 143.4(2) . . . . ? C33 C32 C37 C38 -37.8(3) . . . . ? C35 C36 C40 C42 -66.3(4) . . . . ? C31 C36 C40 C42 115.7(3) . . . . ? C35 C36 C40 C41 60.1(3) . . . . ? C31 C36 C40 C41 -117.9(3) . . . . ? C61 P C51 C54 -68.0(2) . . . . ? Cl P C51 C54 -171.0(2) . . . . ? Pd P C51 C54 62.2(2) . . . . ? C61 P C51 C53 56.3(2) . . . . ? Cl P C51 C53 -46.7(2) . . . . ? Pd P C51 C53 -173.38(17) . . . . ? C61 P C51 C52 176.27(18) . . . . ? Cl P C51 C52 73.27(18) . . . . ? Pd P C51 C52 -53.4(2) . . . . ? C51 P C61 C62 -41.2(3) . . . . ? Cl P C61 C62 60.7(2) . . . . ? Pd P C61 C62 -172.8(2) . . . . ? C51 P C61 C64 -162.70(18) . . . . ? Cl P C61 C64 -60.72(19) . . . . ? Pd P C61 C64 65.7(2) . . . . ? C51 P C61 C63 82.9(2) . . . . ? Cl P C61 C63 -175.08(17) . . . . ? Pd P C61 C63 -48.6(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.533 _refine_diff_density_min -0.434 _refine_diff_density_rms 0.056 #===END data_dal1164 _database_code_depnum_ccdc_archive 'CCDC 847282' #TrackingRef 'BTNHC_Combined-CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H58 Cl N2 P Pd' _chemical_formula_sum 'C39 H58 Cl N2 P Pd' _chemical_formula_weight 727.69 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' 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)/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 12.3612(6) _cell_length_b 21.7925(10) _cell_length_c 14.5546(7) _cell_angle_alpha 90.00 _cell_angle_beta 96.2170(10) _cell_angle_gamma 90.00 _cell_volume 3897.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5809 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 20.70 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.240 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 0.613 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7816 _exptl_absorpt_correction_T_max 0.9747 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 31101 _diffrn_reflns_av_R_equivalents 0.0784 _diffrn_reflns_av_sigmaI/netI 0.0598 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 26.51 _reflns_number_total 8058 _reflns_number_gt 5491 _reflns_threshold_expression I>2\s(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 '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^)+(0.0370P)^2^+3.3703P] 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 8058 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0791 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1023 _refine_ls_wR_factor_gt 0.0875 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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 Pd Pd 0.19652(2) 