# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Stephan, Douglas W.' _publ_contact_author_address ; ; _publ_contact_author_email dstephan@chem.utoronto.ca loop_ _publ_author_name M.Sgro D.W.Stephan # Attachment '- Cif Files-revised.txt' data_C44H37ClN2P2Pd_Compound(2) _database_code_depnum_ccdc_archive 'CCDC 801879' #TrackingRef '- Cif Files-revised.txt' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C44 H37 Cl N2 P2 Pd' _chemical_formula_weight 797.55 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 14.2900(6) _cell_length_b 18.7692(8) _cell_length_c 14.7213(6) _cell_angle_alpha 90.00 _cell_angle_beta 113.361(2) _cell_angle_gamma 90.00 _cell_volume 3624.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9930 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 27.52 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method ? _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 0.709 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6223 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27217 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6375 _reflns_number_gt 5473 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+2.1429P] 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 6375 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0304 _refine_ls_R_factor_gt 0.0232 _refine_ls_wR_factor_ref 0.0587 _refine_ls_wR_factor_gt 0.0554 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.006 _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 Pd1 Pd 0.751825(11) 1.004411(7) 0.507447(10) 0.01422(5) Uani 1 1 d . . . Cl1 Cl 0.72370(4) 0.88562(3) 0.43596(3) 0.02017(11) Uani 1 1 d . . . P1 P 0.67150(4) 1.02914(3) 0.27143(4) 0.01772(12) Uani 1 1 d . . . P2 P 0.80986(4) 0.89845(3) 0.69744(4) 0.01691(12) Uani 1 1 d . . . N1 N 0.70977(13) 1.06381(9) 0.37886(12) 0.0194(4) Uani 1 1 d . . . N2 N 0.80099(13) 0.97787(9) 0.65595(12) 0.0174(4) Uani 1 1 d . . . C1 C 0.77674(15) 1.09839(10) 0.56365(14) 0.0161(4) Uani 1 1 d . . . C2 C 0.75158(15) 1.15750(11) 0.50116(14) 0.0183(4) Uani 1 1 d . . . C4 C 0.77118(16) 1.22569(11) 0.54338(16) 0.0248(5) Uani 1 1 d . . . H4 H 0.7553 1.2659 0.5031 0.030 Uiso 1 1 calc R . . C6 C 0.81439(17) 1.23300(12) 0.64566(17) 0.0278(5) Uani 1 1 d . . . H6 H 0.8271 1.2783 0.6734 0.033 Uiso 1 1 calc R . . C5 C 0.83883(16) 1.17369(11) 0.70705(15) 0.0234(5) Uani 1 1 d . . . H5 H 0.8673 1.1795 0.7754 0.028 Uiso 1 1 calc R . . C3 C 0.82067(15) 1.10573(10) 0.66636(14) 0.0166(4) Uani 1 1 d . . . C7 C 0.70287(16) 1.14201(11) 0.39274(15) 0.0193(4) Uani 1 1 d . . . H7A H 0.6321 1.1569 0.3662 0.023 Uiso 1 1 calc R . . H7B H 0.7378 1.1678 0.3582 0.023 Uiso 1 1 calc R . . C8 C 0.84802(16) 1.03790(10) 0.72431(14) 0.0184(4) Uani 1 1 d . . . H8A H 0.9215 1.0323 0.7542 0.022 Uiso 1 1 calc R . . H8B H 0.8230 1.0388 0.7767 0.022 Uiso 1 1 calc R . . C9 C 0.76547(16) 0.96583(11) 0.26824(15) 0.0205(5) Uani 1 1 d . . . C10 C 0.86638(17) 0.97785(12) 0.33190(17) 0.0270(5) Uani 1 1 d . . . H10 H 0.8838 1.0193 0.3695 0.032 Uiso 1 1 calc R . . C12 C 0.94099(19) 0.92829(13) 0.33948(19) 0.0353(6) Uani 1 1 d . . . H12 H 1.0084 0.9367 0.3817 0.042 Uiso 1 1 calc R . . C14 C 0.9151(2) 0.86640(14) 0.2842(2) 0.0387(6) Uani 1 1 d . . . H14 H 0.9648 0.8326 0.2902 0.046 Uiso 