# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_publication_text _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Richard A. Kemp' _publ_contact_author_address ;Department of Chemistry and Chemical Biology MSC03 2060 University of New Mexico Albuquerque, NM 87131 ; _publ_contact_author_email rakemp@unm.edu _publ_contact_author_phone 505-272-7609 _publ_contact_author_fax 505-272-7336 loop_ _publ_author_name _publ_author_address R.A.Kemp ;Department of Chemistry and Chemical Biology MSC03 2060 University of New Mexico Albuquerque, NM 87131 ; R.Lansing ;Department of Chemistry and Chemical Biology MSC03 2060 University of New Mexico Albuquerque, NM 87131 ; R.Lansing '' K.I.Goldberg ;Department of Chemistry University of Washington Seattle, WA 98195 ; data_rkrl3 _database_code_depnum_ccdc_archive 'CCDC 812749' #TrackingRef 'Compound 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H37 N P2' _chemical_formula_weight 497.57 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 15.4380(11) _cell_length_b 22.8418(16) _cell_length_c 8.1278(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2866.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 228(2) _cell_measurement_reflns_used 9933 _cell_measurement_theta_min 2.66 _cell_measurement_theta_max 24.22 _exptl_crystal_description cut _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.153 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 0.172 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9267 _exptl_absorpt_correction_T_max 0.9729 _exptl_absorpt_process_details 'bruker, sadabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 228(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 '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 36855 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 26.02 _reflns_number_total 5539 _reflns_number_gt 4550 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics '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^)+(0.0684P)^2^+0.2962P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(9) _refine_ls_number_reflns 5539 _refine_ls_number_parameters 316 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.1208 _refine_ls_wR_factor_gt 0.0980 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_restrained_S_all 1.121 _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 N1 N 0.84725(14) 0.43961(10) 0.2125(4) 0.0531(7) Uani 1 1 d . . . H1A H 0.8215 0.4059 0.2204 0.064 Uiso 1 1 calc R . . P1 P 0.90234(4) 0.36524(3) -0.06576(9) 0.03703(17) Uani 1 1 d . . . P2 P 0.66427(4) 0.40671(3) 0.27972(9) 0.03801(18) Uani 1 1 d . . . C1 C 0.97602(16) 0.40136(10) 0.0790(3) 0.0319(6) Uani 1 1 d . . . C2 C 0.93829(16) 0.43858(11) 0.1962(4) 0.0385(6) Uani 1 1 d . . . C3 C 0.99086(18) 0.47190(12) 0.2978(4) 0.0445(7) Uani 1 1 d . . . H3A H 0.9658 0.4962 0.3780 0.053 Uiso 1 1 calc R . . C4 C 1.07957(18) 0.46954(11) 0.2820(4) 0.0425(6) Uani 1 1 d . . . H4A H 1.1142 0.4934 0.3495 0.051 Uiso 1 1 calc R . . C5 C 1.11890(16) 0.43272(11) 0.1685(3) 0.0349(6) Uani 1 1 d . . . C6 C 1.21618(17) 0.43091(14) 0.1530(4) 0.0499(8) Uani 1 1 d . . . H6A H 1.2324 0.4027 0.0692 0.075 Uiso 1 1 calc R . . H6B H 1.2414 0.4195 0.2575 0.075 Uiso 1 1 calc R . . H6C H 1.2374 0.4694 0.1223 0.075 Uiso 1 1 calc R . . C7 C 1.06586(16) 0.39881(10) 0.0691(3) 0.0324(6) Uani 1 1 d . . . H7A H 1.0915 0.3733 -0.0074 0.039 Uiso 1 1 calc R . . C8 C 0.97544(17) 0.32399(11) -0.1989(3) 0.0376(6) Uani 1 1 d . . . C9 C 0.9945(2) 0.34766(14) -0.3526(4) 0.0490(7) Uani 1 1 d . . . H9A H 0.9698 0.3837 -0.3830 0.059 Uiso 1 1 calc R . . C10 C 1.0489(2) 0.31936(17) -0.4608(4) 0.0600(9) Uani 1 1 d . . . H10A H 1.0613 0.3364 -0.5633 0.072 Uiso 1 1 calc R . . C11 C 1.0849(2) 0.26659(16) -0.4203(4) 0.0605(9) Uani 1 1 d . . . H11A H 1.1217 0.2472 -0.4944 0.073 Uiso 1 1 calc R . . C12 C 1.0664(2) 0.24239(14) -0.2695(4) 0.0618(9) Uani 1 1 d . . . H12A H 1.0909 0.2061 -0.2409 0.074 Uiso 1 1 calc R . . C13 C 1.0126(2) 0.27028(12) -0.1598(4) 0.0473(7) Uani 1 1 d . . . H13A H 1.0009 0.2529 -0.0574 0.057 Uiso 1 1 calc R . . C14 C 0.85387(16) 0.30726(11) 0.0617(4) 0.0403(6) Uani 1 1 d . . . C15 C 0.7827(2) 0.27788(14) -0.0031(5) 0.0609(9) Uani 1 1 d . . . H15A H 0.7639 0.2859 -0.1108 0.073 Uiso 1 1 calc R . . C16 C 0.7396(3) 0.23663(16) 0.0917(7) 0.0819(13) Uani 1 1 d . . . H16A H 0.6922 0.2162 0.0470 0.098 Uiso 1 1 calc R . . C17 C 0.7650(3) 0.22538(15) 0.2488(7) 0.0867(16) Uani 1 1 d . . . H17A H 0.7348 0.1977 0.3122 0.104 Uiso 1 1 calc R . . C18 C 0.8343(3) 0.25407(15) 0.3148(5) 0.0694(11) Uani 1 1 d . . . H18A H 0.8518 0.2463 0.4234 0.083 Uiso 1 1 calc R . . C19 C 0.8790(2) 0.29506(13) 0.2202(4) 0.0503(7) Uani 1 1 d . . . H19A H 0.9270 0.3146 0.2654 0.060 Uiso 1 1 calc R . . C20 C 0.79422(16) 0.48914(11) 0.2173(3) 0.0371(6) Uani 1 1 d . . . C21 C 0.82649(17) 0.54530(12) 0.1882(4) 0.0422(7) Uani 1 1 d . . . H21A H 0.8860 0.5506 0.1689 0.051 Uiso 1 1 calc R . . C22 C 0.77181(19) 0.59292(12) 0.1875(4) 0.0448(7) Uani 1 1 d . . . H22A H 0.7950 0.6304 0.1686 0.054 Uiso 1 1 calc R . . C23 C 0.68387(18) 0.58712(11) 0.2137(4) 0.0405(6) Uani 1 1 d . . . C24 C 0.6253(2) 0.64030(13) 0.2135(5) 0.0616(9) Uani 1 1 d . . . H24A H 0.6595 0.6751 0.1928 0.092 Uiso 1 1 calc R . . H24B H 0.5969 0.6437 0.3195 0.092 Uiso 1 1 calc R . . H24C H 0.5819 0.6361 0.1279 0.092 Uiso 1 1 calc R . . C25 C 0.65221(16) 0.53104(11) 0.2417(3) 0.0369(6) Uani 1 1 d . . . H25A H 0.5924 0.5263 0.2587 0.044 Uiso 1 1 calc R . . C26 C 0.70479(15) 0.48153(10) 0.2459(3) 0.0322(6) Uani 1 1 d . . . C27 C 0.6474(2) 0.40505(13) 0.5055(4) 0.0517(8) Uani 1 1 d . . . H27A H 0.6156 0.3684 0.5297 0.062 Uiso 1 1 calc R . . C28 C 0.5937(2) 0.45434(16) 0.5761(4) 0.0595(9) Uani 1 1 d . . . H28A H 0.5888 0.4494 0.6943 0.089 Uiso 1 1 calc R . . H28B H 0.5365 0.4537 0.5271 0.089 Uiso 1 1 calc R . . H28C H 0.6215 0.4915 0.5523 0.089 Uiso 1 1 calc R . . C29 C 0.7346(3) 0.40009(17) 0.5924(6) 0.0791(12) Uani 1 1 d . . . H29A H 0.7256 0.3991 0.7105 0.119 Uiso 1 1 calc R . . H29B H 0.7703 0.4336 0.5642 0.119 Uiso 1 1 calc R . . H29C H 0.7635 0.3644 0.5577 0.119 Uiso 1 1 calc R . . C30 C 0.55258(18) 0.40935(12) 0.1986(4) 0.0437(7) Uani 1 1 d . . . H30A H 0.5215 0.4428 0.2486 0.052 Uiso 1 1 calc R . . C31 C 0.5057(2) 0.35261(17) 0.2423(5) 0.0731(11) Uani 1 1 d . . . H31A H 0.4469 0.3540 0.2004 0.110 Uiso 1 1 calc R . . H31B H 0.5043 0.3480 0.3610 0.110 Uiso 1 1 calc R . . H31C H 0.5359 0.3197 0.1935 0.110 Uiso 1 1 calc R . . C32 C 0.5570(3) 0.41775(17) 0.0134(4) 0.0719(11) Uani 1 1 d . . . H32A H 0.4988 0.4197 -0.0311 0.108 Uiso 1 1 calc R . . H32B H 0.5876 0.3850 -0.0359 0.108 Uiso 1 1 calc R . . H32C H 0.5875 0.4538 -0.0112 0.108 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 N1 0.0314(12) 0.0293(12) 0.099(2) -0.0154(13) 0.0179(13) -0.0021(9) P1 0.0311(3) 0.0316(3) 0.0484(4) 0.0014(3) -0.0083(3) 0.0002(3) P2 0.0317(3) 0.0326(3) 0.0497(4) -0.0004(3) 0.0024(3) -0.0039(3) C1 0.0288(13) 0.0241(12) 0.0429(15) 0.0022(11) 0.0012(11) 0.0000(9) C2 0.0296(13) 0.0314(14) 0.0545(16) -0.0022(12) 0.0099(12) 0.0012(11) C3 0.0436(16) 0.0382(15) 0.0518(17) -0.0145(14) 0.0091(14) -0.0031(12) C4 0.0441(15) 0.0361(14) 0.0471(16) -0.0031(13) -0.0048(13) -0.0076(11) C5 0.0274(13) 0.0319(13) 0.0453(15) 0.0058(11) -0.0005(11) -0.0021(10) C6 0.0311(15) 0.0467(16) 0.072(2) 0.0021(15) -0.0028(14) -0.0004(12) C7 0.0321(13) 0.0282(12) 0.0368(14) 0.0003(11) 0.0036(11) 0.0018(10) C8 0.0393(14) 0.0343(14) 0.0392(14) -0.0019(12) -0.0069(12) -0.0077(11) C9 0.0481(17) 0.0514(17) 0.0475(18) 0.0074(14) -0.0097(14) -0.0147(14) C10 0.062(2) 0.082(3) 0.0356(17) -0.0028(17) 0.0021(14) -0.0303(19) C11 0.065(2) 0.060(2) 0.057(2) -0.0190(17) 0.0162(16) -0.0231(17) C12 0.067(2) 0.0421(17) 0.076(3) -0.0079(17) 0.0225(18) -0.0044(15) C13 0.061(2) 0.0362(16) 0.0446(17) 0.0003(12) 0.0093(14) 0.0010(13) C14 0.0314(14) 0.0289(13) 0.0607(19) -0.0080(13) 0.0056(12) 0.0004(10) C15 0.0493(19) 0.0525(19) 0.081(2) -0.0092(17) -0.0030(17) -0.0172(15) C16 0.059(2) 0.056(2) 0.130(4) -0.011(3) 0.014(3) -0.0288(18) C17 0.088(3) 0.0402(19) 0.132(4) -0.001(2) 0.060(3) -0.0128(19) C18 0.092(3) 0.0419(18) 0.074(2) 0.0102(17) 0.029(2) 0.0018(19) C19 0.0547(18) 0.0354(15) 0.0608(19) 0.0039(14) 0.0060(15) -0.0031(13) C20 0.0333(14) 0.0338(14) 0.0443(15) -0.0072(12) 0.0083(11) -0.0021(11) C21 0.0325(14) 0.0405(15) 0.0537(18) -0.0020(13) 0.0138(12) -0.0069(12) C22 0.0468(17) 0.0380(16) 0.0496(17) 0.0035(13) 0.0094(13) -0.0069(12) C23 0.0403(15) 0.0377(15) 0.0434(15) 0.0071(12) 0.0026(12) 0.0006(11) C24 0.0525(18) 0.0449(17) 0.087(3) 0.0211(17) 0.0022(18) 0.0087(15) C25 0.0310(13) 0.0423(15) 0.0374(15) 0.0017(11) 0.0043(11) -0.0017(11) C26 0.0287(13) 0.0333(13) 0.0347(14) -0.0016(11) 0.0054(10) -0.0016(10) C27 0.057(2) 0.0495(19) 0.0491(17) 0.0182(15) -0.0122(14) -0.0107(14) C28 0.066(2) 0.078(2) 0.0345(16) 0.0065(16) 0.0064(15) -0.0081(18) C29 0.081(3) 0.077(3) 0.079(3) 0.011(2) -0.036(2) 0.011(2) C30 0.0388(16) 0.0482(17) 0.0442(15) 0.0002(13) -0.0058(13) -0.0078(12) C31 0.057(2) 0.077(2) 0.085(3) 0.009(2) -0.0127(19) -0.0314(18) C32 0.097(3) 0.071(2) 0.0478(19) 0.0006(18) -0.0213(19) -0.021(2) _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 N1 C20 1.397(3) . ? N1 C2 1.412(3) . ? P1 C8 1.825(3) . ? P1 C1 1.833(3) . ? P1 C14 1.840(3) . ? P2 C26 1.840(2) . ? P2 C30 1.847(3) . ? P2 C27 1.854(3) . ? C1 C7 1.391(3) . ? C1 C2 1.403(4) . ? C2 C3 1.386(4) . ? C3 C4 1.377(4) . ? C4 C5 1.388(4) . ? C5 C7 1.387(4) . ? C5 C6 1.508(4) . ? C8 C13 1.391(4) . ? C8 C9 1.393(4) . ? C9 C10 1.377(5) . ? C10 C11 1.368(5) . ? C11 C12 1.374(5) . ? C12 C13 1.375(4) . ? C14 C19 1.374(5) . ? C14 C15 1.391(4) . ? C15 C16 1.388(5) . ? C16 C17 1.360(7) . ? C17 C18 1.364(6) . ? C18 C19 1.394(4) . ? C20 C21 1.396(4) . ? C20 C26 1.411(3) . ? C21 C22 1.377(4) . ? C22 C23 1.381(4) . ? C23 C25 1.390(4) . ? C23 C24 1.514(4) . ? C25 C26 1.392(3) . ? C27 C28 1.511(5) . ? C27 C29 1.525(4) . ? C30 C32 1.520(4) . ? C30 C31 1.527(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 C20 N1 C2 126.8(2) . . ? C8 P1 C1 103.25(11) . . ? C8 P1 C14 102.33(12) . . ? C1 P1 C14 102.41(13) . . ? C26 P2 C30 103.52(12) . . ? C26 P2 C27 102.40(13) . . ? C30 P2 C27 102.86(14) . . ? C7 C1 C2 118.6(2) . . ? C7 C1 P1 124.26(19) . . ? C2 C1 P1 116.80(19) . . ? C3 C2 C1 119.6(2) . . ? C3 C2 N1 121.2(2) . . ? C1 C2 N1 119.1(2) . . ? C4 C3 C2 120.4(3) . . ? C3 C4 C5 121.4(3) . . ? C7 C5 C4 117.9(2) . . ? C7 C5 C6 121.6(2) . . ? C4 C5 C6 120.5(2) . . ? C5 C7 C1 122.1(2) . . ? C13 C8 C9 117.4(3) . . ? C13 C8 P1 125.1(2) . . ? C9 C8 P1 117.5(2) . . ? C10 C9 C8 121.3(3) . . ? C11 C10 C9 120.5(3) . . ? C10 C11 C12 119.0(3) . . ? C11 C12 C13 121.1(3) . . ? C12 C13 C8 120.7(3) . . ? C19 C14 C15 118.7(3) . . ? C19 C14 P1 124.0(2) . . ? C15 C14 P1 117.1(3) . . ? C16 C15 C14 119.7(4) . . ? C17 C16 C15 120.7(4) . . ? C16 C17 C18 120.3(4) . . ? C17 C18 C19 119.6(4) . . ? C14 C19 C18 120.9(3) . . ? C21 C20 N1 122.0(2) . . ? C21 C20 C26 119.4(2) . . ? N1 C20 C26 118.6(2) . . ? C22 C21 C20 120.5(2) . . ? C21 C22 C23 121.8(3) . . ? C22 C23 C25 117.4(2) . . ? C22 C23 C24 120.7(2) . . ? C25 C23 C24 122.0(3) . . ? C23 C25 C26 123.2(2) . . ? C25 C26 C20 117.8(2) . . ? C25 C26 P2 124.03(18) . . ? C20 C26 P2 118.14(19) . . ? C28 C27 C29 111.3(3) . . ? C28 C27 P2 116.0(2) . . ? C29 C27 P2 109.6(3) . . ? C32 C30 C31 111.1(3) . . ? C32 C30 P2 108.4(2) . . ? C31 C30 P2 109.4(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.236 _refine_diff_density_min -0.262 _refine_diff_density_rms 0.069 # Attachment 'Compound 3.cif' data_rkrl19 _database_code_depnum_ccdc_archive 'CCDC 812750' #TrackingRef 'Compound 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H39 Cl N P2 Pd' _chemical_formula_weight 677.46 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 9.6912(6) _cell_length_b 11.5459(7) _cell_length_c 28.3155(17) _cell_angle_alpha 90.00 _cell_angle_beta 98.821(3) _cell_angle_gamma 90.00 _cell_volume 3130.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 9646 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 36.32 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1396 _exptl_absorpt_coefficient_mu 0.805 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6445 _exptl_absorpt_correction_T_max 0.8083 _exptl_absorpt_process_details 'Bruker, Sadabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 107611 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_av_sigmaI/netI 0.0203 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 36.38 _reflns_number_total 15154 _reflns_number_gt 13195 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics '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^)+(0.0382P)^2^+1.7872P] 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 15154 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0411 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0962 _refine_ls_wR_factor_gt 0.0856 _refine_ls_goodness_of_fit_ref 1.239 _refine_ls_restrained_S_all 1.239 _refine_ls_shift/su_max 0.004 _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 0.985852(10) 0.280252(9) 0.871749(4) 0.01684(3) Uani 1 1 d . . . P2 P 0.94443(4) 0.08658(3) 0.863412(14) 0.01830(6) Uani 1 1 d . . . Cl1 Cl 1.22354(4) 0.27509(4) 0.86969(2) 0.03353(9) Uani 1 1 d . . . P1 P 0.96484(4) 0.47861(3) 0.868157(13) 0.01708(6) Uani 1 1 d . . . N1 N 0.77813(12) 0.28415(10) 0.87464(5) 0.01858(19) Uani 1 1 d . . . C1 C 0.70446(14) 0.38303(12) 0.85832(5) 0.0180(2) Uani 1 1 d . . . C14 C 1.02406(15) 0.57622(12) 0.91727(5) 0.0206(2) Uani 1 1 d . . . C20 C 0.71542(14) 0.18481(12) 0.88992(5) 0.0185(2) Uani 1 1 d . . . C2 C 0.55900(15) 0.38564(14) 0.84133(6) 0.0223(2) Uani 1 1 d . . . H2A H 0.5072 0.3155 0.8390 0.027 Uiso 1 1 calc R . . C26 C 0.78614(15) 0.07800(12) 0.88918(5) 0.0199(2) Uani 1 1 d . . . C8 C 1.02988(15) 0.53795(12) 0.81612(5) 0.0200(2) Uani 1 1 d . . . C7 C 0.77698(14) 0.48872(12) 0.85661(5) 0.0180(2) Uani 1 1 d . . . C15 C 1.16203(18) 0.61419(16) 0.92569(7) 0.0296(3) Uani 1 1 d . . . H15A H 1.2243 0.5933 0.9043 0.036 Uiso 1 1 calc R . . C6 C 0.70544(15) 0.59213(13) 0.84419(5) 0.0215(2) Uani 1 1 d . . . H6A H 0.7567 0.6624 0.8452 0.026 Uiso 1 1 calc R . . C9 C 1.05657(18) 0.65545(14) 0.81093(6) 0.0258(3) Uani 1 1 d . . . H9A H 1.0442 0.7080 0.8358 0.031 Uiso 1 1 calc R . . C30 C 0.89365(18) 0.04610(15) 0.80013(6) 0.0269(3) Uani 1 1 d . . . H30A H 0.9789 0.0501 0.7842 0.032 Uiso 1 1 calc R . . C4 C 0.56183(16) 0.59504(14) 0.83051(6) 0.0250(3) Uani 1 1 d . . . C21 C 0.59071(16) 0.18469(14) 0.90976(6) 0.0245(3) Uani 1 1 d . . . H21A H 0.5403 0.2548 0.9114 0.029 Uiso 1 1 calc R . . C27 C 1.06626(18) -0.02230(14) 0.89312(7) 0.0279(3) Uani 1 1 d . . . H27A H 1.0143 -0.0967 0.8947 0.033 Uiso 1 1 calc R . . C25 C 0.73410(17) -0.02272(14) 0.90687(6) 0.0258(3) Uani 1 1 d . . . H25A H 0.7842 -0.0932 0.9058 0.031 Uiso 1 1 calc R . . C3 C 0.49132(16) 0.48871(15) 0.82805(6) 0.0256(3) Uani 1 1 d . . . H3A H 0.3938 0.4874 0.8169 0.031 Uiso 1 1 calc R . . C22 C 0.54114(18) 0.08251(16) 0.92687(6) 0.0284(3) Uani 1 1 d . . . H22A H 0.4561 0.0846 0.9397 0.034 Uiso 1 1 calc R . . C10 C 1.1013(2) 0.69643(15) 0.76957(7) 0.0314(3) Uani 1 1 d . . . H10A H 1.1192 0.7767 0.7664 0.038 Uiso 1 1 calc R . . C13 C 1.0494(2) 0.46241(15) 0.77915(6) 0.0306(3) Uani 1 1 d . . . H13A H 1.0321 0.3820 0.7822 0.037 Uiso 1 1 calc R . . C23 C 0.61031(18) -0.02257(15) 0.92612(7) 