0.104518(13) 0.360236(18) 0.03153(9) Uani 1 1 d . . . Cl Cl 0.11310(9) -0.03282(4) 0.22167(7) 0.0458(3) Uani 1 1 d . . . P P 0.14502(8) 0.06237(4) 0.22711(6) 0.0312(2) Uani 1 1 d . . . N1 N 0.1639(2) 0.21343(12) 0.48462(18) 0.0260(6) Uani 1 1 d . . . N2 N 0.3189(2) 0.17466(12) 0.52840(19) 0.0276(6) Uani 1 1 d . . . C1 C 0.2300(2) 0.16564(15) 0.4659(2) 0.0252(7) Uani 1 1 d . . . C2 C 0.2108(3) 0.25035(16) 0.5549(2) 0.0337(8) Uani 1 1 d . . . H2 H 0.1797 0.2859 0.5791 0.040 Uiso 1 1 calc R . . C3 C 0.3088(3) 0.22623(16) 0.5825(3) 0.0354(9) Uani 1 1 d . . . H3 H 0.3610 0.2415 0.6298 0.042 Uiso 1 1 calc R . . C11 C 0.0570(2) 0.22342(15) 0.4359(2) 0.0242(7) Uani 1 1 d . . . C12 C 0.0474(3) 0.26460(15) 0.3625(2) 0.0300(8) Uani 1 1 d . . . C13 C -0.0568(3) 0.27580(16) 0.3193(2) 0.0353(9) Uani 1 1 d . . . H13 H -0.0666 0.3045 0.2700 0.042 Uiso 1 1 calc R . . C14 C -0.1460(3) 0.24584(17) 0.3469(3) 0.0375(9) Uani 1 1 d . . . H14 H -0.2164 0.2534 0.3161 0.045 Uiso 1 1 calc R . . C15 C -0.1328(3) 0.20483(17) 0.4193(3) 0.0359(9) Uani 1 1 d . . . H15 H -0.1949 0.1843 0.4375 0.043 Uiso 1 1 calc R . . C16 C -0.0310(3) 0.19274(15) 0.4666(2) 0.0291(8) Uani 1 1 d . . . C17 C 0.1452(3) 0.29553(18) 0.3274(3) 0.0415(10) Uani 1 1 d . . . H17 H 0.2121 0.2792 0.3641 0.050 Uiso 1 1 calc R . . C18 C 0.1517(5) 0.2793(3) 0.2266(4) 0.101(2) Uani 1 1 d . . . H18A H 0.1550 0.2346 0.2199 0.121 Uiso 1 1 calc R . . H18B H 0.2172 0.2978 0.2059 0.121 Uiso 1 1 calc R . . H18C H 0.0871 0.2951 0.1890 0.121 Uiso 1 1 calc R . . C19 C 0.1447(4) 0.3641(2) 0.3392(3) 0.0626(13) Uani 1 1 d . . . H19A H 0.1441 0.3742 0.4047 0.075 Uiso 1 1 calc R . . H19B H 0.0796 0.3813 0.3039 0.075 Uiso 1 1 calc R . . H19C H 0.2099 0.3816 0.3165 0.075 Uiso 1 1 calc R . . C20 C -0.0186(3) 0.14895(17) 0.5480(3) 0.0377(9) Uani 1 1 d . . . H20 H 0.0609 0.1447 0.5685 0.045 Uiso 1 1 calc R . . C21 C -0.0626(4) 0.08557(18) 0.5228(3) 0.0635(13) Uani 1 1 d . . . H21A H -0.0497 0.0584 0.5765 0.076 Uiso 1 1 calc R . . H21B H -0.0257 0.0691 0.4718 0.076 Uiso 1 1 calc R . . H21C H -0.1410 0.0882 0.5036 0.076 Uiso 1 1 calc R . . C22 C -0.0725(6) 0.1749(2) 0.6279(3) 0.103(2) Uani 1 1 d . . . H22A H -0.0385 0.2142 0.6470 0.123 Uiso 1 1 calc R . . H22B H -0.0639 0.1461 0.6799 0.123 Uiso 1 1 calc R . . H22C H -0.1501 0.1814 0.6087 0.123 Uiso 1 1 calc R . . C31 C 0.4111(3) 0.13328(16) 0.5415(2) 0.0297(8) Uani 1 1 d . . . C32 C 0.4977(3) 0.14213(18) 0.4898(3) 0.0388(9) Uani 1 1 d . . . C33 C 0.5866(3) 0.1030(2) 0.5072(3) 0.0493(10) Uani 1 1 d . . . H33 H 0.6479 0.1082 0.4738 