1 1 calc R . . C13 C 0.8155(2) 0.85491(13) 0.22014(19) 0.0359(6) Uani 1 1 d . . . H13 H 0.7984 0.8135 0.1823 0.043 Uiso 1 1 calc R . . C11 C 0.74046(18) 0.90424(12) 0.21141(17) 0.0271(5) Uani 1 1 d . . . H11 H 0.6735 0.8962 0.1676 0.032 Uiso 1 1 calc R . . C15 C 0.54909(16) 0.98432(11) 0.23002(15) 0.0200(4) Uani 1 1 d . . . C16 C 0.50682(16) 0.96789(11) 0.29772(16) 0.0220(5) Uani 1 1 d . . . H16 H 0.5405 0.9806 0.3639 0.026 Uiso 1 1 calc R . . C18 C 0.41355(17) 0.93222(12) 0.26615(18) 0.0295(5) Uani 1 1 d . . . H18 H 0.3849 0.9214 0.3113 0.035 Uiso 1 1 calc R . . C20 C 0.36390(18) 0.91313(12) 0.16846(19) 0.0342(6) Uani 1 1 d . . . H20 H 0.3021 0.8890 0.1479 0.041 Uiso 1 1 calc R . . C19 C 0.40530(18) 0.92950(13) 0.10076(18) 0.0353(6) Uani 1 1 d . . . H19 H 0.3713 0.9166 0.0348 0.042 Uiso 1 1 calc R . . C17 C 0.49721(17) 0.96511(12) 0.13108(16) 0.0278(5) Uani 1 1 d . . . H17 H 0.5247 0.9764 0.0852 0.033 Uiso 1 1 calc R . . C21 C 0.65674(17) 1.09864(11) 0.18170(14) 0.0225(5) Uani 1 1 d . . . C22 C 0.56563(19) 1.13702(12) 0.14124(16) 0.0298(5) Uani 1 1 d . . . H22 H 0.5088 1.1217 0.1516 0.036 Uiso 1 1 calc R . . C24 C 0.5597(2) 1.19782(13) 0.08563(17) 0.0367(6) Uani 1 1 d . . . H24 H 0.4986 1.2228 0.0582 0.044 Uiso 1 1 calc R . . C26 C 0.6438(2) 1.22132(13) 0.07085(17) 0.0379(6) Uani 1 1 d . . . H26 H 0.6397 1.2625 0.0344 0.045 Uiso 1 1 calc R . . C25 C 0.7340(2) 1.18386(13) 0.11001(16) 0.0347(6) Uani 1 1 d . . . H25 H 0.7905 1.1997 0.0994 0.042 Uiso 1 1 calc R . . C23 C 0.74111(18) 1.12247(12) 0.16537(15) 0.0270(5) Uani 1 1 d . . . H23 H 0.8022 1.0974 0.1915 0.032 Uiso 1 1 calc R . . C27 C 0.69111(16) 0.85284(11) 0.63132(14) 0.0207(5) Uani 1 1 d . . . C31 C 0.59348(19) 0.75158(14) 0.54571(17) 0.0348(6) Uani 1 1 d . . . H31 H 0.5905 0.7041 0.5268 0.042 Uiso 1 1 calc R . . C32 C 0.50543(19) 0.79136(15) 0.51566(17) 0.0380(6) Uani 1 1 d . . . H32 H 0.4433 0.7706 0.4769 0.046 Uiso 1 1 calc R . . C30 C 0.50915(18) 0.86224(14) 0.54302(18) 0.0353(6) Uani 1 1 d . . . H30 H 0.4496 0.8890 0.5230 0.042 Uiso 1 1 calc R . . C28 C 0.60199(17) 0.89307(13) 0.60038(16) 0.0269(5) Uani 1 1 d . . . H28 H 0.6048 0.9408 0.6183 0.032 Uiso 1 1 calc R . . C39 C 0.91234(16) 0.84494(11) 0.69009(15) 0.0211(5) Uani 1 1 d . . . C41 C 0.95861(16) 0.86772(12) 0.62809(16) 0.0240(5) Uani 1 1 d . . . H41 H 0.9374 0.9097 0.5922 0.029 Uiso 1 1 calc R . . C43 C 1.03660(17) 0.82760(13) 0.61983(18) 0.0324(6) Uani 1 1 d . . . H43 H 1.0674 0.8427 0.5781 0.039 Uiso 1 1 calc R . . C44 C 1.06834(18) 0.76560(13) 0.6732(2) 0.0377(6) Uani 1 1 d . . . H44 H 1.1206 0.7390 0.6673 0.045 Uiso 1 1 calc R . . C42 C 1.02349(18) 0.74244(12) 0.73545(19) 0.0365(6) Uani 1 1 d . . . H42 H 1.0456 0.7006 0.7716 0.044 Uiso 1 1 calc R . . C40 C 0.94513(17) 0.78186(12) 0.74382(17) 0.0293(5) Uani 1 1 d . . . H40 H 0.9144 0.7663 0.7853 0.035 Uiso 1 1 calc R . . C33 C 0.83397(17) 0.90286(11) 0.82808(15) 0.0218(5) Uani 1 1 d . . . C34 C 0.75355(18) 0.91398(11) 0.85702(16) 0.0260(5) Uani 1 1 d . . . H34 H 0.6868 0.9134 0.8100 0.031 Uiso 1 1 calc R . . C36 C 0.7726(2) 0.92586(12) 0.95572(17) 0.0341(6) Uani 1 1 d . . . H36 H 0.7186 0.9327 0.9748 0.041 Uiso 1 1 calc R . . C38 C 0.8714(2) 0.92753(13) 1.02569(17) 0.0384(6) Uani 1 1 d . . . H38 H 0.8839 