0.0289(3) Uani 1 1 d . . . C11 C 1.1198(2) 0.62119(17) 0.73313(7) 0.0329(3) Uani 1 1 d . . . H11A H 1.1499 0.6495 0.7049 0.039 Uiso 1 1 calc R . . C12 C 1.0941(2) 0.50435(18) 0.73798(7) 0.0359(4) Uani 1 1 d . . . H12A H 1.1070 0.4523 0.7130 0.043 Uiso 1 1 calc R . . C31 C 0.7881(2) 0.13503(18) 0.77603(6) 0.0347(4) Uani 1 1 d . . . H31A H 0.7607 0.1145 0.7423 0.052 Uiso 1 1 calc R . . H31B H 0.8307 0.2122 0.7783 0.052 Uiso 1 1 calc R . . H31C H 0.7053 0.1352 0.7920 0.052 Uiso 1 1 calc R . . C28 C 1.1872(2) -0.04362(17) 0.86540(8) 0.0365(4) Uani 1 1 d . . . H28A H 1.2501 -0.1020 0.8821 0.055 Uiso 1 1 calc R . . H28B H 1.2385 0.0288 0.8631 0.055 Uiso 1 1 calc R . . H28C H 1.1505 -0.0714 0.8332 0.055 Uiso 1 1 calc R . . C5 C 0.4852(2) 0.70645(17) 0.81686(9) 0.0386(4) Uani 1 1 d . . . H5A H 0.5514 0.7712 0.8209 0.058 Uiso 1 1 calc R . . H5B H 0.4137 0.7183 0.8374 0.058 Uiso 1 1 calc R . . H5C H 0.4407 0.7023 0.7834 0.058 Uiso 1 1 calc R . . C17 C 1.1195(3) 0.7137(2) 0.99643(8) 0.0421(5) Uani 1 1 d . . . H17A H 1.1515 0.7621 1.0230 0.051 Uiso 1 1 calc R . . C16 C 1.2089(2) 0.68238(19) 0.96528(8) 0.0377(4) Uani 1 1 d . . . H16A H 1.3033 0.7076 0.9709 0.045 Uiso 1 1 calc R . . C19 C 0.9359(2) 0.6051(2) 0.94972(8) 0.0421(5) Uani 1 1 d . . . H19A H 0.8425 0.5772 0.9452 0.050 Uiso 1 1 calc R . . C29 C 1.1188(2) 0.0178(2) 0.94419(7) 0.0403(4) Uani 1 1 d . . . H29A H 1.1838 -0.0398 0.9604 0.060 Uiso 1 1 calc R . . H29B H 1.0394 0.0266 0.9616 0.060 Uiso 1 1 calc R . . H29C H 1.1668 0.0923 0.9434 0.060 Uiso 1 1 calc R . . C32 C 0.8338(2) -0.07595(17) 0.79327(8) 0.0405(4) Uani 1 1 d . . . H32A H 0.8092 -0.0923 0.7590 0.061 Uiso 1 1 calc R . . H32B H 0.7500 -0.0819 0.8086 0.061 Uiso 1 1 calc R . . H32C H 0.9035 -0.1321 0.8077 0.061 Uiso 1 1 calc R . . C24 C 0.5564(3) -0.13202(19) 0.94603(9) 0.0440(5) Uani 1 1 d . . . H24A H 0.4589 -0.1209 0.9504 0.066 Uiso 1 1 calc R . . H24B H 0.6130 -0.1501 0.9769 0.066 Uiso 1 1 calc R . . H24C H 0.5623 -0.1961 0.9237 0.066 Uiso 1 1 calc R . . C18 C 0.9839(3) 0.6748(3) 0.98895(9) 0.0528(7) Uani 1 1 d . . . H18A H 0.9226 0.6955 1.0107 0.063 Uiso 1 1 calc R . . C34 C 0.4513(2) 0.45756(18) 0.95493(7) 0.0359(4) Uani 1 1 d . . . H34A H 0.4175 0.4284 0.9239 0.043 Uiso 1 1 calc R . . C33 C 0.5522(2) 0.5424(2) 0.96082(8) 0.0404(4) Uani 1 1 d . . . H33A H 0.5884 0.5716 0.9338 0.049 Uiso 1 1 calc R . . C35 C 0.3992(2) 0.41480(19) 0.99426(9) 0.0404(4) Uani 1 1 d . . . H35A H 0.3298 0.3560 0.9903 0.048 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 0.01510(4) 0.01565(4) 0.02023(5) -0.00170(3) 0.00423(3) -0.00129(3) P2 0.01870(14) 0.01568(14) 0.02118(15) -0.00113(11) 0.00514(12) 0.00029(11) Cl1 0.01642(14) 0.03015(18) 0.0552(3) -0.00352(17) 0.00915(15) -0.00148(13) P1 0.01713(14) 0.01541(14) 0.01920(15) -0.00165(11) 0.00443(11) -0.00159(10) N1 0.0170(4) 0.0154(4) 0.0243(5) -0.0005(4) 0.0062(4) -0.0006(4) C1 0.0177(5) 0.0184(5) 0.0184(5) -0.0009(4) 0.0044(4) -0.0008(4) C14 0.0213(6) 0.0191(5) 0.0209(6) -0.0019(4) 0.0016(4) -0.0016(4) C20 0.0182(5) 0.0187(5) 0.0190(5) -0.0011(4) 0.0044(4) -0.0024(4) C2 0.0174(5) 0.0242(6) 0.0249(6) -0.0004(5) 0.0019(5) -0.0028(5) C26 0.0211(6) 0.0169(5) 0.0226(6) 0.0005(4) 0.0060(5) -0.0022(4) C8 0.0195(5) 0.0196(5) 0.0216(6) -0.0003(4) 0.0053(4) -0.0022(4) C7 0.0172(5) 0.0174(5) 0.0195(5) -0.0008(4) 0.0033(4) -0.0010(4) C15 0.0224(6) 0.0334(8) 0.0314(8) -0.0055(6) -0.0008(6) -0.0036(6) C6 0.0216(6) 0.0198(6) 0.0236(6) 0.0021(5) 0.0045(5) 0.0009(4) C9 0.0329(7) 0.0191(6) 0.0264(7) 0.0017(5) 0.0075(6) -0.0011(5) C30 0.0293(7) 0.0279(7) 0.0243(7) -0.0069(5) 0.0067(5) 0.0001(6) C4 0.0224(6) 0.0263(7) 0.0264(7) 0.0047(5) 0.0039(5) 0.0047(5) C21 0.0202(6) 0.0253(6) 0.0299(7) 0.0012(5) 0.0101(5) -0.0017(5) C27 0.0255(7) 0.0209(6) 0.0372(8) 0.0045(6) 0.0049(6) 0.0042(5) C25 0.0270(7) 0.0202(6) 0.0311(7) 0.0041(5) 0.0073(6) -0.0028(5) C3 0.0189(6) 0.0307(7) 0.0265(7) 0.0034(6) 0.0010(5) 0.0019(5) C22 0.0244(7) 0.0315(8) 0.0315(8) 0.0034(6) 0.0113(6) -0.0059(6) C10 0.0392(9) 0.0231(7) 0.0335(8) 0.0064(6) 0.0107(7) -0.0034(6) C13 0.0422(9) 0.0246(7) 0.0281(7) -0.0047(6) 0.0151(7) -0.0072(6) C23 0.0290(7) 0.0264(7) 0.0324(8) 0.0063(6) 0.0087(6) -0.0076(6) C11 0.0376(9) 0.0345(8) 0.0291(8) 0.0058(6) 0.0131(7) -0.0026(7) C12 0.0491(11) 0.0333(8) 0.0290(8) -0.0048(7) 0.0181(8) -0.0057(8) C31 0.0420(10) 0.0392(9) 0.0210(7) -0.0014(6) -0.0007(6) 0.0035(8) C28 0.0268(8) 0.0307(8) 0.0529(12) -0.0049(8) 0.0089(7) 0.0066(6) C5 0.0307(8) 0.0303(9) 0.0534(12) 0.0102(8) 0.0022(8) 0.0100(7) C17 0.0475(12) 0.0433(11) 0.0315(9) -0.0149(8) -0.0067(8) -0.0056(9) C16 0.0338(9) 0.0395(10) 0.0363(9) -0.0076(8) -0.0060(7) -0.0112(7) C19 0.0300(8) 0.0643(14) 0.0330(9) -0.0246(9) 0.0085(7) -0.0106(9) C29 0.0403(10) 0.0467(11) 0.0323(9) 0.0107(8) 0.0006(8) 0.0104(9) C32 0.0454(11) 0.0286(8) 0.0461(11) -0.0165(8) 0.0022(9) -0.0037(7) C24 0.0465(11) 0.0337(9) 0.0548(13) 0.0147(9) 0.0174(10) -0.0105(8) C18 0.0437(12) 0.0785(18) 0.0363(11) -0.0308(12) 0.0070(9) -0.0055(12) C34 0.0418(10) 0.0360(9) 0.0305(8) -0.0052(7) 0.0072(7) 0.0097(8) C33 0.0400(10) 0.0500(12) 0.0345(9) 0.0101(8) 0.0161(8) 0.0029(9) C35 0.0388(10) 0.0355(9) 0.0469(11) 0.0061(8) 0.0066(8) -0.0046(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.0277(12) . ? Pd1 P2 2.2778(4) . ? Pd1 P1 2.3001(4) . ? Pd1 Cl1 2.3139(4) . ? P2 C26 1.7996(14) . ? P2 C27 1.8377(16) . ? P2 C30 1.8442(17) . ? P1 C7 1.8035(14) . ? P1 C14 1.8134(15) . ? P1 C8 1.8228(15) . ? N1 C1 1.3876(18) . ? N1 C20 1.3976(18) . ? C1 C7 1.4127(19) . ? C1 C2 1.418(2) . ? C14 C19 1.388(2) . ? C14 C15 1.392(2) . ? C20 C21 1.409(2) . ? C20 C26 1.413(2) . ? C2 C3 1.383(2) . ? C26 C25 1.391(2) . ? C8 C9 1.393(2) . ? C8 C13 1.398(2) . ? C7 C6 1.398(2) . ? C15 C16 1.388(3) . ? C6 C4 1.387(2) . ? C9 C10 1.392(2) . ? C30 C32 1.525(3) . ? C30 C31 1.534(3) . ? C4 C3 1.402(2) . ? C4 C5 1.506(2) . ? C21 C22 1.389(2) . ? C27 C28 1.527(3) . ? C27 C29 1.529(3) . ? C25 C23 1.392(2) . ? C22 C23 1.388(3) . ? C10 C11 1.381(3) . ? C13 C12 1.391(2) . ? C23 C24 1.509(2) . ? C11 C12 1.383(3) . ? C17 C18 1.374(3) . ? C17 C16 1.376(3) . ? C19 C18 1.393(3) . ? C34 C33 1.376(3) . ? C34 C35 1.382(3) . ? C33 C35 1.378(3) 3_667 ? C35 C33 1.378(3) 3_667 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 P2 82.28(3) . . ? N1 Pd1 P1 84.14(3) . . ? P2 Pd1 P1 163.724(15) . . ? N1 Pd1 Cl1 179.12(4) . . ? P2 Pd1 Cl1 97.609(15) . . ? P1 Pd1 Cl1 96.100(14) . . ? C26 P2 C27 107.73(7) . . ? C26 P2 C30 105.24(8) . . ? C27 P2 C30 109.17(8) . . ? C26 P2 Pd1 99.19(5) . . ? C27 P2 Pd1 122.24(6) . . ? C30 P2 Pd1 111.47(6) . . ? C7 P1 C14 106.90(7) . . ? C7 P1 C8 107.08(7) . . ? C14 P1 C8 106.15(7) . . ? C7 P1 Pd1 98.77(5) . . ? C14 P1 Pd1 124.71(5) . . ? C8 P1 Pd1 111.76(5) . . ? C1 N1 C20 123.53(12) . . ? C1 N1 Pd1 117.92(9) . . ? C20 N1 Pd1 118.41(9) . . ? N1 C1 C7 119.26(12) . . ? N1 C1 C2 124.35(13) . . ? C7 C1 C2 116.35(13) . . ? C19 C14 C15 118.93(15) . . ? C19 C14 P1 120.14(12) . . ? C15 C14 P1 120.64(12) . . ? N1 C20 C21 124.39(13) . . ? N1 C20 C26 118.48(12) . . ? C21 C20 C26 116.93(13) . . ? C3 C2 C1 121.05(14) . . ? C25 C26 C20 121.40(13) . . ? C25 C26 P2 124.80(12) . . ? C20 C26 P2 113.81(10) . . ? C9 C8 C13 118.69(14) . . ? C9 C8 P1 122.97(12) . . ? C13 C8 P1 118.31(11) . . ? C6 C7 C1 121.07(13) . . ? C6 C7 P1 123.27(11) . . ? C1 C7 P1 115.57(10) . . ? C16 C15 C14 120.22(17) . . ? C4 C6 C7 121.91(14) . . ? C10 C9 C8 120.43(15) . . ? C32 C30 C31 110.30(16) . . ? C32 C30 P2 113.42(14) . . ? C31 C30 P2 108.85(11) . . ? C6 C4 C3 116.97(14) . . ? C6 C4 C5 121.79(16) . . ? C3 C4 C5 121.20(15) . . ? C22 C21 C20 120.25(15) . . ? C28 C27 C29 111.38(16) . . ? C28 C27 P2 111.39(13) . . ? C29 C27 P2 108.84(13) . . ? C26 C25 C23 121.46(15) . . ? C2 C3 C4 122.21(14) . . ? C23 C22 C21 122.92(15) . . ? C11 C10 C9 120.48(16) . . ? C12 C13 C8 120.37(16) . . ? C22 C23 C25 117.03(14) . . ? C22 C23 C24 122.05(17) . . ? C25 C23 C24 120.91(17) . . ? C10 C11 C12 119.57(16) . . ? C11 C12 C13 120.46(17) . . ? C18 C17 C16 119.74(18) . . ? C17 C16 C15 120.46(18) . . ? C14 C19 C18 120.13(19) . . ? C17 C18 C19 120.5(2) . . ? C33 C34 C35 119.8(2) . . ? C34 C33 C35 120.19(19) . 3_667 ? C33 C35 C34 120.0(2) 3_667 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Pd1 P2 C26 -22.01(6) . . . . ? P1 Pd1 P2 C26 -55.75(7) . . . . ? Cl1 Pd1 P2 C26 157.10(5) . . . . ? N1 Pd1 P2 C27 -139.83(8) . . . . ? P1 Pd1 P2 C27 -173.56(8) . . . . ? Cl1 Pd1 P2 C27 39.29(7) . . . . ? N1 Pd1 P2 C30 88.47(7) . . . . ? P1 Pd1 P2 C30 54.73(8) . . . . ? Cl1 Pd1 P2 C30 -92.42(6) . . . . ? N1 Pd1 P1 C7 -12.61(6) . . . . ? P2 Pd1 P1 C7 20.98(7) . . . . ? Cl1 Pd1 P1 C7 168.24(5) . . . . ? N1 Pd1 P1 C14 105.09(7) . . . . ? P2 Pd1 P1 C14 138.67(7) . . . . ? Cl1 Pd1 P1 C14 -74.06(6) . . . . ? N1 Pd1 P1 C8 -125.05(6) . . . . ? P2 Pd1 P1 C8 -91.46(7) . . . . ? Cl1 Pd1 P1 C8 55.80(5) . . . . ? P2 Pd1 N1 C1 -150.57(10) . . . . ? P1 Pd1 N1 C1 20.43(10) . . . . ? Cl1 Pd1 N1 C1 126(2) . . . . ? P2 Pd1 N1 C20 25.31(10) . . . . ? P1 Pd1 N1 C20 -163.69(11) . . . . ? Cl1 Pd1 N1 C20 -58(2) . . . . ? C20 N1 C1 C7 162.05(13) . . . . ? Pd1 N1 C1 C7 -22.30(17) . . . . ? C20 N1 C1 C2 -20.1(2) . . . . ? Pd1 N1 C1 C2 155.51(12) . . . . ? C7 P1 C14 C19 25.23(18) . . . . ? C8 P1 C14 C19 139.29(17) . . . . ? Pd1 P1 C14 C19 -88.63(17) . . . . ? C7 P1 C14 C15 -161.06(13) . . . . ? C8 P1 C14 C15 -47.00(15) . . . . ? Pd1 P1 C14 C15 85.09(14) . . . . ? C1 N1 C20 C21 -28.0(2) . . . . ? Pd1 N1 C20 C21 156.39(12) . . . . ? C1 N1 C20 C26 157.31(14) . . . . ? Pd1 N1 C20 C26 -18.33(18) . . . . ? N1 C1 C2 C3 176.47(14) . . . . ? C7 C1 C2 C3 -5.7(2) . . . . ? N1 C20 C26 C25 175.66(14) . . . . ? C21 C20 C26 C25 0.5(2) . . . . ? N1 C20 C26 P2 -4.69(18) . . . . ? C21 C20 C26 P2 -179.80(12) . . . . ? C27 P2 C26 C25 -31.42(16) . . . . ? C30 P2 C26 C25 84.97(15) . . . . ? Pd1 P2 C26 C25 -159.66(13) . . . . ? C27 P2 C26 C20 148.94(12) . . . . ? C30 P2 C26 C20 -94.66(12) . . . . ? Pd1 P2 C26 C20 20.70(12) . . . . ? C7 P1 C8 C9 86.90(14) . . . . ? C14 P1 C8 C9 -27.04(15) . . . . ? Pd1 P1 C8 C9 -165.97(12) . . . . ? C7 P1 C8 C13 -90.98(14) . . . . ? C14 P1 C8 C13 155.09(14) . . . . ? Pd1 P1 C8 C13 16.15(15) . . . . ? N1 C1 C7 C6 -174.67(13) . . . . ? C2 C1 C7 C6 7.4(2) . . . . ? N1 C1 C7 P1 8.59(17) . . . . ? C2 C1 C7 P1 -169.39(11) . . . . ? C14 P1 C7 C6 59.09(14) . . . . ? C8 P1 C7 C6 -54.34(14) . . . . ? Pd1 P1 C7 C6 -170.43(12) . . . . ? C14 P1 C7 C1 -124.25(11) . . . . ? C8 P1 C7 C1 122.33(11) . . . . ? Pd1 P1 C7 C1 6.23(11) . . . . ? C19 C14 C15 C16 -1.7(3) . . . . ? P1 C14 C15 C16 -175.52(16) . . . . ? C1 C7 C6 C4 -3.6(2) . . . . ? P1 C7 C6 C4 172.89(12) . . . . ? C13 C8 C9 C10 0.3(3) . . . . ? P1 C8 C9 C10 -177.61(14) . . . . ? C26 P2 C30 C32 -60.55(15) . . . . ? C27 P2 C30 C32 54.85(16) . . . . ? Pd1 P2 C30 C32 -167.11(12) . . . . ? C26 P2 C30 C31 62.64(14) . . . . ? C27 P2 C30 C31 178.04(13) . . . . ? Pd1 P2 C30 C31 -43.92(14) . . . . ? C7 C6 C4 C3 -2.1(2) . . . . ? C7 C6 C4 C5 -179.62(17) . . . . ? N1 C20 C21 C22 -175.70(15) . . . . ? C26 C20 C21 C22 -0.9(2) . . . . ? C26 P2 C27 C28 165.19(13) . . . . ? C30 P2 C27 C28 51.40(15) . . . . ? Pd1 P2 C27 C28 -81.24(14) . . . . ? C26 P2 C27 C29 -71.63(15) . . . . ? C30 P2 C27 C29 174.58(13) . . . . ? Pd1 P2 C27 C29 41.94(15) . . . . ? C20 C26 C25 C23 -0.1(3) . . . . ? P2 C26 C25 C23 -179.71(14) . . . . ? C1 C2 C3 C4 0.1(3) . . . . ? C6 C4 C3 C2 3.9(2) . . . . ? C5 C4 C3 C2 -178.64(17) . . . . ? C20 C21 C22 C23 0.9(3) . . . . ? C8 C9 C10 C11 0.0(3) . . . . ? C9 C8 C13 C12 -0.3(3) . . . . ? P1 C8 C13 C12 177.67(16) . . . . ? C21 C22 C23 C25 -0.4(3) . . . . ? C21 C22 C23 C24 178.45(19) . . . . ? C26 C25 C23 C22 0.0(3) . . . . ? C26 C25 C23 C24 -178.86(19) . . . . ? C9 C10 C11 C12 -0.3(3) . . . . ? C10 C11 C12 C13 0.2(3) . . . . ? C8 C13 C12 C11 0.1(3) . . . . ? C18 C17 C16 C15 1.7(4) . . . . ? C14 C15 C16 C17 -0.4(3) . . . . ? C15 C14 C19 C18 2.5(4) . . . . ? P1 C14 C19 C18 176.4(2) . . . . ? C16 C17 C18 C19 -0.8(4) . . . . ? C14 C19 C18 C17 -1.3(4) . . . . ? C35 C34 C33 C35 -0.3(4) . . . 3_667 ? C33 C34 C35 C33 0.3(4) . . . 3_667 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 36.38 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.830 _refine_diff_density_min -1.515 _refine_diff_density_rms 0.157 # Attachment 'Compound 4.cif' data_rkrl31 _database_code_depnum_ccdc_archive 'CCDC 812751' #TrackingRef 'Compound 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H50 Cl N P2 Pd' _chemical_formula_weight 796.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3446(3) _cell_length_b 11.7317(3) _cell_length_c 15.4507(4) _cell_angle_alpha 93.6470(10) _cell_angle_beta 109.9500(10) _cell_angle_gamma 93.1420(10) _cell_volume 1922.61(9) _cell_formula_units_Z 2 _cell_measurement_temperature 188(2) _cell_measurement_reflns_used 9814 _cell_measurement_theta_min 2.70 _cell_measurement_theta_max 35.07 _exptl_crystal_description chip _exptl_crystal_colour purple _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 828 _exptl_absorpt_coefficient_mu 0.667 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7314 _exptl_absorpt_correction_T_max 0.9302 _exptl_absorpt_process_details 'Bruker, Sadabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 188(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 '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 56344 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0338 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 34.34 _reflns_number_total 16083 _reflns_number_gt 13616 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics '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^)+(0.0510P)^2^+0.4909P] 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 16083 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.1030 _refine_ls_wR_factor_gt 0.0929 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_restrained_S_all 1.142 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.425652(10) 0.296209(9) 0.729465(7) 0.01827(4) Uani 1 1 d . . . Cl1 Cl 0.63384(4) 0.31835(4) 0.73846(3) 0.03211(9) Uani 1 1 d . . . P1 P 0.39725(4) 0.48749(3) 0.73086(3) 0.02040(7) Uani 1 1 d . . . P2 P 0.39485(4) 0.09908(3) 0.71182(3) 0.01907(7) Uani 1 1 d . . . N1 N 0.24707(12) 0.28370(11) 0.72941(9) 0.0214(2) Uani 1 1 d . . . C1 C 0.17088(14) 0.37171(13) 0.69704(10) 0.0207(3) Uani 1 1 d . . . C2 C 0.03822(16) 0.35998(15) 0.66345(12) 0.0268(3) Uani 1 1 d . . . H2A H -0.0046 0.2886 0.6650 0.032 Uiso 1 1 calc R . . C3 C -0.03045(16) 0.45048(17) 0.62835(13) 0.0307(3) Uani 1 1 d . . . H3A H -0.1197 0.4394 0.6064 0.037 Uiso 1 1 calc R . . C4 C 0.02605(17) 0.55793(15) 0.62378(12) 0.0289(3) Uani 1 1 d . . . C5 C -0.0510(2) 0.65450(19) 0.58374(16) 0.0400(4) Uani 1 1 d . . . H5A H -0.1404 0.6257 0.5680 0.048 Uiso 1 1 d R . . H5B H -0.0345 0.7173 0.6299 0.048 Uiso 1 1 d R . . H5C H -0.0365 0.6740 0.5312 0.048 Uiso 1 1 d R . . C6 C 0.15607(16) 0.56968(14) 0.65550(12) 0.0261(3) Uani 1 1 d . . . H6A H 0.1977 0.6411 0.6526 0.031 Uiso 1 1 calc R . . C7 C 0.22827(15) 0.47959(13) 0.69174(11) 0.0216(3) Uani 1 1 d . . . C8 C 0.45740(16) 0.57223(14) 0.84137(11) 0.0248(3) Uani 1 1 d . . . C9 C 0.3906(2) 0.6561(2) 0.86483(15) 0.0443(5) Uani 1 1 d . . . H9A H 0.3112 0.6710 0.8223 0.053 Uiso 1 1 calc R . . C10 C 0.4389(2) 0.7193(2) 0.95061(16) 0.0506(6) Uani 1 1 d . . . H10A H 0.3922 0.7768 0.9663 0.061 Uiso 1 1 calc R . . C11 