0.059 Uiso 1 1 calc R . . C34 C 0.5870(3) 0.0570(2) 0.5723(3) 0.0531(12) Uani 1 1 d . . . H34 H 0.6485 0.0308 0.5832 0.064 Uiso 1 1 calc R . . C35 C 0.4996(3) 0.04863(18) 0.6214(3) 0.0477(11) Uani 1 1 d . . . H35 H 0.5011 0.0165 0.6656 0.057 Uiso 1 1 calc R . . C36 C 0.4080(3) 0.08670(16) 0.6073(2) 0.0343(8) Uani 1 1 d . . . C37 C 0.4967(3) 0.1928(2) 0.4178(3) 0.0537(12) Uani 1 1 d . . . H37 H 0.4190 0.2046 0.4004 0.064 Uiso 1 1 calc R . . C38 C 0.5425(4) 0.1716(3) 0.3295(3) 0.0759(16) Uani 1 1 d . . . H38A H 0.4985 0.1376 0.3019 0.091 Uiso 1 1 calc R . . H38B H 0.6179 0.1579 0.3446 0.091 Uiso 1 1 calc R . . H38C H 0.5405 0.2058 0.2856 0.091 Uiso 1 1 calc R . . C39 C 0.5561(4) 0.2497(2) 0.4576(4) 0.0722(15) Uani 1 1 d . . . H39A H 0.5242 0.2630 0.5131 0.087 Uiso 1 1 calc R . . H39B H 0.5489 0.2827 0.4115 0.087 Uiso 1 1 calc R . . H39C H 0.6332 0.2401 0.4737 0.087 Uiso 1 1 calc R . . C40 C 0.3077(3) 0.07560(18) 0.6562(3) 0.0409(9) Uani 1 1 d . . . H40 H 0.2660 0.1150 0.6550 0.049 Uiso 1 1 calc R . . C41 C 0.2347(3) 0.02777(19) 0.6040(3) 0.0486(11) Uani 1 1 d . . . H41A H 0.2203 0.0399 0.5389 0.058 Uiso 1 1 calc R . . H41B H 0.1658 0.0250 0.6313 0.058 Uiso 1 1 calc R . . H41C H 0.2711 -0.0122 0.6081 0.058 Uiso 1 1 calc R . . C42 C 0.3325(4) 0.0562(2) 0.7582(3) 0.0627(13) Uani 1 1 d . . . H42A H 0.3788 0.0872 0.7916 0.075 Uiso 1 1 calc R . . H42B H 0.3702 0.0165 0.7615 0.075 Uiso 1 1 calc R . . H42C H 0.2642 0.0525 0.7863 0.075 Uiso 1 1 calc R . . C51 C 0.0133(3) 0.09007(15) 0.1714(2) 0.0306(8) Uani 1 1 d . . . H51 H 0.0208 0.1355 0.1653 0.037 Uiso 1 1 calc R . . C52 C -0.0247(3) 0.06606(19) 0.0742(2) 0.0407(9) Uani 1 1 d . . . H52A H 0.0302 0.0769 0.0321 0.049 Uiso 1 1 calc R . . H52B H -0.0299 0.0208 0.0761 0.049 Uiso 1 1 calc R . . C53 C -0.1344(3) 0.09244(18) 0.0361(3) 0.0411(9) Uani 1 1 d . . . H53A H -0.1274 0.1373 0.0275 0.049 Uiso 1 1 calc R . . H53B H -0.1575 0.0739 -0.0250 0.049 Uiso 1 1 calc R . . C54 C -0.2203(3) 0.0800(2) 0.1007(3) 0.0475(10) Uani 1 1 d . . . H54A H -0.2899 0.0992 0.0755 0.057 Uiso 1 1 calc R . . H54B H -0.2323 0.0352 0.1049 0.057 Uiso 1 1 calc R . . C55 C -0.1859(3) 0.1053(2) 0.1964(3) 0.0438(9) Uani 1 1 d . . . H55A H -0.2413 0.0945 0.2380 0.053 Uiso 1 1 calc R . . H55B H -0.1817 0.1506 0.1932 0.053 Uiso 1 1 calc R . . C56 C -0.0752(3) 0.07983(18) 0.2362(3) 0.0388(9) Uani 1 1 d . . . H56A H -0.0824 0.0353 0.2476 0.047 Uiso 1 1 calc R . . H56B H -0.0528 0.0999 0.2962 0.047 Uiso 1 1 calc R . . C61 C 0.2354(3) 0.06528(16) 0.1340(2) 0.0330(8) Uani 1 1 d . . . H61 H 0.2006 