0.9358 1.0918 0.046 Uiso 1 1 calc R . . C37 C 0.9517(2) 0.91699(12) 0.99758(17) 0.0359(6) Uani 1 1 d . . . H37 H 1.0182 0.9182 1.0449 0.043 Uiso 1 1 calc R . . C35 C 0.93391(18) 0.90460(12) 0.89945(16) 0.0282(5) Uani 1 1 d . . . H35 H 0.9884 0.8974 0.8810 0.034 Uiso 1 1 calc R . . C29 C 0.68677(18) 0.78182(11) 0.60402(15) 0.0256(5) Uani 1 1 d . . . H29 H 0.7460 0.7546 0.6246 0.031 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 Pd1 0.01658(9) 0.01145(9) 0.01333(8) -0.00040(6) 0.00456(6) -0.00056(6) Cl1 0.0293(3) 0.0139(3) 0.0186(2) -0.00145(18) 0.0109(2) -0.0021(2) P1 0.0199(3) 0.0170(3) 0.0152(3) 0.0013(2) 0.0058(2) -0.0009(2) P2 0.0186(3) 0.0152(3) 0.0152(2) 0.0008(2) 0.0048(2) 0.0001(2) N1 0.0249(10) 0.0137(9) 0.0172(8) 0.0006(7) 0.0058(8) -0.0015(7) N2 0.0211(10) 0.0138(9) 0.0155(8) 0.0002(6) 0.0054(7) 0.0003(7) C1 0.0132(10) 0.0140(11) 0.0213(10) -0.0022(8) 0.0069(9) -0.0013(8) C2 0.0169(11) 0.0156(11) 0.0240(11) -0.0005(8) 0.0098(9) 0.0002(8) C4 0.0287(13) 0.0133(11) 0.0312(12) 0.0022(9) 0.0105(10) 0.0012(9) C6 0.0321(13) 0.0155(12) 0.0336(12) -0.0074(9) 0.0106(11) -0.0014(9) C5 0.0255(12) 0.0219(12) 0.0207(11) -0.0053(9) 0.0072(10) 0.0007(9) C3 0.0145(11) 0.0160(11) 0.0197(10) -0.0023(8) 0.0073(9) -0.0003(8) C7 0.0200(11) 0.0152(11) 0.0230(11) 0.0022(8) 0.0090(9) 0.0005(8) C8 0.0199(11) 0.0188(11) 0.0147(10) -0.0023(8) 0.0049(9) -0.0014(9) C9 0.0255(12) 0.0198(12) 0.0200(10) 0.0048(8) 0.0130(10) 0.0002(9) C10 0.0262(13) 0.0256(13) 0.0318(12) 0.0038(9) 0.0142(11) 0.0000(10) C12 0.0244(13) 0.0426(16) 0.0429(15) 0.0103(12) 0.0177(12) 0.0037(11) C14 0.0390(16) 0.0338(15) 0.0600(17) 0.0137(12) 0.0373(15) 0.0117(12) C13 0.0499(17) 0.0222(13) 0.0517(16) -0.0038(11) 0.0374(14) -0.0010(11) C11 0.0310(13) 0.0262(13) 0.0295(12) -0.0021(9) 0.0178(11) -0.0028(10) C15 0.0190(11) 0.0159(11) 0.0215(10) 0.0005(8) 0.0042(9) 0.0020(8) C16 0.0210(12) 0.0191(11) 0.0235(11) -0.0012(8) 0.0064(9) 0.0029(9) C18 0.0251(13) 0.0242(13) 0.0408(14) 0.0028(10) 0.0148(11) 0.0009(10) C20 0.0192(13) 0.0229(13) 0.0512(16) -0.0062(11) 0.0039(12) -0.0033(10) C19 0.0303(14) 0.0310(14) 0.0303(13) -0.0082(10) -0.0033(11) 0.0006(11) C17 0.0297(13) 0.0270(13) 0.0214(11) -0.0013(9) 0.0044(10) -0.0002(10) C21 0.0322(13) 0.0179(11) 0.0143(10) -0.0002(8) 0.0059(9) -0.0037(9) C22 0.0373(14) 0.0257(13) 0.0270(12) 0.0065(10) 0.0134(11) 0.0034(11) C24 0.0469(16) 0.0262(14) 0.0314(13) 0.0079(10) 0.0097(12) 0.0070(11) C26 0.0572(18) 0.0226(13) 0.0235(12) 0.0046(10) 0.0049(12) -0.0099(12) C25 0.0402(15) 0.0362(15) 0.0216(11) 0.0014(10) 0.0057(11) -0.0212(12) C23 0.0293(13) 0.0286(13) 0.0168(10) 0.0004(9) 0.0026(10) -0.0084(10) C27 0.0239(12) 0.0242(12) 0.0153(10) 0.0005(8) 0.0091(9) -0.0061(9) C31 0.0455(16) 0.0311(14) 0.0288(12) -0.0039(10) 0.0157(12) -0.0185(12) C32 0.0305(15) 0.0571(19) 0.0253(13) -0.0063(11) 0.0100(11) -0.0219(13) C30 0.0213(13) 0.0552(17) 0.0296(12) -0.0001(12) 0.0104(11) -0.0044(11) C28 0.0258(13) 0.0311(13) 0.0263(11) -0.0037(9) 0.0129(10) -0.0042(10) C39 0.0176(11) 0.0163(11) 0.0229(11) -0.0049(8) 0.0009(9) -0.0011(8) C41 0.0185(12) 0.0214(12) 0.0269(11) -0.0057(9) 0.0033(10) -0.0007(9) C43 0.0223(13) 0.0322(14) 0.0413(14) -0.0130(11) 0.0111(11) -0.0024(10) C44 0.0185(13) 0.0280(14) 0.0562(16) -0.0159(12) 