C 0.5539(2) 0.6987(2) 1.01263(13) 0.0397(4) Uani 1 1 d . . . H11A H 0.5871 0.7426 1.0707 0.048 Uiso 1 1 calc R . . C12 C 0.6202(2) 0.6146(2) 0.99023(14) 0.0411(5) Uani 1 1 d . . . H12A H 0.6990 0.5995 1.0335 0.049 Uiso 1 1 calc R . . C13 C 0.57349(19) 0.55108(18) 0.90470(13) 0.0342(4) Uani 1 1 d . . . H13A H 0.6206 0.4935 0.8895 0.041 Uiso 1 1 calc R . . C14 C 0.44471(16) 0.56954(14) 0.65090(11) 0.0247(3) Uani 1 1 d . . . C15 C 0.5573(2) 0.63888(18) 0.68101(14) 0.0369(4) Uani 1 1 d . . . H15A H 0.6080 0.6470 0.7446 0.044 Uiso 1 1 calc R . . C16 C 0.5950(2) 0.69615(19) 0.61763(17) 0.0436(5) Uani 1 1 d . . . H16A H 0.6710 0.7445 0.6383 0.052 Uiso 1 1 calc R . . C17 C 0.5225(2) 0.68313(19) 0.52459(16) 0.0414(5) Uani 1 1 d . . . H17A H 0.5488 0.7227 0.4817 0.050 Uiso 1 1 calc R . . C18 C 0.4123(2) 0.61302(19) 0.49401(14) 0.0381(4) Uani 1 1 d . . . H18A H 0.3626 0.6043 0.4302 0.046 Uiso 1 1 calc R . . C19 C 0.37398(18) 0.55518(18) 0.55684(13) 0.0322(4) Uani 1 1 d . . . H19A H 0.2990 0.5055 0.5355 0.039 Uiso 1 1 calc R . . C20 C 0.20444(14) 0.18394(13) 0.75833(10) 0.0202(3) Uani 1 1 d . . . C21 C 0.11075(15) 0.17937(15) 0.79909(11) 0.0249(3) Uani 1 1 d . . . H21A H 0.0732 0.2472 0.8087 0.030 Uiso 1 1 calc R . . C22 C 0.07282(16) 0.07699(16) 0.82524(12) 0.0281(3) Uani 1 1 d . . . H22A H 0.0096 0.0765 0.8527 0.034 Uiso 1 1 calc R . . C23 C 0.12404(16) -0.02538(16) 0.81276(12) 0.0281(3) Uani 1 1 d . . . C24 C 0.0789(2) -0.13622(19) 0.83881(17) 0.0425(5) Uani 1 1 d . . . H24A H 0.0105 -0.1231 0.8625 0.064 Uiso 1 1 calc R . . H24B H 0.1486 -0.1663 0.8867 0.064 Uiso 1 1 calc R . . H24C H 0.0483 -0.1917 0.7843 0.064 Uiso 1 1 calc R . . C25 C 0.22175(16) -0.01963(15) 0.77750(12) 0.0260(3) Uani 1 1 d . . . H25A H 0.2614 -0.0872 0.7708 0.031 Uiso 1 1 calc R . . C26 C 0.26293(15) 0.08285(13) 0.75169(10) 0.0211(3) Uani 1 1 d . . . C27 C 0.51469(15) 0.00962(14) 0.77924(11) 0.0227(3) Uani 1 1 d . . . H27A H 0.4747 -0.0697 0.7744 0.027 Uiso 1 1 calc R . . C28 C 0.56250(17) 0.05664(17) 0.88101(11) 0.0302(3) Uani 1 1 d . . . H28A H 0.5952 0.1377 0.8863 0.036 Uiso 1 1 calc R . . H28B H 0.4918 0.0538 0.9048 0.036 Uiso 1 1 calc R . . C29 C 0.6666(2) -0.0124(2) 0.93935(13) 0.0392(4) Uani 1 1 d . . . H29A H 0.6982 0.0220 1.0041 0.047 Uiso 1 1 calc R . . H29B H 0.6317 -0.0918 0.9389 0.047 Uiso 1 1 calc R . . C30 C 0.77468(19) -0.0149(2) 0.90248(14) 0.0396(4) Uani 1 1 d . . . H30A H 0.8143 0.0638 0.9078 0.048 Uiso 1 1 calc R . . H30B H 0.8391 -0.0626 0.9399 0.048 Uiso 1 1 calc R . . C31 C 0.72809(19) -0.06332(19) 0.80209(14) 0.0377(4) Uani 1 1 d . . . H31A H 0.6961 -0.1445 0.7978 0.045 Uiso 1 1 calc R . . H31B H 0.7992 -0.0609 0.7787 0.045 Uiso 1 1 calc R . . C32 C 0.62349(17) 0.00380(17) 0.74168(12) 0.0291(3) Uani 1 1 d . . . H32A H 0.5914 -0.0336 0.6778 0.035 Uiso 1 1 calc R . . H32B H 0.6581 0.0825 0.7396 0.035 Uiso 1 1 calc R . . C33 C 0.33957(15) 0.03767(14) 0.59045(10) 0.0222(3) Uani 1 1 d . . . H33A H 0.4111 0.0490 0.5671 0.027 Uiso 1 1 calc R . . C34 C 0.2997(2) -0.09101(15) 0.57746(12) 0.0326(4) Uani 1 1 d . . . H34A H 0.3716 -0.1329 0.6129 0.039 Uiso 1 1 calc R . . H34B H 0.2306 -0.1056 0.6017 0.039 Uiso 1 1 calc R . . C35 C 0.2559(2) -0.13513(17) 0.47513(14) 0.0423(5) Uani 1 1 d . . . H35A H 0.3279 -0.1286 0.4529 0.051 Uiso 1 1 calc R . . H35B H 0.2257 -0.2171 0.4681 0.051 Uiso 1 1 calc R . . C36 C 0.1511(2) -0.06837(18) 0.41654(14) 0.0424(5) Uani 1 1 d . . . H36A H 0.1296 -0.0955 0.3506 0.051 Uiso 1 1 calc R . . H36B H 0.0753 -0.0827 0.4334 0.051 Uiso 1 1 calc R . . C37 C 0.1893(2) 0.05897(17) 0.42997(12) 0.0358(4) Uani 1 1 d . . . H37A H 0.1170 0.1002 0.3942 0.043 Uiso 1 1 calc R . . H37B H 0.2585 0.0743 0.4058 0.043 Uiso 1 1 calc R . . C38 C 0.23255(16) 0.10434(15) 0.53209(11) 0.0264(3) Uani 1 1 d . . . H38A H 0.2616 0.1866 0.5387 0.032 Uiso 1 1 calc R . . H38B H 0.1608 0.0969 0.5546 0.032 Uiso 1 1 calc R . . C44 C 1.1162(3) 0.3503(3) 0.1035(2) 0.0626(8) Uani 1 1 d . . . H44A H 1.2021 0.3361 0.1313 0.075 Uiso 1 1 calc R . . C43 C 1.0602(4) 0.4145(3) 0.1525(2) 0.0661(8) Uani 1 1 d . . . H43A H 1.1073 0.4454 0.2137 0.079 Uiso 1 1 calc R . . C42 C 0.9383(4) 0.4342(3) 0.1144(3) 0.0744(10) Uani 1 1 d . . . H42A H 0.8988 0.4784 0.1487 0.089 Uiso 1 1 calc R . . C41 C 0.8711(3) 0.3894(3) 0.0250(3) 0.0806(11) Uani 1 1 d . . . H41A H 0.7848 0.4026 -0.0023 0.097 Uiso 1 1 calc R . . C40 C 0.9294(3) 0.3253(3) -0.0250(2) 0.0639(8) Uani 1 1 d . . . H40A H 0.8840 0.2954 -0.0867 0.077 Uiso 1 1 calc R . . C39 C 1.0512(3) 0.3062(3) 0.0152(2) 0.0606(7) Uani 1 1 d . . . H39A H 1.0919 0.2619 -0.0181 0.073 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 0.01749(5) 0.01754(6) 0.01835(5) 0.00098(3) 0.00451(4) 0.00118(4) Cl1 0.02120(17) 0.0370(2) 0.0394(2) 0.00855(17) 0.01126(16) 0.00245(15) P1 0.01997(17) 0.01727(17) 0.02101(16) 0.00116(13) 0.00357(14) 0.00028(13) P2 0.01890(16) 0.01808(17) 0.01901(16) 0.00111(12) 0.00486(13) 0.00291(13) N1 0.0202(6) 0.0173(6) 0.0273(6) 0.0031(5) 0.0085(5) 0.0034(4) C1 0.0203(6) 0.0197(7) 0.0196(6) -0.0009(5) 0.0039(5) 0.0022(5) C2 0.0205(7) 0.0244(8) 0.0310(8) 0.0017(6) 0.0031(6) 0.0011(6) C3 0.0199(7) 0.0329(9) 0.0331(8) 0.0037(7) 0.0009(6) 0.0052(6) C4 0.0277(8) 0.0261(8) 0.0283(8) 0.0024(6) 0.0027(6) 0.0089(6) C5 0.0335(10) 0.0340(10) 0.0484(11) 0.0088(8) 0.0063(9) 0.0143(8) C6 0.0267(7) 0.0207(7) 0.0276(7) 0.0019(6) 0.0050(6) 0.0037(6) C7 0.0210(6) 0.0188(7) 0.0219(6) 0.0001(5) 0.0039(5) 0.0014(5) C8 0.0242(7) 0.0220(7) 0.0239(7) -0.0001(5) 0.0034(6) -0.0007(6) C9 0.0372(10) 0.0471(12) 0.0358(10) -0.0153(9) -0.0023(8) 0.0148(9) C10 0.0480(13) 0.0537(14) 0.0384(11) -0.0191(10) 0.0023(10) 0.0153(11) C11 0.0450(11) 0.0418(11) 0.0251(8) -0.0075(7) 0.0055(8) -0.0008(9) C12 0.0363(10) 0.0442(12) 0.0302(9) -0.0029(8) -0.0041(8) 0.0049(9) C13 0.0316(9) 0.0349(10) 0.0284(8) -0.0025(7) 0.0006(7) 0.0076(7) C14 0.0257(7) 0.0203(7) 0.0273(7) 0.0040(5) 0.0078(6) 0.0015(6) C15 0.0381(10) 0.0344(10) 0.0355(9) 0.0002(7) 0.0122(8) -0.0109(8) C16 0.0477(12) 0.0354(11) 0.0517(12) 0.0027(9) 0.0249(10) -0.0114(9) C17 0.0543(13) 0.0355(10) 0.0453(11) 0.0138(8) 0.0288(10) 0.0072(9) C18 0.0436(11) 0.0442(11) 0.0314(9) 0.0124(8) 0.0166(8) 0.0118(9) C19 0.0307(9) 0.0375(10) 0.0275(8) 0.0049(7) 0.0088(7) 0.0010(7) C20 0.0181(6) 0.0210(7) 0.0196(6) 0.0010(5) 0.0042(5) 0.0012(5) C21 0.0227(7) 0.0284(8) 0.0249(7) 0.0028(6) 0.0094(6) 0.0035(6) C22 0.0215(7) 0.0371(9) 0.0265(7) 0.0074(6) 0.0085(6) 0.0016(6) C23 0.0251(7) 0.0296(8) 0.0286(8) 0.0101(6) 0.0069(6) -0.0008(6) C24 0.0384(10) 0.0383(11) 0.0552(13) 0.0198(9) 0.0198(10) -0.0006(9) C25 0.0255(7) 0.0233(7) 0.0293(7) 0.0067(6) 0.0087(6) 0.0032(6) C26 0.0215(6) 0.0199(7) 0.0214(6) 0.0025(5) 0.0064(5) 0.0020(5) C27 0.0217(7) 0.0221(7) 0.0219(6) 0.0019(5) 0.0041(5) 0.0045(5) C28 0.0279(8) 0.0392(10) 0.0212(7) 0.0009(6) 0.0051(6) 0.0069(7) C29 0.0359(10) 0.0499(12) 0.0260(8) 0.0087(8) 0.0012(7) 0.0092(9) C30 0.0285(9) 0.0457(12) 0.0350(9) 0.0016(8) -0.0022(7) 0.0101(8) C31 0.0297(9) 0.0406(11) 0.0363(9) -0.0026(8) 0.0025(8) 0.0147(8) C32 0.0252(8) 0.0348(9) 0.0268(7) 0.0018(6) 0.0073(6) 0.0104(7) C33 0.0222(7) 0.0213(7) 0.0207(6) 0.0003(5) 0.0042(5) 0.0040(5) C34 0.0416(10) 0.0196(7) 0.0271(8) 0.0001(6) -0.0002(7) 0.0040(7) C35 0.0558(13) 0.0245(9) 0.0315(9) -0.0059(7) -0.0033(9) 0.0071(8) C36 0.0482(12) 0.0298(10) 0.0307(9) -0.0033(7) -0.0089(8) 0.0011(8) C37 0.0437(11) 0.0298(9) 0.0241(8) 0.0024(6) -0.0014(7) 0.0078(8) C38 0.0272(8) 0.0226(7) 0.0251(7) 0.0028(5) 0.0028(6) 0.0060(6) C44 0.0496(15) 0.078(2) 0.0592(16) 0.0223(15) 0.0159(13) -0.0045(14) C43 0.091(2) 0.0581(17) 0.0465(14) 0.0050(12) 0.0221(15) -0.0123(16) C42 0.105(3) 0.0445(16) 0.094(3) 0.0184(16) 0.055(2) 0.0237(17) C41 0.0564(18) 0.063(2) 0.117(3) 0.050(2) 0.0131(19) 0.0178(15) C40 0.079(2) 0.0496(15) 0.0494(14) 0.0188(12) 0.0049(14) -0.0095(14) C39 0.080(2) 0.0586(17) 0.0512(14) 0.0132(12) 0.0313(15) 0.0035(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 Pd1 N1 2.0229(13) . ? Pd1 P1 2.2843(4) . ? Pd1 P2 2.3046(4) . ? Pd1 Cl1 2.3171(4) . ? P1 C7 1.7977(16) . ? P1 C8 1.8122(17) . ? P1 C14 1.8141(17) . ? P2 C26 1.8079(16) . ? P2 C27 1.8341(16) . ? P2 C33 1.8453(16) . ? N1 C1 1.390(2) . ? N1 C20 1.398(2) . ? C1 C2 1.410(2) . ? C1 C7 1.411(2) . ? C2 C3 1.380(2) . ? C2 H2A 0.9500 . ? C3 C4 1.400(3) . ? C3 H3A 0.9500 . ? C4 C6 1.382(2) . ? C4 C5 1.503(3) . ? C5 H5A 0.9931 . ? C5 H5B 0.9554 . ? C5 H5C 0.9207 . ? C6 C7 1.400(2) . ? C6 H6A 0.9500 . ? C8 C9 1.378(3) . ? C8 C13 1.393(2) . ? C9 C10 1.393(3) . ? C9 H9A 0.9500 . ? C10 C11 1.374(3) . ? C10 H10A 0.9500 . ? C11 C12 1.370(3) . ? C11 H11A 0.9500 . ? C12 C13 1.391(3) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C15 1.393(2) . ? C14 C19 1.394(2) . ? C15 C16 1.390(3) . ? C15 H15A 0.9500 . ? C16 C17 1.385(3) . ? C16 H16A 0.9500 . ? C17 C18 1.378(3) . ? C17 H17A 0.9500 . ? C18 C19 1.389(3) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 C26 1.405(2) . ? C20 C21 1.409(2) . ? C21 C22 1.384(2) . ? C21 H21A 0.9500 . ? C22 C23 1.393(3) . ? C22 H22A 0.9500 . ? C23 C25 1.392(2) . ? C23 C24 1.500(3) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.396(2) . ? C25 H25A 0.9500 . ? C27 C28 1.532(2) . ? C27 C32 1.536(2) . ? C27 H27A 1.0000 . ? C28 C29 1.528(3) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.519(3) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.518(3) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.530(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C38 1.532(2) . ? C33 C34 1.533(2) . ? C33 H33A 1.0000 . ? C34 C35 1.532(3) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.517(3) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.514(3) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.533(2) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C44 C43 1.361(5) . ? C44 C39 1.362(4) . ? C44 H44A 0.9500 . ? C43 C42 1.345(5) . ? C43 H43A 0.9500 . ? C42 C41 1.382(6) . ? C42 H42A 0.9500 . ? C41 C40 1.389(5) . ? C41 H41A 0.9500 . ? C40 C39 1.345(5) . ? C40 H40A 0.9500 . ? C39 H39A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 P1 82.72(4) . . ? N1 Pd1 P2 82.65(4) . . ? P1 Pd1 P2 164.233(16) . . ? N1 Pd1 Cl1 176.23(4) . . ? P1 Pd1 Cl1 95.239(16) . . ? P2 Pd1 Cl1 99.685(16) . . ? C7 P1 C8 108.22(8) . . ? C7 P1 C14 106.72(8) . . ? C8 P1 C14 105.94(8) . . ? C7 P1 Pd1 99.32(5) . . ? C8 P1 Pd1 117.62(6) . . ? C14 P1 Pd1 118.01(6) . . ? C26 P2 C27 106.92(7) . . ? C26 P2 C33 106.82(7) . . ? C27 P2 C33 107.49(7) . . ? C26 P2 Pd1 98.61(5) . . ? C27 P2 Pd1 121.46(5) . . ? C33 P2 Pd1 114.05(5) . . ? C1 N1 C20 123.03(13) . . ? C1 N1 Pd1 118.86(10) . . ? C20 N1 Pd1 118.05(10) . . ? N1 C1 C2 124.74(15) . . ? N1 C1 C7 118.66(14) . . ? C2 C1 C7 116.50(14) . . ? C3 C2 C1 121.04(16) . . ? C3 C2 H2A 119.5 . . ? C1 C2 H2A 119.5 . . ? C2 C3 C4 122.65(16) . . ? C2 C3 H3A 118.7 . . ? C4 C3 H3A 118.7 . . ? C6 C4 C3 116.65(16) . . ? C6 C4 C5 121.76(17) . . ? C3 C4 C5 121.56(17) . . ? C4 C5 H5A 106.3 . . ? C4 C5 H5B 109.6 . . ? H5A C5 H5B 107.1 . . ? C4 C5 H5C 110.2 . . ? H5A C5 H5C 109.9 . . ? H5B C5 H5C 113.3 . . ? C4 C6 C7 122.01(16) . . ? C4 C6 H6A 119.0 . . ? C7 C6 H6A 119.0 . . ? C6 C7 C1 121.14(15) . . ? C6 C7 P1 124.35(12) . . ? C1 C7 P1 114.47(12) . . ? C9 C8 C13 119.13(16) . . ? C9 C8 P1 121.70(14) . . ? C13 C8 P1 119.16(14) . . ? C8 C9 C10 120.4(2) . . ? C8 C9 H9A 119.8 . . ? C10 C9 H9A 119.8 . . ? C11 C10 C9 120.3(2) . . ? C11 C10 H10A 119.8 . . ? C9 C10 H10A 119.8 . . ? C12 C11 C10 119.66(18) . . ? C12 C11 H11A 120.2 . . ? C10 C11 H11A 120.2 . . ? C11 C12 C13 120.70(19) . . ? C11 C12 H12A 119.7 . . ? C13 C12 H12A 119.7 . . ? C12 C13 C8 119.81(19) . . ? C12 C13 H13A 120.1 . . ? C8 C13 H13A 120.1 . . ? C15 C14 C19 119.27(17) . . ? C15 C14 P1 120.76(14) . . ? C19 C14 P1 119.71(13) . . ? C16 C15 C14 119.75(19) . . ? C16 C15 H15A 120.1 . . ? C14 C15 H15A 120.1 . . ? C17 C16 C15 120.4(2) . . ? C17 C16 H16A 119.8 . . ? C15 C16 H16A 119.8 . . ? C18 C17 C16 120.22(19) . . ? C18 C17 H17A 119.9 . . ? C16 C17 H17A 119.9 . . ? C17 C18 C19 119.79(19) . . ? C17 C18 H18A 120.1 . . ? C19 C18 H18A 120.1 . . ? C18 C19 C14 120.53(18) . . ? C18 C19 H19A 119.7 . . ? C14 C19 H19A 119.7 . . ? N1 C20 C26 118.60(13) . . ? N1 C20 C21 124.05(14) . . ? C26 C20 C21 117.24(14) . . ? C22 C21 C20 120.64(16) . . ? C22 C21 H21A 119.7 . . ? C20 C21 H21A 119.7 . . ? C21 C22 C23 122.38(16) . . ? C21 C22 H22A 118.8 . . ? C23 C22 H22A 118.8 . . ? C25 C23 C22 116.95(16) . . ? C25 C23 C24 121.38(18) . . ? C22 C23 C24 121.64(17) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 C26 121.74(16) . . ? C23 C25 H25A 119.1 . . ? C26 C25 H25A 119.1 . . ? C25 C26 C20 120.78(15) . . ? C25 C26 P2 124.34(13) . . ? C20 C26 P2 114.84(11) . . ? C28 C27 C32 111.02(14) . . ? C28 C27 P2 109.39(12) . . ? C32 C27 P2 111.18(11) . . ? C28 C27 H27A 108.4 . . ? C32 C27 H27A 108.4 . . ? P2 C27 H27A 108.4 . . ? C29 C28 C27 111.25(15) . . ? C29 C28 H28A 109.4 . . ? C27 C28 H28A 109.4 . . ? C29 C28 H28B 109.4 . . ? C27 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C30 C29 C28 111.17(17) . . ? C30 C29 H29A 109.4 . . ? C28 C29 H29A 109.4 . . ? C30 C29 H29B 109.4 . . ? C28 C29 H29B 109.4 . . ? H29A C29 H29B 108.0 . . ? C31 C30 C29 110.61(17) . . ? C31 C30 H30A 109.5 . . ? C29 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 108.1 . . ? C30 C31 C32 111.78(16) . . ? C30 C31 H31A 109.3 . . ? C32 C31 H31A 109.3 . . ? C30 C31 H31B 109.3 . . ? C32 C31 H31B 109.3 . . ? H31A C31 H31B 107.9 . . ? C31 C32 C27 111.25(15) . . ? C31 C32 H32A 109.4 . . ? C27 C32 H32A 109.4 . . ? C31 C32 H32B 109.4 . . ? C27 C32 H32B 109.4 . . ? H32A C32 H32B 108.0 . . ? C38 C33 C34 110.73(14) . . ? C38 C33 P2 109.64(11) . . ? C34 C33 P2 114.13(11) . . ? C38 C33 H33A 107.3 . . ? C34 C33 H33A 107.3 . . ? P2 C33 H33A 107.3 . . ? C35 C34 C33 110.79(16) . . ? C35 C34 H34A 109.5 . . ? C33 C34 H34A 109.5 . . ? C35 C34 H34B 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? C36 C35 C34 111.70(17) . . ? C36 C35 H35A 109.3 . . ? C34 C35 H35A 109.3 . . ? C36 C35 H35B 109.3 . . ? C34 C35 H35B 109.3 . . ? H35A C35 H35B 107.9 . . ? C37 C36 C35 111.45(17) . . ? C37 C36 H36A 109.3 . . ? C35 C36 H36A 109.3 . . ? C37 C36 H36B 109.3 . . ? C35 C36 H36B 109.3 . . ? H36A C36 H36B 108.0 . . ? C36 C37 C38 111.69(16) . . ? C36 C37 H37A 109.3 . . ? C38 C37 H37A 109.3 . . ? C36 C37 H37B 109.3 . . ? C38 C37 H37B 109.3 . . ? H37A C37 H37B 107.9 . . ? C33 C38 C37 110.73(14) . . ? C33 C38 H38A 109.5 . . ? C37 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 108.1 . . ? C43 C44 C39 121.0(3) . . ? C43 C44 H44A 119.5 . . ? C39 C44 H44A 119.5 . . ? C42 C43 C44 120.2(3) . . ? C42 C43 H43A 119.9 . . ? C44 C43 H43A 119.9 . . ? C43 C42 C41 119.3(3) . . ? C43 C42 H42A 120.3 . . ? C41 C42 H42A 120.3 . . ? C42 C41 C40 120.1(3) . . ? C42 C41 H41A 119.9 . . ? C40 C41 H41A 119.9 . . ? C39 C40 C41 119.2(3) . . ? C39 C40 H40A 120.4 . . ? C41 C40 H40A 120.4 . . ? C40 C39 C44 120.1(3) . . ? C40 C39 H39A 119.9 . . ? C44 C39 H39A 119.