0.0416 0.0798 0.040 Uiso 1 1 calc R . . C62 C 0.2512(3) 0.13218(18) 0.1038(3) 0.0457(10) Uani 1 1 d . . . H62A H 0.1797 0.1502 0.0812 0.055 Uiso 1 1 calc R . . H62B H 0.2828 0.1566 0.1575 0.055 Uiso 1 1 calc R . . C63 C 0.3264(4) 0.1350(2) 0.0273(3) 0.0618(13) Uani 1 1 d . . . H63A H 0.2911 0.1142 -0.0285 0.074 Uiso 1 1 calc R . . H63B H 0.3385 0.1784 0.0112 0.074 Uiso 1 1 calc R . . C64 C 0.4352(4) 0.1048(2) 0.0567(3) 0.0629(13) Uani 1 1 d . . . H64A H 0.4796 0.1048 0.0040 0.076 Uiso 1 1 calc R . . H64B H 0.4746 0.1288 0.1075 0.076 Uiso 1 1 calc R . . C65 C 0.4207(3) 0.0397(2) 0.0885(3) 0.0548(12) Uani 1 1 d . . . H65A H 0.4926 0.0223 0.1113 0.066 Uiso 1 1 calc R . . H65B H 0.3896 0.0145 0.0355 0.066 Uiso 1 1 calc R . . C66 C 0.3459(3) 0.03676(18) 0.1652(3) 0.0424(10) Uani 1 1 d . . . H66A H 0.3358 -0.0066 0.1829 0.051 Uiso 1 1 calc R . . H66B H 0.3800 0.0589 0.2203 0.051 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.03026(15) 0.03804(16) 0.02618(14) -0.00560(13) 0.00253(10) 0.00197(14) Cl 0.0631(7) 0.0306(5) 0.0453(6) 0.0040(4) 0.0133(5) 0.0026(5) P 0.0388(5) 0.0287(5) 0.0264(5) -0.0005(4) 0.0055(4) 0.0033(4) N1 0.0235(14) 0.0259(15) 0.0278(15) 0.0010(12) -0.0003(12) -0.0020(12) N2 0.0237(15) 0.0304(16) 0.0277(15) 0.0019(12) -0.0014(12) -0.0020(12) C1 0.0209(17) 0.0265(18) 0.0282(18) 0.0050(14) 0.0027(14) -0.0025(14) C2 0.033(2) 0.0276(19) 0.039(2) -0.0068(16) -0.0005(16) -0.0010(16) C3 0.036(2) 0.030(2) 0.037(2) -0.0042(16) -0.0049(17) -0.0064(16) C11 0.0205(17) 0.0266(18) 0.0250(17) -0.0039(14) 0.0001(13) 0.0025(14) C12 0.0249(18) 0.0290(19) 0.036(2) -0.0001(15) 0.0038(15) 0.0035(15) C13 0.035(2) 0.033(2) 0.036(2) 0.0025(16) -0.0041(16) 0.0085(17) C14 0.0213(18) 0.040(2) 0.050(2) -0.0064(19) -0.0034(17) 0.0074(16) C15 0.0239(18) 0.040(2) 0.044(2) -0.0103(18) 0.0048(16) -0.0051(16) C16 0.0295(19) 0.0277(19) 0.0304(19) -0.0054(15) 0.0039(15) -0.0020(15) C17 0.032(2) 0.046(2) 0.046(2) 0.0196(19) 0.0054(18) -0.0011(18) C18 0.117(5) 0.094(4) 0.107(5) -0.036(4) 0.080(4) -0.040(4) C19 0.057(3) 0.050(3) 0.082(4) -0.004(3) 0.015(3) -0.020(2) C20 0.034(2) 0.045(2) 0.035(2) 0.0028(17) 0.0065(16) -0.0060(17) C21 0.084(4) 0.035(2) 0.069(3) 0.007(2) -0.007(3) -0.007(2) C22 0.200(7) 0.064(4) 0.054(3) 0.005(3) 0.063(4) 0.015(4) C31 0.0223(17) 0.0320(19) 0.0321(19) -0.0027(16) -0.0090(14) -0.0005(15) C32 0.0239(19) 0.047(2) 0.044(2) 0.0004(19) -0.0033(16) -0.0023(17) C33 0.025(2) 0.061(3) 0.061(3) -0.008(2) 0.0020(18) 0.002(2) C34 0.034(2) 0.053(3) 0.068(3) -0.014(2) -0.015(2) 0.011(2) C35 0.048(3) 