0.0038(12) 0.0025(10) C42 0.0266(13) 0.0175(13) 0.0464(15) -0.0029(10) -0.0058(12) 0.0055(10) C40 0.0286(13) 0.0204(12) 0.0309(12) -0.0004(9) 0.0033(10) 0.0007(10) C33 0.0313(13) 0.0133(11) 0.0174(10) 0.0023(8) 0.0061(10) -0.0021(9) C34 0.0351(14) 0.0194(12) 0.0239(11) 0.0019(9) 0.0121(10) -0.0013(10) C36 0.0535(17) 0.0246(13) 0.0313(13) 0.0017(10) 0.0244(13) -0.0009(11) C38 0.0669(19) 0.0268(14) 0.0195(12) 0.0018(10) 0.0150(13) 0.0006(12) C37 0.0457(16) 0.0264(14) 0.0217(12) 0.0019(9) -0.0014(11) 0.0014(11) C35 0.0345(14) 0.0211(12) 0.0234(11) 0.0023(9) 0.0055(10) 0.0024(10) C29 0.0321(13) 0.0228(12) 0.0216(11) 0.0006(9) 0.0103(10) -0.0071(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 1.9207(19) . ? Pd1 N1 2.0701(16) . ? Pd1 N2 2.0744(16) . ? Pd1 Cl1 2.4300(5) . ? P1 N1 1.5931(16) . ? P1 C9 1.808(2) . ? P1 C21 1.808(2) . ? P1 C15 1.815(2) . ? P2 N2 1.5967(17) . ? P2 C27 1.803(2) . ? P2 C39 1.814(2) . ? P2 C33 1.816(2) . ? N1 C7 1.490(3) . ? N2 C8 1.482(3) . ? C1 C2 1.394(3) . ? C1 C3 1.395(3) . ? C2 C4 1.402(3) . ? C2 C7 1.495(3) . ? C4 C6 1.389(3) . ? C6 C5 1.388(3) . ? C5 C3 1.389(3) . ? C3 C8 1.496(3) . ? C9 C11 1.388(3) . ? C9 C10 1.392(3) . ? C10 C12 1.386(3) . ? C12 C14 1.382(4) . ? C14 C13 1.377(4) . ? C13 C11 1.383(3) . ? C15 C16 1.390(3) . ? C15 C17 1.394(3) . ? C16 C18 1.396(3) . ? C18 C20 1.375(3) . ? C20 C19 1.380(4) . ? C19 C17 1.381(3) . ? C21 C23 1.393(3) . ? C21 C22 1.398(3) . ? C22 C24 1.387(3) . ? C24 C26 1.375(4) . ? C26 C25 1.378(4) . ? C25 C23 1.391(3) . ? C27 C29 1.387(3) . ? C27 C28 1.393(3) . ? C31 C32 1.377(4) . ? C31 C29 1.389(3) . ? C32 C30 1.385(4) . ? C30 C28 1.385(3) . ? C39 C41 1.390(3) . ? C39 C40 1.397(3) . ? C41 C43 1.390(3) . ? C43 C44 1.377(4) . ? C44 C42 1.380(4) . ? C42 C40 1.388(3) . ? C33 C34 1.391(3) . ? C33 C35 1.398(3) . ? C34 C36 1.386(3) . ? C36 C38 1.379(4) . ? C38 C37 1.380(4) . ? C37 C35 1.384(3) . ? 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 Pd1 N1 80.58(7) . . ? C1 Pd1 N2 80.74(7) . . ? N1 Pd1 N2 161.31(7) . . ? C1 Pd1 Cl1 178.79(6) . . ? N1 Pd1 Cl1 99.21(5) . . ? N2 Pd1 Cl1 99.48(5) . . ? N1 P1 C9 109.16(9) . . ? N1 P1 C21 108.98(9) . . ? C9 P1 C21 109.14(10) . . ? N1 P1 C15 115.37(9) . . ? C9 P1 C15 108.27(10) . . ? C21 P1 C15 105.74(10) . . ? N2 P2 C27 108.77(9) . . ? N2 P2 C39 115.95(9) . . ? C27 P2 C39 108.31(10) . . ? N2 P2 C33 108.39(9) . . ? C27 P2 C33 109.64(9) . . ? C39 P2 C33 105.65(10) . . ? C7 N1 P1 121.53(13) . . ? C7 N1 Pd1 114.59(12) . . ? P1 N1 Pd1 123.28(9) . . ? C8 N2 P2 120.26(13) . . ? C8 N2 Pd1 113.94(12) . . ? P2 N2 Pd1 124.73(9) . . ? C2 C1 C3 121.60(18) . . ? C2 C1 Pd1 119.42(15) . . ? C3 C1 Pd1 118.98(15) . . ? C1 C2 C4 118.69(18) . . ? C1 C2 C7 116.02(17) . . ? C4 C2 C7 125.28(18) . . ? C6 C4 C2 119.71(19) . . ? C5 C6 C4 121.0(2) . . ? C6 C5 C3 119.99(19) . . ? C5 C3 C1 119.00(18) . . ? C5 C3 C8 125.01(18) . . ? C1 C3 C8 115.95(17) . . ? N1 C7 C2 108.04(16) . . ? N2 C8 C3 108.31(16) . . ? C11 C9 C10 119.4(2) . . ? C11 C9 P1 123.14(17) . . ? C10 C9 P1 117.26(16) . . ? C12 C10 C9 120.3(2) . . ? C14 C12 C10 119.9(2) . . ? C13 C14 C12 119.8(2) . . ? C14 C13 C11 120.7(2) . . ? C13 C11 C9 119.8(2) . . ? C16 C15 C17 119.3(2) . . ? C16 C15 P1 119.81(16) . . ? C17 C15 P1 120.87(16) . . ? C15 