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Pd1 P1 C7 -18.60(7) . . . . ? P2 Pd1 P1 C7 3.42(8) . . . . ? Cl1 Pd1 P1 C7 164.59(5) . . . . ? N1 Pd1 P1 C8 97.72(8) . . . . ? P2 Pd1 P1 C8 119.74(8) . . . . ? Cl1 Pd1 P1 C8 -79.09(7) . . . . ? N1 Pd1 P1 C14 -133.28(7) . . . . ? P2 Pd1 P1 C14 -111.26(8) . . . . ? Cl1 Pd1 P1 C14 49.91(6) . . . . ? N1 Pd1 P2 C26 -19.17(6) . . . . ? P1 Pd1 P2 C26 -41.20(8) . . . . ? Cl1 Pd1 P2 C26 157.83(5) . . . . ? N1 Pd1 P2 C27 -135.13(7) . . . . ? P1 Pd1 P2 C27 -157.15(7) . . . . ? Cl1 Pd1 P2 C27 41.87(6) . . . . ? N1 Pd1 P2 C33 93.66(7) . . . . ? P1 Pd1 P2 C33 71.64(8) . . . . ? Cl1 Pd1 P2 C33 -89.33(6) . . . . ? P1 Pd1 N1 C1 23.13(11) . . . . ? P2 Pd1 N1 C1 -150.98(11) . . . . ? Cl1 Pd1 N1 C1 80.6(6) . . . . ? P1 Pd1 N1 C20 -159.66(11) . . . . ? P2 Pd1 N1 C20 26.24(11) . . . . ? Cl1 Pd1 N1 C20 -102.2(6) . . . . ? C20 N1 C1 C2 -19.8(2) . . . . ? Pd1 N1 C1 C2 157.28(13) . . . . ? C20 N1 C1 C7 164.12(14) . . . . ? Pd1 N1 C1 C7 -18.81(18) . . . . ? N1 C1 C2 C3 -176.81(16) . . . . ? C7 C1 C2 C3 -0.6(2) . . . . ? C1 C2 C3 C4 0.1(3) . . . . ? C2 C3 C4 C6 0.7(3) . . . . ? C2 C3 C4 C5 178.96(19) . . . . ? C3 C4 C6 C7 -0.9(3) . . . . ? C5 C4 C6 C7 -179.15(17) . . . . ? C4 C6 C7 C1 0.3(3) . . . . ? C4 C6 C7 P1 177.99(14) . . . . ? N1 C1 C7 C6 176.86(15) . . . . ? C2 C1 C7 C6 0.5(2) . . . . ? N1 C1 C7 P1 -1.00(18) . . . . ? C2 C1 C7 P1 -177.41(12) . . . . ? C8 P1 C7 C6 74.95(15) . . . . ? C14 P1 C7 C6 -38.68(16) . . . . ? Pd1 P1 C7 C6 -161.78(13) . . . . ? C8 P1 C7 C1 -107.27(12) . . . . ? C14 P1 C7 C1 139.11(12) . . . . ? Pd1 P1 C7 C1 16.01(12) . . . . ? C7 P1 C8 C9 -27.9(2) . . . . ? C14 P1 C8 C9 86.29(19) . . . . ? Pd1 P1 C8 C9 -139.24(17) . . . . ? C7 P1 C8 C13 151.36(15) . . . . ? C14 P1 C8 C13 -94.50(16) . . . . ? Pd1 P1 C8 C13 39.97(17) . . . . ? C13 C8 C9 C10 0.3(4) . . . . ? P1 C8 C9 C10 179.5(2) . . . . ? C8 C9 C10 C11 0.2(4) . . . . ? C9 C10 C11 C12 -0.9(4) . . . . ? C10 C11 C12 C13 1.1(4) . . . . ? C11 C12 C13 C8 -0.6(3) . . . . ? C9 C8 C13 C12 -0.1(3) . . . . ? P1 C8 C13 C12 -179.29(17) . . . . ? C7 P1 C14 C15 147.70(16) . . . . ? C8 P1 C14 C15 32.53(18) . . . . ? Pd1 P1 C14 C15 -101.74(16) . . . . ? C7 P1 C14 C19 -38.26(17) . . . . ? C8 P1 C14 C19 -153.43(15) . . . . ? Pd1 P1 C14 C19 72.31(16) . . . . ? C19 C14 C15 C16 2.5(3) . . . . ? P1 C14 C15 C16 176.55(17) . . . . ? C14 C15 C16 C17 -1.1(4) . . . . ? C15 C16 C17 C18 -0.1(4) . . . . ? C16 C17 C18 C19 -0.1(3) . . . . ? C17 C18 C19 C14 1.5(3) . . . . ? C15 C14 C19 C18 -2.7(3) . . . . ? P1 C14 C19 C18 -176.82(16) . . . . ? C1 N1 C20 C26 152.82(15) . . . . ? Pd1 N1 C20 C26 -24.27(18) . . . . ? C1 N1 C20 C21 -31.1(2) . . . . ? Pd1 N1 C20 C21 151.83(13) . . . . ? N1 C20 C21 C22 179.47(15) . . . . ? C26 C20 C21 C22 -4.4(2) . . . . ? C20 C21 C22 C23 -0.1(3) . . . . ? C21 C22 C23 C25 3.8(3) . . . . ? C21 C22 C23 C24 -178.06(18) . . . . ? C22 C23 C25 C26 -2.9(3) . . . . ? C24 C23 C25 C26 178.95(18) . . . . ? C23 C25 C26 C20 -1.6(3) . . . . ? C23 C25 C26 P2 176.22(13) . . . . ? N1 C20 C26 C25 -178.40(14) . . . . ? C21 C20 C26 C25 5.2(2) . . . . ? N1 C20 C26 P2 3.56(19) . . . . ? C21 C20 C26 P2 -172.81(12) . . . . ? C27 P2 C26 C25 -37.13(16) . . . . ? C33 P2 C26 C25 77.71(15) . . . . ? Pd1 P2 C26 C25 -163.84(13) . . . . ? C27 P2 C26 C20 140.83(12) . . . . ? C33 P2 C26 C20 -104.32(12) . . . . ? Pd1 P2 C26 C20 14.12(12) . . . . ? C26 P2 C27 C28 -64.98(13) . . . . ? C33 P2 C27 C28 -179.38(12) . . . . ? Pd1 P2 C27 C28 46.70(14) . . . . ? C26 P2 C27 C32 172.05(12) . . . . ? C33 P2 C27 C32 57.65(14) . . . . ? Pd1 P2 C27 C32 -76.27(12) . . . . ? C32 C27 C28 C29 -54.6(2) . . . . ? P2 C27 C28 C29 -177.69(14) . . . . ? C27 C28 C29 C30 56.5(2) . . . . ? C28 C29 C30 C31 -57.0(2) . . . . ? C29 C30 C31 C32 56.4(3) . . . . ? C30 C31 C32 C27 -55.0(2) . . . . ? C28 C27 C32 C31 53.7(2) . . . . ? P2 C27 C32 C31 175.76(13) . . . . ? C26 P2 C33 C38 61.61(13) . . . . ? C27 P2 C33 C38 176.07(11) . . . . ? Pd1 P2 C33 C38 -46.21(13) . . . . ? C26 P2 C33 C34 -63.26(14) . . . . ? C27 P2 C33 C34 51.20(15) . . . . ? Pd1 P2 C33 C34 -171.09(11) . . . . ? C38 C33 C34 C35 56.0(2) . . . . ? P2 C33 C34 C35 -179.73(14) . . . . ? C33 C34 C35 C36 -55.4(3) . . . . ? C34 C35 C36 C37 54.9(3) . . . . ? C35 C36 C37 C38 -55.1(3) . . . . ? C34 C33 C38 C37 -56.1(2) . . . . ? P2 C33 C38 C37 177.12(13) . . . . ? C36 C37 C38 C33 55.7(2) . . . . ? C39 C44 C43 C42 0.8(5) . . . . ? C44 C43 C42 C41 -0.5(5) . . . . ? C43 C42 C41 C40 -0.3(5) . . . . ? C42 C41 C40 C39 0.9(5) . . . . ? C41 C40 C39 C44 -0.6(4) . . . . ? C43 C44 C39 C40 -0.2(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 34.34 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.757 _refine_diff_density_min -0.738 _refine_diff_density_rms 0.146 # Attachment 'Compound 5.cif' data_rkrl23m _database_code_depnum_ccdc_archive 'CCDC 812752' #TrackingRef 'Compound 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H39 Cl N P2 Pt' _chemical_formula_weight 766.15 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.7018(3) _cell_length_b 11.5256(4) _cell_length_c 28.4989(10) _cell_angle_alpha 90.00 _cell_angle_beta 100.733(2) _cell_angle_gamma 90.00 _cell_volume 3130.97(18) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 9892 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 28.21 _exptl_crystal_description chip _exptl_crystal_colour orange _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1524 _exptl_absorpt_coefficient_mu 4.694 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4433 _exptl_absorpt_correction_T_max 0.7724 _exptl_absorpt_process_details Bruker,SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 47085 _diffrn_reflns_av_R_equivalents 0.0764 _diffrn_reflns_av_sigmaI/netI 0.0565 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 28.45 _reflns_number_total 7789 _reflns_number_gt 6167 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics '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^)+(0.0123P)^2^+3.5346P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7789 _refine_ls_number_parameters 367 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0501 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0656 _refine_ls_wR_factor_gt 0.0601 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.113243(14) 0.718640(12) 0.128698(5) 0.01785(5) Uani 1 1 d . . . Cl1 Cl 0.35329(10) 0.72246(9) 0.13029(4) 0.0340(2) Uani 1 1 d . . . P1 P 0.09657(9) 0.52145(8) 0.13260(3) 0.0188(2) Uani 1 1 d . . . P2 P 0.08018(10) 0.91247(9) 0.13632(3) 0.0205(2) Uani 1 1 d . . . N1 N -0.0969(3) 0.7154(3) 0.12637(10) 0.0189(6) Uani 1 1 d . . . C1 C -0.0800(3) 0.5100(3) 0.14371(12) 0.0180(7) Uani 1 1 d . . . C2 C -0.1390(4) 0.4071(3) 0.15590(13) 0.0233(8) Uani 1 1 d . . . H2 H -0.0880 0.3370 0.1550 0.028 Uiso 1 1 calc R . . C3 C -0.2685(4) 0.4023(4) 0.16923(14) 0.0268(9) Uani 1 1 d . . . C4 C -0.3366(4) 0.5093(4) 0.17174(13) 0.0266(9) Uani 1 1 d . . . H4 H -0.4228 0.5107 0.1830 0.032 Uiso 1 1 calc R . . C5 C -0.2830(4) 0.6113(3) 0.15846(13) 0.0227(8) Uani 1 1 d . . . H5 H -0.3332 0.6813 0.1605 0.027 Uiso 1 1 calc R . . C6 C -0.1561(4) 0.6148(3) 0.14198(12) 0.0196(8) Uani 1 1 d . . . C7 C -0.3306(5) 0.2906(4) 0.18296(18) 0.0406(11) Uani 1 1 d . . . H7A H -0.2762 0.2251 0.1742 0.061 Uiso 1 1 calc R . . H7B H -0.4280 0.2843 0.1661 0.061 Uiso 1 1 calc R . . H7C H -0.3279 0.2897 0.2175 0.061 Uiso 1 1 calc R . . C8 C -0.1043(4) 0.9210(3) 0.11096(13) 0.0217(8) Uani 1 1 d . . . C9 C -0.1745(4) 1.0223(3) 0.09361(13) 0.0266(9) Uani 1 1 d . . . H9 H -0.1239 1.0932 0.0953 0.032 Uiso 1 1 calc R . . C10 C -0.3164(4) 1.0216(4) 0.07399(14) 0.0309(9) Uani 1 1 d . . . C11 C -0.3852(4) 0.9167(4) 0.07315(13) 0.0293(9) Uani 1 1 d . . . H11 H -0.4827 0.9141 0.0602 0.035 Uiso 1 1 calc R . . C12 C -0.3184(4) 0.8148(3) 0.09034(14) 0.0247(9) Uani 1 1 d . . . H12 H -0.3703 0.7445 0.0884 0.030 Uiso 1 1 calc R . . C13 C -0.1758(4) 0.8143(3) 0.11043(12) 0.0195(8) Uani 1 1 d . . . C14 C -0.3899(5) 1.1312(4) 0.05391(18) 0.0457(12) Uani 1 1 d . . . H14A H -0.4103 1.1794 0.0801 0.068 Uiso 1 1 calc R . . H14B H -0.4778 1.1111 0.0325 0.068 Uiso 1 1 calc R . . H14C H -0.3293 1.1742 0.0361 0.068 Uiso 1 1 calc R . . C15 C 0.1089(4) 0.4246(3) 0.08325(13) 0.0217(8) Uani 1 1 d . . . C16 C 0.2362(4) 0.3875(4) 0.07493(14) 0.0307(10) Uani 1 1 d . . . H16 H 0.3198 0.4085 0.0963 0.037 Uiso 1 1 calc R . . C17 C 0.2437(5) 0.3192(4) 0.03526(16) 0.0383(11) Uani 1 1 d . . . H17 H 0.3323 0.2929 0.0299 0.046 Uiso 1 1 calc R . . C18 C 0.1249(5) 0.2897(4) 0.00403(16) 0.0409(11) Uani 1 1 d . . . H18 H 0.1305 0.2420 -0.0227 0.049 Uiso 1 1 calc R . . C19 C -0.0013(5) 0.3285(5) 0.01125(17) 0.0542(15) Uani 1 1 d . . . H19 H -0.0838 0.3091 -0.0109 0.065 Uiso 1 1 calc R . . C20 C -0.0112(5) 0.3960(4) 0.05046(15) 0.0412(12) Uani 1 1 d . . . H20 H -0.1003 0.4229 0.0551 0.049 Uiso 1 1 calc R . . C21 C 0.2146(4) 0.4612(3) 0.18451(12) 0.0198(8) Uani 1 1 d . . . C22 C 0.2469(4) 0.3437(4) 0.18918(14) 0.0260(8) Uani 1 1 d . . . H22 H 0.2102 0.2915 0.1642 0.031 Uiso 1 1 calc R . . C23 C 0.3325(5) 0.3026(4) 0.23017(15) 0.0327(10) Uani 1 1 d . . . H23 H 0.3539 0.2222 0.2331 0.039 Uiso 1 1 calc R . . C24 C 0.3867(4) 0.3771(4) 0.26663(14) 0.0333(10) Uani 1 1 d . . . H24 H 0.4446 0.3483 0.2948 0.040 Uiso 1 1 calc R . . C25 C 0.3567(4) 0.4929(4) 0.26205(15) 0.0360(10) Uani 1 1 d . . . H25 H 0.3954 0.5447 0.2870 0.043 Uiso 1 1 calc R . . C26 C 0.2705(4) 0.5357(4) 0.22142(14) 0.0321(10) Uani 1 1 d . . . H26 H 0.2496 0.6162 0.2188 0.038 Uiso 1 1 calc R . . C27 C 0.0938(4) 0.9546(3) 0.19935(13) 0.0272(9) Uani 1 1 d . . . H27 H 0.1948 0.9504 0.2150 0.033 Uiso 1 1 calc R . . C28 C 0.0128(5) 0.8681(4) 0.22406(14) 0.0375(11) Uani 1 1 d . . . H28A H 0.0180 0.8913 0.2574 0.056 Uiso 1 1 calc R . . H28B H 0.0538 0.7907 0.2229 0.056 Uiso 1 1 calc R . . H28C H -0.0855 0.8666 0.2078 0.056 Uiso 1 1 calc R . . C29 C 0.0420(5) 1.0776(4) 0.20580(17) 0.0428(12) Uani 1 1 d . . . H29A H -0.0588 1.0823 0.1929 0.064 Uiso 1 1 calc R . . H29B H 0.0923 1.1324 0.1888 0.064 Uiso 1 1 calc R . . H29C H 0.0593 1.0972 0.2399 0.064 Uiso 1 1 calc R . . C30 C 0.1727(4) 1.0203(4) 0.10635(14) 0.0289(9) Uani 1 1 d . . . H30 H 0.1195 1.0950 0.1047 0.035 Uiso 1 1 calc R . . C31 C 0.1726(5) 0.9794(4) 0.05521(15) 0.0428(12) Uani 1 1 d . . . H31A H 0.2164 1.0387 0.0382 0.064 Uiso 1 1 calc R . . H31B H 0.0759 0.9664 0.0387 0.064 Uiso 1 1 calc R . . H31C H 0.2256 0.9068 0.0560 0.064 Uiso 1 1 calc R . . C32 C 0.3202(4) 1.0418(4) 0.13369(17) 0.0397(11) Uani 1 1 d . . . H32A H 0.3737 0.9692 0.1361 0.060 Uiso 1 1 calc R . . H32B H 0.3159 1.0702 0.1658 0.060 Uiso 1 1 calc R . . H32C H 0.3664 1.0999 0.1168 0.060 Uiso 1 1 calc R . . C33 C 0.5919(5) 0.4579(4) 0.03880(16) 0.0410(11) Uani 1 1 d . . . H33 H 0.6556 0.4286 0.0656 0.049 Uiso 1 1 calc R . . C34 C 0.4966(5) 0.5422(4) 0.04483(15) 0.0378(11) Uani 1 1 d . . . H34 H 0.4940 0.5715 0.0758 0.045 Uiso 1 1 calc R . . C35 C 0.4055(5) 0.5835(4) 0.00607(17) 0.0421(11) Uani 1 1 d . . . H35 H 0.3395 0.6417 0.0103 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 Pt1 0.01521(7) 0.01661(8) 0.02180(7) -0.00150(6) 0.00363(5) 0.00056(6) Cl1 0.0179(4) 0.0306(6) 0.0549(6) -0.0050(5) 0.0106(4) -0.0005(4) P1 0.0180(5) 0.0176(5) 0.0206(5) -0.0019(4) 0.0030(4) 0.0017(4) P2 0.0194(5) 0.0171(5) 0.0249(5) -0.0013(4) 0.0037(4) -0.0004(4) N1 0.0162(15) 0.0173(15) 0.0227(15) -0.0016(13) 0.0021(12) 0.0021(14) C1 0.0151(17) 0.021(2) 0.0173(17) -0.0014(14) 0.0020(13) -0.0005(15) C2 0.0228(19) 0.023(2) 0.0242(19) 0.0017(16) 0.0036(15) 0.0020(17) C3 0.026(2) 0.027(2) 0.027(2) 0.0034(17) 0.0050(16) -0.0033(18) C4 0.0183(19) 0.038(3) 0.0242(19) 0.0017(18) 0.0071(15) -0.0005(18) C5 0.0170(18) 0.021(2) 0.030(2) -0.0019(16) 0.0044(15) 0.0020(16) C6 0.0193(18) 0.022(2) 0.0175(17) -0.0037(15) 0.0041(14) -0.0007(16) C7 0.037(3) 0.033(3) 0.055(3) 0.009(2) 0.016(2) -0.008(2) C8 0.0233(19) 0.0197(19) 0.0217(18) -0.0021(15) 0.0034(15) 0.0032(16) C9 0.028(2) 0.021(2) 0.030(2) 0.0021(16) 0.0018(17) 0.0025(17) C10 0.029(2) 0.030(2) 0.034(2) 0.0056(18) 0.0045(18) 0.0093(19) C11 0.022(2) 0.037(2) 0.029(2) 0.0014(18) 0.0022(16) 0.0057(19) C12 0.0175(19) 0.026(2) 0.030(2) -0.0009(16) 0.0032(16) -0.0013(16) C13 0.0180(18) 0.020(2) 0.0207(18) -0.0029(14) 0.0034(14) 0.0025(15) C14 0.041(3) 0.039(3) 0.055(3) 0.011(2) 0.002(2) 0.016(2) C15 0.027(2) 0.0177(19) 0.0214(18) -0.0001(15) 0.0075(15) -0.0016(16) C16 0.025(2) 0.036(3) 0.034(2) -0.0032(19) 0.0109(17) -0.0006(19) C17 0.038(3) 0.039(3) 0.043(3) -0.006(2) 0.020(2) 0.007(2) C18 0.055(3) 0.041(3) 0.030(2) -0.015(2) 0.018(2) 0.000(2) C19 0.041(3) 0.083(4) 0.037(3) -0.032(3) 0.003(2) -0.010(3) C20 0.028(2) 0.060(3) 0.035(2) -0.021(2) 0.0048(18) 0.002(2) C21 0.0154(17) 0.021(2) 0.0236(18) 0.0006(15) 0.0039(14) 0.0028(15) C22 0.029(2) 0.020(2) 0.028(2) 0.0028(17) 0.0045(16) 0.0029(18) C23 0.038(2) 0.025(2) 0.035(2) 0.0066(18) 0.0062(19) 0.0051(19) C24 0.031(2) 0.037(3) 0.029(2) 0.0097(19) -0.0019(17) 0.005(2) C25 0.038(2) 0.036(3) 0.030(2) -0.0078(19) -0.0038(19) 0.004(2) C26 0.035(2) 0.024(2) 0.034(2) -0.0023(18) -0.0025(18) 0.0053(19) C27 0.028(2) 0.027(2) 0.026(2) -0.0104(17) 0.0023(16) -0.0020(18) C28 0.047(3) 0.043(3) 0.025(2) -0.0038(19) 0.0109(19) -0.002(2) C29 0.051(3) 0.030(3) 0.049(3) -0.014(2) 0.014(2) -0.004(2) C30 0.026(2) 0.024(2) 0.038(2) 0.0047(18) 0.0094(18) -0.0030(18) C31 0.044(3) 0.050(3) 0.036(2) 0.013(2) 0.011(2) -0.009(2) C32 0.032(2) 0.034(3) 0.055(3) -0.002(2) 0.012(2) -0.007(2) C33 0.035(2) 0.049(3) 0.034(2) 0.011(2) -0.0049(19) -0.002(2) C34 0.041(3) 0.039(3) 0.032(2) -0.007(2) 0.004(2) -0.015(2) C35 0.039(3) 0.036(3) 0.051(3) 0.004(2) 0.010(2) 0.007(2) _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 Pt1 N1 2.028(3) . ? Pt1 P2 2.2730(10) . ? Pt1 P1 2.2827(10) . ? Pt1 Cl1 2.3213(10) . ? P1 C1 1.804(3) . ? P1 C15 1.817(4) . ? P1 C21 1.831(4) . ? P2 C8 1.804(4) . ? P2 C30 1.835(4) . ? P2 C27 1.842(4) . ? N1 C13 1.401(5) . ? N1 C6 1.403(5) . ? C1 C2 1.388(5) . ? C1 C6 1.413(5) . ? C2 C3 1.380(5) . ? C2 H2 0.9500 . ? C3 C4 1.407(6) . ? C3 C7 1.504(6) . ? C4 C5 1.367(5) . ? C4 H4 0.9500 . ? C5 C6 1.397(5) . ? C5 H5 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.395(5) . ? C8 C13 1.410(5) . ? C9 C10 1.386(5) . ? C9 H9 0.9500 . ? C10 C11 1.380(6) . ? C10 C14 1.509(6) . ? C11 C12 1.386(5) . ? C11 H11 0.9500 . ? C12 C13 1.395(5) . ? C12 H12 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.369(5) . ? C15 C20 1.391(5) . ? C16 C17 1.391(6) . ? C16 H16 0.9500 . ? C17 C18 1.362(6) . ? C17 H17 0.9500 . ? C18 C19 1.355(6) . ? C18 H18 0.9500 . ? C19 C20 1.379(6) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C26 1.387(5) . ? C21 C22 1.391(5) . ? C22 C23 1.384(5) . ? C22 H22 0.9500 . ? C23 C24 1.375(6) . ? C23 H23 0.9500 . ? C24 C25 1.367(6) . ? C24 H24 0.9500 . ? C25 C26 1.387(5) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.521(6) . ? C27 C29 1.527(6) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C32 1.517(6) . ? C30 C31 1.532(6) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C35 1.370(6) 3_665 ? C33 C34 1.374(6) . ? C33 H33 0.9500 . ? C34 C35 1.366(6) . ? C34 H34 0.9500 . ? C35 C33 1.370(6) 3_665 ? C35 H35 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pt1 P2 82.07(9) . . ? N1 Pt1 P1 84.47(9) . . ? P2 Pt1 P1 164.02(3) . . ? N1 Pt1 Cl1 179.26(8) . . ? P2 Pt1 Cl1 97.96(4) . . ? P1 Pt1 Cl1 95.62(4) . . ? C1 P1 C15 107.00(17) . . ? C1 P1 C21 107.58(16) . . ? C15 P1 C21 105.72(17) . . ? C1 P1 Pt1 99.20(12) . . ? C15 P1 Pt1 123.96(12) . . ? C21 P1 Pt1 112.18(13) . . ? C8 P2 C30 108.15(18) . . ? C8 P2 C27 105.19(17) . . ? C30 P2 C27 108.84(19) . . ? C8 P2 Pt1 99.33(13) . . ? C30 P2 Pt1 122.11(14) . . ? C27 P2 Pt1 111.52(13) . . ? C13 N1 C6 123.0(3) . . ? C13 N1 Pt1 118.8(2) . . ? C6 N1 Pt1 118.3(2) . . ? C2 C1 C6 120.1(3) . . ? C2 C1 P1 123.7(3) . . ? C6 C1 P1 116.0(3) . . ? C3 C2 C1 122.8(4) . . ? C3 C2 H2 118.6 . . ? C1 C2 H2 118.6 . . ? C2 C3 C4 116.1(4) . . ? C2 C3 C7 122.3(4) . . ? C4 C3 C7 121.5(4) . . ? C5 C4 C3 122.2(4) . . ? C5 C4 H4 118.9 . . ? C3 C4 H4 118.9 . . ? C4 C5 C6 121.5(4) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 N1 124.7(3) . . ? C5 C6 C1 116.8(3) . . ? N1 C6 C1 118.4(3) . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C13 121.3(3) . . ? C9 C8 P2 124.7(3) . . ? C13 C8 P2 114.0(3) . . ? C10 C9 C8 121.4(4) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C11 C10 C9 116.9(4) . . ? C11 C10 C14 122.3(4) . . ? C9 C10 C14 120.8(4) . . ? C10 C11 C12 123.0(4) . . ? C10 C11 H11 118.5 . . ? C12 C11 H11 118.5 . . ? C11 C12 C13 120.7(4) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C12 C13 N1 125.2(3) . . ? C12 C13 C8 116.7(3) . . ? N1 C13 C8 117.9(3) . . ? C10 C14 H14A 109.5 . . ? C10 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C10 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C20 118.7(4) . . ? C16 C15 P1 121.2(3) . . ? C20 C15 P1 119.9(3) . . ? C15 C16 C17 120.2(4) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C18 C17 C16 120.5(4) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C19 C18 C17 119.8(4) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C20 120.7(4) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C19 C20 C15 120.1(4) . . ? C19 C20 H20 119.9 . . ? C15 C20 H20 119.9 . . ? C26 C21 C22 118.7(3) . . ? C26 C21 P1 118.4(3) . . ? C22 C21 P1 122.8(3) . . ? C23 C22 C21 120.2(4) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C24 C23 C22 120.6(4) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C25 C24 C23 119.5(4) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C24 C25 C26 120.8(4) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C25 C26 C21 120.2(4) . . ? C25 C26 H26 119.9 . . ? C21 C26 H26 119.9 . . ? C28 C27 C29 110.1(3) . . ? C28 C27 P2 109.2(3) . . ? C29 C27 P2 113.4(3) . . ? C28 C27 H27 108.0 . . ? C29 C27 H27 108.0 . . ? P2 C27 H27 108.0 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C32 C30 C31 111.8(3) . . ? C32 C30 P2 111.6(3) . . ? C31 C30 P2 108.7(3) . . ? C32 C30 H30 108.2 . . ? C31 C30 H30 108.2 . . ? P2 C30 H30 108.2 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C35 C33 C34 119.6(4) 3_665 . ? C35 C33 H33 120.2 3_665 . ? C34 C33 H33 120.2 . . ? C35 C34 C33 119.7(4) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C34 C35 C33 120.8(4) . 3_665 ? C34 C35 H35 119.6 . . ? C33 C35 H35 119.6 3_665 . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 28.45 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.984 _refine_diff_density_min -0.761 _refine_diff_density_rms 0.132 # Attachment 'Compound 6.cif' data_rkrl24 _database_code_depnum_ccdc_archive 'CCDC 812753' #TrackingRef 'Compound 6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H50 Cl N P2 Pt' _chemical_formula_weight 885.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3219(5) _cell_length_b 11.7353(5) _cell_length_c 15.5010(6) _cell_angle_alpha 93.810(2) _cell_angle_beta 110.178(2) _cell_angle_gamma 92.996(2) _cell_volume 1922.65(14) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 9990 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 30.93 _exptl_crystal_description chip _exptl_crystal_colour orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.529 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 3.834 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3716 _exptl_absorpt_correction_T_max 0.7193 _exptl_absorpt_process_details 'Bruker, Sadabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 43159 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.0453 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 32.09 _reflns_number_total 13063 _reflns_number_gt 11413 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics '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^)+(0.0640P)^2^+7.8706P] 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 13063 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0514 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.1336 _refine_ls_wR_factor_gt 0.1260 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.157 _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 Pt1 Pt 0.425894(15) 0.295945(14) 0.228589(11) 0.01599(6) Uani 1 1 d . . . Cl1 Cl 0.63496(11) 0.31606(12) 0.23742(10) 0.0285(2) Uani 1 1 d . . . P1 P 0.39910(11) 0.48663(10) 0.22996(8) 0.0175(2) Uani 1 1 d . . . P2 P 0.39563(11) 0.10000(10) 0.21225(8) 0.0169(2) Uani 1 1 d . . . N1 N 0.2453(4) 0.2843(3) 0.2295(3) 0.0193(7) Uani 1 1 d . . . C1 C 0.1709(5) 0.3728(4) 0.1969(4) 0.0217(9) Uani 1 1 d . . . C2 C 0.0373(5) 0.3619(4) 0.1628(4) 0.0246(9) Uani 1 1 d . . . H2A H -0.0063 0.2910 0.1640 0.030 Uiso 1 1 calc R . . C3 C -0.0303(5) 0.4530(5) 0.1277(4) 0.0275(10) Uani 1 1 d . . . H3A H -0.1198 0.4428 0.1057 0.033 Uiso 1 1 calc R . . C4 C 0.0270(5) 0.5596(5) 0.1231(4) 0.0256(10) Uani 1 1 d . . . C5 C -0.0503(6) 0.6571(5) 0.0836(5) 0.0370(13) Uani 1 1 d . . . H5A H 0.0063 0.7245 0.0864 0.055 Uiso 1 1 calc R . . H5B H -0.1042 0.6755 0.1194 0.055 Uiso 1 1 calc R . . H5C H -0.1031 0.6345 0.0192 0.055 Uiso 1 1 calc R . . C6 C 0.1570(5) 0.5711(4) 0.1544(4) 0.0236(9) Uani 1 1 d . . . H6A H 0.1988 0.6420 0.1509 0.028 Uiso 1 1 calc R . . C7 C 0.2293(4) 0.4809(4) 0.1914(3) 0.0199(8) Uani 1 1 d . . . C8 C 0.4467(5) 0.5686(4) 0.1507(4) 0.0231(9) Uani 1 1 d . . . C9 C 0.3751(5) 0.5554(5) 0.0568(4) 0.0281(10) Uani 1 1 d . . . H9A H 0.2990 0.5069 0.0352 0.034 Uiso 1 1 calc R . . C10 C 0.4146(6) 0.6128(6) -0.0053(4) 0.0339(12) Uani 1 1 d . . . H10A H 0.3651 0.6037 -0.0691 0.041 Uiso 1 1 calc R . . C11 C 0.5248(7) 0.6825(5) 0.0252(5) 0.0374(13) Uani 1 1 d . . . H11A H 0.5510 0.7220 -0.0175 0.045 Uiso 1 1 calc R . . C12 C 0.5976(6) 0.6955(6) 0.1177(5) 0.0384(13) Uani 1 1 d . . . H12A H 0.6739 0.7436 0.1384 0.046 Uiso 1 1 calc R . . C13 C 0.5596(6) 0.6379(5) 0.1813(4) 0.0324(12) Uani 1 1 d . . . H13A H 0.6105 0.6462 0.2449 0.039 Uiso 1 1 calc R . . C14 C 0.4601(5) 0.5718(4) 0.3402(3) 0.0211(9) Uani 1 1 d . . . C15 C 0.5730(6) 0.5478(5) 0.4051(4) 0.0318(12) Uani 1 1 d . . . H15A H 0.6181 0.4873 0.3913 0.038 Uiso 1 1 calc R . . C16 C 0.6208(6) 0.6116(6) 0.4902(4) 0.0396(14) Uani 1 1 d . . . H16A H 0.6987 0.5947 0.5341 0.047 Uiso 1 1 calc R . . C17 C 0.5568(6) 0.6989(6) 0.5118(4) 0.0364(13) Uani 1 1 d . . . H17A H 0.5900 0.7420 0.5703 0.044 Uiso 1 1 calc R . . C18 C 0.4434(7) 0.7234(7) 0.4475(5) 0.0469(18) Uani 1 1 d . . . H18A H 0.3985 0.7837 0.4618 0.056 Uiso 1 1 calc R . . C19 C 0.3951(6) 0.6603(6) 0.3622(5) 0.0427(16) Uani 1 1 d . . . H19A H 0.3172 0.6774 0.3185 0.051 Uiso 1 1 calc R . . C20 C 0.2038(4) 0.1845(4) 0.2566(3) 0.0193(8) Uani 1 1 d . . . C21 C 0.1098(4) 0.1806(5) 0.2984(3) 0.0222(9) Uani 1 1 d . . . H21A H 0.0732 0.2487 0.3092 0.027 Uiso 1 1 calc R . . C22 C 0.0719(5) 0.0784(5) 0.3233(4) 0.0271(10) Uani 1 1 d . . . H22A H 0.0077 0.0777 0.3498 0.032 Uiso 1 1 calc R . . C23 C 0.1234(5) -0.0241(5) 0.3113(4) 0.0252(10) Uani 1 1 d . . . C24 C 0.0780(6) -0.1347(6) 0.3373(5) 0.0375(14) Uani 1 1 d . . . H24A H 0.1254 -0.1967 0.3236 0.056 Uiso 1 1 calc R . . H24B H -0.0121 -0.1518 0.3018 0.056 Uiso 1 1 calc R . . H24C H 0.0912 -0.1278 0.4034 0.056 Uiso 1 1 calc R . . C25 C 0.2214(5) -0.0188(4) 0.2771(4) 0.0237(9) Uani 1 1 d . . . H25A H 0.2620 -0.0864 0.2717 0.028 Uiso 1 1 calc R . . C26 C 0.2623(4) 0.0829(4) 0.2503(3) 0.0194(8) Uani 1 1 d . . . C27 C 0.3409(4) 0.0374(4) 0.0911(3) 0.0196(8) Uani 1 1 d . . . H27A H 0.4128 0.0490 0.0683 0.024 Uiso 1 1 calc R . . C28 C 0.3024(6) -0.0913(4) 0.0783(4) 0.0289(11) Uani 1 1 d . . . H28A H 0.2327 -0.1064 0.1018 0.035 Uiso 1 1 calc R . . H28B H 0.3748 -0.1327 0.1141 0.035 Uiso 1 1 calc R . . C29 C 0.2595(7) -0.1354(5) -0.0243(4) 0.0391(15) Uani 1 1 d . . . H29A H 0.3320 -0.1272 -0.0458 0.047 Uiso 1 1 calc R . . H29B H 0.2311 -0.2178 -0.0316 0.047 Uiso 1 1 calc R . . C30 C 0.1525(7) -0.0702(5) -0.0836(4) 0.0385(14) Uani 1 1 d . . . H30A H 0.1313 -0.0972 -0.1494 0.046 Uiso 1 1 calc R . . H30B H 0.0765 -0.0851 -0.0670 0.046 Uiso 1 1 calc R . . C31 C 0.1907(6) 0.0573(5) -0.0693(4) 0.0324(12) Uani 1 1 d . . . H31A H 0.1185 0.0984 -0.1057 0.039 Uiso 1 1 calc R . . H31B H 0.2608 0.0725 -0.0924 0.039 Uiso 1 1 calc R . . C32 C 0.2321(5) 0.1033(4) 0.0314(3) 0.0234(9) Uani 1 1 d . . . H32A H 0.1598 0.0954 0.0532 0.028 Uiso 1 1 calc R . . H32B H 0.2603 0.1857 0.0378 0.028 Uiso 1 1 calc R . . C33 C 0.5156(4) 0.0111(4) 0.2793(3) 0.0212(9) Uani 1 1 d . . . H33A H 0.4754 -0.0681 0.2746 0.025 Uiso 1 1 calc R . . C34 C 0.5639(5) 0.0588(5) 0.3813(4) 0.0272(10) Uani 1 1 d . . . H34A H 0.5970 0.1398 0.3865 0.033 Uiso 1 1 calc R . . H34B H 0.4929 0.0567 0.4048 0.033 Uiso 1 1 calc R . . C35 C 0.6684(6) -0.0104(6) 0.4404(4) 0.0362(13) Uani 1 1 d . . . H35A H 0.7009 0.0250 0.5048 0.043 Uiso 1 1 calc R . . H35B H 0.6332 -0.0894 0.4407 0.043 Uiso 1 1 calc R . . C36 C 0.7763(5) -0.0144(6) 0.4030(5) 0.0366(13) Uani 1 1 d . . . H36A H 0.8406 -0.0627 0.4402 0.044 Uiso 1 1 calc R . . H36B H 0.8168 0.0639 0.4085 0.044 Uiso 1 1 calc R . . C37 C 0.7284(6) -0.0633(6) 0.3015(5) 0.0368(14) Uani 1 1 d . . . H37A H 0.7993 -0.0610 0.2780 0.044 Uiso 1 1 calc R . . H37B H 0.6960 -0.1443 0.2969 0.044 Uiso 1 1 calc R . . C38 C 0.6248(5) 0.0040(5) 0.2429(4) 0.0280(10) Uani 1 1 d . . . H38A H 0.5923 -0.0328 0.1789 0.034 Uiso 1 1 calc R . . H38B H 0.6602 0.0824 0.2414 0.034 Uiso 1 1 calc R . . C44 C -0.0444(10) 0.6908(8) 0.4873(6) 0.062(2) Uani 1 1 d . . . H44A H -0.0827 0.7338 0.5231 0.075 Uiso 1 1 calc R . . C43 C 0.0802(10) 0.6735(8) 0.5236(6) 0.068(3) Uani 1 1 d . . . H43A H 0.1291 0.7028 0.5850 0.082 Uiso 1 1 calc R . . C42 C 0.1344(10) 0.6128(9) 0.4698(9) 0.077(3) Uani 1 1 d . . . H42A H 0.2215 0.6003 0.4943 0.092 Uiso 1 1 calc R . . C41 C 0.0629(12) 0.5697(8) 0.3803(8) 0.072(3) Uani 1 1 d . . . H41A H 0.1007 0.5288 0.3431 0.087 Uiso 1 1 calc R . . C40 C -0.0610(10) 0.5867(8) 0.3469(6) 0.063(2) Uani 1 1 d . . . H40A H -0.1114 0.5565 0.2861 0.076 Uiso 1 1 calc R . . C39 C -0.1143(9) 0.6473(9) 0.4006(7) 0.062(2) Uani 1 1 d . . . H39A H -0.2016 0.6589 0.3765 0.074 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 Pt1 0.01641(8) 0.01548(8) 0.01529(8) 0.00129(5) 0.00459(6) 0.00124(5) Cl1 0.0196(5) 0.0321(6) 0.0358(7) 0.0079(5) 0.0112(5) 0.0028(4) P1 0.0182(5) 0.0157(5) 0.0160(5) 0.0015(4) 0.0028(4) -0.0002(4) P2 0.0187(5) 0.0161(5) 0.0160(5) 0.0023(4) 0.0056(4) 0.0035(4) N1 0.0231(18) 0.0161(17) 0.0163(17) 0.0017(13) 0.0039(14) 0.0002(14) C1 0.021(2) 0.0164(19) 0.029(2) 0.0008(17) 0.0101(18) 0.0037(16) C2 0.019(2) 0.023(2) 0.028(2) 0.0020(18) 0.0031(18) -0.0001(17) C3 0.020(2) 0.027(2) 0.031(3) 0.003(2) 0.0024(19) 0.0038(18) C4 0.027(2) 0.024(2) 0.022(2) 0.0033(18) 0.0031(18) 0.0097(19) C5 0.032(3) 0.030(3) 0.047(4) 0.011(3) 0.008(3) 0.013(2) C6 0.027(2) 0.019(2) 0.025(2) 0.0035(17) 0.0084(19) 0.0049(17) C7 0.0188(19) 0.0151(19) 0.025(2) 0.0029(16) 0.0063(17) 0.0025(15) C8 0.026(2) 0.018(2) 0.025(2) 0.0034(17) 0.0082(18) 0.0010(17) C9 0.029(2) 0.032(3) 0.025(2) 0.006(2) 0.011(2) 0.004(2) C10 0.039(3) 0.042(3) 0.024(3) 0.009(2) 0.014(2) 0.010(2) C11 0.053(4) 0.031(3) 0.041(3) 0.013(2) 0.030(3) 0.006(3) C12 0.041(3) 0.032(3) 0.044(4) 0.002(3) 0.020(3) -0.009(2) C13 0.033(3) 0.032(3) 0.030(3) 0.001(2) 0.011(2) -0.009(2) C14 0.024(2) 0.017(2) 0.020(2) 0.0009(16) 0.0052(17) 0.0006(16) C15 0.032(3) 0.033(3) 0.023(2) -0.002(2) 0.000(2) 0.009(2) C16 0.036(3) 0.042(3) 0.027(3) -0.002(2) -0.006(2) 0.004(3) C17 0.041(3) 0.039(3) 0.024(3) -0.006(2) 0.007(2) 0.000(3) C18 0.044(4) 0.049(4) 0.038(3) -0.019(3) 0.004(3) 0.014(3) C19 0.040(3) 0.042(3) 0.033(3) -0.016(3) -0.001(3) 0.016(3) C20 0.0162(18) 0.019(2) 0.021(2) 0.0003(16) 0.0043(16) 0.0029(15) C21 0.019(2) 0.028(2) 0.021(2) 0.0014(18) 0.0081(17) 0.0039(17) C22 0.021(2) 0.039(3) 0.021(2) 0.006(2) 0.0069(18) 0.002(2) C23 0.025(2) 0.026(2) 0.023(2) 0.0092(18) 0.0066(18) -0.0014(18) C24 0.033(3) 0.035(3) 0.050(4) 0.021(3) 0.017(3) 0.000(2) C25 0.024(2) 0.020(2) 0.026(2) 0.0066(18) 0.0066(18) 0.0022(17) C26 0.0198(19) 0.018(2) 0.020(2) 0.0023(16) 0.0068(16) -0.0005(15) C27 0.022(2) 0.019(2) 0.0149(19) -0.0001(15) 0.0037(16) 0.0042(16) C28 0.038(3) 0.018(2) 0.025(2) -0.0004(18) 0.003(2) 0.0043(19) C29 0.052(4) 0.023(3) 0.029(3) -0.006(2) -0.002(3) 0.006(2) C30 0.045(3) 0.028(3) 0.026(3) -0.003(2) -0.007(2) 0.000(2) C31 0.040(3) 0.027(3) 0.022(2) 0.001(2) 0.000(2) 0.008(2) C32 0.026(2) 0.020(2) 0.021(2) 0.0029(17) 0.0040(18) 0.0046(17) C33 0.020(2) 0.024(2) 0.017(2) 0.0030(16) 0.0037(16) 0.0047(17) C34 0.028(2) 0.032(3) 0.020(2) 0.0017(19) 0.0052(19) 0.007(2) C35 0.035(3) 0.046(3) 0.023(3) 0.010(2) 0.003(2) 0.013(3) C36 0.025(3) 0.040(3) 0.038(3) 0.001(3) 0.001(2) 0.010(2) C37 0.026(3) 0.036(3) 0.043(3) -0.003(3) 0.004(2) 0.014(2) C38 0.025(2) 0.031(3) 0.027(2) 0.001(2) 0.0081(19) 0.010(2) C44 0.089(7) 0.061(5) 0.049(5) 0.007(4) 0.039(5) 0.002(5) C43 0.085(7) 0.055(5) 0.042(4) 0.019(4) -0.006(4) -0.017(5) C42 0.062(6) 0.066(6) 0.103(9) 0.048(6) 0.019(6) 0.023(5) C41 0.106(9) 0.043(5) 0.086(8) 0.019(5) 0.053(7) 0.019(5) C40 0.086(7) 0.057(5) 0.042(4) 0.004(4) 0.017(4) -0.014(5) C39 0.052(5) 0.077(6) 0.059(5) 0.019(5) 0.021(4) -0.008(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N1 2.046(4) . ? Pt1 P1 2.2735(12) . ? Pt1 P2 2.2911(12) . ? Pt1 Cl1 2.3219(12) . ? P1 C7 1.802(5) . ? P1 C8 1.812(5) . ? P1 C14 1.812(5) . ? P2 C26 1.808(5) . ? P2 C33 1.826(5) . ? P2 C27 1.848(5) . ? N1 C1 1.382(6) . ? N1 C20 1.383(6) . ? C1 C2 1.415(7) . ? C1 C7 1.421(7) . ? C2 C3 1.378(7) . ? C2 H2A 0.9500 . ? C3 C4 1.397(8) . ? C3 H3A 0.9500 . ? C4 C6 1.377(7) . ? C4 C5 1.509(7) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.403(7) . ? C6 H6A 0.9500 . ? C8 C9 1.393(7) . ? C8 C13 1.394(7) . ? C9 C10 1.390(8) . ? C9 H9A 0.9500 . ? C10 C11 1.373(10) . ? C10 H10A 0.9500 . ? C11 C12 1.378(10) . ? C11 H11A 0.9500 . ? C12 C13 1.402(9) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C15 1.383(7) . ? C14 C19 1.393(8) . ? C15 C16 1.389(8) . ? C15 H15A 0.9500 . ? C16 C17 1.372(9) . ? C16 H16A 0.9500 . ? C17 C18 1.386(9) . ? C17 H17A 0.9500 . ? C18 C19 1.387(8) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 C26 1.406(6) . ? C20 C21 1.426(6) . ? C21 C22 1.376(8) . ? C21 H21A 0.9500 . ? C22 C23 1.393(8) . ? C22 H22A 0.9500 . ? C23 C25 1.386(7) . ? C23 C24 1.502(8) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.398(7) . ? C25 H25A 0.9500 . ? C27 C28 1.530(7) . ? C27 C32 1.543(7) . ? C27 H27A 1.0000 . ? C28 C29 1.537(8) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.524(9) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.515(9) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.518(7) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C38 1.530(7) . ? C33 C34 1.539(7) . ? C33 H33A 1.0000 . ? C34 C35 1.533(8) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.524(9) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.535(9) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.510(8) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C44 C39 1.351(13) . ? C44 C43 1.359(15) . ? C44 H44A 0.9500 . ? C43 C42 1.378(16) . ? C43 H43A 0.9500 . ? C42 C41 1.387(17) . ? C42 H42A 0.9500 . ? C41 C40 1.348(16) . ? C41 H41A 0.9500 . ? C40 C39 1.369(14) . ? C40 H40A 0.9500 . ? C39 