0.038(2) 0.053(3) 0.002(2) -0.013(2) 0.0050(19) C36 0.035(2) 0.031(2) 0.035(2) -0.0035(16) -0.0074(16) 0.0004(16) C37 0.033(2) 0.072(3) 0.057(3) 0.018(2) 0.008(2) -0.005(2) C38 0.074(4) 0.099(4) 0.055(3) 0.003(3) 0.007(3) -0.029(3) C39 0.082(4) 0.052(3) 0.087(4) 0.009(3) 0.034(3) -0.002(3) C40 0.046(2) 0.035(2) 0.040(2) 0.0085(17) 0.0011(19) -0.0009(18) C41 0.048(3) 0.053(3) 0.043(2) 0.008(2) -0.0028(19) -0.013(2) C42 0.081(3) 0.062(3) 0.042(3) 0.008(2) -0.003(2) -0.024(3) C51 0.039(2) 0.0260(19) 0.0263(18) -0.0029(14) 0.0031(15) 0.0026(15) C52 0.047(2) 0.047(2) 0.029(2) -0.0058(17) 0.0038(17) 0.0038(19) C53 0.047(2) 0.044(2) 0.031(2) -0.0021(17) -0.0028(17) 0.0046(18) C54 0.044(2) 0.048(3) 0.049(3) -0.004(2) -0.001(2) -0.001(2) C55 0.037(2) 0.053(2) 0.042(2) -0.001(2) 0.0069(17) 0.000(2) C56 0.046(2) 0.041(2) 0.031(2) -0.0032(17) 0.0074(17) 0.0031(18) C61 0.040(2) 0.031(2) 0.0288(19) 0.0007(15) 0.0060(16) 0.0013(16) C62 0.048(2) 0.044(2) 0.047(2) 0.012(2) 0.016(2) 0.0088(19) C63 0.068(3) 0.067(3) 0.055(3) 0.022(2) 0.027(2) 0.007(3) C64 0.048(3) 0.085(4) 0.060(3) 0.016(3) 0.025(2) 0.008(3) C65 0.046(3) 0.068(3) 0.052(3) 0.003(2) 0.017(2) 0.018(2) C66 0.045(2) 0.042(2) 0.041(2) 0.0034(18) 0.0104(18) 0.0098(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd C1 2.043(3) . ? Pd P 2.1763(10) . ? Cl P 2.1114(13) . ? P C51 1.841(4) . ? P C61 1.848(3) . ? N1 C1 1.369(4) . ? N1 C2 1.379(4) . ? N1 C11 1.446(4) . ? N2 C1 1.363(4) . ? N2 C3 1.386(4) . ? N2 C31 1.450(4) . ? C2 C3 1.343(5) . ? C11 C12 1.391(5) . ? C11 C16 1.391(4) . ? C12 C13 1.392(5) . ? C12 C17 1.520(5) . ? C13 C14 1.378(5) . ? C14 C15 1.378(5) . ? C15 C16 1.393(5) . ? C16 C20 1.516(5) . ? C17 C19 1.505(6) . ? C17 C18 1.520(6) . ? C20 C22 1.512(6) . ? C20 C21 1.515(5) . ? C31 C32 1.386(5) . ? C31 C36 1.400(5) . ? C32 C33 1.393(5) . ? C32 C37 1.521(5) . ? C33 C34 1.380(6) . ? C34 C35 1.370(6) . ? C35 C36 1.401(5) . ? C36 C40 1.514(5) . ? C37 C39 1.523(6) . ? C37 C38 1.530(6) . ? C40 C41 1.527(5) . ? C40 C42 1.542(5) . ? C51 C52 1.534(5) . ? C51 C56 1.535(5) . ? C52 C53 1.522(5) . ? C53 C54 1.517(5) . ? C54 C55 1.515(5) . ? C55 C56 1.531(5) . ? C61 C66 1.525(5) . ? C61 C62 1.541(5) . ? C62 C63 1.527(5) . ? C63 C64 1.516(6) . ? C64 C65 1.509(6) . ? C65 C66 1.527(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd P 164.03(9) . . ? C51 P C61 104.01(16) . . ? C51 P Cl 98.79(12) . . ? C61 P Cl 97.56(12) . . ? C51 P Pd 114.39(11) . . ? C61 P Pd 119.78(12) . . ? Cl P Pd 118.91(5) . . ? C1 N1 C2 112.3(3) . . ? C1 N1 C11 123.4(3) . . ? C2 N1 