C16 C18 119.8(2) . . ? C20 C18 C16 120.1(2) . . ? C18 C20 C19 120.4(2) . . ? C20 C19 C17 120.0(2) . . ? C19 C17 C15 120.4(2) . . ? C23 C21 C22 119.0(2) . . ? C23 C21 P1 119.96(17) . . ? C22 C21 P1 120.15(16) . . ? C24 C22 C21 120.3(2) . . ? C26 C24 C22 120.3(2) . . ? C24 C26 C25 120.1(2) . . ? C26 C25 C23 120.4(2) . . ? C25 C23 C21 120.0(2) . . ? C29 C27 C28 119.8(2) . . ? C29 C27 P2 122.50(17) . . ? C28 C27 P2 117.52(16) . . ? C32 C31 C29 120.5(2) . . ? C31 C32 C30 120.2(2) . . ? C32 C30 C28 119.7(2) . . ? C30 C28 C27 120.2(2) . . ? C41 C39 C40 119.5(2) . . ? C41 C39 P2 118.32(16) . . ? C40 C39 P2 122.19(17) . . ? C43 C41 C39 119.8(2) . . ? C44 C43 C41 120.1(2) . . ? C43 C44 C42 120.7(2) . . ? C44 C42 C40 119.6(2) . . ? C42 C40 C39 120.2(2) . . ? C34 C33 C35 119.2(2) . . ? C34 C33 P2 119.90(16) . . ? C35 C33 P2 120.34(17) . . ? C36 C34 C33 120.2(2) . . ? C38 C36 C34 120.3(2) . . ? C36 C38 C37 120.0(2) . . ? C38 C37 C35 120.5(2) . . ? C37 C35 C33 119.9(2) . . ? C27 C29 C31 119.6(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.405 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.053 #=== END data_C38H33ClN2P2Pd_Compound(3) _database_code_depnum_ccdc_archive 'CCDC 801880' #TrackingRef '- Cif Files-revised.txt' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C38 H33 Cl N2 P2 Pd' _chemical_formula_weight 721.45 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 11.6687(16) _cell_length_b 24.307(4) _cell_length_c 12.5348(17) _cell_angle_alpha 90.00 _cell_angle_beta 116.372(6) _cell_angle_gamma 90.00 _cell_volume 3185.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1992 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 22.63 _exptl_crystal_description Plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 0.798 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3714 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22255 _diffrn_reflns_av_R_equivalents 0.1286 _diffrn_reflns_av_sigmaI/netI 0.1217 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5543 _reflns_number_gt 3511 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0831P)^2^+6.9609P] 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 5543 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1359 _refine_ls_R_factor_gt 0.0835 _refine_ls_wR_factor_ref 0.2107 _refine_ls_wR_factor_gt 0.1846 _refine_ls_goodness_of_fit_ref 1.150 _refine_ls_restrained_S_all 1.150 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.81012(7) 0.16801(3) 0.02226(6) 0.0258(2) Uani 1 1 d . . . Cl1 Cl 0.5827(2) 0.15093(10) -0.05450(19) 0.0315(6) Uani 1 1 d . . . P1 P 0.7364(2) 0.07077(10) -0.1831(2) 0.0269(6) Uani 1 1 d . . . P2 P 0.8103(2) 0.21855(11) 0.16946(19) 0.0264(6) Uani 1 1 d . . . N1 N 0.8290(7) 0.1195(3) -0.1073(6) 0.0264(18) Uani 1 1 d . . . N2 N 0.9536(7) 0.2438(3) 0.2599(6) 0.0293(19) Uani 1 1 d . . . H2A H 0.9598 0.2761 0.2936 0.035 Uiso 1 1 calc R . . C2 C 1.0316(9) 0.1671(4) -0.0186(8) 0.031(2) Uani 1 1 d . . . C19 C 0.9161(9) -0.0609(4) -0.2492(8) 0.034(2) Uani 1 1 d . . . H19A H 0.9475 -0.0960 -0.2154 0.040 Uiso 1 1 calc R . . C21 C 0.5944(8) 0.0921(4) -0.3155(7) 0.026(2) Uani 1 1 d . . . C15 C 0.8146(8) 0.0251(4) -0.2468(7) 0.023(2) Uani 1 1 d . . . C33 C 0.7479(9) 0.1768(4) 0.2546(7) 