H39A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pt1 P1 83.01(12) . . ? N1 Pt1 P2 82.83(11) . . ? P1 Pt1 P2 164.79(4) . . ? N1 Pt1 Cl1 176.10(11) . . ? P1 Pt1 Cl1 95.26(5) . . ? P2 Pt1 Cl1 99.21(5) . . ? C7 P1 C8 106.7(2) . . ? C7 P1 C14 107.7(2) . . ? C8 P1 C14 105.6(2) . . ? C7 P1 Pt1 99.60(15) . . ? C8 P1 Pt1 118.46(17) . . ? C14 P1 Pt1 117.74(16) . . ? C26 P2 C33 107.2(2) . . ? C26 P2 C27 106.3(2) . . ? C33 P2 C27 107.0(2) . . ? C26 P2 Pt1 99.28(16) . . ? C33 P2 Pt1 121.72(17) . . ? C27 P2 Pt1 113.88(16) . . ? C1 N1 C20 124.6(4) . . ? C1 N1 Pt1 117.9(3) . . ? C20 N1 Pt1 117.4(3) . . ? N1 C1 C2 124.3(4) . . ? N1 C1 C7 119.3(4) . . ? C2 C1 C7 116.3(4) . . ? C3 C2 C1 120.7(5) . . ? C3 C2 H2A 119.6 . . ? C1 C2 H2A 119.6 . . ? C2 C3 C4 123.0(5) . . ? C2 C3 H3A 118.5 . . ? C4 C3 H3A 118.5 . . ? C6 C4 C3 117.1(5) . . ? C6 C4 C5 121.5(5) . . ? C3 C4 C5 121.4(5) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 C7 121.7(5) . . ? C4 C6 H6A 119.1 . . ? C7 C6 H6A 119.1 . . ? C6 C7 C1 121.1(4) . . ? C6 C7 P1 124.7(4) . . ? C1 C7 P1 114.1(3) . . ? C9 C8 C13 119.3(5) . . ? C9 C8 P1 119.8(4) . . ? C13 C8 P1 120.7(4) . . ? C10 C9 C8 120.3(5) . . ? C10 C9 H9A 119.9 . . ? C8 C9 H9A 119.9 . . ? C11 C10 C9 120.4(6) . . ? C11 C10 H10A 119.8 . . ? C9 C10 H10A 119.8 . . ? C10 C11 C12 120.1(6) . . ? C10 C11 H11A 119.9 . . ? C12 C11 H11A 119.9 . . ? C11 C12 C13 120.4(6) . . ? C11 C12 H12A 119.8 . . ? C13 C12 H12A 119.8 . . ? C8 C13 C12 119.5(6) . . ? C8 C13 H13A 120.2 . . ? C12 C13 H13A 120.2 . . ? C15 C14 C19 118.8(5) . . ? C15 C14 P1 119.5(4) . . ? C19 C14 P1 121.7(4) . . ? C14 C15 C16 120.3(5) . . ? C14 C15 H15A 119.8 . . ? C16 C15 H15A 119.8 . . ? C17 C16 C15 120.8(6) . . ? C17 C16 H16A 119.6 . . ? C15 C16 H16A 119.6 . . ? C16 C17 C18 119.3(6) . . ? C16 C17 H17A 120.3 . . ? C18 C17 H17A 120.3 . . ? C17 C18 C19 120.2(6) . . ? C17 C18 H18A 119.9 . . ? C19 C18 H18A 119.9 . . ? C18 C19 C14 120.5(6) . . ? C18 C19 H19A 119.8 . . ? C14 C19 H19A 119.8 . . ? N1 C20 C26 119.9(4) . . ? N1 C20 C21 122.9(4) . . ? C26 C20 C21 117.0(4) . . ? C22 C21 C20 120.1(5) . . ? C22 C21 H21A 119.9 . . ? C20 C21 H21A 119.9 . . ? C21 C22 C23 122.9(5) . . ? C21 C22 H22A 118.5 . . ? C23 C22 H22A 118.5 . . ? C25 C23 C22 117.0(5) . . ? C25 C23 C24 121.3(5) . . ? C22 C23 C24 121.6(5) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 C26 121.9(5) . . ? C23 C25 H25A 119.0 . . ? C26 C25 H25A 119.0 . . ? C25 C26 C20 120.7(4) . . ? C25 C26 P2 124.9(4) . . ? C20 C26 P2 114.2(3) . . ? C28 C27 C32 110.6(4) . . ? C28 C27 P2 114.3(3) . . ? C32 C27 P2 109.8(3) . . ? C28 C27 H27A 107.2 . . ? C32 C27 H27A 107.2 . . ? P2 C27 H27A 107.2 . . ? C27 C28 C29 110.4(5) . . ? C27 C28 H28A 109.6 . . ? C29 C28 H28A 109.6 . . ? C27 C28 H28B 109.6 . . ? C29 C28 H28B 109.6 . . ? H28A C28 H28B 108.1 . . ? C30 C29 C28 111.8(5) . . ? C30 C29 H29A 109.2 . . ? C28 C29 H29A 109.2 . . ? C30 C29 H29B 109.2 . . ? C28 C29 H29B 109.2 . . ? H29A C29 H29B 107.9 . . ? C31 C30 C29 110.4(5) . . ? C31 C30 H30A 109.6 . . ? C29 C30 H30A 109.6 . . ? C31 C30 H30B 109.6 . . ? C29 C30 H30B 109.6 . . ? H30A C30 H30B 108.1 . . ? C30 C31 C32 112.4(5) . . ? C30 C31 H31A 109.1 . . ? C32 C31 H31A 109.1 . . ? C30 C31 H31B 109.1 . . ? C32 C31 H31B 109.1 . . ? H31A C31 H31B 107.9 . . ? C31 C32 C27 110.6(4) . . ? C31 C32 H32A 109.5 . . ? C27 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? C27 C32 H32B 109.5 . . ? H32A C32 H32B 108.1 . . ? C38 C33 C34 110.8(4) . . ? C38 C33 P2 111.9(4) . . ? C34 C33 P2 109.2(3) . . ? C38 C33 H33A 108.3 . . ? C34 C33 H33A 108.3 . . ? P2 C33 H33A 108.3 . . ? C35 C34 C33 111.4(4) . . ? C35 C34 H34A 109.3 . . ? C33 C34 H34A 109.3 . . ? C35 C34 H34B 109.3 . . ? C33 C34 H34B 109.3 . . ? H34A C34 H34B 108.0 . . ? C36 C35 C34 110.8(5) . . ? C36 C35 H35A 109.5 . . ? C34 C35 H35A 109.5 . . ? C36 C35 H35B 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 108.1 . . ? C35 C36 C37 111.0(5) . . ? C35 C36 H36A 109.4 . . ? C37 C36 H36A 109.4 . . ? C35 C36 H36B 109.4 . . ? C37 C36 H36B 109.4 . . ? H36A C36 H36B 108.0 . . ? C38 C37 C36 111.3(5) . . ? C38 C37 H37A 109.4 . . ? C36 C37 H37A 109.4 . . ? C38 C37 H37B 109.4 . . ? C36 C37 H37B 109.4 . . ? H37A C37 H37B 108.0 . . ? C37 C38 C33 112.3(5) . . ? C37 C38 H38A 109.2 . . ? C33 C38 H38A 109.2 . . ? C37 C38 H38B 109.2 . . ? C33 C38 H38B 109.2 . . ? H38A C38 H38B 107.9 . . ? C39 C44 C43 120.5(9) . . ? C39 C44 H44A 119.8 . . ? C43 C44 H44A 119.8 . . ? C44 C43 C42 118.8(9) . . ? C44 C43 H43A 120.6 . . ? C42 C43 H43A 120.6 . . ? C43 C42 C41 120.6(10) . . ? C43 C42 H42A 119.7 . . ? C41 C42 H42A 119.7 . . ? C40 C41 C42 119.2(10) . . ? C40 C41 H41A 120.4 . . ? C42 C41 H41A 120.4 . . ? C41 C40 C39 120.0(9) . . ? C41 C40 H40A 120.0 . . ? C39 C40 H40A 120.0 . . ? C44 C39 C40 121.0(9) . . ? C44 C39 H39A 119.5 . . ? C40 C39 H39A 119.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Pt1 P1 C7 -18.7(2) . . . . ? P2 Pt1 P1 C7 2.8(2) . . . . ? Cl1 Pt1 P1 C7 164.78(17) . . . . ? N1 Pt1 P1 C8 -133.8(2) . . . . ? P2 Pt1 P1 C8 -112.3(2) . . . . ? Cl1 Pt1 P1 C8 49.7(2) . . . . ? N1 Pt1 P1 C14 97.2(2) . . . . ? P2 Pt1 P1 C14 118.6(2) . . . . ? Cl1 Pt1 P1 C14 -79.32(19) . . . . ? N1 Pt1 P2 C26 -18.02(19) . . . . ? P1 Pt1 P2 C26 -39.5(2) . . . . ? Cl1 Pt1 P2 C26 158.62(16) . . . . ? N1 Pt1 P2 C33 -135.0(2) . . . . ? P1 Pt1 P2 C33 -156.5(2) . . . . ? Cl1 Pt1 P2 C33 41.6(2) . . . . ? N1 Pt1 P2 C27 94.5(2) . . . . ? P1 Pt1 P2 C27 73.0(2) . . . . ? Cl1 Pt1 P2 C27 -88.84(17) . . . . ? P1 Pt1 N1 C1 23.4(3) . . . . ? P2 Pt1 N1 C1 -151.0(4) . . . . ? Cl1 Pt1 N1 C1 87.2(18) . . . . ? P1 Pt1 N1 C20 -161.1(3) . . . . ? P2 Pt1 N1 C20 24.5(3) . . . . ? Cl1 Pt1 N1 C20 -97.3(17) . . . . ? C20 N1 C1 C2 -18.3(8) . . . . ? Pt1 N1 C1 C2 156.8(4) . . . . ? C20 N1 C1 C7 165.5(5) . . . . ? Pt1 N1 C1 C7 -19.3(6) . . . . ? N1 C1 C2 C3 -177.2(5) . . . . ? C7 C1 C2 C3 -0.9(8) . . . . ? C1 C2 C3 C4 0.3(9) . . . . ? C2 C3 C4 C6 0.8(8) . . . . ? C2 C3 C4 C5 179.6(6) . . . . ? C3 C4 C6 C7 -1.4(8) . . . . ? C5 C4 C6 C7 179.8(5) . . . . ? C4 C6 C7 C1 0.9(8) . . . . ? C4 C6 C7 P1 177.6(4) . . . . ? N1 C1 C7 C6 176.8(5) . . . . ? C2 C1 C7 C6 0.3(7) . . . . ? N1 C1 C7 P1 -0.3(6) . . . . ? C2 C1 C7 P1 -176.7(4) . . . . ? C8 P1 C7 C6 -37.3(5) . . . . ? C14 P1 C7 C6 75.6(5) . . . . ? Pt1 P1 C7 C6 -161.1(4) . . . . ? C8 P1 C7 C1 139.6(4) . . . . ? C14 P1 C7 C1 -107.4(4) . . . . ? Pt1 P1 C7 C1 15.9(4) . . . . ? C7 P1 C8 C9 -38.5(5) . . . . ? C14 P1 C8 C9 -152.8(4) . . . . ? Pt1 P1 C8 C9 72.7(5) . . . . ? C7 P1 C8 C13 146.7(5) . . . . ? C14 P1 C8 C13 32.3(5) . . . . ? Pt1 P1 C8 C13 -102.2(5) . . . . ? C13 C8 C9 C10 -1.4(8) . . . . ? P1 C8 C9 C10 -176.3(4) . . . . ? C8 C9 C10 C11 0.4(9) . . . . ? C9 C10 C11 C12 0.4(10) . . . . ? C10 C11 C12 C13 -0.2(10) . . . . ? C9 C8 C13 C12 1.6(9) . . . . ? P1 C8 C13 C12 176.5(5) . . . . ? C11 C12 C13 C8 -0.8(10) . . . . ? C7 P1 C14 C15 148.8(5) . . . . ? C8 P1 C14 C15 -97.5(5) . . . . ? Pt1 P1 C14 C15 37.4(5) . . . . ? C7 P1 C14 C19 -30.2(6) . . . . ? C8 P1 C14 C19 83.5(6) . . . . ? Pt1 P1 C14 C19 -141.6(5) . . . . ? C19 C14 C15 C16 -0.5(10) . . . . ? P1 C14 C15 C16 -179.5(5) . . . . ? C14 C15 C16 C17 0.4(11) . . . . ? C15 C16 C17 C18 -0.2(11) . . . . ? C16 C17 C18 C19 0.1(12) . . . . ? C17 C18 C19 C14 -0.2(13) . . . . ? C15 C14 C19 C18 0.4(11) . . . . ? P1 C14 C19 C18 179.4(6) . . . . ? C1 N1 C20 C26 152.4(5) . . . . ? Pt1 N1 C20 C26 -22.7(6) . . . . ? C1 N1 C20 C21 -32.9(7) . . . . ? Pt1 N1 C20 C21 151.9(4) . . . . ? N1 C20 C21 C22 179.5(5) . . . . ? C26 C20 C21 C22 -5.7(7) . . . . ? C20 C21 C22 C23 1.4(8) . . . . ? C21 C22 C23 C25 3.3(8) . . . . ? C21 C22 C23 C24 -178.7(5) . . . . ? C22 C23 C25 C26 -3.8(8) . . . . ? C24 C23 C25 C26 178.2(5) . . . . ? C23 C25 C26 C20 -0.5(8) . . . . ? C23 C25 C26 P2 175.7(4) . . . . ? N1 C20 C26 C25 -179.8(4) . . . . ? C21 C20 C26 C25 5.2(7) . . . . ? N1 C20 C26 P2 3.6(6) . . . . ? C21 C20 C26 P2 -171.4(4) . . . . ? C33 P2 C26 C25 -35.6(5) . . . . ? C27 P2 C26 C25 78.6(5) . . . . ? Pt1 P2 C26 C25 -163.1(4) . . . . ? C33 P2 C26 C20 140.8(4) . . . . ? C27 P2 C26 C20 -105.0(4) . . . . ? Pt1 P2 C26 C20 13.4(4) . . . . ? C26 P2 C27 C28 -63.4(4) . . . . ? C33 P2 C27 C28 50.9(4) . . . . ? Pt1 P2 C27 C28 -171.7(3) . . . . ? C26 P2 C27 C32 61.6(4) . . . . ? C33 P2 C27 C32 175.9(3) . . . . ? Pt1 P2 C27 C32 -46.7(4) . . . . ? C32 C27 C28 C29 55.9(6) . . . . ? P2 C27 C28 C29 -179.5(4) . . . . ? C27 C28 C29 C30 -56.2(7) . . . . ? C28 C29 C30 C31 55.5(8) . . . . ? C29 C30 C31 C32 -55.8(8) . . . . ? C30 C31 C32 C27 56.3(7) . . . . ? C28 C27 C32 C31 -56.0(6) . . . . ? P2 C27 C32 C31 176.9(4) . . . . ? C26 P2 C33 C38 171.2(4) . . . . ? C27 P2 C33 C38 57.5(4) . . . . ? Pt1 P2 C33 C38 -75.9(4) . . . . ? C26 P2 C33 C34 -65.8(4) . . . . ? C27 P2 C33 C34 -179.5(4) . . . . ? Pt1 P2 C33 C34 47.1(4) . . . . ? C38 C33 C34 C35 -54.4(6) . . . . ? P2 C33 C34 C35 -178.1(4) . . . . ? C33 C34 C35 C36 55.9(7) . . . . ? C34 C35 C36 C37 -56.2(7) . . . . ? C35 C36 C37 C38 56.0(8) . . . . ? C36 C37 C38 C33 -55.1(7) . . . . ? C34 C33 C38 C37 54.2(6) . . . . ? P2 C33 C38 C37 176.4(4) . . . . ? C39 C44 C43 C42 1.2(14) . . . . ? C44 C43 C42 C41 -0.2(15) . . . . ? C43 C42 C41 C40 -0.9(15) . . . . ? C42 C41 C40 C39 1.0(14) . . . . ? C43 C44 C39 C40 -1.1(14) . . . . ? C41 C40 C39 C44 -0.1(15) . . . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 32.09 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 3.968 _refine_diff_density_min -1.729 _refine_diff_density_rms 0.223 # Attachment 'Compound 7.cif' data_rkrl34 _database_code_depnum_ccdc_archive 'CCDC 812754' #TrackingRef 'Compound 7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H37 N Ni P2' _chemical_formula_weight 556.28 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' Ni Ni 0.3393 1.1124 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.3808(8) _cell_length_b 14.9010(10) _cell_length_c 18.6532(11) _cell_angle_alpha 90.00 _cell_angle_beta 122.533(4) _cell_angle_gamma 90.00 _cell_volume 2901.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 188(2) _cell_measurement_reflns_used 7604 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.00 _exptl_crystal_description ? _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.274 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 0.800 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7954 _exptl_absorpt_correction_T_max 0.9243 _exptl_absorpt_process_details 'Bruker, SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 188(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 '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 31034 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 26.73 _reflns_number_total 5933 _reflns_number_gt 4560 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics '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^)+(0.0661P)^2^+2.7369P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5933 _refine_ls_number_parameters 328 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0649 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.1317 _refine_ls_wR_factor_gt 0.1158 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.008 _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 Ni1 Ni 0.33697(3) 0.67197(3) 0.77933(2) 0.02595(13) Uani 1 1 d D . . P1 P 0.47375(7) 0.62078(5) 0.75350(5) 0.02360(18) Uani 1 1 d . . . P2 P 0.18456(7) 0.71758(5) 0.79195(5) 0.02319(18) Uani 1 1 d . . . N1 N 0.2111(2) 0.65844(17) 0.66003(15) 0.0254(5) Uani 1 1 d . . . C1 C 0.2362(3) 0.5987(2) 0.61353(17) 0.0232(6) Uani 1 1 d . . . C2 C 0.1453(3) 0.5566(2) 0.53667(19) 0.0297(7) Uani 1 1 d . . . H2A H 0.0575 0.5725 0.5097 0.036 Uiso 1 1 calc R . . C3 C 0.1809(3) 0.4929(2) 0.49968(19) 0.0315(7) Uani 1 1 d . . . H3A H 0.1161 0.4657 0.4481 0.038 Uiso 1 1 calc R . . C4 C 0.3073(3) 0.4665(2) 0.53457(19) 0.0297(7) Uani 1 1 d . . . C5 C 0.3433(4) 0.3956(2) 0.4936(2) 0.0424(8) Uani 1 1 d . . . H5A H 0.2665 0.3757 0.4405 0.064 Uiso 1 1 calc R . . H5B H 0.3819 0.3444 0.5323 0.064 Uiso 1 1 calc R . . H5C H 0.4050 0.4205 0.4814 0.064 Uiso 1 1 calc R . . C6 C 0.3986(3) 0.5068(2) 0.61121(19) 0.0280(6) Uani 1 1 d . . . H6A H 0.4859 0.4898 0.6377 0.034 Uiso 1 1 calc R . . C7 C 0.3654(3) 0.5714(2) 0.65008(17) 0.0241(6) Uani 1 1 d . . . C8 C 0.5720(3) 0.7032(2) 0.74302(18) 0.0259(6) Uani 1 1 d . . . C9 C 0.5949(3) 0.7008(2) 0.6778(2) 0.0327(7) Uani 1 1 d . . . H9A H 0.5561 0.6555 0.6355 0.039 Uiso 1 1 calc R . . C10 C 0.6736(4) 0.7640(2) 0.6742(2) 0.0411(8) Uani 1 1 d . . . H10A H 0.6882 0.7623 0.6291 0.049 Uiso 1 1 calc R . . C11 C 0.7311(3) 0.8295(2) 0.7359(3) 0.0410(8) Uani 1 1 d . . . H11A H 0.7866 0.8720 0.7339 0.049 Uiso 1 1 calc R . . C12 C 0.7084(3) 0.8335(2) 0.8004(2) 0.0407(8) Uani 1 1 d . . . H12A H 0.7472 0.8792 0.8424 0.049 Uiso 1 1 calc R . . C13 C 0.6293(3) 0.7712(2) 0.8039(2) 0.0346(7) Uani 1 1 d . . . H13A H 0.6134 0.7744 0.8483 0.042 Uiso 1 1 calc R . . C14 C 0.5846(3) 0.5319(2) 0.81774(18) 0.0290(7) Uani 1 1 d . . . C15 C 0.5439(3) 0.4733(2) 0.8572(2) 0.0414(8) Uani 1 1 d . . . H15A H 0.4635 0.4825 0.8513 0.050 Uiso 1 1 calc R . . C16 C 0.6204(4) 0.4021(3) 0.9048(3) 0.0538(10) Uani 1 1 d . . . H16A H 0.5922 0.3618 0.9310 0.065 Uiso 1 1 calc R . . C17 C 0.7378(5) 0.3896(3) 0.9143(3) 0.0565(11) Uani 1 1 d . . . H17A H 0.7895 0.3399 0.9461 0.068 Uiso 1 1 calc R . . C18 C 0.7803(4) 0.4477(3) 0.8788(2) 0.0604(13) Uani 1 1 d . . . H18A H 0.8624 0.4392 0.8872 0.073 Uiso 1 1 calc R . . C19 C 0.7035(3) 0.5205(3) 0.8294(2) 0.0458(9) Uani 1 1 d . . . H19A H 0.7333 0.5611 0.8045 0.055 Uiso 1 1 calc R . . C20 C 0.0978(3) 0.7075(2) 0.62467(17) 0.0233(6) Uani 1 1 d . . . C21 C 0.0156(3) 0.7316(2) 0.53888(18) 0.0299(7) Uani 1 1 d . . . H21A H 0.0321 0.7089 0.4981 0.036 Uiso 1 1 calc R . . C22 C -0.0880(3) 0.7872(2) 0.51236(19) 0.0326(7) Uani 1 1 d . . . H22A H -0.1395 0.8028 0.4539 0.039 Uiso 1 1 calc R . . C23 C -0.1201(3) 0.8212(2) 0.5676(2) 0.0321(7) Uani 1 1 d . . . C24 C -0.2339(4) 0.8827(3) 0.5363(2) 0.0474(9) Uani 1 1 d . . . H24A H -0.2766 0.8911 0.4748 0.071 Uiso 1 1 calc R . . H24B H -0.2048 0.9410 0.5648 0.071 Uiso 1 1 calc R . . H24C H -0.2941 0.8561 0.5490 0.071 Uiso 1 1 calc R . . C25 C -0.0405(3) 0.7978(2) 0.65298(19) 0.0282(7) Uani 1 1 d . . . H25A H -0.0596 0.8199 0.6927 0.034 Uiso 1 1 calc R . . C26 C 0.0661(3) 0.7429(2) 0.68197(17) 0.0241(6) Uani 1 1 d . . . C27 C 0.2033(3) 0.8187(2) 0.85399(19) 0.0300(7) Uani 1 1 d . . . H27A H 0.1177 0.8359 0.8432 0.036 Uiso 1 1 calc R . . C28 C 0.2946(4) 0.7993(2) 0.9493(2) 0.0431(9) Uani 1 1 d . . . H28A H 0.3038 0.8534 0.9821 0.065 Uiso 1 1 calc R . . H28B H 0.3786 0.7817 0.9605 0.065 Uiso 1 1 calc R . . H28C H 0.2597 0.7505 0.9661 0.065 Uiso 1 1 calc R . . C29 C 0.2532(4) 0.8953(2) 0.8261(2) 0.0488(10) Uani 1 1 d . . . H29A H 0.2626 0.9492 0.8591 0.073 Uiso 1 1 calc R . . H29B H 0.1927 0.9073 0.7655 0.073 Uiso 1 1 calc R . . H29C H 0.3366 0.8788 0.8357 0.073 Uiso 1 1 calc R . . C30 C 0.1157(3) 0.6304(2) 0.8262(2) 0.0310(7) Uani 1 1 d . . . H30A H 0.1838 0.6125 0.8854 0.037 Uiso 1 1 calc R . . C31 C 0.0002(4) 0.6602(3) 0.8281(3) 0.0531(10) Uani 1 1 d . . . H31A H -0.0299 0.6102 0.8470 0.080 Uiso 1 1 calc R . . H31B H -0.0683 0.6788 0.7709 0.080 Uiso 1 1 calc R . . H31C H 0.0242 0.7107 0.8674 0.080 Uiso 1 1 calc R . . C32 C 0.0843(5) 0.5480(3) 0.7697(3) 0.0569(11) Uani 1 1 d . . . H32A H 0.0480 0.5011 0.7875 0.085 Uiso 1 1 calc R . . H32B H 0.1627 0.5256 0.7749 0.085 Uiso 