C11 124.3(3) . . ? C1 N2 C3 112.4(3) . . ? C1 N2 C31 124.3(3) . . ? C3 N2 C31 123.2(3) . . ? N2 C1 N1 102.3(3) . . ? N2 C1 Pd 132.8(2) . . ? N1 C1 Pd 124.7(2) . . ? C3 C2 N1 106.7(3) . . ? C2 C3 N2 106.3(3) . . ? C12 C11 C16 123.5(3) . . ? C12 C11 N1 118.1(3) . . ? C16 C11 N1 118.4(3) . . ? C11 C12 C13 117.3(3) . . ? C11 C12 C17 122.6(3) . . ? C13 C12 C17 120.1(3) . . ? C14 C13 C12 121.0(3) . . ? C13 C14 C15 119.9(3) . . ? C14 C15 C16 121.7(3) . . ? C11 C16 C15 116.6(3) . . ? C11 C16 C20 122.5(3) . . ? C15 C16 C20 121.0(3) . . ? C19 C17 C12 112.9(3) . . ? C19 C17 C18 110.0(4) . . ? C12 C17 C18 110.4(3) . . ? C22 C20 C21 110.6(4) . . ? C22 C20 C16 110.5(3) . . ? C21 C20 C16 112.4(3) . . ? C32 C31 C36 123.6(3) . . ? C32 C31 N2 119.0(3) . . ? C36 C31 N2 117.5(3) . . ? C31 C32 C33 117.2(4) . . ? C31 C32 C37 121.7(3) . . ? C33 C32 C37 121.1(4) . . ? C34 C33 C32 120.9(4) . . ? C35 C34 C33 120.7(4) . . ? C34 C35 C36 121.1(4) . . ? C31 C36 C35 116.6(4) . . ? C31 C36 C40 121.5(3) . . ? C35 C36 C40 121.8(3) . . ? C32 C37 C39 111.2(4) . . ? C32 C37 C38 112.5(4) . . ? C39 C37 C38 111.0(4) . . ? C36 C40 C41 110.2(3) . . ? C36 C40 C42 114.1(3) . . ? C41 C40 C42 109.7(3) . . ? C52 C51 C56 110.5(3) . . ? C52 C51 P 117.5(2) . . ? C56 C51 P 109.7(2) . . ? C53 C52 C51 112.2(3) . . ? C54 C53 C52 111.3(3) . . ? C55 C54 C53 111.0(3) . . ? C54 C55 C56 111.5(3) . . ? C55 C56 C51 112.5(3) . . ? C66 C61 C62 109.5(3) . . ? C66 C61 P 111.1(2) . . ? C62 C61 P 110.3(2) . . ? C63 C62 C61 110.6(3) . . ? C64 C63 C62 111.6(4) . . ? C65 C64 C63 111.3(4) . . ? C64 C65 C66 111.4(3) . . ? C61 C66 C65 111.0(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 C1 Pd P C51 -43.4(4) . . . . ? C1 Pd P C61 81.1(4) . . . . ? C1 Pd P Cl -159.6(3) . . . . ? C3 N2 C1 N1 -0.8(3) . . . . ? C31 N2 C1 N1 175.6(3) . . . . ? C3 N2 C1 Pd 174.0(2) . . . . ? C31 N2 C1 Pd -9.6(5) . . . . ? C2 N1 C1 N2 0.5(3) . . . . ? C11 N1 C1 N2 -179.3(3) . . . . ? C2 N1 C1 Pd -174.8(2) . . . . ? C11 N1 C1 Pd 5.3(4) . . . . ? P Pd C1 N2 -133.4(3) . . . . ? P Pd C1 N1 40.4(5) . . . . ? C1 N1 C2 C3 -0.1(4) . . . . ? C11 N1 C2 C3 179.7(3) . . . . ? N1 C2 C3 N2 -0.4(4) . . . . ? C1 N2 C3 C2 0.8(4) . . . . ? C31 N2 C3 C2 -175.6(3) . . . . ? C1 N1 C11 C12 -96.4(4) . . . . ? C2 N1 C11 C12 83.9(4) . . . . ? C1 N1 C11 C16 85.4(4) . . . . ? C2 N1 C11 C16 -94.3(4) . . . . ? C16 C11 C12 C13 1.1(5) . . . . ? N1 C11 C12 C13 -177.0(3) . . . . ? C16 C11 C12 C17 -177.3(3) . . . . ? N1 C11 C12 C17 4.6(5) . . . . ? C11 C12 C13 C14 -1.7(5) . . . . ? C17 C12 C13 C14 176.6(3) . . . . ? C12 