0.031(2) Uani 1 1 d . . . C1 C 0.9966(9) 0.1818(4) 0.0690(8) 0.026(2) Uani 1 1 d . . . C7 C 0.9318(9) 0.1408(4) -0.1330(8) 0.030(2) Uani 1 1 d . . . H7A H 0.8974 0.1685 -0.1976 0.036 Uiso 1 1 calc R . . H7B H 0.9708 0.1106 -0.1585 0.036 Uiso 1 1 calc R . . C9 C 0.6954(9) 0.0273(4) -0.0895(8) 0.027(2) Uani 1 1 d . . . C23 C 0.5129(9) 0.0543(4) -0.3955(8) 0.031(2) Uani 1 1 d . . . H23A H 0.5268 0.0160 -0.3799 0.037 Uiso 1 1 calc R . . C28 C 0.7604(11) 0.3317(4) 0.1629(8) 0.039(3) Uani 1 1 d . . . H28A H 0.8505 0.3365 0.1960 0.047 Uiso 1 1 calc R . . C18 C 0.8830(9) 0.0063(4) -0.3997(8) 0.033(2) Uani 1 1 d . . . H18A H 0.8902 0.0177 -0.4690 0.039 Uiso 1 1 calc R . . C22 C 0.5777(9) 0.1481(4) -0.3387(7) 0.029(2) Uani 1 1 d . . . H22A H 0.6349 0.1736 -0.2831 0.035 Uiso 1 1 calc R . . C27 C 0.7099(9) 0.2792(4) 0.1366(8) 0.029(2) Uani 1 1 d . . . C3 C 1.0928(9) 0.2021(4) 0.1788(8) 0.028(2) Uani 1 1 d . . . C13 C 0.7760(9) -0.0208(4) 0.1001(8) 0.037(3) Uani 1 1 d . . . H13A H 0.8403 -0.0255 0.1795 0.044 Uiso 1 1 calc R . . C36 C 0.6452(13) 0.1692(7) 0.3831(10) 0.069(4) Uani 1 1 d . . . H36A H 0.6072 0.1864 0.4277 0.083 Uiso 1 1 calc R . . C16 C 0.8265(9) 0.0412(4) -0.3462(8) 0.032(2) Uani 1 1 d . . . H16A H 0.7963 0.0764 -0.3797 0.038 Uiso 1 1 calc R . . C11 C 0.7924(9) 0.0183(4) 0.0271(8) 0.036(3) Uani 1 1 d . . . H11A H 0.8692 0.0391 0.0558 0.043 Uiso 1 1 calc R . . C24 C 0.4766(9) 0.1672(4) -0.4441(8) 0.030(2) Uani 1 1 d . . . H24A H 0.4648 0.2054 -0.4616 0.036 Uiso 1 1 calc R . . C17 C 0.8597(9) -0.0268(4) -0.1985(8) 0.030(2) Uani 1 1 d . . . H17A H 0.8513 -0.0387 -0.1300 0.035 Uiso 1 1 calc R . . C35 C 0.7537(10) 0.1202(5) 0.2525(8) 0.043(3) Uani 1 1 d . . . H35A H 0.7905 0.1030 0.2071 0.051 Uiso 1 1 calc R . . C25 C 0.4094(8) 0.0727(4) -0.5001(8) 0.031(2) Uani 1 1 d . . . H25A H 0.3512 0.0471 -0.5545 0.037 Uiso 1 1 calc R . . C6 C 1.2494(10) 0.1962(4) 0.1018(10) 0.042(3) Uani 1 1 d . . . H6A H 1.3340 0.2022 0.1116 0.050 Uiso 1 1 calc R . . C4 C 1.1555(10) 0.1738(4) -0.0042(9) 0.040(3) Uani 1 1 d . . . H4A H 1.1769 0.1632 -0.0660 0.048 Uiso 1 1 calc R . . C14 C 0.6680(11) -0.0526(4) 0.0584(8) 0.045(3) Uani 1 1 d . . . H14A H 0.6600 -0.0812 0.1064 0.053 Uiso 1 1 calc R . . C5 C 1.2162(9) 0.2092(4) 0.1901(9) 0.035(2) Uani 1 1 d . . . H5A H 1.2800 0.2237 0.2626 0.043 Uiso 1 1 calc R . . C8 C 1.0685(9) 0.2126(4) 0.2833(8) 0.030(2) Uani 1 1 d . . . H8A H 1.0632 0.1767 0.3182 0.035 Uiso 1 1 calc R . . H8B H 1.1429 0.2326 0.3438 0.035 Uiso 1 1 calc R . . C34 C 0.6932(10) 0.2010(6) 0.3211(9) 0.050(3) Uani 1 1 d . . . H34A H 0.6887 0.2399 0.3240 0.061 Uiso 1 1 calc R . . C29 C 0.5767(10) 0.2732(5) 0.0842(8) 0.046(3) Uani 1 1 d . . . H29A H 0.5387 0.2379 0.0612 0.055 Uiso 1 1 calc R . . C32 C 0.5531(14) 0.3710(6) 0.0947(11) 0.063(4) Uani 1 1 d . . . H32A H 0.4987 0.4020 0.0813 0.076 Uiso 1 1 calc R . . C26 C 0.3934(9) 0.1282(4) -0.5228(8) 0.032(2) Uani 1 1 d . . . H26A H 0.3239 0.1405 -0.5941 0.038 Uiso 1 1 calc R . . C38 C 0.6521(12) 0.1134(8) 0.3807(9) 0.073(5) Uani 1 1 d . . . H38A H 0.6193 0.0917 0.4239 0.088 Uiso 1 1 calc R . . C37 C 0.7066(11) 0.0879(5) 0.3157(9) 0.054(4) Uani 1 1 d . . . H37A H 0.7118 0.0489 0.3143 0.065 Uiso 1 1 calc R . . C30 C 0.6824(14) 0.3779(5) 0.1421(9) 0.053(3) Uani 