1 1 calc R . . H32C H 0.0219 0.5643 0.7103 0.085 Uiso 1 1 calc R . . H1 H 0.455(4) 0.671(3) 0.9024(19) 0.068 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0233(2) 0.0367(2) 0.0175(2) -0.00203(16) 0.01079(17) 0.00300(16) P1 0.0224(4) 0.0288(4) 0.0190(4) -0.0014(3) 0.0107(3) 0.0015(3) P2 0.0256(4) 0.0275(4) 0.0178(3) 0.0017(3) 0.0125(3) 0.0030(3) N1 0.0226(12) 0.0341(14) 0.0193(12) -0.0024(10) 0.0111(11) 0.0012(11) C1 0.0258(14) 0.0291(15) 0.0173(13) -0.0004(11) 0.0132(12) -0.0040(12) C2 0.0243(15) 0.0366(17) 0.0254(15) -0.0040(13) 0.0114(13) -0.0059(13) C3 0.0361(17) 0.0343(17) 0.0239(15) -0.0078(13) 0.0159(14) -0.0115(14) C4 0.0413(18) 0.0262(15) 0.0267(15) -0.0029(12) 0.0217(15) -0.0036(14) C5 0.056(2) 0.0369(19) 0.0367(18) -0.0090(15) 0.0262(18) 0.0005(17) C6 0.0303(16) 0.0284(16) 0.0271(15) -0.0016(12) 0.0166(14) 0.0003(13) C7 0.0254(14) 0.0285(15) 0.0195(13) -0.0007(12) 0.0128(13) -0.0027(12) C8 0.0236(14) 0.0267(15) 0.0262(15) 0.0002(12) 0.0127(13) 0.0035(12) C9 0.0381(18) 0.0317(17) 0.0330(17) -0.0060(13) 0.0222(16) -0.0045(14) C10 0.050(2) 0.041(2) 0.047(2) -0.0043(16) 0.0356(19) -0.0042(17) C11 0.0400(19) 0.0292(17) 0.061(2) -0.0020(16) 0.0322(19) -0.0033(15) C12 0.043(2) 0.0310(18) 0.048(2) -0.0122(15) 0.0241(18) -0.0050(16) C13 0.0380(18) 0.0360(18) 0.0313(17) -0.0060(14) 0.0195(16) -0.0002(15) C14 0.0304(16) 0.0303(16) 0.0186(14) -0.0027(12) 0.0081(13) 0.0051(13) C15 0.0341(18) 0.0361(19) 0.042(2) 0.0039(16) 0.0124(16) -0.0023(16) C16 0.061(3) 0.036(2) 0.051(2) 0.0131(18) 0.021(2) 0.0020(19) C17 0.077(3) 0.047(2) 0.046(2) 0.0154(18) 0.033(2) 0.033(2) C18 0.058(3) 0.091(3) 0.043(2) 0.020(2) 0.034(2) 0.043(2) C19 0.045(2) 0.066(3) 0.0326(18) 0.0139(18) 0.0252(17) 0.0245(19) C20 0.0206(13) 0.0289(15) 0.0195(13) 0.0008(12) 0.0101(12) -0.0038(12) C21 0.0301(16) 0.0392(18) 0.0181(14) -0.0025(13) 0.0114(13) -0.0052(14) C22 0.0302(16) 0.0405(18) 0.0191(14) 0.0064(13) 0.0080(14) 0.0012(14) C23 0.0282(16) 0.0343(17) 0.0290(16) 0.0046(14) 0.0122(14) 0.0034(14) C24 0.042(2) 0.059(2) 0.0366(19) 0.0132(18) 0.0180(17) 0.0182(19) C25 0.0302(16) 0.0295(16) 0.0274(15) 0.0041(13) 0.0172(14) 0.0037(13) C26 0.0256(14) 0.0272(15) 0.0191(13) 0.0016(12) 0.0118(13) -0.0020(12) C27 0.0376(17) 0.0291(16) 0.0241(15) -0.0015(13) 0.0171(14) 0.0054(14) C28 0.057(2) 0.041(2) 0.0264(17) -0.0042(15) 0.0190(17) 0.0056(18) C29 0.063(3) 0.038(2) 0.041(2) -0.0033(16) 0.025(2) -0.0109(19) C30 0.0348(17) 0.0319(17) 0.0268(16) 0.0073(13) 0.0170(15) 0.0009(14) C31 0.052(2) 0.058(3) 0.068(3) 0.013(2) 0.044(2) 0.0009(19) C32 0.079(3) 0.035(2) 0.062(3) -0.0028(19) 0.041(2) -0.013(2) _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 Ni1 N1 1.921(2) . ? Ni1 P2 2.1344(8) . ? Ni1 P1 2.1353(8) . ? Ni1 H1 1.95(3) . ? P1 C7 1.811(3) . ? P1 C8 1.812(3) . ? P1 C14 1.817(3) . ? P2 C26 1.807(3) . ? P2 C27 1.838(3) . ? P2 C30 1.845(3) . ? N1 C1 1.390(4) . ? N1 C20 1.394(4) . ? C1 C2 1.407(4) . ? C1 C7 1.419(4) . ? C2 C3 1.379(4) . ? C2 H2A 0.9500 . ? C3 C4 1.390(4) . ? C3 H3A 0.9500 . ? C4 C6 1.394(4) . ? C4 C5 1.505(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.394(4) . ? C6 H6A 0.9500 . ? C8 C9 1.390(4) . ? C8 C13 1.397(4) . ? C9 C10 1.383(5) . ? C9 H9A 0.9500 . ? C10 C11 1.380(5) . ? C10 H10A 0.9500 . ? C11 C12 1.377(5) . ? C11 H11A 0.9500 . ? C12 C13 1.376(5) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C19 1.378(5) . ? C14 C15 1.400(5) . ? C15 C16 1.381(5) . ? C15 H15A 0.9500 . ? C16 C17 1.379(6) . ? C16 H16A 0.9500 . ? C17 C18 1.357(6) . ? C17 H17A 0.9500 . ? C18 C19 1.409(5) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 C21 1.405(4) . ? C20 C26 1.423(4) . ? C21 C22 1.376(4) . ? C21 H21A 0.9500 . ? C22 C23 1.385(5) . ? C22 H22A 0.9500 . ? C23 C25 1.393(4) . ? C23 C24 1.510(5) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.391(4) . ? C25 H25A 0.9500 . ? C27 C29 1.516(5) . ? C27 C28 1.536(4) . ? C27 H27A 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.515(5) . ? C30 C32 1.527(5) . ? C30 H30A 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 P2 86.95(8) . . ? N1 Ni1 P1 87.06(8) . . ? P2 Ni1 P1 173.77(3) . . ? N1 Ni1 H1 172.3(13) . . ? P2 Ni1 H1 91.0(13) . . ? P1 Ni1 H1 94.7(13) . . ? C7 P1 C8 108.43(13) . . ? C7 P1 C14 105.71(14) . . ? C8 P1 C14 104.61(14) . . ? C7 P1 Ni1 99.34(10) . . ? C8 P1 Ni1 116.24(10) . . ? C14 P1 Ni1 121.38(11) . . ? C26 P2 C27 107.12(14) . . ? C26 P2 C30 107.19(14) . . ? C27 P2 C30 106.54(14) . . ? C26 P2 Ni1 99.62(10) . . ? C27 P2 Ni1 120.74(11) . . ? C30 P2 Ni1 114.48(11) . . ? C1 N1 C20 123.2(2) . . ? C1 N1 Ni1 118.41(19) . . ? C20 N1 Ni1 118.42(19) . . ? N1 C1 C2 126.6(3) . . ? N1 C1 C7 117.1(2) . . ? C2 C1 C7 116.1(3) . . ? C3 C2 C1 121.4(3) . . ? C3 C2 H2A 119.3 . . ? C1 C2 H2A 119.3 . . ? C2 C3 C4 122.9(3) . . ? C2 C3 H3A 118.6 . . ? C4 C3 H3A 118.6 . . ? C3 C4 C6 116.5(3) . . ? C3 C4 C5 121.8(3) . . ? C6 C4 C5 121.7(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C4 121.8(3) . . ? C7 C6 H6A 119.1 . . ? C4 C6 H6A 119.1 . . ? C6 C7 C1 121.3(3) . . ? C6 C7 P1 125.3(2) . . ? C1 C7 P1 113.2(2) . . ? C9 C8 C13 118.5(3) . . ? C9 C8 P1 122.8(2) . . ? C13 C8 P1 118.7(2) . . ? C10 C9 C8 120.4(3) . . ? C10 C9 H9A 119.8 . . ? C8 C9 H9A 119.8 . . ? C11 C10 C9 120.1(3) . . ? C11 C10 H10A 119.9 . . ? C9 C10 H10A 119.9 . . ? C12 C11 C10 120.3(3) . . ? C12 C11 H11A 119.9 . . ? C10 C11 H11A 119.9 . . ? C13 C12 C11 119.8(3) . . ? C13 C12 H12A 120.1 . . ? C11 C12 H12A 120.1 . . ? C12 C13 C8 120.9(3) . . ? C12 C13 H13A 119.5 . . ? C8 C13 H13A 119.5 . . ? C19 C14 C15 119.7(3) . . ? C19 C14 P1 123.9(3) . . ? C15 C14 P1 116.4(2) . . ? C16 C15 C14 120.1(4) . . ? C16 C15 H15A 119.9 . . ? C14 C15 H15A 119.9 . . ? C17 C16 C15 119.8(4) . . ? C17 C16 H16A 120.1 . . ? C15 C16 H16A 120.1 . . ? C18 C17 C16 120.7(4) . . ? C18 C17 H17A 119.7 . . ? C16 C17 H17A 119.7 . . ? C17 C18 C19 120.5(4) . . ? C17 C18 H18A 119.7 . . ? C19 C18 H18A 119.7 . . ? C14 C19 C18 119.1(4) . . ? C14 C19 H19A 120.4 . . ? C18 C19 H19A 120.4 . . ? N1 C20 C21 126.9(3) . . ? N1 C20 C26 116.9(2) . . ? C21 C20 C26 116.0(3) . . ? C22 C21 C20 121.8(3) . . ? C22 C21 H21A 119.1 . . ? C20 C21 H21A 119.1 . . ? C21 C22 C23 122.6(3) . . ? C21 C22 H22A 118.7 . . ? C23 C22 H22A 118.7 . . ? C22 C23 C25 116.7(3) . . ? C22 C23 C24 121.1(3) . . ? C25 C23 C24 122.3(3) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C23 122.1(3) . . ? C26 C25 H25A 118.9 . . ? C23 C25 H25A 118.9 . . ? C25 C26 C20 120.8(3) . . ? C25 C26 P2 125.8(2) . . ? C20 C26 P2 113.1(2) . . ? C29 C27 C28 110.9(3) . . ? C29 C27 P2 109.7(2) . . ? C28 C27 P2 109.8(2) . . ? C29 C27 H27A 108.8 . . ? C28 C27 H27A 108.8 . . ? P2 C27 H27A 108.8 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 C32 111.0(3) . . ? C31 C30 P2 114.8(2) . . ? C32 C30 P2 108.7(2) . . ? C31 C30 H30A 107.3 . . ? C32 C30 H30A 107.3 . . ? P2 C30 H30A 107.3 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ni1 P1 C7 -16.87(12) . . . . ? P2 Ni1 P1 C7 -1.0(4) . . . . ? N1 Ni1 P1 C8 99.13(13) . . . . ? P2 Ni1 P1 C8 115.0(3) . . . . ? N1 Ni1 P1 C14 -131.81(14) . . . . ? P2 Ni1 P1 C14 -115.9(3) . . . . ? N1 Ni1 P2 C26 -16.96(12) . . . . ? P1 Ni1 P2 C26 -32.8(4) . . . . ? N1 Ni1 P2 C27 -133.59(14) . . . . ? P1 Ni1 P2 C27 -149.5(3) . . . . ? N1 Ni1 P2 C30 97.02(14) . . . . ? P1 Ni1 P2 C30 81.1(4) . . . . ? P2 Ni1 N1 C1 -156.6(2) . . . . ? P1 Ni1 N1 C1 21.7(2) . . . . ? P2 Ni1 N1 C20 22.0(2) . . . . ? P1 Ni1 N1 C20 -159.7(2) . . . . ? C20 N1 C1 C2 -21.7(5) . . . . ? Ni1 N1 C1 C2 156.9(2) . . . . ? C20 N1 C1 C7 163.8(3) . . . . ? Ni1 N1 C1 C7 -17.7(3) . . . . ? N1 C1 C2 C3 -174.7(3) . . . . ? C7 C1 C2 C3 -0.1(4) . . . . ? C1 C2 C3 C4 -0.7(5) . . . . ? C2 C3 C4 C6 1.3(5) . . . . ? C2 C3 C4 C5 179.0(3) . . . . ? C3 C4 C6 C7 -1.2(4) . . . . ? C5 C4 C6 C7 -178.9(3) . . . . ? C4 C6 C7 C1 0.5(5) . . . . ? C4 C6 C7 P1 174.5(2) . . . . ? N1 C1 C7 C6 175.3(3) . . . . ? C2 C1 C7 C6 0.1(4) . . . . ? N1 C1 C7 P1 0.6(3) . . . . ? C2 C1 C7 P1 -174.5(2) . . . . ? C8 P1 C7 C6 77.0(3) . . . . ? C14 P1 C7 C6 -34.7(3) . . . . ? Ni1 P1 C7 C6 -161.1(2) . . . . ? C8 P1 C7 C1 -108.6(2) . . . . ? C14 P1 C7 C1 139.7(2) . . . . ? Ni1 P1 C7 C1 13.2(2) . . . . ? C7 P1 C8 C9 -23.5(3) . . . . ? C14 P1 C8 C9 88.9(3) . . . . ? Ni1 P1 C8 C9 -134.3(2) . . . . ? C7 P1 C8 C13 157.7(2) . . . . ? C14 P1 C8 C13 -89.8(3) . . . . ? Ni1 P1 C8 C13 46.9(3) . . . . ? C13 C8 C9 C10 0.6(5) . . . . ? P1 C8 C9 C10 -178.2(3) . . . . ? C8 C9 C10 C11 0.6(5) . . . . ? C9 C10 C11 C12 -1.4(6) . . . . ? C10 C11 C12 C13 0.9(6) . . . . ? C11 C12 C13 C8 0.4(5) . . . . ? C9 C8 C13 C12 -1.1(5) . . . . ? P1 C8 C13 C12 177.7(3) . . . . ? C7 P1 C14 C19 96.0(3) . . . . ? C8 P1 C14 C19 -18.4(3) . . . . ? Ni1 P1 C14 C19 -152.3(3) . . . . ? C7 P1 C14 C15 -84.5(3) . . . . ? C8 P1 C14 C15 161.2(2) . . . . ? Ni1 P1 C14 C15 27.2(3) . . . . ? C19 C14 C15 C16 -2.6(5) . . . . ? P1 C14 C15 C16 177.8(3) . . . . ? C14 C15 C16 C17 0.9(6) . . . . ? C15 C16 C17 C18 1.3(7) . . . . ? C16 C17 C18 C19 -1.8(7) . . . . ? C15 C14 C19 C18 2.2(5) . . . . ? P1 C14 C19 C18 -178.3(3) . . . . ? C17 C18 C19 C14 0.0(6) . . . . ? C1 N1 C20 C21 -24.7(5) . . . . ? Ni1 N1 C20 C21 156.8(3) . . . . ? C1 N1 C20 C26 160.3(3) . . . . ? Ni1 N1 C20 C26 -18.2(3) . . . . ? N1 C20 C21 C22 -174.0(3) . . . . ? C26 C20 C21 C22 1.0(4) . . . . ? C20 C21 C22 C23 -1.6(5) . . . . ? C21 C22 C23 C25 1.1(5) . . . . ? C21 C22 C23 C24 179.5(3) . . . . ? C22 C23 C25 C26 0.0(5) . . . . ? C24 C23 C25 C26 -178.4(3) . . . . ? C23 C25 C26 C20 -0.5(5) . . . . ? C23 C25 C26 P2 173.2(2) . . . . ? N1 C20 C26 C25 175.6(3) . . . . ? C21 C20 C26 C25 0.0(4) . . . . ? N1 C20 C26 P2 1.1(3) . . . . ? C21 C20 C26 P2 -174.5(2) . . . . ? C27 P2 C26 C25 -34.7(3) . . . . ? C30 P2 C26 C25 79.4(3) . . . . ? Ni1 P2 C26 C25 -161.1(3) . . . . ? C27 P2 C26 C20 139.5(2) . . . . ? C30 P2 C26 C20 -106.4(2) . . . . ? Ni1 P2 C26 C20 13.0(2) . . . . ? C26 P2 C27 C29 -62.6(3) . . . . ? C30 P2 C27 C29 -177.1(2) . . . . ? Ni1 P2 C27 C29 50.1(3) . . . . ? C26 P2 C27 C28 175.3(2) . . . . ? C30 P2 C27 C28 60.8(3) . . . . ? Ni1 P2 C27 C28 -72.0(3) . . . . ? C26 P2 C30 C31 -65.6(3) . . . . ? C27 P2 C30 C31 48.8(3) . . . . ? Ni1 P2 C30 C31 -175.0(2) . . . . ? C26 P2 C30 C32 59.4(3) . . . . ? C27 P2 C30 C32 173.8(3) . . . . ? Ni1 P2 C30 C32 -50.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 1.867 _refine_diff_density_min -0.430 _refine_diff_density_rms 0.080 # Attachment 'Compound 10.cif' data_rkrl27t _database_code_depnum_ccdc_archive 'CCDC 812755' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40.50 H45 N P2 Pd' _chemical_formula_weight 714.12 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3866(5) _cell_length_b 11.4791(5) _cell_length_c 14.9377(7) _cell_angle_alpha 91.051(2) _cell_angle_beta 108.575(2) _cell_angle_gamma 94.265(2) _cell_volume 1843.81(14) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 9975 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 32.42 _exptl_crystal_description chip _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.286 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 742 _exptl_absorpt_coefficient_mu 0.618 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8594 _exptl_absorpt_correction_T_max 0.9586 _exptl_absorpt_process_details 'Bruker, SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 41162 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 29.57 _reflns_number_total 10335 _reflns_number_gt 9148 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics '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^)+(0.0635P)^2^+0.7974P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10335 _refine_ls_number_parameters 392 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.1162 _refine_ls_wR_factor_gt 0.1020 _refine_ls_goodness_of_fit_ref 1.162 _refine_ls_restrained_S_all 1.164 _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 Pd1 Pd 0.918683(15) 0.283987(14) 0.226836(11) 0.02034(6) Uani 1 1 d D . . N1 N 0.74116(18) 0.27386(17) 0.23932(14) 0.0231(4) Uani 1 1 d . . . P1 P 0.89726(5) 0.47893(5) 0.22747(4) 0.02129(12) Uani 1 1 d . . . P2 P 0.88555(5) 0.08682(5) 0.21297(4) 0.01873(11) Uani 1 1 d . . . C1 C 0.6693(2) 0.36669(19) 0.20765(16) 0.0220(4) Uani 1 1 d . . . C2 C 0.5379(2) 0.3610(2) 0.17986(19) 0.0288(5) Uani 1 1 d . . . H2A H 0.4929 0.2910 0.1877 0.035 Uiso 1 1 calc R . . C3 C 0.4737(2) 0.4558(2) 0.1415(2) 0.0331(5) Uani 1 1 d . . . H3A H 0.3855 0.4484 0.1236 0.040 Uiso 1 1 calc R . . C4 C 0.5329(2) 0.5608(2) 0.12809(19) 0.0310(5) Uani 1 1 d . . . C5 C 0.4604(3) 0.6610(3) 0.0823(2) 0.0432(7) Uani 1 1 d . . . H5A H 0.3712 0.6394 0.0681 0.065 Uiso 1 1 calc R . . H5B H 0.4779 0.6784 0.0236 0.065 Uiso 1 1 calc R . . H5C H 0.4850 0.7302 0.1256 0.065 Uiso 1 1 calc R . . C6 C 0.6627(2) 0.5679(2) 0.15589(18) 0.0276(5) Uani 1 1 d . . . H6A H 0.7064 0.6388 0.1483 0.033 Uiso 1 1 calc R . . C7 C 0.7298(2) 0.4741(2) 0.19444(16) 0.0230(4) Uani 1 1 d . . . C8 C 0.9590(2) 0.5640(2) 0.33906(16) 0.0254(4) Uani 1 1 d . . . C9 C 1.0748(3) 0.5430(3) 0.40125(19) 0.0350(6) Uani 1 1 d . . . H9A H 1.1208 0.4848 0.3853 0.042 Uiso 1 1 calc R . . C10 C 1.1233(3) 0.6071(3) 0.4869(2) 0.0427(7) Uani 1 1 d . . . H10A H 1.2032 0.5938 0.5286 0.051 Uiso 1 1 calc R . . C11 C 1.0560(3) 0.6897(3) 0.5114(2) 0.0432(7) Uani 1 1 d . . . H11A H 1.0888 0.7325 0.5703 0.052 Uiso 1 1 calc R . . C12 C 0.9410(3) 0.7103(3) 0.4504(2) 0.0462(7) Uani 1 1 d . . . H12A H 0.8946 0.7674 0.4673 0.055 Uiso 1 1 calc R . . C13 C 0.8923(3) 0.6476(2) 0.3641(2) 0.0370(6) Uani 1 1 d . . . H13A H 0.8130 0.6624 0.3223 0.044 Uiso 1 1 calc R . . C14 C 0.9416(2) 0.5691(2) 0.14267(17) 0.0244(4) Uani 1 1 d . . . C15 C 1.0517(3) 0.6416(2) 0.1713(2) 0.0347(6) Uani 1 1 d . . . H15A H 1.1000 0.6501 0.2363 0.042 Uiso 1 1 calc R . . C16 C 1.0909(3) 0.7016(3) 0.1044(2) 0.0424(7) Uani 1 1 d . . . H16A H 1.1661 0.7511 0.1240 0.051 Uiso 1 1 calc R . . C17 C 1.0216(3) 0.6900(2) 0.0103(2) 0.0391(6) Uani 1 1 d . . . H17A H 1.0488 0.7314 -0.0350 0.047 Uiso 1 1 calc R . . C18 C 0.9122(3) 0.6178(3) -0.0186(2) 0.0359(6) Uani 1 1 d . . . H18A H 0.8640 0.6101 -0.0836 0.043 Uiso 1 1 calc R . . C19 C 0.8730(2) 0.5568(2) 0.04705(18) 0.0299(5) Uani 1 1 d . . . H19A H 0.7987 0.5062 0.0268 0.036 Uiso 1 1 calc R . . C20 C 0.69788(19) 0.16974(19) 0.26824(15) 0.0209(4) Uani 1 1 d . . . C21 C 0.6060(2) 0.1581(2) 0.31296(17) 0.0266(5) Uani 1 1 d . . . H21A H 0.5695 0.2257 0.3256 0.032 Uiso 1 1 calc R . . C22 C 0.5678(2) 0.0505(2) 0.33871(17) 0.0285(5) Uani 1 1 d . . . H22A H 0.5046 0.0463 0.3677 0.034 Uiso 1 1 calc R . . C23 C 0.6184(2) -0.0518(2) 0.32381(17) 0.0279(5) Uani 1 1 d . . . C24 C 0.5749(3) -0.1687(3) 0.3518(2) 0.0428(7) Uani 1 1 d . . . H24A H 0.6209 -0.2298 0.3350 0.064 Uiso 1 1 calc R . . H24B H 0.4858 -0.1857 0.3183 0.064 Uiso 1 1 calc R . . H24C H 0.5896 -0.1667 0.4201 0.064 Uiso 1 1 calc R . . C25 C 0.7146(2) -0.0411(2) 0.28518(17) 0.0254(4) Uani 1 1 d . . . H25A H 0.7535 -0.1089 0.2765 0.030 Uiso 1 1 calc R . . C26 C 0.7559(2) 0.06674(19) 0.25866(15) 0.0210(4) Uani 1 1 d . . . C27 C 1.0063(2) -0.00403(19) 0.28086(15) 0.0211(4) Uani 1 1 d . . . H27A H 0.9695 -0.0863 0.2786 0.025 Uiso 1 1 calc R . . C28 C 1.1132(2) -0.0018(2) 0.23931(17) 0.0285(5) Uani 1 1 d . . . H28A H 1.1429 0.0803 0.2344 0.034 Uiso 1 1 calc R . . H28B H 1.0825 -0.0389 0.1748 0.034 Uiso 1 1 calc R . . C29 C 1.2217(3) -0.0665(3) 0.30062(19) 0.0355(6) Uani 1 1 d . . . H29A H 1.1944 -0.1505 0.3001 0.043 Uiso 1 1 calc R . . H29B H 1.2908 -0.0597 0.2737 0.043 Uiso 1 1 calc R . . C30 C 1.2677(2) -0.0164(3) 0.40206(19) 0.0346(6) Uani 1 1 d . . . H30A H 1.3352 -0.0617 0.4406 0.042 Uiso 1 1 calc R . . H30B H 1.3018 0.0657 0.4034 0.042 Uiso 1 1 calc R . . C31 C 1.1619(2) -0.0214(3) 0.44382(18) 0.0363(6) Uani 1 1 d . . . H31A H 1.1927 0.0136 0.5090 0.044 Uiso 1 1 calc R . . H31B H 1.1323 -0.1041 0.4470 0.044 Uiso 1 1 calc R . . C32 C 1.0538(2) 0.0442(2) 0.38416(16) 0.0286(5) Uani 1 1 d . . . H32A H 1.0815 0.1283 0.3859 0.034 Uiso 1 1 calc R . . H32B H 0.9851 0.0368 0.4114 0.034 Uiso 1 1 calc R . . C33 C 0.8286(2) 0.02609(19) 0.09036(16) 0.0215(4) Uani 1 1 d . . . H33A H 0.8982 0.0390 0.0634 0.026 Uiso 1 1 calc R . . C34 C 0.7216(2) 0.0957(2) 0.03222(17) 0.0260(5) Uani 1 1 d . . . H34A H 0.6520 0.0870 0.0585 0.031 Uiso 1 1 calc R . . H34B H 0.7507 0.1797 0.0368 0.031 Uiso 1 1 calc R . . C35 C 0.6760(3) 0.0525(2) -0.07141(18) 0.0346(6) Uani 1 1 d . . . H35A H 0.6044 0.0956 -0.1065 0.042 Uiso 1 1 calc R . . H35B H 0.7431 0.0690 -0.0994 0.042 Uiso 1 1 calc R . . C36 C 0.6370(3) -0.0776(2) -0.0821(2) 0.0379(6) Uani 1 1 d . . . H36A H 0.6127 -0.1033 -0.1496 0.046 Uiso 1 1 calc R . . H36B H 0.5637 -0.0932 -0.0607 0.046 Uiso 1 1 calc R . . C37 C 0.7415(3) -0.1472(2) -0.02490(19) 0.0356(6) Uani 1 1 d . . . H37A H 0.8111 -0.1391 -0.0512 0.043 Uiso 1 1 calc R . . H37B H 0.7115 -0.2310 -0.0299 0.043 Uiso 1 1 calc R . . C38 C 0.7884(2) -0.1051(2) 0.07950(18) 0.0290(5) Uani 1 1 d . . . H38A H 0.7215 -0.1214 0.1078 0.035 Uiso 1 1 calc R . . H38B H 0.8597 -0.1488 0.1140 0.035 Uiso 1 1 calc R . . C39 C 0.5000 0.5000 0.5000 0.34(2) Uiso 1 2 d S . . C40 C 0.439(2) 0.450(2) 0.4337(19) 0.319(10) Uiso 1 1 d . . . C41 C 0.3550(16) 0.3696(14) 0.3623(12) 0.244(7) Uiso 1 1 d . . . H1 H 1.052(3) 0.292(3) 0.218(2) 0.044(9) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01908(9) 0.01862(9) 0.02185(10) 0.00039(6) 0.00450(6) 0.00184(6) N1 0.0196(9) 0.0206(9) 0.0280(10) 0.0008(7) 0.0057(7) 0.0028(7) P1 0.0209(3) 0.0179(3) 0.0231(3) -0.0001(2) 0.0044(2) 0.0007(2) P2 0.0178(2) 0.0185(2) 0.0188(3) 0.00081(19) 0.00414(19) 0.00276(19) C1 0.0199(10) 0.0216(10) 0.0222(10) -0.0017(8) 0.0035(8) 0.0027(8) C2 0.0204(10) 0.0252(11) 0.0360(13) 0.0027(9) 0.0023(9) 0.0010(9) C3 0.0206(11) 0.0337(13) 0.0400(14) 0.0033(10) 0.0014(10) 0.0079(10) C4 0.0290(12) 0.0274(12) 0.0343(13) 0.0027(10) 0.0053(10) 0.0092(10) C5 0.0357(14) 0.0340(14) 0.0565(19) 0.0112(13) 0.0066(13) 0.0154(12) C6 0.0288(12) 0.0219(11) 0.0302(12) 0.0014(9) 0.0065(9) 0.0047(9) C7 0.0204(10) 0.0227(10) 0.0240(11) -0.0011(8) 0.0043(8) 0.0027(8) C8 0.0284(11) 0.0221(10) 0.0230(11) 0.0007(8) 0.0053(9) -0.0025(9) C9 0.0295(12) 0.0394(15) 0.0310(13) 0.0003(11) 0.0033(10) 0.0002(11) C10 0.0391(15) 0.0468(17) 0.0295(14) 0.0025(12) -0.0042(11) -0.0072(13) C11 0.0599(19) 0.0387(15) 0.0231(13) -0.0035(11) 0.0054(12) -0.0088(14) C12 0.062(2) 0.0391(16) 0.0327(15) -0.0097(12) 0.0093(14) 0.0075(14) C13 0.0424(15) 0.0324(13) 0.0303(13) -0.0054(10) 0.0030(11) 0.0067(11) C14 0.0269(11) 0.0198(10) 0.0274(11) 0.0011(8) 0.0100(9) 0.0027(8) C15 0.0390(14) 0.0304(13) 0.0334(13) -0.0026(10) 0.0125(11) -0.0076(11) C16 0.0506(17) 0.0331(14) 0.0472(17) -0.0006(12) 0.0238(14) -0.0098(13) C17 0.0543(17) 0.0306(13) 0.0423(16) 0.0098(11) 0.0283(14) 0.0070(12) C18 0.0426(15) 0.0394(15) 0.0301(13) 0.0084(11) 0.0151(11) 0.0143(12) C19 0.0297(12) 0.0307(12) 0.0295(12) 0.0032(9) 0.0087(10) 0.0062(10) C20 0.0163(9) 0.0233(10) 0.0202(10) 0.0001(8) 0.0019(7) 0.0019(8) C21 0.0203(10) 0.0331(12) 0.0258(11) 0.0008(9) 0.0059(9) 0.0058(9) C22 0.0177(10) 0.0430(14) 0.0246(11) 0.0060(10) 0.0066(8) 0.0010(9) C23 0.0216(10) 0.0326(12) 0.0263(11) 0.0080(9) 0.0039(9) -0.0021(9) C24 0.0381(15) 0.0401(16) 0.0529(18) 0.0149(13) 0.0191(13) -0.0022(12) C25 0.0248(11) 0.0249(11) 0.0257(11) 0.0046(8) 0.0066(9) 0.0030(9) C26 0.0186(9) 0.0234(10) 0.0197(10) 0.0017(8) 0.0041(8) 0.0024(8) C27 0.0186(9) 0.0217(10) 0.0203(10) 0.0010(8) 0.0022(8) 0.0036(8) C28 0.0240(11) 0.0409(14) 0.0203(11) -0.0009(9) 0.0049(9) 0.0108(10) C29 0.0269(12) 0.0469(16) 0.0300(13) -0.0023(11) 0.0024(10) 0.0167(11) C30 0.0195(11) 0.0524(17) 0.0277(12) 0.0000(11) 0.0009(9) 0.0055(10) C31 0.0247(12) 0.0600(18) 0.0216(12) 0.0092(11) 0.0024(9) 0.0082(12) C32 0.0235(11) 0.0422(14) 0.0199(11) 0.0004(9) 0.0059(9) 0.0069(10) C33 0.0210(10) 0.0212(10) 0.0204(10) 0.0002(8) 0.0039(8) 0.0037(8) C34 0.0270(11) 0.0232(11) 0.0236(11) 0.0009(8) 0.0009(9) 0.0077(9) C35 0.0429(15) 0.0274(12) 0.0242(12) 0.0004(9) -0.0032(10) 0.0077(11) C36 0.0387(14) 0.0296(13) 0.0312(13) -0.0029(10) -0.0083(11) 0.0013(11) C37 0.0420(15) 0.0232(12) 0.0316(13) -0.0053(9) -0.0028(11) 0.0058(10) C38 0.0336(12) 0.0198(10) 0.0270(12) 0.0004(8) 0.0001(9) 0.0041(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.0833(19) . ? Pd1 P2 2.2614(6) . ? Pd1 P1 2.2692(6) . ? Pd1 H1 1.55(3) . ? N1 C20 1.387(3) . ? N1 C1 1.390(3) . ? P1 C7 1.808(2) . ? P1 C14 1.819(2) . ? P1 C8 1.822(2) . ? P2 C26 1.816(2) . ? P2 C27 1.836(2) . ? P2 C33 1.841(2) . ? C1 C7 1.415(3) . ? C1 C2 1.415(3) . ? C2 C3 1.386(3) . ? C2 H2A 0.9500 . ? C3 C4 1.386(4) . ? C3 H3A 0.9500 . ? C4 C6 1.398(4) . ? C4 C5 1.511(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.393(3) . ? C6 H6A 0.9500 . ? C8 C13 1.383(4) . ? C8 C9 1.391(4) . ? C9 C10 1.393(4) . ? C9 H9A 0.9500 . ? C10 C11 1.377(5) . ? C10 H10A 0.9500 . ? C11 C12 1.376(5) . ? C11 H11A 0.9500 . ? C12 C13 1.392(4) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C19 1.391(3) . ? C14 C15 1.393(4) . ? C15 C16 1.391(4) . ? C15 H15A 0.9500 . ? C16 C17 1.374(5) . ? C16 H16A 0.9500 . ? C17 C18 1.384(4) . ? C17 H17A 0.9500 . ? C18 C19 1.381(4) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 C21 1.410(3) . ? C20 C26 1.423(3) . ? C21 C22 1.380(4) . ? C21 H21A 0.9500 . ? C22 C23 1.390(4) . ? C22 H22A 0.9500 . ? C23 C25 1.390(3) . ? C23 C24 1.509(4) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.400(3) . ? C25 H25A 0.9500 . ? C27 C28 1.531(3) . ? C27 C32 1.540(3) . ? C27 H27A 1.0000 . ? C28 C29 1.535(3) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.523(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.521(4) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.530(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C38 1.531(3) . ? C33 C34 1.541(3) . ? C33 H33A 1.0000 . ? C34 C35 1.527(3) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.517(4) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.518(4) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.534(4) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.13(3) . ? C39 C40 1.13(3) 2_666 ? C40 C41 1.44(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 N1 Pd1 P2 83.42(5) . . ? N1 Pd1 P1 82.93(5) . . ? P2 Pd1 P1 165.11(2) . . ? N1 Pd1 H1 179.5(13) . . ? P2 Pd1 H1 96.8(13) . . ? P1 Pd1 H1 96.9(13) . . ? C20 N1 C1 124.38(19) . . ? C20 N1 Pd1 117.72(14) . . ? C1 N1 Pd1 117.46(15) . . ? C7 P1 C14 106.42(11) . . ? C7 P1 C8 106.63(11) . . ? C14 P1 C8 104.51(11) . . ? C7 P1 Pd1 98.97(8) . . ? C14 P1 Pd1 120.05(8) . . ? C8 P1 Pd1 118.77(8) . . ? C26 P2 C27 107.33(10) . . ? C26 P2 C33 106.32(10) . . ? C27 P2 C33 107.40(10) . . ? C26 P2 Pd1 99.74(7) . . ? C27 P2 Pd1 120.14(7) . . ? C33 P2 Pd1 114.57(7) . . ? N1 C1 C7 118.2(2) . . ? N1 C1 C2 125.4(2) . . ? C7 C1 C2 116.1(2) . . ? C3 C2 C1 121.2(2) . . ? C3 C2 H2A 119.4 . . ? C1 C2 H2A 119.4 . . ? C2 C3 C4 122.7(2) . . ? C2 C3 H3A 118.7 . . ? C4 C3 H3A 118.7 . . ? C3 C4 C6 116.7(2) . . ? C3 C4 C5 121.6(2) . . ? C6 C4 C5 121.6(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C4 121.9(2) . . ? C7 C6 H6A 119.1 . . ? C4 C6 H6A 119.1 . . ? C6 C7 C1 121.4(2) . . ? C6 C7 P1 122.94(19) . . ? C1 C7 P1 115.68(16) . . ? C13 C8 C9 119.2(2) . . ? C13 C8 P1 121.48(19) . . ? C9 C8 P1 119.3(2) . . ? C8 C9 C10 120.0(3) . . ? C8 C9 H9A 120.0 . . ? C10 C9 H9A 120.0 . . ? C11 C10 C9 120.3(3) . . ? C11 C10 H10A 119.9 . . ? C9 C10 H10A 119.9 . . ? C12 C11 C10 119.9(3) . . ? C12 C11 H11A 120.1 . . ? C10 C11 H11A 120.1 . . ? C11 C12 C13 120.3(3) . . ? C11 C12 H12A 119.9 . . ? C13 C12 H12A 119.9 . . ? C8 C13 C12 120.3(3) . . ? C8 C13 H13A 119.8 . . ? C12 C13 H13A 119.8 . . ? C19 C14 C15 119.2(2) . . ? C19 C14 P1 120.22(19) . . ? C15 C14 P1 120.19(19) . . ? C16 C15 C14 119.8(3) . . ? C16 C15 H15A 120.1 . . ? C14 C15 H15A 120.1 . . ? C17 C16 C15 120.5(3) . . ? C17 C16 H16A 119.8 . . ? C15 C16 H16A 119.8 . . ? C16 C17 C18 120.0(3) . . ? C16 C17 H17A 120.0 . . ? C18 C17 H17A 120.0 . . ? C19 C18 C17 120.1(3) . . ? C19 C18 H18A 120.0 . . ? C17 C18 H18A 120.0 . . ? C18 C19 C14 120.4(3) . . ? C18 C19 H19A 119.8 . . ? C14 C19 H19A 119.8 . . ? N1 C20 C21 125.3(2) . . ? N1 C20 C26 118.2(2) . . ? C21 C20 C26 116.3(2) . . ? C22 C21 C20 121.4(2) . . ? C22 C21 H21A 119.3 . . ? C20 C21 H21A 119.3 . . ? C21 C22 C23 122.5(2) . . ? C21 C22 H22A 118.7 . . ? C23 C22 H22A 118.7 . . ? C22 C23 C25 117.0(2) . . ? C22 C23 C24 121.8(2) . . ? C25 C23 C24 121.2(2) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 C26 121.9(2) . . ? C23 C25 H25A 119.1 . . ? C26 C25 H25A 119.1 . . ? C25 C26 C20 120.7(2) . . ? C25 C26 P2 123.71(17) . . ? C20 C26 P2 115.57(17) . . ? C28 C27 C32 110.39(19) . . ? C28 C27 P2 110.30(16) . . ? C32 C27 P2 108.24(15) . . ? C28 C27 H27A 109.3 . . ? C32 C27 H27A 109.3 . . ? P2 C27 H27A 109.3 . . ? C27 C28 C29 111.5(2) . . ? C27 C28 H28A 109.3 . . ? C29 C28 H28A 109.3 . . ? C27 C28 H28B 109.3 . . ? C29 C28 H28B 109.3 . . ? H28A C28 H28B 108.0 . . ? C30 C29 C28 111.2(2) . . ? C30 C29 H29A 109.4 . . ? C28 C29 H29A 109.4 . . ? C30 C29 H29B 109.4 . . ? C28 C29 H29B 109.4 . . ? H29A C29 H29B 108.0 . . ? C31 C30 C29 110.4(2) . . ? C31 C30 H30A 109.6 . . ? C29 C30 H30A 109.6 . . ? C31 C30 H30B 109.6 . . ? C29 C30 H30B 109.6 . . ? H30A C30 H30B 108.1 . . ? C30 C31 C32 111.1(2) . . ? C30 C31 H31A 109.4 . . ? C32 C31 H31A 109.4 . . ? C30 C31 H31B 109.4 . . ? C32 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? C31 C32 C27 111.3(2) . . ? C31 C32 H32A 109.4 . . ? C27 C32 H32A 109.4 . . ? C31 C32 H32B 109.4 . . ? C27 C32 H32B 109.4 . . ? H32A C32 H32B 108.0 . . ? C38 C33 C34 110.46(19) . . ? C38 C33 P2 115.06(16) . . ? C34 C33 P2 109.01(15) . . ? C38 C33 H33A 107.3 . . ? C34 C33 H33A 107.3 . . ? P2 C33 H33A 107.3 . . ? C35 C34 C33 110.86(19) . . ? C35 C34 H34A 109.5 . . ? C33 C34 H34A 109.5 . . ? C35 C34 H34B 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? C36 C35 C34 111.7(2) . . ? C36 C35 H35A 109.3 . . ? C34 C35 H35A 109.3 . . ? C36 C35 H35B 109.3 . . ? C34 C35 H35B 109.3 . . ? H35A C35 H35B 107.9 . . ? C35 C36 C37 111.3(2) . . ? C35 C36 H36A 109.4 . . ? C37 C36 H36A 109.4 . . ? C35 C36 H36B 109.4 . . ? C37 C36 H36B 109.4 . . ? H36A C36 H36B 108.0 . . ? C36 C37 C38 111.4(2) . . ? C36 C37 H37A 109.3 . . ? C38 C37 H37A 109.3 . . ? C36 C37 H37B 109.3 . . ? C38 C37 H37B 109.3 . . ? H37A C37 H37B 108.0 . . ? C33 C38 C37 111.2(2) . . ? C33 C38 H38A 109.4 . . ? C37 C38 H38A 109.4 . . ? C33 C38 H38B 109.4 . . ? C37 C38 H38B 109.4 . . ? H38A C38 H38B 108.0 . . ? C40 C39 C40 180(2) . 2_666 ? C39 C40 C41 168(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 P2 Pd1 N1 C20 22.43(15) . . . . ? P1 Pd1 N1 C20 -163.54(16) . . . . ? P2 Pd1 N1 C1 -150.27(16) . . . . ? P1 Pd1 N1 C1 23.76(15) . . . . ? N1 Pd1 P1 C7 -20.07(10) . . . . ? P2 Pd1 P1 C7 3.62(12) . . . . ? N1 Pd1 P1 C14 -135.03(11) . . . . ? P2 Pd1 P1 C14 -111.33(12) . . . . ? N1 Pd1 P1 C8 94.58(11) . . . . ? P2 Pd1 P1 C8 118.28(12) . . . . ? N1 Pd1 P2 C26 -16.68(9) . . . . ? P1 Pd1 P2 C26 -40.35(12) . . . . ? N1 Pd1 P2 C27 -133.37(10) . . . . ? P1 Pd1 P2 C27 -157.04(11) . . . . ? N1 Pd1 P2 C33 96.40(10) . . . . ? P1 Pd1 P2 C33 72.73(12) . . . . ? C20 N1 C1 C7 170.3(2) . . . . ? Pd1 N1 C1 C7 -17.6(3) . . . . ? C20 N1 C1 C2 -15.1(4) . . . . ? Pd1 N1 C1 C2 157.1(2) . . . . ? N1 C1 C2 C3 -174.3(2) . . . . ? C7 C1 C2 C3 0.4(4) . . . . ? C1 C2 C3 C4 -0.1(4) . . . . ? C2 C3 C4 C6 -0.4(4) . . . . ? C2 C3 C4 C5 177.4(3) . . . . ? C3 C4 C6 C7 0.6(4) . . . . ? C5 C4 C6 C7 -177.2(3) . . . . ? C4 C6 C7 C1 -0.3(4) . . . . ? C4 C6 C7 P1 177.9(2) . . . . ? N1 C1 C7 C6 174.9(2) . . . . ? C2 C1 C7 C6 -0.2(3) . . . . ? N1 C1 C7 P1 -3.4(3) . . . . ? C2 C1 C7 P1 -178.51(18) . . . . ? C14 P1 C7 C6 -34.2(2) . . . . ? C8 P1 C7 C6 76.9(2) . . . . ? Pd1 P1 C7 C6 -159.32(19) . . . . ? C14 P1 C7 C1 144.03(17) . . . . ? C8 P1 C7 C1 -104.83(18) . . . . ? Pd1 P1 C7 C1 18.93(18) . . . . ? C7 P1 C8 C13 -26.2(3) . . . . ? C14 P1 C8 C13 86.3(2) . . . . ? Pd1 P1 C8 C13 -136.7(2) . . . . ? C7 P1 C8 C9 152.6(2) . . . . ? C14 P1 C8 C9 -94.9(2) . . . . ? Pd1 P1 C8 C9 42.1(2) . . . . ? C13 C8 C9 C10 -1.1(4) . . . . ? P1 C8 C9 C10 -179.9(2) . . . . ? C8 C9 C10 C11 1.4(5) . . . . ? C9 C10 C11 C12 -1.0(5) . . . . ? C10 C11 C12 C13 0.2(5) . . . . ? C9 C8 C13 C12 0.3(4) . . . . ? P1 C8 C13 C12 179.1(2) . . . . ? C11 C12 C13 C8 0.2(5) . . . . ? C7 P1 C14 C19 -42.2(2) . . . . ? C8 P1 C14 C19 -154.8(2) . . . . ? Pd1 P1 C14 C19 68.8(2) . . . . ? C7 P1 C14 C15 144.7(2) . . . . ? C8 P1 C14 C15 32.1(2) . . . . ? Pd1 P1 C14 C15 -104.3(2) . . . . ? C19 C14 C15 C16 0.7(4) . . . . ? P1 C14 C15 C16 173.8(2) . . . . ? C14 C15 C16 C17 0.1(5) . . . . ? C15 C16 C17 C18 -0.2(5) . . . . ? C16 C17 C18 C19 -0.5(4) . . . . ? C17 C18 C19 C14 1.2(4) . . . . ? C15 C14 C19 C18 -1.3(4) . . . . ? P1 C14 C19 C18 -174.5(2) . . . . ? C1 N1 C20 C21 -32.3(3) . . . . ? Pd1 N1 C20 C21 155.54(18) . . . . ? C1 N1 C20 C26 152.4(2) . . . . ? Pd1 N1 C20 C26 -19.7(3) . . . . ? N1 C20 C21 C22 179.5(2) . . . . ? C26 C20 C21 C22 -5.1(3) . . . . ? C20 C21 C22 C23 1.1(4) . . . . ? C21 C22 C23 C25 2.9(4) . . . . ? C21 C22 C23 C24 -179.5(2) . . . . ? C22 C23 C25 C26 -2.6(4) . . . . ? C24 C23 C25 C26 179.8(2) . . . . ? C23 C25 C26 C20 -1.6(4) . . . . ? C23 C25 C26 P2 177.08(18) . . . . ? N1 C20 C26 C25 -178.9(2) . . . . ? C21 C20 C26 C25 5.4(3) . . . . ? N1 C20 C26 P2 2.3(3) . . . . ? C21 C20 C26 P2 -173.42(16) . . . . ? C27 P2 C26 C25 -39.7(2) . . . . ? C33 P2 C26 C25 75.0(2) . . . . ? Pd1 P2 C26 C25 -165.62(18) . . . . ? C27 P2 C26 C20 139.11(17) . . . . ? C33 P2 C26 C20 -106.19(17) . . . . ? Pd1 P2 C26 C20 13.15(17) . . . . ? C26 P2 C27 C28 173.96(16) . . . . ? C33 P2 C27 C28 59.98(18) . . . . ? Pd1 P2 C27 C28 -73.33(17) . . . . ? C26 P2 C27 C32 -65.18(18) . . . . ? C33 P2 C27 C32 -179.16(16) . . . . ? Pd1 P2 C27 C32 47.53(18) . . . . ? C32 C27 C28 C29 54.5(3) . . . . ? P2 C27 C28 C29 174.05(18) . . . . ? C27 C28 C29 C30 -56.0(3) . . . . ? C28 C29 C30 C31 56.9(3) . . . . ? C29 C30 C31 C32 -57.3(3) . . . . ? C30 C31 C32 C27 56.7(3) . . . . ? C28 C27 C32 C31 -54.9(3) . . . . ? P2 C27 C32 C31 -175.68(18) . . . . ? C26 P2 C33 C38 -62.61(19) . . . . ? C27 P2 C33 C38 52.0(2) . . . . ? Pd1 P2 C33 C38 -171.74(15) . . . . ? C26 P2 C33 C34 62.08(18) . . . . ? C27 P2 C33 C34 176.74(16) . . . . ? Pd1 P2 C33 C34 -47.05(18) . . . . ? C38 C33 C34 C35 -55.7(3) . . . . ? P2 C33 C34 C35 177.00(18) . . . . ? C33 C34 C35 C36 56.0(3) . . . . ? C34 C35 C36 C37 -55.7(3) . . . . ? C35 C36 C37 C38 55.3(4) . . . . ? C34 C33 C38 C37 55.5(3) . . . . ? P2 C33 C38 C37 179.49(18) . . . . ? C36 C37 C38 C33 -55.6(3) . . . . ? C40 C39 C40 C41 -60(43) 2_666 . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 29.57 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.456 _refine_diff_density_min -1.170 _refine_diff_density_rms 0.198