C13 C14 C15 1.1(5) . . . . ? C13 C14 C15 C16 0.4(5) . . . . ? C12 C11 C16 C15 0.3(5) . . . . ? N1 C11 C16 C15 178.4(3) . . . . ? C12 C11 C16 C20 -178.8(3) . . . . ? N1 C11 C16 C20 -0.7(5) . . . . ? C14 C15 C16 C11 -1.0(5) . . . . ? C14 C15 C16 C20 178.1(3) . . . . ? C11 C12 C17 C19 -116.4(4) . . . . ? C13 C12 C17 C19 65.3(5) . . . . ? C11 C12 C17 C18 120.0(4) . . . . ? C13 C12 C17 C18 -58.2(5) . . . . ? C11 C16 C20 C22 112.6(4) . . . . ? C15 C16 C20 C22 -66.4(5) . . . . ? C11 C16 C20 C21 -123.4(4) . . . . ? C15 C16 C20 C21 57.6(5) . . . . ? C1 N2 C31 C32 89.9(4) . . . . ? C3 N2 C31 C32 -94.1(4) . . . . ? C1 N2 C31 C36 -91.0(4) . . . . ? C3 N2 C31 C36 85.0(4) . . . . ? C36 C31 C32 C33 -1.7(5) . . . . ? N2 C31 C32 C33 177.3(3) . . . . ? C36 C31 C32 C37 179.0(4) . . . . ? N2 C31 C32 C37 -1.9(5) . . . . ? C31 C32 C33 C34 1.0(6) . . . . ? C37 C32 C33 C34 -179.7(4) . . . . ? C32 C33 C34 C35 0.0(6) . . . . ? C33 C34 C35 C36 -0.4(6) . . . . ? C32 C31 C36 C35 1.4(5) . . . . ? N2 C31 C36 C35 -177.7(3) . . . . ? C32 C31 C36 C40 -174.8(3) . . . . ? N2 C31 C36 C40 6.2(5) . . . . ? C34 C35 C36 C31 -0.3(6) . . . . ? C34 C35 C36 C40 175.9(4) . . . . ? C31 C32 C37 C39 96.2(4) . . . . ? C33 C32 C37 C39 -83.1(5) . . . . ? C31 C32 C37 C38 -138.6(4) . . . . ? C33 C32 C37 C38 42.2(5) . . . . ? C31 C36 C40 C41 92.3(4) . . . . ? C35 C36 C40 C41 -83.6(4) . . . . ? C31 C36 C40 C42 -143.7(4) . . . . ? C35 C36 C40 C42 40.3(5) . . . . ? C61 P C51 C52 43.1(3) . . . . ? Cl P C51 C52 -57.0(3) . . . . ? Pd P C51 C52 175.6(2) . . . . ? C61 P C51 C56 170.4(2) . . . . ? Cl P C51 C56 70.3(2) . . . . ? Pd P C51 C56 -57.1(3) . . . . ? C56 C51 C52 C53 53.1(4) . . . . ? P C51 C52 C53 -180.0(3) . . . . ? C51 C52 C53 C54 -55.9(4) . . . . ? C52 C53 C54 C55 56.7(4) . . . . ? C53 C54 C55 C56 -55.8(5) . . . . ? C54 C55 C56 C51 54.3(4) . . . . ? C52 C51 C56 C55 -52.3(4) . . . . ? P C51 C56 C55 176.6(3) . . . . ? C51 P C61 C66 -173.5(3) . . . . ? Cl P C61 C66 -72.4(3) . . . . ? Pd P C61 C66 57.2(3) . . . . ? C51 P C61 C62 64.9(3) . . . . ? Cl P C61 C62 166.0(3) . . . . ? Pd P C61 C62 -64.4(3) . . . . ? C66 C61 C62 C63 57.0(4) . . . . ? P C61 C62 C63 179.6(3) . . . . ? C61 C62 C63 C64 -56.1(5) . . . . ? C62 C63 C64 C65 54.9(5) . . . . ? C63 C64 C65 C66 -55.0(5) . . . . ? C62 C61 C66 C65 -57.5(4) . . . . ? P C61 C66 C65 -179.5(3) . . . . ? C64 C65 C66 C61 56.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.51 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.009 _refine_diff_density_min -0.704 _refine_diff_density_rms 0.077 #===END