1 1 d . . . H30A H 0.7188 0.4137 0.1606 0.063 Uiso 1 1 calc R . . C20 C 0.9268(9) -0.0438(4) -0.3499(9) 0.037(3) Uani 1 1 d . . . H20A H 0.9655 -0.0675 -0.3849 0.045 Uiso 1 1 calc R . . C31 C 0.5019(12) 0.3190(6) 0.0665(10) 0.062(4) Uani 1 1 d . . . H31A H 0.4118 0.3147 0.0337 0.074 Uiso 1 1 calc R . . C12 C 0.5692(10) -0.0427(5) -0.0555(8) 0.047(3) Uani 1 1 d . . . H12A H 0.4916 -0.0629 -0.0828 0.057 Uiso 1 1 calc R . . C10 C 0.5844(10) -0.0036(4) -0.1281(8) 0.042(3) Uani 1 1 d . . . H10A H 0.5177 0.0021 -0.2059 0.050 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 Pd1 0.0146(4) 0.0357(4) 0.0168(3) -0.0005(3) -0.0024(3) -0.0007(3) Cl1 0.0181(13) 0.0385(14) 0.0225(11) 0.0015(9) -0.0048(10) -0.0021(10) P1 0.0184(14) 0.0337(14) 0.0171(11) -0.0010(10) -0.0024(10) -0.0005(11) P2 0.0143(13) 0.0436(16) 0.0132(11) 0.0002(10) -0.0012(10) -0.0008(11) N1 0.017(4) 0.034(5) 0.020(4) 0.004(3) 0.001(3) -0.004(3) N2 0.014(4) 0.041(5) 0.021(4) -0.011(3) -0.003(3) 0.001(4) C2 0.019(5) 0.029(5) 0.035(5) -0.003(4) 0.003(4) -0.007(4) C19 0.028(6) 0.042(6) 0.021(5) -0.001(4) 0.002(4) 0.007(5) C21 0.009(5) 0.040(6) 0.021(5) -0.006(4) -0.002(4) -0.001(4) C15 0.002(5) 0.040(6) 0.020(4) 0.000(4) -0.001(4) 0.001(4) C33 0.013(5) 0.062(8) 0.008(4) -0.004(4) -0.006(4) 0.000(5) C1 0.017(5) 0.034(6) 0.022(5) 0.001(4) 0.003(4) 0.004(4) C7 0.023(6) 0.041(6) 0.024(5) -0.002(4) 0.008(4) -0.008(5) C9 0.016(5) 0.036(6) 0.021(5) -0.003(4) 0.000(4) -0.002(4) C23 0.023(6) 0.036(6) 0.023(5) -0.001(4) 0.001(4) -0.001(4) C28 0.042(7) 0.051(7) 0.024(5) 0.003(5) 0.015(5) 0.014(6) C18 0.025(6) 0.045(6) 0.023(5) -0.006(4) 0.007(4) -0.008(5) C22 0.023(6) 0.041(6) 0.009(4) -0.002(4) -0.008(4) -0.001(4) C27 0.017(5) 0.049(7) 0.022(5) 0.001(4) 0.010(4) 0.014(5) C3 0.014(5) 0.037(6) 0.024(5) 0.006(4) 0.001(4) -0.002(4) C13 0.011(5) 0.060(7) 0.026(5) 0.007(5) -0.005(4) -0.003(5) C36 0.052(9) 0.121(13) 0.033(7) 0.015(8) 0.018(6) -0.015(9) C16 0.020(6) 0.043(6) 0.027(5) 0.001(4) 0.005(4) -0.001(4) C11 0.019(6) 0.056(7) 0.023(5) -0.004(5) 0.000(4) -0.005(5) C24 0.024(6) 0.039(6) 0.027(5) 0.001(4) 0.011(4) 0.006(5) C17 0.015(5) 0.044(6) 0.022(5) -0.004(4) 0.001(4) -0.008(4) C35 0.024(6) 0.068(8) 0.016(5) 0.009(5) -0.010(4) 0.000(5) C25 0.011(5) 0.050(7) 0.021(5) -0.005(4) -0.003(4) -0.005(4) C6 0.014(6) 0.049(7) 0.054(7) -0.005(5) 0.007(5) -0.003(5) C4 0.031(6) 0.049(7) 0.038(6) -0.006(5) 0.014(5) -0.011(5) C14 0.047(8) 0.049(7) 0.024(5) 0.008(5) 0.004(5) 0.005(6) C5 0.017(6) 0.038(6) 0.034(5) -0.003(4) -0.004(4) -0.006(4) C8 0.011(5) 0.037(6) 0.027(5) -0.005(4) -0.003(4) 0.001(4) C34 0.029(7) 0.085(9) 0.026(6) 0.006(5) 0.001(5) 0.001(6) C29 0.017(6) 0.083(9) 0.024(5) -0.013(5) -0.003(4) 0.017(6) C32 0.053(10) 0.091(11) 0.045(7) 0.016(7) 0.022(7) 0.039(8) C26 0.014(5) 0.049(7) 0.020(5) 0.000(4) -0.004(4) 0.004(4) C38 0.038(8) 0.148(15) 0.016(6) 0.028(7) -0.005(5) -0.030(9) C37 0.041(8) 0.077(9) 0.021(5) 0.020(5) -0.008(5) -0.019(6) C30 0.083(11) 0.048(7) 0.034(6) 0.009(5) 0.032(7) 0.026(7) C20 0.014(6) 0.046(7) 0.041(6) -0.015(5) 0.003(5) -0.003(5) C31 0.026(7) 0.108(12) 0.039(7) -0.007(7) 0.002(5) 0.027(7) C12 0.031(7) 0.080(8) 0.016(5) 0.003(5) -0.003(5) -0.019(6) C10 0.031(7) 0.059(7) 0.021(5) 0.005(5) -0.001(5) -0.012(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 2.015(9) . ? Pd1 N1 2.096(7) . ? Pd1 P2 2.216(3) . ? Pd1 Cl1 2.423(2) . ? P1 N1 1.601(7) . ? P1 C9 1.794(10) . ? P1 C21 1.823(9) . ? P1 C15 1.831(9) . ? P2 N2 1.666(7) . ? P2 C27 1.812(9) . ? P2 C33 1.840(10) . ? N1 C7 1.467(12) . ? N2 C8 1.452(11) . ? C2 C4 1.384(14) . ? C2 C1 1.378(13) . ? C2 C7 1.528(12) . ? C19 C17 1.377(13) . ? C19 C20 1.387(14) . ? C21 C23 1.381(12) . ? C21 C22 1.387(12) . ? C15 C16 1.371(12) . ? C15 C17 1.398(13) . ? C33 C35 1.377(14) . ? C33 C34 1.387(15) . ? C1 C3 1.423(12) . ? C9 C10 1.386(13) . ? C9 C11 1.412(12) . ? C23 C25 1.403(12) . ? C28 C27 1.384(14) . ? C28 C30 1.395(14) . ? C18 C20 1.361(14) . ? C18 C16 1.411(13) . ? C22 C24 1.404(12) . ? C27 C29 1.400(13) . ? C3 C5 1.394(13) . ? C3 C8 1.480(13) . ? C13 C14 1.369(14) . ? C13 C11 1.391(13) . ? C36 C38 1.361(19) . ? C36 C34 1.378(17) . ? C24 C26 1.401(13) . ? C35 C37 1.390(15) . ? C25 C26 1.375(13) . ? C6 C5 1.363(14) . ? C6 C4 1.403(14) . ? C14 C12 1.401(13) . ? C29 C31 1.370(16) . ? C32 C30 1.364(18) . ? C32 C31 1.376(18) . ? C38 C37 1.382(19) . ? C12 C10 1.381(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 N1 81.2(3) . . ? C1 Pd1 P2 93.7(3) . . ? N1 Pd1 P2 174.5(2) . . ? C1 Pd1 Cl1 174.2(3) . . ? N1 Pd1 Cl1 94.0(2) . . ? P2 Pd1 Cl1 91.22(9) . . ? N1 P1 C9 110.7(4) . . ? N1 P1 C21 115.5(4) . . ? C9 P1 C21 111.4(4) . . ? N1 P1 C15 111.8(4) . . ? C9 P1 C15 104.9(4) . . ? C21 P1 C15 101.7(4) . . ? N2 P2 C27 102.0(4) . . ? N2 P2 C33 110.1(4) . . ? C27 P2 C33 101.4(5) . . ? N2 P2 Pd1 113.6(3) . . ? C27 P2 Pd1 120.0(3) . . ? C33 P2 Pd1 108.8(3) . . ? C7 N1 P1 122.3(6) . . ? C7 N1 Pd1 110.4(5) . . ? P1 N1 Pd1 126.9(4) . . ? C8 N2 P2 120.2(6) . . ? C4 C2 C1 121.8(9) . . ? C4 C2 C7 119.2(9) . . ? C1 C2 C7 119.0(8) . . ? C17 C19 C20 119.7(9) . . ? C23 C21 C22 120.8(8) . . ? C23 C21 P1 121.7(7) . . ? C22 C21 P1 117.1(6) . . ? C16 C15 C17 118.8(9) . . ? C16 C15 P1 119.7(7) . . ? C17 C15 P1 121.5(7) . . ? C35 C33 C34 118.3(10) . . ? C35 C33 P2 120.3(8) . . ? C34 C33 P2 121.4(9) . . ? C2 C1 C3 118.4(9) . . ? C2 C1 Pd1 112.9(6) . . ? C3 C1 Pd1 128.7(7) . . ? N1 C7 C2 107.4(7) . . ? C10 C9 C11 118.1(9) . . ? C10 C9 P1 124.8(7) . . ? C11 C9 P1 116.4(7) . . ? C21 C23 C25 119.8(9) . . ? C27 C28 C30 121.6(11) . . ? C20 C18 C16 118.7(9) . . ? C21 C22 C24 120.2(8) . . ? C28 C27 C29 118.3(9) . . ? C28 C27 P2 122.2(8) . . ? C29 C27 P2 119.5(8) . . ? C5 C3 C1 118.5(9) . . ? C5 C3 C8 118.9(8) . . ? C1 C3 C8 122.5(8) . . ? C14 C13 C11 120.4(9) . . ? C38 C36 C34 120.2(14) . . ? C15 C16 C18 121.1(9) . . ? C13 C11 C9 120.4(9) . . ? C26 C24 C22 117.9(9) . . ? C19 C17 C15 120.5(9) . . ? C33 C35 C37 121.2(11) . . ? C26 C25 C23 119.2(8) . . ? C5 C6 C4 118.3(10) . . ? C2 C4 C6 120.1(10) . . ? C13 C14 C12 119.6(10) . . ? C6 C5 C3 122.8(9) . . ? N2 C8 C3 115.7(7) . . ? C36 C34 C33 120.9(13) . . ? C31 C29 C27 119.1(12) . . ? C30 C32 C31 119.6(12) . . ? C25 C26 C24 122.1(8) . . ? C36 C38 C37 120.5(12) . . ? C38 C37 C35 119.0(13) . . ? C32 C30 C28 119.1(12) . . ? C18 C20 C19 121.2(10) . . ? C29 C31 C32 122.2(12) . . ? C10 C12 C14 120.1(10) . . ? C12 C10 C9 121.2(9) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.065 _refine_diff_density_min -1.836 _refine_diff_density_rms 0.148